# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zhong-Min Su' _publ_contact_author_email ZMSU@NENU.EDU.CN _publ_section_title ; pH-dependent self-assembly of divalent metals with a new ligand containing polycarboxylate: syntheses, crystal structures, luminescent and magnetic properties ; loop_ _publ_author_name 'Zhong-Min Su.' 'Lei Chen.' 'Ya-Qian Lan.' 'Kui-Zhan Shao.' 'Xin-long Wang.' ; Guang-Juan Xu ; 'Guang-Sheng Yang.' 'Ya-Hui Zhao.' # Attachment '1-6.cif' data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 743096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Cd N2 O9' _chemical_formula_sum 'C26 H22 Cd N2 O9' _chemical_formula_weight 618.86 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c 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 10.695(1) _cell_length_b 19.671(2) _cell_length_c 11.881(1) _cell_angle_alpha 90.0 _cell_angle_beta 98.661(1) _cell_angle_gamma 90.0 _cell_volume 2471.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8053 _exptl_absorpt_correction_T_max 0.8486 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 12243 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4343 _reflns_number_gt 3871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+1.7230P] 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 4343 _refine_ls_number_parameters 359 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.503741(16) 0.311936(8) 0.621735(15) 0.02399(7) Uani 1 1 d . . . C1 C 0.5486(2) 0.17018(13) 0.6430(2) 0.0266(5) Uani 1 1 d . . . C2 C 0.5870(2) 0.09712(12) 0.6304(2) 0.0269(5) Uani 1 1 d . . . C3 C 0.6599(3) 0.08170(13) 0.5472(2) 0.0349(6) Uani 1 1 d . . . H3 H 0.6837 0.1161 0.5011 0.042 Uiso 1 1 calc R . . C4 C 0.6980(3) 0.01538(14) 0.5318(2) 0.0376(7) Uani 1 1 d . . . C5 C 0.6621(3) -0.03610(13) 0.5988(2) 0.0342(6) Uani 1 1 d . . . H5 H 0.6865 -0.0807 0.5876 0.041 Uiso 1 1 calc R . . C6 C 0.5893(2) -0.02102(12) 0.6834(2) 0.0260(5) Uani 1 1 d . . . C7 C 0.5516(2) 0.04543(12) 0.6988(2) 0.0261(5) Uani 1 1 d . . . H7 H 0.5026 0.0554 0.7550 0.031 Uiso 1 1 calc R . . C8 C 0.5542(2) -0.07776(12) 0.7564(2) 0.0266(5) Uani 1 1 d . . . C9 C 0.8238(4) -0.05752(16) 0.4332(3) 0.0584(10) Uani 1 1 d . . . H9A H 0.7570 -0.0896 0.4065 0.070 Uiso 1 1 calc R . . H9B H 0.8687 -0.0739 0.5051 0.070 Uiso 1 1 calc R . . C10 C 0.9131(3) -0.05138(15) 0.3475(3) 0.0459(8) Uani 1 1 d . . . C11 C 0.9222(4) 0.00726(17) 0.2848(3) 0.0620(10) Uani 1 1 d . . . H11 H 0.8726 0.0448 0.2961 0.074 Uiso 1 1 calc R . . C12 C 1.0043(3) 0.01057(17) 0.2056(3) 0.0588(10) Uani 1 1 d . . . H12 H 1.0100 0.0505 0.1647 0.071 Uiso 1 1 calc R . . C13 C 1.0779(3) -0.04459(15) 0.1864(2) 0.0379(7) Uani 1 1 d . . . C14 C 1.0693(3) -0.10290(15) 0.2495(3) 0.0459(8) Uani 1 1 d . . . H14 H 1.1185 -0.1405 0.2378 0.055 Uiso 1 1 calc R . . C15 C 0.9885(3) -0.10608(15) 0.3297(3) 0.0514(8) Uani 1 1 d . . . H15 H 0.9849 -0.1455 0.3722 0.062 Uiso 1 1 calc R . . C16 C 1.1633(3) -0.04365(16) 0.0998(3) 0.0399(7) Uani 1 1 d . . . C17 C -0.1621(2) 0.22886(14) 0.3969(2) 0.0331(6) Uani 1 1 d . . . H17 H -0.1560 0.2447 0.4712 0.040 Uiso 1 1 calc R . . C18 C -0.2785(2) 0.21059(14) 0.3377(2) 0.0328(6) Uani 1 1 d . . . H18 H -0.3496 0.2150 0.3735 0.039 Uiso 1 1 calc R . . C19 C -0.1892(3) 0.17981(14) 0.1828(2) 0.0356(6) Uani 1 1 d . . . H19 H -0.1974 0.1621 0.1095 0.043 Uiso 1 1 calc R . . C20 C -0.0702(2) 0.19740(14) 0.2360(2) 0.0351(6) Uani 1 1 d . . . H20 H -0.0006 0.1918 0.1986 0.042 Uiso 1 1 calc R . . C21 C -0.0547(2) 0.22351(13) 0.3455(2) 0.0288(6) Uani 1 1 d . . . C22 C 0.0708(2) 0.24634(13) 0.4031(2) 0.0275(6) Uani 1 1 d . . . C23 C 0.1823(2) 0.21656(14) 0.3809(2) 0.0369(7) Uani 1 1 d . . . H23 H 0.1797 0.1817 0.3277 0.044 Uiso 1 1 calc R . . C24 C 0.2967(2) 0.23870(14) 0.4377(2) 0.0371(7) Uani 1 1 d . . . H24 H 0.3702 0.2184 0.4211 0.045 Uiso 1 1 calc R . . C25 C 0.2003(2) 0.31831(13) 0.5354(2) 0.0333(6) Uani 1 1 d . . . H25 H 0.2060 0.3536 0.5880 0.040 Uiso 1 1 calc R . . C26 C 0.0824(2) 0.29951(14) 0.4811(2) 0.0345(6) Uani 1 1 d . . . H26 H 0.0108 0.3223 0.4967 0.041 Uiso 1 1 calc R . . N1 N -0.2933(2) 0.18687(10) 0.23110(18) 0.0300(5) Uani 1 1 d . . . N2 N 0.30679(19) 0.28808(11) 0.51582(19) 0.0314(5) Uani 1 1 d . . . O1 O 0.57130(18) 0.21055(9) 0.56575(15) 0.0338(4) Uani 1 1 d . . . O2 O 0.49757(19) 0.18853(9) 0.72577(17) 0.0378(5) Uani 1 1 d . . . O3 O 0.49161(19) -0.06592(9) 0.83569(17) 0.0400(5) Uani 1 1 d . . . O4 O 0.59055(18) -0.13692(8) 0.73803(16) 0.0358(4) Uani 1 1 d . . . O5 O 0.7715(2) 0.00731(10) 0.4479(2) 0.0624(7) Uani 1 1 d . . . O6 O 1.1844(2) 0.01748(11) 0.0619(2) 0.0605(6) Uani 1 1 d . . . H6 H 1.2322 0.0147 0.0142 0.091 Uiso 1 1 calc R . . O7 O 1.2082(2) -0.09487(11) 0.06537(19) 0.0498(6) Uani 1 1 d . . . O1W O 0.5493(2) 0.35873(11) 0.44803(16) 0.0409(5) Uani 1 1 d D . . O2W O 0.3467(2) 0.03036(13) 0.9241(2) 0.0595(6) Uani 1 1 d D . . H1A H 0.6244(17) 0.3770(17) 0.443(3) 0.072(12) Uiso 1 1 d D . . H2A H 0.382(3) -0.0023(15) 0.888(3) 0.102(16) Uiso 1 1 d D . . H1B H 0.527(3) 0.3422(16) 0.3781(14) 0.056(10) Uiso 1 1 d D . . H2B H 0.412(3) 0.057(2) 0.947(5) 0.15(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02564(11) 0.02064(11) 0.02555(11) -0.00338(7) 0.00339(7) 0.00199(7) C1 0.0288(12) 0.0229(13) 0.0276(14) -0.0016(11) 0.0027(10) 0.0004(10) C2 0.0344(13) 0.0206(12) 0.0262(14) 0.0001(11) 0.0057(11) -0.0001(10) C3 0.0488(16) 0.0225(14) 0.0378(16) 0.0078(12) 0.0206(13) 0.0027(12) C4 0.0525(17) 0.0295(15) 0.0368(16) 0.0044(13) 0.0259(13) 0.0066(13) C5 0.0479(16) 0.0199(13) 0.0385(16) 0.0022(12) 0.0181(13) 0.0041(11) C6 0.0327(13) 0.0218(13) 0.0242(13) 0.0016(10) 0.0066(10) -0.0018(10) C7 0.0333(13) 0.0233(13) 0.0234(13) -0.0002(10) 0.0096(10) -0.0019(10) C8 0.0307(13) 0.0234(13) 0.0260(14) 0.0019(11) 0.0054(10) -0.0031(10) C9 0.088(3) 0.0332(17) 0.066(2) 0.0080(16) 0.051(2) 0.0145(17) C10 0.063(2) 0.0359(17) 0.0461(18) 0.0024(14) 0.0304(15) 0.0095(14) C11 0.086(3) 0.0383(18) 0.075(3) 0.0150(18) 0.054(2) 0.0232(17) C12 0.084(2) 0.0384(18) 0.065(2) 0.0141(17) 0.0470(19) 0.0173(17) C13 0.0445(16) 0.0365(16) 0.0353(16) -0.0037(13) 0.0142(12) 0.0016(13) C14 0.0560(19) 0.0342(16) 0.0520(19) -0.0028(15) 0.0229(15) 0.0113(14) C15 0.075(2) 0.0315(16) 0.056(2) 0.0079(15) 0.0359(17) 0.0138(16) C16 0.0428(16) 0.0414(17) 0.0378(17) -0.0077(14) 0.0135(13) -0.0007(13) C17 0.0338(14) 0.0417(16) 0.0235(14) -0.0044(12) 0.0036(11) -0.0006(12) C18 0.0308(14) 0.0376(15) 0.0308(15) 0.0039(12) 0.0074(11) 0.0006(12) C19 0.0355(15) 0.0429(16) 0.0282(14) -0.0079(12) 0.0043(11) -0.0023(12) C20 0.0277(13) 0.0458(17) 0.0325(15) -0.0059(13) 0.0071(11) -0.0007(12) C21 0.0300(13) 0.0276(14) 0.0288(14) 0.0001(11) 0.0042(11) 0.0013(11) C22 0.0264(13) 0.0293(14) 0.0264(14) -0.0001(11) 0.0022(10) -0.0002(10) C23 0.0356(15) 0.0363(15) 0.0369(16) -0.0137(13) -0.0004(12) 0.0038(12) C24 0.0299(14) 0.0393(16) 0.0414(17) -0.0140(14) 0.0029(12) 0.0066(12) C25 0.0340(14) 0.0304(15) 0.0351(15) -0.0109(12) 0.0041(12) -0.0010(11) C26 0.0289(14) 0.0407(16) 0.0338(15) -0.0084(13) 0.0041(11) 0.0044(12) N1 0.0293(11) 0.0333(12) 0.0267(12) 0.0028(10) 0.0024(9) -0.0029(9) N2 0.0278(11) 0.0319(12) 0.0343(13) -0.0060(10) 0.0046(9) -0.0002(9) O1 0.0517(11) 0.0197(9) 0.0308(10) 0.0043(8) 0.0089(8) 0.0061(8) O2 0.0526(12) 0.0279(10) 0.0358(11) -0.0016(8) 0.0164(9) 0.0090(8) O3 0.0612(12) 0.0254(10) 0.0395(11) 0.0018(9) 0.0279(9) -0.0023(9) O4 0.0509(11) 0.0189(9) 0.0416(11) 0.0053(8) 0.0195(9) 0.0034(8) O5 0.1031(19) 0.0311(11) 0.0696(16) 0.0148(11) 0.0673(15) 0.0223(12) O6 0.0848(17) 0.0426(13) 0.0661(16) -0.0017(12) 0.0505(13) -0.0002(12) O7 0.0562(13) 0.0453(13) 0.0536(14) -0.0136(11) 0.0266(11) 0.0015(10) O1W 0.0537(13) 0.0428(12) 0.0278(11) 0.0017(9) 0.0115(9) -0.0112(10) O2W 0.0591(14) 0.0554(15) 0.0727(18) -0.0208(13) 0.0381(13) -0.0121(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.2554(18) . ? Cd1 O4 2.3046(19) 2_656 ? Cd1 N2 2.333(2) . ? Cd1 N1 2.356(2) 4_666 ? Cd1 O1W 2.376(2) . ? Cd1 O3 2.4543(19) 2_656 ? Cd1 C8 2.731(2) 2_656 ? C1 O2 1.248(3) . ? C1 O1 1.264(3) . ? C1 C2 1.509(3) . ? C2 C3 1.381(4) . ? C2 C7 1.389(3) . ? C3 C4 1.387(4) . ? C3 H3 0.9300 . ? C4 O5 1.368(3) . ? C4 C5 1.378(4) . ? C5 C6 1.394(4) . ? C5 H5 0.9300 . ? C6 C7 1.388(3) . ? C6 C8 1.495(3) . ? C7 H7 0.9300 . ? C8 O4 1.256(3) . ? C8 O3 1.257(3) . ? C8 Cd1 2.731(2) 2_646 ? C9 O5 1.414(3) . ? C9 C10 1.502(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.380(4) . ? C10 C11 1.384(4) . ? C11 C12 1.381(4) . ? C11 H11 0.9300 . ? C12 C13 1.379(4) . ? C12 H12 0.9300 . ? C13 C14 1.381(4) . ? C13 C16 1.476(4) . ? C14 C15 1.380(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.214(3) . ? C16 O6 1.316(4) . ? C17 C18 1.382(4) . ? C17 C21 1.384(4) . ? C17 H17 0.9300 . ? C18 N1 1.336(3) . ? C18 H18 0.9300 . ? C19 N1 1.334(4) . ? C19 C20 1.377(4) . ? C19 H19 0.9300 . ? C20 C21 1.385(4) . ? C20 H20 0.9300 . ? C21 C22 1.481(4) . ? C22 C23 1.389(4) . ? C22 C26 1.391(4) . ? C23 C24 1.376(4) . ? C23 H23 0.9300 . ? C24 N2 1.336(3) . ? C24 H24 0.9300 . ? C25 N2 1.336(3) . ? C25 C26 1.377(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N1 Cd1 2.356(2) 4_465 ? O3 Cd1 2.4543(19) 2_646 ? O4 Cd1 2.3046(19) 2_646 ? O6 H6 0.8200 . ? O1W H1A 0.890(10) . ? O1W H1B 0.891(10) . ? O2W H2A 0.888(10) . ? O2W H2B 0.889(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O4 142.54(6) . 2_656 ? O1 Cd1 N2 88.08(7) . . ? O4 Cd1 N2 91.14(8) 2_656 . ? O1 Cd1 N1 82.06(7) . 4_666 ? O4 Cd1 N1 93.68(8) 2_656 4_666 ? N2 Cd1 N1 168.97(8) . 4_666 ? O1 Cd1 O1W 88.27(7) . . ? O4 Cd1 O1W 128.90(7) 2_656 . ? N2 Cd1 O1W 84.03(8) . . ? N1 Cd1 O1W 100.53(8) 4_666 . ? O1 Cd1 O3 158.28(7) . 2_656 ? O4 Cd1 O3 54.63(6) 2_656 2_656 ? N2 Cd1 O3 107.26(7) . 2_656 ? N1 Cd1 O3 83.58(7) 4_666 2_656 ? O1W Cd1 O3 78.42(7) . 2_656 ? O1 Cd1 C8 165.30(7) . 2_656 ? O4 Cd1 C8 27.24(7) 2_656 2_656 ? N2 Cd1 C8 100.78(8) . 2_656 ? N1 Cd1 C8 87.92(7) 4_666 2_656 ? O1W Cd1 C8 104.19(8) . 2_656 ? O3 Cd1 C8 27.39(7) 2_656 2_656 ? O2 C1 O1 123.0(2) . . ? O2 C1 C2 120.8(2) . . ? O1 C1 C2 116.2(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 118.2(2) . . ? C7 C2 C1 122.5(2) . . ? C2 C3 C4 120.6(2) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O5 C4 C5 125.2(2) . . ? O5 C4 C3 114.7(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 119.7(2) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 120.0(2) . . ? C7 C6 C8 121.6(2) . . ? C5 C6 C8 118.4(2) . . ? C6 C7 C2 120.2(2) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O4 C8 O3 121.0(2) . . ? O4 C8 C6 118.6(2) . . ? O3 C8 C6 120.3(2) . . ? O4 C8 Cd1 57.12(12) . 2_646 ? O3 C8 Cd1 63.96(13) . 2_646 ? C6 C8 Cd1 175.66(18) . 2_646 ? O5 C9 C10 108.4(2) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C15 C10 C11 118.5(3) . . ? C15 C10 C9 119.2(3) . . ? C11 C10 C9 122.4(3) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 118.5(3) . . ? C12 C13 C16 122.3(3) . . ? C14 C13 C16 119.2(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? O7 C16 O6 123.1(3) . . ? O7 C16 C13 122.9(3) . . ? O6 C16 C13 114.0(3) . . ? C18 C17 C21 120.0(3) . . ? C18 C17 H17 120.0 . . ? C21 C17 H17 120.0 . . ? N1 C18 C17 122.8(2) . . ? N1 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? N1 C19 C20 123.4(3) . . ? N1 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C21 119.7(2) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C17 C21 C20 116.9(2) . . ? C17 C21 C22 121.8(2) . . ? C20 C21 C22 121.3(2) . . ? C23 C22 C26 116.7(2) . . ? C23 C22 C21 121.9(2) . . ? C26 C22 C21 121.4(2) . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N2 C24 C23 123.0(2) . . ? N2 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N2 C25 C26 122.9(2) . . ? N2 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C25 C26 C22 119.9(2) . . ? C25 C26 H26 120.1 . . ? C22 C26 H26 120.1 . . ? C19 N1 C18 117.1(2) . . ? C19 N1 Cd1 121.55(18) . 4_465 ? C18 N1 Cd1 119.13(17) . 4_465 ? C25 N2 C24 117.5(2) . . ? C25 N2 Cd1 122.74(17) . . ? C24 N2 Cd1 119.53(17) . . ? C1 O1 Cd1 103.67(16) . . ? C8 O3 Cd1 88.65(15) . 2_646 ? C8 O4 Cd1 95.64(15) . 2_646 ? C4 O5 C9 118.4(2) . . ? C16 O6 H6 109.5 . . ? Cd1 O1W H1A 121(2) . . ? Cd1 O1W H1B 127(2) . . ? H1A O1W H1B 101.9(14) . . ? H2A O2W H2B 102.2(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -170.4(3) . . . . ? O1 C1 C2 C3 9.5(4) . . . . ? O2 C1 C2 C7 9.8(4) . . . . ? O1 C1 C2 C7 -170.3(2) . . . . ? C7 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C4 -180.0(3) . . . . ? C2 C3 C4 O5 -178.9(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? O5 C4 C5 C6 178.5(3) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C4 C5 C6 C7 0.9(4) . . . . ? C4 C5 C6 C8 -178.7(2) . . . . ? C5 C6 C7 C2 -0.4(4) . . . . ? C8 C6 C7 C2 179.2(2) . . . . ? C3 C2 C7 C6 0.0(4) . . . . ? C1 C2 C7 C6 179.8(2) . . . . ? C7 C6 C8 O4 179.6(2) . . . . ? C5 C6 C8 O4 -0.8(4) . . . . ? C7 C6 C8 O3 -1.6(4) . . . . ? C5 C6 C8 O3 178.0(2) . . . . ? C7 C6 C8 Cd1 168(2) . . . 2_646 ? C5 C6 C8 Cd1 -13(2) . . . 2_646 ? O5 C9 C10 C15 171.6(3) . . . . ? O5 C9 C10 C11 -8.8(5) . . . . ? C15 C10 C11 C12 0.5(6) . . . . ? C9 C10 C11 C12 -179.1(4) . . . . ? C10 C11 C12 C13 0.7(6) . . . . ? C11 C12 C13 C14 -1.1(6) . . . . ? C11 C12 C13 C16 177.9(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C16 C13 C14 C15 -178.7(3) . . . . ? C13 C14 C15 C10 0.9(5) . . . . ? C11 C10 C15 C14 -1.3(5) . . . . ? C9 C10 C15 C14 178.3(3) . . . . ? C12 C13 C16 O7 -164.3(3) . . . . ? C14 C13 C16 O7 14.6(5) . . . . ? C12 C13 C16 O6 14.5(4) . . . . ? C14 C13 C16 O6 -166.6(3) . . . . ? C21 C17 C18 N1 0.6(4) . . . . ? N1 C19 C20 C21 0.4(4) . . . . ? C18 C17 C21 C20 -2.1(4) . . . . ? C18 C17 C21 C22 176.3(2) . . . . ? C19 C20 C21 C17 1.6(4) . . . . ? C19 C20 C21 C22 -176.8(2) . . . . ? C17 C21 C22 C23 151.0(3) . . . . ? C20 C21 C22 C23 -30.8(4) . . . . ? C17 C21 C22 C26 -29.9(4) . . . . ? C20 C21 C22 C26 148.3(3) . . . . ? C26 C22 C23 C24 1.9(4) . . . . ? C21 C22 C23 C24 -179.0(3) . . . . ? C22 C23 C24 N2 0.6(5) . . . . ? N2 C25 C26 C22 0.8(4) . . . . ? C23 C22 C26 C25 -2.5(4) . . . . ? C21 C22 C26 C25 178.3(3) . . . . ? C20 C19 N1 C18 -1.9(4) . . . . ? C20 C19 N1 Cd1 161.2(2) . . . 4_465 ? C17 C18 N1 C19 1.4(4) . . . . ? C17 C18 N1 Cd1 -162.1(2) . . . 