# 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_author_name 'Zhong-Min Su' _publ_contact_author_name 'Lian-Jie Li' _publ_contact_author_email lilj161@nenu.edu.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 851183' #TrackingRef '- 851183-851185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H33 N2 O18 Zn3' _chemical_formula_sum 'C45 H33 N2 O18 Zn3' _chemical_formula_weight 1085.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0060(13) _cell_length_b 13.6370(14) _cell_length_c 14.1040(15) _cell_angle_alpha 79.9710(17) _cell_angle_beta 64.3890(15) _cell_angle_gamma 71.2760(15) _cell_volume 2134.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1102 _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.690 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 10810 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7380 _reflns_number_gt 4035 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0555P)^2^+2.2314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7380 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1682 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.4206(7) 0.4994(6) 1.1886(6) 0.0342(19) Uani 1 1 d . . . C2 C 0.5053(8) 0.4131(7) 1.2244(7) 0.050(2) Uani 1 1 d . . . H2A H 0.4654 0.3607 1.2645 0.060 Uiso 1 1 calc R . . H2B H 0.5727 0.3809 1.1630 0.060 Uiso 1 1 calc R . . C3 C 0.4775(7) 0.4623(6) 1.3927(6) 0.034(2) Uani 1 1 d . . . C4 C 0.3677(8) 0.4489(6) 1.4430(7) 0.049(2) Uani 1 1 d . . . H4 H 0.3320 0.4317 1.4061 0.059 Uiso 1 1 calc R . . C5 C 0.3084(7) 0.4614(7) 1.5522(7) 0.048(2) Uani 1 1 d . . . H5 H 0.2340 0.4497 1.5876 0.058 Uiso 1 1 calc R . . C6 C 0.3561(7) 0.4898(6) 1.6070(7) 0.042(2) Uani 1 1 d . . . H6 H 0.3151 0.4981 1.6791 0.051 Uiso 1 1 calc R . . C7 C 0.4686(6) 0.5066(6) 1.5536(6) 0.0325(19) Uani 1 1 d . . . C8 C 0.4757(8) 0.1578(7) 1.1580(6) 0.038(2) Uani 1 1 d . . . C9 C 0.4174(8) 0.0777(7) 1.2314(7) 0.052(2) Uani 1 1 d . . . H9A H 0.3378 0.1126 1.2786 0.062 Uiso 1 1 calc R . . H9B H 0.4108 0.0319 1.1901 0.062 Uiso 1 1 calc R . . C10 C 0.4567(7) 0.0553(6) 1.3854(7) 0.041(2) Uani 1 1 d . . . C11 C 0.3878(7) 0.1514(7) 1.4198(7) 0.048(2) Uani 1 1 d . . . H11 H 0.3567 0.1989 1.3764 0.057 Uiso 1 1 calc R . . C12 C 0.3631(8) 0.1796(7) 1.5198(8) 0.055(3) Uani 1 1 d . . . H12 H 0.3136 0.2451 1.5419 0.065 Uiso 1 1 calc R . . C13 C 0.4079(7) 0.1162(6) 1.5848(7) 0.046(2) Uani 1 1 d . . . H13 H 0.3876 0.1368 1.6516 0.055 Uiso 1 1 calc R . . C14 C 0.4882(7) 0.0152(6) 1.5503(6) 0.041(2) Uani 1 1 d . . . C15 C 0.4155(7) 0.3141(7) 0.8835(6) 0.038(2) Uani 1 1 d . . . C16 C 0.3405(7) 0.3064(7) 0.8288(7) 0.048(2) Uani 1 1 d . . . H16A H 0.3889 0.3021 0.7539 0.057 Uiso 1 1 calc R . . H16B H 0.3175 0.2426 0.8532 0.057 Uiso 1 1 calc R . . C17 C 0.1467(7) 0.4002(7) 0.9446(7) 0.045(2) Uani 1 1 d . . . C18 C 0.1475(8) 0.3372(7) 1.0314(7) 0.050(2) Uani 1 1 d . . . H18 H 0.2102 0.2779 1.0250 0.060 Uiso 1 1 calc R . . C19 C 0.0537(7) 0.3621(7) 1.1295(7) 0.049(2) Uani 1 1 d . . . H19 H 0.0557 0.3208 1.1889 0.059 Uiso 1 1 calc R . . C20 C -0.0416(7) 0.4474(7) 1.1386(7) 0.046(2) Uani 1 1 d . . . H20 H -0.1028 0.4636 1.2045 0.056 Uiso 1 1 calc R . . C21 C -0.0482(6) 0.5113(6) 1.0493(6) 0.038(2) Uani 1 1 d . . . C22 C 0.9101(7) 0.2776(6) 0.8230(7) 0.036(2) Uani 1 1 d . . . C23 C 1.0261(7) 0.3082(7) 0.7642(6) 0.042(2) Uani 1 1 d . . . H23A H 1.0219 0.3663 0.7981 0.051 Uiso 1 1 calc R . . H23B H 1.0909 0.2507 0.7696 0.051 Uiso 1 1 calc R . . C24 C 0.9913(6) 0.4333(6) 0.6289(6) 0.0329(19) Uani 1 1 d . . . C25 C 0.9081(7) 0.5045(6) 0.6993(6) 0.041(2) Uani 1 1 d . . . H25 H 0.8841 0.4895 0.7713 0.049 Uiso 1 1 calc R . . C26 C 0.8595(7) 0.6013(7) 0.6606(7) 0.047(2) Uani 1 1 d . . . H26 H 0.8036 0.6514 0.7081 0.056 Uiso 1 1 calc R . . C27 C 0.8909(7) 0.6250(6) 0.5557(7) 0.040(2) Uani 1 1 d . . . H27 H 0.8587 0.6910 0.5327 0.048 Uiso 1 1 calc R . . C28 C 0.9732(6) 0.5485(6) 0.4812(6) 0.0325(19) Uani 1 1 d . . . C29 C 0.8005(8) 0.0415(7) 0.8756(7) 0.043(2) Uani 1 1 d . . . C30 C 0.8721(8) -0.0672(6) 0.8289(7) 0.052(3) Uani 1 1 d . . . H30A H 0.9510 -0.0849 0.8278 0.062 Uiso 1 1 calc R . . H30B H 0.8334 -0.1185 0.8737 0.062 Uiso 1 1 calc R . . C31 C 0.9531(7) -0.0156(6) 0.6455(6) 0.037(2) Uani 1 1 d . . . C32 C 1.0105(7) 0.0425(6) 0.6627(7) 0.046(2) Uani 1 1 d . . . H32 H 1.0034 0.0480 0.7302 0.055 Uiso 1 1 calc R . . C33 C 1.0820(7) 0.0950(7) 0.5744(7) 0.048(2) Uani 1 1 d . . . H33 H 1.1212 0.1355 0.5853 0.058 Uiso 1 1 calc R . . C34 C 1.0942(7) 0.0876(6) 0.4757(7) 0.044(2) Uani 1 1 d . . . H34 H 1.1411 0.1228 0.4197 0.053 Uiso 1 1 calc R . . C35 C 1.0362(6) 0.0269(6) 0.4574(6) 0.0325(19) Uani 1 1 d . . . C36 C 0.6747(7) 0.1736(6) 0.6366(6) 0.042(2) Uani 1 1 d . . . H36 H 0.6241 0.1423 0.6935 0.051 Uiso 1 1 calc R . . C37 C 0.8013(7) 0.2734(6) 0.5722(6) 0.040(2) Uani 1 1 d . . . H37 H 0.8416 0.3128 0.5831 0.048 Uiso 1 1 calc R . . C38 C 0.8196(7) 0.2627(6) 0.4708(6) 0.040(2) Uani 1 1 d . . . H38 H 0.8719 0.2935 0.4149 0.048 Uiso 1 1 calc R . . C39 C 0.7606(6) 0.2063(6) 0.4526(6) 0.0309(19) Uani 1 1 d . . . C40 C 0.6886(7) 0.1587(7) 0.5395(6) 0.046(2) Uani 1 1 d . . . H40 H 0.6499 0.1165 0.5307 0.055 Uiso 1 1 calc R . . C41 C 0.7688(6) 0.1952(6) 0.3456(6) 0.0342(19) Uani 1 1 d . . . C42 C 0.7412(7) 0.1166(6) 0.3212(6) 0.039(2) Uani 1 1 d . . . H42 H 0.7227 0.0633 0.3708 0.047 Uiso 1 1 calc R . . C43 C 0.7406(8) 0.1160(7) 0.2245(7) 0.050(2) Uani 1 1 d . . . H43 H 0.7181 0.0631 0.2118 0.060 Uiso 1 1 calc R . . C44 C 0.8049(7) 0.2596(6) 0.1667(6) 0.039(2) Uani 1 1 d . . . H44 H 0.8299 0.3082 0.1133 