# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Su, Zhi' 'Zhao, Yue' 'Sun, Wei-Yin' _publ_contact_author_name 'Sun, Wei-Yin' _publ_contact_author_email sunwy@nju.edu.cn _publ_section_title ; Anion- and auxiliary ligand-directed synthesis of cadmium(II) complexes with 3,5-di(1H-imidazol-1-yl)benzoate ; # Attachment '- sunwy.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 788701' #TrackingRef '- sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H14 Cd N4 O7' _chemical_formula_sum 'C21 H14 Cd N4 O7' _chemical_formula_weight 546.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 7.5092(16) _cell_length_b 10.629(2) _cell_length_c 13.198(3) _cell_angle_alpha 93.501(4) _cell_angle_beta 98.322(3) _cell_angle_gamma 108.989(4) _cell_volume 979.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 932 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7994 _exptl_absorpt_correction_T_max 0.8918 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4815 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3364 _reflns_number_gt 3269 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.1321P] 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 3364 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 C1 C 1.0411(4) 0.8607(3) 0.8180(2) 0.0254(6) Uani 1 1 d . . . C2 C 1.0955(4) 0.8477(3) 0.9211(2) 0.0268(6) Uani 1 1 d . . . H15 H 1.1873 0.9189 0.9641 0.032 Uiso 1 1 calc R . . C3 C 1.0120(4) 0.7281(3) 0.9591(2) 0.0259(6) Uani 1 1 d . . . C4 C 0.8819(4) 0.6182(3) 0.8964(2) 0.0270(6) Uani 1 1 d . . . H13 H 0.8312 0.5370 0.9222 0.032 Uiso 1 1 calc R . . C5 C 0.8291(4) 0.6327(3) 0.7939(2) 0.0243(6) Uani 1 1 d . . . C6 C 0.9069(4) 0.7528(3) 0.7552(2) 0.0262(6) Uani 1 1 d . . . H11 H 0.8687 0.7609 0.6864 0.031 Uiso 1 1 calc R . . C7 C 1.1208(4) 0.9943(3) 0.7773(2) 0.0263(6) Uani 1 1 d . . . C8 C 1.2301(5) 0.7702(3) 1.1309(2) 0.0358(7) Uani 1 1 d . . . H18 H 1.3488 0.8010 1.1106 0.043 Uiso 1 1 calc R . . C9 C 1.1956(5) 0.7645(3) 1.2282(2) 0.0336(7) Uani 1 1 d . . . H17 H 1.2889 0.7901 1.2872 0.040 Uiso 1 1 calc R . . C10 C 0.9225(5) 0.6906(3) 1.1287(2) 0.0306(7) Uani 1 1 d . . . H16 H 0.7915 0.6561 1.1046 0.037 Uiso 1 1 calc R . . C11 C 0.6852(5) 0.4935(3) 0.6242(2) 0.0333(7) Uani 1 1 d . . . H20 H 0.7738 0.5384 0.5847 0.040 Uiso 1 1 calc R . . C12 C 0.5255(5) 0.3868(3) 0.5912(2) 0.0340(7) Uani 1 1 d . . . H21 H 0.4849 0.3452 0.5238 0.041 Uiso 1 1 calc R . . C13 C 0.5346(4) 0.4321(3) 0.7531(2) 0.0270(6) Uani 1 1 d . . . H19 H 0.5050 0.4299 0.8191 0.032 Uiso 1 1 calc R . . C14 C 0.7327(5) 1.2486(3) 0.3877(2) 0.0290(7) Uani 1 1 d . . . C15 C 0.5817(5) 1.1376(3) 0.3371(2) 0.0343(7) Uani 1 1 d . . . H6 H 0.5383 1.0617 0.3704 0.041 Uiso 1 1 calc R . . C16 C 0.4959(5) 1.1397(3) 0.2376(2) 0.0340(7) Uani 1 1 d . . . H7 H 0.3952 1.0651 0.2043 0.041 Uiso 1 1 calc R . . C17 C 0.5593(4) 1.2527(3) 0.1873(2) 0.0295(7) Uani 1 1 d . . . C18 C 0.7021(5) 1.3660(3) 0.2404(2) 0.0296(7) Uani 1 1 d . . . H3 H 0.7406 1.4437 0.2085 0.036 Uiso 1 1 calc R . . C19 C 0.7873(5) 1.3643(3) 0.3399(2) 0.0305(7) Uani 1 1 d . . . H4 H 0.8817 1.4411 0.3751 0.037 Uiso 1 1 calc R . . C20 C 0.8504(5) 1.2378(3) 0.4874(2) 0.0312(7) Uani 1 1 d . . . C21 C 0.4850(5) 1.2546(3) 0.0768(2) 0.0325(7) Uani 1 1 d . . . Cd1 Cd 1.12367(3) 1.21198(2) 0.641054(15) 0.02569(9) Uani 1 1 d . . . H2 H 0.342(7) 1.137(5) -0.027(4) 0.064(14) Uiso 1 1 d . . . N1 N 1.0015(4) 0.7153(3) 1.2271(2) 0.0323(6) Uani 1 1 d . . . N2 N 1.0553(4) 0.7213(2) 1.06812(19) 0.0264(5) Uani 1 1 d . . . N3 N 0.4308(4) 0.3486(2) 0.67283(19) 0.0279(5) Uani 1 1 d . . . N4 N 0.6911(3) 0.5223(2) 0.72709(18) 0.0254(5) Uani 1 1 d . . . O1 O 1.2440(3) 1.0903(2) 0.83414(17) 0.0376(5) Uani 1 1 d . . . O2 O 1.0535(3) 1.0021(2) 0.68523(16) 0.0340(5) Uani 1 1 d . . . O3 O 0.7911(4) 1.1378(2) 0.53459(17) 0.0388(6) Uani 1 1 d . . . O4 O 1.0108(3) 1.3272(2) 0.51663(18) 0.0397(6) Uani 1 1 d . . . O5 O 0.3699(5) 1.1360(3) 0.0327(2) 0.0550(8) Uani 1 1 d . . . O6 O 0.5265(4) 1.3521(2) 0.03133(19) 0.0454(6) Uani 1 1 d . . . O7 O 1.2099(3) 1.1191(2) 0.49401(17) 0.0360(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 C1 0.0303(16) 0.0235(14) 0.0202(14) 0.0053(11) 0.0041(12) 0.0057(12) C2 0.0280(16) 0.0253(15) 0.0196(14) 0.0014(11) -0.0009(12) 0.0014(12) C3 0.0293(16) 0.0282(15) 0.0195(14) 0.0060(12) 0.0038(12) 0.0086(12) C4 0.0300(16) 0.0230(14) 0.0239(15) 0.0055(12) 0.0040(12) 0.0035(12) C5 0.0237(15) 0.0226(14) 0.0219(14) 0.0013(11) 0.0012(11) 0.0031(12) C6 0.0259(16) 0.0307(16) 0.0179(14) 0.0039(12) 0.0001(11) 0.0056(12) C7 0.0299(16) 0.0247(15) 0.0207(15) 0.0042(12) 0.0013(12) 0.0053(13) C8 0.0325(18) 0.047(2) 0.0253(16) 0.0054(14) 0.0044(14) 0.0100(15) C9 0.0328(18) 0.0411(18) 0.0241(16) 0.0027(13) -0.0031(13) 0.0125(14) C10 0.0281(17) 0.0352(17) 0.0220(15) 0.0050(13) 0.0016(12) 0.0027(13) C11 0.0319(18) 0.0335(17) 0.0253(16) 0.0051(13) 0.0048(13) -0.0017(14) C12 0.0344(18) 0.0362(17) 0.0214(15) 0.0011(13) -0.0006(13) 0.0012(14) C13 0.0239(16) 0.0265(15) 0.0261(15) 0.0035(12) 0.0029(12) 0.0030(12) C14 0.0315(17) 0.0323(16) 0.0229(15) 0.0014(12) 0.0028(13) 0.0114(13) C15 0.0371(19) 0.0317(17) 0.0287(17) 0.0086(13) 0.0028(14) 0.0046(14) C16 0.0343(18) 0.0286(16) 0.0295(17) 0.0032(13) -0.0022(14) 0.0011(13) C17 0.0299(17) 0.0314(16) 0.0254(16) 0.0016(12) -0.0008(13) 0.0106(13) C18 0.0306(17) 0.0265(15) 0.0310(17) 0.0058(12) 0.0009(13) 0.0100(13) C19 0.0311(17) 0.0273(15) 0.0286(16) -0.0009(12) -0.0022(13) 0.0079(13) C20 0.0394(19) 0.0351(17) 0.0207(15) -0.0001(13) 0.0011(13) 0.0170(15) C21 0.0314(18) 0.0360(18) 0.0276(16) 0.0013(14) -0.0017(13) 0.0115(14) Cd1 0.02614(14) 0.02481(14) 0.01954(13) 0.00374(9) 0.00023(9) 0.00118(9) N1 0.0346(15) 0.0380(15) 0.0226(13) 0.0074(11) 0.0037(11) 0.0098(12) N2 0.0283(14) 0.0219(12) 0.0237(13) 0.0028(10) 0.0031(10) 0.0022(10) N3 0.0240(13) 0.0276(13) 0.0263(13) 0.0034(10) 0.0015(10) 0.0019(10) N4 0.0247(13) 0.0230(12) 0.0224(12) 0.0026(10) 0.0005(10) 0.0015(10) O1 0.0459(14) 0.0264(11) 0.0260(12) 0.0054(9) -0.0042(10) -0.0029(10) O2 0.0444(14) 0.0262(11) 0.0210(11) 0.0065(8) -0.0039(9) 0.0014(10) O3 0.0537(16) 0.0356(13) 0.0236(11) 0.0072(10) -0.0002(10) 0.0128(11) O4 0.0380(14) 0.0439(14) 0.0293(12) 0.0050(10) -0.0078(10) 0.0088(11) O5 0.077(2) 0.0374(14) 0.0249(13) 0.0036(11) -0.0168(13) -0.0033(13) O6 0.0588(17) 0.0375(13) 0.0323(13) 0.0123(11) -0.0010(12) 0.0085(12) O7 0.0414(14) 0.0303(12) 0.0282(12) -0.0006(9) 0.0044(10) 0.0027(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 C1 C6 1.382(4) . ? C1 C2 1.391(4) . ? C1 C7 1.516(4) . ? C2 C3 1.383(4) . ? C2 H15 0.9300 . ? C3 C4 1.382(4) . ? C3 N2 1.440(4) . ? C4 C5 1.386(4) . ? C4 H13 0.9300 . ? C5 C6 1.383(4) . ? C5 N4 1.430(4) . ? C6 H11 0.9300 . ? C7 O1 1.245(4) . ? C7 O2 1.266(4) . ? C8 C9 1.347(5) . ? C8 N2 1.367(4) . ? C8 H18 0.9300 . ? C9 N1 1.377(4) . ? C9 H17 0.9300 . ? C10 N1 1.319(4) . ? C10 N2 1.338(4) . ? C10 H16 0.9300 . ? C11 C12 1.348(5) . ? C11 N4 1.365(4) . ? C11 H20 0.9300 . ? C12 N3 1.385(4) . ? C12 H21 0.9300 . ? C13 N3 1.309(4) . ? C13 N4 1.357(4) . ? C13 H19 0.9300 . ? C14 C19 1.386(4) . ? C14 C15 1.392(5) . ? C14 C20 1.507(4) . ? C15 C16 1.381(4) . ? C15 H6 0.9300 . ? C16 C17 1.388(4) . ? C16 H7 0.9300 . ? C17 C18 1.390(4) . ? C17 C21 1.489(4) . ? C18 C19 1.380(4) . ? C18 H3 0.9300 . ? C19 H4 0.9300 . ? C20 O3 1.253(4) . ? C20 O4 1.256(4) . ? C21 O6 1.205(4) . ? C21 O5 1.315(4) . ? Cd1 N3 2.252(3) 1_665 ? Cd1 O2 2.253(2) . ? Cd1 N1 2.300(3) 2_777 ? Cd1 O4 2.331(2) . ? Cd1 O7 2.388(2) . ? Cd1 O3 2.530(3) . ? N1 Cd1 2.300(3) 2_777 ? N3 Cd1 2.252(2) 1_445 ? O5 H2 0.79(5) . ? 