4_465 ? C26 C25 N2 C24 1.7(4) . . . . ? C26 C25 N2 Cd1 -173.2(2) . . . . ? C23 C24 N2 C25 -2.4(4) . . . . ? C23 C24 N2 Cd1 172.6(2) . . . . ? O1 Cd1 N2 C25 158.6(2) . . . . ? O4 Cd1 N2 C25 16.0(2) 2_656 . . . ? N1 Cd1 N2 C25 132.0(4) 4_666 . . . ? O1W Cd1 N2 C25 -113.0(2) . . . . ? O3 Cd1 N2 C25 -37.1(2) 2_656 . . . ? C8 Cd1 N2 C25 -9.6(2) 2_656 . . . ? O1 Cd1 N2 C24 -16.2(2) . . . . ? O4 Cd1 N2 C24 -158.8(2) 2_656 . . . ? N1 Cd1 N2 C24 -42.8(5) 4_666 . . . ? O1W Cd1 N2 C24 72.2(2) . . . . ? O3 Cd1 N2 C24 148.1(2) 2_656 . . . ? C8 Cd1 N2 C24 175.6(2) 2_656 . . . ? O2 C1 O1 Cd1 1.3(3) . . . . ? C2 C1 O1 Cd1 -178.63(17) . . . . ? O4 Cd1 O1 C1 -1.6(2) 2_656 . . . ? N2 Cd1 O1 C1 -90.98(16) . . . . ? N1 Cd1 O1 C1 84.06(16) 4_666 . . . ? O1W Cd1 O1 C1 -175.06(16) . . . . ? O3 Cd1 O1 C1 133.1(2) 2_656 . . . ? C8 Cd1 O1 C1 36.6(4) 2_656 . . . ? O4 C8 O3 Cd1 -2.2(2) . . . 2_646 ? C6 C8 O3 Cd1 179.1(2) . . . 2_646 ? O3 C8 O4 Cd1 2.3(3) . . . 2_646 ? C6 C8 O4 Cd1 -178.92(19) . . . 2_646 ? C5 C4 O5 C9 -5.1(5) . . . . ? C3 C4 O5 C9 174.4(3) . . . . ? C10 C9 O5 C4 -172.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O2W 0.82 1.77 2.572(3) 165.1 1_654 O1W H1A O7 0.890(10) 1.891(11) 2.777(3) 173(3) 2_755 O2W H2A O3 0.888(10) 1.882(15) 2.753(3) 166(4) . O1W H1B O2 0.891(10) 1.889(11) 2.775(3) 173(3) 4_565 O2W H2B O1W 0.889(10) 2.21(2) 3.057(3) 160(5) 4_566 O2W H2B O3 0.889(10) 2.63(5) 3.184(4) 121(5) 3_657 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.473 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.062 #===========================end data_complex-2 _database_code_depnum_ccdc_archive 'CCDC 743097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H51 Cd3 N6 O18.50' _chemical_formula_sum 'C62 H51 Cd3 N6 O18.50' _chemical_formula_weight 1513.29 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 8.1950(10) _cell_length_b 12.6310(10) _cell_length_c 14.2990(10) _cell_angle_alpha 98.7220(10) _cell_angle_beta 97.5150(10) _cell_angle_gamma 93.2990(10) _cell_volume 1445.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 757 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7656 _exptl_absorpt_correction_T_max 0.8342 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7340 _diffrn_reflns_av_R_equivalents 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5007 _reflns_number_gt 4524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.9171P] 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 5007 _refine_ls_number_parameters 420 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.5000 0.0000 0.0000 0.02925(7) Uani 1 2 d S . . Cd2 Cd 0.50547(2) -0.310745(13) 0.440048(11) 0.02368(6) Uani 1 1 d . . . C1 C 1.4246(3) 0.20405(19) 0.04257(17) 0.0278(5) Uani 1 1 d . . . C2 C 1.3879(3) 0.31931(18) 0.06169(17) 0.0269(5) Uani 1 1 d . . . C3 C 1.4320(3) 0.37997(19) 0.15203(17) 0.0289(5) Uani 1 1 d . . . H3 H 1.4928 0.3508 0.2001 0.035 Uiso 1 1 calc R . . C4 C 1.4224(3) 0.54817(19) 0.26960(17) 0.0291(5) Uani 1 1 d . . . C5 C 1.3852(3) 0.48405(18) 0.17037(16) 0.0268(5) Uani 1 1 d . . . C6 C 1.3010(3) 0.5291(2) 0.09738(17) 0.0328(6) Uani 1 1 d . . . H6 H 1.2704 0.5991 0.1097 0.039 Uiso 1 1 calc R . . C7 C 1.2622(3) 0.4704(2) 0.00613(17) 0.0335(6) Uani 1 1 d . . . C8 C 1.3034(3) 0.36458(19) -0.01097(17) 0.0312(6) Uani 1 1 d . . . H8 H 1.2741 0.3240 -0.0714 0.037 Uiso 1 1 calc R . . C9 C 1.1536(3) 0.6187(2) -0.05976(18) 0.0358(6) Uani 1 1 d . . . H9A H 1.2586 0.6614 -0.0445 0.043 Uiso 1 1 calc R . . H9B H 1.0895 0.6372 -0.0080 0.043 Uiso 1 1 calc R . . C10 C 1.0621(3) 0.6418(2) -0.15186(18) 0.0325(6) Uani 1 1 d . . . C11 C 0.9689(4) 0.7291(2) -0.15067(19) 0.0411(7) Uani 1 1 d . . . H11 H 0.9702 0.7762 -0.0938 0.049 Uiso 1 1 calc R . . C12 C 0.8732(3) 0.7480(2) -0.23293(19) 0.0396(6) Uani 1 1 d . . . H12 H 0.8112 0.8075 -0.2305 0.047 Uiso 1 1 calc R . . C13 C 0.8687(3) 0.6799(2) -0.31824(17) 0.0309(6) Uani 1 1 d . . . C14 C 0.9683(4) 0.5948(2) -0.3203(2) 0.0477(8) Uani 1 1 d . . . H14 H 0.9705 0.5495 -0.3777 0.057 Uiso 1 1 calc R . . C15 C 1.0649(4) 0.5762(2) -0.2380(2) 0.0496(8) Uani 1 1 d . . . H15 H 1.1318 0.5191 -0.2410 0.060 Uiso 1 1 calc R . . C16 C 0.7512(3) 0.6923(2) -0.40430(18) 0.0317(6) Uani 1 1 d . . . C17 C 1.1601(3) -0.0146(2) 0.0887(2) 0.0396(6) Uani 1 1 d . . . H17 H 1.1427 0.0430 0.0560 0.048 Uiso 1 1 calc R . . C18 C 1.0383(3) -0.0468(2) 0.1385(2) 0.0408(7) Uani 1 1 d . . . H18 H 0.9420 -0.0113 0.1388 0.049 Uiso 1 1 calc R . . C19 C 1.0598(3) -0.1324(2) 0.18819(17) 0.0288(5) Uani 1 1 d . . . C20 C 1.2078(3) -0.1799(2) 0.18521(19) 0.0357(6) Uani 1 1 d . . . H20 H 1.2295 -0.2365 0.2184 0.043 Uiso 1 1 calc R . . C21 C 1.3228(3) -0.1431(2) 0.13293(19) 0.0361(6) Uani 1 1 d . . . H21 H 1.4203 -0.1771 0.1312 0.043 Uiso 1 1 calc R . . C22 C 0.9342(3) -0.1687(2) 0.24448(17) 0.0289(5) Uani 1 1 d . . . C23 C 0.9417(3) -0.2647(2) 0.2803(2) 0.0399(7) Uani 1 1 d . . . H23 H 1.0253 -0.3092 0.2674 0.048 Uiso 1 1 calc R . . C24 C 0.8251(3) -0.2941(2) 0.3349(2) 0.0415(7) Uani 1 1 d . . . H24 H 0.8337 -0.3583 0.3588 0.050 Uiso 1 1 calc R . . C25 C 0.6926(3) -0.1438(2) 0.3194(2) 0.0430(7) Uani 1 1 d . . . H25 H 0.6063 -0.1015 0.3321 0.052 Uiso 1 1 calc R . . C26 C 0.8044(3) -0.1080(2) 0.2650(2) 0.0415(7) Uani 1 1 d . . . H26 H 0.7926 -0.0433 0.2421 0.050 Uiso 1 1 calc R . . C27 C 0.3125(4) -0.0886(2) 0.4334(2) 0.0478(8) Uani 1 1 d . . . H27 H 0.3971 -0.0720 0.3993 0.057 Uiso 1 1 calc R . . C28 C 0.1939(4) -0.0164(2) 0.4442(2) 0.0483(8) Uani 1 1 d . . . H28 H 0.2002 0.0464 0.4180 0.058 Uiso 1 1 calc R . . C29 C 0.0663(3) -0.03731(18) 0.49390(17) 0.0271(5) Uani 1 1 d . . . C30 C 0.0683(4) -0.1311(2) 0.5308(2) 0.0492(8) Uani 1 1 d . . . H30 H -0.0145 -0.1493 0.5656 0.059 Uiso 1 1 calc R . . C31 C 0.1921(4) -0.1991(2) 0.5168(2) 0.0517(8) Uani 1 1 d . . . H31 H 0.1896 -0.2620 0.5431 0.062 Uiso 1 1 calc R . . N1 N 1.3013(3) -0.06118(16) 0.08464(15) 0.0322(5) Uani 1 1 d . . . N2 N 0.7003(3) -0.23487(17) 0.35507(15) 0.0321(5) Uani 1 1 d . . . N3 N 0.3144(2) -0.17977(16) 0.46800(14) 0.0302(5) Uani 1 1 d . . . O1 O 1.5299(2) 0.16858(14) 0.09990(13) 0.0395(4) Uani 1 1 d . . . O2 O 1.3498(2) 0.14498(13) -0.03165(12) 0.0317(4) Uani 1 1 d . . . O3 O 1.5210(2) 0.51565(14) 0.33104(12) 0.0396(4) Uani 1 1 d . . . O4 O 1.3544(2) 0.63448(14) 0.28735(12) 0.0401(5) Uani 1 1 d . . . O5 O 1.1802(3) 0.50796(14) -0.07022(13) 0.0482(5) Uani 1 1 d . . . O6 O 0.7409(2) 0.62174(14) -0.47736(12) 0.0400(4) Uani 1 1 d . . . O7 O 0.6639(2) 0.77062(15) -0.40283(13) 0.0431(5) Uani 1 1 d . . . O1W O 0.3506(2) -0.40979(14) 0.52622(14) 0.0344(4) Uani 1 1 d D . . O2W O 0.5021(4) 0.0788(2) 0.2882(2) 0.1069(11) Uani 1 1 d D . . H2A H 0.4531 0.1237 0.3284 0.160 Uiso 1 1 d RD . . H2B H 0.5903 0.1215 0.2813 0.160 Uiso 1 1 d RD . . O3W O 0.7626(14) 0.1497(11) 0.2404(9) 0.102(4) Uani 0.25 1 d P . . H1A H 0.309(3) -0.4745(12) 0.4959(16) 0.051(9) Uiso 1 1 d D . . H1B H 0.396(4) -0.426(2) 0.5823(11) 0.067(11) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03384(15) 0.02027(13) 0.03757(15) 0.00619(10) 0.01608(11) 0.00611(10) Cd2 0.02680(10) 0.02377(10) 0.02103(9) 0.00393(7) 0.00290(7) 0.00700(7) C1 0.0302(13) 0.0257(13) 0.0295(13) 0.0045(10) 0.0105(11) 0.0042(10) C2 0.0320(13) 0.0231(12) 0.0263(12) 0.0041(10) 0.0050(10) 0.0067(10) C3 0.0321(13) 0.0276(13) 0.0273(13) 0.0060(10) 0.0013(10) 0.0076(10) C4 0.0356(14) 0.0262(13) 0.0244(13) 0.0032(10) 0.0016(11) 0.0020(11) C5 0.0321(13) 0.0239(12) 0.0239(12) 0.0040(10) 0.0003(10) 0.0051(10) C6 0.0446(15) 0.0224(13) 0.0294(13) 0.0018(10) -0.0017(11) 0.0098(11) C7 0.0454(15) 0.0285(13) 0.0251(13) 0.0048(10) -0.0040(11) 0.0106(12) C8 0.0390(14) 0.0271(13) 0.0254(13) 0.0002(10) 0.0002(11) 0.0068(11) C9 0.0448(16) 0.0293(14) 0.0313(14) 0.0048(11) -0.0056(12) 0.0110(12) C10 0.0353(14) 0.0312(14) 0.0300(13) 0.0067(11) -0.0028(11) 0.0052(11) C11 0.0547(18) 0.0355(15) 0.0291(14) -0.0018(11) -0.0059(12) 0.0145(13) C12 0.0459(16) 0.0339(15) 0.0371(15) 0.0043(12) -0.0051(12) 0.0164(12) C13 0.0314(13) 0.0326(14) 0.0283(13) 0.0082(11) -0.0006(11) 0.0026(11) C14 0.066(2) 0.0470(18) 0.0274(14) 0.0007(12) -0.0035(13) 0.0205(15) C15 0.067(2) 0.0443(17) 0.0353(16) 0.0018(13) -0.0055(14) 0.0284(15) C16 0.0324(14) 0.0326(14) 0.0299(14) 0.0115(11) -0.0006(11) -0.0044(11) C17 0.0403(16) 0.0400(16) 0.0466(17) 0.0224(13) 0.0143(13) 0.0106(12) C18 0.0333(14) 0.0451(16) 0.0538(18) 0.0244(14) 0.0183(13) 0.0146(12) C19 0.0297(13) 0.0300(13) 0.0274(13) 0.0056(10) 0.0056(10) 0.0021(10) C20 0.0393(15) 0.0339(14) 0.0405(15) 0.0158(12) 0.0150(12) 0.0110(12) C21 0.0367(15) 0.0345(15) 0.0429(16) 0.0112(12) 0.0164(12) 0.0130(12) C22 0.0297(13) 0.0316(13) 0.0255(12) 0.0042(10) 0.0049(10) 0.0021(10) C23 0.0427(16) 0.0357(15) 0.0480(17) 0.0106(13) 0.0225(13) 0.0119(12) C24 0.0485(17) 0.0315(15) 0.0527(18) 0.0148(13) 0.0257(14) 0.0079(12) C25 0.0375(15) 0.0524(18) 0.0477(17) 0.0201(14) 0.0185(13) 0.0173(13) C26 0.0421(16) 0.0436(16) 0.0478(17) 0.0228(13) 0.0175(13) 0.0137(13) C27 0.0451(17) 0.0435(17) 0.068(2) 0.0215(15) 0.0344(15) 0.0201(14) C28 0.0504(18) 0.0347(16) 0.073(2) 0.0236(15) 0.0343(16) 0.0189(13) C29 0.0273(13) 0.0247(13) 0.0284(13) 0.0008(10) 0.0035(10) 0.0061(10) C30 0.0457(17) 0.0383(16) 0.078(2) 0.0265(15) 0.0345(16) 0.0212(13) C31 0.0511(18) 0.0389(16) 0.079(2) 0.0299(16) 0.0288(17) 0.0236(14) N1 0.0338(12) 0.0288(11) 0.0370(12) 0.0074(9) 0.0133(9) 0.0038(9) N2 0.0315(11) 0.0368(12) 0.0300(11) 0.0078(9) 0.0089(9) 0.0031(9) N3 0.0298(11) 0.0298(11) 0.0318(11) 0.0028(9) 0.0062(9) 0.0109(9) O1 0.0499(11) 0.0282(10) 0.0374(10) 0.0010(8) -0.0041(9) 0.0142(8) O2 0.0372(10) 0.0251(9) 0.0315(9) 0.0001(7) 0.0035(8) 0.0051(7) O3 0.0560(12) 0.0345(10) 0.0248(9) 0.0038(8) -0.0099(8) 0.0115(9) O4 0.0532(12) 0.0304(10) 0.0319(10) -0.0055(8) -0.0056(8) 0.0174(9) O5 0.0796(15) 0.0308(10) 0.0281(10) 0.0008(8) -0.0179(10) 0.0201(10) O6 0.0520(12) 0.0348(10) 0.0293(10) 0.0075(8) -0.0090(8) -0.0010(9) O7 0.0461(11) 0.0467(12) 0.0361(11) 0.0115(9) -0.0051(9) 0.0131(9) O1W 0.0404(11) 0.0277(10) 0.0378(11) 0.0123(8) 0.0053(9) 0.0077(8) O2W 0.147(3) 0.088(2) 0.079(2) -0.0111(16) -0.0029(19) 0.059(2) O3W 0.081(8) 0.121(10) 0.108(10) 0.059(8) -0.006(7) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.317(2) . ? Cd1 N1 2.317(2) 2_855 ? Cd1 O2 2.3319(17) . ? Cd1 O2 2.3319(17) 2_855 ? Cd1 O1 2.3581(17) . ? Cd1 O1 2.3581(17) 2_855 ? Cd1 C1 2.683(2) 2_855 ? Cd2 O1W 2.3213(18) . ? Cd2 O4 2.3484(17) 1_445 ? Cd2 N3 2.3686(19) . ? Cd2 N2 2.372(2) . ? Cd2 O6 2.3963(18) 1_546 ? Cd2 O7 2.4845(18) 1_546 ? Cd2 O3 2.5103(17) 1_445 ? C1 O1 1.260(3) . ? C1 O2 1.263(3) . ? C1 C2 1.495(3) . ? C2 C8 1.387(3) . ? C2 C3 1.390(3) . ? C3 C5 1.387(3) . ? C3 H3 0.9300 . ? C4 O3 1.247(3) . ? C4 O4 1.260(3) . ? C4 C5 1.507(3) . ? C5 C6 1.388(3) . ? C6 C7 1.387(3) . ? C6 H6 0.9300 . ? C7 O5 1.367(3) . ? C7 C8 1.391(3) . ? C8 H8 0.9300 . ? C9 O5 1.416(3) . ? C9 C10 1.505(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.376(4) . ? C10 C15 1.380(4) . ? C11 C12 1.386(4) . ? C11 H11 0.9300 . ? C12 C13 1.377(4) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 C16 1.494(3) . ? C14 C15 1.388(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.253(3) . ? C16 O6 1.256(3) . ? C17 N1 1.332(3) . ? C17 C18 1.376(4) . ? C17 H17 0.9300 . ? C18 C19 1.388(4) . ? C18 H18 0.9300 . ? C19 C20 1.387(3) . ? C19 C22 1.480(3) . ? C20 C21 1.379(3) . ? C20 H20 0.9300 . ? C21 N1 1.336(3) . ? C21 H21 0.9300 . ? C22 C26 1.383(3) . ? C22 C23 1.387(4) . ? C23 C24 1.380(4) . ? C23 H23 0.9300 . ? C24 N2 1.337(3) . ? C24 H24 0.9300 . ? C25 N2 1.329(3) . ? C25 C26 1.377(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N3 1.320(3) . ? C27 C28 1.378(4) . ? C27 H27 0.9300 . ? C28 C29 1.373(3) . ? C28 H28 0.9300 . ? C29 C30 1.369(4) . ? C29 C29 1.489(4) 2_556 ? C30 C31 1.382(4) . ? C30 H30 0.9300 . ? C31 N3 1.325(3) . ? C31 H31 0.9300 . ? O3 Cd2 2.5103(17) 1_665 ? O4 Cd2 2.3484(17) 1_665 ? O6 Cd2 2.3963(18) 1_564 ? O7 Cd2 2.4845(18) 1_564 ? O1W H1A 0.891(10) . ? O1W H1B 0.896(10) . ? O2W H2A 0.8948 . ? O2W H2B 0.9011 . ? 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 N1 Cd1 N1 180.00(13) . 2_855 ? N1 Cd1 O2 91.41(7) . . ? N1 Cd1 O2 88.59(7) 2_855 . ? N1 Cd1 O2 88.59(7) . 2_855 ? N1 Cd1 O2 91.41(7) 2_855 2_855 ? O2 Cd1 O2 180.00(12) . 2_855 ? N1 Cd1 O1 90.66(7) . . ? N1 Cd1 O1 89.34(7) 2_855 . ? O2 Cd1 O1 56.06(6) . . ? O2 Cd1 O1 123.94(6) 2_855 . ? N1 Cd1 O1 89.34(7) . 2_855 ? N1 Cd1 O1 90.66(7) 2_855 2_855 ? O2 Cd1 O1 123.94(6) . 2_855 ? O2 Cd1 O1 56.06(6) 2_855 2_855 ? O1 Cd1 O1 180.00(10) . 2_855 ? N1 Cd1 C1 88.07(7) . 2_855 ? N1 Cd1 C1 91.93(7) 2_855 2_855 ? O2 Cd1 C1 151.93(7) . 2_855 ? O2 Cd1 C1 28.07(7) 2_855 2_855 ? O1 Cd1 C1 151.99(7) . 2_855 ? O1 Cd1 C1 28.01(7) 2_855 2_855 ? O1W Cd2 O4 98.88(7) . 1_445 ? O1W Cd2 N3 84.74(7) . . ? O4 Cd2 N3 88.10(6) 1_445 . ? O1W Cd2 N2 169.03(7) . . ? O4 Cd2 N2 83.87(7) 1_445 . ? N3 Cd2 N2 106.03(7) . . ? O1W Cd2 O6 85.68(6) . 1_546 ? O4 Cd2 O6 132.16(6) 1_445 1_546 ? N3 Cd2 O6 139.62(7) . 1_546 ? N2 Cd2 O6 84.65(7) . 1_546 ? O1W Cd2 O7 86.01(7) . 1_546 ? O4 Cd2 O7 172.79(6) 1_445 1_546 ? N3 Cd2 O7 87.07(7) . 1_546 ? N2 Cd2 O7 92.32(7) . 1_546 ? O6 Cd2 O7 53.15(6) 1_546 1_546 ? O1W Cd2 O3 86.61(6) . 1_445 ? O4 Cd2 O3 53.51(6) 1_445 1_445 ? N3 Cd2 O3 138.63(6) . 1_445 ? N2 Cd2 O3 86.55(7) . 1_445 ? O6 Cd2 O3 79.56(6) 1_546 1_445 ? O7 Cd2 O3 132.54(6) 1_546 1_445 ? O1 C1 O2 121.7(2) . . ? O1 C1 C2 119.5(2) . . ? O2 C1 C2 118.7(2) . . ? C8 C2 C3 119.9(2) . . ? C8 C2 C1 119.3(2) . . ? C3 C2 C1 120.8(2) . . ? C5 C3 C2 119.9(2) . . ? C5 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? O3 C4 O4 121.9(2) . . ? O3 C4 C5 119.5(2) . . ? O4 C4 C5 118.6(2) . . ? C3 C5 C6 119.9(2) . . ? C3 C5 C4 120.5(2) . . ? C6 C5 C4 119.6(2) . . ? C7 C6 C5 120.4(2) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O5 C7 C6 124.6(2) . . ? O5 C7 C8 115.9(2) . . ? C6 C7 C8 119.4(2) . . ? C2 C8 C7 120.3(2) . . ? C2 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? O5 C9 C10 108.9(2) . . ? O5 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O5 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C15 118.5(2) . . ? C11 C10 C9 119.6(2) . . ? C15 C10 C9 121.9(2) . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 120.9(2) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 118.0(2) . . ? C12 C13 C16 121.2(2) . . ? C14 C13 C16 120.7(2) . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C10 C15 C14 120.4(3) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O7 C16 O6 121.1(2) . . ? O7 C16 C13 120.5(2) . . ? O6 C16 C13 118.4(2) . . ? N1 C17 C18 123.8(2) . . ? N1 C17 H17 118.1 . . ? C18 C17 H17 118.1 . . ? C17 C18 C19 119.8(2) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 116.5(2) . . ? C20 C19 C22 121.6(2) . . ? C18 C19 C22 121.9(2) . . ? C21 C20 C19 120.0(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? N1 C21 C20 123.4(2) . . ? N1 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? C26 C22 C23 116.6(2) . . ? C26 C22 C19 121.7(2) . . ? C23 C22 C19 121.7(2) . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N2 C24 C23 123.3(2) . . ? N2 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? N2 C25 C26 124.1(3) . . ? N2 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C25 C26 C22 119.7(3) . . ? C25 C26 H26 120.2 . . ? C22 C26 H26 120.2 . . ? N3 C27 C28 124.6(2) . . ? N3 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C29 C28 C27 119.9(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 115.8(2) . . ? C30 C29 C29 122.2(3) . 2_556 ? C28 C29 C29 121.9(3) . 2_556 ? C29 C30 C31 120.6(3) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? N3 C31 C30 123.8(3) . . ? N3 C31 H31 118.1 . . ? C30 C31 H31 118.1 . . ? C17 N1 C21 116.6(2) . . ? C17 N1 Cd1 121.19(17) . . ? C21 N1 Cd1 122.21(17) . . ? C25 N2 C24 116.4(2) . . ? C25 N2 Cd2 127.12(17) . . ? C24 N2 Cd2 116.32(16) . . ? C27 N3 C31 115.3(2) . . ? C27 N3 Cd2 124.93(17) . . ? C31 N3 Cd2 119.63(17) . . ? C1 O1 Cd1 90.50(14) . . ? C1 O2 Cd1 91.63(14) . . ? C4 O3 Cd2 88.45(14) . 1_665 ? C4 O4 Cd2 95.69(14) . 1_665 ? C7 O5 C9 117.99(19) . . ? C16 O6 Cd2 94.60(15) . 1_564 ? C16 O7 Cd2 90.55(15) . 1_564 ? Cd2 O1W H1A 115.5(18) . . ? Cd2 O1W H1B 120(2) . . ? H1A O1W H1B 100.9(14) . . ? H2A O2W H2B 100.7 . . ? 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 O1 C1 C2 C8 164.9(2) . . . . ? O2 C1 C2 C8 -14.4(3) . . . . ? O1 C1 C2 C3 -17.5(4) . . . . ? O2 C1 C2 C3 163.2(2) . . . . ? C8 C2 C3 C5 2.7(4) . . . . ? C1 C2 C3 C5 -174.8(2) . . . . ? C2 C3 C5 C6 -2.9(4) . . . . ? C2 C3 C5 C4 176.0(2) . . . . ? O3 C4 C5 C3 13.1(4) . . . . ? O4 C4 C5 C3 -168.1(2) . . . . ? O3 C4 C5 C6 -168.0(2) . . . . ? O4 C4 C5 C6 10.8(4) . . . . ? C3 C5 C6 C7 0.4(4) . . . . ? C4 C5 C6 C7 -178.5(2) . . . . ? C5 C6 C7 O5 -179.8(3) . . . . ? C5 C6 C7 C8 2.2(4) . . . . ? C3 C2 C8 C7 -0.1(4) . . . . ? C1 C2 C8 C7 177.5(2) . . . . ? O5 C7 C8 C2 179.5(2) . . . . ? C6 C7 C8 C2 -2.4(4) . . . . ? O5 C9 C10 C11 155.7(3) . . . . ? O5 C9 C10 C15 -22.5(4) . . . . ? C15 C10 C11 C12 3.3(4) . . . . ? C9 C10 C11 C12 -175.0(3) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 -2.9(4) . . . . ? C11 C12 C13 C16 172.7(3) . . . . ? C12 C13 C14 C15 2.5(4) . . . . ? C16 C13 C14 C15 -173.1(3) . . . . ? C11 C10 C15 C14 -3.6(5) . . . . ? C9 C10 C15 C14 174.7(3) . . . . ? C13 C14 C15 C10 0.7(5) . . . . ? C12 C13 C16 O7 6.1(4) . . . . ? C14 C13 C16 O7 -178.4(3) . . . . ? C12 C13 C16 O6 -173.1(2) . . . . ? C14 C13 C16 O6 2.4(4) . . . . ? N1 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? C17 C18 C19 C22 178.7(3) . . . . ? C18 C19 C20 C21 -1.4(4) . . . . ? C22 C19 C20 C21 -179.2(2) . . . . ? C19 C20 C21 N1 1.1(4) . . . . ? C20 C19 C22 C26 165.6(2) . . . . ? C18 C19 C22 C26 -12.0(4) . . . . ? C20 C19 C22 C23 -13.7(4) . . . . ? C18 C19 C22 C23 168.6(3) . . . . ? C26 C22 C23 C24 -1.3(4) . . . . ? C19 C22 C23 C24 178.0(3) . . . . ? C22 C23 C24 N2 1.0(5) . . . . ? N2 C25 C26 C22 0.1(5) . . . . ? C23 C22 C26 C25 0.8(4) . . . . ? C19 C22 C26 C25 -178.5(3) . . . . ? N3 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 0.7(4) . . . . ? C27 C28 C29 C29 -178.9(3) . . . 2_556 ? C28 C29 C30 C31 -0.5(5) . . . . ? C29 C29 C30 C31 179.1(3) 2_556 . . . ? C29 C30 C31 N3 -0.2(5) . . . . ? C18 C17 N1 C21 -0.5(4) . . . . ? C18 C17 N1 Cd1 -179.4(2) . . . . ? C20 C21 N1 C17 -0.1(4) . . . . ? C20 C21 N1 Cd1 178.8(2) . . . . ? N1 Cd1 N1 C17 -123(100) 2_855 . . . ? O2 Cd1 N1 C17 5.7(2) . . . . ? O2 Cd1 N1 C17 -174.3(2) 2_855 . . . ? O1 Cd1 N1 C17 61.7(2) . . . . ? O1 Cd1 N1 C17 -118.3(2) 2_855 . . . ? C1 Cd1 N1 C17 -146.3(2) 2_855 . . . ? N1 Cd1 N1 C21 58(100) 2_855 . . . ? O2 Cd1 N1 C21 -173.2(2) . . . . ? O2 Cd1 N1 C21 6.8(2) 2_855 . . . ? O1 Cd1 N1 C21 -117.1(2) . . . . ? O1 Cd1 N1 C21 62.9(2) 2_855 . . . ? C1 Cd1 N1 C21 34.9(2) 2_855 . . . ? C26 C25 N2 C24 -0.5(4) . . . . ? C26 C25 N2 Cd2 -175.3(2) . . . . ? C23 C24 N2 C25 0.0(4) . . . . ? C23 C24 N2 Cd2 175.3(2) . . . . ? O1W Cd2 N2 C25 -176.5(3) . . . . ? O4 Cd2 N2 C25 78.4(2) 1_445 . . . ? N3 Cd2 N2 C25 -7.9(2) . . . . ? O6 Cd2 N2 C25 -148.2(2) 1_546 . . . ? O7 Cd2 N2 C25 -95.5(2) 1_546 . . . ? O3 Cd2 N2 C25 132.0(2) 1_445 . . . ? O1W Cd2 N2 C24 8.8(5) . . . . ? O4 Cd2 N2 C24 -96.40(19) 1_445 . . . ? N3 Cd2 N2 C24 177.35(19) . . . . ? O6 Cd2 N2 C24 37.08(19) 1_546 . . . ? O7 Cd2 N2 C24 89.73(19) 1_546 . . . ? O3 Cd2 N2 C24 -42.75(19) 1_445 . . . ? C28 C27 N3 C31 -0.7(5) . . . . ? C28 C27 N3 Cd2 175.1(2) . . . . ? C30 C31 N3 C27 0.8(5) . . . . ? C30 C31 N3 Cd2 -175.2(3) . . . . ? O1W Cd2 N3 C27 -176.1(2) . . . . ? O4 Cd2 N3 C27 -77.0(2) 1_445 . . . ? N2 Cd2 N3 C27 6.0(2) . . . . ? O6 Cd2 N3 C27 106.9(2) 1_546 . . . ? O7 Cd2 N3 C27 97.6(2) 1_546 . . . ? O3 Cd2 N3 C27 -97.3(2) 1_445 . . . ? O1W Cd2 N3 C31 -0.5(2) . . . . ? O4 Cd2 N3 C31 98.6(2) 1_445 . . . ? N2 Cd2 N3 C31 -178.4(2) . . . . ? O6 Cd2 N3 C31 -77.5(2) 1_546 . . . ? O7 Cd2 N3 C31 -86.8(2) 1_546 . . . ? O3 Cd2 N3 C31 78.3(2) 1_445 . . . ? O2 C1 O1 Cd1 2.9(2) . . . . ? C2 C1 O1 Cd1 -176.34(19) . . . . ? N1 Cd1 O1 C1 -92.87(15) . . . . ? N1 Cd1 O1 C1 87.13(15) 2_855 . . . ? O2 Cd1 O1 C1 -1.61(13) . . . . ? O2 Cd1 O1 C1 178.39(13) 2_855 . . . ? O1 Cd1 O1 C1 -133(100) 2_855 . . . ? C1 Cd1 O1 C1 180.0 2_855 . . . ? O1 C1 O2 Cd1 -2.9(2) . . . . ? C2 C1 O2 Cd1 176.32(19) . . . . ? N1 Cd1 O2 C1 91.45(14) . . . . ? N1 Cd1 O2 C1 -88.55(14) 2_855 . . . ? O2 Cd1 O2 C1 179(100) 2_855 . . . ? O1 Cd1 O2 C1 1.61(13) . . . . ? O1 Cd1 O2 C1 -178.39(13) 2_855 . . . ? C1 Cd1 O2 C1 180.0 2_855 . . . ? O4 C4 O3 Cd2 -6.2(2) . . . 1_665 ? C5 C4 O3 Cd2 172.5(2) . . . 1_665 ? O3 C4 O4 Cd2 6.7(3) . . . 1_665 ? C5 C4 O4 Cd2 -172.07(19) . . . 1_665 ? C6 C7 O5 C9 9.6(4) . . . . ? C8 C7 O5 C9 -172.4(2) . . . . ? C10 C9 O5 C7 179.9(2) . . . . ? O7 C16 O6 Cd2 -8.2(2) . . . 1_564 ? C13 C16 O6 Cd2 171.00(19) . . . 1_564 ? O6 C16 O7 Cd2 7.8(2) . . . 1_564 ? C13 C16 O7 Cd2 -171.3(2) . . . 1_564 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.267 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.055 #===========================end data_complex-3 _database_code_depnum_ccdc_archive 'CCDC 743098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Co N2 O8' _chemical_formula_sum 'C26 H20 Co N2 O8' _chemical_formula_weight 547.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c 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 11.410(2) _cell_length_b 16.341(3) _cell_length_c 13.791(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.474(4) _cell_angle_gamma 90.00 _cell_volume 2543.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8392 _exptl_absorpt_correction_T_max 0.8683 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 12713 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4472 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.9536P] 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 4472 _refine_ls_number_parameters 346 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Co Co 0.45960(4) 0.11699(3) 0.46719(4) 0.02201(18) Uani 1 1 d . . . C1 C 0.5298(3) 0.4668(2) 0.1657(3) 0.0242(9) Uani 1 1 d . . . C2 C 0.5514(3) 0.4452(2) 0.2718(3) 0.0255(9) Uani 1 1 d . . . C3 C 0.5088(3) 0.3714(2) 0.3029(3) 0.0278(10) Uani 1 1 d . . . H3 H 0.4645 0.3369 0.2579 0.033 Uiso 1 1 calc R . . C4 C 0.5320(4) 0.3494(3) 0.4001(3) 0.0284(9) Uani 1 1 d . . . C5 C 0.5978(4) 0.4008(3) 0.4685(3) 0.0406(12) Uani 1 1 d . . . H5 H 0.6115 0.3864 0.5344 0.049 Uiso 1 1 calc R . . C6 C 0.6425(4) 0.4735(3) 0.4372(3) 0.0385(11) Uani 1 1 d . . . C7 C 0.6176(4) 0.4962(3) 0.3391(3) 0.0329(10) Uani 1 1 d . . . H7 H 0.6455 0.5458 0.3187 0.039 Uiso 1 1 calc R . . C8 C 0.4918(3) 0.2671(3) 0.4300(3) 0.0289(10) Uani 1 1 d . . . C9 C 0.7545(5) 0.5025(4) 0.5945(4) 0.0711(18) Uani 1 1 d . . . H9A H 0.7859 0.4473 0.5970 0.085 Uiso 1 1 calc R . . H9B H 0.6902 0.5047 0.6333 0.085 Uiso 1 1 calc R . . C10 C 0.8508(5) 0.5629(4) 0.6333(4) 0.0583(16) Uani 1 1 d . . . C11 C 0.9689(6) 0.5450(4) 0.6326(5) 0.0790(19) Uani 1 1 d . . . H11 H 0.9897 0.4939 0.6106 0.095 Uiso 1 1 calc R . . C12 C 1.0579(6) 0.6019(4) 0.6640(5) 0.0743(18) Uani 1 1 d . . . H12 H 1.1370 0.5890 0.6627 0.089 Uiso 1 1 calc R . . C13 C 1.0268(5) 0.6780(3) 0.6972(4) 0.0512(14) Uani 1 1 d . . . C14 C 0.9091(5) 0.6965(4) 0.6982(4) 0.0623(16) Uani 1 1 d . . . H14 H 0.8883 0.7472 0.7210 0.075 Uiso 1 1 calc R . . C15 C 0.8223(5) 0.6403(4) 0.6656(5) 0.0708(18) Uani 1 1 d . . . H15 H 0.7432 0.6543 0.6650 0.085 Uiso 1 1 calc R . . C16 C 1.1188(5) 0.7379(4) 0.7369(4) 0.0539(14) Uani 1 1 d D . . C17 C 0.7247(4) 0.1337(4) 0.5450(4) 0.0584(16) Uani 1 1 d . . . H17 H 0.6944 0.1500 0.6010 0.070 Uiso 1 1 calc R . . C18 C 0.8454(4) 0.1374(4) 0.5459(4) 0.0652(18) Uani 1 1 d . . . H18 H 0.8938 0.1568 0.6013 0.078 Uiso 1 1 calc R . . C19 C 0.8951(3) 0.1127(3) 0.4655(3) 0.0323(10) Uani 1 1 d . . . C20 C 0.8172(4) 0.0845(3) 0.3878(3) 0.0393(11) Uani 1 1 d . . . H20 H 0.8452 0.0656 0.3319 0.047 Uiso 1 1 calc R . . C21 C 0.6981(4) 0.0841(3) 0.3920(3) 0.0372(11) Uani 1 1 d . . . H21 H 0.6478 0.0655 0.3372 0.045 Uiso 1 1 calc R . . C22 C 1.0250(3) 0.1164(3) 0.4646(3) 0.0324(10) Uani 1 1 d . . . C23 C 1.0769(4) 0.0853(4) 0.3896(4) 0.0670(18) Uani 1 1 d . . . H23 H 1.0300 0.0619 0.3359 0.080 Uiso 1 1 calc R . . C24 C 1.1973(4) 0.0883(4) 0.3925(4) 0.0615(17) Uani 1 1 d . . . H24 H 1.2293 0.0648 0.3409 0.074 Uiso 1 1 calc R . . C25 C 1.2208(4) 0.1536(4) 0.5345(5) 0.079(2) Uani 1 1 d . . . H25 H 1.2697 0.1782 0.5863 0.095 Uiso 1 1 calc R . . C26 C 1.1013(4) 0.1528(5) 0.5377(4) 0.083(2) Uani 1 1 d . . . H26 H 1.0719 0.1771 0.5901 0.100 Uiso 1 1 calc R . . H6 H 1.264(2) 0.754(4) 0.761(5) 0.15(4) Uiso 1 1 d D . . H1A H 0.553(4) 0.289(3) 0.647(2) 0.08(2) Uiso 1 1 d D . . H1B H 0.541(4) 0.300(4) 0.746(3) 0.09(2) Uiso 1 1 d D . . N1 N 0.6495(3) 0.1082(2) 0.4686(3) 0.0319(8) Uani 1 1 d . . . N2 N 1.2706(3) 0.1224(2) 0.4638(3) 0.0306(8) Uani 1 1 d . . . O1 O 0.5709(2) 0.53442(17) 0.1409(2) 0.0307(7) Uani 1 1 d . . . O2 O 0.4723(2) 0.41699(17) 0.1081(2) 0.0320(7) Uani 1 1 d . . . O3 O 0.4594(3) 0.21499(17) 0.3636(2) 0.0355(7) Uani 1 1 d . . . O4 O 0.4942(3) 0.24827(17) 0.5187(2) 0.0360(7) Uani 1 1 d . . . O5 O 0.7139(3) 0.5258(2) 0.4961(2) 0.0637(12) Uani 1 1 d . . . O6 O 1.2275(4) 0.7182(3) 0.7215(3) 0.0696(11) Uani 1 1 d D . . O7 O 1.0985(4) 0.7995(3) 0.7807(3) 0.0697(11) Uani 1 1 d . . . O1W O 0.5898(3) 0.3090(2) 0.7031(3) 0.0491(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0210(3) 0.0235(3) 0.0218(3) -0.0001(2) 0.0043(2) 0.0000(2) C1 0.020(2) 0.027(2) 0.027(2) -0.0023(18) 0.0056(17) 0.0057(17) C2 0.029(2) 0.026(2) 0.021(2) 0.0034(17) 0.0030(17) -0.0016(18) C3 0.028(2) 0.024(2) 0.030(2) 0.0000(17) 0.0003(17) -0.0035(18) C4 0.036(2) 0.026(2) 0.024(2) 0.0063(18) 0.0059(18) -0.0052(19) C5 0.053(3) 0.039(3) 0.028(3) 0.007(2) -0.002(2) -0.010(2) C6 0.051(3) 0.035(3) 0.027(3) -0.001(2) -0.002(2) -0.016(2) C7 0.044(3) 0.024(2) 0.030(3) 0.0038(19) 0.0023(19) -0.011(2) C8 0.025(2) 0.032(2) 0.030(3) 0.003(2) 0.0021(18) -0.0027(18) C9 0.091(5) 0.079(4) 0.038(3) -0.001(3) -0.008(3) -0.034(4) C10 0.065(4) 0.073(4) 0.033(3) -0.003(3) -0.006(3) -0.024(3) C11 0.090(5) 0.066(4) 0.078(5) -0.021(4) 0.004(4) -0.013(4) C12 0.059(4) 0.087(5) 0.074(5) -0.017(4) -0.001(3) -0.008(3) C13 0.053(3) 0.056(4) 0.041(3) 0.000(3) -0.006(2) -0.015(3) C14 0.059(4) 0.063(4) 0.063(4) -0.007(3) 0.001(3) -0.010(3) C15 0.054(4) 0.084(5) 0.071(4) -0.007(4) -0.003(3) -0.016(3) C16 0.060(4) 0.060(4) 0.041(3) 0.006(3) 0.004(3) -0.003(3) C17 0.026(3) 0.103(5) 0.047(3) -0.036(3) 0.008(2) -0.001(3) C18 0.023(2) 0.130(6) 0.040(3) -0.038(3) -0.002(2) -0.006(3) C19 0.023(2) 0.041(3) 0.032(3) -0.004(2) 0.0038(18) 0.002(2) C20 0.029(2) 0.056(3) 0.035(3) -0.008(2) 0.014(2) -0.007(2) C21 0.026(2) 0.055(3) 0.031(3) -0.007(2) 0.0040(19) -0.011(2) C22 0.021(2) 0.043(3) 0.033(3) 0.000(2) 0.0033(18) 0.001(2) C23 0.025(3) 0.122(5) 0.051(4) -0.035(3) -0.002(2) 0.004(3) C24 0.030(3) 0.120(5) 0.035(3) -0.029(3) 0.005(2) 0.007(3) C25 0.031(3) 0.134(6) 0.073(4) -0.067(4) 0.013(3) -0.013(3) C26 0.026(3) 0.159(6) 0.069(4) -0.069(4) 0.017(3) -0.013(3) N1 0.0251(18) 0.043(2) 0.028(2) -0.0019(17) 0.0037(15) -0.0002(17) N2 0.0245(18) 0.036(2) 0.032(2) 0.0001(17) 0.0052(15) 0.0028(16) O1 0.0287(16) 0.0327(17) 0.0299(17) 0.0091(13) 0.0014(13) -0.0050(13) O2 0.0353(17) 0.0353(17) 0.0254(17) -0.0018(13) 0.0042(13) -0.0055(14) O3 0.0443(18) 0.0307(17) 0.0311(18) 0.0046(14) 0.0047(14) -0.0086(14) O4 0.0469(18) 0.0347(17) 0.0269(18) 0.0084(13) 0.0076(14) -0.0051(14) O5 0.099(3) 0.054(2) 0.029(2) 0.0037(16) -0.0209(19) -0.041(2) O6 0.055(3) 0.080(3) 0.071(3) -0.004(2) 0.001(2) -0.011(2) O7 0.072(3) 0.066(3) 0.070(3) -0.007(2) 0.008(2) -0.018(2) O1W 0.049(2) 0.061(2) 0.037(2) -0.0010(18) 0.0036(18) -0.0048(18) _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 Co O1 2.003(3) 2_645 ? Co O2 2.006(3) 4_566 ? Co O3 2.146(3) . ? Co N2 2.151(3) 1_455 ? Co N1 2.169(3) . ? Co O4 2.276(3) . ? C1 O2 1.254(5) . ? C1 O1 1.267(5) . ? C1 C2 1.489(5) . ? C2 C7 1.386(5) . ? C2 C3 1.391(5) . ? C3 C4 1.376(5) . ? C3 H3 0.9300 . ? C4 C5 1.397(6) . ? C4 C8 1.499(6) . ? C5 C6 1.386(6) . ? C5 H5 0.9300 . ? C6 O5 1.363(5) . ? C6 C7 1.391(6) . ? C7 H7 0.9300 . ? C8 O4 1.258(5) . ? C8 O3 1.264(5) . ? C9 O5 1.420(6) . ? C9 C10 1.515(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.380(8) . ? C10 C15 1.395(8) . ? C11 C12 1.398(8) . ? C11 H11 0.9300 . ? C12 C13 1.388(8) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C13 C16 1.481(7) . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.213(6) . ? C16 O6 1.329(7) . ? C17 N1 1.324(5) . ? C17 C18 1.376(6) . ? C17 H17 0.9300 . ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 C20 1.368(6) . ? C19 C22 1.485(5) . ? C20 C21 1.368(6) . ? C20 H20 0.9300 . ? C21 N1 1.323(5) . ? C21 H21 0.9300 . ? C22 C23 1.363(6) . ? C22 C26 1.368(6) . ? C23 C24 1.370(6) . ? C23 H23 0.9300 . ? C24 N2 1.317(6) . ? C24 H24 0.9300 . ? C25 N2 1.302(6) . ? C25 C26 1.371(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N2 Co 2.151(3) 1_655 ? O1 Co 2.003(3) 2_655 ? O2 Co 2.006(3) 4_565 ? O6 H6 0.87(2) . ? O1W H1A 0.883(19) . ? O1W H1B 0.885(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co O2 120.96(12) 2_645 4_566 ? O1 Co O3 91.41(12) 2_645 . ? O2 Co O3 147.60(12) 4_566 . ? O1 Co N2 87.02(12) 2_645 1_455 ? O2 Co N2 87.79(12) 4_566 1_455 ? O3 Co N2 92.99(12) . 1_455 ? O1 Co N1 91.48(12) 2_645 . ? O2 Co N1 92.50(12) 4_566 . ? O3 Co N1 87.61(12) . . ? N2 Co N1 178.41(13) 1_455 . ? O1 Co O4 150.52(11) 2_645 . ? O2 Co O4 88.51(11) 4_566 . ? O3 Co O4 59.15(11) . . ? N2 Co O4 95.45(12) 1_455 . ? N1 Co O4 86.13(12) . . ? O2 C1 O1 125.1(4) . . ? O2 C1 C2 117.6(4) . . ? O1 C1 C2 117.3(3) . . ? C7 C2 C3 119.7(4) . . ? C7 C2 C1 120.7(4) . . ? C3 C2 C1 119.6(4) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 C8 118.7(4) . . ? C5 C4 C8 120.7(4) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? O5 C6 C5 124.5(4) . . ? O5 C6 C7 115.5(4) . . ? C5 C6 C7 119.9(4) . . ? C2 C7 C6 120.3(4) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? O4 C8 O3 120.1(4) . . ? O4 C8 C4 121.5(4) . . ? O3 C8 C4 118.3(4) . . ? O5 C9 C10 106.3(4) . . ? O5 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O5 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? C11 C10 C15 118.0(5) . . ? C11 C10 C9 121.1(6) . . ? C15 C10 C9 120.8(6) . . ? C10 C11 C12 121.4(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 C16 119.3(5) . . ? C12 C13 C16 120.9(5) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 121.2(6) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O7 C16 O6 122.1(5) . . ? O7 C16 C13 123.8(6) . . ? O6 C16 C13 114.1(5) . . ? N1 C17 C18 123.5(5) . . ? N1 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 115.6(4) . . ? C20 C19 C22 122.8(4) . . ? C18 C19 C22 121.6(4) . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? N1 C21 C20 124.6(4) . . ? N1 C21 H21 117.7 . . ? C20 C21 H21 117.7 . . ? C23 C22 C26 114.9(4) . . ? C23 C22 C19 122.5(4) . . ? C26 C22 C19 122.6(4) . . ? C22 C23 C24 120.7(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? N2 C24 C23 124.1(5) . . ? N2 C24 H24 117.9 . . ? C23 C24 H24 117.9 . . ? N2 C25 C26 124.5(5) . . ? N2 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C22 C26 C25 120.6(5) . . ? C22 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C21 N1 C17 115.4(4) . . ? C21 N1 Co 123.3(3) . . ? C17 N1 Co 121.1(3) . . ? C25 N2 C24 115.2(4) . . ? C25 N2 Co 123.1(3) . 1_655 ? C24 N2 Co 121.5(3) . 1_655 ? C1 O1 Co 139.3(3) . 2_655 ? C1 O2 Co 138.6(3) . 4_565 ? C8 O3 Co 92.8(2) . . ? C8 O4 Co 87.1(2) . . ? C6 O5 C9 119.0(4) . . ? C16 O6 H6 96(2) . . ? H1A O1W H1B 105(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 177.9(4) . . . . ? O1 C1 C2 C7 -2.3(6) . . . . ? O2 C1 C2 C3 0.6(5) . . . . ? O1 C1 C2 C3 -179.7(4) . . . . ? C7 C2 C3 C4 0.2(6) . . . . ? C1 C2 C3 C4 177.6(4) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? C2 C3 C4 C8 -175.9(4) . . . . ? C3 C4 C5 C6 -1.7(7) . . . . ? C8 C4 C5 C6 174.5(4) . . . . ? C4 C5 C6 O5 -175.7(5) . . . . ? C4 C5 C6 C7 2.6(7) . . . . ? C3 C2 C7 C6 0.7(7) . . . . ? C1 C2 C7 C6 -176.7(4) . . . . ? O5 C6 C7 C2 176.3(4) . . . . ? C5 C6 C7 C2 -2.1(7) . . . . ? C3 C4 C8 O4 -169.1(4) . . . . ? C5 C4 C8 O4 14.6(6) . . . . ? C3 C4 C8 O3 13.7(6) . . . . ? C5 C4 C8 O3 -162.5(4) . . . . ? O5 C9 C10 C11 -96.0(7) . . . . ? O5 C9 C10 C15 80.2(7) . . . . ? C15 C10 C11 C12 0.7(9) . . . . ? C9 C10 C11 C12 177.0(6) . . . . ? C10 C11 C12 C13 0.4(10) . . . . ? C11 C12 C13 C14 -0.4(9) . . . . ? C11 C12 C13 C16 176.2(5) . . . . ? C12 C13 C14 C15 -0.6(9) . . . . ? C16 C13 C14 C15 -177.3(5) . . . . ? C13 C14 C15 C10 1.7(9) . . . . ? C11 C10 C15 C14 -1.7(9) . . . . ? C9 C10 C15 C14 -178.0(5) . . . . ? C14 C13 C16 O7 8.6(8) . . . . ? C12 C13 C16 O7 -168.0(6) . . . . ? C14 C13 C16 O6 -172.2(5) . . . . ? C12 C13 C16 O6 11.1(8) . . . . ? N1 C17 C18 C19 -1.1(10) . . . . ? C17 C18 C19 C20 -0.6(8) . . . . ? C17 C18 C19 C22 179.8(5) . . . . ? C18 C19 C20 C21 1.7(7) . . . . ? C22 C19 C20 C21 -178.7(4) . . . . ? C19 C20 C21 N1 -1.3(8) . . . . ? C20 C19 C22 C23 -5.8(8) . . . . ? C18 C19 C22 C23 173.8(6) . . . . ? C20 C19 C22 C26 172.6(5) . . . . ? C18 C19 C22 C26 -7.8(8) . . . . ? C26 C22 C23 C24 2.9(9) . . . . ? C19 C22 C23 C24 -178.6(5) . . . . ? C22 C23 C24 N2 -2.1(10) . . . . ? C23 C22 C26 C25 -2.4(10) . . . . ? C19 C22 C26 C25 179.1(6) . . . . ? N2 C25 C26 C22 1.1(12) . . . . ? C20 C21 N1 C17 -0.3(7) . . . . ? C20 C21 N1 Co 174.2(4) . . . . ? C18 C17 N1 C21 1.5(8) . . . . ? C18 C17 N1 Co -173.1(5) . . . . ? O1 Co N1 C21 24.4(4) 2_645 . . . ? O2 Co N1 C21 145.4(4) 4_566 . . . ? O3 Co N1 C21 -67.0(4) . . . . ? N2 Co N1 C21 45(5) 1_455 . . . ? O4 Co N1 C21 -126.2(4) . . . . ? O1 Co N1 C17 -161.5(4) 2_645 . . . ? O2 Co N1 C17 -40.4(4) 4_566 . . . ? O3 Co N1 C17 107.2(4) . . . . ? N2 Co N1 C17 -141(5) 1_455 . . . ? O4 Co N1 C17 48.0(4) . . . . ? C26 C25 N2 C24 -0.1(10) . . . . ? C26 C25 N2 Co -175.1(6) . . . 1_655 ? C23 C24 N2 C25 0.6(9) . . . . ? C23 C24 N2 Co 175.7(5) . . . 1_655 ? O2 C1 O1 Co 23.9(6) . . . 2_655 ? C2 C1 O1 Co -155.8(3) . . . 2_655 ? O1 C1 O2 Co 28.6(6) . . . 4_565 ? C2 C1 O2 Co -151.7(3) . . . 4_565 ? O4 C8 O3 Co -9.5(4) . . . . ? C4 C8 O3 Co 167.8(3) . . . . ? O1 Co O3 C8 -173.1(2) 2_645 . . . ? O2 Co O3 C8 9.2(4) 4_566 . . . ? N2 Co O3 C8 99.8(3) 1_455 . . . ? N1 Co O3 C8 -81.7(3) . . . . ? O4 Co O3 C8 5.3(2) . . . . ? O3 C8 O4 Co 8.9(4) . . . . ? C4 C8 O4 Co -168.2(4) . . . . ? O1 Co O4 C8 -1.9(4) 2_645 . . . ? O2 Co O4 C8 176.8(2) 4_566 . . . ? O3 Co O4 C8 -5.3(2) . . . . ? N2 Co O4 C8 -95.5(2) 1_455 . . . ? N1 Co O4 C8 84.2(2) . . . . ? C5 C6 O5 C9 5.5(8) . . . . ? C7 C6 O5 C9 -172.9(5) . . . . ? C10 C9 O5 C6 168.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O1W 0.87(2) 1.90(2) 2.644(5) 144(4) 2_756 O1W H1A O4 0.883(19) 1.92(2) 2.798(5) 172(5) . O1W H1B O3 0.885(19) 2.00(2) 2.870(5) 169(5) 4_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.917 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.075 # Attachment '4.cif' data_complex-4 _database_code_depnum_ccdc_archive 'CCDC 743099' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H14 Co2 N O10.25' _chemical_formula_sum 'C21 H14 Co2 N O10.25' _chemical_formula_weight 562.19 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' Co Co 0.3494 0.9721 '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 8.2632(8) _cell_length_b 11.0605(11) _cell_length_c 12.7617(12) _cell_angle_alpha 80.7092(12) _cell_angle_beta 81.0167(13) _cell_angle_gamma 69.1695(11) _cell_volume 1069.64(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 566 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7282 _exptl_absorpt_correction_T_max 0.8058 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5476 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3720 _reflns_number_gt 2926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered C atoms (C17,C18,C20,C21)were refined using C atoms split over two sites, with a total occupancy of 1.The ISOR instructions were applied for C9 C17B C18B C20B O3W atoms owing to the higher temperature parameters. The DFIX instructions were used to restrain the bond length between C8 and H8. ; _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^+1.8622P] 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 3720 _refine_ls_number_parameters 358 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.048 _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 Co1 Co 0.51321(7) 0.52488(5) 0.37153(4) 0.01983(17) Uani 1 1 d . . . Co2 Co 0.19873(8) 0.73526(6) 0.47684(5) 0.0334(2) Uani 1 1 d . . . C1 C -0.5698(6) 1.2232(4) -0.3936(4) 0.0287(10) Uani 1 1 d . . . C2 C -0.5222(6) 1.0830(4) -0.3451(4) 0.0276(10) Uani 1 1 d . . . C3 C -0.5970(6) 0.9995(4) -0.3726(3) 0.0259(9) Uani 1 1 d . . . H3 H -0.6790 1.0296 -0.4216 0.031 Uiso 1 1 calc R . . C4 C -0.5485(6) 0.8709(4) -0.3264(3) 0.0276(10) Uani 1 1 d . . . C5 C -0.4320(7) 0.8278(4) -0.2502(4) 0.0391(12) Uani 1 1 d . . . H5 H -0.4010 0.7420 -0.2185 0.047 Uiso 1 1 calc R . . C6 C -0.3616(7) 0.9122(5) -0.2209(4) 0.0446(14) Uani 1 1 d . . . C7 C -0.4042(7) 1.0395(5) -0.2700(4) 0.0398(12) Uani 1 1 d . . . H7 H -0.3535 1.0952 -0.2524 0.048 Uiso 1 1 calc R . . C8 C -0.6125(6) 0.7748(5) -0.3638(4) 0.0310(11) Uani 1 1 d . . . C9 C -0.1530(11) 0.9362(7) -0.1225(6) 0.090(3) Uani 1 1 d U . . H9A H -0.2275 1.0242 -0.1106 0.108 Uiso 1 1 calc R . . H9B H -0.0681 0.9406 -0.1834 0.108 Uiso 1 1 calc R . . C10 C -0.0626(11) 0.8678(6) -0.0247(6) 0.071(2) Uani 1 1 d . . . C11 C 0.1091(10) 0.7885(7) -0.0310(5) 0.070(2) Uani 1 1 d . . . H11 H 0.1723 0.7755 -0.0976 0.084 Uiso 1 1 calc R . . C12 C 0.1895(8) 0.7278(6) 0.0599(4) 0.0520(15) Uani 1 1 d . . . H12 H 0.3048 0.6727 0.0538 0.062 Uiso 1 1 calc R . . C13 C 0.0996(7) 0.7484(5) 0.1594(4) 0.0388(12) Uani 1 1 d . . . C14 C -0.0715(8) 0.8288(6) 0.1654(5) 0.0586(16) Uani 1 1 d . . . H14 H -0.1338 0.8448 0.2319 0.070 Uiso 1 1 calc R . . C15 C -0.1530(9) 0.8863(6) 0.0738(6) 0.072(2) Uani 1 1 d . . . H15 H -0.2700 0.9379 0.0796 0.086 Uiso 1 1 calc R . . C16 C 0.1852(6) 0.6929(5) 0.2598(4) 0.0351(11) Uani 1 1 d . A . C19 C 0.9395(6) 0.5078(4) 0.0496(4) 0.0328(11) Uani 1 1 d . . . C17A C 0.665(2) 0.6130(14) 0.1488(13) 0.036(3) Uani 0.66(3) 1 d P A 1 H17A H 0.5574 0.6798 0.1511 0.043 Uiso 0.66(3) 1 calc PR A 1 C18A C 0.7720(18) 0.6047(13) 0.0561(12) 0.033(3) Uani 0.66(3) 1 d P A 1 H18A H 0.7354 0.6632 -0.0036 0.040 Uiso 0.66(3) 1 calc PR A 1 C20A C 0.9758(19) 0.424(2) 0.1407(10) 0.057(5) Uani 0.66(3) 1 d P A 1 H20A H 1.0816 0.3555 0.1418 0.068 Uiso 0.66(3) 1 calc PR A 1 C21A C 0.857(2) 0.439(2) 0.2320(12) 0.056(5) Uani 0.66(3) 1 d P A 1 H21A H 0.8876 0.3804 0.2927 0.068 Uiso 0.66(3) 1 calc PR A 1 C17B C 0.660(4) 0.567(4) 0.140(3) 0.052(8) Uani 0.34(3) 1 d PU A 2 H17B H 0.5420 0.6063 0.1334 0.062 Uiso 0.34(3) 1 calc PR A 2 C18B C 0.774(4) 0.555(4) 0.045(2) 0.051(8) Uani 0.34(3) 1 d PU A 2 H18B H 0.7293 0.5816 -0.0207 0.061 Uiso 0.34(3) 1 calc PR A 2 C20B C 1.000(3) 0.473(2) 0.1510(17) 0.024(4) Uani 0.34(3) 1 d PU A 2 H20B H 1.1192 0.4427 0.1573 0.029 Uiso 0.34(3) 1 calc PR A 2 C21B C 0.884(4) 0.483(3) 0.239(2) 0.029(5) Uani 0.34(3) 1 d P A 2 H21B H 0.9267 0.4575 0.3056 0.034 Uiso 0.34(3) 1 calc PR A 2 H8 H 0.268(7) 0.495(5) 0.504(5) 0.057(19) Uiso 1 1 d D . . N1 N 0.7058(5) 0.5291(4) 0.2372(3) 0.0304(9) Uani 1 1 d . . . O1 O -0.4614(4) 1.2794(3) -0.3878(2) 0.0270(7) Uani 1 1 d . . . O2 O -0.7088(5) 1.2771(3) -0.4336(3) 0.0467(9) Uani 1 1 d . . . O3 O -0.7438(4) 0.8197(3) -0.4146(3) 0.0422(9) Uani 1 1 d . . . O4 O -0.5264(5) 0.6568(3) -0.3428(3) 0.0389(8) Uani 1 1 d . . . O5 O -0.2544(6) 0.8622(4) -0.1414(4) 0.0736(15) Uani 1 1 d . . . O6 O 0.3233(4) 0.5982(3) 0.2586(2) 0.0332(7) Uani 1 1 d . . . O7 O 0.1094(5) 0.7512(4) 0.3402(3) 0.0591(12) Uani 1 1 d . . . O8 O 0.3210(4) 0.5436(3) 0.5086(2) 0.0249(6) Uani 1 1 d D . . O1W O -0.0605(5) 0.7596(4) 0.5462(3) 0.0519(10) Uani 1 1 d . . . O2W O 0.0730(11) 0.9632(8) 0.4225(9) 0.188(4) Uani 1 1 d . . . O3W O 0.110(3) 0.447(2) 0.3589(16) 0.085(6) Uani 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0253(3) 0.0180(3) 0.0179(3) -0.0004(2) -0.0036(2) -0.0095(2) Co2 0.0293(4) 0.0400(4) 0.0335(4) -0.0097(3) -0.0104(3) -0.0096(3) C1 0.033(3) 0.026(2) 0.030(2) 0.0026(19) -0.008(2) -0.013(2) C2 0.029(2) 0.026(2) 0.031(2) -0.0004(19) -0.0062(19) -0.0125(19) C3 0.030(2) 0.026(2) 0.024(2) -0.0027(18) -0.0071(19) -0.0111(19) C4 0.032(2) 0.027(2) 0.030(2) -0.0056(19) -0.005(2) -0.015(2) C5 0.055(3) 0.023(2) 0.044(3) 0.004(2) -0.023(3) -0.016(2) C6 0.065(4) 0.028(3) 0.050(3) 0.010(2) -0.038(3) -0.020(3) C7 0.056(3) 0.029(3) 0.045(3) 0.007(2) -0.028(3) -0.023(2) C8 0.042(3) 0.032(3) 0.027(2) -0.009(2) 0.003(2) -0.023(2) C9 0.124(6) 0.079(4) 0.098(5) 0.033(4) -0.080(5) -0.064(4) C10 0.106(6) 0.056(4) 0.078(5) 0.036(4) -0.073(5) -0.055(4) C11 0.099(6) 0.093(5) 0.041(3) 0.020(3) -0.036(4) -0.059(5) C12 0.054(4) 0.068(4) 0.040(3) 0.006(3) -0.022(3) -0.027(3) C13 0.041(3) 0.041(3) 0.042(3) 0.004(2) -0.019(2) -0.020(2) C14 0.047(3) 0.065(4) 0.063(4) -0.010(3) -0.029(3) -0.007(3) C15 0.065(4) 0.062(4) 0.092(6) 0.004(4) -0.054(4) -0.013(3) C16 0.030(3) 0.049(3) 0.032(3) 0.001(2) -0.009(2) -0.021(2) C19 0.037(3) 0.031(2) 0.026(2) 0.0009(19) 0.003(2) -0.011(2) C17A 0.040(6) 0.025(6) 0.031(5) 0.000(5) 0.006(4) -0.002(5) C18A 0.041(5) 0.021(5) 0.028(6) 0.006(4) 0.002(4) -0.006(5) C20A 0.042(7) 0.059(10) 0.034(6) 0.006(6) 0.002(5) 0.018(6) C21A 0.046(8) 0.072(12) 0.025(6) 0.020(7) 0.006(5) -0.003(7) C17B 0.026(9) 0.072(18) 0.036(12) 0.010(13) 0.011(8) -0.004(13) C18B 0.063(13) 0.064(17) 0.014(8) -0.007(12) 0.001(8) -0.009(13) C20B 0.028(8) 0.024(9) 0.025(8) -0.013(7) -0.001(6) -0.010(7) C21B 0.030(10) 0.039(12) 0.023(8) -0.006(9) 0.000(7) -0.019(8) N1 0.035(2) 0.030(2) 0.022(2) 0.0024(16) -0.0019(17) -0.0081(18) O1 0.0306(17) 0.0229(15) 0.0320(17) 0.0006(13) -0.0084(14) -0.0142(13) O2 0.043(2) 0.0336(19) 0.070(3) 0.0137(17) -0.0316(19) -0.0181(17) O3 0.037(2) 0.0382(19) 0.060(2) -0.0196(17) -0.0130(18) -0.0148(16) O4 0.059(2) 0.0250(18) 0.041(2) -0.0056(14) -0.0101(17) -0.0220(17) O5 0.112(4) 0.040(2) 0.092(3) 0.035(2) -0.083(3) -0.043(2) O6 0.0326(18) 0.0359(18) 0.0306(17) -0.0020(14) -0.0132(14) -0.0078(15) O7 0.036(2) 0.087(3) 0.039(2) -0.020(2) -0.0142(18) 0.006(2) O8 0.0238(16) 0.0311(17) 0.0233(15) -0.0003(13) -0.0069(13) -0.0129(14) O1W 0.034(2) 0.073(3) 0.054(2) -0.020(2) -0.0048(18) -0.0178(19) O2W 0.134(7) 0.123(6) 0.310(13) -0.061(7) -0.013(7) -0.034(5) O3W 0.102(12) 0.108(12) 0.084(11) 0.037(10) -0.033(10) -0.093(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 Co1 O4 2.063(3) 2_565 ? Co1 O8 2.082(3) 2_666 ? Co1 O1 2.090(3) 2_575 ? Co1 O6 2.150(3) . ? Co1 O8 2.154(3) . ? Co1 N1 2.156(4) . ? Co2 O7 1.956(4) . ? Co2 O3 1.989(3) 1_656 ? Co2 O8 2.001(3) . ? Co2 O1W 2.126(4) . ? Co2 O1 2.251(3) 2_575 ? Co2 O2W 2.390(9) . ? C1 O2 1.237(5) . ? C1 O1 1.276(5) . ? C1 C2 1.509(6) . ? C2 C7 1.382(6) . ? C2 C3 1.391(6) . ? C3 C4 1.389(6) . ? C3 H3 0.9300 . ? C4 C5 1.384(6) . ? C4 C8 1.510(6) . ? C5 C6 1.384(7) . ? C5 H5 0.9300 . ? C6 O5 1.368(6) . ? C6 C7 1.389(6) . ? C7 H7 0.9300 . ? C8 O4 1.252(6) . ? C8 O3 1.256(6) . ? C9 O5 1.430(7) . ? C9 C10 1.507(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.364(10) . ? C10 C11 1.375(10) . ? C11 C12 1.382(8) . ? C11 H11 0.9300 . ? C12 C13 1.376(8) . ? C12 H12 0.9300 . ? C13 C14 1.374(7) . ? C13 C16 1.496(7) . ? C14 C15 1.387(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.245(6) . ? C16 O7 1.259(6) . ? C19 C18B 1.29(3) . ? C19 C20A 1.367(13) . ? C19 C20B 1.41(2) . ? C19 C18A 1.417(15) . ? C19 C19 1.478(9) 2_765 ? C17A N1 1.344(17) . ? C17A C18A 1.36(2) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? C20A C21A 1.393(18) . ? C20A H20A 0.9300 . ? C21A N1 1.291(16) . ? C21A H21A 0.9300 . ? C17B N1 1.31(4) . ? C17B C18B 1.40(4) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? C20B C21B 1.35(3) . ? C20B H20B 0.9300 . ? C21B N1 1.38(3) . ? C21B H21B 0.9300 . ? O1 Co1 2.090(3) 2_575 ? O1 Co2 2.251(3) 2_575 ? O3 Co2 1.989(3) 1_454 ? O4 Co1 2.063(3) 2_565 ? O8 Co1 2.082(3) 2_666 ? O8 H8 0.