0.047 Uiso 1 1 calc R . . C45 C 0.8053(7) 0.2663(7) 0.2636(6) 0.045(2) Uani 1 1 d . . . H45 H 0.8303 0.3189 0.2738 0.054 Uiso 1 1 calc R . . N1 N 0.7288(5) 0.2303(5) 0.6563(5) 0.0319(16) Uani 1 1 d . . . N2 N 0.7704(6) 0.1871(5) 0.1473(5) 0.0370(17) Uani 1 1 d . . . O1 O 0.5122(4) 0.2425(4) 0.8620(4) 0.0429(15) Uani 1 1 d . . . O2 O 0.3801(5) 0.3860(4) 0.9438(4) 0.0432(15) Uani 1 1 d . . . O1W O 0.4126(16) 0.0688(15) 0.9793(16) 0.317(9) Uiso 1 1 d . . . O3 O 0.3986(5) 0.4788(4) 1.1146(4) 0.0417(14) Uani 1 1 d . . . O2W O 0.8698(12) -0.1219(11) 1.0891(12) 0.222(6) Uiso 1 1 d . . . O4 O 0.3805(5) 0.5841(4) 1.2290(4) 0.0406(14) Uani 1 1 d . . . O5 O 0.4056(5) 0.2388(5) 1.1415(5) 0.0534(17) Uani 1 1 d . . . O6 O 0.5830(5) 0.1380(5) 1.1198(5) 0.0577(18) Uani 1 1 d . . . O7 O 0.7327(5) 0.1023(4) 0.8407(4) 0.0424(15) Uani 1 1 d . . . O8 O 0.8212(5) 0.0533(4) 0.9526(4) 0.0463(15) Uani 1 1 d . . . O9 O 0.8516(4) 0.2777(4) 0.7724(4) 0.0384(14) Uani 1 1 d . . . O10 O 0.8875(5) 0.2510(5) 0.9186(5) 0.0560(17) Uani 1 1 d . . . O11 O 0.8815(5) -0.0700(4) 0.7243(4) 0.0501(16) Uani 1 1 d . . . O12 O 1.0515(4) 0.3361(4) 0.6556(4) 0.0421(14) Uani 1 1 d . . . O13 O 0.5470(5) 0.4471(5) 1.2870(4) 0.0502(16) Uani 1 1 d . . . O14 O 0.4822(5) 0.0162(4) 1.2931(5) 0.0532(16) Uani 1 1 d . . . O15 O 0.2375(5) 0.3892(4) 0.8449(4) 0.0488(16) Uani 1 1 d . . . O16 O 0.6362(4) 0.3096(4) 0.9688(4) 0.0334(13) Uani 1 1 d . . . Zn1 Zn 0.68671(8) 0.26092(7) 0.81010(7) 0.0311(3) Uani 1 1 d . . . Zn2 Zn 0.46218(8) 0.34844(7) 1.04087(7) 0.0394(3) Uani 1 1 d . . . Zn3 Zn 0.74480(8) 0.19107(7) 1.01438(7) 0.0379(3) 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 0.037(5) 0.035(5) 0.029(5) 0.002(4) -0.013(4) -0.009(4) C2 0.067(6) 0.049(6) 0.035(5) -0.014(4) -0.030(5) 0.004(5) C3 0.035(5) 0.039(5) 0.028(5) 0.001(4) -0.017(4) -0.005(4) C4 0.060(6) 0.048(6) 0.059(7) -0.008(5) -0.036(5) -0.019(5) C5 0.039(5) 0.059(6) 0.051(6) -0.001(5) -0.015(5) -0.023(5) C6 0.042(5) 0.048(5) 0.029(5) 0.000(4) -0.011(4) -0.006(4) C7 0.034(5) 0.040(5) 0.026(4) 0.006(4) -0.015(4) -0.014(4) C8 0.047(6) 0.043(5) 0.027(5) 0.007(4) -0.017(4) -0.019(5) C9 0.060(6) 0.058(6) 0.048(6) 0.016(5) -0.030(5) -0.029(5) C10 0.044(5) 0.035(5) 0.044(6) 0.010(4) -0.018(4) -0.016(4) C11 0.051(6) 0.040(6) 0.052(6) 0.014(5) -0.027(5) -0.014(4) C12 0.058(6) 0.034(5) 0.061(7) 0.005(5) -0.022(5) -0.006(4) C13 0.058(6) 0.033(5) 0.041(6) 0.000(4) -0.013(5) -0.015(4) C14 0.044(5) 0.040(5) 0.041(5) 0.010(4) -0.010(5) -0.030(4) C15 0.037(5) 0.047(6) 0.025(5) 0.001(4) -0.009(4) -0.010(4) C16 0.039(5) 0.056(6) 0.043(6) -0.010(5) -0.023(4) 0.007(4) C17 0.034(5) 0.054(6) 0.041(6) -0.008(5) -0.010(4) -0.012(4) C18 0.056(6) 0.048(6) 0.040(6) 0.015(5) -0.017(5) -0.019(5) C19 0.041(5) 0.051(6) 0.055(7) 0.011(5) -0.021(5) -0.015(5) C20 0.048(6) 0.050(6) 0.036(5) 0.008(5) -0.008(4) -0.025(5) C21 0.037(5) 0.042(5) 0.037(5) -0.004(4) -0.014(4) -0.015(4) C22 0.041(5) 0.033(5) 0.031(5) 0.001(4) -0.015(4) -0.007(4) C23 0.054(5) 0.058(6) 0.022(5) 0.016(4) -0.016(4) -0.033(5) C24 0.026(4) 0.036(5) 0.035(5) 0.010(4) -0.013(4) -0.012(4) C25 0.047(5) 0.048(6) 0.017(4) 0.003(4) -0.007(4) -0.012(4) C26 0.053(6) 0.042(6) 0.035(6) -0.007(4) -0.007(4) -0.013(4) C27 0.041(5) 0.038(5) 0.039(5) -0.001(4) -0.016(4) -0.009(4) C28 0.034(5) 0.036(5) 0.026(5) 0.005(4) -0.009(4) -0.015(4) C29 0.049(6) 0.043(6) 0.031(5) -0.007(4) -0.004(4) -0.022(5) C30 0.070(6) 0.036(5) 0.035(6) 0.001(4) -0.013(5) -0.008(5) C31 0.039(5) 0.025(4) 0.037(5) -0.005(4) -0.010(4) -0.004(4) C32 0.049(5) 0.044(5) 0.046(6) -0.013(5) -0.017(5) -0.011(4) C33 0.042(5) 0.061(6) 0.046(6) -0.022(5) -0.008(5) -0.024(5) C34 0.044(5) 0.041(5) 0.047(6) -0.009(4) -0.010(4) -0.018(4) C35 0.029(4) 0.030(4) 0.031(5) -0.007(4) -0.005(4) -0.006(3) C36 0.057(6) 0.053(6) 0.024(5) 0.001(4) -0.009(4) -0.035(5) C37 0.052(5) 0.052(5) 0.025(5) -0.003(4) -0.016(4) -0.025(4) C38 0.049(5) 0.058(6) 0.021(5) 0.007(4) -0.013(4) -0.031(5) C39 0.033(4) 0.035(5) 0.026(5) -0.001(4) -0.011(4) -0.012(4) C40 0.061(6) 0.059(6) 0.028(5) 0.003(4) -0.015(4) -0.037(5) C41 0.031(4) 0.037(5) 0.030(5) -0.002(4) -0.011(4) -0.005(4) C42 0.059(6) 0.037(5) 0.032(5) 0.005(4) -0.025(4) -0.022(4) C43 0.068(6) 0.064(6) 0.038(6) -0.002(5) -0.029(5) -0.034(5) C44 0.056(5) 0.045(5) 0.023(5) 0.004(4) -0.018(4) -0.022(4) C45 0.057(6) 0.056(6) 0.032(5) 0.003(5) -0.020(4) -0.030(5) N1 0.038(4) 0.035(4) 0.027(4) -0.004(3) -0.014(3) -0.014(3) N2 0.050(4) 0.043(4) 0.020(4) 0.001(3) -0.013(3) -0.018(4) O1 0.033(3) 0.044(4) 0.045(4) -0.005(3) -0.015(3) -0.003(3) O2 0.046(3) 0.049(4) 0.035(4) -0.013(3) -0.018(3) -0.004(3) O3 0.053(4) 0.040(3) 0.037(4) -0.013(3) -0.021(3) -0.008(3) O4 0.056(4) 0.029(3) 0.036(3) -0.008(3) -0.024(3) 0.000(3) O5 0.046(4) 0.052(4) 0.050(4) 0.006(3) -0.015(3) -0.007(3) O6 0.047(4) 0.064(4) 0.057(4) 0.026(3) -0.022(3) -0.023(3) O7 0.049(4) 0.034(3) 0.041(4) 0.003(3) -0.025(3) -0.001(3) O8 0.055(4) 0.042(4) 0.041(4) -0.008(3) -0.024(3) -0.003(3) O9 0.040(3) 0.056(4) 0.027(3) -0.003(3) -0.014(3) -0.022(3) O10 0.056(4) 0.088(5) 0.035(4) 0.016(3) -0.023(3) -0.037(4) O11 0.069(4) 0.040(3) 0.030(4) -0.004(3) -0.003(3) -0.024(3) O12 0.038(3) 0.047(4) 0.036(4) 0.009(3) -0.013(3) -0.013(3) O13 0.046(4) 0.073(4) 0.032(4) -0.015(3) -0.021(3) -0.004(3) O14 0.066(4) 0.052(4) 0.044(4) 0.011(3) -0.026(3) -0.020(3) O15 0.038(3) 0.061(4) 0.040(4) 0.001(3) -0.014(3) -0.007(3) O16 0.038(3) 0.041(3) 0.023(3) 0.001(2) -0.018(2) -0.007(2) Zn1 0.0348(5) 0.0350(5) 0.0232(5) -0.0026(4) -0.0134(4) -0.0062(4) Zn2 0.0407(6) 0.0447(6) 