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 C6 C1 C2 119.2(3) . . ? C6 C1 C7 120.7(3) . . ? C2 C1 C7 119.9(3) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H15 120.3 . . ? C1 C2 H15 120.3 . . ? C4 C3 C2 121.8(3) . . ? C4 C3 N2 119.6(3) . . ? C2 C3 N2 118.5(3) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 H13 121.0 . . ? C5 C4 H13 121.0 . . ? C6 C5 C4 121.0(3) . . ? C6 C5 N4 119.3(3) . . ? C4 C5 N4 119.7(3) . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H11 119.8 . . ? C5 C6 H11 119.8 . . ? O1 C7 O2 123.2(3) . . ? O1 C7 C1 120.2(3) . . ? O2 C7 C1 116.6(3) . . ? C9 C8 N2 106.2(3) . . ? C9 C8 H18 126.9 . . ? N2 C8 H18 126.9 . . ? C8 C9 N1 109.9(3) . . ? C8 C9 H17 125.1 . . ? N1 C9 H17 125.1 . . ? N1 C10 N2 111.3(3) . . ? N1 C10 H16 124.3 . . ? N2 C10 H16 124.3 . . ? C12 C11 N4 106.2(3) . . ? C12 C11 H20 126.9 . . ? N4 C11 H20 126.9 . . ? C11 C12 N3 109.7(3) . . ? C11 C12 H21 125.1 . . ? N3 C12 H21 125.1 . . ? N3 C13 N4 111.0(3) . . ? N3 C13 H19 124.5 . . ? N4 C13 H19 124.5 . . ? C19 C14 C15 119.2(3) . . ? C19 C14 C20 120.1(3) . . ? C15 C14 C20 120.3(3) . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H6 119.8 . . ? C14 C15 H6 119.8 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H7 119.9 . . ? C17 C16 H7 119.9 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 C21 122.1(3) . . ? C18 C17 C21 118.7(3) . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H3 119.7 . . ? C17 C18 H3 119.7 . . ? C18 C19 C14 120.2(3) . . ? C18 C19 H4 119.9 . . ? C14 C19 H4 119.9 . . ? O3 C20 O4 122.5(3) . . ? O3 C20 C14 119.6(3) . . ? O4 C20 C14 117.8(3) . . ? O6 C21 O5 123.1(3) . . ? O6 C21 C17 124.6(3) . . ? O5 C21 C17 112.2(3) . . ? N3 Cd1 O2 118.80(9) 1_665 . ? N3 Cd1 N1 102.82(10) 1_665 2_777 ? O2 Cd1 N1 93.78(9) . 2_777 ? N3 Cd1 O4 97.33(9) 1_665 . ? O2 Cd1 O4 139.09(8) . . ? N1 Cd1 O4 96.33(9) 2_777 . ? N3 Cd1 O7 84.81(9) 1_665 . ? O2 Cd1 O7 83.63(8) . . ? N1 Cd1 O7 172.23(9) 2_777 . ? O4 Cd1 O7 81.09(8) . . ? N3 Cd1 O3 150.48(8) 1_665 . ? O2 Cd1 O3 87.51(8) . . ? N1 Cd1 O3 87.37(9) 2_777 . ? O4 Cd1 O3 53.64(8) . . ? O7 Cd1 O3 85.20(8) . . ? C10 N1 C9 105.2(3) . . ? C10 N1 Cd1 125.8(2) . 2_777 ? C9 N1 Cd1 119.7(2) . 2_777 ? C10 N2 C8 107.4(3) . . ? C10 N2 C3 123.5(3) . . ? C8 N2 C3 127.7(3) . . ? C13 N3 C12 105.7(3) . . ? C13 N3 Cd1 132.2(2) . 1_445 ? C12 N3 Cd1 119.6(2) . 1_445 ? C13 N4 C11 107.4(2) . . ? C13 N4 C5 126.1(2) . . ? C11 N4 C5 126.4(2) . . ? C7 O2 Cd1 114.87(18) . . ? C20 O3 Cd1 86.9(2) . . ? C20 O4 Cd1 96.08(19) . . ? C21 O5 H2 111(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.736 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.080 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 788702' #TrackingRef '- sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H32 Cd2 N8 O13' _chemical_formula_sum 'C34 H32 Cd2 N8 O13' _chemical_formula_weight 985.48 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2200(18) _cell_length_b 18.831(4) _cell_length_c 10.750(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.087(2) _cell_angle_gamma 90.00 _cell_volume 1810.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4726 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.11 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8058 _exptl_absorpt_correction_T_max 0.9063 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9751 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3556 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3556 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 C1 C 0.7717(3) 0.34880(17) 0.2240(3) 0.0250(7) Uani 1 1 d . . . C2 C 0.7368(3) 0.35205(17) 0.3426(3) 0.0256(7) Uani 1 1 d . . . H2 H 0.6437 0.3684 0.3489 0.031 Uiso 1 1 calc R . . C3 C 0.8420(3) 0.33076(16) 0.4512(3) 0.0241(6) Uani 1 1 d . . . C4 C 0.9835(3) 0.30821(16) 0.4456(3) 0.0255(7) Uani 1 1 d . . . H4 H 1.0531 0.2938 0.5193 0.031 Uiso 1 1 calc R . . C5 C 1.0180(3) 0.30780(17) 0.3275(3) 0.0251(7) Uani 1 1 d . . . C6 C 0.9140(3) 0.32745(16) 0.2171(3) 0.0275(7) Uani 1 1 d . . . H6 H 0.9392 0.3264 0.1384 0.033 Uiso 1 1 calc R . . C7 C 0.6588(3) 0.36671(17) 0.1015(3) 0.0277(7) Uani 1 1 d . . . C8 C 0.9093(3) 0.34792(18) 0.6895(3) 0.0275(7) Uani 1 1 d . . . H8 H 1.0126 0.3516 0.7033 0.033 Uiso 1 1 calc R . . C9 C 0.8296(3) 0.35320(18) 0.7784(3) 0.0289(7) Uani 1 1 d . . . H9 H 0.8696 0.3616 0.8653 0.035 Uiso 1 1 calc R . . C10 C 0.6714(3) 0.33489(18) 0.5995(3) 0.0307(7) Uani 1 1 d . . . H10 H 0.5822 0.3282 0.5380 0.037 Uiso 1 1 calc R . . C11 C 1.2424(4) 0.31564(19) 0.2371(4) 0.0381(8) Uani 1 1 d . . . H11 H 1.2160 0.3557 0.1861 0.046 Uiso 1 1 calc R . . C12 C 1.3641(4) 0.27501(19) 0.2473(3) 0.0384(8) Uani 1 1 d . . . H12 H 1.4378 0.2828 0.2031 0.046 Uiso 1 1 calc R . . C13 C 1.2415(3) 0.22815(18) 0.3723(3) 0.0321(8) Uani 1 1 d . . . H13 H 1.2109 0.1984 0.4301 0.039 Uiso 1 1 calc R . . C14 C 0.1268(3) 0.47314(16) 0.5852(3) 0.0301(7) Uani 1 1 d . . . C15 C 0.1132(3) 0.47081(17) 0.4526(3) 0.0323(8) Uani 1 1 d . . . H15 H 0.1897 0.4513 0.4209 0.039 Uiso 1 1 calc R . . C16 C 0.0115(3) 0.50306(17) 0.6304(3) 0.0330(8) Uani 1 1 d . . . H16 H 0.0195 0.5053 0.7183 0.040 Uiso 1 1 calc R . . C17 C 0.2611(3) 0.44129(18) 0.6754(3) 0.0330(8) Uani 1 1 d . . . Cd1 Cd 0.50825(2) 0.381659(12) 0.83577(2) 0.02648(10) Uani 1 1 d . . . N1 N 0.6810(3) 0.34449(15) 0.7224(2) 0.0298(6) Uani 1 1 d . . . N2 N 0.8082(3) 0.33599(13) 0.5742(2) 0.0245(6) Uani 1 1 d . . . N3 N 1.3649(3) 0.21984(15) 0.3328(3) 0.0337(6) Uani 1 1 d . . . N4 N 1.1654(3) 0.28599(13) 0.3171(2) 0.0255(6) Uani 1 1 d . . . O1 O 0.5319(3) 0.38806(13) 0.1034(2) 0.0408(6) Uani 1 1 d . . . O2 O 0.6991(3) 0.35611(18) 0.0009(2) 0.0547(8) Uani 1 1 d . . . O3 O 0.2707(3) 0.44206(14) 0.7937(2) 0.0433(6) Uani 1 1 d . . . O4 O 0.3591(3) 0.41272(15) 0.6290(2) 0.0452(6) Uani 1 1 d . . . O5 O 0.6066(3) 0.49807(13) 0.8262(3) 0.0508(7) Uani 1 1 d . . . O6 O 0.4804(7) 0.4743(4) 0.4410(6) 0.0725(19) Uani 0.50 1 d P . . O7 O 0.8724(3) 0.54421(18) -0.0019(3) 0.0670(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 C1 0.0262(15) 0.0271(16) 0.0211(16) 0.0010(13) 0.0049(13) 0.0002(13) C2 0.0244(15) 0.0277(16) 0.0249(16) -0.0023(14) 0.0066(13) -0.0002(13) C3 0.0278(15) 0.0261(16) 0.0196(15) 0.0004(13) 0.0082(12) 0.0000(13) C4 0.0277(16) 0.0282(17) 0.0203(16) 0.0015(13) 0.0051(13) 0.0026(13) C5 0.0252(15) 0.0255(16) 0.0251(17) -0.0019(13) 0.0070(13) 0.0023(13) C6 0.0316(16) 0.0318(17) 0.0202(16) -0.0011(14) 0.0080(13) 0.0004(14) C7 0.0258(16) 0.0345(18) 0.0216(17) 0.0032(13) 0.0033(13) -0.0029(13) C8 0.0230(15) 0.0357(18) 0.0230(16) 0.0014(14) 0.0044(13) -0.0001(14) C9 0.0300(17) 0.0363(18) 0.0190(16) 0.0003(14) 0.0035(13) 0.0016(15) C10 0.0218(15) 0.045(2) 0.0253(17) 0.0008(15) 0.0063(13) 0.0025(14) C11 0.0375(19) 0.036(2) 0.045(2) 0.0073(17) 0.0175(17) 0.0027(16) C12 0.0303(17) 0.046(2) 0.043(2) 0.0025(17) 0.0169(16) -0.0046(16) C13 0.0299(17) 0.040(2) 0.0285(18) 0.0014(15) 0.0099(14) 0.0030(15) C14 0.0241(16) 0.0229(16) 0.039(2) 0.0041(14) -0.0008(14) -0.0005(13) C15 0.0278(16) 0.0276(17) 