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O8 95.35(13) 2_565 2_666 ? O4 Co1 O1 170.29(13) 2_565 2_575 ? O8 Co1 O1 93.81(12) 2_666 2_575 ? O4 Co1 O6 85.28(13) 2_565 . ? O8 Co1 O6 174.97(12) 2_666 . ? O1 Co1 O6 85.32(12) 2_575 . ? O4 Co1 O8 97.06(13) 2_565 . ? O8 Co1 O8 80.96(12) 2_666 . ? O1 Co1 O8 81.22(12) 2_575 . ? O6 Co1 O8 94.01(12) . . ? O4 Co1 N1 89.92(14) 2_565 . ? O8 Co1 N1 98.34(13) 2_666 . ? O1 Co1 N1 91.91(13) 2_575 . ? O6 Co1 N1 86.64(13) . . ? O8 Co1 N1 173.01(13) . . ? O7 Co2 O3 148.86(17) . 1_656 ? O7 Co2 O8 103.58(15) . . ? O3 Co2 O8 106.41(14) 1_656 . ? O7 Co2 O1W 85.71(15) . . ? O3 Co2 O1W 95.57(14) 1_656 . ? O8 Co2 O1W 102.85(14) . . ? O7 Co2 O1 88.90(14) . 2_575 ? O3 Co2 O1 87.78(13) 1_656 2_575 ? O8 Co2 O1 80.81(11) . 2_575 ? O1W Co2 O1 174.07(13) . 2_575 ? O7 Co2 O2W 73.5(3) . . ? O3 Co2 O2W 75.8(3) 1_656 . ? O8 Co2 O2W 174.1(3) . . ? O1W Co2 O2W 82.2(2) . . ? O1 Co2 O2W 93.9(2) 2_575 . ? O2 C1 O1 124.3(4) . . ? O2 C1 C2 119.9(4) . . ? O1 C1 C2 115.8(4) . . ? C7 C2 C3 120.3(4) . . ? C7 C2 C1 118.2(4) . . ? C3 C2 C1 121.5(4) . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 C8 119.3(4) . . ? C3 C4 C8 120.5(4) . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? O5 C6 C5 115.7(4) . . ? O5 C6 C7 124.3(4) . . ? C5 C6 C7 120.0(5) . . ? C2 C7 C6 119.8(4) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O4 C8 O3 126.0(4) . . ? O4 C8 C4 116.4(4) . . ? O3 C8 C4 117.7(4) . . ? O5 C9 C10 106.9(5) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? C15 C10 C11 118.6(6) . . ? C15 C10 C9 119.1(8) . . ? C11 C10 C9 122.3(8) . . ? C10 C11 C12 121.2(7) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 118.3(5) . . ? C14 C13 C16 119.6(5) . . ? C12 C13 C16 122.1(5) . . ? C13 C14 C15 121.1(6) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 120.5(7) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O6 C16 O7 125.1(4) . . ? O6 C16 C13 119.9(4) . . ? O7 C16 C13 114.9(5) . . ? C18B C19 C20A 110.0(14) . . ? C18B C19 C20B 118.1(15) . . ? C20A C19 C20B 28.3(8) . . ? C18B C19 C18A 24.2(16) . . ? C20A C19 C18A 114.5(8) . . ? C20B C19 C18A 109.8(10) . . ? C18B C19 C19 120.3(13) . 2_765 ? C20A C19 C19 122.3(7) . 2_765 ? C20B C19 C19 121.6(10) . 2_765 ? C18A C19 C19 123.1(7) . 2_765 ? N1 C17A C18A 123.1(13) . . ? N1 C17A H17A 118.5 . . ? C18A C17A H17A 118.5 . . ? C17A C18A C19 120.6(12) . . ? C17A C18A H18A 119.7 . . ? C19 C18A H18A 119.7 . . ? C19 C20A C21A 120.9(11) . . ? C19 C20A H20A 119.5 . . ? C21A C20A H20A 119.5 . . ? N1 C21A C20A 123.8(12) . . ? N1 C21A H21A 118.1 . . ? C20A C21A H21A 118.1 . . ? N1 C17B C18B 126(3) . . ? N1 C17B H17B 116.9 . . ? C18B C17B H17B 116.9 . . ? C19 C18B C17B 120(3) . . ? C19 C18B H18B 120.2 . . ? C17B C18B H18B 120.2 . . ? C21B C20B C19 119.2(19) . . ? C21B C20B H20B 120.4 . . ? C19 C20B H20B 120.4 . . ? C20B C21B N1 124(2) . . ? C20B C21B H21B 118.0 . . ? N1 C21B H21B 118.0 . . ? C21A N1 C17B 108.2(15) . . ? C21A N1 C17A 117.0(10) . . ? C17B N1 C17A 23.7(17) . . ? C21A N1 C21B 27.1(10) . . ? C17B N1 C21B 112.6(18) . . ? C17A N1 C21B 109.6(14) . . ? C21A N1 Co1 121.0(7) . . ? C17B N1 Co1 120.8(14) . . ? C17A N1 Co1 121.2(8) . . ? C21B N1 Co1 126.3(12) . . ? C1 O1 Co1 128.0(3) . 2_575 ? C1 O1 Co2 132.4(3) . 2_575 ? Co1 O1 Co2 90.96(11) 2_575 2_575 ? C8 O3 Co2 126.8(3) . 1_454 ? C8 O4 Co1 140.7(3) . 2_565 ? C6 O5 C9 117.6(4) . . ? C16 O6 Co1 129.9(3) . . ? C16 O7 Co2 128.2(3) . . ? Co2 O8 Co1 119.64(15) . 2_666 ? Co2 O8 Co1 96.31(12) . . ? Co1 O8 Co1 99.04(12) 2_666 . ? Co2 O8 H8 117(4) . . ? Co1 O8 H8 114(4) 2_666 . ? Co1 O8 H8 106(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -157.4(5) . . . . ? O1 C1 C2 C7 21.0(6) . . . . ? O2 C1 C2 C3 21.1(7) . . . . ? O1 C1 C2 C3 -160.5(4) . . . . ? C7 C2 C3 C4 -1.9(7) . . . . ? C1 C2 C3 C4 179.6(4) . . . . ? C2 C3 C4 C5 2.7(7) . . . . ? C2 C3 C4 C8 -173.2(4) . . . . ? C3 C4 C5 C6 -1.0(8) . . . . ? C8 C4 C5 C6 175.0(5) . . . . ? C4 C5 C6 O5 177.0(5) . . . . ? C4 C5 C6 C7 -1.7(9) . . . . ? C3 C2 C7 C6 -0.7(8) . . . . ? C1 C2 C7 C6 177.8(5) . . . . ? O5 C6 C7 C2 -176.1(5) . . . . ? C5 C6 C7 C2 2.5(9) . . . . ? C5 C4 C8 O4 -16.4(6) . . . . ? C3 C4 C8 O4 159.6(4) . . . . ? C5 C4 C8 O3 165.0(4) . . . . ? C3 C4 C8 O3 -19.0(6) . . . . ? O5 C9 C10 C15 -80.2(9) . . . . ? O5 C9 C10 C11 100.7(8) . . . . ? C15 C10 C11 C12 0.3(10) . . . . ? C9 C10 C11 C12 179.4(6) . . . . ? C10 C11 C12 C13 -1.7(9) . . . . ? C11 C12 C13 C14 1.1(8) . . . . ? C11 C12 C13 C16 -175.2(5) . . . . ? C12 C13 C14 C15 0.9(9) . . . . ? C16 C13 C14 C15 177.3(5) . . . . ? C11 C10 C15 C14 1.6(10) . . . . ? C9 C10 C15 C14 -177.5(6) . . . . ? C13 C14 C15 C10 -2.3(10) . . . . ? C14 C13 C16 O6 163.3(5) . . . . ? C12 C13 C16 O6 -20.5(7) . . . . ? C14 C13 C16 O7 -18.5(7) . . . . ? C12 C13 C16 O7 157.8(5) . . . . ? N1 C17A C18A C19 -2.5(18) . . . . ? C18B C19 C18A C17A 88(4) . . . . ? C20A C19 C18A C17A 2.9(16) . . . . ? C20B C19 C18A C17A -27.3(14) . . . . ? C19 C19 C18A C17A 178.6(9) 2_765 . . . ? C18B C19 C20A C21A -28.0(19) . . . . ? C20B C19 C20A C21A 84(3) . . . . ? C18A C19 C20A C21A -2.3(18) . . . . ? C19 C19 C20A C21A -178.0(10) 2_765 . . . ? C19 C20A C21A N1 1(2) . . . . ? C20A C19 C18B C17B 28(3) . . . . ? C20B C19 C18B C17B -2(3) . . . . ? C18A C19 C18B C17B -77(4) . . . . ? C19 C19 C18B C17B 178.9(17) 2_765 . . . ? N1 C17B C18B C19 -3(4) . . . . ? C18B C19 C20B C21B 4(2) . . . . ? C20A C19 C20B C21B -76(3) . . . . ? C18A C19 C20B C21B 28.6(17) . . . . ? C19 C19 C20B C21B -176.8(13) 2_765 . . . ? C19 C20B C21B N1 -1(2) . . . . ? C20A C21A N1 C17B 23(2) . . . . ? C20A C21A N1 C17A -0.5(19) . . . . ? C20A C21A N1 C21B -81(4) . . . . ? C20A C21A N1 Co1 169.2(10) . . . . ? C18B C17B N1 C21A -23(3) . . . . ? C18B C17B N1 C17A 93(6) . . . . ? C18B C17B N1 C21B 5(3) . . . . ? C18B C17B N1 Co1 -169(2) . . . . ? C18A C17A N1 C21A 1.2(18) . . . . ? C18A C17A N1 C17B -72(5) . . . . ? C18A C17A N1 C21B 29.7(16) . . . . ? C18A C17A N1 Co1 -168.5(9) . . . . ? C20B C21B N1 C21A 83(4) . . . . ? C20B C21B N1 C17B -3(3) . . . . ? C20B C21B N1 C17A -28(2) . . . . ? C20B C21B N1 Co1 171.3(12) . . . . ? O4 Co1 N1 C21A -57.0(14) 2_565 . . . ? O8 Co1 N1 C21A 38.4(14) 2_666 . . . ? O1 Co1 N1 C21A 132.5(14) 2_575 . . . ? O6 Co1 N1 C21A -142.3(14) . . . . ? O8 Co1 N1 C21A 122.1(17) . . . . ? O4 Co1 N1 C17B 85(2) 2_565 . . . ? O8 Co1 N1 C17B 180(2) 2_666 . . . ? O1 Co1 N1 C17B -86(2) 2_575 . . . ? O6 Co1 N1 C17B -1(2) . . . . ? O8 Co1 N1 C17B -96(3) . . . . ? O4 Co1 N1 C17A 112.3(8) 2_565 . . . ? O8 Co1 N1 C17A -152.3(8) 2_666 . . . ? O1 Co1 N1 C17A -58.2(8) 2_575 . . . ? O6 Co1 N1 C17A 27.0(8) . . . . ? O8 Co1 N1 C17A -68.6(14) . . . . ? O4 Co1 N1 C21B -89.1(13) 2_565 . . . ? O8 Co1 N1 C21B 6.3(13) 2_666 . . . ? O1 Co1 N1 C21B 100.5(13) 2_575 . . . ? O6 Co1 N1 C21B -174.3(13) . . . . ? O8 Co1 N1 C21B 90.0(17) . . . . ? O2 C1 O1 Co1 31.3(7) . . . 2_575 ? C2 C1 O1 Co1 -147.1(3) . . . 2_575 ? O2 C1 O1 Co2 -106.7(5) . . . 2_575 ? C2 C1 O1 Co2 74.9(5) . . . 2_575 ? O4 C8 O3 Co2 -26.2(7) . . . 1_454 ? C4 C8 O3 Co2 152.2(3) . . . 1_454 ? O3 C8 O4 Co1 3.9(8) . . . 2_565 ? C4 C8 O4 Co1 -174.5(3) . . . 2_565 ? C5 C6 O5 C9 168.3(6) . . . . ? C7 C6 O5 C9 -13.0(10) . . . . ? C10 C9 O5 C6 174.1(6) . . . . ? O7 C16 O6 Co1 -15.5(8) . . . . ? C13 C16 O6 Co1 162.6(3) . . . . ? O4 Co1 O6 C16 140.6(4) 2_565 . . . ? O8 Co1 O6 C16 43.2(16) 2_666 . . . ? O1 Co1 O6 C16 -37.0(4) 2_575 . . . ? O8 Co1 O6 C16 43.8(4) . . . . ? N1 Co1 O6 C16 -129.2(4) . . . . ? O6 C16 O7 Co2 11.9(8) . . . . ? C13 C16 O7 Co2 -166.3(3) . . . . ? O3 Co2 O7 C16 122.1(5) 1_656 . . . ? O8 Co2 O7 C16 -42.0(5) . . . . ? O1W Co2 O7 C16 -144.2(5) . . . . ? O1 Co2 O7 C16 38.3(5) 2_575 . . . ? O2W Co2 O7 C16 132.7(6) . . . . ? O7 Co2 O8 Co1 166.63(17) . . . 2_666 ? O3 Co2 O8 Co1 -4.9(2) 1_656 . . 2_666 ? O1W Co2 O8 Co1 -104.73(17) . . . 2_666 ? O1 Co2 O8 Co1 80.03(16) 2_575 . . 2_666 ? O2W Co2 O8 Co1 107(2) . . . 2_666 ? O7 Co2 O8 Co1 62.46(16) . . . . ? O3 Co2 O8 Co1 -109.06(14) 1_656 . . . ? O1W Co2 O8 Co1 151.10(13) . . . . ? O1 Co2 O8 Co1 -24.15(11) 2_575 . . . ? O2W Co2 O8 Co1 2(2) . . . . ? O4 Co1 O8 Co2 -144.24(14) 2_565 . . . ? O8 Co1 O8 Co2 121.43(17) 2_666 . . . ? O1 Co1 O8 Co2 26.11(12) 2_575 . . . ? O6 Co1 O8 Co2 -58.52(13) . . . . ? N1 Co1 O8 Co2 36.6(11) . . . . ? O4 Co1 O8 Co1 94.33(14) 2_565 . . 2_666 ? O8 Co1 O8 Co1 0.0 2_666 . . 2_666 ? O1 Co1 O8 Co1 -95.32(13) 2_575 . . 2_666 ? O6 Co1 O8 Co1 -179.95(13) . . . 2_666 ? N1 Co1 O8 Co1 -84.8(11) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.542 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.089 # Attachment '5.cif' data_complex-5 _database_code_depnum_ccdc_archive 'CCDC 743100' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H40 N8 O17 Zn2' _chemical_formula_sum 'C56 H40 N8 O17 Zn2' _chemical_formula_weight 1227.70 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/c' 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 10.001(2) _cell_length_b 20.682(3) _cell_length_c 13.341(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.525(6) _cell_angle_gamma 90.00 _cell_volume 2759.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8042 _exptl_absorpt_correction_T_max 0.8477 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13975 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4843 _reflns_number_gt 3511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered C27 C28 atoms were refined using C atoms split over two sites C27A and C27B,C28A and C28B, with a total occupancy of 1,respectively. ; _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^)+(0.0704P)^2^+1.4662P] 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 4843 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.30927(4) 0.246980(18) 0.21327(3) 0.04145(16) Uani 1 1 d . . . C1 C 0.8728(4) -0.15472(18) -0.2702(3) 0.0458(9) Uani 1 1 d . . . C2 C 0.9485(4) -0.09308(17) -0.2526(3) 0.0412(8) Uani 1 1 d . . . C3 C 1.0809(4) -0.08900(17) -0.2814(3) 0.0426(8) Uani 1 1 d . . . H3 H 1.1218 -0.1244 -0.3114 0.051 Uiso 1 1 calc R . . C4 C 1.1526(4) -0.03262(17) -0.2660(3) 0.0439(9) Uani 1 1 d . . . C5 C 1.0926(4) 0.02081(18) -0.2212(3) 0.0494(9) Uani 1 1 d . . . H5 H 1.1407 0.0587 -0.2107 0.059 Uiso 1 1 calc R . . C6 C 0.9600(4) 0.01644(18) -0.1928(3) 0.0524(10) Uani 1 1 d . . . C7 C 0.8889(4) -0.04030(19) -0.2089(3) 0.0525(10) Uani 1 1 d . . . H7 H 0.7998 -0.0427 -0.1899 0.063 Uiso 1 1 calc R . . C8 C 1.2931(4) -0.02794(19) -0.3017(3) 0.0555(11) Uani 1 1 d . . . C9 C 0.9415(5) 0.1262(2) -0.1360(4) 0.0697(14) Uani 1 1 d . . . H9A H 0.9597 0.1466 -0.1998 0.084 Uiso 1 1 calc R . . H9B H 1.0245 0.1231 -0.0981 0.084 Uiso 1 1 calc R . . C10 C 0.8394(4) 0.16479(19) -0.0783(3) 0.0561(11) Uani 1 1 d . . . C11 C 0.8072(4) 0.1459(2) 0.0181(3) 0.0629(12) Uani 1 1 d . . . H11 H 0.8532 0.1119 0.0482 0.075 Uiso 1 1 calc R . . C12 C 0.7064(4) 0.1775(2) 0.0705(3) 0.0571(11) Uani 1 1 d . . . H12 H 0.6844 0.1639 0.1347 0.069 Uiso 1 1 calc R . . C13 C 0.6394(4) 0.22876(18) 0.0272(3) 0.0478(9) Uani 1 1 d . . . C14 C 0.6751(4) 0.24863(18) -0.0679(3) 0.0573(11) Uani 1 1 d . . . H14 H 0.6326 0.2841 -0.0969 0.069 Uiso 1 1 calc R . . C15 C 0.7731(4) 0.2164(2) -0.1203(3) 0.0617(12) Uani 1 1 d . . . H15 H 0.7946 0.2298 -0.1847 0.074 Uiso 1 1 calc R . . C16 C 0.5267(4) 0.2600(2) 0.0818(4) 0.0544(11) Uani 1 1 d . . . C17 C 0.1751(4) 0.35373(19) 0.1031(3) 0.0457(9) Uani 1 1 d . . . H17 H 0.2510 0.3794 0.1097 0.055 Uiso 1 1 calc R . . C18 C 0.0399(4) 0.2725(2) 0.1071(3) 0.0597(11) Uani 1 1 d . . . H18 H 0.0062 0.2311 0.1175 0.072 Uiso 1 1 calc R . . C19 C -0.0284(4) 0.3222(2) 0.0655(3) 0.0640(12) Uani 1 1 d . . . H19 H -0.1167 0.3217 0.0430 0.077 Uiso 1 1 calc R . . C20 C 0.0286(4) 0.4378(2) 0.0299(3) 0.0472(9) Uani 1 1 d . . . C21 C 0.1260(4) 0.4740(2) -0.0173(3) 0.0521(10) Uani 1 1 d . . . H21 H 0.2100 0.4564 -0.0288 0.063 Uiso 1 1 calc R . . C22 C -0.0977(4) 0.4637(2) 0.0473(3) 0.0533(10) Uani 1 1 d . . . H22 H -0.1626 0.4390 0.0789 0.064 Uiso 1 1 calc R . . C23 C 0.4114(4) 0.35394(17) 0.3441(3) 0.0430(9) Uani 1 1 d . . . H23 H 0.4719 0.3681 0.2964 0.052 Uiso 1 1 calc R . . C24 C 0.2627(4) 0.29802(18) 0.4221(3) 0.0492(9) Uani 1 1 d . . . H24 H 0.2011 0.2658 0.4370 0.059 Uiso 1 1 calc R . . C25 C 0.2938(4) 0.34792(18) 0.4816(3) 0.0487(9) Uani 1 1 d . . . H25 H 0.2585 0.3568 0.5443 0.058 Uiso 1 1 calc R . . C26 C 0.4465(4) 0.44325(16) 0.4655(3) 0.0408(8) Uani 1 1 d . . . C27A C 0.4933(7) 0.4872(3) 0.3979(5) 0.050(2) Uani 0.576(7) 1 d P . 1 H27A H 0.4904 0.4781 0.3296 0.060 Uiso 0.576(7) 1 calc PR . 1 C28A C 0.4551(7) 0.4548(3) 0.5684(5) 0.049(2) Uani 0.576(7) 1 d P . 1 H28A H 0.4263 0.4237 0.6137 0.059 Uiso 0.576(7) 1 calc PR . 1 C27B C 0.5763(8) 0.4562(4) 0.4443(7) 0.041(2) Uani 0.424(7) 1 d P . 