# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Spyros Perlepes' _publ_contact_author_email PERLEPES@PATREAS.UPATRAS.GR _publ_section_title ; A tetrahedron in a cube: a dodecanuclear ZnII benzoate cluster from the use of 2-pyridinealdoxime ; loop_ _publ_author_name 'Spyros Perlepes' 'Vlasoula Bekiari' 'Michalis Kaplanis' 'Eugenia Katsoulakou' 'Konstantis F. Konidaris' ; E.Manessi-Zoupa ; 'Catherine Raptopoulou' 'Aris Terzis' # end Validation Reply Form # Attachment 'Complex_2.cif' data_pemi70 _database_code_depnum_ccdc_archive 'CCDC 746014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C140 H114 N10 O42 Zn12' _chemical_formula_weight 3392.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' '-x, -y+1/2, -z+1/4' 'x+1/2, y, -z+3/4' 'y, -x, -z' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' '-x+1/2, -y+1, -z+3/4' 'x+1, y+1/2, -z+5/4' 'y+1/2, -x+1/2, -z+1/2' '-y+1, x+1, -z+1' _cell_length_a 34.710(10) _cell_length_b 34.710(10) _cell_length_c 14.862(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17906(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 27 _exptl_crystal_description parall _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6880 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The crystals had poor diffraction ability (despite their sufficient size) and the data were collected in increasing 2theta shells. The data collection was terminated when almost half of the collected shell data were unobserved. ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'P21 Nicolet upgraded by Crystal Logic' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.9 _diffrn_reflns_number 5227 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 51.96 _reflns_number_total 5006 _reflns_number_gt 3263 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.1515P)^2^+26.3312P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 5006 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2441 _refine_ls_wR_factor_gt 0.2053 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.00843(3) 0.04745(3) 0.91925(8) 0.0598(4) Uani 1 1 d . . . Zn2 Zn 0.04262(4) 0.12046(4) 1.03339(9) 0.0725(5) Uani 1 1 d . . . Zn3 Zn 0.07686(4) 0.10429(4) 0.83074(9) 0.0800(5) Uani 1 1 d . . . O1 O 0.00673(15) 0.03805(15) 1.0670(4) 0.0573(14) Uani 1 1 d . . . N1 N 0.0400(2) 0.1389(2) 1.1693(6) 0.081(2) Uani 1 1 d . . . N2 N 0.0169(2) 0.0731(2) 1.1044(5) 0.0627(19) Uani 1 1 d . . . O11 O -0.02869(18) 0.09297(17) 0.9353(4) 0.0703(17) Uani 1 1 d . . . O12 O 0.0030(2) 0.14817(18) 0.9635(5) 0.0804(18) Uani 1 1 d . . . O21 O 0.0055(2) 0.04969(19) 0.7828(4) 0.0773(18) Uani 1 1 d . . . O22 O 0.0299(2) 0.1081(2) 0.7530(5) 0.091(2) Uani 1 1 d . . . O31 O 0.0881(2) 0.1552(2) 1.0132(5) 0.091(2) Uani 1 1 d . . . O32 O 0.0926(2) 0.1565(2) 0.8631(5) 0.097(2) Uani 1 1 d . . . O41 O 0.1169(2) 0.0854(3) 0.7480(7) 0.117(3) Uani 1 1 d . . . O42 O 0.1383(3) 0.0705(4) 0.8839(9) 0.147(4) Uani 1 1 d . . . O51 O 0.05677(16) 0.07880(16) 0.9397(4) 0.0638(15) Uani 1 1 d . . . C1 C 0.0529(4) 0.1723(4) 1.2014(9) 0.104(4) Uani 1 1 d . . . H1 H 0.0656 0.1893 1.1633 0.135 Uiso 1 1 calc R . . C2 C 0.0475(4) 0.1821(4) 1.2925(11) 0.124(5) Uani 1 1 d . . . H2 H 0.0570 0.2055 1.3141 0.162 Uiso 1 1 calc R . . C3 C 0.0288(5) 0.1581(4) 1.3486(9) 0.116(5) Uani 1 1 d . . . H3 H 0.0257 0.1644 1.4090 0.151 Uiso 1 1 calc R . . C4 C 0.0145(4) 0.1246(4) 1.3151(8) 0.099(4) Uani 1 1 d . . . H4 H 0.0006 0.1079 1.3518 0.128 Uiso 1 1 calc R . . C5 C 0.0209(3) 0.1156(3) 1.2244(7) 0.077(3) Uani 1 1 d . . . C6 C 0.0087(3) 0.0786(3) 1.1870(7) 0.069(2) Uani 1 1 d . . . H6 H -0.0041 0.0602 1.2213 0.090 Uiso 1 1 calc R . . C11 C -0.0239(3) 0.1294(3) 0.9285(7) 0.077(3) Uani 1 1 d . . . C12 C -0.0515(4) 0.1506(3) 0.8689(10) 0.105(4) Uani 1 1 d . . . C13 C -0.0818(4) 0.1302(4) 0.8294(11) 0.135(6) Uani 1 1 d . . . H13 