# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yangguang Li' _publ_contact_author_email liyg658@nenu.edu.cn loop_ _publ_author_name 'Xin Wang' 'Wei Yao' 'Yan-Fei Qi' 'Ming-Fa Luo' 'Yong-Hui Wang' 'Hong-Wei Xie' 'Yang Yu' 'Yang-Guang Li' data_wyh1 _database_code_depnum_ccdc_archive 'CCDC 771007' #TrackingRef '747_web_deposit_cif_file_0_wangxin_1269392369.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 Cd3 N6 O15.50' _chemical_formula_weight 1402.30 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' Cd Cd -0.8075 1.2024 '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 32.207(6) _cell_length_b 13.378(3) _cell_length_c 15.871(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.05(3) _cell_angle_gamma 90.00 _cell_volume 6837(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7699 _exptl_absorpt_correction_T_max 0.8051 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March,1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 32051 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7784 _reflns_number_gt 5840 _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^)+(0.0955P)^2^+23.3672P] 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 7784 _refine_ls_number_parameters 401 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1826 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.066 _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 Cd1 Cd 0.606010(13) 0.69508(3) 0.23557(3) 0.02376(15) Uani 1 1 d . . . Cd2 Cd 0.5000 0.77497(4) 0.2500 0.02235(16) Uani 1 2 d S . . O1 O 0.55887(13) 0.7705(3) 0.3423(3) 0.0307(10) Uani 1 1 d . . . O2 O 0.62626(14) 0.8015(3) 0.3467(3) 0.0377(11) Uani 1 1 d . . . O3 O 0.53108(14) 1.1165(3) 0.6672(3) 0.0370(10) Uani 1 1 d . . . O4 O 0.59681(14) 1.1680(4) 0.6541(3) 0.0387(11) Uani 1 1 d . . . O5 O 0.59067(13) 0.5867(3) 0.1230(3) 0.0349(10) Uani 1 1 d . . . O6 O 0.53544(14) 0.6471(3) 0.1852(3) 0.0326(10) Uani 1 1 d . . . N1 N 0.61699(18) 0.5566(4) 0.3215(3) 0.0365(13) Uani 1 1 d . . . N2 N 0.67577(17) 0.6989(4) 0.1983(4) 0.0374(13) Uani 1 1 d . . . C1 C 0.58404(19) 0.8900(5) 0.4434(4) 0.0312(14) Uani 1 1 d . . . C2 C 0.6162(2) 0.9545(5) 0.4667(4) 0.0324(14) Uani 1 1 d . . . H2 H 0.6422 0.9496 0.4395 0.032 Uiso 1 1 calc R . . C3 C 0.61085(19) 1.0251(5) 0.5283(4) 0.0323(14) Uani 1 1 d . . . H3 H 0.6329 1.0697 0.5422 0.032 Uiso 1 1 calc R . . C4 C 0.57333(19) 1.0320(5) 0.5708(4) 0.0284(13) Uani 1 1 d . . . C5 C 0.54208(19) 0.9649(5) 0.5502(4) 0.0314(14) Uani 1 1 d . . . H5 H 0.5169 0.9667 0.5804 0.031 Uiso 1 1 calc R . . C6 C 0.54670(19) 0.8940(5) 0.4854(4) 0.0305(13) Uani 1 1 d . . . H6 H 0.5246 0.8498 0.4707 0.030 Uiso 1 1 calc R . . C7 C 0.5902(2) 0.8161(4) 0.3730(4) 0.0279(13) Uani 1 1 d . . . C8 C 0.56661(19) 1.1130(5) 0.6364(4) 0.0276(13) Uani 1 1 d . . . C9 C 0.52497(18) 0.5478(5) 0.0609(4) 0.0268(12) Uani 1 1 d . . . C10 C 0.54218(19) 0.4831(5) 0.0040(4) 0.0332(14) Uani 1 1 d . . . H10 H 0.5713 0.4712 0.0068 0.033 Uiso 1 1 calc R . . C11 C 0.51820(19) 0.4342(5) -0.0579(4) 0.0329(14) Uani 1 1 d . . . H11 H 0.5307 0.3901 -0.0968 0.033 Uiso 1 1 calc R . . C12 C 0.55159(18) 0.5971(4) 0.1263(4) 0.0258(12) Uani 1 1 d . . . C13 C 0.6436(2) 0.5590(6) 0.3879(5) 0.0472(19) Uani 1 1 d . . . H13 H 0.6564 0.6207 0.4027 0.047 Uiso 1 1 calc R . . C14 C 0.6532(2) 0.4741(6) 0.4358(5) 0.050(2) Uani 1 1 d . . . H14 H 0.6729 0.4783 0.4809 0.050 Uiso 1 1 calc R . . C15 C 0.6340(2) 0.3842(6) 0.4180(4) 0.0404(16) Uani 1 1 d . . . C16 C 0.6057(3) 0.3833(6) 0.3525(5) 0.050(2) Uani 1 1 d . . . H16 H 0.5907 0.3240 0.3393 0.050 Uiso 1 1 calc R . . C17 C 0.5991(3) 0.4701(6) 0.3052(5) 0.053(2) Uani 1 1 d . . . H17 H 0.5804 0.4664 0.2583 0.053 Uiso 1 1 calc R . . C18 C 0.6947(3) 0.7870(7) 0.1962(6) 0.059(2) Uani 1 1 d . . . H18 H 0.6791 0.8460 0.2066 0.059 Uiso 1 1 calc R . . C19 C 0.7361(3) 0.7948(7) 0.1793(7) 0.071(3) Uani 1 1 d . . . H19 H 0.7492 0.8584 0.1815 0.071 Uiso 1 1 calc R . . C20 C 0.7594(2) 0.7104(7) 0.1587(6) 0.055(2) Uani 1 1 d . . . C21 C 0.7382(3) 0.6201(7) 0.1575(7) 0.070(3) Uani 1 1 d . . . H21 H 0.7520 0.5598 0.1433 0.070 Uiso 1 1 calc R . . C22 C 0.6973(2) 0.6195(6) 0.1770(6) 0.056(2) Uani 1 1 d . . . H22 H 0.6832 0.5571 0.1751 0.056 Uiso 1 1 calc R . . C23 C 0.6442(2) 0.2903(6) 0.4671(5) 0.0466(18) Uani 1 1 d . . . H23A H 0.6251 0.2360 0.4491 0.047 Uiso 1 1 calc R . . H23B H 0.6402 0.3025 0.5279 0.047 Uiso 1 1 calc R . . C24 C 0.6894(2) 0.2578(7) 0.4526(5) 0.053(2) Uani 1 1 d . . . H24A H 0.7082 0.3151 0.4631 0.053 Uiso 1 1 calc R . . H24B H 0.6971 0.2040 0.4928 0.053 Uiso 1 1 calc R . . C25 C 0.8053(2) 0.7205(8) 0.1369(6) 0.067(3) Uani 1 1 d . . . H25A H 0.8189 0.7678 0.1767 0.067 Uiso 1 1 calc R . . H25B H 0.8190 0.6548 0.1434 0.067 Uiso 1 1 calc R . . C27 C 0.5654(5) 0.9147(12) 0.7852(10) 0.131(5) Uani 1 1 d U . . H27A H 0.5454 0.8606 0.7751 0.131 Uiso 0.50 1 calc PR A 1 H27B H 0.5533 0.9783 0.7666 0.131 Uiso 0.50 1 calc PR A 1 H27C H 0.5723 0.9183 0.8455 0.131 Uiso 0.50 1 calc PR A 1 H27D H 0.5722 0.9305 0.7268 0.131 Uiso 0.50 1 calc PR A 2 H27F H 0.5911 0.9073 0.8186 0.131 Uiso 0.50 1 calc PR A 2 H27G H 0.5487 0.9688 0.8086 0.131 Uiso 0.50 1 calc PR A 2 N3A N 0.6033(5) 0.8948(14) 0.7380(10) 0.073(5) Uani 0.50 1 d PU B 1 C26A C 0.6100(7) 0.8081(15) 0.6787(14) 0.077(6) Uani 0.50 1 d PU B 1 H26A H 0.5857 0.7642 0.6791 0.077 Uiso 0.50 1 calc PR B 1 H26B H 0.6346 0.7705 0.6972 0.077 Uiso 0.50 1 calc PR B 1 H26C H 0.6140 0.8335 0.6215 0.077 Uiso 0.50 1 calc PR B 1 C28A C 0.6326(6) 0.9606(15) 0.7458(12) 0.065(5) Uani 0.50 1 d PU B 1 H28A H 0.6277 1.0168 0.7808 0.065 Uiso 0.50 1 calc PR B 1 O7A O 0.6664(5) 0.9554(12) 0.7109(10) 0.091(5) Uani 0.50 1 d PU B 1 N3B N 0.5423(8) 0.8226(18) 0.7875(16) 0.111(7) Uani 0.50 1 d PU B 2 C26B C 0.5297(8) 0.791(2) 0.8684(16) 0.094(7) Uani 0.50 1 d PU B 2 H26D H 0.5150 0.7268 0.8633 0.094 Uiso 0.50 1 calc PR B 2 H26E H 0.5113 0.8409 0.8927 0.094 Uiso 0.50 1 calc PR B 2 H26F H 0.5543 0.7822 0.9051 0.094 Uiso 0.50 1 calc PR B 2 C28B C 0.5391(7) 0.7659(18) 0.7113(14) 0.082(6) Uani 0.50 1 d PU B 2 H28B H 0.5538 0.7844 0.6623 0.082 Uiso 0.50 1 calc PR B 2 O7B O 0.5071(6) 0.6617(14) 0.7128(11) 0.106(6) Uani 0.50 1 d PU . 