# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2157 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'JCS Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to JCS Dalton Trans. Xiao-Ming Chen July 6, 2000 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Hydrothermal synthesis and crystal structures of three-dimensional coordination frameworks constructed with mixed N- and O-donor ligands: [M(tp)(4,4'-bipy)] (M=Co(II), Cd(II) and Zn(II); tp= terephthalate; 4,4'-bipy=4,4'-bipyridine) ; loop_ _publ_author_name _publ_author_address 'Tao Jun' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Co N2 O4' _chemical_formula_weight 379.23 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' 'Co' 'Co' 0.3494 0.9721 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 16.623(3) _cell_length_b 10.299(2) _cell_length_c 11.368(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.23(3) _cell_angle_gamma 90.00 _cell_volume 1698.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8687 _exptl_absorpt_correction_T_max 0.9598 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5166 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.04 _reflns_number_total 1968 _reflns_number_gt 1695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker,1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.4702P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1968 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.86449(2) 0.5000 0.84461(3) 0.02323(14) Uani 1 d S . . O1 O 0.93886(10) 0.33589(14) 0.89647(14) 0.0361(4) Uani 1 d . . . O2 O 0.73457(10) 0.60580(16) 0.73792(16) 0.0441(4) Uani 1 d . . . N1 N 0.85075(17) 0.5000 1.0225(2) 0.0333(5) Uani 1 d S . . N2 N 0.86759(18) 0.5000 1.6575(2) 0.0333(5) Uani 1 d S . . C1 C 0.84692(17) 0.6102(2) 1.0811(2) 0.0430(6) Uani 1 d . . . H1 H 0.8495 0.6906 1.0359 0.080 Uiso 1 d R . . C2 C 0.84549(18) 0.6149(2) 1.2012(2) 0.0452(6) Uani 1 d . . . H2 H 0.8344 0.7002 1.2229 0.080 Uiso 1 d R . . C3 C 0.8468(2) 0.5000 1.2657(3) 0.0343(7) Uani 1 d S . . C4 C 0.8519(2) 0.5000 1.4003(3) 0.0360(7) Uani 1 d S . . C5 C 0.8539(3) 0.6115(3) 1.4658(3) 0.0891(13) Uani 1 d . . . H5 H 0.8393 0.6859 1.4195 0.080 Uiso 1 d R . . C6 C 0.8627(3) 0.6075(3) 1.5927(3) 0.0824(12) Uani 1 d . . . H6 H 0.8885 0.6876 1.6551 0.080 Uiso 1 d R . . C7 C 1.0000 0.2806(3) 1.0000 0.0284(6) Uani 1 d S . . C8 C 1.0000 0.1352(3) 1.0000 0.0305(6) Uani 1 d S . . C9 C 0.92660(15) 0.0671(2) 0.8994(2) 0.0432(6) Uani 1 d . . . H9 H 0.8764 0.1131 0.8368 0.080 Uiso 1 d R . . C10 C 0.6933(2) 0.5000 0.6979(3) 0.0338(6) Uani 1 d S . . C11 C 0.5925(2) 0.5000 0.5960(3) 0.0380(7) Uani 1 d S . . C12 C 0.5637(3) 0.4433(6) 0.4719(5) 