# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H74 Co3 N12 O18' _chemical_formula_weight 1740.36 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.585(5) _cell_length_b 13.726(2) _cell_length_c 23.486(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.409(7) _cell_angle_gamma 90.00 _cell_volume 7890(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3596 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.9209 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37420 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7130 _reflns_number_gt 5149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+21.5948P] 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 7130 _refine_ls_number_parameters 582 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.16903(13) 0.2242(3) 0.22006(13) 0.0348(8) Uani 1 1 d . . . H1A H 0.1442 0.1950 0.2371 0.042 Uiso 1 1 calc R . . N2 N 0.50158(13) 0.1507(2) 0.18029(13) 0.0303(7) Uani 1 1 d . . . N3 N 0.50581(13) 0.3696(2) 0.31593(13) 0.0313(7) Uani 1 1 d . . . N4 N 0.32615(12) 0.4276(2) 0.51653(13) 0.0283(7) Uani 1 1 d . . . N5 N 0.33000(13) 1.1127(2) 0.52757(13) 0.0293(7) Uani 1 1 d . . . Co2 Co 0.331505(19) 0.27059(3) 0.521708(19) 0.01931(14) Uani 1 1 d . . . Co1 Co 0.5000 0.25828(5) 0.2500 0.02036(17) Uani 1 2 d S . . O1 O -0.10973(11) 0.2135(2) 0.10479(13) 0.0442(7) Uani 1 1 d . . . O2 O -0.08236(11) 0.2379(2) 0.02029(13) 0.0414(7) Uani 1 1 d . . . O3 O 0.23055(10) 0.2254(2) 0.42868(11) 0.0331(6) Uani 1 1 d . . . O4 O 0.31843(10) 0.26369(18) 0.43537(10) 0.0266(6) Uani 1 1 d . . . O5 O 0.36807(12) 0.2062(3) 0.17752(12) 0.0528(9) Uani 1 1 d . . . O6 O 0.41544(10) 0.26125(19) 0.25585(11) 0.0314(6) Uani 1 1 d . . . O7 O 0.18662(12) 0.2950(3) 0.13672(13) 0.0575(10) Uani 1 1 d . . . C1 C -0.01381(16) 0.2338(3) 0.09892(17) 0.0321(9) Uani 1 1 d . . . C2 C -0.00035(18) 0.2240(4) 0.1572(2) 0.0561(14) Uani 1 1 d . . . H2A H -0.0277 0.2129 0.1812 0.067 Uiso 1 1 calc R . . C3 C 0.05354(18) 0.2305(4) 0.18022(19) 0.0576(15) Uani 1 1 d . . . H3A H 0.0620 0.2235 0.2194 0.069 Uiso 1 1 calc R . . C4 C 0.09469(16) 0.2474(3) 0.14561(16) 0.0333(9) Uani 1 1 d . . . C5 C 0.08078(17) 0.2590(3) 0.08744(17) 0.0397(10) Uani 1 1 d . . . H5A H 0.1079 0.2725 0.0635 0.048 Uiso 1 1 calc R . . C6 C 0.02724(17) 0.2507(3) 0.06460(17) 0.0376(10) Uani 1 1 d . . . H6A H 0.0189 0.2567 0.0253 0.045 Uiso 1 1 calc R . . C7 C 0.22137(14) 0.2320(3) 0.25084(15) 0.0269(8) Uani 1 1 d . . . C8 C 0.22301(14) 0.2342(3) 0.31016(15) 0.0253(8) Uani 1 1 d . . . H8A H 0.1908 0.2302 0.3278 0.030 Uiso 1 1 calc R . . C9 C 0.27292(14) 0.2423(2) 0.34321(14) 0.0212(7) Uani 1 1 d . . . C10 C 0.32094(15) 0.2470(3) 0.31667(15) 0.0247(8) Uani 1 1 d . . . H10A H 0.3542 0.2539 0.3387 0.030 Uiso 1 1 calc R . . C11 C 0.31977(15) 0.2414(3) 0.25696(15) 0.0256(8) Uani 1 1 d . . . C12 C 0.26971(15) 0.2337(3) 0.22465(15) 0.0293(8) Uani 1 1 d . . . H12A H 0.2685 0.2295 0.1850 0.035 Uiso 1 1 calc R . . C13 C -0.07220(16) 0.2274(3) 0.07322(18) 0.0325(9) Uani 1 1 d . . . C14 C 0.27373(14) 0.2445(2) 0.40719(14) 0.0192(7) Uani 1 1 d . . . C15 C 0.37195(15) 0.2367(3) 0.22726(15) 0.0281(8) Uani 1 1 d . . . C16 C 0.15413(16) 0.2578(3) 0.16679(16) 0.0344(9) Uani 1 1 d . . . C17 C 0.47130(17) 0.0709(3) 0.17332(17) 0.0372(10) Uani 1 1 d . . . H17A H 0.4513 0.0512 0.2030 0.045 Uiso 1 1 calc R . . C18 C 0.46801(18) 0.0155(3) 0.12394(17) 0.0419(11) Uani 1 1 d . . . H18A H 0.4471 -0.0410 0.1218 0.050 Uiso 1 1 calc R . . C19 C 0.49550(17) 0.0430(3) 0.07750(16) 0.0335(9) Uani 1 1 d . . . C20 C 0.52867(17) 0.1249(3) 0.08570(17) 0.0383(10) Uani 1 1 d . . . H20A H 0.5494 0.1458 0.0569 0.046 Uiso 1 1 calc R . . C21 C 0.53070(16) 0.1749(3) 0.13655(16) 0.0361(10) Uani 1 1 d . . . H21A H 0.5536 0.2289 0.1411 0.043 Uiso 1 1 calc R . . C22 C 0.48819(17) -0.0104(3) 0.02363(16) 0.0384(10) Uani 1 1 d . . . H22A H 0.4649 -0.0640 0.0222 0.046 Uiso 1 1 calc R . . C23 C 0.54275(17) 0.3599(3) 0.36105(18) 0.0436(11) Uani 1 1 d . . . H23A H 0.5734 0.3219 0.3570 0.052 Uiso 1 1 calc R . . C24 C 0.53795(17) 0.4029(3) 0.41292(18) 0.0446(11) Uani 1 1 d . . . H24A H 0.5649 0.3931 0.4429 0.053 Uiso 1 1 calc R . . C25 C 0.49323(17) 0.4609(3) 0.42090(17) 0.0365(10) Uani 1 1 d . . . C26 C 0.45640(19) 0.4753(3) 0.37342(17) 0.0457(11) Uani 1 1 d . . . H26A H 0.4265 0.5162 0.3757 0.055 Uiso 1 1 calc R . . C27 C 0.46402(19) 0.4291(3) 0.32276(17) 0.0404(11) Uani 1 1 d . . . H27A H 0.4386 0.4400 0.2915 0.048 Uiso 1 1 calc R . . C28 C 0.48345(18) 0.5035(3) 0.47613(17) 0.0403(10) Uani 1 1 d . . . H28A H 0.4513 0.5385 0.4779 0.048 Uiso 1 1 calc R . . C29 C 0.32155(17) 0.4818(3) 0.56281(17) 0.0345(9) Uani 1 1 d . . . H29A H 0.3209 0.4503 0.5978 0.041 Uiso 1 1 calc R . . C30 C 0.31768(17) 0.5823(3) 0.56188(18) 0.0365(10) Uani 1 1 d . . . H30A H 0.3152 0.6166 0.5957 0.044 Uiso 1 1 calc R . . C31 C 0.31744(16) 0.6319(3) 0.51037(17) 0.0322(9) Uani 1 1 d . . . C32 C 0.32070(19) 0.5756(3) 0.46212(18) 0.0420(11) Uani 1 1 d . . . H32A H 0.3196 0.6050 0.4264 0.050 Uiso 1 1 calc R . . C33 C 0.32563(18) 0.4757(3) 0.46686(17) 0.0396(10) Uani 1 1 d . . . H33A H 0.3288 0.4398 0.4338 0.047 Uiso 1 1 calc R . . C34 C 0.31500(17) 0.7387(3) 0.50429(18) 0.0355(9) Uani 1 1 d . . . H34A H 0.3038 0.7636 0.4682 0.043 Uiso 1 1 calc R . . C35 C 0.32740(18) 0.8021(3) 0.54590(18) 0.0388(10) Uani 1 1 d . . . H35A H 0.3364 0.7782 0.5826 0.047 Uiso 1 1 calc R . . C36 C 0.32774(16) 0.9084(3) 0.53749(17) 0.0345(9) Uani 1 1 d . . . C37 C 0.3287(2) 0.9688(3) 0.58452(18) 0.0451(11) Uani 1 1 d . . . H37A H 0.3289 0.9421 0.6210 0.054 Uiso 1 1 calc R . . C38 C 0.32921(19) 1.0680(3) 0.57767(18) 0.0407(10) Uani 1 1 d . . . H38A H 0.3290 1.1065 0.6102 0.049 Uiso 1 1 calc R . . C39 C 0.33021(18) 1.0545(3) 0.48221(17) 0.0390(10) Uani 1 1 d . . . H39A H 0.3315 1.0832 0.4465 0.047 Uiso 1 1 calc R . . C40 C 0.32858(18) 0.9539(3) 0.48522(18) 0.0411(10) Uani 1 1 d . . . H40A H 0.3280 0.9170 0.4520 0.049 Uiso 1 1 calc R . . O1W O 0.39288(15) 0.6009(3) 0.20805(15) 0.0719(11) Uani 1 1 d D . . H1WA H 0.3982 0.6213 0.1655 0.108 Uiso 1 1 d RD . . H1WB H 0.3645 0.5552 0.2136 0.108 Uiso 1 1 d RD . . O01 O 0.3026(9) 0.4906(12) 0.2029(8) 0.220(4) Uani 0.50 1 d PDU A 1 N01 N 0.2126(9) 0.4856(15) 0.2328(7) 0.220(4) Uani 0.50 1 d PDU A 1 C01 C 0.2547(9) 0.476(4) 0.1917(8) 0.220(4) Uani 0.50 1 d PDU A 1 C02 C 0.2358(11) 0.4847(14) 0.2948(6) 0.221(4) Uani 0.50 1 d PDU A 1 C03 C 0.1552(9) 0.4875(13) 0.2038(9) 0.222(4) Uani 0.50 1 d PDU A 1 O1' O 0.3018(10) 0.4620(11) 0.1915(8) 0.220(4) Uani 0.50 1 d PDU B 2 N1' N 0.2357(8) 0.4866(16) 0.2541(7) 0.220(4) Uani 0.50 1 d PDU B 2 C1' C 0.2546(9) 0.483(3) 0.1979(7) 0.220(4) Uani 0.50 1 d PDU B 2 C2' C 0.2774(10) 0.5017(13) 0.3043(6) 0.218(4) Uani 0.50 1 d PDU B 2 C3' C 0.1758(9) 0.4739(13) 0.2588(9) 0.219(4) Uani 0.50 1 d PDU B 2 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 N1 0.0171(17) 0.064(2) 0.0224(17) 0.0031(15) -0.0019(13) -0.0078(15) N2 0.0275(18) 0.0415(19) 0.0221(16) -0.0064(14) 0.0043(14) -0.0032(14) N3 0.0322(19) 0.0401(19) 0.0218(16) -0.0065(14) 0.0042(14) -0.0035(15) N4 0.0285(18) 0.0273(16) 0.0290(17) -0.0011(13) 0.0027(14) -0.0016(13) N5 0.0317(19) 0.0252(16) 0.0304(18) -0.0011(14) 0.0003(14) 0.0002(13) Co2 0.0168(3) 0.0244(2) 0.0166(2) -0.00073(19) 0.00068(18) -0.00002(18) Co1 0.0174(4) 0.0308(4) 0.0131(3) 0.000 0.0024(3) 0.000 O1 0.0228(16) 0.062(2) 0.0466(18) -0.0006(15) -0.0021(14) -0.0007(13) O2 0.0267(16) 0.0578(19) 0.0371(17) 0.0066(14) -0.0111(13) -0.0010(13) O3 0.0230(15) 0.0532(17) 0.0242(14) 0.0012(12) 0.0084(11) -0.0008(12) O4 0.0236(14) 0.0367(14) 0.0185(12) -0.0009(10) -0.0038(11) -0.0059(11) O5 0.0359(18) 0.095(3) 0.0283(16) -0.0187(16) 0.0085(14) -0.0140(17) O6 0.0149(14) 0.0550(17) 0.0246(14) -0.0002(12) 0.0027(11) -0.0035(11) O7 0.0262(17) 0.111(3) 0.0338(17) 0.0254(18) -0.0051(14) -0.0162(17) C1 0.022(2) 0.042(2) 0.030(2) -0.0007(17) -0.0067(17) 0.0019(16) C2 0.021(2) 0.113(4) 0.035(2) 0.005(3) 0.0017(19) -0.008(2) C3 0.025(2) 0.123(5) 0.024(2) 0.012(3) -0.0042(19) -0.007(3) C4 0.021(2) 0.054(3) 0.024(2) -0.0001(18) -0.0034(16) -0.0036(17) C5 0.023(2) 0.071(3) 0.025(2) 0.004(2) -0.0008(17) -0.0032(19) C6 0.024(2) 0.062(3) 0.025(2) 0.0017(19) -0.0066(17) -0.0002(18) C7 0.0151(19) 0.046(2) 0.0186(18) 0.0018(16) -0.0041(15) -0.0012(16) C8 0.0167(19) 0.036(2) 0.0232(18) 0.0006(15) 0.0029(15) -0.0019(15) C9 0.0209(19) 0.0260(18) 0.0165(17) -0.0017(13) 0.0003(14) -0.0018(14) C10 0.0169(19) 0.035(2) 0.0220(18) 0.0000(15) -0.0011(15) -0.0020(14) C11 0.021(2) 0.036(2) 0.0201(18) 0.0009(15) 0.0016(15) -0.0015(15) C12 0.023(2) 0.049(2) 0.0155(17) 0.0007(16) -0.0008(15) -0.0036(17) C13 0.022(2) 0.033(2) 0.043(2) -0.0020(18) 0.0001(19) -0.0001(16) C14 0.024(2) 0.0170(16) 0.0169(17) -0.0005(13) 0.0039(15) 0.0028(13) C15 0.023(2) 0.043(2) 0.0185(18) 0.0019(16) 0.0038(16) 0.0000(16) C16 0.019(2) 0.061(3) 0.023(2) 0.0002(18) -0.0013(17) -0.0049(18) C17 0.042(3) 0.041(2) 0.030(2) -0.0037(18) 0.0104(19) -0.0063(19) C18 0.051(3) 0.038(2) 0.037(2) -0.0075(19) 0.009(2) -0.011(2) C19 0.037(2) 0.037(2) 0.026(2) -0.0065(17) 0.0004(18) 0.0001(18) C20 0.038(3) 0.050(3) 0.029(2) -0.0114(18) 0.0131(19) -0.0073(19) C21 0.033(2) 0.047(2) 0.030(2) -0.0131(18) 0.0099(18) -0.0101(18) C22 0.043(3) 0.039(2) 0.033(2) -0.0155(19) 0.0025(19) -0.0035(19) C23 0.025(2) 0.068(3) 0.038(2) -0.023(2) 0.0006(19) 0.003(2) C24 0.032(2) 0.071(3) 0.030(2) -0.022(2) -0.0042(19) 0.004(2) C25 0.042(3) 0.039(2) 0.029(2) -0.0098(17) 0.0065(19) -0.0024(18) C26 0.056(3) 0.047(3) 0.033(2) -0.0114(19) -0.004(2) 0.020(2) C27 0.055(3) 0.037(2) 0.028(2) -0.0058(17) -0.005(2) 0.013(2) C28 0.042(3) 0.049(3) 0.031(2) -0.0134(19) 0.0067(18) 0.007(2) C29 0.040(2) 0.031(2) 0.031(2) -0.0003(17) 0.0018(18) -0.0012(17) C30 0.043(3) 0.030(2) 0.037(2) -0.0080(17) 0.0058(19) -0.0004(18) C31 0.025(2) 0.029(2) 0.042(2) 0.0035(17) 0.0017(18) -0.0017(15) C32 0.061(3) 0.031(2) 0.033(2) 0.0038(18) 0.001(2) -0.004(2) C33 0.058(3) 0.031(2) 0.030(2) 0.0027(17) 0.006(2) -0.0036(19) C34 0.030(2) 0.036(2) 0.040(2) 0.0035(18) 0.0032(18) 0.0029(17) C35 0.046(3) 0.033(2) 0.036(2) -0.0015(19) 0.002(2) 0.0024(19) C36 0.036(2) 0.027(2) 0.041(2) 0.0018(17) 0.0013(19) 0.0011(17) C37 0.067(3) 0.033(2) 0.035(2) 0.0039(18) 0.003(2) 0.000(2) C38 0.062(3) 0.027(2) 0.033(2) -0.0024(17) 0.001(2) 0.0024(19) C39 0.057(3) 0.030(2) 0.029(2) 0.0008(17) 0.000(2) 0.0049(19) C40 0.054(3) 0.029(2) 0.040(2) -0.0093(18) 0.005(2) 0.0014(19) O1W 0.058(2) 0.106(3) 0.052(2) -0.005(2) 0.0045(18) 0.017(2) O01 0.474(13) 0.062(4) 0.141(5) -0.032(4) 0.119(6) -0.074(7) N01 0.475(13) 0.061(3) 0.141(5) -0.034(4) 0.121(6) -0.070(7) C01 0.475(13) 0.061(3) 0.141(5) -0.033(4) 0.122(6) -0.071(7) C02 0.476(13) 0.063(4) 0.140(5) -0.033(4) 0.122(6) -0.070(7) C03 0.474(13) 0.064(4) 0.146(6) -0.036(5) 0.121(7) -0.070(7) O1' 0.475(13) 0.063(4) 0.141(5) -0.033(4) 0.120(6) -0.072(7) N1' 0.475(13) 0.061(3) 0.140(5) -0.033(4) 0.121(6) -0.071(7) C1' 0.475(13) 0.061(3) 0.141(5) -0.033(4) 0.122(6) -0.071(7) C2' 0.474(13) 0.061(4) 0.137(5) -0.031(5) 0.122(7) -0.072(7) C3' 0.473(13) 0.062(3) 0.140(5) -0.034(4) 0.121(6) -0.070(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C16 1.351(5) . ? N1 C7 1.419(5) . ? N1 H1A 0.8600 . ? N2 C17 1.326(5) . ? N2 C21 1.348(5) . ? N2 Co1 2.208(3) . ? N3 C27 1.334(5) . ? N3 C23 1.336(5) . ? N3 Co1 2.171(3) . ? N4 C29 1.331(5) . ? N4 C33 1.339(5) . ? N4 Co2 2.162(3) . ? N5 C38 1.329(5) . ? N5 C39 1.332(5) . ? N5 Co2 2.172(3) 1_565 ? Co2 O3 2.006(3) 7_556 ? Co2 O4 2.025(2) . ? Co2 O2 2.124(3) 8_556 ? Co2 N5 2.172(3) 1_545 ? Co2 O1 2.326(3) 8_556 ? Co1 O6 2.097(2) 2_655 ? Co1 O6 2.097(2) . ? Co1 N3 2.171(3) 2_655 ? Co1 N2 2.208(3) 2_655 ? O1 C13 1.251(5) . ? O1 Co2 2.326(3) 8_455 ? O2 C13 1.253(5) . ? O2 Co2 2.124(3) 8_455 ? O3 C14 1.245(4) . ? O3 Co2 2.006(3) 7_556 ? O4 C14 1.256(4) . ? O5 C15 1.236(4) . ? O6 C15 1.254(4) . ? O7 C16 1.226(5) . ? C1 C6 1.369(6) . ? C1 C2 1.385(6) . ? C1 C13 1.507(5) . ? C2 C3 1.386(6) . ? C2 H2A 0.9300 . ? C3 C4 1.376(6) . ? C3 H3A 0.9300 . ? C4 C5 1.386(5) . ? C4 C16 1.506(5) . ? C5 C6 1.378(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.389(5) . ? C7 C8 1.390(5) . ? C8 C9 1.393(5) . ? C8 H8A 0.9300 . ? C9 C10 1.388(5) . ? C9 C14 1.501(4) . ? C10 C11 1.402(5) . ? C10 H10A 0.9300 . ? C11 C12 1.388(5) . ? C11 C15 1.518(5) . ? C12 H12A 0.9300 . ? C17 C18 1.382(5) . ? C17 H17A 0.9300 . ? C18 C19 1.388(6) . ? C18 H18A 0.9300 . ? C19 C20 1.392(5) . ? C19 C22 1.459(5) . ? C20 C21 1.374(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C22 1.331(8) 5_655 ? C22 H22A 0.9300 . ? C23 C24 1.369(5) . ? C23 H23A 0.9300 . ? C24 C25 1.384(6) . ? C24 H24A 0.9300 . ? C25 C26 1.383(6) . ? C25 C28 1.464(5) . ? C26 C27 1.376(5) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C28 1.325(8) 5_666 ? C28 H28A 0.9300 . ? C29 C30 1.383(5) . ? C29 H29A 0.9300 . ? C30 C31 1.388(5) . ? C30 H30A 0.9300 . ? C31 C32 1.380(6) . ? C31 C34 1.473(5) . ? C32 C33 1.381(6) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.322(6) . ? C34 H34A 0.9300 . ? C35 C36 1.473(5) . ? C35 H35A 0.9300 . ? C36 C37 1.379(6) . ? C36 C40 1.379(6) . ? C37 C38 1.372(6) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.384(5) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? O1W H1WA 1.0570 . ? O1W H1WB 0.9566 . ? O01 C01 1.200(11) . ? N01 C01 1.486(10) . ? N01 C03 1.509(10) . ? N01 C02 1.512(10) . ? O1' C1' 1.217(10) . ? N1' C1' 1.440(10) . ? N1' C3' 1.497(10) . ? N1' C2' 1.504(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 N1 C7 126.8(3) . . ? C16 N1 H1A 116.6 . . ? C7 N1 H1A 116.6 . . ? C17 N2 C21 116.3(3) . . ? C17 N2 Co1 126.5(3) . . ? C21 N2 Co1 116.6(3) . . ? C27 N3 C23 116.1(3) . . ? C27 N3 Co1 121.1(3) . . ? C23 N3 Co1 119.3(3) . . ? C29 N4 C33 116.2(3) . . ? C29 N4 Co2 121.4(3) . . ? C33 N4 Co2 122.4(3) . . ? C38 N5 C39 115.6(3) . . ? C38 N5 Co2 121.3(3) . 1_565 ? C39 N5 Co2 123.1(3) . 1_565 ? O3 Co2 O4 121.69(10) 7_556 . ? O3 Co2 O2 145.55(11) 7_556 8_556 ? O4 Co2 O2 92.64(11) . 8_556 ? O3 Co2 N4 87.67(11) 7_556 . ? O4 Co2 N4 89.27(11) . . ? O2 Co2 N4 96.29(11) 8_556 . ? O3 Co2 N5 88.42(12) 7_556 1_545 ? O4 Co2 N5 90.85(11) . 1_545 ? O2 Co2 N5 88.22(12) 8_556 1_545 ? N4 Co2 N5 175.48(12) . 1_545 ? O3 Co2 O1 87.50(11) 7_556 8_556 ? O4 Co2 O1 150.66(11) . 8_556 ? O2 Co2 O1 58.47(11) 8_556 8_556 ? N4 Co2 O1 89.05(11) . 8_556 ? N5 Co2 O1 93.05(11) 1_545 8_556 ? O6 Co1 O6 177.77(15) 2_655 . ? O6 Co1 N3 86.48(11) 2_655 2_655 ? O6 Co1 N3 91.95(11) . 2_655 ? O6 Co1 N3 91.95(11) 2_655 . ? O6 Co1 N3 86.48(11) . . ? N3 Co1 N3 90.49(17) 2_655 . ? O6 Co1 N2 98.54(11) 2_655 2_655 ? O6 Co1 N2 82.97(11) . 2_655 ? N3 Co1 N2 174.43(11) 2_655 2_655 ? N3 Co1 N2 86.95(12) . 2_655 ? O6 Co1 N2 82.97(11) 2_655 . ? O6 Co1 N2 98.54(11) . . ? N3 Co1 N2 86.95(12) 2_655 . ? N3 Co1 N2 174.44(12) . . ? N2 Co1 N2 96.03(17) 2_655 . ? C13 O1 Co2 85.6(2) . 8_455 ? C13 O2 Co2 94.8(2) . 8_455 ? C14 O3 Co2 162.4(2) . 7_556 ? C14 O4 Co2 125.9(2) . . ? C15 O6 Co1 139.5(2) . . ? C6 C1 C2 118.6(4) . . ? C6 C1 C13 120.1(4) . . ? C2 C1 C13 121.3(4) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 118.4(4) . . ? C3 C4 C16 124.5(4) . . ? C5 C4 C16 117.2(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C1 C6 C5 121.0(4) . . ? C1 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C12 C7 C8 119.9(3) . . ? C12 C7 N1 123.2(3) . . ? C8 C7 N1 116.8(3) . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 C14 121.1(3) . . ? C8 C9 C14 119.2(3) . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C12 C11 C10 119.0(3) . . ? C12 C11 C15 119.3(3) . . ? C10 C11 C15 121.5(3) . . ? C11 C12 C7 120.7(3) . . ? C11 C12 H12A 119.6 . . ? C7 C12 H12A 119.6 . . ? O1 C13 O2 121.1(4) . . ? O1 C13 C1 120.0(4) . . ? O2 C13 C1 118.9(4) . . ? O3 C14 O4 124.6(3) . . ? O3 C14 C9 118.0(3) . . ? O4 C14 C9 117.4(3) . . ? O5 C15 O6 125.7(4) . . ? O5 C15 C11 117.1(3) . . ? O6 C15 C11 117.2(3) . . ? O7 C16 N1 122.7(4) . . ? O7 C16 C4 120.9(3) . . ? N1 C16 C4 116.3(3) . . ? N2 C17 C18 123.1(4) . . ? N2 C17 H17A 118.5 . . ? C18 C17 H17A 118.5 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 115.7(4) . . ? C18 C19 C22 121.0(4) . . ? C20 C19 C22 123.3(4) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? N2 C21 C20 124.1(4) . . ? N2 C21 H21A 118.0 . . ? C20 C21 H21A 118.0 . . ? C22 C22 C19 125.9(5) 5_655 . ? C22 C22 H22A 117.0 5_655 . ? C19 C22 H22A 117.0 . . ? N3 C23 C24 123.6(4) . . ? N3 C23 H23A 118.2 . . ? C24 C23 H23A 118.2 . . ? C23 C24 C25 120.3(4) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 116.2(4) . . ? C26 C25 C28 120.5(4) . . ? C24 C25 C28 123.3(4) . . ? C27 C26 C25 119.9(4) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? N3 C27 C26 123.7(4) . . ? N3 C27 H27A 118.1 . . ? C26 C27 H27A 118.1 . . ? C28 C28 C25 125.6(5) 5_666 . ? C28 C28 H28A 117.2 5_666 . ? C25 C28 H28A 117.2 . . ? N4 C29 C30 123.8(4) . . ? N4 C29 H29A 118.1 . . ? C30 C29 H29A 118.1 . . ? C29 C30 C31 119.9(4) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 116.4(4) . . ? C32 C31 C34 118.8(4) . . ? C30 C31 C34 124.7(4) . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? N4 C33 C32 123.6(4) . . ? N4 C33 H33A 118.2 . . ? C32 C33 H33A 118.2 . . ? C35 C34 C31 125.3(4) . . ? C35 C34 H34A 117.3 . . ? C31 C34 H34A 117.3 . . ? C34 C35 C36 123.8(4) . . ? C34 C35 H35A 118.1 . . ? C36 C35 H35A 118.1 . . ? C37 C36 C40 116.1(4) . . ? C37 C36 C35 119.2(4) . . ? C40 C36 C35 124.7(4) . . ? C38 C37 C36 120.1(4) . . ? C38 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? N5 C38 C37 124.3(4) . . ? N5 C38 H38A 117.8 . . ? C37 C38 H38A 117.8 . . ? N5 C39 C40 123.7(4) . . ? N5 C39 H39A 118.1 . . ? C40 C39 H39A 118.1 . . ? C36 C40 C39 120.0(4) . . ? C36 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? H1WA O1W H1WB 117.4 . . ? C01 N01 C03 112.7(9) . . ? C01 N01 C02 113.7(10) . . ? C03 N01 C02 133.5(15) . . ? O01 C01 N01 125.0(13) . . ? C1' N1' C3' 118.0(10) . . ? C1' N1' C2' 117.9(10) . . ? C3' N1' C2' 124.1(16) . . ? O1' C1' N1' 121.1(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.709 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 918287' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H62 Cd3 N10 O17' _chemical_formula_weight 1772.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.1977(17) _cell_length_b 13.9528(10) _cell_length_c 25.1006(18) _cell_angle_alpha 90.00 _cell_angle_beta 96.677(2) _cell_angle_gamma 90.00 _cell_volume 8417.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8176 _exptl_absorpt_correction_T_max 0.9138 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47373 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7370 _reflns_number_gt 6325 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+185.3079P] 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 7370 _refine_ls_number_parameters 606 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd2 Cd 0.0000 0.26758(6) 0.2500 0.0322(2) Uani 1 2 d S . . Cd1 Cd 0.229958(19) 0.23640(4) 0.921029(18) 0.02375(17) Uani 1 1 d . . . O2 O 0.2282(2) 0.2322(5) 0.8282(2) 0.0534(17) Uani 1 1 d . . . O4 O -0.1771(2) 0.2690(5) 0.4275(2) 0.0494(15) Uani 1 1 d . . . O6 O -0.0060(2) 0.2641(6) 0.3390(2) 0.063(2) Uani 1 1 d . . . N3 N 0.2286(3) 0.4016(5) 0.9251(3) 0.0494(19) Uani 1 1 d . . . O7 O 0.1191(3) 0.2420(8) 0.5618(2) 0.094(3) Uani 1 1 d . . . O1 O 0.1453(2) 0.2355(5) 0.8550(2) 0.0484(15) Uani 1 1 d . . . O3 O -0.1727(2) 0.2392(5) 0.5137(2) 0.0510(16) Uani 1 1 d . . . N2 N 0.2257(3) 1.0717(5) 0.9285(3) 0.0393(15) Uani 1 1 d . . . C1 C 0.1512(4) 0.2375(10) 0.7605(3) 0.0694(19) Uani 1 1 d U . . C2 C 0.0946(4) 0.2415(10) 0.7468(3) 0.0718(18) Uani 1 1 d U . . H2A H 0.0712 0.2449 0.7736 0.086 Uiso 1 1 calc R . . C3 C 0.0720(4) 0.2403(10) 0.6934(3) 0.0722(17) Uani 1 1 d U . . H3A H 0.0336 0.2392 0.6847 0.087 Uiso 1 1 calc R . . C4 C 0.1064(4) 0.2407(10) 0.6530(3) 0.0696(18) Uani 1 1 d U . . C5 C 0.1627(4) 0.2388(10) 0.6677(3) 0.0686(19) Uani 1 1 d U . . H5A H 0.1865 0.2387 0.6412 0.082 Uiso 1 1 calc R . . C6 C 0.1851(3) 0.2370(8) 0.7208(3) 0.051(2) Uani 1 1 d . . . H6A H 0.2235 0.2355 0.7295 0.061 Uiso 1 1 calc R . . C7 C 0.0015(3) 0.2495(7) 0.5282(3) 0.041(2) Uani 1 1 d . . . C8 C -0.0562(3) 0.2497(6) 0.5250(3) 0.0374(18) Uani 1 1 d . . . H8A H -0.0734 0.2468 0.5562 0.045 Uiso 1 1 calc R . . C9 C -0.0882(3) 0.2543(5) 0.4758(3) 0.0271(14) Uani 1 1 d . . . C10 C -0.0624(3) 0.2594(5) 0.4292(3) 0.0261(14) Uani 1 1 d . . . H10A H -0.0839 0.2627 0.3960 0.031 Uiso 1 1 calc R . . C11 C -0.0049(3) 0.2594(5) 0.4321(3) 0.0279(15) Uani 1 1 d . . . C12 C 0.0272(3) 0.2535(6) 0.4816(3) 0.0333(17) Uani 1 1 d . . . H12A H 0.0658 0.2523 0.4835 0.040 Uiso 1 1 calc R . . C13 C 0.1761(3) 0.2350(6) 0.8181(3) 0.0390(18) Uani 1 1 d . . . C14 C -0.1507(3) 0.2541(5) 0.4725(3) 0.0255(14) Uani 1 1 d . . . C15 C 0.0233(3) 0.2643(6) 0.3823(3) 0.0342(17) Uani 1 1 d U . . C16 C 0.0859(3) 0.2446(8) 0.5943(3) 0.055(3) Uani 1 1 d . . . C17 C 0.2694(4) 1.0185(7) 0.9280(4) 0.057(2) Uani 1 1 d . . . H17A H 0.3039 1.0474 0.9271 0.069 Uiso 1 1 calc R . . C18 C 0.2660(5) 0.9169(8) 0.9289(5) 0.072(3) Uani 1 1 d U A . H18A H 0.2982 0.8808 0.9284 0.086 Uiso 1 1 calc R . . C19 C 0.2170(5) 0.8720(8) 0.9305(4) 0.068(3) Uani 1 1 d U . . C20 C 0.1715(6) 0.9286(8) 0.9327(5) 0.080(4) Uani 1 1 d . A . H20A H 0.1368 0.9015 0.9354 0.096 Uiso 1 1 calc R . . C21 C 0.1775(5) 1.0253(7) 0.9310(5) 0.066(3) Uani 1 1 d . . . H21A H 0.1456 1.0623 0.9317 0.079 Uiso 1 1 calc R A . C22 C 0.2021(7) 0.7700(13) 0.9279(7) 0.040(2) Uani 0.50 1 d PDU A 1 H22A H 0.1649 0.7517 0.9228 0.048 Uiso 0.50 1 calc PR A 1 C23 C 0.2432(7) 0.7017(12) 0.9331(6) 0.038(2) Uani 0.50 1 d PDU A 1 H23A H 0.2801 0.7213 0.9387 0.046 Uiso 0.50 1 calc PR A 1 C22' C 0.2425(8) 0.7609(15) 0.9343(7) 0.046(2) Uani 0.50 1 d PU A 2 H22B H 0.2796 0.7423 0.9406 0.055 Uiso 0.50 1 calc PR A 2 C23' C 0.2021(8) 0.7104(14) 0.9269(7) 0.045(2) Uani 0.50 1 d PU A 2 H23B H 0.1647 0.7274 0.9211 0.053 Uiso 0.50 1 calc PR A 2 C24 C 0.1816(5) 0.4492(7) 0.9283(4) 0.060(3) Uani 1 1 d . . . H24A H 0.1484 0.4160 0.9291 0.072 Uiso 1 1 calc R . . C25 C 0.1821(7) 0.5507(9) 0.9303(4) 0.085(4) Uani 1 1 d . A . H25A H 0.1490 0.5837 0.9319 0.102 Uiso 1 1 calc R . . C26 C 0.2310(8) 0.6014(8) 0.9300(4) 0.084(4) Uani 1 1 d U . . C27 C 0.2790(7) 0.5484(8) 0.9257(5) 0.082(4) Uani 1 1 d . A . H27A H 0.3128 0.5793 0.9239 0.098 Uiso 1 1 calc R . . C28 C 0.2760(5) 0.4504(7) 0.9242(4) 0.066(3) Uani 1 1 d . . . H28A H 0.3087 0.4160 0.9225 0.079 Uiso 1 1 calc R A . N1 N 0.0309(3) 0.2468(8) 0.5804(3) 0.073(3) Uani 1 1 d . . . H1A H 0.0108 0.2466 0.6065 0.087 Uiso 1 1 calc R . . C39 C 0.2271(7) 0.0061(16) 0.2668(9) 0.056(7) Uani 0.50 1 d PDU . 1 H39A H 0.2282 -0.0426 0.2922 0.067 Uiso 0.50 1 calc PR . 1 C40 C 0.2718(6) 0.0206(15) 0.2427(10) 0.053(5) Uani 0.50 1 d PD . 1 H40A H 0.2699 0.0603 0.2128 0.064 Uiso 0.50 1 calc PR . 1 C34 C 0.4227(4) -0.0573(9) 0.2997(4) 0.050(4) Uani 0.50 1 d PG . 1 H34A H 0.4512 -0.0532 0.3278 0.060 Uiso 0.50 1 calc PR . 1 C35 C 0.3702(4) -0.0215(10) 0.3058(4) 0.053(5) Uani 0.50 1 d PG . 1 H35A H 0.3635 0.0065 0.3381 0.064 Uiso 0.50 1 calc PR . 1 C36 C 0.3276(3) -0.0277(10) 0.2637(5) 0.046(5) Uani 0.50 1 d PGD . 1 C37 C 0.3375(4) -0.0696(11) 0.2155(4) 0.061(6) Uani 0.50 1 d PG . 1 H37A H 0.3090 -0.0737 0.1874 0.074 Uiso 0.50 1 calc PR . 1 C38 C 0.3900(5) -0.1054(10) 0.2094(3) 0.054(6) Uani 0.50 1 d PG . 1 H38A H 0.3966 -0.1334 0.1771 0.065 Uiso 0.50 1 calc PR . 1 N5 N 0.4326(3) -0.0992(9) 0.2515(4) 0.037(3) Uani 0.50 1 d PGU . 1 C39' C 0.2262(7) 0.0071(14) 0.2379(12) 0.055(5) Uani 0.50 1 d PD . 2 H39B H 0.2289 -0.0186 0.2041 0.066 Uiso 0.50 1 calc PR . 2 C40' C 0.2728(8) 0.000(3) 0.2717(8) 0.079(9) Uani 0.50 1 d PD . 2 H40B H 0.2754 0.0130 0.3082 0.095 Uiso 0.50 1 calc PR . 2 C34' C 0.4136(4) -0.0532(9) 0.2160(5) 0.056(5) Uani 0.50 1 d PG . 2 H34B H 0.4418 -0.0328 0.1965 0.068 Uiso 0.50 1 calc PR . 2 C35' C 0.3638(5) -0.0026(8) 0.2130(5) 0.056(5) Uani 0.50 1 d PG . 2 H35B H 0.3588 0.0518 0.1916 0.068 Uiso 0.50 1 calc PR . 2 C36' C 0.3216(4) -0.0332(8) 0.2421(5) 0.036(5) Uani 0.50 1 d PGDU . 2 C37' C 0.3291(4) -0.1144(8) 0.2742(5) 0.041(4) Uani 0.50 1 d PG . 2 H37B H 0.3009 -0.1349 0.2936 0.049 Uiso 0.50 1 calc PR . 2 C38' C 0.3788(4) -0.1651(7) 0.2771(4) 0.048(4) Uani 0.50 1 d PG . 2 H38B H 0.3839 -0.2195 0.2986 0.058 Uiso 0.50 1 calc PR . 2 N5' N 0.4211(4) -0.1345(8) 0.2481(5) 0.034(4) Uani 0.50 1 d PGU . 2 N4 N 0.0777(4) 0.1712(8) 0.2531(5) 0.032(4) Uani 0.50 1 d PG . 1 C29 C 0.1197(4) 0.1996(7) 0.2231(4) 0.047(4) Uani 0.50 1 d PG . 1 H29A H 0.1154 0.2546 0.2022 0.056 Uiso 0.50 1 calc PR . 1 C30 C 0.1681(4) 0.1456(8) 0.2245(5) 0.047(4) Uani 0.50 1 d PG . 1 H30A H 0.1962 0.1646 0.2044 0.057 Uiso 0.50 1 calc PR . 1 C31 C 0.1746(4) 0.0633(8) 0.2557(5) 0.039(5) Uani 0.50 1 d PGDU . 1 C32 C 0.1326(5) 0.0349(7) 0.2857(5) 0.044(4) Uani 0.50 1 d PGU . 1 H32A H 0.1369 -0.0201 0.3067 0.053 Uiso 0.50 1 calc PR . 1 C33 C 0.0841(4) 0.0889(8) 0.2844(5) 0.042(4) Uani 0.50 1 d PGU . 1 H33A H 0.0561 0.0699 0.3044 0.050 Uiso 0.50 1 calc PR . 1 N4' N 0.0679(4) 0.1358(11) 0.2508(5) 0.049(6) Uani 0.50 1 d PG . 2 C29' C 0.0774(4) 0.0861(11) 0.2047(5) 0.070(6) Uani 0.50 1 d PG . 2 H29B H 0.0495 0.0819 0.1760 0.084 Uiso 0.50 1 calc PR . 2 C30' C 0.1286(5) 0.0427(10) 0.2015(5) 0.061(5) Uani 0.50 1 d PG . 2 H30B H 0.1350 0.0095 0.1707 0.073 Uiso 0.50 1 calc PR . 2 C31' C 0.1704(4) 0.0490(11) 0.2444(5) 0.052(6) Uani 0.50 1 d PGDU . 2 C32' C 0.1609(5) 0.0987(12) 0.2904(5) 0.070(7) Uani 0.50 1 d PG . 2 H32B H 0.1888 0.1028 0.3191 0.085 Uiso 0.50 1 calc PR . 2 C33' C 0.1096(6) 0.1420(11) 0.2936(4) 0.070(7) Uani 0.50 1 d PG . 2 H33B H 0.1033 0.1753 0.3245 0.084 Uiso 0.50 1 calc PR . 2 O1W O -0.0498(5) 0.3446(11) 0.6476(5) 0.057(3) Uani 0.50 1 d P . . O2W O 0.0449(6) 0.1268(14) 0.8526(6) 0.188(7) Uani 1 1 d . . . O5 O 0.0708(5) 0.3040(10) 0.3874(5) 0.059(3) Uani 0.60 1 d PU . . O5' O 0.0717(5) 0.2320(16) 0.3851(5) 0.056(5) Uani 0.40 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 Cd2 0.0144(3) 0.0628(5) 0.0201(3) 0.000 0.0046(3) 0.000 Cd1 0.0183(3) 0.0329(3) 0.0195(3) -0.00090(19) 0.00026(17) 0.0019(2) O2 0.032(3) 0.099(5) 0.027(3) -0.005(3) -0.009(2) 0.002(3) O4 0.020(3) 0.087(5) 0.040(3) 0.012(3) -0.002(2) -0.004(3) O6 0.031(3) 0.136(7) 0.022(3) 0.002(3) 0.008(2) -0.006(4) N3 0.071(5) 0.026(3) 0.049(4) 0.005(3) -0.002(4) -0.004(4) O7 0.027(3) 0.226(11) 0.028(3) 0.005(5) -0.002(3) -0.004(5) O1 0.039(3) 0.081(4) 0.024(3) 0.001(3) -0.002(2) 0.009(3) O3 0.030(3) 0.089(5) 0.037(3) -0.002(3) 0.018(2) -0.010(3) N2 0.043(4) 0.033(3) 0.041(4) -0.001(3) -0.001(3) 0.000(3) C1 0.028(3) 0.152(6) 0.026(3) -0.001(3) -0.004(2) -0.004(3) C2 0.029(2) 0.156(5) 0.029(2) -0.001(3) -0.003(2) -0.003(3) C3 0.029(2) 0.156(5) 0.030(2) 0.000(3) -0.003(2) -0.004(3) C4 0.027(2) 0.153(5) 0.027(2) 0.000(3) -0.003(2) -0.005(3) C5 0.026(3) 0.152(6) 0.027(3) 0.001(3) -0.002(2) -0.005(3) C6 0.028(4) 0.090(7) 0.031(4) -0.004(4) -0.007(3) -0.002(4) C7 0.021(4) 0.080(6) 0.020(3) 0.002(4) -0.003(3) -0.005(4) C8 0.024(4) 0.070(6) 0.018(3) -0.001(3) 0.003(3) 0.000(4) C9 0.021(3) 0.039(4) 0.021(3) 0.000(3) 0.002(3) -0.001(3) C10 0.018(3) 0.037(4) 0.023(3) -0.001(3) 0.000(3) 0.005(3) C11 0.021(3) 0.039(4) 0.023(3) 0.001(3) 0.002(3) -0.001(3) C12 0.018(3) 0.059(5) 0.023(3) 0.007(3) 0.002(3) -0.003(3) C13 0.038(4) 0.054(5) 0.022(4) -0.003(3) -0.007(3) 0.004(4) C14 0.021(3) 0.028(4) 0.027(3) -0.001(3) 0.004(3) -0.002(3) C15 0.023(4) 0.065(5) 0.015(3) 0.007(3) 0.002(3) 0.000(3) C16 0.026(4) 0.107(8) 0.029(4) -0.007(5) -0.002(3) -0.007(5) C17 0.058(6) 0.045(5) 0.070(6) -0.006(5) 0.014(5) 0.004(4) C18 0.086(6) 0.048(5) 0.083(8) -0.001(5) 0.021(6) 0.023(4) C19 0.090(5) 0.054(4) 0.059(4) -0.005(4) 0.005(4) 0.001(3) C20 0.101(10) 0.052(6) 0.083(8) -0.016(6) -0.005(7) -0.021(6) C21 0.062(7) 0.047(6) 0.083(8) 0.003(5) -0.014(6) -0.003(5) C22 0.036(3) 0.044(3) 0.042(3) -0.001(3) 0.006(3) 0.000(3) C23 0.033(4) 0.042(4) 0.039(4) -0.001(4) 0.008(4) -0.001(4) C22' 0.041(3) 0.053(3) 0.044(3) 0.000(4) 0.006(3) 0.000(3) C23' 0.039(4) 0.051(4) 0.044(4) 0.000(4) 0.006(4) 0.000(4) C24 0.063(7) 0.043(5) 0.071(7) -0.001(5) -0.002(5) 0.012(5) C25 0.136(12) 0.061(7) 0.057(7) -0.002(6) 0.009(7) 0.040(8) C26 0.174(15) 0.043(5) 0.035(5) 0.002(4) 0.013(7) -0.023(8) C27 0.131(12) 0.040(6) 0.073(8) 0.003(5) 0.010(8) -0.026(7) C28 0.075(7) 0.043(6) 0.075(7) 0.006(5) -0.006(6) -0.022(5) N1 0.022(3) 0.178(10) 0.017(3) 0.002(5) -0.002(3) -0.007(5) C39 0.055(7) 0.056(7) 0.056(7) 0.000(2) 0.007(2) 0.000(2) C40 0.025(11) 0.059(12) 0.074(16) 0.007(12) 0.000(10) 0.012(8) C34 0.028(9) 0.060(11) 0.064(12) -0.014(9) 0.015(8) 0.004(8) C35 0.042(10) 0.068(13) 0.049(10) -0.017(9) -0.001(8) 0.018(9) C36 0.019(8) 0.084(15) 0.036(11) -0.013(10) 0.006(7) 0.017(8) C37 0.060(13) 0.099(17) 0.023(8) 0.005(9) -0.005(8) 0.042(12) C38 0.051(12) 0.087(16) 0.027(9) 0.001(9) 0.018(8) 0.039(11) N5 0.031(7) 0.044(9) 0.036(8) -0.003(7) 0.003(6) -0.006(7) C39' 0.031(12) 0.045(11) 0.090(19) -0.010(11) 0.010(10) 0.017(8) C40' 0.064(16) 0.16(3) 0.014(9) -0.008(13) 0.000(10) 0.010(15) C34' 0.052(13) 0.058(13) 0.061(13) 0.008(11) 0.015(10) 0.012(10) C35' 0.049(11) 0.063(13) 0.061(12) 0.024(10) 0.020(9) 0.018(10) C36' 0.036(5) 0.036(5) 0.036(5) 0.001(2) 0.004(2) 0.001(2) C37' 0.017(7) 0.048(10) 0.058(10) 0.022(8) 0.011(7) 0.004(7) C38' 0.037(9) 0.059(11) 0.050(10) 0.015(8) 0.013(8) 0.009(8) N5' 0.034(4) 0.034(4) 0.034(4) 0.000(2) 0.004(2) 0.000(2) N4 0.016(7) 0.050(11) 0.031(8) 0.009(6) 0.011(5) 0.012(7) C29 0.034(9) 0.058(11) 0.052(10) 0.007(8) 0.020(8) 0.012(8) C30 0.039(9) 0.062(11) 0.045(10) 0.007(8) 0.023(8) 0.019(8) C31 0.039(5) 0.040(5) 0.040(5) 0.0001(10) 0.0046(11) 0.0002(10) C32 0.043(4) 0.045(4) 0.045(4) 0.002(2) 0.006(2) 0.001(2) C33 0.041(4) 0.043(4) 0.042(4) 0.002(2) 0.006(2) 0.001(2) N4' 0.037(10) 0.040(11) 0.073(13) 0.006(9) 0.029(9) 0.010(8) C29' 0.056(13) 0.079(15) 0.072(14) -0.022(12) -0.009(11) -0.008(11) C30' 0.042(11) 0.082(15) 0.059(12) -0.023(11) 0.006(9) 0.008(10) C31' 0.052(6) 0.052(6) 0.052(6) 0.0000(10) 0.0063(12) 0.0002(10) C32' 0.059(13) 0.115(19) 0.031(9) -0.011(10) -0.021(9) 0.030(13) C33' 0.072(15) 0.098(18) 0.039(11) 0.007(11) 0.000(10) 0.033(14) O1W 0.025(6) 0.098(11) 0.047(7) -0.011(7) 0.006(5) 0.006(6) O2W 0.141(11) 0.29(2) 0.127(11) -0.079(12) -0.006(9) 0.058(12) O5 0.058(3) 0.062(3) 0.058(4) 0.000(2) 0.007(2) -0.002(2) O5' 0.018(7) 0.137(18) 0.013(6) 0.013(8) 0.005(5) 0.026(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd2 O6 2.255(5) . ? Cd2 O6 2.255(5) 2 ? Cd2 N4 2.305(7) 2 ? Cd2 N4 2.305(7) . ? Cd2 N5' 2.344(10) 4 ? Cd2 N5' 2.344(10) 3_455 ? Cd2 N4' 2.465(10) . ? Cd2 N4' 2.465(10) 2 ? Cd2 N5 2.476(13) 4 ? Cd2 N5 2.48(3) 3_455 ? Cd1 O4 2.237(5) 8_556 ? Cd1 O3 2.267(5) 2_556 ? Cd1 N3 2.308(7) . ? Cd1 N2 2.309(7) 1_545 ? Cd1 O2 2.326(5) . ? Cd1 O1 2.481(5) . ? Cd1 C13 2.756(7) . ? O2 C13 1.257(10) . ? O4 C14 1.249(8) . ? O4 Cd1 2.237(5) 8_455 ? O6 C15 1.227(9) . ? N3 C24 1.327(12) . ? N3 C28 1.336(12) . ? O7 C16 1.210(11) . ? O1 C13 1.254(10) . ? O3 C14 1.233(8) . ? O3 Cd1 2.267(5) 2_556 ? N2 C17 1.293(11) . ? N2 C21 1.342(12) . ? N2 Cd1 2.309(6) 1_565 ? C1 C6 1.364(12) . ? C1 C2 1.373(12) . ? C1 C13 1.499(10) . ? C2 C3 1.388(12) . ? C2 H2A 0.9300 . ? C3 C4 1.385(13) . ? C3 H3A 0.9300 . ? C4 C5 1.369(12) . ? C4 C16 1.500(11) . ? C5 C6 1.378(11) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.387(10) . ? C7 C8 1.389(10) . ? C7 N1 1.417(9) . ? C8 C9 1.381(9) . ? C8 H8A 0.9300 . ? C9 C10 1.389(9) . ? C9 C14 1.503(9) . ? C10 C11 1.385(9) . ? C10 H10A 0.9300 . ? C11 C12 1.390(9) . ? C11 C15 1.495(9) . ? C12 H12A 0.9300 . ? C15 O5' 1.248(15) . ? C15 O5 1.269(14) . ? C16 N1 1.335(10) . ? C17 C18 1.419(14) . ? C17 H17A 0.9300 . ? C18 C19 1.347(16) . ? C18 H18A 0.9300 . ? C19 C20 1.361(17) . ? C19 C22 1.47(2) . ? C19 C22' 1.67(2) . ? C20 C21 1.357(15) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.372(16) . ? C22 H22A 0.9300 . ? C23 C26 1.43(2) . ? C23 H23A 0.9300 . ? C22' C23' 1.20(3) . ? C22' H22B 0.9300 . ? C23' C26 1.67(2) . ? C23' H23B 0.9300 . ? C24 C25 1.418(16) . ? C24 H24A 0.9300 . ? C25 C26 1.379(19) . ? C25 H25A 0.9300 . ? C26 C27 1.391(19) . ? C27 C28 1.370(14) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? N1 H1A 0.8600 . ? C39 C40 1.314(10) . ? C39 C31 1.500(16) . ? C39 H39A 0.9300 . ? C40 C36 1.545(15) . ? C40 H40A 0.9300 . ? C34 C35 1.3900 . ? C34 N5 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C37 H37A 0.9300 . ? C38 N5 1.3900 . ? C38 H38A 0.9300 . ? N5 Cd2 2.476(9) 3_545 ? C39' C40' 1.33(3) . ? C39' C31' 1.499(14) . ? C39' H39B 0.9300 . ? C40' C36' 1.538(16) . ? C40' H40B 0.9300 . ? C34' C35' 1.3900 . ? C34' N5' 1.3900 . ? C34' H34B 0.9300 . ? C35' C36' 1.3900 . ? C35' H35B 0.9300 . ? C36' C37' 1.3900 . ? C37' C38' 1.3900 . ? C37' H37B 0.9300 . ? C38' N5' 1.3900 . ? C38' H38B 0.9300 . ? N5' Cd2 2.344(7) 3_545 ? N4 C29 1.3900 . ? N4 C33 1.3900 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? N4' C29' 1.3900 . ? N4' C33' 1.3900 . ? C29' C30' 1.3900 . ? C29' H29B 0.9300 . ? C30' C31' 1.3900 . ? C30' H30B 0.9300 . ? C31' C32' 1.3900 . ? C32' C33' 1.3900 . ? C32' H32B 0.9300 . ? C33' H33B 0.9300 . ? O5 O5' 1.01(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 Cd2 O6 177.5(4) . 