0.0297(6) -0.0076(5) -0.0130(5) -0.0063(5) Zn3 0.0442(6) 0.0445(6) 0.0256(6) 0.0000(4) -0.0177(5) -0.0088(5) _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 O4 1.231(8) . ? C1 O3 1.288(9) . ? C1 C2 1.516(11) . ? C2 O13 1.418(9) . ? C3 C4 1.349(11) . ? C3 O13 1.380(9) . ? C3 C7 1.417(11) 2_668 ? C4 C5 1.406(11) . ? C5 C6 1.342(11) . ? C6 C7 1.402(10) . ? C7 C7 1.384(14) 2_668 ? C7 C3 1.417(11) 2_668 ? C8 O6 1.213(9) . ? C8 O5 1.246(9) . ? C8 C9 1.517(11) . ? C9 O14 1.448(10) . ? C10 C11 1.360(11) . ? C10 O14 1.357(10) . ? C10 C14 1.441(12) 2_658 ? C11 C12 1.399(12) . ? C12 C13 1.338(12) . ? C13 C14 1.447(11) . ? C14 C10 1.441(12) 2_658 ? C14 C14 1.423(16) 2_658 ? C15 O2 1.248(9) . ? C15 O1 1.270(9) . ? C15 C16 1.517(11) . ? C16 O15 1.406(8) . ? C17 C18 1.369(11) . ? C17 O15 1.385(9) . ? C17 C21 1.433(11) 2_567 ? C18 C19 1.399(11) . ? C19 C20 1.377(11) . ? C20 C21 1.421(11) . ? C21 C21 1.412(15) 2_567 ? C21 C17 1.433(11) 2_567 ? C22 O9 1.246(9) . ? C22 O10 1.261(9) . ? C22 C23 1.531(10) . ? C23 O12 1.429(9) . ? C24 C25 1.355(10) . ? C24 O12 1.388(9) . ? C24 C28 1.415(10) 2_766 ? C25 C26 1.397(11) . ? C26 C27 1.362(11) . ? C27 C28 1.425(10) . ? C28 C28 1.415(14) 2_766 ? C28 C24 1.415(10) 2_766 ? C29 O7 1.212(10) . ? C29 O8 1.274(10) . ? C29 C30 1.556(11) . ? C30 O11 1.432(10) . ? C31 C32 1.359(11) . ? C31 O11 1.384(9) . ? C31 C35 1.428(11) 2_756 ? C32 C33 1.429(11) . ? C33 C34 1.351(11) . ? C34 C35 1.402(10) . ? C35 C31 1.428(11) 2_756 ? C35 C35 1.423(14) 2_756 ? C36 N1 1.327(9) . ? C36 C40 1.345(11) . ? C37 N1 1.337(9) . ? C37 C38 1.371(10) . ? C38 C39 1.365(10) . ? C39 C40 1.387(10) . ? C39 C41 1.498(10) . ? C41 C42 1.370(10) . ? C41 C45 1.391(11) . ? C42 C43 1.369(11) . ? C43 N2 1.336(10) . ? C44 N2 1.318(9) . ? C44 C45 1.389(11) . ? N1 Zn1 2.079(6) . ? N2 Zn3 2.030(6) 1_554 ? O1 Zn1 2.148(5) . ? O2 Zn2 1.987(5) . ? O3 Zn2 1.970(5) . ? O4 Zn1 2.088(5) 2_667 ? O5 Zn2 1.964(6) . ? O6 Zn3 2.249(6) . ? O7 Zn1 2.071(5) . ? O8 Zn3 1.975(5) . ? O9 Zn1 2.055(5) . ? O10 Zn3 2.088(5) . ? O16 Zn2 1.966(5) . ? O16 Zn3 1.995(5) . ? O16 Zn1 2.202(5) . ? Zn1 O4 2.088(5) 2_667 ? Zn3 N2 2.030(6) 1_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 C1 O3 124.7(7) . . ? O4 C1 C2 118.7(7) . . ? O3 C1 C2 116.5(7) . . ? O13 C2 C1 113.5(7) . . ? C4 C3 O13 124.4(8) . . ? C4 C3 C7 121.5(8) . 2_668 ? O13 C3 C7 114.1(7) . 2_668 ? C3 C4 C5 118.8(8) . . ? C6 C5 C4 121.9(8) . . ? C5 C6 C7 118.9(8) . . ? C7 C7 C6 121.3(9) 2_668 . ? C7 C7 C3 117.5(9) 2_668 2_668 ? C6 C7 C3 121.2(7) . 2_668 ? O6 C8 O5 126.2(8) . . ? O6 C8 C9 118.9(8) . . ? O5 C8 C9 114.8(8) . . ? O14 C9 C8 113.1(7) . . ? C11 C10 O14 126.7(8) . . ? C11 C10 C14 119.3(9) . 2_658 ? O14 C10 C14 114.0(7) . 2_658 ? C10 C11 C12 120.7(9) . . ? C13 C12 C11 122.7(9) . . ? C12 C13 C14 119.4(9) . . ? C10 C14 C14 119.4(10) 2_658 2_658 ? C10 C14 C13 122.3(8) 2_658 . ? C14 C14 C13 118.4(10) 2_658 . ? O2 C15 O1 125.8(8) . . ? O2 C15 C16 120.2(7) . . ? O1 C15 C16 114.0(7) . . ? O15 C16 C15 115.0(7) . . ? C18 C17 O15 125.8(8) . . ? C18 C17 C21 121.3(8) . 2_567 ? O15 C17 C21 112.9(8) . 2_567 ? C17 C18 C19 119.8(9) . . ? C20 C19 C18 120.4(9) . . ? C19 C20 C21 121.2(8) . . ? C20 C21 C21 118.6(10) . 2_567 ? C20 C21 C17 122.8(7) . 2_567 ? C21 C21 C17 118.6(10) 2_567 2_567 ? O9 C22 O10 127.6(8) . . ? O9 C22 C23 118.2(7) . . ? O10 C22 C23 114.2(7) . . ? O12 C23 C22 113.5(7) . . ? C25 C24 O12 124.4(7) . . ? C25 C24 C28 122.8(7) . 2_766 ? O12 C24 C28 112.8(7) . 2_766 ? C24 C25 C26 118.0(7) . . ? C27 C26 C25 122.5(8) . . ? C26 C27 C28 120.0(8) . . ? C28 C28 C27 118.2(9) 2_766 . ? C28 C28 C24 118.4(9) 2_766 2_766 ? C27 C28 C24 123.2(7) . 2_766 ? O7 C29 O8 127.5(8) . . ? O7 C29 C30 121.1(8) . . ? O8 C29 C30 111.3(8) . . ? O11 C30 C29 111.9(7) . . ? C32 C31 O11 123.8(8) . . ? C32 C31 C35 122.1(8) . 2_756 ? O11 C31 C35 114.1(7) . 2_756 ? C31 C32 C33 118.4(8) . . ? C34 C33 C32 121.8(8) . . ? C33 C34 C35 120.0(8) . . ? C34 C35 C31 122.3(7) . 2_756 ? C34 C35 C35 120.4(10) . 2_756 ? C31 C35 C35 117.3(9) 2_756 2_756 ? N1 C36 C40 124.1(7) . . ? N1 C37 C38 123.6(8) . . ? C39 C38 C37 119.5(7) . . ? C38 C39 C40 116.9(7) . . ? C38 C39 C41 123.6(7) . . ? C40 C39 C41 119.4(7) . . ? C36 C40 C39 119.9(8) . . ? C42 C41 C45 115.6(8) . . ? C42 C41 C39 123.5(7) . . ? C45 C41 C39 120.9(7) . . ? C41 C42 C43 120.5(8) . . ? N2 C43 C42 123.8(8) . . ? N2 C44 C45 122.7(8) . . ? C41 C45 C44 120.6(8) . . ? C37 N1 C36 116.0(7) . . ? C37 N1 Zn1 123.1(5) . . ? C36 N1 Zn1 120.6(5) . . ? C44 N2 C43 116.7(7) . . ? C44 N2 Zn3 122.3(5) . 1_554 ? C43 N2 Zn3 120.7(6) . 1_554 ? C15 O1 Zn1 126.9(5) . . ? C15 O2 Zn2 110.3(5) . . ? C1 O3 Zn2 128.1(5) . . ? C1 O4 Zn1 138.1(5) . 2_667 ? C8 O5 Zn2 121.7(5) . . ? C8 O6 Zn3 147.5(6) . . ? C29 O7 Zn1 136.0(6) . . ? C29 O8 Zn3 116.1(6) . . ? C22 O9 Zn1 135.3(5) . . ? C22 O10 Zn3 122.8(5) . . ? C31 O11 C30 117.2(7) . . ? C24 O12 C23 118.7(6) . . ? C3 O13 C2 120.0(7) . . ? C10 O14 C9 116.7(7) . . ? C17 O15 C16 118.5(7) . . ? Zn2 O16 Zn3 124.5(3) . . ? Zn2 O16 Zn1 108.4(2) . . ? Zn3 O16 Zn1 99.3(2) . . ? O9 Zn1 N1 92.7(2) . . ? O9 Zn1 O4 93.1(2) . 2_667 ? N1 Zn1 O4 86.7(2) . 2_667 ? O9 Zn1 O7 95.5(2) . . ? N1 Zn1 O7 87.9(2) . . ? O4 Zn1 O7 170.0(2) 2_667 . ? O9 Zn1 O1 175.6(2) . . ? N1 Zn1 O1 91.6(2) . . ? O4 Zn1 O1 88.2(2) 2_667 . ? O7 Zn1 O1 83.6(2) . . ? O9 Zn1 O16 87.25(19) . . ? N1 Zn1 O16 174.4(2) . . ? O4 Zn1 O16 87.71(19) 2_667 . ? O7 Zn1 O16 97.8(2) . . ? O1 Zn1 O16 88.61(19) . . ? O5 Zn2 O16 111.8(2) . . ? O5 Zn2 O3 109.1(2) . . ? O16 Zn2 O3 112.3(2) . . ? O5 Zn2 O2 109.0(3) . . ? O16 Zn2 O2 113.8(2) . . ? O3 Zn2 O2 100.3(2) . . ? O8 Zn3 O16 125.6(2) . . ? O8 Zn3 N2 109.6(3) . 