0.0572(15) Uani 0.50 d P . . H12 H 0.6096 0.3879 0.4571 0.080 Uiso 0.50 d PR . . C13 C 0.5293(3) 0.5561(5) 0.6245(5) 0.0569(15) Uani 0.50 d P . . H13 H 0.5467 0.5848 0.7144 0.080 Uiso 0.50 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0287(2) 0.0209(2) 0.0187(2) 0.000 0.01053(15) 0.000 O1 0.0462(9) 0.0254(8) 0.0311(8) 0.0038(6) 0.0145(7) 0.0075(6) O2 0.0322(8) 0.0341(9) 0.0505(10) -0.0043(7) 0.0081(7) 0.0010(6) N1 0.0420(14) 0.0352(14) 0.0265(12) 0.000 0.0196(11) 0.000 N2 0.0480(15) 0.0300(13) 0.0254(12) 0.000 0.0207(11) 0.000 C1 0.0683(16) 0.0345(13) 0.0386(12) 0.0066(10) 0.0360(12) 0.0081(11) C2 0.0755(17) 0.0324(13) 0.0419(13) 0.0019(10) 0.0398(12) 0.0075(11) C3 0.0478(18) 0.0339(16) 0.0276(14) 0.000 0.0233(13) 0.000 C4 0.0533(19) 0.0333(16) 0.0297(15) 0.000 0.0266(14) 0.000 C5 0.213(4) 0.0307(15) 0.0575(18) 0.0049(13) 0.092(3) 0.0025(19) C6 0.190(4) 0.0330(15) 0.0505(16) -0.0038(12) 0.079(2) -0.0036(18) C7 0.0352(14) 0.0232(14) 0.0301(14) 0.000 0.0185(12) 0.000 C8 0.0325(15) 0.0214(13) 0.0311(14) 0.000 0.0105(11) 0.000 C9 0.0375(12) 0.0256(12) 0.0403(12) 0.0046(9) -0.0015(9) 0.0033(9) C10 0.0299(15) 0.0376(17) 0.0301(15) 0.000 0.0117(12) 0.000 C11 0.0304(16) 0.0395(18) 0.0367(16) 0.000 0.0106(13) 0.000 C12 0.036(2) 0.079(4) 0.049(3) -0.018(3) 0.015(2) 0.009(2) C13 0.037(2) 0.082(4) 0.040(2) -0.020(2) 0.010(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0053(15) 6_565 ? Co1 O1 2.0053(14) . ? Co1 N1 2.143(2) . ? Co1 N2 2.153(2) 1_554 ? Co1 O2 2.1827(17) 6_565 ? Co1 O2 2.1827(16) . ? Co1 C10 2.499(3) . ? O1 C7 1.2545(19) . ? O2 C10 1.249(2) . ? N1 C1 1.334(3) . ? N1 C1 1.334(3) 6_565 ? N2 C6 1.310(3) 6_565 ? N2 C6 1.310(3) . ? N2 Co1 2.153(2) 1_556 ? C1 C2 1.378(3) . ? C2 C3 1.387(3) . ? C3 C2 1.387(3) 6_565 ? C3 C4 1.490(4) . ? C4 C5 1.360(3) . ? C4 C5 1.360(3) 6_565 ? C5 C6 1.377(4) . ? C7 O1 1.2545(19) 2_757 ? C7 C8 1.498(4) . ? C8 C9 1.387(3) . ? C8 C9 1.387(3) 2_757 ? C9 C9 1.382(4) 6 ? C10 O2 1.249(2) 6_565 ? C10 C11 1.501(4) . ? C11 C13 1.369(6) 6_565 ? C11 C13 1.369(6) . ? C11 C12 1.378(6) . ? C11 C12 1.378(6) 6_565 ? C12 C12 1.167(12) 6_565 ? C12 C13 1.392(6) 5_666 ? C12 C13 1.813(7) 2_656 ? C13 C13 1.155(11) 6_565 ? C13 C12 1.392(6) 5_666 ? C13 C12 1.813(7) 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 O1 Co1 O1 114.89(9) 6_565 . ? O1 Co1 N1 93.27(6) 6_565 . ? O1 Co1 N1 93.27(6) . . ? O1 Co1 N2 88.95(6) 6_565 1_554 ? O1 Co1 N2 88.95(6) . 1_554 ? N1 Co1 N2 175.86(9) . 1_554 ? O1 Co1 O2 152.23(6) 6_565 6_565 ? O1 Co1 O2 92.48(6) . 6_565 ? N1 Co1 O2 89.53(8) . 