2 OW1 O 0.4956(11) 0.698(2) 0.643(2) 0.200(13) Uiso 0.50 1 d P C 3 OW2 O 0.7298(12) 0.968(3) 0.541(2) 0.121(12) Uiso 0.25 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 Cd1 0.0271(2) 0.0233(2) 0.0209(2) -0.00194(15) -0.00069(16) 0.00060(16) Cd2 0.0253(3) 0.0235(3) 0.0184(3) 0.000 0.0020(2) 0.000 O1 0.038(2) 0.032(2) 0.022(2) -0.0021(18) -0.0070(18) -0.0010(19) O2 0.037(2) 0.040(3) 0.036(3) -0.015(2) 0.002(2) 0.005(2) O3 0.037(2) 0.037(3) 0.038(3) -0.015(2) 0.008(2) 0.002(2) O4 0.041(3) 0.033(2) 0.042(3) -0.017(2) -0.002(2) -0.003(2) O5 0.032(2) 0.043(3) 0.030(2) -0.010(2) -0.0008(19) -0.002(2) O6 0.041(2) 0.029(2) 0.027(2) -0.0108(18) 0.0016(19) 0.0011(19) N1 0.044(3) 0.034(3) 0.031(3) 0.001(2) -0.004(2) 0.003(3) N2 0.033(3) 0.037(3) 0.042(3) -0.004(2) 0.004(3) -0.001(2) C1 0.036(3) 0.035(3) 0.022(3) -0.002(3) -0.003(3) 0.000(3) C2 0.030(3) 0.035(4) 0.032(3) -0.009(3) 0.002(3) 0.001(3) C3 0.027(3) 0.033(3) 0.036(3) -0.006(3) -0.001(3) -0.004(3) C4 0.037(3) 0.029(3) 0.019(3) -0.002(2) -0.003(2) 0.004(3) C5 0.026(3) 0.038(4) 0.030(3) -0.007(3) 0.005(2) -0.002(3) C6 0.031(3) 0.033(3) 0.027(3) -0.002(3) -0.003(3) -0.002(3) C7 0.036(3) 0.026(3) 0.022(3) -0.003(2) 0.001(2) 0.003(3) C8 0.031(3) 0.028(3) 0.023(3) 0.001(2) -0.002(2) 0.006(3) C9 0.028(3) 0.030(3) 0.022(3) -0.004(2) 0.002(2) -0.004(2) C10 0.022(3) 0.047(4) 0.031(3) -0.014(3) 0.002(2) -0.004(3) C11 0.032(3) 0.036(4) 0.031(3) -0.015(3) 0.004(3) 0.003(3) C12 0.031(3) 0.023(3) 0.024(3) -0.003(2) 0.001(2) 0.000(2) C13 0.051(4) 0.046(4) 0.045(4) 0.003(3) -0.019(4) -0.004(4) C14 0.052(4) 0.055(5) 0.043(4) 0.010(4) -0.017(4) 0.001(4) C15 0.044(4) 0.041(4) 0.037(4) 0.010(3) 0.015(3) 0.012(3) C16 0.069(5) 0.031(4) 0.049(4) 0.007(3) -0.019(4) -0.009(4) C17 0.070(5) 0.032(4) 0.057(5) 0.003(3) -0.028(4) -0.005(4) C18 0.038(4) 0.054(5) 0.086(7) -0.017(5) 0.010(4) -0.005(4) C19 0.053(5) 0.056(6) 0.105(8) -0.017(5) 0.026(5) -0.027(4) C20 0.033(4) 0.073(6) 0.060(5) 0.014(4) 0.003(4) 0.003(4) C21 0.048(5) 0.042(5) 0.123(9) 0.006(5) 0.030(5) 0.000(4) C22 0.040(4) 0.040(4) 0.088(6) 0.004(4) 0.017(4) -0.008(3) C23 0.041(4) 0.049(5) 0.050(4) 0.018(4) 0.007(3) 0.011(3) C24 0.046(4) 0.063(5) 0.050(5) 0.020(4) 0.009(4) 0.012(4) C25 0.032(4) 0.090(7) 0.078(7) 0.024(5) 0.004(4) -0.007(4) C27 0.145(9) 0.118(9) 0.129(9) 0.004(7) -0.025(7) 0.000(7) N3A 0.080(8) 0.068(8) 0.071(8) 0.012(6) -0.017(7) 0.000(7) C26A 0.094(10) 0.066(9) 0.070(9) 0.006(7) -0.018(8) -0.003(8) C28A 0.066(8) 0.061(8) 0.068(8) 0.001(7) -0.015(7) 0.005(7) O7A 0.105(8) 0.083(8) 0.084(8) 0.012(6) -0.023(7) 0.004(7) N3B 0.120(11) 0.097(10) 0.117(11) 0.001(8) 0.001(8) 0.005(8) C26B 0.090(10) 0.101(11) 0.091(10) 0.009(8) 0.007(8) 0.024(8) C28B 0.086(9) 0.092(10) 0.068(9) -0.010(8) 0.003(8) 0.013(8) O7B 0.112(9) 0.106(9) 0.100(9) -0.018(7) -0.001(8) 0.028(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 Cd1 O4 2.258(4) 6_575 ? Cd1 N1 2.324(5) . ? Cd1 N2 2.334(6) . ? Cd1 O5 2.347(4) . ? Cd1 O2 2.350(4) . ? Cd1 O6 2.480(4) . ? Cd1 O1 2.507(4) . ? Cd2 O3 2.211(4) 6_575 ? Cd2 O3 2.211(4) 5_676 ? Cd2 O6 2.309(4) . ? Cd2 O6 2.309(4) 2_655 ? Cd2 O1 2.375(4) . ? Cd2 O1 2.375(4) 2_655 ? O1 C7 1.268(7) . ? O2 C7 1.257(8) . ? O3 C8 1.253(7) . ? O3 Cd2 2.211(4) 5_676 ? O4 C8 1.247(7) . ? O4 Cd1 2.258(4) 6_576 ? O5 C12 1.268(7) . ? O6 C12 1.269(7) . ? N1 C17 1.317(9) . ? N1 C13 1.346(8) . ? N2 C22 1.317(10) . ? N2 C18 1.327(10) . ? C1 C6 1.386(9) . ? C1 C2 1.394(9) . ? C1 C7 1.508(8) . ? C2 C3 1.373(9) . ? C2 H2 0.9500 . ? C3 C4 1.398(9) . ? C3 H3 0.9500 . ? C4 C5 1.383(9) . ? C4 C8 1.521(8) . ? C5 C6 1.410(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C9 C10 1.375(8) . ? C9 C11 1.411(8) 5_665 ? C9 C12 1.487(8) . ? C10 C11 1.401(8) . ? C10 H10 0.9500 . ? C11 C9 1.411(8) 5_665 ? C11 H11 0.9500 . ? C13 C14 1.399(10) . ? C13 H13 0.9500 . ? C14 C15 1.378(11) . ? C14 H14 0.9500 . ? C15 C16 1.370(10) . ? C15 C23 1.512(9) . ? C16 C17 1.397(10) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.369(12) . ? C18 H18 0.9500 . ? C19 C20 1.398(13) . ? C19 H19 0.9500 . ? C20 C21 1.388(12) . ? C20 C25 1.529(11) . ? C21 C22 1.357(11) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.540(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.518(12) 4_645 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C24 1.518(12) 4_655 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 N3B 1.44(3) . ? C27 N3A 1.47(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27F 0.9800 . ? C27 H27G 0.9800 . ? N3A C28A 1.29(2) . ? N3A C26A 1.51(3) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C28A O7A 1.23(2) . ? C28A H28A 0.9500 . ? N3B C26B 1.42(3) . ? N3B C28B 1.43(3) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C28B O7B 1.73(3) . ? C28B H28B 0.9500 . ? O7B O7B 1.27(3) 2_656 ? 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 Cd1 N1 178.34(19) 6_575 . ? O4 Cd1 N2 87.35(19) 6_575 . ? N1 Cd1 N2 91.7(2) . . ? O4 Cd1 O5 92.39(17) 6_575 . ? N1 Cd1 O5 88.99(18) . . ? N2 Cd1 O5 90.61(18) . . ? O4 Cd1 O2 88.27(17) 6_575 . ? N1 Cd1 O2 90.30(18) . . ? N2 Cd1 O2 85.51(18) . . ? O5 Cd1 O2 176.04(16) . . ? O4 Cd1 O6 85.15(16) 6_575 . ? N1 Cd1 O6 96.41(17) . . ? N2 Cd1 O6 143.56(17) . . ? O5 Cd1 O6 54.23(14) . . ? O2 Cd1 O6 129.72(15) . . ? O4 Cd1 O1 89.17(16) 6_575 . ? N1 Cd1 O1 90.66(17) . . ? N2 Cd1 O1 139.47(17) . . ? O5 Cd1 O1 129.89(14) . . ? O2 Cd1 O1 54.01(15) . . ? O6 Cd1 O1 76.07(13) . . ? O3 Cd2 O3 97.9(3) 6_575 5_676 ? O3 Cd2 O6 89.35(17) 6_575 . ? O3 Cd2 O6 169.93(17) 5_676 . ? O3 Cd2 O6 169.93(17) 6_575 2_655 ? O3 Cd2 O6 89.35(17) 5_676 2_655 ? O6 Cd2 O6 84.4(2) . 2_655 ? O3 Cd2 O1 91.05(16) 6_575 . ? O3 Cd2 O1 90.86(16) 5_676 . ? O6 Cd2 O1 81.98(15) . . ? O6 Cd2 O1 95.85(15) 2_655 . ? O3 Cd2 O1 90.86(16) 6_575 2_655 ? O3 Cd2 O1 91.05(16) 5_676 2_655 ? O6 Cd2 O1 95.85(15) . 2_655 ? O6 Cd2 O1 81.98(15) 2_655 2_655 ? O1 Cd2 O1 177.1(2) . 2_655 ? C7 O1 Cd2 147.6(4) . . ? C7 O1 Cd1 88.0(4) . . ? Cd2 O1 Cd1 94.60(14) . . ? C7 O2 Cd1 95.5(4) . . ? C8 O3 Cd2 133.1(4) . 