1_556 ? O16 Zn3 N2 124.1(2) . 1_556 ? O8 Zn3 O10 94.6(2) . . ? O16 Zn3 O10 90.0(2) . . ? N2 Zn3 O10 94.2(2) 1_556 . ? O8 Zn3 O6 89.2(2) . . ? O16 Zn3 O6 86.7(2) . . ? N2 Zn3 O6 85.7(2) 1_556 . ? O10 Zn3 O6 176.0(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.801 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.148 data_2 _database_code_depnum_ccdc_archive 'CCDC 851184' #TrackingRef '- 851183-851185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Cd N4 O6' _chemical_formula_sum 'C28 H24 Cd N4 O6' _chemical_formula_weight 624.91 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.005(2) _cell_length_b 11.303(3) _cell_length_c 12.206(3) _cell_angle_alpha 100.797(3) _cell_angle_beta 107.308(4) _cell_angle_gamma 98.944(4) _cell_volume 1261.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 7467 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5506 _reflns_number_gt 4025 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0783P)^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 5506 _refine_ls_number_parameters 352 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.001 _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 0.0086(6) 0.3396(5) 0.5142(4) 0.0386(12) Uani 1 1 d . . . C2 C -0.0662(7) 0.2716(5) 0.4019(5) 0.0482(15) Uani 1 1 d . . . H2 H -0.0773 0.1863 0.3828 0.058 Uiso 1 1 calc R . . C3 C -0.1273(8) 0.3323(5) 0.3142(5) 0.0597(18) Uani 1 1 d . . . H3 H -0.1811 0.2860 0.2377 0.072 Uiso 1 1 calc R . . C4 C -0.1082(7) 0.4588(5) 0.3404(5) 0.0473(14) Uani 1 1 d . . . H4 H -0.1470 0.4977 0.2815 0.057 Uiso 1 1 calc R . . C5 C -0.0306(5) 0.5287(4) 0.4552(4) 0.0321(11) Uani 1 1 d . . . C6 C 0.0889(6) 0.1696(5) 0.5783(4) 0.0397(12) Uani 1 1 d . . . H6A H 0.1437 0.1635 0.5248 0.048 Uiso 1 1 calc R . . H6B H -0.0039 0.1125 0.5391 0.048 Uiso 1 1 calc R . . C7 C 0.1686(6) 0.1361(5) 0.6921(5) 0.0360(11) Uani 1 1 d . . . C8 C 0.3527(7) 0.4661(6) 0.4599(6) 0.0557(16) Uani 1 1 d . . . H8 H 0.2529 0.4421 0.4327 0.067 Uiso 1 1 calc R . . C9 C 0.4321(7) 0.4174(6) 0.5461(6) 0.0565(17) Uani 1 1 d . . . H9 H 0.3852 0.3620 0.5775 0.068 Uiso 1 1 calc R . . C10 C 0.5803(6) 0.4497(5) 0.5866(5) 0.0446(13) Uani 1 1 d . . . C11 C 0.6700(7) 0.3933(7) 0.6759(6) 0.0623(18) Uani 1 1 d . . . H11A H 0.6913 0.3209 0.6338 0.075 Uiso 1 1 calc R . . H11B H 0.7606 0.4522 0.7198 0.075 Uiso 1 1 calc R . . C12 C 0.5577(6) 0.2423(5) 0.7654(5) 0.0448(13) Uani 1 1 d . . . H12 H 0.5597 0.1723 0.7124 0.054 Uiso 1 1 calc R . . C13 C 0.5267(9) 0.3596(6) 0.9067(6) 0.071(2) Uani 1 1 d . . . H13 H 0.5029 0.3876 0.9736 0.085 Uiso 1 1 calc R . . C14 C 0.5837(10) 0.4324(6) 0.8503(6) 0.078(2) Uani 1 1 d . . . H14 H 0.6046 0.5184 0.8691 0.093 Uiso 1 1 calc R . . C15 C 0.5424(6) 0.0428(5) 0.4820(4) 0.0426(13) Uani 1 1 d . . . C16 C 0.6931(6) 0.0763(6) 0.5396(5) 0.0466(14) Uani 1 1 d . . . H16 H 0.7505 0.1325 0.5163 0.056 Uiso 1 1 calc R . . C17 C 0.7532(7) 0.0250(6) 0.6300(5) 0.0516(15) Uani 1 1 d . . . H17 H 0.8522 0.0475 0.6681 0.062 Uiso 1 1 calc R . . C18 C 0.6711(6) -0.0598(6) 0.6667(5) 0.0529(15) Uani 1 1 d . . . H18 H 0.7150 -0.0922 0.7292 0.064 Uiso 1 1 calc R . . C19 C 0.5260(6) -0.0954(5) 0.6110(5) 0.0454(14) Uani 1 1 d . . . C20 C 0.4938(7) -0.2370(5) 0.7276(4) 0.0499(15) Uani 1 1 d . . . H20A H 0.5810 -0.2589 0.7196 0.060 Uiso 1 1 calc R . . H20B H 0.4261 -0.3131 0.7172 0.060 Uiso 1 1 calc R . . C21 C 0.5291(6) -0.1582(5) 0.8530(5) 0.0387(12) Uani 1 1 d . . . C22 C 0.1966(6) -0.1033(5) 0.9991(5) 0.0403(12) Uani 1 1 d . . . H22 H 0.2850 -0.0980 1.0555 0.048 Uiso 1 1 calc R . . C23 C -0.0322(6) -0.1510(5) 0.9040(6) 0.0534(16) Uani 1 1 d . . . H23 H -0.1305 -0.1838 0.8799 0.064 Uiso 1 1 calc R . . C24 C 0.0359(6) -0.0805(5) 0.8512(5) 0.0460(14) Uani 1 1 d . . . H24 H -0.0087 -0.0549 0.7842 0.055 Uiso 1 1 calc R . . C25 C 0.0513(8) -0.2341(5) 1.0856(5) 0.0520(15) Uani 1 1 d . . . H25A H -0.0278 -0.2141 1.1103 0.062 Uiso 1 1 calc R . . H25B H 0.1376 -0.2084 1.1549 0.062 Uiso 1 1 calc R . . C26 C 0.0217(6) -0.3728(5) 1.0372(5) 0.0388(12) Uani 1 1 d . . . C27 C 0.0803(9) -0.4252(6) 0.9579(7) 0.085(3) Uani 1 1 d . . . H27 H 0.1356 -0.3750 0.9277 0.102 Uiso 1 1 calc R . . C28 C 0.0582(9) -0.5533(5) 0.9218(7) 0.074(2) Uani 1 1 d . . . H28 H 0.0997 -0.5877 0.8683 0.089 Uiso 1 1 calc R . . N1 N 0.5080(5) 0.2380(4) 0.8522(4) 0.0462(11) Uani 1 1 d . . . N2 N 0.6051(6) 0.3568(5) 0.7606(4) 0.0503(12) Uani 1 1 d . . . N3 N 0.1792(5) -0.0521(4) 0.9099(4) 0.0384(10) Uani 1 1 d . . . N4 N 0.0698(5) -0.1648(4) 0.9988(4) 0.0385(10) Uani 1 1 d . . . O1 O 0.4948(5) -0.0584(4) 0.8672(5) 0.0701(14) Uani 1 1 d . . . O2 O 0.5947(5) -0.2043(4) 0.9302(3) 0.0624(12) Uani 1 1 d . . . O3 O 0.1829(4) 0.2009(4) 0.7898(3) 0.0460(9) Uani 1 1 d . . . O4 O 0.2143(5) 0.0397(3) 0.6772(3) 0.0514(10) Uani 1 1 d . . . O5 O 0.4353(5) -0.1806(4) 0.6359(3) 0.0585(11) Uani 1 1 d . . . O6 O 0.0697(5) 0.2912(3) 0.6062(3) 0.0532(11) Uani 1 1 d . . . Cd1 Cd 0.35252(4) 0.08194(3) 0.88074(3) 0.03501(14) Uani 1 1 d U . . 