6_565 ? N2 Co1 O2 86.88(8) 1_554 6_565 ? O1 Co1 O2 92.48(6) 6_565 . ? O1 Co1 O2 152.23(6) . . ? N1 Co1 O2 89.53(8) . . ? N2 Co1 O2 86.88(8) 1_554 . ? O2 Co1 O2 59.90(9) 6_565 . ? O1 Co1 C10 122.27(4) 6_565 . ? O1 Co1 C10 122.27(5) . . ? N1 Co1 C10 91.05(10) . . ? N2 Co1 C10 84.81(10) 1_554 . ? O2 Co1 C10 29.99(4) 6_565 . ? O2 Co1 C10 29.99(4) . . ? C7 O1 Co1 139.37(14) . . ? C10 O2 Co1 89.18(15) . . ? C1 N1 C1 116.7(3) . 6_565 ? C1 N1 Co1 121.66(13) . . ? C1 N1 Co1 121.66(13) 6_565 . ? C6 N2 C6 115.3(3) 6_565 . ? C6 N2 Co1 122.06(15) 6_565 1_556 ? C6 N2 Co1 122.06(15) . 1_556 ? N1 C1 C2 123.6(2) . . ? C1 C2 C3 119.4(2) . . ? C2 C3 C2 117.1(3) 6_565 . ? C2 C3 C4 121.42(13) 6_565 . ? C2 C3 C4 121.42(13) . . ? C5 C4 C5 115.2(3) . 6_565 ? C5 C4 C3 122.42(15) . . ? C5 C4 C3 122.42(15) 6_565 . ? C4 C5 C6 120.7(3) . . ? N2 C6 C5 124.0(3) . . ? O1 C7 O1 126.0(3) 2_757 . ? O1 C7 C8 116.98(13) 2_757 . ? O1 C7 C8 116.98(13) . . ? C9 C8 C9 119.3(3) . 2_757 ? C9 C8 C7 120.34(14) . . ? C9 C8 C7 120.34(14) 2_757 . ? C9 C9 C8 120.34(14) 6 . ? O2 C10 O2 121.4(3) . 6_565 ? O2 C10 C11 119.27(14) . . ? O2 C10 C11 119.27(14) 6_565 . ? O2 C10 Co1 60.83(14) . . ? O2 C10 Co1 60.83(14) 6_565 . ? C11 C10 Co1 173.3(2) . . ? C13 C11 C13 49.9(5) 6_565 . ? C13 C11 C12 98.1(4) 6_565 . ? C13 C11 C12 119.9(4) . . ? C13 C11 C12 119.9(4) 6_565 6_565 ? C13 C11 C12 98.1(4) . 6_565 ? C12 C11 C12 50.1(5) . 6_565 ? C13 C11 C10 120.9(3) 6_565 . ? C13 C11 C10 120.9(3) . . ? C12 C11 C10 119.2(3) . . ? C12 C11 C10 119.2(3) 6_565 . ? C12 C12 C11 64.9(3) 6_565 . ? C12 C12 C13 89.8(3) 6_565 5_666 ? C11 C12 C13 120.1(4) . 5_666 ? C12 C12 C13 50.2(2) 6_565 2_656 ? C11 C12 C13 96.6(3) . 2_656 ? C13 C12 C13 39.6(4) 5_666 2_656 ? C13 C13 C11 65.1(2) 6_565 . ? C13 C13 C12 90.2(3) 6_565 5_666 ? C11 C13 C12 120.1(4) . 5_666 ? C13 C13 C12 50.2(2) 6_565 2_656 ? C11 C13 C12 96.5(4) . 2_656 ? C12 C13 C12 40.1(4) 5_666 2_656 ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.418 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.061 #==================================END data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Cd N2 O4' _chemical_formula_weight 432.70 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 16.108(3) _cell_length_b 11.675(2) _cell_length_c 20.171(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.99(3) _cell_angle_gamma 90.00 _cell_volume 3517.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7427 _exptl_absorpt_correction_T_max 0.9394 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12474 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5064 _reflns_number_gt 4139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.2296P] 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 0.00000(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5064 