# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email sunwy@nju.edu.cn loop_ _publ_author_name 'Hai-Wei Kuai' 'Jian Fan' 'Qing Liu' 'Wei-Yin Sun' data_1 _database_code_depnum_ccdc_archive 'CCDC 846234' #TrackingRef '- CE-ART-01-2012-025062.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H17 Cd N3 O6, H2 O' _chemical_formula_sum 'C15 H19 Cd N3 O7' _chemical_formula_weight 465.73 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1534(13) _cell_length_b 10.1725(13) _cell_length_c 11.3570(14) _cell_angle_alpha 114.9560(10) _cell_angle_beta 90.045(2) _cell_angle_gamma 118.9180(10) _cell_volume 899.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3533 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7872 _exptl_absorpt_correction_T_max 0.7872 _exptl_absorpt_process_details 'SADABS Bruker, 2000' _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 4940 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3462 _reflns_number_gt 3187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 0.82 0.005 O7 H19 was used to fix the O-H distance of water molecule. ; _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^)+(0.0474P)^2^] 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 3462 _refine_ls_number_parameters 237 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.56147(2) 0.45916(3) 0.727211(19) 0.02909(10) Uani 1 1 d . . . N11 N 0.9566(3) 1.3522(3) 1.3083(2) 0.0329(6) Uani 1 1 d . . . N12 N 1.2030(3) 1.4360(4) 1.3240(3) 0.0385(6) Uani 1 1 d . . . N61 N 0.1027(3) 0.1838(4) 0.8023(3) 0.0482(8) Uani 1 1 d . . . O1 O 0.6238(3) 0.7195(3) 0.9028(2) 0.0427(6) Uani 1 1 d . . . O2 O 0.5415(3) 0.6904(3) 0.7098(2) 0.0412(6) Uani 1 1 d . . . O3 O 0.5636(4) 1.1985(3) 0.7104(2) 0.0511(7) Uani 1 1 d . . . O4 O 0.6631(3) 1.4381(3) 0.8996(2) 0.0499(7) Uani 1 1 d . . . O5 O 0.4316(4) 0.2662(4) 0.5051(2) 0.0674(9) Uani 1 1 d . . . H17 H 0.3706 0.1581 0.4868 0.081 Uiso 1 1 d R . . H16 H 0.4377 0.2847 0.4351 0.081 Uiso 1 1 d R . . O6 O 0.3081(3) 0.3265(4) 0.7365(3) 0.0528(7) Uani 1 1 d . . . O7 O 0.3002(4) 0.9325(4) 0.4975(3) 0.0758(9) Uani 1 1 d D . . H18 H 0.3747 1.0065 0.5748 0.091 Uiso 1 1 d R . . H19 H 0.3202 0.8578 0.4587 0.091 Uiso 1 1 d RD . . C1 C 0.7421(3) 1.2267(4) 1.1162(3) 0.0286(6) Uani 1 1 d . . . C2 C 0.7029(3) 1.0565(4) 1.0451(3) 0.0279(6) Uani 1 1 d . . . H1 H 0.7185 1.0064 1.0913 0.033 Uiso 1 1 calc R . . C3 C 0.6412(3) 0.9619(4) 0.9075(3) 0.0261(6) Uani 1 1 d . . . C4 C 0.6181(3) 1.0375(4) 0.8386(3) 0.0272(6) Uani 1 1 d . . . H2 H 0.5767 0.9745 0.7459 0.033 Uiso 1 1 calc R . . C5 C 0.6567(3) 1.2062(4) 0.9074(3) 0.0278(6) Uani 1 1 d . . . C6 C 0.7189(3) 1.3009(4) 1.0467(3) 0.0292(6) Uani 1 1 d . . . H3 H 0.7448 1.4139 1.0929 0.035 Uiso 1 1 calc R . . C11 C 0.8045(4) 1.3246(4) 1.2668(3) 0.0369(7) Uani 1 1 d . . . H5 H 0.8144 1.4348 1.3010 0.044 Uiso 1 1 calc R . . H4 H 0.7311 1.2618 1.3059 0.044 Uiso 1 1 calc R . . C12 C 1.0847(4) 1.4313(5) 1.2713(3) 0.0400(8) Uani 1 1 d . . . H6 H 1.0894 1.4774 1.2149 0.048 Uiso 1 1 calc R . . C13 C 1.1468(4) 1.3567(5) 1.4002(3) 0.0426(8) Uani 1 1 d . . . H7 H 1.2048 1.3417 1.4510 0.051 Uiso 1 1 calc R . . C14 C 0.9958(4) 1.3037(5) 1.3911(4) 0.0433(8) Uani 1 1 d . . . H8 H 0.9311 1.2457 1.4328 0.052 Uiso 1 1 calc R . . C31 C 0.5992(4) 0.7792(4) 0.8351(3) 0.0290(6) Uani 1 1 d . . . C51 C 0.6254(4) 1.2866(4) 0.8348(3) 0.0325(7) Uani 1 1 d . . . C61 C 0.2523(4) 0.2709(4) 0.8139(3) 0.0384(7) Uani 1 1 d . . . H9 H 0.3201 0.2920 0.8839 0.046 Uiso 1 1 calc R . . C62 C 0.0413(5) 0.1299(6) 0.9007(4) 0.0678(12) Uani 1 1 d . . . H10 H 0.1255 0.1601 0.9656 0.102 Uiso 1 1 calc R . . H12 H -0.0307 0.0080 0.8559 0.102 Uiso 1 1 calc R . . H11 H -0.0113 0.1862 0.9455 0.102 Uiso 1 1 calc R . . C63 C -0.0104(5) 0.1479(8) 0.6960(5) 0.0881(17) Uani 1 1 d . . . H15 H 0.0429 0.1917 0.6390 0.132 Uiso 1 1 calc R . . H13 H -0.0663 0.2021 0.7354 0.132 Uiso 1 1 calc R . . H14 H -0.0822 0.0263 0.6438 0.132 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03266(15) 0.02940(15) 0.02827(14) 0.01450(11) 0.00721(9) 0.01812(11) N11 0.0322(14) 0.0422(15) 0.0249(12) 0.0152(11) 0.0055(10) 0.0211(12) N12 0.0353(15) 0.0458(17) 0.0365(15) 0.0198(13) 0.0080(12) 0.0231(14) N61 0.0319(16) 0.059(2) 0.0470(17) 0.0266(16) 0.0103(13) 0.0186(15) O1 0.0642(16) 0.0401(13) 0.0373(12) 0.0219(11) 0.0083(11) 0.0342(13) O2 0.0585(16) 0.0324(13) 0.0312(12) 0.0135(10) 0.0066(11) 0.0248(12) O3 0.0737(19) 0.0451(15) 0.0353(13) 0.0192(12) -0.0034(12) 0.0325(14) O4 0.082(2) 0.0419(14) 0.0432(14) 0.0237(12) 0.0143(13) 0.0422(14) O5 0.095(2) 0.0445(16) 0.0278(13) 0.0168(12) -0.0001(13) 0.0146(15) O6 0.0408(15) 0.0596(17) 0.0530(16) 0.0314(14) 0.0150(13) 0.0198(13) O7 0.0521(18) 0.073(2) 0.066(2) 0.0146(17) 0.0068(15) 0.0253(17) C1 0.0231(14) 0.0359(16) 0.0283(14) 0.0148(13) 0.0074(12) 0.0173(13) C2 0.0295(15) 0.0366(16) 0.0306(15) 0.0208(13) 0.0101(12) 0.0225(13) C3 0.0223(14) 0.0280(15) 0.0328(15) 0.0159(12) 0.0092(11) 0.0157(12) C4 0.0279(15) 0.0303(15) 0.0264(14) 0.0146(12) 0.0079(12) 0.0168(13) C5 0.0277(15) 0.0333(16) 0.0333(15) 0.0200(13) 0.0111(12) 0.0203(13) C6 0.0277(15) 0.0268(15) 0.0339(15) 0.0133(12) 0.0090(12) 0.0162(13) C11 0.0333(17) 0.049(2) 0.0284(15) 0.0127(15) 0.0081(13) 0.0268(16) C12 0.0388(18) 0.052(2) 0.0394(17) 0.0289(16) 0.0129(14) 0.0257(17) C13 0.043(2) 0.058(2) 0.0396(18) 0.0283(17) 0.0096(15) 0.0317(18) C14 0.045(2) 0.057(2) 0.0390(18) 0.0307(17) 0.0149(16) 0.0282(18) C31 0.0305(15) 0.0312(16) 0.0336(16) 0.0182(13) 0.0121(13) 0.0199(13) C51 0.0338(16) 0.0368(17) 0.0385(17) 0.0232(14) 0.0100(13) 0.0224(14) C61 0.0320(17) 0.0423(19) 0.0373(17) 0.0155(15) 0.0088(14) 0.0205(15) C62 0.043(2) 0.090(3) 0.066(3) 0.047(3) 0.021(2) 0.025(2) C63 0.041(3) 0.125(5) 0.082(3) 0.060(3) 0.002(2) 0.026(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 Cd1 O6 2.283(3) . ? Cd1 N12 2.292(3) 2_777 ? Cd1 O5 2.295(3) . ? Cd1 O1 2.305(2) . ? Cd1 O4 2.347(2) 1_545 ? Cd1 O2 2.542(2) . ? Cd1 O3 2.588(3) 1_545 ? N11 C12 1.338(4) . ? N11 C14 1.368(4) . ? N11 C11 1.467(4) . ? N12 C12 1.313(4) . ? N12 C13 1.367(4) . ? N12 Cd1 2.292(3) 2_777 ? N61 C61 1.307(4) . ? N61 C62 1.458(5) . ? N61 C63 1.459(5) . ? O1 C31 1.250(4) . ? O2 C31 1.259(4) . ? O3 C51 1.257(4) . ? O3 Cd1 2.588(3) 1_565 ? O4 C51 1.239(4) . ? O4 Cd1 2.347(2) 1_565 ? O5 H17 0.8853 . ? O5 H16 0.8867 . ? O6 C61 1.234(4) . ? O7 H18 0.8946 . ? O7 H19 0.8250 . ? C1 C6 1.387(4) . ? C1 C2 1.400(4) . ? C1 C11 1.506(4) . ? C2 C3 1.381(4) . ? C2 H1 0.9300 . ? C3 C4 1.392(4) . ? C3 C31 1.502(4) . ? C4 C5 1.389(4) . ? C4 H2 0.9300 . ? C5 C6 1.398(4) . ? C5 C51 1.506(4) . ? C6 H3 0.9300 . ? C11 H5 0.9700 . ? C11 H4 0.9700 . ? C12 H6 0.9300 . ? C13 C14 1.343(5) . ? C13 H7 0.9300 . ? C14 H8 0.9300 . ? C61 H9 0.9300 . ? C62 H10 0.9600 . ? C62 H12 0.9600 . ? C62 H11 0.9600 . ? C63 H15 0.9600 . ? C63 H13 0.9600 . ? C63 H14 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cd1 N12 169.48(9) . 