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 0.055(3) 0.030(3) 0.035(3) 0.013(2) 0.014(2) 0.016(2) C2 0.077(4) 0.024(3) 0.035(3) 0.004(2) 0.011(3) 0.006(3) C3 0.094(5) 0.037(3) 0.032(3) 0.003(2) 0.002(3) 0.012(3) C4 0.071(4) 0.038(3) 0.029(3) 0.012(2) 0.006(3) 0.016(3) C5 0.041(3) 0.028(2) 0.029(2) 0.011(2) 0.012(2) 0.006(2) C6 0.052(3) 0.032(3) 0.034(3) 0.008(2) 0.012(2) 0.011(2) C7 0.045(3) 0.030(3) 0.038(3) 0.014(2) 0.017(2) 0.010(2) C8 0.048(3) 0.064(4) 0.068(4) 0.033(3) 0.031(3) 0.008(3) C9 0.063(4) 0.059(4) 0.061(4) 0.033(3) 0.034(3) 0.005(3) C10 0.053(3) 0.045(3) 0.053(3) 0.024(3) 0.033(3) 0.015(3) C11 0.062(4) 0.073(5) 0.076(5) 0.040(4) 0.045(4) 0.016(4) C12 0.054(3) 0.042(3) 0.047(3) 0.015(3) 0.025(3) 0.013(3) C13 0.114(6) 0.047(4) 0.059(4) 0.007(3) 0.053(4) -0.004(4) C14 0.130(7) 0.042(4) 0.070(5) 0.013(3) 0.058(5) 0.001(4) C15 0.046(3) 0.050(3) 0.027(3) 0.005(2) 0.006(2) 0.018(3) C16 0.050(3) 0.057(4) 0.034(3) 0.008(3) 0.014(3) 0.015(3) C17 0.049(3) 0.071(4) 0.038(3) 0.017(3) 0.013(3) 0.020(3) C18 0.047(3) 0.075(4) 0.037(3) 0.024(3) 0.007(3) 0.017(3) C19 0.051(3) 0.055(4) 0.028(3) 0.011(3) 0.011(2) 0.012(3) C20 0.070(4) 0.047(3) 0.032(3) 0.012(3) 0.012(3) 0.017(3) C21 0.039(3) 0.033(3) 0.043(3) 0.005(2) 0.018(2) 0.002(2) C22 0.040(3) 0.034(3) 0.045(3) 0.011(2) 0.012(2) 0.004(2) C23 0.034(3) 0.045(3) 0.078(4) 0.014(3) 0.017(3) 0.004(3) C24 0.043(3) 0.039(3) 0.052(3) 0.019(3) 0.008(3) 0.006(2) C25 0.078(4) 0.032(3) 0.057(4) 0.014(3) 0.039(3) 0.008(3) C26 0.050(3) 0.031(3) 0.041(3) 0.014(2) 0.023(3) 0.004(2) C27 0.138(7) 0.033(3) 0.126(7) 0.022(4) 0.109(6) 0.012(4) C28 0.125(7) 0.036(3) 0.098(6) 0.020(3) 0.091(5) 0.016(4) N1 0.065(3) 0.036(2) 0.045(3) 0.015(2) 0.026(2) 0.009(2) N2 0.061(3) 0.051(3) 0.050(3) 0.024(2) 0.027(3) 0.012(2) N3 0.036(2) 0.037(2) 0.046(3) 0.018(2) 0.016(2) 0.0055(19) N4 0.044(3) 0.028(2) 0.048(3) 0.0123(19) 0.023(2) 0.0033(19) O1 0.049(3) 0.058(3) 0.094(4) -0.012(3) 0.027(3) 0.017(2) O2 0.087(3) 0.058(3) 0.032(2) 0.018(2) 0.009(2) 0.000(2) O3 0.060(3) 0.051(2) 0.035(2) 0.0160(18) 0.0180(18) 0.0251(19) O4 0.075(3) 0.037(2) 0.046(2) 0.0139(18) 0.016(2) 0.024(2) O5 0.054(3) 0.068(3) 0.042(2) 0.023(2) -0.0003(19) 0.004(2) O6 0.098(3) 0.0306(19) 0.0325(19) 0.0130(16) 0.017(2) 0.024(2) Cd1 0.0382(2) 0.0349(2) 0.0341(2) 0.01493(15) 0.01265(15) 0.00597(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 C1 C2 1.359(7) . ? C1 O6 1.363(6) . ? C1 C5 1.430(7) 2_566 ? C2 C3 1.417(8) . ? C3 C4 1.375(8) . ? C4 C5 1.392(7) . ? C5 C5 1.408(9) 2_566 ? C5 C1 1.430(7) 2_566 ? C6 O6 1.409(6) . ? C6 C7 1.530(7) . ? C7 O3 1.232(6) . ? C7 O4 1.249(6) . ? C7 Cd1 2.724(5) . ? C8 C9 1.377(9) . ? C8 C10 1.381(7) 2_666 ? C9 C10 1.380(8) . ? C10 C8 1.381(7) 2_666 ? C10 C11 1.503(9) . ? C11 N2 1.461(7) . ? C12 N1 1.303(7) . ? C12 N2 1.326(7) . ? C13 C14 1.333(9) . ? C13 N1 1.368(8) . ? C14 N2 1.350(8) . ? C15 C15 1.407(11) 2_656 ? C15 C16 1.415(8) . ? C15 C19 1.423(7) 2_656 ? C16 C17 1.367(8) . ? C17 C18 1.389(8) . ? C18 C19 1.364(8) . ? C19 O5 1.359(7) . ? C19 C15 1.423(7) 2_656 ? C20 O5 1.413(6) . ? C20 C21 1.526(7) . ? C21 O1 1.227(7) . ? C21 O2 1.230(7) . ? C22 N3 1.306(7) . ? C22 N4 1.347(7) . ? C23 C24 1.341(8) . ? C23 N4 1.349(7) . ? C24 N3 1.353(7) . ? C25 N4 1.467(7) . ? C25 C26 1.516(7) . ? C26 C28 1.332(7) 2_547 ? C26 C27 1.365(8) . ? C27 C28 1.394(8) . ? C28 C26 1.332(7) 2_547 ? N1 Cd1 2.314(4) . ? N3 Cd1 2.276(4) . ? O1 Cd1 2.305(4) . ? O2 Cd1 2.317(4) 2_657 ? O3 Cd1 2.463(4) . ? O4 Cd1 2.370(4) . ? Cd1 O2 2.317(4) 2_657 ? 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 O6 124.4(5) . . ? C2 C1 C5 121.3(5) . 2_566 ? O6 C1 C5 114.2(4) . 2_566 ? C1 C2 C3 119.2(5) . . ? C4 C3 C2 121.0(5) . . ? C3 C4 C5 119.9(5) . . ? C4 C5 C5 120.6(6) . 2_566 ? C4 C5 C1 121.5(4) . 2_566 ? C5 C5 C1 117.9(5) 2_566 2_566 ? O6 C6 C7 109.4(4) . . ? O3 C7 O4 124.1(5) . . ? O3 C7 C6 120.7(5) . . ? O4 C7 C6 115.2(5) . . ? O3 C7 Cd1 64.7(3) . . ? O4 C7 Cd1 60.4(3) . . ? C6 C7 Cd1 169.5(4) . . ? C9 C8 C10 120.7(6) . 2_666 ? C8 C9 C10 120.9(5) . . ? C9 C10 C8 118.4(5) . 2_666 ? C9 C10 C11 122.2(5) . . ? C8 C10 C11 119.4(5) 2_666 . ? N2 C11 C10 115.4(5) . . ? N1 C12 N2 112.9(5) . . ? C14 C13 N1 110.3(6) . . ? C13 C14 N2 106.5(6) . . ? C15 C15 C16 119.6(6) 2_656 . ? C15 C15 C19 119.0(6) 2_656 2_656 ? C16 C15 C19 121.4(5) . 2_656 ? C17 C16 C15 119.1(6) . . ? C16 C17 C18 122.1(6) . . ? C19 C18 C17 119.9(5) . . ? O5 C19 C18 125.3(5) . . ? O5 C19 C15 114.4(5) . 2_656 ? C18 C19 C15 120.3(5) . 2_656 ? O5 C20 C21 115.2(5) . . ? O1 C21 O2 127.2(6) . . ? O1 C21 C20 119.5(5) . . ? O2 C21 C20 113.3(5) . . ? N3 C22 N4 111.1(5) . . ? C24 C23 N4 106.5(5) . . ? C23 C24 N3 110.0(5) . . ? N4 C25 C26 112.8(4) . . ? C28 C26 C27 118.6(5) 2_547 . ? C28 C26 C25 118.9(5) 2_547 . ? C27 C26 C25 122.4(5) . . ? C26 C27 C28 120.6(5) . . ? C26 C28 C27 120.8(6) 2_547 . ? C12 N1 C13 103.8(5) . . ? C12 N1 Cd1 130.9(4) . . ? C13 N1 Cd1 122.1(4) . . ? C12 N2 C14 106.4(5) . . ? C12 N2 C11 126.5(5) . . ? C14 N2 C11 127.0(5) . . ? C22 N3 C24 105.6(4) . . ? C22 N3 Cd1 125.8(4) . . ? C24 N3 Cd1 127.9(4) . . ? C22 N4 C23 106.7(4) . . ? C22 N4 C25 125.1(5) . . ? C23 N4 C25 128.1(5) . . ? C21 O1 Cd1 159.3(4) . . ? C21 O2 Cd1 112.4(4) . 2_657 ? C7 O3 Cd1 88.4(3) . . ? C7 O4 Cd1 92.4(3) . . ? C19 O5 C20 118.3(5) . . ? C1 O6 C6 117.4(4) . . ? N3 Cd1 O1 94.29(17) . . ? N3 Cd1 N1 171.87(16) . . ? O1 Cd1 N1 93.83(18) . . ? N3 Cd1 O2 89.96(15) . 2_657 ? O1 Cd1 O2 114.58(18) . 2_657 ? N1 Cd1 O2 86.87(16) . 2_657 ? N3 Cd1 O4 90.28(15) . . ? O1 Cd1 O4 98.48(16) . . ? N1 Cd1 O4 88.30(16) . . ? O2 Cd1 O4 146.82(16) 2_657 . ? N3 Cd1 O3 93.32(15) . . ? O1 Cd1 O3 151.35(17) . . ? N1 Cd1 O3 79.39(16) . . ? O2 Cd1 O3 93.00(15) 2_657 . ? O4 Cd1 O3 53.88(13) . . ? N3 Cd1 C7 94.74(15) . . ? O1 Cd1 C7 124.76(17) . . ? N1 Cd1 C7 80.40(16) . . ? O2 Cd1 C7 119.80(16) 2_657 . ? O4 Cd1 C7 27.25(14) . . ? O3 Cd1 C7 26.87(13) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.056 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.116 data_3 _database_code_depnum_ccdc_archive 'CCDC 851185' #TrackingRef '- 851183-851185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Cd N4 O8' _chemical_formula_sum 'C26 H20 Cd N4 O8' _chemical_formula_weight 628.86 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3610(19) _cell_length_b 12.7130(19) _cell_length_c 12.755(3) _cell_angle_alpha 111.843(2) _cell_angle_beta 105.938(2) _cell_angle_gamma 97.104(2) _cell_volume 1310.