5_676 ? C8 O4 Cd1 134.5(4) . 6_576 ? C12 O5 Cd1 95.5(3) . . ? C12 O6 Cd2 158.7(4) . . ? C12 O6 Cd1 89.4(3) . . ? Cd2 O6 Cd1 97.01(15) . . ? C17 N1 C13 116.4(6) . . ? C17 N1 Cd1 121.6(4) . . ? C13 N1 Cd1 121.9(5) . . ? C22 N2 C18 117.8(7) . . ? C22 N2 Cd1 124.2(5) . . ? C18 N2 Cd1 118.0(5) . . ? C6 C1 C2 119.7(6) . . ? C6 C1 C7 120.5(6) . . ? C2 C1 C7 119.7(6) . . ? C3 C2 C1 120.8(6) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.7(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.3(6) . . ? C5 C4 C8 120.8(6) . . ? C3 C4 C8 120.8(6) . . ? C4 C5 C6 121.6(6) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 118.8(6) . . ? C1 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? O2 C7 O1 122.1(5) . . ? O2 C7 C1 118.8(5) . . ? O1 C7 C1 119.1(6) . . ? O4 C8 O3 127.2(6) . . ? O4 C8 C4 117.0(5) . . ? O3 C8 C4 115.8(5) . . ? C10 C9 C11 119.6(5) . 5_665 ? C10 C9 C12 120.2(5) . . ? C11 C9 C12 120.2(5) 5_665 . ? C9 C10 C11 122.1(6) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C9 118.4(6) . 5_665 ? C10 C11 H11 120.8 . . ? C9 C11 H11 120.8 5_665 . ? O5 C12 O6 120.5(5) . . ? O5 C12 C9 118.9(5) . . ? O6 C12 C9 120.6(5) . . ? N1 C13 C14 122.5(7) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 120.2(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 116.9(6) . . ? C16 C15 C23 121.2(7) . . ? C14 C15 C23 121.8(7) . . ? C15 C16 C17 119.6(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N1 C17 C16 124.2(7) . . ? N1 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? N2 C18 C19 121.4(8) . . ? N2 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C20 120.9(8) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 116.1(7) . . ? C21 C20 C25 123.5(9) . . ? C19 C20 C25 120.4(8) . . ? C22 C21 C20 118.7(8) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N2 C22 C21 124.9(8) . . ? N2 C22 H22 117.6 . . ? C21 C22 H22 117.6 . . ? C15 C23 C24 110.8(6) . . ? C15 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? C15 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 110.8(7) 4_645 . ? C25 C24 H24A 109.5 4_645 . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 4_645 . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C20 111.5(7) 4_655 . ? C24 C25 H25A 109.3 4_655 . ? C20 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 4_655 . ? C20 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N3B C27 N3A 107.1(17) . . ? N3B C27 H27A 15.0 . . ? N3A C27 H27A 109.5 . . ? N3B C27 H27B 123.1 . . ? N3A C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3B C27 H27C 97.2 . . ? N3A C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3B C27 H27D 109.5 . . ? N3A C27 H27D 49.7 . . ? H27A C27 H27D 99.3 . . ? H27B C27 H27D 67.8 . . ? H27C C27 H27D 149.7 . . ? N3B C27 H27F 109.5 . . ? N3A C27 H27F 63.7 . . ? H27A C27 H27F 124.2 . . ? H27B C27 H27F 125.4 . . ? H27C C27 H27F 45.8 . . ? H27D C27 H27F 109.5 . . ? N3B C27 H27G 109.5 . . ? N3A C27 H27G 142.7 . . ? H27A C27 H27G 104.0 . . ? H27B C27 H27G 41.7 . . ? H27C C27 H27G 73.0 . . ? H27D C27 H27G 109.5 . . ? H27F C27 H27G 109.5 . . ? C28A N3A C27 116.0(18) . . ? C28A N3A C26A 118.0(19) . . ? C27 N3A C26A 125.9(17) . . ? N3A C26A H26A 109.5 . . ? N3A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? N3A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? O7A C28A N3A 124(2) . . ? O7A C28A H28A 117.8 . . ? N3A C28A H28A 117.8 . . ? C26B N3B C28B 126(2) . . ? C26B N3B C27 116(2) . . ? C28B N3B C27 117(2) . . ? N3B C26B H26D 109.5 . . ? N3B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? N3B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? N3B C28B O7B 117(2) . . ? N3B C28B H28B 121.7 . . ? O7B C28B H28B 121.7 . . ? O7B O7B C28B 103.7(14) 2_656 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.226 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.157 data_test _database_code_depnum_ccdc_archive 'CCDC 790253' #TrackingRef 'web_deposit_cif_file_0_wangxin_1282551306.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 N4 O4 Zn' _chemical_formula_weight 503.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 ? _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.640(2) _cell_length_b 20.436(4) _cell_length_c 9.7263(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2313.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8266 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 20589 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2693 _reflns_number_gt 2337 _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. During the refinement, the carboxylate ligands are disordered in two position with the site occupancies of 25% and 25%, respectively. Some the disordered carboxylate rings exhibit poor structural precision and must be fixed in a chemically suitable positions with restraint commands. All these commands lead to a restraint number 18. ; _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^+4.2931P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(2) _refine_ls_number_reflns 2693 _refine_ls_number_parameters 180 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.274 _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 0.52967(5) 0.2500 0.16422(6) 0.03437(19) Uani 1 2 d S . . O1 O 0.4896(3) 0.2500 0.4577(5) 0.0775(17) Uani 1 2 d S . . O2 O 0.6357(3) 0.2500 0.3164(4) 0.0458(9) Uani 1 2 d S . . O4 O 0.6693(6) 0.3321(3) 0.9686(8) 0.0670(18) Uani 0.50 1 d P . . N1 N 0.4237(2) 0.16868(15) 0.1610(3) 0.0374(7) Uani 1 1 d . . . N2 N 0.1166(2) 0.00313(13) 0.0483(3) 0.0358(6) Uani 1 1 d . . . C1 C 0.3427(3) 0.16024(18) 0.2564(4) 0.0409(8) Uani 1 1 d . . . H1A H 0.3346 0.1925 0.3261 0.049 Uiso 1 1 calc R . . C2 C 0.2702(3) 0.10683(19) 0.2585(5) 0.0451(9) Uani 1 1 d . . . H2A H 0.2140 0.1027 0.3288 0.054 Uiso 1 1 calc R . . C3 C 0.2796(3) 0.05946(19) 0.1583(4) 0.0431(9) Uani 1 1 d . . . C4 C 0.3638(4) 0.0681(2) 0.0597(4) 0.0524(10) Uani 1 1 d . . . H4A H 0.3739 0.0363 -0.0105 0.063 Uiso 1 1 calc R . . C5 C 0.4329(3) 0.1225(2) 0.0631(4) 0.0485(9) Uani 1 1 d . . . H5A H 0.4894 0.1277 -0.0065 0.058 Uiso 1 1 calc R . . C6 C 0.2029(4) 0.0000(2) 0.1574(5) 0.0511(10) Uani 1 1 d . . . H6A H 0.2506 -0.0396 0.1445 0.061 Uiso 1 1 calc R . . H6B H 0.1638 -0.0037 0.2474 0.061 Uiso 1 1 calc R . . C7 C 0.0349(3) 0.05623(16) 0.0718(4) 0.0371(8) Uani 1 1 d . . . H7A H 0.0766 0.0984 0.0757 0.045 Uiso 1 1 calc R . . H7B H -0.0042 0.0496 0.1611 0.045 Uiso 1 1 calc R . . C8 C 0.0532(3) -0.05849(16) 0.0420(4) 0.0393(8) Uani 1 1 d . . . H8A H 0.0144 -0.0664 0.1310 0.047 Uiso 1 1 calc R . . H8B H 0.1074 -0.0950 0.0252 0.047 Uiso 1 1 calc R . . C9 C 0.6774(5) 0.2500 0.5540(6) 0.0494(13) Uani 0.50 2 d SPDU . 