2_777 ? O6 Cd1 O5 77.67(11) . . ? N12 Cd1 O5 91.88(11) 2_777 . ? O6 Cd1 O1 92.84(10) . . ? N12 Cd1 O1 95.01(10) 2_777 . ? O5 Cd1 O1 144.37(10) . . ? O6 Cd1 O4 96.69(10) . 1_545 ? N12 Cd1 O4 91.29(10) 2_777 1_545 ? O5 Cd1 O4 132.48(10) . 1_545 ? O1 Cd1 O4 82.33(8) . 1_545 ? O6 Cd1 O2 90.96(10) . . ? N12 Cd1 O2 88.12(9) 2_777 . ? O5 Cd1 O2 92.01(9) . . ? O1 Cd1 O2 53.45(7) . . ? O4 Cd1 O2 135.48(8) 1_545 . ? O6 Cd1 O3 87.80(10) . 1_545 ? N12 Cd1 O3 91.71(10) 2_777 1_545 ? O5 Cd1 O3 80.23(9) . 1_545 ? O1 Cd1 O3 134.26(8) . 1_545 ? O4 Cd1 O3 52.29(8) 1_545 1_545 ? O2 Cd1 O3 172.23(7) . 1_545 ? C12 N11 C14 106.7(3) . . ? C12 N11 C11 125.9(3) . . ? C14 N11 C11 127.5(3) . . ? C12 N12 C13 104.9(3) . . ? C12 N12 Cd1 123.1(2) . 2_777 ? C13 N12 Cd1 131.9(2) . 2_777 ? C61 N61 C62 121.8(3) . . ? C61 N61 C63 121.4(3) . . ? C62 N61 C63 116.7(3) . . ? C31 O1 Cd1 97.98(19) . . ? C31 O2 Cd1 86.65(18) . . ? C51 O3 Cd1 86.76(19) . 1_565 ? C51 O4 Cd1 98.5(2) . 1_565 ? Cd1 O5 H17 115.2 . . ? Cd1 O5 H16 128.7 . . ? H17 O5 H16 116.0 . . ? C61 O6 Cd1 128.9(3) . . ? H18 O7 H19 104.1 . . ? C6 C1 C2 119.2(3) . . ? C6 C1 C11 121.0(3) . . ? C2 C1 C11 119.8(3) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H1 119.5 . . ? C1 C2 H1 119.5 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 C31 119.5(3) . . ? C4 C3 C31 121.2(3) . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H2 119.8 . . ? C3 C4 H2 119.8 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C51 120.8(3) . . ? C6 C5 C51 119.3(3) . . ? C1 C6 C5 120.2(3) . . ? C1 C6 H3 119.9 . . ? C5 C6 H3 119.9 . . ? N11 C11 C1 112.1(2) . . ? N11 C11 H5 109.2 . . ? C1 C11 H5 109.2 . . ? N11 C11 H4 109.2 . . ? C1 C11 H4 109.2 . . ? H5 C11 H4 107.9 . . ? N12 C12 N11 112.0(3) . . ? N12 C12 H6 124.0 . . ? N11 C12 H6 124.0 . . ? C14 C13 N12 110.4(3) . . ? C14 C13 H7 124.8 . . ? N12 C13 H7 124.8 . . ? C13 C14 N11 106.1(3) . . ? C13 C14 H8 127.0 . . ? N11 C14 H8 127.0 . . ? O1 C31 O2 121.6(3) . . ? O1 C31 C3 118.0(3) . . ? O2 C31 C3 120.4(3) . . ? O4 C51 O3 122.2(3) . . ? O4 C51 C5 118.8(3) . . ? O3 C51 C5 119.0(3) . . ? O6 C61 N61 123.3(3) . . ? O6 C61 H9 118.3 . . ? N61 C61 H9 118.3 . . ? N61 C62 H10 109.5 . . ? N61 C62 H12 109.5 . . ? H10 C62 H12 109.5 . . ? N61 C62 H11 109.5 . . ? H10 C62 H11 109.5 . . ? H12 C62 H11 109.5 . . ? N61 C63 H15 109.5 . . ? N61 C63 H13 109.5 . . ? H15 C63 H13 109.5 . . ? N61 C63 H14 109.5 . . ? H15 C63 H14 109.5 . . ? H13 C63 H14 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cd1 O1 C31 -92.3(2) . . . . ? N12 Cd1 O1 C31 80.7(2) 2_777 . . . ? O5 Cd1 O1 C31 -19.6(3) . . . . ? O4 Cd1 O1 C31 171.3(2) 1_545 . . . ? O2 Cd1 O1 C31 -3.21(18) . . . . ? O3 Cd1 O1 C31 178.01(18) 1_545 . . . ? O6 Cd1 O2 C31 95.99(19) . . . . ? N12 Cd1 O2 C31 -94.5(2) 2_777 . . . ? O5 Cd1 O2 C31 173.7(2) . . . . ? O1 Cd1 O2 C31 3.16(18) . . . . ? O4 Cd1 O2 C31 -4.6(2) 1_545 . . . ? O3 Cd1 O2 C31 176.7(5) 1_545 . . . ? N12 Cd1 O6 C61 141.5(5) 2_777 . . . ? O5 Cd1 O6 C61 134.5(3) . . . . ? O1 Cd1 O6 C61 -80.2(3) . . . . ? O4 Cd1 O6 C61 2.4(3) 1_545 . . . ? O2 Cd1 O6 C61 -133.6(3) . . . . ? O3 Cd1 O6 C61 54.0(3) 1_545 . . . ? C6 C1 C2 C3 -0.2(4) . . . . ? C11 C1 C2 C3 178.1(3) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C1 C2 C3 C31 -179.4(3) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C31 C3 C4 C5 179.6(3) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C3 C4 C5 C51 -177.2(3) . . . . ? C2 C1 C6 C5 0.2(4) . . . . ? C11 C1 C6 C5 -178.1(3) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? C51 C5 C6 C1 177.2(3) . . . . ? C12 N11 C11 C1 57.5(4) . . . . ? C14 N11 C11 C1 -122.7(3) . . . . ? C6 C1 C11 N11 -116.3(3) . . . . ? C2 C1 C11 N11 65.4(4) . . . . ? C13 N12 C12 N11 -0.7(4) . . . . ? Cd1 N12 C12 N11 175.0(2) 2_777 . . . ? C14 N11 C12 N12 0.4(4) . . . . ? C11 N11 C12 N12 -179.7(3) . . . . ? C12 N12 C13 C14 0.8(4) . . . . ? Cd1 N12 C13 C14 -174.4(2) 2_777 . . . ? N12 C13 C14 N11 -0.6(4) . . . . ? C12 N11 C14 C13 0.1(4) . . . . ? C11 N11 C14 C13 -179.7(3) . . . . ? Cd1 O1 C31 O2 6.1(3) . . . . ? Cd1 O1 C31 C3 -173.7(2) . . . . ? Cd1 O2 C31 O1 -5.5(3) . . . . ? Cd1 O2 C31 C3 174.3(3) . . . . ? C2 C3 C31 O1 -0.9(4) . . . . ? C4 C3 C31 O1 179.6(3) . . . . ? C2 C3 C31 O2 179.4(3) . . . . ? C4 C3 C31 O2 -0.2(4) . . . . ? Cd1 O4 C51 O3 5.2(4) 1_565 . . . ? Cd1 O4 C51 C5 -175.6(2) 1_565 . . . ? Cd1 O3 C51 O4 -4.7(3) 1_565 . . . ? Cd1 O3 C51 C5 176.1(3) 1_565 . . . ? C4 C5 C51 O4 -179.2(3) . . . . ? C6 C5 C51 O4 3.6(4) . . . . ? C4 C5 C51 O3 0.1(5) . . . . ? C6 C5 C51 O3 -177.1(3) . . . . ? Cd1 O6 C61 N61 -173.9(3) . . . . ? C62 N61 C61 O6 -175.8(4) . . . . ? C63 N61 C61 O6 -0.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.707 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.091 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 846235' #TrackingRef '- CE-ART-01-2012-025062.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H12 Cd N2 O6), 5(H2 O)' _chemical_formula_sum 'C24 H34 Cd2 N4 O17' _chemical_formula_weight 875.35 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 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.262(4) _cell_length_b 17.100(7) _cell_length_c 10.488(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.160(5) _cell_angle_gamma 90.00 _cell_volume 1607.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6326 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7664 _exptl_absorpt_correction_T_max 0.7664 _exptl_absorpt_process_details 'SADABS Bruker, 2000' _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 8044 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3102 _reflns_number_gt 2890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 0.82 0.005 O6 H11 O6 H12 and DFIX 0.82 0.005 O5 H9 O5 H10 were used to fix the O-H distances of water molecule. ; _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^)+(0.0570P)^2^+1.7316P] 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 3102 _refine_ls_number_parameters 217 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.118 _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 0.39621(3) 1.018047(16) 0.21443(3) 0.03280(14) Uani 1 1 d . . . N11 N 0.1657(3) 0.72096(18) 0.5630(3) 0.0339(7) Uani 1 1 d . . . N12 N 0.1780(3) 0.61953(19) 0.4404(4) 0.0366(7) Uani 1 1 d . . . O1 O 0.2936(3) 0.93820(18) 0.3174(3) 0.0415(6) Uani 1 1 d . . . O2 O 0.1366(4) 1.03350(19) 0.2061(4) 0.0498(8) Uani 1 1 d . . . O3 O -0.3580(3) 1.02984(19) 0.2119(3) 0.0446(7) Uani 1 1 d . . . O4 O -0.3843(3) 0.9471(2) 0.3591(3) 0.0464(7) Uani 1 1 d . . . O5 O 0.3386(3) 0.92719(18) 0.0309(3) 0.0469(7) Uani 1 1 d D . . H9 H 0.2641 0.8993 -0.0051 0.056 Uiso 1 1 d RD . . H10 H 0.3417 0.9533 -0.0330 0.056 Uiso 1 1 d RD . . O6 O 0.4666(4) 1.1027(2) 0.4163(4) 0.0703(11) Uani 1 1 d D . . H12 H 0.5433 1.0889 0.4890 0.084 Uiso 1 1 d RD . . H11 H 0.4868 1.1471 0.4014 0.084 Uiso 1 1 d RD . . O7 O 0.0744(4) 