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 6646 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4520 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0176P)^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 4520 _refine_ls_number_parameters 370 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.3492(9) 0.7148(6) 0.5956(6) 0.053(2) Uani 1 1 d . . . H1 H 0.3748 0.6474 0.5529 0.063 Uiso 1 1 calc R . . C2 C 0.4500(8) 0.8107(7) 0.6886(6) 0.052(2) Uani 1 1 d . . . H2 H 0.5560 0.8235 0.7198 0.062 Uiso 1 1 calc R . . C3 C 0.2175(8) 0.8322(6) 0.6538(6) 0.0357(19) Uani 1 1 d . . . H3 H 0.1351 0.8651 0.6604 0.043 Uiso 1 1 calc R . . C4 C 0.4209(8) 0.9985(6) 0.8283(6) 0.0372(19) Uani 1 1 d . . . C5 C 0.5574(8) 1.0694(6) 0.8489(6) 0.044(2) Uani 1 1 d . . . H5 H 0.6119 1.0436 0.7974 0.053 Uiso 1 1 calc R . . C6 C 0.6157(8) 1.1790(6) 0.9453(6) 0.046(2) Uani 1 1 d . . . H6 H 0.7091 1.2268 0.9595 0.055 Uiso 1 1 calc R . . C7 C 0.5309(9) 1.2159(6) 1.0202(6) 0.043(2) Uani 1 1 d . . . C8 C 0.3913(8) 1.1450(7) 0.9972(6) 0.051(2) Uani 1 1 d . . . H8 H 0.3348 1.1709 1.0471 0.062 Uiso 1 1 calc R . . C9 C 0.3350(8) 1.0364(6) 0.9010(6) 0.042(2) Uani 1 1 d . . . H9 H 0.2405 0.9891 0.8852 0.051 Uiso 1 1 calc R . . C10 C 0.7393(9) 1.3768(7) 1.1908(7) 0.053(2) Uani 1 1 d . . . H10 H 0.8181 1.3425 1.1762 0.063 Uiso 1 1 calc R . . C11 C 0.5106(10) 1.4044(7) 1.1732(8) 0.080(3) Uani 1 1 d . . . H11 H 0.4049 1.3952 1.1463 0.096 Uiso 1 1 calc R . . C12 C 0.6153(10) 1.4958(7) 1.2694(8) 0.069(3) Uani 1 1 d . . . H12 H 0.5933 1.5606 1.3208 0.083 Uiso 1 1 calc R . . C13 C -0.1069(8) 0.7908(6) 0.3928(7) 0.043(2) Uani 1 1 d . . . C14 C -0.1533(8) 0.8915(7) 0.3663(6) 0.051(2) Uani 1 1 d . . . H14A H -0.0640 0.9389 0.3661 0.061 Uiso 1 1 calc R . . H14B H -0.2294 0.8588 0.2859 0.061 Uiso 1 1 calc R . . C16 C -0.3671(9) 0.9271(7) 0.4314(7) 0.044(2) Uani 1 1 d . . . C17 C -0.4578(10) 0.8181(7) 0.3564(7) 0.057(2) Uani 1 1 d . . . H17 H -0.4179 0.7614 0.3114 0.069 Uiso 1 1 calc R . . C18 C -0.4214(7) 1.0145(7) 0.5063(7) 0.040(2) Uani 1 1 d . . . C19 C -0.3276(9) 1.1274(7) 0.5860(7) 0.047(2) Uani 1 1 d . . . H19 H -0.2252 1.1466 0.5929 0.057 Uiso 1 1 calc R . . C20 C -0.3875(9) 1.2091(7) 0.6533(7) 0.053(2) Uani 1 1 d . . . H20 H -0.3250 1.2836 0.7061 0.064 Uiso 1 1 calc R . . C21 C 0.1332(8) 0.4165(7) 0.3511(7) 0.042(2) Uani 1 1 d . . . C22 C 0.1904(9) 0.3076(6) 0.3253(6) 0.060(3) Uani 1 1 d . . . H22A H 0.3016 0.3288 0.3597 0.072 Uiso 1 1 calc R . . H22B H 0.1506 0.2622 0.3623 0.072 Uiso 1 1 calc R . . C24 C 0.0950(8) 0.1185(6) 0.1537(6) 0.0411(19) Uani 1 1 d . . . C25 C 0.1177(8) 0.0578(7) 0.2227(6) 0.043(2) Uani 1 1 d . . . H25 H 0.1648 0.0973 0.3059 0.052 Uiso 1 1 calc R . . C26 C 0.0695(8) -0.0637(7) 0.1672(6) 0.047(2) Uani 1 1 d . . . H26 H 0.0842 -0.1055 0.2140 0.056 Uiso 1 1 calc R . . C27 C 0.0010(7) -0.1228(6) 0.0451(6) 0.042(2) Uani 1 1 d . . . H27 H -0.0290 -0.2042 0.0097 0.050 Uiso 1 1 calc R . . C28 C 0.0249(8) 0.0618(6) 0.0278(6) 0.0361(18) Uani 1 1 d . . . Cd1 Cd -0.01485(6) 0.60331(5) 0.42226(5) 0.03815(19) Uani 1 1 d . . . N1 N 0.2043(6) 0.7303(5) 0.5728(5) 0.0390(16) Uani 1 1 d . . . N2 N 0.3626(6) 0.8857(5) 0.7276(5) 0.0382(16) Uani 1 1 d . . . N3 N 0.5894(7) 1.3272(5) 1.1222(5) 0.0473(18) Uani 1 1 d . . . N4 N 0.7617(7) 1.4783(5) 1.2800(5) 0.0525(18) Uani 1 1 d . . . O1 O -0.1229(5) 0.7780(4) 0.4805(4) 0.0484(14) Uani 1 1 d . . . O2 O -0.0510(5) 0.7256(4) 0.3224(4) 0.0504(14) Uani 1 1 d . . . O3 O 0.1043(6) 0.4546(4) 0.4462(4) 0.0539(15) Uani 1 1 d . . . O4 O 0.1127(7) 0.4652(5) 0.2830(5) 0.0737(19) Uani 1 1 d . . . O5 O 0.1424(6) 0.2388(4) 0.1986(4) 0.0580(15) Uani 1 1 d . . . O6 O -0.2137(6) 0.9654(4) 0.4470(5) 0.0557(15) Uani 1 1 d . . . O1W O 0.1888(16) 0.4829(14) 0.0950(12) 0.109(5) Uani 0.50 1 d PU A 1 O2W O 0.995(4) 0.417(2) 0.0429(18) 0.269(14) Uani 0.50 1 d PU B 2 O3W O 0.237(3) 0.3869(16) 0.9300(12) 0.207(10) Uani 0.50 1 d PU C 2 O4W O 0.019(3) 0.6463(17) 0.1111(15) 0.218(10) Uani 0.50 1 d PU D 3 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 0.049(6) 0.032(5) 0.054(5) 0.000(4) 0.009(4) 0.015(4) C2 0.026(5) 0.043(5) 0.055(5) -0.002(4) -0.001(4) 0.010(4) C3 0.019(4) 0.029(5) 0.040(4) 0.005(4) -0.002(3) -0.003(3) C4 0.030(5) 0.032(5) 0.037(4) 0.008(4) 0.006(4) 0.000(4) C5 0.032(5) 0.029(5) 0.050(5) 0.000(4) 0.012(4) -0.004(4) C6 0.026(5) 0.041(5) 0.049(5) 0.006(4) 0.006(4) -0.006(4) C7 0.039(5) 0.019(4) 0.041(5) -0.004(4) 0.001(4) 0.000(4) C8 0.034(5) 0.058(6) 0.041(5) 0.003(4) 0.011(4) 0.000(4) C9 0.022(4) 0.042(5) 0.041(5) 0.004(4) 0.003(4) -0.005(4) C10 0.036(5) 0.043(6) 0.053(5) 0.003(4) 0.004(4) 0.001(4) C11 0.046(6) 0.045(6) 0.100(8) -0.007(5) 0.001(5) 0.023(5) C12 0.053(7) 0.048(6) 0.085(7) 0.008(5) 0.021(5) 0.016(5) C13 0.030(5) 0.032(5) 0.049(5) 0.012(4) -0.002(4) 0.003(4) C14 0.045(5) 0.062(6) 0.065(6) 0.038(5) 0.027(4) 0.022(5) C16 0.044(5) 0.051(6) 0.060(5) 0.036(5) 0.029(4) 0.021(4) C17 0.064(7) 0.050(6) 0.057(6) 0.015(5) 0.024(5) 0.030(5) C18 0.043(5) 0.041(5) 0.054(5) 0.031(4) 0.024(5) 0.020(5) C19 0.039(5) 0.052(6) 0.067(6) 0.035(5) 0.025(4) 0.019(4) C20 0.040(5) 0.035(5) 0.071(6) 0.019(4) 0.006(4) 0.002(4) C21 0.044(5) 