0.039(2) 0.0019(15) 0.0040(15) 0.0038(14) C16 0.0340(18) 0.0303(18) 0.0306(18) 0.0024(15) 0.0000(14) 0.0003(14) C17 0.0245(16) 0.0335(19) 0.037(2) 0.0091(15) -0.0014(15) -0.0016(14) Cd1 0.02029(13) 0.03527(16) 0.02295(14) 0.00358(10) 0.00348(9) 0.00316(9) N1 0.0266(13) 0.0425(17) 0.0209(14) 0.0003(13) 0.0065(11) 0.0051(12) N2 0.0259(13) 0.0290(14) 0.0189(13) 0.0023(11) 0.0060(11) 0.0028(11) N3 0.0270(14) 0.0406(17) 0.0352(16) 0.0018(13) 0.0107(12) 0.0045(12) N4 0.0281(13) 0.0285(14) 0.0206(13) -0.0004(11) 0.0071(11) 0.0038(11) O1 0.0313(13) 0.0514(16) 0.0369(14) 0.0025(12) 0.0026(11) 0.0111(11) O2 0.0342(14) 0.109(2) 0.0200(13) 0.0057(14) 0.0049(11) 0.0134(15) O3 0.0348(13) 0.0540(17) 0.0359(15) 0.0063(12) -0.0016(11) 0.0101(12) O4 0.0329(13) 0.0618(17) 0.0401(15) 0.0166(14) 0.0072(11) 0.0165(13) O5 0.0393(14) 0.0368(14) 0.0739(19) -0.0064(14) 0.0094(14) -0.0015(12) O6 0.059(4) 0.095(5) 0.064(4) 0.023(4) 0.015(3) -0.007(3) O7 0.0454(16) 0.090(2) 0.063(2) 0.0021(17) 0.0081(15) 0.0018(16) _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 C1 C2 1.390(4) . ? C1 C6 1.391(4) . ? C1 C7 1.505(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.387(4) . ? C3 N2 1.434(4) . ? C4 C5 1.382(4) . ? C4 H4 0.9300 . ? C5 C6 1.383(4) . ? C5 N4 1.450(4) . ? C6 H6 0.9300 . ? C7 O1 1.241(4) . ? C7 O2 1.243(4) . ? C8 C9 1.344(4) . ? C8 N2 1.377(4) . ? C8 H8 0.9300 . ? C9 N1 1.365(4) . ? C9 H9 0.9300 . ? C10 N1 1.315(4) . ? C10 N2 1.354(4) . ? C10 H10 0.9300 . ? C11 C12 1.341(5) . ? C11 N4 1.360(4) . ? C11 H11 0.9300 . ? C12 N3 1.386(4) . ? C12 H12 0.9300 . ? C13 N3 1.317(4) . ? C13 N4 1.352(4) . ? C13 H13 0.9300 . ? C14 C16 1.391(4) . ? C14 C15 1.401(5) . ? C14 C17 1.500(4) . ? C15 C16 1.364(4) 3_566 ? C15 H15 0.9300 . ? C16 C15 1.364(4) 3_566 ? C16 H16 0.9300 . ? C17 O4 1.255(4) . ? C17 O3 1.252(4) . ? Cd1 O2 2.227(2) 1_556 ? Cd1 N3 2.319(3) 4_466 ? Cd1 N1 2.336(3) . ? Cd1 O4 2.385(2) . ? Cd1 O3 2.411(2) . ? N3 Cd1 2.319(3) 4_665 ? O2 Cd1 2.227(2) 1_554 ? O6 O6 1.565(13) 3_666 ? 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 C2 C1 C6 119.6(3) . . ? C2 C1 C7 121.8(3) . . ? C6 C1 C7 118.6(3) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 N2 119.5(3) . . ? C4 C3 N2 118.6(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 N4 118.4(3) . . ? C4 C5 N4 120.2(3) . . ? C5 C6 C1 119.8(3) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? O1 C7 O2 123.3(3) . . ? O1 C7 C1 120.8(3) . . ? O2 C7 C1 115.8(3) . . ? C9 C8 N2 106.5(3) . . ? C9 C8 H8 126.7 . . ? N2 C8 H8 126.7 . . ? C8 C9 N1 110.0(3) . . ? C8 C9 H9 125.0 . . ? N1 C9 H9 125.0 . . ? N1 C10 N2 111.2(3) . . ? N1 C10 H10 124.4 . . ? N2 C10 H10 124.4 . . ? C12 C11 N4 105.6(3) . . ? C12 C11 H11 127.2 . . ? N4 C11 H11 127.2 . . ? C11 C12 N3 110.5(3) . . ? C11 C12 H12 124.7 . . ? N3 C12 H12 124.7 . . ? N3 C13 N4 110.5(3) . . ? N3 C13 H13 124.7 . . ? N4 C13 H13 124.7 . . ? C16 C14 C15 118.8(3) . . ? C16 C14 C17 121.1(3) . . ? C15 C14 C17 120.1(3) . . ? C16 C15 C14 120.4(3) 3_566 . ? C16 C15 H15 119.8 3_566 . ? C14 C15 H15 119.8 . . ? C15 C16 C14 120.8(3) 3_566 . ? C15 C16 H16 119.6 3_566 . ? C14 C16 H16 119.6 . . ? O4 C17 O3 121.9(3) . . ? O4 C17 C14 118.4(3) . . ? O3 C17 C14 119.7(3) . . ? O2 Cd1 N3 99.77(11) 1_556 4_466 ? O2 Cd1 N1 81.03(9) 1_556 . ? N3 Cd1 N1 101.80(10) 4_466 . ? O2 Cd1 O4 163.88(9) 1_556 . ? N3 Cd1 O4 89.54(10) 4_466 . ? N1 Cd1 O4 84.22(9) . . ? O2 Cd1 O3 139.21(9) 1_556 . ? N3 Cd1 O3 84.13(9) 4_466 . ? N1 Cd1 O3 138.34(9) . . ? O4 Cd1 O3 54.39(8) . . ? C10 N1 C9 106.0(2) . . ? C10 N1 Cd1 132.6(2) . . ? C9 N1 Cd1 118.2(2) . . ? C10 N2 C8 106.4(3) . . ? C10 N2 C3 127.4(3) . . ? C8 N2 C3 126.2(2) . . ? C13 N3 C12 105.0(3) . . ? C13 N3 Cd1 128.9(2) . 4_665 ? C12 N3 Cd1 122.5(2) . 4_665 ? C13 N4 C11 108.3(3) . . ? C13 N4 C5 126.1(3) . . ? C11 N4 C5 125.1(3) . . ? C7 O2 Cd1 108.3(2) . 1_554 ? C17 O3 Cd1 91.2(2) . . ? C17 O4 Cd1 92.4(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.599 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.097 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 788703' #TrackingRef '- sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Cd N4 O4' _chemical_formula_sum 'C17 H11 Cd N4 O4' _chemical_formula_weight 447.70 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 'P 21/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 6.059(4) _cell_length_b 17.373(12) _cell_length_c 14.478(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.0000(10) _cell_angle_gamma 90.00 _cell_volume 1524.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5232 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 28.33 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7579 _exptl_absorpt_correction_T_max 0.9303 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8083 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2997 _reflns_number_gt 2685 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2997 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 0.4850(4) 0.52322(15) 0.14413(18) 0.0227(6) Uani 1 1 d . . . C2 C 0.6794(4) 0.55058(16) 0.18237(18) 0.0236(6) Uani 1 1 d . . . H2 H 0.7477 0.5244 0.2306 0.028 Uiso 1 1 calc R . . C3 C 0.7708(4) 0.61842(16) 0.14684(18) 0.0227(6) Uani 1 1 d . . . C4 C 0.6750(5) 0.65720(15) 0.0744(2) 0.0246(6) Uani 1 1 d . . . H6 H 0.7406 0.7011 0.0499 0.030 Uiso 1 1 calc R . . C5 C 0.4786(4) 0.62937(16) 0.03861(17) 0.0213(5) Uani 1 1 d . . . C6 C 0.3834(4) 0.56249(16) 0.07273(18) 0.0233(6) Uani 1 1 d . . . H4 H 0.2522 0.5442 0.0477 0.028 Uiso 1 1 calc R . . C7 C 0.3683(4) 0.45334(17) 0.18443(19) 0.0262(6) Uani 1 1 d . . . C8 C 1.0954(4) 0.61524(18) 0.25357(18) 0.0257(6) Uani 1 1 d . . . H7 H 1.0802 0.5658 0.2774 0.031 Uiso 1 1 calc R . . C9 C 1.2508(5) 0.66782(17) 0.2761(2) 0.0275(6) Uani 1 1 d . . . H8 H 1.3615 0.6602 0.3196 0.033 Uiso 1 1 calc R . . C10 C 1.0466(5) 0.72193(17) 0.17428(19) 0.0270(6) Uani 1 1 d . . . H9 H 0.9860 0.7577 0.1338 0.032 Uiso 1 1 calc R . . C11 C 0.3993(5) 0.74664(18) -0.0571(2) 0.0318(7) Uani 1 1 d . . . H10 H 0.4962 0.7814 -0.0299 0.038 Uiso 1 1 calc R . . C12 C 0.2619(5) 0.76049(18) -0.1273(2) 0.0317(7) Uani 1 1 d . . . H11 H 0.2472 0.8074 -0.1575 0.038 Uiso 1 1 calc R . . C13 C 0.2149(5) 0.64249(17) -0.0905(2) 0.0280(6) Uani 1 1 d . . . H12 H 0.1643 0.5920 -0.0891 0.034 Uiso 1 1 calc R . . C14 C -0.3440(5) 0.45665(17) 0.44963(18) 0.0253(6) Uani 1 1 d . . . C15 C -0.3208(5) 0.53574(18) 0.4590(2) 0.0359(7) Uani 1 1 d . . . H15 H -0.2019 0.5606 0.4315 0.043 Uiso 1 1 calc R . . C16 C -0.4739(6) 0.57821(18) 0.5093(2) 0.0375(7) Uani 1 1 d . . . H16 H -0.4542 0.6310 0.5157 0.045 Uiso 1 1 calc R . . C17 C -0.1806(5) 0.41099(17) 0.39188(18) 0.0261(6) Uani 1 1 d . . . Cd1 Cd 0.09537(3) 0.345999(11) 0.260705(12) 0.02067(10) Uani 1 1 d . . . N1 N 1.2218(4) 0.73443(13) 0.22537(16) 0.0247(5) Uani 1 1 d . . . N2 N 0.9649(4) 0.64994(12) 0.18818(16) 0.0219(5) Uani 1 1 d . . . N3 N 0.1455(4) 0.69480(14) -0.14810(16) 0.0274(5) Uani 1 1 d . . . N4 N 0.3697(4) 0.67126(14) -0.03309(15) 0.0242(5) Uani 1 1 d . . . O1 O 0.1876(4) 0.43482(14) 0.14687(14) 0.0386(5) Uani 1 1 d . . . O2 O 0.4445(3) 0.41937(14) 0.25158(14) 0.0350(5) Uani 1 1 d . . . O3 O -0.0475(3) 0.44709(13) 0.34029(14) 0.0333(5) Uani 1 1 d . . . O4 O -0.1815(4) 0.33867(11) 0.39572(15) 0.0334(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 