# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1775 data_1a _publ_contact_author_name 'Dr. Andrea Erxleben' _publ_contact_author_address ; Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_mail 'AERX@platon.chemie.uni-dortmund.de' _publ_contact_author_fax '+49(0)231-7553797' _publ_contact_author_phone '+49(0)231-7553845' _publ_contact_letter ? _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_title ; Di- and polynuclear Zn(II) Schiff base complexes: synthesis, structural studies and reaction with amino acid ester ; _publ_author_address ; Andrea Erxleben, Jolante Hermannn' Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Zn2(C17H27N4O)(CH3CO2)2]ClO4 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H33 Cl N4 O9 Zn2' _chemical_formula_weight 651.70 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7170(10) _cell_length_b 11.2850(10) _cell_length_c 15.0570(10) _cell_angle_alpha 99.370(10) _cell_angle_beta 94.00(3) _cell_angle_gamma 104.04(3) _cell_volume 1408.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4573 _cell_measurement_theta_min 4.56 _cell_measurement_theta_max 25.03 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.850 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.607 _exptl_absorpt_correction_T_max 0.655 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD ' _diffrn_measurement_method 'profile fitted ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4573 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4573 _reflns_number_observed 3164 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, The Netherlands)' _computing_cell_refinement 'Denzo, Scalepack (Z. Otwinowski, W. Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack (Z. Otwinowski, W. Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL PLUS' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'U(iso) = 1.2 x U(C(bonded)) ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4562 _refine_ls_number_parameters 350 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all 0.1581 _refine_ls_wR_factor_obs 0.1276 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_restrained_S_all 1.176 _refine_ls_restrained_S_obs 1.160 _refine_ls_shift/esd_max -0.154 _refine_ls_shift/esd_mean 0.016 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.12606(4) 0.39327(3) 0.17658(2) 0.04780(11) Uani 1 d . . Zn2 Zn 0.10648(4) 0.63963(3) 0.31431(2) 0.04678(10) Uani 1 d . . Cl1 Cl 0.3070(2) 0.90299(14) 0.74354(10) 0.1052(4) Uani 1 d D . C1 C 0.2279(3) 0.4299(3) 0.3826(2) 0.0476(9) Uani 1 d . . C2 C 0.2928(3) 0.3255(3) 0.3676(2) 0.0487(9) Uani 1 d . . C3 C 0.3619(4) 0.2876(3) 0.4421(2) 0.0577(10) Uani 1 d . . H3 H 0.4058(4) 0.2201(3) 0.4308(2) 0.069 Uiso 1 calc R . C4 C 0.3677(4) 0.3449(4) 0.5299(2) 0.0597(10) Uani 1 d . . C5 C 0.3058(4) 0.4452(4) 0.5438(2) 0.0595(10) Uani 1 d . . H5 H 0.3101(4) 0.4861(4) 0.6032(2) 0.071 Uiso 1 calc R . C6 C 0.2358(4) 0.4911(3) 0.4744(2) 0.0520(9) Uani 1 d . . C7 C 0.4443(4) 0.3003(4) 0.6084(3) 0.0871(13) Uani 1 d . . H7A H 0.4812(4) 0.2291(4) 0.5850(3) 0.105 Uiso 1 calc R . H7B H 0.3671(4) 0.2780(4) 0.6493(3) 0.105 Uiso 1 calc R . H7C H 0.5325(4) 0.3657(4) 0.6399(3) 0.105 Uiso 1 calc R . C8 C 0.2895(4) 0.2486(3) 0.2810(3) 0.0583(10) Uani 1 d . . H8 H 0.3402(4) 0.1849(3) 0.2807(3) 0.070 Uiso 1 calc R . C9 C 0.2250(5) 0.1616(4) 0.1260(3) 0.0834(13) Uani 1 d . . H9A H 0.1358(5) 0.0900(4) 0.1237(3) 0.100 Uiso 1 calc R . H9B H 0.3225(5) 0.1350(4) 0.1310(3) 0.100 Uiso 1 calc R . C10 C 0.2121(5) 0.2149(4) 0.0411(3) 0.0781(13) Uani 1 d . . H10A H 0.3108(5) 0.2756(4) 0.0382(3) 0.094 Uiso 1 calc R . H10B H 0.1949(5) 0.1491(4) -0.0116(3) 0.094 Uiso 1 calc R . C11 C 0.0930(6) 0.3482(5) -0.0319(4) 0.107(2) Uiso 1 d . . H11A H 0.1952(6) 0.4073(5) -0.0225(4) 0.129 Uiso 1 calc R . H11B H 0.0107(6) 0.3914(5) -0.0307(4) 0.129 Uiso 1 calc R . H11C H 0.0815(6) 0.2942(5) -0.0896(4) 0.129 Uiso 1 calc R . C12 C -0.0738(5) 0.1859(5) 0.0246(3) 0.100(2) Uani 1 d . . H12A H -0.1556(5) 0.2295(5) 0.0246(3) 0.119 Uiso 1 calc R . H12B H -0.0845(5) 0.1376(5) 0.0718(3) 0.119 Uiso 1 calc R . H12C H -0.0838(5) 0.1318(5) -0.0329(3) 0.119 Uiso 1 calc R . C13 C 0.1814(4) 0.5996(3) 0.5020(2) 0.0563(10) Uani 1 d . . H13 H 0.1840(4) 0.6255(3) 