0.037(5) 0.036(5) 0.010(4) 0.009(4) 0.005(4) C22 0.071(6) 0.051(6) 0.040(5) -0.002(4) 0.014(4) 0.033(5) C24 0.043(5) 0.035(5) 0.041(5) 0.007(4) 0.017(4) 0.016(4) C25 0.046(5) 0.045(5) 0.031(4) 0.003(4) 0.018(4) 0.019(4) C26 0.051(5) 0.050(6) 0.042(5) 0.016(4) 0.021(4) 0.021(4) C27 0.036(5) 0.038(5) 0.047(5) 0.008(4) 0.019(4) 0.011(4) C28 0.043(5) 0.037(5) 0.036(4) 0.014(4) 0.024(4) 0.016(4) Cd1 0.0371(3) 0.0260(3) 0.0347(3) 0.0037(2) 0.0029(2) 0.0034(2) N1 0.035(4) 0.031(4) 0.038(4) 0.008(3) 0.006(3) 0.008(3) N2 0.025(4) 0.032(4) 0.040(4) 0.006(3) 0.001(3) 0.003(3) N3 0.030(4) 0.031(4) 0.047(4) -0.002(3) -0.005(3) -0.001(3) N4 0.047(5) 0.028(4) 0.049(4) -0.005(3) 0.000(3) 0.002(3) O1 0.059(4) 0.050(4) 0.047(3) 0.028(3) 0.023(3) 0.019(3) O2 0.053(4) 0.046(4) 0.055(3) 0.020(3) 0.021(3) 0.022(3) O3 0.070(4) 0.038(3) 0.057(3) 0.012(3) 0.037(3) 0.017(3) O4 0.100(5) 0.073(5) 0.068(4) 0.041(4) 0.034(4) 0.043(4) O5 0.095(5) 0.034(3) 0.032(3) 0.002(3) 0.024(3) 0.006(3) O6 0.050(4) 0.048(4) 0.076(4) 0.023(3) 0.036(3) 0.020(3) O1W 0.069(10) 0.167(16) 0.110(12) 0.067(11) 0.043(9) 0.038(10) O2W 0.50(4) 0.24(3) 0.131(18) 0.096(18) 0.13(2) 0.22(3) O3W 0.37(3) 0.165(19) 0.059(10) 0.061(12) 0.007(14) 0.072(19) O4W 0.44(4) 0.148(19) 0.097(14) 0.064(13) 0.107(18) 0.09(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.344(9) . ? C1 N1 1.362(8) . ? C1 H1 0.9300 . ? C2 N2 1.374(8) . ? C2 H2 0.9300 . ? C3 N1 1.287(7) . ? C3 N2 1.336(7) . ? C3 H3 0.9300 . ? C4 C5 1.367(9) . ? C4 C9 1.383(8) . ? C4 N2 1.434(8) . ? C5 C6 1.386(9) . ? C5 H5 0.9300 . ? C6 C7 1.393(9) . ? C6 H6 0.9300 . ? C7 C8 1.381(9) . ? C7 N3 1.428(8) . ? C8 C9 1.376(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N4 1.308(8) . ? C10 N3 1.353(8) . ? C10 H10 0.9300 . ? C11 C12 1.346(10) . ? C11 N3 1.379(8) . ? C11 H11 0.9300 . ? C12 N4 1.394(8) . ? C12 H12 0.9300 . ? C13 O2 1.255(8) . ? C13 O1 1.234(8) . ? C13 C14 1.523(9) . ? C13 Cd1 2.750(7) . ? C14 O6 1.412(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C17 1.353(10) . ? C16 O6 1.391(8) . ? C16 C18 1.422(9) . ? C17 C20 1.407(9) 2_476 ? C17 H17 0.9300 . ? C18 C19 1.406(10) . ? C18 C18 1.422(13) 2_476 ? C19 C20 1.369(9) . ? C19 H19 0.9300 . ? C20 C17 1.407(9) 2_476 ? C20 H20 0.9300 . ? C21 O4 1.230(8) . ? C21 O3 1.246(7) . ? C21 C22 1.501(9) . ? C22 O5 1.425(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.362(9) . ? C24 O5 1.380(8) . ? C24 C28 1.405(9) . ? C25 C26 1.390(9) . ? C25 H25 0.9300 . ? C26 C27 1.365(8) . ? C26 H26 0.9300 . ? C27 C28 1.408(9) 2 ? C27 H27 0.9300 . ? C28 C28 1.414(13) 2 ? C28 C27 1.408(9) 2 ? Cd1 N4 2.267(6) 1_444 ? Cd1 N1 2.283(6) . ? Cd1 O2 2.350(5) . ? Cd1 O3 2.383(5) . ? Cd1 O3 2.366(5) 2_566 ? Cd1 O1 2.500(5) . ? Cd1 O4 2.651(5) . ? N4 Cd1 2.267(6) 1_666 ? O3 Cd1 2.366(5) 2_566 ? 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 N1 110.5(6) . . ? C2 C1 H1 124.7 . . ? N1 C1 H1 124.7 . . ? C1 C2 N2 105.2(7) . . ? C1 C2 H2 127.4 . . ? N2 C2 H2 127.4 . . ? N1 C3 N2 112.6(6) . . ? N1 C3 H3 123.7 . . ? N2 C3 H3 123.7 . . ? C5 C4 C9 120.6(7) . . ? C5 C4 N2 120.0(6) . . ? C9 C4 N2 119.4(6) . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 118.3(7) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C6 C7 C8 120.4(7) . . ? C6 C7 N3 119.8(7) . . ? C8 C7 N3 119.9(7) . . ? C9 C8 C7 120.5(7) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 119.1(7) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? N4 C10 N3 112.9(7) . . ? N4 C10 H10 123.6 . . ? N3 C10 H10 123.6 . . ? C12 C11 N3 107.1(7) . . ? C12 C11 H11 126.4 . . ? N3 C11 H11 126.4 . . ? C11 C12 N4 109.5(7) . . ? C11 C12 H12 125.3 . . ? N4 C12 H12 125.3 . . ? O2 C13 O1 123.7(7) . . ? O2 C13 C14 116.3(7) . . ? O1 C13 C14 120.0(7) . . ? O2 C13 Cd1 58.4(4) . . ? O1 C13 Cd1 65.3(4) . . ? C14 C13 Cd1 174.7(6) . . ? O6 C14 C13 115.9(6) . . ? O6 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? O6 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C17 C16 O6 125.3(7) . . ? C17 C16 C18 121.8(8) . . ? O6 C16 C18 112.9(7) . . ? C16 C17 C20 119.8(7) . 2_476 ? C16 C17 H17 120.1 . . ? C20 C17 H17 120.1 2_476 . ? C19 C18 C18 120.3(8) . 2_476 ? C19 C18 C16 122.4(7) . . ? C18 C18 C16 117.2(9) 2_476 . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C17 120.9(7) . 2_476 ? C19 C20 H20 119.6 . . ? C17 C20 H20 119.6 2_476 . ? O4 C21 O3 121.1(7) . . ? O4 C21 C22 123.1(7) . . ? O3 C21 C22 115.7(7) . . ? O5 C22 C21 110.3(6) . . ? O5 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? O5 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C25 C24 O5 124.2(7) . . ? C25 C24 C28 122.0(7) . . ? O5 C24 C28 113.8(7) . . ? C24 C25 C26 119.3(7) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.9(7) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.8(7) . 2 ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 2 . ? C24 C28 C28 118.4(8) . 2 ? C24 C28 C27 122.9(7) . 2 ? C28 C28 C27 118.6(8) 2 2 ? N4 Cd1 N1 177.1(2) 1_444 . ? N4 Cd1 O2 87.0(2) 1_444 . ? N1 Cd1 O2 94.34(19) . . ? N4 Cd1 O3 95.5(2) 1_444 . ? N1 Cd1 O3 84.87(19) . . ? O2 Cd1 O3 146.23(17) . . ? N4 Cd1 O3 84.0(2) 1_444 2_566 ? N1 Cd1 O3 93.36(19) . 2_566 ? O2 Cd1 O3 141.06(16) . 2_566 ? O3 Cd1 O3 72.51(18) . 