# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Key Lab of Polyoxometalate Science Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= data_1 _database_code_depnum_ccdc_archive 'CCDC 826242' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H25 N7 O4 Zn, H2 O ' _chemical_formula_sum 'C35 H27 N7 O5 Zn' _chemical_formula_weight 691.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.17650(10) _cell_length_b 16.0472(2) _cell_length_c 20.1566(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.6190(10) _cell_angle_gamma 90.00 _cell_volume 3275.84(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5715 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 67.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17945 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.41 _diffrn_reflns_theta_max 67.21 _reflns_number_total 5715 _reflns_number_gt 4374 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5715 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.004 _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 0.39457(3) 0.15471(2) 0.055533(19) 0.04934(16) Uani 1 1 d . . . C1 C 0.8937(3) 0.19902(18) 0.07030(14) 0.0465(6) Uani 1 1 d . . . H1 H 0.8877 0.1584 0.0372 0.056 Uiso 1 1 calc R . . C2 C 1.0174(2) 0.22821(17) 0.09555(14) 0.0464(6) Uani 1 1 d . . . C3 C 1.0250(3) 0.28882(18) 0.14470(15) 0.0521(6) Uani 1 1 d . . . H3 H 1.1071 0.3087 0.1621 0.063 Uiso 1 1 calc R . . C4 C 0.9122(3) 0.3199(2) 0.16793(17) 0.0606(8) Uani 1 1 d . . . H4 H 0.9186 0.3605 0.2010 0.073 Uiso 1 1 calc R . . C5 C 0.7892(3) 0.29120(18) 0.14254(16) 0.0561(7) Uani 1 1 d . . . H5 H 0.7131 0.3129 0.1580 0.067 Uiso 1 1 calc R . . C6 C 0.7801(3) 0.22937(17) 0.09354(14) 0.0458(6) Uani 1 1 d . . . C7 C 0.6500(3) 0.18965(18) 0.06987(15) 0.0490(6) Uani 1 1 d . . . C8 C 1.1385(3) 0.1910(2) 0.07098(18) 0.0599(8) Uani 1 1 d . . . C9 C 0.1335(3) -0.20427(18) -0.33837(15) 0.0543(7) Uani 1 1 d . . . C10 C 0.2646(3) -0.2123(2) -0.31238(18) 0.0646(8) Uani 1 1 d . . . H10 H 0.3094 -0.1663 -0.2934 0.078 Uiso 1 1 calc R . . C11 C 0.3289(3) -0.2876(2) -0.31443(19) 0.0653(8) Uani 1 1 d . . . H9 H 0.4165 -0.2924 -0.2968 0.078 Uiso 1 1 calc R . . C12 C 0.2634(3) -0.35580(18) -0.34262(16) 0.0581(7) Uani 1 1 d . . . C13 C 0.1337(3) -0.34927(19) -0.36806(18) 0.0620(8) Uani 1 1 d . . . H13 H 0.0892 -0.3956 -0.3867 0.074 Uiso 1 1 calc R . . C14 C 0.0695(3) -0.2737(2) -0.36584(17) 0.0629(8) Uani 1 1 d . . . H12 H -0.0183 -0.2695 -0.3832 0.075 Uiso 1 1 calc R . . C15 C 0.3232(3) -0.4842(2) -0.39988(16) 0.0617(8) Uani 1 1 d . . . H16 H 0.2727 -0.4730 -0.4399 0.074 Uiso 1 1 calc R . . C16 C 0.4542(4) -0.5431(2) -0.3255(2) 0.0762(10) Uani 1 1 d . . . H17 H 0.5123 -0.5814 -0.3040 0.091 Uiso 1 1 calc R . . C17 C 0.4160(4) -0.4711(2) -0.2986(2) 0.0825(11) Uani 1 1 d . . . H15 H 0.4419 -0.4510 -0.2560 0.099 Uiso 1 1 calc R . . C18 C 0.1171(3) -0.06778(18) -0.28633(14) 0.0549(7) Uani 1 1 d . . . C19 C 0.1034(4) -0.0827(2) -0.21996(16) 0.0703(9) Uani 1 1 d . . . H19 H 0.0603 -0.1305 -0.2075 0.084 Uiso 1 1 calc R . . C20 C 0.1539(4) -0.0266(2) -0.17187(16) 0.0673(9) Uani 1 1 d . . . H20 H 0.1431 -0.0360 -0.1272 0.081 Uiso 1 1 calc R . . C21 C 0.2199(3) 0.04291(17) -0.19038(14) 0.0506(6) Uani 1 1 d . . . C22 C 0.2344(3) 0.05880(19) -0.25625(14) 0.0550(7) Uani 1 1 d . . . H22 H 0.2789 0.1062 -0.2684 0.066 Uiso 1 1 calc R . . C23 C 0.1816(3) 0.0032(2) -0.30427(15) 0.0575(7) Uani 1 1 d . . . H23 H 0.1897 0.0137 -0.3490 0.069 Uiso 1 1 calc R . . C24 C 0.2934(5) 0.1843(2) -0.14644(18) 0.0815(11) Uani 1 1 d . . . H26 H 0.2727 0.2162 -0.1846 0.098 Uiso 1 1 calc R . . C25 C 0.3455(5) 0.2114(3) -0.08731(19) 0.0830(11) Uani 1 1 d . . . H25 H 0.3684 0.2664 -0.0774 0.100 Uiso 1 1 calc R . . C26 C 0.3161(3) 0.0806(2) -0.07713(15) 0.0611(8) Uani 1 1 d . . . H24 H 0.3130 0.0273 -0.0593 0.073 Uiso 1 1 calc R . . C27 C -0.0265(3) -0.09930(19) -0.38694(15) 0.0564(7) Uani 1 1 d . . . C28 C -0.1227(3) -0.0435(2) -0.37173(17) 0.0663(8) Uani 1 1 d . . . H28 H -0.1230 -0.0242 -0.3283 0.080 Uiso 1 1 calc R . . C29 C -0.2181(3) -0.0161(2) -0.42008(18) 0.0683(9) Uani 1 1 d . . . H29 H -0.2824 0.0212 -0.4090 0.082 Uiso 1 1 calc R . . C30 C -0.2184(3) -0.0440(2) -0.48501(16) 0.0591(7) Uani 1 1 d . . . C31 C -0.1209(3) -0.0971(2) -0.50118(16) 0.0657(8) Uani 1 1 d . . . H31 H -0.1194 -0.1147 -0.5450 0.079 Uiso 1 1 calc R . . C32 C -0.0246(4) -0.1246(2) -0.45292(16) 0.0645(8) Uani 1 1 d . . . H32 H 0.0415 -0.1602 -0.4646 0.077 Uiso 1 1 calc R . . C33 C -0.3638(4) 0.0587(3) -0.5495(2) 0.0779(10) Uani 1 1 d . . . H33 H -0.3356 0.1076 -0.5277 0.094 Uiso 1 1 calc R . . C34 C -0.4567(4) 0.0510(3) -0.6016(2) 0.0889(12) Uani 1 1 d . . . H34 H -0.5035 0.0955 -0.6219 0.107 Uiso 1 1 calc R . . C35 C -0.3890(4) -0.0705(3) -0.57948(17) 0.0711(9) Uani 1 1 d . . . H35 H -0.3774 -0.1280 -0.5802 0.085 Uiso 1 1 calc R . . N1 N 0.0681(3) -0.12664(16) -0.33620(13) 0.0635(7) Uani 1 1 d . . . N2 N 0.2760(2) 0.09949(15) -0.13997(12) 0.0529(6) Uani 1 1 d . . . N3 N 0.3607(3) 0.14627(16) -0.04301(13) 0.0579(6) Uani 1 1 d . . . N4 N 0.3315(3) -0.43383(16) -0.34649(13) 0.0585(6) Uani 1 1 d . . . N5 N 0.3956(3) -0.55142(15) -0.38839(14) 0.0583(6) Uani 1 1 d . . . N6 N -0.3203(3) -0.01906(18) -0.53550(14) 0.0643(7) Uani 1 1 d . . . N7 N -0.4736(3) -0.0302(2) -0.62087(17) 0.0815(9) Uani 1 1 d . . . O1 O 1.1280(2) 0.1299(2) 0.0345(2) 0.1222(15) Uani 1 1 d . . . O2 O 1.24963(18) 0.22412(13) 0.08915(11) 0.0557(5) Uani 1 1 d . . . O3 O 0.54640(18) 0.22489(13) 0.08676(11) 0.0577(5) Uani 1 1 d . . . O4 O 0.64813(19) 0.12443(14) 0.03747(12) 0.0651(6) Uani 1 1 d . . . O1W O 0.5968(7) -0.2614(5) -0.2081(3) 0.128(3) Uani 0.50 1 d P . . O2W O 0.0248(9) 0.0006(5) -0.0284(4) 0.125(3) 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 0.0433(2) 0.0478(2) 0.0561(2) -0.00663(16) 0.00080(16) -0.00671(14) C1 0.0406(14) 0.0485(15) 0.0498(14) -0.0025(11) 0.0016(11) -0.0064(11) C2 0.0360(13) 0.0460(14) 0.0569(15) 0.0008(12) 0.0031(11) -0.0043(10) C3 0.0442(14) 0.0507(15) 0.0603(16) -0.0038(13) -0.0007(12) -0.0099(12) C4 0.0595(17) 0.0555(16) 0.0668(19) -0.0159(15) 0.0059(14) -0.0130(14) C5 0.0451(14) 0.0499(15) 0.0744(19) -0.0107(14) 0.0118(13) -0.0039(12) C6 0.0394(13) 0.0435(13) 0.0543(15) -0.0017(11) 0.0035(11) -0.0060(10) C7 0.0380(14) 0.0474(15) 0.0616(16) 0.0000(13) 0.0048(12) -0.0045(11) C8 0.0372(14) 0.0597(17) 0.083(2) -0.0127(16) 0.0049(13) -0.0057(12) C9 0.0623(17) 0.0470(15) 0.0526(16) -0.0065(12) 0.0007(13) 0.0058(13) C10 0.0635(18) 0.0518(17) 0.076(2) -0.0139(15) -0.0049(16) 0.0001(14) C11 0.0527(17) 0.0604(18) 0.080(2) -0.0109(16) -0.0055(15) 0.0018(14) C12 0.0607(18) 0.0493(15) 0.0629(18) -0.0068(13) -0.0008(14) 0.0048(13) C13 0.0618(18) 0.0481(16) 0.074(2) -0.0127(14) -0.0049(15) 0.0017(13) C14 0.0555(17) 0.0591(18) 0.0709(19) -0.0109(15) -0.0098(15) 0.0069(14) C15 0.072(2) 0.0534(17) 0.0584(17) 0.0004(14) 0.0020(15) 0.0172(15) C16 0.071(2) 0.066(2) 0.085(2) -0.0062(18) -0.0239(19) 0.0186(17) C17 0.082(2) 0.070(2) 0.088(3) -0.0167(19) -0.029(2) 0.0176(19) C18 0.0687(18) 0.0458(15) 0.0481(15) -0.0086(12) -0.0056(13) 0.0096(13) C19 0.104(3) 0.0504(17) 0.0562(18) -0.0019(14) 0.0046(17) -0.0142(17) C20 0.096(2) 0.0590(18) 0.0467(16) -0.0040(14) 0.0062(16) -0.0145(17) C21 0.0557(16) 0.0453(14) 0.0496(15) -0.0047(11) -0.0007(12) 0.0041(12) C22 0.0595(17) 0.0546(16) 0.0499(15) 0.0047(13) -0.0002(13) -0.0012(13) C23 0.0661(18) 0.0607(17) 0.0446(15) 0.0004(13) -0.0003(13) 0.0042(14) C24 0.129(3) 0.0570(19) 0.0569(19) 0.0033(16) 0.003(2) -0.026(2) C25 0.114(3) 0.067(2) 0.068(2) -0.0075(17) 0.009(2) -0.037(2) C26 0.078(2) 0.0504(16) 0.0520(16) -0.0054(13) -0.0081(15) 0.0021(15) C27 0.0631(17) 0.0502(16) 0.0544(16) -0.0078(13) -0.0013(13) 0.0051(13) C28 0.0673(19) 0.073(2) 0.0577(17) -0.0201(15) 0.0004(15) 0.0120(16) C29 0.0602(18) 0.072(2) 0.072(2) -0.0147(17) 0.0049(16) 0.0141(16) C30 0.0605(17) 0.0568(17) 0.0591(17) -0.0007(14) 0.0022(14) 0.0068(14) C31 0.077(2) 0.070(2) 0.0489(16) -0.0047(14) 0.0026(15) 0.0175(17) C32 0.073(2) 0.0649(18) 0.0551(17) -0.0075(14) 0.0037(15) 0.0192(16) C33 0.072(2) 0.069(2) 0.092(3) 0.0019(19) 0.006(2) 0.0148(18) C34 0.066(2) 0.100(3) 0.099(3) 0.024(3) 0.000(2) 0.022(2) C35 0.072(2) 0.080(2) 0.0605(18) 0.0002(17) 0.0018(16) 0.0018(18) N1 0.0804(18) 0.0503(13) 0.0563(14) -0.0124(11) -0.0112(13) 0.0114(13) N2 0.0577(14) 0.0497(13) 0.0506(13) -0.0068(10) 0.0026(10) -0.0028(11) N3 0.0537(14) 0.0599(15) 0.0594(14) -0.0079(12) 0.0016(11) -0.0016(11) N4 0.0579(14) 0.0494(13) 0.0665(15) -0.0046(11) -0.0031(12) 0.0087(11) N5 0.0553(14) 0.0491(13) 0.0698(16) 0.0013(12) 0.0026(12) 0.0095(11) N6 0.0603(15) 0.0697(17) 0.0621(15) 0.0016(13) 0.0021(12) 0.0050(13) N7 0.0656(18) 0.101(3) 0.0761(19) 0.0053(18) -0.0031(15) 0.0092(17) O1 0.0463(13) 0.119(2) 0.205(4) -0.102(3) 0.0294(17) -0.0222(14) O2 0.0363(9) 0.0614(12) 0.0684(12) -0.0067(10) 0.0003(8) -0.0053(8) O3 0.0376(10) 0.0545(11) 0.0814(14) -0.0137(10) 0.0082(9) -0.0030(8) O4 0.0438(11) 0.0618(12) 0.0888(16) -0.0237(12) 0.0023(10) -0.0069(9) O1W 0.120(5) 0.182(7) 0.073(3) -0.071(4) -0.044(3) 0.089(5) O2W 0.170(8) 0.089(4) 0.119(5) -0.030(4) 0.024(5) -0.043(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.9650(19) . ? Zn1 N3 1.987(3) . ? Zn1 N5 2.006(3) 4_556 ? Zn1 O2 2.018(2) 1_455 ? C1 C6 1.378(4) . ? C1 C2 1.392(4) . ? C1 H1 0.9300 . ? C2 C3 1.385(4) . ? C2 C8 1.497(4) . ? C3 C4 1.375(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 C6 1.397(4) . ? C5 H5 0.9300 . ? C6 C7 1.505(4) . ? C7 O4 1.233(4) . ? C7 O3 1.272(3) . ? C8 O1 1.223(4) . ? C8 O2 1.271(3) . ? C9 C14 1.379(4) . ? C9 C10 1.391(5) . ? C9 N1 1.415(4) . ? C10 C11 1.377(5) . ? C10 H10 0.9300 . ? C11 C12 1.375(4) . ? C11 H9 0.9300 . ? C12 C13 1.373(5) . ? C12 N4 1.437(4) . ? C13 C14 1.380(4) . ? C13 H13 0.9300 . ? C14 H12 0.9300 . ? C15 N5 1.313(4) . ? C15 N4 1.342(4) . ? C15 H16 0.9300 . ? C16 C17 1.349(5) . ? C16 N5 1.354(5) . ? C16 H17 0.9300 . ? C17 N4 1.367(4) . ? C17 H15 0.9300 . ? C18 C19 1.379(5) . ? C18 C23 1.380(5) . ? C18 N1 1.433(4) . ? C19 C20 1.384(5) . ? C19 H19 0.9300 . ? C20 C21 1.372(5) . ? C20 H20 0.9300 . ? C21 C22 1.374(4) . ? C21 N2 1.439(4) . ? C22 C23 1.386(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.329(5) . ? C24 N2 1.381(5) . ? C24 H26 0.9300 . ? C25 N3 1.374(5) . ? C25 H25 0.9300 . ? C26 N3 1.314(4) . ? C26 N2 1.327(4) . ? C26 H24 0.9300 . ? C27 C28 1.383(5) . ? C27 C32 1.392(4) . ? C27 N1 1.404(4) . ? C28 C29 1.378(5) . ? C28 H28 0.9300 . ? C29 C30 1.383(5) . ? C29 H29 0.9300 . ? C30 C31 1.371(5) . ? C30 N6 1.437(4) . ? C31 C32 1.384(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.349(6) . ? C33 N6 1.345(5) . ? C33 H33 0.9300 . ? C34 N7 1.367(6) . ? C34 H34 0.9300 . ? C35 N7 1.310(5) . ? C35 N6 1.355(5) . ? C35 H35 0.9300 . ? N5 Zn1 2.006(3) 4 ? O2 Zn1 2.018(2) 1_655 ? O2W O2W 1.295(15) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 N3 114.41(10) . . ? O3 Zn1 N5 109.43(10) . 4_556 ? N3 Zn1 N5 119.85(11) . 4_556 ? O3 Zn1 O2 98.85(8) . 1_455 ? N3 Zn1 O2 108.21(10) . 1_455 ? N5 Zn1 O2 103.32(10) 4_556 1_455 ? C6 C1 C2 121.0(3) . . ? C6 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C8 121.8(2) . . ? C1 C2 C8 119.3(2) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 119.5(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 119.4(2) . . ? C1 C6 C7 119.0(2) . . ? C5 C6 C7 121.4(2) . . ? O4 C7 O3 123.3(2) . . ? O4 C7 C6 119.7(2) . . ? O3 C7 C6 117.0(2) . . ? O1 C8 O2 122.1(3) . . ? O1 C8 C2 119.5(3) . . ? O2 C8 C2 118.4(3) . . ? C14 C9 C10 118.3(3) . . ? C14 C9 N1 121.3(3) . . ? C10 C9 N1 120.4(3) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.9(3) . . ? C10 C11 H9 120.1 . . ? C12 C11 H9 120.1 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 N4 119.9(3) . . ? C11 C12 N4 119.9(3) . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 121.1(3) . . ? C9 C14 H12 119.4 . . ? C13 C14 H12 119.4 . . ? N5 C15 N4 111.3(3) . . ? N5 C15 H16 124.4 . . ? N4 C15 H16 124.4 . . ? C17 C16 N5 110.1(3) . . ? C17 C16 H17 125.0 . . ? N5 C16 H17 125.0 . . ? C16 C17 N4 106.0(3) . . ? C16 C17 H15 127.0 . . ? N4 C17 H15 127.0 . . ? C19 C18 C23 119.5(3) . . ? C19 C18 N1 120.3(3) . . ? C23 C18 N1 120.1(3) . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.7(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 121.0(3) . . ? C22 C21 N2 119.5(3) . . ? C20 C21 N2 119.5(3) . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C18 C23 C22 120.7(3) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 N2 106.3(3) . . ? C25 C24 H26 126.8 . . ? N2 C24 H26 126.8 . . ? C24 C25 N3 110.1(3) . . ? C24 C25 H25 125.0 . . ? N3 C25 H25 125.0 . . ? N3 C26 N2 112.0(3) . . ? N3 C26 H24 124.0 . . ? N2 C26 H24 124.0 . . ? C28 C27 C32 118.5(3) . . ? C28 C27 N1 119.4(3) . . ? C32 C27 N1 122.1(3) . . ? C29 C28 C27 121.0(3) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 119.4(3) . . ? C31 C30 N6 119.6(3) . . ? C29 C30 N6 121.0(3) . . ? C30 C31 C32 120.7(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 120.2(3) . . ? C31 C32 H32 119.9 . . ? C27 C32 H32 119.9 . . ? C34 C33 N6 105.6(4) . . ? C34 C33 H33 127.2 . . ? N6 C33 H33 127.2 . . ? C33 C34 N7 111.6(4) . . ? C33 C34 H34 124.2 . . ? N7 C34 H34 124.2 . . ? N7 C35 N6 112.4(4) . . ? N7 C35 H35 123.8 . . ? N6 C35 H35 123.8 . . ? C27 N1 C9 122.9(2) . . ? C27 N1 C18 118.1(2) . . ? C9 N1 C18 118.0(2) . . ? C26 N2 C24 106.5(3) . . ? C26 N2 C21 126.4(3) . . ? C24 N2 C21 127.0(3) . . ? C26 N3 C25 105.0(3) . . ? C26 N3 Zn1 126.5(2) . . ? C25 N3 Zn1 126.5(2) . . ? C15 N4 C17 106.8(3) . . ? C15 N4 C12 125.1(3) . . ? C17 N4 C12 128.1(3) . . ? C15 N5 C16 105.8(3) . . ? C15 N5 Zn1 127.4(2) . 4 ? C16 N5 Zn1 125.9(2) . 4 ? C33 N6 C35 106.9(3) . . ? C33 N6 C30 127.3(3) . . ? C35 N6 C30 125.7(3) . . ? C35 N7 C34 103.5(3) . . ? C8 O2 Zn1 109.35(19) . 1_655 ? C7 O3 Zn1 107.80(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.1(4) . . . . ? C6 C1 C2 C8 177.4(3) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C8 C2 C3 C4 -177.8(3) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C2 C1 C6 C5 0.9(4) . . . . ? C2 C1 C6 C7 -173.7(3) . . . . ? C4 C5 C6 C1 -1.2(4) . . . . ? C4 C5 C6 C7 173.2(3) . . . . ? C1 C6 C7 O4 9.5(4) . . . . ? C5 C6 C7 O4 -165.0(3) . . . . ? C1 C6 C7 O3 -172.7(3) . . . . ? C5 C6 C7 O3 12.8(4) . . . . ? C3 C2 C8 O1 169.9(4) . . . . ? C1 C2 C8 O1 -7.5(5) . . . . ? C3 C2 C8 O2 -9.9(5) . . . . ? C1 C2 C8 O2 172.7(3) . . . . ? C14 C9 C10 C11 0.3(5) . . . . ? N1 C9 C10 C11 -179.9(3) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? C10 C11 C12 C13 -0.7(6) . . . . ? C10 C11 C12 N4 178.2(3) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? N4 C12 C13 C14 -178.3(3) . . . . ? C10 C9 C14 C13 -0.4(5) . . . . ? N1 C9 C14 C13 179.8(3) . . . . ? C12 C13 C14 C9 -0.1(6) . . . . ? N5 C16 C17 N4 -0.2(5) . . . . ? C23 C18 C19 C20 0.2(6) . . . . ? N1 C18 C19 C20 178.4(3) . . . . ? C18 C19 C20 C21 -1.4(6) . . . . ? C19 C20 C21 C22 1.4(5) . . . . ? C19 C20 C21 N2 -177.9(3) . . . . ? C20 C21 C22 C23 -0.3(5) . . . . ? N2 C21 C22 C23 179.0(3) . . . . ? C19 C18 C23 C22 1.0(5) . . . . ? N1 C18 C23 C22 -177.2(3) . . . . ? C21 C22 C23 C18 -0.9(5) . . . . ? N2 C24 C25 N3 -0.6(5) . . . . ? C32 C27 C28 C29 2.7(5) . . . . ? N1 C27 C28 C29 -179.2(3) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C28 C29 C30 C31 -2.0(6) . . . . ? C28 C29 C30 N6 177.2(3) . . . . ? C29 C30 C31 C32 1.8(6) . . . . ? N6 C30 C31 C32 -177.4(3) . . . . ? C30 C31 C32 C27 0.6(6) . . . . ? C28 C27 C32 C31 -2.9(6) . . . . ? N1 C27 C32 C31 179.1(3) . . . . ? N6 C33 C34 N7 0.3(5) . . . . ? C28 C27 N1 C9 153.6(3) . . . . ? C32 C27 N1 C9 -28.3(5) . . . . ? C28 C27 N1 C18 -37.6(5) . . . . ? C32 C27 N1 C18 140.4(3) . . . . ? C14 C9 N1 C27 -35.4(5) . . . . ? C10 C9 N1 C27 144.9(3) . . . . ? C14 C9 N1 C18 155.9(3) . . . . ? C10 C9 N1 C18 -23.9(5) . . . . ? C19 C18 N1 C27 121.3(4) . . . . ? C23 C18 N1 C27 -60.5(4) . . . . ? C19 C18 N1 C9 -69.4(4) . . . . ? C23 C18 N1 C9 108.7(3) . . . . ? N3 C26 N2 C24 -1.5(4) . . . . ? N3 C26 N2 C21 -178.8(3) . . . . ? C25 C24 N2 C26 1.2(5) . . . . ? C25 C24 N2 C21 178.6(3) . . . . ? C22 C21 N2 C26 -152.3(3) . . . . ? C20 C21 N2 C26 27.0(5) . . . . ? C22 C21 N2 C24 30.8(5) . . . . ? C20 C21 N2 C24 -149.9(4) . . . . ? N2 C26 N3 C25 1.1(4) . . . . ? N2 C26 N3 Zn1 165.8(2) . . . . ? C24 C25 N3 C26 -0.2(5) . . . . ? C24 C25 N3 Zn1 -165.0(3) . . . . ? O3 Zn1 N3 C26 145.3(3) . . . . ? N5 Zn1 N3 C26 12.3(3) 4_556 . . . ? O2 Zn1 N3 C26 -105.7(3) 1_455 . . . ? O3 Zn1 N3 C25 -53.1(3) . . . . ? N5 Zn1 N3 C25 173.9(3) 4_556 . . . ? O2 Zn1 N3 C25 56.0(3) 1_455 . . . ? N5 C15 N4 C17 0.8(4) . . . . ? N5 C15 N4 C12 -179.4(3) . . . . ? C16 C17 N4 C15 -0.4(5) . . . . ? C16 C17 N4 C12 179.9(3) . . . . ? C13 C12 N4 C15 42.5(5) . . . . ? C11 C12 N4 C15 -136.5(4) . . . . ? C13 C12 N4 C17 -137.8(4) . . . . ? C11 C12 N4 C17 43.2(5) . . . . ? N4 C15 N5 C16 -1.0(4) . . . . ? N4 C15 N5 Zn1 168.7(2) . . . 4 ? C17 C16 N5 C15 0.7(5) . . . . ? C17 C16 N5 Zn1 -169.1(3) . . . 4 ? C34 C33 N6 C35 -0.2(4) . . . . ? C34 C33 N6 C30 178.3(3) . . . . ? N7 C35 N6 C33 0.2(4) . . . . ? N7 C35 N6 C30 -178.4(3) . . . . ? C31 C30 N6 C33 -131.5(4) . . . . ? C29 C30 N6 C33 49.3(5) . . . . ? C31 C30 N6 C35 46.8(5) . . . . ? C29 C30 N6 C35 -132.4(4) . . . . ? N6 C35 N7 C34 0.0(4) . . . . ? C33 C34 N7 C35 -0.2(5) . . . . ? O1 C8 O2 Zn1 -5.0(5) . . . 1_655 ? C2 C8 O2 Zn1 174.8(2) . . . 1_655 ? O4 C7 O3 Zn1 2.4(4) . . . . ? C6 C7 O3 Zn1 -175.3(2) . . . . ? N3 Zn1 O3 C7 -65.7(2) . . . . ? N5 Zn1 O3 C7 72.0(2) 4_556 . . . ? O2 Zn1 O3 C7 179.63(19) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 67.21 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.910 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.067 data_2 _database_code_depnum_ccdc_archive 'CCDC 826243' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 N7 O7 Zn2, 2(H2 O)' _chemical_formula_sum 'C36 H28 N7 O9 S0 Zn2' _chemical_formula_weight 833.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.4447(10) _cell_length_b 16.3875(6) _cell_length_c 10.3920(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3652.