H -0.0843 0.1039 0.8395 0.175 Uiso 1 1 calc R . . C14 C -0.1088(6) 0.1496(6) 0.7739(16) 0.205(10) Uani 1 1 d . . . H14 H -0.1297 0.1374 0.7469 0.267 Uiso 1 1 calc R . . C15 C -0.1005(10) 0.1917(7) 0.763(2) 0.248(15) Uani 1 1 d . . . H15 H -0.1166 0.2060 0.7258 0.322 Uiso 1 1 calc R . . C16 C -0.0722(9) 0.2096(7) 0.802(2) 0.255(17) Uani 1 1 d . . . H16 H -0.0685 0.2359 0.7937 0.332 Uiso 1 1 calc R . . C17 C -0.0487(5) 0.1898(4) 0.8545(14) 0.169(8) Uani 1 1 d . . . H17 H -0.0290 0.2031 0.8835 0.220 Uiso 1 1 calc R . . C21 C 0.0085(3) 0.0795(3) 0.7353(7) 0.074(3) Uani 1 1 d . . . C22 C -0.0146(3) 0.0835(3) 0.6514(6) 0.075(3) Uani 1 1 d . . . C23 C -0.0326(3) 0.0513(4) 0.6149(8) 0.098(3) Uani 1 1 d . . . H23 H -0.0306 0.0274 0.6430 0.128 Uiso 1 1 calc R . . C24 C -0.0540(4) 0.0553(5) 0.5346(9) 0.122(5) Uani 1 1 d . . . H24 H -0.0661 0.0342 0.5083 0.159 Uiso 1 1 calc R . . C25 C -0.0565(5) 0.0915(5) 0.4961(10) 0.132(6) Uani 1 1 d . . . H25 H -0.0699 0.0944 0.4423 0.172 Uiso 1 1 calc R . . C26 C -0.0400(5) 0.1230(4) 0.5346(11) 0.124(5) Uani 1 1 d . . . H26 H -0.0434 0.1474 0.5096 0.161 Uiso 1 1 calc R . . C27 C -0.0188(4) 0.1186(4) 0.6087(8) 0.099(4) Uani 1 1 d . . . H27 H -0.0064 0.1400 0.6327 0.128 Uiso 1 1 calc R . . C31 C 0.1013(3) 0.1680(3) 0.9416(10) 0.091(3) Uani 1 1 d . . . C32 C 0.1305(4) 0.2001(4) 0.9463(10) 0.102(4) Uani 1 1 d . . . C33 C 0.1468(4) 0.2141(4) 0.8684(12) 0.128(5) Uani 1 1 d . . . H33 H 0.1399 0.2036 0.8132 0.167 Uiso 1 1 calc R . . C34 C 0.1732(6) 0.2437(6) 0.8721(17) 0.181(9) Uani 1 1 d . . . H34 H 0.1861 0.2514 0.8203 0.236 Uiso 1 1 calc R . . C35 C 0.1802(8) 0.2610(7) 0.951(2) 0.209(11) Uani 1 1 d . . . H35 H 0.1975 0.2814 0.9535 0.271 Uiso 1 1 calc R . . C36 C 0.1616(7) 0.2484(7) 1.0275(19) 0.232(13) Uani 1 1 d . . . H36 H 0.1650 0.2614 1.0817 0.301 Uiso 1 1 calc R . . C37 C 0.1377(5) 0.2163(6) 1.0230(14) 0.177(8) Uani 1 1 d . . . H37 H 0.1270 0.2063 1.0754 0.230 Uiso 1 1 calc R . . C41 C 0.1424(4) 0.0732(4) 0.8015(13) 0.114(4) Uani 1 1 d . . . C42 C 0.1811(4) 0.0622(4) 0.7602(12) 0.110(4) Uani 1 1 d . . . C43 C 0.1890(4) 0.0713(5) 0.6733(12) 0.129(5) Uani 1 1 d . . . H43 H 0.1709 0.0838 0.6376 0.168 Uiso 1 1 calc R . . C44 C 0.2256(6) 0.0612(7) 0.6385(15) 0.168(9) Uani 1 1 d . . . H44 H 0.2314 0.0667 0.5788 0.219 Uiso 1 1 calc R . . C45 C 0.2517(6) 0.0442(8) 0.689(2) 0.181(12) Uani 1 1 d . . . H45 H 0.2757 0.0381 0.6654 0.235 Uiso 1 1 calc R . . C46 C 0.2435(6) 0.0356(6) 0.7750(19) 0.173(9) Uani 1 1 d . . . H46 H 0.2621 0.0237 0.8105 0.225 Uiso 1 1 calc R . . C47 C 0.2078(4) 0.0444(5) 0.8119(13) 0.137(6) Uani 1 1 d . . . H47 H 0.2023 0.0381 0.8714 0.179 Uiso 1 1 calc R . . NS1 N 0.1333(9) 0.7318(10) -0.016(2) 0.154(10) Uiso 0.50 1 d P . . CS1 C 0.1295(10) 0.7605(11) 0.002(2) 0.131(10) Uiso 0.50 1 d P . . CS2 C 0.1270(11) 0.7983(12) 0.011(3) 0.158(13) Uiso 0.50 1 d P . . O1W O 0.4767(10) 0.2895(11) 0.067(3) 0.257(16) Uiso 0.50 1 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 0.0610(7) 0.0539(7) 0.0646(7) 0.0038(5) -0.0004(5) -0.0018(5) Zn2 0.0755(9) 0.0640(8) 0.0781(9) -0.0048(6) -0.0016(7) -0.0093(6) Zn3 0.0818(9) 0.0767(9) 0.0816(9) 0.0017(7) 0.0068(7) -0.0171(7) O1 0.050(3) 0.053(3) 0.069(4) -0.004(3) 0.002(3) 0.000(3) N1 0.081(6) 0.070(5) 0.092(6) -0.016(5) -0.005(5) -0.006(5) N2 0.059(4) 0.061(5) 0.068(5) -0.004(4) 0.001(4) 0.002(4) O11 0.072(4) 0.053(4) 0.086(4) 0.004(3) 0.003(3) 0.005(3) O12 0.078(4) 0.063(4) 0.100(5) 0.000(4) -0.011(4) -0.005(4) O21 0.102(5) 0.068(4) 0.062(4) 0.007(3) -0.001(3) 0.000(4) O22 0.094(5) 0.089(5) 0.089(5) 0.016(4) -0.008(4) -0.010(4) O31 0.088(5) 0.087(5) 0.099(5) -0.007(4) -0.002(4) -0.033(4) O32 0.120(6) 0.077(5) 0.094(6) 0.004(4) 0.000(5) -0.025(4) O41 0.074(5) 0.134(7) 0.142(8) -0.017(6) -0.001(5) -0.002(5) O42 0.107(7) 0.189(11) 0.143(9) 0.027(8) 0.022(7) 0.010(7) O51 