0.8507(2) 0.9028(5) 0.0753(11) Uani 1 1 d . . . O8 O 0.4704(10) 0.7929(4) 0.3162(10) 0.130(3) Uani 0.80 1 d P . . O9 O 0.3171(12) 0.2618(4) 0.3210(9) 0.128(3) Uani 0.70 1 d P . . C1 C 0.0385(4) 0.8496(2) 0.4950(4) 0.0316(7) Uani 1 1 d . . . C2 C 0.1251(4) 0.8796(2) 0.4385(4) 0.0316(7) Uani 1 1 d . . . H1 H 0.2178 0.8575 0.4656 0.038 Uiso 1 1 calc R . . C3 C 0.0750(4) 0.9421(2) 0.3418(4) 0.0294(7) Uani 1 1 d . . . C4 C -0.0658(4) 0.9738(2) 0.2991(4) 0.0299(7) Uani 1 1 d . . . H2 H -0.0999 1.0158 0.2346 0.036 Uiso 1 1 calc R . . C5 C -0.1555(4) 0.9429(2) 0.3524(4) 0.0299(7) Uani 1 1 d . . . C6 C -0.1023(4) 0.8803(2) 0.4505(4) 0.0323(7) Uani 1 1 d . . . H3 H -0.1617 0.8591 0.4861 0.039 Uiso 1 1 calc R . . C11 C 0.0992(5) 0.7841(2) 0.6064(4) 0.0392(8) Uani 1 1 d . . . H5 H 0.1739 0.8053 0.6994 0.047 Uiso 1 1 calc R . . H4 H 0.0188 0.7630 0.6196 0.047 Uiso 1 1 calc R . . C12 C 0.0900(4) 0.6636(2) 0.4689(4) 0.0378(8) Uani 1 1 d . . . H6 H -0.0122 0.6558 0.4286 0.045 Uiso 1 1 calc R . . C13 C 0.3187(4) 0.6508(2) 0.5203(4) 0.0396(9) Uani 1 1 d . . . H7 H 0.4047 0.6317 0.5226 0.048 Uiso 1 1 calc R . . C14 C 0.3120(4) 0.7140(2) 0.5951(4) 0.0403(9) Uani 1 1 d . . . H8 H 0.3909 0.7463 0.6562 0.048 Uiso 1 1 calc R . . C31 C 0.1726(4) 0.9743(2) 0.2835(4) 0.0338(8) Uani 1 1 d . . . C51 C -0.3084(4) 0.9753(2) 0.3044(4) 0.0361(9) 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 0.02510(18) 0.0426(2) 0.0344(2) 0.00729(10) 0.01739(14) 0.00186(9) N11 0.0358(16) 0.0354(16) 0.0368(16) 0.0026(13) 0.0225(13) 0.0039(13) N12 0.0298(15) 0.0405(17) 0.0411(17) -0.0057(14) 0.0186(14) -0.0027(13) O1 0.0266(13) 0.0604(18) 0.0447(15) 0.0084(13) 0.0231(12) 0.0038(12) O2 0.0397(16) 0.0524(17) 0.068(2) 0.0225(16) 0.0346(16) 0.0085(13) O3 0.0290(14) 0.0665(19) 0.0413(16) 0.0112(14) 0.0195(13) 0.0119(13) O4 0.0276(13) 0.073(2) 0.0479(16) 0.0083(15) 0.0254(12) 0.0038(13) O5 0.0506(17) 0.0551(17) 0.0410(15) 0.0037(13) 0.0272(14) -0.0023(14) O6 0.068(2) 0.060(2) 0.0499(19) -0.0069(16) 0.0037(17) 0.0060(18) O7 0.071(2) 0.071(2) 0.091(3) 0.010(2) 0.045(2) 0.015(2) O8 0.193(8) 0.066(3) 0.209(9) 0.013(5) 0.159(7) 0.026(4) O9 0.189(9) 0.079(5) 0.093(5) -0.007(4) 0.052(6) 0.005(5) C1 0.0355(17) 0.0339(17) 0.0309(17) -0.0032(15) 0.0205(15) 0.0012(14) C2 0.0254(16) 0.0385(18) 0.0344(18) -0.0014(15) 0.0174(15) 0.0027(14) C3 0.0209(15) 0.0381(18) 0.0304(17) -0.0030(14) 0.0135(14) -0.0033(13) C4 0.0238(17) 0.0368(18) 0.0314(18) 0.0008(14) 0.0152(15) 0.0004(13) C5 0.0226(15) 0.0423(19) 0.0258(16) -0.0037(14) 0.0125(13) -0.0008(14) C6 0.0281(17) 0.0399(19) 0.0360(18) -0.0025(15) 0.0212(15) -0.0033(14) C11 0.049(2) 0.0388(19) 0.039(2) 0.0025(16) 0.0285(18) 0.0073(17) C12 0.0329(18) 0.0385(19) 0.047(2) -0.0005(17) 0.0236(17) 0.0002(15) C13 0.0299(18) 0.048(2) 0.039(2) -0.0017(17) 0.0158(16) 0.0057(16) C14 0.0320(18) 0.044(2) 0.039(2) -0.0050(17) 0.0124(16) 0.0002(16) C31 0.0242(17) 0.047(2) 0.0341(19) -0.0031(16) 0.0170(15) -0.0042(14) C51 0.0236(17) 0.053(2) 0.0326(19) -0.0033(16) 0.0147(15) 0.0024(15) _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 N12 2.241(3) 2 ? Cd1 O1 2.291(3) . ? Cd1 O5 2.315(3) . ? Cd1 O4 2.349(3) 1_655 ? Cd1 O6 2.369(4) . ? Cd1 O3 2.543(3) 1_655 ? Cd1 O2 2.636(3) . ? N11 C12 1.339(5) . ? N11 C14 1.374(5) . ? N11 C11 1.464(5) . ? N12 C12 1.317(5) . ? N12 C13 1.376(5) . ? N12 Cd1 2.241(3) 2_545 ? O1 C31 1.272(5) . ? O2 C31 1.236(5) . ? O3 C51 1.260(5) . ? O3 Cd1 2.543(3) 1_455 ? O4 C51 1.268(5) . ? O4 Cd1 2.349(3) 1_455 ? O5 H9 0.8211 . ? O5 H10 0.8189 . ? O6 H12 0.8195 . ? O6 H11 0.8216 . ? C1 C2 1.384(5) . ? C1 C6 1.386(5) . ? C1 C11 1.516(5) . ? C2 C3 1.389(5) . ? C2 H1 0.9300 . ? C3 C4 1.397(5) . ? C3 C31 1.509(5) . ? C4 C5 1.393(5) . ? C4 H2 0.9300 . ? C5 C6 1.398(5) . ? C5 C51 1.500(5) . ? C6 H3 0.9300 . ? C11 H5 0.9700 . ? C11 H4 0.9700 . ? C12 H6 0.9300 . ? C13 C14 1.357(6) . ? C13 H7 0.9300 . ? C14 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Cd1 O1 136.98(11) 2 . ? N12 Cd1 O5 93.35(12) 2 . ? O1 Cd1 O5 90.14(11) . . ? N12 Cd1 O4 138.45(11) 2 1_655 ? O1 Cd1 O4 84.48(10) . 1_655 ? O5 Cd1 O4 88.07(11) . 1_655 ? N12 Cd1 O6 91.26(13) 2 . ? O1 Cd1 O6 87.30(13) . . ? O5 Cd1 O6 175.24(11) . . ? O4 Cd1 O6 87.69(12) 1_655 . ? N12 Cd1 O3 85.38(11) 2 1_655 ? O1 Cd1 O3 137.58(10) . 1_655 ? O5 Cd1 O3 84.10(11) . 1_655 ? O4 Cd1 O3 53.43(10) 1_655 1_655 ? O6 Cd1 O3 95.10(13) . 1_655 ? N12 Cd1 O2 85.26(10) 2 . ? O1 Cd1 O2 52.12(9) . . ? O5 Cd1 O2 101.27(11) . . ? O4 Cd1 O2 135.12(10) 1_655 . ? O6 Cd1 O2 80.29(13) . . ? O3 Cd1 O2 169.47(11) 1_655 . ? C12 N11 C14 106.8(3) . . ? C12 N11 C11 125.4(3) . . ? C14 N11 C11 127.4(3) . . ? C12 N12 C13 105.7(3) . . ? C12 N12 Cd1 125.4(3) . 2_545 ? C13 N12 Cd1 128.8(3) . 2_545 ? C31 O1 Cd1 100.9(2) . . ? C31 O2 Cd1 85.5(2) . . ? C51 O3 Cd1 88.0(2) . 1_455 ? C51 O4 Cd1 96.8(2) . 1_455 ? Cd1 O5 H9 125.2 . . ? Cd1 O5 H10 102.6 . . ? H9 O5 H10 109.8 . . ? Cd1 O6 H12 113.1 . . ? Cd1 O6 H11 113.0 . . ? H12 O6 H11 103.0 . . ? C2 C1 C6 119.8(3) . . ? C2 C1 C11 119.6(3) . . ? C6 C1 C11 120.6(3) . . ? C1 C2 C3 120.7(3) . . ? C1 C2 H1 119.6 . . ? C3 C2 H1 119.6 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 C31 119.6(3) . . ? C4 C3 C31 121.1(3) . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H2 119.8 . . ? C3 C4 H2 119.8 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 C51 120.9(3) . . ? C6 C5 C51 120.0(3) . . ? C1 C6 C5 120.5(3) . . ? C1 C6 H3 119.8 . . ? C5 C6 H3 119.8 . . ? N11 C11 C1 112.6(3) . . ? N11 C11 H5 109.1 . . ? C1 C11 H5 109.1 . . ? N11 C11 H4 109.1 . . ? C1 C11 H4 109.1 . . ? H5 C11 H4 107.8 . . ? N12 C12 N11 111.8(3) . . ? N12 C12 H6 124.1 . . ? N11 C12 H6 124.1 . . ? C14 C13 N12 109.1(3) . . ? C14 C13 H7 125.4 . . ? N12 C13 H7 125.4 . . ? C13 C14 N11 106.5(3) . . ? C13 C14 H8 126.7 . . ? N11 C14 H8 126.7 . . ? O2 C31 O1 121.3(4) . . ? O2 C31 C3 121.3(3) . . ? O1 C31 C3 117.4(3) . . ? O3 C51 O4 121.6(3) . . ? O3 C51 C5 119.7(4) . . ? O4 C51 C5 118.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Cd1 O1 C31 -11.1(3) 2 . . . ? O5 Cd1 O1 C31 -106.2(2) . . . . ? O4 Cd1 O1 C31 165.8(3) 1_655 . . . ? O6 Cd1 O1 C31 77.8(2) . . . . ? O3 Cd1 O1 C31 172.5(2) 1_655 . . . ? O2 Cd1 O1 C31 -1.9(2) . . . . ? N12 Cd1 O2 C31 175.7(3) 2 . . . ? O1 Cd1 O2 C31 2.0(2) . . . . ? O5 Cd1 O2 C31 83.2(3) . . . . ? O4 Cd1 O2 C31 -15.5(3) 1_655 . . . ? O6 Cd1 O2 C31 -92.2(3) . . . . ? O3 Cd1 O2 C31 -156.9(5) 1_655 . . . ? C6 C1 C2 C3 2.5(5) . . . . ? C11 C1 C2 C3 -176.8(3) . . . . ? C1 C2 C3 C4 -1.4(5) . . . . ? C1 C2 C3 C31 179.2(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C31 C3 C4 C5 179.2(3) . . . . ? C3 C4 C5 C6 0.7(5) . . . . ? C3 C4 C5 C51 -178.5(3) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? C11 C1 C6 C5 177.3(3) . . . . ? C4 C5 C6 C1 0.5(5) . . . . ? C51 C5 C6 C1 179.7(3) . . . . ? C12 N11 C11 C1 -80.6(5) . . . . ? C14 N11 C11 C1 90.7(5) . . . . ? C2 C1 C11 N11 -47.3(5) . . . . ? C6 C1 C11 N11 133.4(4) . . . . ? C13 N12 C12 N11 -0.4(4) . . . . ? Cd1 N12 C12 N11 -178.4(2) 2_545 . . . ? C14 N11 C12 N12 1.1(5) . . . . ? C11 N11 C12 N12 173.9(3) . . . . ? C12 N12 C13 C14 -0.4(5) . . . . ? Cd1 N12 C13 C14 177.5(3) 2_545 . . . ? N12 C13 C14 N11 1.1(5) . . . . ? C12 N11 C14 C13 -1.3(4) . . . . ? C11 N11 C14 C13 -173.9(3) . . . . ? Cd1 O2 C31 O1 -3.3(4) . . . . ? Cd1 O2 C31 C3 176.5(3) . . . . ? Cd1 O1 C31 O2 3.8(5) . . . . ? Cd1 O1 C31 C3 -175.9(3) . . . . ? C2 C3 C31 O2 -174.5(4) . . . . ? C4 C3 C31 O2 6.1(6) . . . . ? C2 C3 C31 O1 5.3(5) . . . . ? C4 C3 C31 O1 -174.1(3) . . . . ? Cd1 O3 C51 O4 -5.1(4) 1_455 . . . ? Cd1 O3 C51 C5 175.3(3) 1_455 . . . ? Cd1 O4 C51 O3 5.6(4) 1_455 . . . ? Cd1 O4 C51 C5 -174.8(3) 1_455 . . . ? C4 C5 C51 O3 1.8(6) . . . . ? C6 C5 C51 O3 -177.4(4) . . . . ? C4 C5 C51 O4 -177.8(3) . . . . ? C6 C5 C51 O4 3.