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 6.739 _refine_ls_shift/su_mean 0.030 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.079178(9) 0.294646(12) 0.196553(7) 0.02591(6) Uani 1 d . . . N1 N 0.07459(12) 0.49096(16) 0.19131(9) 0.0357(4) Uani 1 d . . . N2 N 0.06357(13) 1.09506(17) 0.19068(11) 0.0414(5) Uani 1 d . . . O1 O 0.06798(13) 0.31191(18) 0.06458(11) 0.0605(6) Uani 1 d . . . O2 O 0.18894(12) 0.26367(19) 0.15411(9) 0.0564(5) Uani 1 d . . . O3 O 0.19536(12) 0.28333(15) 0.30819(8) 0.0460(4) Uani 1 d . . . C2 C 0.02672(18) 0.6654(2) 0.12549(14) 0.0446(6) Uani 1 d . . . H2A H -0.0056 0.7023 0.0807 0.080 Uiso 1 d R . . C3 C 0.06944(14) 0.7304(2) 0.18634(13) 0.0369(5) Uani 1 d . . . C4 C 0.11496(17) 0.6716(2) 0.24958(14) 0.0450(6) Uani 1 d . . . H4A H 0.1460 0.7133 0.2928 0.080 Uiso 1 d R . . C5 C 0.11548(17) 0.5541(2) 0.24980(13) 0.0436(5) Uani 1 d . . . H5A H 0.1468 0.5152 0.2941 0.080 Uiso 1 d R . . C6 C 0.06758(15) 0.85718(19) 0.18569(12) 0.0373(5) Uani 1 d . . . C7 C -0.00840(17) 0.9184(2) 0.14593(15) 0.0519(7) Uani 1 d . . . H7A H -0.0610 0.8787 0.1155 0.080 Uiso 1 d R . . C8 C -0.00791(17) 1.0363(2) 0.15020(15) 0.0523(6) Uani 1 d . . . H8A H -0.0614 1.0778 0.1233 0.080 Uiso 1 d R . . C9 C 0.13771(16) 1.0370(2) 0.22800(15) 0.0471(6) Uani 1 d . . . H9A H 0.1901 1.0793 0.2565 0.080 Uiso 1 d R . . C10 C 0.14207(16) 0.9193(2) 0.22723(15) 0.0469(6) Uani 1 d . . . H10A H 0.1963 0.8803 0.2554 0.080 Uiso 1 d R . . C11 C 0.14727(16) 0.2819(2) 0.08946(13) 0.0402(5) Uani 1 d . . . C12 C 0.19910(17) 0.2651(2) 0.04172(12) 0.0417(5) Uani 1 d . . . C13 C 0.2469(2) 0.1648(3) 0.04671(16) 0.0577(7) Uani 1 d . . . C14 C 0.2028(2) 0.3511(3) -0.00419(15) 0.0567(7) Uani 1 d . . . C15 C 0.15346(14) 0.28676(17) 0.34891(11) 0.0308(4) Uani 1 d . . . C1 C 0.03163(18) 0.54813(19) 0.13008(13) 0.0448(6) Uani 1 d . . . H1A H 0.0026 0.5043 0.0873 0.080 Uiso 1 d R . . C16 C 0.20288(13) 0.26848(18) 0.42731(10) 0.0298(4) Uani 1 d . . . C18 C 0.15898(15) 0.2757(2) 0.47492(12) 0.0407(5) Uani 1 d . . . C17 C 0.29357(15) 0.2433(2) 0.45260(12) 0.0417(5) Uani 1 d . . . O4 O 0.07059(11) 0.30383(15) 0.32525(9) 0.0473(4) Uani 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 0.02943(9) 0.02490(8) 0.02414(8) 0.00047(5) 0.01087(6) 0.00118(5) N1 0.0443(11) 0.0245(9) 0.0361(10) 0.0009(7) 0.0127(9) 0.0002(7) N2 0.0421(11) 0.0282(10) 0.0531(12) 0.0002(8) 0.0169(10) 0.0003(8) O1 0.0437(11) 0.0946(17) 0.0467(11) -0.0070(10) 0.0210(9) 0.0135(10) O2 0.0492(11) 0.0926(15) 0.0335(9) -0.0031(9) 0.0226(8) 0.0030(10) O3 0.0457(10) 0.0675(12) 0.0242(8) 0.0031(7) 0.0123(7) 0.0034(8) C2 0.0543(15) 0.0323(11) 0.0406(13) 0.0053(10) 