0.065(4) 0.054(3) 0.072(4) 0.001(3) 0.003(3) -0.008(3) C1 0.106(9) 0.087(8) 0.119(10) -0.029(7) 0.004(8) -0.015(7) C2 0.127(12) 0.112(11) 0.134(12) -0.058(10) -0.017(10) 0.005(9) C3 0.155(13) 0.102(10) 0.091(9) -0.034(8) 0.001(9) -0.016(9) C4 0.113(9) 0.093(9) 0.091(8) -0.020(7) 0.004(7) 0.012(7) C5 0.082(7) 0.075(7) 0.074(7) -0.019(6) 0.001(5) 0.002(6) C6 0.071(6) 0.060(6) 0.076(7) 0.002(5) -0.003(5) 0.008(5) C11 0.080(7) 0.076(7) 0.074(6) 0.000(6) 0.011(6) 0.000(6) C12 0.109(9) 0.056(6) 0.150(11) 0.011(7) -0.019(9) 0.012(6) C13 0.115(11) 0.105(10) 0.184(15) 0.033(10) -0.060(11) -0.002(9) C14 0.176(18) 0.165(17) 0.28(3) 0.023(17) -0.149(18) 0.022(14) C15 0.33(4) 0.15(2) 0.26(3) 0.08(2) -0.11(3) 0.06(2) C16 0.27(3) 0.119(16) 0.38(4) 0.08(2) -0.18(3) -0.005(18) C17 0.154(15) 0.089(10) 0.26(2) 0.037(12) -0.100(15) -0.009(10) C21 0.068(6) 0.082(7) 0.073(7) -0.003(6) 0.002(5) -0.002(6) C22 0.075(6) 0.081(7) 0.069(6) 0.006(6) 0.004(5) 0.010(5) C23 0.110(9) 0.111(9) 0.073(7) 0.003(7) -0.006(7) -0.016(8) C24 0.132(12) 0.151(14) 0.084(9) -0.017(9) -0.004(8) -0.042(10) C25 0.144(13) 0.160(15) 0.094(10) 0.056(11) -0.009(9) 0.021(12) C26 0.159(14) 0.079(9) 0.134(13) 0.012(8) -0.021(11) 0.011(9) C27 0.120(10) 0.091(8) 0.086(8) 0.019(7) -0.031(7) 0.005(7) C31 0.085(8) 0.077(7) 0.112(10) -0.007(7) 0.011(7) -0.010(6) C32 0.098(9) 0.083(8) 0.126(11) -0.012(8) 0.009(8) -0.026(7) C33 0.127(12) 0.094(10) 0.164(14) -0.008(10) 0.019(11) -0.015(9) C34 0.175(18) 0.170(19) 0.20(2) 0.007(17) 0.053(16) -0.077(16) C35 0.24(3) 0.17(2) 0.22(3) -0.037(19) 0.03(2) -0.105(19) C36 0.26(3) 0.21(2) 0.22(3) -0.06(2) 0.02(2) -0.16(2) C37 0.163(16) 0.183(18) 0.185(18) -0.054(15) 0.019(13) -0.110(14) C41 0.081(9) 0.106(10) 0.154(14) -0.013(10) 0.015(10) 0.001(7) C42 0.081(9) 0.095(9) 0.155(13) -0.022(9) 0.011(9) -0.023(7) C43 0.100(11) 0.155(14) 0.132(12) -0.013(11) 0.017(9) -0.011(9) C44 0.127(15) 0.20(2) 0.18(2) -0.052(16) 0.075(15) -0.057(15) C45 0.082(12) 0.19(2) 0.27(3) -0.08(2) 0.036(18) -0.019(13) C46 0.104(15) 0.164(18) 0.25(3) -0.033(19) 0.014(16) -0.001(12) C47 0.079(9) 0.141(13) 0.192(17) -0.001(12) -0.005(11) 0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O51 2.023(6) . ? Zn1 O21 2.033(6) . ? Zn1 O11 2.053(6) . ? Zn1 O1 2.153(5) 7_557 ? Zn1 O1 2.155(6) 16_446 ? Zn1 O1 2.220(6) . ? Zn2 O12 1.975(7) . ? Zn2 O31 2.008(7) . ? Zn2 O51 2.066(6) . ? Zn2 N1 2.121(9) . ? Zn2 N2 2.148(8) . ? Zn3 O32 1.952(8) . ? Zn3 O41 1.968(9) . ? Zn3 O51 1.973(6) . ? Zn3 O22 2.003(7) . ? Zn3 C41 2.554(14) . ? O1 N2 1.384(9) . ? O1 Zn1 2.153(5) 16_446 ? O1 Zn1 2.155(6) 7_557 ? N1 C5 1.327(13) . ? N1 C1 1.331(14) . ? N2 C6 1.274(12) . ? O11 C11 1.278(11) . ? O12 C11 1.252(12) . ? O21 C21 1.256(12) . ? O22 C21 1.267(12) . ? O31 C31 1.242(14) . ? O32 C31 1.270(14) . ? O41 C41 1.263(17) . ? O42 C41 1.236(18) . ? C1 C2 1.409(19) . ? C1 H1 0.9300 . ? C2 C3 1.345(19) . ? C2 H2 0.9300 . ? C3 C4 1.359(16) . ? C3 H3 0.9300 . ? C4 C5 1.401(15) . ? C4 H4 0.9300 . ? C5 C6 1.465(13) . ? C6 H6 0.9300 . ? C11 C12 1.498(16) . ? C12 C17 1.382(17) . ? C12 C13 1.396(17) . ? C13 C14 1.420(19) . ? C13 H13 0.9300 . ? C14 C15 1.50(3) . ? C14 H14 0.9300 . ? C15 C16 1.30(3) . ? C15 H15 0.9300 . ? C16 C17 1.32(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C21 C22 1.489(14) . ? C22 C27 1.382(14) . ? C22 C23 1.391(15) . ? C23 C24 1.413(17) . ? C23 H23 0.9300 . ? C24 C25 1.382(19) . ? C24 H24 0.9300 . ? C25 C26 1.36(2) . ? C25 H25 0.9300 . ? C26 C27 1.332(17) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C31 C32 1.507(16) . ? C32 C37 1.30(2) . ? C32 C33 1.376(19) . ? C33 C34 1.38(2) . ? C33 H33 0.9300 . ? C34 C35 1.33(3) . ? C34 H34 0.9300 . ? C35 C36 1.38(3) . ? C35 H35 0.9300 . ? C36 C37 1.39(2) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C41 C42 1.527(18) . ? C42 C47 1.35(2) . ? C42 C43 1.36(2) . ? C43 C44 1.42(2) . ? C43 H43 0.9300 . ? C44 C45 1.32(3) . ? C44 H44 0.9300 . ? C45 C46 1.34(3) . ? C45 H45 0.9300 . ? C46 C47 1.39(2) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? NS1 CS1 1.04(4) . ? CS1 CS2 1.32(4) . ? 