C1 0.0206(13) 0.0208(14) 0.0267(13) -0.0019(10) -0.0017(11) -0.0019(11) C2 0.0223(13) 0.0225(14) 0.0262(13) 0.0019(11) -0.0040(11) -0.0014(12) C3 0.0179(12) 0.0213(14) 0.0290(13) -0.0046(11) -0.0045(11) -0.0024(11) C4 0.0235(14) 0.0215(15) 0.0289(14) 0.0019(10) -0.0043(12) -0.0051(11) C5 0.0208(13) 0.0218(13) 0.0214(12) -0.0009(10) -0.0058(10) -0.0015(12) C6 0.0212(13) 0.0217(13) 0.0270(13) -0.0033(11) -0.0047(11) -0.0050(11) C7 0.0223(13) 0.0268(15) 0.0294(14) -0.0033(11) 0.0023(11) -0.0019(13) C8 0.0238(15) 0.0187(15) 0.0348(15) 0.0001(11) -0.0083(12) 0.0033(11) C9 0.0202(14) 0.0250(14) 0.0374(16) -0.0022(12) -0.0091(12) 0.0012(12) C10 0.0260(14) 0.0223(14) 0.0328(14) 0.0031(11) -0.0079(12) -0.0047(12) C11 0.0318(16) 0.0247(15) 0.0388(16) 0.0048(12) -0.0141(13) -0.0118(13) C12 0.0328(16) 0.0268(16) 0.0353(15) 0.0063(12) -0.0075(13) -0.0063(13) C13 0.0271(15) 0.0224(14) 0.0344(15) 0.0005(11) -0.0127(13) -0.0037(12) C14 0.0290(14) 0.0236(14) 0.0233(13) 0.0006(11) -0.0015(11) 0.0031(13) C15 0.0365(17) 0.0262(15) 0.0450(17) -0.0045(13) 0.0134(14) -0.0043(14) C16 0.0468(19) 0.0204(14) 0.0454(17) -0.0028(13) 0.0123(15) 0.0000(14) C17 0.0250(14) 0.0286(16) 0.0245(13) -0.0026(11) -0.0070(11) 0.0049(12) Cd1 0.02048(14) 0.01748(14) 0.02407(14) 0.00113(7) -0.00346(9) 0.00180(7) N1 0.0196(11) 0.0200(12) 0.0345(12) -0.0009(9) -0.0063(9) -0.0031(10) N2 0.0189(12) 0.0196(12) 0.0272(12) -0.0007(8) -0.0064(10) -0.0029(9) N3 0.0258(12) 0.0242(13) 0.0323(12) 0.0011(10) -0.0089(10) -0.0026(10) N4 0.0237(12) 0.0245(11) 0.0245(12) -0.0013(9) -0.0080(10) -0.0031(10) O1 0.0325(11) 0.0443(13) 0.0392(11) 0.0097(10) -0.0130(9) -0.0215(11) O2 0.0302(11) 0.0339(13) 0.0408(12) 0.0142(9) -0.0106(9) -0.0064(10) O3 0.0292(11) 0.0306(12) 0.0401(11) -0.0012(9) 0.0086(9) 0.0018(10) O4 0.0405(13) 0.0198(11) 0.0398(12) -0.0016(8) 0.0003(10) 0.0090(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.383(4) . ? C1 C2 1.386(4) . ? C1 C7 1.521(4) . ? C2 C3 1.400(4) . ? C2 H2 0.9300 . ? C3 C4 1.375(4) . ? C3 N2 1.429(4) . ? C4 C5 1.385(4) . ? C4 H6 0.9300 . ? C5 C6 1.388(4) . ? C5 N4 1.429(4) . ? C6 H4 0.9300 . ? C7 O2 1.227(4) . ? C7 O1 1.264(3) . ? C8 C9 1.351(4) . ? C8 N2 1.373(3) . ? C8 H7 0.9300 . ? C9 N1 1.382(4) . ? C9 H8 0.9300 . ? C10 N1 1.312(4) . ? C10 N2 1.360(4) . ? C10 H9 0.9300 . ? C11 C12 1.336(4) . ? C11 N4 1.367(4) . ? C11 H10 0.9300 . ? C12 N3 1.375(4) . ? C12 H11 0.9300 . ? C13 N3 1.303(4) . ? C13 N4 1.349(4) . ? C13 H12 0.9300 . ? C14 C15 1.388(4) . ? C14 C16 1.392(4) 3_466 ? C14 C17 1.519(4) . ? C15 C16 1.391(4) . ? C15 H15 0.9300 . ? C16 C14 1.392(4) 3_466 ? C16 H16 0.9300 . ? C17 O4 1.258(4) . ? C17 O3 1.266(4) . ? Cd1 N1 2.242(3) 2_645 ? Cd1 O3 2.272(2) . ? Cd1 N3 2.300(3) 3_565 ? Cd1 O1 2.326(2) . ? Cd1 O2 2.473(3) . ? Cd1 O4 2.579(3) . ? N1 Cd1 2.242(3) 2_655 ? N3 Cd1 2.300(2) 3_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 C6 C1 C2 120.5(2) . . ? C6 C1 C7 118.3(2) . . ? C2 C1 C7 121.0(2) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 121.7(2) . . ? C4 C3 N2 118.6(2) . . ? C2 C3 N2 119.6(2) . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H6 120.8 . . ? C5 C4 H6 120.8 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 N4 119.4(2) . . ? C6 C5 N4 119.5(2) . . ? C1 C6 C5 119.6(2) . . ? C1 C6 H4 120.2 . . ? C5 C6 H4 120.2 . . ? O2 C7 O1 123.0(3) . . ? O2 C7 C1 120.9(3) . . ? O1 C7 C1 116.1(3) . . ? C9 C8 N2 105.7(3) . . ? C9 C8 H7 127.1 . . ? N2 C8 H7 127.1 . . ? C8 C9 N1 110.5(3) . . ? C8 C9 H8 124.8 . . ? N1 C9 H8 124.8 . . ? N1 C10 N2 111.3(3) . . ? N1 C10 H9 124.4 . . ? N2 C10 H9 124.4 . . ? C12 C11 N4 106.5(3) . . ? C12 C11 H10 126.7 . . ? N4 C11 H10 126.7 . . ? C11 C12 N3 109.7(3) . . ? C11 C12 H11 125.2 . . ? N3 C12 H11 125.2 . . ? N3 C13 N4 111.1(3) . . ? N3 C13 H12 124.4 . . ? N4 C13 H12 124.4 . . ? C15 C14 C16 118.0(3) . 3_466 ? C15 C14 C17 120.3(3) . . ? C16 C14 C17 121.6(3) 3_466 . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C14 121.4(3) . 3_466 ? C15 C16 H16 119.3 . . ? C14 C16 H16 119.3 3_466 . ? O4 C17 O3 121.6(3) . . ? O4 C17 C14 119.6(3) . . ? O3 C17 C14 118.8(3) . . ? N1 Cd1 O3 144.21(8) 2_645 . ? N1 Cd1 N3 96.36(9) 2_645 3_565 ? O3 Cd1 N3 110.85(9) . 3_565 ? N1 Cd1 O1 121.25(9) 2_645 . ? O3 Cd1 O1 86.45(10) . . ? N3 Cd1 O1 81.64(9) 3_565 . ? N1 Cd1 O2 91.60(9) 2_645 . ? O3 Cd1 O2 87.39(9) . . ? N3 Cd1 O2 131.58(8) 3_565 . ? O1 Cd1 O2 54.18(7) . . ? N1 Cd1 O4 102.16(8) 2_645 . ? O3 Cd1 O4 53.55(7) . . ? N3 Cd1 O4 96.27(10) 3_565 . ? O1 Cd1 O4 136.56(8) . . ? O2 Cd1 O4 128.48(8) . . ? C10 N1 C9 105.3(2) . . ? C10 N1 Cd1 126.4(2) . 2_655 ? C9 N1 Cd1 127.86(19) . 2_655 ? C10 N2 C8 107.2(2) . . ? C10 N2 C3 126.2(2) . . ? C8 N2 C3 126.5(2) . . ? C13 N3 C12 105.8(2) . . ? C13 N3 Cd1 116.3(2) . 3_565 ? C12 N3 Cd1 137.44(19) . 3_565 ? C13 N4 C11 106.8(2) . . ? C13 N4 C5 125.4(2) . . ? C11 N4 C5 127.7(2) . . ? C7 O1 Cd1 94.14(18) . . ? C7 O2 Cd1 88.20(18) . . ? C17 O3 Cd1 99.16(18) . . ? C17 O4 Cd1 85.08(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.632 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.144 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 788704' #TrackingRef '- sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H30 Cd3 N8 O14, 2(H2O)' _chemical_formula_sum 'C42 H34 Cd3 N8 O16' _chemical_formula_weight 1247.94 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.254(3) _cell_length_b 9.984(5) _cell_length_c 13.965(5) _cell_angle_alpha 78.013(13) _cell_angle_beta 87.68(4) _cell_angle_gamma 69.43(2) _cell_volume 1053.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3915 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.785 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5333 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3735 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3735 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.2172(4) 0.8690(4) 0.2958(2) 0.0258(7) Uani 1 1 d . . . C2 C 0.2649(5) 0.7378(4) 0.3639(2) 0.0294(8) Uani 1 1 d . . . H2A H 0.3110 0.7315 0.4250 0.035 Uiso 1 1 calc R . . C3 C 0.2437(4) 0.6153(4) 0.3409(2) 0.0274(7) Uani 1 1 d . . . C4 C 0.1743(4) 0.6235(4) 0.2521(2) 0.0275(7) Uani 1 1 d . . . H4A H 0.1617 0.5416 0.2363 0.033 Uiso 1 1 calc R . . C5 C 0.1224(4) 0.7573(4) 0.1850(2) 0.0241(7) Uani 1 1 d . . . C6 C 0.1427(4) 0.8803(4) 0.2053(2) 0.0257(7) Uani 1 1 d . . . H6A H 0.1076 0.9683 0.1598 0.031 Uiso 1 1 calc R . . C7 C 0.2540(4) 0.9968(4) 0.3200(2) 0.0269(7) Uani 1 1 d . . . C8 C 0.2775(6) 0.4663(4) 0.5128(3) 0.0425(10) Uani 1 1 d . . . H9A H 0.2367 0.5414 0.5471 0.051 Uiso 1 1 calc R . . C9 C 0.3342(6) 0.3219(4) 0.5510(3) 0.0424(10) Uani 1 1 d . . . H8A H 0.3399 0.2803 0.6174 0.051 Uiso 1 1 calc R . . C10 C 0.3550(5) 0.3445(4) 0.3960(3) 0.0352(9) Uani 1 1 d . . . H7A H 0.3768 0.3227 0.3341 0.042 Uiso 1 1 calc R . . C11 C 0.0885(5) 0.6520(4) 0.0431(3) 0.0303(8) Uani 1 1 d . . . H12A H 0.1843 0.5660 0.0558 0.036 Uiso 1 1 calc R . . C12 C -0.0330(5) 0.6928(4) -0.0286(2) 0.0301(8) Uani 1 1 d . . . H11A H -0.0348 0.6386 -0.0750 0.036 Uiso 1 1 calc R . . C13 C -0.1055(4) 0.8664(4) 0.0514(2) 0.0235(7) Uani 1 1 d . . . H10A H -0.1641 0.9531 0.0722 0.028 Uiso 1 1 calc R . . C14 C 0.6375(4) 0.6327(4) 0.1645(3) 0.0266(7) Uani 1 1 d . . . C15 C 0.7845(5) 0.5725(4) 0.2267(2) 0.0298(8) Uani 1 1 d . . . H32A