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5382 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 26.4 _exptl_crystal_description BLOCK _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14049 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.1198 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5382 _reflns_number_gt 3214 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 5382 _refine_ls_number_parameters 496 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _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 0.57626(4) 1.00579(5) 0.47324(11) 0.0362(2) Uani 1 1 d . . . Zn2 Zn 0.72040(4) 1.03924(5) 1.31734(9) 0.0354(2) Uani 1 1 d . . . C1 C 0.6792(3) 0.8862(4) 0.7519(7) 0.0312(17) Uani 1 1 d . . . C2 C 0.7017(4) 0.8070(4) 0.7656(8) 0.0352(19) Uani 1 1 d . . . H2 H 0.6962 0.7695 0.6994 0.042 Uiso 1 1 calc R . . C3 C 0.7315(4) 0.7838(4) 0.8751(8) 0.035(2) Uani 1 1 d . . . C4 C 0.7381(3) 0.8383(4) 0.9748(9) 0.0373(18) Uani 1 1 d . . . H4 H 0.7591 0.8223 1.0489 0.045 Uiso 1 1 calc R . . C5 C 0.7136(3) 0.9183(4) 0.9668(8) 0.0339(17) Uani 1 1 d . . . C6 C 0.6856(3) 0.9400(4) 0.8537(7) 0.0295(19) Uani 1 1 d . . . H6 H 0.6702 0.9927 0.8449 0.035 Uiso 1 1 calc R . . C7 C 0.6434(4) 0.9097(5) 0.6320(8) 0.042(2) Uani 1 1 d . . . C8 C 0.7588(4) 0.6984(5) 0.8891(9) 0.038(2) Uani 1 1 d . . . C9 C 0.7151(4) 0.9781(5) 1.0752(8) 0.041(2) Uani 1 1 d . . . C10 C 0.4346(4) 0.5767(4) 0.1999(8) 0.037(2) Uani 1 1 d . . . C11 C 0.4952(4) 0.5999(4) 0.2423(9) 0.044(2) Uani 1 1 d . . . H11 H 0.5282 0.5633 0.2363 0.053 Uiso 1 1 calc R . . C12 C 0.5047(3) 0.6764(4) 0.2920(8) 0.037(2) Uani 1 1 d . . . H12 H 0.5442 0.6912 0.3211 0.045 Uiso 1 1 calc R . . C13 C 0.4570(3) 0.7311(4) 0.2992(10) 0.040(2) Uani 1 1 d . . . C14 C 0.3985(4) 0.7095(5) 0.2583(10) 0.058(3) Uani 1 1 d . . . H14 H 0.3659 0.7468 0.2640 0.069 Uiso 1 1 calc R . . C15 C 0.3877(4) 0.6324(5) 0.2083(10) 0.057(3) Uani 1 1 d . . . H15 H 0.3480 0.6185 0.1801 0.068 Uiso 1 1 calc R . . C16 C 0.5159(4) 0.8447(4) 0.4008(9) 0.040(2) Uani 1 1 d . . . H16 H 0.5500 0.8139 0.4270 0.048 Uiso 1 1 calc R . . C17 C 0.4568(5) 0.9446(5) 0.3597(12) 0.082(4) Uani 1 1 d . . . H17 H 0.4421 0.9978 0.3521 0.098 Uiso 1 1 calc R . . C18 C 0.4272(4) 0.8772(5) 0.3142(13) 0.074(3) Uani 1 1 d . . . H18 H 0.3887 0.8748 0.2735 0.089 Uiso 1 1 calc R . . C19 C 0.4316(4) 0.4275(4) 0.2078(8) 0.036(2) Uani 1 1 d . . . C20 C 0.4582(4) 0.3589(4) 0.1487(8) 0.050(2) Uani 1 1 d . . . H20 H 0.4685 0.3602 0.0618 0.060 Uiso 1 1 calc R . . C21 C 0.4688(4) 0.2898(5) 0.2198(10) 0.056(3) Uani 1 1 d . . . H21 H 0.4862 0.2441 0.1807 0.067 Uiso 1 1 calc R . . C22 C 0.4541(4) 0.2875(4) 0.3476(9) 0.041(2) Uani 1 1 d . . . C23 C 0.4280(4) 0.3524(4) 0.4079(9) 0.045(2) Uani 1 1 d . . . H23 H 0.4179 0.3502 0.4949 0.053 Uiso 1 1 calc R . . C24 C 0.4168(4) 0.4237(4) 0.3341(9) 0.042(2) Uani 1 1 d . . . H24 H 0.3988 0.4689 0.3735 0.050 Uiso 1 1 calc R . . C25 C 0.5196(4) 0.1668(4) 0.4066(9) 0.044(2) Uani 1 1 d . . . H25 H 0.5503 0.1751 0.3448 0.053 Uiso 1 1 calc R . . C26 C 0.4658(4) 0.1158(5) 0.5618(9) 0.047(2) Uani 1 1 d . . . H26 H 0.4529 0.0813 0.6275 0.056 Uiso 1 1 calc R . . C27 C 0.4348(4) 0.1837(5) 0.5216(9) 0.049(2) Uani 1 1 d . . . H27 H 0.3977 0.2042 0.5549 0.059 Uiso 1 1 calc R . . C28 C 0.3484(3) 0.5229(4) -0.2337(8) 0.035(2) Uani 1 1 d . . . C29 C 0.3910(3) 0.5790(4) -0.1877(10) 0.0410(18) Uani 1 1 d . . . H29 H 0.4023 0.6237 -0.2377 0.049 Uiso 1 1 calc R . . C30 C 0.4166(4) 0.5687(5) -0.0687(8) 0.045(2) Uani 1 1 d . . . H30 H 0.4461 0.6060 -0.0397 0.054 Uiso 1 1 calc R . . C31 C 0.4003(3) 0.5050(4) 0.0089(7) 0.0321(19) Uani 1 1 d . . . C32 C 0.3588(4) 0.4474(4) -0.0392(9) 0.043(2) Uani 1 1 d . . . H32 H 0.3489 0.4013 0.0090 0.051 Uiso 1 1 calc R . . C33 C 0.3326(4) 0.4589(4) -0.1573(8) 0.043(2) Uani 1 1 d . . . H33 H 0.3030 0.4218 -0.1865 0.051 Uiso 1 1 calc R . . C34 C 0.2885(4) 0.4820(5) -0.4271(8) 0.038(2) Uani 1 1 d . . . H34 H 0.2810 0.4286 -0.4009 0.045 Uiso 1 1 calc R . . C35 C 0.2887(4) 0.5926(5) -0.5349(10) 0.052(2) Uani 1 1 d . . . H35 H 0.2816 0.6307 -0.5996 0.062 Uiso 1 1 calc R . . C36 C 0.3205(5) 0.6072(5) -0.4267(9) 0.059(3) Uani 1 1 d . . . H36 H 0.3387 0.6563 -0.4023 0.071 Uiso 1 1 calc R . . O1 O 0.6207(3) 0.9809(3) 0.6304(6) 0.0501(16) Uani 1 1 d . . . O2 O 0.6386(3) 0.8610(3) 0.5416(6) 0.0544(16) Uani 1 1 d . . . O3 O 0.7522(3) 0.6526(3) 0.7927(6) 0.0537(16) Uani 1 1 d . . . O4 O 0.7822(3) 0.6779(3) 0.9892(7) 0.0692(18) Uani 1 1 d . . . O5 O 0.7412(3) 0.9551(3) 1.1812(6) 0.0492(16) Uani 1 1 d . . . O6 O 0.6915(4) 1.0442(4) 1.0634(6) 0.077(2) Uani 1 1 d . . . O7 O 0.6300(2) 1.0307(3) 1.3331(7) 0.0525(15) Uani 1 1 d . . . N1 N 0.4242(3) 0.5014(4) 0.1367(7) 0.0411(16) Uani 1 1 d . . . N2 N 0.4667(3) 0.8136(3) 0.3412(7) 0.0437(19) Uani 1 1 d . . . N3 N 0.5114(3) 0.9228(3) 0.4186(7) 0.0410(18) Uani 1 1 d . . . N4 N 0.4686(3) 0.2153(3) 0.4233(7) 0.0420(18) Uani 1 1 d . . . N5 N 0.5192(3) 0.1062(3) 0.4906(8) 0.0406(17) Uani 1 1 d . . . N6 N 0.3209(3) 0.5361(4) -0.3594(6) 0.0350(15) Uani 1 1 d . . . N7 N 0.2681(2) 0.5139(4) -0.5368(8) 0.0372(15) Uani 1 1 d . . . O1W O 0.6680(5) 0.8076(8) 0.2900(12) 0.168(5) Uani 1 1 d . . . O2W O 0.3805(6) 0.8058(6) -0.3435(13) 0.064(4) Uani 0.50 1 d P . . O3W O 0.2640(6) 0.8047(7) 0.2428(15) 0.083(5) 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 0.0432(5) 0.0283(4) 0.0371(5) 0.0010(5) -0.0080(6) 0.0017(4) Zn2 0.0431(5) 0.0299(4) 0.0333(5) -0.0042(4) -0.0047(6) -0.0045(4) C1 0.038(5) 0.026(4) 0.030(4) -0.003(3) -0.007(4) 0.002(3) C2 0.047(5) 0.034(4) 0.025(4) -0.007(3) 0.004(4) -0.004(4) C3 0.042(5) 0.029(4) 0.036(5) -0.004(4) -0.002(4) -0.006(3) C4 0.038(4) 0.041(4) 0.033(4) -0.002(4) -0.008(5) 0.009(3) C5 0.037(4) 0.033(4) 0.032(4) -0.008(4) -0.003(5) 0.000(3) C6 0.030(4) 0.028(4) 0.031(5) -0.001(3) 0.002(4) 0.009(3) C7 0.046(6) 0.041(5) 0.039(6) -0.003(4) 0.004(4) 0.003(4) C8 0.048(6) 0.032(4) 0.033(5) -0.001(4) -0.006(4) 0.012(4) C9 0.037(5) 0.043(5) 0.043(5) -0.007(4) -0.007(4) 0.006(4) C10 0.048(6) 0.027(4) 0.037(5) 0.002(4) -0.014(4) -0.001(4) C11 0.047(5) 0.035(4) 0.051(6) 0.007(4) -0.021(5) 0.015(4) C12 0.035(5) 0.028(4) 0.049(6) 0.004(4) -0.025(4) 0.001(3) C13 0.046(5) 0.029(4) 0.044(6) 0.004(4) 0.002(5) -0.011(3) C14 0.024(5) 0.052(5) 0.098(8) -0.018(5) -0.003(5) -0.004(4) C15 0.033(5) 0.037(5) 0.100(8) -0.020(5) -0.026(5) 0.001(4) C16 0.036(5) 0.039(4) 0.046(5) -0.007(4) -0.012(4) -0.004(4) C17 0.068(7) 0.048(6) 0.129(12) -0.012(6) -0.037(7) 0.015(5) C18 0.051(6) 0.050(5) 0.121(9) -0.025(7) -0.026(8) 0.013(4) C19 0.038(5) 0.029(4) 0.042(6) 0.001(4) -0.026(4) 0.001(4) C20 0.087(8) 0.035(5) 0.028(5) -0.002(4) -0.014(5) 0.014(4) C21 0.075(7) 0.043(5) 0.050(7) -0.009(5) -0.018(6) 0.021(5) C22 0.034(5) 0.028(4) 0.060(8) 0.007(4) -0.011(4) 0.008(3) C23 0.044(5) 0.040(5) 0.050(5) 0.009(4) 0.004(5) 0.007(4) C24 0.050(5) 0.030(4) 0.045(6) -0.001(4) -0.004(5) 0.003(3) C25 0.048(6) 0.035(4) 0.049(6) 0.006(4) 0.014(5) 0.012(4) C26 0.053(6) 0.035(5) 0.052(6) 0.006(4) 0.019(5) 0.013(4) C27 0.056(6) 0.038(5) 0.053(6) -0.002(4) 0.015(5) 0.008(4) C28 0.033(5) 0.030(4) 0.042(5) -0.004(3) -0.005(4) 0.006(3) C29 0.041(5) 0.043(4) 0.039(5) 0.015(5) -0.003(5) -0.005(3) C30 0.032(5) 0.054(5) 0.049(6) 0.004(4) -0.009(4) 0.000(4) C31 0.033(4) 0.032(4) 0.032(5) -0.001(4) -0.016(3) 0.009(4) C32 0.056(5) 0.033(4) 0.038(5) 0.010(4) -0.014(5) -0.008(4) C33 0.045(5) 0.039(4) 0.043(6) 0.001(4) -0.018(4) -0.006(4) C34 0.044(5) 0.035(5) 0.033(5) 0.000(4) -0.010(4) 0.001(4) C35 0.065(6) 0.042(5) 0.048(6) 0.007(5) -0.019(6) -0.010(4) C36 0.084(7) 0.043(5) 0.049(6) 0.014(5) -0.022(6) -0.010(5) O1 0.061(4) 0.045(3) 0.044(4) -0.001(3) -0.014(3) 0.015(3) O2 0.063(4) 0.059(4) 0.042(4) -0.008(3) -0.016(3) 0.006(3) O3 0.078(4) 0.033(3) 0.050(4) -0.004(3) 0.006(3) 0.019(3) O4 0.098(5) 0.040(3) 0.070(5) -0.003(3) -0.020(5) 0.025(3) O5 0.057(4) 0.058(4) 0.033(3) -0.017(3) -0.013(3) 0.020(3) O6 0.131(6) 0.042(4) 0.057(4) -0.018(3) -0.019(4) 0.032(4) O7 0.039(3) 0.069(3) 0.050(4) 0.005(3) -0.002(3) -0.004(3) N1 0.053(4) 0.027(3) 0.043(4) 0.003(3) -0.023(3) -0.002(3) N2 0.039(4) 0.032(3) 0.061(6) -0.005(3) -0.007(4) -0.004(3) N3 0.042(4) 0.025(3) 0.056(5) -0.006(3) -0.010(4) 0.002(3) N4 0.051(4) 0.022(3) 0.053(5) 0.002(3) -0.009(4) -0.004(3) N5 0.048(4) 0.025(3) 0.049(5) -0.005(3) -0.017(4) 0.002(3) N6 0.035(4) 0.039(3) 0.031(4) 0.006(3) -0.008(3) 0.007(3) N7 0.036(3) 0.041(4) 0.035(4) 0.007(4) -0.009(4) 0.001(3) O1W 0.125(8) 0.261(12) 0.119(10) -0.061(9) -0.005(7) -0.033(7) O2W 0.069(9) 0.048(7) 0.075(10) -0.024(7) -0.019(7) 0.033(6) O3W 0.085(10) 0.049(7) 0.114(13) -0.010(8) -0.008(9) 0.056(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O7 1.901(6) 1_554 ? Zn1 O1 1.934(6) . ? Zn1 N3 2.027(6) . ? Zn1 N5 2.059(6) 1_565 ? Zn2 O7 1.951(5) . ? Zn2 O3 1.965(5) 3_655 ? Zn2 N7 2.025(7) 4_567 ? Zn2 O5 2.026(5) . ? C1 C6 1.383(9) . ? C1 C2 1.393(10) . ? C1 C7 1.513(11) . ? C2 C3 1.359(10) . ? C2 H2 0.9300 . ? C3 C4 1.375(11) . ? C3 C8 1.525(10) . ? C4 C5 1.414(9) . ? C4 H4 0.9300 . ? C5 C6 1.368(10) . ? C5 C9 1.494(11) . ? C6 H6 0.9300 . ? C7 O2 1.236(9) . ? C7 O1 1.265(9) . ? C8 O4 1.202(10) . ? C8 O3 1.260(9) . ? C9 O6 1.201(9) . ? C9 O5 1.292(10) . ? C10 C15 1.361(11) . ? C10 N1 1.415(9) . ? C10 C11 1.422(11) . ? C11 C12 1.373(9) . ? C11 H11 0.9300 . ? C12 C13 1.362(9) . ? C12 H12 0.9300 . ? C13 C14 1.370(10) . ? C13 N2 1.436(9) . ? C14 C15 1.386(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N3 1.297(8) . ? C16 N2 1.326(9) . ? C16 H16 0.9300 . ? C17 C18 1.358(12) . ? C17 N3 1.368(11) . ? C17 H17 0.9300 . ? C18 N2 1.372(10) . ? C18 H18 0.9300 . ? C19 C24 1.351(12) . ? C19 C20 1.402(11) . ? C19 N1 1.427(9) . ? C20 C21 1.371(11) . ? C20 H20 0.9300 . ? C21 C22 1.365(13) . ? C21 H21 0.9300 . ? C22 C23 1.356(11) . ? C22 N4 1.453(10) . ? C23 C24 1.420(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N5 1.322(10) . ? C25 N4 1.363(9) . ? C25 H25 0.9300 . ? C26 C27 1.362(11) . ? C26 N5 1.372(11) . ? C26 H26 0.9300 . ? C27 N4 1.356(10) . ? C27 H27 0.9300 . ? C28 C33 1.359(11) . ? C28 C29 1.382(10) . ? C28 N6 1.450(9) . ? C29 C30 1.363(11) . ? C29 H29 0.9300 . ? C30 C31 1.364(10) . ? C30 H30 0.9300 . ? C31 C32 1.390(10) . ? C31 N1 1.425(9) . ? C32 C33 1.362(11) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N6 1.327(9) . ? C34 N7 1.328(10) . ? C34 H34 0.9300 . ? C35 C36 1.336(12) . ? C35 N7 1.364(9) . ? C35 H35 0.9300 . ? C36 N6 1.359(10) . ? C36 H36 0.9300 . ? O3 Zn2 1.965(5) 3_644 ? O7 Zn1 1.901(6) 1_556 ? N5 Zn1 2.059(6) 1_545 ? N7 Zn2 2.025(7) 4_463 ? 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 O7 Zn1 O1 113.2(2) 1_554 . ? O7 Zn1 N3 110.2(3) 1_554 . ? O1 Zn1 N3 115.7(3) . . ? O7 Zn1 N5 104.8(3) 1_554 1_565 ? O1 Zn1 N5 112.8(3) . 1_565 ? N3 Zn1 N5 98.8(2) . 1_565 ? O7 Zn2 O3 112.1(2) . 3_655 ? O7 Zn2 N7 114.1(3) . 4_567 ? O3 Zn2 N7 110.6(2) 3_655 4_567 ? O7 Zn2 O5 103.2(3) . . ? O3 Zn2 O5 119.1(3) 3_655 . ? N7 Zn2 O5 96.8(2) 4_567 . ? C6 C1 C2 118.8(7) . . ? C6 C1 C7 121.2(6) . . ? C2 C1 C7 119.8(7) . . ? C3 C2 C1 120.6(7) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 119.9(7) . . ? C2 C3 C8 121.1(7) . . ? C4 C3 C8 119.0(8) . . ? C3 C4 C5 121.3(8) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 117.1(7) . . ? C6 C5 C9 119.1(6) . . ? C4 C5 C9 123.8(8) . . ? C5 C6 C1 122.3(6) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? O2 C7 O1 123.5(8) . . ? O2 C7 C1 120.3(7) . . ? O1 C7 C1 116.2(7) . . ? O4 C8 O3 124.6(7) . . ? O4 C8 C3 120.0(8) . . ? O3 C8 C3 115.3(7) . . ? O6 C9 O5 122.2(7) . . ? O6 C9 C5 120.4(8) . . ? O5 C9 C5 117.4(7) . . ? C15 C10 N1 119.8(7) . . ? C15 C10 C11 118.4(7) . . ? N1 C10 C11 121.4(7) . . ? C12 C11 C10 119.8(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.6(7) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.1(7) . . ? C12 C13 N2 121.7(6) . . ? C14 C13 N2 118.0(7) . . ? C13 C14 C15 120.2(8) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 120.9(8) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N3 C16 N2 112.7(7) . . ? N3 C16 H16 123.6 . . ? N2 C16 H16 123.6 . . ? C18 C17 N3 110.0(8) . . ? C18 C17 H17 125.0 . . ? N3 C17 H17 125.0 . . ? C17 C18 N2 105.0(8) . . ? C17 C18 H18 127.5 . . ? N2 C18 H18 127.5 . . ? C24 C19 C20 118.9(7) . . ? C24 C19 N1 121.0(7) . . ? C20 C19 N1 119.9(8) . . ? C21 C20 C19 119.6(8) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.6(8) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 121.5(8) . . ? C23 C22 N4 118.4(8) . . ? C21 C22 N4 120.0(8) . . ? C22 C23 C24 117.8(8) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? C19 C24 C23 121.5(8) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? N5 C25 N4 110.4(7) . . ? N5 C25 H25 124.8 . . ? N4 C25 H25 124.8 . . ? C27 C26 N5 109.7(8) . . ? C27 C26 H26 125.2 . . ? N5 C26 H26 125.2 . . ? N4 C27 C26 106.3(8) . . ? N4 C27 H27 126.8 . . ? C26 C27 H27 126.8 . . ? C33 C28 C29 118.4(8) . . ? C33 C28 N6 122.7(7) . . ? C29 C28 N6 118.9(7) . . ? C30 C29 C28 119.9(7) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 121.8(7) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C32 118.1(7) . . ? C30 C31 N1 119.4(7) . . ? C32 C31 N1 122.5(7) . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C28 C33 C32 122.1(7) . . ? C28 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? N6 C34 N7 111.4(7) . . ? N6 C34 H34 124.3 . . ? N7 C34 H34 124.3 . . ? C36 C35 N7 110.2(8) . . ? C36 C35 H35 124.9 . . ? N7 C35 H35 124.9 . . ? C35 C36 N6 106.4(7) . . ? C35 C36 H36 126.8 . . ? N6 C36 H36 126.8 . . ? C7 O1 Zn1 113.3(5) . . ? C8 O3 Zn2 115.2(5) . 3_644 ? C9 O5 Zn2 107.5(5) . . ? Zn1 O7 Zn2 133.0(4) 1_556 . ? C10 N1 C31 116.9(6) . . ? C10 N1 C19 118.8(7) . . ? C31 N1 C19 123.9(6) . . ? C16 N2 C18 107.1(6) . . ? C16 N2 C13 128.3(6) . . ? C18 N2 C13 124.3(7) . . ? C16 N3 C17 105.0(7) . . ? C16 N3 Zn1 130.6(5) . . ? C17 N3 Zn1 122.5(5) . . ? C27 N4 C25 107.6(7) . . ? C27 N4 C22 127.2(7) . . ? C25 N4 C22 125.2(7) . . ? C25 N5 C26 106.0(6) . . ? C25 N5 Zn1 122.6(6) . 1_545 ? C26 N5 Zn1 129.4(5) . 1_545 ? C34 N6 C36 107.3(7) . . ? C34 N6 C28 126.2(6) . . ? C36 N6 C28 126.4(7) . . ? C34 N7 C35 104.7(7) . . ? C34 N7 Zn2 129.8(5) . 4_463 ? C35 N7 Zn2 125.5(6) . 4_463 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.7(11) . . . . ? C7 C1 C2 C3 -177.0(7) . . . . ? C1 C2 C3 C4 1.9(11) . . . . ? C1 C2 C3 C8 -177.3(7) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C8 C3 C4 C5 -179.9(7) . . . . ? C3 C4 C5 C6 -2.8(11) . . . . ? C3 C4 C5 C9 175.4(7) . . . . ? C4 C5 C6 C1 2.0(11) . . . . ? C9 C5 C6 C1 -176.3(7) . . . . ? C2 C1 C6 C5 0.7(11) . . . . ? C7 C1 C6 C5 174.9(7) . . . . ? C6 C1 C7 O2 179.6(7) . . . . ? C2 C1 C7 O2 -6.3(12) . . . . ? C6 C1 C7 O1 0.9(11) . . . . ? C2 C1 C7 O1 175.1(7) . . . . ? C2 C3 C8 O4 -176.2(8) . . . . ? C4 C3 C8 O4 4.6(12) . . . . ? C2 C3 C8 O3 0.8(11) . . . . ? C4 C3 C8 O3 -178.4(7) . . . . ? C6 C5 C9 O6 0.7(12) . . . . ? C4 C5 C9 O6 -177.4(8) . . . . ? C6 C5 C9 O5 179.0(7) . . . . ? C4 C5 C9 O5 0.9(12) . . . . ? C15 C10 C11 C12 1.0(13) . . . . ? N1 C10 C11 C12 173.8(7) . . . . ? C10 C11 C12 C13 -1.1(13) . . . . ? C11 C12 C13 C14 0.9(14) . . . . ? C11 C12 C13 N2 -174.9(8) . . . . ? C12 C13 C14 C15 -0.6(14) . . . . ? N2 C13 C14 C15 175.4(9) . . . . ? N1 C10 C15 C14 -173.6(9) . . . . ? C11 C10 C15 C14 -0.7(14) . . . . ? C13 C14 C15 C10 0.5(15) . . . . ? N3 C17 C18 N2 -2.8(14) . . . . ? C24 C19 C20 C21 -0.2(13) . . . . ? N1 C19 C20 C21 175.8(7) . . . . ? C19 C20 C21 C22 -0.4(14) . . . . ? C20 C21 C22 C23 0.8(14) . . . . ? C20 C21 C22 N4 -176.9(7) . . . . ? C21 C22 C23 C24 -0.5(13) . . . . ? N4 C22 C23 C24 177.2(7) . . . . ? C20 C19 C24 C23 0.5(12) . . . . ? N1 C19 C24 C23 -175.5(7) . . . . ? C22 C23 C24 C19 -0.1(12) . . . . ? N5 C26 C27 N4 1.1(10) . . . . ? C33 C28 C29 C30 0.7(11) . . . . ? N6 C28 C29 C30 178.8(7) . . . . ? C28 C29 C30 C31 -1.6(12) . . . . ? C29 C30 C31 C32 3.5(12) . . . . ? C29 C30 C31 N1 -174.3(7) . . . . ? C30 C31 C32 C33 -4.5(11) . . . . ? N1 C31 C32 C33 173.2(7) . . . . ? C29 C28 C33 C32 -1.9(12) . . . . ? N6 C28 C33 C32 -179.9(7) . . . . ? C31 C32 C33 C28 3.8(12) . . . . ? N7 C35 C36 N6 0.8(11) . . . . ? O2 C7 O1 Zn1 1.0(11) . . . . ? C1 C7 O1 Zn1 179.6(5) . . . . ? O7 Zn1 O1 C7 -77.7(6) 1_554 . . . ? N3 Zn1 O1 C7 50.9(6) . . . . ? N5 Zn1 O1 C7 163.6(5) 1_565 . . . ? O4 C8 O3 Zn2 3.0(12) . . . 3_644 ? C3 C8 O3 Zn2 -174.0(5) . . . 3_644 ? O6 C9 O5 Zn2 9.6(11) . . . . ? C5 C9 O5 Zn2 -168.7(6) . . . . ? O7 Zn2 O5 C9 64.0(6) . . . . ? O3 Zn2 O5 C9 -60.9(6) 3_655 . . . ? N7 Zn2 O5 C9 -179.2(5) 4_567 . . . ? O3 Zn2 O7 Zn1 -109.7(4) 3_655 . . 1_556 ? N7 Zn2 O7 Zn1 17.1(5) 4_567 . . 1_556 ? O5 Zn2 O7 Zn1 120.9(4) . . . 1_556 ? C15 C10 N1 C31 53.5(11) . . . . ? C11 C10 N1 C31 -119.1(8) . . . . ? C15 C10 N1 C19 -119.8(9) . . . . ? C11 C10 N1 C19 67.6(10) . . . . ? C30 C31 N1 C10 32.6(10) . . . . ? C32 C31 N1 C10 -145.1(8) . . . . ? C30 C31 N1 C19 -154.4(7) . . . . ? C32 C31 N1 C19 27.9(11) . . . . ? C24 C19 N1 C10 34.1(11) . . . . ? C20 C19 N1 C10 -141.9(8) . . . . ? C24 C19 N1 C31 -138.8(8) . . . . ? C20 C19 N1 C31 45.3(11) . . . . ? N3 C16 N2 C18 1.9(11) . . . . ? N3 C16 N2 C13 176.2(8) . . . . ? C17 C18 N2 C16 0.6(13) . . . . ? C17 C18 N2 C13 -173.9(9) . . . . ? C12 C13 N2 C16 -14.5(14) . . . . ? C14 C13 N2 C16 169.6(9) . . . . ? C12 C13 N2 C18 158.9(10) . . . . ? C14 C13 N2 C18 -17.0(14) . . . . ? N2 C16 N3 C17 -3.6(11) . . . . ? N2 C16 N3 Zn1 -167.6(6) . . . . ? C18 C17 N3 C16 3.9(12) . . . . ? C18 C17 N3 Zn1 169.6(8) . . . . ? O7 Zn1 N3 C16 76.4(8) 1_554 . . . ? O1 Zn1 N3 C16 -53.6(8) . . . . ? N5 Zn1 N3 C16 -174.2(8) 1_565 . . . ? O7 Zn1 N3 C17 -85.2(8) 1_554 . . . ? O1 Zn1 N3 C17 144.8(7) . . . . ? N5 Zn1 N3 C17 24.2(8) 1_565 . . . ? C26 C27 N4 C25 -0.5(9) . . . . ? C26 C27 N4 C22 179.2(7) . . . . ? N5 C25 N4 C27 -0.3(9) . . . . ? N5 C25 N4 C22 -180.0(7) . . . . ? C23 C22 N4 C27 37.4(11) . . . . ? C21 C22 N4 C27 -144.9(9) . . . . ? C23 C22 N4 C25 -143.0(8) . . . . ? C21 C22 N4 C25 34.8(12) . . . . ? N4 C25 N5 C26 0.9(9) . . . . ? N4 C25 N5 Zn1 166.1(5) . . . 1_545 ? C27 C26 N5 C25 -1.2(10) . . . . ? C27 C26 N5 Zn1 -165.0(6) . . . 1_545 ? N7 C34 N6 C36 1.5(9) . . . . ? N7 C34 N6 C28 178.2(6) . . . . ? C35 C36 N6 C34 -1.4(10) . . . . ? C35 C36 N6 C28 -178.0(7) . . . . ? C33 C28 N6 C34 -15.0(11) . . . . ? C29 C28 N6 C34 167.0(7) . . . . ? C33 C28 N6 C36 161.0(8) . . . . ? C29 C28 N6 C36 -16.9(11) . . . . ? N6 C34 N7 C35 -0.9(9) . . . . ? N6 C34 N7 Zn2 176.7(5) . . . 4_463 ? C36 C35 N7 C34 0.0(10) . . . . ? C36 C35 N7 Zn2 -177.7(6) . . . 4_463 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.935 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.082 data_3 _database_code_depnum_ccdc_archive 'CCDC 826244' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C37 H23 N7 O8 Zn2), 7(H2 O)' _chemical_formula_sum 'C74 H53 N14 O23 Zn4' _chemical_formula_weight 1767.78 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7970(4) _cell_length_b 7.7300(2) _cell_length_c 26.6750(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.466(2) _cell_angle_gamma 90.00 _cell_volume 3662.99(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6681 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 25.4 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1798 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15894 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6681 _reflns_number_gt 4451 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6681 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _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 0.80343(2) -0.43200(4) -0.024002(13) 0.02726(11) Uani 1 1 d . . . Zn2 Zn 0.69659(2) 0.02353(4) 0.036673(13) 0.02705(11) Uani 1 1 d . . . C1 C 0.92569(17) -0.0288(4) 0.01192(10) 0.0240(7) Uani 1 1 d . . . C2 C 0.97485(18) -0.1653(4) 0.00585(11) 0.0270(7) Uani 1 1 d . . . H3 H 0.9574 -0.2774 0.0102 0.032 Uiso 1 1 calc R . . C3 C 1.04880(18) -0.1424(4) -0.00636(10) 0.0240(7) Uani 1 1 d . . . C4 C 0.84661(18) -0.0701(4) 0.02393(10) 0.0244(7) Uani 1 1 d . . . C5 C 1.09406(18) -0.3076(4) -0.01314(13) 0.0298(8) Uani 1 1 d . . . C6 C 0.65589(19) -0.4585(4) -0.02638(13) 0.0330(8) Uani 1 1 d . . . C7 C 0.57546(17) -0.4763(4) -0.01138(11) 0.0264(7) Uani 1 1 d . . . C8 C 0.59066(19) -0.2511(4) 0.05783(12) 0.0305(8) Uani 1 1 d . . . C9 C 0.54633(18) -0.3883(4) 0.02899(11) 0.0259(7) Uani 1 1 d . . . C10 C 0.47169(18) -0.4143(4) 0.03946(11) 0.0284(7) Uani 1 1 d . . . H10 H 0.4528 -0.3558 0.0664 0.034 Uiso 1 1 calc R . . C11 C 0.7198(2) 0.3143(4) 0.10431(11) 0.0341(8) Uani 1 1 d . . . H11 H 0.7680 0.3287 0.0934 0.041 Uiso 1 1 calc R . . C12 C 0.6092(2) 0.2147(5) 0.11426(13) 0.0485(10) Uani 1 1 d . . . H12 H 0.5664 0.1454 0.1112 0.058 Uiso 1 1 calc R . . C13 C 0.6173(2) 0.3546(5) 0.14338(14) 0.0506(11) Uani 1 1 d . . . H13 H 0.5818 0.3999 0.1639 0.061 Uiso 1 1 calc R . . C14 C 0.72069(19) 0.5711(4) 0.15951(11) 0.0321(8) Uani 1 1 d . . . C15 C 0.7669(2) 0.6727(4) 0.13241(12) 0.0407(9) Uani 1 1 d . . . H15 H 0.7764 0.6420 0.0997 0.049 Uiso 1 1 calc R . . C16 C 0.7990(2) 0.8195(5) 0.15336(12) 0.0437(10) Uani 1 1 d . . . H16 H 0.8302 0.8873 0.1347 0.052 Uiso 1 1 calc R . . C17 C 0.7854(2) 0.8676(4) 0.20223(11) 0.0349(8) Uani 1 1 d . . . C18 C 0.7375(2) 0.7657(4) 0.22862(11) 0.0379(9) Uani 1 1 d . . . H18 H 0.7268 0.7972 0.2611 0.045 Uiso 1 1 calc R . . C19 C 0.7055(2) 0.6177(4) 0.20747(11) 0.0372(9) Uani 1 1 d . . . H19 H 0.6737 0.5499 0.2257 0.045 Uiso 1 1 calc R . . C20 C 0.7874(2) 1.1065(4) 0.26346(11) 0.0351(8) Uani 1 1 d . . . C21 C 0.7137(2) 1.1527(5) 0.26042(12) 0.0453(10) Uani 1 1 d . . . H21 H 0.6842 1.1295 0.2312 0.054 Uiso 1 1 calc R . . C22 C 0.6815(2) 1.2340(5) 0.30026(12) 0.0424(9) Uani 1 1 d . . . H22 H 0.6309 1.2644 0.2980 0.051 Uiso 1 1 calc R . . C23 C 0.7256(2) 1.2690(4) 0.34323(11) 0.0336(8) Uani 1 1 d . . . C24 C 0.8004(2) 1.2267(4) 0.34646(12) 0.0382(9) Uani 1 1 d . . . H24 H 0.8301 1.2532 0.3753 0.046 Uiso 1 1 calc R . . C25 C 0.8317(2) 1.1443(4) 0.30671(12) 0.0403(9) Uani 1 1 d . . . H25 H 0.8824 1.1142 0.3089 0.048 Uiso 1 1 calc R . . C26 C 0.7196(2) 1.3449(4) 0.43335(11) 0.0338(8) Uani 1 1 d . . . H26 H 0.7639 1.2893 0.4444 0.041 Uiso 1 1 calc R . . C27 C 0.6268(2) 1.4439(5) 0.38435(13) 0.0426(9) Uani 1 1 d . . . H27 H 0.5950 1.4687 0.3563 0.051 Uiso 1 1 calc R . . C28 C 0.6174(2) 1.4936(5) 0.43173(12) 0.0405(9) Uani 1 1 d . . . H28 H 0.5779 1.5610 0.4420 0.049 Uiso 1 1 calc R . . C29 C 0.8902(2) 1.0730(5) 0.20714(11) 0.0375(9) Uani 1 1 d . . . C30 C 0.9500(2) 0.9599(5) 0.20448(13) 0.0505(10) Uani 1 1 d . . . H30 H 0.9456 0.8473 0.2162 0.061 Uiso 1 1 calc R . . C31 C 1.0161(2) 1.0119(5) 0.18464(14) 0.0514(10) Uani 1 1 d . . . H31 H 1.0555 0.9340 0.1823 0.062 Uiso 