0.5641(2) 0.068 Uiso 1 calc R . C14 C 0.0828(5) 0.7777(4) 0.4949(3) 0.0745(12) Uani 1 d . . H14A H 0.0081(5) 0.7551(4) 0.5379(3) 0.089 Uiso 1 calc R . H14B H 0.1761(5) 0.8385(4) 0.5278(3) 0.089 Uiso 1 calc R . C15 C 0.0093(5) 0.8327(4) 0.4265(3) 0.0915(15) Uani 1 d . . H15A H -0.1000(5) 0.7847(4) 0.4081(3) 0.110 Uiso 1 calc R . H15B H 0.0079(5) 0.9168(4) 0.4528(3) 0.110 Uiso 1 calc R . C16 C 0.2557(6) 0.9202(6) 0.3707(4) 0.120(2) Uiso 1 d . . H16A H 0.3118(6) 0.9212(6) 0.3181(4) 0.144 Uiso 1 calc R . H16B H 0.3132(6) 0.8929(6) 0.4166(4) 0.144 Uiso 1 calc R . H16C H 0.2461(6) 1.0024(6) 0.3933(4) 0.144 Uiso 1 calc R . C17 C 0.0096(6) 0.8740(6) 0.2729(4) 0.121(2) Uiso 1 d . . H17A H -0.0943(6) 0.8177(6) 0.2571(4) 0.145 Uiso 1 calc R . H17B H 0.0671(6) 0.8728(6) 0.2209(4) 0.145 Uiso 1 calc R . H17C H -0.0007(6) 0.9566(6) 0.2933(4) 0.145 Uiso 1 calc R . C18 C 0.3225(4) 0.6385(3) 0.1658(2) 0.0529(9) Uani 1 d . . C19 C 0.4503(5) 0.7207(4) 0.1259(3) 0.0831(14) Uani 1 d . . H19A H 0.4615(5) 0.8059(4) 0.1530(3) 0.100 Uiso 1 calc R . H19B H 0.4223(5) 0.7094(4) 0.0617(3) 0.100 Uiso 1 calc R . H19C H 0.5491(5) 0.6995(4) 0.1373(3) 0.100 Uiso 1 calc R . C20 C -0.1707(4) 0.4787(3) 0.2014(2) 0.0538(9) Uani 1 d . . C21 C -0.3478(4) 0.4356(4) 0.1750(3) 0.0824(14) Uani 1 d . . H21A H -0.3997(4) 0.4860(4) 0.2137(3) 0.099 Uiso 1 calc R . H21B H -0.3852(4) 0.3503(4) 0.1812(3) 0.099 Uiso 1 calc R . H21C H -0.3716(4) 0.4428(4) 0.1132(3) 0.099 Uiso 1 calc R . N1 N 0.2248(3) 0.2576(3) 0.2041(2) 0.0578(8) Uani 1 d . . N2 N 0.0803(3) 0.2742(3) 0.0402(2) 0.0599(8) Uani 1 d . . N3 N 0.1299(3) 0.6650(3) 0.4517(2) 0.0556(8) Uani 1 d . . N4 N 0.0970(3) 0.8352(3) 0.3464(2) 0.0613(9) Uani 1 d . . O1 O 0.1648(2) 0.4697(2) 0.31509(14) 0.0479(6) Uani 1 d . . O2 O 0.2922(3) 0.5241(2) 0.1382(2) 0.0627(7) Uani 1 d . . O3 O 0.2513(3) 0.6904(2) 0.2248(2) 0.0602(6) Uiso 1 d . . O4 O -0.0863(3) 0.4220(2) 0.1571(2) 0.0603(7) Uani 1 d . . O5 O -0.1199(2) 0.5700(2) 0.2657(2) 0.0581(7) Uani 1 d . . O10 O 0.3273(9) 1.0038(6) 0.6923(5) 0.144(3) Uani 0.60 d PD . O11 O 0.3846(13) 0.9260(11) 0.8233(7) 0.230(5) Uiso 0.60 d PD . O12 O 0.1420(6) 0.8527(7) 0.7375(5) 0.135(3) Uani 0.60 d PD . O13 O 0.3607(8) 0.8079(8) 0.6891(7) 0.224(4) Uani 0.60 d PD . O20 O 0.2347(11) 0.9792(10) 0.7992(8) 0.163(5) Uani 0.40 d PD . O21 O 0.2189(17) 0.7889(9) 0.7239(7) 0.168(6) Uani 0.40 d PD . O22 O 0.4477(9) 0.9144(11) 0.8032(7) 0.183(4) Uani 0.40 d PD . O23 O 0.3698(13) 0.9492(11) 0.6732(7) 0.152(6) Uani 0.40 d PD . 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 0.0541(2) 0.0477(2) 0.0424(2) 0.0051(2) 0.0030(2) 0.0173(2) Zn2 0.0493(2) 0.0463(2) 0.0440(2) 0.0045(2) 0.00554(15) 0.01353(15) Cl1 0.1059(8) 0.1071(9) 0.0927(9) 0.0106(8) -0.0194(7) 0.0224(7) C1 0.044(2) 0.049(2) 0.047(2) 0.0162(15) 0.0017(13) 0.0029(13) C2 0.047(2) 0.049(2) 0.050(2) 0.0156(15) 0.0045(13) 0.0078(13) C3 0.044(2) 0.059(2) 0.072(2) 0.027(2) -0.0024(15) 0.0099(14) C4 0.044(2) 0.083(2) 0.053(2) 0.032(2) 0.0014(14) 0.006(2) C5 0.050(2) 0.083(2) 0.044(2) 0.020(2) 0.0030(14) 0.009(2) C6 0.053(2) 0.058(2) 0.044(2) 0.015(2) 0.0090(14) 0.0093(14) C7 0.062(2) 0.127(3) 0.084(3) 0.061(2) -0.005(2) 0.023(2) C8 0.057(2) 0.051(2) 0.072(2) 0.021(2) 0.005(2) 0.0174(14) C9 0.108(3) 0.071(2) 0.073(3) -0.012(2) -0.011(2) 0.050(2) C10 0.092(2) 0.080(3) 0.061(2) -0.007(2) 0.018(2) 0.031(2) C12 0.092(3) 0.093(3) 0.087(3) -0.025(3) -0.004(3) 0.005(3) C13 0.056(2) 0.069(2) 0.040(2) 0.007(2) 0.0086(14) 0.010(2) C14 0.101(3) 0.067(2) 0.052(2) -0.008(2) 0.019(2) 0.025(2) C15 0.111(3) 0.078(3) 0.094(3) 0.004(2) 0.032(3) 0.045(2) C18 0.056(2) 0.058(2) 0.049(2) 0.012(2) 0.0094(14) 0.0199(14) C19 0.082(2) 0.072(3) 0.091(3) 0.015(2) 0.036(2) 0.005(2) C20 0.049(2) 0.061(2) 0.052(2) 0.016(2) 0.0016(14) 0.0133(14) C21 0.051(2) 0.093(3) 0.094(3) 0.002(3) -0.011(2) 0.018(2) N1 0.069(2) 0.051(2) 0.055(2) 0.0049(14) 0.0018(14) 0.0232(12) N2 0.074(2) 0.060(2) 0.046(2) 0.0077(14) 0.0049(13) 0.0208(14) N3 0.0601(15) 0.057(2) 0.045(2) -0.0027(13) 0.0064(12) 0.0123(13) N4 0.065(2) 0.051(2) 0.068(2) 0.0081(14) 0.0147(14) 0.0159(13) O1 0.0559(11) 0.0502(12) 0.0390(11) 0.0092(10) -0.0012(9) 0.0176(9) O2 0.0686(13) 0.0557(14) 0.0625(15) 0.0062(12) 0.0183(11) 0.0139(11) O4 