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 O51 Zn1 O21 99.9(3) . . ? O51 Zn1 O11 95.1(2) . . ? O21 Zn1 O11 93.1(3) . . ? O51 Zn1 O1 93.4(2) . 7_557 ? O21 Zn1 O1 98.8(2) . 7_557 ? O11 Zn1 O1 164.0(2) . 7_557 ? O51 Zn1 O1 163.7(2) . 16_446 ? O21 Zn1 O1 94.7(3) . 16_446 ? O11 Zn1 O1 91.4(2) . 16_446 ? O1 Zn1 O1 77.0(2) 7_557 16_446 ? O51 Zn1 O1 87.3(2) . . ? O21 Zn1 O1 172.3(2) . . ? O11 Zn1 O1 89.0(2) . . ? O1 Zn1 O1 77.9(2) 7_557 . ? O1 Zn1 O1 77.9(2) 16_446 . ? O12 Zn2 O31 100.2(3) . . ? O12 Zn2 O51 98.8(3) . . ? O31 Zn2 O51 97.6(3) . . ? O12 Zn2 N1 108.9(3) . . ? O31 Zn2 N1 89.7(3) . . ? O51 Zn2 N1 149.6(3) . . ? O12 Zn2 N2 110.0(3) . . ? O31 Zn2 N2 149.3(3) . . ? O51 Zn2 N2 83.9(3) . . ? N1 Zn2 N2 75.2(3) . . ? O32 Zn3 O41 105.4(4) . . ? O32 Zn3 O51 108.2(3) . . ? O41 Zn3 O51 127.8(4) . . ? O32 Zn3 O22 108.0(3) . . ? O41 Zn3 O22 103.6(4) . . ? O51 Zn3 O22 102.4(3) . . ? O32 Zn3 C41 100.6(4) . . ? O41 Zn3 C41 28.9(5) . . ? O51 Zn3 C41 105.4(5) . . ? O22 Zn3 C41 130.9(5) . . ? N2 O1 Zn1 127.2(4) . 16_446 ? N2 O1 Zn1 116.9(4) . 7_557 ? Zn1 O1 Zn1 101.9(2) 16_446 7_557 ? N2 O1 Zn1 105.2(4) . . ? Zn1 O1 Zn1 100.8(2) 16_446 . ? Zn1 O1 Zn1 100.8(2) 7_557 . ? C5 N1 C1 118.4(10) . . ? C5 N1 Zn2 115.2(6) . . ? C1 N1 Zn2 126.1(9) . . ? C6 N2 O1 117.5(7) . . ? C6 N2 Zn2 116.9(6) . . ? O1 N2 Zn2 125.6(5) . . ? C11 O11 Zn1 132.1(6) . . ? C11 O12 Zn2 118.9(6) . . ? C21 O21 Zn1 126.0(6) . . ? C21 O22 Zn3 123.1(7) . . ? C31 O31 Zn2 129.3(8) . . ? C31 O32 Zn3 125.9(7) . . ? C41 O41 Zn3 102.2(9) . . ? Zn3 O51 Zn1 114.3(3) . . ? Zn3 O51 Zn2 108.9(3) . . ? Zn1 O51 Zn2 106.3(3) . . ? N1 C1 C2 120.8(13) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 C1 120.5(13) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 118.7(13) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.0(13) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.5(10) . . ? N1 C5 C6 116.4(9) . . ? C4 C5 C6 121.0(11) . . ? N2 C6 C5 115.6(9) . . ? N2 C6 H6 122.2 . . ? C5 C6 H6 122.2 . . ? O12 C11 O11 125.4(10) . . ? O12 C11 C12 117.7(9) . . ? O11 C11 C12 116.7(10) . . ? C17 C12 C13 119.0(12) . . ? C17 C12 C11 122.2(13) . . ? C13 C12 C11 118.8(10) . . ? C12 C13 C14 120.2(14) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 113.4(17) . . ? C13 C14 H14 123.3 . . ? C15 C14 H14 123.3 . . ? C16 C15 C14 124(2) . . ? C16 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C15 C16 C17 119(2) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C12 124.3(17) . . ? C16 C17 H17 117.9 . . ? C12 C17 H17 117.9 . . ? O21 C21 O22 125.2(9) . . ? O21 C21 C22 120.1(10) . . ? O22 C21 C22 114.6(10) . . ? C27 C22 C23 118.9(10) . . ? C27 C22 C21 121.5(11) . . ? C23 C22 C21 119.6(10) . . ? C22 C23 C24 119.0(12) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 118.3(14) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C26 C25 C24 121.9(14) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 C25 119.1(13) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C22 122.6(13) . . ? C26 C27 H27 118.7 . . ? C22 C27 H27 118.7 . . ? O31 C31 O32 125.9(10) . . ? O31 C31 C32 118.3(12) . . ? O32 C31 C32 115.8(12) . . ? C37 C32 C33 120.5(14) . . ? C37 C32 C31 119.5(14) . . ? C33 C32 C31 119.9(14) . . ? C32 C33 C34 120.2(18) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119(2) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 120(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C37 119(2) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C32 C37 C36 120(2) . . ? C32 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? O42 C41 O41 124.6(14) . . ? O42 C41 