1 1 calc R . . C32 C 1.0234(2) 1.1793(4) 0.16837(11) 0.0347(8) Uani 1 1 d . . . C33 C 0.9667(2) 1.2949(5) 0.17259(12) 0.0438(9) Uani 1 1 d . . . H33 H 0.9728 1.4092 0.1627 0.053 Uiso 1 1 calc R . . C34 C 0.8992(2) 1.2423(5) 0.19178(13) 0.0450(9) Uani 1 1 d . . . H34 H 0.8601 1.3211 0.1943 0.054 Uiso 1 1 calc R . . C35 C 1.1617(2) 1.1714(5) 0.15786(13) 0.0452(10) Uani 1 1 d . . . H35 H 1.1763 1.1015 0.1851 0.054 Uiso 1 1 calc R . . C36 C 1.0942(2) 1.3240(4) 0.10327(11) 0.0339(8) Uani 1 1 d . . . H36 H 1.0531 1.3777 0.0866 0.041 Uiso 1 1 calc R . . C37 C 1.2068(2) 1.2359(5) 0.12362(13) 0.0432(9) Uani 1 1 d . . . H37 H 1.2585 1.2182 0.1234 0.052 Uiso 1 1 calc R . . O1 O 0.82234(13) -0.2206(3) 0.01959(8) 0.0350(6) Uani 1 1 d . . . O2 O 0.80730(12) 0.0539(3) 0.03898(8) 0.0308(5) Uani 1 1 d . . . O1W O 0.5770(2) -0.3846(6) -0.15810(14) 0.1211(14) Uani 1 1 d . . . O3 O 1.08465(17) -0.3882(3) -0.05206(10) 0.0623(8) Uani 1 1 d . . . O2W O 0.5397(3) 1.6072(7) 0.27763(14) 0.1504(19) Uani 1 1 d . . . O4 O 1.13469(13) -0.3560(3) 0.02509(8) 0.0360(6) Uani 1 1 d . . . O3W O 0.5095(3) -0.2558(10) 0.18620(16) 0.226(4) Uani 1 1 d . . . O5 O 0.70910(13) -0.5011(3) 0.00499(9) 0.0410(6) Uani 1 1 d . . . O4W O 0.9764(7) 1.6587(15) 0.1155(4) 0.177(4) Uiso 0.50 1 d P . . O6 O 0.66710(15) -0.4127(4) -0.06924(10) 0.0587(8) Uani 1 1 d . . . O7 O 0.64281(14) -0.1873(3) 0.03436(8) 0.0430(6) Uani 1 1 d . . . O8 O 0.57348(16) -0.2058(4) 0.09946(9) 0.0631(8) Uani 1 1 d . . . N1 N 0.82064(17) 1.0152(4) 0.22384(10) 0.0458(8) Uani 1 1 d . . . N2 N 0.67376(16) 0.1888(3) 0.08954(9) 0.0343(7) Uani 1 1 d . . . N3 N 0.68787(16) 0.4191(3) 0.13725(9) 0.0330(7) Uani 1 1 d . . . N4 N 0.69207(17) 1.3499(3) 0.38508(9) 0.0340(7) Uani 1 1 d . . . N5 N 0.67529(16) 1.4294(3) 0.46263(9) 0.0324(7) Uani 1 1 d . . . N6 N 1.09078(16) 1.2279(4) 0.14493(9) 0.0342(7) Uani 1 1 d . . . N7 N 1.16448(15) 1.3320(3) 0.08901(9) 0.0319(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0216(2) 0.0234(2) 0.0375(2) 0.00057(15) 0.00751(15) -0.00048(17) Zn2 0.0220(2) 0.0270(2) 0.0329(2) -0.00600(16) 0.00816(15) -0.00590(17) C1 0.0191(17) 0.0220(16) 0.0311(16) -0.0018(13) 0.0044(13) -0.0003(15) C2 0.026(2) 0.0166(16) 0.0384(18) 0.0016(13) 0.0052(14) -0.0038(15) C3 0.0211(19) 0.0240(17) 0.0270(16) -0.0005(13) 0.0019(13) 0.0002(14) C4 0.0219(18) 0.0284(18) 0.0228(15) 0.0020(13) 0.0005(13) -0.0033(16) C5 0.021(2) 0.0278(18) 0.041(2) 0.0014(16) 0.0059(15) 0.0013(15) C6 0.021(2) 0.0266(18) 0.053(2) -0.0072(16) 0.0076(17) -0.0067(16) C7 0.0169(17) 0.0244(17) 0.0385(18) 0.0015(14) 0.0070(13) -0.0025(15) C8 0.0216(19) 0.0299(18) 0.040(2) -0.0050(15) 0.0043(15) -0.0037(16) C9 0.0199(18) 0.0230(16) 0.0347(17) 0.0007(14) 0.0016(14) -0.0050(14) C10 0.0240(19) 0.0248(17) 0.0372(18) -0.0064(14) 0.0094(14) -0.0056(15) C11 0.030(2) 0.036(2) 0.0369(18) -0.0101(16) 0.0111(15) -0.0042(17) C12 0.031(2) 0.051(2) 0.066(2) -0.023(2) 0.0211(19) -0.0137(19) C13 0.035(2) 0.054(2) 0.066(2) -0.027(2) 0.0252(19) -0.011(2) C14 0.037(2) 0.0291(18) 0.0307(17) -0.0052(15) 0.0056(15) -0.0063(17) C15 0.053(3) 0.043(2) 0.0272(17) -0.0084(16) 0.0131(16) -0.0110(19) C16 0.054(3) 0.047(2) 0.0324(19) -0.0065(17) 0.0162(17) -0.021(2) C17 0.037(2) 0.0359(19) 0.0320(18) -0.0063(15) 0.0067(15) -0.0089(17) C18 0.045(2) 0.044(2) 0.0253(17) -0.0068(16) 0.0111(16) -0.0085(19) C19 0.041(2) 0.037(2) 0.0341(18) -0.0029(16) 0.0134(16) -0.0102(17) C20 0.042(2) 0.0317(19) 0.0332(18) -0.0079(15) 0.0135(16) -0.0134(18) C21 0.047(3) 0.056(2) 0.0328(19) -0.0102(17) 0.0029(17) -0.007(2) C22 0.040(2) 0.051(2) 0.036(2) -0.0045(17) 0.0016(17) -0.0004(19) C23 0.040(2) 0.0273(18) 0.0341(19) -0.0021(15) 0.0064(16) -0.0032(17) C24 0.044(3) 0.039(2) 0.0307(18) -0.0098(15) -0.0003(16) -0.0039(18) C25 0.040(2) 0.040(2) 0.042(2) -0.0073(17) 0.0112(17) -0.0045(18) C26 0.037(2) 0.0307(19) 0.0334(19) 0.0015(15) 0.0023(16) 0.0080(17) C27 0.037(2) 0.048(2) 0.042(2) -0.0021(17) -0.0081(16) 0.010(2) C28 0.033(2) 0.047(2) 0.041(2) -0.0096(17) -0.0010(16) 0.0107(19) C29 0.040(2) 0.042(2) 0.0320(18) -0.0118(16) 0.0130(15) -0.0162(19) C30 0.055(3) 0.040(2) 0.059(2) 0.0054(18) 0.018(2) -0.009(2) C31 0.047(3) 0.043(2) 0.066(2) 0.0045(19) 0.022(2) 0.000(2) C32 0.033(2) 0.040(2) 0.0318(18) 0.0000(15) 0.0086(15) -0.0071(18) C33 0.045(3) 0.040(2) 0.048(2) 0.0036(17) 0.0122(18) -0.007(2) C34 0.041(2) 0.044(2) 0.052(2) -0.0057(18) 0.0133(18) -0.0050(19) C35 0.040(3) 0.048(2) 0.047(2) 0.0172(18) 0.0008(18) -0.002(2) C36 0.031(2) 0.038(2) 0.0338(18) 0.0033(16) 0.0032(15) -0.0002(17) C37 0.029(2) 0.046(2) 0.055(2) 0.0143(18) 0.0034(18) 0.0019(18) O1 0.0302(14) 0.0260(13) 0.0504(14) -0.0075(10) 0.0144(11) -0.0111(11) O2 0.0186(12) 0.0264(12) 0.0484(13) -0.0038(10) 0.0109(10) -0.0007(10) O1W 0.107(3) 0.143(4) 0.109(3) -0.008(3) -0.024(2) 0.015(3) O3 0.074(2) 0.0477(16) 0.0633(17) -0.0277(14) -0.0129(15) 0.0205(15) O2W 0.175(5) 0.190(5) 0.085(3) 0.020(3) -0.009(3) 0.034(4) O4 0.0300(15) 0.0299(12) 0.0483(13) 0.0038(11) 0.0029(11) 0.0082(11) O3W 0.132(4) 0.457(10) 0.097(3) 0.129(5) 0.063(3) 0.159(6) O5 0.0195(14) 0.0368(14) 0.0674(16) 0.0017(12) 0.0067(12) -0.0069(11) O6 0.0393(17) 0.084(2) 0.0553(17) 0.0101(15) 0.0221(13) -0.0102(15) O7 0.0424(16) 0.0390(14) 0.0495(14) -0.0098(11) 0.0179(12) -0.0238(13) O8 0.061(2) 0.077(2) 0.0538(16) -0.0290(15) 0.0245(14) -0.0382(16) N1 0.051(2) 0.0482(19) 0.0404(16) -0.0206(14) 0.0218(14) -0.0272(17) N2 0.0310(18) 0.0316(16) 0.0411(16) -0.0118(13) 0.0101(13) -0.0047(14) N3 0.0327(18) 0.0318(16) 0.0354(15) -0.0104(12) 0.0101(12) -0.0051(14) N4 0.042(2) 0.0294(15) 0.0306(15) -0.0030(12) 0.0013(13) 0.0024(14) N5 0.0326(18) 0.0318(15) 0.0332(14) -0.0011(12) 0.0046(13) 0.0072(14) N6 0.0289(18) 0.0388(17) 0.0355(16) 0.0054(13) 0.0071(13) -0.0054(14) N7 0.0250(17) 0.0336(16) 0.0375(15) 0.0030(12) 0.0054(13) 0.0000(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.964(2) . ? Zn1 O4 1.976(2) 3_745 ? Zn1 N7 2.013(2) 3_765 ? Zn1 O1 2.022(2) . ? Zn2 O7 1.889(2) . ? Zn2 N2 1.964(2) . ? Zn2 O2 1.981(2) . ? Zn2 N5 2.022(2) 4_575 ? C1 C2 1.386(4) . ? C1 C3 1.410(4) 3_755 ? C1 C4 1.497(4) . ? C2 C3 1.386(4) . ? C2 H3 0.9300 . ? C3 C1 1.410(4) 3_755 ? C3 C5 1.526(4) . ? C4 O1 1.244(3) . ? C4 O2 1.266(4) . ? C5 O3 1.214(4) . ? C5 O4 1.270(4) . ? C6 O6 1.225(4) . ? C6 O5 1.269(4) . ? C6 C7 1.516(4) . ? C7 C10 1.380(4) 3_645 ? C7 C9 1.399(4) . ? C8 O8 1.221(4) . ? C8 O7 1.252(4) . ? C8 C9 1.506(4) . ? C9 C10 1.388(4) . ? C10 C7 1.380(4) 3_645 ? C10 H10 0.9300 . ? C11 N2 1.314(4) . ? C11 N3 1.346(4) . ? C11 H11 0.9300 . ? C12 C13 1.334(5) . ? C12 N2 1.374(4) . ? C12 H12 0.9300 . ? C13 N3 1.370(4) . ? C13 H13 0.9300 . ? C14 C19 1.372(4) . ? C14 C15 1.374(4) . ? C14 N3 1.425(4) . ? C15 C16 1.374(5) . ? C15 H15 0.9300 . ? C16 C17 1.391(4) . ? C16 H16 0.9300 . ? C17 C18 1.384(4) . ? C17 N1 1.408(4) . ? C18 C19 1.384(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.358(5) . ? C20 C25 1.389(5) . ? C20 N1 1.428(4) . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C22 C23 1.376(5) . ? C22 H22 0.9300 . ? C23 C24 1.369(5) . ? C23 N4 1.440(4) . ? C24 C25 1.382(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 N5 1.316(4) . ? C26 N4 1.350(4) . ? C26 H26 0.9300 . ? C27 C28 1.341(4) . ? C27 N4 1.370(4) . ? C27 H27 0.9300 . ? C28 N5 1.372(4) . ? C28 H28 0.9300 . ? C29 C30 1.382(5) . ? C29 C34 1.383(5) . ? C29 N1 1.414(4) . ? C30 C31 1.378(5) . ? C30 H30 0.9300 . ? C31 C32 1.374(5) . ? C31 H31 0.9300 . ? C32 C33 1.358(5) . ? C32 N6 1.435(4) . ? C33 C34 1.394(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C37 1.347(5) . ? C35 N6 1.360(5) . ? C35 H35 0.9300 . ? C36 N7 1.331(4) . ? C36 N6 1.341(4) . ? C36 H36 0.9300 . ? C37 N7 1.374(4) . ? C37 H37 0.9300 . ? O4 Zn1 1.976(2) 3_745 ? N5 Zn2 2.022(2) 4_576 ? N7 Zn1 2.013(2) 3_765 ? 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 O5 Zn1 O4 105.71(9) . 3_745 ? O5 Zn1 N7 137.51(11) . 3_765 ? O4 Zn1 N7 96.81(10) 3_745 3_765 ? O5 Zn1 O1 96.30(9) . . ? O4 Zn1 O1 127.26(10) 3_745 . ? N7 Zn1 O1 97.99(9) 3_765 . ? O7 Zn2 N2 117.29(10) . . ? O7 Zn2 O2 127.16(10) . . ? N2 Zn2 O2 98.58(10) . . ? O7 Zn2 N5 93.37(10) . 4_575 ? N2 Zn2 N5 123.35(11) . 4_575 ? O2 Zn2 N5 97.84(10) . 4_575 ? C2 C1 C3 119.5(3) . 3_755 ? C2 C1 C4 118.1(3) . . ? C3 C1 C4 122.4(3) 3_755 . ? C3 C2 C1 123.0(3) . . ? C3 C2 H3 118.5 . . ? C1 C2 H3 118.5 . . ? C2 C3 C1 117.4(3) . 3_755 ? C2 C3 C5 115.9(3) . . ? C1 C3 C5 126.7(3) 3_755 . ? O1 C4 O2 122.8(3) . . ? O1 C4 C1 120.4(3) . . ? O2 C4 C1 116.8(3) . . ? O3 C5 O4 125.3(3) . . ? O3 C5 C3 119.0(3) . . ? O4 C5 C3 115.5(3) . . ? O6 C6 O5 122.3(3) . . ? O6 C6 C7 118.8(3) . . ? O5 C6 C7 118.8(3) . . ? C10 C7 C9 118.3(3) 3_645 . ? C10 C7 C6 117.7(3) 3_645 . ? C9 C7 C6 124.0(3) . . ? O8 C8 O7 125.2(3) . . ? O8 C8 C9 121.0(3) . . ? O7 C8 C9 113.8(3) . . ? C10 C9 C7 119.2(3) . . ? C10 C9 C8 118.5(3) . . ? C7 C9 C8 121.9(3) . . ? C7 C10 C9 122.5(3) 3_645 . ? C7 C10 H10 118.7 3_645 . ? C9 C10 H10 118.7 . . ? N2 C11 N3 111.1(3) . . ? N2 C11 H11 124.4 . . ? N3 C11 H11 124.4 . . ? C13 C12 N2 109.5(3) . . ? C13 C12 H12 125.3 . . ? N2 C12 H12 125.3 . . ? C12 C13 N3 107.0(3) . . ? C12 C13 H13 126.5 . . ? N3 C13 H13 126.5 . . ? C19 C14 C15 119.9(3) . . ? C19 C14 N3 120.4(3) . . ? C15 C14 N3 119.7(3) . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 118.1(3) . . ? C18 C17 N1 121.7(3) . . ? C16 C17 N1 120.2(3) . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 119.8(3) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C25 119.5(3) . . ? C21 C20 N1 121.8(3) . . ? C25 C20 N1 118.6(3) . . ? C20 C21 C22 121.0(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 119.1(4) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 120.6(3) . . ? C24 C23 N4 120.1(3) . . ? C22 C23 N4 119.3(3) . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 119.9(4) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? N5 C26 N4 110.9(3) . . ? N5 C26 H26 124.6 . . ? N4 C26 H26 124.6 . . ? C28 C27 N4 107.0(3) . . ? C28 C27 H27 126.5 . . ? N4 C27 H27 126.5 . . ? C27 C28 N5 109.4(3) . . ? C27 C28 H28 125.3 . . ? N5 C28 H28 125.3 . . ? C30 C29 C34 118.7(3) . . ? C30 C29 N1 120.5(3) . . ? C34 C29 N1 120.7(4) . . ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.7(4) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.6(3) . . ? C33 C32 N6 120.6(3) . . ? C31 C32 N6 118.8(3) . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C29 C34 C33 120.1(4) . . ? C29 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C37 C35 N6 106.9(3) . . ? C37 C35 H35 126.5 . . ? N6 C35 H35 126.5 . . ? N7 C36 N6 110.7(3) . . ? N7 C36 H36 124.7 . . ? N6 C36 H36 124.7 . . ? C35 C37 N7 109.3(3) . . ? C35 C37 H37 125.3 . . ? N7 C37 H37 125.3 . . ? C4 O1 Zn1 148.7(2) . . ? C4 O2 Zn2 117.89(19) . . ? C5 O4 Zn1 121.5(2) . 3_745 ? C6 O5 Zn1 106.9(2) . . ? C8 O7 Zn2 135.5(2) . . ? C17 N1 C29 120.2(3) . . ? C17 N1 C20 120.6(3) . . ? C29 N1 C20 119.1(3) . . ? C11 N2 C12 105.8(3) . . ? C11 N2 Zn2 122.9(2) . . ? C12 N2 Zn2 130.9(2) . . ? C11 N3 C13 106.5(3) . . ? C11 N3 C14 126.1(3) . . ? C13 N3 C14 127.3(3) . . ? C26 N4 C27 106.7(3) . . ? C26 N4 C23 125.7(3) . . ? C27 N4 C23 127.6(3) . . ? C26 N5 C28 106.1(3) . . ? C26 N5 Zn2 125.8(2) . 4_576 ? C28 N5 Zn2 127.7(2) . 4_576 ? C36 N6 C35 107.5(3) . . ? C36 N6 C32 125.9(3) . . ? C35 N6 C32 126.3(3) . . ? C36 N7 C37 105.6(3) . . ? C36 N7 Zn1 125.8(2) . 3_765 ? C37 N7 Zn1 127.9(2) . 3_765 ? 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 C3 C1 C2 C3 -1.0(5) 3_755 . . . ? C4 C1 C2 C3 178.6(3) . . . . ? C1 C2 C3 C1 1.0(5) . . . 3_755 ? C1 C2 C3 C5 -178.2(3) . . . . ? C2 C1 C4 O1 -12.7(4) . . . . ? C3 C1 C4 O1 166.9(3) 3_755 . . . ? C2 C1 C4 O2 166.4(3) . . . . ? C3 C1 C4 O2 -14.0(4) 3_755 . . . ? C2 C3 C5 O3 78.3(4) . . . . ? C1 C3 C5 O3 -100.8(4) 3_755 . . . ? C2 C3 C5 O4 -96.2(3) . . . . ? C1 C3 C5 O4 84.7(4) 3_755 . . . ? O6 C6 C7 C10 56.7(4) . . . 3_645 ? O5 C6 C7 C10 -119.4(3) . . . 3_645 ? O6 C6 C7 C9 -123.1(4) . . . . ? O5 C6 C7 C9 60.8(4) . . . . ? C10 C7 C9 C10 0.3(5) 3_645 . . . ? C6 C7 C9 C10 -180.0(3) . . . . ? C10 C7 C9 C8 -172.6(3) 3_645 . . . ? C6 C7 C9 C8 7.2(5) . . . . ? O8 C8 C9 C10 25.1(5) . . . . ? O7 C8 C9 C10 -152.4(3) . . . . ? O8 C8 C9 C7 -162.0(3) . . . . ? O7 C8 C9 C7 20.5(4) . . . . ? C7 C9 C10 C7 -0.3(5) . . . 3_645 ? C8 C9 C10 C7 172.9(3) . . . 3_645 ? N2 C12 C13 N3 0.0(5) . . . . ? C19 C14 C15 C16 1.1(6) . . . . ? N3 C14 C15 C16 -179.9(3) . . . . ? C14 C15 C16 C17 0.0(6) . . . . ? C15 C16 C17 C18 -1.3(6) . . . . ? C15 C16 C17 N1 177.9(4) . . . . ? C16 C17 C18 C19 1.5(5) . . . . ? N1 C17 C18 C19 -177.7(4) . . . . ? C15 C14 C19 C18 -0.9(5) . . . . ? N3 C14 C19 C18 -179.8(3) . . . . ? C17 C18 C19 C14 -0.5(6) . . . . ? C25 C20 C21 C22 -1.3(5) . . . . ? N1 C20 C21 C22 176.9(3) . . . . ? C20 C21 C22 C23 0.5(5) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C21 C22 C23 N4 -178.7(3) . . . . ? C22 C23 C24 C25 -1.6(5) . . . . ? N4 C23 C24 C25 178.1(3) . . . . ? C23 C24 C25 C20 0.7(5) . . . . ? C21 C20 C25 C24 0.7(5) . . . . ? N1 C20 C25 C24 -177.5(3) . . . . ? N4 C27 C28 N5 -1.1(4) . . . . ? C34 C29 C30 C31 -3.2(5) . . . . ? N1 C29 C30 C31 175.0(3) . . . . ? C29 C30 C31 C32 1.6(6) . . . . ? C30 C31 C32 C33 1.3(6) . . . . ? C30 C31 C32 N6 -176.1(3) . . . . ? C31 C32 C33 C34 -2.5(5) . . . . ? N6 C32 C33 C34 174.9(3) . . . . ? C30 C29 C34 C33 2.0(5) . . . . ? N1 C29 C34 C33 -176.2(3) . . . . ? C32 C33 C34 C29 0.8(5) . . . . ? N6 C35 C37 N7 -0.4(4) . . . . ? O2 C4 O1 Zn1 125.7(4) . . . . ? C1 C4 O1 Zn1 -55.2(5) . . . . ? O5 Zn1 O1 C4 -145.1(4) . . . . ? O4 Zn1 O1 C4 99.6(4) 3_745 . . . ? N7 Zn1 O1 C4 -5.3(4) 3_765 . . . ? O1 C4 O2 Zn2 -18.0(4) . . . . ? C1 C4 O2 Zn2 162.87(19) . . . . ? O7 Zn2 O2 C4 21.0(2) . . . . ? N2 Zn2 O2 C4 155.1(2) . . . . ? N5 Zn2 O2 C4 -79.3(2) 4_575 . . . ? O3 C5 O4 Zn1 5.2(5) . . . 3_745 ? C3 C5 O4 Zn1 179.33(19) . . . 3_745 ? O6 C6 O5 Zn1 11.4(4) . . . . ? C7 C6 O5 Zn1 -172.7(2) . . . . ? O4 Zn1 O5 C6 -124.4(2) 3_745 . . . ? N7 Zn1 O5 C6 -5.2(3) 3_765 . . . ? O1 Zn1 O5 C6 104.0(2) . . . . ? O8 C8 O7 Zn2 -21.4(6) . . . . ? C9 C8 O7 Zn2 155.9(2) . . . . ? N2 Zn2 O7 C8 4.0(4) . . . . ? O2 Zn2 O7 C8 131.0(3) . . . . ? N5 Zn2 O7 C8 -126.5(3) 4_575 . . . ? C18 C17 N1 C29 152.8(4) . . . . ? C16 C17 N1 C29 -26.4(5) . . . . ? C18 C17 N1 C20 -26.0(5) . . . . ? C16 C17 N1 C20 154.8(4) . . . . ? C30 C29 N1 C17 -51.4(5) . . . . ? C34 C29 N1 C17 126.7(4) . . . . ? C30 C29 N1 C20 127.5(4) . . . . ? C34 C29 N1 C20 -54.4(5) . . . . ? C21 C20 N1 C17 -48.4(5) . . . . ? C25 C20 N1 C17 129.7(3) . . . . ? C21 C20 N1 C29 132.7(4) . . . . ? C25 C20 N1 C29 -49.1(5) . . . . ? N3 C11 N2 C12 0.0(4) . . . . ? N3 C11 N2 Zn2 173.9(2) . . . . ? C13 C12 N2 C11 0.0(4) . . . . ? C13 C12 N2 Zn2 -173.2(3) . . . . ? O7 Zn2 N2 C11 160.3(2) . . . . ? O2 Zn2 N2 C11 20.4(3) . . . . ? N5 Zn2 N2 C11 -84.9(3) 4_575 . . . ? O7 Zn2 N2 C12 -27.5(4) . . . . ? O2 Zn2 N2 C12 -167.4(3) . . . . ? N5 Zn2 N2 C12 87.3(3) 4_575 . . . ? N2 C11 N3 C13 0.0(4) . . . . ? N2 C11 N3 C14 -177.7(3) . . . . ? C12 C13 N3 C11 0.0(4) . . . . ? C12 C13 N3 C14 177.7(3) . . . . ? C19 C14 N3 C11 -146.9(3) . . . . ? C15 C14 N3 C11 34.1(5) . . . . ? C19 C14 N3 C13 35.9(5) . . . . ? C15 C14 N3 C13 -143.1(4) . . . . ? N5 C26 N4 C27 0.3(4) . . . . ? N5 C26 N4 C23 -179.1(3) . . . . ? C28 C27 N4 C26 0.5(4) . . . . ? C28 C27 N4 C23 179.8(3) . . . . ? C24 C23 N4 C26 -21.2(5) . . . . ? C22 C23 N4 C26 158.5(3) . . . . ? C24 C23 N4 C27 159.7(3) . . . . ? C22 C23 N4 C27 -20.7(5) . . . . ? N4 C26 N5 C28 -0.9(4) . . . . ? N4 C26 N5 Zn2 -174.4(2) . . . 4_576 ? C27 C28 N5 C26 1.3(4) . . . . ? C27 C28 N5 Zn2 174.5(2) . . . 4_576 ? N7 C36 N6 C35 -0.2(4) . . . . ? N7 C36 N6 C32 -174.4(3) . . . . ? C37 C35 N6 C36 0.3(4) . . . . ? C37 C35 N6 C32 174.5(3) . . . . ? C33 C32 N6 C36 -41.4(5) . . . . ? C31 C32 N6 C36 136.1(4) . . . . ? C33 C32 N6 C35 145.5(4) . . . . ? C31 C32 N6 C35 -37.0(5) . . . . ? N6 C36 N7 C37 0.0(4) . . . . ? N6 C36 N7 Zn1 171.0(2) . . . 3_765 ? C35 C37 N7 C36 0.2(4) . . . . ? C35 C37 N7 Zn1 -170.5(2) . . . 3_765 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.657 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.066 data_4 _database_code_depnum_ccdc_archive 'CCDC 826245' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H25 Mn N7 O4, H2 O' _chemical_formula_sum 'C35 H27 Mn N7 O5' _chemical_formula_weight 680.58 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3128(8) _cell_length_b 29.2377(18) _cell_length_c 10.1543(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.132(6) _cell_angle_gamma 90.00 _cell_volume 3173.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5774 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 25.4 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20600 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_av_sigmaI/netI 0.1675 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5774 _reflns_number_gt 2726 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0001P)^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 5774 _refine_ls_number_parameters 439 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0403 _refine_ls_goodness_of_fit_ref 0.806 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.097 _refine_ls_shift/su_mean 0.003 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 Mn1 Mn 0.89731(4) 0.524202(16) 0.63699(4) 0.02893(12) Uani 1 1 d . . . C1 C 0.5224(3) 0.21700(10) 0.6897(3) 0.0333(8) Uani 1 1 d . . . C2 C 0.5709(3) 0.21361(10) 0.5810(3) 0.0400(8) Uani 1 1 d . . . H2 H 0.5468 0.2344 0.5077 0.048 Uiso 1 1 calc R . . C3 C 0.6543(3) 0.17965(11) 0.5819(3) 0.0410(8) Uani 1 1 d . . . H3 H 0.6884 0.1782 0.5102 0.049 Uiso 1 1 calc R . . C4 C 0.6887(3) 0.14759(10) 0.6869(3) 0.0312(8) Uani 1 1 d . . . C5 C 0.6404(3) 0.15041(10) 0.7938(3) 0.0364(8) Uani 1 1 d . . . H5 H 0.6630 0.1289 0.8652 0.044 Uiso 1 1 calc R . . C6 C 0.5581(3) 0.18514(10) 0.7960(3) 0.0370(8) Uani 1 1 d . . . H6 H 0.5265 0.1871 0.8697 0.044 Uiso 1 1 calc R . . C7 C 0.7853(3) 0.09425(11) 0.5616(3) 0.0563(10) Uani 1 1 d . . . H7 H 0.7382 0.1022 0.4708 0.068 Uiso 1 1 calc R . . C8 C 0.8786(3) 0.06358(12) 0.6004(3) 0.0554(10) Uani 1 1 d . . . H8 H 0.9068 0.0464 0.5396 0.067 Uiso 1 1 calc R . . C9 C 0.8588(3) 0.09069(10) 0.7874(3) 0.0365(8) Uani 1 1 d . . . H9 H 0.8693 0.0962 0.8808 0.044 Uiso 1 1 calc R . . C10 C 0.3323(3) 0.24659(11) 0.7301(3) 0.0359(8) Uani 1 1 d . . . C11 C 0.2706(3) 0.20472(11) 0.7059(3) 0.0418(8) Uani 1 1 d . . . H11 H 0.2969 0.1821 0.6574 0.050 Uiso 1 1 calc R . . C12 C 0.1707(3) 0.19619(11) 0.7526(3) 0.0477(9) Uani 1 1 d . . . H12 H 0.1307 0.1679 0.7363 0.057 Uiso 1 1 calc R . . C13 C 0.1866(3) 0.27152(12) 0.8428(3) 0.0466(9) Uani 1 1 d . . . H13 H 0.1572 0.2943 0.8879 0.056 Uiso 1 1 calc R . . C14 C 0.1310(3) 0.22963(13) 0.8232(3) 0.0430(9) Uani 1 1 d . . . C15 C 0.2866(3) 0.28048(11) 0.7961(3) 0.0426(9) Uani 1 1 d . . . H15 H 0.3232 0.3093 0.8092 0.051 Uiso 1 1 calc R . . C16 C -0.1085(4) 0.22648(17) 0.9811(4) 0.0767(13) Uani 1 1 d . . . H16 H -0.1724 0.2385 1.0094 0.092 Uiso 1 1 calc R . . C17 C 0.0248(3) 0.18091(14) 0.9503(4) 0.0650(11) Uani 1 1 d . . . H17 H 0.0740 0.1552 0.9535 0.078 Uiso 1 1 calc R . . C18 C -0.0493(3) 0.25011(14) 0.9033(4) 0.0727(12) Uani 1 1 d . . . H18 H -0.0633 0.2801 0.8718 0.087 Uiso 1 1 calc R . . C19 C 0.4761(3) 0.29817(11) 0.6608(3) 0.0335(7) Uani 1 1 d . . . C20 C 0.6006(3) 0.31085(11) 0.7085(3) 0.0392(8) Uani 1 1 d . . . H20 H 0.6596 0.2909 0.7650 0.047 Uiso 1 1 calc R . . C21 C 0.6388(3) 0.35246(11) 0.6736(3) 0.0383(8) Uani 1 1 d . . . H21 H 0.7232 0.3601 0.7049 0.046 Uiso 1 1 calc RD . . C22 C 0.5515(3) 0.38294(10) 0.5920(2) 0.0297(7) Uani 1 1 d . . . C23 C 0.4261(3) 0.37142(11) 0.5457(2) 0.0322(8) Uani 1 1 d . . . H23 H 0.3670 0.3920 0.4922 0.039 Uiso 1 1 calc R . . C24 C 0.3889(3) 0.32898(10) 0.5797(2) 0.0339(8) Uani 1 1 d . . . H24 H 0.3046 0.3211 0.5477 0.041 Uiso 1 1 calc R . . C25 C 0.5416(3) 0.44904(11) 0.4299(3) 0.0394(8) Uani 1 1 d . . . H25 H 0.4653 0.4431 0.3613 0.047 Uiso 1 1 calc R . . C26 C 0.6228(3) 0.48284(11) 0.4295(3) 0.0423(8) Uani 1 1 d . . . H26 H 0.6115 0.5042 0.3584 0.051 Uiso 1 1 calc R . . C27 C 0.7020(3) 0.44650(11) 0.6172(3) 0.0430(9) Uani 1 1 d . . . H27 H 0.7563 0.4373 0.7036 0.052 Uiso 1 1 calc R . . C28 C 0.8137(3) 0.56523(10) 0.2070(2) 0.0294(7) Uani 1 1 d . . . C29 C 0.7031(3) 0.58821(10) 0.1844(3) 0.0431(9) Uani 1 1 d . . . H30 H 0.6777 0.5959 0.2599 0.052 Uiso 1 1 