2 ? O6 Cd2 N4 82.8(3) . 2 ? O6 Cd2 N4 95.7(3) 2 2 ? O6 Cd2 N4 95.7(3) . . ? O6 Cd2 N4 82.8(3) 2 . ? N4 Cd2 N4 108.6(6) 2 . ? O6 Cd2 N5' 97.9(16) . 4 ? O6 Cd2 N5' 83.5(16) 2 4 ? N4 Cd2 N5' 179.3(16) 2 4 ? N4 Cd2 N5' 71.3(16) . 4 ? O6 Cd2 N5' 84(2) . 3_455 ? O6 Cd2 N5' 98(2) 2 3_455 ? N4 Cd2 N5' 71(2) 2 3_455 ? N4 Cd2 N5' 179(2) . 3_455 ? N5' Cd2 N5' 109(3) 4 3_455 ? O6 Cd2 N4' 95.5(4) . . ? O6 Cd2 N4' 82.6(4) 2 . ? N4 Cd2 N4' 96.1(5) 2 . ? N4 Cd2 N4' 12.6(4) . . ? N5' Cd2 N4' 83.9(15) 4 . ? N5' Cd2 N4' 167(2) 3_455 . ? O6 Cd2 N4' 82.6(4) . 2 ? O6 Cd2 N4' 95.5(4) 2 2 ? N4 Cd2 N4' 12.6(4) 2 2 ? N4 Cd2 N4' 96.1(5) . 2 ? N5' Cd2 N4' 167.4(16) 4 2 ? N5' Cd2 N4' 84(2) 3_455 2 ? N4' Cd2 N4' 83.5(7) . 2 ? O6 Cd2 N5 98.6(15) . 4 ? O6 Cd2 N5 83.3(15) 2 4 ? N4 Cd2 N5 166.8(18) 2 4 ? N4 Cd2 N5 84.4(19) . 4 ? N5' Cd2 N5 13(2) 4 4 ? N5' Cd2 N5 96(3) 3_455 4 ? N4' Cd2 N5 96.9(19) . 4 ? N4' Cd2 N5 178.7(14) 2 4 ? O6 Cd2 N5 83.3(18) . 3_455 ? O6 Cd2 N5 98.6(17) 2 3_455 ? N4 Cd2 N5 84(2) 2 3_455 ? N4 Cd2 N5 167(2) . 3_455 ? N5' Cd2 N5 96(3) 4 3_455 ? N5' Cd2 N5 13(3) 3_455 3_455 ? N4' Cd2 N5 178.7(16) . 3_455 ? N4' Cd2 N5 97(2) 2 3_455 ? N5 Cd2 N5 83(4) 4 3_455 ? O4 Cd1 O3 130.0(2) 8_556 2_556 ? O4 Cd1 N3 92.9(3) 8_556 . ? O3 Cd1 N3 86.4(3) 2_556 . ? O4 Cd1 N2 90.8(2) 8_556 1_545 ? O3 Cd1 N2 85.5(3) 2_556 1_545 ? N3 Cd1 N2 171.7(3) . 1_545 ? O4 Cd1 O2 88.5(2) 8_556 . ? O3 Cd1 O2 141.5(2) 2_556 . ? N3 Cd1 O2 94.1(3) . . ? N2 Cd1 O2 93.5(2) 1_545 . ? O4 Cd1 O1 142.49(19) 8_556 . ? O3 Cd1 O1 87.5(2) 2_556 . ? N3 Cd1 O1 91.1(2) . . ? N2 Cd1 O1 90.5(2) 1_545 . ? O2 Cd1 O1 54.03(19) . . ? O4 Cd1 C13 115.5(2) 8_556 . ? O3 Cd1 C13 114.6(2) 2_556 . ? N3 Cd1 C13 92.3(3) . . ? N2 Cd1 C13 92.8(2) 1_545 . ? O2 Cd1 C13 27.0(2) . . ? O1 Cd1 C13 27.1(2) . . ? C13 O2 Cd1 95.9(5) . . ? C14 O4 Cd1 117.7(5) . 8_455 ? C15 O6 Cd2 141.3(5) . . ? C24 N3 C28 119.4(9) . . ? C24 N3 Cd1 121.2(7) . . ? C28 N3 Cd1 119.4(7) . . ? C13 O1 Cd1 88.8(4) . . ? C14 O3 Cd1 165.5(6) . 2_556 ? C17 N2 C21 116.1(8) . . ? C17 N2 Cd1 121.8(6) . 1_565 ? C21 N2 Cd1 122.1(6) . 1_565 ? C6 C1 C2 118.9(8) . . ? C6 C1 C13 119.8(8) . . ? C2 C1 C13 121.3(8) . . ? C1 C2 C3 120.8(9) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 120.3(8) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 117.7(8) . . ? C5 C4 C16 118.2(8) . . ? C3 C4 C16 124.1(8) . . ? C4 C5 C6 122.0(9) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C1 C6 C5 120.2(8) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C12 C7 C8 119.8(6) . . ? C12 C7 N1 123.6(7) . . ? C8 C7 N1 116.6(6) . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 119.7(6) . . ? C8 C9 C14 120.3(6) . . ? C10 C9 C14 120.1(6) . . ? C11 C10 C9 120.2(6) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 120.1(6) . . ? C10 C11 C15 120.7(6) . . ? C12 C11 C15 119.2(6) . . ? C7 C12 C11 119.8(6) . . ? C7 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? O1 C13 O2 121.2(7) . . ? O1 C13 C1 120.3(7) . . ? O2 C13 C1 118.5(7) . . ? O1 C13 Cd1 64.2(4) . . ? O2 C13 Cd1 57.1(4) . . ? C1 C13 Cd1 175.2(6) . . ? O3 C14 O4 124.0(6) . . ? O3 C14 C9 118.9(6) . . ? O4 C14 C9 117.0(6) . . ? O6 C15 O5' 119.4(9) . . ? O6 C15 O5 120.9(8) . . ? O5' C15 O5 47.1(10) . . ? O6 C15 C11 117.9(6) . . ? O5' C15 C11 116.9(8) . . ? O5 C15 C11 115.6(8) . . ? O7 C16 N1 122.9(7) . . ? O7 C16 C4 119.4(7) . . ? N1 C16 C4 117.6(7) . . ? N2 C17 C18 121.6(10) . . ? N2 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? C19 C18 C17 121.2(10) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 116.7(11) . . ? C18 C19 C22 131.5(12) . . ? C20 C19 C22 111.7(12) . . ? C18 C19 C22' 96.5(11) . . ? C20 C19 C22' 146.5(12) . . ? C22 C19 C22' 35.8(9) . . ? C21 C20 C19 119.1(12) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? N2 C21 C20 125.3(11) . . ? N2 C21 H21A 117.4 . . ? C20 C21 H21A 117.4 . . ? C23 C22 C19 119.9(16) . . ? C23 C22 H22A 120.1 . . ? C19 C22 H22A 120.1 . . ? C22 C23 C26 122.2(17) . . ? C22 C23 H23A 118.9 . . ? C26 C23 H23A 118.9 . . ? C23' C22' C19 104.3(17) . . ? C23' C22' H22B 127.9 . . ? C19 C22' H22B 127.9 . . ? C22' C23' C26 101.4(18) . . ? C22' C23' H23B 129.3 . . ? C26 C23' H23B 129.3 . . ? N3 C24 C25 119.8(11) . . ? N3 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C26 C25 C24 121.1(12) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C25 C26 C27 116.9(11) . . ? C25 C26 C23 132.3(15) . . ? C27 C26 C23 110.9(14) . . ? C25 C26 C23' 96.4(13) . . ? C27 C26 C23' 145.9(13) . . ? C23 C26 C23' 36.4(9) . . ? C28 C27 C26 119.4(13) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? N3 C28 C27 123.4(12) . . ? N3 C28 H28A 118.3 . . ? C27 C28 H28A 118.3 . . ? C16 N1 C7 128.4(7) . . ? C16 N1 H1A 115.8 . . ? C7 N1 H1A 115.8 . . ? C40 C39 C31 124.0(16) . . ? C40 C39 H39A 118.0 . . ? C31 C39 H39A 118.0 . . ? C39 C40 C36 120.5(17) . . ? C39 C40 H40A 119.7 . . ? C36 C40 H40A 119.7 . . ? C35 C34 N5 120.0 . . ? C35 C34 H34A 120.0 . . ? N5 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 C40 96.8(11) . . ? C35 C36 C40 140.7(12) . . ? C36 C37 C38 120.0 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? N5 C38 C37 120.0 . . ? N5 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 N5 C34 120.0 . . ? C38 N5 Cd2 112.0(5) . 3_545 ? C34 N5 Cd2 120.6(5) . 3_545 ? C40' C39' C31' 132(2) . . ? C40' C39' H39B 114.1 . . ? C31' C39' H39B 114.1 . . ? C39' C40' C36' 110.8(16) . . ? C39' C40' H40B 124.6 . . ? C36' C40' H40B 124.6 . . ? C35' C34' N5' 120.0 . . ? C35' C34' H34B 120.0 . . ? N5' C34' H34B 120.0 . . ? C36' C35' C34' 120.0 . . ? C36' C35' H35B 120.0 . . ? C34' C35' H35B 120.0 . . ? C35' C36' C37' 120.0 . . ? C35' C36' C40' 144.6(15) . . ? C37' C36' C40' 91.2(14) . . ? C36' C37' C38' 120.0 . . ? C36' C37' H37B 120.0 . . ? C38' C37' H37B 120.0 . . ? N5' C38' C37' 120.0 . . ? N5' C38' H38B 120.0 . . ? C37' C38' H38B 120.0 . . ? C38' N5' C34' 120.0 . . ? C38' N5' Cd2 117.2(5) . 3_545 ? C34' N5' Cd2 122.6(5) . 3_545 ? C29 N4 C33 120.0 . . ? C29 N4 Cd2 117.4(5) . . ? C33 N4 Cd2 122.6(5) . . ? C30 C29 N4 120.0 . . ? C30 C29 H29A 120.0 . . ? N4 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 C39 125.5(10) . . ? C32 C31 C39 114.0(10) . . ? C33 C32 C31 120.0 . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 N4 120.0 . . ? C32 C33 H33A 120.0 . . ? N4 C33 H33A 120.0 . . ? C29' N4' C33' 120.0 . . ? C29' N4' Cd2 122.7(7) . . ? C33' N4' Cd2 112.5(7) . . ? C30' C29' N4' 120.0 . . ? C30' C29' H29B 120.0 . . ? N4' C29' H29B 120.0 . . ? C29' C30' C31' 120.0 . . ? C29' C30' H30B 120.0 . . ? C31' C30' H30B 120.0 . . ? C32' C31' C30' 120.0 . . ? C32' C31' C39' 121.5(13) . . ? C30' C31' C39' 118.4(13) . . ? C31' C32' C33' 120.0 . . ? C31' C32' H32B 120.0 . . ? C33' C32' H32B 120.0 . . ? C32' C33' N4' 120.0 . . ? C32' C33' H33B 120.0 . . ? N4' C33' H33B 120.0 . . ? O5' O5 C15 65.3(11) . . ? O5 O5' C15 67.5(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cd1 O2 C13 -180.0(6) 8_556 . . . ? O3 Cd1 O2 C13 2.1(8) 2_556 . . . ? N3 Cd1 O2 C13 -87.2(6) . . . . ? N2 Cd1 O2 C13 89.3(6) 1_545 . . . ? O1 Cd1 O2 C13 1.3(5) . . . . ? O6 Cd2 O6 C15 91.8(11) 2 . . . ? N4 Cd2 O6 C15 146.0(12) 2 . . . ? N4 Cd2 O6 C15 37.9(12) . . . . ? N5' Cd2 O6 C15 -34.0(19) 4 . . . ? N5' Cd2 O6 C15 -142(2) 3_455 . . . ? N4' Cd2 O6 C15 50.5(12) . . . . ? N4' Cd2 O6 C15 133.2(12) 2 . . . ? N5 Cd2 O6 C15 -47(2) 4 . . . ? N5 Cd2 O6 C15 -129(2) 3_455 . . . ? O4 Cd1 N3 C24 -173.2(7) 8_556 . . . ? O3 Cd1 N3 C24 -43.4(7) 2_556 . . . ? N2 Cd1 N3 C24 -57(2) 1_545 . . . ? O2 Cd1 N3 C24 98.1(7) . . . . ? O1 Cd1 N3 C24 44.1(7) . . . . ? C13 Cd1 N3 C24 71.1(7) . . . . ? O4 Cd1 N3 C28 6.8(7) 8_556 . . . ? O3 Cd1 N3 C28 136.7(7) 2_556 . . . ? N2 Cd1 N3 C28 123.1(17) 1_545 . . . ? O2 Cd1 N3 C28 -81.9(7) . . . . ? O1 Cd1 N3 C28 -135.9(7) . . . . ? C13 Cd1 N3 C28 -108.9(7) . . . . ? O4 Cd1 O1 C13 -3.3(7) 8_556 . . . ? O3 Cd1 O1 C13 179.3(5) 2_556 . . . ? N3 Cd1 O1 C13 92.9(5) . . . . ? N2 Cd1 O1 C13 -95.2(5) 1_545 . . . ? O2 Cd1 O1 C13 -1.2(5) . . . . ? C6 C1 C2 C3 3(2) . . . . ? C13 C1 C2 C3 -177.7(12) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C2 C3 C4 C16 -176.8(13) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C16 C4 C5 C6 178.8(12) . . . . ? C2 C1 C6 C5 -1.1(19) . . . . ? C13 C1 C6 C5 179.7(11) . . . . ? C4 C5 C6 C1 0(2) . . . . ? C12 C7 C8 C9 -0.2(14) . . . . ? N1 C7 C8 C9 178.7(9) . . . . ? C7 C8 C9 C10 -0.5(12) . . . . ? C7 C8 C9 C14 179.7(7) . . . . ? C8 C9 C10 C11 0.3(11) . . . . ? C14 C9 C10 C11 -180.0(6) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C9 C10 C11 C15 179.6(7) . . . . ? C8 C7 C12 C11 1.1(13) . . . . ? N1 C7 C12 C11 -177.7(9) . . . . ? C10 C11 C12 C7 -1.3(12) . . . . ? C15 C11 C12 C7 179.7(8) . . . . ? Cd1 O1 C13 O2 2.2(9) . . . . ? Cd1 O1 C13 C1 -178.0(9) . . . . ? Cd1 O2 C13 O1 -2.3(9) . . . . ? Cd1 O2 C13 C1 177.8(8) . . . . ? C6 C1 C13 O1 180.0(10) . . . . ? C2 C1 C13 O1 0.7(18) . . . . ? C6 C1 C13 O2 -0.2(17) . . . . ? C2 C1 C13 O2 -179.4(11) . . . . ? C6 C1 C13 Cd1 22(10) . . . . ? C2 C1 C13 Cd1 -157(8) . . . . ? O4 Cd1 C13 O1 177.8(5) 8_556 . . . ? O3 Cd1 C13 O1 -0.8(6) 2_556 . . . ? N3 Cd1 C13 O1 -87.9(5) . . . . ? N2 Cd1 C13 O1 85.6(5) 1_545 . . . ? O2 Cd1 C13 O1 177.8(9) . . . . ? O4 Cd1 C13 O2 0.0(6) 8_556 . . . ? O3 Cd1 C13 O2 -178.5(5) 2_556 . . . ? N3 Cd1 C13 O2 94.3(6) . . . . ? N2 Cd1 C13 O2 -92.2(6) 1_545 . . . ? O1 Cd1 C13 O2 -177.8(9) . . . . ? O4 Cd1 C13 C1 -24(9) 8_556 . . . ? O3 Cd1 C13 C1 158(9) 2_556 . . . ? N3 Cd1 C13 C1 71(9) . . . . ? N2 Cd1 C13 C1 -116(9) 1_545 . . . ? O2 Cd1 C13 C1 -24(8) . . . . ? O1 Cd1 C13 C1 159(9) . . . . ? Cd1 O3 C14 O4 -31(3) 2_556 . . . ? Cd1 O3 C14 C9 149.0(19) 2_556 . . . ? Cd1 O4 C14 O3 -2.0(10) 8_455 . . . ? Cd1 O4 C14 C9 177.7(5) 8_455 . . . ? C8 C9 C14 O3 -8.0(11) . . . . ? C10 C9 C14 O3 172.3(7) . . . . ? C8 C9 C14 O4 172.3(7) . . . . ? C10 C9 C14 O4 -7.5(10) . . . . ? Cd2 O6 C15 O5' -27(2) . . . . ? Cd2 O6 C15 O5 28.3(17) . . . . ? Cd2 O6 C15 C11 -179.2(7) . . . . ? C10 C11 C15 O6 -3.0(12) . . . . ? C12 C11 C15 O6 176.0(8) . . . . ? C10 C11 C15 O5' -156.1(14) . . . . ? C12 C11 C15 O5' 22.9(16) . . . . ? C10 C11 C15 O5 150.9(10) . . . . ? C12 C11 C15 O5 -30.0(13) . . . . ? C5 C4 C16 O7 3.0(19) . . . . ? C3 C4 C16 O7 -178.0(13) . . . . ? C5 C4 C16 N1 -179.7(12) . . . . ? C3 C4 C16 N1 -1(2) . . . . ? C21 N2 C17 C18 1.4(15) . . . . ? Cd1 N2 C17 C18 -175.6(8) 1_565 . . . ? N2 C17 C18 C19 -0.3(18) . . . . ? C17 C18 C19 C20 -1.8(18) . . . . ? C17 C18 C19 C22 175.2(13) . . . . ? C17 C18 C19 C22' -177.0(12) . . . . ? C18 C19 C20 C21 2.7(18) . . . . ? C22 C19 C20 C21 -174.9(12) . . . . ? C22' C19 C20 C21 173.9(17) . . . . ? C17 N2 C21 C20 -0.5(16) . . . . ? Cd1 N2 C21 C20 176.5(9) 1_565 . . . ? C19 C20 C21 N2 -1.6(19) . . . . ? C18 C19 C22 C23 12(2) . . . . ? C20 C19 C22 C23 -170.9(14) . . . . ? C22' C19 C22 C23 -1.4(15) . . . . ? C19 C22 C23 C26 -179.0(13) . . . . ? C18 C19 C22' C23' -168.8(15) . . . . ? C20 C19 C22' C23' 19(3) . . . . ? C22 C19 C22' C23' 1.1(16) . . . . ? C19 C22' C23' C26 178.9(10) . . . . ? C28 N3 C24 C25 0.4(15) . . . . ? Cd1 N3 C24 C25 -179.6(8) . . . . ? N3 C24 C25 C26 -1.1(17) . . . . ? C24 C25 C26 C27 2.2(17) . . . . ? C24 C25 C26 C23 -178.2(13) . . . . ? C24 C25 C26 C23' 174.8(11) . . . . ? C22 C23 C26 C25 -11(2) . . . . ? C22 C23 C26 C27 168.2(14) . . . . ? C22 C23 C26 C23' 0.3(15) . . . . ? C22' C23' C26 C25 170.5(14) . . . . ? C22' C23' C26 C27 -21(3) . . . . ? C22' C23' C26 C23 -0.7(15) . . . . ? C25 C26 C27 C28 -2.6(17) . . . . ? C23 C26 C27 C28 177.7(12) . . . . ? C23' C26 C27 C28 -169.4(16) . . . . ? C24 N3 C28 C27 -0.9(16) . . . . ? Cd1 N3 C28 C27 179.1(9) . . . . ? C26 C27 C28 N3 2.0(18) . . . . ? O7 C16 N1 C7 -2(2) . . . . ? C4 C16 N1 C7 -179.3(11) . . . . ? C12 C7 N1 C16 -2.3(18) . . . . ? C8 C7 N1 C16 178.9(11) . . . . ? C31 C39 C40 C36 168.2(18) . . . . ? N5 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C34 C35 C36 C40 -156.9(19) . . . . ? C39 C40 C36 C37 127(2) . . . . ? C39 C40 C36 C35 -73(3) . . . . ? C35 C36 C37 C38 0.0 . . . . ? C40 C36 C37 C38 165.5(12) . . . . ? C36 C37 C38 N5 0.0 . . . . ? C37 C38 N5 C34 0.0 . . . . ? C37 C38 N5 Cd2 150.1(7) . . . 3_545 ? C35 C34 N5 C38 0.0 . . . . ? C35 C34 N5 Cd2 -147.5(8) . . . 3_545 ? C31' C39' C40' C36' -170(2) . . . . ? N5' C34' C35' C36' 0.0 . . . . ? C34' C35' C36' C37' 0.0 . . . . ? C34' C35' C36' C40' 148(2) . . . . ? C39' C40' C36' C35' 87(3) . . . . ? C39' C40' C36' C37' -120(2) . . . . ? C35' C36' C37' C38' 0.0 . . . . ? C40' C36' C37' C38' -162.3(13) . . . . ? C36' C37' C38' N5' 0.0 . . . . ? C37' C38' N5' C34' 0.0 . . . . ? C37' C38' N5' Cd2 -174.8(8) . . . 3_545 ? C35' C34' N5' C38' 0.0 . . . . ? C35' C34' N5' Cd2 174.5(8) . . . 