0.0103(11) 0.0020(11) C3 0.0361(12) 0.0272(11) 0.0478(14) 0.0014(9) 0.0162(11) 0.0006(8) C4 0.0499(14) 0.0320(12) 0.0436(14) -0.0019(10) 0.0064(11) -0.0010(10) C5 0.0542(14) 0.0297(12) 0.0390(13) 0.0029(9) 0.0084(11) -0.0003(10) C6 0.0422(12) 0.0254(11) 0.0452(13) 0.0020(9) 0.0173(10) 0.0021(8) C7 0.0437(14) 0.0318(12) 0.0638(17) -0.0017(11) 0.0013(12) 0.0009(10) C8 0.0457(14) 0.0322(12) 0.0667(17) 0.0028(12) 0.0071(12) 0.0063(10) C9 0.0380(12) 0.0294(12) 0.0691(17) -0.0010(11) 0.0145(12) 0.0005(10) C10 0.0360(12) 0.0303(12) 0.0674(17) 0.0027(11) 0.0114(11) 0.0039(9) C11 0.0405(13) 0.0494(14) 0.0358(12) -0.0074(10) 0.0202(10) -0.0033(10) C12 0.0417(13) 0.0580(15) 0.0292(11) -0.0043(10) 0.0177(10) 0.0038(11) C13 0.0665(18) 0.0643(18) 0.0543(17) 0.0091(14) 0.0363(15) 0.0136(15) C14 0.0691(18) 0.0610(18) 0.0519(16) 0.0065(13) 0.0365(14) 0.0156(14) C15 0.0335(10) 0.0297(10) 0.0233(9) 0.0007(7) 0.0039(8) -0.0054(8) C1 0.0589(15) 0.0290(11) 0.0384(12) 0.0002(9) 0.0088(11) -0.0003(10) C16 0.0278(10) 0.0368(11) 0.0231(9) 0.0017(8) 0.0075(8) -0.0002(8) C18 0.0271(10) 0.0666(17) 0.0265(11) 0.0061(10) 0.0080(9) 0.0071(10) C17 0.0297(11) 0.0675(16) 0.0263(11) 0.0037(11) 0.0086(9) 0.0074(11) O4 0.0282(8) 0.0682(13) 0.0355(9) 0.0148(8) 0.0004(7) -0.0022(7) _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 O2 2.2636(17) . ? Cd1 O4 2.2869(18) 2 ? Cd1 N1 2.2944(19) . ? Cd1 O3 2.3312(19) . ? Cd1 N2 2.342(2) 1_545 ? Cd1 O1 2.608(2) . ? N1 C5 1.337(3) . ? N1 C1 1.345(3) . ? N2 C8 1.326(3) . ? N2 C9 1.334(3) . ? N2 Cd1 2.342(2) 1_565 ? O1 C11 1.235(3) . ? O2 C11 1.241(3) . ? O3 C15 1.244(3) . ? C2 C1 1.373(3) . ? C2 C3 1.387(3) . ? C3 C4 1.391(3) . ? C3 C6 1.480(3) . ? C4 C5 1.371(3) . ? C6 C10 1.384(3) . ? C6 C7 1.385(3) . ? C7 C8 1.379(3) . ? C9 C10 1.377(3) . ? C11 C12 1.505(3) . ? C12 C14 1.383(4) . ? C12 C13 1.384(4) . ? C13 C14 1.395(4) 7 ? C14 C13 1.395(4) 7 ? C15 O4 1.254(3) . ? C15 C16 1.496(3) . ? C16 C17 1.387(3) . ? C16 C18 1.392(3) . ? C18 C17 1.391(3) 7_556 ? C17 C18 1.391(3) 7_556 ? O4 Cd1 2.2869(18) 2 ? 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 O2 Cd1 O4 148.42(7) . 2 ? O2 Cd1 N1 99.11(7) . . ? O4 Cd1 N1 86.03(6) 2 . ? O2 Cd1 O3 84.15(7) . . ? O4 Cd1 O3 126.58(7) 2 . ? N1 Cd1 O3 95.83(6) . . ? O2 Cd1 N2 84.61(7) . 1_545 ? O4 Cd1 N2 87.21(6) 2 1_545 ? N1 Cd1 N2 172.15(7) . 1_545 ? O3 Cd1 N2 91.41(6) . 1_545 ? O2 Cd1 O1 52.52(7) . . ? O4 Cd1 O1 97.78(7) 2 . ? N1 Cd1 O1 83.51(6) . . ? O3 Cd1 O1 135.57(6) . . ? N2 Cd1 O1 93.45(7) 1_545 . ? C5 N1 C1 116.8(2) . . ? C5 N1 Cd1 120.91(15) . . ? C1 N1 Cd1 122.32(15) . . ? C8 N2 C9 118.2(2) . . ? C8 N2 Cd1 126.73(16) . 1_565 ? C9 N2 Cd1 114.86(16) . 