calc R . . C30 C 0.6289(3) 0.60018(11) 0.0516(3) 0.0540(10) Uani 1 1 d . . . H31 H 0.5542 0.6158 0.0377 0.065 Uiso 1 1 calc R . . C31 C 0.6665(3) 0.58868(10) -0.0603(3) 0.0461(9) Uani 1 1 d . . . H32 H 0.6185 0.5977 -0.1497 0.055 Uiso 1 1 calc R . . C32 C 0.7746(3) 0.56400(10) -0.0410(2) 0.0296(7) Uani 1 1 d . . . C33 C 0.8493(2) 0.55244(9) 0.0933(2) 0.0297(7) Uani 1 1 d . . . H33 H 0.9231 0.5362 0.1072 0.036 Uiso 1 1 calc R . . C34 C 0.8940(3) 0.55262(10) 0.3529(2) 0.0298(7) Uani 1 1 d . . . C35 C 0.8125(3) 0.54938(11) -0.1637(3) 0.0332(8) Uani 1 1 d . . . N1 N 0.4398(2) 0.25376(9) 0.6907(2) 0.0368(7) Uani 1 1 d . . . N2 N 0.5940(2) 0.42529(8) 0.5515(2) 0.0327(6) Uani 1 1 d . . . N3 N 0.7237(2) 0.48123(9) 0.5482(2) 0.0387(6) Uani 1 1 d . . . N4 N 0.0347(3) 0.21956(11) 0.8828(3) 0.0542(8) Uani 1 1 d . . . N5 N -0.0616(3) 0.18305(13) 1.0115(3) 0.0770(10) Uani 1 1 d . . . N6 N 0.7728(2) 0.11155(8) 0.6812(2) 0.0357(7) Uani 1 1 d . . . N7 N 0.9266(2) 0.06140(8) 0.74411(19) 0.0372(7) Uani 1 1 d . . . O1 O 0.77844(17) 0.57355(7) -0.27281(16) 0.0419(6) Uani 1 1 d . . . O2 O 0.87581(17) 0.51343(7) -0.15360(15) 0.0338(5) Uani 1 1 d . . . O3 O 1.00013(18) 0.53602(7) 0.37154(15) 0.0411(6) Uani 1 1 d . . . O4 O 0.85010(17) 0.56104(7) 0.44853(15) 0.0448(6) Uani 1 1 d . . . O1W O 0.9422(3) 0.35988(11) 0.7688(3) 0.1058(10) Uani 1 1 d D . . H1WA H 0.900(3) 0.3700(15) 0.679(2) 0.159 Uiso 1 1 d D . . H1WB H 1.000(3) 0.3460(14) 0.743(4) 0.159 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 Mn1 0.0323(3) 0.0343(3) 0.02086(18) 0.0003(2) 0.00960(17) -0.0015(3) C1 0.0310(19) 0.027(2) 0.0418(17) -0.0015(16) 0.0121(15) 0.0005(16) C2 0.051(2) 0.032(2) 0.0366(17) 0.0073(15) 0.0146(16) 0.0118(18) C3 0.050(2) 0.046(2) 0.0332(17) 0.0007(17) 0.0213(15) 0.0056(19) C4 0.0277(19) 0.032(2) 0.0314(16) -0.0051(16) 0.0063(14) 0.0025(16) C5 0.045(2) 0.028(2) 0.0371(16) 0.0097(15) 0.0142(16) 0.0043(17) C6 0.037(2) 0.039(2) 0.0409(17) 0.0080(16) 0.0203(15) 0.0100(17) C7 0.066(3) 0.066(3) 0.0286(17) -0.0013(18) 0.0049(16) 0.038(2) C8 0.062(3) 0.064(3) 0.0359(18) -0.0060(17) 0.0110(17) 0.026(2) C9 0.040(2) 0.039(2) 0.0286(15) -0.0018(16) 0.0094(15) 0.0037(18) C10 0.036(2) 0.034(2) 0.0360(17) -0.0001(16) 0.0094(16) 0.0025(18) C11 0.038(2) 0.035(2) 0.0527(19) -0.0067(17) 0.0160(16) 0.0039(19) C12 0.042(2) 0.044(3) 0.057(2) -0.0087(18) 0.0164(17) -0.0143(19) C13 0.043(2) 0.051(3) 0.0480(18) -0.0079(18) 0.0187(17) 0.010(2) C14 0.029(2) 0.048(3) 0.0509(19) -0.0077(19) 0.0113(16) -0.0039(19) C15 0.044(2) 0.036(2) 0.0486(18) -0.0056(17) 0.0156(17) -0.0038(18) C16 0.055(3) 0.090(4) 0.098(3) -0.021(3) 0.044(2) -0.011(3) C17 0.046(3) 0.060(3) 0.092(3) -0.002(2) 0.027(2) -0.009(2) C18 0.047(3) 0.081(3) 0.098(3) 0.002(3) 0.033(2) 0.007(3) C19 0.032(2) 0.034(2) 0.0360(17) 0.0000(16) 0.0131(15) 0.0025(18) C20 0.038(2) 0.034(2) 0.0401(17) 0.0044(16) 0.0041(15) 0.0075(18) C21 0.031(2) 0.038(2) 0.0417(17) -0.0058(17) 0.0052(15) -0.0061(18) C22 0.031(2) 0.030(2) 0.0263(15) -0.0022(15) 0.0061(14) 0.0037(18) C23 0.032(2) 0.029(2) 0.0351(16) -0.0011(15) 0.0102(15) 0.0081(16) C24 0.0222(18) 0.038(2) 0.0401(16) -0.0031(16) 0.0077(14) -0.0006(17) C25 0.041(2) 0.036(2) 0.0326(17) -0.0012(16) 0.0011(15) 0.0014(19) C26 0.047(2) 0.038(2) 0.0378(16) 0.0048(16) 0.0081(16) -0.0051(19) C27 0.045(2) 0.042(2) 0.0322(16) 0.0030(17) 0.0003(16) -0.006(2) C28 0.037(2) 0.032(2) 0.0197(14) 0.0014(14) 0.0104(13) 0.0066(17) C29 0.053(2) 0.051(2) 0.0274(16) -0.0027(16) 0.0166(16) 0.0183(19) C30 0.049(2) 0.069(3) 0.0403(17) 0.0005(18) 0.0087(17) 0.040(2) C31 0.056(2) 0.051(2) 0.0241(15) 0.0001(16) 0.0033(15) 0.016(2) C32 0.036(2) 0.028(2) 0.0227(14) 0.0006(14) 0.0062(13) 0.0073(16) C33 0.0279(18) 0.035(2) 0.0261(14) 0.0025(14) 0.0082(13) 0.0084(15) C34 0.039(2) 0.027(2) 0.0239(14) 0.0039(14) 0.0107(15) 0.0000(17) C35 0.037(2) 0.039(2) 0.0216(15) -0.0044(16) 0.0060(14) -0.0072(18) N1 0.0332(18) 0.0302(18) 0.0512(15) 0.0025(13) 0.0197(13) 0.0071(14) N2 0.0322(17) 0.0317(17) 0.0294(13) -0.0040(13) 0.0035(12) -0.0022(14) N3 0.0359(16) 0.0395(19) 0.0368(13) 0.0013(14) 0.0067(12) -0.0083(14) N4 0.045(2) 0.055(2) 0.0658(18) -0.0015(17) 0.0223(16) -0.0022(18) N5 0.056(2) 0.087(3) 0.097(2) -0.006(2) 0.0385(19) -0.017(2) N6 0.0391(18) 0.0380(18) 0.0275(13) -0.0034(13) 0.0073(12) 0.0079(14) N7 0.0374(17) 0.0428(18) 0.0291(13) -0.0042(12) 0.0076(12) 0.0101(14) O1 0.0597(15) 0.0447(15) 0.0237(9) 0.0086(10) 0.0168(9) 0.0090(12) O2 0.0418(13) 0.0364(15) 0.0250(9) 0.0000(9) 0.0135(9) 0.0066(11) O3 0.0375(13) 0.0501(16) 0.0323(10) -0.0033(10) 0.0067(9) 0.0131(12) O4 0.0589(15) 0.0572(15) 0.0239(9) 0.0083(10) 0.0214(10) 0.0149(12) O1W 0.071(2) 0.090(3) 0.171(2) -0.016(2) 0.0596(19) -0.0041(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mn1 O4 2.1065(16) . ? Mn1 O3 2.126(2) 3_766 ? Mn1 O2 2.2402(15) 1_556 ? Mn1 N7 2.243(2) 2_756 ? Mn1 N3 2.256(2) . ? Mn1 O1 2.3530(18) 1_556 ? Mn1 C35 2.614(3) 1_556 ? C1 C6 1.382(3) . ? C1 C2 1.388(3) . ? C1 N1 1.427(3) . ? C2 C3 1.368(3) . ? C2 H2 0.9300 . ? C3 C4 1.376(3) . ? C3 H3 0.9300 . ? C4 C5 1.369(3) . ? C4 N6 1.433(3) . ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.342(4) . ? C7 N6 1.365(3) . ? C7 H7 0.9300 . ? C8 N7 1.382(3) . ? C8 H8 0.9300 . ? C9 N7 1.318(3) . ? C9 N6 1.339(3) . ? C9 H9 0.9300 . ? C10 C15 1.388(4) . ? C10 C11 1.391(4) . ? C10 N1 1.414(3) . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 C14 1.372(4) . ? C12 H12 0.9300 . ? C13 C14 1.361(4) . ? C13 C15 1.388(4) . ? C13 H13 0.9300 . ? C14 N4 1.439(4) . ? C15 H15 0.9300 . ? C16 C18 1.376(4) . ? C16 N5 1.372(4) . ? C16 H16 0.9300 . ? C17 N5 1.320(4) . ? C17 N4 1.346(4) . ? C17 H17 0.9300 . ? C18 N4 1.370(4) . ? C18 H18 0.9300 . ? C19 C20 1.382(4) . ? C19 C24 1.389(3) . ? C19 N1 1.424(3) . ? C20 C21 1.376(4) . ? C20 H20 0.9300 . ? C21 C22 1.386(3) . ? C21 H21 0.9300 . ? C22 C23 1.382(3) . ? C22 N2 1.436(3) . ? C23 C24 1.390(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.350(4) . ? C25 N2 1.371(3) . ? C25 H25 0.9300 . ? C26 N3 1.362(3) . ? C26 H26 0.9300 . ? C27 N3 1.302(3) . ? C27 N2 1.337(3) . ? C27 H27 0.9300 . ? C28 C29 1.372(3) . ? C28 C33 1.392(3) . ? C28 C34 1.508(3) . ? C29 C30 1.379(3) . ? C29 H30 0.9300 . ? C30 C31 1.380(3) . ? C30 H31 0.9300 . ? C31 C32 1.377(3) . ? C31 H32 0.9300 . ? C32 C33 1.390(3) . ? C32 C35 1.507(3) . ? C33 H33 0.9300 . ? C34 O3 1.251(3) . ? C34 O4 1.251(3) . ? C35 O2 1.257(3) . ? C35 O1 1.263(3) . ? C35 Mn1 2.614(3) 1_554 ? N7 Mn1 2.243(2) 2_746 ? O1 Mn1 2.3530(18) 1_554 ? O2 Mn1 2.2402(15) 1_554 ? O3 Mn1 2.126(2) 3_766 ? O1W H1WA 0.933(17) . ? O1W H1WB 0.877(18) . ? 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 Mn1 O3 111.45(7) . 3_766 ? O4 Mn1 O2 149.33(7) . 1_556 ? O3 Mn1 O2 98.78(7) 3_766 1_556 ? O4 Mn1 N7 99.04(8) . 2_756 ? O3 Mn1 N7 91.34(8) 3_766 2_756 ? O2 Mn1 N7 84.88(7) 1_556 2_756 ? O4 Mn1 N3 89.61(8) . . ? O3 Mn1 N3 86.43(8) 3_766 . ? O2 Mn1 N3 87.13(7) 1_556 . ? N7 Mn1 N3 171.29(8) 2_756 . ? O4 Mn1 O1 91.89(7) . 1_556 ? O3 Mn1 O1 155.91(6) 3_766 1_556 ? O2 Mn1 O1 57.53(6) 1_556 1_556 ? N7 Mn1 O1 90.75(8) 2_756 1_556 ? N3 Mn1 O1 87.90(8) . 1_556 ? O4 Mn1 C35 120.76(9) . 1_556 ? O3 Mn1 C35 127.48(9) 3_766 1_556 ? O2 Mn1 C35 28.72(7) 1_556 1_556 ? N7 Mn1 C35 86.17(8) 2_756 1_556 ? N3 Mn1 C35 88.51(8) . 1_556 ? O1 Mn1 C35 28.86(7) 1_556 1_556 ? C6 C1 C2 118.8(3) . . ? C6 C1 N1 121.8(2) . . ? C2 C1 N1 119.4(3) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.3(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.2(3) . . ? C5 C4 N6 121.2(3) . . ? C3 C4 N6 119.5(3) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 N6 106.7(2) . . ? C8 C7 H7 126.7 . . ? N6 C7 H7 126.7 . . ? C7 C8 N7 109.9(3) . . ? C7 C8 H8 125.1 . . ? N7 C8 H8 125.1 . . ? N7 C9 N6 112.1(2) . . ? N7 C9 H9 124.0 . . ? N6 C9 H9 123.9 . . ? C15 C10 C11 118.0(3) . . ? C15 C10 N1 121.5(3) . . ? C11 C10 N1 120.6(3) . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C14 C12 C11 119.6(3) . . ? C14 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C15 120.6(3) . . ? C14 C13 H13 119.7 . . ? C15 C13 H13 119.7 . . ? C13 C14 C12 120.2(3) . . ? C13 C14 N4 120.0(3) . . ? C12 C14 N4 119.7(3) . . ? C10 C15 C13 120.3(3) . . ? C10 C15 H15 119.8 . . ? C13 C15 H15 119.8 . . ? C18 C16 N5 111.7(3) . . ? C18 C16 H16 124.2 . . ? N5 C16 H16 124.2 . . ? N5 C17 N4 113.5(4) . . ? N5 C17 H17 123.2 . . ? N4 C17 H17 123.2 . . ? N4 C18 C16 104.6(4) . . ? N4 C18 H18 127.7 . . ? C16 C18 H18 127.7 . . ? C20 C19 C24 118.5(3) . . ? C20 C19 N1 120.1(3) . . ? C24 C19 N1 121.3(3) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 N2 121.0(3) . . ? C21 C22 N2 119.1(3) . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 120.8(3) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 N2 106.2(3) . . ? C26 C25 H25 126.9 . . ? N2 C25 H25 126.9 . . ? C25 C26 N3 110.2(3) . . ? C25 C26 H26 124.9 . . ? N3 C26 H26 124.9 . . ? N3 C27 N2 113.3(2) . . ? N3 C27 H27 123.3 . . ? N2 C27 H27 123.3 . . ? C29 C28 C33 119.2(2) . . ? C29 C28 C34 120.4(2) . . ? C33 C28 C34 120.3(3) . . ? C28 C29 C30 121.2(2) . . ? C28 C29 H30 119.4 . . ? C30 C29 H30 119.4 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 H31 120.3 . . ? C31 C30 H31 120.3 . . ? C32 C31 C30 120.6(2) . . ? C32 C31 H32 119.7 . . ? C30 C31 H32 119.7 . . ? C31 C32 C33 119.6(2) . . ? C31 C32 C35 120.7(2) . . ? C33 C32 C35 119.7(3) . . ? C32 C33 C28 120.0(3) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? O3 C34 O4 124.4(2) . . ? O3 C34 C28 118.8(2) . . ? O4 C34 C28 116.8(3) . . ? O2 C35 O1 122.8(2) . . ? O2 C35 C32 118.6(3) . . ? O1 C35 C32 118.6(3) . . ? O2 C35 Mn1 58.91(13) . 1_554 ? O1 C35 Mn1 64.04(13) . 1_554 ? C32 C35 Mn1 175.31(19) . 1_554 ? C10 N1 C19 122.0(3) . . ? C10 N1 C1 121.1(3) . . ? C19 N1 C1 116.8(2) . . ? C27 N2 C25 105.6(2) . . ? C27 N2 C22 126.4(2) . . ? C25 N2 C22 127.4(2) . . ? C27 N3 C26 104.6(2) . . ? C27 N3 Mn1 120.81(19) . . ? C26 N3 Mn1 134.6(2) . . ? C17 N4 C18 107.0(3) . . ? C17 N4 C14 126.0(3) . . ? C18 N4 C14 126.1(3) . . ? C17 N5 C16 103.2(3) . . ? C9 N6 C7 106.7(2) . . ? C9 N6 C4 128.3(2) . . ? C7 N6 C4 124.9(2) . . ? C9 N7 C8 104.6(2) . . ? C9 N7 Mn1 130.32(18) . 2_746 ? C8 N7 Mn1 124.27(19) . 2_746 ? C35 O1 Mn1 87.10(16) . 1_554 ? C35 O2 Mn1 92.37(15) . 1_554 ? C34 O3 Mn1 145.6(2) . 3_766 ? C34 O4 Mn1 123.88(18) . . ? H1WA O1W H1WB 93(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.1(4) . . . . ? N1 C1 C2 C3 177.2(3) . . . . ? C1 C2 C3 C4 2.0(4) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C2 C3 C4 N6 177.7(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? N6 C4 C5 C6 -179.1(3) . . . . ? C4 C5 C6 C1 0.9(5) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? N1 C1 C6 C5 -178.6(3) . . . . ? N6 C7 C8 N7 -0.5(4) . . . . ? C15 C10 C11 C12 -3.4(4) . . . . ? N1 C10 C11 C12 175.4(2) . . . . ? C10 C11 C12 C14 0.5(4) . . . . ? C15 C13 C14 C12 -2.2(4) . . . . ? C15 C13 C14 N4 174.5(3) . . . . ? C11 C12 C14 C13 2.3(4) . . . . ? C11 C12 C14 N4 -174.4(3) . . . . ? C11 C10 C15 C13 3.5(4) . . . . ? N1 C10 C15 C13 -175.3(2) . . . . ? C14 C13 C15 C10 -0.7(4) . . . . ? N5 C16 C18 N4 1.5(4) . . . . ? C24 C19 C20 C21 -1.8(4) . . . . ? N1 C19 C20 C21 175.9(2) . . . . ? C19 C20 C21 C22 1.4(4) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C20 C21 C22 N2 -177.2(2) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? N2 C22 C23 C24 176.0(2) . . . . ? C20 C19 C24 C23 0.7(4) . . . . ? N1 C19 C24 C23 -177.0(2) . . . . ? C22 C23 C24 C19 0.7(4) . . . . ? N2 C25 C26 N3 -0.7(3) . . . . ? C33 C28 C29 C30 -2.2(5) . . . . ? C34 C28 C29 C30 179.7(3) . . . . ? C28 C29 C30 C31 0.2(5) . . . . ? C29 C30 C31 C32 2.5(5) . . . . ? C30 C31 C32 C33 -3.0(5) . . . . ? C30 C31 C32 C35 176.9(3) . . . . ? C31 C32 C33 C28 1.0(4) . . . . ? C35 C32 C33 C28 -179.0(3) . . . . ? C29 C28 C33 C32 1.6(4) . . . . ? C34 C28 C33 C32 179.7(3) . . . . ? C29 C28 C34 O3 -172.6(3) . . . . ? C33 C28 C34 O3 9.4(4) . . . . ? C29 C28 C34 O4 5.2(4) . . . . ? C33 C28 C34 O4 -172.8(3) . . . . ? C31 C32 C35 O2 -151.1(3) . . . . ? C33 C32 C35 O2 28.9(4) . . . . ? C31 C32 C35 O1 28.3(4) . . . . ? C33 C32 C35 O1 -151.7(3) . . . . ? C31 C32 C35 Mn1 152(3) . . . 1_554 ? C33 C32 C35 Mn1 -28(3) . . . 1_554 ? C15 C10 N1 C19 -26.9(4) . . . . ? C11 C10 N1 C19 154.4(3) . . . . ? C15 C10 N1 C1 148.2(3) . . . . ? C11 C10 N1 C1 -30.6(4) . . . . ? C20 C19 N1 C10 138.2(3) . . . . ? C24 C19 N1 C10 -44.2(4) . . . . ? C20 C19 N1 C1 -37.1(3) . . . . ? C24 C19 N1 C1 140.6(2) . . . . ? C6 C1 N1 C10 -42.8(4) . . . . ? C2 C1 N1 C10 138.8(3) . . . . ? C6 C1 N1 C19 132.5(3) . . . . ? C2 C1 N1 C19 -45.8(3) . . . . ? N3 C27 N2 C25 -0.6(3) . . . . ? N3 C27 N2 C22 171.7(2) . . . . ? C26 C25 N2 C27 0.8(3) . . . . ? C26 C25 N2 C22 -171.4(2) . . . . ? C23 C22 N2 C27 159.3(3) . . . . ? C21 C22 N2 C27 -23.6(4) . . . . ? C23 C22 N2 C25 -30.1(4) . . . . ? C21 C22 N2 C25 147.1(3) . . . . ? N2 C27 N3 C26 0.1(3) . . . . ? N2 C27 N3 Mn1 178.60(17) . . . . ? C25 C26 N3 C27 0.4(3) . . . . ? C25 C26 N3 Mn1 -177.78(19) . . . . ? O4 Mn1 N3 C27 174.4(2) . . . . ? O3 Mn1 N3 C27 62.9(2) 3_766 . . . ? O2 Mn1 N3 C27 -36.1(2) 1_556 . . . ? N7 Mn1 N3 C27 -12.5(7) 2_756 . . . ? O1 Mn1 N3 C27 -93.7(2) 1_556 . . . ? C35 Mn1 N3 C27 -64.8(2) 1_556 . . . ? O4 Mn1 N3 C26 -7.6(3) . . . . ? O3 Mn1 N3 C26 -119.2(3) 3_766 . . . ? O2 Mn1 N3 C26 141.8(3) 1_556 . . . ? N7 Mn1 N3 C26 165.5(5) 2_756 . . . ? O1 Mn1 N3 C26 84.3(3) 1_556 . . . ? C35 Mn1 N3 C26 113.1(3) 1_556 . . . ? N5 C17 N4 C18 1.5(4) . . . . ? N5 C17 N4 C14 171.0(3) . . . . ? C16 C18 N4 C17 -1.7(4) . . . . ? C16 C18 N4 C14 -171.2(3) . . . . ? C13 C14 N4 C17 -135.4(3) . . . . ? C12 C14 N4 C17 41.3(4) . . . . ? C13 C14 N4 C18 32.1(4) . . . . ? C12 C14 N4 C18 -151.2(3) . . . . ? N4 C17 N5 C16 -0.6(4) . . . . ? C18 C16 N5 C17 -0.6(4) . . . . ? N7 C9 N6 C7 0.6(4) . . . . ? N7 C9 N6 C4 -175.0(3) . . . . ? C8 C7 N6 C9 -0.1(4) . . . . ? C8 C7 N6 C4 175.8(3) . . . . ? C5 C4 N6 C9 -33.6(5) . . . . ? C3 C4 N6 C9 147.3(3) . . . . ? C5 C4 N6 C7 151.5(3) . . . . ? C3 C4 N6 C7 -27.6(4) . . . . ? N6 C9 N7 C8 -0.9(3) . . . . ? N6 C9 N7 Mn1 168.94(19) . . . 2_746 ? C7 C8 N7 C9 0.8(4) . . . . ? C7 C8 N7 Mn1 -169.8(2) . . . 2_746 ? O2 C35 O1 Mn1 -5.0(3) . . . 1_554 ? C32 C35 O1 Mn1 175.7(2) . . . 1_554 ? O1 C35 O2 Mn1 5.2(3) . . . 1_554 ? C32 C35 O2 Mn1 -175.4(2) . . . 1_554 ? O4 C34 O3 Mn1 101.1(3) . . . 3_766 ? C28 C34 O3 Mn1 -81.3(4) . . . 3_766 ? O3 C34 O4 Mn1 -29.7(4) . . . . ? C28 C34 O4 Mn1 152.65(18) . . . . ? O3 Mn1 O4 C34 -10.8(2) 3_766 . . . ? O2 Mn1 O4 C34 179.45(19) 1_556 . . . ? N7 Mn1 O4 C34 84.2(2) 2_756 . . . ? N3 Mn1 O4 C34 -96.8(2) . . . . ? O1 Mn1 O4 C34 175.3(2) 1_556 . . . ? C35 Mn1 O4 C34 175.1(2) 1_556 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.225 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.046 data_5 _database_code_depnum_ccdc_archive 'CCDC 826246' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C63 H52 O6 N14 Cu2),2(C8 H4 O4), 3(C H4 O), 8(H2 O)' _chemical_formula_sum 'C145 H140 Cu4 N28 O31' _chemical_formula_weight 3025.01 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8890(13) _cell_length_b 15.7580(10) _cell_length_c 21.9600(12) _cell_angle_alpha 91.108(5) _cell_angle_beta 107.134(6) _cell_angle_gamma 115.870(7) _cell_volume 4071.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14596 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 25.4 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1570 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27063 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.1381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 25.35 _reflns_number_total 14596 _reflns_number_gt 6961 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0920P)^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 14596 _refine_ls_number_parameters 983 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.888 _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 Cu1 Cu 0.59964(4) 0.50116(3) 0.35581(3) 0.04185(18) Uani 1 1 d . . . Cu2 Cu -0.29634(4) -0.69969(3) 0.13957(3) 0.04036(18) Uani 1 1 d . . . C1 C 0.1819(4) -0.2154(3) 0.3967(2) 0.0500(13) Uani 1 1 d . . . C2 C 0.0967(4) -0.2975(3) 0.4045(3) 0.0566(14) Uani 1 1 d . . . H2 H 0.0774 -0.2981 0.4417 0.068 Uiso 1 1 calc R . . C3 C 0.0392(4) -0.3790(3) 0.3578(3) 0.0570(14) Uani 1 1 d . . . H3 H -0.0155 -0.4347 0.3648 0.068 Uiso 1 1 calc R . . C4 C 0.0621(4) -0.3787(3) 0.3014(2) 0.0474(12) Uani 1 1 d . . . C5 C 0.1470(5) -0.2968(4) 0.2922(3) 0.0673(16) Uani 1 1 d . . . H5 H 0.1641 -0.2962 0.2543 0.081 Uiso 1 1 calc R . . C6 C 0.2061(5) -0.2161(3) 0.3396(3) 0.0637(15) Uani 1 1 d . . . H6 H 0.2630 -0.1613 0.3332 0.076 Uiso 1 1 calc R . . C7 C 0.0407(5) -0.4947(5) 0.2132(3) 0.090(2) Uani 1 1 d . . . H7 H 0.1143 -0.4657 0.2120 0.108 Uiso 1 1 calc R . . C8 C -0.0463(5) -0.5757(4) 0.1757(3) 0.0764(18) Uani 1 1 d . . . H8 H -0.0424 -0.6126 0.1438 0.092 Uiso 1 1 calc R . . C9 C -0.1101(4) -0.5269(3) 0.2380(2) 0.0457(12) Uani 1 1 d . . . H9 H -0.1584 -0.5226 0.2581 0.055 Uiso 1 1 calc R . . C10 C 0.2489(4) -0.1409(3) 0.5111(2) 0.0465(12) Uani 1 1 d . . . C11 C 0.2933(5) -0.1953(3) 0.5432(3) 0.0620(15) Uani 1 1 d . . . H11 H 0.3185 -0.2288 0.5220 0.074 Uiso 1 1 calc R . . C12 C 0.3014(5) -0.2015(4) 0.6074(3) 0.0638(15) Uani 1 1 d . . . H12 H 0.3319 -0.2390 0.6290 0.077 Uiso 1 1 calc R . . C13 C 0.2643(4) -0.1524(3) 0.6387(2) 0.0472(12) Uani 1 1 d . . . C14 C 0.2188(5) -0.0988(4) 0.6057(3) 0.0737(17) Uani 1 1 d . . . H14 H 0.1934 -0.0651 0.6266 0.088 Uiso 1 1 calc R . . C15 C 0.2101(5) -0.0937(4) 0.5427(3) 0.0723(17) Uani 1 1 d . . . H15 H 0.1773 -0.0577 0.5209 0.087 Uiso 1 1 calc R . . C16 C 0.2637(4) -0.2317(3) 0.7349(2) 0.0495(13) Uani 1 1 d . . . H16 H 0.2421 -0.2921 0.7136 0.059 Uiso 1 1 calc R . . C17 C 0.3169(6) -0.1162(4) 0.8090(3) 0.0785(19) Uani 1 1 d . . . H17 H 0.3386 -0.0808 0.8494 0.094 Uiso 1 1 calc R . . C18 C 0.3111(6) -0.0823(4) 0.7535(3) 0.085(2) Uani 1 1 d . . . H18 H 0.3281 -0.0194 0.7486 0.102 Uiso 1 1 calc R . . C19 C 0.2787(4) -0.0383(3) 0.4294(2) 0.0497(13) Uani 1 1 d . . . C20 C 0.3770(4) 0.0357(3) 0.4696(3) 0.0609(15) Uani 1 1 d . . . H20 H 0.4222 0.0241 0.5056 0.073 Uiso 1 1 calc R . . C21 C 0.4102(5) 0.1300(3) 0.4566(3) 0.0620(15) Uani 1 1 d . . . H21 H 0.4751 0.1810 0.4850 0.074 Uiso 1 1 calc R . . C22 C 0.3468(4) 0.1453(3) 0.4025(3) 0.0514(13) Uani 1 1 d . . . C23 C 0.2479(4) 0.0713(3) 0.3617(3) 0.0628(15) Uani 1 1 d . . . H23 H 0.2037 0.0831 0.3254 0.075 Uiso 1 1 calc R . . C24 C 0.2143(5) -0.0210(3) 0.3750(3) 0.0607(15) Uani 1 1 d . . . H24 H 0.1481 -0.0714 0.3470 0.073 Uiso 1 1 calc R . . C25 C 0.4804(4) 0.3071(3) 0.3891(2) 0.0489(13) Uani 1 1 d . . . H25 H 0.5446 0.2979 0.3994 0.059 Uiso 1 1 calc R . . C26 C 0.3051(5) 0.2799(4) 0.3691(4) 0.083(2) Uani 1 1 d . . . H26 H 0.2277 0.2506 0.3629 0.100 Uiso 1 1 calc R . . C27 C 0.3687(5) 0.3684(4) 0.3608(3) 0.080(2) Uani 1 1 d . . . H27 H 0.3415 0.4121 0.3483 0.096 Uiso 1 1 calc R . . C28 C 0.9263(4) 0.7671(3) 0.1123(2) 0.0517(13) Uani 1 1 d . . . C29 C 0.8618(4) 0.6721(3) 0.1167(3) 0.0524(13) Uani 1 1 d . . . H29 H 0.8401 0.6238 0.0830 0.063 Uiso 1 1 calc R . . C30 C 0.8299(4) 0.6487(3) 0.1698(2) 0.0525(13) Uani 1 1 d . . . H30 H 0.7867 0.5848 0.1717 0.063 Uiso 1 1 calc R . . C31 C 0.8605(4) 0.7177(3) 0.2198(2) 0.0451(12) Uani 1 1 d . . . C32 C 0.9242(4) 0.8131(3) 0.2175(3) 0.0594(14) Uani 1 1 d . . . H32 H 0.9439 0.8609 0.2511 0.071 Uiso 1 1 calc R . . C33 C 0.9577(4) 0.8359(3) 0.1643(3) 0.0607(15) Uani 1 1 d . . . H33 H 1.0031 0.8997 0.1633 0.073 Uiso 1 1 calc R . . C34 C 0.8706(4) 0.7416(3) 0.3364(3) 0.0599(15) Uani 1 1 d . . . H34 H 0.9344 0.8010 0.3519 0.072 Uiso 1 1 calc R . . C35 C 0.8083(4) 0.6884(3) 0.3701(3) 0.0590(14) Uani 1 1 d . . . H35 H 0.8230 0.7045 0.4140 0.071 Uiso 1 1 calc R . . C36 C 0.7312(4) 0.6104(3) 0.2737(2) 0.0466(12) Uani 1 1 d . . . H36 H 0.6829 0.5632 0.2374 0.056 Uiso 1 1 calc R . . C37 C 0.8801(4) 0.7325(3) -0.0054(3) 0.0520(13) Uani 1 1 d . . . C38 C 0.7701(4) 0.7224(4) -0.0291(3) 0.0611(14) Uani 1 1 d . . . H38 H 0.7466 0.7546 -0.0056 0.073 Uiso 1 1 calc R . . C39 C 0.6970(4) 0.6644(4) -0.0874(3) 0.0559(14) Uani 1 1 d . . . H39 H 0.6239 0.6579 -0.1038 0.067 Uiso 1 1 calc R . . C40 C 0.7316(4) 0.6159(3) -0.1217(2) 0.0496(13) Uani 1 1 d . . . C41 C 0.8413(4) 0.6264(4) -0.0988(3) 0.0600(14) Uani 1 1 d . . . H41 H 0.8654 0.5945 -0.1221 0.072 Uiso 1 1 calc R . . C42 C 0.9142(4) 0.6863(4) -0.0398(3) 