3_545 ? O6 Cd2 N4 C29 -135.6(6) . . . . ? O6 Cd2 N4 C29 46.4(6) 2 . . . ? N4 Cd2 N4 C29 140.1(8) 2 . . . ? N5' Cd2 N4 C29 -39.1(18) 4 . . . ? N5' Cd2 N4 C29 -133(100) 3_455 . . . ? N4' Cd2 N4 C29 135(3) . . . . ? N4' Cd2 N4 C29 141.2(6) 2 . . . ? N5 Cd2 N4 C29 -37.5(16) 4 . . . ? N5 Cd2 N4 C29 -50(8) 3_455 . . . ? O6 Cd2 N4 C33 42.8(7) . . . . ? O6 Cd2 N4 C33 -135.2(7) 2 . . . ? N4 Cd2 N4 C33 -41.6(6) 2 . . . ? N5' Cd2 N4 C33 139.2(18) 4 . . . ? N5' Cd2 N4 C33 46(100) 3_455 . . . ? N4' Cd2 N4 C33 -47(2) . . . . ? N4' Cd2 N4 C33 -40.4(8) 2 . . . ? N5 Cd2 N4 C33 140.8(16) 4 . . . ? N5 Cd2 N4 C33 128(8) 3_455 . . . ? C33 N4 C29 C30 0.0 . . . . ? Cd2 N4 C29 C30 178.4(9) . . . . ? N4 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C29 C30 C31 C39 -171.3(17) . . . . ? C40 C39 C31 C30 -9(3) . . . . ? C40 C39 C31 C32 180(2) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C39 C31 C32 C33 172.2(15) . . . . ? C31 C32 C33 N4 0.0 . . . . ? C29 N4 C33 C32 0.0 . . . . ? Cd2 N4 C33 C32 -178.3(9) . . . . ? O6 Cd2 N4' C29' 162.1(8) . . . . ? O6 Cd2 N4' C29' -16.2(8) 2 . . . ? N4 Cd2 N4' C29' 78.8(9) 2 . . . ? N4 Cd2 N4' C29' -106(2) . . . . ? N5' Cd2 N4' C29' -100.5(18) 4 . . . ? N5' Cd2 N4' C29' 77(10) 3_455 . . . ? N4' Cd2 N4' C29' 80.2(9) 2 . . . ? N5 Cd2 N4' C29' -98.5(16) 4 . . . ? N5 Cd2 N4' C29' -173(100) 3_455 . . . ? O6 Cd2 N4' C33' -42.6(7) . . . . ? O6 Cd2 N4' C33' 139.1(7) 2 . . . ? N4 Cd2 N4' C33' -125.9(7) 2 . . . ? N4 Cd2 N4' C33' 49(2) . . . . ? N5' Cd2 N4' C33' 54.9(17) 4 . . . ? N5' Cd2 N4' C33' -127(10) 3_455 . . . ? N4' Cd2 N4' C33' -124.5(9) 2 . . . ? N5 Cd2 N4' C33' 56.8(16) 4 . . . ? N5 Cd2 N4' C33' -17(100) 3_455 . . . ? C33' N4' C29' C30' 0.0 . . . . ? Cd2 N4' C29' C30' 153.6(10) . . . . ? N4' C29' C30' C31' 0.0 . . . . ? C29' C30' C31' C32' 0.0 . . . . ? C29' C30' C31' C39' -175.9(16) . . . . ? C40' C39' C31' C32' 6(4) . . . . ? C40' C39' C31' C30' -178(3) . . . . ? C30' C31' C32' C33' 0.0 . . . . ? C39' C31' C32' C33' 175.7(16) . . . . ? C31' C32' C33' N4' 0.0 . . . . ? C29' N4' C33' C32' 0.0 . . . . ? Cd2 N4' C33' C32' -156.1(9) . . . . ? O6 C15 O5 O5' -102.9(13) . . . . ? C11 C15 O5 O5' 104.0(12) . . . . ? O6 C15 O5' O5 106.4(14) . . . . ? C11 C15 O5' O5 -100.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.305 _refine_diff_density_min -4.106 _refine_diff_density_rms 0.145 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 142 55 ' ' 2 0.000 0.000 0.500 142 55 ' ' 3 0.500 0.000 0.500 144 51 ' ' 4 0.500 0.000 1.000 144 52 ' ' 5 0.000 0.069 0.750 9 2 ' ' 6 0.500 0.105 0.250 10 1 ' ' 7 0.000 0.395 0.750 10 1 ' ' 8 0.500 0.430 0.250 9 2 ' ' 9 0.000 0.500 0.500 144 51 ' ' 10 0.500 0.500 0.500 142 55 ' ' 11 0.500 0.500 0.000 142 55 ' ' 12 1.000 0.500 1.000 144 52 ' ' 13 0.500 0.569 0.750 9 2 ' ' 14 0.000 0.605 0.250 10 1 ' ' 15 0.500 0.895 0.750 10 1 ' ' 16 0.000 0.930 0.250 9 2 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 918288' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 N6 O27 Zn4' _chemical_formula_weight 1510.58 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.157(2) _cell_length_b 16.6590(12) _cell_length_c 14.5584(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.284(3) _cell_angle_gamma 90.00 _cell_volume 6817.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8270 _exptl_absorpt_correction_T_max 0.8594 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39343 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6003 _reflns_number_gt 4417 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+18.7645P] 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 6003 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.301581(18) 0.14792(3) 0.64098(4) 0.03029(18) Uani 1 1 d . . . Zn2 Zn 0.211436(17) 0.24730(3) 0.57495(4) 0.02905(17) Uani 1 1 d . . . O1 O 0.25858(12) 0.0785(2) 0.7048(3) 0.0440(9) Uani 1 1 d . . . O2 O 0.19425(11) 0.15504(19) 0.6763(2) 0.0374(8) Uani 1 1 d . . . O3 O 0.17581(12) -0.25977(18) 0.7872(3) 0.0383(8) Uani 1 1 d . . . O4 O 0.24227(11) -0.19207(19) 0.8258(2) 0.0360(8) Uani 1 1 d . . . O5 O -0.16355(11) -0.1888(2) 0.5134(3) 0.0402(8) Uani 1 1 d . . . O6 O -0.19503(12) -0.0662(2) 0.5157(3) 0.0421(9) Uani 1 1 d . . . O7 O 0.03772(12) 0.0706(2) 0.6472(3) 0.0528(10) Uani 1 1 d . . . N1 N -0.13813(14) 0.5833(2) 0.6342(3) 0.0384(10) Uani 1 1 d . . . N2 N 0.15495(14) 0.3202(2) 0.6155(3) 0.0384(10) Uani 1 1 d . . . N3 N 0.06046(15) -0.0587(3) 0.6580(3) 0.0494(12) Uani 1 1 d . . . H3B H 0.0500 -0.1070 0.6513 0.059 Uiso 1 1 calc R . . C1 C -0.02061(16) -0.0305(3) 0.6092(3) 0.0357(12) Uani 1 1 d . . . C2 C -0.0293(2) -0.1093(4) 0.5871(5) 0.067(2) Uani 1 1 d . . . H2A H -0.0043 -0.1458 0.5901 0.080 Uiso 1 1 calc R . . C3 C -0.0748(2) -0.1357(3) 0.5604(5) 0.0636(19) Uani 1 1 d . . . H3A H -0.0801 -0.1896 0.5466 0.076 Uiso 1 1 calc R . . C4 C -0.11204(16) -0.0824(3) 0.5543(3) 0.0341(11) Uani 1 1 d . . . C5 C -0.10304(18) -0.0034(3) 0.5737(4) 0.0488(15) Uani 1 1 d . . . H5A H -0.1278 0.0335 0.5685 0.059 Uiso 1 1 calc R . . C6 C -0.05768(18) 0.0225(3) 0.6010(4) 0.0507(15) Uani 1 1 d . . . H6A H -0.0524 0.0766 0.6139 0.061 Uiso 1 1 calc R . . C7 C 0.10918(17) -0.0523(3) 0.6869(4) 0.0368(12) Uani 1 1 d . . . C8 C 0.13558(17) 0.0177(3) 0.6815(3) 0.0331(11) Uani 1 1 d . . . H8A H 0.1214 0.0647 0.6591 0.040 Uiso 1 1 calc R . . C9 C 0.18373(16) 0.0167(3) 0.7100(3) 0.0297(10) Uani 1 1 d . . . C10 C 0.20480(16) -0.0519(3) 0.7447(3) 0.0324(11) Uani 1 1 d . . . H10A H 0.2368 -0.0513 0.7641 0.039 Uiso 1 1 calc R . . C11 C 0.17877(16) -0.1224(3) 0.7511(3) 0.0318(11) Uani 1 1 d . . . C12 C 0.13079(17) -0.1215(3) 0.7211(4) 0.0378(12) Uani 1 1 d . . . H12A H 0.1130 -0.1684 0.7241 0.045 Uiso 1 1 calc R . . C13 C 0.21370(16) 0.0894(3) 0.6956(3) 0.0317(11) Uani 1 1 d . . . C14 C 0.20108(16) -0.1961(3) 0.7913(3) 0.0297(10) Uani 1 1 d . . . C15 C -0.16112(17) -0.1136(3) 0.5252(3) 0.0351(11) Uani 1 1 d . . . C16 C 0.02824(16) -0.0009(3) 0.6396(3) 0.0361(12) Uani 1 1 d . . . C17 C -0.09592(19) 0.6191(4) 0.6315(5) 0.0581(17) Uani 1 1 d . . . H17A H -0.0945 0.6749 0.6317 0.070 Uiso 1 1 calc R . . C18 C -0.0542(2) 0.5759(4) 0.6284(5) 0.0632(18) Uani 1 1 d . . . H18A H -0.0252 0.6027 0.6273 0.076 Uiso 1 1 calc R . . C19 C -0.0553(2) 0.4937(3) 0.6271(4) 0.0492(14) Uani 1 1 d . . . C20 C -0.0988(2) 0.4569(4) 0.6283(5) 0.0569(16) Uani 1 1 d . . . H20A H -0.1010 0.4012 0.6277 0.068 Uiso 1 1 calc R . . C21 C -0.1394(2) 0.5034(3) 0.6305(4) 0.0505(15) Uani 1 1 d . . . H21A H -0.1688 0.4779 0.6294 0.061 Uiso 1 1 calc R . . C22 C 0.1126(2) 0.2876(4) 0.6282(5) 0.0561(16) Uani 1 1 d . . . H22A H 0.1105 0.2321 0.6335 0.067 Uiso 1 1 calc R . . C23 C 0.0719(2) 0.3325(4) 0.6337(5) 0.0606(18) Uani 1 1 d . . . H23A H 0.0431 0.3073 0.6425 0.073 Uiso 1 1 calc R . . C24 C 0.07391(19) 0.4161(3) 0.6260(4) 0.0465(14) Uani 1 1 d . . . C25 C 0.1183(2) 0.4493(3) 0.6172(4) 0.0503(15) Uani 1 1 d . . . H25A H 0.1219 0.5047 0.6146 0.060 Uiso 1 1 calc R . . C26 C 0.15702(19) 0.3998(3) 0.6122(4) 0.0441(13) Uani 1 1 d . . . H26A H 0.1866 0.4235 0.6063 0.053 Uiso 1 1 calc R . . C27 C -0.0125(2) 0.4427(4) 0.6253(5) 0.0604(17) Uani 1 1 d . . . H27A H -0.0173 0.3875 0.6232 0.072 Uiso 1 1 calc R . . C28 C 0.0320(2) 0.4679(4) 0.6263(4) 0.0571(16) Uani 1 1 d . . . H28A H 0.0371 0.5231 0.6274 0.069 Uiso 1 1 calc R . . O1W O 0.26709(10) 0.17449(17) 0.5270(2) 0.0287(7) Uani 1 1 d . . . O2W O 0.5000 -0.3096(5) 0.7500 0.125(3) Uani 1 2 d S . . O3W O 0.4370(5) -0.2496(6) 0.6056(10) 0.110(4) Uani 0.50 1 d P . . O4W O 0.3375(6) -0.2850(9) 0.566(2) 0.470(19) Uani 1 1 d . . . O5W O 0.2788(4) -0.4086(5) 0.4972(7) 0.186(4) Uani 1 1 d . . . O6W O 0.2056(5) -0.4219(9) 0.6039(8) 0.124(5) Uani 0.50 1 d P . . O7W O 0.1365(4) -0.3263(7) 0.6174(8) 0.101(4) Uani 0.50 1 d P . . O8W O 0.0430(5) -0.2955(11) 0.5902(14) 0.167(7) Uani 0.50 1 d P . . O9W O 0.0268(5) -0.2389(9) 0.7234(14) 0.164(8) Uani 0.50 1 d P . . O10W O 0.2899(4) -0.1627(6) 0.6453(8) 0.089(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 0.0150(3) 0.0213(3) 0.0540(4) -0.0012(2) -0.0037(2) 0.0030(2) Zn2 0.0141(3) 0.0223(3) 0.0505(4) -0.0010(2) -0.0008(2) 0.0033(2) O1 0.0209(19) 0.037(2) 0.073(3) 0.0157(18) -0.0056(17) -0.0024(15) O2 0.0275(19) 0.0244(17) 0.060(2) 0.0064(15) 0.0031(16) -0.0011(14) O3 0.0298(19) 0.0254(17) 0.059(2) 0.0075(15) -0.0057(16) -0.0047(14) O4 0.0214(18) 0.0288(18) 0.057(2) 0.0091(15) -0.0040(16) -0.0008(14) O5 0.0210(18) 0.0332(19) 0.065(2) 0.0008(17) -0.0077(16) -0.0061(15) O6 0.0189(18) 0.0370(19) 0.070(2) -0.0048(17) -0.0042(16) -0.0011(15) O7 0.027(2) 0.035(2) 0.095(3) -0.003(2) -0.0113(19) -0.0053(16) N1 0.020(2) 0.031(2) 0.064(3) -0.0009(19) -0.0027(19) 0.0085(17) N2 0.022(2) 0.033(2) 0.061(3) -0.001(2) 0.0040(19) 0.0072(18) N3 0.027(2) 0.033(2) 0.085(4) 0.009(2) -0.019(2) -0.0079(19) C1 0.020(3) 0.036(3) 0.050(3) 0.007(2) -0.006(2) -0.008(2) C2 0.026(3) 0.043(3) 0.128(6) -0.005(4) -0.024(3) 0.004(3) C3 0.028(3) 0.033(3) 0.127(6) -0.003(3) -0.017(3) -0.004(2) C4 0.020(2) 0.037(3) 0.045(3) 0.006(2) -0.004(2) -0.003(2) C5 0.022(3) 0.040(3) 0.083(4) -0.011(3) -0.010(3) 0.004(2) C6 0.027(3) 0.032(3) 0.091(5) -0.011(3) -0.017(3) -0.003(2) C7 0.019(2) 0.033(3) 0.056(3) 0.005(2) -0.009(2) -0.005(2) C8 0.025(3) 0.029(2) 0.044(3) 0.007(2) -0.007(2) 0.000(2) C9 0.020(2) 0.030(2) 0.039(3) 0.005(2) -0.0017(19) -0.0037(19) C10 0.017(2) 0.033(3) 0.046(3) 0.007(2) -0.003(2) -0.003(2) C11 0.020(2) 0.027(2) 0.048(3) 0.002(2) 0.000(2) -0.0008(19) C12 0.026(3) 0.030(3) 0.057(3) 0.004(2) -0.005(2) -0.006(2) C13 0.022(3) 0.027(2) 0.045(3) 0.006(2) -0.004(2) -0.001(2) C14 0.021(3) 0.026(2) 0.042(3) 0.002(2) 0.004(2) -0.0003(19) C15 0.023(3) 0.040(3) 0.041(3) 0.001(2) -0.002(2) -0.007(2) C16 0.018(3) 0.044(3) 0.046(3) 0.004(2) -0.006(2) -0.005(2) C17 0.026(3) 0.039(3) 0.110(5) -0.008(3) 0.006(3) 0.006(2) C18 0.023(3) 0.052(4) 0.115(6) -0.004(4) 0.005(3) 0.005(3) C19 0.038(3) 0.046(3) 0.063(4) -0.004(3) 0.000(3) 0.020(3) C20 0.038(3) 0.036(3) 0.096(5) 0.002(3) 0.001(3) 0.017(3) C21 0.031(3) 0.036(3) 0.084(4) -0.005(3) -0.001(3) 0.002(2) C22 0.032(3) 0.042(3) 0.096(5) 0.010(3) 0.016(3) 0.008(3) C23 0.025(3) 0.054(4) 0.104(5) 0.009(3) 0.014(3) 0.008(3) C24 0.032(3) 0.048(3) 0.060(4) 0.000(3) 0.005(3) 0.020(3) C25 0.038(3) 0.034(3) 0.079(4) -0.003(3) 0.006(3) 0.015(2) C26 0.030(3) 0.035(3) 0.067(4) -0.003(3) 0.006(3) 0.006(2) C27 0.045(4) 0.051(4) 0.085(5) 0.001(3) 0.002(3) 0.020(3) C28 0.035(3) 0.058(4) 0.079(4) 0.003(3) 0.005(3) 0.019(3) O1W 0.0150(16) 0.0196(15) 0.0508(19) 0.0000(14) -0.0023(13) 0.0016(12) O2W 0.123(8) 0.069(5) 0.189(10) 0.000 0.047(7) 0.000 O3W 0.112(10) 0.055(7) 0.157(12) 0.030(7) -0.029(9) -0.010(6) O4W 0.227(16) 0.178(13) 1.00(6) -0.22(2) 0.01(2) 0.020(11) O5W 0.234(11) 0.102(6) 0.220(10) 0.002(6) -0.017(8) 0.045(7) O6W 0.116(11) 0.164(13) 0.089(8) 0.000(8) -0.015(7) -0.045(10) O7W 0.116(10) 0.096(8) 0.087(7) -0.033(6) -0.044(7) 0.015(7) O8W 0.073(9) 0.179(16) 0.24(2) 0.066(15) -0.027(11) -0.024(10) O9W 0.129(12) 0.133(12) 0.22(2) 0.075(13) -0.087(14) -0.046(9) O10W 0.089(8) 0.076(7) 0.104(8) 0.006(6) 0.035(6) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1W 1.926(3) . ? Zn1 O3 1.946(3) 4_556 ? Zn1 O1 1.948(3) . ? Zn1 N1 2.017(4) 3_545 ? Zn1 Zn2 3.1349(7) . ? Zn2 O5 2.055(3) 5_556 ? Zn2 O1W 2.090(3) 7_556 ? Zn2 N2 2.111(4) . ? Zn2 O1W 2.131(3) . ? Zn2 O4 2.143(3) 4_556 ? Zn2 O2 2.204(3) . ? O1 C13 1.276(5) . ? O2 C13 1.248(5) . ? O3 C14 1.276(5) . ? O3 Zn1 1.946(3) 4_546 ? O4 C14 1.239(5) . ? O4 Zn2 2.143(3) 4_546 ? O5 C15 1.265(6) . ? O5 Zn2 2.055(3) 5_556 ? O6 C15 1.240(6) . ? O7 C16 1.225(6) . ? N1 C17 1.333(7) . ? N1 C21 1.333(7) . ? N1 Zn1 2.017(4) 3_455 ? N2 C26 1.330(6) . ? N2 C22 1.332(7) . ? N3 C16 1.340(6) . ? N3 C7 1.416(6) . ? N3 H3B 0.8600 . ? C1 C6 1.367(7) . ? C1 C2 1.370(8) . ? C1 C16 1.503(6) . ? C2 C3 1.389(8) . ? C2 H2A 0.9300 . ? C3 C4 1.372(7) . ? C3 H3A 0.9300 . ? C4 C5 1.367(7) . ? C4 C15 1.514(6) . ? C5 C6 1.385(7) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.384(7) . ? C7 C8 1.387(7) . ? C8 C9 1.395(6) . ? C8 H8A 0.9300 . ? C9 C10 1.370(6) . ? C9 C13 1.498(6) . ? C10 C11 1.390(6) . ? C10 H10A 0.9300 . ? C11 C12 1.396(6) . ? C11 C14 1.485(6) . ? C12 H12A 0.9300 . ? C17 C18 1.381(8) . ? C17 H17A 0.9300 . ? C18 C19 1.371(8) . ? C18 H18A 0.9300 . ? C19 C20 1.371(8) . ? C19 C27 1.476(7) . ? C20 C21 1.383(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.375(8) . ? C22 H22A 0.9300 . ? C23 C24 1.399(8) . ? C23 H23A 0.9300 . ? C24 C25 1.379(8) . ? C24 C28 1.462(7) . ? C25 C26 1.372(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.322(9) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? O1W Zn2 2.090(3) 7_556 ? O9W O9W 1.74(4) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Zn1 O3 114.51(13) . 4_556 ? O1W Zn1 O1 104.55(14) . . ? O3 Zn1 O1 113.92(16) 4_556 . ? O1W Zn1 N1 117.68(16) . 3_545 ? O3 Zn1 N1 101.41(15) 4_556 3_545 ? O1 Zn1 N1 104.74(16) . 3_545 ? O1W Zn1 Zn2 41.83(9) . . ? O3 Zn1 Zn2 88.95(10) 4_556 . ? O1 Zn1 Zn2 86.87(10) . . ? N1 Zn1 Zn2 159.32(13) 3_545 . ? O5 Zn2 O1W 93.28(13) 5_556 7_556 ? O5 Zn2 N2 88.27(15) 5_556 . ? O1W Zn2 N2 95.35(14) 7_556 . ? O5 Zn2 O1W 89.62(13) 5_556 . ? O1W Zn2 O1W 82.77(12) 7_556 . ? N2 Zn2 O1W 177.09(15) . . ? O5 Zn2 O4 176.00(14) 5_556 4_556 ? O1W Zn2 O4 89.74(13) 7_556 4_556 ? N2 Zn2 O4 88.83(14) . 4_556 ? O1W Zn2 O4 93.37(12) . 4_556 ? O5 Zn2 O2 85.82(13) 5_556 . ? O1W Zn2 O2 173.65(12) 7_556 . ? N2 Zn2 O2 90.91(15) . . ? O1W Zn2 O2 90.93(12) . . ? O4 Zn2 O2 91.46(13) 4_556 . ? O5 Zn2 Zn1 115.59(10) 5_556 . ? O1W Zn2 Zn1 106.56(8) 7_556 . ? N2 Zn2 Zn1 145.84(12) . . ? O1W Zn2 Zn1 37.07(9) . . ? O4 Zn2 Zn1 65.90(8) 4_556 . ? O2 Zn2 Zn1 68.36(8) . . ? C13 O1 Zn1 120.3(3) . . ? C13 O2 Zn2 130.6(3) . . ? C14 O3 Zn1 117.8(3) . 4_546 ? C14 O4 Zn2 140.1(3) . 4_546 ? C15 O5 Zn2 125.7(3) . 5_556 ? C17 N1 C21 117.9(4) . . ? C17 N1 Zn1 121.1(3) . 3_455 ? C21 N1 Zn1 120.9(4) . 3_455 ? C26 N2 C22 116.9(4) . . ? C26 N2 Zn2 121.9(3) . . ? C22 N2 Zn2 119.9(4) . . ? C16 N3 C7 129.7(4) . . ? C16 N3 H3B 115.2 . . ? C7 N3 H3B 115.2 . . ? C6 C1 C2 118.2(5) . . ? C6 C1 C16 119.7(5) . . ? C2 C1 C16 122.1(5) . . ? C1 C2 C3 121.3(5) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 118.5(5) . . ? C5 C4 C15 122.9(4) . . ? C3 C4 C15 118.6(5) . . ? C4 C5 C6 121.1(5) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 120.7(5) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C12 C7 C8 119.7(4) . . ? C12 C7 N3 116.2(4) . . ? C8 C7 N3 124.1(4) . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 C13 119.4(4) . . ? C8 C9 C13 119.6(4) . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 C14 120.8(4) . . ? C12 C11 C14 120.8(4) . . ? C7 C12 C11 121.2(4) . . ? C7 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? O2 C13 O1 124.5(4) . . ? O2 C13 C9 119.8(4) . . ? O1 C13 C9 115.7(4) . . ? O4 C14 O3 124.8(4) . . ? O4 C14 C11 118.7(4) . . ? O3 C14 C11 116.5(4) . . ? O6 C15 O5 125.4(4) . . ? O6 C15 C4 119.8(4) . . ? O5 C15 C4 114.8(4) . . ? O7 C16 N3 122.7(4) . . ? O7 C16 C1 122.4(4) . . ? N3 C16 C1 114.9(4) . . ? N1 C17 C18 122.0(5) . . ? N1 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? C19 C18 C17 120.1(6) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 117.9(5) . . ? C20 C19 C27 118.3(5) . . ? C18 C19 C27 123.8(6) . . ? C19 C20 C21 119.3(5) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? N1 C21 C20 122.7(5) . . ? N1 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? N2 C22 C23 122.8(5) . . ? N2 C22 H22A 118.6 . . ? C23 C22 H22A 118.6 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 116.6(5) . . ? C25 C24 C28 119.9(5) . . ? C23 C24 C28 123.5(5) . . ? C26 C25 C24 119.4(5) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? N2 C26 C25 124.1(5) . . ? N2 C26 H26A 117.9 . . ? C25 C26 H26A 117.9 . . ? C28 C27 C19 126.3(6) . . ? C28 C27 H27A 116.9 . . ? C19 C27 H27A 116.9 . . ? C27 C28 C24 125.3(6) . . ? C27 C28 H28A 117.4 . . ? C24 C28 H28A 117.4 . . ? Zn1 O1W Zn2 127.09(15) . 7_556 ? Zn1 O1W Zn2 101.10(14) . . ? Zn2 O1W Zn2 97.23(12) 7_556 . ? 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 O1W Zn1 Zn2 O5 49.73(17) . . . 5_556 ? O3 Zn1 Zn2 O5 179.71(16) 4_556 . . 5_556 ? O1 Zn1 Zn2 O5 -66.26(16) . . . 5_556 ? N1 Zn1 Zn2 O5 58.9(4) 3_545 . . 5_556 ? O1W Zn1 Zn2 O1W -52.31(19) . . . 7_556 ? O3 Zn1 Zn2 O1W 77.67(14) 4_556 . . 7_556 ? O1 Zn1 Zn2 O1W -168.31(15) . . . 7_556 ? N1 Zn1 Zn2 O1W -43.1(4) 3_545 . . 7_556 ? O1W Zn1 Zn2 N2 -180.0(2) . . . . ? O3 Zn1 Zn2 N2 -50.0(2) 4_556 . . . ? O1 Zn1 Zn2 N2 64.0(2) . . . . ? N1 Zn1 Zn2 N2 -170.8(4) 3_545 . . . ? O3 Zn1 Zn2 O1W 129.98(17) 4_556 . . . ? O1 Zn1 Zn2 O1W -116.00(18) . . . . ? N1 Zn1 Zn2 O1W 9.2(4) 3_545 . . . ? O1W Zn1 Zn2 O4 -134.36(16) . . . 