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.961 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.140 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 846236' #TrackingRef '- CE-ART-01-2012-025062.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H20 Cd2 N4 O10), 2(H O0.5)' _chemical_formula_sum 'C48 H42 Cd4 N8 O21' _chemical_formula_weight 1516.50 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1431(7) _cell_length_b 10.1077(8) _cell_length_c 15.6537(18) _cell_angle_alpha 95.1900(10) _cell_angle_beta 91.9440(10) _cell_angle_gamma 116.7120(10) _cell_volume 1282.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1682 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 23.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7026 _exptl_absorpt_correction_T_max 0.7240 _exptl_absorpt_process_details 'SADABS Bruker, 2000' _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 6588 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4458 _reflns_number_gt 3128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 1.38 0.01 H20 H19 and DFIX 0.82 0.01 O10 H19 O10 H20 were used to fix the O-H distances of water molecule. simu 0.005 Cd1 O1 and delu 0.005 Cd1 O1 were used to fix the Cd1 and O1 atoms. ; _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^)]' _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 4458 _refine_ls_number_parameters 364 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.895 _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 0.09475(5) 0.16826(4) 0.42107(2) 0.027 Uani 1 1 d U . . Cd2 Cd 0.94893(5) -0.19322(4) 0.92005(3) 0.03306(13) Uani 1 1 d . . . N11 N -0.3813(6) 0.5478(5) 0.1054(3) 0.0343(12) Uani 1 1 d . . . N12 N -0.2400(6) 0.6993(5) 0.0118(3) 0.0365(13) Uani 1 1 d . . . N111 N 0.3325(5) 0.2165(4) 0.4962(3) 0.0287(11) Uani 1 1 d . . . N112 N 0.5158(5) 0.1741(5) 0.5700(3) 0.0317(12) Uani 1 1 d . . . O1 O -0.1349(5) 0.1945(4) 0.3407(2) 0.0416(10) Uani 1 1 d U . . O2 O 0.0695(5) 0.3863(4) 0.4167(2) 0.0383(10) Uani 1 1 d . . . O3 O 0.0522(4) 0.8784(4) 0.4593(2) 0.0338(10) Uani 1 1 d . . . O4 O -0.0304(4) 0.9406(4) 0.3410(2) 0.0377(10) Uani 1 1 d . . . O5 O 0.8249(5) 0.6053(4) 0.8088(2) 0.0402(11) Uani 1 1 d . . . O6 O 0.9893(4) 0.5877(4) 0.9083(2) 0.0375(10) Uani 1 1 d . . . O7 O 0.8120(5) -0.0891(4) 0.8529(2) 0.0551(13) Uani 1 1 d . . . O8 O 0.8600(5) 0.0673(4) 0.9697(2) 0.0494(12) Uani 1 1 d . . . O9 O 0.2552(4) 0.2519(4) 0.3072(2) 0.0373(10) Uani 1 1 d . . . H18 H 0.2263 0.1841 0.2590 0.045 Uiso 1 1 d R . . H17 H 0.2754 0.3356 0.2984 0.045 Uiso 1 1 d R . . O10 O 1.1514(5) -0.0687(4) 0.8265(3) 0.0696(15) Uani 1 1 d D . . H20 H 1.2294 -0.0637 0.8577 0.083 Uiso 1 1 d RD . . H19 H 1.1413 -0.1113 0.7782 0.083 Uiso 1 1 d RD . . O11 O 0.5989(10) 0.1146(10) 0.0647(6) 0.073(3) Uani 0.50 1 d P . . C1 C -0.2937(6) 0.4887(6) 0.2398(3) 0.0285(14) Uani 1 1 d . . . C2 C -0.2436(6) 0.3903(5) 0.2715(3) 0.0295(14) Uani 1 1 d . . . H1 H -0.2919 0.2915 0.2467 0.035 Uiso 1 1 calc R . . C3 C -0.1234(6) 0.4357(5) 0.3392(3) 0.0237(13) Uani 1 1 d . . . C4 C -0.0549(6) 0.5832(5) 0.3762(3) 0.0277(13) Uani 1 1 d . . . H2 H 0.0238 0.6147 0.4227 0.033 Uiso 1 1 calc R . . C5 C -0.1006(6) 0.6834(5) 0.3459(3) 0.0222(12) Uani 1 1 d . . . C6 C -0.2176(6) 0.6369(5) 0.2772(3) 0.0293(14) Uani 1 1 d . . . H3 H -0.2463 0.7054 0.2554 0.035 Uiso 1 1 calc R . . C11 C -0.4240(7) 0.4359(6) 0.1663(3) 0.0380(16) Uani 1 1 d . . . H4 H -0.4354 0.3428 0.1367 0.046 Uiso 1 1 calc R . . H5 H -0.5285 0.4178 0.1883 0.046 Uiso 1 1 calc R . . C12 C -0.2608(7) 0.5818(6) 0.0522(4) 0.0382(16) Uani 1 1 d . . . H6 H -0.1992 0.5300 0.0445 0.046 Uiso 1 1 calc R . . C13 C -0.3521(7) 0.7443(6) 0.0434(4) 0.0435(17) Uani 1 1 d . . . H7 H -0.3655 0.8250 0.0276 0.052 Uiso 1 1 calc R . . C14 C -0.4399(7) 0.6522(6) 0.1014(4) 0.0420(16) Uani 1 1 d . . . H8 H -0.5225 0.6583 0.1320 0.050 Uiso 1 1 calc R . . C31 C -0.0597(7) 0.3318(6) 0.3674(4) 0.0312(14) Uani 1 1 d . . . C51 C -0.0221(6) 0.8453(6) 0.3846(4) 0.0284(14) Uani 1 1 d . . . C101 C 0.6651(6) 0.1615(6) 0.7056(3) 0.0250(13) Uani 1 1 d . . . C102 C 0.6927(6) 0.0702(6) 0.7574(3) 0.0307(14) Uani 1 1 d . . . H9 H 0.6505 -0.0309 0.7385 0.037 Uiso 1 1 calc R . . C103 C 0.7823(6) 0.1258(6) 0.8372(3) 0.0277(13) Uani 1 1 d . . . C104 C 0.8430(6) 0.2770(5) 0.8651(3) 0.0276(13) Uani 1 1 d . . . H10 H 0.9011 0.3161 0.9188 0.033 Uiso 1 1 calc R . . C105 C 0.8172(6) 0.3684(5) 0.8134(3) 0.0238(13) Uani 1 1 d . . . C106 C 0.7276(6) 0.3105(5) 0.7344(3) 0.0267(13) Uani 1 1 d . . . H11 H 0.7094 0.3733 0.7004 0.032 Uiso 1 1 calc R . . C111 C 0.5757(7) 0.0892(6) 0.6180(3) 0.0409(16) Uani 1 1 d . . . H12 H 0.6490 0.0664 0.5832 0.049 Uiso 1 1 calc R . . H13 H 0.4827 -0.0049 0.6255 0.049 Uiso 1 1 calc R . . C112 C 0.3581(7) 0.1372(6) 0.5514(3) 0.0325(14) Uani 1 1 d . . . H14 H 0.2733 0.0618 0.5755 0.039 Uiso 1 1 calc R . . C113 C 0.4900(8) 0.3124(6) 0.4783(4) 0.0516(19) Uani 1 1 d . . . H15 H 0.5145 0.3837 0.4403 0.062 Uiso 1 1 calc R . . C114 C 0.6028(7) 0.2894(7) 0.5226(4) 0.054(2) Uani 1 1 d . . . H16 H 0.7164 0.3405 0.5216 0.065 Uiso 1 1 calc R . . C131 C 0.8204(7) 0.0283(6) 0.8913(4) 0.0326(14) Uani 1 1 d . . . C151 C 0.8825(7) 0.5312(6) 0.8457(4) 0.0309(14) 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 0.034 0.025 0.025 0.003 -0.003 0.017 Cd2 0.0518(3) 0.0229(2) 0.0234(2) 0.00068(18) -0.0054(2) 0.0170(2) N11 0.034(3) 0.033(3) 0.030(3) 0.003(2) -0.008(2) 0.011(2) N12 0.044(3) 0.024(3) 0.039(3) 0.004(2) 0.000(3) 0.013(2) N111 0.027(3) 0.029(3) 0.030(3) 0.011(2) -0.004(2) 0.012(2) N112 0.031(3) 0.035(3) 0.028(3) 0.002(2) -0.008(2) 0.014(2) O1 0.065(3) 0.021(2) 0.041(3) 0.0000(19) -0.005(2) 0.024(2) O2 0.055(3) 0.031(2) 0.040(3) 0.0036(19) -0.004(2) 0.030(2) O3 0.038(2) 0.030(2) 0.028(2) -0.0049(18) 0.0019(19) 0.0128(18) O4 0.053(3) 0.020(2) 0.043(3) 0.0012(19) -0.002(2) 0.0200(19) O5 0.071(3) 0.026(2) 0.030(2) 0.0016(18) -0.009(2) 0.029(2) O6 0.053(3) 0.027(2) 0.032(2) -0.0064(18) -0.013(2) 0.0200(19) O7 0.112(4) 0.049(3) 