1_565 ? C11 O1 Cd1 84.12(15) . . ? C11 O2 Cd1 100.27(15) . . ? C15 O3 Cd1 101.43(14) . . ? C1 C2 C3 119.3(2) . . ? C2 C3 C4 117.3(2) . . ? C2 C3 C6 122.5(2) . . ? C4 C3 C6 120.2(2) . . ? C5 C4 C3 119.8(2) . . ? N1 C5 C4 123.3(2) . . ? C10 C6 C7 117.3(2) . . ? C10 C6 C3 120.6(2) . . ? C7 C6 C3 122.1(2) . . ? C8 C7 C6 119.7(2) . . ? N2 C8 C7 122.6(2) . . ? N2 C9 C10 122.7(2) . . ? C9 C10 C6 119.6(2) . . ? O1 C11 O2 123.1(2) . . ? O1 C11 C12 120.9(2) . . ? O2 C11 C12 116.0(2) . . ? C14 C12 C13 120.1(2) . . ? C14 C12 C11 120.5(2) . . ? C13 C12 C11 119.4(2) . . ? C12 C13 C14 120.2(3) . 7 ? C12 C14 C13 119.7(3) . 7 ? O3 C15 O4 121.2(2) . . ? O3 C15 C16 119.21(19) . . ? O4 C15 C16 119.6(2) . . ? N1 C1 C2 123.6(2) . . ? C17 C16 C18 119.8(2) . . ? C17 C16 C15 119.30(19) . . ? C18 C16 C15 120.93(19) . . ? C17 C18 C16 119.6(2) 7_556 . ? C16 C17 C18 120.6(2) . 7_556 ? C15 O4 Cd1 164.10(15) . 2 ? _diffrn_measured_fraction_theta_max 0.470 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.470 _refine_diff_density_max 0.782 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.077 #==================================END data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 O4 Zn' _chemical_formula_weight 385.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.187(2) _cell_length_b 10.276(2) _cell_length_c 10.976(2) _cell_angle_alpha 67.89(3) _cell_angle_beta 68.19(3) _cell_angle_gamma 65.69(3) _cell_volume 845.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7566 _exptl_absorpt_correction_T_max 0.9037 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6923 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 30.04 _reflns_number_total 4698 _reflns_number_gt 3816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.4967P] 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 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4698 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 3.713 _refine_ls_shift/su_mean 0.019 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.12037(4) 0.38499(3) 0.14717(3) 0.02858(12) Uani 1 d . . . O3 O 0.0663(3) 0.6032(2) 0.1162(2) 0.0416(5) Uani 1 d . . . O4 O -0.0012(3) 0.6889(2) -0.0811(2) 0.0413(5) Uani 1 d . . . N1 N 0.3223(3) 0.3700(3) -0.0329(2) 0.0388(5) Uani 1 d . . . N2 N 0.9191(3) 0.3824(3) -0.6669(3) 0.0417(6) Uani 1 d . . . C7 C 0.0644(4) 0.8804(3) 0.0996(3) 0.0433(7) Uani 1 d . . . H7A H 0.1092 0.7976 0.1683 0.080 Uiso 1 d R . . O1 O 0.2714(3) 0.3080(2) 0.2714(2) 0.0489(5) Uani 1 d . . . C5 C 0.0249(3) 0.7053(3) 0.0154(3) 0.0323(5) Uani 1 d . . . C14 C 0.6932(4) 0.3682(3) -0.4104(3) 0.0400(6) Uani 1 d . . . C11 C 0.5701(4) 0.3641(3) -0.2770(3) 0.0384(6) Uani 1 d . . . C6 C 