4_556 ? O3 Zn1 Zn2 O4 -4.38(15) 4_556 . . 4_556 ? O1 Zn1 Zn2 O4 109.64(15) . . . 4_556 ? N1 Zn1 Zn2 O4 -125.2(4) 3_545 . . 4_556 ? O1W Zn1 Zn2 O2 123.66(16) . . . . ? O3 Zn1 Zn2 O2 -106.36(15) 4_556 . . . ? O1 Zn1 Zn2 O2 7.66(15) . . . . ? N1 Zn1 Zn2 O2 132.9(4) 3_545 . . . ? O1W Zn1 O1 C13 -33.4(4) . . . . ? O3 Zn1 O1 C13 92.3(4) 4_556 . . . ? N1 Zn1 O1 C13 -157.8(4) 3_545 . . . ? Zn2 Zn1 O1 C13 4.9(4) . . . . ? O5 Zn2 O2 C13 92.7(4) 5_556 . . . ? O1W Zn2 O2 C13 10.6(13) 7_556 . . . ? N2 Zn2 O2 C13 -179.1(4) . . . . ? O1W Zn2 O2 C13 3.1(4) . . . . ? O4 Zn2 O2 C13 -90.3(4) 4_556 . . . ? Zn1 Zn2 O2 C13 -27.0(4) . . . . ? O5 Zn2 N2 C26 -125.8(4) 5_556 . . . ? O1W Zn2 N2 C26 -32.6(4) 7_556 . . . ? O1W Zn2 N2 C26 -82(3) . . . . ? O4 Zn2 N2 C26 57.0(4) 4_556 . . . ? O2 Zn2 N2 C26 148.4(4) . . . . ? Zn1 Zn2 N2 C26 97.7(4) . . . . ? O5 Zn2 N2 C22 41.2(5) 5_556 . . . ? O1W Zn2 N2 C22 134.4(5) 7_556 . . . ? O1W Zn2 N2 C22 85(3) . . . . ? O4 Zn2 N2 C22 -136.0(5) 4_556 . . . ? O2 Zn2 N2 C22 -44.5(5) . . . . ? Zn1 Zn2 N2 C22 -95.3(5) . . . . ? C6 C1 C2 C3 -2.4(11) . . . . ? C16 C1 C2 C3 179.1(6) . . . . ? C1 C2 C3 C4 1.0(12) . . . . ? C2 C3 C4 C5 0.9(10) . . . . ? C2 C3 C4 C15 -179.8(6) . . . . ? C3 C4 C5 C6 -1.4(9) . . . . ? C15 C4 C5 C6 179.3(5) . . . . ? C2 C1 C6 C5 1.8(9) . . . . ? C16 C1 C6 C5 -179.6(6) . . . . ? C4 C5 C6 C1 0.0(10) . . . . ? C16 N3 C7 C12 165.4(6) . . . . ? C16 N3 C7 C8 -15.6(9) . . . . ? C12 C7 C8 C9 0.5(8) . . . . ? N3 C7 C8 C9 -178.4(5) . . . . ? C7 C8 C9 C10 -1.2(8) . . . . ? C7 C8 C9 C13 173.8(5) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C13 C9 C10 C11 -174.2(5) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C9 C10 C11 C14 -178.1(4) . . . . ? C8 C7 C12 C11 0.6(8) . . . . ? N3 C7 C12 C11 179.6(5) . . . . ? C10 C11 C12 C7 -1.0(8) . . . . ? C14 C11 C12 C7 177.4(5) . . . . ? Zn2 O2 C13 O1 43.5(7) . . . . ? Zn2 O2 C13 C9 -136.9(4) . . . . ? Zn1 O1 C13 O2 -26.6(7) . . . . ? Zn1 O1 C13 C9 153.9(3) . . . . ? C10 C9 C13 O2 -170.0(5) . . . . ? C8 C9 C13 O2 14.8(7) . . . . ? C10 C9 C13 O1 9.6(7) . . . . ? C8 C9 C13 O1 -165.6(5) . . . . ? Zn2 O4 C14 O3 -24.0(8) 4_546 . . . ? Zn2 O4 C14 C11 156.2(4) 4_546 . . . ? Zn1 O3 C14 O4 11.8(6) 4_546 . . . ? Zn1 O3 C14 C11 -168.4(3) 4_546 . . . ? C10 C11 C14 O4 5.7(7) . . . . ? C12 C11 C14 O4 -172.6(5) . . . . ? C10 C11 C14 O3 -174.0(5) . . . . ? C12 C11 C14 O3 7.6(7) . . . . ? Zn2 O5 C15 O6 29.0(7) 5_556 . . . ? Zn2 O5 C15 C4 -151.6(3) 5_556 . . . ? C5 C4 C15 O6 2.1(8) . . . . ? C3 C4 C15 O6 -177.2(6) . . . . ? C5 C4 C15 O5 -177.3(5) . . . . ? C3 C4 C15 O5 3.4(7) . . . . ? C7 N3 C16 O7 -1.0(9) . . . . ? C7 N3 C16 C1 179.3(5) . . . . ? C6 C1 C16 O7 -8.8(8) . . . . ? C2 C1 C16 O7 169.7(6) . . . . ? C6 C1 C16 N3 170.9(5) . . . . ? C2 C1 C16 N3 -10.6(8) . . . . ? C21 N1 C17 C18 -2.4(10) . . . . ? Zn1 N1 C17 C18 178.8(5) 3_455 . . . ? N1 C17 C18 C19 0.7(11) . . . . ? C17 C18 C19 C20 0.4(11) . . . . ? C17 C18 C19 C27 -179.0(6) . . . . ? C18 C19 C20 C21 0.2(10) . . . . ? C27 C19 C20 C21 179.7(6) . . . . ? C17 N1 C21 C20 3.0(9) . . . . ? Zn1 N1 C21 C20 -178.2(5) 3_455 . . . ? C19 C20 C21 N1 -2.0(10) . . . . ? C26 N2 C22 C23 3.0(9) . . . . ? Zn2 N2 C22 C23 -164.7(5) . . . . ? N2 C22 C23 C24 -0.1(11) . . . . ? C22 C23 C24 C25 -2.9(10) . . . . ? C22 C23 C24 C28 176.8(6) . . . . ? C23 C24 C25 C26 3.0(9) . . . . ? C28 C24 C25 C26 -176.7(6) . . . . ? C22 N2 C26 C25 -2.9(9) . . . . ? Zn2 N2 C26 C25 164.5(5) . . . . ? C24 C25 C26 N2 -0.1(9) . . . . ? C20 C19 C27 C28 -178.1(7) . . . . ? C18 C19 C27 C28 1.3(11) . . . . ? C19 C27 C28 C24 179.0(6) . . . . ? C25 C24 C28 C27 173.0(7) . . . . ? C23 C24 C28 C27 -6.6(11) . . . . ? O3 Zn1 O1W Zn2 50.7(2) 4_556 . . 7_556 ? O1 Zn1 O1W Zn2 176.01(18) . . . 7_556 ? N1 Zn1 O1W Zn2 -68.3(2) 3_545 . . 7_556 ? Zn2 Zn1 O1W Zn2 108.0(2) . . . 7_556 ? O3 Zn1 O1W Zn2 -57.35(17) 4_556 . . . ? O1 Zn1 O1W Zn2 68.00(16) . . . . ? N1 Zn1 O1W Zn2 -176.34(14) 3_545 . . . ? O5 Zn2 O1W Zn1 -136.51(14) 5_556 . . . ? O1W Zn2 O1W Zn1 130.13(18) 7_556 . . . ? N2 Zn2 O1W Zn1 180(100) . . . . ? O4 Zn2 O1W Zn1 40.82(14) 4_556 . . . ? O2 Zn2 O1W Zn1 -50.70(14) . . . . ? O5 Zn2 O1W Zn2 93.36(14) 5_556 . . 7_556 ? O1W Zn2 O1W Zn2 0.0 7_556 . . 7_556 ? N2 Zn2 O1W Zn2 50(3) . . . 7_556 ? O4 Zn2 O1W Zn2 -89.30(13) 4_556 . . 7_556 ? O2 Zn2 O1W Zn2 179.18(13) . . . 7_556 ? Zn1 Zn2 O1W Zn2 -130.13(18) . . . 7_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.656 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 918289' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H66 Co7 N12 O38' _chemical_formula_weight 2264.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6563(6) _cell_length_b 14.3534(10) _cell_length_c 15.5710(10) _cell_angle_alpha 87.588(2) _cell_angle_beta 74.823(2) _cell_angle_gamma 85.179(2) _cell_volume 2075.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1147 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5508 _exptl_absorpt_correction_T_max 0.7008 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23900 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7267 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+2.5879P] 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 7267 _refine_ls_number_parameters 646 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.058 _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 1.5000 0.5000 0.0000 0.02520(17) Uani 1 2 d S . . Co2 Co 1.59069(5) 0.24776(3) 0.20346(3) 0.02246(14) Uani 1 1 d . . . Co3 Co 0.63237(5) 0.10928(3) 1.05213(3) 0.02308(14) Uani 1 1 d . . . Co4 Co 0.86728(5) 0.25000(3) 0.99317(3) 0.02240(14) Uani 1 1 d . . . N1 N -0.0503(3) 0.1232(2) 1.42878(19) 0.0322(7) Uani 1 1 d . . . H1A H 0.0020 0.1543 1.4525 0.039 Uiso 1 1 calc R . . N2 N 0.9917(3) 0.3866(3) 0.4476(2) 0.0348(8) Uani 1 1 d . A . H2B H 0.9046 0.4102 0.4662 0.042 Uiso 1 1 calc R . . N3 N 1.0929(3) 0.2285(2) 0.9211(2) 0.0310(7) Uani 1 1 d . . . N4 N 1.5388(3) 0.2257(2) 0.3451(2) 0.0293(7) Uani 1 1 d . . . N5 N 1.3672(5) 0.1898(3) 0.6205(2) 0.0532(10) Uani 1 1 d . . . N6 N 1.3932(4) 0.2437(3) 0.6726(2) 0.0492(10) Uani 1 1 d . . . O1 O 0.4049(3) 0.11770(19) 1.08641(17) 0.0306(6) Uani 1 1 d . . . O2 O 0.4013(3) 0.18565(19) 1.21173(16) 0.0289(6) Uani 1 1 d . . . O3 O -0.1248(3) 0.10599(18) 1.05443(15) 0.0271(5) Uani 1 1 d . . . O4 O -0.2959(2) 0.10277(18) 1.17921(16) 0.0258(5) Uani 1 1 d . . . O5 O -0.3577(3) 0.10488(19) 1.91845(16) 0.0316(6) Uani 1 1 d . . . O6 O -0.1665(3) 0.18825(19) 1.88401(16) 0.0322(6) Uani 1 1 d . . . O7 O -0.2458(4) 0.0416(3) 1.45927(19) 0.0608(10) Uani 1 1 d . . . O8 O 0.6189(3) 0.4121(2) 0.89939(17) 0.0375(6) Uani 1 1 d . . . O9 O 0.8272(3) 0.38210(18) 0.93543(16) 0.0301(6) Uani 1 1 d . . . O10 O 0.7592(3) 0.3139(2) 0.21468(16) 0.0332(6) Uani 1 1 d . . . O11 O 0.9290(3) 0.31608(19) 0.08601(16) 0.0309(6) Uani 1 1 d . . . O12 O 1.4087(3) 0.39073(19) 0.08241(16) 0.0311(6) Uani 1 1 d . . . O13 O 1.4786(3) 0.38462(18) 0.20830(16) 0.0278(5) Uani 1 1 d . . . O14 O 1.1959(6) 0.3594(7) 0.4920(4) 0.054(2) Uani 0.50 1 d PU A 1 O14' O 1.1562(10) 0.2963(8) 0.4870(6) 0.081(2) Uani 0.50 1 d PU A 2 C1 C 0.1846(4) 0.1311(2) 1.2016(2) 0.0219(7) Uani 1 1 d . . . C2 C 0.1333(4) 0.1337(2) 1.2931(2) 0.0241(7) Uani 1 1 d . . . H2A H 0.1954 0.1456 1.3273 0.029 Uiso 1 1 calc R . . C3 C -0.0081(4) 0.1189(2) 1.3348(2) 0.0244(7) Uani 1 1 d . . . C4 C -0.1037(4) 0.1057(3) 1.2840(2) 0.0248(7) Uani 1 1 d . . . H4A H -0.1996 0.0969 1.3115 0.030 Uiso 1 1 calc R . . C5 C -0.0538(4) 0.1056(2) 1.1914(2) 0.0218(7) Uani 1 1 d . . . C6 C 0.0903(4) 0.1162(2) 1.1495(2) 0.0222(7) Uani 1 1 d . . . H6A H 0.1236 0.1133 1.0879 0.027 Uiso 1 1 calc R . . C7 C -0.2299(4) 0.1220(3) 1.7663(2) 0.0263(7) Uani 1 1 d . . . C8 C -0.3366(4) 0.0928(3) 1.7309(2) 0.0322(8) Uani 1 1 d . . . H8A H -0.4257 0.0809 1.7685 0.039 Uiso 1 1 calc R . . C9 C -0.3116(4) 0.0813(3) 1.6409(3) 0.0339(9) Uani 1 1 d . . . H9A H -0.3848 0.0625 1.6184 0.041 Uiso 1 1 calc R . . C10 C -0.1784(4) 0.0973(3) 1.5823(2) 0.0281(8) Uani 1 1 d . . . C11 C -0.0704(4) 0.1231(3) 1.6186(2) 0.0330(9) Uani 1 1 d . . . H11A H 0.0204 0.1318 1.5815 0.040 Uiso 1 1 calc R . . C12 C -0.0960(4) 0.1359(3) 1.7087(2) 0.0327(9) Uani 1 1 d . . . H12A H -0.0227 0.1542 1.7314 0.039 Uiso 1 1 calc R . . C13 C 0.3414(3) 0.1462(2) 1.1628(2) 0.0220(7) Uani 1 1 d . . . C14 C -0.1627(4) 0.1034(2) 1.1380(2) 0.0219(7) Uani 1 1 d . . . C15 C -0.2536(4) 0.1394(2) 1.8636(2) 0.0248(7) Uani 1 1 d . . . C16 C -0.1616(4) 0.0847(3) 1.4857(2) 0.0322(8) Uani 1 1 d . . . C17 C 0.9719(4) 0.3686(3) 0.6043(3) 0.0378(9) Uani 1 1 d . A . C18 C 0.8242(4) 0.3622(3) 0.6312(3) 0.0397(10) Uani 1 1 d . . . H18A H 0.7736 0.3535 0.5892 0.048 Uiso 1 1 calc R . . C19 C 0.7521(4) 0.3686(3) 0.7204(3) 0.0357(9) Uani 1 1 d . . . H19A H 0.6531 0.3642 0.7382 0.043 Uiso 1 1 calc R . . C20 C 0.8275(4) 0.3816(3) 0.7835(2) 0.0293(8) Uani 1 1 d . . . C21 C 0.9742(4) 0.3881(3) 0.7554(3) 0.0374(9) Uani 1 1 d . . . H21A H 1.0249 0.3980 0.7970 0.045 Uiso 1 1 calc R . . C22 C 1.0465(4) 0.3804(4) 0.6677(3) 0.0442(11) Uani 1 1 d . . . H22A H 1.1459 0.3830 0.6504 0.053 Uiso 1 1 calc R . . C23 C 0.9874(4) 0.3563(2) 0.2156(2) 0.0239(7) Uani 1 1 d . . . C24 C 0.9460(4) 0.3636(3) 0.3072(2) 0.0277(8) Uani 1 1 d . . . H24A H 0.8503 0.3579 0.3376 0.033 Uiso 1 1 calc R . . C25 C 1.0444(4) 0.3793(3) 0.3545(2) 0.0270(8) Uani 1 1 d . . . C26 C 1.1887(4) 0.3869(3) 0.3090(2) 0.0261(8) Uani 1 1 d . . . H26A H 1.2567 0.3953 0.3401 0.031 Uiso 1 1 calc R . . C27 C 1.2289(4) 0.3818(2) 0.2173(2) 0.0232(7) Uani 1 1 d . . . C28 C 1.1292(4) 0.3668(2) 0.1700(2) 0.0236(7) Uani 1 1 d . . . H28A H 1.1575 0.3639 0.1083 0.028 Uiso 1 1 calc R . . C29 C 0.7515(4) 0.3916(3) 0.8796(2) 0.0282(8) Uani 1 1 d . . . C30 C 0.8832(4) 0.3276(2) 0.1676(2) 0.0233(7) Uani 1 1 d . . . C31 C 1.3827(4) 0.3874(2) 0.1657(2) 0.0231(7) Uani 1 1 d . . . C32 C 1.0576(5) 0.3623(4) 0.5094(3) 0.0511(12) Uani 1 1 d . . . C33 C 1.1291(5) 0.1531(3) 0.8699(3) 0.0398(9) Uani 1 1 d . . . H33A H 1.0812 0.0996 0.8898 0.048 Uiso 1 1 calc R . . C34 C 1.2325(4) 0.1491(3) 0.7896(3) 0.0384(9) Uani 1 1 d . . . H34A H 1.2535 0.0953 0.7560 0.046 Uiso 1 1 calc R . . C35 C 1.3040(4) 0.2300(3) 0.7615(3) 0.0413(10) Uani 1 1 d . . . C36 C 1.2840(5) 0.3043(4) 0.8190(3) 0.0467(11) Uani 1 1 d . . . H36A H 1.3408 0.3549 0.8053 0.056 Uiso 1 1 calc R . . C37 C 1.1761(4) 0.3001(3) 0.8975(3) 0.0426(10) Uani 1 1 d . . . H37A H 1.1606 0.3499 0.9360 0.051 Uiso 1 1 calc R . . C38 C 1.4384(5) 0.2039(3) 0.5284(3) 0.0428(10) Uani 1 1 d . . . C39 C 1.4253(5) 0.1342(4) 0.4731(3) 0.0487(11) Uani 1 1 d . . . H39A H 1.3826 0.0796 0.4960 0.058 Uiso 1 1 calc R . . C40 C 1.4783(5) 0.1488(3) 0.3822(3) 0.0395(9) Uani 1 1 d . . . H40A H 1.4711 0.1017 0.3447 0.047 Uiso 1 1 calc R . . C41 C 1.5543(5) 0.2899(3) 0.4011(3) 0.0430(10) Uani 1 1 d . . . H41A H 1.5991 0.3434 0.3769 0.052 Uiso 1 1 calc R . . C42 C 1.5078(5) 0.2817(4) 0.4928(3) 0.0463(11) Uani 1 1 d . . . H42A H 1.5231 0.3275 0.5291 0.056 Uiso 1 1 calc R . . O1W O 0.6512(2) 0.24619(17) 1.06498(15) 0.0224(5) Uani 1 1 d . . . O2W O 0.6256(3) -0.03445(18) 1.05803(18) 0.0338(6) Uani 1 1 d . . . O3W O 1.6655(3) 0.49111(19) 0.06896(17) 0.0333(6) Uani 1 1 d . . . O4W O 1.5390(8) 0.5112(4) 0.3388(4) 0.118(2) Uani 1 1 d . . . O5W O 0.6884(5) 0.4855(4) 0.4795(3) 0.0884(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0180(3) 0.0374(4) 0.0180(3) 0.0012(3) -0.0003(3) -0.0047(3) Co2 0.0143(2) 0.0353(3) 0.0178(2) -0.00051(19) -0.00197(18) -0.00889(19) Co3 0.0180(3) 0.0335(3) 0.0182(2) -0.00108(19) -0.00311(18) -0.00897(19) Co4 0.0170(2) 0.0340(3) 0.0163(2) -0.00004(19) -0.00260(18) -0.00826(19) N1 0.0235(16) 0.057(2) 0.0171(15) -0.0025(14) -0.0032(12) -0.0162(15) N2 0.0185(16) 0.065(2) 0.0195(16) -0.0045(15) -0.0015(13) -0.0038(15) N3 0.0217(16) 0.0468(19) 0.0230(16) -0.0002(14) -0.0020(13) -0.0069(14) N4 0.0219(16) 0.0443(19) 0.0217(15) 0.0002(13) -0.0039(12) -0.0088(13) N5 0.056(3) 0.067(3) 0.029(2) -0.0030(18) 0.0041(18) -0.013(2) N6 0.037(2) 0.074(3) 0.030(2) 0.0004(19) 0.0022(16) -0.0057(19) O1 0.0182(12) 0.0465(16) 0.0261(14) -0.0102(11) -0.0003(10) -0.0101(11) O2 0.0186(12) 0.0461(15) 0.0224(13) -0.0028(11) -0.0028(10) -0.0113(11) O3 0.0238(13) 0.0406(14) 0.0173(12) -0.0011(10) -0.0051(10) -0.0045(11) O4 0.0136(12) 0.0385(14) 0.0254(13) 0.0034(10) -0.0041(10) -0.0077(10) O5 0.0310(14) 0.0462(16) 0.0179(12) 0.0001(11) -0.0022(11) -0.0178(12) O6 0.0298(14) 0.0485(16) 0.0191(12) -0.0059(11) -0.0030(11) -0.0157(12) O7 0.065(2) 0.098(3) 0.0255(15) 0.0019(16) -0.0076(15) -0.056(2) O8 0.0254(15) 0.0555(18) 0.0284(14) -0.0091(13) -0.0015(11) 0.0012(12) O9 0.0326(14) 0.0368(14) 0.0196(12) 0.0008(10) -0.0044(11) -0.0031(11) O10 0.0182(13) 0.0579(17) 0.0244(13) -0.0047(12) -0.0025(10) -0.0154(12) O11 0.0240(13) 0.0512(16) 0.0187(13) -0.0038(11) -0.0041(10) -0.0133(11) O12 0.0247(13) 0.0478(16) 0.0196(13) 0.0024(11) -0.0012(10) -0.0130(11) O13 0.0174(12) 0.0388(14) 0.0283(13) -0.0003(11) -0.0066(10) -0.0064(10) O14 0.015(3) 0.125(7) 0.021(2) -0.004(4) -0.005(2) 0.000(3) O14' 0.047(4) 0.142(7) 0.039(3) 0.008(4) 0.006(3) 0.027(4) C1 0.0152(16) 0.0271(18) 0.0234(17) 0.0007(13) -0.0039(14) -0.0051(13) C2 0.0172(17) 0.0332(19) 0.0230(18) 0.0004(14) -0.0064(14) -0.0052(14) C3 0.0214(18) 0.0325(19) 0.0192(17) 0.0005(14) -0.0034(14) -0.0064(14) C4 0.0162(17) 0.036(2) 0.0205(17) 0.0017(14) -0.0012(14) -0.0054(14) C5 0.0177(17) 0.0262(17) 0.0224(17) 0.0008(13) -0.0061(14) -0.0055(13) C6 0.0180(17) 0.0288(18) 0.0194(17) 0.0010(13) -0.0035(13) -0.0047(13) C7 0.0251(19) 0.0329(19) 0.0201(17) 0.0011(14) -0.0033(14) -0.0064(15) C8 0.0204(18) 0.053(2) 0.0211(18) -0.0003(16) -0.0005(15) -0.0094(17) C9 0.026(2) 0.049(2) 0.028(2) -0.0001(17) -0.0082(16) -0.0132(17) C10 0.0263(19) 0.038(2) 0.0185(17) -0.0006(15) -0.0026(14) -0.0067(15) C11 0.0210(19) 0.053(2) 0.0238(19) -0.0018(17) -0.0009(15) -0.0113(17) C12 0.0228(19) 0.052(2) 0.0246(19) -0.0040(17) -0.0044(15) -0.0126(17) C13 0.0159(16) 0.0317(18) 0.0187(17) 0.0004(14) -0.0039(14) -0.0061(14) C14 0.0209(18) 0.0255(17) 0.0204(17) 0.0003(13) -0.0066(14) -0.0045(13) C15 0.0214(18) 0.0310(18) 0.0220(18) 0.0001(14) -0.0051(14) -0.0032(14) C16 0.030(2) 0.043(2) 0.0245(19) -0.0010(16) -0.0061(16) -0.0108(17) C17 0.028(2) 0.059(3) 0.0213(19) 0.0040(17) 0.0004(16) 0.0051(18) C18 0.032(2) 0.061(3) 0.027(2) -0.0004(18) -0.0079(17) -0.0058(19) C19 0.026(2) 0.054(3) 0.0246(19) 0.0019(17) -0.0032(16) -0.0043(18) C20 0.029(2) 0.035(2) 0.0209(18) 0.0015(15) -0.0022(15) 0.0004(15) C21 0.028(2) 0.056(3) 0.027(2) 0.0037(18) -0.0055(17) -0.0065(18) C22 0.022(2) 0.081(3) 0.027(2) 0.006(2) -0.0031(16) -0.002(2) C23 0.0164(17) 0.0355(19) 0.0211(17) -0.0026(14) -0.0061(14) -0.0044(14) C24 0.0149(17) 0.043(2) 0.0236(18) -0.0018(15) 0.0002(14) -0.0078(15) C25 0.0202(18) 0.043(2) 0.0172(17) -0.0012(15) -0.0019(14) -0.0064(15) C26 0.0179(17) 0.039(2) 0.0222(18) 0.0003(15) -0.0053(14) -0.0087(15) C27 0.0170(17) 0.0290(18) 0.0234(17) 0.0000(14) -0.0040(14) -0.0049(14) C28 0.0201(17) 0.0324(19) 0.0177(17) -0.0007(14) -0.0029(14) -0.0052(14) C29 0.028(2) 0.0278(18) 0.0264(19) 0.0014(15) -0.0031(16) -0.0021(15) C30 0.0184(17) 0.0289(18) 0.0241(18) -0.0008(14) -0.0074(14) -0.0047(14) C31 0.0180(17) 0.0278(18) 0.0230(18) 0.0004(14) -0.0032(14) -0.0055(13) C32 0.033(2) 0.090(4) 0.023(2) 0.001(2) -0.0016(18) 0.014(2) C33 0.035(2) 0.046(2) 0.036(2) 0.0048(18) -0.0073(18) -0.0030(18) C34 0.033(2) 0.053(3) 0.027(2) -0.0023(18) -0.0028(17) 0.0005(18) C35 0.027(2) 0.065(3) 0.030(2) 0.004(2) -0.0030(17) -0.0063(19) C36 0.034(2) 0.065(3) 0.038(2) -0.001(2) 