0.030(3) 0.001(2) -0.004(2) 0.060(3) O8 0.077(3) 0.030(2) 0.031(3) 0.0059(19) -0.019(2) 0.017(2) O9 0.059(3) 0.033(2) 0.024(2) 0.0083(18) 0.004(2) 0.0238(19) O10 0.077(3) 0.051(3) 0.051(3) -0.013(2) 0.009(3) 0.006(2) O11 0.079(7) 0.128(8) 0.055(6) -0.006(6) 0.007(5) 0.087(6) C1 0.034(3) 0.023(3) 0.024(3) 0.008(3) 0.000(3) 0.009(3) C2 0.043(4) 0.015(3) 0.027(3) 0.002(2) 0.003(3) 0.010(3) C3 0.035(3) 0.020(3) 0.018(3) 0.005(2) 0.003(3) 0.014(3) C4 0.033(3) 0.029(3) 0.020(3) 0.000(3) -0.002(3) 0.014(3) C5 0.029(3) 0.022(3) 0.017(3) 0.001(2) 0.001(2) 0.013(2) C6 0.042(4) 0.024(3) 0.030(3) 0.009(3) 0.004(3) 0.021(3) C11 0.044(4) 0.029(3) 0.036(4) 0.011(3) -0.005(3) 0.011(3) C12 0.041(4) 0.034(4) 0.041(4) 0.004(3) -0.001(3) 0.019(3) C13 0.050(4) 0.039(4) 0.043(4) 0.012(3) -0.001(3) 0.020(3) C14 0.044(4) 0.051(4) 0.039(4) 0.000(3) 0.000(3) 0.030(3) C31 0.040(4) 0.033(4) 0.027(3) 0.005(3) 0.003(3) 0.022(3) C51 0.034(4) 0.027(3) 0.030(4) 0.003(3) 0.014(3) 0.019(3) C101 0.030(3) 0.028(3) 0.020(3) 0.000(2) -0.002(3) 0.016(3) C102 0.040(4) 0.027(3) 0.027(3) -0.003(3) -0.002(3) 0.019(3) C103 0.039(4) 0.026(3) 0.022(3) 0.004(3) -0.001(3) 0.018(3) C104 0.039(4) 0.021(3) 0.022(3) 0.000(2) -0.004(3) 0.014(3) C105 0.033(3) 0.019(3) 0.020(3) 0.001(2) 0.001(3) 0.013(2) C106 0.040(4) 0.030(3) 0.021(3) 0.006(3) 0.001(3) 0.025(3) C111 0.055(4) 0.044(4) 0.033(4) -0.007(3) -0.020(3) 0.035(3) C112 0.032(4) 0.031(3) 0.030(4) 0.002(3) 0.000(3) 0.011(3) C113 0.053(5) 0.044(4) 0.045(4) 0.016(3) -0.014(4) 0.010(3) C114 0.030(4) 0.070(5) 0.046(4) 0.025(4) -0.004(3) 0.004(3) C131 0.042(4) 0.026(3) 0.032(4) 0.007(3) -0.002(3) 0.017(3) C151 0.043(4) 0.027(3) 0.024(3) 0.005(3) 0.006(3) 0.017(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 Cd1 N111 2.262(4) . ? Cd1 O4 2.278(3) 1_545 ? Cd1 O3 2.301(3) 2_566 ? Cd1 O9 2.319(3) . ? Cd1 O2 2.323(3) . ? Cd1 O1 2.538(4) . ? Cd2 N12 2.234(4) 1_646 ? Cd2 O8 2.247(4) 2_757 ? Cd2 O7 2.254(4) . ? Cd2 O10 2.361(4) . ? Cd2 O5 2.370(3) 1_545 ? Cd2 O6 2.396(4) 1_545 ? Cd2 C151 2.707(5) 1_545 ? N11 C12 1.341(6) . ? N11 C14 1.387(7) . ? N11 C11 1.471(6) . ? N12 C12 1.337(6) . ? N12 C13 1.384(7) . ? N12 Cd2 2.234(4) 1_464 ? N111 C112 1.313(6) . ? N111 C113 1.384(6) . ? N112 C112 1.331(6) . ? N112 C114 1.380(6) . ? N112 C111 1.454(6) . ? O1 C31 1.261(6) . ? O2 C31 1.252(6) . ? O3 C51 1.270(6) . ? O3 Cd1 2.301(3) 2_566 ? O4 C51 1.258(6) . ? O4 Cd1 2.278(3) 1_565 ? O5 C151 1.259(6) . ? O5 Cd2 2.370(3) 1_565 ? O6 C151 1.254(6) . ? O6 Cd2 2.396(4) 1_565 ? O7 C131 1.250(6) . ? O8 C131 1.243(6) . ? O8 Cd2 2.247(4) 2_757 ? O9 H18 0.9168 . ? O9 H17 0.8076 . ? O10 H20 0.8296 . ? O10 H19 0.8174 . ? C1 C2 1.388(7) . ? C1 C6 1.395(6) . ? C1 C11 1.501(7) . ? C2 C3 1.386(7) . ? C2 H1 0.9300 . ? C3 C4 1.389(6) . ? C3 C31 1.502(7) . ? C4 C5 1.371(7) . ? C4 H2 0.9300 . ? C5 C6 1.378(7) . ? C5 C51 1.515(6) . ? C6 H3 0.9300 . ? C11 H4 0.9700 . ? C11 H5 0.9700 . ? C12 H6 0.9300 . ? C13 C14 1.366(7) . ? C13 H7 0.9300 . ? C14 H8 0.9300 . ? C101 C106 1.373(6) . ? C101 C102 1.379(7) . ? C101 C111 1.513(6) . ? C102 C103 1.392(7) . ? C102 H9 0.9300 . ? C103 C104 1.391(6) . ? C103 C131 1.499(7) . ? C104 C105 1.372(7) . ? C104 H10 0.9300 . ? C105 C106 1.383(6) . ? C105 C151 1.505(7) . ? C106 H11 0.9300 . ? C111 H12 0.9700 . ? C111 H13 0.9700 . ? C112 H14 0.9300 . ? C113 C114 1.340(8) . ? C113 H15 0.9300 . ? C114 H16 0.9300 . ? C151 Cd2 2.707(5) 1_565 ? 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 N111 Cd1 O4 114.63(14) . 1_545 ? N111 Cd1 O3 93.41(14) . 2_566 ? O4 Cd1 O3 101.06(12) 1_545 2_566 ? N111 Cd1 O9 85.42(14) . . ? O4 Cd1 O9 86.96(12) 1_545 . ? O3 Cd1 O9 171.59(12) 2_566 . ? N111 Cd1 O2 110.36(14) . . ? O4 Cd1 O2 132.88(14) 1_545 . ? O3 Cd1 O2 89.35(13) 2_566 . ? O9 Cd1 O2 83.28(13) . . ? N111 Cd1 O1 163.65(13) . . ? O4 Cd1 O1 80.40(13) 1_545 . ? O3 Cd1 O1 89.67(13) 2_566 . ? O9 Cd1 O1 89.20(12) . . ? O2 Cd1 O1 53.57(12) . . ? N12 Cd2 O8 90.70(15) 1_646 2_757 ? N12 Cd2 O7 96.00(17) 1_646 . ? O8 Cd2 O7 121.97(14) 2_757 . ? N12 Cd2 O10 177.34(15) 1_646 . ? O8 Cd2 O10 87.70(14) 2_757 . ? O7 Cd2 O10 83.07(16) . . ? N12 Cd2 O5 94.52(14) 1_646 1_545 ? O8 Cd2 O5 150.67(15) 2_757 1_545 ? O7 Cd2 O5 86.18(14) . 1_545 ? O10 Cd2 O5 87.91(12) . 1_545 ? N12 Cd2 O6 87.79(15) 1_646 1_545 ? O8 Cd2 O6 96.47(13) 2_757 1_545 ? O7 Cd2 O6 141.22(13) . 1_545 ? O10 Cd2 O6 94.49(14) . 1_545 ? O5 Cd2 O6 55.03(12) 1_545 1_545 ? N12 Cd2 C151 88.53(16) 1_646 1_545 ? O8 Cd2 C151 124.06(17) 2_757 1_545 ? O7 Cd2 C151 113.71(17) . 1_545 ? O10 Cd2 C151 94.13(14) . 1_545 ? O5 Cd2 C151 27.70(14) 1_545 1_545 ? O6 Cd2 C151 27.59(14) 1_545 1_545 ? C12 N11 C14 107.1(5) . . ? C12 N11 C11 125.8(5) . . ? C14 N11 C11 126.5(5) . . ? C12 N12 C13 105.3(5) . . ? C12 N12 Cd2 126.5(4) . 1_464 ? C13 N12 Cd2 128.1(4) . 1_464 ? C112 N111 C113 102.8(5) . . ? C112 N111 Cd1 128.3(4) . . ? C113 N111 Cd1 127.0(4) . . ? C112 N112 C114 105.8(5) . . ? C112 N112 C111 124.9(5) . . ? C114 N112 C111 128.4(5) . . ? C31 O1 Cd1 87.0(3) . . ? C31 O2 Cd1 97.2(3) . . ? C51 O3 Cd1 120.2(3) . 2_566 ? C51 O4 Cd1 108.7(4) . 1_565 ? C151 O5 Cd2 91.2(3) . 1_565 ? C151 O6 Cd2 90.2(3) . 1_565 ? C131 O7 Cd2 116.0(4) . . ? C131 O8 Cd2 150.8(4) . 2_757 ? Cd1 O9 H18 115.1 . . ? Cd1 O9 H17 114.3 . . ? H18 O9 H17 115.0 . . ? Cd2 O10 H20 95.3 . . ? Cd2 O10 H19 117.0 . . ? H20 O10 H19 113.8 . . ? C2 C1 C6 118.1(5) . . ? C2 C1 C11 120.3(5) . . ? C6 C1 C11 121.6(5) . . ? C3 C2 C1 121.6(5) . . ? C3 C2 H1 119.2 . . ? C1 C2 H1 119.2 . . ? C2 C3 C4 118.2(5) . . ? C2 C3 C31 121.0(5) . . ? C4 C3 C31 120.7(5) . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H2 119.2 . . ? C3 C4 H2 119.2 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 C51 121.5(5) . . ? C6 C5 C51 119.1(5) . . ? C5 C6 C1 121.1(5) . . ? C5 C6 H3 119.4 . . ? C1 C6 H3 119.4 . . ? N11 C11 C1 110.6(4) . . ? N11 C11 H4 109.5 . . ? C1 C11 H4 109.5 . . ? N11 C11 H5 109.5 . . ? C1 C11 H5 109.5 . . ? H4 C11 H5 108.1 . . ? N12 C12 N11 111.8(5) . . ? N12 C12 H6 124.1 . . ? N11 C12 H6 124.1 . . ? C14 C13 N12 109.6(6) . . ? C14 C13 H7 125.2 . . ? N12 C13 H7 125.2 . . ? C13 C14 N11 106.2(5) . . ? C13 C14 H8 126.9 . . ? N11 C14 H8 126.9 . . ? O2 C31 O1 122.1(5) . . ? O2 C31 C3 118.0(5) . . ? O1 C31 C3 119.9(5) . . ? O4 C51 O3 123.2(5) . . ? O4 C51 C5 118.9(5) . . ? O3 C51 C5 117.9(5) . . ? C106 C101 C102 118.6(5) . . ? C106 C101 C111 125.0(5) . . ? C102 C101 C111 116.4(5) . . ? C101 C102 C103 121.7(5) . . ? C101 C102 H9 119.2 . . ? C103 C102 H9 119.2 . . ? C104 C103 C102 118.5(5) . . ? C104 C103 C131 119.7(5) . . ? C102 C103 C131 121.7(5) . . ? C105 C104 C103 120.0(5) . . ? C105 C104 H10 120.0 . . ? C103 C104 H10 120.0 . . ? C104 C105 C106 120.4(5) . . ? C104 C105 C151 118.8(5) . . ? C106 C105 C151 120.7(5) . . ? C101 C106 C105 120.8(5) . . ? C101 C106 H11 119.6 . . ? C105 C106 H11 119.6 . . ? N112 C111 C101 117.0(5) . . ? N112 C111 H12 108.1 . . ? C101 C111 H12 108.1 . . ? N112 C111 H13 108.1 . . ? C101 C111 H13 108.1 . . ? H12 C111 H13 107.3 . . ? N111 C112 N112 114.2(5) . . ? N111 C112 H14 122.9 . . ? N112 C112 H14 122.9 . . ? C114 C113 N111 111.4(6) . . ? C114 C113 H15 124.3 . . ? N111 C113 H15 124.3 . . ? C113 C114 N112 105.8(5) . . ? C113 C114 H16 127.1 . . ? N112 C114 H16 127.1 . . ? O8 C131 O7 123.8(5) . . ? O8 C131 C103 119.9(5) . . ? O7 C131 C103 116.3(5) . . ? O6 C151 O5 122.4(5) . . ? O6 C151 C105 119.7(5) . . ? O5 C151 C105 117.9(5) . . ? O6 C151 Cd2 62.2(3) . 