C42 118.8(16) . . ? O41 C41 C42 116.6(16) . . ? O42 C41 Zn3 76.2(9) . . ? O41 C41 Zn3 48.8(7) . . ? C42 C41 Zn3 163.4(13) . . ? C47 C42 C43 120.5(15) . . ? C47 C42 C41 119.2(16) . . ? C43 C42 C41 120.2(16) . . ? C42 C43 C44 118.1(18) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 121(2) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 120(2) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C47 121(3) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C42 C47 C46 119(2) . . ? C42 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? NS1 CS1 CS2 170(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 51.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.870 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.141 # start Validation Reply Form _vrf_THETM01_pemi70 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The crystals had poor diffraction ability (despite their sufficient size) and the data were collected in increasing 2theta shells. The data collection was terminated when almost half of the collected shell data were unobserved. ; _vrf_PLAT023_pemi70 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 51.96 Deg. RESPONSE: The crystals had poor diffraction ability (despite their sufficient size) and the data were collected in increasing 2theta shells. The data collection was terminated when almost half of the collected shell data were unobserved. ; _vrf_PLAT601_pemi70 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 1031.00 A**3 RESPONSE: The structure contains MeCN and Water solvate molecules. We assume that some of these solvate molecules leave the crystal during the data collection. This explains the poor diffraction ability of the crystals and the large voids in the structure. As shown above the largest electronic density found in the difference maps is less than 1 e/A, so we avoided to include partially occupied solvate molecules to account this alert. ; _vrf_PLAT234_pemi70 ; PROBLEM: Large Hirshfeld Difference C15 -- C16 .. 0.33 Ang. RESPONSE: This alert is generated to the poor diffraction data. No action taken. ; # end Validation Reply Form # Attachment 'Complex_1.cif' data_peey1165 _database_code_depnum_ccdc_archive 'CCDC 746015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 N4 O7 Zn' _chemical_formula_weight 583.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 9.61760(10) _cell_length_b 9.76330(10) _cell_length_c 15.08780(10) _cell_angle_alpha 81.2177(10) _cell_angle_beta 82.0550(10) _cell_angle_gamma 73.1590(10) _cell_volume 1333.45(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17062 _cell_measurement_theta_min 6.97 _cell_measurement_theta_max 71.68 _exptl_crystal_description parall _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.53 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku, R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16821 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 6.97 _diffrn_reflns_theta_max 65.00 _reflns_number_total 4273 _reflns_number_gt 4009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0319P)^2^+0.7457P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4273 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.006 _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 NI Zn 0.20755(2) 0.41343(3) 0.232370(16) 0.02223(10) Uani 1 1 d . . . O1 O 0.39642(14) 0.31819(15) 0.15820(10) 0.0294(3) Uani 1 1 d . . . O2 O 0.35005(15) 0.14845(16) 0.09231(10) 0.0348(4) Uani 1 1 d . . . N21 N 0.19970(16) 0.62452(18) 0.15644(11) 0.0232(4) Uani 1 1 d . . . N22 N 0.32031(16) 0.51302(19) 0.30807(11) 0.0251(4) Uani 1 1 d . . . N31 N -0.00873(17) 0.50628(19) 0.30119(11) 0.0264(4) Uani 1 1 d . . . N32 N 0.05445(17) 0.36831(19) 0.15593(11) 0.0266(4) Uani 1 1 d . . . O11 O 0.21244(17) 0.22660(17) 0.31202(10) 0.0403(4) Uani 1 1 d . . . O12 O 