0.0581(14) Uani 1 1 d . . . H42 H 0.9882 0.6947 -0.0237 0.070 Uiso 1 1 calc R . . C43 C 0.6337(5) 0.4629(4) -0.2012(3) 0.0726(18) Uani 1 1 d . . . H43 H 0.6701 0.4294 -0.1792 0.087 Uiso 1 1 calc R . . C44 C 0.5492(5) 0.4307(3) -0.2591(3) 0.0645(16) Uani 1 1 d . . . H44 H 0.5171 0.3702 -0.2836 0.077 Uiso 1 1 calc R . . C45 C 0.5839(4) 0.5736(3) -0.2282(2) 0.0523(13) Uani 1 1 d . . . H45 H 0.5814 0.6316 -0.2270 0.063 Uiso 1 1 calc R . . C46 C 1.0601(4) 0.8688(3) 0.0591(2) 0.0491(12) Uani 1 1 d . . . C47 C 1.0625(4) 0.9228(3) 0.0114(3) 0.0549(13) Uani 1 1 d . . . H47 H 0.9951 0.9099 -0.0213 0.066 Uiso 1 1 calc R . . C48 C 1.1637(4) 0.9968(3) 0.0109(3) 0.0557(14) Uani 1 1 d . . . H48 H 1.1641 1.0338 -0.0216 0.067 Uiso 1 1 calc R . . C49 C 1.2628(4) 1.0153(3) 0.0582(2) 0.0492(13) Uani 1 1 d . . . C50 C 1.2626(4) 0.9607(3) 0.1063(3) 0.0609(15) Uani 1 1 d . . . H50 H 1.3303 0.9725 0.1384 0.073 Uiso 1 1 calc R . . C51 C 1.1609(4) 0.8883(4) 0.1063(3) 0.0648(16) Uani 1 1 d . . . H51 H 1.1603 0.8517 0.1391 0.078 Uiso 1 1 calc R . . C52 C 1.3929(4) 1.1176(4) 0.0015(3) 0.0659(16) Uani 1 1 d . . . H52 H 1.3442 1.0931 -0.0411 0.079 Uiso 1 1 calc R . . C53 C 1.4626(4) 1.1440(3) 0.1074(2) 0.0485(12) Uani 1 1 d . . . H53 H 1.4680 1.1397 0.1503 0.058 Uiso 1 1 calc R . . C54 C 1.5012(4) 1.1877(4) 0.0216(3) 0.0636(15) Uani 1 1 d . . . H54 H 1.5403 1.2204 -0.0053 0.076 Uiso 1 1 calc R . . C55 C 0.8941(4) 0.4796(3) 0.4558(2) 0.0436(12) Uani 1 1 d . . . C56 C 0.9443(4) 0.5501(3) 0.5104(2) 0.0527(13) Uani 1 1 d . . . H56 H 0.9067 0.5838 0.5175 0.063 Uiso 1 1 calc R . . C57 C 1.0496(4) 0.5704(3) 0.5543(2) 0.0515(13) Uani 1 1 d . . . H57 H 1.0826 0.6178 0.5905 0.062 Uiso 1 1 calc R . . C58 C 0.7818(4) 0.4612(3) 0.4062(3) 0.0476(13) Uani 1 1 d . . . C59 C 0.1049(5) -0.4249(4) 0.0393(3) 0.0576(14) Uani 1 1 d . . . C60 C 0.0958(5) -0.4722(4) -0.0177(3) 0.0698(16) Uani 1 1 d . . . H60 H 0.1594 -0.4530 -0.0304 0.084 Uiso 1 1 calc R . . C61 C -0.0069(5) -0.5478(4) -0.0562(3) 0.0691(16) Uani 1 1 d . . . H61 H -0.0105 -0.5803 -0.0933 0.083 Uiso 1 1 calc R . . C62 C 0.2152(5) -0.3452(4) 0.0823(3) 0.0740(17) Uani 1 1 d . . . C63 C -0.4415(4) -0.5338(3) 0.0475(2) 0.0409(11) Uani 1 1 d . . . C64 C -0.4525(4) -0.5547(3) -0.0161(2) 0.0478(12) Uani 1 1 d . . . H64 H -0.4204 -0.5910 -0.0272 0.057 Uiso 1 1 calc R . . C65 C -0.5114(4) -0.5214(3) -0.0634(2) 0.0458(12) Uani 1 1 d . . . H65 H -0.5195 -0.5363 -0.1064 0.055 Uiso 1 1 calc R . . C66 C -0.3843(4) -0.5760(3) 0.0994(2) 0.0411(12) Uani 1 1 d . . . C67 C 0.0007(8) 0.0223(6) 0.4404(6) 0.117(3) Uani 1 1 d D . . C68 C -0.0817(8) -0.0634(6) 0.4464(7) 0.131(4) Uani 1 1 d . . . H68 H -0.1369 -0.1064 0.4095 0.157 Uiso 1 1 calc R . . C69 C 0.0834(10) 0.0865(7) 0.4928(7) 0.133(4) Uani 1 1 d . . . H69 H 0.1393 0.1439 0.4884 0.159 Uiso 1 1 calc R . . C70 C -0.0050(9) 0.0452(8) 0.3707(7) 0.132(4) Uani 1 1 d D . . C71 C 0.4298(13) 0.6574(13) 0.4186(8) 0.107(5) Uani 0.50 1 d P . . C72 C 0.608(2) -0.2028(19) 0.3721(12) 0.188(11) Uani 0.50 1 d P . . C73 C -0.2299(8) -0.8263(5) 0.0497(4) 0.114(3) Uani 1 1 d . . . H73A H -0.1971 -0.8223 0.0163 0.171 Uiso 1 1 calc R . . H73B H -0.3064 -0.8772 0.0350 0.171 Uiso 1 1 calc R . . H73C H -0.1858 -0.8389 0.0877 0.171 Uiso 1 1 calc R . . C74 C 0.0541(17) 0.3331(17) 0.3259(12) 0.151(8) Uani 0.50 1 d P . . O1 O -0.3258(3) -0.6099(2) 0.08403(15) 0.0447(8) Uani 1 1 d . . . O2 O -0.4002(3) -0.5759(2) 0.15262(16) 0.0513(8) Uani 1 1 d . . . O3 O 0.2293(4) -0.3311(3) 0.1411(2) 0.0961(14) Uani 1 1 d . . . O4 O 0.2887(4) -0.2966(3) 0.0568(2) 0.0917(14) Uani 1 1 d . . . O5 O 0.7557(3) 0.4186(2) 0.35037(19) 0.0655(10) Uani 1 1 d . . . O6 O 0.7204(3) 0.4894(2) 0.42429(16) 0.0531(9) Uani 1 1 d . . . O7 O -0.0649(7) -0.0221(5) 0.3253(4) 0.162(3) Uani 1 1 d . . . O8 O 0.0512(6) 0.1305(5) 0.3673(4) 0.151(3) Uani 1 1 d . . . O7W O 0.6477(13) -0.1635(19) 0.1596(7) 0.263(12) Uani 0.50 1 d P . . O12 O 0.4929(18) -0.2100(13) 0.3474(9) 0.196(7) Uani 0.50 1 d P . . O13 O 0.0586(14) 0.2976(9) 0.3827(8) 0.165(5) Uani 0.50 1 d P . . O14 O 0.3181(15) 0.5968(12) 0.4150(11) 0.221(9) Uani 0.50 1 d P . . N1 N 0.2441(4) -0.1321(2) 0.44563(19) 0.0559(11) Uani 1 1 d . . . N2 N 0.3786(3) 0.2413(3) 0.3889(2) 0.0524(11) Uani 1 1 d . . . N3 N 0.4788(3) 0.3864(2) 0.37311(19) 0.0465(10) Uani 1 1 d . . . N4 N 0.0004(3) -0.4626(3) 0.2535(2) 0.0481(10) Uani 1 1 d . . . N5 N -0.1412(3) -0.5961(3) 0.19118(19) 0.0456(10) Uani 1 1 d . . . N6 N 0.2757(4) -0.1560(3) 0.7052(2) 0.0529(11) Uani 1 1 d . . . N7 N 0.2857(3) -0.2115(3) 0.7967(2) 0.0479(10) Uani 1 1 d . . . N8 N 0.9553(3) 0.7915(3) 0.0572(2) 0.0629(12) Uani 1 1 d . . . N9 N 0.8223(3) 0.6918(2) 0.27442(19) 0.0465(10) Uani 1 1 d . . . N10 N 0.7197(3) 0.6067(2) 0.33101(19) 0.0455(10) Uani 1 1 d . . . N11 N 0.6552(3) 0.5535(3) -0.18147(19) 0.0485(10) Uani 1 1 d . . . N12 N 0.5182(3) 0.4997(3) -0.27594(19) 0.0478(10) Uani 1 1 d . . . N13 N 1.3688(3) 1.0898(3) 0.05610(19) 0.0523(11) Uani 1 1 d . . . N14 N 1.5454(3) 1.2036(2) 0.08847(19) 0.0485(10) Uani 1 1 d . . . O1W O 0.5891(4) 0.6067(3) 0.4241(3) 0.1064(16) Uani 1 1 d . . . O2W O 0.3807(10) -0.1758(8) 0.2303(5) 0.117(4) Uani 0.50 1 d PD . . O3W O 0.4668(7) -0.1207(7) 0.1255(4) 0.219(4) Uani 1 1 d . . . O4W O 0.4080(11) 0.1427(7) 0.2486(5) 0.135(5) Uani 0.50 1 d P . . O5W O -0.2829(12) -0.1280(10) 0.2899(7) 0.165(5) Uiso 0.50 1 d P . . O6W O 0.5623(4) 0.3172(3) 0.2481(2) 0.0887(13) Uani 1 1 d D . . O9 O -0.2302(3) -0.7404(2) 0.06425(17) 0.0597(9) Uani 1 1 d . . . H6WA H 0.575(5) 0.350(4) 0.218(2) 0.090 Uiso 1 1 d D . . H2WA H 0.423(5) -0.156(4) 0.208(3) 0.090 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 Cu1 0.0361(3) 0.0375(3) 0.0417(4) 0.0140(2) 0.0100(3) 0.0100(2) Cu2 0.0321(3) 0.0359(3) 0.0407(4) 0.0110(2) 0.0082(2) 0.0074(2) C1 0.054(3) 0.033(2) 0.050(3) 0.014(2) 0.016(3) 0.010(2) C2 0.059(3) 0.052(3) 0.050(3) 0.017(3) 0.025(3) 0.014(3) C3 0.057(3) 0.039(3) 0.051(3) 0.011(2) 0.021(3) 0.000(2) C4 0.039(3) 0.044(3) 0.046(3) 0.009(2) 0.010(2) 0.010(2) C5 0.068(4) 0.059(3) 0.053(3) 0.010(3) 0.034(3) 0.001(3) C6 0.070(4) 0.043(3) 0.052(4) 0.007(3) 0.030(3) -0.003(2) C7 0.037(3) 0.108(5) 0.086(5) -0.037(4) 0.029(3) -0.004(3) C8 0.046(3) 0.084(4) 0.077(4) -0.023(3) 0.028(3) 0.007(3) C9 0.035(3) 0.039(3) 0.059(3) 0.011(2) 0.018(2) 0.012(2) C10 0.055(3) 0.033(2) 0.044(3) 0.011(2) 0.017(2) 0.013(2) C11 0.088(4) 0.054(3) 0.051(4) 0.011(3) 0.027(3) 0.036(3) C12 0.075(4) 0.066(3) 0.059(4) 0.023(3) 0.019(3) 0.043(3) C13 0.056(3) 0.046(3) 0.046(3) 0.016(2) 0.022(2) 0.025(2) C14 0.098(5) 0.094(4) 0.069(4) 0.039(3) 0.042(4) 0.069(4) C15 0.108(5) 0.085(4) 0.062(4) 0.047(3) 0.044(4) 0.067(4) C16 0.059(3) 0.039(3) 0.042(3) 0.011(2) 0.013(3) 0.017(2) C17 0.123(6) 0.061(4) 0.065(4) 0.023(3) 0.042(4) 0.047(4) C18 0.149(6) 0.057(4) 0.074(5) 0.031(3) 0.054(4) 0.058(4) C19 0.063(3) 0.032(2) 0.051(3) 0.015(2) 0.024(3) 0.015(2) C20 0.060(3) 0.042(3) 0.060(4) 0.016(2) 0.008(3) 0.013(2) C21 0.059(3) 0.045(3) 0.059(4) 0.010(2) 0.012(3) 0.008(2) C22 0.053(3) 0.041(3) 0.063(4) 0.022(2) 0.027(3) 0.018(2) C23 0.053(3) 0.052(3) 0.063(4) 0.020(3) 0.008(3) 0.014(3) C24 0.064(3) 0.038(3) 0.054(3) 0.014(2) 0.007(3) 0.009(2) C25 0.040(3) 0.043(3) 0.053(3) 0.014(2) 0.015(2) 0.010(2) C26 0.061(4) 0.065(4) 0.142(6) 0.042(4) 0.052(4) 0.032(3) C27 0.059(4) 0.065(4) 0.131(6) 0.049(4) 0.047(4) 0.033(3) C28 0.034(3) 0.053(3) 0.046(3) 0.005(2) 0.013(2) 0.002(2) C29 0.043(3) 0.043(3) 0.053(3) 0.000(2) 0.015(2) 0.005(2) C30 0.050(3) 0.040(3) 0.049(3) 0.008(2) 0.016(3) 0.005(2) C31 0.039(3) 0.042(3) 0.044(3) 0.008(2) 0.016(2) 0.008(2) C32 0.054(3) 0.045(3) 0.059(4) 0.002(2) 0.024(3) 0.002(2) C33 0.052(3) 0.047(3) 0.060(4) 0.013(3) 0.024(3) -0.001(2) C34 0.056(3) 0.044(3) 0.048(3) 0.000(2) 0.019(3) -0.005(2) C35 0.055(3) 0.052(3) 0.049(3) 0.001(2) 0.020(3) 0.006(3) C36 0.038(3) 0.037(2) 0.045(3) 0.007(2) 0.010(2) 0.002(2) C37 0.036(3) 0.050(3) 0.046(3) 0.009(2) 0.016(3) -0.001(2) C38 0.040(3) 0.062(3) 0.067(4) 0.008(3) 0.024(3) 0.008(2) C39 0.030(3) 0.060(3) 0.060(4) 0.005(3) 0.008(3) 0.010(2) C40 0.033(3) 0.046(3) 0.052(3) 0.015(2) 0.006(3) 0.008(2) C41 0.044(3) 0.069(3) 0.063(4) 0.011(3) 0.013(3) 0.026(3) C42 0.035(3) 0.070(3) 0.051(4) 0.005(3) 0.005(3) 0.014(3) C43 0.070(4) 0.062(4) 0.071(4) 0.014(3) -0.004(3) 0.035(3) C44 0.073(4) 0.046(3) 0.057(4) 0.008(2) -0.003(3) 0.028(3) C45 0.042(3) 0.054(3) 0.052(3) 0.019(3) 0.013(3) 0.016(2) C46 0.033(3) 0.055(3) 0.043(3) 0.006(2) 0.015(2) 0.005(2) C47 0.031(3) 0.058(3) 0.057(3) 0.009(3) 0.010(2) 0.009(2) C48 0.043(3) 0.053(3) 0.058(3) 0.015(2) 0.020(3) 0.009(2) C49 0.035(3) 0.046(3) 0.049(3) 0.004(2) 0.013(2) 0.004(2) C50 0.036(3) 0.063(3) 0.053(3) 0.014(3) 0.009(2) -0.001(2) C51 0.049(3) 0.059(3) 0.056(4) 0.018(3) 0.010(3) 0.004(3) C52 0.051(3) 0.071(3) 0.042(3) 0.006(3) 0.014(3) -0.001(3) C53 0.035(3) 0.048(3) 0.040(3) 0.007(2) 0.012(2) 0.000(2) C54 0.046(3) 0.066(3) 0.046(3) 0.008(3) 0.016(3) -0.003(3) C55 0.041(3) 0.043(3) 0.039(3) 0.019(2) 0.010(2) 0.015(2) C56 0.051(3) 0.045(3) 0.057(3) 0.017(2) 0.011(3) 0.022(2) C57 0.046(3) 0.044(3) 0.046(3) 0.004(2) 0.005(3) 0.011(2) C58 0.045(3) 0.043(3) 0.050(4) 0.024(2) 0.015(3) 0.016(2) C59 0.061(4) 0.054(3) 0.069(4) 0.029(3) 0.029(3) 0.030(3) C60 0.072(4) 0.061(3) 0.090(5) 0.026(3) 0.044(4) 0.031(3) C61 0.072(4) 0.068(4) 0.073(4) 0.017(3) 0.035(3) 0.031(3) C62 0.071(4) 0.086(4) 0.067(5) 0.033(4) 0.023(4) 0.037(4) C63 0.030(2) 0.043(2) 0.038(3) 0.010(2) 0.009(2) 0.008(2) C64 0.055(3) 0.055(3) 0.045(3) 0.013(2) 0.022(2) 0.031(2) C65 0.058(3) 0.050(3) 0.036(3) 0.012(2) 0.017(2) 0.029(2) C66 0.029(2) 0.030(2) 0.046(3) 0.007(2) 0.006(2) 0.0021(19) C67 0.113(7) 0.065(5) 0.213(11) 0.023(6) 0.100(8) 0.045(5) C68 0.115(7) 0.063(5) 0.230(12) -0.001(6) 0.098(8) 0.032(5) C69 0.142(9) 0.073(6) 0.215(12) 0.034(7) 0.112(9) 0.044(6) C70 0.136(8) 0.099(7) 0.234(14) 0.059(9) 0.135(9) 0.070(7) C71 0.068(9) 0.159(14) 0.111(12) -0.001(10) 0.016(9) 0.078(10) C72 0.114(16) 0.20(2) 0.17(2) 0.003(17) 0.086(16) -0.020(16) C73 0.150(7) 0.089(5) 0.137(7) 0.016(5) 0.085(6) 0.062(5) C74 0.126(15) 0.21(2) 0.156(19) 0.088(17) 0.051(14) 0.105(15) O1 0.0402(18) 0.0457(17) 0.047(2) 0.0186(14) 0.0155(16) 0.0178(15) O2 0.056(2) 0.061(2) 0.038(2) 0.0159(16) 0.0169(17) 0.0271(17) O3 0.082(3) 0.113(3) 0.068(3) 0.028(3) 0.024(2) 0.023(3) O4 0.069(3) 0.100(3) 0.071(3) 0.018(2) 0.027(2) 0.007(2) O5 0.067(2) 0.066(2) 0.051(3) 0.0015(19) 0.0001(19) 0.0322(19) O6 0.0435(19) 0.068(2) 0.044(2) 0.0231(16) 0.0131(17) 0.0226(17) O7 0.210(8) 0.101(5) 0.178(7) 0.012(4) 0.084(6) 0.063(5) O8 0.135(5) 0.111(4) 0.254(8) 0.067(5) 0.116(5) 0.063(4) O7W 0.121(11) 0.57(4) 0.120(12) 0.062(16) 0.005(9) 0.204(18) O12 0.208(18) 0.209(15) 0.191(16) 0.080(12) 0.052(13) 0.122(14) O13 0.232(16) 0.128(10) 0.186(15) 0.009(9) 0.109(13) 0.104(11) O14 0.142(14) 0.185(14) 0.31(2) 0.034(14) 0.011(14) 0.096(12) N1 0.077(3) 0.034(2) 0.045(3) 0.0126(18) 0.026(2) 0.012(2) N2 0.050(2) 0.041(2) 0.063(3) 0.0196(19) 0.028(2) 0.013(2) N3 0.047(3) 0.034(2) 0.054(3) 0.0148(17) 0.018(2) 0.0145(17) N4 0.036(2) 0.047(2) 0.047(3) 0.0043(19) 0.011(2) 0.0090(19) N5 0.034(2) 0.043(2) 0.044(2) 0.0047(19) 0.0081(19) 0.0076(17) N6 0.067(3) 0.045(2) 0.046(3) 0.017(2) 0.018(2) 0.026(2) N7 0.047(2) 0.042(2) 0.049(3) 0.0162(18) 0.015(2) 0.0154(18) N8 0.039(2) 0.063(3) 0.047(3) 0.002(2) 0.018(2) -0.0126(19) N9 0.040(2) 0.039(2) 0.051(3) 0.0106(19) 0.017(2) 0.0085(17) N10 0.041(2) 0.035(2) 0.046(3) 0.0105(18) 0.0106(19) 0.0080(17) N11 0.037(2) 0.048(2) 0.047(2) 0.0131(19) 0.003(2) 0.0145(18) N12 0.037(2) 0.042(2) 0.047(3) 0.0101(19) 0.0047(19) 0.0098(18) N13 0.034(2) 0.048(2) 0.049(3) 0.0075(19) 0.013(2) -0.0027(18) N14 0.035(2) 0.045(2) 0.046(3) 0.0055(18) 0.0151(19) 0.0007(17) O1W 0.112(4) 0.071(3) 0.152(5) 0.005(3) 0.071(3) 0.040(3) O2W 0.107(8) 0.118(8) 0.066(7) -0.021(5) 0.027(5) 0.002(6) O3W 0.158(7) 0.227(8) 0.171(7) -0.035(6) 0.052(6) 0.008(6) O4W 0.170(10) 0.088(6) 0.085(7) -0.007(5) 0.074(7) -0.012(6) O6W 0.096(3) 0.095(3) 0.082(3) 0.039(2) 0.030(3) 0.049(3) O9 0.059(2) 0.056(2) 0.063(2) 0.0041(17) 0.0273(18) 0.0219(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 O6 1.976(3) . ? Cu1 N3 1.997(4) . ? Cu1 N10 1.998(4) . ? Cu1 N12 2.011(4) 2_665 ? Cu1 O1W 2.299(5) . ? Cu2 O1 1.983(3) . ? Cu2 N14 1.993(3) 1_335 ? Cu2 N5 2.003(4) . ? Cu2 N7 2.017(4) 2_546 ? Cu2 O9 2.316(4) . ? C1 C2 1.377(6) . ? C1 C6 1.391(7) . ? C1 N1 1.426(6) . ? C2 C3 1.383(7) . ? C2 H2 0.9300 . ? C3 C4 1.365(7) . ? C3 H3 0.9300 . ? C4 C5 1.385(6) . ? C4 N4 1.419(6) . ? C5 C6 1.382(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.340(7) . ? C7 N4 1.369(7) . ? C7 H7 0.9300 . ? C8 N5 1.362(7) . ? C8 H8 0.9300 . ? C9 N5 1.310(6) . ? C9 N4 1.349(5) . ? C9 H9 0.9300 . ? C10 C11 1.357(7) . ? C10 C15 1.371(7) . ? C10 N1 1.431(6) . ? C11 C12 1.390(7) . ? C11 H11 0.9300 . ? C12 C13 1.370(7) . ? C12 H12 0.9300 . ? C13 C14 1.363(7) . ? C13 N6 1.425(6) . ? C14 C15 1.359(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N7 1.301(6) . ? C16 N6 1.341(5) . ? C16 H16 0.9300 . ? C17 C18 1.336(8) . ? C17 N7 1.365(6) . ? C17 H17 0.9300 . ? C18 N6 1.365(7) . ? C18 H18 0.9300 . ? C19 C20 1.365(7) . ? C19 C24 1.379(6) . ? C19 N1 1.430(5) . ? C20 C21 1.412(6) . ? C20 H20 0.9300 . ? C21 C22 1.351(7) . ? C21 H21 0.9300 . ? C22 C23 1.373(7) . ? C22 N2 1.444(6) . ? C23 C24 1.386(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N3 1.311(5) . ? C25 N2 1.337(6) . ? C25 H25 0.9300 . ? C26 C27 1.337(7) . ? C26 N2 1.376(7) . ? C26 H26 0.9300 . ? C27 N3 1.366(6) . ? C27 H27 0.9300 . ? C28 C33 1.383(7) . ? C28 C29 1.393(6) . ? C28 N8 1.394(6) . ? C29 C30 1.369(7) . ? C29 H29 0.9300 . ? C30 C31 1.357(7) . ? C30 H30 0.9300 . ? C31 C32 1.384(6) . ? C31 N9 1.448(6) . ? C32 C33 1.379(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.329(7) . ? C34 N9 1.371(6) . ? C34 H34 0.9300 . ? C35 N10 1.363(6) . ? C35 H35 0.9300 . ? C36 N10 1.314(6) . ? C36 N9 1.347(5) . ? C36 H36 0.9300 . ? C37 C42 1.346(7) . ? C37 C38 1.395(7) . ? C37 N8 1.450(6) . ? C38 C39 1.373(7) . ? C38 H38 0.9300 . ? C39 C40 1.376(7) . ? C39 H39 0.9300 . ? C40 C41 1.389(7) . ? C40 N11 1.426(6) . ? C41 C42 1.393(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.351(7) . ? C43 N11 1.359(6) . ? C43 H43 0.9300 . ? C44 N12 1.355(6) . ? C44 H44 0.9300 . ? C45 N12 1.323(6) . ? C45 N11 1.349(6) . ? C45 H45 0.9300 . ? C46 C47 1.362(7) . ? C46 C51 1.373(7) . ? C46 N8 1.421(6) . ? C47 C48 1.384(6) . ? C47 H47 0.9300 . ? C48 C49 1.362(7) . ? C48 H48 0.9300 . ? C49 C50 1.375(7) . ? C49 N13 1.443(6) . ? C50 C51 1.376(7) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C54 1.348(7) . ? C52 N13 1.368(6) . ? C52 H52 0.9300 . ? C53 N14 1.315(6) . ? C53 N13 1.350(6) . ? C53 H53 0.9300 . ? C54 N14 1.384(6) . ? C54 H54 0.9300 . ? C55 C57 1.382(7) 2_766 ? C55 C56 1.393(7) . ? C55 C58 1.515(7) . ? C56 C57 1.386(7) . ? C56 H56 0.9300 . ? C57 C55 1.382(7) 2_766 ? C57 H57 0.9300 . ? C58 O5 1.257(6) . ? C58 O6 1.268(6) . ? C59 C60 1.389(8) . ? C59 C61 1.403(8) 2_545 ? C59 C62 1.496(8) . ? C60 C61 1.391(8) . ? C60 H60 0.9300 . ? C61 C59 1.403(8) 2_545 ? C61 H61 0.9300 . ? C62 O3 1.247(7) . ? C62 O4 1.270(7) . ? C63 C64 1.377(7) . ? C63 C65 1.388(6) 2_445 ? C63 C66 1.525(6) . ? C64 C65 1.386(6) . ? C64 H64 0.9300 . ? C65 C63 1.388(6) 2_445 ? C65 H65 0.9300 . ? C66 O2 1.252(6) . ? C66 O1 1.264(6) . ? C67 C69 1.351(14) . ? C67 C68 1.378(11) . ? C67 C70 1.567(12) . ? C68 C69 1.394(14) 2_556 ? C68 H68 0.9300 . ? C69 C68 1.394(14) 2_556 ? C69 H69 0.9300 . ? C70 O7 1.230(12) . ? C70 O8 1.244(10) . ? C71 O14 1.40(2) . ? C72 O12 1.47(3) . ? C73 O9 1.387(7) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 O13 1.37(2) . ? N7 Cu2 2.017(4) 2_546 ? N12 Cu1 2.011(4) 2_665 ? N14 Cu2 1.993(3) 1_775 ? O2W H2WA 0.84(2) . ? O6W H6WA 0.86(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 O6 Cu1 N3 91.62(14) . . ? O6 Cu1 N10 89.03(14) . . ? N3 Cu1 N10 173.91(17) . . ? O6 Cu1 N12 170.31(17) . 2_665 ? N3 Cu1 N12 89.16(15) . 2_665 ? N10 Cu1 N12 89.18(15) . 2_665 ? O6 Cu1 O1W 93.10(18) . . ? N3 Cu1 O1W 93.63(17) . . ? N10 Cu1 O1W 92.37(17) . . ? N12 Cu1 O1W 96.48(18) 2_665 . ? O1 Cu2 N14 86.15(14) . 1_335 ? O1 Cu2 N5 91.07(13) . . ? N14 Cu2 N5 176.16(16) 1_335 . ? O1 Cu2 N7 169.66(16) . 2_546 ? N14 Cu2 N7 90.57(15) 1_335 2_546 ? N5 Cu2 N7 91.71(15) . 2_546 ? O1 Cu2 O9 87.33(13) . . ? N14 Cu2 O9 90.25(15) 1_335 . ? N5 Cu2 O9 92.27(15) . . ? N7 Cu2 O9 102.50(15) 2_546 . ? C2 C1 C6 118.0(4) . . ? C2 C1 N1 121.2(5) . . ? C6 C1 N1 120.8(4) . . ? C1 C2 C3 120.9(5) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 N4 119.8(4) . . ? C5 C4 N4 120.8(5) . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.1(4) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C8 C7 N4 107.0(5) . . ? C8 C7 H7 126.5 . . ? N4 C7 H7 126.5 . . ? C7 C8 N5 109.9(5) . . ? C7 C8 H8 125.0 . . ? N5 C8 H8 125.0 . . ? N5 C9 N4 112.0(5) . . ? N5 C9 H9 124.0 . . ? N4 C9 H9 124.0 . . ? C11 C10 C15 118.8(5) . . ? C11 C10 N1 120.5(5) . . ? C15 C10 N1 120.7(4) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 118.8(5) . . ? C14 C13 N6 121.1(5) . . ? C12 C13 N6 120.1(4) . . ? C15 C14 C13 121.1(6) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C10 120.8(5) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? N7 C16 N6 112.7(4) . . ? N7 C16 H16 123.6 . . ? N6 C16 H16 123.6 . . ? C18 C17 N7 108.7(5) . . ? C18 C17 H17 125.7 . . ? N7 C17 H17 125.7 . . ? C17 C18 N6 108.2(5) . . ? C17 C18 H18 125.9 . . ? N6 C18 H18 125.9 . . ? C20 C19 C24 119.6(4) . . ? C20 C19 N1 118.9(4) . . ? C24 C19 N1 121.5(4) . . ? C19 C20 C21 120.1(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.4(5) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 120.9(4) . . ? C21 C22 N2 120.1(4) . . ? C23 C22 N2 118.8(4) . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 120.2(4) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? N3 C25 N2 112.0(4) . . ? N3 C25 H25 124.0 . . ? N2 C25 H25 124.0 . . ? C27 C26 N2 105.2(5) . . ? C27 C26 H26 127.4 . . ? N2 C26 H26 127.4 . . ? C26 C27 N3 111.3(5) . . ? C26 C27 H27 124.4 . . ? N3 C27 H27 124.4 . . ? C33 C28 C29 117.0(5) . . ? C33 C28 N8 121.8(4) . . ? C29 C28 N8 121.2(5) . . ? C30 C29 C28 121.1(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.3(5) . . ? C30 C31 N9 119.9(4) . . ? C32 C31 N9 119.7(4) . . ? C33 C32 C31 118.5(5) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C32 C33 C28 122.4(4) . . ? C32 C33 H33 118.8 . . ? C28 C33 H33 118.8 . . ? C35 C34 N9 106.6(4) . . ? C35 C34 H34 126.7 . . ? N9 C34 H34 126.7 . . ? C34 C35 N10 110.3(5) . . ? C34 C35 H35 124.9 . . ? N10 C35 H35 124.9 . . ? N10 C36 N9 111.0(4) . . ? N10 C36 H36 124.5 . . ? N9 C36 H36 124.5 . . ? C42 C37 C38 120.2(5) . . ? C42 C37 N8 121.0(5) . . ? C38 C37 N8 118.8(5) . . ? C39 C38 C37 119.3(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 120.3(5) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C41 120.7(5) . . ? C39 C40 N11 120.6(4) . . ? C41 C40 N11 118.6(5) . . ? C40 C41 C42 117.8(5) . . ? C40 C41 H41 121.1 . . ? C42 C41 H41 121.1 . . ? C37 C42 C41 121.6(5) . . ? C37 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C44 C43 N11 106.7(4) . . ? C44 C43 H43 126.6 . . ? N11 C43 H43 126.6 . . ? C43 C44 N12 109.8(5) . . ? C43 C44 H44 125.1 . . ? N12 C44 H44 125.1 . . ? N12 C45 N11 110.8(4) . . ? N12 C45 H45 124.6 . . ? N11 C45 H45 124.6 . . ? C47 C46 C51 118.5(4) . . ? C47 C46 N8 119.5(4) . . ? C51 C46 N8 121.9(4) . . ? C46 C47 C48 120.9(5) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C49 C48 C47 119.7(5) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C50 120.3(4) . . ? C48 C49 N13 119.6(4) . . ? C50 C49 N13 120.0(4) . . ? C49 C50 C51 119.0(5) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C46 C51 C50 121.5(5) . . ? C46 C51 H51 119.2 . . ? C50 C51 H51 119.2 . . ? C54 C52 N13 106.3(4) . . ? C54 C52 H52 126.9 . . ? N13 C52 H52 126.9 . . ? N14 C53 N13 110.9(4) . . ? N14 C53 H53 124.5 . . ? N13 C53 H53 124.5 . . ? C52 C54 N14 109.6(4) . . ? C52 C54 H54 125.2 . . ? N14 C54 H54 125.2 . . ? C57 C55 C56 119.3(4) 2_766 . ? C57 C55 C58 120.3(5) 2_766 . ? C56 C55 C58 120.3(5) . . ? C57 C56 C55 120.5(5) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C55 C57 C56 120.1(5) 2_766 . ? C55 C57 H57 119.9 2_766 . ? C56 C57 H57 119.9 . . ? O5 C58 O6 124.7(5) . . ? O5 C58 C55 117.9(5) . . ? O6 C58 C55 117.5(5) . . ? C60 C59 C61 118.6(5) . 