0.0544(12) 0.073(2) 0.0513(14) -0.0003(12) -0.0010(10) 0.0226(11) O5 0.0494(11) 0.0620(14) 0.0592(15) -0.0009(12) 0.0022(10) 0.0164(10) O10 0.185(6) 0.123(5) 0.150(6) 0.069(4) 0.031(5) 0.056(4) O12 0.081(3) 0.183(6) 0.155(6) 0.063(5) 0.033(3) 0.033(4) O13 0.150(4) 0.247(7) 0.250(10) -0.122(6) -0.060(5) 0.137(4) O20 0.143(7) 0.142(8) 0.231(13) 0.044(9) 0.075(8) 0.066(6) O21 0.274(15) 0.108(8) 0.094(7) 0.018(6) -0.033(9) 0.011(10) O22 0.159(5) 0.265(9) 0.134(8) -0.058(7) -0.084(5) 0.162(5) O23 0.132(8) 0.135(10) 0.150(10) -0.003(9) 0.037(7) -0.026(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 O4 1.966(2) . ? Zn1 O2 1.991(2) . ? Zn1 N1 2.013(3) . ? Zn1 O1 2.093(2) . ? Zn1 N2 2.216(3) . ? Zn2 O3 1.969(2) . ? Zn2 O5 1.976(2) . ? Zn2 N3 2.031(3) . ? Zn2 O1 2.101(2) . ? Zn2 N4 2.204(3) . ? Cl1 O21 1.304(10) . ? Cl1 O11 1.291(10) . ? Cl1 O23 1.347(10) . ? Cl1 O20 1.394(10) . ? Cl1 O12 1.403(5) . ? Cl1 O22 1.435(7) . ? Cl1 O13 1.433(7) . ? Cl1 O10 1.459(7) . ? C1 O1 1.315(4) . ? C1 C2 1.419(5) . ? C1 C6 1.430(4) . ? C2 C3 1.411(5) . ? C2 C8 1.439(5) . ? C3 C4 1.366(5) . ? C4 C5 1.361(6) . ? C4 C7 1.530(5) . ? C5 C6 1.405(5) . ? C6 C13 1.429(5) . ? C8 N1 1.282(5) . ? C9 N1 1.464(5) . ? C9 C10 1.507(6) . ? C10 N2 1.463(5) . ? C11 N2 1.467(6) . ? C12 N2 1.443(5) . ? C13 N3 1.271(5) . ? C14 C15 1.473(7) . ? C14 N3 1.493(5) . ? C15 N4 1.472(5) . ? C16 N4 1.462(6) . ? C17 N4 1.483(7) . ? C18 O2 1.247(4) . ? C18 O3 1.266(4) . ? C18 C19 1.495(5) . ? C20 O4 1.246(4) . ? C20 O5 1.260(4) . ? C20 C21 1.506(4) . ? O10 O23 0.817(14) . ? O11 O22 0.676(15) . ? O11 O20 1.61(2) . ? O12 O21 1.103(15) . ? O12 O20 1.568(12) . ? O13 O21 1.36(2) . ? O13 O23 1.635(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O2 111.38(11) . . ? O4 Zn1 N1 139.08(11) . . ? O2 Zn1 N1 108.53(11) . . ? O4 Zn1 O1 95.41(9) . . ? O2 Zn1 O1 96.66(9) . . ? N1 Zn1 O1 88.57(10) . . ? O4 Zn1 N2 88.62(11) . . ? O2 Zn1 N2 92.63(11) . . ? N1 Zn1 N2 80.85(12) . . ? O1 Zn1 N2 167.73(10) . . ? O3 Zn2 O5 115.32(10) . . ? O3 Zn2 N3 133.98(10) . . ? O5 Zn2 N3 110.00(11) . . ? O3 Zn2 O1 94.59(10) . . ? O5 Zn2 O1 97.25(9) . . ? N3 Zn2 O1 87.17(11) . . ? O3 Zn2 N4 86.93(11) . . ? O5 Zn2 N4 96.56(10) . . ? N3 Zn2 N4 80.35(12) . . ? O1 Zn2 N4 163.90(10) . . ? O21 Cl1 O11 111.1(7) . . ? O21 Cl1 O23 115.4(7) . . ? O11 Cl1 O23 122.7(7) . . ? O21 Cl1 O20 111.3(8) . . ? O11 Cl1 O20 73.5(7) . . ? O23 Cl1 O20 115.9(7) . . ? O21 Cl1 O12 47.9(7) . . ? O11 Cl1 O12 116.4(6) . . ? O23 Cl1 O12 119.2(6) . . ? O20 Cl1 O12 68.2(5) . . ? O21 Cl1 O22 111.9(7) . . ? O11 Cl1 O22 28.1(6) . . ? O23 Cl1 O22 101.4(6) . . ? O20 Cl1 O22 99.3(6) . . ? O12 Cl1 O22 139.1(6) . . ? O21 Cl1 O13 59.3(7) . . ? O11 Cl1 O13 107.5(7) . . ? O23 Cl1 O13 72.0(7) . . ? O20 Cl1 O13 170.4(6) . . ? O12 Cl1 O13 103.5(4) . . ? O22 Cl1 O13 83.9(5) . . ? O21 Cl1 O10 131.1(6) . . ? O11 Cl1 O10 117.7(6) . . ? O23 Cl1 O10 33.5(6) . . ? O20 Cl1 O10 82.5(6) . . ? O12 Cl1 O10 105.3(5) . . ? O22 Cl1 O10 111.5(6) . . ? O13 Cl1 O10 104.9(5) . . ? O1 C1 C2 121.6(3) . . ? O1 C1 C6 121.3(3) . . ? C2 C1 C6 117.1(3) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 C8 115.1(3) . . ? C1 C2 C8 125.4(3) . . ? C4 C3 C2 123.5(3) . . ? C5 C4 C3 116.7(3) . . ? C5 C4 C7 121.8(3) . . ? C3 C4 C7 121.5(4) . . ? C4 C5 C6 124.3(3) . . ? C5 C6 C13 116.2(3) . . ? C5 C6 C1 118.9(3) . . ? C13 C6 C1 124.9(3) . . ? N1 C8 C2 127.5(3) . . ? N1 C9 C10 108.5(3) . . ? N2 C10 C9 110.5(3) . . ? N3 C13 C6 127.6(3) . . ? C15 C14 N3 111.1(3) . . ? N4 C15 C14 111.3(4) . . ? O2 C18 O3 124.4(3) . . ? O2 C18 C19 118.1(3) . . ? O3 C18 C19 117.5(3) . . ? O4 C20 O5 125.4(3) . . ? O4 C20 C21 117.2(3) . . ? O5 C20 C21 117.4(3) . . ? C8 N1 C9 117.7(3) . . ? C8 N1 Zn1 127.2(2) . . ? C9 N1 Zn1 115.1(2) . . ? C12 N2 C10 112.9(3) . . ? C12 N2 C11 108.5(4) . . ? C10 N2 C11 108.9(3) . . ? C12 N2 Zn1 112.8(3) . . ? C10 N2 Zn1 101.8(2) . . ? C11 N2 Zn1 111.8(3) . . ? C13 N3 C14 119.0(3) . . ? C13 N3 Zn2 128.1(2) . . ? C14 N3 Zn2 113.0(2) . . ? C16 N4 C15 110.1(4) . . ? C16 N4 C17 109.8(4) . . ? C15 N4 C17 110.8(4) . . ? C16 N4 Zn2 112.0(3) . . ? C15 N4 Zn2 100.6(2) . . ? C17 N4 Zn2 113.3(3) . . ? C1 O1 Zn1 129.4(2) . . ? C1 O1 Zn2 129.2(2) . . ? Zn1 O1 Zn2 100.92(9) . . ? C18 O2 Zn1 