1_565 ? O5 C151 Cd2 61.1(3) . 1_565 ? C105 C151 Cd2 169.3(4) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cd1 N111 C112 -54.9(5) 1_545 . . . ? O3 Cd1 N111 C112 48.9(5) 2_566 . . . ? O9 Cd1 N111 C112 -139.5(5) . . . . ? O2 Cd1 N111 C112 139.5(4) . . . . ? O1 Cd1 N111 C112 149.4(4) . . . . ? O4 Cd1 N111 C113 106.4(5) 1_545 . . . ? O3 Cd1 N111 C113 -149.8(5) 2_566 . . . ? O9 Cd1 N111 C113 21.8(5) . . . . ? O2 Cd1 N111 C113 -59.2(5) . . . . ? O1 Cd1 N111 C113 -49.3(8) . . . . ? N111 Cd1 O1 C31 -10.0(6) . . . . ? O4 Cd1 O1 C31 -167.7(3) 1_545 . . . ? O3 Cd1 O1 C31 91.0(3) 2_566 . . . ? O9 Cd1 O1 C31 -80.6(3) . . . . ? O2 Cd1 O1 C31 1.6(3) . . . . ? N111 Cd1 O2 C31 174.9(3) . . . . ? O4 Cd1 O2 C31 12.9(4) 1_545 . . . ? O3 Cd1 O2 C31 -91.7(3) 2_566 . . . ? O9 Cd1 O2 C31 92.4(3) . . . . ? O1 Cd1 O2 C31 -1.6(3) . . . . ? N12 Cd2 O7 C131 79.2(4) 1_646 . . . ? O8 Cd2 O7 C131 -15.4(5) 2_757 . . . ? O10 Cd2 O7 C131 -98.3(4) . . . . ? O5 Cd2 O7 C131 173.4(4) 1_545 . . . ? O6 Cd2 O7 C131 173.2(3) 1_545 . . . ? C151 Cd2 O7 C131 170.3(4) 1_545 . . . ? C6 C1 C2 C3 1.0(8) . . . . ? C11 C1 C2 C3 179.9(5) . . . . ? C1 C2 C3 C4 1.1(8) . . . . ? C1 C2 C3 C31 -174.4(5) . . . . ? C2 C3 C4 C5 -1.7(7) . . . . ? C31 C3 C4 C5 173.8(5) . . . . ? C3 C4 C5 C6 0.2(8) . . . . ? C3 C4 C5 C51 -178.1(4) . . . . ? C4 C5 C6 C1 1.9(8) . . . . ? C51 C5 C6 C1 -179.7(4) . . . . ? C2 C1 C6 C5 -2.5(8) . . . . ? C11 C1 C6 C5 178.6(5) . . . . ? C12 N11 C11 C1 70.9(7) . . . . ? C14 N11 C11 C1 -98.6(6) . . . . ? C2 C1 C11 N11 -138.9(5) . . . . ? C6 C1 C11 N11 40.0(7) . . . . ? C13 N12 C12 N11 1.7(6) . . . . ? Cd2 N12 C12 N11 177.7(3) 1_464 . . . ? C14 N11 C12 N12 -1.8(6) . . . . ? C11 N11 C12 N12 -173.0(5) . . . . ? C12 N12 C13 C14 -0.9(6) . . . . ? Cd2 N12 C13 C14 -176.8(4) 1_464 . . . ? N12 C13 C14 N11 -0.2(7) . . . . ? C12 N11 C14 C13 1.2(6) . . . . ? C11 N11 C14 C13 172.3(5) . . . . ? Cd1 O2 C31 O1 3.1(6) . . . . ? Cd1 O2 C31 C3 -176.1(4) . . . . ? Cd1 O1 C31 O2 -2.8(5) . . . . ? Cd1 O1 C31 C3 176.3(5) . . . . ? C2 C3 C31 O2 166.2(5) . . . . ? C4 C3 C31 O2 -9.1(8) . . . . ? C2 C3 C31 O1 -13.0(8) . . . . ? C4 C3 C31 O1 171.7(5) . . . . ? Cd1 O4 C51 O3 -2.9(6) 1_565 . . . ? Cd1 O4 C51 C5 178.6(3) 1_565 . . . ? Cd1 O3 C51 O4 103.5(5) 2_566 . . . ? Cd1 O3 C51 C5 -78.1(5) 2_566 . . . ? C4 C5 C51 O4 159.5(5) . . . . ? C6 C5 C51 O4 -18.9(7) . . . . ? C4 C5 C51 O3 -19.1(7) . . . . ? C6 C5 C51 O3 162.6(5) . . . . ? C106 C101 C102 C103 -0.3(8) . . . . ? C111 C101 C102 C103 176.1(5) . . . . ? C101 C102 C103 C104 0.8(8) . . . . ? C101 C102 C103 C131 -176.5(5) . . . . ? C102 C103 C104 C105 -1.4(8) . . . . ? C131 C103 C104 C105 176.0(5) . . . . ? C103 C104 C105 C106 1.5(8) . . . . ? C103 C104 C105 C151 179.3(5) . . . . ? C102 C101 C106 C105 0.4(8) . . . . ? C111 C101 C106 C105 -175.7(5) . . . . ? C104 C105 C106 C101 -1.0(8) . . . . ? C151 C105 C106 C101 -178.7(4) . . . . ? C112 N112 C111 C101 -113.0(6) . . . . ? C114 N112 C111 C101 79.3(7) . . . . ? C106 C101 C111 N112 -16.2(8) . . . . ? C102 C101 C111 N112 167.7(5) . . . . ? C113 N111 C112 N112 0.1(6) . . . . ? Cd1 N111 C112 N112 164.9(3) . . . . ? C114 N112 C112 N111 0.2(6) . . . . ? C111 N112 C112 N111 -169.7(5) . . . . ? C112 N111 C113 C114 -0.5(7) . . . . ? Cd1 N111 C113 C114 -165.5(4) . . . . ? N111 C113 C114 N112 0.7(7) . . . . ? C112 N112 C114 C113 -0.5(7) . . . . ? C111 N112 C114 C113 169.0(5) . . . . ? Cd2 O8 C131 O7 92.5(9) 2_757 . . . ? Cd2 O8 C131 C103 -86.4(10) 2_757 . . . ? Cd2 O7 C131 O8 -19.3(8) . . . . ? Cd2 O7 C131 C103 159.6(4) . . . . ? C104 C103 C131 O8 22.0(8) . . . . ? C102 C103 C131 O8 -160.7(5) . . . . ? C104 C103 C131 O7 -157.0(5) . . . . ? C102 C103 C131 O7 20.3(8) . . . . ? Cd2 O6 C151 O5 11.1(6) 1_565 . . . ? Cd2 O6 C151 C105 -168.0(4) 1_565 . . . ? Cd2 O5 C151 O6 -11.2(6) 1_565 . . . ? Cd2 O5 C151 C105 167.9(4) 1_565 . . . ? C104 C105 C151 O6 16.4(7) . . . . ? C106 C105 C151 O6 -165.9(5) . . . . ? C104 C105 C151 O5 -162.7(5) . . . . ? C106 C105 C151 O5 15.0(8) . . . . ? C104 C105 C151 Cd2 -81(2) . . . 1_565 ? C106 C105 C151 Cd2 97(2) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.614 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.100 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 846237' #TrackingRef '- CE-ART-01-2012-025062.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 N2 O4 Zn' _chemical_formula_sum 'C12 H8 N2 O4 Zn' _chemical_formula_weight 309.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.3889(4) _cell_length_b 11.0946(7) _cell_length_c 16.6876(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.6880(10) _cell_angle_gamma 90.00 _cell_volume 1177.03(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2707 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 2.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6791 _exptl_absorpt_correction_T_max 0.7039 _exptl_absorpt_process_details 'SADABS Bruker, 2000' _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 7209 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2808 _reflns_number_gt 2168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^] 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 2808 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.65410(4) 0.14948(2) -0.003891(14) 0.03160(9) Uani 1 1 d . . . N11 N 0.0837(3) 0.62254(16) 0.16043(11) 0.0323(4) Uani 1 1 d . . . N12 N 0.1645(3) 0.74474(15) 0.06476(10) 0.0316(4) Uani 1 1 d . . . O1 O 0.4864(2) 0.23725(15) 0.07105(9) 0.0446(4) Uani 1 1 d . . . O2 O 0.8133(3) 0.25034(17) 0.12582(10) 0.0575(5) Uani 1 1 d . . . O3 O 0.7191(2) 0.50081(13) 0.45962(9) 0.0373(4) Uani 1 1 d . . . O4 O 0.9517(2) 0.38884(15) 0.40129(9) 0.0395(4) Uani 1 1 d . . . C1 C 0.3071(3) 0.48411(18) 0.24702(13) 0.0292(5) Uani 1 1 d . . . C2 C 0.3616(3) 0.40948(19) 0.18556(12) 0.0316(5) Uani 1 1 d . . . H1 H 0.2706 0.4012 0.1388 0.038 Uiso 1 1 calc R . . C3 C 0.5514(3) 0.34713(18) 0.19338(12) 0.0288(5) Uani 1 1 d . . . C4 C 0.6813(3) 0.35707(18) 0.26449(12) 0.0279(4) Uani 1 1 d . . . H2 H 0.8073 0.3145 0.2705 0.034 Uiso 1 1 calc R . . C5 C 0.6274(3) 0.42904(18) 0.32666(12) 0.0271(5) Uani 1 1 d . . . C6 C 0.4388(3) 0.49348(18) 0.31745(13) 0.0305(5) Uani 1 1 d . . . H3 H 0.4019 0.5428 0.3589 0.037 Uiso 1 1 calc R . . C11 C 0.1042(3) 0.5554(2) 0.23651(14) 0.0399(6) Uani 1 1 d . . . H5 H -0.0140 0.5007 0.2376 0.048 Uiso 1 1 calc R . . H4 H 0.1006 0.6114 