0.0118(3) 0.8579(3) 0.0079(3) 0.0329(5) Uani 1 d . . . C2 C 0.4122(4) 0.0823(3) 0.4018(3) 0.0413(7) Uani 1 d . . . C1 C 0.3147(4) 0.1699(3) 0.2970(3) 0.0431(7) Uani 1 d . . . C8 C 0.0534(4) 1.0226(3) 0.0921(3) 0.0425(7) Uani 1 d . . . C13 C 0.3908(4) 0.4780(4) -0.0969(4) 0.0488(8) Uani 1 d . . . H13A H 0.3534 0.5583 -0.0568 0.080 Uiso 1 d R . . C9 C 0.3837(4) 0.2556(3) -0.0866(3) 0.0502(8) Uani 1 d . . . H9A H 0.3404 0.1742 -0.0395 0.080 Uiso 1 d R . . C12 C 0.5115(4) 0.4803(4) -0.2172(4) 0.0511(8) Uani 1 d . . . H12A H 0.5554 0.5616 -0.2604 0.080 Uiso 1 d R . . O2 O 0.2803(5) 0.1070(3) 0.2423(3) 0.0835(11) Uani 1 d . . . C4 C 0.5700(6) -0.0128(6) 0.3689(5) 0.0888(16) Uani 1 d . . . C10 C 0.5050(4) 0.2487(4) -0.2062(4) 0.0510(8) Uani 1 d . . . H10A H 0.5454 0.1636 -0.2404 0.080 Uiso 1 d R . . C17 C 0.8754(7) 0.4791(5) -0.5996(4) 0.0930(19) Uani 1 d . . . H17A H 0.9227 0.5582 -0.6414 0.080 Uiso 1 d R . . C18 C 0.7660(7) 0.4756(5) -0.4732(5) 0.094(2) Uani 1 d . . . H18A H 0.7408 0.5500 -0.4291 0.080 Uiso 1 d R . . C16 C 0.8497(6) 0.2775(5) -0.6066(4) 0.0844(17) Uani 1 d . . . H16A H 0.8758 0.2059 -0.6540 0.080 Uiso 1 d R . . C15 C 0.7410(7) 0.2658(5) -0.4801(5) 0.0913(19) Uani 1 d . . . H15A H 0.6982 0.1838 -0.4395 0.080 Uiso 1 d R . . C3 C 0.3444(6) 0.0959(6) 0.5292(5) 0.0889(17) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03149(18) 0.02956(16) 0.02324(16) -0.00559(11) -0.00749(11) -0.00911(12) O3 0.0584(13) 0.0264(8) 0.0311(10) -0.0032(7) -0.0085(9) -0.0115(9) O4 0.0530(13) 0.0386(10) 0.0425(11) -0.0121(9) -0.0143(10) -0.0210(9) N1 0.0351(12) 0.0450(13) 0.0303(11) -0.0113(10) 0.0007(10) -0.0140(10) N2 0.0431(14) 0.0509(14) 0.0318(12) -0.0145(11) 0.0021(10) -0.0227(12) C7 0.065(2) 0.0279(12) 0.0411(15) 0.0007(11) -0.0319(15) -0.0109(13) O1 0.0567(14) 0.0397(11) 0.0469(12) 0.0014(9) -0.0288(11) -0.0099(10) C5 0.0327(13) 0.0287(11) 0.0301(12) -0.0063(10) -0.0032(10) -0.0103(10) C14 0.0384(15) 0.0479(15) 0.0308(13) -0.0133(12) 0.0022(11) -0.0183(13) C11 0.0347(14) 0.0446(15) 0.0336(13) -0.0144(12) 0.0009(11) -0.0155(12) C6 0.0406(14) 0.0259(11) 0.0328(13) -0.0038(10) -0.0138(11) -0.0107(10) C2 0.0528(18) 0.0312(12) 0.0416(15) -0.0024(11) -0.0259(14) -0.0090(12) C1 0.0475(17) 0.0401(14) 0.0420(16) 0.0015(12) -0.0229(14) -0.0153(13) C8 0.063(2) 0.0310(12) 0.0410(15) -0.0027(11) -0.0305(15) -0.0134(13) C13 0.0452(17) 0.0584(18) 0.0494(18) -0.0309(16) 0.0062(14) -0.0237(15) C9 0.0536(19) 0.0392(15) 0.0420(16) -0.0112(13) 0.0098(14) -0.0189(14) C12 0.0483(18) 0.0539(18) 0.0535(19) -0.0262(16) 0.0114(15) -0.0294(15) O2 0.139(3) 0.0571(15) 0.090(2) 0.0038(15) -0.086(2) -0.0351(18) C4 0.065(3) 0.119(4) 