H 0.8318 0.6340 0.2476 0.036 Uiso 1 1 calc R . . C16 C 0.8610(5) 0.4226(4) 0.2579(3) 0.0348(8) Uani 1 1 d . . . H31A H 0.9619 0.3836 0.2971 0.042 Uiso 1 1 calc R . . C17 C 0.7870(5) 0.3308(4) 0.2305(3) 0.0329(8) Uani 1 1 d . . . H30A H 0.8370 0.2301 0.2524 0.040 Uiso 1 1 calc R . . C18 C 0.6382(4) 0.3889(3) 0.1706(2) 0.0258(7) Uani 1 1 d . . . C19 C 0.5658(4) 0.5392(3) 0.1352(2) 0.0249(7) Uani 1 1 d . . . H28A H 0.4699 0.5773 0.0921 0.030 Uiso 1 1 calc R . . C20 C 0.5561(5) 0.7937(4) 0.1335(3) 0.0312(8) Uani 1 1 d . . . C21 C 0.5514(5) 0.2893(4) 0.1467(3) 0.0292(8) Uani 1 1 d . . . Cd1 Cd 0.5000 1.0000 0.5000 0.02989(13) Uani 1 2 d S . . Cd2 Cd 0.41144(3) 1.09757(2) 0.105515(17) 0.02499(11) Uani 1 1 d . . . N1 N 0.3824(4) 0.2456(3) 0.4775(2) 0.0353(7) Uani 1 1 d . . . N2 N 0.2916(4) 0.4812(3) 0.4124(2) 0.0303(7) Uani 1 1 d . . . N3 N -0.1551(4) 0.8273(3) -0.0233(2) 0.0266(6) Uani 1 1 d . . . N4 N 0.0428(4) 0.7631(3) 0.09407(19) 0.0245(6) Uani 1 1 d . . . O1 O 0.2595(4) 1.0994(3) 0.25264(18) 0.0354(6) Uani 1 1 d . . . O2 O 0.2767(4) 0.9888(3) 0.41025(18) 0.0352(6) Uani 1 1 d . . . O3 O 0.4659(4) 0.8520(3) 0.0541(2) 0.0377(6) Uani 1 1 d . . . O4 O 0.5807(4) 0.8695(3) 0.1897(2) 0.0426(7) Uani 1 1 d . . . O5 O 0.4005(3) 0.3408(3) 0.1116(2) 0.0383(6) Uani 1 1 d . . . O6 O 0.6353(4) 0.1523(3) 0.1656(2) 0.0403(7) Uani 1 1 d . . . O7 O 0.3158(5) 0.9879(4) 0.6347(2) 0.0578(9) Uani 1 1 d . . . O8 O 0.9342(15) 0.1312(14) 0.4598(8) 0.361(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 C1 0.0246(17) 0.0285(18) 0.0253(17) -0.0060(14) -0.0022(13) -0.0101(14) C2 0.035(2) 0.0292(19) 0.0232(17) -0.0047(14) -0.0070(15) -0.0104(16) C3 0.0271(17) 0.0244(17) 0.0286(17) 0.0005(14) -0.0039(14) -0.0093(14) C4 0.0283(18) 0.0212(17) 0.0322(18) -0.0040(14) -0.0018(14) -0.0081(14) C5 0.0219(16) 0.0278(17) 0.0224(16) -0.0037(13) -0.0043(13) -0.0086(14) C6 0.0275(17) 0.0261(17) 0.0225(16) -0.0025(13) -0.0024(14) -0.0091(14) C7 0.0264(18) 0.0302(19) 0.0264(18) -0.0089(15) -0.0025(14) -0.0103(15) C8 0.067(3) 0.032(2) 0.0255(19) -0.0065(16) 0.0005(19) -0.012(2) C9 0.064(3) 0.033(2) 0.0248(19) -0.0006(16) -0.0057(18) -0.012(2) C10 0.046(2) 0.0266(19) 0.0286(18) -0.0033(15) -0.0022(17) -0.0088(17) C11 0.0284(18) 0.0239(18) 0.0347(19) -0.0107(15) -0.0060(15) -0.0009(15) C12 0.0336(19) 0.0282(18) 0.0295(18) -0.0114(15) -0.0023(15) -0.0086(15) C13 0.0239(17) 0.0236(17) 0.0230(16) -0.0029(13) -0.0048(13) -0.0090(14) C14 0.0278(18) 0.0234(18) 0.0306(18) -0.0062(14) 0.0067(15) -0.0116(15) C15 0.0330(19) 0.0299(19) 0.0316(18) -0.0074(15) -0.0014(15) -0.0164(16) C16 0.0304(19) 0.033(2) 0.040(2) -0.0065(16) -0.0070(16) -0.0104(16) C17 0.033(2) 0.0206(17) 0.042(2) -0.0018(15) -0.0064(16) -0.0078(15) C18 0.0284(18) 0.0214(17) 0.0284(17) -0.0064(14) 0.0013(14) -0.0090(14) C19 0.0255(17) 0.0216(16) 0.0283(17) -0.0041(13) -0.0004(14) -0.0098(14) C20 0.0288(19) 0.0224(18) 0.042(2) -0.0045(16) 0.0095(17) -0.0113(15) C21 0.034(2) 0.0226(17) 0.0303(18) -0.0018(14) -0.0012(15) -0.0114(15) Cd1 0.0407(2) 0.0218(2) 0.0261(2) -0.00140(15) -0.01080(16) -0.01033(17) Cd2 0.02730(17) 0.02133(16) 0.02603(16) -0.00388(10) -0.00793(10) -0.00776(11) N1 0.0470(19) 0.0261(16) 0.0282(16) 0.0010(13) -0.0101(14) -0.0098(15) N2 0.0377(17) 0.0258(15) 0.0246(14) -0.0019(12) -0.0059(13) -0.0088(13) N3 0.0269(15) 0.0264(15) 0.0253(14) -0.0042(12) -0.0065(12) -0.0078(12) N4 0.0258(14) 0.0259(15) 0.0219(13) -0.0047(11) -0.0059(11) -0.0086(12) O1 0.0504(16) 0.0281(14) 0.0294(13) -0.0073(11) 0.0027(12) -0.0154(12) O2 0.0473(16) 0.0353(15) 0.0270(13) -0.0080(11) -0.0073(11) -0.0176(13) O3 0.0379(15) 0.0248(13) 0.0417(16) 0.0015(12) 0.0030(13) -0.0051(12) O4 0.0447(16) 0.0229(13) 0.0625(18) -0.0139(13) -0.0002(14) -0.0118(12) O5 0.0351(15) 0.0286(14) 0.0523(17) -0.0100(12) -0.0090(13) -0.0104(12) O6 0.0454(16) 0.0193(13) 0.0561(17) -0.0055(12) -0.0126(13) -0.0110(12) O7 0.066(2) 0.066(2) 0.0363(16) 0.0003(15) 0.0030(15) -0.0239(18) O8 0.292(14) 0.308(15) 0.316(14) 0.047(11) 0.205(12) 0.016(11) _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 C1 C2 1.388(5) . ? C1 C6 1.394(4) . ? C1 C7 1.514(5) . ? C2 C3 1.395(5) . ? C2 H2A 0.9300 . ? C3 C4 1.362(5) . ? C3 N2 1.432(4) . ? C4 C5 1.398(5) . ? C4 H4A 0.9300 . ? C5 C6 1.382(5) . ? C5 N4 1.434(4) . ? C6 H6A 0.9300 . ? C7 O1 1.251(4) . ? C7 O2 1.264(4) . ? C8 C9 1.344(5) . ? C8 N2 1.383(5) . ? C8 H9A 0.9300 . ? C9 N1 1.367(5) . ? C9 H8A 0.9300 . ? C10 N1 1.312(5) . ? C10 N2 1.345(5) . ? C10 H7A 0.9300 . ? C11 C12 1.342(5) . ? C11 N4 1.375(4) . ? C11 H12A 0.9300 . ? C12 N3 1.382(4) . ? C12 H11A 0.9300 . ? C13 N3 1.313(4) . ? C13 N4 1.354(4) . ? C13 H10A 0.9300 . ? C14 C15 1.395(5) . ? C14 C19 1.398(5) . ? C14 C20 1.483(5) . ? C15 C16 1.384(5) . ? C15 H32A 0.9300 . ? C16 C17 1.385(5) . ? C16 H31A 0.9300 . ? C17 C18 1.388(5) . ? C17 H30A 0.9300 . ? C18 C19 1.393(5) . ? C18 C21 1.507(5) . ? C19 H28A 0.9300 . ? C20 O4 1.263(4) . ? C20 O3 1.272(5) . ? C21 O5 1.246(4) . ? C21 O6 1.273(4) . ? C21 Cd2 2.720(4) 1_545 ? Cd1 N1 2.255(3) 2_666 ? Cd1 N1 2.255(3) 1_565 ? Cd1 O2 2.317(3) 2_676 ? Cd1 O2 2.317(3) . ? Cd1 O7 2.380(3) . ? Cd1 O7 2.380(3) 2_676 ? Cd2 N3 2.254(3) 2_575 ? Cd2 O4 2.303(3) . ? Cd2 O6 2.333(3) 1_565 ? Cd2 O1 2.363(3) . ? Cd2 O5 2.417(3) 1_565 ? Cd2 O3 2.441(3) 2_675 ? Cd2 O3 2.581(3) . ? Cd2 C21 2.720(4) 1_565 ? N1 Cd1 2.255(3) 1_545 ? N3 Cd2 2.254(3) 2_575 ? O3 Cd2 2.441(3) 2_675 ? O5 Cd2 2.417(3) 1_545 ? O6 Cd2 2.333(3) 1_545 ? 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 C2 C1 C6 120.1(3) . . ? C2 C1 C7 118.9(3) . . ? C6 C1 C7 120.9(3) . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 N2 120.0(3) . . ? C2 C3 N2 119.5(3) . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 122.0(3) . . ? C6 C5 N4 120.8(3) . . ? C4 C5 N4 117.2(3) . . ? C5 C6 C1 118.3(3) . . ? C5 C6 H6A 120.8 . . ? C1 C6 H6A 120.8 . . ? O1 C7 O2 125.3(3) . . ? O1 C7 C1 119.9(3) . . ? O2 C7 C1 114.8(3) . . ? C9 C8 N2 106.6(3) . . ? C9 C8 H9A 126.7 . . ? N2 C8 H9A 126.7 . . ? C8 C9 N1 109.8(3) . . ? C8 C9 H8A 125.1 . . ? N1 C9 H8A 125.1 . . ? N1 C10 N2 112.0(3) . . ? N1 C10 H7A 124.0 . . ? N2 C10 H7A 124.0 . . ? C12 C11 N4 106.1(3) . . ? C12 C11 H12A 127.0 . . ? N4 C11 H12A 127.0 . . ? C11 C12 N3 109.9(3) . . ? C11 C12 H11A 125.1 . . ? N3 C12 H11A 125.1 . . ? N3 C13 N4 110.6(3) . . ? N3 C13 H10A 124.7 . . ? N4 C13 H10A 124.7 . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C20 119.9(3) . . ? C19 C14 C20 121.1(3) . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H32A 119.6 . . ? C14 C15 H32A 119.6 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H31A 120.1 . . ? C17 C16 H31A 120.1 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H30A 120.0 . . ? C18 C17 H30A 120.0 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 C21 119.8(3) . . ? C19 C18 C21 119.9(3) . . ? C18 C19 C14 119.9(3) . . ? C18 C19 H28A 120.1 . . ? C14 C19 H28A 120.1 . . ? O4 C20 O3 121.9(3) . . ? O4 C20 C14 116.8(3) . . ? O3 C20 C14 121.2(3) . . ? O5 C21 O6 121.6(3) . . ? O5 C21 C18 120.3(3) . . ? O6 C21 C18 118.1(3) . . ? O5 C21 Cd2 62.70(19) . 1_545 ? O6 C21 Cd2 58.89(18) . 1_545 ? C18 C21 Cd2 176.9(2) . 