1 H9 H 0.7485 0.2500 0.4962 0.059 Uiso 0.50 2 calc SPR . 1 C10 C 0.7008(7) 0.1896(3) 0.6255(8) 0.0411(16) Uiso 0.50 1 d PD . 1 H10A H 0.7243 0.1557 0.5584 0.049 Uiso 0.50 1 calc PR . 1 H10B H 0.6299 0.1743 0.6717 0.049 Uiso 0.50 1 calc PR . 1 C11 C 0.7942(7) 0.1984(4) 0.7305(8) 0.046(2) Uani 0.50 1 d PD . 1 H11A H 0.8660 0.2110 0.6828 0.055 Uiso 0.50 1 calc PR . 1 H11B H 0.8080 0.1560 0.7769 0.055 Uiso 0.50 1 calc PR . 1 C12 C 0.7667(4) 0.2500 0.8392(5) 0.0343(10) Uani 0.50 2 d SPD . 1 C9A C 0.6774(5) 0.2500 0.5540(6) 0.0494(13) Uani 0.50 2 d SPDU . 2 H9A H 0.7596 0.2500 0.5240 0.059 Uiso 0.50 2 calc SPR . 2 C10A C 0.6473(7) 0.1945(4) 0.6545(8) 0.0472(18) Uiso 0.50 1 d PD . 2 H10C H 0.6405 0.1531 0.6021 0.057 Uiso 0.50 1 calc PR . 2 H10D H 0.5715 0.2038 0.6962 0.057 Uiso 0.50 1 calc PR . 2 C11A C 0.7364(8) 0.1848(3) 0.7711(9) 0.0464(19) Uani 0.50 1 d PD . 2 H11C H 0.7047 0.1545 0.8410 0.056 Uiso 0.50 1 calc PR . 2 H11D H 0.8070 0.1647 0.7329 0.056 Uiso 0.50 1 calc PR . 2 C12A C 0.7667(4) 0.2500 0.8392(5) 0.0343(10) Uani 0.50 2 d SPD . 2 C13 C 0.5926(4) 0.2500 0.4364(5) 0.0401(11) Uani 1 2 d S . . C14 C 0.6773(6) 0.2738(3) 0.9430(7) 0.0349(15) Uani 0.50 1 d P . . O3 O 0.6185(5) 0.2300(3) 1.0033(6) 0.057(2) Uani 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 0.0299(3) 0.0463(3) 0.0269(3) 0.000 -0.0040(2) 0.000 O1 0.030(2) 0.166(6) 0.036(2) 0.000 0.0006(17) 0.000 O2 0.0332(18) 0.079(3) 0.0257(18) 0.000 -0.0021(14) 0.000 O4 0.062(4) 0.070(4) 0.069(5) -0.027(4) 0.014(3) 0.000(3) N1 0.0324(14) 0.0442(16) 0.0356(17) 0.0039(13) -0.0073(12) -0.0039(12) N2 0.0324(13) 0.0326(14) 0.0425(17) 0.0018(12) -0.0055(12) -0.0040(11) C1 0.0356(18) 0.0448(19) 0.042(2) -0.0005(16) -0.0017(15) -0.0006(15) C2 0.0337(18) 0.053(2) 0.048(2) 0.0068(19) -0.0016(16) -0.0049(16) C3 0.0367(18) 0.045(2) 0.048(2) 0.0073(17) -0.0167(16) -0.0054(15) C4 0.056(2) 0.058(2) 0.043(2) -0.0093(19) -0.0082(18) -0.0112(19) C5 0.043(2) 0.062(2) 0.040(2) -0.0031(18) -0.0024(16) -0.0108(18) C6 0.049(2) 0.046(2) 0.059(3) 0.0116(19) -0.0200(19) -0.0124(17) C7 0.0398(18) 0.0309(15) 0.041(2) -0.0034(14) -0.0044(15) -0.0054(13) C8 0.0385(17) 0.0298(16) 0.050(2) 0.0024(15) -0.0071(15) -0.0032(13) C9 0.0480(15) 0.0520(15) 0.0481(15) 0.000 0.0000(8) 0.000 C11 0.035(4) 0.063(5) 0.040(5) -0.001(4) -0.006(3) 0.017(4) C12 0.032(2) 0.050(3) 0.021(2) 0.000 -0.0021(17) 0.000 C9A 0.0480(15) 0.0520(15) 0.0481(15) 0.000 0.0000(8) 0.000 C11A 0.064(6) 0.039(4) 0.037(5) 0.001(3) -0.004(4) 0.015(4) C12A 0.032(2) 0.050(3) 0.021(2) 0.000 -0.0021(17) 0.000 C13 0.032(2) 0.063(3) 0.025(3) 0.000 -0.0024(18) 0.000 C14 0.033(3) 0.050(4) 0.021(3) -0.006(2) -0.006(3) -0.002(3) O3 0.058(3) 0.077(6) 0.036(3) -0.001(2) 0.014(3) -0.013(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 O3 1.920(6) 1_554 ? Zn1 O3 1.920(6) 8_564 ? Zn1 O2 1.927(4) . ? Zn1 N1 2.070(3) . ? Zn1 N1 2.070(3) 8_565 ? O1 C13 1.216(6) . ? O2 C13 1.270(6) . ? O4 C14 1.221(9) . ? O4 O3 1.440(9) 8_565 ? N1 C1 1.334(5) . ? N1 C5 1.346(5) . ? N2 C7 1.460(4) . ? N2 C8 1.461(4) . ? N2 C6 1.463(5) . ? C1 C2 1.380(5) . ? C1 H1A 0.9500 . ? C2 C3 1.378(6) . ? C2 H2A 0.9500 . ? C3 C4 1.383(6) . ? C3 C6 1.507(5) . ? C4 C5 1.371(6) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.509(5) 5 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C7 1.509(5) 5 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.443(7) . ? C9 C10 1.443(7) 8_565 ? C9 C13 1.511(7) . ? C9 H9 1.0000 . ? C10 C11 1.502(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.527(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C11 1.527(7) 8_565 ? C12 C14 1.529(8) 8_565 ? C12 C14 1.529(8) . ? C10A C11A 1.550(8) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A C14 1.996(12) 8_565 ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C14 O3 0.905(8) 8_565 ? C14 C14 0.972(14) 8_565 ? C14 O3 1.271(8) . ? C14 C11A 1.996(12) 8_565 ? O3 O3 0.819(12) 8_565 ? O3 C14 0.905(8) 8_565 ? O3 O4 1.440(9) 8_565 ? O3 Zn1 1.920(6) 1_556 ? 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 O3 24.6(3) 1_554 8_564 ? O3 Zn1 O2 106.3(2) 1_554 . ? O3 Zn1 O2 106.3(2) 8_564 . ? O3 Zn1 N1 97.89(19) 1_554 . ? O3 Zn1 N1 118.7(2) 8_564 . ? O2 Zn1 N1 113.14(10) . . ? O3 Zn1 N1 118.7(2) 1_554 8_565 ? O3 Zn1 N1 97.89(19) 8_564 8_565 ? O2 Zn1 N1 113.14(10) . 8_565 ? N1 Zn1 N1 106.84(17) . 8_565 ? C13 O2 Zn1 116.9(3) . . ? C14 O4 O3 38.7(4) . 8_565 ? C1 N1 C5 117.2(3) . . ? C1 N1 Zn1 121.0(3) . . ? C5 N1 Zn1 121.8(3) . . ? C7 N2 C8 108.6(3) . . ? C7 N2 C6 111.5(3) . . ? C8 N2 C6 109.9(3) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 117.1(4) . . ? C2 C3 C6 121.6(4) . . ? C4 C3 C6 121.2(4) . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C5 C4 122.6(4) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? N2 C6 C3 112.1(3) . . ? N2 C6 H6A 109.2 . . ? C3 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C3 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 110.5(3) . 5 ? N2 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 5 . ? N2 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 5 . ? H7A C7 H7B 108.1 . . ? N2 C8 C7 110.4(3) . 5 ? N2 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 5 . ? N2 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 5 . ? H8A C8 H8B 108.1 . . ? C10 C9 C10 117.6(7) . 