126.9(2) . . ? C18 O3 Zn2 137.3(2) . . ? C20 O4 Zn1 136.8(2) . . ? C20 O5 Zn2 124.6(2) . . ? O23 O10 Cl1 65.7(9) . . ? O22 O11 Cl1 87.9(13) . . ? O22 O11 O20 137.6(17) . . ? Cl1 O11 O20 56.2(6) . . ? O21 O12 Cl1 61.3(6) . . ? O21 O12 O20 111.9(8) . . ? Cl1 O12 O20 55.6(4) . . ? O21 O13 Cl1 55.6(5) . . ? O21 O13 O23 96.5(7) . . ? Cl1 O13 O23 51.6(5) . . ? Cl1 O20 O12 56.2(4) . . ? Cl1 O20 O11 50.3(5) . . ? O12 O20 O11 92.3(7) . . ? O12 O21 Cl1 70.7(7) . . ? O12 O21 O13 129.4(11) . . ? Cl1 O21 O13 65.1(7) . . ? O11 O22 Cl1 64.0(11) . . ? O10 O23 Cl1 80.8(10) . . ? O10 O23 O13 135.8(13) . . ? Cl1 O23 O13 56.5(5) . . ? _refine_diff_density_max 0.755 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.080 #===END data_2 _publ_contact_author_name 'Dr. Andrea Erxleben' _publ_contact_author_address ; Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_mail 'AERX@platon.chemie.uni-dortmund.de' _publ_contact_author_fax '+49(0)231-7553797' _publ_contact_author_phone '+49(0)231-7553845' _publ_contact_letter ? _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_title ; Di- and polynuclear Zn(II) Schiff base complexes: synthesis, structural studies and reaction with amino acid ester ; _publ_author_address ; Andrea Erxleben, Jolante Hermann Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H51 N4 O26.50 Zn5' _chemical_formula_weight 1266.64 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.192(2) _cell_length_b 11.841(2) _cell_length_c 14.520(3) _cell_angle_alpha 100.61(3) _cell_angle_beta 91.98(3) _cell_angle_gamma 102.71(3) _cell_volume 1346.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4087 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 24.39 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 645 _exptl_absorpt_coefficient_mu 2.278 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6587 _exptl_absorpt_correction_T_max 0.8043 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'profile fitted ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4087 _diffrn_reflns_av_R_equivalents 0.096 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 24.39 _reflns_number_total 4064 _reflns_number_gt 2213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, The Netherlands)' _computing_cell_refinement 'Denzo, Scalepack (Z. Otwinowski, W. Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack (Z. Otwinowski, W. Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL PLUS' _computing_publication_material SHELXL-97 _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 w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'U(iso) = 1.2 x U(C(bonded)) ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4064 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2177 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.371 _refine_ls_restrained_S_all 1.371 _refine_ls_shift/su_max 0.010 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.22369(18) 0.64082(13) 0.22118(11) 0.0425(5) Uani 1 d . . . Zn3 Zn 0.0000 0.0000 0.0000 0.0452(6) Uani 1 d S . . Zn2 Zn -0.12170(18) 0.39512(13) 0.20833(11) 0.0419(5) Uani 1 d . . . O1 O -0.1777(10) 0.5267(7) 0.3075(5) 0.040(2) Uani 1 d . . . O3 O -0.2616(11) 0.7767(7) 0.1565(6) 0.049(2) Uani 1 d . . . O9 O -0.3472(10) 0.3459(7) 0.1425(6) 0.052(2) Uani 1 d . . . O4 O -0.0470(11) 0.2489(7) 0.1333(6) 0.052(2) Uani 1 d . . . C13 C -0.0190(15) 0.1725(11) 0.1800(11) 0.049(4) Uani 1 d . . . O5 O 0.0248(10) 0.0819(8) 0.1480(7) 0.055(3) Uani 1 d . . . N2 N -0.0960(13) 0.3074(8) 0.3119(7) 0.043(3) Uani 1 d . . . O8 O -0.3926(11) 0.5218(8) 0.1333(6) 0.050(2) Uani 1 d . . . O7 O 0.0433(11) 0.4927(9) 0.1436(7) 0.059(3) Uani 1 d . . . C10 C -0.3186(16) 0.8539(14) 0.2072(10) 0.053(4) Uani 1 d . . . O6 O 0.0099(11) 0.6775(8) 0.1878(7) 0.059(3) Uani 1 d . . . O2 O -0.3567(12) 0.9390(9) 0.1811(7) 0.069(3) Uani 1 d . . . N1 N -0.3001(13) 0.7402(9) 0.3303(8) 0.051(3) Uani 1 d . . . C6 C -0.1957(15) 0.4348(11) 0.4402(8) 0.041(3) Uani 1 d . . . C2 C -0.2740(17) 0.6221(11) 0.4493(9) 0.045(3) Uani 1 d . . . C11 C -0.1328(15) 0.3330(11) 0.3984(9) 0.041(3) Uani 1 d . . . H11 H -0.1174 0.2814 0.4373 0.050 Uiso 1 calc R . . C4 C -0.2894(16) 0.5286(12) 0.5869(9) 0.047(3) Uani 1 d . . . O10 O 0.2567(10) 0.0206(8) -0.0065(6) 