0.36797(16) 0.19650(17) 0.41461(10) 0.0366(4) Uani 1 1 d . . . O21 O 0.38964(17) 0.4530(2) 0.38395(10) 0.0354(4) Uani 1 1 d . . . O31 O 0.08433(17) 0.29982(18) 0.07962(10) 0.0365(4) Uani 1 1 d . . . C1 C 0.4283(2) 0.1914(2) 0.13466(13) 0.0268(5) Uani 1 1 d . . . C2 C 0.5705(2) 0.0891(2) 0.16072(13) 0.0267(5) Uani 1 1 d . . . C3 C 0.6438(3) 0.1196(3) 0.22432(16) 0.0384(6) Uani 1 1 d . . . C4 C 0.7749(3) 0.0246(3) 0.24864(18) 0.0491(7) Uani 1 1 d . . . C5 C 0.8323(3) -0.1006(3) 0.20864(17) 0.0455(7) Uani 1 1 d . . . C6 C 0.7599(3) -0.1311(3) 0.14554(18) 0.0419(6) Uani 1 1 d . . . C7 C 0.6283(2) -0.0378(3) 0.12166(16) 0.0328(5) Uani 1 1 d . . . C11 C 0.2794(2) 0.1571(2) 0.37816(13) 0.0280(5) Uani 1 1 d . . . C12 C 0.2439(2) 0.0185(2) 0.41594(13) 0.0280(5) Uani 1 1 d . . . C13 C 0.3225(3) -0.0764(3) 0.48210(16) 0.0388(6) Uani 1 1 d . . . C14 C 0.2822(3) -0.1995(3) 0.51890(17) 0.0451(6) Uani 1 1 d . . . C15 C 0.1633(3) -0.2289(3) 0.49191(17) 0.0418(6) Uani 1 1 d . . . C16 C 0.0858(3) -0.1348(3) 0.42612(16) 0.0395(6) Uani 1 1 d . . . C17 C 0.1265(2) -0.0142(3) 0.38781(15) 0.0332(5) Uani 1 1 d . . . C21 C 0.1453(2) 0.6772(2) 0.07719(14) 0.0277(5) Uani 1 1 d . . . C22 C 0.1431(2) 0.8142(3) 0.03555(15) 0.0343(5) Uani 1 1 d . . . C23 C 0.1967(2) 0.9003(3) 0.07773(16) 0.0369(6) Uani 1 1 d . . . C24 C 0.2526(2) 0.8479(3) 0.15993(15) 0.0316(5) Uani 1 1 d . . . C25 C 0.25390(19) 0.7096(2) 0.19675(13) 0.0251(5) Uani 1 1 d . . . C26 C 0.3207(2) 0.6419(2) 0.28043(14) 0.0267(5) Uani 1 1 d . . . C31 C -0.0389(2) 0.5725(3) 0.37499(15) 0.0339(5) Uani 1 1 d . . . C32 C -0.1798(3) 0.6223(3) 0.41561(17) 0.0419(6) Uani 1 1 d . . . C33 C -0.2929(3) 0.5988(3) 0.37890(17) 0.0447(6) Uani 1 1 d . . . C34 C -0.2638(2) 0.5296(3) 0.30284(16) 0.0384(6) Uani 1 1 d . . . C35 C -0.1197(2) 0.4844(2) 0.26502(14) 0.0295(5) Uani 1 1 d . . . C36 C -0.0806(2) 0.4091(3) 0.18438(15) 0.0314(5) Uani 1 1 d . . . O1M O 0.6032(2) 0.4681(3) 0.13154(15) 0.0696(7) Uani 1 1 d . . . C1M C 0.5871(3) 0.5860(4) 0.0678(2) 0.0478(7) Uani 1 1 d . . . H21O H 0.384(3) 0.365(3) 0.396(2) 0.061(10) Uiso 1 1 d . . . H31O H 0.167(3) 0.261(3) 0.0780(19) 0.055(9) Uiso 1 1 d . . . H3 H 0.605(3) 0.203(3) 0.2494(17) 0.045(7) Uiso 1 1 d . . . H4 H 0.819(3) 0.043(3) 0.2919(18) 0.051(8) Uiso 1 1 d . . . H5 H 0.921(3) -0.164(3) 0.2233(17) 0.053(8) Uiso 1 1 d . . . H6 H 0.797(3) -0.212(3) 0.1162(17) 0.046(7) Uiso 1 1 d . . . H7 H 0.583(2) -0.058(3) 0.0846(16) 0.033(7) Uiso 1 1 d . . . H13 H 0.404(3) -0.058(3) 0.5020(16) 0.045(7) Uiso 1 1 d . . . H14 H 0.339(3) -0.268(3) 0.5606(19) 0.065(9) Uiso 1 1 d . . . H15 H 0.135(3) -0.307(3) 0.5181(16) 0.039(7) Uiso 1 1 d . . . H16 H 0.005(3) -0.154(3) 0.4105(17) 0.050(8) Uiso 1 1 d . . . H17 H 0.074(3) 0.056(3) 0.3427(17) 0.049(7) Uiso 1 1 d . . . H21 H 0.110(2) 0.617(2) 0.0520(14) 0.022(6) Uiso 1 1 d . . . H22 H 0.108(3) 0.843(3) -0.0193(17) 0.041(7) Uiso 1 1 d . . . H23 H 0.198(2) 0.988(3) 0.0537(16) 0.037(7) Uiso 1 1 d . . . H24 H 0.288(2) 0.903(3) 0.1878(15) 0.034(7) Uiso 1 1 d . . . H26 H 0.359(2) 0.695(3) 0.3122(15) 0.031(6) Uiso 1 1 d . . . H31 H 0.043(2) 0.584(2) 0.3980(14) 0.028(6) Uiso 1 1 d . . . H32 H -0.196(3) 0.674(3) 0.4666(19) 0.054(8) Uiso 1 1 d . . . H33 H -0.390(3) 0.629(3) 0.4052(17) 0.052(7) Uiso 1 1 d . . . H34 H -0.332(3) 0.510(3) 0.2765(16) 0.040(7) Uiso 1 1 d . . . H36 H -0.151(3) 0.389(3) 0.1558(16) 0.042(7) Uiso 1 1 d . . . H1OM H 0.544(3) 0.432(3) 0.1351(18) 0.048(9) Uiso 1 1 d . . . H1CM H 0.498(4) 0.628(4) 0.048(2) 0.078(10) Uiso 1 1 d . . . H2CM H 0.618(5) 0.656(6) 0.085(3) 0.16(2) Uiso 1 1 d . . . H3CM H 0.639(4) 0.561(5) 0.015(3) 0.115(15) Uiso 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 NI 0.01939(14) 0.02163(17) 0.02639(15) 0.00069(11) -0.00636(10) -0.00671(11) O1 0.0205(7) 0.0219(8) 0.0459(9) -0.0080(6) -0.0011(6) -0.0050(6) O2 0.0281(7) 