2_545 ? C60 C59 C62 121.9(6) . . ? C61 C59 C62 119.5(6) 2_545 . ? C59 C60 C61 121.2(6) . . ? C59 C60 H60 119.4 . . ? C61 C60 H60 119.4 . . ? C60 C61 C59 120.2(6) . 2_545 ? C60 C61 H61 119.9 . . ? C59 C61 H61 119.9 2_545 . ? O3 C62 O4 124.1(6) . . ? O3 C62 C59 117.7(6) . . ? O4 C62 C59 118.2(6) . . ? C64 C63 C65 119.4(4) . 2_445 ? C64 C63 C66 120.2(4) . . ? C65 C63 C66 120.3(4) 2_445 . ? C63 C64 C65 119.7(4) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C63 120.9(4) . 2_445 ? C64 C65 H65 119.6 . . ? C63 C65 H65 119.6 2_445 . ? O2 C66 O1 125.4(4) . . ? O2 C66 C63 118.3(5) . . ? O1 C66 C63 116.2(5) . . ? C69 C67 C68 121.6(11) . . ? C69 C67 C70 120.2(10) . . ? C68 C67 C70 118.2(11) . . ? C67 C68 C69 120.8(10) . 2_556 ? C67 C68 H68 119.6 . . ? C69 C68 H68 119.6 2_556 . ? C67 C69 C68 117.5(9) . 2_556 ? C67 C69 H69 121.2 . . ? C68 C69 H69 121.2 2_556 . ? O7 C70 O8 126.7(12) . . ? O7 C70 C67 117.3(9) . . ? O8 C70 C67 116.0(11) . . ? O9 C73 H73A 109.5 . . ? O9 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O9 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C66 O1 Cu2 114.2(3) . . ? C58 O6 Cu1 117.1(3) . . ? C1 N1 C19 121.3(4) . . ? C1 N1 C10 119.8(3) . . ? C19 N1 C10 117.3(4) . . ? C25 N2 C26 106.9(4) . . ? C25 N2 C22 128.1(4) . . ? C26 N2 C22 124.9(4) . . ? C25 N3 C27 104.5(4) . . ? C25 N3 Cu1 129.1(3) . . ? C27 N3 Cu1 125.7(3) . . ? C9 N4 C7 105.7(4) . . ? C9 N4 C4 127.2(5) . . ? C7 N4 C4 127.1(4) . . ? C9 N5 C8 105.4(4) . . ? C9 N5 Cu2 130.1(3) . . ? C8 N5 Cu2 123.8(4) . . ? C16 N6 C18 104.8(4) . . ? C16 N6 C13 127.0(4) . . ? C18 N6 C13 128.0(4) . . ? C16 N7 C17 105.6(4) . . ? C16 N7 Cu2 125.1(3) . 2_546 ? C17 N7 Cu2 128.5(4) . 2_546 ? C28 N8 C46 123.2(4) . . ? C28 N8 C37 119.8(4) . . ? C46 N8 C37 116.8(4) . . ? C36 N9 C34 106.5(4) . . ? C36 N9 C31 125.3(4) . . ? C34 N9 C31 128.2(4) . . ? C36 N10 C35 105.6(4) . . ? C36 N10 Cu1 126.9(3) . . ? C35 N10 Cu1 127.5(4) . . ? C45 N11 C43 106.8(4) . . ? C45 N11 C40 124.6(4) . . ? C43 N11 C40 128.5(4) . . ? C45 N12 C44 105.9(4) . . ? C45 N12 Cu1 124.2(3) . 2_665 ? C44 N12 Cu1 130.0(3) . 2_665 ? C53 N13 C52 107.5(4) . . ? C53 N13 C49 126.4(4) . . ? C52 N13 C49 126.1(4) . . ? C53 N14 C54 105.7(4) . . ? C53 N14 Cu2 130.7(3) . 1_775 ? C54 N14 Cu2 123.6(3) . 1_775 ? C73 O9 Cu2 128.2(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 C6 C1 C2 C3 2.0(8) . . . . ? N1 C1 C2 C3 -177.9(5) . . . . ? C1 C2 C3 C4 -3.1(8) . . . . ? C2 C3 C4 C5 2.6(8) . . . . ? C2 C3 C4 N4 -178.6(4) . . . . ? C3 C4 C5 C6 -1.1(8) . . . . ? N4 C4 C5 C6 -179.8(5) . . . . ? C4 C5 C6 C1 0.0(9) . . . . ? C2 C1 C6 C5 -0.4(8) . . . . ? N1 C1 C6 C5 179.4(5) . . . . ? N4 C7 C8 N5 0.1(8) . . . . ? C15 C10 C11 C12 -1.3(8) . . . . ? N1 C10 C11 C12 177.9(5) . . . . ? C10 C11 C12 C13 0.0(8) . . . . ? C11 C12 C13 C14 0.7(8) . . . . ? C11 C12 C13 N6 -178.0(5) . . . . ? C12 C13 C14 C15 0.0(9) . . . . ? N6 C13 C14 C15 178.6(5) . . . . ? C13 C14 C15 C10 -1.3(9) . . . . ? C11 C10 C15 C14 2.0(9) . . . . ? N1 C10 C15 C14 -177.3(5) . . . . ? N7 C17 C18 N6 0.1(8) . . . . ? C24 C19 C20 C21 2.3(9) . . . . ? N1 C19 C20 C21 -176.7(5) . . . . ? C19 C20 C21 C22 -3.2(9) . . . . ? C20 C21 C22 C23 3.1(9) . . . . ? C20 C21 C22 N2 179.3(5) . . . . ? C21 C22 C23 C24 -2.1(9) . . . . ? N2 C22 C23 C24 -178.3(5) . . . . ? C20 C19 C24 C23 -1.3(9) . . . . ? N1 C19 C24 C23 177.6(5) . . . . ? C22 C23 C24 C19 1.2(9) . . . . ? N2 C26 C27 N3 1.4(8) . . . . ? C33 C28 C29 C30 1.0(7) . . . . ? N8 C28 C29 C30 -177.5(5) . . . . ? C28 C29 C30 C31 -0.1(8) . . . . ? C29 C30 C31 C32 0.4(8) . . . . ? C29 C30 C31 N9 177.6(4) . . . . ? C30 C31 C32 C33 -1.6(8) . . . . ? N9 C31 C32 C33 -178.8(5) . . . . ? C31 C32 C33 C28 2.6(8) . . . . ? C29 C28 C33 C32 -2.2(8) . . . . ? N8 C28 C33 C32 176.2(5) . . . . ? N9 C34 C35 N10 -1.4(6) . . . . ? C42 C37 C38 C39 0.5(7) . . . . ? N8 C37 C38 C39 -178.0(4) . . . . ? C37 C38 C39 C40 0.8(7) . . . . ? C38 C39 C40 C41 -1.6(7) . . . . ? C38 C39 C40 N11 178.4(4) . . . . ? C39 C40 C41 C42 1.0(7) . . . . ? N11 C40 C41 C42 -179.0(4) . . . . ? C38 C37 C42 C41 -1.1(8) . . . . ? N8 C37 C42 C41 177.3(4) . . . . ? C40 C41 C42 C37 0.4(8) . . . . ? N11 C43 C44 N12 0.4(7) . . . . ? C51 C46 C47 C48 -1.0(8) . . . . ? N8 C46 C47 C48 -178.1(5) . . . . ? C46 C47 C48 C49 0.8(8) . . . . ? C47 C48 C49 C50 0.1(8) . . . . ? C47 C48 C49 N13 177.4(5) . . . . ? C48 C49 C50 C51 -0.9(8) . . . . ? N13 C49 C50 C51 -178.2(5) . . . . ? C47 C46 C51 C50 0.2(9) . . . . ? N8 C46 C51 C50 177.2(5) . . . . ? C49 C50 C51 C46 0.7(9) . . . . ? N13 C52 C54 N14 0.4(7) . . . . ? C57 C55 C56 C57 0.2(8) 2_766 . . . ? C58 C55 C56 C57 -176.8(4) . . . . ? C55 C56 C57 C55 -0.2(8) . . . 2_766 ? C57 C55 C58 O5 -16.9(6) 2_766 . . . ? C56 C55 C58 O5 160.0(4) . . . . ? C57 C55 C58 O6 162.5(4) 2_766 . . . ? C56 C55 C58 O6 -20.6(6) . . . . ? C61 C59 C60 C61 -2.7(8) 2_545 . . . ? C62 C59 C60 C61 178.4(5) . . . . ? C59 C60 C61 C59 2.7(9) . . . 2_545 ? C60 C59 C62 O3 -153.1(6) . . . . ? C61 C59 C62 O3 27.9(8) 2_545 . . . ? C60 C59 C62 O4 26.5(8) . . . . ? C61 C59 C62 O4 -152.5(5) 2_545 . . . ? C65 C63 C64 C65 -0.8(7) 2_445 . . . ? C66 C63 C64 C65 175.6(4) . . . . ? C63 C64 C65 C63 0.8(7) . . . 2_445 ? C64 C63 C66 O2 -162.6(4) . . . . ? C65 C63 C66 O2 13.8(6) 2_445 . . . ? C64 C63 C66 O1 16.3(6) . . . . ? C65 C63 C66 O1 -167.4(4) 2_445 . . . ? C69 C67 C68 C69 0.8(15) . . . 2_556 ? C70 C67 C68 C69 -177.9(8) . . . 2_556 ? C68 C67 C69 C68 -0.8(15) . . . 2_556 ? C70 C67 C69 C68 177.9(7) . . . 2_556 ? C69 C67 C70 O7 164.6(9) . . . . ? C68 C67 C70 O7 -16.7(12) . . . . ? C69 C67 C70 O8 -16.3(12) . . . . ? C68 C67 C70 O8 162.5(7) . . . . ? O2 C66 O1 Cu2 17.9(5) . . . . ? C63 C66 O1 Cu2 -160.9(3) . . . . ? N14 Cu2 O1 C66 78.2(3) 1_335 . . . ? N5 Cu2 O1 C66 -99.1(3) . . . . ? N7 Cu2 O1 C66 6.5(9) 2_546 . . . ? O9 Cu2 O1 C66 168.6(3) . . . . ? O5 C58 O6 Cu1 -18.4(6) . . . . ? C55 C58 O6 Cu1 162.2(3) . . . . ? N3 Cu1 O6 C58 108.2(3) . . . . ? N10 Cu1 O6 C58 -65.8(3) . . . . ? N12 Cu1 O6 C58 13.6(10) 2_665 . . . ? O1W Cu1 O6 C58 -158.1(3) . . . . ? C2 C1 N1 C19 -142.4(5) . . . . ? C6 C1 N1 C19 37.8(7) . . . . ? C2 C1 N1 C10 22.3(7) . . . . ? C6 C1 N1 C10 -157.5(5) . . . . ? C20 C19 N1 C1 -148.7(5) . . . . ? C24 C19 N1 C1 32.3(8) . . . . ? C20 C19 N1 C10 46.2(7) . . . . ? C24 C19 N1 C10 -132.8(5) . . . . ? C11 C10 N1 C1 59.7(7) . . . . ? C15 C10 N1 C1 -121.1(5) . . . . ? C11 C10 N1 C19 -134.9(5) . . . . ? C15 C10 N1 C19 44.3(7) . . . . ? N3 C25 N2 C26 2.1(6) . . . . ? N3 C25 N2 C22 178.7(5) . . . . ? C27 C26 N2 C25 -2.1(7) . . . . ? C27 C26 N2 C22 -178.8(5) . . . . ? C21 C22 N2 C25 50.1(8) . . . . ? C23 C22 N2 C25 -133.7(6) . . . . ? C21 C22 N2 C26 -134.0(6) . . . . ? C23 C22 N2 C26 42.3(8) . . . . ? N2 C25 N3 C27 -1.2(6) . . . . ? N2 C25 N3 Cu1 -172.2(3) . . . . ? C26 C27 N3 C25 -0.2(7) . . . . ? C26 C27 N3 Cu1 171.2(5) . . . . ? O6 Cu1 N3 C25 -36.7(4) . . . . ? N10 Cu1 N3 C25 59.4(16) . . . . ? N12 Cu1 N3 C25 133.7(4) 2_665 . . . ? O1W Cu1 N3 C25 -129.9(4) . . . . ? O6 Cu1 N3 C27 154.1(5) . . . . ? N10 Cu1 N3 C27 -109.8(14) . . . . ? N12 Cu1 N3 C27 -35.5(5) 2_665 . . . ? O1W Cu1 N3 C27 60.9(5) . . . . ? N5 C9 N4 C7 0.0(6) . . . . ? N5 C9 N4 C4 179.5(4) . . . . ? C8 C7 N4 C9 0.0(7) . . . . ? C8 C7 N4 C4 -179.6(5) . . . . ? C3 C4 N4 C9 35.9(7) . . . . ? C5 C4 N4 C9 -145.4(5) . . . . ? C3 C4 N4 C7 -144.7(6) . . . . ? C5 C4 N4 C7 34.0(8) . . . . ? N4 C9 N5 C8 0.0(5) . . . . ? N4 C9 N5 Cu2 -170.2(3) . . . . ? C7 C8 N5 C9 -0.1(7) . . . . ? C7 C8 N5 Cu2 170.9(5) . . . . ? O1 Cu2 N5 C9 79.9(4) . . . . ? N14 Cu2 N5 C9 36(3) 1_335 . . . ? N7 Cu2 N5 C9 -90.1(4) 2_546 . . . ? O9 Cu2 N5 C9 167.3(4) . . . . ? O1 Cu2 N5 C8 -88.7(4) . . . . ? N14 Cu2 N5 C8 -132(2) 1_335 . . . ? N7 Cu2 N5 C8 101.3(4) 2_546 . . . ? O9 Cu2 N5 C8 -1.3(4) . . . . ? N7 C16 N6 C18 1.7(6) . . . . ? N7 C16 N6 C13 176.4(4) . . . . ? C17 C18 N6 C16 -1.0(7) . . . . ? C17 C18 N6 C13 -175.6(5) . . . . ? C14 C13 N6 C16 144.5(5) . . . . ? C12 C13 N6 C16 -36.9(8) . . . . ? C14 C13 N6 C18 -42.1(8) . . . . ? C12 C13 N6 C18 136.6(6) . . . . ? N6 C16 N7 C17 -1.6(6) . . . . ? N6 C16 N7 Cu2 -172.1(3) . . . 2_546 ? C18 C17 N7 C16 0.9(7) . . . . ? C18 C17 N7 Cu2 170.9(4) . . . 2_546 ? C33 C28 N8 C46 36.2(8) . . . . ? C29 C28 N8 C46 -145.4(5) . . . . ? C33 C28 N8 C37 -148.3(5) . . . . ? C29 C28 N8 C37 30.1(8) . . . . ? C47 C46 N8 C28 -143.0(5) . . . . ? C51 C46 N8 C28 40.0(8) . . . . ? C47 C46 N8 C37 41.4(7) . . . . ? C51 C46 N8 C37 -135.6(6) . . . . ? C42 C37 N8 C28 -117.2(6) . . . . ? C38 C37 N8 C28 61.3(7) . . . . ? C42 C37 N8 C46 58.6(7) . . . . ? C38 C37 N8 C46 -123.0(5) . . . . ? N10 C36 N9 C34 0.2(5) . . . . ? N10 C36 N9 C31 178.8(4) . . . . ? C35 C34 N9 C36 0.8(6) . . . . ? C35 C34 N9 C31 -177.8(5) . . . . ? C30 C31 N9 C36 -21.8(7) . . . . ? C32 C31 N9 C36 155.4(5) . . . . ? C30 C31 N9 C34 156.4(5) . . . . ? C32 C31 N9 C34 -26.3(7) . . . . ? N9 C36 N10 C35 -1.0(5) . . . . ? N9 C36 N10 Cu1 -179.4(3) . . . . ? C34 C35 N10 C36 1.5(6) . . . . ? C34 C35 N10 Cu1 179.9(4) . . . . ? O6 Cu1 N10 C36 123.5(4) . . . . ? N3 Cu1 N10 C36 27.3(16) . . . . ? N12 Cu1 N10 C36 -46.9(4) 2_665 . . . ? O1W Cu1 N10 C36 -143.4(4) . . . . ? O6 Cu1 N10 C35 -54.5(4) . . . . ? N3 Cu1 N10 C35 -150.7(13) . . . . ? N12 Cu1 N10 C35 135.0(4) 2_665 . . . ? O1W Cu1 N10 C35 38.6(4) . . . . ? N12 C45 N11 C43 0.6(6) . . . . ? N12 C45 N11 C40 -175.7(4) . . . . ? C44 C43 N11 C45 -0.6(6) . . . . ? C44 C43 N11 C40 175.5(5) . . . . ? C39 C40 N11 C45 42.9(7) . . . . ? C41 C40 N11 C45 -137.2(5) . . . . ? C39 C40 N11 C43 -132.5(6) . . . . ? C41 C40 N11 C43 47.4(7) . . . . ? N11 C45 N12 C44 -0.3(6) . . . . ? N11 C45 N12 Cu1 -179.5(3) . . . 2_665 ? C43 C44 N12 C45 -0.1(7) . . . . ? C43 C44 N12 Cu1 179.0(4) . . . 2_665 ? N14 C53 N13 C52 -0.9(6) . . . . ? N14 C53 N13 C49 178.4(4) . . . . ? C54 C52 N13 C53 0.3(6) . . . . ? C54 C52 N13 C49 -179.0(5) . . . . ? C48 C49 N13 C53 150.1(5) . . . . ? C50 C49 N13 C53 -32.6(8) . . . . ? C48 C49 N13 C52 -30.7(8) . . . . ? C50 C49 N13 C52 146.6(6) . . . . ? N13 C53 N14 C54 1.1(6) . . . . ? N13 C53 N14 Cu2 -179.3(3) . . . 1_775 ? C52 C54 N14 C53 -0.9(6) . . . . ? C52 C54 N14 Cu2 179.5(4) . . . 1_775 ? O1 Cu2 O9 C73 -152.2(5) . . . . ? N14 Cu2 O9 C73 -66.1(6) 1_335 . . . ? N5 Cu2 O9 C73 116.8(5) . . . . ? N7 Cu2 O9 C73 24.5(6) 2_546 . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.900 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.076 data_6 _database_code_depnum_ccdc_archive 'CCDC 826247' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H42 Co3 N14 O12' _chemical_formula_sum 'C78 H42 Co3 N14 O12' _chemical_formula_weight 1544.05 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 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6440(5) _cell_length_b 10.7230(5) _cell_length_c 16.1450(9) _cell_angle_alpha 92.596(4) _cell_angle_beta 103.076(4) _cell_angle_gamma 96.167(4) _cell_volume 1779.94(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6402 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 785 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11608 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.2036 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6402 _reflns_number_gt 2830 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6402 _refine_ls_number_parameters 523 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1500 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.835 _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 Co1 Co 0.0000 0.5000 1.0000 0.0252(3) Uani 1 2 d S . . Co2 Co -0.15686(7) 0.18397(7) 1.21762(5) 0.0352(3) Uani 1 1 d . . . C1 C -0.2900(5) 0.1691(5) 0.9772(3) 0.0297(14) Uani 1 1 d . . . C2 C -0.2977(5) 0.0443(5) 0.9910(4) 0.0319(14) Uani 1 1 d . . . H2 H -0.2368 0.0160 1.0347 0.038 Uiso 1 1 calc R . . C3 C -0.3963(5) -0.0417(5) 0.9401(4) 0.0367(15) Uani 1 1 d . . . H3 H -0.3983 -0.1273 0.9475 0.044 Uiso 1 1 calc R . . C4 C -0.4896(5) 0.0021(5) 0.8793(4) 0.0349(15) Uani 1 1 d . . . C5 C -0.4837(5) 0.1272(6) 0.8653(4) 0.0431(17) Uani 1 1 d . . . H5 H -0.5481 0.1559 0.8241 0.052 Uiso 1 1 calc R . . C6 C -0.3814(5) 0.2114(6) 0.9124(4) 0.0416(17) Uani 1 1 d . . . H6 H -0.3743 0.2956 0.9006 0.050 Uiso 1 1 calc R . . C7 C -0.1837(5) 0.2642(5) 1.0309(4) 0.0327(14) Uani 1 1 d . . . C8 C -0.6076(6) -0.0872(6) 0.8327(4) 0.0390(16) Uani 1 1 d . . . C9 C -0.0467(6) 0.3798(6) 1.5125(5) 0.0501(18) Uani 1 1 d . . . H9 H -0.0774 0.2981 1.5212 0.060 Uiso 1 1 calc R . . C10 C -0.0488(5) 0.4129(5) 1.4314(4) 0.0403(16) Uani 1 1 d . . . C11 C -0.0003(6) 0.5337(5) 1.4185(4) 0.0468(17) Uani 1 1 d . . . H11 H 0.0006 0.5564 1.3637 0.056 Uiso 1 1 calc R . . C12 C -0.0974(6) 0.3171(6) 1.3565(5) 0.0478(18) Uani 1 1 d . . . C13 C 0.5013(6) 0.1501(8) 0.5784(5) 0.060(4) Uani 0.50 1 d PG . . C14 C 0.6249(7) 0.1807(6) 0.5647(5) 0.087(3) Uani 1 1 d G . . C15 C 0.7270(5) 0.1183(7) 0.6052(6) 0.104(4) Uani 1 1 d G . . C16 C 0.7056(6) 0.0254(7) 0.6595(6) 0.066(4) Uani 0.50 1 d PG . . C17 C 0.5820(7) -0.0051(7) 0.6732(5) 0.049(4) Uani 0.50 1 d PG . . C18 C 0.4799(5) 0.0572(8) 0.6327(6) 0.057(4) Uani 0.50 1 d PG . . C13' C 0.5838(12) 0.2758(12) 0.5986(8) 0.041(3) Uani 0.50 1 d P . . C16' C 0.7617(11) 0.1296(14) 0.6793(8) 0.038(3) Uani 0.50 1 d P . . C17' C 0.7458(11) 0.2400(13) 0.7211(9) 0.048(4) Uani 0.50 1 d P . . C18' C 0.6556(11) 0.3149(11) 0.6803(8) 0.040(3) Uani 0.50 1 d P . . C19 C 0.9287(6) -0.0397(8) 0.7014(5) 0.065(2) Uani 1 1 d . . . H19 H 0.9508 -0.0353 0.6490 0.079 Uiso 1 1 calc R . . C20 C 0.9232(6) -0.0845(7) 0.8293(5) 0.0566(19) Uani 1 1 d . . . H20 H 0.9424 -0.1188 0.8819 0.068 Uiso 1 1 calc R . . C21 C 0.8279(7) -0.0124(10) 0.8040(5) 0.089(3) Uani 1 1 d . . . H21 H 0.7713 0.0135 0.8357 0.107 Uiso 1 1 calc R . . C22 C 0.3367(8) 0.2555(9) 0.6136(4) 0.083(3) Uani 1 1 d G . . C23 C 0.3983(7) 0.3442(10) 0.6797(6) 0.090(7) Uiso 0.50 1 d PG . . C24 C 0.3363(8) 0.3738(8) 0.7438(5) 0.083(5) Uiso 0.50 1 d PG . . C25 C 0.2128(8) 0.3146(7) 0.7418(4) 0.082(3) Uani 1 1 d G . . C26 C 0.1512(7) 0.2259(8) 0.6757(5) 0.063(4) Uiso 0.50 1 d PG . . C27 C 0.2132(8) 0.1963(8) 0.6116(5) 0.075(5) Uani 0.50 1 d PG . . C23' C 0.3832(11) 0.4615(12) 0.6669(8) 0.041(3) Uani 0.50 1 d P . . C24' C 0.3048(12) 0.4587(13) 0.7277(9) 0.054(4) Uani 0.50 1 d P . . C26' C 0.2551(12) 0.2353(12) 0.6971(9) 0.049(4) Uani 0.50 1 d P . . C27' C 0.3897(12) 0.3520(12) 0.6226(12) 0.055(5) Uani 0.50 1 d P . . C28 C 0.1246(6) 0.4229(6) 0.8468(4) 0.0380(15) Uani 1 1 d . . . H28 H 0.1464 0.5056 0.8354 0.046 Uiso 1 1 calc R . . C29 C 0.0503(9) 0.2619(6) 0.9001(5) 0.080(3) Uani 1 1 d . . . H29 H 0.0080 0.2113 0.9332 0.096 Uiso 1 1 calc R . . C30 C 0.1122(2) 0.2187(2) 0.84273(17) 0.098(3) Uani 1 1 d . . . H30 H 0.1222 0.1355 0.8297 0.118 Uiso 1 1 calc R . . C32 C 0.3147(2) 0.3470(2) 0.29889(17) 0.060(2) Uani 1 1 d R . . C33 C 0.2515(2) 0.3776(2) 0.35826(17) 0.0397(15) Uani 1 1 d R . . C34 C 0.2916(2) 0.3579(2) 0.44312(17) 0.0451(16) Uani 1 1 d R . . C35 C 0.3804(2) 0.2624(2) 0.46386(17) 0.037(3) Uani 0.50 1 d PR . . C36 C 0.4314(2) 0.2088(2) 0.40230(17) 0.048(3) Uani 0.50 1 d PR . . C37 C 0.3929(2) 0.2413(2) 0.31719(17) 0.045(3) Uani 0.50 1 d PR . . C35' C 0.4263(2) 0.3520(2) 0.47590(17) 0.033(3) Uani 0.50 1 d PR . . C36' C 0.5073(2) 0.3529(2) 0.41966(17) 0.041(3) Uani 0.50 1 d PR . . C37' C 0.4607(2) 0.3599(2) 0.33168(17) 0.035(3) Uani 0.50 1 d PR . . C38 C 0.1570(2) 0.4063(2) 0.17216(17) 0.0404(15) Uani 1 1 d R . . H38 H 0.0915 0.4186 0.2001 0.048 Uiso 1 1 d R . . C39 C 0.3423(6) 0.3632(6) 0.1503(4) 0.0490(17) Uani 1 1 d . . . H39 H 0.4258 0.3409 0.1571 0.059 Uiso 1 1 calc R . . C40 C 0.2646(6) 0.3952(7) 0.0776(5) 0.061(2) Uani 1 1 d . . . H40 H 0.2873 0.3986 0.0254 0.073 Uiso 1 1 calc R . . N1' N 0.4743(8) 0.3421(10) 0.5637(6) 0.040(3) Uani 0.50 1 d P . . N1 N 0.4109(11) 0.2336(11) 0.5493(8) 0.057(3) Uani 0.50 1 d PU . . N2 N 0.1569(6) 0.3225(5) 0.8078(4) 0.0598(16) Uani 1 1 d . . . N3 N 0.0581(4) 0.3898(4) 0.9033(3) 0.0376(12) Uani 1 1 d . . . N4 N 0.2734(4) 0.3703(4) 0.2115(3) 0.0360(12) Uani 1 1 d . . . N5 N 0.1473(4) 0.4221(4) 0.0920(3) 0.0327(12) Uani 1 1 d . . . N6 N 0.8305(6) 0.0149(9) 0.7238(4) 0.112(3) Uani 1 1 d . . . N7 N 0.9880(4) -0.1000(5) 0.7658(3) 0.0447(13) Uani 1 1 d . . . O1 O -0.6076(4) -0.2016(4) 0.8298(3) 0.0549(13) Uani 1 1 d . . . O2 O -0.7094(4) -0.0359(4) 0.7999(3) 0.0444(11) Uani 1 1 d . . . O3 O -0.1514(4) 0.3587(3) 0.9964(3) 0.0465(12) Uani 1 1 d . . . O4 O -0.1328(4) 0.2429(4) 1.1063(3) 0.0526(13) Uani 1 1 d . . . O5 O -0.1278(5) 0.2062(4) 1.3681(3) 0.0671(15) Uani 1 1 d . . . O6 O -0.0998(5) 0.3529(4) 1.2828(3) 0.0633(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0288(6) 0.0251(6) 0.0190(7) 0.0029(5) 0.0016(5) -0.0007(4) Co2 0.0385(5) 0.0317(4) 0.0274(6) 0.0019(4) -0.0052(4) -0.0035(4) C1 0.025(3) 0.041(3) 0.019(3) -0.003(3) 0.000(3) -0.003(3) C2 0.033(3) 0.040(3) 0.019(3) 0.000(3) 0.003(3) -0.003(3) C3 0.034(3) 0.043(3) 0.033(4) 0.001(3) 0.010(3) -0.001(3) C4 0.030(3) 0.041(4) 0.030(4) -0.005(3) 0.004(3) -0.004(3) C5 0.030(3) 0.050(4) 0.042(4) 0.001(3) -0.002(3) -0.007(3) C6 0.040(3) 0.041(3) 0.036(4) 0.006(3) -0.006(3) 0.000(3) C7 0.026(3) 0.042(3) 0.026(4) 0.007(3) -0.001(3) -0.001(3) C8 0.033(3) 0.052(4) 0.027(4) -0.003(3) 0.003(3) -0.005(3) C9 0.059(4) 0.035(3) 0.048(5) -0.002(3) -0.003(4) 0.002(3) C10 0.037(3) 0.042(4) 0.036(4) -0.008(3) -0.005(3) 0.014(3) C11 0.058(4) 0.041(3) 0.038(4) -0.008(3) 0.004(3) 0.011(3) C12 0.039(4) 0.044(4) 0.051(5) -0.011(4) -0.006(3) 0.003(3) C13 0.063(9) 0.088(11) 0.030(9) 0.013(8) -0.007(7) 0.041(9) C14 0.081(6) 0.093(6) 0.101(8) 0.049(6) 0.032(6) 0.035(5) C15 0.107(7) 0.114(7) 0.139(11) 0.093(8) 0.083(8) 0.081(6) C16 0.073(11) 0.055(9) 0.079(13) 0.028(9) 0.020(9) 0.030(8) C17 0.028(7) 0.050(8) 0.064(10) 0.002(7) 0.000(7) 0.001(6) C18 0.069(9) 0.064(8) 0.033(9) 0.003(7) -0.016(7) 0.046(7) C13' 0.049(7) 0.054(8) 0.029(8) 0.010(6) 0.017(6) 0.024(6) C16' 0.031(7) 0.082(10) 0.010(7) 0.005(7) 0.011(5) 0.035(7) C17' 0.031(7) 0.063(8) 0.048(9) -0.003(7) 0.004(6) 0.011(6) C18' 0.035(7) 0.050(7) 0.026(8) 0.006(6) -0.011(6) 0.003(6) C19 0.043(4) 0.137(7) 0.026(4) 0.025(4) 0.009(3) 0.045(4) C20 0.042(4) 0.089(5) 0.037(5) 0.017(4) 0.007(4) 0.002(4) C21 0.049(4) 0.197(10) 0.031(5) 0.013(6) 0.016(4) 0.035(5) C22 0.061(6) 0.105(8) 0.078(7) -0.026(6) -0.005(5) 0.048(5) C25 0.130(8) 0.103(6) 0.026(5) 0.009(4) 0.007(5) 0.096(6) C27 0.073(11) 0.088(11) 0.066(13) 0.018(9) -0.006(9) 0.057(9) C23' 0.043(7) 0.059(8) 0.032(8) 0.020(6) 0.022(6) 0.018(6) C24' 0.050(8) 0.073(9) 0.046(10) 0.017(7) 0.016(7) 0.031(7) C26' 0.038(7) 0.051(8) 0.042(9) 0.007(7) -0.017(7) -0.002(6) C27' 0.036(8) 0.023(7) 0.082(14) -0.026(7) -0.033(8) 0.012(6) C28 0.046(4) 0.050(4) 0.022(4) 0.008(3) 0.011(3) 0.020(3) C29 0.163(8) 0.040(4) 0.050(5) 0.004(4) 0.047(5) 0.018(4) C30 0.224(11) 0.043(4) 0.048(6) 0.014(4) 0.057(7) 0.046(6) C32 0.050(4) 0.122(6) 0.018(4) 0.026(4) 0.009(3) 0.044(4) C33 0.035(3) 0.055(4) 0.032(4) 0.010(3) 0.009(3) 0.011(3) C34 0.041(4) 0.067(4) 0.027(4) 0.011(3) 0.002(3) 0.018(3) C35 0.038(7) 0.057(8) 0.018(7) 0.020(6) 0.006(6) 0.010(6) C36 0.053(8) 0.063(8) 0.038(9) 0.018(7) 0.020(7) 0.024(6) C37 0.055(8) 0.048(7) 0.033(8) 0.015(6) 0.004(6) 0.016(6) C35' 0.037(7) 0.042(7) 0.025(8) 0.003(6) 0.012(6) 0.015(6) C36' 0.026(6) 0.051(7) 0.041(9) 0.010(6) -0.001(6) 0.007(5) C37' 0.039(7) 0.040(7) 0.025(7) 0.002(5) 0.001(6) 0.013(5) C38 0.032(3) 0.057(4) 0.038(4) 0.006(3) 0.012(3) 0.017(3) C39 0.036(3) 0.075(5) 0.039(5) 0.008(3) 0.008(3) 0.020(3) C40 0.053(4) 0.101(6) 0.037(5) 0.026(4) 0.012(4) 0.034(4) N1' 0.026(5) 0.079(8) 0.021(6) 0.005(5) 0.002(5) 0.041(5) N1 0.057(3) 0.058(3) 0.057(3) 0.0043(11) 0.0138(12) 0.0082(11) N2 0.098(5) 0.074(4) 0.027(4) 0.010(3) 0.033(3) 0.055(3) N3 0.047(3) 0.036(3) 0.027(3) 0.004(2) 0.001(3) 0.012(2) N4 0.033(3) 0.051(3) 0.025(3) 0.008(2) 0.004(2) 0.014(2) N5 0.037(3) 0.036(3) 0.025(3) 0.008(2) 0.004(2) 0.003(2) N6 0.069(4) 0.257(10) 0.033(4) 0.043(5) 0.013(4) 0.101(5) N7 0.031(3) 0.072(3) 0.031(3) 0.007(3) 0.007(3) 0.004(2) O1 0.050(3) 0.048(3) 0.059(3) -0.021(2) 0.004(2) 0.000(2) O2 0.032(2) 0.050(2) 0.041(3) -0.002(2) -0.005(2) -0.007(2) O3 0.047(2) 0.038(2) 0.045(3) 0.014(2) -0.003(2) -0.016(2) O4 0.048(3) 0.063(3) 0.032(3) 0.012(2) -0.011(2) -0.018(2) O5 0.085(3) 0.047(3) 0.062(4) -0.016(2) 0.020(3) -0.018(3) O6 0.082(3) 0.052(3) 0.039(3) -0.004(2) -0.021(3) 0.008(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 2.079(3) 2_567 ? Co1 O3 2.079(3) . ? Co1 N3 2.154(5) 2_567 ? Co1 N3 2.154(5) . ? Co1 N5 2.168(5) 1_556 ? Co1 N5 2.168(5) 2_566 ? Co2 O2 1.980(3) 2_457 ? Co2 O4 1.992(5) . ? Co2 O6 2.015(4) . ? Co2 N7 2.065(5) 2_657 ? Co2 O5 2.377(5) . ? Co2 C12 2.518(7) . ? C1 C2 1.364(7) . ? C1 C6 1.387(7) . ? C1 C7 1.517(7) . ? C2 C3 1.400(7) . ? C2 H2 0.9300 . ? C3 C4 1.368(8) . ? C3 H3 0.9300 . ? C4 C5 1.367(8) . ? C4 C8 1.520(7) . ? C5 C6 1.390(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O3 1.234(6) . ? C7 O4 1.257(6) . ? C8 O1 1.225(7) . ? C8 O2 1.286(7) . ? C9 C10 1.368(9) . ? C9 C11 1.381(8) 2_568 ? C9 H9 0.9300 . ? C10 C11 1.384(8) . ? C10 C12 1.509(9) . ? C11 C9 1.381(8) 2_568 ? C11 H11 0.9300 . ? C12 O5 1.232(7) . ? C12 O6 1.263(8) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 N1 1.402(13) . ? C13 C13' 1.507(15) . ? C14 C13' 1.298(14) . ? C14 C15 1.3900 . ? C15 C16' 1.166(13) . ? C15 C16 1.3900 . ? C16 C16' 1.203(16) . ? C16 C17 1.3900 . ? C16 N6 1.509(9) . ? C17 C18 1.3900 . ? C13' C18' 1.388(16) . ? C13' N1' 1.449(15) . ? C13' N1 1.831(17) . ? C16' C17' 1.381(18) . ? C16' N6 1.613(15) . ? C17' C18' 1.388(16) . ? C19 N7 1.322(8) . ? C19 N6 1.361(9) . ? C19 H19 0.9300 . ? C20 C21 1.342(10) . ? C20 N7 1.372(8) . ? C20 H20 0.9300 . ? C21 N6 1.346(10) . ? C21 H21 0.9300 . ? C22 C27' 1.111(13) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C22 N1 1.463(14) . ? C22 C26' 1.771(16) . ? C23 C27' 0.913(19) . ? C23 C23' 1.304(15) . ? C23 C24 1.3900 . ? C23 C26' 1.899(14) . ? C23 C24' 1.904(17) . ? C24 C24' 1.028(15) . ? C24 C25 1.3900 . ? C24 C26' 1.688(13) . ? C24 C23' 1.721(16) . ? C25 C26' 1.273(15) . ? C25 N2 1.336(8) . ? C25 C26 1.3900 . ? C25 C24' 1.791(16) . ? C26 C26' 1.073(13) . ? C26 C27 1.3900 . ? C27 C26' 1.382(14) . ? C23' C27' 1.362(18) . ? C23' C24' 1.425(18) . ? C27' N1' 1.46(2) . ? C27' N1 1.763(19) . ? C28 N3 1.314(7) . ? C28 N2 1.338(8) . ? C28 H28 0.9300 . ? C29 C30 1.345(9) . ? C29 N3 1.362(8) . ? C29 H29 0.9300 . ? C30 N2 1.359(7) . ? C30 H30 0.9300 . ? C32 C33 1.3382 . ? C32 N4 1.422(5) . ? C32 C37 1.4781 . ? C32 C37' 1.5133 . ? C33 C34 1.3730 . ? C34 C35' 1.4206 . ? C34 C35 1.4659 . ? C35 C35' 1.0187 . ? C35 C36 1.3683 . ? C35 N1 1.401(13) . ? C35 N1' 1.813(10) . ? C35 C36' 1.8685 . ? C36 C37 1.4132 . ? C36 C36' 1.6460 . ? C36 C35' 1.9116 . ? C37 C37' 1.3762 . ? C35' C36' 1.3860 . ? C35' N1' 1.406(10) . ? C35' N1 1.796(13) . ? C36' C37' 1.4028 . ? C38 N5 1.295(5) . ? C38 N4 1.362(5) . ? C38 H38 0.9300 . ? C39 C40 1.356(9) . ? C39 N4 1.361(8) . ? C39 H39 0.9300 . ? C40 N5 1.378(8) . ? C40 H40 0.9300 . ? N1' N1 1.265(13) . ? N5 Co1 2.168(4) 1_554 ? N7 Co2 2.065(5) 2_657 ? O2 Co2 1.980(3) 2_457 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O3 180.0(2) 2_567 . ? O3 Co1 N3 88.59(18) 2_567 2_567 ? O3 Co1 N3 91.41(18) . 