2 H27B H 0.6269 0.4276 0.4065 0.049 Uiso 0.424(7) 1 calc PR . 2 C28B C 0.3686(8) 0.4867(4) 0.5194(7) 0.043(3) Uani 0.424(7) 1 d P . 2 H28B H 0.2791 0.4775 0.5310 0.052 Uiso 0.424(7) 1 calc PR . 2 N1 N 0.1681(3) 0.29282(15) 0.1317(2) 0.0464(8) Uani 1 1 d . . . N2 N 0.0580(3) 0.37396(16) 0.0631(2) 0.0489(8) Uani 1 1 d . . . N3 N 0.3359(3) 0.30175(14) 0.3351(2) 0.0430(7) Uani 1 1 d . . . N4 N 0.3885(3) 0.38357(13) 0.4317(2) 0.0396(7) Uani 1 1 d . . . O1 O 0.7549(3) -0.15804(12) -0.2322(2) 0.0519(7) Uani 1 1 d . . . O2 O 0.9250(3) -0.19861(14) -0.3167(2) 0.0720(9) Uani 1 1 d . . . O3 O 1.3527(3) 0.02248(14) -0.3090(3) 0.0738(9) Uani 1 1 d . . . O4 O 1.3440(3) -0.08413(14) -0.3246(3) 0.0934(13) Uani 1 1 d . . . H4 H 1.4208 -0.0793 -0.3441 0.140 Uiso 1 1 calc R . . O5 O 0.8869(3) 0.06523(14) -0.1507(3) 0.0827(11) Uani 1 1 d . . . O6 O 0.4809(3) 0.22821(15) 0.1548(2) 0.0620(8) Uani 1 1 d . . . O7 O 0.4811(3) 0.31285(15) 0.0537(3) 0.0829(11) Uani 1 1 d . . . O1W O 0.5837(3) 0.89505(18) 0.6088(3) 0.0893(11) Uani 1 1 d . . . O2W O 0.6119(5) 0.4190(3) 0.1500(6) 0.081(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0419(3) 0.0359(3) 0.0467(3) -0.00746(18) 0.00873(18) -0.00182(18) C1 0.050(2) 0.041(2) 0.047(2) -0.0009(17) 0.0083(18) -0.0078(18) C2 0.045(2) 0.041(2) 0.0378(19) 0.0007(15) 0.0069(16) -0.0053(16) C3 0.045(2) 0.040(2) 0.043(2) -0.0022(16) 0.0028(16) 0.0027(16) C4 0.042(2) 0.039(2) 0.051(2) 0.0015(16) 0.0044(17) -0.0039(16) C5 0.055(2) 0.040(2) 0.054(2) -0.0044(17) 0.0092(19) -0.0096(18) C6 0.056(2) 0.039(2) 0.063(3) -0.0105(18) 0.024(2) -0.0047(18) C7 0.050(2) 0.050(2) 0.058(2) -0.0038(19) 0.0236(19) -0.0070(19) C8 0.043(2) 0.043(2) 0.080(3) -0.003(2) 0.006(2) 0.0000(18) C9 0.068(3) 0.049(2) 0.092(4) -0.019(2) 0.034(3) -0.010(2) C10 0.055(2) 0.042(2) 0.072(3) -0.013(2) 0.021(2) -0.0082(19) C11 0.064(3) 0.054(3) 0.071(3) 0.000(2) 0.017(2) 0.010(2) C12 0.056(3) 0.059(3) 0.056(3) -0.004(2) 0.018(2) -0.004(2) C13 0.041(2) 0.040(2) 0.063(3) -0.0118(18) 0.0090(18) -0.0097(17) C14 0.056(2) 0.045(2) 0.071(3) 0.003(2) 0.013(2) -0.0004(19) C15 0.072(3) 0.054(3) 0.060(3) -0.001(2) 0.026(2) -0.007(2) C16 0.042(2) 0.050(3) 0.072(3) -0.015(2) 0.013(2) -0.0102(19) C17 0.037(2) 0.052(2) 0.048(2) -0.0060(18) 0.0020(16) 0.0003(17) C18 0.057(3) 0.060(3) 0.062(3) -0.005(2) -0.005(2) -0.016(2) C19 0.049(2) 0.074(3) 0.069(3) -0.002(2) -0.014(2) -0.007(2) C20 0.042(2) 0.061(2) 0.038(2) -0.0024(18) -0.0029(16) 0.0052(19) C21 0.040(2) 0.071(3) 0.045(2) 0.001(2) 0.0023(17) 0.0115(19) C22 0.040(2) 0.072(3) 0.048(2) 0.008(2) 0.0053(17) 0.006(2) C23 0.047(2) 0.039(2) 0.043(2) -0.0040(16) 0.0051(16) -0.0033(17) C24 0.057(2) 0.044(2) 0.046(2) -0.0024(17) 0.0067(18) -0.0084(19) C25 0.058(2) 0.050(2) 0.038(2) -0.0015(17) 0.0090(18) -0.0081(19) C26 0.048(2) 0.0354(19) 0.039(2) -0.0025(15) -0.0017(16) 0.0036(16) C27A 0.067(5) 0.045(4) 0.038(4) -0.005(3) 0.000(3) -0.008(4) C28A 0.061(5) 0.043(4) 0.045(4) -0.004(3) 0.002(3) -0.005(3) C27B 0.036(5) 0.040(5) 0.047(5) -0.006(4) 0.008(4) 0.000(4) C28B 0.032(5) 0.041(5) 0.058(6) -0.010(4) 0.008(4) -0.001(4) N1 0.0432(18) 0.0455(19) 0.0506(19) -0.0082(14) 0.0020(14) -0.0019(14) N2 0.0432(18) 0.055(2) 0.0485(19) -0.0029(15) -0.0034(14) 0.0017(16) N3 0.0475(18) 0.0371(16) 0.0444(17) -0.0032(13) -0.0001(14) -0.0016(14) N4 0.0446(17) 0.0356(15) 0.0385(17) -0.0045(12) -0.0007(13) -0.0015(13) O1 0.0473(15) 0.0434(15) 0.0652(18) -0.0005(13) 0.0132(13) -0.0054(12) O2 0.0661(19) 0.0579(18) 0.092(2) -0.0313(17) 0.0252(17) -0.0163(15) O3 0.0525(17) 0.0467(17) 0.123(3) -0.0036(17) 0.0207(17) -0.0108(14) O4 0.0519(19) 0.0493(19) 0.180(4) -0.019(2) 0.037(2) -0.0013(15) O5 0.071(2) 0.0524(18) 0.126(3) -0.0340(18) 0.0481(19) -0.0139(16) O6 0.0464(16) 0.0769(19) 0.0629(18) -0.0063(16) 0.0174(14) 0.0048(15) O7 0.068(2) 0.054(2) 0.127(3) -0.0033(19) 0.033(2) 0.0049(16) O1W 0.060(2) 0.089(2) 0.119(3) 0.001(2) 0.013(2) 0.0002(18) O2W 0.041(3) 0.074(4) 0.129(6) -0.033(4) 0.020(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.931(3) . ? Zn1 O1 1.965(3) 3_655 ? Zn1 N3 1.997(3) . ? Zn1 N1 2.013(3) . ? C1 O2 1.219(4) . ? C1 O1 1.290(4) . ? C1 C2 1.500(5) . ? C2 C7 1.375(5) . ? C2 C3 1.385(5) . ? C3 C4 1.383(5) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 C8 1.491(5) . ? C5 C6 1.385(5) . ? C5 H5 0.9300 . ? C6 O5 1.370(4) . ? C6 C7 1.388(5) . ? C7 H7 0.9300 . ? C8 O3 1.206(5) . ? C8 O4 1.306(5) . ? C9 O5 1.387(5) . ? C9 C10 1.513(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.373(6) . ? C10 C11 1.385(6) . ? C11 C12 1.393(5) . ? C11 H11 0.9300 . ? C12 C13 1.379(6) . ? C12 H12 0.9300 . ? C13 C14 1.384(6) . ? C13 C16 1.494(5) . ? C14 C15 1.380(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.242(5) . ? C16 O6 1.264(5) . ? C17 N1 1.318(5) . ? C17 N2 1.349(5) . ? C17 H17 0.9300 . ? C18 C19 1.351(6) . ? C18 N1 1.386(5) . ? C18 H18 0.9300 . ? C19 N2 1.376(5) . ? C19 H19 0.9300 . ? C20 C21 1.384(5) . ? C20 C22 1.393(5) . ? C20 N2 1.423(5) . ? C21 C22 1.379(5) 3_565 ? C21 H21 0.9300 . ? C22 C21 1.379(5) 3_565 ? C22 H22 0.9300 . ? C23 N3 1.322(4) . ? C23 N4 1.341(4) . ? C23 H23 0.9300 . ? C24 C25 1.337(5) . ? C24 N3 1.380(5) . ? C24 H24 0.9300 . ? C25 N4 1.377(5) . ? C25 H25 0.9300 . ? C26 C27B 1.358(9) . ? C26 C27A 1.367(8) . ? C26 C28B 1.393(9) . ? C26 C28A 1.395(7) . ? C26 N4 1.435(4) . ? C27A C28A 1.379(9) 3_666 ? C27A H27A 0.9300 . ? C28A C27A 1.379(9) 3_666 ? C28A H28A 0.9300 . ? C27B C28B 1.388(11) 3_666 ? C27B H27B 0.9300 . ? C28B C27B 1.388(11) 3_666 ? C28B H28B 0.9300 . ? O1 Zn1 1.965(2) 3_655 ? O4 H4 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O1 98.98(12) . 3_655 ? O6 Zn1 N3 109.30(13) . . ? O1 Zn1 N3 117.89(12) 3_655 . ? O6 Zn1 N1 119.85(13) . . ? O1 Zn1 N1 106.39(12) 3_655 . ? N3 Zn1 N1 105.12(12) . . ? O2 C1 O1 123.9(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 C2 116.4(3) . . ? C7 C2 C3 119.2(3) . . ? C7 C2 C1 121.4(3) . . ? C3 C2 C1 119.4(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 C8 119.7(3) . . ? C5 C4 C8 119.7(3) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? O5 C6 C5 125.5(3) . . ? O5 C6 C7 114.3(3) . . ? C5 C6 C7 120.2(3) . . ? C2 C7 C6 120.9(3) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O3 C8 O4 123.8(4) . . ? O3 C8 C4 123.4(4) . . ? O4 C8 C4 112.8(3) . . ? O5 C9 C10 106.6(3) . . ? O5 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O5 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C15 C10 C11 118.9(4) . . ? C15 C10 C9 121.9(4) . . ? C11 C10 C9 119.2(4) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 C16 119.6(4) . . ? C14 C13 C16 121.4(4) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C10 C15 C14 120.7(4) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O7 C16 O6 123.7(4) . . ? O7 C16 C13 120.7(4) . . ? O6 C16 C13 115.6(4) . . ? N1 C17 N2 111.2(3) . . ? N1 C17 H17 124.4 . . ? N2 C17 H17 124.4 . . ? C19 C18 N1 109.2(4) . . ? C19 C18 H18 125.4 . . ? N1 C18 H18 125.4 . . ? C18 C19 N2 106.7(4) . . ? C18 C19 H19 126.7 . . ? N2 C19 H19 126.7 . . ? C21 C20 C22 120.8(4) . . ? C21 C20 N2 119.9(3) . . ? C22 C20 N2 119.3(4) . . ? C22 C21 C20 119.6(4) 3_565 . ? C22 C21 H21 120.2 3_565 . ? C20 C21 H21 120.2 . . ? C21 C22 C20 119.6(4) 3_565 . ? C21 C22 H22 120.2 3_565 . ? C20 C22 H22 120.2 . . ? N3 C23 N4 110.5(3) . . ? N3 C23 H23 124.7 . . ? N4 C23 H23 124.7 . . ? C25 C24 N3 109.5(3) . . ? C25 C24 H24 125.3 . . ? N3 C24 H24 125.3 . . ? C24 C25 N4 106.5(3) . . ? C24 C25 H25 126.8 . . ? N4 C25 H25 126.8 . . ? C27B C26 C27A 52.9(5) . . ? C27B C26 C28B 121.3(6) . . ? C27A C26 C28B 96.2(5) . . ? C27B C26 C28A 96.9(5) . . ? C27A C26 C28A 121.1(5) . . ? C28B C26 C28A 54.0(5) . . ? C27B C26 N4 119.3(5) . . ? C27A C26 N4 120.3(4) . . ? C28B C26 N4 119.4(5) . . ? C28A C26 N4 118.5(4) . . ? C26 C27A C28A 119.5(6) . 3_666 ? C26 C27A H27A 120.2 . . ? C28A C27A H27A 120.2 3_666 . ? C27A C28A C26 119.3(6) 3_666 . ? C27A C28A H28A 120.3 3_666 . ? C26 C28A H28A 120.3 . . ? C26 C27B C28B 118.2(7) . 3_666 ? C26 C27B H27B 120.9 . . ? C28B C27B H27B 120.9 3_666 . ? C27B C28B C26 120.5(7) 3_666 . ? C27B C28B H28B 119.8 3_666 . ? C26 C28B H28B 119.8 . . ? C17 N1 C18 105.9(3) . . ? C17 N1 Zn1 124.6(3) . . ? C18 N1 Zn1 128.9(3) . . ? C17 N2 C19 107.1(3) . . ? C17 N2 C20 125.9(3) . . ? C19 N2 C20 126.9(3) . . ? C23 N3 C24 106.0(3) . . ? C23 N3 Zn1 127.5(2) . . ? C24 N3 Zn1 125.8(2) . . ? C23 N4 C25 107.5(3) . . ? C23 N4 C26 126.5(3) . . ? C25 N4 C26 125.9(3) . . ? C1 O1 Zn1 113.6(2) . 3_655 ? C8 O4 H4 109.5 . . ? C6 O5 C9 121.1(3) . . ? C16 O6 Zn1 122.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 173.8(4) . . . . ? O1 C1 C2 C7 -7.7(5) . . . . ? O2 C1 C2 C3 -5.8(6) . . . . ? O1 C1 C2 C3 172.8(3) . . . . ? C7 C2 C3 C4 0.4(6) . . . . ? C1 C2 C3 C4 179.9(3) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C2 C3 C4 C8 -177.2(3) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C8 C4 C5 C6 177.0(4) . . . . ? C4 C5 C6 O5 -178.1(4) . . . . ? C4 C5 C6 C7 -0.1(6) . . . . ? C3 C2 C7 C6 -0.6(6) . . . . ? C1 C2 C7 C6 179.9(4) . . . . ? O5 C6 C7 C2 178.7(4) . . . . ? C5 C6 C7 C2 0.4(6) . . . . ? C3 C4 C8 O3 164.9(4) . . . . ? C5 C4 C8 O3 -12.3(7) . . . . ? C3 C4 C8 O4 -14.7(6) . . . . ? C5 C4 C8 O4 168.2(4) . . . . ? O5 C9 C10 C15 -112.4(5) . . . . ? O5 C9 C10 C11 64.7(6) . . . . ? C15 C10 C11 C12 2.0(7) . . . . ? C9 C10 C11 C12 -175.2(4) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? C11 C12 C13 C14 -0.8(6) . . . . ? C11 C12 C13 C16 176.8(4) . . . . ? C12 C13 C14 C15 2.1(6) . . . . ? C16 C13 C14 C15 -175.4(4) . . . . ? C11 C10 C15 C14 -0.7(7) . . . . ? C9 C10 C15 C14 176.4(4) . . . . ? C13 C14 C15 C10 -1.4(7) . . . . ? C12 C13 C16 O7 166.8(4) . . . . ? C14 C13 C16 O7 -15.6(6) . . . . ? C12 C13 C16 O6 -15.1(6) . . . . ? C14 C13 C16 O6 162.4(4) . . . . ? N1 C18 C19 N2 0.6(5) . . . . ? C22 C20 C21 C22 0.1(7) . . . 3_565 ? N2 C20 C21 C22 -178.6(3) . . . 3_565 ? C21 C20 C22 C21 -0.1(7) . . . 3_565 ? N2 C20 C22 C21 178.6(3) . . . 3_565 ? N3 C24 C25 N4 -0.2(4) . . . . ? C27B C26 C27A C28A -76.5(8) . . . 3_666 ? C28B C26 C27A C28A 48.5(8) . . . 3_666 ? C28A C26 C27A C28A -2.7(11) . . . 3_666 ? N4 C26 C27A C28A 178.0(5) . . . 3_666 ? C27B C26 C28A C27A 53.2(8) . . . 3_666 ? C27A C26 C28A C27A 2.7(11) . . . 3_666 ? C28B C26 C28A C27A -70.8(8) . . . 3_666 ? N4 C26 C28A C27A -178.0(5) . . . 3_666 ? C27A C26 C27B C28B 74.5(8) . . . 3_666 ? C28B C26 C27B C28B 2.1(13) . . . 3_666 ? C28A C26 C27B C28B -49.6(9) . . . 3_666 ? N4 C26 C27B C28B -177.9(6) . . . 3_666 ? C27B C26 C28B C27B -2.1(13) . . . 3_666 ? C27A C26 C28B C27B -52.0(9) . . . 3_666 ? C28A C26 C28B C27B 72.3(9) . . . 3_666 ? N4 C26 C28B C27B 177.9(7) . . . 3_666 ? N2 C17 N1 C18 1.0(4) . . . . ? N2 C17 N1 Zn1 -170.4(2) . . . . ? C19 C18 N1 C17 -1.0(5) . . . . ? C19 C18 N1 Zn1 170.0(3) . . . . ? O6 Zn1 N1 C17 -68.9(3) . . . . ? O1 Zn1 N1 C17 -179.8(3) 3_655 . . . ? N3 Zn1 N1 C17 54.5(3) . . . . ? O6 Zn1 N1 C18 121.7(3) . . . . ? O1 Zn1 N1 C18 10.8(4) 3_655 . . . ? N3 Zn1 N1 C18 -115.0(3) . . . . ? N1 C17 N2 C19 -0.7(4) . . . . ? N1 C17 N2 C20 176.3(3) . . . . ? C18 C19 N2 C17 0.0(5) . . . . ? C18 C19 N2 C20 -176.9(4) . . . . ? C21 C20 N2 C17 37.4(5) . . . . ? C22 C20 N2 C17 -141.3(4) . . . . ? C21 C20 N2 C19 -146.2(4) . . . . ? C22 C20 N2 C19 35.0(6) . . . . ? N4 C23 N3 C24 -0.6(4) . . . . ? N4 C23 N3 Zn1 170.4(2) . . . . ? C25 C24 N3 C23 0.5(4) . . . . ? C25 C24 N3 Zn1 -170.7(3) . . . . ? O6 Zn1 N3 C23 47.1(3) . . . . ? O1 Zn1 N3 C23 159.0(3) 3_655 . . . ? N1 Zn1 N3 C23 -82.7(3) . . . . ? O6 Zn1 N3 C24 -143.5(3) . . . . ? O1 Zn1 N3 C24 -31.7(3) 3_655 . . . ? N1 Zn1 N3 C24 86.6(3) . . . . ? N3 C23 N4 C25 0.5(4) . . . . ? N3 C23 N4 C26 -176.6(3) . . . . ? C24 C25 N4 C23 -0.2(4) . . . . ? C24 C25 N4 C26 177.0(3) . . . . ? C27B C26 N4 C23 -37.8(7) . . . . ? C27A C26 N4 C23 24.0(6) . . . . ? C28B C26 N4 C23 142.1(6) . . . . ? C28A C26 N4 C23 -155.4(5) . . . . ? C27B C26 N4 C25 145.6(6) . . . . ? C27A C26 N4 C25 -152.6(5) . . . . ? C28B C26 N4 C25 -34.5(7) . . . . ? C28A C26 N4 C25 28.0(6) . . . . ? O2 C1 O1 Zn1 20.3(5) . . . 3_655 ? C2 C1 O1 Zn1 -158.2(3) . . . 3_655 ? C5 C6 O5 C9 2.3(7) . . . . ? C7 C6 O5 C9 -175.8(4) . . . . ? C10 C9 O5 C6 -173.8(4) . . . . ? O7 C16 O6 Zn1 14.7(6) . . . . ? C13 C16 O6 Zn1 -163.4(3) . . . . ? O1 Zn1 O6 C16 138.4(3) 3_655 . . . ? N3 Zn1 O6 C16 -97.8(3) . . . . ? N1 Zn1 O6 C16 23.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.819 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.068 #===========================end data_complex-6 _database_code_depnum_ccdc_archive 'CCDC 743101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 N8 O17 Zn3' _chemical_formula_sum 'C56 H44 N8 O17 Zn3' _chemical_formula_weight 1297.