1_545 ? N1 Cd1 N1 180.00(16) 2_666 1_565 ? N1 Cd1 O2 92.18(11) 2_666 2_676 ? N1 Cd1 O2 87.82(11) 1_565 2_676 ? N1 Cd1 O2 87.82(11) 2_666 . ? N1 Cd1 O2 92.18(11) 1_565 . ? O2 Cd1 O2 180.000(1) 2_676 . ? N1 Cd1 O7 92.48(12) 2_666 . ? N1 Cd1 O7 87.52(12) 1_565 . ? O2 Cd1 O7 95.42(11) 2_676 . ? O2 Cd1 O7 84.58(11) . . ? N1 Cd1 O7 87.52(12) 2_666 2_676 ? N1 Cd1 O7 92.48(12) 1_565 2_676 ? O2 Cd1 O7 84.58(11) 2_676 2_676 ? O2 Cd1 O7 95.42(11) . 2_676 ? O7 Cd1 O7 180.000(1) . 2_676 ? N3 Cd2 O4 130.78(10) 2_575 . ? N3 Cd2 O6 149.70(10) 2_575 1_565 ? O4 Cd2 O6 79.44(10) . 1_565 ? N3 Cd2 O1 88.26(10) 2_575 . ? O4 Cd2 O1 82.36(10) . . ? O6 Cd2 O1 94.83(10) 1_565 . ? N3 Cd2 O5 95.10(10) 2_575 1_565 ? O4 Cd2 O5 132.20(9) . 1_565 ? O6 Cd2 O5 55.10(9) 1_565 1_565 ? O1 Cd2 O5 87.15(9) . 1_565 ? N3 Cd2 O3 86.20(10) 2_575 2_675 ? O4 Cd2 O3 108.86(10) . 2_675 ? O6 Cd2 O3 84.98(10) 1_565 2_675 ? O1 Cd2 O3 168.48(9) . 2_675 ? O5 Cd2 O3 83.30(9) 1_565 2_675 ? N3 Cd2 O3 85.17(10) 2_575 . ? O4 Cd2 O3 53.60(10) . . ? O6 Cd2 O3 121.71(9) 1_565 . ? O1 Cd2 O3 108.89(9) . . ? O5 Cd2 O3 163.96(9) 1_565 . ? O3 Cd2 O3 80.71(9) 2_675 . ? N3 Cd2 C21 122.11(11) 2_575 1_565 ? O4 Cd2 C21 106.43(11) . 1_565 ? O6 Cd2 C21 27.85(10) 1_565 1_565 ? O1 Cd2 C21 91.62(10) . 1_565 ? O5 Cd2 C21 27.26(10) 1_565 1_565 ? O3 Cd2 C21 82.82(10) 2_675 1_565 ? O3 Cd2 C21 146.94(10) . 1_565 ? C10 N1 C9 105.7(3) . . ? C10 N1 Cd1 129.2(3) . 1_545 ? C9 N1 Cd1 125.0(2) . 1_545 ? C10 N2 C8 105.9(3) . . ? C10 N2 C3 127.3(3) . . ? C8 N2 C3 126.7(3) . . ? C13 N3 C12 106.0(3) . . ? C13 N3 Cd2 132.3(2) . 2_575 ? C12 N3 Cd2 119.2(2) . 2_575 ? C13 N4 C11 107.4(3) . . ? C13 N4 C5 126.6(3) . . ? C11 N4 C5 125.2(3) . . ? C7 O1 Cd2 130.9(2) . . ? C7 O2 Cd1 132.7(2) . . ? C20 O3 Cd2 123.7(2) . 2_675 ? C20 O3 Cd2 85.7(2) . . ? Cd2 O3 Cd2 99.29(9) 2_675 . ? C20 O4 Cd2 98.7(2) . . ? C21 O5 Cd2 90.0(2) . 1_545 ? C21 O6 Cd2 93.3(2) . 1_545 ? 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 C6 C1 C2 C3 2.1(5) . . . . ? C7 C1 C2 C3 -175.5(3) . . . . ? C1 C2 C3 C4 -0.8(5) . . . . ? C1 C2 C3 N2 -179.3(3) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? N2 C3 C4 C5 177.6(3) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C3 C4 C5 N4 -177.2(3) . . . . ? C4 C5 C6 C1 -0.1(5) . . . . ? N4 C5 C6 C1 178.5(3) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? C7 C1 C6 C5 175.9(3) . . . . ? C2 C1 C7 O1 159.5(3) . . . . ? C6 C1 C7 O1 -18.0(5) . . . . ? C2 C1 C7 O2 -20.6(5) . . . . ? C6 C1 C7 O2 161.8(3) . . . . ? N2 C8 C9 N1 -0.5(5) . . . . ? N4 C11 C12 N3 -0.4(4) . . . . ? C19 C14 C15 C16 1.2(5) . . . . ? C20 C14 C15 C16 178.9(3) . . . . ? C14 C15 C16 C17 -2.8(6) . . . . ? C15 C16 C17 C18 1.2(6) . . . . ? C16 C17 C18 C19 2.1(5) . . . . ? C16 C17 C18 C21 -175.9(3) . . . . ? C17 C18 C19 C14 -3.6(5) . . . . ? C21 C18 C19 C14 174.3(3) . . . . ? C15 C14 C19 C18 2.0(5) . . . . ? C20 C14 C19 C18 -175.7(3) . . . . ? C15 C14 C20 O4 -25.1(5) . . . . ? C19 C14 C20 O4 152.5(3) . . . . ? C15 C14 C20 O3 154.9(3) . . . . ? C19 C14 C20 O3 -27.4(5) . . . . ? C17 C18 C21 O5 164.5(3) . . . . ? C19 C18 C21 O5 -13.4(5) . . . . ? C17 C18 C21 O6 -13.9(5) . . . . ? C19 C18 C21 O6 168.1(3) . . . . ? N2 C10 N1 C9 0.0(5) . . . . ? N2 C10 N1 Cd1 -176.2(3) . . . 1_545 ? C8 C9 N1 C10 0.3(5) . . . . ? C8 C9 N1 Cd1 176.7(3) . . . 1_545 ? N1 C10 N2 C8 -0.3(5) . . . . ? N1 C10 N2 C3 -178.7(3) . . . . ? C9 C8 N2 C10 0.5(5) . . . . ? C9 C8 N2 C3 178.9(4) . . . . ? C4 C3 N2 C10 34.0(6) . . . . ? C2 C3 N2 C10 -147.5(4) . . . . ? C4 C3 N2 C8 -144.0(4) . . . . ? C2 C3 N2 C8 34.5(6) . . . . ? N4 C13 N3 C12 0.1(4) . . . . ? N4 C13 N3 Cd2 161.5(2) . . . 2_575 ? C11 C12 N3 C13 0.2(4) . . . . ? C11 C12 N3 Cd2 -164.2(2) . . . 2_575 ? N3 C13 N4 C11 -0.3(4) . . . . ? N3 C13 N4 C5 -170.6(3) . . . . ? C12 C11 N4 C13 0.4(4) . . . . ? C12 C11 N4 C5 170.9(3) . . . . ? C6 C5 N4 C13 -46.6(5) . . . . ? C4 C5 N4 C13 132.0(3) . . . . ? C6 C5 N4 C11 144.8(3) . . . . ? C4 C5 N4 C11 -36.6(5) . . . . ? O2 C7 O1 Cd2 129.9(3) . . . . ? C1 C7 O1 Cd2 -50.3(5) . . . . ? N3 Cd2 O1 C7 110.5(3) 2_575 . . . ? O4 Cd2 O1 C7 -21.0(3) . . . . ? O6 Cd2 O1 C7 -99.7(3) 1_565 . . . ? O5 Cd2 O1 C7 -154.3(3) 1_565 . . . ? O3 Cd2 O1 C7 171.8(4) 2_675 . . . ? O3 Cd2 O1 C7 26.2(3) . . . . ? C21 Cd2 O1 C7 -127.4(3) 1_565 . . . ? O1 C7 O2 Cd1 -55.1(5) . . . . ? C1 C7 O2 Cd1 125.0(3) . . . . ? N1 Cd1 O2 C7 -91.7(3) 2_666 . . . ? N1 Cd1 O2 C7 88.3(3) 1_565 . . . ? O7 Cd1 O2 C7 175.6(3) . . . . ? O7 Cd1 O2 C7 -4.4(3) 2_676 . . . ? O4 C20 O3 Cd2 95.4(4) . . . 2_675 ? C14 C20 O3 Cd2 -84.6(4) . . . 2_675 ? O4 C20 O3 Cd2 -2.8(3) . . . . ? C14 C20 O3 Cd2 177.1(3) . . . . ? N3 Cd2 O3 C20 -149.6(2) 2_575 . . . ? O4 Cd2 O3 C20 1.6(2) . . . . ? O6 Cd2 O3 C20 45.3(2) 1_565 . . . ? O1 Cd2 O3 C20 -63.1(2) . . . . ? O5 Cd2 O3 C20 118.8(3) 1_565 . . . ? O3 Cd2 O3 C20 123.5(2) 2_675 . . . ? C21 Cd2 O3 C20 62.4(3) 1_565 . . . ? N3 Cd2 O3 Cd2 86.93(11) 2_575 . . 2_675 ? O4 Cd2 O3 Cd2 -121.84(14) . . . 2_675 ? O6 Cd2 O3 Cd2 -78.16(13) 1_565 . . 2_675 ? O1 Cd2 O3 Cd2 173.43(9) . . . 2_675 ? O5 Cd2 O3 Cd2 -4.7(4) 1_565 . . 2_675 ? O3 Cd2 O3 Cd2 0.0 2_675 . . 2_675 ? C21 Cd2 O3 Cd2 -61.1(2) 1_565 . . 2_675 ? O3 C20 O4 Cd2 3.2(4) . . . . ? C14 C20 O4 Cd2 -176.7(3) . . . . ? N3 Cd2 O4 C20 37.6(3) 2_575 . . . ? O6 Cd2 O4 C20 -145.0(2) 1_565 . . . ? O1 Cd2 O4 C20 118.6(2) . . . . ? O5 Cd2 O4 C20 -162.3(2) 1_565 . . . ? O3 Cd2 O4 C20 -64.0(2) 2_675 . . . ? O3 Cd2 O4 C20 -1.7(2) . . . . ? C21 Cd2 O4 C20 -151.9(2) 1_565 . . . ? O6 C21 O5 Cd2 -2.2(4) . . . 1_545 ? C18 C21 O5 Cd2 179.5(3) . . . 1_545 ? O5 C21 O6 Cd2 2.2(4) . . . 1_545 ? C18 C21 O6 Cd2 -179.3(3) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.218 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.115 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 788705' #TrackingRef '- sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 Cd2 N4 O9, H2 O' _chemical_formula_sum 'C22 H16 Cd2 N4 O10' _chemical_formula_weight 721.19 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 10.5555(7) _cell_length_b 10.755(1) _cell_length_c 10.9889(8) _cell_angle_alpha 70.527(10) _cell_angle_beta 81.613(2) _cell_angle_gamma 85.3430(10) _cell_volume 1162.86(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4246 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5780 _exptl_absorpt_correction_T_max 0.6491 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6020 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -12 _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 9 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4142 _reflns_number_gt 3622 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4142 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 C1 C 0.5515(3) 0.4013(3) 0.3818(3) 0.0218(7) Uani 1 1 d . . . C2 C 0.6019(3) 0.4922(3) 0.2658(3) 0.0248(7) Uani 1 1 d . . . H2 H 0.6901 0.4988 0.2435 0.030 Uiso 1 1 calc R . . C3 C 0.5196(3) 0.5731(3) 0.1834(3) 0.0241(7) Uani 1 1 d . . . C4 C 0.3881(3) 0.5662(3) 0.2155(3) 0.0274(8) Uani 1 1 d . . . H4 H 0.3332 0.6201 0.1592 0.033 Uiso 1 1 calc R . . C5 C 0.3400(3) 0.4766(3) 0.3339(3) 0.0249(7) Uani 1 1 d . . . C6 C 0.4200(3) 0.3967(3) 0.4165(3) 0.0245(7) Uani 1 1 d . . . H6 H 0.3862 0.3390 0.4963 0.029 Uiso 1 1 calc R . . C7 C 0.6371(3) 0.2975(3) 0.4635(3) 0.0238(7) Uani 1 1 d . . . C8 C 0.6756(4) 0.6225(3) -0.0177(3) 0.0334(8) Uani 1 1 d . . . H8 H 0.7246 0.5441 0.0030 0.040 Uiso 1 1 calc R . . C9 C 0.6921(4) 0.7268(4) -0.1279(4) 0.0364(9) Uani 1 1 d . . . H9 H 