8_565 ? C10 C9 C13 119.2(4) . . ? C10 C9 C13 119.2(4) 8_565 . ? C10 C9 H9 96.6 . . ? C10 C9 H9 96.6 8_565 . ? C13 C9 H9 96.6 . . ? C9 C10 C11 111.2(6) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 113.7(6) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C11 87.3(8) . 8_565 ? C11 C12 C14 112.3(5) . 8_565 ? C11 C12 C14 145.0(5) 8_565 8_565 ? C11 C12 C14 145.0(5) . . ? C11 C12 C14 112.3(5) 8_565 . ? C14 C12 C14 37.1(6) 8_565 . ? C11A C10A H10C 108.8 . . ? C11A C10A H10D 108.7 . . ? H10C C10A H10D 107.6 . . ? C10A C11A C14 109.2(6) . 8_565 ? C10A C11A H11C 109.4 . . ? C14 C11A H11C 64.0 8_565 . ? C10A C11A H11D 109.4 . . ? C14 C11A H11D 140.9 8_565 . ? H11C C11A H11D 108.0 . . ? O1 C13 O2 123.1(5) . . ? O1 C13 C9 121.0(5) . . ? O2 C13 C9 116.0(4) . . ? O3 C14 C14 85.1(6) 8_565 8_565 ? O3 C14 O4 83.8(7) 8_565 . ? C14 C14 O4 167.4(5) 8_565 . ? O3 C14 O3 39.9(7) 8_565 . ? C14 C14 O3 45.2(4) 8_565 . ? O4 C14 O3 123.5(7) . . ? O3 C14 C12 156.3(8) 8_565 . ? C14 C14 C12 71.5(3) 8_565 . ? O4 C14 C12 119.8(7) . . ? O3 C14 C12 116.6(5) . . ? O3 C14 C11A 147.1(8) 8_565 8_565 ? C14 C14 C11A 115.1(3) 8_565 8_565 ? O4 C14 C11A 77.5(6) . 8_565 ? O3 C14 C11A 150.6(6) . 8_565 ? C12 C14 C11A 49.3(3) . 8_565 ? O3 O3 C14 94.9(6) 8_565 8_565 ? O3 O3 C14 45.2(4) 8_565 . ? C14 O3 C14 49.7(8) 8_565 . ? O3 O3 O4 151.8(3) 8_565 8_565 ? C14 O3 O4 57.5(6) 8_565 8_565 ? C14 O3 O4 106.9(5) . 8_565 ? O3 O3 Zn1 77.69(17) 8_565 1_556 ? C14 O3 Zn1 162.5(7) 8_565 1_556 ? C14 O3 Zn1 121.1(5) . 1_556 ? O4 O3 Zn1 126.9(4) 8_565 1_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.988 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.071 # Attachment 'web_deposit_cif_file_1_wangxin_1282551306.cif' data_wx234-2 _database_code_depnum_ccdc_archive 'CCDC 790254' #TrackingRef 'web_deposit_cif_file_1_wangxin_1282551306.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Cd N2 O5' _chemical_formula_weight 434.76 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.910(3) _cell_length_b 5.8674(12) _cell_length_c 17.368(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.49(3) _cell_angle_gamma 90.00 _cell_volume 1634.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6928 _exptl_absorpt_correction_T_max 0.7911 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11904 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2867 _reflns_number_gt 2486 _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. During the refinement, the command 'omit-3 50' was used to omit the weak reflections above 50 degree. The H atoms on water molecules cannot be found from the weak residual electron peaks and directly included in the final molecular formula. ; _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^)+(0.0270P)^2^+1.1372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(2) _refine_ls_number_reflns 2867 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Cd1 Cd 1.0000 0.34807(5) 0.2500 0.01804(10) Uani 1 2 d S . . Cd2 Cd 0.5000 0.45819(6) 0.2500 0.01775(10) Uani 1 2 d S . . O1 O 0.56098(15) 0.7303(4) 0.19303(14) 0.0324(6) Uani 1 1 d . . . O2 O 0.53650(14) 0.4056(4) 0.12723(13) 0.0273(5) Uani 1 1 d . . . O1W O 0.93807(14) 0.0626(4) 0.29651(13) 0.0274(5) Uani 1 1 d . . . O5 O 0.89092(13) 0.6203(4) 0.23966(13) 0.0264(5) Uani 1 1 d . . . O6 O 0.90166(13) 0.4418(4) 0.13174(13) 0.0251(5) Uani 1 1 d . . . N1 N 0.38220(14) 0.2520(5) 0.18599(14) 0.0207(5) Uani 1 1 d . . . N3 N 0.08164(15) -0.0432(4) 0.05814(15) 0.0176(5) Uani 1 1 d . . . C1 C 0.38567(19) 0.0575(6) 0.14797(19) 0.0234(7) Uani 1 1 d . . . H1 H 0.4381 0.0075 0.1451 0.028 Uiso 1 1 calc R . . C2 C 0.31581(18) -0.0755(5) 0.11229(18) 0.0212(7) Uani 1 1 d . . . H2 H 0.3208 -0.2138 0.0858 0.025 Uiso 1 1 calc R . . C3 C 0.23857(18) -0.0055(5) 0.11549(18) 0.0189(6) Uani 1 1 d . . . C4 C 0.23509(18) 0.1990(6) 0.15512(19) 0.0232(7) Uani 1 1 d . . . H4 H 0.1835 0.2547 0.1584 0.028 Uiso 1 1 calc R . . C5 C 0.30786(18) 0.3190(6) 0.18952(19) 0.0225(7) Uani 1 1 d . . . H5 H 0.3050 0.4568 0.2172 0.027 Uiso 1 1 calc R . . C6 C 0.16371(19) -0.1591(6) 0.0802(2) 0.0242(7) Uani 1 1 d . . . H6A H 0.1692 -0.2337 0.0310 0.029 Uiso 1 1 calc R . . H6B H 0.1647 -0.2804 0.1201 0.029 Uiso 1 1 calc R . . C8 C 0.01609(17) -0.2195(5) 0.03383(18) 0.0211(6) Uani 1 1 d . . . H8A H 0.0229 -0.3272 0.0794 0.025 Uiso 1 1 calc R . . H8B H 0.0221 -0.3064 -0.0129 0.025 Uiso 1 1 calc R . . C11 C 0.06989(18) 0.1140(5) -0.01064(18) 0.0196(6) Uani 1 1 d . . . H11A H 0.0766 0.0301 -0.0576 0.024 Uiso 1 1 calc R . . H11B H 0.1127 0.2355 0.0045 0.024 Uiso 1 1 calc R . . C19 C 0.56261(17) 0.6064(5) 0.13391(18) 0.0188(7) Uani 1 1 d . . . C20 C 0.59395(17) 0.7088(5) 0.06812(17) 0.0186(6) Uani 1 1 d . . . H20 H 0.5439 0.7672 0.0245 0.022 Uiso 1 1 calc R . . C21 C 0.63433(18) 0.5283(5) 0.02899(18) 0.0201(7) Uani 1 1 d . . . H21A H 0.5972 0.3938 0.0142 0.024 Uiso 1 1 calc R . . H21B H 0.6412 0.5908 -0.0215 0.024 Uiso 1 1 calc R . . C22 C 0.71925(18) 0.4546(5) 0.08620(18) 0.0188(6) Uani 1 1 d . . . H22A H 0.7446 0.3433 0.0582 0.023 Uiso 1 1 calc R . . H22B H 0.7118 0.3788 0.1344 0.023 Uiso 1 1 calc R . . C23 C 0.77785(17) 0.6601(5) 0.11362(18) 0.0181(6) Uani 1 1 d . . . H23 H 0.7847 0.7314 0.0639 0.022 Uiso 1 1 calc R . . C24 C 0.73870(18) 0.8377(5) 0.15429(19) 0.0209(7) Uani 1 1 d . . . H24A H 0.7757 0.9725 0.1688 0.025 Uiso 1 1 calc R . . H24B H 0.7329 0.7736 0.2050 0.025 Uiso 1 1 calc R . . C25 C 0.65243(18) 0.9116(5) 0.09784(19) 0.0211(7) Uani 1 1 d . . . H25A H 0.6270 1.0187 0.1273 0.025 Uiso 1 1 calc R . . H25B H 0.6593 0.9930 0.0504 0.025 Uiso 1 1 calc R . . C26 C 0.86246(17) 0.5729(5) 0.16477(18) 0.0190(6) 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 Cd1 0.01353(15) 0.01890(18) 0.02020(17) 0.000 0.00324(12) 0.000 Cd2 0.01194(15) 0.02201(19) 0.01911(17) 0.000 0.00466(12) 0.000 O1 0.0453(14) 0.0248(13) 0.0372(13) -0.0065(11) 0.0276(11) -0.0034(12) O2 0.0316(12) 0.0275(13) 0.0246(12) 0.0000(10) 0.0114(10) -0.0093(11) O1W 0.0348(12) 0.0248(13) 0.0263(12) -0.0026(10) 0.0148(10) -0.0092(11) O5 0.0227(11) 0.0273(13) 0.0241(12) -0.0046(10) 0.0003(9) 0.0050(10) O6 0.0191(10) 0.0313(13) 0.0245(11) -0.0003(10) 0.0062(9) 0.0090(10) N1 0.0185(12) 