2_567 ? O3 Co1 N3 91.41(18) 2_567 . ? O3 Co1 N3 88.59(18) . . ? N3 Co1 N3 180.000(1) 2_567 . ? O3 Co1 N5 82.65(16) 2_567 1_556 ? O3 Co1 N5 97.35(16) . 1_556 ? N3 Co1 N5 93.18(18) 2_567 1_556 ? N3 Co1 N5 86.82(18) . 1_556 ? O3 Co1 N5 97.35(16) 2_567 2_566 ? O3 Co1 N5 82.65(16) . 2_566 ? N3 Co1 N5 86.82(18) 2_567 2_566 ? N3 Co1 N5 93.18(18) . 2_566 ? N5 Co1 N5 180.000(1) 1_556 2_566 ? O2 Co2 O4 110.83(17) 2_457 . ? O2 Co2 O6 142.9(2) 2_457 . ? O4 Co2 O6 95.4(2) . . ? O2 Co2 N7 101.67(19) 2_457 2_657 ? O4 Co2 N7 90.7(2) . 2_657 ? O6 Co2 N7 103.80(19) . 2_657 ? O2 Co2 O5 95.35(16) 2_457 . ? O4 Co2 O5 153.24(15) . . ? O6 Co2 O5 58.78(19) . . ? N7 Co2 O5 89.2(2) 2_657 . ? O2 Co2 C12 120.6(2) 2_457 . ? O4 Co2 C12 124.9(2) . . ? O6 Co2 C12 29.8(2) . . ? N7 Co2 C12 97.0(2) 2_657 . ? O5 Co2 C12 28.97(19) . . ? C2 C1 C6 119.6(5) . . ? C2 C1 C7 121.8(5) . . ? C6 C1 C7 118.5(5) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 C8 119.5(5) . . ? C3 C4 C8 119.5(5) . . ? C4 C5 C6 120.1(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.6(5) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? O3 C7 O4 123.8(5) . . ? O3 C7 C1 116.6(5) . . ? O4 C7 C1 119.6(5) . . ? O1 C8 O2 121.9(5) . . ? O1 C8 C4 122.0(6) . . ? O2 C8 C4 116.0(6) . . ? C10 C9 C11 120.8(6) . 2_568 ? C10 C9 H9 119.6 . . ? C11 C9 H9 119.6 2_568 . ? C9 C10 C11 119.7(6) . . ? C9 C10 C12 120.4(6) . . ? C11 C10 C12 119.8(7) . . ? C9 C11 C10 119.5(6) 2_568 . ? C9 C11 H11 120.3 2_568 . ? C10 C11 H11 120.3 . . ? O5 C12 O6 121.6(6) . . ? O5 C12 C10 120.3(7) . . ? O6 C12 C10 118.0(6) . . ? O5 C12 Co2 69.1(4) . . ? O6 C12 Co2 52.5(3) . . ? C10 C12 Co2 169.8(6) . . ? C14 C13 C18 120.0 . . ? C14 C13 N1 116.0(7) . . ? C18 C13 N1 122.8(7) . . ? C14 C13 C13' 53.0(6) . . ? C18 C13 C13' 129.3(6) . . ? N1 C13 C13' 77.9(7) . . ? C13' C14 C15 125.0(7) . . ? C13' C14 C13 68.1(7) . . ? C15 C14 C13 120.0 . . ? C16' C15 C16 55.3(8) . . ? C16' C15 C14 119.5(8) . . ? C16 C15 C14 120.0 . . ? C16' C16 C15 52.9(6) . . ? C16' C16 C17 120.2(7) . . ? C15 C16 C17 120.0 . . ? C16' C16 N6 72.0(8) . . ? C15 C16 N6 109.5(6) . . ? C17 C16 N6 124.6(6) . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C14 C13' C18' 113.5(11) . . ? C14 C13' N1' 129.0(11) . . ? C18' C13' N1' 117.5(11) . . ? C14 C13' C13 58.9(6) . . ? C18' C13' C13 122.0(10) . . ? N1' C13' C13 91.9(8) . . ? C14 C13' N1 96.9(9) . . ? C18' C13' N1 134.9(11) . . ? N1' C13' N1 43.4(6) . . ? C13 C13' N1 48.5(5) . . ? C15 C16' C16 71.8(8) . . ? C15 C16' C17' 118.4(13) . . ? C16 C16' C17' 139.0(12) . . ? C15 C16' N6 116.0(10) . . ? C16 C16' N6 62.8(8) . . ? C17' C16' N6 125.6(11) . . ? C16' C17' C18' 119.3(12) . . ? C13' C18' C17' 118.7(11) . . ? N7 C19 N6 109.4(6) . . ? N7 C19 H19 125.3 . . ? N6 C19 H19 125.3 . . ? C21 C20 N7 109.8(7) . . ? C21 C20 H20 125.1 . . ? N7 C20 H20 125.1 . . ? C20 C21 N6 106.5(7) . . ? C20 C21 H21 126.8 . . ? N6 C21 H21 126.8 . . ? C27' C22 C23 41.0(10) . . ? C27' C22 C27 139.0(9) . . ? C23 C22 C27 120.0 . . ? C27' C22 N1 85.3(12) . . ? C23 C22 N1 115.0(8) . . ? C27 C22 N1 125.0(8) . . ? C27' C22 C26' 108.1(11) . . ? C23 C22 C26' 72.7(4) . . ? C27 C22 C26' 50.1(4) . . ? N1 C22 C26' 162.9(9) . . ? C27' C23 C23' 73.5(12) . . ? C27' C23 C22 52.9(8) . . ? C23' C23 C22 116.7(9) . . ? C27' C23 C24 139.5(11) . . ? C23' C23 C24 79.4(8) . . ? C22 C23 C24 120.0 . . ? C27' C23 C26' 109.4(10) . . ? C23' C23 C26' 118.6(8) . . ? C22 C23 C26' 62.9(5) . . ? C24 C23 C26' 59.4(5) . . ? C27' C23 C24' 111.7(12) . . ? C23' C23 C24' 48.5(7) . . ? C22 C23 C24' 121.7(5) . . ? C24 C23 C24' 31.8(5) . . ? C26' C23 C24' 78.3(7) . . ? C24' C24 C25 94.3(10) . . ? C24' C24 C23 102.8(11) . . ? C25 C24 C23 120.0 . . ? C24' C24 C26' 122.4(11) . . ? C25 C24 C26' 47.7(5) . . ? C23 C24 C26' 75.5(6) . . ? C24' C24 C23' 55.8(10) . . ? C25 C24 C23' 127.2(6) . . ? C23 C24 C23' 48.1(6) . . ? C26' C24 C23' 108.7(8) . . ? C26' C25 N2 141.4(9) . . ? C26' C25 C24 78.5(6) . . ? N2 C25 C24 122.9(7) . . ? C26' C25 C26 47.3(6) . . ? N2 C25 C26 116.2(7) . . ? C24 C25 C26 120.0 . . ? C26' C25 C24' 101.9(9) . . ? N2 C25 C24' 113.2(7) . . ? C24 C25 C24' 34.9(5) . . ? C26 C25 C24' 124.0(6) . . ? C26' C26 C25 60.7(8) . . ? C26' C26 C27 66.8(8) . . ? C25 C26 C27 120.0 . . ? C26' C27 C26 45.5(6) . . ? C26' C27 C22 79.4(6) . . ? C26 C27 C22 120.0 . . ? C23 C23' C27' 40.0(9) . . ? C23 C23' C24' 88.3(10) . . ? C27' C23' C24' 118.6(13) . . ? C23 C23' C24 52.5(5) . . ? C27' C23' C24 88.5(10) . . ? C24' C23' C24 36.6(7) . . ? C24 C24' C23' 87.5(12) . . ? C24 C24' C25 50.7(7) . . ? C23' C24' C25 120.0(11) . . ? C24 C24' C23 45.4(7) . . ? C23' C24' C23 43.2(7) . . ? C25 C24' C23 81.3(6) . . ? C26 C26' C25 72.1(9) . . ? C26 C26' C27 67.6(7) . . ? C25 C26' C27 130.1(10) . . ? C26 C26' C24 119.7(11) . . ? C25 C26' C24 53.8(5) . . ? C27 C26' C24 129.5(10) . . ? C26 C26' C22 113.4(10) . . ? C25 C26' C22 131.2(10) . . ? C27 C26' C22 50.5(5) . . ? C24 C26' C22 88.2(7) . . ? C26 C26' C23 136.8(11) . . ? C25 C26' C23 96.7(7) . . ? C27 C26' C23 93.0(8) . . ? C24 C26' C23 45.1(3) . . ? C22 C26' C23 44.3(4) . . ? C23 C27' C22 86.2(14) . . ? C23 C27' C23' 66.5(12) . . ? C22 C27' C23' 135.9(16) . . ? C23 C27' N1' 135.1(13) . . ? C22 C27' N1' 100.7(11) . . ? C23' C27' N1' 123.2(13) . . ? C23 C27' N1 125.0(13) . . ? C22 C27' N1 55.8(8) . . ? C23' C27' N1 166.9(15) . . ? N1' C27' N1 45.0(7) . . ? N3 C28 N2 111.5(6) . . ? N3 C28 H28 124.3 . . ? N2 C28 H28 124.3 . . ? C30 C29 N3 110.9(6) . . ? C30 C29 H29 124.5 . . ? N3 C29 H29 124.5 . . ? C29 C30 N2 105.3(4) . . ? C29 C30 H30 127.3 . . ? N2 C30 H30 127.3 . . ? C33 C32 N4 123.5(2) . . ? C33 C32 C37 115.5 . . ? N4 C32 C37 116.0(2) . . ? C33 C32 C37' 113.5 . . ? N4 C32 C37' 114.1(2) . . ? C37 C32 C37' 54.8 . . ? C32 C33 C34 124.1 . . ? C33 C34 C35' 117.5 . . ? C33 C34 C35 116.2 . . ? C35' C34 C35 41.3 . . ? C35' C35 C36 105.5 . . ? C35' C35 N1 94.5(5) . . ? C36 C35 N1 123.4(5) . . ? C35' C35 C34 67.0 . . ? C36 C35 C34 120.6 . . ? N1 C35 C34 116.0(5) . . ? C35' C35 N1' 50.5(4) . . ? C36 C35 N1' 125.2(3) . . ? N1 C35 N1' 44.1(5) . . ? C34 C35 N1' 95.9(3) . . ? C35' C35 C36' 46.8 . . ? C36 C35 C36' 58.7 . . ? N1 C35 C36' 119.2(5) . . ? C34 C35 C36' 92.0 . . ? N1' C35 C36' 82.8(4) . . ? C35 C36 C37 119.5 . . ? C35 C36 C36' 76.0 . . ? C37 C36 C36' 84.3 . . ? C35 C36 C35' 30.9 . . ? C37 C36 C35' 108.0 . . ? C36' C36 C35' 45.1 . . ? C37' C37 C36 95.2 . . ? C37' C37 C32 63.9 . . ? C36 C37 C32 119.0 . . ? C35 C35' C36' 100.9 . . ? C35 C35' N1' 95.5(5) . . ? C36' C35' N1' 121.3(4) . . ? C35 C35' C34 71.7 . . ? C36' C35' C34 118.8 . . ? N1' C35' C34 119.9(4) . . ? C35 C35' N1 51.1(4) . . ? C36' C35' N1 125.1(4) . . ? N1' C35' N1 44.5(5) . . ? C34 C35' N1 97.6(4) . . ? C35 C35' C36 43.6 . . ? C36' C35' C36 57.3 . . ? N1' C35' C36 116.4(4) . . ? C34 C35' C36 94.1 . . ? N1 C35' C36 82.2(4) . . ? C35' C36' C37' 122.2 . . ? C35' C36' C36 77.6 . . ? C37' C36' C36 84.6 . . ? C35' C36' C35 32.4 . . ? C37' C36' C35 109.6 . . ? C36 C36' C35 45.3 . . ? C37 C37' C36' 95.7 . . ? C37 C37' C32 61.3 . . ? C36' C37' C32 116.6 . . ? N5 C38 N4 113.1(4) . . ? N5 C38 H38 123.5 . . ? N4 C38 H38 123.4 . . ? C40 C39 N4 106.2(6) . . ? C40 C39 H39 126.9 . . ? N4 C39 H39 126.9 . . ? C39 C40 N5 110.5(6) . . ? C39 C40 H40 124.7 . . ? N5 C40 H40 124.7 . . ? N1 N1' C35' 84.3(8) . . ? N1 N1' C13' 84.6(9) . . ? C35' N1' C13' 123.8(9) . . ? N1 N1' C27' 80.3(9) . . ? C35' N1' C27' 120.4(8) . . ? C13' N1' C27' 111.6(10) . . ? N1 N1' C35 50.4(7) . . ? C35' N1' C35 34.0(2) . . ? C13' N1' C35 110.3(8) . . ? C27' N1' C35 109.1(7) . . ? N1' N1 C35 85.6(8) . . ? N1' N1 C13 105.5(9) . . ? C35 N1 C13 121.5(10) . . ? N1' N1 C22 93.5(10) . . ? C35 N1 C22 127.2(9) . . ? C13 N1 C22 109.6(10) . . ? N1' N1 C27' 54.7(8) . . ? C35 N1 C27' 114.8(9) . . ? C13 N1 C27' 118.1(10) . . ? C22 N1 C27' 38.9(7) . . ? N1' N1 C35' 51.2(6) . . ? C35 N1 C35' 34.4(3) . . ? C13 N1 C35' 126.1(9) . . ? C22 N1 C35' 118.5(8) . . ? C27' N1 C35' 88.6(8) . . ? N1' N1 C13' 52.0(7) . . ? C35 N1 C13' 111.7(8) . . ? C13 N1 C13' 53.6(6) . . ? C22 N1 C13' 108.5(9) . . ? C27' N1 C13' 84.0(8) . . ? C35' N1 C13' 87.9(6) . . ? C25 N2 C28 130.2(6) . . ? C25 N2 C30 122.1(5) . . ? C28 N2 C30 107.6(5) . . ? C28 N3 C29 104.7(6) . . ? C28 N3 Co1 131.1(4) . . ? C29 N3 Co1 123.3(5) . . ? C39 N4 C38 105.9(4) . . ? C39 N4 C32 127.2(4) . . ? C38 N4 C32 126.9(4) . . ? C38 N5 C40 104.3(4) . . ? C38 N5 Co1 130.7(3) . 1_554 ? C40 N5 Co1 124.4(4) . 1_554 ? C21 N6 C19 108.3(7) . . ? C21 N6 C16 120.2(7) . . ? C19 N6 C16 121.2(7) . . ? C21 N6 C16' 122.3(8) . . ? C19 N6 C16' 126.3(8) . . ? C16 N6 C16' 45.2(5) . . ? C19 N7 C20 106.0(6) . . ? C19 N7 Co2 130.4(5) . 2_657 ? C20 N7 Co2 123.2(5) . 2_657 ? C8 O2 Co2 100.1(3) . 2_457 ? C7 O3 Co1 143.5(4) . . ? C7 O4 Co2 148.1(4) . . ? C12 O5 Co2 81.9(4) . . ? C12 O6 Co2 97.7(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 C6 C1 C2 C3 0.5(8) . . . . ? C7 C1 C2 C3 -179.6(5) . . . . ? C1 C2 C3 C4 -3.8(8) . . . . ? C2 C3 C4 C5 3.3(9) . . . . ? C2 C3 C4 C8 -171.1(5) . . . . ? C3 C4 C5 C6 0.5(9) . . . . ? C8 C4 C5 C6 174.9(6) . . . . ? C2 C1 C6 C5 3.3(9) . . . . ? C7 C1 C6 C5 -176.6(6) . . . . ? C4 C5 C6 C1 -3.9(9) . . . . ? C2 C1 C7 O3 151.8(6) . . . . ? C6 C1 C7 O3 -28.3(8) . . . . ? C2 C1 C7 O4 -27.3(8) . . . . ? C6 C1 C7 O4 152.6(6) . . . . ? C5 C4 C8 O1 165.7(6) . . . . ? C3 C4 C8 O1 -19.9(9) . . . . ? C5 C4 C8 O2 -17.7(9) . . . . ? C3 C4 C8 O2 156.8(6) . . . . ? C11 C9 C10 C11 1.6(10) 2_568 . . . ? C11 C9 C10 C12 178.5(6) 2_568 . . . ? C9 C10 C11 C9 -1.6(10) . . . 2_568 ? C12 C10 C11 C9 -178.5(6) . . . 2_568 ? C9 C10 C12 O5 -4.7(9) . . . . ? C11 C10 C12 O5 172.3(6) . . . . ? C9 C10 C12 O6 178.6(6) . . . . ? C11 C10 C12 O6 -4.4(9) . . . . ? C9 C10 C12 Co2 -161(2) . . . . ? C11 C10 C12 Co2 16(3) . . . . ? O2 Co2 C12 O5 32.6(4) 2_457 . . . ? O4 Co2 C12 O5 -171.3(3) . . . . ? O6 Co2 C12 O5 179.0(6) . . . . ? N7 Co2 C12 O5 -75.5(4) 2_657 . . . ? O2 Co2 C12 O6 -146.4(4) 2_457 . . . ? O4 Co2 C12 O6 9.7(5) . . . . ? N7 Co2 C12 O6 105.5(4) 2_657 . . . ? O5 Co2 C12 O6 -179.0(6) . . . . ? O2 Co2 C12 C10 -169(2) 2_457 . . . ? O4 Co2 C12 C10 -13(3) . . . . ? O6 Co2 C12 C10 -23(2) . . . . ? N7 Co2 C12 C10 83(2) 2_657 . . . ? O5 Co2 C12 C10 158(3) . . . . ? C18 C13 C14 C13' -118.7(8) . . . . ? N1 C13 C14 C13' 48.8(9) . . . . ? C18 C13 C14 C15 0.0 . . . . ? N1 C13 C14 C15 167.6(9) . . . . ? C13' C13 C14 C15 118.7(8) . . . . ? C13' C14 C15 C16' 18.4(12) . . . . ? C13 C14 C15 C16' -64.6(9) . . . . ? C13' C14 C15 C16 83.0(8) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C16' -107.0(9) . . . . ? C16' C15 C16 C17 107.0(9) . . . . ? C14 C15 C16 C17 0.0 . . . . ? C16' C15 C16 N6 -47.2(8) . . . . ? C14 C15 C16 N6 -154.2(8) . . . . ? C16' C16 C17 C18 61.9(7) . . . . ? C15 C16 C17 C18 0.0 . . . . ? N6 C16 C17 C18 150.1(9) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? N1 C13 C18 C17 -166.7(10) . . . . ? C13' C13 C18 C17 -64.9(7) . . . . ? C15 C14 C13' C18' 2.3(14) . . . . ? C13 C14 C13' C18' 114.4(11) . . . . ? C15 C14 C13' N1' -176.1(9) . . . . ? C13 C14 C13' N1' -63.9(12) . . . . ? C15 C14 C13' C13 -112.1(5) . . . . ? C15 C14 C13' N1 -143.6(6) . . . . ? C13 C14 C13' N1 -31.5(5) . . . . ? C18 C13 C13' C14 101.1(6) . . . . ? N1 C13 C13' C14 -136.2(8) . . . . ? C14 C13 C13' C18' -99.8(12) . . . . ? C18 C13 C13' C18' 1.3(15) . . . . ? N1 C13 C13' C18' 124.0(13) . . . . ? C14 C13 C13' N1' 135.7(10) . . . . ? C18 C13 C13' N1' -123.2(7) . . . . ? N1 C13 C13' N1' -0.5(9) . . . . ? C14 C13 C13' N1 136.2(8) . . . . ? C18 C13 C13' N1 -122.7(9) . . . . ? C14 C15 C16' C16 107.9(6) . . . . ? C16 C15 C16' C17' -136.5(14) . . . . ? C14 C15 C16' C17' -28.6(15) . . . . ? C16 C15 C16' N6 46.0(8) . . . . ? C14 C15 C16' N6 153.9(7) . . . . ? C17 C16 C16' C15 -106.5(6) . . . . ? N6 C16 C16' C15 133.3(7) . . . . ? C15 C16 C16' C17' 112.7(19) . . . . ? C17 C16 C16' C17' 6(2) . . . . ? N6 C16 C16' C17' -114.0(18) . . . . ? C15 C16 C16' N6 -133.3(7) . . . . ? C17 C16 C16' N6 120.1(7) . . . . ? C15 C16' C17' C18' 20.3(19) . . . . ? C16 C16' C17' C18' -74(2) . . . . ? N6 C16' C17' C18' -162.4(11) . . . . ? C14 C13' C18' C17' -9.9(17) . . . . ? N1' C13' C18' C17' 168.7(11) . . . . ? C13 C13' C18' C17' 56.9(17) . . . . ? N1 C13' C18' C17' 118.3(15) . . . . ? C16' C17' C18' C13' 0.1(19) . . . . ? N7 C20 C21 N6 1.5(10) . . . . ? C27 C22 C23 C27' -131.6(13) . . . . ? N1 C22 C23 C27' 47.7(13) . . . . ? C26' C22 C23 C27' -148.7(14) . . . . ? C27' C22 C23 C23' 38.6(13) . . . . ? C27 C22 C23 C23' -93.0(8) . . . . ? N1 C22 C23 C23' 86.3(10) . . . . ? C26' C22 C23 C23' -110.1(9) . . . . ? C27' C22 C23 C24 131.6(13) . . . . ? C27 C22 C23 C24 0.0 . . . . ? N1 C22 C23 C24 179.3(8) . . . . ? C26' C22 C23 C24 -17.1(4) . . . . ? C27' C22 C23 C26' 148.7(14) . . . . ? C27 C22 C23 C26' 17.1(4) . . . . ? N1 C22 C23 C26' -163.6(9) . . . . ? C27' C22 C23 C24' 94.4(14) . . . . ? C27 C22 C23 C24' -37.1(6) . . . . ? N1 C22 C23 C24' 142.1(10) . . . . ? C26' C22 C23 C24' -54.3(8) . . . . ? C27' C23 C24 C24' -36.2(16) . . . . ? C23' C23 C24 C24' 12.1(10) . . . . ? C22 C23 C24 C24' -102.8(10) . . . . ? C26' C23 C24 C24' -120.5(11) . . . . ? C27' C23 C24 C25 66.6(13) . . . . ? C23' C23 C24 C25 114.8(8) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C26' C23 C24 C25 -17.8(5) . . . . ? C24' C23 C24 C25 102.8(10) . . . . ? C27' C23 C24 C26' 84.3(13) . . . . ? C23' C23 C24 C26' 132.6(9) . . . . ? C22 C23 C24 C26' 17.8(5) . . . . ? C24' C23 C24 C26' 120.5(11) . . . . ? C27' C23 C24 C23' -48.3(14) . . . . ? C22 C23 C24 C23' -114.8(8) . . . . ? C26' C23 C24 C23' -132.6(9) . . . . ? C24' C23 C24 C23' -12.1(10) . . . . ? C24' C24 C25 C26' 131.1(12) . . . . ? C23 C24 C25 C26' 23.5(6) . . . . ? C23' C24 C25 C26' 81.6(9) . . . . ? C24' C24 C25 N2 -84.0(11) . . . . ? C23 C24 C25 N2 168.5(6) . . . . ? C26' C24 C25 N2 145.0(9) . . . . ? C23' C24 C25 N2 -133.5(8) . . . . ? C24' C24 C25 C26 107.5(10) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C26' C24 C25 C26 -23.5(6) . . . . ? C23' C24 C25 C26 58.0(7) . . . . ? C23 C24 C25 C24' -107.5(10) . . . . ? C26' C24 C25 C24' -131.1(12) . . . . ? C23' C24 C25 C24' -49.5(11) . . . . ? N2 C25 C26 C26' -137.0(11) . . . . ? C24 C25 C26 C26' 32.2(9) . . . . ? C24' C25 C26 C26' 73.4(11) . . . . ? C26' C25 C26 C27 -32.2(9) . . . . ? N2 C25 C26 C27 -169.3(5) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C24' C25 C26 C27 41.2(6) . . . . ? C25 C26 C27 C26' 30.4(8) . . . . ? C26' C26 C27 C22 -30.4(8) . . . . ? C25 C26 C27 C22 0.0 . . . . ? C27' C22 C27 C26' -69.9(16) . . . . ? C23 C22 C27 C26' -21.5(6) . . . . ? N1 C22 C27 C26' 159.3(10) . . . . ? C27' C22 C27 C26 -48.3(15) . . . . ? C23 C22 C27 C26 0.0 . . . . ? N1 C22 C27 C26 -179.2(9) . . . . ? C26' C22 C27 C26 21.5(6) . . . . ? C22 C23 C23' C27' -31.3(10) . . . . ? C24 C23 C23' C27' -149.6(9) . . . . ? C26' C23 C23' C27' -103.5(12) . . . . ? C24' C23 C23' C27' -141.2(12) . . . . ? C27' C23 C23' C24' 141.2(12) . . . . ? C22 C23 C23' C24' 109.9(8) . . . . ? C24 C23 C23' C24' -8.5(7) . . . . ? C26' C23 C23' C24' 37.7(12) . . . . ? C27' C23 C23' C24 149.6(9) . . . . ? C22 C23 C23' C24 118.4(3) . . . . ? C26' C23 C23' C24 46.2(8) . . . . ? C24' C23 C23' C24 8.5(7) . . . . ? C24' C24 C23' C23 -165.7(11) . . . . ? C25 C24 C23' C23 -99.3(7) . . . . ? C26' C24 C23' C23 -48.8(8) . . . . ? C24' C24 C23' C27' -146.8(13) . . . . ? C25 C24 C23' C27' -80.4(9) . . . . ? C23 C24 C23' C27' 19.0(6) . . . . ? C26' C24 C23' C27' -29.8(10) . . . . ? C25 C24 C23' C24' 66.4(12) . . . . ? C23 C24 C23' C24' 165.7(12) . . . . ? C26' C24 C23' C24' 116.9(12) . . . . ? C25 C24 C24' C23' -133.0(7) . . . . ? C23 C24 C24' C23' -10.8(9) . . . . ? C26' C24 C24' C23' -91.7(13) . . . . ? C23 C24 C24' C25 122.1(3) . . . . ? C26' C24 C24' C25 41.3(9) . . . . ? C23' C24 C24' C25 133.0(7) . . . . ? C25 C24 C24' C23 -122.1(3) . . . . ? C26' C24 C24' C23 -80.8(10) . . . . ? C23' C24 C24' C23 10.8(9) . . . . ? C23 C23' C24' C24 11.3(9) . . . . ? C27' C23' C24' C24 38.6(15) . . . . ? C23 C23' C24' C25 -29.6(12) . . . . ? C27' C23' C24' C25 -2.3(17) . . . . ? C24 C23' C24' C25 -40.8(7) . . . . ? C27' C23' C24' C23 27.3(9) . . . . ? C24 C23' C24' C23 -11.3(9) . . . . ? C26' C25 C24' C24 -49.0(11) . . . . ? N2 C25 C24' C24 114.7(10) . . . . ? C26 C25 C24' C24 -95.0(9) . . . . ? C26' C25 C24' C23' 8.5(13) . . . . ? N2 C25 C24' C23' 172.2(10) . . . . ? C24 C25 C24' C23' 57.6(11) . . . . ? C26 C25 C24' C23' -37.4(13) . . . . ? C26' C25 C24' C23 -11.4(8) . . . . ? N2 C25 C24' C23 152.2(6) . . . . ? C24 C25 C24' C23 37.6(5) . . . . ? C26 C25 C24' C23 -57.4(7) . . . . ? C27' C23 C24' C24 155.6(10) . . . . ? C23' C23 C24' C24 -164.1(13) . . . . ? C22 C23 C24' C24 96.8(9) . . . . ? C26' C23 C24' C24 49.2(9) . . . . ? C27' C23 C24' C23' -40.3(13) . . . . ? C22 C23 C24' C23' -99.1(11) . . . . ? C24 C23 C24' C23' 164.1(13) . . . . ? C26' C23 C24' C23' -146.7(10) . . . . ? C27' C23 C24' C25 114.1(10) . . . . ? C23' C23 C24' C25 154.4(11) . . . . ? C22 C23 C24' C25 55.2(7) . . . . ? C24 C23 C24' C25 -41.6(6) . . . . ? C26' C23 C24' C25 7.6(6) . . . . ? C27 C26 C26' C25 149.9(7) . . . . ? C25 C26 C26' C27 -149.9(7) . . . . ? C25 C26 C26' C24 -26.0(7) . . . . ? C27 C26 C26' C24 123.9(13) . . . . ? C25 C26 C26' C22 -127.9(11) . . . . ? C27 C26 C26' C22 22.0(5) . . . . ? C25 C26 C26' C23 -80.6(15) . . . . ? C27 C26 C26' C23 69.3(15) . . . . ? N2 C25 C26' C26 78.7(15) . . . . ? C24 C25 C26' C26 -151.9(7) . . . . ? C24' C25 C26' C26 -125.7(8) . . . . ? N2 C25 C26' C27 116.1(15) . . . . ? C24 C25 C26' C27 -114.5(14) . . . . ? C26 C25 C26' C27 37.4(8) . . . . ? C24' C25 C26' C27 -88.3(14) . . . . ? N2 C25 C26' C24 -129.4(13) . . . . ? C26 C25 C26' C24 151.9(7) . . . . ? C24' C25 C26' C24 26.2(6) . . . . ? N2 C25 C26' C22 -175.5(10) . . . . ? C24 C25 C26' C22 -46.2(9) . . . . ? C26 C25 C26' C22 105.7(13) . . . . ? C24' C25 C26' C22 -20.0(12) . . . . ? N2 C25 C26' C23 -144.1(12) . . . . ? C24 C25 C26' C23 -14.8(3) . . . . ? C26 C25 C26' C23 137.1(10) . . . . ? C24' C25 C26' C23 11.4(8) . . . . ? C22 C27 C26' C26 153.6(6) . . . . ? C26 C27 C26' C25 -38.7(10) . . . . ? C22 C27 C26' C25 114.9(14) . . . . ? C26 C27 C26' C24 -110.8(14) . . . . ? C22 C27 C26' C24 42.7(10) . . . . ? C26 C27 C26' C22 -153.6(6) . . . . ? C26 C27 C26' C23 -140.1(9) . . . . ? C22 C27 C26' C23 13.5(3) . . . . ? C24' C24 C26' C26 -32(2) . . . . ? C25 C24 C26' C26 31.1(9) . . . . ? C23 C24 C26' C26 -128.0(13) . . . . ? C23' C24 C26' C26 -92.6(15) . . . . ? C24' C24 C26' C25 -62.9(15) . . . . ? C23 C24 C26' C25 -159.1(5) . . . . ? C23' C24 C26' C25 -123.7(8) . . . . ? C24' C24 C26' C27 53(2) . . . . ? C25 C24 C26' C27 115.5(13) . . . . ? C23 C24 C26' C27 -43.6(11) . . . . ? C23' C24 C26' C27 -8.2(14) . . . . ? C24' C24 C26' C22 84.2(14) . . . . ? C25 C24 C26' C22 147.1(8) . . . . ? C23 C24 C26' C22 -12.0(3) . . . . ? C23' C24 C26' C22 23.4(8) . . . . ? C24' C24 C26' C23 96.2(13) . . . . ? C25 C24 C26' C23 159.1(5) . . . . ? C23' C24 C26' C23 35.4(7) . . . . ? C27' C22 C26' C26 112.9(12) . . . . ? C23 C22 C26' C26 133.9(11) . . . . ? C27 C22 C26' C26 -26.7(7) . . . . ? N1 C22 C26' C26 -107(3) . . . . ? C27' C22 C26' C25 26.8(14) . . . . ? C23 C22 C26' C25 47.8(10) . . . . ? C27 C22 C26' C25 -112.8(13) . . . . ? N1 C22 C26' C25 167(3) . . . . ? C27' C22 C26' C27 139.6(9) . . . . ? C23 C22 C26' C27 160.6(5) . . . . ? N1 C22 C26' C27 -80(3) . . . . ? C27' C22 C26' C24 -8.8(10) . . . . ? C23 C22 C26' C24 12.1(3) . . . . ? C27 C22 C26' C24 -148.4(8) . . . . ? N1 C22 C26' C24 132(3) . . . . ? C27' C22 C26' C23 -21.0(9) . . . . ? C27 C22 C26' C23 -160.6(5) . . . . ? N1 C22 C26' C23 120(3) . . . . ? C27' C23 C26' C26 -49(2) . . . . ? C23' C23 C26' C26 32(2) . . . . ? C22 C23 C26' C26 -74.9(16) . . . . ? C24 C23 C26' C26 87.8(17) . . . . ? C24' C23 C26' C26 60.2(18) . . . . ? C27' C23 C26' C25 -119.9(13) . . . . ? C23' C23 C26' C25 -38.6(13) . . . . ? C22 C23 C26' C25 -145.9(8) . . . . ? C24 C23 C26' C25 16.9(4) . . . . ? C24' C23 C26' C25 -10.7(8) . . . . ? C27' C23 C26' C27 11.1(13) . . . . ? C23' C23 C26' C27 92.4(12) . . . . ? C22 C23 C26' C27 -14.9(4) . . . . ? C24 C23 C26' C27 147.8(8) . . . . ? C24' C23 C26' C27 120.2(9) . . . . ? C27' C23 C26' C24 -136.7(11) . . . . ? C23' C23 C26' C24 -55.5(10) . . . . ? C22 C23 C26' C24 -162.7(4) . . . . ? C24' C23 C26' C24 -27.6(6) . . . . ? C27' C23 C26' C22 26.0(11) . . . . ? C23' C23 C26' C22 107.3(10) . . . . ? C24 C23 C26' C22 162.7(4) . . . . ? C24' C23 C26' C22 135.1(6) . . . . ? C23' C23 C27' C22 -144.5(10) . . . . ? C24 C23 C27' C22 -94.5(12) . . . . ? C26' C23 C27' C22 -29.3(12) . . . . ? C24' C23 C27' C22 -114.1(8) . . . . ? C22 C23 C27' C23' 144.5(10) . . . . ? C24 C23 C27' C23' 49.9(13) . . . . ? C26' C23 C27' C23' 115.1(10) . . . . ? C24' C23 C27' C23' 30.3(9) . . . . ? C23' C23 C27' N1' 114.2(18) . . . . ? C22 C23 C27' N1' -101.4(18) . . . . ? C24 C23 C27' N1' 164.1(11) . . . . ? C26' C23 C27' N1' -130.7(15) . . . . ? C24' C23 C27' N1' 144.5(15) . . . . ? C23' C23 C27' N1 172.8(15) . . . . ? C22 C23 C27' N1 -42.7(9) . . . . ? C24 C23 C27' N1 -137.3(12) . . . . ? C26' C23 C27' N1 -72.1(16) . . . . ? C24' C23 C27' N1 -156.8(11) . . . . ? C27 C22 C27' C23 80.7(15) . . . . ? N1 C22 C27' C23 -137.8(11) . . . . ? C26' C22 C27' C23 31.4(13) . . . . ? C23 C22 C27' C23' -50.0(18) . . . . ? C27 C22 C27' C23' 31(3) . . . . ? N1 C22 C27' C23' 172.2(19) . . . . ? C26' C22 C27' C23' -19(2) . . . . ? C23 C22 C27' N1' 135.2(14) . . . . ? C27 C22 C27' N1' -144.1(9) . . . . ? N1 C22 C27' N1' -2.5(9) . . . . ? C26' C22 C27' N1' 166.7(8) . . . . ? C23 C22 C27' N1 137.8(11) . . . . ? C27 C22 C27' N1 -141.6(14) . . . . ? C26' C22 C27' N1 169.2(9) . . . . ? C24' C23' C27' C23 -45.5(13) . . . . ? C24 C23' C27' C23 -23.7(7) . . . . ? C23 C23' C27' C22 56.5(19) . . . . ? C24' C23' C27' C22 11(3) . . . . ? C24 C23' C27' C22 32.8(19) . . . . ? C23 C23' C27' N1' -129.7(15) . . . . ? C24' C23' C27' N1' -175.3(11) . . . . ? C24 C23' C27' N1' -153.4(12) . . . . ? C23 C23' C27' N1 -153(5) . . . . ? C24' C23' C27' N1 161(4) . . . . ? C24 C23' C27' N1 -177(5) . . . . ? N3 C29 C30 N2 -1.5(8) . . . . ? N4 C32 C33 C34 -178.7(2) . . . . ? C37 C32 C33 C34 27.4 . . . . ? C37' C32 C33 C34 -33.3 . . . . ? C32 C33 C34 C35' 25.4 . . . . ? C32 C33 C34 C35 -21.2 . . . . ? C33 C34 C35 C35' 102.6 . . . . ? C33 C34 C35 C36 7.7 . . . . ? C35' C34 C35 C36 -94.9 . . . . ? C33 C34 C35 N1 -173.8(5) . . . . ? C35' C34 C35 N1 83.5(5) . . . . ? C33 C34 C35 N1' 145.0(4) . . . . ? C35' C34 C35 N1' 42.4(4) . . . . ? C33 C34 C35 C36' 62.1 . . . . ? C35' C34 C35 C36' -40.5 . . . . ? C35' C35 C36 C37 -75.2 . . . . ? N1 C35 C36 C37 178.5(6) . . . . ? C34 C35 C36 C37 -3.2 . . . . ? N1' C35 C36 C37 -127.5(4) . . . . ? C36' C35 C36 C37 -75.0 . . . . ? C35' C35 C36 C36' -0.2 . . . . ? N1 C35 C36 C36' -106.4(6) . . . . ? C34 C35 C36 C36' 71.9 . . . . ? N1' C35 C36 C36' -52.5(4) . . . . ? N1 C35 C36 C35' -106.2(6) . . . . ? C34 C35 C36 C35' 72.1 . . . . ? N1' C35 C36 C35' -52.3(4) . . . . ? C36' C35 C36 C35' 0.2 . . . . ? C35 C36 C37 C37' 72.6 . . . . ? C36' C36 C37 C37' 2.2 . . . . ? C35' C36 C37 C37' 41.1 . . . . ? C35 C36 C37 C32 9.6 . . . . ? C36' C36 C37 C32 -60.8 . . . . ? C35' C36 C37 C32 -21.9 . . . . ? C33 C32 C37 C37' -101.9 . . . . ? N4 C32 C37 C37' 102.3(2) . . . . ? C33 C32 C37 C36 -20.8 . . . . ? N4 C32 C37 C36 -176.7(2) . . . . ? C37' C32 C37 C36 81.0 . . . . ? C36 C35 C35' C36' 0.2 . . . . ? N1 C35 C35' C36' 126.7(5) . . . . ? C34 C35 C35' C36' -116.9 . . . . ? N1' C35 C35' C36' 123.4(4) . . . . ? C36 C35 C35' N1' -123.2(4) . . . . ? N1 C35 C35' N1' 3.3(6) . . . . ? C34 C35 C35' N1' 119.7(4) . . . . ? C36' C35 C35' N1' -123.4(4) . . . . ? C36 C35 C35' C34 117.1 . . . . ? N1 C35 C35' C34 -116.4(5) . . . . ? N1' C35 C35' C34 -119.7(4) . . . . ? C36' C35 C35' C34 116.9 . . . . ? C36 C35 C35' N1 -126.5(5) . . . . ? C34 C35 C35' N1 116.4(5) . . . . ? N1' C35 C35' N1 -3.3(6) . . . . ? C36' C35 C35' N1 -126.7(5) . . . . ? N1 C35 C35' C36 126.5(5) . . . . ? C34 C35 C35' C36 -117.1 . . . . ? N1' C35 C35' C36 123.2(4) . . . . ? C36' C35 C35' C36 -0.2 . . . . ? C33 C34 C35' C35 -99.3 . . . . ? C33 C34 C35' C36' -6.7 . . . . ? C35 C34 C35' C36' 92.6 . . . . ? C33 C34 C35' N1' 174.9(5) . . . . ? C35 C34 C35' N1' -85.8(5) . . . . ? C33 C34 C35' N1 -144.0(4) . . . . ? C35 C34 C35' N1 -44.7(4) . . . . ? C33 C34 C35' C36 -61.3 . . . . ? C35 C34 C35' C36 38.0 . . . . ? C37 C36 C35' C35 117.8 . . . . ? C36' C36 C35' C35 179.7 . . . . ? C35 C36 C35' C36' -179.7 . . . . ? C37 C36 C35' C36' -61.9 . . . . ? C35 C36 C35' N1' 68.5(5) . . . . ? C37 C36 C35' N1' -173.7(5) . . . . ? C36' C36 C35' N1' -111.8(5) . . . . ? C35 C36 C35' C34 -57.9 . . . . ? C37 C36 C35' C34 59.9 . . . . ? C36' C36 C35' C34 121.8 . . . . ? C35 C36 C35' N1 39.2(4) . . . . ? C37 C36 C35' N1 156.9(4) . . . . ? C36' C36 C35' N1 -141.1(4) . . . . ? C35 C35' C36' C37' 75.3 . . . . ? N1' C35' C36' C37' 178.6(5) . . . . ? C34 C35' C36' C37' 0.2 . . . . ? N1 C35' C36' C37' 124.9(5) . . . . ? C36 C35' C36' C37' 75.4 . . . . ? C35 C35' C36' C36 -0.2 . . . . ? N1' C35' C36' C36 103.1(5) . . . . ? C34 C35' C36' C36 -75.2 . . . . ? N1 C35' C36' C36 49.5(5) . . . . ? N1' C35' C36' C35 103.3(5) . . . . ? C34 C35' C36' C35 -75.0 . . . . ? N1 C35' C36' C35 49.7(5) . . . . ? C36 C35' C36' C35 0.2 . . . . ? C35 C36 C36' C35' 0.1 . . . . ? C37 C36 C36' C35' 122.5 . . . . ? C35 C36 C36' C37' -124.5 . . . . ? C37 C36 C36' C37' -2.2 . . . . ? C35' C36 C36' C37' -124.7 . . . . ? C37 C36 C36' C35 122.4 . . . . ? C35' C36 C36' C35 -0.1 . . . . ? C36 C35 C36' C35' -179.7 . . . . ? N1 C35 C36' C35' -66.3(6) . . . . ? C34 C35 C36' C35' 55.2 . . . . ? N1' C35 C36' C35' -40.5(3) . . . . ? C35' C35 C36' C37' -119.7 . . . . ? C36 C35 C36' C37' 60.5 . . . . ? N1 C35 C36' C37' 174.0(6) . . . . ? C34 C35 C36' C37' -64.5 . . . . ? N1' C35 C36' C37' -160.2(3) . . . . ? C35' C35 C36' C36 179.7 . . . . ? N1 C35 C36' C36 113.5(6) . . . . ? C34 C35 C36' C36 -125.1 . . . . ? N1' C35 C36' C36 139.2(3) . . . . ? C36 C37 C37' C36' -2.6 . . . . ? C32 C37 C37' C36' 117.3 . . . . ? C36 C37 C37' C32 -119.8 . . . . ? C35' C36' C37' C37 -69.5 . . . . ? C36 C36' C37' C37 2.2 . . . . ? C35 C36' C37' C37 -36.2 . . . . ? C35' C36' C37' C32 -8.8 . . . . ? C36 C36' C37' C32 62.9 . . . . ? C35 C36' C37' C32 24.5 . . . . ? C33 C32 C37' C37 105.4 . . . . ? N4 C32 C37' C37 -105.8(2) . . . . ? C33 C32 C37' C36' 23.9 . . . . ? N4 C32 C37' C36' 172.6(2) . . . . ? C37 C32 C37' C36' -81.6 . . . . ? N4 C39 C40 N5 -0.2(8) . . . . ? C35 C35' N1' N1 -3.7(7) . . . . ? C36' C35' N1' N1 -109.9(7) . . . . ? C34 C35' N1' N1 68.4(8) . . . . ? C36 C35' N1' N1 -43.8(7) . . . . ? C35 C35' N1' C13' 75.9(10) . . . . ? C36' C35' N1' C13' -30.3(12) . . . . ? C34 C35' N1' C13' 148.0(8) . . . . ? N1 C35' N1' C13' 79.6(12) . . . . ? C36 C35' N1' C13' 35.8(12) . . . . ? C35 C35' N1' C27' -78.9(10) . . . . ? C36' C35' N1' C27' 174.8(8) . . . . ? C34 C35' N1' C27' -6.9(12) . . . . ? N1 C35' N1' C27' -75.3(11) . . . . ? C36 C35' N1' C27' -119.1(9) . . . . ? C36' C35' N1' C35 -106.3(3) . . . . ? C34 C35' N1' C35 72.1(3) . . . . ? N1 C35' N1' C35 3.7(7) . . . . ? C36 C35' N1' C35 -40.14(18) . . . . ? C14 C13' N1' N1 50.8(15) . . . . ? C18' C13' N1' N1 -127.5(13) . . . . ? C13 C13' N1' N1 0.6(9) . . . . ? C14 C13' N1' C35' -28.6(19) . . . . ? C18' C13' N1' C35' 153.1(10) . . . . ? C13 C13' N1' C35' -78.9(11) . . . . ? N1 C13' N1' C35' -79.5(11) . . . . ? C14 C13' N1' C27' 128.2(13) . . . . ? C18' C13' N1' C27' -50.1(15) . . . . ? C13 C13' N1' C27' 77.9(10) . . . . ? N1 C13' N1' C27' 77.4(10) . . . . ? C14 C13' N1' C35 6.7(16) . . . . ? C18' C13' N1' C35 -171.6(10) . . . . ? C13 C13' N1' C35 -43.5(9) . . . . ? N1 C13' N1' C35 -44.1(7) . . . . ? C23 C27' N1' N1 98.3(18) . . . . ? C22 C27' N1' N1 2.9(11) . . . . ? C23' C27' N1' N1 -172.7(14) . . . . ? C23 C27' N1' C35' 175.8(14) . . . . ? C22 C27' N1' C35' 80.4(13) . . . . ? C23' C27' N1' C35' -95.2(14) . . . . ? N1 C27' N1' C35' 77.5(10) . . . . ? C23 C27' N1' C13' 18(2) . . . . ? C22 C27' N1' C13' -77.3(12) . . . . ? C23' C27' N1' C13' 107.1(14) . . . . ? N1 C27' N1' C13' -80.2(11) . . . . ? C23 C27' N1' C35 140.3(15) . . . . ? C22 C27' N1' C35 44.9(11) . . . . ? C23' C27' N1' C35 -130.7(12) . . . . ? N1 C27' N1' C35 42.0(7) . . . . ? C35' C35 N1' N1 175.3(9) . . . . ? C36 C35 N1' N1 -103.8(8) . . . . ? C34 C35 N1' N1 121.8(8) . . . . ? C36' C35 N1' N1 -146.9(8) . . . . ? C36 C35 N1' C35' 80.9(3) . . . . ? N1 C35 N1' C35' -175.3(9) . . . . ? C34 C35 N1' C35' -53.5(3) . . . . ? C36' C35 N1' C35' 37.8(2) . . . . ? C35' C35 N1' C13' -120.7(9) . . . . ? C36 C35 N1' C13' -39.7(10) . . . . ? N1 C35 N1' C13' 64.1(11) . . . . ? C34 C35 N1' C13' -174.1(8) . . . . ? C36' C35 N1' C13' -82.9(8) . . . . ? C35' C35 N1' C27' 116.4(9) . . . . ? C36 C35 N1' C27' -162.7(6) . . . . ? N1 C35 N1' C27' -58.9(10) . . . . ? C34 C35 N1' C27' 62.9(8) . . . . ? C36' C35 N1' C27' 154.2(8) . . . . ? C35' N1' N1 C35 2.7(5) . . . . ? C13' N1' N1 C35 -122.1(8) . . . . ? C27' N1' N1 C35 124.8(8) . . . . ? C35' N1' N1 C13 124.2(9) . . . . ? C13' N1' N1 C13 -0.6(10) . . . . ? C27' N1' N1 C13 -113.7(10) . . . . ? C35 N1' N1 C13 121.5(11) . . . . ? C35' N1' N1 C22 -124.4(7) . . . . ? C13' N1' N1 C22 110.9(9) . . . . ? C27' N1' N1 C22 -2.2(8) . . . . ? C35 N1' N1 C22 -127.0(9) . . . . ? C35' N1' N1 C27' -122.2(7) . . . . ? C13' N1' N1 C27' 113.1(10) . . . . ? C35 N1' N1 C27' -124.8(8) . . . . ? C13' N1' N1 C35' -124.8(8) . . . . ? C27' N1' N1 C35' 122.2(7) . . . . ? C35 N1' N1 C35' -2.7(5) . . . . ? C35' N1' N1 C13' 124.8(8) . . . . ? C27' N1' N1 C13' -113.1(10) . . . . ? C35 N1' N1 C13' 122.1(8) . . . . ? C35' C35 N1 N1' -3.7(7) . . . . ? C36 C35 N1 N1' 108.2(6) . . . . ? C34 C35 N1 N1' -70.2(7) . . . . ? C36' C35 N1 N1' 38.3(8) . . . . ? C35' C35 N1 C13 -109.2(9) . . . . ? C36 C35 N1 C13 2.7(12) . . . . ? C34 C35 N1 C13 -175.7(7) . . . . ? N1' C35 N1 C13 -105.5(12) . . . . ? C36' C35 N1 C13 -67.2(10) . . . . ? C35' C35 N1 C22 87.4(11) . . . . ? C36 C35 N1 C22 -160.8(8) . . . . ? C34 C35 N1 C22 20.8(13) . . . . ? N1' C35 N1 C22 91.0(13) . . . . ? C36' C35 N1 C22 129.3(9) . . . . ? C35' C35 N1 C27' 43.9(9) . . . . ? C36 C35 N1 C27' 155.7(6) . . . . ? C34 C35 N1 C27' -22.6(10) . . . . ? N1' C35 N1 C27' 47.5(8) . . . . ? C36' C35 N1 C27' 85.9(9) . . . . ? C36 C35 N1 C35' 111.9(3) . . . . ? C34 C35 N1 C35' -66.5(2) . . . . ? N1' C35 N1 C35' 3.7(7) . . . . ? C36' C35 N1 C35' 42.0(3) . . . . ? C35' C35 N1 C13' -49.5(8) . . . . ? C36 C35 N1 C13' 62.3(9) . . . . ? C34 C35 N1 C13' -116.1(7) . . . . ? N1' C35 N1 C13' -45.9(7) . . . . ? C36' C35 N1 C13' -7.6(10) . . . . ? C14 C13 N1 N1' -37.4(12) . . . . ? C18 C13 N1 N1' 129.8(9) . . . . ? C13' C13 N1 N1' 0.6(10) . . . . ? C14 C13 N1 C35 57.0(11) . . . . ? C18 C13 N1 C35 -135.8(8) . . . . ? C13' C13 N1 C35 95.0(10) . . . . ? C14 C13 N1 C22 -136.9(8) . . . . ? C18 C13 N1 C22 30.3(12) . . . . ? C13' C13 N1 C22 -99.0(10) . . . . ? C14 C13 N1 C27' -95.2(11) . . . . ? C18 C13 N1 C27' 72.0(12) . . . . ? C13' C13 N1 C27' -57.3(11) . . . . ? C14 C13 N1 C35' 15.6(13) . . . . ? C18 C13 N1 C35' -177.2(6) . . . . ? C13' C13 N1 C35' 53.6(10) . . . . ? C14 C13 N1 C13' -38.0(7) . . . . ? C18 C13 N1 C13' 129.2(8) . . . . ? C27' C22 N1 N1' 2.9(10) . . . . ? C23 C22 N1 N1' -26.2(10) . . . . ? C27 C22 N1 N1' 153.0(8) . . . . ? C26' C22 N1 N1' -140(3) . . . . ? C27' C22 N1 C35 -84.2(12) . . . . ? C23 C22 N1 C35 -113.3(10) . . . . ? C27 C22 N1 C35 65.9(13) . . . . ? C26' C22 N1 C35 133(2) . . . . ? C27' C22 N1 C13 110.7(11) . . . . ? C23 C22 N1 C13 81.6(9) . . . . ? C27 C22 N1 C13 -99.2(10) . . . . ? C26' C22 N1 C13 -32(3) . . . . ? C23 C22 N1 C27' -29.1(8) . . . . ? C27 C22 N1 C27' 150.1(11) . . . . ? C26' C22 N1 C27' -143(3) . . . . ? C27' C22 N1 C35' -44.2(10) . . . . ? C23 C22 N1 C35' -73.3(9) . . . . ? C27 C22 N1 C35' 105.9(9) . . . . ? C26' C22 N1 C35' 173(2) . . . . ? C27' C22 N1 C13' 53.8(11) . . . . ? C23 C22 N1 C13' 24.7(10) . . . . ? C27 C22 N1 C13' -156.1(7) . . . . ? C26' C22 N1 C13' -89(3) . . . . ? C23 C27' N1 N1' -121.5(16) . . . . ? C22 C27' N1 N1' -176.5(13) . . . . ? C23' C27' N1 N1' 28(5) . . . . ? C23 C27' N1 C35 174.1(12) . . . . ? C22 C27' N1 C35 119.1(11) . . . . ? C23' C27' N1 C35 -36(5) . . . . ? N1' C27' N1 C35 -64.4(9) . . . . ? C23 C27' N1 C13 -32(2) . . . . ? C22 C27' N1 C13 -86.8(12) . . . . ? C23' C27' N1 C13 118(5) . . . . ? N1' C27' N1 C13 89.7(11) . . . . ? C23 C27' N1 C22 55.0(14) . . . . ? C23' C27' N1 C22 -155(5) . . . . ? N1' C27' N1 C22 176.5(13) . . . . ? C23 C27' N1 C35' -162.8(14) . . . . ? C22 C27' N1 C35' 142.2(9) . . . . ? C23' C27' N1 C35' -13(5) . . . . ? N1' C27' N1 C35' -41.3(6) . . . . ? C23 C27' N1 C13' -74.8(15) . . . . ? C22 C27' N1 C13' -129.7(10) . . . . ? C23' C27' N1 C13' 75(5) . . . . ? N1' C27' N1 C13' 46.8(7) . . . . ? C35 C35' N1 N1' 175.3(9) . . . . ? C36' C35' N1 N1' 101.1(7) . . . . ? C34 C35' N1 N1' -125.6(6) . . . . ? C36 C35' N1 N1' 141.3(7) . . . . ? C36' C35' N1 C35 -74.3(5) . . . . ? N1' C35' N1 C35 -175.3(9) . . . . ? C34 C35' N1 C35 59.1(4) . . . . ? C36 C35' N1 C35 -34.1(3) . . . . ? C35 C35' N1 C13 94.6(11) . . . . ? C36' C35' N1 C13 20.3(12) . . . . ? N1' C35' N1 C13 -80.7(11) . . . . ? C34 C35' N1 C13 153.7(10) . . . . ? C36 C35' N1 C13 60.5(10) . . . . ? C35 C35' N1 C22 -115.0(10) . . . . ? C36' C35' N1 C22 170.7(6) . . . . ? N1' C35' N1 C22 69.6(10) . . . . ? C34 C35' N1 C22 -55.9(9) . . . . ? C36 C35' N1 C22 -149.1(9) . . . . ? C35 C35' N1 C27' -141.0(8) . . . . ? C36' C35' N1 C27' 144.7(5) . . . . ? N1' C35' N1 C27' 43.7(7) . . . . ? C34 C35' N1 C27' -81.9(6) . . . . ? C36 C35' N1 C27' -175.1(6) . . . . ? C35 C35' N1 C13' 135.0(8) . . . . ? C36' C35' N1 C13' 60.7(7) . . . . ? N1' C35' N1 C13' -40.3(7) . . . . ? C34 C35' N1 C13' -165.9(5) . . . . ? C36 C35' N1 C13' 100.9(6) . . . . ? C14 C13' N1 N1' -142.6(12) . . . . ? C18' C13' N1 N1' 84.0(16) . . . . ? C13 C13' N1 N1' -179.3(12) . . . . ? C14 C13' N1 C35 -77.3(10) . . . . ? C18' C13' N1 C35 149.3(13) . . . . ? N1' C13' N1 C35 65.3(10) . . . . ? C13 C13' N1 C35 -113.9(11) . . . . ? C14 C13' N1 C13 36.6(7) . . . . ? C18' C13' N1 C13 -96.8(15) . . . . ? N1' C13' N1 C13 179.3(12) . . . . ? C14 C13' N1 C22 137.8(9) . . . . ? C18' C13' N1 C22 4.4(18) . . . . ? N1' C13' N1 C22 -79.6(10) . . . . ? C13 C13' N1 C22 101.1(10) . . . . ? C14 C13' N1 C27' 168.4(9) . . . . ? C18' C13' N1 C27' 35.0(16) . . . . ? N1' C13' N1 C27' -49.0(9) . . . . ? C13 C13' N1 C27' 131.7(10) . . . . ? C14 C13' N1 C35' -102.8(8) . . . . ? C18' C13' N1 C35' 123.8(14) . . . . ? N1' C13' N1 C35' 39.8(7) . . . . ? C13 C13' N1 C35' -139.4(9) . . . . ? C26' C25 N2 C28 177.1(11) . . . . ? C24 C25 N2 C28 61.5(9) . . . . ? C26 C25 N2 C28 -129.5(8) . . . . ? C24' C25 N2 C28 23.2(10) . . . . ? C26' C25 N2 C30 -8.8(16) . . . . ? C24 C25 N2 C30 -124.3(7) . . . . ? C26 C25 N2 C30 44.6(8) . . . . ? C24' C25 N2 C30 -162.7(6) . . . . ? N3 C28 N2 C25 172.9(7) . . . . ? N3 C28 N2 C30 -1.9(7) . . . . ? C29 C30 N2 C25 -173.3(7) . . . . ? C29 C30 N2 C28 2.0(7) . . . . ? N2 C28 N3 C29 0.9(7) . . . . ? N2 C28 N3 Co1 170.0(4) . . . . ? C30 C29 N3 C28 0.4(8) . . . . ? C30 C29 N3 Co1 -169.8(4) . . . . ? O3 Co1 N3 C28 -24.1(5) 2_567 . . . ? O3 Co1 N3 C28 155.9(5) . . . . ? N3 Co1 N3 C28 172(100) 2_567 . . . ? N5 Co1 N3 C28 -106.6(5) 1_556 . . . ? N5 Co1 N3 C28 73.4(5) 2_566 . . . ? O3 Co1 N3 C29 143.2(6) 2_567 . . . ? O3 Co1 N3 C29 -36.8(6) . . . . ? N3 Co1 N3 C29 -21(100) 2_567 . . . ? N5 Co1 N3 C29 60.7(6) 1_556 . . . ? N5 Co1 N3 C29 -119.3(6) 2_566 . . . ? C40 C39 N4 C38 0.0(7) . . . . ? C40 C39 N4 C32 -179.0(5) . . . . ? N5 C38 N4 C39 0.1(5) . . . . ? N5 C38 N4 C32 179.1(3) . . . . ? C33 C32 N4 C39 167.4(4) . . . . ? C37 C32 N4 C39 -38.8(6) . . . . ? C37' C32 N4 C39 22.2(6) . . . . ? C33 C32 N4 C38 -11.4(6) . . . . ? C37 C32 N4 C38 142.4(4) . . . . ? C37' C32 N4 C38 -156.6(3) . . . . ? N4 C38 N5 C40 -0.2(5) . . . . ? N4 C38 N5 Co1 -171.3(3) . . . 1_554 ? C39 C40 N5 C38 0.2(7) . . . . ? C39 C40 N5 Co1 172.1(4) . . . 1_554 ? C20 C21 N6 C19 -0.8(11) . . . . ? C20 C21 N6 C16 144.7(8) . . . . ? C20 C21 N6 C16' -162.0(8) . . . . ? N7 C19 N6 C21 -0.3(10) . . . . ? N7 C19 N6 C16 -145.3(7) . . . . ? N7 C19 N6 C16' 160.0(9) . . . . ? C16' C16 N6 C21 107.1(11) . . . . ? C15 C16 N6 C21 145.1(9) . . . . ? C17 C16 N6 C21 -7.6(13) . . . . ? C16' C16 N6 C19 -111.9(11) . . . . ? C15 C16 N6 C19 -74.0(10) . . . . ? C17 C16 N6 C19 133.3(8) . . . . ? C15 C16 N6 C16' 38.0(7) . . . . ? C17 C16 N6 C16' -114.8(9) . . . . ? C15 C16' N6 C21 -152.3(10) . . . . ? C16 C16' N6 C21 -102.1(10) . . . . ? C17' C16' N6 C21 30.4(18) . . . . ? C15 C16' N6 C19 50.0(15) . . . . ? C16 C16' N6 C19 100.2(11) . . . . ? C17' C16' N6 C19 -127.3(12) . . . . ? C15 C16' N6 C16 -50.2(9) . . . . ? C17' C16' N6 C16 132.5(16) . . . . ? N6 C19 N7 C20 1.2(8) . . . . ? N6 C19 N7 Co2 -171.4(5) . . . 2_657 ? C21 C20 N7 C19 -1.7(8) . . . . ? C21 C20 N7 Co2 171.6(5) . . . 2_657 ? O1 C8 O2 Co2 14.2(7) . . . 2_457 ? C4 C8 O2 Co2 -162.5(4) . . . 2_457 ? O4 C7 O3 Co1 23.4(11) . . . . ? C1 C7 O3 Co1 -155.7(5) . . . . ? O3 Co1 O3 C7 161(100) 2_567 . . . ? N3 Co1 O3 C7 -84.4(7) 2_567 . . . ? N3 Co1 O3 C7 95.6(7) . . . . ? N5 Co1 O3 C7 9.0(7) 1_556 . . . ? N5 Co1 O3 C7 -171.0(7) 2_566 . . . ? O3 C7 O4 Co2 137.1(6) . . . . ? C1 C7 O4 Co2 -43.8(11) . . . . ? O2 Co2 O4 C7 40.3(8) 2_457 . . . ? O6 Co2 O4 C7 -112.9(8) . . . . ? N7 Co2 O4 C7 143.1(8) 2_657 . . . ? O5 Co2 O4 C7 -127.1(7) . . . . ? C12 Co2 O4 C7 -117.8(8) . . . . ? O6 C12 O5 Co2 1.0(6) . . . . ? C10 C12 O5 Co2 -175.6(5) . . . . ? O2 Co2 O5 C12 -152.3(4) 2_457 . . . ? O4 Co2 O5 C12 16.0(6) . . . . ? O6 Co2 O5 C12 -0.6(4) . . . . ? N7 Co2 O5 C12 106.1(4) 2_657 . . . ? O5 C12 O6 Co2 -1.1(7) . . . . ? C10 C12 O6 Co2 175.5(4) . . . . ? O2 Co2 O6 C12 52.2(5) 2_457 . . . ? O4 Co2 O6 C12 -172.0(4) . . . . ? N7 Co2 O6 C12 -79.9(4) 2_657 . . . ? O5 Co2 O6 C12 0.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.969 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.086