0.7559 0.7321 -0.1972 0.044 Uiso 1 1 calc R . . C10 C 0.5305(3) 0.7777(3) -0.0095(3) 0.0252(7) Uani 1 1 d . . . H10 H 0.4612 0.8235 0.0204 0.030 Uiso 1 1 calc R . . C11 C 0.1063(4) 0.5408(4) 0.3226(4) 0.0463(11) Uani 1 1 d . . . H11 H 0.1111 0.6309 0.2787 0.056 Uiso 1 1 calc R . . C12 C -0.0001(4) 0.4704(4) 0.3591(4) 0.0448(11) Uani 1 1 d . . . H12 H -0.0824 0.5043 0.3443 0.054 Uiso 1 1 calc R . . C13 C 0.1557(3) 0.3335(3) 0.4227(3) 0.0271(8) Uani 1 1 d . . . H13 H 0.2029 0.2566 0.4595 0.032 Uiso 1 1 calc R . . C14 C 1.1846(3) 1.0933(3) -0.1888(3) 0.0224(7) Uani 1 1 d . . . C15 C 1.0735(3) 1.0611(3) -0.2261(3) 0.0197(7) Uani 1 1 d . . . C16 C 0.9529(3) 1.1020(3) -0.1771(3) 0.0202(7) Uani 1 1 d . . . C17 C 0.9461(3) 1.1690(3) -0.0867(3) 0.0249(7) Uani 1 1 d . . . H17 H 0.8664 1.1930 -0.0509 0.030 Uiso 1 1 calc R . . C18 C 1.0547(3) 1.1996(3) -0.0501(3) 0.0289(8) Uani 1 1 d . . . H18 H 1.0486 1.2445 0.0098 0.035 Uiso 1 1 calc R . . C19 C 1.1728(3) 1.1640(3) -0.1019(3) 0.0285(8) Uani 1 1 d . . . H19 H 1.2463 1.1876 -0.0786 0.034 Uiso 1 1 calc R . . C20 C 1.3189(3) 1.0521(3) -0.2349(3) 0.0246(7) Uani 1 1 d . . . C21 C 1.0840(3) 0.9796(3) -0.3166(3) 0.0219(7) Uani 1 1 d . . . C22 C 0.8288(3) 1.0813(3) -0.2176(3) 0.0217(7) Uani 1 1 d . . . Cd1 Cd 0.91125(2) 1.16285(2) -0.52130(2) 0.02035(9) Uani 1 1 d . . . Cd2 Cd 0.59620(2) 1.02440(2) -0.27848(2) 0.02257(9) Uani 1 1 d . . . N1 N 0.6015(3) 0.8236(3) -0.1229(3) 0.0291(7) Uani 1 1 d . . . N2 N 0.5718(3) 0.6558(3) 0.0572(3) 0.0248(6) Uani 1 1 d . . . N3 N 0.0315(3) 0.3403(3) 0.4216(3) 0.0301(7) Uani 1 1 d . . . N4 N 0.2061(3) 0.4545(3) 0.3624(3) 0.0286(7) Uani 1 1 d . . . O1 O 0.7529(2) 0.3178(2) 0.4515(3) 0.0356(6) Uani 1 1 d . . . O2 O 0.5836(3) 0.1928(3) 0.5333(3) 0.0470(7) Uani 1 1 d . . . O3 O 1.4094(2) 1.0955(3) -0.2006(3) 0.0435(7) Uani 1 1 d . . . O4 O 1.3341(2) 0.9782(3) -0.3028(3) 0.0362(6) Uani 1 1 d . . . O5 O 1.0989(2) 1.0395(2) -0.4385(2) 0.0237(5) Uani 1 1 d . . . O6 O 1.0748(2) 0.8580(2) -0.2700(2) 0.0307(6) Uani 1 1 d . . . O7 O 0.8302(2) 1.0422(2) -0.3160(2) 0.0255(5) Uani 1 1 d . . . O8 O 0.7253(2) 1.1038(3) -0.1566(2) 0.0356(6) Uani 1 1 d . . . O9 O 0.6180(3) 0.9062(3) -0.4259(3) 0.0333(6) Uani 1 1 d . . . H114 H 0.653(5) 0.940(5) -0.500(5) 0.069(18) Uiso 1 1 d . . . H113 H 0.555(6) 0.890(6) -0.433(5) 0.07(2) Uiso 1 1 d . . . O10 O 0.7330(4) 0.2953(4) 0.1096(4) 0.0608(10) Uani 1 1 d . . . H111 H 0.762(7) 0.236(7) 0.157(6) 0.08(2) Uiso 1 1 d . . . H112 H 0.801(12) 0.320(12) 0.118(11) 0.09(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0191(16) 0.0174(16) 0.0255(17) -0.0015(13) -0.0043(13) -0.0021(13) C2 0.0198(16) 0.0232(17) 0.0290(18) -0.0041(14) -0.0044(14) -0.0030(13) C3 0.0246(17) 0.0184(16) 0.0248(17) 0.0004(14) -0.0035(14) -0.0058(13) C4 0.0238(18) 0.0199(17) 0.0324(19) 0.0031(15) -0.0101(15) -0.0047(14) C5 0.0166(16) 0.0190(16) 0.0355(19) -0.0032(15) -0.0045(14) -0.0015(13) C6 0.0250(18) 0.0199(16) 0.0225(17) 0.0013(14) -0.0013(14) -0.0052(13) C7 0.0223(18) 0.0199(16) 0.0250(17) -0.0019(14) -0.0025(14) -0.0010(13) C8 0.041(2) 0.0249(18) 0.031(2) -0.0057(16) -0.0021(17) 0.0034(16) C9 0.042(2) 0.035(2) 0.0259(19) -0.0053(17) 0.0010(17) 0.0014(17) C10 0.0223(17) 0.0232(17) 0.0264(18) -0.0018(14) -0.0065(14) -0.0013(13) C11 0.028(2) 0.0234(19) 0.071(3) 0.0085(19) -0.012(2) 0.0004(16) C12 0.0196(18) 0.030(2) 0.070(3) 0.004(2) -0.0102(19) -0.0006(15) C13 0.0188(17) 0.0193(17) 0.036(2) 0.0008(15) -0.0039(14) -0.0038(13) C14 0.0193(16) 0.0233(17) 0.0219(17) -0.0030(14) -0.0041(13) -0.0016(13) C15 0.0181(16) 0.0169(15) 0.0191(16) 0.0007(13) -0.0022(13) -0.0008(12) C16 0.0191(16) 0.0162(15) 0.0210(16) -0.0001(13) -0.0033(13) -0.0004(12) C17 0.0217(17) 0.0256(17) 0.0250(17) -0.0072(14) 0.0003(14) 0.0031(13) C18 0.0281(19) 0.0323(19) 0.0305(19) -0.0161(16) -0.0031(15) 0.0000(15) C19 0.0230(17) 0.0336(19) 0.0317(19) -0.0116(16) -0.0079(15) -0.0050(15) C20 0.0189(17) 0.0282(18) 0.0205(17) 0.0004(15) -0.0031(13) 0.0004(14) C21 0.0106(15) 0.0263(18) 0.0283(18) -0.0072(15) -0.0064(13) 0.0021(12) C22 0.0188(16) 0.0165(16) 0.0234(17) 0.0021(13) -0.0024(13) -0.0016(12) Cd1 0.01648(13) 0.01938(14) 0.02262(14) -0.00333(10) -0.00237(10) -0.00141(9) Cd2 0.01681(14) 0.02195(14) 0.02254(14) 0.00148(10) -0.00245(10) -0.00193(9) N1 0.0346(17) 0.0244(15) 0.0220(15) 0.0006(12) -0.0022(13) -0.0024(13) N2 0.0254(15) 0.0199(14) 0.0231(14) 0.0019(12) -0.0043(12) -0.0033(11) N3 0.0201(15) 0.0198(14) 0.0445(18) -0.0028(13) -0.0036(13) -0.0018(11) N4 0.0175(14) 0.0199(14) 0.0396(17) 0.0018(13) -0.0024(13) -0.0025(11) O1 0.0185(12) 0.0268(13) 0.0507(16) 0.0017(12) -0.0061(11) 0.0021(10) O2 0.0331(15) 0.0342(15) 0.0525(17) 0.0199(13) -0.0165(13) -0.0077(12) O3 0.0154(12) 0.0662(19) 0.0604(18) -0.0355(16) -0.0048(12) -0.0019(12) O4 0.0249(13) 0.0464(15) 0.0399(15) -0.0196(13) -0.0024(11) 0.0059(11) O5 0.0206(11) 0.0268(12) 0.0213(12) -0.0046(10) -0.0027(9) -0.0011(9) O6 0.0373(14) 0.0209(13) 0.0324(14) -0.0065(11) -0.0055(11) -0.0005(10) O7 0.0193(11) 0.0312(13) 0.0235(12) -0.0048(10) -0.0018(9) -0.0063(10) O8 0.0141(12) 0.0532(16) 0.0440(15) -0.0234(13) -0.0008(11) -0.0002(11) O9 0.0309(16) 0.0334(15) 0.0331(16) -0.0070(13) -0.0034(13) -0.0046(12) O10 0.078(3) 0.043(2) 0.057(2) -0.0102(18) -0.0193(19) 0.0174(19) _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 C1 C6 1.385(4) . ? C1 C2 1.386(4) . ? C1 C7 1.507(4) . ? C2 C3 1.383(5) . ? C2 H2 0.9300 . ? C3 C4 1.383(5) . ? C3 N2 1.433(4) . ? C4 C5 1.389(4) . ? C4 H4 0.9300 . ? C5 C6 1.364(5) . ? C5 N4 1.424(4) . ? C6 H6 0.9300 . ? C7 O1 1.240(4) . ? C7 O2 1.256(4) . ? C8 C9 1.349(5) . ? C8 N2 1.371(4) . ? C8 H8 0.9300 . ? C9 N1 1.365(5) . ? C9 H9 0.9300 . ? C10 N1 1.317(4) . ? C10 N2 1.343(4) . ? C10 H10 0.9300 . ? C11 C12 1.341(5) . ? C11 N4 1.367(5) . ? C11 H11 0.9300 . ? C12 N3 1.375(5) . ? C12 H12 0.9300 . ? C13 N3 1.308(4) . ? C13 N4 1.361(4) . ? C13 H13 0.9300 . ? C14 C19 1.393(5) . ? C14 C15 1.401(4) . ? C14 C20 1.516(4) . ? C15 C16 1.404(4) . ? C15 C21 1.518(5) . ? C16 C17 1.400(5) . ? C16 C22 1.499(4) . ? C17 C18 1.367(5) . ? C17 H17 0.9300 . ? C18 C19 1.374(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O4 1.248(4) . ? C20 O3 1.252(4) . ? C21 O6 1.241(4) . ? C21 O5 1.270(4) . ? C21 Cd1 2.702(3) 2_774 ? C22 O8 1.246(4) . ? C22 O7 1.281(4) . ? Cd1 N3 2.238(3) 1_664 ? Cd1 O1 2.241(2) 1_564 ? Cd1 O7 2.274(2) . ? Cd1 O6 2.360(2) 2_774 ? Cd1 O5 2.375(2) 2_774 ? Cd1 O5 2.409(2) . ? Cd1 C21 2.702(3) 2_774 ? Cd2 O3 2.215(2) 1_455 ? Cd2 O2 2.263(2) 1_564 ? Cd2 N1 2.266(3) . ? Cd2 O9 2.348(3) . ? Cd2 O7 2.457(2) . ? N3 Cd1 2.238(3) 1_446 ? O1 Cd1 2.241(2) 1_546 ? O2 Cd2 2.263(2) 1_546 ? O3 Cd2 2.215(2) 1_655 ? O5 Cd1 2.375(2) 2_774 ? O6 Cd1 2.360(2) 2_774 ? O9 H114 0.82(5) . ? O9 H113 0.72(6) . ? O10 H111 0.75(7) . ? O10 H112 0.81(13) . ? 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 C6 C1 C2 119.7(3) . . ? C6 C1 C7 119.3(3) . . ? C2 C1 C7 120.6(3) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 121.3(3) . . ? C2 C3 N2 118.9(3) . . ? C4 C3 N2 119.5(3) . . ? C3 C4 C5 118.3(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 121.1(3) . . ? C6 C5 N4 118.7(3) . . ? C4 C5 N4 119.6(3) . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O1 C7 O2 125.6(3) . . ? O1 C7 C1 118.9(3) . . ? O2 C7 C1 115.3(3) . . ? C9 C8 N2 105.8(3) . . ? C9 C8 H8 127.1 . . ? N2 C8 H8 127.1 . . ? C8 C9 N1 110.1(3) . . ? C8 C9 H9 124.9 . . ? N1 C9 H9 124.9 . . ? N1 C10 N2 110.9(3) . . ? N1 C10 H10 124.6 . . ? N2 C10 H10 124.6 . . ? C12 C11 N4 106.8(3) . . ? C12 C11 H11 126.6 . . ? N4 C11 H11 126.6 . . ? C11 C12 N3 109.5(3) . . ? C11 C12 H12 125.3 . . ? N3 C12 H12 125.3 . . ? N3 C13 N4 110.6(3) . . ? N3 C13 H13 124.7 . . ? N4 C13 H13 124.7 . . ? C19 C14 C15 119.0(3) . . ? C19 C14 C20 117.3(3) . . ? C15 C14 C20 123.7(3) . . ? C14 C15 C16 119.7(3) . . ? C14 C15 C21 119.9(3) . . ? C16 C15 C21 120.4(3) . . ? C17 C16 C15 119.0(3) . . ? C17 C16 C22 116.9(3) . . ? C15 C16 C22 124.1(3) . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C14 121.2(3) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? O4 C20 O3 123.7(3) . . ? O4 C20 C14 119.8(3) . . ? O3 C20 C14 116.6(3) . . ? O6 C21 O5 122.3(3) . . ? O6 C21 C15 119.5(3) . . ? O5 C21 C15 118.2(3) . . ? O6 C21 Cd1 60.80(18) . 2_774 ? O5 C21 Cd1 61.48(17) . 2_774 ? C15 C21 Cd1 176.8(2) . 2_774 ? O8 C22 O7 120.6(3) . . ? O8 C22 C16 119.8(3) . . ? O7 C22 C16 119.6(3) . . ? N3 Cd1 O1 81.76(9) 1_664 1_564 ? N3 Cd1 O7 126.70(10) 1_664 . ? O1 Cd1 O7 95.36(8) 1_564 . ? N3 Cd1 O6 97.09(10) 1_664 2_774 ? O1 Cd1 O6 96.34(9) 1_564 2_774 ? O7 Cd1 O6 135.85(8) . 2_774 ? N3 Cd1 O5 141.36(9) 1_664 2_774 ? O1 Cd1 O5 123.70(8) 1_564 2_774 ? O7 Cd1 O5 83.04(8) . 2_774 ? O6 Cd1 O5 55.35(7) 2_774 2_774 ? N3 Cd1 O5 85.47(9) 1_664 . ? O1 Cd1 O5 158.25(9) 1_564 . ? O7 Cd1 O5 78.30(8) . . ? O6 Cd1 O5 102.68(8) 2_774 . ? O5 Cd1 O5 76.60(8) 2_774 . ? N3 Cd1 C21 120.16(10) 1_664 2_774 ? O1 Cd1 C21 112.28(10) 1_564 2_774 ? O7 Cd1 C21 110.15(9) . 2_774 ? O6 Cd1 C21 27.33(9) 2_774 2_774 ? O5 Cd1 C21 28.03(9) 2_774 2_774 ? O5 Cd1 C21 89.36(8) . 2_774 ? O3 Cd2 O2 88.31(11) 1_455 1_564 ? O3 Cd2 N1 97.03(11) 1_455 . ? O2 Cd2 N1 164.94(11) 1_564 . ? O3 Cd2 O9 123.58(10) 1_455 . ? O2 Cd2 O9 79.95(11) 1_564 . ? N1 Cd2 O9 85.39(10) . . ? O3 Cd2 O7 147.29(9) 1_455 . ? O2 Cd2 O7 88.83(8) 1_564 . ? N1 Cd2 O7 94.06(9) . . ? O9 Cd2 O7 87.86(10) . . ? C10 N1 C9 105.8(3) . . ? C10 N1 Cd2 130.3(2) . . ? C9 N1 Cd2 123.8(2) . . ? C10 N2 C8 107.4(3) . . ? C10 N2 C3 127.7(3) . . ? C8 N2 C3 124.9(3) . . ? C13 N3 C12 106.3(3) . . ? C13 N3 Cd1 123.5(2) . 1_446 ? C12 N3 Cd1 129.2(2) . 1_446 ? C13 N4 C11 106.8(3) . . ? C13 N4 C5 123.9(3) . . ? C11 N4 C5 128.8(3) . . ? C7 O1 Cd1 125.7(2) . 1_546 ? C7 O2 Cd2 141.6(2) . 1_546 ? C20 O3 Cd2 110.7(2) . 1_655 ? C21 O5 Cd1 90.49(19) . 2_774 ? C21 O5 Cd1 114.19(19) . . ? Cd1 O5 Cd1 103.40(8) 2_774 . ? C21 O6 Cd1 91.9(2) . 2_774 ? C22 O7 Cd1 123.00(18) . . ? C22 O7 Cd2 91.53(18) . . ? Cd1 O7 Cd2 115.19(9) . . ? Cd2 O9 H114 119(4) . . ? Cd2 O9 H113 108(5) . . ? H114 O9 H113 105(5) . . ? H111 O10 H112 75(9) . . ? 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 C6 C1 C2 C3 -3.0(5) . . . . ? C7 C1 C2 C3 170.3(3) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? C1 C2 C3 N2 -172.8(3) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? N2 C3 C4 C5 174.4(3) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C3 C4 C5 N4 -171.8(3) . . . . ? C4 C5 C6 C1 -1.7(5) . . . . ? N4 C5 C6 C1 169.8(3) . . . . ? C2 C1 C6 C5 3.4(5) . . . . ? C7 C1 C6 C5 -170.0(3) . . . . ? C6 C1 C7 O1 -163.5(3) . . . . ? C2 C1 C7 O1 23.3(5) . . . . ? C6 C1 C7 O2 20.8(5) . . . . ? C2 C1 C7 O2 -152.5(3) . . . . ? N2 C8 C9 N1 0.1(4) . . . . ? N4 C11 C12 N3 0.0(5) . . . . ? C19 C14 C15 C16 0.9(5) . . . . ? C20 C14 C15 C16 179.1(3) . . . . ? C19 C14 C15 C21 -177.7(3) . . . . ? C20 C14 C15 C21 0.6(5) . . . . ? C14 C15 C16 C17 -3.0(4) . . . . ? C21 C15 C16 C17 175.5(3) . . . . ? C14 C15 C16 C22 175.6(3) . . . . ? C21 C15 C16 C22 -5.9(5) . . . . ? C15 C16 C17 C18 2.8(5) . . . . ? C22 C16 C17 C18 -175.9(3) . . . . ? C16 C17 C18 C19 -0.3(5) . . . . ? C17 C18 C19 C14 -2.0(5) . . . . ? C15 C14 C19 C18 1.7(5) . . . . ? C20 C14 C19 C18 -176.7(3) . . . . ? C19 C14 C20 O4 173.3(3) . . . . ? C15 C14 C20 O4 -5.0(5) . . . . ? C19 C14 C20 O3 -6.5(5) . . . . ? C15 C14 C20 O3 175.3(3) . . . . ? C14 C15 C21 O6 94.1(4) . . . . ? C16 C15 C21 O6 -84.4(4) . . . . ? C14 C15 C21 O5 -87.6(4) . . . . ? C16 C15 C21 O5 93.9(4) . . . . ? C17 C16 C22 O8 -11.4(4) . . . . ? C15 C16 C22 O8 170.0(3) . . . . ? C17 C16 C22 O7 167.7(3) . . . . ? C15 C16 C22 O7 -10.9(4) . . . . ? N2 C10 N1 C9 -0.3(4) . . . . ? N2 C10 N1 Cd2 -175.5(2) . . . . ? C8 C9 N1 C10 0.1(4) . . . . ? C8 C9 N1 Cd2 175.7(2) . . . . ? O3 Cd2 N1 C10 -12.9(3) 1_455 . . . ? O2 Cd2 N1 C10 -123.1(4) 1_564 . . . ? O9 Cd2 N1 C10 -136.3(3) . . . . ? O7 Cd2 N1 C10 136.2(3) . . . . ? O3 Cd2 N1 C9 172.7(3) 1_455 . . . ? O2 Cd2 N1 C9 62.5(5) 1_564 . . . ? O9 Cd2 N1 C9 49.3(3) . . . . ? O7 Cd2 N1 C9 -38.2(3) . . . . ? N1 C10 N2 C8 0.4(4) . . . . ? N1 C10 N2 C3 -179.7(3) . . . . ? C9 C8 N2 C10 -0.3(4) . . . . ? C9 C8 N2 C3 179.8(3) . . . . ? C2 C3 N2 C10 -144.8(3) . . . . ? C4 C3 N2 C10 41.4(5) . . . . ? C2 C3 N2 C8 35.1(5) . . . . ? C4 C3 N2 C8 -138.6(4) . . . . ? N4 C13 N3 C12 -0.3(4) . . . . ? N4 C13 N3 Cd1 169.4(2) . . . 1_446 ? C11 C12 N3 C13 0.2(5) . . . . ? C11 C12 N3 Cd1 -168.7(3) . . . 1_446 ? N3 C13 N4 C11 0.3(4) . . . . ? N3 C13 N4 C5 -172.0(3) . . . . ? C12 C11 N4 C13 -0.2(5) . . . . ? C12 C11 N4 C5 171.7(4) . . . . ? C6 C5 N4 C13 -32.4(5) . . . . ? C4 C5 N4 C13 139.2(4) . . . . ? C6 C5 N4 C11 157.0(4) . . . . ? C4 C5 N4 C11 -31.4(6) . . . . ? O2 C7 O1 Cd1 26.3(5) . . . 1_546 ? C1 C7 O1 Cd1 -149.0(2) . . . 1_546 ? O1 C7 O2 Cd2 32.7(6) . . . 1_546 ? C1 C7 O2 Cd2 -151.9(3) . . . 1_546 ? O4 C20 O3 Cd2 0.5(4) . . . 1_655 ? C14 C20 O3 Cd2 -179.8(2) . . . 1_655 ? O6 C21 O5 Cd1 1.8(3) . . . 2_774 ? C15 C21 O5 Cd1 -176.4(2) . . . 2_774 ? O6 C21 O5 Cd1 106.8(3) . . . . ? C15 C21 O5 Cd1 -71.5(3) . . . . ? Cd1 C21 O5 Cd1 104.95(14) 2_774 . . . ? N3 Cd1 O5 C21 117.8(2) 1_664 . . . ? O1 Cd1 O5 C21 63.7(3) 1_564 . . . ? O7 Cd1 O5 C21 -11.2(2) . . . . ? O6 Cd1 O5 C21 -146.0(2) 2_774 . . . ? O5 Cd1 O5 C21 -96.7(2) 2_774 . . . ? C21 Cd1 O5 C21 -121.90(19) 2_774 . . . ? N3 Cd1 O5 Cd1 -145.52(10) 1_664 . . 2_774 ? O1 Cd1 O5 Cd1 160.38(18) 1_564 . . 2_774 ? O7 Cd1 O5 Cd1 85.53(9) . . . 2_774 ? O6 Cd1 O5 Cd1 -49.26(9) 2_774 . . 2_774 ? O5 Cd1 O5 Cd1 0.0 2_774 . . 2_774 ? C21 Cd1 O5 Cd1 -25.20(9) 2_774 . . 2_774 ? O5 C21 O6 Cd1 -1.8(3) . . . 2_774 ? C15 C21 O6 Cd1 176.4(2) . . . 2_774 ? O8 C22 O7 Cd1 115.9(3) . . . . ? C16 C22 O7 Cd1 -63.1(3) . . . . ? O8 C22 O7 Cd2 -5.7(3) . . . . ? C16 C22 O7 Cd2 175.2(2) . . . . ? N3 Cd1 O7 C22 12.8(3) 1_664 . . . ? O1 Cd1 O7 C22 -70.9(2) 1_564 . . . ? O6 Cd1 O7 C22 -175.7(2) 2_774 . . . ? O5 Cd1 O7 C22 165.8(2) 2_774 . . . ? O5 Cd1 O7 C22 88.1(2) . . . . ? C21 Cd1 O7 C22 173.0(2) 2_774 . . . ? N3 Cd1 O7 Cd2 122.76(11) 1_664 . . . ? O1 Cd1 O7 Cd2 39.05(11) 1_564 . . . ? O6 Cd1 O7 Cd2 -65.78(15) 2_774 . . . ? O5 Cd1 O7 Cd2 -84.32(10) 2_774 . . . ? O5 Cd1 O7 Cd2 -162.01(11) . . . . ? C21 Cd1 O7 Cd2 -77.06(12) 2_774 . . . ? O3 Cd2 O7 C22 28.0(3) 1_455 . . . ? O2 Cd2 O7 C22 113.06(18) 1_564 . . . ? N1 Cd2 O7 C22 -81.74(18) . . . . ? O9 Cd2 O7 C22 -166.95(18) . . . . ? O3 Cd2 O7 Cd1 -99.92(18) 1_455 . . . ? O2 Cd2 O7 Cd1 -14.87(12) 1_564 . . . ? N1 Cd2 O7 Cd1 150.33(11) . . . . ? O9 Cd2 O7 Cd1 65.11(11) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.694 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.109 #====END