0.0013(19) -0.017(2) C37 0.031(2) 0.061(3) 0.034(2) -0.008(2) -0.0008(18) -0.013(2) C38 0.031(2) 0.065(3) 0.028(2) 0.0042(19) -0.0009(17) -0.006(2) C39 0.048(3) 0.062(3) 0.033(2) 0.008(2) -0.002(2) -0.016(2) C40 0.038(2) 0.049(2) 0.031(2) 0.0004(18) -0.0062(18) -0.0108(19) C41 0.039(2) 0.059(3) 0.030(2) -0.0001(19) -0.0024(18) -0.016(2) C42 0.044(3) 0.062(3) 0.032(2) -0.008(2) -0.0048(19) -0.012(2) O1W 0.0170(12) 0.0327(13) 0.0175(11) 0.0001(10) -0.0022(9) -0.0084(10) O2W 0.0349(15) 0.0355(14) 0.0355(15) 0.0005(11) -0.0153(12) -0.0094(12) O3W 0.0249(14) 0.0438(15) 0.0316(14) -0.0026(12) -0.0062(11) -0.0067(12) O4W 0.165(6) 0.094(4) 0.119(5) 0.011(3) -0.077(4) -0.018(4) O5W 0.064(3) 0.117(4) 0.078(3) 0.005(3) -0.014(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O8 2.085(3) 2_766 ? Co1 O8 2.085(3) 1_654 ? Co1 O12 2.087(2) 2_865 ? Co1 O12 2.087(2) . ? Co1 O3W 2.139(2) 2_865 ? Co1 O3W 2.139(3) . ? Co2 O10 2.001(2) 1_655 ? Co2 O2 2.073(2) 1_654 ? Co2 O1W 2.082(2) 1_654 ? Co2 N4 2.146(3) . ? Co2 O13 2.156(3) . ? Co2 O4 2.267(3) 1_754 ? Co3 O1W 2.012(2) . ? Co3 O5 2.062(2) 1_654 ? Co3 O2W 2.067(3) . ? Co3 O1 2.115(2) . ? Co3 O4 2.257(2) 1_655 ? Co3 O3 2.351(2) 1_655 ? Co4 O11 2.002(2) 1_556 ? Co4 O6 2.061(2) 1_654 ? Co4 O1W 2.097(2) . ? Co4 O9 2.114(3) . ? Co4 N3 2.176(3) . ? Co4 O3 2.244(3) 1_655 ? N1 C16 1.344(5) . ? N1 C3 1.415(4) . ? N1 H1A 0.8600 . ? N2 C32 1.307(5) . ? N2 C25 1.411(5) . ? N2 H2B 0.8600 . ? N3 C37 1.337(5) . ? N3 C33 1.339(6) . ? N4 C40 1.332(5) . ? N4 C41 1.338(5) . ? N5 N6 1.229(5) . ? N5 C38 1.433(5) . ? N6 C35 1.442(5) . ? O1 C13 1.254(4) . ? O2 C13 1.248(4) . ? O2 Co2 2.073(2) 1_456 ? O3 C14 1.257(4) . ? O3 Co4 2.244(3) 1_455 ? O3 Co3 2.351(2) 1_455 ? O4 C14 1.279(4) . ? O4 Co3 2.257(2) 1_455 ? O4 Co2 2.267(3) 1_356 ? O5 C15 1.259(4) . ? O5 Co3 2.062(2) 1_456 ? O6 C15 1.248(4) . ? O6 Co4 2.061(2) 1_456 ? O7 C16 1.222(5) . ? O8 C29 1.248(5) . ? O8 Co1 2.085(3) 1_456 ? O9 C29 1.271(4) . ? O10 C30 1.256(4) . ? O10 Co2 2.001(2) 1_455 ? O11 C30 1.245(4) . ? O11 Co4 2.002(2) 1_554 ? O12 C31 1.255(4) . ? O13 C31 1.269(4) . ? O14 C32 1.289(8) . ? O14' C32 1.277(10) . ? C1 C2 1.381(5) . ? C1 C6 1.404(4) . ? C1 C13 1.507(5) . ? C2 C3 1.380(5) . ? C2 H2A 0.9300 . ? C3 C4 1.392(5) . ? C4 C5 1.395(5) . ? C4 H4A 0.9300 . ? C5 C6 1.392(5) . ? C5 C14 1.504(4) . ? C6 H6A 0.9300 . ? C7 C8 1.389(5) . ? C7 C12 1.392(5) . ? C7 C15 1.501(5) . ? C8 C9 1.374(5) . ? C8 H8A 0.9300 . ? C9 C10 1.398(5) . ? C9 H9A 0.9300 . ? C10 C11 1.393(5) . ? C10 C16 1.487(5) . ? C11 C12 1.376(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C17 C18 1.388(6) . ? C17 C22 1.388(6) . ? C17 C32 1.495(6) . ? C18 C19 1.384(6) . ? C18 H18A 0.9300 . ? C19 C20 1.394(5) . ? C19 H19A 0.9300 . ? C20 C21 1.379(6) . ? C20 C29 1.491(5) . ? C21 C22 1.366(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.383(5) . ? C23 C28 1.385(5) . ? C23 C30 1.493(4) . ? C24 C25 1.382(5) . ? C24 H24A 0.9300 . ? C25 C26 1.399(5) . ? C26 C27 1.381(5) . ? C26 H26A 0.9300 . ? C27 C28 1.390(5) . ? C27 C31 1.499(5) . ? C28 H28A 0.9300 . ? C33 C34 1.380(6) . ? C33 H33A 0.9300 . ? C34 C35 1.397(6) . ? C34 H34A 0.9300 . ? C35 C36 1.389(7) . ? C36 C37 1.387(6) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 C42 1.372(7) . ? C38 C39 1.382(7) . ? C39 C40 1.386(6) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C42 1.382(6) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? O1W Co2 2.082(2) 1_456 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Co1 O8 180.00(13) 2_766 1_654 ? O8 Co1 O12 94.19(11) 2_766 2_865 ? O8 Co1 O12 85.81(11) 1_654 2_865 ? O8 Co1 O12 85.81(11) 2_766 . ? O8 Co1 O12 94.19(11) 1_654 . ? O12 Co1 O12 179.999(1) 2_865 . ? O8 Co1 O3W 93.19(10) 2_766 2_865 ? O8 Co1 O3W 86.81(10) 1_654 2_865 ? O12 Co1 O3W 87.69(10) 2_865 2_865 ? O12 Co1 O3W 92.31(10) . 2_865 ? O8 Co1 O3W 86.80(10) 2_766 . ? O8 Co1 O3W 93.20(10) 1_654 . ? O12 Co1 O3W 92.31(10) 2_865 . ? O12 Co1 O3W 87.69(10) . . ? O3W Co1 O3W 179.998(1) 2_865 . ? O10 Co2 O2 171.18(10) 1_655 1_654 ? O10 Co2 O1W 95.25(9) 1_655 1_654 ? O2 Co2 O1W 93.11(9) 1_654 1_654 ? O10 Co2 N4 87.47(11) 1_655 . ? O2 Co2 N4 84.70(10) 1_654 . ? O1W Co2 N4 170.75(11) 1_654 . ? O10 Co2 O13 86.05(11) 1_655 . ? O2 Co2 O13 90.60(10) 1_654 . ? O1W Co2 O13 93.79(9) 1_654 . ? N4 Co2 O13 95.21(11) . . ? O10 Co2 O4 97.56(10) 1_655 1_754 ? O2 Co2 O4 86.79(9) 1_654 1_754 ? O1W Co2 O4 78.87(9) 1_654 1_754 ? N4 Co2 O4 92.02(11) . 1_754 ? O13 Co2 O4 172.06(9) . 1_754 ? O1W Co3 O5 100.77(10) . 1_654 ? O1W Co3 O2W 170.30(10) . . ? O5 Co3 O2W 88.18(10) 1_654 . ? O1W Co3 O1 96.23(10) . . ? O5 Co3 O1 91.55(10) 1_654 . ? O2W Co3 O1 87.16(11) . . ? O1W Co3 O4 80.56(9) . 1_655 ? O5 Co3 O4 160.09(10) 1_654 1_655 ? O2W Co3 O4 89.75(10) . 1_655 ? O1 Co3 O4 108.13(9) . 1_655 ? O1W Co3 O3 79.58(9) . 1_655 ? O5 Co3 O3 103.51(9) 1_654 1_655 ? O2W Co3 O3 94.80(10) . 1_655 ? O1 Co3 O3 164.85(9) . 1_655 ? O4 Co3 O3 56.94(8) 1_655 1_655 ? O11 Co4 O6 170.91(10) 1_556 1_654 ? O11 Co4 O1W 95.77(9) 1_556 . ? O6 Co4 O1W 92.92(9) 1_654 . ? O11 Co4 O9 88.31(10) 1_556 . ? O6 Co4 O9 88.72(10) 1_654 . ? O1W Co4 O9 92.12(10) . . ? O11 Co4 N3 88.34(11) 1_556 . ? O6 Co4 N3 83.48(11) 1_654 . ? O1W Co4 N3 170.37(11) . . ? O9 Co4 N3 96.72(11) . . ? O11 Co4 O3 96.95(10) 1_556 1_655 ? O6 Co4 O3 87.11(10) 1_654 1_655 ? O1W Co4 O3 80.41(9) . 1_655 ? O9 Co4 O3 171.23(10) . 1_655 ? N3 Co4 O3 90.47(11) . 1_655 ? C16 N1 C3 128.2(3) . . ? C16 N1 H1A 115.9 . . ? C3 N1 H1A 115.9 . . ? C32 N2 C25 128.7(3) . . ? C32 N2 H2B 115.6 . . ? C25 N2 H2B 115.6 . . ? C37 N3 C33 116.6(4) . . ? C37 N3 Co4 121.5(3) . . ? C33 N3 Co4 116.2(3) . . ? C40 N4 C41 116.3(3) . . ? C40 N4 Co2 120.6(3) . . ? C41 N4 Co2 122.9(3) . . ? N6 N5 C38 116.0(4) . . ? N5 N6 C35 111.2(4) . . ? C13 O1 Co3 116.8(2) . . ? C13 O2 Co2 139.4(2) . 1_456 ? C14 O3 Co4 114.6(2) . 1_455 ? C14 O3 Co3 89.54(19) . 1_455 ? Co4 O3 Co3 84.72(8) 1_455 1_455 ? C14 O4 Co3 93.28(19) . 1_455 ? C14 O4 Co2 113.4(2) . 1_356 ? Co3 O4 Co2 85.48(8) 1_455 1_356 ? C15 O5 Co3 118.3(2) . 1_456 ? C15 O6 Co4 140.4(2) . 1_456 ? C29 O8 Co1 127.4(2) . 1_456 ? C29 O9 Co4 121.1(2) . . ? C30 O10 Co2 137.3(2) . 1_455 ? C30 O11 Co4 136.1(2) . 1_554 ? C31 O12 Co1 125.7(2) . . ? C31 O13 Co2 111.2(2) . . ? C2 C1 C6 119.5(3) . . ? C2 C1 C13 117.3(3) . . ? C6 C1 C13 123.2(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 N1 117.1(3) . . ? C4 C3 N1 123.1(3) . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 121.0(3) . . ? C6 C5 C14 120.7(3) . . ? C4 C5 C14 118.0(3) . . ? C5 C6 C1 119.0(3) . . ? C5 C6 H6A 120.5 . . ? C1 C6 H6A 120.5 . . ? C8 C7 C12 118.4(3) . . ? C8 C7 C15 122.7(3) . . ? C12 C7 C15 118.9(3) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 117.6(3) . . ? C11 C10 C16 124.6(3) . . ? C9 C10 C16 117.8(3) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C7 121.0(3) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? O2 C13 O1 123.9(3) . . ? O2 C13 C1 115.9(3) . . ? O1 C13 C1 120.1(3) . . ? O3 C14 O4 120.2(3) . . ? O3 C14 C5 120.9(3) . . ? O4 C14 C5 118.8(3) . . ? O6 C15 O5 124.7(3) . . ? O6 C15 C7 116.3(3) . . ? O5 C15 C7 119.0(3) . . ? O7 C16 N1 121.5(3) . . ? O7 C16 C10 121.4(3) . . ? N1 C16 C10 117.1(3) . . ? C18 C17 C22 119.5(4) . . ? C18 C17 C32 123.2(4) . . ? C22 C17 C32 117.3(4) . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 118.9(3) . . ? C21 C20 C29 119.9(3) . . ? C19 C20 C29 121.1(3) . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C17 120.1(4) . . ? C21 C22 H22A 119.9 . . ? C17 C22 H22A 119.9 . . ? C24 C23 C28 119.6(3) . . ? C24 C23 C30 119.8(3) . . ? C28 C23 C30 120.3(3) . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 N2 117.0(3) . . ? C26 C25 N2 123.5(3) . . ? C27 C26 C25 119.2(3) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 C31 121.2(3) . . ? C28 C27 C31 117.7(3) . . ? C23 C28 C27 119.5(3) . . ? C23 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? O8 C29 O9 124.5(3) . . ? O8 C29 C20 117.9(3) . . ? O9 C29 C20 117.6(3) . . ? O11 C30 O10 126.5(3) . . ? O11 C30 C23 117.1(3) . . ? O10 C30 C23 116.3(3) . . ? O12 C31 O13 124.1(3) . . ? O12 C31 C27 117.3(3) . . ? O13 C31 C27 118.5(3) . . ? O14' C32 O14 47.2(5) . . ? O14' C32 N2 113.6(6) . . ? O14 C32 N2 120.5(5) . . ? O14' C32 C17 119.2(5) . . ? O14 C32 C17 118.6(4) . . ? N2 C32 C17 117.9(4) . . ? N3 C33 C34 124.7(4) . . ? N3 C33 H33A 117.7 . . ? C34 C33 H33A 117.7 . . ? C33 C34 C35 116.6(4) . . ? C33 C34 H34A 121.7 . . ? C35 C34 H34A 121.7 . . ? C36 C35 C34 119.8(4) . . ? C36 C35 N6 116.9(4) . . ? C34 C35 N6 123.2(4) . . ? C37 C36 C35 117.3(4) . . ? C37 C36 H36A 121.3 . . ? C35 C36 H36A 121.3 . . ? N3 C37 C36 123.8(4) . . ? N3 C37 H37A 118.1 . . ? C36 C37 H37A 118.1 . . ? C42 C38 C39 119.7(4) . . ? C42 C38 N5 125.3(4) . . ? C39 C38 N5 114.9(4) . . ? C38 C39 C40 117.5(4) . . ? C38 C39 H39A 121.2 . . ? C40 C39 H39A 121.2 . . ? N4 C40 C39 124.3(4) . . ? N4 C40 H40A 117.9 . . ? C39 C40 H40A 117.9 . . ? N4 C41 C42 124.1(4) . . ? N4 C41 H41A 118.0 . . ? C42 C41 H41A 118.0 . . ? C38 C42 C41 117.9(4) . . ? C38 C42 H42A 121.0 . . ? C41 C42 H42A 121.0 . . ? Co3 O1W Co2 97.18(10) . 1_456 ? Co3 O1W Co4 97.81(10) . . ? Co2 O1W Co4 121.42(10) 1_456 . ? 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 O11 Co4 N3 C37 -55.4(3) 1_556 . . . ? O6 Co4 N3 C37 120.6(3) 1_654 . . . ? O1W Co4 N3 C37 -171.0(5) . . . . ? O9 Co4 N3 C37 32.7(3) . . . . ? O3 Co4 N3 C37 -152.4(3) 1_655 . . . ? O11 Co4 N3 C33 152.0(3) 1_556 . . . ? O6 Co4 N3 C33 -32.0(3) 1_654 . . . ? O1W Co4 N3 C33 36.5(8) . . . . ? O9 Co4 N3 C33 -119.9(3) . . . . ? O3 Co4 N3 C33 55.0(3) 1_655 . . . ? O10 Co2 N4 C40 -147.0(3) 1_655 . . . ? O2 Co2 N4 C40 37.1(3) 1_654 . . . ? O1W Co2 N4 C40 -39.6(8) 1_654 . . . ? O13 Co2 N4 C40 127.2(3) . . . . ? O4 Co2 N4 C40 -49.5(3) 1_754 . . . ? O10 Co2 N4 C41 38.2(3) 1_655 . . . ? O2 Co2 N4 C41 -137.7(3) 1_654 . . . ? O1W Co2 N4 C41 145.6(6) 1_654 . . . ? O13 Co2 N4 C41 -47.6(3) . . . . ? O4 Co2 N4 C41 135.7(3) 1_754 . . . ? C38 N5 N6 C35 173.5(4) . . . . ? O1W Co3 O1 C13 -61.0(3) . . . . ? O5 Co3 O1 C13 -162.1(3) 1_654 . . . ? O2W Co3 O1 C13 109.8(3) . . . . ? O4 Co3 O1 C13 21.0(3) 1_655 . . . ? O3 Co3 O1 C13 11.9(5) 1_655 . . . ? O11 Co4 O9 C29 -164.0(3) 1_556 . . . ? O6 Co4 O9 C29 24.6(3) 1_654 . . . ? O1W Co4 O9 C29 -68.3(3) . . . . ? N3 Co4 O9 C29 107.9(3) . . . . ? O3 Co4 O9 C29 -36.9(7) 1_655 . . . ? O8 Co1 O12 C31 -36.7(3) 2_766 . . . ? O8 Co1 O12 C31 143.3(3) 1_654 . . . ? O12 Co1 O12 C31 86(18) 2_865 . . . ? O3W Co1 O12 C31 -129.7(3) 2_865 . . . ? O3W Co1 O12 C31 50.3(3) . . . . ? O10 Co2 O13 C31 151.1(2) 1_655 . . . ? O2 Co2 O13 C31 -37.1(2) 1_654 . . . ? O1W Co2 O13 C31 56.1(2) 1_654 . . . ? N4 Co2 O13 C31 -121.8(2) . . . . ? O4 Co2 O13 C31 33.7(7) 1_754 . . . ? C6 C1 C2 C3 2.0(5) . . . . ? C13 C1 C2 C3 -178.8(3) . . . . ? C1 C2 C3 C4 -3.2(5) . . . . ? C1 C2 C3 N1 -179.9(3) . . . . ? C16 N1 C3 C2 -157.5(4) . . . . ? C16 N1 C3 C4 25.9(6) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? N1 C3 C4 C5 177.8(3) . . . . ? C3 C4 C5 C6 1.7(5) . . . . ? C3 C4 C5 C14 -172.3(3) . . . . ? C4 C5 C6 C1 -2.8(5) . . . . ? C14 C5 C6 C1 171.1(3) . . . . ? C2 C1 C6 C5 0.9(5) . . . . ? C13 C1 C6 C5 -178.2(3) . . . . ? C12 C7 C8 C9 -2.3(6) . . . . ? C15 C7 C8 C9 177.4(4) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C8 C9 C10 C11 1.6(6) . . . . ? C8 C9 C10 C16 -179.0(4) . . . . ? C9 C10 C11 C12 -2.5(6) . . . . ? C16 C10 C11 C12 178.0(4) . . . . ? C10 C11 C12 C7 1.1(6) . . . . ? C8 C7 C12 C11 1.4(6) . . . . ? C15 C7 C12 C11 -178.4(4) . . . . ? Co2 O2 C13 O1 14.1(6) 1_456 . . . ? Co2 O2 C13 C1 -167.7(3) 1_456 . . . ? Co3 O1 C13 O2 14.1(5) . . . . ? Co3 O1 C13 C1 -164.1(2) . . . . ? C2 C1 C13 O2 -19.9(5) . . . . ? C6 C1 C13 O2 159.2(3) . . . . ? C2 C1 C13 O1 158.4(3) . . . . ? C6 C1 C13 O1 -22.5(5) . . . . ? Co4 O3 C14 O4 84.6(3) 1_455 . . . ? Co3 O3 C14 O4 0.6(3) 1_455 . . . ? Co4 O3 C14 C5 -92.4(3) 1_455 . . . ? Co3 O3 C14 C5 -176.4(3) 1_455 . . . ? Co3 O4 C14 O3 -0.7(3) 1_455 . . . ? Co2 O4 C14 O3 -87.2(3) 1_356 . . . ? Co3 O4 C14 C5 176.5(3) 1_455 . . . ? Co2 O4 C14 C5 90.0(3) 1_356 . . . ? C6 C5 C14 O3 3.9(5) . . . . ? C4 C5 C14 O3 177.9(3) . . . . ? C6 C5 C14 O4 -173.2(3) . . . . ? C4 C5 C14 O4 0.8(5) . . . . ? Co4 O6 C15 O5 -6.0(7) 1_456 . . . ? Co4 O6 C15 C7 173.9(3) 1_456 . . . ? Co3 O5 C15 O6 -10.8(5) 1_456 . . . ? Co3 O5 C15 C7 169.2(2) 1_456 . . . ? C8 C7 C15 O6 -161.4(4) . . . . ? C12 C7 C15 O6 18.3(5) . . . . ? C8 C7 C15 O5 18.5(5) . . . . ? C12 C7 C15 O5 -161.7(4) . . . . ? C3 N1 C16 O7 -2.4(7) . . . . ? C3 N1 C16 C10 177.8(4) . . . . ? C11 C10 C16 O7 162.5(4) . . . . ? C9 C10 C16 O7 -17.0(6) . . . . ? C11 C10 C16 N1 -17.8(6) . . . . ? C9 C10 C16 N1 162.8(4) . . . . ? C22 C17 C18 C19 0.8(7) . . . . ? C32 C17 C18 C19 180.0(4) . . . . ? C17 C18 C19 C20 0.0(7) . . . . ? C18 C19 C20 C21 0.2(6) . . . . ? C18 C19 C20 C29 178.1(4) . . . . ? C19 C20 C21 C22 -1.2(7) . . . . ? C29 C20 C21 C22 -179.2(4) . . . . ? C20 C21 C22 C17 2.0(7) . . . . ? C18 C17 C22 C21 -1.8(7) . . . . ? C32 C17 C22 C21 179.0(5) . . . . ? C28 C23 C24 C25 -1.4(6) . . . . ? C30 C23 C24 C25 172.4(3) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C23 C24 C25 N2 179.4(3) . . . . ? C32 N2 C25 C24 148.1(5) . . . . ? C32 N2 C25 C26 -31.8(7) . . . . ? C24 C25 C26 C27 2.3(6) . . . . ? N2 C25 C26 C27 -177.9(4) . . . . ? C25 C26 C27 C28 -1.7(5) . . . . ? C25 C26 C27 C31 -178.7(3) . . . . ? C24 C23 C28 C27 1.9(5) . . . . ? C30 C23 C28 C27 -171.8(3) . . . . ? C26 C27 C28 C23 -0.4(5) . . . . ? C31 C27 C28 C23 176.7(3) . . . . ? Co1 O8 C29 O9 34.7(5) 1_456 . . . ? Co1 O8 C29 C20 -142.5(3) 1_456 . . . ? Co4 O9 C29 O8 92.3(4) . . . . ? Co4 O9 C29 C20 -90.5(3) . . . . ? C21 C20 C29 O8 159.8(4) . . . . ? C19 C20 C29 O8 -18.1(5) . . . . ? C21 C20 C29 O9 -17.6(5) . . . . ? C19 C20 C29 O9 164.5(4) . . . . ? Co4 O11 C30 O10 -16.0(6) 1_554 . . . ? Co4 O11 C30 C23 160.8(3) 1_554 . . . ? Co2 O10 C30 O11 15.7(6) 1_455 . . . ? Co2 O10 C30 C23 -161.2(3) 1_455 . . . ? C24 C23 C30 O11 -175.3(3) . . . . ? C28 C23 C30 O11 -1.6(5) . . . . ? C24 C23 C30 O10 1.9(5) . . . . ? C28 C23 C30 O10 175.6(3) . . . . ? Co1 O12 C31 O13 -64.2(5) . . . . ? Co1 O12 C31 C27 118.8(3) . . . . ? Co2 O13 C31 O12 -75.5(4) . . . . ? Co2 O13 C31 C27 101.4(3) . . . . ? C26 C27 C31 O12 -173.7(3) . . . . ? C28 C27 C31 O12 9.2(5) . . . . ? C26 C27 C31 O13 9.1(5) . . . . ? C28 C27 C31 O13 -167.9(3) . . . . ? C25 N2 C32 O14' -27.2(9) . . . . ? C25 N2 C32 O14 25.7(9) . . . . ? C25 N2 C32 C17 -173.9(4) . . . . ? C18 C17 C32 O14' -118.5(8) . . . . ? C22 C17 C32 O14' 60.7(9) . . . . ? C18 C17 C32 O14 -172.9(6) . . . . ? C22 C17 C32 O14 6.3(9) . . . . ? C18 C17 C32 N2 26.3(8) . . . . ? C22 C17 C32 N2 -154.5(5) . . . . ? C37 N3 C33 C34 -8.9(6) . . . . ? Co4 N3 C33 C34 145.1(4) . . . . ? N3 C33 C34 C35 0.7(6) . . . . ? C33 C34 C35 C36 8.8(6) . . . . ? C33 C34 C35 N6 -167.4(4) . . . . ? N5 N6 C35 C36 -157.8(4) . . . . ? N5 N6 C35 C34 18.5(6) . . . . ? C34 C35 C36 C37 -9.6(7) . . . . ? N6 C35 C36 C37 166.8(4) . . . . ? C33 N3 C37 C36 8.0(6) . . . . ? Co4 N3 C37 C36 -144.5(4) . . . . ? C35 C36 C37 N3 1.0(7) . . . . ? N6 N5 C38 C42 -13.8(7) . . . . ? N6 N5 C38 C39 170.4(4) . . . . ? C42 C38 C39 C40 -2.9(7) . . . . ? N5 C38 C39 C40 173.1(4) . . . . ? C41 N4 C40 C39 3.4(6) . . . . ? Co2 N4 C40 C39 -171.7(4) . . . . ? C38 C39 C40 N4 -1.0(7) . . . . ? C40 N4 C41 C42 -2.1(7) . . . . ? Co2 N4 C41 C42 172.9(4) . . . . ? C39 C38 C42 C41 4.1(7) . . . . ? N5 C38 C42 C41 -171.5(4) . . . . ? N4 C41 C42 C38 -1.6(7) . . . . ? O5 Co3 O1W Co2 167.04(10) 1_654 . . 1_456 ? O2W Co3 O1W Co2 -35.8(6) . . . 1_456 ? O1 Co3 O1W Co2 74.26(10) . . . 1_456 ? O4 Co3 O1W Co2 -33.14(9) 1_655 . . 