0.0256(15) 0.0182(12) -0.0006(12) 0.0058(10) -0.0016(12) N3 0.0147(11) 0.0164(14) 0.0213(13) -0.0030(11) 0.0052(10) -0.0051(11) C1 0.0178(15) 0.0284(19) 0.0251(16) 0.0036(14) 0.0084(13) 0.0042(14) C2 0.0234(15) 0.0183(16) 0.0216(16) 0.0000(13) 0.0065(12) 0.0040(14) C3 0.0165(14) 0.0205(17) 0.0181(15) 0.0022(13) 0.0030(11) -0.0011(13) C4 0.0153(14) 0.0247(18) 0.0304(17) -0.0039(14) 0.0082(12) 0.0002(14) C5 0.0207(15) 0.0231(17) 0.0246(16) -0.0068(14) 0.0084(12) -0.0040(13) C6 0.0201(15) 0.0207(17) 0.0315(17) -0.0053(14) 0.0079(13) -0.0017(14) C8 0.0211(14) 0.0189(17) 0.0235(15) 0.0000(13) 0.0074(12) -0.0051(14) C11 0.0186(14) 0.0200(17) 0.0210(15) -0.0028(13) 0.0073(12) -0.0089(13) C19 0.0103(13) 0.0219(17) 0.0229(16) 0.0055(13) 0.0032(11) 0.0038(13) C20 0.0138(13) 0.0204(17) 0.0198(14) 0.0006(13) 0.0028(11) -0.0012(13) C21 0.0173(14) 0.0238(17) 0.0181(15) -0.0015(13) 0.0040(12) -0.0017(13) C22 0.0169(14) 0.0200(17) 0.0204(15) -0.0008(13) 0.0071(12) 0.0005(13) C23 0.0146(14) 0.0184(16) 0.0203(15) 0.0004(13) 0.0044(11) -0.0023(13) C24 0.0192(15) 0.0164(16) 0.0258(16) -0.0017(13) 0.0054(12) -0.0019(13) C25 0.0192(15) 0.0174(16) 0.0275(17) 0.0051(14) 0.0085(13) 0.0026(13) C26 0.0157(14) 0.0161(16) 0.0245(16) 0.0051(13) 0.0052(12) 0.0003(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 Cd1 O1W 2.257(2) . ? Cd1 O1W 2.257(2) 2_755 ? Cd1 O6 2.263(2) 2_755 ? Cd1 O6 2.263(2) . ? Cd1 O5 2.404(2) 2_755 ? Cd1 O5 2.404(2) . ? Cd1 C26 2.675(3) 2_755 ? Cd1 C26 2.675(3) . ? Cd2 O1 2.289(2) 2_655 ? Cd2 O1 2.289(2) . ? Cd2 N1 2.294(3) . ? Cd2 N1 2.294(3) 2_655 ? Cd2 O2 2.420(2) 2_655 ? Cd2 O2 2.420(2) . ? Cd2 C19 2.701(3) 2_655 ? Cd2 C19 2.701(3) . ? O1 C19 1.266(4) . ? O2 C19 1.251(4) . ? O5 C26 1.267(4) . ? O6 C26 1.265(4) . ? N1 C1 1.329(4) . ? N1 C5 1.337(4) . ? N3 C11 1.472(4) . ? N3 C8 1.477(4) . ? N3 C6 1.483(4) . ? C1 C2 1.387(5) . ? C1 H1 0.9500 . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.394(5) . ? C3 C6 1.516(4) . ? C4 C5 1.379(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C11 1.513(4) 3 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C11 C8 1.513(4) 3 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C19 C20 1.527(4) . ? C20 C25 1.528(4) . ? C20 C21 1.531(4) . ? C20 H20 1.0000 . ? C21 C22 1.527(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.537(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C26 1.514(4) . ? C23 C24 1.523(4) . ? C23 H23 1.0000 . ? C24 C25 1.539(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? 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 Cd1 O1W 84.13(12) . 2_755 ? O1W Cd1 O6 98.42(8) . 2_755 ? O1W Cd1 O6 102.38(8) 2_755 2_755 ? O1W Cd1 O6 102.38(8) . . ? O1W Cd1 O6 98.42(8) 2_755 . ? O6 Cd1 O6 151.86(12) 2_755 . ? O1W Cd1 O5 154.03(8) . 2_755 ? O1W Cd1 O5 95.04(8) 2_755 2_755 ? O6 Cd1 O5 56.28(8) 2_755 2_755 ? O6 Cd1 O5 103.41(8) . 2_755 ? O1W Cd1 O5 95.04(8) . . ? O1W Cd1 O5 154.03(8) 2_755 . ? O6 Cd1 O5 103.41(8) 2_755 . ? O6 Cd1 O5 56.28(8) . . ? O5 Cd1 O5 96.69(11) 2_755 . ? O1W Cd1 C26 126.07(9) . 2_755 ? O1W Cd1 C26 98.24(9) 2_755 2_755 ? O6 Cd1 C26 28.14(9) 2_755 2_755 ? O6 Cd1 C26 129.95(9) . 2_755 ? O5 Cd1 C26 28.24(8) 2_755 2_755 ? O5 Cd1 C26 103.04(8) . 2_755 ? O1W Cd1 C26 98.24(9) . . ? O1W Cd1 C26 126.07(9) 2_755 . ? O6 Cd1 C26 129.95(9) 2_755 . ? O6 Cd1 C26 28.14(9) . . ? O5 Cd1 C26 103.04(8) 2_755 . ? O5 Cd1 C26 28.24(8) . . ? C26 Cd1 C26 120.92(13) 2_755 . ? O1 Cd2 O1 91.53(12) 2_655 . ? O1 Cd2 N1 97.84(9) 2_655 . ? O1 Cd2 N1 126.82(9) . . ? O1 Cd2 N1 126.82(9) 2_655 2_655 ? O1 Cd2 N1 97.84(9) . 2_655 ? N1 Cd2 N1 116.35(14) . 2_655 ? O1 Cd2 O2 55.42(8) 2_655 2_655 ? O1 Cd2 O2 138.21(8) . 2_655 ? N1 Cd2 O2 86.26(8) . 2_655 ? N1 Cd2 O2 86.02(8) 2_655 2_655 ? O1 Cd2 O2 138.21(8) 2_655 . ? O1 Cd2 O2 55.42(8) . . ? N1 Cd2 O2 86.02(8) . . ? N1 Cd2 O2 86.26(8) 2_655 . ? O2 Cd2 O2 165.34(11) 2_655 . ? O1 Cd2 C19 27.85(9) 2_655 2_655 ? O1 Cd2 C19 115.79(9) . 2_655 ? N1 Cd2 C19 92.63(9) . 2_655 ? N1 Cd2 C19 107.08(9) 2_655 2_655 ? O2 Cd2 C19 27.58(9) 2_655 2_655 ? O2 Cd2 C19 165.59(9) . 2_655 ? O1 Cd2 C19 115.79(9) 2_655 . ? O1 Cd2 C19 27.85(9) . . ? N1 Cd2 C19 107.08(9) . . ? N1 Cd2 C19 92.63(9) 2_655 . ? O2 Cd2 C19 165.59(9) 2_655 . ? O2 Cd2 C19 27.58(9) . . ? C19 Cd2 C19 142.44(14) 2_655 . ? C19 O1 Cd2 94.50(19) . . ? C19 O2 Cd2 88.81(18) . . ? C26 O5 Cd1 87.89(18) . . ? C26 O6 Cd1 94.36(18) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Cd2 121.7(2) . . ? C5 N1 Cd2 120.5(2) . . ? C11 N3 C8 108.1(2) . . ? C11 N3 C6 111.8(2) . . ? C8 N3 C6 108.0(2) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 117.5(3) . . ? C2 C3 C6 118.9(3) . . ? C4 C3 C6 123.4(3) . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N3 C6 C3 115.2(3) . . ? N3 C6 H6A 108.5 . . ? C3 C6 H6A 108.5 . . ? N3 C6 H6B 108.5 . . ? C3 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N3 C8 C11 111.1(3) . 3 ? N3 C8 H8A 109.4 . . ? C11 C8 H8A 109.4 3 . ? N3 C8 H8B 109.4 . . ? C11 C8 H8B 109.4 3 . ? H8A C8 H8B 108.0 . . ? N3 C11 C8 110.1(2) . 3 ? N3 C11 H11A 109.6 . . ? C8 C11 H11A 109.6 3 . ? N3 C11 H11B 109.6 . . ? C8 C11 H11B 109.6 3 . ? H11A C11 H11B 108.2 . . ? O2 C19 O1 121.3(3) . . ? O2 C19 C20 119.8(3) . . ? O1 C19 C20 118.9(3) . . ? O2 C19 Cd2 63.61(16) . . ? O1 C19 Cd2 57.65(16) . . ? C20 C19 Cd2 175.2(2) . . ? C19 C20 C25 113.2(3) . . ? C19 C20 C21 111.7(3) . . ? C25 C20 C21 110.9(2) . . ? C19 C20 H20 106.9 . . ? C25 C20 H20 106.9 . . ? C21 C20 H20 106.9 . . ? C22 C21 C20 111.5(2) . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 111.1(3) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C26 C23 C24 115.3(2) . . ? C26 C23 C22 108.3(2) . . ? C24 C23 C22 110.4(2) . . ? C26 C23 H23 107.5 . . ? C24 C23 H23 107.5 . . ? C22 C23 H23 107.5 . . ? C23 C24 C25 111.1(2) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C20 C25 C24 112.1(3) . . ? C20 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C20 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O6 C26 O5 121.1(3) . . ? O6 C26 C23 118.2(3) . . ? O5 C26 C23 120.6(3) . . ? O6 C26 Cd1 57.50(15) . . ? O5 C26 Cd1 63.87(15) . . ? C23 C26 Cd1 170.