0.0292(9) 0.0496(9) -0.0098(7) -0.0113(6) -0.0056(6) N21 0.0192(8) 0.0208(9) 0.0292(9) -0.0011(7) -0.0027(6) -0.0056(7) N22 0.0213(8) 0.0286(10) 0.0260(8) 0.0004(7) -0.0051(6) -0.0084(7) N31 0.0256(8) 0.0268(10) 0.0277(9) -0.0002(7) -0.0025(6) -0.0101(7) N32 0.0257(9) 0.0259(10) 0.0285(9) -0.0006(7) -0.0081(7) -0.0065(7) O11 0.0460(9) 0.0348(10) 0.0447(9) 0.0182(7) -0.0235(7) -0.0212(7) O12 0.0414(8) 0.0322(9) 0.0400(9) 0.0060(7) -0.0166(7) -0.0153(7) O21 0.0416(9) 0.0361(10) 0.0338(8) 0.0066(7) -0.0196(6) -0.0172(8) O31 0.0274(8) 0.0442(11) 0.0395(9) -0.0143(7) -0.0105(6) -0.0043(7) C1 0.0238(10) 0.0244(12) 0.0306(11) -0.0012(9) 0.0001(8) -0.0065(9) C2 0.0227(9) 0.0248(12) 0.0300(11) 0.0004(9) -0.0008(8) -0.0052(8) C3 0.0362(12) 0.0348(15) 0.0417(13) -0.0089(11) -0.0085(10) -0.0013(11) C4 0.0395(13) 0.0565(19) 0.0484(15) -0.0062(13) -0.0209(11) -0.0009(12) C5 0.0302(12) 0.0412(16) 0.0527(15) 0.0049(12) -0.0080(10) 0.0058(11) C6 0.0379(13) 0.0279(14) 0.0519(15) -0.0048(11) 0.0009(11) 0.0011(11) C7 0.0291(11) 0.0289(13) 0.0393(13) -0.0055(10) -0.0037(9) -0.0053(9) C11 0.0255(10) 0.0259(12) 0.0296(11) 0.0010(9) -0.0030(8) -0.0046(9) C12 0.0287(10) 0.0255(12) 0.0277(10) 0.0001(9) -0.0030(8) -0.0058(9) C13 0.0376(13) 0.0360(15) 0.0440(13) 0.0088(11) -0.0143(10) -0.0143(11) C14 0.0523(15) 0.0354(15) 0.0468(14) 0.0151(12) -0.0200(12) -0.0142(12) C15 0.0530(15) 0.0292(14) 0.0455(14) 0.0064(11) -0.0073(11) -0.0192(12) C16 0.0398(13) 0.0342(15) 0.0492(14) -0.0022(11) -0.0118(10) -0.0157(11) C17 0.0345(11) 0.0293(13) 0.0347(12) 0.0015(10) -0.0096(9) -0.0067(10) C21 0.0264(10) 0.0274(13) 0.0300(11) -0.0039(9) -0.0049(8) -0.0073(9) C22 0.0386(12) 0.0313(13) 0.0312(12) 0.0051(10) -0.0089(9) -0.0085(10) C23 0.0410(13) 0.0277(14) 0.0407(13) 0.0070(11) -0.0050(10) -0.0124(10) C24 0.0330(11) 0.0279(13) 0.0377(12) -0.0037(10) -0.0036(9) -0.0144(10) C25 0.0193(9) 0.0253(12) 0.0299(10) -0.0022(9) -0.0005(7) -0.0061(8) C26 0.0241(10) 0.0292(13) 0.0302(11) -0.0052(9) -0.0042(8) -0.0113(9) C31 0.0345(12) 0.0357(14) 0.0349(12) -0.0040(10) -0.0002(9) -0.0165(10) C32 0.0458(14) 0.0421(15) 0.0367(13) -0.0078(11) 0.0078(10) -0.0141(11) C33 0.0300(12) 0.0533(17) 0.0433(14) -0.0026(12) 0.0061(10) -0.0056(11) C34 0.0239(11) 0.0503(16) 0.0402(13) 0.0002(11) -0.0042(9) -0.0113(10) C35 0.0253(10) 0.0302(12) 0.0321(11) 0.0041(9) -0.0054(8) -0.0090(9) C36 0.0227(10) 0.0373(14) 0.0376(12) -0.0028(10) -0.0107(9) -0.0108(9) O1M 0.0528(12) 0.0824(17) 0.0866(15) 0.0375(13) -0.0378(11) -0.0488(12) C1M 0.0423(15) 0.0467(18) 0.0537(17) 0.0019(14) -0.0033(12) -0.0158(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 NI O11 2.0174(14) . ? NI O1 2.0479(13) . ? NI N32 2.1663(17) . ? NI N22 2.1723(17) . ? NI N21 2.1860(16) . ? NI N31 2.1965(16) . ? O1 C1 1.279(3) . ? O2 C1 1.244(3) . ? N21 C21 1.340(3) . ? N21 C25 1.350(3) . ? N22 C26 1.265(3) . ? N22 O21 1.371(2) . ? N31 C31 1.328(3) . ? N31 C35 1.346(3) . ? N32 C36 1.276(3) . ? N32 O31 1.374(2) . ? O11 C11 1.261(2) . ? O12 C11 1.249(3) . ? O21 H21O 0.86(3) . ? O31 H31O 0.78(3) . ? C1 C2 1.504(3) . ? C2 C3 1.379(3) . ? C2 C7 1.388(3) . ? C3 C4 1.389(3) . ? C3 H3 0.91(3) . ? C4 C5 1.380(4) . ? C4 H4 0.89(3) . ? C5 C6 1.368(4) . ? C5 H5 0.93(3) . ? C6 C7 1.385(3) . ? C6 H6 0.92(3) . ? C7 H7 0.83(2) . ? C11 C12 1.500(3) . ? C12 C17 1.393(3) . ? C12 C13 1.395(3) . ? C13 C14 1.382(3) . ? C13 H13 0.95(3) . ? C14 C15 1.382(4) . ? C14 H14 0.94(3) . ? C15 C16 1.383(3) . ? C15 H15 0.90(3) . ? C16 C17 1.368(3) . ? C16 H16 0.92(3) . ? C17 H17 0.97(3) . ? C21 C22 1.384(3) . ? C21 H21 0.91(2) . ? C22 C23 1.372(4) . ? C22 H22 0.91(2) . ? C23 C24 1.386(3) . ? C23 H23 0.88(3) . ? C24 C25 1.377(3) . ? C24 H24 0.90(2) . ? C25 C26 1.472(3) . ? C26 H26 0.93(2) . ? C31 C32 1.389(3) . ? C31 H31 0.95(2) . ? C32 C33 1.376(4) . ? C32 H32 0.96(3) . ? C33 C34 1.375(4) . ? C33 H33 0.94(3) . ? C34 C35 1.395(3) . ? C34 H34 0.89(3) . ? C35 C36 1.466(3) . ? C36 H36 0.93(2) . ? O1M C1M 1.369(3) . ? O1M H1OM 0.75(3) . ? C1M H1CM 0.91(3) . ? C1M H2CM 0.91(5) . ? C1M H3CM 0.91(4) . ? 