0.2810 0.048 Uiso 1 1 calc R . . C12 C 0.2229(3) 0.7014(2) 0.13682(13) 0.0332(5) Uani 1 1 d . . . H6 H 0.3464 0.7231 0.1677 0.040 Uiso 1 1 calc R . . C13 C -0.0255(4) 0.6920(2) 0.04158(15) 0.0454(6) Uani 1 1 d . . . H7 H -0.1072 0.7063 -0.0068 0.054 Uiso 1 1 calc R . . C14 C -0.0759(4) 0.6161(2) 0.09991(15) 0.0463(6) Uani 1 1 d . . . H8 H -0.1960 0.5686 0.0990 0.056 Uiso 1 1 calc R . . C31 C 0.6249(4) 0.2731(2) 0.12599(13) 0.0345(5) Uani 1 1 d . . . C51 C 0.7763(3) 0.44067(19) 0.40195(12) 0.0300(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03827(17) 0.03293(15) 0.02344(14) 0.00217(11) 0.00227(10) 0.00276(12) N11 0.0268(10) 0.0333(10) 0.0366(11) 0.0059(8) 0.0029(8) 0.0034(8) N12 0.0342(11) 0.0320(10) 0.0277(10) 0.0018(8) -0.0008(8) 0.0001(8) O1 0.0432(10) 0.0587(11) 0.0313(9) -0.0166(8) 0.0002(7) 0.0007(8) O2 0.0464(11) 0.0848(15) 0.0410(11) -0.0194(9) 0.0021(9) 0.0198(10) O3 0.0423(10) 0.0412(9) 0.0291(9) -0.0104(7) 0.0064(7) -0.0084(8) O4 0.0360(9) 0.0554(10) 0.0260(8) -0.0053(7) -0.0031(7) 0.0048(8) C1 0.0275(12) 0.0292(11) 0.0315(12) 0.0073(9) 0.0064(9) 0.0017(9) C2 0.0323(13) 0.0351(12) 0.0262(11) 0.0024(9) -0.0022(9) -0.0010(10) C3 0.0327(12) 0.0290(11) 0.0245(10) -0.0004(9) 0.0013(9) -0.0017(10) C4 0.0278(11) 0.0277(11) 0.0280(11) 0.0006(9) 0.0016(8) 0.0006(9) C5 0.0302(12) 0.0277(11) 0.0236(10) 0.0006(8) 0.0029(8) -0.0048(9) C6 0.0373(13) 0.0276(11) 0.0281(12) -0.0010(9) 0.0095(9) -0.0025(10) C11 0.0379(13) 0.0422(14) 0.0418(14) 0.0142(11) 0.0146(11) 0.0079(11) C12 0.0297(12) 0.0347(12) 0.0346(13) 0.0056(10) -0.0004(10) -0.0007(10) C13 0.0415(15) 0.0532(15) 0.0391(14) 0.0011(12) -0.0081(11) -0.0037(12) C14 0.0360(14) 0.0521(16) 0.0491(16) -0.0002(12) -0.0046(12) -0.0130(12) C31 0.0430(14) 0.0351(13) 0.0250(11) -0.0001(9) 0.0013(10) 0.0024(11) C51 0.0362(13) 0.0299(12) 0.0241(11) 0.0008(9) 0.0036(9) -0.0102(10) _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 1.9504(14) 2_645 ? Zn1 O1 1.9815(16) . ? Zn1 O4 1.9878(14) 4_565 ? Zn1 N12 1.9965(18) 3_665 ? N11 C12 1.335(3) . ? N11 C14 1.364(3) . ? N11 C11 1.467(3) . ? N12 C12 1.314(3) . ? N12 C13 1.368(3) . ? N12 Zn1 1.9965(18) 3_665 ? O1 C31 1.273(2) . ? O2 C31 1.231(3) . ? O3 C51 1.255(2) . ? O3 Zn1 1.9504(14) 2_655 ? O4 C51 1.260(3) . ? O4 Zn1 1.9878(14) 4_666 ? C1 C6 1.380(3) . ? C1 C2 1.389(3) . ? C1 C11 1.514(3) . ? C2 C3 1.391(3) . ? C2 H1 0.9300 . ? C3 C4 1.383(3) . ? C3 C31 1.505(3) . ? C4 C5 1.380(3) . ? C4 H2 0.9300 . ? C5 C6 1.396(3) . ? C5 C51 1.504(3) . ? C6 H3 0.9300 . ? C11 H5 0.9700 . ? C11 H4 0.9700 . ? C12 H6 0.9300 . ? C13 C14 1.350(3) . ? C13 H7 0.9300 . ? C14 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 114.01(7) 2_645 . ? O3 Zn1 O4 109.49(6) 2_645 4_565 ? O1 Zn1 O4 104.93(6) . 4_565 ? O3 Zn1 N12 116.71(7) 2_645 3_665 ? O1 Zn1 N12 114.19(7) . 3_665 ? O4 Zn1 N12 94.90(7) 4_565 3_665 ? C12 N11 C14 106.69(19) . . ? C12 N11 C11 125.70(18) . . ? C14 N11 C11 127.6(2) . . ? C12 N12 C13 105.43(19) . . ? C12 N12 Zn1 123.62(15) . 3_665 ? C13 N12 Zn1 130.62(15) . 3_665 ? C31 O1 Zn1 103.14(14) . . ? C51 O3 Zn1 126.77(14) . 2_655 ? C51 O4 Zn1 126.83(14) . 4_666 ? C6 C1 C2 119.82(19) . . ? C6 C1 C11 120.2(2) . . ? C2 C1 C11 120.03(19) . . ? C1 C2 C3 120.49(19) . . ? C1 C2 H1 119.8 . . ? C3 C2 H1 119.8 . . ? C4 C3 C2 118.96(19) . . ? C4 C3 C31 118.66(19) . . ? C2 C3 C31 122.34(18) . . ? C5 C4 C3 121.20(19) . . ? C5 C4 H2 119.4 . . ? C3 C4 H2 119.4 . . ? C4 C5 C6 119.37(18) . . ? C4 C5 C51 119.57(19) . . ? C6 C5 C51 121.01(19) . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H3 119.9 . . ? C5 C6 H3 119.9 . . ? N11 C11 C1 111.57(18) . . ? N11 C11 H5 109.3 . . ? C1 C11 H5 109.3 . . ? N11 C11 H4 109.3 . . ? C1 C11 H4 109.3 . . ? H5 C11 H4 108.0 . . ? N12 C12 N11 111.86(19) . . ? N12 C12 H6 124.1 . . ? N11 C12 H6 124.1 . . ? C14 C13 N12 109.3(2) . . ? C14 C13 H7 125.3 . . ? N12 C13 H7 125.3 . . ? C13 C14 N11 106.7(2) . . ? C13 C14 H8 126.7 . . ? N11 C14 H8 126.7 . . ? O2 C31 O1 123.0(2) . . ? O2 C31 C3 119.45(19) . . ? O1 C31 C3 117.6(2) . . ? O3 C51 O4 125.17(19) . . ? O3 C51 C5 118.6(2) . . ? O4 C51 C5 116.27(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C31 67.96(15) 2_645 . . . ? O4 Zn1 O1 C31 -172.25(14) 4_565 . . . ? N12 Zn1 O1 C31 -69.73(15) 3_665 . . . ? C6 C1 C2 C3 -2.1(3) . . . . ? C11 C1 C2 C3 177.56(19) . . . . ? C1 C2 C3 C4 2.4(3) . . . . ? C1 C2 C3 C31 -175.1(2) . . . . ? C2 C3 C4 C5 -1.2(3) . . . . ? C31 C3 C4 C5 176.39(19) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C3 C4 C5 C51 -177.98(19) . . . . ? C2 C1 C6 C5 0.6(3) . . . . ? C11 C1 C6 C5 -179.08(19) . . . . ? C4 C5 C6 C1 0.6(3) . . . . ? C51 C5 C6 C1 178.23(18) . . . . ? C12 N11 C11 C1 -55.7(3) . . . . ? C14 N11 C11 C1 123.1(2) . . . . ? C6 C1 C11 N11 129.3(2) . . . . ? C2 C1 C11 N11 -50.4(3) . . . . ? C13 N12 C12 N11 1.2(3) . . . . ? Zn1 N12 C12 N11 -172.85(14) 3_665 . . . ? C14 N11 C12 N12 -0.8(3) . . . . ? C11 N11 C12 N12 178.18(19) . . . . ? C12 N12 C13 C14 -1.1(3) . . . . ? Zn1 N12 C13 C14 172.36(17) 3_665 . . . ? N12 C13 C14 N11 0.6(3) . . . . ? C12 N11 C14 C13 0.1(3) . . . . ? C11 N11 C14 C13 -178.9(2) . . . . ? Zn1 O1 C31 O2 -1.1(3) . . . . ? Zn1 O1 C31 C3 178.59(15) . . . . ? C4 C3 C31 O2 -19.3(3) . . . . ? C2 C3 C31 O2 158.2(2) . . . . ? C4 C3 C31 O1 161.0(2) . . . . ? C2 C3 C31 O1 -21.5(3) . . . . ? Zn1 O3 C51 O4 63.5(3) 2_655 . . . ? Zn1 O3 C51 C5 -115.89(18) 2_655 . . . ? Zn1 O4 C51 O3 16.9(3) 4_666 . . . ? Zn1 O4 C51 C5 -163.67(13) 4_666 . . . ? C4 C5 C51 O3 -175.86(19) . . . . ? C6 C5 C51 O3 6.5(3) . . . . ? C4 C5 C51 O4 4.7(3) . . . . ? C6 C5 C51 O4 -172.94(19) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.538 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.060 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 846238' #TrackingRef '- CE-ART-01-2012-025062.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 N2 O5 Zn' _chemical_formula_sum 'C12 H10 N2 O5 Zn' _chemical_formula_weight 327.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1525(10) _cell_length_b 13.5590(14) _cell_length_c 17.9533(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2471.