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.742 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.093 # Attachment 'web_deposit_cif_file_2_wangxin_1282551306.cif' data_wx090825a _database_code_depnum_ccdc_archive 'CCDC 790255' #TrackingRef 'web_deposit_cif_file_2_wangxin_1282551306.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 N2 O10 Zn' _chemical_formula_weight 541.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 10.677(2) _cell_length_b 10.741(2) _cell_length_c 12.069(2) _cell_angle_alpha 81.66(3) _cell_angle_beta 89.72(3) _cell_angle_gamma 68.68(3) _cell_volume 1274.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7921 _exptl_absorpt_correction_T_max 0.8222 _exptl_absorpt_process_details 'ABSORB by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 12533 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5734 _reflns_number_gt 4626 _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. During the refinement, the command 'omi-3 50' was used to omit the weak reflections above 50 degree. The restrain command 'isor' was used to restrain the non-H atoms with NPD and ADP problems. ; _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^)+(0.0734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(2) _refine_ls_number_reflns 5734 _refine_ls_number_parameters 343 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.051 _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 0.70720(3) 0.09275(3) 0.48905(2) 0.03283(11) Uani 1 1 d . . . O1 O 0.8265(2) 0.1926(2) 0.49646(17) 0.0512(5) Uani 1 1 d . . . O2 O 0.7461(3) 0.2252(2) 0.6628(2) 0.0614(6) Uani 1 1 d . . . O3 O 0.4519(2) 0.7069(2) 0.6629(2) 0.0640(6) Uani 1 1 d . . . O4 O 0.4880(2) 0.8181(2) 0.50672(17) 0.0518(5) Uani 1 1 d . . . N1 N 0.7695(2) -0.0059(2) 0.35419(17) 0.0368(5) Uani 1 1 d . . . N2 N 0.7585(2) -0.0628(2) 0.62152(17) 0.0337(4) Uani 1 1 d . . . C1 C 0.8818(3) 0.3506(3) 0.5845(2) 0.0398(6) Uani 1 1 d . . . H1A H 0.9807 0.3005 0.5811 0.048 Uiso 1 1 calc R . . C2 C 0.8601(3) 0.4189(3) 0.6892(2) 0.0428(6) Uani 1 1 d . . . H2A H 0.8810 0.3485 0.7564 0.051 Uiso 1 1 calc R . . H2B H 0.9236 0.4666 0.6914 0.051 Uiso 1 1 calc R . . C3 C 0.7172(3) 0.5195(3) 0.6940(2) 0.0396(6) Uani 1 1 d . . . H3A H 0.6550 0.4698 0.7048 0.048 Uiso 1 1 calc R . . H3B H 0.7124 0.5668 0.7594 0.048 Uiso 1 1 calc R . . C4 C 0.6720(2) 0.6233(2) 0.5884(2) 0.0358(5) Uani 1 1 d . . . H4A H 0.7315 0.6773 0.5828 0.043 Uiso 1 1 calc R . . C5 C 0.6902(3) 0.5532(3) 0.4843(2) 0.0389(5) Uani 1 1 d . . . H5A H 0.6299 0.5015 0.4862 0.047 Uiso 1 1 calc R . . H5B H 0.6647 0.6223 0.4162 0.047 Uiso 1 1 calc R . . C6 C 0.8354(3) 0.4578(3) 0.4791(2) 0.0438(6) Uani 1 1 d . . . H6A H 0.8947 0.5108 0.4711 0.053 Uiso 1 1 calc R . . H6B H 0.8436 0.4123 0.4123 0.053 Uiso 1 1 calc R . . C7 C 0.8123(3) 0.2488(3) 0.5843(2) 0.0399(6) Uani 1 1 d . . . C8 C 0.5275(3) 0.7215(3) 0.5886(2) 0.0401(6) Uani 1 1 d . . . C9 C 0.7343(3) -0.1072(3) 0.3332(2) 0.0404(6) Uani 1 1 d . . . H9A H 0.6827 -0.1397 0.3859 0.049 Uiso 1 1 calc R . . C10 C 0.7694(3) -0.1670(3) 0.2383(2) 0.0446(6) Uani 1 1 d . . . H10A H 0.7419 -0.2392 0.2269 0.053 Uiso 1 1 calc R . . C11 C 0.8440(2) -0.1229(3) 0.1599(2) 0.0365(5) Uani 1 1 d . . . C12 C 0.8809(3) -0.0180(3) 0.1823(3) 0.0554(8) Uani 1 1 d . . . H12A H 0.9331 0.0159 0.1313 0.066 Uiso 1 1 calc R . . C13 C 0.8418(4) 0.0373(3) 0.2786(3) 0.0557(8) Uani 1 1 d . . . H13A H 0.8676 0.1099 0.2919 0.067 Uiso 1 1 calc R . . C14 C 0.8852(3) -0.1508(3) 0.6392(2) 0.0393(6) Uani 1 1 d . . . H14A H 0.9470 -0.1500 0.5825 0.047 Uiso 1 1 calc R . . C15 C 0.9300(3) -0.2422(3) 0.7357(2) 0.0410(6) Uani 1 1 d . . . H15A H 1.0211 -0.3028 0.7447 0.049 Uiso 1 1 calc R . . C16 C 0.8430(3) -0.2465(2) 0.8195(2) 0.0364(5) Uani 1 1 d . . . C17 C 0.7115(3) -0.1559(3) 0.7992(2) 0.0449(6) Uani 1 1 d . . . H17A H 0.6470 -0.1558 0.8537 0.054 Uiso 1 1 calc R . . C18 C 0.6736(3) -0.0668(3) 0.7015(2) 0.0417(6) Uani 1 1 d . . . H18A H 0.5830 -0.0051 0.6904 0.050 Uiso 1 1 calc R . . C19 C 0.8864(3) -0.1822(3) 0.0538(2) 0.0450(6) Uani 1 1 d . . . H19A H 0.8539 -0.1080 -0.0106 0.054 Uiso 1 1 calc R . . H19B H 0.9860 -0.2185 0.0550 0.054 Uiso 1 1 calc R . . C20 C 0.8380(3) -0.2925(3) 0.0335(2) 0.0439(6) Uani 1 1 d . . . H20A H 0.7384 -0.2568 0.0292 0.053 Uiso 1 1 calc R . . H20B H 0.8694 -0.3673 0.0975 0.053 Uiso 1 1 calc R . . C21 C 0.8894(3) -0.3471(3) 0.9253(2) 0.0470(7) Uani 1 1 d . . . H21A H 0.9890 -0.3832 0.9310 0.056 Uiso 1 1 calc R . . H21B H 0.8604 -0.4236 0.9191 0.056 Uiso 1 1 calc R . . O1W O 0.5123(3) 0.7255(4) 0.2288(3) 0.0997(10) Uani 1 1 d D . . H1AW H 0.437(2) 0.726(4) 0.204(4) 0.100 Uiso 1 1 d D . . H1BW H 0.573(3) 0.648(2) 0.231(4) 0.100 Uiso 1 1 d D . . O2W O 0.4453(3) 0.8977(3) 0.0230(3) 0.0886(8) Uani 1 1 d D . . H2AW H 0.509(2) 0.887(3) 0.0674(14) 0.089 Uiso 1 1 d D . . H2BW H 0.461(4) 0.840(3) -0.020(3) 0.089 Uiso 1 1 d D . . O3W O 0.6926(4) 0.4555(5) 0.2238(3) 0.1139(12) Uani 1 1 d D . . H3AW H 0.735(3) 0.481(2) 0.171(3) 0.114 Uiso 1 1 d D . . H3BW H 0.6264(19) 0.440(3) 0.197(3) 0.114 Uiso 1 1 d D . . O4W O 0.2110(3) 0.8264(5) 0.0967(3) 0.1056(11) Uani 1 1 d D . . H4AW H 0.277(3) 0.849(5) 0.073(3) 0.106 Uiso 1 1 d D . . H4BW H 0.220(4) 0.804(5) 0.1677(10) 0.106 Uiso 1 1 d D . . O5W O 0.4921(4) 0.3213(5) 0.0995(3) 0.1157(13) Uani 1 1 d D . . H5AW H 0.510(5) 0.320(5) 0.1692(11) 0.116 Uiso 1 1 d D . . H5BW H 0.547(4) 0.348(5) 0.060(3) 0.116 Uiso 1 1 d D . . O6W O 0.7122(6) 0.4178(6) -0.0003(3) 0.1461(16) Uani 1 1 d DU . . H6AW H 0.6453(18) 0.469(3) -0.042(3) 0.146 Uiso 1 1 d D . . H6BW H 0.754(5) 0.344(3) -0.023(5) 0.146 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 0.03839(18) 0.03014(16) 0.02683(15) -0.00595(11) 0.00405(11) -0.00832(12) O1 0.0574(12) 0.0540(12) 0.0510(12) -0.0242(10) 0.0101(9) -0.0249(10) O2 0.0809(16) 0.0541(13) 0.0640(14) -0.0234(11) 0.0279(12) -0.0373(12) O3 0.0502(13) 0.0576(13) 0.0681(15) 0.0018(11) 0.0190(11) -0.0055(11) O4 0.0480(12) 0.0448(11) 0.0477(11) 0.0059(9) 