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 O11 NI O1 91.39(6) . . ? O11 NI N32 88.58(6) . . ? O1 NI N32 98.20(6) . . ? O11 NI N22 101.34(6) . . ? O1 NI N22 92.60(6) . . ? N32 NI N22 165.18(6) . . ? O11 NI N21 175.16(7) . . ? O1 NI N21 91.69(6) . . ? N32 NI N21 94.67(6) . . ? N22 NI N21 74.79(6) . . ? O11 NI N31 88.11(7) . . ? O1 NI N31 173.14(6) . . ? N32 NI N31 74.95(6) . . ? N22 NI N31 94.21(6) . . ? N21 NI N31 89.28(6) . . ? C1 O1 NI 124.84(12) . . ? C21 N21 C25 118.17(18) . . ? C21 N21 NI 127.29(15) . . ? C25 N21 NI 114.53(12) . . ? C26 N22 O21 115.65(18) . . ? C26 N22 NI 116.91(13) . . ? O21 N22 NI 127.43(14) . . ? C31 N31 C35 118.44(18) . . ? C31 N31 NI 127.46(14) . . ? C35 N31 NI 114.00(14) . . ? C36 N32 O31 114.93(17) . . ? C36 N32 NI 117.09(15) . . ? O31 N32 NI 127.98(12) . . ? C11 O11 NI 135.99(15) . . ? N22 O21 H21O 107(2) . . ? N32 O31 H31O 104(2) . . ? O2 C1 O1 124.51(18) . . ? O2 C1 C2 118.72(19) . . ? O1 C1 C2 116.77(18) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 120.4(2) . . ? C7 C2 C1 120.2(2) . . ? C2 C3 C4 120.3(2) . . ? C2 C3 H3 118.6(16) . . ? C4 C3 H3 121.1(16) . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.7(17) . . ? C3 C4 H4 119.4(18) . . ? C6 C5 C4 120.0(2) . . ? C6 C5 H5 119.6(17) . . ? C4 C5 H5 120.4(17) . . ? C5 C6 C7 120.6(2) . . ? C5 C6 H6 122.0(16) . . ? C7 C6 H6 117.3(16) . . ? C6 C7 C2 119.9(2) . . ? C6 C7 H7 120.1(17) . . ? C2 C7 H7 120.0(17) . . ? O12 C11 O11 125.2(2) . . ? O12 C11 C12 119.03(18) . . ? O11 C11 C12 115.71(19) . . ? C17 C12 C13 118.8(2) . . ? C17 C12 C11 119.89(18) . . ? C13 C12 C11 121.2(2) . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 119.4(15) . . ? C12 C13 H13 120.8(15) . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 118.8(18) . . ? C13 C14 H14 120.4(18) . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15 120.5(15) . . ? C16 C15 H15 120.2(15) . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 121.0(17) . . ? C15 C16 H16 118.5(17) . . ? C16 C17 C12 120.8(2) . . ? C16 C17 H17 123.6(15) . . ? C12 C17 H17 115.5(15) . . ? N21 C21 C22 122.6(2) . . ? N21 C21 H21 115.7(13) . . ? C22 C21 H21 121.7(13) . . ? C23 C22 C21 118.6(2) . . ? C23 C22 H22 122.3(16) . . ? C21 C22 H22 119.0(16) . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H23 121.9(16) . . ? C24 C23 H23 118.6(16) . . ? C25 C24 C23 118.8(2) . . ? C25 C24 H24 121.3(15) . . ? C23 C24 H24 120.0(15) . . ? N21 C25 C24 122.25(19) . . ? N21 C25 C26 115.41(18) . . ? C24 C25 C26 122.3(2) . . ? N22 C26 C25 118.0(2) . . ? N22 C26 H26 122.1(14) . . ? C25 C26 H26 119.9(14) . . ? N31 C31 C32 123.0(2) . . ? N31 C31 H31 115.0(13) . . ? C32 C31 H31 122.0(13) . . ? C33 C32 C31 118.4(2) . . ? C33 C32 H32 122.2(16) . . ? C31 C32 H32 119.4(16) . . ? C34 C33 C32 119.4(2) . . ? C34 C33 H33 119.5(16) . . ? C32 C33 H33 121.1(16) . . ? C33 C34 C35 118.9(2) . . ? C33 C34 H34 123.9(16) . . ? C35 C34 H34 117.2(16) . . ? N31 C35 C34 121.7(2) . . ? N31 C35 C36 116.36(17) . . ? C34 C35 C36 121.9(2) . . ? N32 C36 C35 117.54(19) . . ? N32 C36 H36 120.9(15) . . ? C35 C36 H36 121.6(15) . . ? C1M O1M H1OM 114(2) . . ? O1M C1M H1CM 119(2) . . ? O1M C1M H2CM 112(3) . . ? H1CM C1M H2CM 107(4) . . ? O1M C1M H3CM 111(3) . . ? H1CM C1M H3CM 99(3) . . ? H2CM C1M H3CM 108(4) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.305 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.049 # start Validation Reply Form _vrf_PLAT029_peey1165 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94 RESPONSE: This is a usual problem with small unit cells and Cu radiation. All possible images were collected. ;