0.056(2) Uani 1 d . . . C12 C -0.0372(17) 0.2000(12) 0.2842(10) 0.055(4) Uani 1 d . . . H12A H -0.1159 0.1346 0.3015 0.066 Uiso 1 calc R . . H12B H 0.0704 0.2083 0.3179 0.066 Uiso 1 calc R . . C1 C -0.2137(14) 0.5262(11) 0.3951(9) 0.039(3) Uani 1 d . . . C8 C -0.3086(15) 0.7229(11) 0.4151(9) 0.046(3) Uani 1 d . . . H8 H -0.3400 0.7806 0.4588 0.056 Uiso 1 calc R . . C14 C 0.0888(18) 0.6029(14) 0.1482(9) 0.054(4) Uani 1 d . . . C5 C -0.2369(15) 0.4373(12) 0.5334(9) 0.048(3) Uani 1 d . . . H5 H -0.2280 0.3733 0.5605 0.058 Uiso 1 calc R . . C3 C -0.3117(16) 0.6195(14) 0.5421(10) 0.061(4) Uani 1 d . . . H3 H -0.3533 0.6807 0.5753 0.073 Uiso 1 calc R . . C16 C -0.4342(16) 0.4121(13) 0.1188(9) 0.045(3) Uani 1 d . . . C7 C -0.3364(18) 0.5300(14) 0.6880(8) 0.067(4) Uani 1 d . . . H7A H -0.3694 0.6020 0.7120 0.080 Uiso 1 calc R . . H7B H -0.2414 0.5247 0.7262 0.080 Uiso 1 calc R . . H7C H -0.4279 0.4640 0.6892 0.080 Uiso 1 calc R . . C9 C -0.347(2) 0.8423(13) 0.3069(10) 0.072(5) Uani 1 d . . . H9A H -0.2829 0.9126 0.3489 0.086 Uiso 1 calc R . . H9B H -0.4651 0.8371 0.3166 0.086 Uiso 1 calc R . . C17 C -0.6100(17) 0.3544(12) 0.0659(10) 0.063(4) Uani 1 d . . . H17A H -0.6297 0.2701 0.0577 0.076 Uiso 1 calc R . . H17B H -0.6137 0.3764 0.0056 0.076 Uiso 1 calc R . . H17C H -0.6951 0.3814 0.1019 0.076 Uiso 1 calc R . . C15 C 0.2450(17) 0.6502(13) 0.1056(12) 0.077(5) Uani 1 d . . . H15A H 0.2639 0.7346 0.1145 0.092 Uiso 1 calc R . . H15B H 0.2340 0.6170 0.0395 0.092 Uiso 1 calc R . . H15C H 0.3381 0.6297 0.1350 0.092 Uiso 1 calc R . . O11 O -0.0082(10) -0.1585(7) 0.0431(6) 0.047(2) Uani 1 d . . . O2W O 0.5107(12) -0.1186(9) -0.1529(9) 0.091(4) Uani 1 d . . . O3W O -0.1117(15) -0.9265(9) -0.2629(8) 0.093(4) Uani 1 d . . . O1W O 0.6033(18) -1.1179(12) -0.3328(9) 0.122(5) Uani 1 d . . . O4W O 0.4005(18) -0.1080(12) -0.4853(10) 0.124(5) Uani 1 d . . . O5W O 0.090(2) -0.082(2) -0.5435(13) 0.077(6) Uani 0.50 d P . . 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 0.0497(10) 0.0386(10) 0.0430(10) 0.0115(8) 0.0105(7) 0.0142(7) Zn3 0.0511(14) 0.0373(13) 0.0494(15) 0.0128(11) 0.0052(11) 0.0115(10) Zn2 0.0501(10) 0.0384(10) 0.0424(10) 0.0128(8) 0.0057(7) 0.0167(7) O1 0.058(6) 0.044(5) 0.022(5) 0.006(4) 0.004(4) 0.020(4) O3 0.074(6) 0.042(6) 0.042(6) 0.010(5) 0.016(5) 0.030(5) O9 0.053(6) 0.045(6) 0.057(6) 0.004(5) -0.002(5) 0.018(5) O4 0.083(7) 0.043(6) 0.046(6) 0.021(5) 0.014(5) 0.036(5) C13 0.041(8) 0.016(7) 0.076(12) -0.012(7) 0.011(7) -0.008(6) O5 0.055(6) 0.053(6) 0.071(7) 0.024(5) 0.013(5) 0.028(5) N2 0.058(7) 0.029(6) 0.043(7) 0.001(5) 0.002(5) 0.014(5) O8 0.062(6) 0.037(6) 0.050(6) 0.013(5) -0.002(4) 0.009(5) O7 0.070(7) 0.051(7) 0.064(7) 0.015(5) 0.020(5) 0.024(5) C10 0.045(9) 0.074(11) 0.048(10) 0.033(9) 0.013(7) 0.012(8) O6 0.049(6) 0.050(6) 0.085(8) 0.024(6) 0.024(5) 0.014(5) O2 0.080(7) 0.066(7) 0.078(8) 0.013(6) 0.006(6) 0.053(6) N1 0.071(8) 0.035(7) 0.060(8) 0.016(6) 0.022(6) 0.032(6) C6 0.053(8) 0.041(8) 0.031(8) 0.010(6) 0.002(6) 0.016(6) C2 0.077(10) 0.030(8) 0.027(8) 0.005(6) 0.008(7) 0.011(7) C11 0.048(8) 0.041(8) 0.036(8) 0.011(7) 0.005(6) 0.008(6) C4 0.059(9) 0.042(9) 0.036(8) 0.005(7) 0.011(6) 0.003(7) O10 0.050(6) 0.060(6) 0.058(6) 0.015(5) 0.008(5) 0.011(5) C12 0.055(9) 0.059(10) 0.064(11) 0.025(8) 0.010(7) 0.029(7) C1 0.031(7) 0.040(8) 0.039(9) 0.003(7) 0.003(6) -0.005(6) C8 0.057(9) 0.045(9) 0.038(9) -0.003(7) 0.006(7) 0.023(7) C14 0.067(10) 0.062(11) 0.045(9) 0.022(8) 0.013(7) 0.029(9) C5 0.050(8) 0.060(10) 0.037(8) 0.013(7) 0.005(6) 0.014(7) C3 0.055(9) 0.071(11) 0.049(10) -0.006(8) 0.000(7) 0.013(8) C16 0.050(9) 0.052(10) 0.033(8) 0.005(7) -0.002(6) 0.013(7) C7 0.085(11) 0.095(12) 0.023(8) 0.018(8) 0.006(7) 0.021(9) C9 0.121(13) 0.052(10) 0.051(10) 0.013(8) 0.015(9) 0.036(9) C17 0.072(11) 0.047(9) 0.066(11) 0.010(8) 0.005(8) 0.007(8) C15 0.066(10) 0.055(10) 0.121(15) 0.039(10) 0.044(10) 0.014(8) O11 0.052(5) 0.035(5) 0.057(6) 0.018(4) 0.000(4) 0.011(4) O2W 0.061(7) 0.065(7) 0.156(12) 0.041(8) -0.010(7) 0.023(6) O3W 0.117(9) 0.065(7) 0.098(9) 0.042(7) -0.029(7) 0.012(7) O1W 0.141(12) 0.118(11) 0.100(11) 0.018(9) -0.012(9) 0.019(9) O4W 0.130(11) 0.124(12) 0.117(12) 0.026(10) 0.010(9) 0.026(9) O5W 0.065(13) 0.120(19) 0.045(12) 