1_456 ? O3 Co3 O1W Co2 -91.02(9) 1_655 . . 1_456 ? O5 Co3 O1W Co4 -69.75(11) 1_654 . . . ? O2W Co3 O1W Co4 87.4(6) . . . . ? O1 Co3 O1W Co4 -162.54(10) . . . . ? O4 Co3 O1W Co4 90.06(9) 1_655 . . . ? O3 Co3 O1W Co4 32.18(8) 1_655 . . . ? O11 Co4 O1W Co3 -129.93(11) 1_556 . . . ? O6 Co4 O1W Co3 52.74(11) 1_654 . . . ? O9 Co4 O1W Co3 141.56(10) . . . . ? N3 Co4 O1W Co3 -15.0(6) . . . . ? O3 Co4 O1W Co3 -33.83(9) 1_655 . . . ? O11 Co4 O1W Co2 -26.53(15) 1_556 . . 1_456 ? O6 Co4 O1W Co2 156.13(14) 1_654 . . 1_456 ? O9 Co4 O1W Co2 -115.04(14) . . . 1_456 ? N3 Co4 O1W Co2 88.4(6) . . . 1_456 ? O3 Co4 O1W Co2 69.57(13) 1_655 . . 1_456 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.992 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 935235' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 N5 Ni O8' _chemical_formula_weight 587.16 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1907(4) _cell_length_b 10.2746(4) _cell_length_c 13.2039(6) _cell_angle_alpha 80.3210(10) _cell_angle_beta 81.0010(10) _cell_angle_gamma 66.2780(10) _cell_volume 1241.64(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9063 _exptl_absorpt_correction_T_max 0.9310 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14465 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4324 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+1.3587P] 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 4324 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.95135(3) 0.26422(4) 0.56604(2) 0.01756(13) Uani 1 1 d . . . O1 O 0.6345(2) 0.3368(2) 0.49879(16) 0.0322(5) Uani 1 1 d . . . O2 O 0.80793(19) 0.1711(2) 0.58814(14) 0.0215(4) Uani 1 1 d . . . O3 O 0.1475(2) 0.0882(2) 0.58476(16) 0.0258(5) Uani 1 1 d . . . O4 O 0.1450(2) 0.3047(2) 0.54877(14) 0.0228(4) Uani 1 1 d . . . O5 O 0.5863(3) -0.6598(3) 1.2298(2) 0.0554(7) Uani 1 1 d . . . O6 O 0.6154(4) -0.5109(3) 1.31945(19) 0.0647(9) Uani 1 1 d . . . H6B H 0.6199 -0.5744 1.3672 0.097 Uiso 1 1 calc R . . O7 O 0.6846(3) -0.0647(3) 0.87996(18) 0.0440(6) Uani 1 1 d . . . N1 N 0.5796(3) -0.1628(3) 0.7904(2) 0.0316(6) Uani 1 1 d . . . N2 N 0.9775(2) 0.2568(3) 0.40699(17) 0.0221(5) Uani 1 1 d . . . N3 N 0.9345(3) 0.2569(3) -0.26857(18) 0.0274(6) Uani 1 1 d . . . N4 N 0.9367(3) 0.1962(3) 0.0551(2) 0.0382(7) Uani 1 1 d . . . N5 N 0.9885(3) 0.2701(3) 0.08669(19) 0.0351(6) Uani 1 1 d . . . C1 C 0.5902(3) 0.1389(3) 0.5935(2) 0.0203(6) Uani 1 1 d . . . C2 C 0.6363(3) 0.0199(3) 0.6667(2) 0.0249(6) Uani 1 1 d . . . H2A H 0.7282 -0.0133 0.6878 0.030 Uiso 1 1 calc R . . C3 C 0.5439(3) -0.0490(3) 0.7080(2) 0.0259(6) Uani 1 1 d . . . C4 C 0.4099(3) -0.0039(3) 0.6719(2) 0.0256(6) Uani 1 1 d . . . H4A H 0.3505 -0.0535 0.6966 0.031 Uiso 1 1 calc R . . C5 C 0.3647(3) 0.1151(3) 0.5993(2) 0.0215(6) Uani 1 1 d . . . C6 C 0.4535(3) 0.1882(3) 0.5610(2) 0.0210(6) Uani 1 1 d . . . H6A H 0.4218 0.2698 0.5139 0.025 Uiso 1 1 calc R . . C7 C 0.6331(3) -0.2632(3) 0.9661(2) 0.0313(7) Uani 1 1 d . . . C8 C 0.6144(4) -0.2219(4) 1.0629(3) 0.0412(8) Uani 1 1 d . . . H8A H 0.6081 -0.1307 1.0693 0.049 Uiso 1 1 calc R . . C9 C 0.6046(4) -0.3133(4) 1.1512(3) 0.0426(9) Uani 1 1 d . . . H9A H 0.5905 -0.2835 1.2162 0.051 Uiso 1 1 calc R . . C10 C 0.6164(3) -0.4503(3) 1.1412(2) 0.0330(7) Uani 1 1 d . . . C11 C 0.6386(4) -0.4939(4) 1.0441(3) 0.0368(8) Uani 1 1 d . . . H11A H 0.6480 -0.5861 1.0377 0.044 Uiso 1 1 calc R . . C12 C 0.6468(4) -0.4015(4) 0.9567(2) 0.0351(7) Uani 1 1 d . . . H12A H 0.6615 -0.4314 0.8917 0.042 Uiso 1 1 calc R . . C13 C 0.6845(3) 0.2217(3) 0.55580(19) 0.0203(6) Uani 1 1 d . . . C14 C 0.2128(3) 0.1705(3) 0.5738(2) 0.0197(6) Uani 1 1 d . . . C15 C 0.6037(4) -0.5522(4) 1.2339(3) 0.0387(8) Uani 1 1 d . . . C16 C 0.6371(3) -0.1547(3) 0.8755(2) 0.0314(7) Uani 1 1 d . . . C17 C 0.9457(3) 0.1608(3) 0.3691(2) 0.0260(6) Uani 1 1 d . . . H17A H 0.9215 0.0933 0.4154 0.031 Uiso 1 1 calc R . . C18 C 0.9470(3) 0.1569(3) 0.2655(2) 0.0295(7) Uani 1 1 d . . . H18A H 0.9224 0.0898 0.2424 0.035 Uiso 1 1 calc R . . C19 C 0.9858(3) 0.2553(3) 0.1965(2) 0.0297(7) Uani 1 1 d . . . C20 C 1.0251(4) 0.3509(4) 0.2341(2) 0.0365(8) Uani 1 1 d . . . H20A H 1.0557 0.4153 0.1891 0.044 Uiso 1 1 calc R . . C21 C 1.0181(4) 0.3490(4) 0.3390(2) 0.0328(7) Uani 1 1 d . . . H21A H 1.0428 0.4148 0.3639 0.039 Uiso 1 1 calc R . . C22 C 0.9403(4) 0.2168(4) -0.0556(2) 0.0336(7) Uani 1 1 d . . . C23 C 0.8483(3) 0.1809(3) -0.09912(17) 0.0436(9) Uani 1 1 d . . . H23A H 0.7871 0.1420 -0.0580 0.052 Uiso 1 1 calc R . . C24 C 0.8476(3) 0.2034(3) -0.20542(17) 0.0390(8) Uani 1 1 d R . . H24A H 0.7833 0.1804 -0.2344 0.047 Uiso 1 1 d R . . C25 C 1.0239(4) 0.2905(4) -0.2239(2) 0.0387(8) Uani 1 1 d . . . H25A H 1.0854 0.3278 -0.2662 0.046 Uiso 1 1 calc R . . C26 C 1.0302(4) 0.2731(4) -0.1190(3) 0.0438(9) Uani 1 1 d . . . H26A H 1.0938 0.2987 -0.0915 0.053 Uiso 1 1 calc R . . O1W O 0.7927(2) 0.4683(2) 0.55295(16) 0.0284(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01815(19) 0.0225(2) 0.01550(19) 0.00103(13) -0.00323(13) -0.01215(15) O1 0.0319(11) 0.0343(13) 0.0346(12) 0.0169(10) -0.0133(9) -0.0217(10) O2 0.0206(10) 0.0276(11) 0.0211(10) 0.0043(8) -0.0062(8) -0.0155(9) O3 0.0225(10) 0.0257(11) 0.0344(11) 0.0031(9) -0.0063(9) -0.0162(9) O4 0.0220(10) 0.0243(11) 0.0256(10) 0.0032(8) -0.0061(8) -0.0136(9) O5 0.083(2) 0.0522(17) 0.0461(15) 0.0192(13) -0.0223(14) -0.0450(16) O6 0.123(3) 0.0531(17) 0.0275(14) 0.0156(12) -0.0146(15) -0.0495(19) O7 0.0583(16) 0.0461(15) 0.0366(13) 0.0109(11) -0.0121(11) -0.0327(13) N1 0.0311(14) 0.0307(15) 0.0320(14) 0.0172(11) -0.0129(11) -0.0155(12) N2 0.0254(12) 0.0260(13) 0.0190(12) 0.0003(10) -0.0029(10) -0.0151(11) N3 0.0338(14) 0.0345(15) 0.0181(12) -0.0023(10) -0.0036(10) -0.0175(12) N4 0.0493(17) 0.0477(18) 0.0194(13) -0.0044(12) -0.0049(12) -0.0201(15) N5 0.0421(16) 0.0448(17) 0.0183(13) -0.0039(11) -0.0033(11) -0.0164(14) C1 0.0226(14) 0.0255(15) 0.0170(13) 0.0014(11) -0.0019(11) -0.0152(12) C2 0.0236(14) 0.0297(17) 0.0243(15) 0.0045(12) -0.0063(12) -0.0149(13) C3 0.0245(14) 0.0260(16) 0.0278(15) 0.0071(12) -0.0063(12) -0.0131(13) C4 0.0221(14) 0.0266(16) 0.0315(16) 0.0049(12) -0.0048(12) -0.0153(13) C5 0.0199(13) 0.0243(15) 0.0231(14) -0.0002(11) -0.0043(11) -0.0117(12) C6 0.0211(14) 0.0220(15) 0.0207(14) 0.0039(11) -0.0052(11) -0.0104(12) C7 0.0278(16) 0.0314(18) 0.0291(17) 0.0101(13) -0.0063(13) -0.0096(14) C8 0.054(2) 0.0280(19) 0.0379(19) 0.0050(14) -0.0055(16) -0.0155(17) C9 0.060(2) 0.037(2) 0.0272(17) 0.0032(14) -0.0027(16) -0.0186(18) C10 0.0332(17) 0.0318(18) 0.0303(17) 0.0084(13) -0.0068(13) -0.0123(14) C11 0.0417(19) 0.0348(19) 0.0344(18) 0.0082(14) -0.0090(15) -0.0181(16) C12 0.0383(18) 0.0343(19) 0.0295(17) 0.0040(14) -0.0068(14) -0.0124(15) C13 0.0230(14) 0.0280(16) 0.0136(13) 0.0008(11) -0.0022(11) -0.0148(12) C14 0.0206(13) 0.0251(16) 0.0169(13) 0.0003(11) -0.0018(10) -0.0134(12) C15 0.0421(19) 0.040(2) 0.0325(18) 0.0132(15) -0.0090(15) -0.0192(17) C16 0.0280(16) 0.0330(18) 0.0310(17) 0.0080(13) -0.0041(13) -0.0137(14) C17 0.0309(16) 0.0306(17) 0.0208(14) -0.0023(12) 0.0004(12) -0.0176(14) C18 0.0382(17) 0.0338(18) 0.0243(15) -0.0059(13) -0.0042(13) -0.0207(15) C19 0.0332(16) 0.0371(18) 0.0186(14) -0.0020(13) -0.0018(12) -0.0140(14) C20 0.056(2) 0.041(2) 0.0216(15) 0.0019(14) 0.0005(14) -0.0325(18) C21 0.0486(19) 0.0389(19) 0.0233(15) -0.0022(13) -0.0018(14) -0.0310(17) C22 0.0418(18) 0.0387(19) 0.0194(15) -0.0027(13) -0.0047(13) -0.0144(16) C23 0.059(2) 0.064(3) 0.0229(16) -0.0065(16) 0.0029(15) -0.042(2) C24 0.045(2) 0.062(2) 0.0245(16) -0.0079(15) -0.0027(14) -0.0343(19) C25 0.046(2) 0.058(2) 0.0239(16) -0.0058(15) 0.0002(14) -0.0333(18) C26 0.048(2) 0.071(3) 0.0259(17) -0.0098(17) -0.0038(15) -0.035(2) O1W 0.0279(11) 0.0223(11) 0.0356(12) 0.0000(9) -0.0054(9) -0.0107(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.0083(18) . ? Ni1 O1W 2.069(2) . ? Ni1 N2 2.086(2) . ? Ni1 O3 2.103(2) 1_655 ? Ni1 O4 2.1465(18) 1_655 ? Ni1 N3 2.154(2) 1_556 ? Ni1 C14 2.454(3) 1_655 ? O1 C13 1.249(3) . ? O2 C13 1.265(3) . ? O3 C14 1.249(3) . ? O3 Ni1 2.103(2) 1_455 ? O4 C14 1.280(3) . ? O4 Ni1 2.1465(18) 1_455 ? O5 C15 1.199(4) . ? O6 C15 1.309(4) . ? O6 H6B 0.8200 . ? O7 C16 1.216(4) . ? N1 C16 1.374(4) . ? N1 C3 1.427(4) . ? N2 C21 1.337(4) . ? N2 C17 1.343(4) . ? N3 C25 1.337(4) . ? N3 C24 1.337(3) . ? N3 Ni1 2.154(2) 1_554 ? N4 N5 1.236(4) . ? N4 C22 1.438(4) . ? N5 C19 1.429(4) . ? C1 C6 1.388(4) . ? C1 C2 1.390(4) . ? C1 C13 1.504(4) . ? C2 C3 1.389(4) . ? C2 H2A 0.9300 . ? C3 C4 1.388(4) . ? C4 C5 1.385(4) . ? C4 H4A 0.9300 . ? C5 C6 1.383(4) . ? C5 C14 1.492(4) . ? C6 H6A 0.9300 . ? C7 C8 1.375(5) . ? C7 C12 1.396(5) . ? C7 C16 1.499(4) . ? C8 C9 1.387(5) . ? C8 H8A 0.9300 . ? C9 C10 1.391(5) . ? C9 H9A 0.9300 . ? C10 C11 1.385(5) . ? C10 C15 1.496(4) . ? C11 C12 1.380(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 Ni1 2.454(3) 1_455 ? C17 C18 1.372(4) . ? C17 H17A 0.9300 . ? C18 C19 1.381(4) . ? C18 H18A 0.9300 . ? C19 C20 1.384(4) . ? C20 C21 1.374(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.366(4) . ? C22 C26 1.378(5) . ? C23 C24 1.3842 . ? C23 H23A 0.9300 . ? C24 H24A 0.9301 . ? C25 C26 1.374(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O1W 92.86(8) . . ? O2 Ni1 N2 92.19(8) . . ? O1W Ni1 N2 92.22(9) . . ? O2 Ni1 O3 102.57(7) . 1_655 ? O1W Ni1 O3 163.98(7) . 1_655 ? N2 Ni1 O3 91.50(9) . 1_655 ? O2 Ni1 O4 164.45(8) . 1_655 ? O1W Ni1 O4 102.67(8) . 1_655 ? N2 Ni1 O4 88.02(8) . 1_655 ? O3 Ni1 O4 61.89(7) 1_655 1_655 ? O2 Ni1 N3 87.23(8) . 1_556 ? O1W Ni1 N3 91.67(9) . 1_556 ? N2 Ni1 N3 176.09(10) . 1_556 ? O3 Ni1 N3 84.86(9) 1_655 1_556 ? O4 Ni1 N3 91.50(8) 1_655 1_556 ? O2 Ni1 C14 133.09(8) . 1_655 ? O1W Ni1 C14 133.66(8) . 1_655 ? N2 Ni1 C14 91.66(9) . 1_655 ? O3 Ni1 C14 30.59(8) 1_655 1_655 ? O4 Ni1 C14 31.42(8) 1_655 1_655 ? N3 Ni1 C14 85.92(9) 1_556 1_655 ? C13 O2 Ni1 127.00(17) . . ? C14 O3 Ni1 90.44(17) . 1_455 ? C14 O4 Ni1 87.67(15) . 1_455 ? C15 O6 H6B 109.5 . . ? C16 N1 C3 121.8(3) . . ? C21 N2 C17 117.4(2) . . ? C21 N2 Ni1 122.90(19) . . ? C17 N2 Ni1 119.65(18) . . ? C25 N3 C24 116.5(2) . . ? C25 N3 Ni1 120.7(2) . 1_554 ? C24 N3 Ni1 122.36(17) . 1_554 ? N5 N4 C22 111.9(3) . . ? N4 N5 C19 114.3(3) . . ? C6 C1 C2 120.5(2) . . ? C6 C1 C13 119.8(2) . . ? C2 C1 C13 119.6(2) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 N1 117.9(2) . . ? C2 C3 N1 122.1(3) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C6 C5 C4 120.3(2) . . ? C6 C5 C14 121.6(2) . . ? C4 C5 C14 117.7(2) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C8 C7 C12 119.2(3) . . ? C8 C7 C16 117.3(3) . . ? C12 C7 C16 123.5(3) . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 C15 118.8(3) . . ? C9 C10 C15 121.2(3) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C7 119.9(3) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? O1 C13 O2 124.8(2) . . ? O1 C13 C1 118.4(2) . . ? O2 C13 C1 116.7(2) . . ? O3 C14 O4 119.6(2) . . ? O3 C14 C5 120.2(2) . . ? O4 C14 C5 120.0(2) . . ? O3 C14 Ni1 58.98(14) . 1_455 ? O4 C14 Ni1 60.91(13) . 1_455 ? C5 C14 Ni1 169.43(19) . 1_455 ? O5 C15 O6 124.2(3) . . ? O5 C15 C10 123.6(3) . . ? O6 C15 C10 112.2(3) . . ? O7 C16 N1 123.7(3) . . ? O7 C16 C7 121.3(3) . . ? N1 C16 C7 115.0(3) . . ? N2 C17 C18 123.5(3) . . ? N2 C17 H17A 118.2 . . ? C18 C17 H17A 118.2 . . ? C17 C18 C19 118.3(3) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 120.8 . . ? C18 C19 C20 118.9(3) . . ? C18 C19 N5 126.0(3) . . ? C20 C19 N5 115.1(3) . . ? C21 C20 C19 118.9(3) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? N2 C21 C20 122.9(3) . . ? N2 C21 H21A 118.6 . . ? C20 C21 H21A 118.6 . . ? C23 C22 C26 118.9(3) . . ? C23 C22 N4 118.1(3) . . ? C26 C22 N4 123.1(3) . . ? C22 C23 C24 118.90(16) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? N3 C24 C23 123.31(14) . . ? N3 C24 H24A 118.3 . . ? C23 C24 H24A 118.4 . . ? N3 C25 C26 123.9(3) . . ? N3 C25 H25A 118.1 . . ? C26 C25 H25A 118.1 . . ? C25 C26 C22 118.6(3) . . ? C25 C26 H26A 120.7 . . ? C22 C26 H26A 120.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Ni1 O2 C13 27.5(2) . . . . ? N2 Ni1 O2 C13 -64.9(2) . . . . ? O3 Ni1 O2 C13 -156.9(2) 1_655 . . . ? O4 Ni1 O2 C13 -155.3(3) 1_655 . . . ? N3 Ni1 O2 C13 119.0(2) 1_556 . . . ? C14 Ni1 O2 C13 -159.2(2) 1_655 . . . ? O2 Ni1 N2 C21 153.7(2) . . . . ? O1W Ni1 N2 C21 60.7(2) . . . . ? O3 Ni1 N2 C21 -103.7(2) 1_655 . . . ? O4 Ni1 N2 C21 -41.9(2) 1_655 . . . ? N3 Ni1 N2 C21 -124.8(12) 1_556 . . . ? C14 Ni1 N2 C21 -73.1(2) 1_655 . . . ? O2 Ni1 N2 C17 -22.8(2) . . . . ? O1W Ni1 N2 C17 -115.8(2) . . . . ? O3 Ni1 N2 C17 79.8(2) 1_655 . . . ? O4 Ni1 N2 C17 141.6(2) 1_655 . . . ? N3 Ni1 N2 C17 58.7(13) 1_556 . . . ? C14 Ni1 N2 C17 110.4(2) 1_655 . . . ? C22 N4 N5 C19 179.2(3) . . . . ? C6 C1 C2 C3 -0.5(4) . . . . ? C13 C1 C2 C3 174.4(3) . . . . ? C1 C2 C3 C4 3.6(5) . . . . ? C1 C2 C3 N1 -173.8(3) . . . . ? C16 N1 C3 C4 -132.4(3) . . . . ? C16 N1 C3 C2 45.1(4) . . . . ? C2 C3 C4 C5 -3.9(5) . . . . ? N1 C3 C4 C5 173.6(3) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C3 C4 C5 C14 -172.0(3) . . . . ? C4 C5 C6 C1 2.0(4) . . . . ? C14 C5 C6 C1 174.8(3) . . . . ? C2 C1 C6 C5 -2.3(4) . . . . ? C13 C1 C6 C5 -177.2(2) . . . . ? C12 C7 C8 C9 -1.9(5) . . . . ? C16 C7 C8 C9 177.9(3) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? C8 C9 C10 C15 -178.8(3) . . . . ? C9 C10 C11 C12 -1.1(5) . . . . ? C15 C10 C11 C12 178.2(3) . . . . ? C10 C11 C12 C7 0.2(5) . . . . ? C8 C7 C12 C11 1.3(5) . . . . ? C16 C7 C12 C11 -178.5(3) . . . . ? Ni1 O2 C13 O1 4.3(4) . . . . ? Ni1 O2 C13 C1 -172.82(17) . . . . ? C6 C1 C13 O1 2.7(4) . . . . ? C2 C1 C13 O1 -172.3(3) . . . . ? C6 C1 C13 O2 -180.0(2) . . . . ? C2 C1 C13 O2 5.1(4) . . . . ? Ni1 O3 C14 O4 -6.4(3) 1_455 . . . ? Ni1 O3 C14 C5 167.8(2) 1_455 . . . ? Ni1 O4 C14 O3 6.3(2) 1_455 . . . ? Ni1 O4 C14 C5 -167.9(2) 1_455 . . . ? C6 C5 C14 O3 160.7(3) . . . . ? C4 C5 C14 O3 -26.4(4) . . . . ? C6 C5 C14 O4 -25.1(4) . . . . ? C4 C5 C14 O4 147.8(3) . . . . ? C6 C5 C14 Ni1 -117.0(10) . . . 1_455 ? C4 C5 C14 Ni1 55.9(12) . . . 1_455 ? C11 C10 C15 O5 -13.6(5) . . . . ? C9 C10 C15 O5 165.7(4) . . . . ? C11 C10 C15 O6 165.7(3) . . . . ? C9 C10 C15 O6 -15.0(5) . . . . ? C3 N1 C16 O7 -13.1(5) . . . . ? C3 N1 C16 C7 164.9(3) . . . . ? C8 C7 C16 O7 31.6(5) . . . . ? C12 C7 C16 O7 -148.6(3) . . . . ? C8 C7 C16 N1 -146.4(3) . . . . ? C12 C7 C16 N1 33.3(4) . . . . ? C21 N2 C17 C18 -2.9(4) . . . . ? Ni1 N2 C17 C18 173.8(2) . . . . ? N2 C17 C18 C19 1.3(5) . . . . ? C17 C18 C19 C20 1.6(5) . . . . ? C17 C18 C19 N5 -177.8(3) . . . . ? N4 N5 C19 C18 7.8(5) . . . . ? N4 N5 C19 C20 -171.6(3) . . . . ? C18 C19 C20 C21 -2.9(5) . . . . ? N5 C19 C20 C21 176.6(3) . . . . ? C17 N2 C21 C20 1.5(5) . . . . ? Ni1 N2 C21 C20 -175.1(3) . . . . ? C19 C20 C21 N2 1.3(5) . . . . ? N5 N4 C22 C23 -159.2(3) . . . . ? N5 N4 C22 C26 19.6(5) . . . . ? C26 C22 C23 C24 -0.5(4) . . . . ? N4 C22 C23 C24 178.4(2) . . . . ? C25 N3 C24 C23 -0.8(3) . . . . ? Ni1 N3 C24 C23 171.56(8) 1_554 . . . ? C22 C23 C24 N3 1.1(2) . . . . ? C24 N3 C25 C26 0.0(5) . . . . ? Ni1 N3 C25 C26 -172.5(3) 1_554 . . . ? N3 C25 C26 C22 0.5(6) . . . . ? C23 C22 C26 C25 -0.2(5) . . . . ? N4 C22 C26 C25 -179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.813 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 935236' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H29 N4 O11 Zn' _chemical_formula_weight 698.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0093(8) _cell_length_b 9.0265(9) _cell_length_c 22.400(2) _cell_angle_alpha 86.845(4) _cell_angle_beta 85.477(4) _cell_angle_gamma 68.016(3) _cell_volume 1496.