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6384 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6232 _exptl_absorpt_correction_T_max 0.6894 _exptl_absorpt_process_details 'SADABS Bruker, 2000' _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 13830 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2942 _reflns_number_gt 2404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^] 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 2942 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.22913(3) 0.177804(17) 0.173635(12) 0.02920(11) Uani 1 1 d . . . N11 N 0.19329(19) 0.31013(13) 0.37730(10) 0.0332(4) Uani 1 1 d . . . N12 N 0.23365(17) 0.22372(13) 0.27742(10) 0.0334(4) Uani 1 1 d . . . O1 O 0.53983(15) 0.54952(12) 0.29733(8) 0.0417(4) Uani 1 1 d . . . O2 O 0.61948(16) 0.64628(12) 0.38540(8) 0.0420(4) Uani 1 1 d . . . O3 O 0.35323(14) 0.73171(10) 0.60216(8) 0.0353(3) Uani 1 1 d . . . O4 O 0.20322(17) 0.62596(11) 0.64237(9) 0.0421(4) Uani 1 1 d . . . O5 O 0.11928(16) 0.05509(10) 0.17971(7) 0.0365(4) Uani 1 1 d . . . H9 H 0.0794 0.0452 0.2189 0.044 Uiso 1 1 d R . . H10 H 0.1459 -0.0019 0.1693 0.044 Uiso 1 1 d R . . C1 C 0.23290(19) 0.46602(15) 0.44306(12) 0.0304(4) Uani 1 1 d . . . C2 C 0.3344(2) 0.48920(15) 0.39436(10) 0.0305(4) Uani 1 1 d . . . H1 H 0.3427 0.4551 0.3496 0.037 Uiso 1 1 calc R . . C3 C 0.42369(19) 0.56315(13) 0.41225(10) 0.0271(4) Uani 1 1 d . . . C4 C 0.4094(2) 0.61456(13) 0.47816(10) 0.0285(4) Uani 1 1 d . . . H2 H 0.4696 0.6638 0.4902 0.034 Uiso 1 1 calc R . . C5 C 0.3067(2) 0.59387(14) 0.52659(10) 0.0275(4) Uani 1 1 d . . . C6 C 0.21947(19) 0.51857(15) 0.50850(11) 0.0297(4) Uani 1 1 d . . . H3 H 0.1510 0.5034 0.5409 0.036 Uiso 1 1 calc R . . C11 C 0.1368(2) 0.38381(16) 0.42673(13) 0.0425(5) Uani 1 1 d . . . H4 H 0.1111 0.3526 0.4731 0.051 Uiso 1 1 calc R . . H5 H 0.0583 0.4112 0.4039 0.051 Uiso 1 1 calc R . . C12 C 0.1563(2) 0.28988(15) 0.30789(12) 0.0360(5) Uani 1 1 d . . . H6 H 0.0848 0.3189 0.2840 0.043 Uiso 1 1 calc R . . C13 C 0.3261(2) 0.20068(17) 0.33090(11) 0.0373(5) Uani 1 1 d . . . H7 H 0.3940 0.1553 0.3254 0.045 Uiso 1 1 calc R . . C14 C 0.3021(2) 0.25452(17) 0.39229(12) 0.0384(5) Uani 1 1 d . . . H8 H 0.3503 0.2540 0.4364 0.046 Uiso 1 1 calc R . . C31 C 0.53455(19) 0.58672(14) 0.35993(11) 0.0306(4) Uani 1 1 d . . . C51 C 0.2863(2) 0.65289(15) 0.59651(12) 0.0294(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03679(18) 0.02718(16) 0.02363(15) 0.00048(8) 0.00313(9) 0.00304(9) N11 0.0358(10) 0.0318(9) 0.0320(9) -0.0070(7) 0.0043(7) -0.0078(7) N12 0.0437(11) 0.0283(9) 0.0283(8) -0.0016(7) 0.0019(7) 0.0023(7) O1 0.0355(9) 0.0606(10) 0.0289(7) -0.0011(7) 0.0035(6) -0.0032(7) O2 0.0394(9) 0.0442(9) 0.0424(9) -0.0038(7) 0.0096(7) -0.0138(7) O3 0.0366(8) 0.0278(7) 0.0416(8) -0.0119(6) 0.0017(6) -0.0018(6) O4 0.0614(11) 0.0301(8) 0.0349(8) -0.0070(7) 0.0131(8) -0.0048(7) O5 0.0495(10) 0.0265(7) 0.0334(7) -0.0001(6) 0.0126(6) 0.0000(6) C1 0.0332(11) 0.0274(10) 0.0307(10) -0.0047(9) 0.0021(8) -0.0035(8) C2 0.0340(11) 0.0298(10) 0.0276(9) -0.0050(8) 0.0035(8) -0.0013(8) C3 0.0296(10) 0.0241(9) 0.0276(9) 0.0037(7) 0.0010(8) -0.0002(7) C4 0.0314(10) 0.0218(9) 0.0323(9) 0.0010(7) -0.0037(8) -0.0001(7) C5 0.0346(10) 0.0217(9) 0.0262(9) -0.0013(7) -0.0015(8) 0.0026(7) C6 0.0330(11) 0.0259(10) 0.0300(10) -0.0012(8) 0.0050(8) 0.0002(7) C11 0.0394(13) 0.0419(12) 0.0463(12) -0.0174(10) 0.0129(10) -0.0123(10) C12 0.0433(13) 0.0311(11) 0.0337(10) -0.0023(9) -0.0028(9) 0.0006(9) C13 0.0393(13) 0.0331(11) 0.0396(12) 0.0017(9) 0.0008(9) 0.0005(10) C14 0.0416(12) 0.0387(12) 0.0349(11) 0.0004(9) -0.0060(10) -0.0060(10) C31 0.0288(10) 0.0292(10) 0.0339(10) 0.0081(8) 0.0003(8) 0.0021(8) C51 0.0356(11) 0.0219(9) 0.0307(10) -0.0033(8) -0.0021(8) 0.0027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.9152(15) 4_645 ? Zn1 O3 1.9624(14) 2_564 ? Zn1 N12 1.9650(18) . ? Zn1 O5 2.0060(14) . ? N11 C12 1.330(3) . ? N11 C14 1.365(3) . ? N11 C11 1.454(3) . ? N12 C12 1.312(3) . ? N12 C13 1.379(3) . ? O1 C31 1.233(3) . ? O2 C31 1.267(2) . ? O2 Zn1 1.9152(15) 4_655 ? O3 C51 1.271(2) . ? O3 Zn1 1.9624(14) 2_565 ? O4 C51 1.234(3) . ? O5 H9 0.8232 . ? O5 H10 0.8397 . ? C1 C6 1.381(3) . ? C1 C2 1.388(3) . ? C1 C11 1.510(3) . ? C2 C3 1.389(3) . ? C2 H1 0.9300 . ? C3 C4 1.381(3) . ? C3 C31 1.500(3) . ? C4 C5 1.386(3) . ? C4 H2 0.9300 . ? C5 C6 1.390(3) . ? C5 C51 1.503(3) . ? C6 H3 0.9300 . ? C11 H4 0.9700 . ? C11 H5 0.9700 . ? C12 H6 0.9300 . ? C13 C14 1.344(3) . ? C13 H7 0.9300 . ? C14 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O3 96.87(6) 4_645 2_564 ? O2 Zn1 N12 125.21(7) 4_645 . ? O3 Zn1 N12 115.59(7) 2_564 . ? O2 Zn1 O5 106.93(6) 4_645 . ? O3 Zn1 O5 108.50(6) 2_564 . ? N12 Zn1 O5 102.95(7) . . ? C12 N11 C14 107.43(18) . . ? C12 N11 C11 127.0(2) . . ? C14 N11 C11 125.34(19) . . ? C12 N12 C13 105.79(18) . . ? C12 N12 Zn1 126.73(15) . . ? C13 N12 Zn1 127.20(15) . . ? C31 O2 Zn1 119.26(13) . 4_655 ? C51 O3 Zn1 110.50(13) . 2_565 ? Zn1 O5 H9 117.1 . . ? Zn1 O5 H10 124.9 . . ? H9 O5 H10 101.4 . . ? C6 C1 C2 119.51(18) . . ? C6 C1 C11 118.85(18) . . ? C2 C1 C11 121.64(18) . . ? C1 C2 C3 120.16(18) . . ? C1 C2 H1 119.9 . . ? C3 C2 H1 119.9 . . ? C4 C3 C2 119.59(18) . . ? C4 C3 C31 120.51(17) . . ? C2 C3 C31 119.90(17) . . ? C3 C4 C5 120.95(17) . . ? C3 C4 H2 119.5 . . ? C5 C4 H2 119.5 . . ? C4 C5 C6 118.76(17) . . ? C4 C5 C51 121.34(17) . . ? C6 C5 C51 119.87(18) . . ? C1 C6 C5 120.99(18) . . ? C1 C6 H3 119.5 . . ? C5 C6 H3 119.5 . . ? N11 C11 C1 111.79(17) . . ? N11 C11 H4 109.3 . . ? C1 C11 H4 109.3 . . ? N11 C11 H5 109.3 . . ? C1 C11 H5 109.3 . . ? H4 C11 H5 107.9 . . ? N12 C12 N11 111.3(2) . . ? N12 C12 H6 124.4 . . ? N11 C12 H6 124.4 . . ? C14 C13 N12 109.0(2) . . ? C14 C13 H7 125.5 . . ? N12 C13 H7 125.5 . . ? C13 C14 N11 106.55(19) . . ? C13 C14 H8 126.7 . . ? N11 C14 H8 126.7 . . ? O1 C31 O2 124.07(19) . . ? O1 C31 C3 121.07(18) . . ? O2 C31 C3 114.86(18) . . ? O4 C51 O3 124.14(18) . . ? O4 C51 C5 119.62(18) . . ? O3 C51 C5 116.14(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 N12 C12 142.43(17) 4_645 . . . ? O3 Zn1 N12 C12 22.4(2) 2_564 . . . ? O5 Zn1 N12 C12 -95.69(19) . . . . ? O2 Zn1 N12 C13 -30.6(2) 4_645 . . . ? O3 Zn1 N12 C13 -150.63(17) 2_564 . . . ? O5 Zn1 N12 C13 91.27(18) . . . . ? C6 C1 C2 C3 1.6(3) . . . . ? C11 C1 C2 C3 -177.9(2) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C1 C2 C3 C31 178.99(18) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C31 C3 C4 C5 179.49(17) . . . . ? C3 C4 C5 C6 1.4(3) . . . . ? C3 C4 C5 C51 -176.79(17) . . . . ? C2 C1 C6 C5 -0.5(3) . . . . ? C11 C1 C6 C5 179.0(2) . . . . ? C4 C5 C6 C1 -1.0(3) . . . . ? C51 C5 C6 C1 177.27(18) . . . . ? C12 N11 C11 C1 -113.3(2) . . . . ? C14 N11 C11 C1 60.9(3) . . . . ? C6 C1 C11 N11 -154.4(2) . . . . ? C2 C1 C11 N11 25.0(3) . . . . ? C13 N12 C12 N11 -0.2(2) . . . . ? Zn1 N12 C12 N11 -174.44(14) . . . . ? C14 N11 C12 N12 0.7(3) . . . . ? C11 N11 C12 N12 175.81(19) . . . . ? C12 N12 C13 C14 -0.4(2) . . . . ? Zn1 N12 C13 C14 173.77(16) . . . . ? N12 C13 C14 N11 0.9(3) . . . . ? C12 N11 C14 C13 -1.0(3) . . . . ? C11 N11 C14 C13 -176.15(19) . . . . ? Zn1 O2 C31 O1 -2.9(3) 4_655 . . . ? Zn1 O2 C31 C3 176.95(13) 4_655 . . . ? C4 C3 C31 O1 -171.60(18) . . . . ? C2 C3 C31 O1 8.3(3) . . . . ? C4 C3 C31 O2 8.5(3) . . . . ? C2 C3 C31 O2 -171.57(19) . . . . ? Zn1 O3 C51 O4 -17.6(3) 2_565 . . . ? Zn1 O3 C51 C5 158.73(14) 2_565 . . . ? C4 C5 C51 O4 -172.08(19) . . . . ? C6 C5 C51 O4 9.7(3) . . . . ? C4 C5 C51 O3 11.4(3) . . . . ? C6 C5 C51 O3 -166.77(18) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.559 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.086 #====END