0.006(12) -0.012(10) 0.031(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.965(8) . ? Zn1 O8 1.971(9) . ? Zn1 N1 1.998(11) . ? Zn1 O3 2.080(8) . ? Zn1 O1 2.088(8) . ? Zn3 O10 2.070(8) . ? Zn3 O10 2.070(8) 2 ? Zn3 O11 2.073(7) . ? Zn3 O11 2.073(7) 2 ? Zn3 O5 2.171(10) 2 ? Zn3 O5 2.171(10) . ? Zn2 O7 1.962(9) . ? Zn2 O9 1.966(9) . ? Zn2 N2 2.009(10) . ? Zn2 O1 2.060(8) . ? Zn2 O4 2.092(8) . ? O1 C1 1.316(14) . ? O3 C10 1.249(16) . ? O9 C16 1.253(14) . ? O4 C13 1.279(15) . ? C13 O5 1.222(13) . ? C13 C12 1.508(18) . ? N2 C11 1.299(15) . ? N2 C12 1.451(15) . ? O8 C16 1.244(15) . ? O7 C14 1.264(15) . ? C10 O2 1.236(15) . ? C10 C9 1.501(18) . ? O6 C14 1.272(15) . ? N1 C8 1.287(15) . ? N1 C9 1.440(16) . ? C6 C1 1.395(16) . ? C6 C5 1.404(16) . ? C6 C11 1.453(16) . ? C2 C3 1.396(18) . ? C2 C1 1.448(16) . ? C2 C8 1.452(16) . ? C4 C5 1.369(17) . ? C4 C3 1.396(18) . ? C4 C7 1.529(16) . ? C14 C15 1.484(18) . ? C16 C17 1.559(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O8 119.0(4) . . ? O6 Zn1 N1 121.1(4) . . ? O8 Zn1 N1 119.1(4) . . ? O6 Zn1 O3 87.4(3) . . ? O8 Zn1 O3 92.4(3) . . ? N1 Zn1 O3 81.2(4) . . ? O6 Zn1 O1 93.3(3) . . ? O8 Zn1 O1 96.0(3) . . ? N1 Zn1 O1 89.9(4) . . ? O3 Zn1 O1 170.0(3) . . ? O10 Zn3 O10 180.0 . 2 ? O10 Zn3 O11 88.6(3) . . ? O10 Zn3 O11 91.4(3) 2 . ? O10 Zn3 O11 91.4(3) . 2 ? O10 Zn3 O11 88.6(3) 2 2 ? O11 Zn3 O11 180.0 . 2 ? O10 Zn3 O5 87.0(3) . 2 ? O10 Zn3 O5 93.0(3) 2 2 ? O11 Zn3 O5 93.1(3) . 2 ? O11 Zn3 O5 86.9(3) 2 2 ? O10 Zn3 O5 93.0(3) . . ? O10 Zn3 O5 87.0(3) 2 . ? O11 Zn3 O5 86.9(3) . . ? O11 Zn3 O5 93.1(3) 2 . ? O5 Zn3 O5 180.0 2 . ? O7 Zn2 O9 113.6(4) . . ? O7 Zn2 N2 132.0(4) . . ? O9 Zn2 N2 112.9(4) . . ? O7 Zn2 O1 99.1(4) . . ? O9 Zn2 O1 95.1(3) . . ? N2 Zn2 O1 88.2(3) . . ? O7 Zn2 O4 87.0(4) . . ? O9 Zn2 O4 92.4(4) . . ? N2 Zn2 O4 79.6(4) . . ? O1 Zn2 O4 167.4(3) . . ? C1 O1 Zn2 129.7(8) . . ? C1 O1 Zn1 128.7(8) . . ? Zn2 O1 Zn1 99.9(3) . . ? C10 O3 Zn1 114.7(8) . . ? C16 O9 Zn2 126.6(9) . . ? C13 O4 Zn2 116.8(8) . . ? O5 C13 O4 125.9(14) . . ? O5 C13 C12 117.8(13) . . ? O4 C13 C12 116.2(11) . . ? C13 O5 Zn3 124.7(9) . . ? C11 N2 C12 117.2(11) . . ? C11 N2 Zn2 127.6(8) . . ? C12 N2 Zn2 115.2(8) . . ? C16 O8 Zn1 133.4(8) . . ? C14 O7 Zn2 132.8(9) . . ? O2 C10 O3 124.9(12) . . ? O2 C10 C9 116.8(14) . . ? O3 C10 C9 118.3(12) . . ? C14 O6 Zn1 125.6(9) . . ? C8 N1 C9 119.4(11) . . ? C8 N1 Zn1 127.5(9) . . ? C9 N1 Zn1 113.1(9) . . ? C1 C6 C5 120.4(12) . . ? C1 C6 C11 124.9(11) . . ? C5 C6 C11 114.7(11) . . ? C3 C2 C1 119.8(12) . . ? C3 C2 C8 114.2(12) . . ? C1 C2 C8 125.9(11) . . ? N2 C11 C6 126.1(11) . . ? C5 C4 C3 116.6(12) . . ? C5 C4 C7 123.4(12) . . ? C3 C4 C7 119.9(12) . . ? N2 C12 C13 112.0(11) . . ? O1 C1 C6 122.2(11) . . ? O1 C1 C2 120.9(11) . . ? C6 C1 C2 116.9(11) . . ? N1 C8 C2 126.5(12) . . ? O7 C14 O6 124.5(13) . . ? O7 C14 C15 118.6(13) . . ? O6 C14 C15 116.9(13) . . ? C4 C5 C6 123.7(12) . . ? C2 C3 C4 122.5(13) . . ? O8 C16 O9 125.7(12) . . ? O8 C16 C17 115.9(11) . . ? O9 C16 C17 118.4(12) . . ? N1 C9 C10 112.6(12) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.39 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.942 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.158 #===END data_4 _publ_contact_author_name 'Dr. Andrea Erxleben' _publ_contact_author_address ; Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_mail 'AERX@platon.chemie.uni-dortmund.de' _publ_contact_author_fax '+49(0)231-7553797' _publ_contact_author_phone '+49(0)231-7553845' _publ_contact_letter ? _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_title ; Di- and polynuclear Zn(II) Schiff base complexes: synthesis, structural studies and reaction with amino acid ester ; _publ_author_address ; Andrea Erxleben, Jolante Hermann Universitaet Dortmund Fachbereich Chemie, ACIII Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 N2 O8 Zn' _chemical_formula_weight 395.66 _chemical_melting_point ? _chemical_compound_source ? 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.290(4) _cell_length_b 8.514(2) _cell_length_c 19.488(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.13(3) _cell_angle_gamma 90.00 _cell_volume 3199.