2_566 ? N4 Cd1 O1 95.31(19) 1_444 . ? N1 Cd1 O1 83.38(18) . . ? O2 Cd1 O1 53.71(15) . . ? O3 Cd1 O1 157.87(16) . . ? O3 Cd1 O1 89.52(16) 2_566 . ? N4 Cd1 O4 83.9(2) 1_444 . ? N1 Cd1 O4 98.53(19) . . ? O2 Cd1 O4 96.72(17) . . ? O3 Cd1 O4 50.39(16) . . ? O3 Cd1 O4 119.73(17) 2_566 . ? O1 Cd1 O4 150.35(17) . . ? N4 Cd1 C13 91.0(2) 1_444 . ? N1 Cd1 C13 88.9(2) . . ? O2 Cd1 C13 27.07(18) . . ? O3 Cd1 C13 170.4(2) . . ? O3 Cd1 C13 115.3(2) 2_566 . ? O1 Cd1 C13 26.64(17) . . ? O4 Cd1 C13 123.8(2) . . ? C3 N1 C1 105.2(6) . . ? C3 N1 Cd1 127.4(5) . . ? C1 N1 Cd1 127.4(5) . . ? C3 N2 C2 106.5(6) . . ? C3 N2 C4 128.4(6) . . ? C2 N2 C4 125.1(6) . . ? C10 N3 C11 105.7(6) . . ? C10 N3 C7 125.2(6) . . ? C11 N3 C7 129.1(7) . . ? C10 N4 C12 104.8(6) . . ? C10 N4 Cd1 129.2(5) . 1_666 ? C12 N4 Cd1 126.0(5) . 1_666 ? C13 O1 Cd1 88.1(4) . . ? C13 O2 Cd1 94.5(4) . . ? C21 O3 Cd1 100.3(5) . . ? C21 O3 Cd1 143.3(5) . 2_566 ? Cd1 O3 Cd1 107.49(18) . 2_566 ? C21 O4 Cd1 87.8(4) . . ? C24 O5 C22 119.1(6) . . ? C16 O6 C14 117.7(6) . . ? 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 N1 C1 C2 N2 2.7(9) . . . . ? C9 C4 C5 C6 2.3(11) . . . . ? N2 C4 C5 C6 179.7(6) . . . . ? C4 C5 C6 C7 -0.7(11) . . . . ? C5 C6 C7 C8 -0.9(11) . . . . ? C5 C6 C7 N3 178.5(7) . . . . ? C6 C7 C8 C9 0.9(12) . . . . ? N3 C7 C8 C9 -178.5(6) . . . . ? C7 C8 C9 C4 0.7(11) . . . . ? C5 C4 C9 C8 -2.3(11) . . . . ? N2 C4 C9 C8 -179.7(6) . . . . ? N3 C11 C12 N4 0.6(11) . . . . ? O2 C13 C14 O6 -179.0(6) . . . . ? O1 C13 C14 O6 -0.1(10) . . . . ? Cd1 C13 C14 O6 -180(100) . . . . ? O6 C16 C17 C20 -178.6(6) . . . 2_476 ? C18 C16 C17 C20 3.3(12) . . . 2_476 ? C17 C16 C18 C19 178.9(7) . . . . ? O6 C16 C18 C19 0.6(10) . . . . ? C17 C16 C18 C18 -4.0(12) . . . 2_476 ? O6 C16 C18 C18 177.6(7) . . . 2_476 ? C18 C18 C19 C20 1.1(13) 2_476 . . . ? C16 C18 C19 C20 178.1(6) . . . . ? C18 C19 C20 C17 -0.2(11) . . . 2_476 ? O4 C21 C22 O5 -30.1(11) . . . . ? O3 C21 C22 O5 148.7(7) . . . . ? O5 C24 C25 C26 -177.9(6) . . . . ? C28 C24 C25 C26 -0.3(11) . . . . ? C24 C25 C26 C27 0.4(11) . . . . ? C25 C26 C27 C28 -1.0(10) . . . 2 ? C25 C24 C28 C28 0.8(12) . . . 2 ? O5 C24 C28 C28 178.6(7) . . . 2 ? C25 C24 C28 C27 179.4(6) . . . 2 ? O5 C24 C28 C27 -2.8(10) . . . 2 ? O2 C13 Cd1 N4 -81.3(4) . . . 1_444 ? O1 C13 Cd1 N4 99.8(4) . . . 1_444 ? C14 C13 Cd1 N4 -81(6) . . . 1_444 ? O2 C13 Cd1 N1 101.7(4) . . . . ? O1 C13 Cd1 N1 -77.2(4) . . . . ? C14 C13 Cd1 N1 102(6) . . . . ? O1 C13 Cd1 O2 -178.9(7) . . . . ? C14 C13 Cd1 O2 1(5) . . . . ? O2 C13 Cd1 O3 51.9(14) . . . . ? O1 C13 Cd1 O3 -127.0(12) . . . . ? C14 C13 Cd1 O3 52(6) . . . . ? O2 C13 Cd1 O3 -165.1(4) . . . 2_566 ? O1 C13 Cd1 O3 16.0(5) . . . 2_566 ? C14 C13 Cd1 O3 -165(6) . . . 2_566 ? O2 C13 Cd1 O1 178.9(7) . . . . ? C14 C13 Cd1 O1 179(100) . . . . ? O2 C13 Cd1 O4 2.1(5) . . . . ? O1 C13 Cd1 O4 -176.8(4) . . . . ? C14 C13 Cd1 O4 3(6) . . . . ? N2 C3 N1 C1 1.0(8) . . . . ? N2 C3 N1 Cd1 -178.6(4) . . . . ? C2 C1 N1 C3 -2.3(9) . . . . ? C2 C1 N1 Cd1 177.3(5) . . . . ? N4 Cd1 N1 C3 -51(5) 1_444 . . . ? O2 Cd1 N1 C3 65.8(6) . . . . ? O3 Cd1 N1 C3 -148.1(6) . . . . ? O3 Cd1 N1 C3 -76.0(6) 2_566 . . . ? O1 Cd1 N1 C3 13.2(6) . . . . ? O4 Cd1 N1 C3 163.3(6) . . . . ? C13 Cd1 N1 C3 39.3(6) . . . . ? N4 Cd1 N1 C1 130(4) 1_444 . . . ? O2 Cd1 N1 C1 -113.7(6) . . . . ? O3 Cd1 N1 C1 32.4(6) . . . . ? O3 Cd1 N1 C1 104.5(6) 2_566 . . . ? O1 Cd1 N1 C1 -166.4(6) . . . . ? O4 Cd1 N1 C1 -16.2(6) . . . . ? C13 Cd1 N1 C1 -140.2(6) . . . . ? N1 C3 N2 C2 0.6(9) . . . . ? N1 C3 N2 C4 -179.3(6) . . . . ? C1 C2 N2 C3 -2.0(9) . . . . ? C1 C2 N2 C4 178.0(7) . . . . ? C5 C4 N2 C3 -140.7(8) . . . . ? C9 C4 N2 C3 36.7(11) . . . . ? C5 C4 N2 C2 39.4(11) . . . . ? C9 C4 N2 C2 -143.2(7) . . . . ? N4 C10 N3 C11 -0.2(10) . . . . ? N4 C10 N3 C7 -178.9(7) . . . . ? C12 C11 N3 C10 -0.2(10) . . . . ? C12 C11 N3 C7 178.4(8) . . . . ? C6 C7 N3 C10 -35.1(11) . . . . ? C8 C7 N3 C10 144.3(8) . . . . ? C6 C7 N3 C11 146.6(8) . . . . ? C8 C7 N3 C11 -34.0(13) . . . . ? N3 C10 N4 C12 0.6(9) . . . . ? N3 C10 N4 Cd1 -179.0(5) . . . 1_666 ? C11 C12 N4 C10 -0.7(10) . . . . ? C11 C12 N4 Cd1 178.9(6) . . . 1_666 ? O2 C13 O1 Cd1 -1.1(7) . . . . ? C14 C13 O1 Cd1 -179.9(6) . . . . ? N4 Cd1 O1 C13 -81.7(4) 1_444 . . . ? N1 Cd1 O1 C13 101.0(4) . . . . ? O2 Cd1 O1 C13 0.6(4) . . . . ? O3 Cd1 O1 C13 159.3(5) . . . . ? O3 Cd1 O1 C13 -165.6(4) 2_566 . . . ? O4 Cd1 O1 C13 5.4(6) . . . . ? O1 C13 O2 Cd1 1.2(8) . . . . ? C14 C13 O2 Cd1 -179.9(6) . . . . ? N4 Cd1 O2 C13 98.2(4) 1_444 . . . ? N1 Cd1 O2 C13 -79.1(4) . . . . ? O3 Cd1 O2 C13 -166.4(4) . . . . ? O3 Cd1 O2 C13 21.7(5) 2_566 . . . ? O1 Cd1 O2 C13 -0.6(4) . . . . ? O4 Cd1 O2 C13 -178.2(4) . . . . ? O4 C21 O3 Cd1 7.2(9) . . . . ? C22 C21 O3 Cd1 -171.6(6) . . . . ? O4 C21 O3 Cd1 146.0(6) . . . 2_566 ? C22 C21 O3 Cd1 -32.7(12) . . . 2_566 ? N4 Cd1 O3 C21 73.7(5) 1_444 . . . ? N1 Cd1 O3 C21 -109.2(5) . . . . ? O2 Cd1 O3 C21 -19.1(6) . . . . ? O3 Cd1 O3 C21 155.6(6) 2_566 . . . ? O1 Cd1 O3 C21 -167.3(5) . . . . ? O4 Cd1 O3 C21 -3.7(4) . . . . ? C13 Cd1 O3 C21 -59.2(14) . . . . ? N4 Cd1 O3 Cd1 -81.9(2) 1_444 . . 2_566 ? N1 Cd1 O3 Cd1 95.2(2) . . . 2_566 ? O2 Cd1 O3 Cd1 -174.7(2) . . . 2_566 ? O3 Cd1 O3 Cd1 0.0 2_566 . . 2_566 ? O1 Cd1 O3 Cd1 37.0(5) . . . 2_566 ? O4 Cd1 O3 Cd1 -159.3(3) . . . 2_566 ? C13 Cd1 O3 Cd1 145.2(12) . . . 2_566 ? O3 C21 O4 Cd1 -6.4(8) . . . . ? C22 C21 O4 Cd1 172.3(7) . . . . ? N4 Cd1 O4 C21 -98.6(5) 1_444 . . . ? N1 Cd1 O4 C21 79.7(5) . . . . ? O2 Cd1 O4 C21 175.2(5) . . . . ? O3 Cd1 O4 C21 3.7(4) . . . . ? O3 Cd1 O4 C21 -19.1(5) 2_566 . . . ? O1 Cd1 O4 C21 171.3(4) . . . . ? C13 Cd1 O4 C21 174.2(5) . . . . ? C25 C24 O5 C22 -13.1(10) . . . . ? C28 C24 O5 C22 169.1(6) . . . . ? C21 C22 O5 C24 -140.3(7) . . . . ? C17 C16 O6 C14 9.9(11) . . . . ? C18 C16 O6 C14 -171.8(6) . . . . ? C13 C14 O6 C16 -80.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.619 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.115