0.0013(9) -0.0044(9) N1 0.0407(12) 0.0372(11) 0.0322(10) -0.0081(9) 0.0055(9) -0.0131(9) N2 0.0387(11) 0.0309(10) 0.0295(10) -0.0047(8) 0.0027(8) -0.0102(9) C1 0.0297(12) 0.0406(14) 0.0467(15) -0.0147(12) 0.0002(10) -0.0070(10) C2 0.0420(15) 0.0409(14) 0.0434(15) -0.0086(12) -0.0117(11) -0.0118(12) C3 0.0491(15) 0.0344(13) 0.0328(13) -0.0091(10) -0.0012(11) -0.0110(11) C4 0.0371(13) 0.0309(12) 0.0399(13) -0.0068(10) -0.0023(10) -0.0127(10) C5 0.0439(15) 0.0387(13) 0.0321(13) -0.0047(10) 0.0006(10) -0.0132(11) C6 0.0412(15) 0.0478(15) 0.0455(15) -0.0126(12) 0.0121(12) -0.0181(12) C7 0.0370(13) 0.0333(13) 0.0456(15) -0.0105(11) -0.0006(11) -0.0067(11) C8 0.0429(15) 0.0334(13) 0.0444(15) -0.0105(11) -0.0005(11) -0.0127(11) C9 0.0472(15) 0.0442(14) 0.0343(13) -0.0075(11) 0.0094(11) -0.0215(12) C10 0.0580(17) 0.0460(15) 0.0387(14) -0.0128(12) 0.0073(12) -0.0273(14) C11 0.0365(13) 0.0403(13) 0.0304(12) -0.0073(10) 0.0023(10) -0.0109(11) C12 0.075(2) 0.0649(19) 0.0453(16) -0.0192(15) 0.0271(15) -0.0440(18) C13 0.081(2) 0.0598(18) 0.0485(17) -0.0224(15) 0.0237(15) -0.0469(18) C14 0.0379(14) 0.0424(14) 0.0344(13) -0.0069(11) 0.0074(10) -0.0108(11) C15 0.0367(14) 0.0388(13) 0.0383(14) -0.0050(11) -0.0010(11) -0.0033(11) C16 0.0491(15) 0.0278(11) 0.0319(12) -0.0096(10) 0.0010(10) -0.0119(11) C17 0.0469(16) 0.0463(15) 0.0368(14) -0.0042(12) 0.0129(11) -0.0126(13) C18 0.0373(14) 0.0406(14) 0.0398(14) -0.0018(11) 0.0067(11) -0.0072(11) C19 0.0516(16) 0.0544(17) 0.0332(13) -0.0145(12) 0.0093(11) -0.0213(14) C20 0.0618(17) 0.0388(14) 0.0267(12) -0.0052(11) 0.0045(11) -0.0132(13) C21 0.0695(19) 0.0333(13) 0.0309(13) -0.0060(11) -0.0004(12) -0.0098(13) O1W 0.080(2) 0.133(3) 0.084(2) 0.006(2) 0.0008(18) -0.045(2) O2W 0.089(2) 0.098(2) 0.0750(19) -0.0175(16) 0.0124(16) -0.0279(17) O3W 0.139(3) 0.166(4) 0.0659(19) -0.019(2) 0.0172(19) -0.090(3) O4W 0.085(2) 0.158(3) 0.077(2) -0.005(2) 0.0103(17) -0.054(2) O5W 0.145(3) 0.167(4) 0.072(2) -0.040(2) 0.043(2) -0.093(3) O6W 0.198(5) 0.147(4) 0.086(3) -0.029(3) 0.025(3) -0.050(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 1.950(2) . ? Zn1 O4 1.956(2) 2_666 ? Zn1 N1 2.047(2) . ? Zn1 N2 2.053(2) . ? O1 C7 1.277(3) . ? O2 C7 1.230(3) . ? O3 C8 1.235(3) . ? O4 C8 1.273(3) . ? O4 Zn1 1.956(2) 2_666 ? N1 C9 1.330(3) . ? N1 C13 1.331(4) . ? N2 C18 1.328(3) . ? N2 C14 1.335(3) . ? C1 C2 1.526(4) . ? C1 C7 1.529(4) . ? C1 C6 1.535(4) . ? C1 H1A 1.0000 . ? C2 C3 1.522(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.518(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C8 1.519(4) . ? C4 C5 1.532(3) . ? C4 H4A 1.0000 . ? C5 C6 1.523(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 C10 1.379(4) . ? C9 H9A 0.9500 . ? C10 C11 1.374(4) . ? C10 H10A 0.9500 . ? C11 C12 1.383(4) . ? C11 C19 1.507(3) . ? C12 C13 1.376(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.372(4) . ? C14 H14A 0.9500 . ? C15 C16 1.377(4) . ? C15 H15A 0.9500 . ? C16 C17 1.385(4) . ? C16 C21 1.504(4) . ? C17 C18 1.365(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.504(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.527(3) 1_554 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C20 1.527(3) 1_556 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O1W H1AW 0.852(10) . ? O1W H1BW 0.846(10) . ? O2W H2AW 0.831(10) . ? O2W H2BW 0.834(10) . ? O3W H3AW 0.845(10) . ? O3W H3BW 0.856(10) . ? O4W H4AW 0.853(10) . ? O4W H4BW 0.852(10) . ? O5W H5AW 0.860(10) . ? O5W H5BW 0.853(10) . ? O6W H6AW 0.837(10) . ? O6W H6BW 0.839(10) . ? 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 O4 121.17(9) . 2_666 ? O1 Zn1 N1 103.64(8) . . ? O4 Zn1 N1 114.59(9) 2_666 . ? O1 Zn1 N2 108.54(9) . . ? O4 Zn1 N2 104.56(9) 2_666 . ? N1 Zn1 N2 102.84(8) . . ? C7 O1 Zn1 112.40(18) . . ? C8 O4 Zn1 108.00(18) . 2_666 ? C9 N1 C13 117.1(2) . . ? C9 N1 Zn1 123.27(17) . . ? C13 N1 Zn1 119.52(18) . . ? C18 N2 C14 117.4(2) . . ? C18 N2 Zn1 121.21(17) . . ? C14 N2 Zn1 120.52(17) . . ? C2 C1 C7 113.8(2) . . ? C2 C1 C6 110.1(2) . . ? C7 C1 C6 109.8(2) . . ? C2 C1 H1A 107.6 . . ? C7 C1 H1A 107.6 . . ? C6 C1 H1A 107.6 . . ? C3 C2 C1 113.3(2) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 112.3(2) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C8 113.6(2) . . ? C3 C4 C5 110.6(2) . . ? C8 C4 C5 109.7(2) . . ? C3 C4 H4A 107.6 . . ? C8 C4 H4A 107.6 . . ? C5 C4 H4A 107.6 . . ? C6 C5 C4 111.1(2) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 111.7(2) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? O2 C7 O1 123.1(2) . . ? O2 C7 C1 121.9(2) . . ? O1 C7 C1 115.0(2) . . ? O3 C8 O4 121.9(3) . . ? O3 C8 C4 121.9(3) . . ? O4 C8 C4 116.3(2) . . ? N1 C9 C10 122.8(2) . . ? N1 C9 H9A 118.6 . . ? C10 C9 H9A 118.6 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 116.6(2) . . ? C10 C11 C19 124.0(2) . . ? C12 C11 C19 119.5(2) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? N1 C13 C12 123.2(3) . . ? N1 C13 H13A 118.4 . . ? C12 C13 H13A 118.4 . . ? N2 C14 C15 122.9(2) . . ? N2 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C17 116.3(2) . . ? C15 C16 C21 121.0(2) . . ? C17 C16 C21 122.6(2) . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? N2 C18 C17 122.6(2) . . ? N2 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? C20 C19 C11 116.2(2) . . ? C20 C19 H19A 108.2 . . ? C11 C19 H19A 108.2 . . ? C20 C19 H19B 108.2 . . ? C11 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? C19 C20 C21 111.8(2) . 1_554 ? C19 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 1_554 . ? C19 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 1_554 . ? H20A C20 H20B 107.9 . . ? C16 C21 C20 115.5(2) . 1_556 ? C16 C21 H21A 108.4 . . ? C20 C21 H21A 108.4 1_556 . ? C16 C21 H21B 108.4 . . ? C20 C21 H21B 108.4 1_556 . ? H21A C21 H21B 107.5 . . ? H1AW O1W H1BW 110.9(17) . . ? H2AW O2W H2BW 114.9(19) . . ? H3AW O3W H3BW 110.3(17) . . ? H4AW O4W H4BW 109.6(17) . . ? H5AW O5W H5BW 109.2(17) . . ? H6AW O6W H6BW 114.0(19) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.393 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.063