0.053(2) -0.010(3) -0.030(2) 0.000(3) C10 0.0546(19) 0.0440(16) 0.0463(18) -0.0210(14) 0.0097(15) -0.0197(14) C17 0.137(4) 0.100(3) 0.057(2) -0.047(2) 0.049(3) -0.094(3) C18 0.138(5) 0.091(3) 0.062(3) -0.053(2) 0.049(3) -0.082(3) C16 0.110(4) 0.078(3) 0.063(3) -0.046(2) 0.045(3) -0.063(3) C15 0.123(4) 0.083(3) 0.069(3) -0.048(2) 0.055(3) -0.079(3) C3 0.063(3) 0.123(4) 0.054(2) -0.023(3) -0.030(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.998(2) 2_565 ? Zn1 O3 2.0065(19) . ? Zn1 O1 2.025(2) . ? Zn1 N1 2.154(2) . ? Zn1 N2 2.186(3) 1_456 ? O3 C5 1.257(3) . ? O4 C5 1.250(3) . ? O4 Zn1 1.998(2) 2_565 ? N1 C9 1.333(4) . ? N1 C13 1.334(4) . ? N2 C17 1.304(4) . ? N2 C16 1.312(4) . ? N2 Zn1 2.186(3) 1_654 ? C7 C6 1.388(4) . ? C7 C8 1.395(4) . ? O1 C1 1.253(4) . ? C5 C6 1.495(3) . ? C14 C18 1.354(5) . ? C14 C15 1.364(5) . ? C14 C11 1.479(4) . ? C11 C10 1.382(4) . ? C11 C12 1.394(4) . ? C6 C8 1.393(4) 2_575 ? C2 C3 1.339(5) . ? C2 C4 1.377(6) . ? C2 C1 1.503(4) . ? C1 O2 1.216(4) . ? C8 C6 1.393(4) 2_575 ? C13 C12 1.373(4) . ? C9 C10 1.373(4) . ? C4 C3 1.407(6) 2_656 ? C17 C18 1.376(5) . ? C16 C15 1.373(5) . ? C3 C4 1.407(6) 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 Zn1 O3 120.11(9) 2_565 . ? O4 Zn1 O1 139.75(9) 2_565 . ? O3 Zn1 O1 99.33(10) . . ? O4 Zn1 N1 91.07(10) 2_565 . ? O3 Zn1 N1 94.88(10) . . ? O1 Zn1 N1 93.44(10) . . ? O4 Zn1 N2 86.76(10) 2_565 1_456 ? O3 Zn1 N2 89.40(10) . 1_456 ? O1 Zn1 N2 85.87(10) . 1_456 ? N1 Zn1 N2 175.72(9) . 1_456 ? C5 O3 Zn1 127.53(19) . . ? C5 O4 Zn1 149.5(2) . 2_565 ? C9 N1 C13 116.8(3) . . ? C9 N1 Zn1 122.6(2) . . ? C13 N1 Zn1 120.6(2) . . ? C17 N2 C16 115.4(3) . . ? C17 N2 Zn1 119.8(2) . 1_654 ? C16 N2 Zn1 124.2(2) . 1_654 ? C6 C7 C8 120.4(2) . . ? C1 O1 Zn1 104.86(19) . . ? O4 C5 O3 125.4(2) . . ? O4 C5 C6 117.4(2) . . ? O3 C5 C6 117.2(2) . . ? C18 C14 C15 114.9(3) . . ? C18 C14 C11 122.1(3) . . ? C15 C14 C11 122.9(3) . . ? C10 C11 C12 116.5(3) . . ? C10 C11 C14 122.9(3) . . ? C12 C11 C14 120.6(3) . . ? C7 C6 C8 120.2(2) . 2_575 ? C7 C6 C5 120.4(2) . . ? C8 C6 C5 119.4(2) 2_575 . ? C3 C2 C4 119.4(3) . . ? C3 C2 C1 119.6(3) . . ? C4 C2 C1 121.0(3) . . ? O2 C1 O1 123.1(3) . . ? O2 C1 C2 120.4(3) . . ? O1 C1 C2 116.5(3) . . ? C7 C8 C6 119.3(3) . 2_575 ? N1 C13 C12 123.4(3) . . ? N1 C9 C10 123.4(3) . . ? C13 C12 C11 119.7(3) . . ? C2 C4 C3 119.2(4) . 2_656 ? C9 C10 C11 120.0(3) . . ? N2 C17 C18 124.4(3) . . ? C14 C18 C17 120.6(3) . . ? N2 C16 C15 123.5(3) . . ? C14 C15 C16 121.1(3) . . ? C2 C3 C4 121.3(4) . 2_656 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.171 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.087 #_eof #End of Crystallographic Information File