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5372 _cell_measurement_theta_min 4.79 _cell_measurement_theta_max 25.58 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method ? _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.580 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6934 _exptl_absorpt_correction_T_max 0.7428 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Nonius KappaCCD ' _diffrn_measurement_method ' profile fitted ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5372 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.79 _diffrn_reflns_theta_max 25.58 _reflns_number_total 2920 _reflns_number_observed 1864 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, The Netherlands) ' _computing_cell_refinement 'Denzo, Scalepack (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo, Scalepack (Otwinowski, Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL PLUS ' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Fourier-difference map ' _refine_ls_hydrogen_treatment isotropically _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2909 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_obs 0.0430 _refine_ls_wR_factor_all 0.1189 _refine_ls_wR_factor_obs 0.0880 _refine_ls_goodness_of_fit_all 0.940 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.139 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.30503(2) 0.13543(5) 0.35230(2) 0.0384(2) Uani 1 d . . N1 N 0.4174(2) -0.1636(4) 0.5365(2) 0.0487(9) Uani 1 d . . H1 H 0.4151(23) -0.0966(48) 0.5045(24) 0.058 Uiso 1 d . . N2 N 0.2103(2) 0.1975(3) 0.3589(2) 0.0376(7) Uani 1 d . . O1 O 0.32175(14) 0.0131(3) 0.44616(15) 0.0490(7) Uani 1 d . . O2 O 0.60202(14) -0.2321(3) 0.6116(2) 0.0506(7) Uani 1 d . . O3 O 0.5431(2) -0.0075(4) 0.5839(2) 0.0779(11) Uani 1 d . . O4 O 0.1840(2) 0.4850(3) 0.2195(2) 0.0531(8) Uani 1 d . . O5 O 0.27326(14) 0.3250(3) 0.27049(14) 0.0461(7) Uani 1 d . . C1 C 0.2819(2) -0.0079(4) 0.4856(2) 0.0373(9) Uani 1 d . . C2 C 0.3055(2) -0.1037(4) 0.5491(2) 0.0398(9) Uani 1 d . . C3 C 0.2619(2) -0.1358(5) 0.5910(2) 0.0422(9) Uani 1 d . . H3 H 0.2785(21) -0.1894(45) 0.6303(23) 0.051 Uiso 1 d . . C4 C 0.1960(2) -0.0717(4) 0.5749(2) 0.0395(9) Uani 1 d . . C5 C 0.1748(2) 0.0248(5) 0.5150(2) 0.0394(10) Uani 1 d . . H5 H 0.1384(22) 0.0559(49) 0.5050(23) 0.047 Uiso 1 d . . C6 C 0.2145(2) 0.0577(4) 0.4694(2) 0.0370(9) Uani 1 d . . C7 C 0.1488(3) -0.1121(6) 0.6186(3) 0.0503(11) Uani 1 d . . H7A H 0.1415(22) -0.2155(53) 0.6173(23) 0.060 Uiso 1 d . . H7B H 0.1143(23) -0.0407(51) 0.6072(23) 0.060 Uiso 1 d . . H7C H 0.1722(23) -0.0865(48) 0.6674(26) 0.060 Uiso 1 d . . C8 C 0.3715(2) -0.1786(5) 0.5689(2) 0.0464(10) Uani 1 d . . H8 H 0.3878(21) -0.2428(43) 0.6177(23) 0.056 Uiso 1 d . . C9 C 0.4831(2) -0.2532(5) 0.5573(3) 0.0614(13) Uani 1 d . . H9A H 0.4804(23) -0.3499(50) 0.5937(25) 0.074 Uiso 1 d . . H9B H 0.4888(23) -0.3114(56) 0.5119(26) 0.074 Uiso 1 d . . C10 C 0.5474(2) -0.1528(5) 0.5869(2) 0.0491(10) Uani 1 d . . C11 C 0.1847(2) 0.1602(5) 0.4091(2) 0.0398(10) Uani 1 d . . H11 H 0.1483(21) 0.1819(47) 0.4078(22) 0.048 Uiso 1 d . . C12 C 0.1695(2) 0.2996(5) 0.3018(2) 0.0411(10) Uani 1 d . . H12A H 0.1373(22) 0.2384(46) 0.2686(23) 0.049 Uiso 1 d . . H12B H 0.1458(20) 0.3799(43) 0.3197(21) 0.049 Uiso 1 d . . C13 C 0.2140(2) 0.3765(5) 0.2614(2) 0.0387(9) Uani 1 d . . O1W O 0.1046(2) -0.1354(5) 0.2721(2) 0.1013(13) Uani 1 d . . O2W O 0.5000 -0.4191(9) 0.2500 0.136(2) Uiso 1 d S . O3W O 0.5168(16) -0.2231(34) 0.3619(18) 0.139(10) Uiso 0.25 d P . O4W O 0.5000 0.0960(15) 0.2500 0.104(4) Uiso 0.50 d SP . O5W O 0.5229(8) -0.2875(19) 0.3995(9) 0.078(4) Uiso 0.25 d P . O6W O 0.4532(10) 0.0869(24) 0.2472(10) 0.112(6) Uiso 0.25 d P . O7W O 0.5066(12) -0.1598(26) 0.3231(12) 0.095(8) Uiso 0.25 d P . O8W O 0.5278(10) -0.1539(24) 0.3490(12) 0.071(5) Uiso 0.25 d P . 