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/n 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 13.345(4) _cell_length_b 16.436(2) _cell_length_c 25.792(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.127(3) _cell_angle_gamma 90.0 _cell_volume 5657(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'total reflection' _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7391 _exptl_absorpt_correction_T_max 0.7944 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 28156 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9955 _reflns_number_gt 6805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^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 9955 _refine_ls_number_parameters 781 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Zn1 Zn 0.22840(2) -0.04315(2) 0.750429(15) 0.03760(11) Uani 1 1 d . . . Zn2 Zn 0.55721(2) 0.15867(2) 0.979541(15) 0.03951(11) Uani 1 1 d . . . Zn3 Zn 0.44861(2) 0.36969(2) 0.993918(15) 0.03822(11) Uani 1 1 d . . . C1 C 0.6227(2) 0.30362(19) 1.03705(13) 0.0388(8) Uani 1 1 d . . . C2 C 0.7063(2) 0.29799(19) 1.07541(12) 0.0356(7) Uani 1 1 d . . . C3 C 0.7121(2) 0.35195(18) 1.11646(13) 0.0383(8) Uani 1 1 d . . . H3 H 0.6622 0.3908 1.1210 0.046 Uiso 1 1 calc R . . C4 C 0.7923(2) 0.34823(18) 1.15091(12) 0.0368(8) Uani 1 1 d . . . C5 C 0.8643(2) 0.2885(2) 1.14442(13) 0.0437(8) Uani 1 1 d . . . H5 H 0.9173 0.2851 1.1678 0.052 Uiso 1 1 calc R . . C6 C 0.8586(2) 0.2341(2) 1.10379(14) 0.0486(9) Uani 1 1 d . . . C7 C 0.7794(2) 0.2387(2) 1.06883(13) 0.0461(9) Uani 1 1 d . . . H7 H 0.7754 0.2024 1.0412 0.055 Uiso 1 1 calc R . . C8 C 0.8017(2) 0.4091(2) 1.19434(14) 0.0437(8) Uani 1 1 d . . . C9 C 0.9294(3) 0.1226(3) 1.05761(17) 0.0900(17) Uani 1 1 d . . . H9A H 0.9271 0.1523 1.0251 0.108 Uiso 1 1 calc R . . H9B H 0.8692 0.0898 1.0602 0.108 Uiso 1 1 calc R . . C10 C 1.0216(3) 0.0687(3) 1.05941(18) 0.0694(13) Uani 1 1 d . . . C11 C 1.1067(3) 0.0910(3) 1.03318(18) 0.0775(13) Uani 1 1 d . . . H11 H 1.1089 0.1405 1.0158 0.093 Uiso 1 1 calc R . . C12 C 1.1901(3) 0.0396(2) 1.03259(17) 0.0660(12) Uani 1 1 d . . . H12 H 1.2472 0.0544 1.0142 0.079 Uiso 1 1 calc R . . C13 C 1.1878(2) -0.0326(2) 1.05908(14) 0.0489(9) Uani 1 1 d . . . C14 C 1.1030(3) -0.0537(3) 1.08615(15) 0.0662(12) Uani 1 1 d . . . H14 H 1.1013 -0.1022 1.1048 0.079 Uiso 1 1 calc R . . C15 C 1.0199(3) -0.0030(3) 1.08571(16) 0.0745(13) Uani 1 1 d . . . H15 H 0.9624 -0.0182 1.1036 0.089 Uiso 1 1 calc R . . C16 C 1.2773(3) -0.0882(2) 1.05870(16) 0.0510(10) Uani 1 1 d . . . C17 C 0.1497(2) 0.0816(2) 0.81186(14) 0.0480(9) Uani 1 1 d . . . C18 C 0.1768(2) 0.15115(19) 0.84675(13) 0.0396(8) Uani 1 1 d . . . C19 C 0.1132(2) 0.2162(2) 0.85270(13) 0.0477(9) Uani 1 1 d . . . H19 H 0.0525 0.2169 0.8349 0.057 Uiso 1 1 calc R . . C20 C 0.1383(2) 0.2808(2) 0.88488(13) 0.0459(9) Uani 1 1 d . . . C21 C 0.2292(2) 0.2808(2) 0.91110(13) 0.0438(9) Uani 1 1 d . . . H21 H 0.2469 0.3242 0.9323 0.053 Uiso 1 1 calc R . . C22 C 0.2932(2) 0.21479(18) 0.90507(12) 0.0359(8) Uani 1 1 d . . . C23 C 0.2680(2) 0.15041(18) 0.87314(12) 0.0379(8) Uani 1 1 d . . . H23 H 0.3116 0.1068 0.8693 0.045 Uiso 1 1 calc R . . C24 C 0.3890(2) 0.2132(2) 0.93535(13) 0.0393(8) Uani 1 1 d . . . C25 C 0.0865(2) 0.4062(2) 0.92403(16) 0.0699(13) Uani 1 1 d . . . H25A H 0.1376 0.4421 0.9102 0.084 Uiso 1 1 calc R . . H25B H 0.1099 0.3848 0.9570 0.084 Uiso 1 1 calc R . . C26 C -0.0107(2) 0.4522(2) 0.93140(15) 0.0553(10) Uani 1 1 d . . . C27 C -0.0878(3) 0.4170(2) 0.95806(16) 0.0651(11) Uani 1 1 d . . . H27 H -0.0811 0.3639 0.9699 0.078 Uiso 1 1 calc R . . C28 C -0.1759(2) 0.4594(2) 0.96767(15) 0.0542(10) Uani 1 1 d . . . H28 H -0.2273 0.4347 0.9861 0.065 Uiso 1 1 calc R . . C29 C -0.1871(2) 0.5376(2) 0.94997(13) 0.0415(8) Uani 1 1 d . . . C30 C -0.1096(2) 0.5731(2) 0.92294(14) 0.0560(10) Uani 1 1 d . . . H30 H -0.1165 0.6260 0.9106 0.067 Uiso 1 1 calc R . . C31 C -0.0215(2) 0.5308(2) 0.91406(15) 0.0608(11) Uani 1 1 d . . . H31 H 0.0307 0.5557 0.8962 0.073 Uiso 1 1 calc R . . C32 C -0.2822(2) 0.5847(2) 0.96041(15) 0.0472(9) Uani 1 1 d . . . C33 C 0.0326(2) -0.1015(2) 0.77622(13) 0.0474(9) Uani 1 1 d . . . H33 H 0.0284 -0.0567 0.7981 0.057 Uiso 1 1 calc R . . C34 C 0.0866(2) -0.1888(2) 0.72176(14) 0.0533(10) Uani 1 1 d . . . H34 H 0.1279 -0.2156 0.6983 0.064 Uiso 1 1 calc R . . C35 C -0.0063(2) -0.2132(2) 0.73569(14) 0.0515(9) Uani 1 1 d . . . H35 H -0.0400 -0.2593 0.7240 0.062 Uiso 1 1 calc R . . C36 C -0.1348(2) -0.15250(19) 0.79685(12) 0.0390(8) Uani 1 1 d . . . C37 C -0.1786(2) -0.0774(2) 0.80269(13) 0.0464(9) Uani 1 1 d . . . H37 H -0.1498 -0.0317 0.7875 0.056 Uiso 1 1 calc R . . C38 C -0.2652(2) -0.0699(2) 0.83115(13) 0.0472(9) Uani 1 1 d . . . H38 H -0.2942 -0.0190 0.8361 0.057 Uiso 1 1 calc R . . C39 C -0.3085(2) -0.1380(2) 0.85213(13) 0.0412(8) Uani 1 1 d . . . C40 C -0.2673(2) -0.2136(2) 0.84510(14) 0.0550(10) Uani 1 1 d . . . H40 H -0.2982 -0.2595 0.8588 0.066 Uiso 1 1 calc R . . C41 C -0.1792(2) -0.2207(2) 0.81748(14) 0.0501(9) Uani 1 1 d . . . H41 H -0.1500 -0.2715 0.8128 0.060 Uiso 1 1 calc R . . C42 C -0.4141(2) -0.1638(2) 0.92895(13) 0.0463(9) Uani 1 1 d . . . H42 H -0.3754 -0.2058 0.9426 0.056 Uiso 1 1 calc R . . C43 C -0.5276(3) -0.0725(2) 0.91891(15) 0.0605(11) Uani 1 1 d . . . H43 H -0.5835 -0.0399 0.9247 0.073 Uiso 1 1 calc R . . C44 C -0.4682(3) -0.0678(2) 0.87744(15) 0.0593(10) Uani 1 1 d . . . H44 H -0.4742 -0.0316 0.8499 0.071 Uiso 1 1 calc R . . C45 C 0.5968(2) 0.3802(2) 0.90802(14) 0.0472(9) Uani 1 1 d . . . H45 H 0.6340 0.3374 0.9216 0.057 Uiso 1 1 calc R . . C46 C 0.4829(3) 0.4690(2) 0.89601(16) 0.0642(11) Uani 1 1 d . . . H46 H 0.4246 0.4994 0.9000 0.077 Uiso 1 1 calc R . . C47 C 0.5504(3) 0.4803(2) 0.85820(15) 0.0665(12) Uani 1 1 d . . . H47 H 0.5483 0.5192 0.8321 0.080 Uiso 1 1 calc R . . C48 C 0.7137(2) 0.4093(2) 0.83746(13) 0.0402(8) Uani 1 1 d . . . C49 C 0.7667(2) 0.4749(2) 0.81871(13) 0.0478(9) Uani 1 1 d . . . H49 H 0.7430 0.5276 0.8233 0.057 Uiso 1 1 calc R . . C50 C 0.8555(2) 0.4609(2) 0.79296(13) 0.0490(9) Uani 1 1 d . . . H50 H 0.8918 0.5044 0.7796 0.059 Uiso 1 1 calc R . . C51 C 0.8904(2) 0.3826(2) 0.78703(13) 0.0391(8) Uani 1 1 d . . . C52 C 0.8370(2) 0.3175(2) 0.80485(14) 0.0495(9) Uani 1 1 d . . . H52 H 0.8606 0.2647 0.8002 0.059 Uiso 1 1 calc R . . C53 C 0.7472(2) 0.3314(2) 0.82997(14) 0.0488(9) Uani 1 1 d . . . H53 H 0.7093 0.2877 0.8418 0.059 Uiso 1 1 calc R . . C54 C 1.0650(2) 0.4193(2) 0.76938(13) 0.0464(9) Uani 1 1 d . . . H54 H 1.0632 0.4673 0.7885 0.056 Uiso 1 1 calc R . . C55 C 1.0190(2) 0.3051(2) 0.73308(14) 0.0507(9) Uani 1 1 d . . . H55 H 0.9817 0.2603 0.7225 0.061 Uiso 1 1 calc R . . C56 C 1.1158(2) 0.3205(2) 0.72238(14) 0.0506(9) Uani 1 1 d . . . H56 H 1.1569 0.2875 0.7023 0.061 Uiso 1 1 calc R . . H1A H 0.032(3) 0.614(4) 0.6623(12) 0.22(4) Uiso 1 1 d D . . H2A H 0.0562(18) 0.887(3) 0.2430(13) 0.12(2) Uiso 1 1 d D . . H3A H 0.6484(12) 0.122(3) 0.7973(17) 0.14(2) Uiso 1 1 d D . . H1B H 0.046(3) 0.596(3) 0.7141(14) 0.15(2) Uiso 1 1 d D . . H2B H 0.159(2) 0.879(3) 0.2382(12) 0.14(2) Uiso 1 1 d D . . H3B H 0.718(3) 0.130(4) 0.8368(5) 0.16(3) Uiso 1 1 d D . . N1 N 0.11079(18) -0.11813(15) 0.74748(10) 0.0413(7) Uani 1 1 d . . . N2 N -0.04071(18) -0.15666(15) 0.77040(10) 0.0409(7) Uani 1 1 d . . . N3 N -0.39612(18) -0.12708(16) 0.88366(11) 0.0439(7) Uani 1 1 d . . . N4 N -0.49411(19) -0.13268(17) 0.95182(11) 0.0480(7) Uani 1 1 d . . . N5 N 0.51176(18) 0.40672(16) 0.92782(11) 0.0449(7) Uani 1 1 d . . . N6 N 0.62286(18) 0.42260(16) 0.86603(11) 0.0429(7) Uani 1 1 d . . . N7 N 0.98624(18) 0.36988(16) 0.76316(10) 0.0415(7) Uani 1 1 d . . . N8 N 1.14512(18) 0.39228(16) 0.74540(11) 0.0452(7) Uani 1 1 d . . . O1 O 0.55210(15) 0.35195(13) 1.04659(9) 0.0496(6) Uani 1 1 d . . . O2 O 0.62898(14) 0.26160(13) 0.99614(8) 0.0396(5) Uani 1 1 d . . . O3 O 0.74139(16) 0.46975(13) 1.19141(9) 0.0492(6) Uani 1 1 d . . . O4 O 0.86643(18) 0.39970(15) 1.22773(10) 0.0654(8) Uani 1 1 d . . . O5 O 0.93490(16) 0.17840(16) 1.10034(10) 0.0690(8) Uani 1 1 d . . . O6 O 1.34036(17) -0.07538(15) 1.02266(10) 0.0604(7) Uani 1 1 d . . . O7 O 1.28748(19) -0.14273(18) 1.09102(11) 0.0743(8) Uani 1 1 d . . . O8 O 0.21054(16) 0.02159(13) 0.81263(9) 0.0503(6) Uani 1 1 d . . . O9 O 0.07346(18) 0.08504(16) 0.78518(11) 0.0747(9) Uani 1 1 d . . . O10 O 0.45547(14) 0.16094(13) 0.92327(9) 0.0508(6) Uani 1 1 d . . . O11 O 0.39916(14) 0.26002(13) 0.97302(9) 0.0442(6) Uani 1 1 d . . . O12 O 0.06730(16) 0.34134(15) 0.88868(10) 0.0649(8) Uani 1 1 d . . . O13 O -0.30022(19) 0.64718(17) 0.93629(12) 0.0767(9) Uani 1 1 d . . . O14 O -0.33924(16) 0.55553(14) 0.99523(10) 0.0546(7) Uani 1 1 d . . . O1W O -0.0031(2) 0.59860(18) 0.69035(14) 0.0694(8) Uani 1 1 d D . . O2W O 0.1104(3) 0.8770(2) 0.26229(13) 0.0831(9) Uani 1 1 d D . . O3W O 0.7136(3) 0.13144(19) 0.80212(15) 0.0803(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0337(2) 0.0306(2) 0.0485(3) 0.00143(18) 0.00429(17) -0.00225(16) Zn2 0.03140(19) 0.0395(2) 0.0477(3) -0.00345(19) 0.00187(17) 0.01193(16) Zn3 0.02984(19) 0.0380(2) 0.0468(3) -0.00372(19) 0.00053(16) 0.01157(16) C1 0.0357(17) 0.0347(19) 0.046(2) -0.0013(17) 0.0009(16) 0.0069(15) C2 0.0299(16) 0.0372(19) 0.040(2) -0.0040(16) -0.0041(14) 0.0093(14) C3 0.0347(17) 0.0297(18) 0.050(2) -0.0012(16) -0.0009(15) 0.0109(14) C4 0.0342(17) 0.0336(19) 0.043(2) -0.0045(16) -0.0023(15) 0.0063(14) C5 0.0368(17) 0.046(2) 0.048(2) -0.0071(18) -0.0096(15) 0.0112(16) C6 0.0361(18) 0.051(2) 0.059(2) -0.0169(19) -0.0086(16) 0.0201(16) C7 0.0381(18) 0.052(2) 0.048(2) -0.0165(18) -0.0098(16) 0.0183(16) C8 0.045(2) 0.036(2) 0.050(2) -0.0057(17) -0.0040(17) 0.0005(16) C9 0.074(3) 0.107(4) 0.089(3) -0.060(3) -0.031(2) 0.061(3) C10 0.056(3) 0.077(3) 0.074(3) -0.036(3) -0.017(2) 0.038(2) C11 0.074(3) 0.058(3) 0.101(4) -0.015(3) -0.018(3) 0.027(2) C12 0.051(2) 0.059(3) 0.088(3) -0.012(2) -0.001(2) 0.023(2) C13 0.044(2) 0.051(2) 0.052(2) -0.0193(19) -0.0070(17) 0.0231(17) C14 0.055(2) 0.083(3) 0.061(3) -0.007(2) 0.004(2) 0.028(2) C15 0.051(2) 0.110(4) 0.063(3) -0.020(3) 0.001(2) 0.033(3) C16 0.046(2) 0.053(3) 0.054(3) -0.022(2) -0.006(2) 0.0172(19) C17 0.044(2) 0.042(2) 0.058(3) -0.0083(19) 0.0010(18) -0.0013(17) C18 0.0332(17) 0.040(2) 0.046(2) -0.0085(17) 0.0029(15) 0.0060(15) C19 0.0361(18) 0.056(2) 0.051(2) -0.0148(19) -0.0072(16) 0.0104(17) C20 0.0344(18) 0.053(2) 0.051(2) -0.0135(19) -0.0014(16) 0.0203(16) C21 0.0394(18) 0.042(2) 0.050(2) -0.0165(17) -0.0062(16) 0.0147(15) C22 0.0292(16) 0.0377(19) 0.041(2) -0.0081(16) 0.0005(14) 0.0099(14) C23 0.0315(16) 0.0337(19) 0.048(2) -0.0044(16) 0.0011(15) 0.0100(14) C24 0.0314(17) 0.038(2) 0.048(2) 0.0024(18) 0.0006(15) 0.0038(15) C25 0.045(2) 0.072(3) 0.093(3) -0.040(3) -0.010(2) 0.0293(19) C26 0.039(2) 0.060(3) 0.066(3) -0.027(2) -0.0047(19) 0.0182(19) C27 0.062(2) 0.041(2) 0.093(3) -0.006(2) -0.002(2) 0.0224(19) C28 0.043(2) 0.046(2) 0.074(3) -0.003(2) 0.0082(18) 0.0121(17) C29 0.0388(18) 0.042(2) 0.043(2) -0.0104(17) 0.0002(16) 0.0127(16) C30 0.048(2) 0.055(2) 0.064(3) 0.000(2) 0.0112(19) 0.0153(18) C31 0.044(2) 0.067(3) 0.072(3) -0.009(2) 0.0133(19) 0.0138(19) C32 0.0394(19) 0.049(2) 0.053(3) -0.011(2) -0.0007(18) 0.0141(17) C33 0.051(2) 0.043(2) 0.049(2) -0.0157(17) 0.0119(18) -0.0161(17) C34 0.049(2) 0.045(2) 0.065(3) -0.009(2) 0.0140(19) -0.0018(18) C35 0.054(2) 0.036(2) 0.065(3) -0.0150(19) 0.0079(19) -0.0120(17) C36 0.0374(18) 0.041(2) 0.039(2) -0.0017(16) 0.0042(15) -0.0099(15) C37 0.054(2) 0.034(2) 0.052(2) 0.0042(17) 0.0084(18) -0.0094(16) C38 0.052(2) 0.034(2) 0.055(2) 0.0040(17) 0.0083(18) 0.0001(16) C39 0.0398(18) 0.042(2) 0.042(2) 0.0052(17) 0.0039(15) -0.0008(16) C40 0.055(2) 0.041(2) 0.069(3) 0.0105(19) 0.021(2) -0.0020(18) C41 0.050(2) 0.034(2) 0.066(3) 0.0053(18) 0.0179(18) -0.0002(16) C42 0.0418(19) 0.043(2) 0.054(2) 0.0111(18) 0.0113(17) 0.0099(16) C43 0.057(2) 0.056(2) 0.069(3) 0.011(2) 0.014(2) 0.0253(19) C44 0.064(2) 0.056(2) 0.057(3) 0.019(2) 0.007(2) 0.020(2) C45 0.0411(19) 0.045(2) 0.056(3) 0.0083(19) 0.0064(17) 0.0108(16) C46 0.065(2) 0.054(3) 0.073(3) 0.017(2) 0.019(2) 0.035(2) C47 0.074(3) 0.056(3) 0.069(3) 0.022(2) 0.018(2) 0.034(2) C48 0.0360(18) 0.042(2) 0.042(2) 0.0000(17) 0.0026(15) 0.0024(15) C49 0.051(2) 0.036(2) 0.056(2) -0.0005(18) 0.0062(18) 0.0032(16) C50 0.049(2) 0.042(2) 0.056(2) 0.0068(18) 0.0096(18) -0.0038(17) C51 0.0335(17) 0.042(2) 0.042(2) -0.0011(16) 0.0010(15) -0.0008(15) C52 0.0453(19) 0.0297(19) 0.073(3) -0.0030(18) 0.0099(18) -0.0027(16) C53 0.0407(19) 0.038(2) 0.068(3) 0.0028(19) 0.0148(18) -0.0053(16) C54 0.046(2) 0.037(2) 0.056(2) -0.0119(18) 0.0061(17) -0.0055(16) C55 0.048(2) 0.040(2) 0.063(3) -0.0127(19) 0.0026(18) -0.0067(17) C56 0.044(2) 0.041(2) 0.066(3) -0.0100(19) 0.0124(18) -0.0001(16) N1 0.0399(15) 0.0360(16) 0.0481(18) -0.0066(14) 0.0088(13) -0.0085(12) N2 0.0413(15) 0.0373(16) 0.0441(18) -0.0059(14) 0.0100(13) -0.0124(13) N3 0.0422(15) 0.0410(17) 0.0484(19) 0.0091(15) 0.0087(14) 0.0048(13) N4 0.0449(16) 0.0432(17) 0.056(2) 0.0096(15) 0.0090(14) 0.0121(14) N5 0.0408(16) 0.0399(17) 0.0539(19) 0.0010(15) 0.0088(14) 0.0090(13) N6 0.0406(15) 0.0423(17) 0.0460(18) 0.0047(15) 0.0078(13) 0.0054(13) N7 0.0357(15) 0.0397(16) 0.0491(18) -0.0052(14) 0.0057(13) -0.0068(13) N8 0.0396(15) 0.0387(17) 0.057(2) -0.0075(14) 0.0114(14) -0.0034(13) O1 0.0366(12) 0.0544(15) 0.0576(16) -0.0168(12) -0.0100(11) 0.0233(11) O2 0.0358(12) 0.0430(13) 0.0399(14) -0.0071(11) -0.0035(10) 0.0072(10) O3 0.0550(14) 0.0389(14) 0.0536(16) -0.0120(12) -0.0069(11) 0.0151(11) O4 0.0690(17) 0.0557(17) 0.071(2) -0.0225(14) -0.0355(14) 0.0178(13) O5 0.0532(14) 0.0774(19) 0.0763(19) -0.0369(16) -0.0260(13) 0.0445(14) O6 0.0466(14) 0.0599(17) 0.0747(19) -0.0077(14) 0.0071(14) 0.0257(12) O7 0.0748(18) 0.074(2) 0.075(2) 0.0011(17) -0.0006(15) 0.0370(15) O8 0.0570(14) 0.0401(14) 0.0539(16) -0.0101(12) -0.0048(12) 0.0075(12) O9 0.0601(16) 0.0618(18) 0.102(2) -0.0287(17) -0.0355(16) 0.0106(14) O10 0.0329(12) 0.0535(15) 0.0659(17) -0.0165(13) -0.0087(11) 0.0217(11) O11 0.0441(13) 0.0399(14) 0.0485(15) -0.0091(12) -0.0082(11) 0.0046(10) O12 0.0494(14) 0.0697(18) 0.0754(19) -0.0362(15) -0.0217(13) 0.0372(13) O13 0.0680(17) 0.0677(19) 0.094(2) 0.0219(17) 0.0152(15) 0.0389(15) O14 0.0419(13) 0.0555(16) 0.0665(18) -0.0018(13) 0.0141(13) 0.0191(12) O1W 0.0605(16) 0.074(2) 0.074(2) -0.0151(17) -0.0107(17) -0.0034(15) O2W 0.0654(19) 0.083(2) 0.100(3) -0.006(2) -0.011(2) 0.0009(18) O3W 0.086(3) 0.062(2) 0.092(3) 0.0006(19) 0.0076(17) -0.0034(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O8 1.940(2) . ? Zn1 O3 1.950(2) 4_565 ? Zn1 N8 1.996(3) 2_646 ? Zn1 N1 1.997(2) . ? Zn2 O6 1.935(2) 3_757 ? Zn2 O10 1.986(2) . ? Zn2 O2 1.990(2) . ? Zn2 N4 2.008(3) 3_557 ? Zn3 O14 1.929(2) 3_567 ? Zn3 O1 1.957(2) . ? Zn3 O11 1.993(2) . ? Zn3 N5 1.998(3) . ? C1 O1 1.257(3) . ? C1 O2 1.264(3) . ? C1 C2 1.493(4) . ? C2 C3 1.383(4) . ? C2 C7 1.390(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 C8 1.507(4) . ? C5 C6 1.380(4) . ? C5 H5 0.9300 . ? C6 O5 1.372(3) . ? C6 C7 1.390(4) . ? C7 H7 0.9300 . ? C8 O4 1.228(4) . ? C8 O3 1.283(4) . ? C9 O5 1.435(4) . ? C9 C10 1.517(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.361(6) . ? C10 C11 1.373(6) . ? C11 C12 1.397(5) . ? C11 H11 0.9300 . ? C12 C13 1.370(5) . ? C12 H12 0.9300 . ? C13 C14 1.376(5) . ? C13 C16 1.504(4) . ? C14 C15 1.387(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.231(4) . ? C16 O6 1.273(4) . ? C17 O9 1.228(4) . ? C17 O8 1.278(4) . ? C17 C18 1.498(4) . ? C18 C19 1.373(4) . ? C18 C23 1.393(4) . ? C19 C20 1.388(4) . ? C19 H19 0.9300 . ? C20 O12 1.378(3) . ? C20 C21 1.387(4) . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.382(4) . ? C22 C24 1.497(4) . ? C23 H23 0.9300 . ? C24 O11 1.246(4) . ? C24 O10 1.274(3) . ? C25 O12 1.426(4) . ? C25 C26 1.514(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.367(5) . ? C26 C31 1.373(5) . ? C27 C28 1.389(4) . ? C27 H27 0.9300 . ? C28 C29 1.371(4) . ? C28 H28 0.9300 . ? C29 C30 1.378(4) . ? C29 C32 1.512(4) . ? C30 C31 1.386(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O13 1.224(4) . ? C32 O14 1.273(4) . ? C33 N1 1.310(4) . ? C33 N2 1.342(4) . ? C33 H33 0.9300 . ? C34 C35 1.353(4) . ? C34 N1 1.375(4) . ? C34 H34 0.9300 . ? C35 N2 1.371(4) . ? C35 H35 0.9300 . ? C36 C37 1.375(4) . ? C36 C41 1.376(4) . ? C36 N2 1.431(4) . ? C37 C38 1.376(4) . ? C37 H37 0.9300 . ? C38 C39 1.372(4) . ? C38 H38 0.9300 . ? C39 C40 1.371(4) . ? C39 N3 1.437(4) . ? C40 C41 1.380(4) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 N4 1.324(4) . ? C42 N3 1.337(4) . ? C42 H42 0.9300 . ? C43 C44 1.336(5) . ? C43 N4 1.378(4) . ? C43 H43 0.9300 . ? C44 N3 1.378(4) . ? C44 H44 0.9300 . ? C45 N5 1.320(4) . ? C45 N6 1.334(4) . ? C45 H45 0.9300 . ? C46 C47 1.342(5) . ? C46 N5 1.367(4) . ? C46 H46 0.9300 . ? C47 N6 1.369(4) . ? C47 H47 0.9300 . ? C48 C53 1.368(4) . ? C48 C49 1.378(4) . ? C48 N6 1.437(4) . ? C49 C50 1.379(4) . ? C49 H49 0.9300 . ? C50 C51 1.378(4) . ? C50 H50 0.9300 . ? C51 C52 1.366(4) . ? C51 N7 1.436(4) . ? C52 C53 1.383(4) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 N8 1.314(4) . ? C54 N7 1.338(4) . ? C54 H54 0.9300 . ? C55 C56 1.345(4) . ? C55 N7 1.388(4) . ? C55 H55 0.9300 . ? C56 N8 1.377(4) . ? C56 H56 0.9300 . ? N4 Zn2 2.008(3) 3_557 ? N8 Zn1 1.996(3) 2_656 ? O3 Zn1 1.950(2) 4_666 ? O6 Zn2 1.935(2) 3_757 ? O14 Zn3 1.929(2) 3_567 ? O1W H1A 0.898(10) . ? O1W H1B 0.900(10) . ? O2W H2A 0.894(10) . ? O2W H2B 0.898(10) . ? O3W H3A 0.892(10) . ? O3W H3B 0.898(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Zn1 O3 108.51(10) . 4_565 ? O8 Zn1 N8 110.63(10) . 2_646 ? O3 Zn1 N8 107.11(10) 4_565 2_646 ? O8 Zn1 N1 105.79(10) . . ? O3 Zn1 N1 115.04(10) 4_565 . ? N8 Zn1 N1 109.77(11) 2_646 . ? O6 Zn2 O10 118.28(10) 3_757 . ? O6 Zn2 O2 105.54(10) 3_757 . ? O10 Zn2 O2 117.98(9) . . ? O6 Zn2 N4 99.96(11) 3_757 3_557 ? O10 Zn2 N4 111.17(11) . 3_557 ? O2 Zn2 N4 101.17(10) . 3_557 ? O14 Zn3 O1 121.82(10) 3_567 . ? O14 Zn3 O11 111.43(9) 3_567 . ? O1 Zn3 O11 106.60(9) . . ? O14 Zn3 N5 104.50(11) 3_567 . ? O1 Zn3 N5 109.83(11) . . ? O11 Zn3 N5 100.64(10) . . ? O1 C1 O2 124.1(3) . . ? O1 C1 C2 118.0(3) . . ? O2 C1 C2 117.9(3) . . ? C3 C2 C7 120.3(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 119.1(3) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.2(3) . . ? C5 C4 C8 120.3(3) . . ? C3 C4 C8 120.5(3) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? O5 C6 C5 116.3(3) . . ? O5 C6 C7 123.9(3) . . ? C5 C6 C7 119.8(3) . . ? C6 C7 C2 119.5(3) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O4 C8 O3 125.4(3) . . ? O4 C8 C4 119.6(3) . . ? O3 C8 C4 114.9(3) . . ? O5 C9 C10 108.0(3) . . ? O5 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? O5 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C15 C10 C11 119.5(4) . . ? C15 C10 C9 120.5(4) . . ? C11 C10 C9 120.1(5) . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.5(3) . . ? C12 C13 C16 120.2(4) . . ? C14 C13 C16 120.3(4) . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 120.7(4) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O7 C16 O6 122.9(3) . . ? O7 C16 C13 121.6(4) . . ? O6 C16 C13 115.5(4) . . ? O9 C17 O8 124.7(3) . . ? O9 C17 C18 120.0(3) . . ? O8 C17 C18 115.3(3) . . ? C19 C18 C23 119.4(3) . . ? C19 C18 C17 120.8(3) . . ? C23 C18 C17 119.8(3) . . ? C18 C19 C20 120.9(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? O12 C20 C21 124.4(3) . . ? O12 C20 C19 115.5(3) . . ? C21 C20 C19 120.0(3) . . ? C20 C21 C22 118.8(3) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 121.0(3) . . ? C23 C22 C24 120.3(3) . . ? C21 C22 C24 118.7(3) . . ? C22 C23 C18 119.8(3) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? O11 C24 O10 122.2(3) . . ? O11 C24 C22 119.2(3) . . ? O10 C24 C22 118.6(3) . . ? O12 C25 C26 107.5(3) . . ? O12 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O12 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C27 C26 C31 118.9(3) . . ? C27 C26 C25 119.8(4) . . ? C31 C26 C25 121.2(4) . . ? C26 C27 C28 121.0(4) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.0(3) . . ? C28 C29 C32 120.8(3) . . ? C30 C29 C32 120.3(3) . . ? C29 C30 C31 120.6(4) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C26 C31 C30 120.4(4) . . ? C26 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? O13 C32 O14 123.9(3) . . ? O13 C32 C29 120.2(3) . . ? O14 C32 C29 115.9(3) . . ? N1 C33 N2 112.2(3) . . ? N1 C33 H33 123.9 . . ? N2 C33 H33 123.9 . . ? C35 C34 N1 109.7(3) . . ? C35 C34 H34 125.1 . . ? N1 C34 H34 125.1 . . ? C34 C35 N2 106.3(3) . . ? C34 C35 H35 126.9 . . ? N2 C35 H35 126.9 . . ? C37 C36 C41 120.3(3) . . ? C37 C36 N2 118.0(3) . . ? C41 C36 N2 121.7(3) . . ? C36 C37 C38 119.8(3) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 119.5(3) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 121.2(3) . . ? C38 C39 N3 117.7(3) . . ? C40 C39 N3 121.0(3) . . ? C39 C40 C41 119.1(3) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C36 C41 C40 120.0(3) . . ? C36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? N4 C42 N3 111.1(3) . . ? N4 C42 H42 124.4 . . ? N3 C42 H42 124.4 . . ? C44 C43 N4 110.0(3) . . ? C44 C43 H43 125.0 . . ? N4 C43 H43 125.0 . . ? C43 C44 N3 106.3(3) . . ? C43 C44 H44 126.8 . . ? N3 C44 H44 126.8 . . ? N5 C45 N6 111.6(3) . . ? N5 C45 H45 124.2 . . ? N6 C45 H45 124.2 . . ? C47 C46 N5 110.5(3) . . ? C47 C46 H46 124.7 . . ? N5 C46 H46 124.7 . . ? C46 C47 N6 105.8(3) . . ? C46 C47 H47 127.1 . . ? N6 C47 H47 127.1 . . ? C53 C48 C49 121.0(3) . . ? C53 C48 N6 119.4(3) . . ? C49 C48 N6 119.6(3) . . ? C48 C49 C50 118.8(3) . . ? C48 C49 H49 120.6 . . ? C50 C49 H49 120.6 . . ? C51 C50 C49 120.0(3) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 121.2(3) . . ? C52 C51 N7 119.7(3) . . ? C50 C51 N7 119.0(3) . . ? C51 C52 C53 118.7(3) . . ? C51 C52 H52 120.6 . . ? C53 C52 H52 120.6 . . ? C48 C53 C52 120.3(3) . . ? C48 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? N8 C54 N7 112.2(3) . . ? N8 C54 H54 123.9 . . ? N7 C54 H54 123.9 . . ? C56 C55 N7 105.9(3) . . ? C56 C55 H55 127.0 . . ? N7 C55 H55 127.0 . . ? C55 C56 N8 110.2(3) . . ? C55 C56 H56 124.9 . . ? N8 C56 H56 124.9 . . ? C33 N1 C34 105.2(3) . . ? C33 N1 Zn1 118.5(2) . . ? C34 N1 Zn1 136.3(2) . . ? C33 N2 C35 106.6(3) . . ? C33 N2 C36 123.6(3) . . ? C35 N2 C36 129.7(3) . . ? C42 N3 C44 107.2(3) . . ? C42 N3 C39 125.8(3) . . ? C44 N3 C39 126.2(3) . . ? C42 N4 C43 105.3(3) . . ? C42 N4 Zn2 130.6(2) . 3_557 ? C43 N4 Zn2 124.0(2) . 3_557 ? C45 N5 C46 104.9(3) . . ? C45 N5 Zn3 126.5(2) . . ? C46 N5 Zn3 128.4(2) . . ? C45 N6 C47 107.2(3) . . ? C45 N6 C48 123.9(3) . . ? C47 N6 C48 128.8(3) . . ? C54 N7 C55 106.5(3) . . ? C54 N7 C51 124.1(3) . . ? C55 N7 C51 129.3(3) . . ? C54 N8 C56 105.2(3) . . ? C54 N8 Zn1 118.9(2) . 2_656 ? C56 N8 Zn1 135.9(2) . 2_656 ? C1 O1 Zn3 119.1(2) . . ? C1 O2 Zn2 127.7(2) . . ? C8 O3 Zn1 119.4(2) . 4_666 ? C6 O5 C9 116.0(2) . . ? C16 O6 Zn2 111.9(2) . 3_757 ? C17 O8 Zn1 119.3(2) . . ? C24 O10 Zn2 108.0(2) . . ? C24 O11 Zn3 143.5(2) . . ? C20 O12 C25 117.6(2) . . ? C32 O14 Zn3 108.4(2) . 3_567 ? H1A O1W H1B 100.4(15) . . ? H2A O2W H2B 101.0(15) . . ? H3A O3W H3B 101.6(15) . . ? 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 O1 C1 C2 C3 -8.3(5) . . . . ? O2 C1 C2 C3 169.2(3) . . . . ? O1 C1 C2 C7 172.8(3) . . . . ? O2 C1 C2 C7 -9.6(5) . . . . ? C7 C2 C3 C4 1.2(5) . . . . ? C1 C2 C3 C4 -177.6(3) . . . . ? C2 C3 C4 C5 -1.9(5) . . . . ? C2 C3 C4 C8 177.2(3) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C8 C4 C5 C6 -177.7(3) . . . . ? C4 C5 C6 O5 178.7(3) . . . . ? C4 C5 C6 C7 -0.2(5) . . . . ? O5 C6 C7 C2 -179.3(3) . . . . ? C5 C6 C7 C2 -0.4(5) . . . . ? C3 C2 C7 C6 -0.1(5) . . . . ? C1 C2 C7 C6 178.7(3) . . . . ? C5 C4 C8 O4 -9.0(5) . . . . ? C3 C4 C8 O4 171.9(3) . . . . ? C5 C4 C8 O3 168.3(3) . . . . ? C3 C4 C8 O3 -10.8(4) . . . . ? O5 C9 C10 C15 91.0(5) . . . . ? O5 C9 C10 C11 -90.8(5) . . . . ? C15 C10 C11 C12 1.4(6) . . . . ? C9 C10 C11 C12 -176.8(4) . . . . ? C10 C11 C12 C13 -1.3(6) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C11 C12 C13 C16 -179.9(3) . . . . ? C12 C13 C14 C15 1.3(6) . . . . ? C16 C13 C14 C15 -178.9(3) . . . . ? C11 C10 C15 C14 -0.2(6) . . . . ? C9 C10 C15 C14 178.0(3) . . . . ? C13 C14 C15 C10 -1.2(6) . . . . ? C12 C13 C16 O7 162.5(4) . . . . ? C14 C13 C16 O7 -17.3(5) . . . . ? C12 C13 C16 O6 -18.2(5) . . . . ? C14 C13 C16 O6 162.0(3) . . . . ? O9 C17 C18 C19 5.5(5) . . . . ? O8 C17 C18 C19 -174.5(3) . . . . ? O9 C17 C18 C23 -173.9(3) . . . . ? O8 C17 C18 C23 6.2(5) . . . . ? C23 C18 C19 C20 -0.4(5) . . . . ? C17 C18 C19 C20 -179.8(3) . . . . ? C18 C19 C20 O12 -178.4(3) . . . . ? C18 C19 C20 C21 0.8(5) . . . . ? O12 C20 C21 C22 178.2(3) . . . . ? C19 C20 C21 C22 -0.9(5) . . . . ? C20 C21 C22 C23 0.7(5) . . . . ? C20 C21 C22 C24 -177.2(3) . . . . ? C21 C22 C23 C18 -0.4(5) . . . . ? C24 C22 C23 C18 177.5(3) . . . . ? C19 C18 C23 C22 0.2(5) . . . . ? C17 C18 C23 C22 179.6(3) . . . . ? C23 C22 C24 O11 -162.0(3) . . . . ? C21 C22 C24 O11 15.9(5) . . . . ? C23 C22 C24 O10 14.4(5) . . . . ? C21 C22 C24 O10 -167.7(3) . . . . ? O12 C25 C26 C27 70.3(5) . . . . ? O12 C25 C26 C31 -113.1(4) . . . . ? C31 C26 C27 C28 0.0(6) . . . . ? C25 C26 C27 C28 176.7(3) . . . . ? C26 C27 C28 C29 0.6(6) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C27 C28 C29 C32 -179.6(3) . . . . ? C28 C29 C30 C31 -0.4(5) . . . . ? C32 C29 C30 C31 178.8(3) . . . . ? C27 C26 C31 C30 -0.8(6) . . . . ? C25 C26 C31 C30 -177.4(3) . . . . ? C29 C30 C31 C26 1.0(6) . . . . ? C28 C29 C32 O13 -165.4(4) . . . . ? C30 C29 C32 O13 15.4(5) . . . . ? C28 C29 C32 O14 15.1(5) . . . . ? C30 C29 C32 O14 -164.1(3) . . . . ? N1 C34 C35 N2 0.4(4) . . . . ? C41 C36 C37 C38 2.7(5) . . . . ? N2 C36 C37 C38 -175.2(3) . . . . ? C36 C37 C38 C39 -1.9(5) . . . . ? C37 C38 C39 C40 -0.3(5) . . . . ? C37 C38 C39 N3 177.1(3) . . . . ? C38 C39 C40 C41 1.7(5) . . . . ? N3 C39 C40 C41 -175.6(3) . . . . ? C37 C36 C41 C40 -1.3(5) . . . . ? N2 C36 C41 C40 176.6(3) . . . . ? C39 C40 C41 C36 -0.9(5) . . . . ? N4 C43 C44 N3 0.9(5) . . . . ? N5 C46 C47 N6 0.9(5) . . . . ? C53 C48 C49 C50 -1.2(5) . . . . ? N6 C48 C49 C50 177.8(3) . . . . ? C48 C49 C50 C51 -0.9(5) . . . . ? C49 C50 C51 C52 2.1(5) . . . . ? C49 C50 C51 N7 -175.9(3) . . . . ? C50 C51 C52 C53 -1.0(5) . . . . ? N7 C51 C52 C53 176.9(3) . . . . ? C49 C48 C53 C52 2.3(5) . . . . ? N6 C48 C53 C52 -176.7(3) . . . . ? C51 C52 C53 C48 -1.1(5) . . . . ? N7 C55 C56 N8 0.8(4) . . . . ? N2 C33 N1 C34 -0.4(4) . . . . ? N2 C33 N1 Zn1 179.9(2) . . . . ? C35 C34 N1 C33 0.0(4) . . . . ? C35 C34 N1 Zn1 179.6(3) . . . . ? O8 Zn1 N1 C33 16.4(3) . . . . ? O3 Zn1 N1 C33 -103.3(3) 4_565 . . . ? N8 Zn1 N1 C33 135.8(3) 2_646 . . . ? O8 Zn1 N1 C34 -163.1(3) . . . . ? O3 Zn1 N1 C34 77.2(4) 4_565 . . . ? N8 Zn1 N1 C34 -43.7(4) 2_646 . . . ? N1 C33 N2 C35 0.6(4) . . . . ? N1 C33 N2 C36 -179.3(3) . . . . ? C34 C35 N2 C33 -0.6(4) . . . . ? C34 C35 N2 C36 179.3(3) . . . . ? C37 C36 N2 C33 39.3(5) . . . . ? C41 C36 N2 C33 -138.6(4) . . . . ? C37 C36 N2 C35 -140.5(4) . . . . ? C41 C36 N2 C35 41.5(5) . . . . ? N4 C42 N3 C44 1.0(4) . . . . ? N4 C42 N3 C39 171.2(3) . . . . ? C43 C44 N3 C42 -1.2(4) . . . . ? C43 C44 N3 C39 -171.4(3) . . . . ? C38 C39 N3 C42 -136.1(4) . . . . ? C40 C39 N3 C42 41.2(5) . . . . ? C38 C39 N3 C44 32.3(5) . . . . ? C40 C39 N3 C44 -150.4(4) . . . . ? N3 C42 N4 C43 -0.4(4) . . . . ? N3 C42 N4 Zn2 -178.1(2) . . . 3_557 ? C44 C43 N4 C42 -0.4(4) . . . . ? C44 C43 N4 Zn2 177.5(3) . . . 3_557 ? N6 C45 N5 C46 0.4(4) . . . . ? N6 C45 N5 Zn3 -174.2(2) . . . . ? C47 C46 N5 C45 -0.8(5) . . . . ? C47 C46 N5 Zn3 173.6(3) . . . . ? O14 Zn3 N5 C45 171.1(3) 3_567 . . . ? O1 Zn3 N5 C45 38.9(3) . . . . ? O11 Zn3 N5 C45 -73.2(3) . . . . ? O14 Zn3 N5 C46 -2.1(3) 3_567 . . . ? O1 Zn3 N5 C46 -134.3(3) . . . . ? O11 Zn3 N5 C46 113.5(3) . . . . ? N5 C45 N6 C47 0.2(4) . . . . ? N5 C45 N6 C48 177.7(3) . . . . ? C46 C47 N6 C45 -0.7(4) . . . . ? C46 C47 N6 C48 -178.0(3) . . . . ? C53 C48 N6 C45 39.1(5) . . . . ? C49 C48 N6 C45 -139.9(3) . . . . ? C53 C48 N6 C47 -144.0(4) . . . . ? C49 C48 N6 C47 37.0(5) . . . . ? N8 C54 N7 C55 0.7(4) . . . . ? N8 C54 N7 C51 177.1(3) . . . . ? C56 C55 N7 C54 -0.9(4) . . . . ? C56 C55 N7 C51 -177.0(3) . . . . ? C52 C51 N7 C54 -142.1(3) . . . . ? C50 C51 N7 C54 35.8(5) . . . . ? C52 C51 N7 C55 33.4(5) . . . . ? C50 C51 N7 C55 -148.7(3) . . . . ? N7 C54 N8 C56 -0.2(4) . . . . ? N7 C54 N8 Zn1 180.0(2) . . . 2_656 ? C55 C56 N8 C54 -0.4(4) . . . . ? C55 C56 N8 Zn1 179.3(3) . . . 2_656 ? O2 C1 O1 Zn3 -3.9(4) . . . . ? C2 C1 O1 Zn3 173.5(2) . . . . ? O14 Zn3 O1 C1 -178.7(2) 3_567 . . . ? O11 Zn3 O1 C1 52.0(3) . . . . ? N5 Zn3 O1 C1 -56.2(3) . . . . ? O1 C1 O2 Zn2 -79.2(4) . . . . ? C2 C1 O2 Zn2 103.4(3) . . . . ? O6 Zn2 O2 C1 -112.8(2) 3_757 . . . ? O10 Zn2 O2 C1 112.4(2) . . . . ? N4 Zn2 O2 C1 -9.0(2) 3_557 . . . ? O4 C8 O3 Zn1 -13.5(5) . . . 4_666 ? C4 C8 O3 Zn1 169.4(2) . . . 4_666 ? C5 C6 O5 C9 -179.2(4) . . . . ? C7 C6 O5 C9 -0.2(6) . . . . ? C10 C9 O5 C6 177.9(4) . . . . ? O7 C16 O6 Zn2 6.8(5) . . . 3_757 ? C13 C16 O6 Zn2 -172.5(2) . . . 3_757 ? O9 C17 O8 Zn1 31.0(5) . . . . ? C18 C17 O8 Zn1 -149.0(2) . . . . ? O3 Zn1 O8 C17 44.7(3) 4_565 . . . ? N8 Zn1 O8 C17 161.9(2) 2_646 . . . ? N1 Zn1 O8 C17 -79.2(3) . . . . ? O11 C24 O10 Zn2 8.7(4) . . . . ? C22 C24 O10 Zn2 -167.6(2) . . . . ? O6 Zn2 O10 C24 172.2(2) 3_757 . . . ? O2 Zn2 O10 C24 -58.7(2) . . . . ? N4 Zn2 O10 C24 57.4(2) 3_557 . . . ? O10 C24 O11 Zn3 92.0(4) . . . . ? C22 C24 O11 Zn3 -91.7(4) . . . . ? O14 Zn3 O11 C24 103.8(3) 3_567 . . . ? O1 Zn3 O11 C24 -121.1(3) . . . . ? N5 Zn3 O11 C24 -6.5(3) . . . . ? C21 C20 O12 C25 -3.4(5) . . . . ? C19 C20 O12 C25 175.7(3) . . . . ? C26 C25 O12 C20 -166.0(3) . . . . ? O13 C32 O14 Zn3 -4.6(4) . . . 3_567 ? C29 C32 O14 Zn3 174.9(2) . . . 3_567 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.401 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.057