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17593 _diffrn_reflns_av_R_equivalents 0.1312 _diffrn_reflns_av_sigmaI/netI 0.1486 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5247 _reflns_number_gt 2737 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^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 5247 _refine_ls_number_parameters 497 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1568 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2180 _refine_ls_wR_factor_gt 0.1678 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.07809(11) -0.34106(9) 0.49074(4) 0.0372(3) Uani 1 1 d . . . O2 O -0.1350(6) -0.1655(5) 0.4673(2) 0.0365(12) Uani 1 1 d . . . O4 O -0.8448(6) 0.4475(5) 0.4576(2) 0.0369(12) Uani 1 1 d . . . O1W O 0.2724(6) -0.2683(5) 0.4450(2) 0.0470(13) Uani 1 1 d . . . N1 N -0.6322(8) 0.1137(8) 0.2688(3) 0.0404(16) Uani 1 1 d . . . O3 O -0.5980(6) 0.3735(5) 0.5088(2) 0.0421(13) Uani 1 1 d . . . O1 O -0.1083(7) -0.2678(6) 0.3782(2) 0.0648(17) Uani 1 1 d . . . C13 C -0.1879(9) -0.1642(8) 0.4153(3) 0.0355(17) Uani 1 1 d . . . N2 N 0.1031(8) -0.2766(6) 0.5733(2) 0.0376(14) Uani 1 1 d . . . C17 C -0.0006(9) -0.1313(8) 0.5937(3) 0.0387(18) Uani 1 1 d . . . H17A H -0.0829 -0.0606 0.5685 0.046 Uiso 1 1 calc R . . C20 C 0.2402(11) -0.3320(9) 0.6677(3) 0.054(2) Uani 1 1 d . . . H20A H 0.3252 -0.4031 0.6920 0.064 Uiso 1 1 calc R . . C16 C -0.7177(10) 0.2410(9) 0.2347(3) 0.048(2) Uani 1 1 d . . . C2 C -0.4239(9) -0.0170(8) 0.3444(3) 0.0334(16) Uani 1 1 d . . . H2A H -0.3670 -0.0987 0.3176 0.040 Uiso 1 1 calc R . . C6 C -0.4397(9) 0.0958(7) 0.4390(3) 0.0316(16) Uani 1 1 d . . . H6A H -0.3917 0.0926 0.4758 0.038 Uiso 1 1 calc R . . C14 C -0.6789(9) 0.3546(7) 0.4675(3) 0.0318(16) Uani 1 1 d . . . C5 C -0.5926(8) 0.2233(7) 0.4239(3) 0.0267(15) Uani 1 1 d . . . C23 C 0.0736(13) 0.0229(10) 0.7662(4) 0.072(3) Uani 1 1 d . . . H23A H 0.0090 0.1027 0.7396 0.086 Uiso 1 1 calc R . . O7 O -0.7687(8) 0.3789(6) 0.2530(2) 0.0726(19) Uani 1 1 d . . . C4 C -0.6594(9) 0.2313(8) 0.3680(3) 0.0321(16) Uani 1 1 d . . . H4A H -0.7624 0.3174 0.3580 0.039 Uiso 1 1 calc R . . C3 C -0.5756(9) 0.1138(8) 0.3273(3) 0.0321(16) Uani 1 1 d . . . C1 C -0.3579(9) -0.0270(7) 0.3996(3) 0.0309(16) Uani 1 1 d . . . C18 C 0.0090(9) -0.0830(8) 0.6488(3) 0.0363(17) Uani 1 1 d . . . H18A H -0.0670 0.0186 0.6606 0.044 Uiso 1 1 calc R . . C19 C 0.1294(10) -0.1820(9) 0.6879(3) 0.0421(19) Uani 1 1 d . . . C22 C 0.1447(11) -0.1309(9) 0.7489(3) 0.046(2) Uani 1 1 d . . . C21 C 0.2218(11) -0.3736(9) 0.6107(3) 0.051(2) Uani 1 1 d . . . H21A H 0.2960 -0.4746 0.5977 0.062 Uiso 1 1 calc R . . O6 O -0.7722(11) 0.0144(9) -0.0269(3) 0.099(2) Uani 1 1 d . A . H6B H -0.7944 0.0108 -0.0618 0.148 Uiso 1 1 calc R . . N3 N 0.1831(12) -0.0404(10) 0.8626(3) 0.074(2) Uani 1 1 d . . . C26 C 0.2432(17) -0.2387(12) 0.7903(4) 0.100(4) Uani 1 1 d . . . H26A H 0.3020 -0.3455 0.7807 0.120 Uiso 1 1 calc R . . O5 O -0.978(5) 0.253(6) -0.036(2) 0.104(10) Uani 0.50 1 d PU A 1 O5' O -0.897(5) 0.274(6) -0.041(2) 0.109(10) Uani 0.50 1 d PU A 2 C25 C 0.2549(17) -0.1886(14) 0.8462(4) 0.103(4) Uani 1 1 d . . . H25A H 0.3181 -0.2654 0.8741 0.124 Uiso 1 1 calc R . . C24 C 0.0958(16) 0.0630(12) 0.8232(5) 0.092(4) Uani 1 1 d . . . H24A H 0.0450 0.1699 0.8334 0.110 Uiso 1 1 calc R . . C7 C -0.810(2) 0.182(2) 0.0547(5) 0.054(11) Uani 0.50 1 d PG A 1 C8 C -0.848(2) 0.3323(16) 0.0773(7) 0.082(9) Uani 0.50 1 d PG A 1 H8A H -0.8957 0.4231 0.0528 0.098 Uiso 0.50 1 calc PR A 1 C9 C -0.816(2) 0.3472(14) 0.1363(8) 0.074(8) Uani 0.50 1 d PG A 1 H9A H -0.8423 0.4479 0.1514 0.088 Uiso 0.50 1 calc PR A 1 C10 C -0.745(2) 0.2116(17) 0.1728(5) 0.041(16) Uani 0.50 1 d PG A 1 C11 C -0.707(2) 0.0611(14) 0.1503(6) 0.050(5) Uani 0.50 1 d PG A 1 H11A H -0.6593 -0.0297 0.1747 0.060 Uiso 0.50 1 calc PR A 1 C12 C -0.739(2) 0.0462(15) 0.0912(6) 0.057(7) Uani 0.50 1 d PGU A 1 H12A H -0.7128 -0.0545 0.0761 0.069 Uiso 0.50 1 calc PR A 1 C7' C -0.818(2) 0.165(2) 0.0546(6) 0.072(14) Uani 0.50 1 d PG A 2 C8' C -0.9345(19) 0.2972(18) 0.0856(8) 0.071(7) Uani 0.50 1 d PG A 2 H8'A H -1.0346 0.3698 0.0675 0.086 Uiso 0.50 1 calc PR A 2 C9' C -0.9019(19) 0.3206(16) 0.1437(8) 0.062(7) Uani 0.50 1 d PG A 2 H9'A H -0.9802 0.4088 0.1645 0.075 Uiso 0.50 1 calc PR A 2 C10' C -0.752(2) 0.2121(19) 0.1708(6) 0.054(19) Uani 0.50 1 d PGU A 2 C11' C -0.6354(17) 0.0802(16) 0.1398(6) 0.051(6) Uani 0.50 1 d PGU A 2 H11B H -0.5353 0.0076 0.1579 0.061 Uiso 0.50 1 calc PR A 2 C12' C -0.668(2) 0.0568(17) 0.0816(6) 0.051(5) Uani 0.50 1 d PG A 2 H12B H -0.5897 -0.0314 0.0609 0.061 Uiso 0.50 1 calc PR A 2 C15 C -0.8460(15) 0.1543(13) -0.0096(4) 0.075(3) Uani 1 1 d . . . O4W O 0.8878(10) -0.3755(8) 0.2677(3) 0.103(2) Uani 1 1 d . . . O2W O 0.5204(12) -0.2447(9) 0.2434(3) 0.113(3) Uani 1 1 d . . . O3W O 0.2950(11) -0.3485(10) 0.3259(3) 0.121(3) Uani 1 1 d . . . N01 N 0.493(3) -0.376(2) 0.1504(9) 0.144(5) Uani 0.50 1 d PGU B 1 C01 C 0.615(3) -0.358(2) 0.1055(12) 0.135(4) Uani 0.50 1 d PGU B 1 H01A H 0.6991 -0.3156 0.1143 0.162 Uiso 0.50 1 calc PR B 1 C02 C 0.610(3) -0.404(3) 0.0476(11) 0.139(4) Uani 0.50 1 d PGU B 1 H02A H 0.6918 -0.3915 0.0176 0.167 Uiso 0.50 1 calc PR B 1 C03 C 0.485(4) -0.467(2) 0.0345(9) 0.137(5) Uani 0.50 1 d PGU . 1 C04 C 0.363(3) -0.486(2) 0.0794(12) 0.140(5) Uani 0.50 1 d PGU B 1 H04A H 0.2788 -0.5282 0.0706 0.168 Uiso 0.50 1 calc PR B 1 C05 C 0.367(3) -0.440(2) 0.1374(10) 0.141(5) Uani 0.50 1 d PGU B 1 H05A H 0.2862 -0.4523 0.1674 0.169 Uiso 0.50 1 calc PR B 1 N1' N 0.526(4) -0.356(2) 0.1391(9) 0.141(5) Uani 0.50 1 d PGU C 2 C1' C 0.683(3) -0.412(3) 0.1021(12) 0.137(5) Uani 0.50 1 d PGU C 2 H1'A H 0.7914 -0.4156 0.1154 0.164 Uiso 0.50 1 calc PR C 2 C2' C 0.678(3) -0.463(2) 0.0450(12) 0.139(4) Uani 0.50 1 d PGU C 2 H2'A H 0.7827 -0.5002 0.0202 0.166 Uiso 0.50 1 calc PR C 2 C3' C 0.515(4) -0.457(2) 0.0250(9) 0.138(5) Uani 0.50 1 d PGU . 2 C4' C 0.358(3) -0.401(2) 0.0621(11) 0.140(5) Uani 0.50 1 d PGU C 2 H4'A H 0.2499 -0.3972 0.0487 0.168 Uiso 0.50 1 calc PR C 2 C5' C 0.364(3) -0.350(2) 0.1191(10) 0.143(5) Uani 0.50 1 d PGU C 2 H5'A H 0.2586 -0.3127 0.1439 0.172 Uiso 0.50 1 calc PR C 2 H1A H -0.594(10) 0.023(9) 0.258(3) 0.05(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0377(5) 0.0277(5) 0.0369(5) -0.0088(3) -0.0134(4) 0.0018(3) O2 0.037(3) 0.029(2) 0.037(3) 0.000(2) -0.012(2) -0.001(2) O4 0.033(3) 0.022(2) 0.044(3) -0.009(2) -0.015(2) 0.006(2) O1W 0.043(3) 0.044(3) 0.050(3) 0.000(2) -0.011(3) -0.011(2) N1 0.049(4) 0.034(4) 0.026(4) -0.011(3) -0.016(3) 0.004(3) O3 0.035(3) 0.046(3) 0.043(3) -0.019(2) -0.015(2) -0.006(2) O1 0.063(4) 0.051(3) 0.050(3) -0.023(3) -0.015(3) 0.019(3) C13 0.036(4) 0.031(4) 0.037(5) -0.010(3) -0.004(4) -0.007(3) N2 0.042(4) 0.036(3) 0.032(3) -0.007(3) -0.009(3) -0.008(3) C17 0.038(4) 0.034(4) 0.042(5) -0.010(3) -0.004(4) -0.008(3) C20 0.058(5) 0.052(5) 0.033(5) -0.005(4) -0.018(4) 0.002(4) C16 0.047(5) 0.046(5) 0.033(5) -0.008(4) -0.012(4) 0.006(4) C2 0.037(4) 0.033(4) 0.027(4) -0.011(3) 0.001(3) -0.008(3) C6 0.030(4) 0.025(3) 0.036(4) -0.001(3) -0.011(3) -0.005(3) C14 0.034(4) 0.018(3) 0.037(4) -0.003(3) 0.000(3) -0.002(3) C5 0.027(4) 0.019(3) 0.030(4) 0.000(3) -0.006(3) -0.003(3) C23 0.098(8) 0.050(5) 0.054(6) -0.025(4) -0.020(5) -0.007(5) O7 0.101(5) 0.045(3) 0.042(3) -0.009(3) -0.031(3) 0.013(3) C4 0.036(4) 0.036(4) 0.021(4) -0.003(3) -0.006(3) -0.010(3) C3 0.029(4) 0.035(4) 0.028(4) -0.007(3) -0.006(3) -0.006(3) C1 0.035(4) 0.025(3) 0.029(4) -0.005(3) -0.009(3) -0.006(3) C18 0.038(4) 0.035(4) 0.030(4) -0.007(3) -0.008(3) -0.004(3) C19 0.052(5) 0.044(4) 0.031(4) -0.016(3) -0.001(4) -0.016(4) C22 0.061(5) 0.050(5) 0.031(4) -0.006(4) -0.010(4) -0.022(4) C21 0.065(6) 0.043(5) 0.039(5) -0.012(4) -0.018(4) -0.008(4) O6 0.145(7) 0.092(5) 0.044(4) -0.015(4) -0.033(4) -0.020(5) N3 0.105(7) 0.070(5) 0.048(5) -0.014(4) -0.021(5) -0.027(5) C26 0.183(12) 0.061(6) 0.039(6) -0.013(5) -0.046(7) -0.018(7) O5 0.13(3) 0.094(12) 0.074(9) -0.008(8) -0.081(19) -0.018(16) O5' 0.16(3) 0.087(12) 0.068(9) -0.004(8) -0.08(2) -0.017(17) C25 0.160(12) 0.083(8) 0.052(6) -0.002(6) -0.049(7) -0.020(8) C24 0.125(10) 0.063(6) 0.065(7) -0.032(6) -0.026(7) -0.001(6) C7 0.045(19) 0.07(2) 0.03(3) -0.010(16) -0.014(16) 0.002(16) C8 0.12(2) 0.068(14) 0.051(14) -0.003(11) -0.061(15) -0.011(14) C9 0.11(2) 0.063(13) 0.048(13) 0.005(10) -0.053(14) -0.031(13) C10 0.038(17) 0.05(2) 0.018(14) -0.011(7) -0.013(8) 0.004(7) C11 0.084(14) 0.043(10) 0.028(9) 0.010(7) -0.023(9) -0.027(10) C12 0.058(7) 0.057(7) 0.057(7) -0.002(2) -0.005(2) -0.021(3) C7' 0.12(4) 0.07(2) 0.04(3) 0.023(18) -0.03(2) -0.04(2) C8' 0.082(17) 0.077(15) 0.059(14) -0.025(11) -0.025(13) -0.025(13) C9' 0.072(16) 0.049(11) 0.046(12) -0.030(9) -0.017(11) 0.007(11) C10' 0.054(19) 0.054(19) 0.054(19) -0.002(2) -0.003(2) -0.020(7) C11' 0.051(6) 0.051(6) 0.051(6) -0.002(2) -0.004(2) -0.019(3) C12' 0.075(14) 0.063(12) 0.012(8) -0.014(7) -0.004(9) -0.021(10) C15 0.100(8) 0.067(7) 0.044(6) -0.010(5) -0.029(6) -0.011(6) O4W 0.106(6) 0.097(5) 0.083(5) -0.017(4) -0.010(4) -0.010(4) O2W 0.166(8) 0.088(5) 0.094(6) 0.003(4) -0.030(5) -0.054(5) O3W 0.125(7) 0.137(7) 0.074(5) -0.018(5) -0.015(5) -0.015(5) N01 0.182(10) 0.113(8) 0.126(9) -0.011(7) -0.049(8) -0.034(8) C01 0.175(10) 0.111(8) 0.118(8) -0.013(7) -0.046(8) -0.042(8) C02 0.178(10) 0.119(8) 0.121(8) -0.016(7) -0.045(8) -0.048(8) C03 0.175(10) 0.122(8) 0.121(8) -0.019(7) -0.044(8) -0.052(8) C04 0.176(10) 0.122(9) 0.123(9) -0.017(7) -0.047(8) -0.045(8) C05 0.176(11) 0.117(9) 0.125(9) -0.016(8) -0.050(9) -0.041(9) N1' 0.182(10) 0.110(7) 0.121(8) -0.008(7) -0.048(8) -0.036(8) C1' 0.178(10) 0.114(8) 0.118(8) -0.010(7) -0.048(8) -0.043(8) C2' 0.177(10) 0.118(8) 0.120(8) -0.015(7) -0.045(8) -0.047(8) C3' 0.176(10) 0.123(8) 0.121(9) -0.018(7) -0.044(8) -0.053(8) C4' 0.173(10) 0.124(8) 0.125(9) -0.024(7) -0.047(8) -0.047(8) C5' 0.178(10) 0.119(8) 0.126(9) -0.016(7) -0.048(8) -0.038(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.930(4) . ? Zn1 O4 1.943(4) 1_645 ? Zn1 N2 2.016(6) . ? Zn1 O1W 2.085(5) . ? O2 C13 1.269(8) . ? O4 C14 1.308(7) . ? O4 Zn1 1.943(4) 1_465 ? N1 C16 1.331(9) . ? N1 C3 1.419(8) . ? N1 H1A 0.80(7) . ? O3 C14 1.225(7) . ? O1 C13 1.235(8) . ? C13 C1 1.508(9) . ? N2 C21 1.340(9) . ? N2 C17 1.345(8) . ? C17 C18 1.349(9) . ? C17 H17A 0.9300 . ? C20 C21 1.384(10) . ? C20 C19 1.389(10) . ? C20 H20A 0.9300 . ? C16 O7 1.239(8) . ? C16 C10 1.474(13) . ? C16 C10' 1.533(13) . ? C2 C1 1.368(9) . ? C2 C3 1.402(9) . ? C2 H2A 0.9300 . ? C6 C5 1.381(8) . ? C6 C1 1.383(9) . ? C6 H6A 0.9300 . ? C14 C5 1.497(8) . ? C5 C4 1.387(8) . ? C23 C22 1.355(10) . ? C23 C24 1.387(12) . ? C23 H23A 0.9300 . ? C4 C3 1.373(8) . ? C4 H4A 0.9300 . ? C18 C19 1.377(9) . ? C18 H18A 0.9300 . ? C19 C22 1.495(10) . ? C22 C26 1.368(11) . ? C21 H21A 0.9300 . ? O6 C15 1.247(10) . ? O6 H6B 0.8200 . ? N3 C24 1.288(11) . ? N3 C25 1.305(12) . ? C26 C25 1.376(12) . ? C26 H26A 0.9300 . ? O5 C15 1.27(4) . ? O5' C15 1.20(5) . ? C25 H25A 0.9300 . ? C24 H24A 0.9300 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 C15 1.543(14) . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C7' C8' 1.3900 . ? C7' C12' 1.3900 . ? C7' C15 1.487(14) . ? C8' C9' 1.3900 . ? C8' H8'A 0.9300 . ? C9' C10' 1.3900 . ? C9' H9'A 0.9300 . ? C10' C11' 1.3900 . ? C11' C12' 1.3900 . ? C11' H11B 0.9300 . ? C12' H12B 0.9300 . ? N01 C01 1.3900 . ? N01 C05 1.3900 . ? C01 C02 1.3900 . ? C01 H01A 0.9300 . ? C02 C03 1.3900 . ? C02 H02A 0.9300 . ? C03 C04 1.3900 . ? C03 C03 1.65(4) 2_645 ? C04 C05 1.3900 . ? C04 H04A 0.9300 . ? C05 H05A 0.9300 . ? N1' C1' 1.3900 . ? N1' C5' 1.3900 . ? C1' C2' 1.3900 . ? C1' H1'A 0.9300 . ? C2' C3' 1.3900 . ? C2' H2'A 0.9300 . ? C3' C4' 1.3900 . ? C3' C3' 1.48(4) 2_645 ? C4' C5' 1.3900 . ? C4' H4'A 0.9300 . ? C5' H5'A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O4 122.92(19) . 1_645 ? O2 Zn1 N2 101.2(2) . . ? O4 Zn1 N2 129.8(2) 1_645 . ? O2 Zn1 O1W 98.68(18) . . ? O4 Zn1 O1W 97.84(19) 1_645 . ? N2 Zn1 O1W 97.8(2) . . ? C13 O2 Zn1 118.5(4) . . ? C14 O4 Zn1 114.6(4) . 1_465 ? C16 N1 C3 126.8(6) . . ? C16 N1 H1A 125(5) . . ? C3 N1 H1A 108(5) . . ? O1 C13 O2 123.5(6) . . ? O1 C13 C1 119.9(7) . . ? O2 C13 C1 116.6(6) . . ? C21 N2 C17 116.3(6) . . ? C21 N2 Zn1 122.8(5) . . ? C17 N2 Zn1 120.9(5) . . ? N2 C17 C18 123.3(7) . . ? N2 C17 H17A 118.4 . . ? C18 C17 H17A 118.4 . . ? C21 C20 C19 118.8(7) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? O7 C16 N1 122.1(7) . . ? O7 C16 C10 120.8(8) . . ? N1 C16 C10 117.0(8) . . ? O7 C16 C10' 120.2(9) . . ? N1 C16 C10' 117.7(9) . . ? C10 C16 C10' 1.6(10) . . ? C1 C2 C3 121.4(6) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C5 C6 C1 120.1(6) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? O3 C14 O4 122.9(6) . . ? O3 C14 C5 121.9(6) . . ? O4 C14 C5 115.1(6) . . ? C6 C5 C4 119.8(6) . . ? C6 C5 C14 119.0(6) . . ? C4 C5 C14 121.1(5) . . ? C22 C23 C24 120.9(9) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C3 C4 C5 120.9(6) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C3 C2 118.1(6) . . ? C4 C3 N1 124.8(6) . . ? C2 C3 N1 117.1(6) . . ? C2 C1 C6 119.5(6) . . ? C2 C1 C13 120.2(6) . . ? C6 C1 C13 120.2(6) . . ? C17 C18 C19 121.0(6) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 117.0(6) . . ? C18 C19 C22 122.1(6) . . ? C20 C19 C22 120.9(7) . . ? C23 C22 C26 115.2(7) . . ? C23 C22 C19 123.7(7) . . ? C26 C22 C19 121.0(7) . . ? N2 C21 C20 123.6(7) . . ? N2 C21 H21A 118.2 . . ? C20 C21 H21A 118.2 . . ? C15 O6 H6B 109.5 . . ? C24 N3 C25 116.4(8) . . ? C22 C26 C25 119.8(9) . . ? C22 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? N3 C25 C26 124.2(10) . . ? N3 C25 H25A 117.9 . . ? C26 C25 H25A 117.9 . . ? N3 C24 C23 123.3(9) . . ? N3 C24 H24A 118.3 . . ? C23 C24 H24A 118.3 . . ? C8 C7 C12 120.0 . . ? C8 C7 C15 123.5(11) . . ? C12 C7 C15 116.5(11) . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 C16 124.5(10) . . ? C9 C10 C16 115.5(10) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? C8' C7' C12' 120.0 . . ? C8' C7' C15 118.1(11) . . ? C12' C7' C15 121.5(12) . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8'A 120.0 . . ? C9' C8' H8'A 120.0 . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9'A 120.0 . . ? C8' C9' H9'A 120.0 . . ? C9' C10' C11' 120.0 . . ? C9' C10' C16 119.2(11) . . ? C11' C10' C16 120.8(11) . . ? C12' C11' C10' 120.0 . . ? C12' C11' H11B 120.0 . . ? C10' C11' H11B 120.0 . . ? C11' C12' C7' 120.0 . . ? C11' C12' H12B 120.0 . . ? C7' C12' H12B 120.0 . . ? O5' C15 O6 127(3) . . ? O5' C15 O5 35(3) . . ? O6 C15 O5 120(2) . . ? O5' C15 C7' 120(2) . . ? O6 C15 C7' 111.4(10) . . ? O5 C15 C7' 124(2) . . ? O5' C15 C7 114(2) . . ? O6 C15 C7 115.6(10) . . ? O5 C15 C7 122(2) . . ? C7' C15 C7 6.6(10) . . ? C01 N01 C05 120.0 . . ? N01 C01 C02 120.0 . . ? N01 C01 H01A 120.0 . . ? C02 C01 H01A 120.0 . . ? C03 C02 C01 120.0 . . ? C03 C02 H02A 120.0 . . ? C01 C02 H02A 120.0 . . ? C02 C03 C04 120.0 . . ? C02 C03 C03 113(3) . 2_645 ? C04 C03 C03 127(3) . 2_645 ? C03 C04 C05 120.0 . . ? C03 C04 H04A 120.0 . . ? C05 C04 H04A 120.0 . . ? C04 C05 N01 120.0 . . ? C04 C05 H05A 120.0 . . ? N01 C05 H05A 120.0 . . ? C1' N1' C5' 120.0 . . ? C2' C1' N1' 120.0 . . ? C2' C1' H1'A 120.0 . . ? N1' C1' H1'A 120.0 . . ? C1' C2' C3' 120.0 . . ? C1' C2' H2'A 120.0 . . ? C3' C2' H2'A 120.0 . . ? C2' C3' C4' 120.0 . . ? C2' C3' C3' 129(3) . 2_645 ? C4' C3' C3' 109(3) . 2_645 ? C5' C4' C3' 120.0 . . ? C5' C4' H4'A 120.0 . . ? C3' C4' H4'A 120.0 . . ? C4' C5' N1' 120.0 . . ? C4' C5' H5'A 120.0 . . ? N1' C5' H5'A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.709 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 935237'