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 0.0368(3) 0.0426(3) 0.0374(3) -0.0014(2) 0.0137(2) -0.0005(2) N1 0.037(2) 0.052(2) 0.055(2) 0.007(2) 0.012(2) -0.001(2) N2 0.036(2) 0.039(2) 0.036(2) 0.0026(14) 0.009(2) 0.0007(15) O1 0.040(2) 0.061(2) 0.049(2) 0.0143(14) 0.0187(14) 0.0093(13) O2 0.035(2) 0.048(2) 0.065(2) 0.0022(14) 0.0092(14) 0.0033(13) O3 0.054(2) 0.054(2) 0.116(3) -0.001(2) 0.012(2) 0.003(2) O4 0.059(2) 0.048(2) 0.055(2) 0.0193(15) 0.020(2) 0.0035(14) O5 0.042(2) 0.052(2) 0.046(2) 0.0042(13) 0.0155(13) -0.0022(14) C1 0.038(2) 0.038(2) 0.038(2) 0.000(2) 0.015(2) -0.002(2) C2 0.040(2) 0.041(2) 0.034(2) 0.001(2) 0.006(2) -0.003(2) C3 0.048(2) 0.042(2) 0.035(2) 0.004(2) 0.010(2) -0.003(2) C4 0.045(2) 0.040(2) 0.036(2) -0.001(2) 0.016(2) -0.004(2) C5 0.035(2) 0.044(2) 0.040(2) 0.001(2) 0.013(2) 0.002(2) C6 0.040(2) 0.038(2) 0.032(2) 0.002(2) 0.010(2) 0.002(2) C7 0.060(3) 0.047(3) 0.050(3) 0.003(2) 0.025(2) -0.005(2) C8 0.041(2) 0.049(3) 0.042(2) 0.001(2) 0.004(2) -0.002(2) C9 0.042(3) 0.053(3) 0.082(4) 0.003(3) 0.010(3) 0.002(2) C10 0.045(3) 0.049(3) 0.052(3) 0.000(2) 0.013(2) -0.001(2) C11 0.034(2) 0.044(2) 0.043(2) -0.001(2) 0.014(2) 0.001(2) C12 0.037(2) 0.047(2) 0.039(2) 0.006(2) 0.011(2) 0.002(2) C13 0.044(2) 0.037(2) 0.033(2) -0.006(2) 0.008(2) -0.003(2) O1W 0.088(3) 0.141(4) 0.086(3) 0.008(3) 0.043(2) 0.034(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 O4 1.960(3) 4_545 ? Zn1 O2 1.976(3) 5_656 ? Zn1 N2 2.036(3) . ? Zn1 O1 2.040(3) . ? Zn1 O5 2.219(3) . ? N1 C8 1.284(5) . ? N1 C9 1.478(5) . ? N1 H1 0.84(4) . ? N2 C11 1.282(5) . ? N2 C12 1.451(5) . ? O1 C1 1.290(4) . ? O2 C10 1.258(5) . ? O2 Zn1 1.976(3) 5_656 ? O3 C10 1.240(5) . ? O4 C13 1.257(4) . ? O4 Zn1 1.960(3) 4 ? O5 C13 1.239(4) . ? C1 C6 1.419(5) . ? C1 C2 1.434(5) . ? C2 C3 1.405(5) . ? C2 C8 1.424(6) . ? C3 C4 1.387(5) . ? C3 H3 0.86(4) . ? C4 C5 1.382(6) . ? C4 C7 1.506(5) . ? C5 C6 1.403(5) . ? C5 H5 0.75(4) . ? C6 C11 1.437(6) . ? C7 H7A 0.89(4) . ? C7 H7B 0.90(4) . ? C7 H7C 0.95(5) . ? C8 H8 1.06(4) . ? C9 C10 1.516(6) . ? C9 H9A 1.10(5) . ? C9 H9B 1.05(5) . ? C11 H11 0.75(4) . ? C12 C13 1.518(5) . ? C12 H12A 0.92(4) . ? C12 H12B 0.96(4) . ? O3W O8W 0.70(3) . ? O3W O5W 0.89(3) . ? O3W O7W 0.90(3) . ? O4W O6W 0.94(2) 2_655 ? O4W O6W 0.94(2) . ? O5W O8W 1.53(3) . ? O5W O7W 1.79(3) . ? O7W O8W 0.55(3) . ? 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 O4 Zn1 O2 102.64(12) 4_545 5_656 ? O4 Zn1 N2 122.25(13) 4_545 . ? O2 Zn1 N2 133.22(12) 5_656 . ? O4 Zn1 O1 106.41(12) 4_545 . ? O2 Zn1 O1 91.10(12) 5_656 . ? N2 Zn1 O1 88.46(11) . . ? O4 Zn1 O5 91.97(11) 4_545 . ? O2 Zn1 O5 89.12(11) 5_656 . ? N2 Zn1 O5 77.72(11) . . ? O1 Zn1 O5 161.09(10) . . ? C8 N1 C9 123.0(4) . . ? C8 N1 H1 123.6(31) . . ? C9 N1 H1 113.2(31) . . ? C11 N2 C12 117.7(3) . . ? C11 N2 Zn1 126.7(3) . . ? C12 N2 Zn1 115.5(2) . . ? C1 O1 Zn1 130.2(2) . . ? C10 O2 Zn1 122.8(3) . 5_656 ? C13 O4 Zn1 143.5(3) . 4 ? C13 O5 Zn1 114.3(2) . . ? O1 C1 C6 123.5(3) . . ? O1 C1 C2 119.4(3) . . ? C6 C1 C2 117.1(3) . . ? C3 C2 C8 117.7(4) . . ? C3 C2 C1 120.7(4) . . ? C8 C2 C1 121.5(4) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3 119.3(28) . . ? C2 C3 H3 118.5(28) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C7 121.8(4) . . ? C3 C4 C7 121.4(4) . . ? C4 C5 C6 124.3(4) . . ? C4 C5 H5 116.9(34) . . ? C6 C5 H5 118.5(34) . . ? C5 C6 C1 119.0(3) . . ? C5 C6 C11 117.4(3) . . ? C1 C6 C11 123.5(3) . . ? C4 C7 H7A 109.7(28) . . ? C4 C7 H7B 106.7(27) . . ? H7A C7 H7B 123.4(42) . . ? C4 C7 H7C 107.9(26) . . ? H7A C7 H7C 106.5(38) . . ? H7B C7 H7C 101.6(37) . . ? N1 C8 C2 126.0(4) . . ? N1 C8 H8 115.0(22) . . ? C2 C8 H8 118.6(22) . . ? N1 C9 C10 114.1(4) . . ? N1 C9 H9A 109.9(24) . . ? C10 C9 H9A 112.7(24) . . ? N1 C9 H9B 109.8(26) . . ? C10 C9 H9B 106.3(25) . . ? H9A C9 H9B 103.4(35) . . ? O3 C10 O2 126.5(4) . . ? O3 C10 C9 120.3(4) . . ? O2 C10 C9 113.2(4) . . ? N2 C11 C6 127.4(4) . . ? N2 C11 H11 122.6(33) . . ? C6 C11 H11 109.5(32) . . ? N2 C12 C13 111.5(3) . . ? N2 C12 H12A 108.0(25) . . ? C13 C12 H12A 106.6(25) . . ? N2 C12 H12B 112.2(23) . . ? C13 C12 H12B 109.1(23) . . ? H12A C12 H12B 109.2(35) . . ? O5 C13 O4 127.2(4) . . ? O5 C13 C12 118.7(4) . . ? O4 C13 C12 114.0(3) . . ? O8W O3W O5W 146.1(62) . . ? O8W O3W O7W 38.0(26) . . ? O5W O3W O7W 175.1(52) . . ? O6W O4W O6W 170.5(35) 2_655 . ? O3W O5W O8W 14.9(27) . . ? O3W O5W O7W 2.5(26) . . ? O8W O5W O7W 17.0(10) . . ? O8W O7W O3W 51.5(31) . . ? O8W O7W O5W 53.5(38) . . ? O3W O7W O5W 2.5(26) . . ? O7W O8W O3W 90.5(42) . . ? O7W O8W O5W 109.5(44) . . ? O3W O8W O5W 19.0(36) . . ? _refine_diff_density_max 0.544 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.071 #===END