Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Lindoy, Leonard F.' 'Fenton, Ronald R.' 'Gauci, Robert' 'Junk, Peter C.' 'Luckay, Robert C.' 'Meehan, George V.' 'Price, Jason R.' 'Turner, Peter' 'Wei, Gang' _publ_contact_author_name 'Prof Leonard F Lindoy' _publ_contact_author_address ; School of Chemistry University of Sydney F11 Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email 'LINDOY@CHEM.USYD.EDU.AU' _publ_section_title ; Macrocyclic ligand design. Structure-function relationships involving the interaction of pyridinyl-containing, mixed oxygen-nitrogen donor macrocycles with cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II), silver(I) and lead(II) ; data_lfl18 _database_code_CSD 178685 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.20 H42 N6 O9.80 Zn' _chemical_formula_weight 699.26 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 tetragonal _symmetry_space_group_name_H-M 'I -4 ' _symmetry_Int_Tables_number 82 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 27.980(9) _cell_length_b 27.980(9) _cell_length_c 8.878(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6950(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 2.813 _cell_measurement_theta_max 28.166 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.369 _exptl_crystal_size_mid 0.222 _exptl_crystal_size_min 0.202 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2941 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) and SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 402 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.002 _diffrn_reflns_number 31347 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.26 _reflns_number_total 8146 _reflns_number_gt 7680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997), xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). ; _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^)+(0.0600P)^2^+3.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(9) _refine_ls_number_reflns 8145 _refine_ls_number_parameters 402 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.399088(9) 0.125128(9) 0.32426(3) 0.02795(8) Uani 1 1 d . . . O1 O 0.25702(6) 0.19754(7) 0.4631(2) 0.0396(4) Uani 1 1 d . . . O2 O 0.42802(6) 0.25482(6) 0.6237(2) 0.0368(4) Uani 1 1 d . . . O3 O 0.46123(6) 0.09977(7) 0.1777(2) 0.0379(4) Uani 1 1 d . . . O4 O 0.38975(6) 0.08113(7) 0.1090(2) 0.0388(4) Uani 1 1 d . . . O5 O 0.44935(8) 0.06799(7) -0.0433(2) 0.0428(4) Uani 1 1 d . . . O6 O 0.40255(9) 0.18087(7) 0.1732(3) 0.0535(5) Uani 1 1 d . . . O7 O 0.38879(14) 0.25413(10) 0.1155(4) 0.0876(10) Uani 1 1 d . . . O8 O 0.36358(9) 0.22416(9) 0.3268(3) 0.0652(6) Uani 1 1 d . . . O9 O 0.34129(7) 0.17028(7) 0.6966(2) 0.0409(4) Uani 1 1 d . . . H9O H 0.3407 0.1983 0.6627 0.061 Uiso 1 1 calc R . . O10 O 0.4775(2) 0.3838(2) 0.5577(7) 0.1091(15) Uiso 0.80 1 d P . . N1 N 0.43644(7) 0.15678(7) 0.5060(2) 0.0286(4) Uani 1 1 d . . . H1N H 0.4149 0.1770 0.5540 0.034 Uiso 1 1 calc R . . N2 N 0.40996(7) 0.06120(7) 0.4506(2) 0.0296(4) Uani 1 1 d . . . H2N H 0.4165 0.0361 0.3851 0.036 Uiso 1 1 calc R . . N3 N 0.32690(7) 0.11525(7) 0.3824(2) 0.0319(4) Uani 1 1 d . . . H3N H 0.3214 0.1328 0.4695 0.038 Uiso 1 1 calc R . . N4 N 0.32001(8) 0.26674(7) 0.6230(3) 0.0342(4) Uani 1 1 d . . . N5 N 0.43363(8) 0.08230(7) 0.0773(2) 0.0312(4) Uani 1 1 d . . . N6 N 0.38402(10) 0.21996(10) 0.2072(3) 0.0537(7) Uani 1 1 d . . . C1 C 0.44939(10) 0.11942(9) 0.6173(3) 0.0385(5) Uani 1 1 d . . . H1A H 0.4253 0.1191 0.6990 0.046 Uiso 1 1 calc R . . H1B H 0.4807 0.1273 0.6625 0.046 Uiso 1 1 calc R . . C2 C 0.45203(9) 0.07032(9) 0.5466(3) 0.0376(6) Uani 1 1 d . . . H2A H 0.4815 0.0678 0.4852 0.045 Uiso 1 1 calc R . . H2B H 0.4537 0.0458 0.6269 0.045 Uiso 1 1 calc R . . C3 C 0.36478(9) 0.05160(9) 0.5307(3) 0.0342(5) Uani 1 1 d . . . H3A H 0.3628 0.0714 0.6229 0.041 Uiso 1 1 calc R . . H3B H 0.3630 0.0175 0.5601 0.041 Uiso 1 1 calc R . . C4 C 0.32394(9) 0.06392(9) 0.4241(3) 0.0331(5) Uani 1 1 d . . . H4A H 0.3260 0.0439 0.3324 0.040 Uiso 1 1 calc R . . H4B H 0.2929 0.0574 0.4737 0.040 Uiso 1 1 calc R . . C5 C 0.28986(9) 0.12967(10) 0.2707(3) 0.0369(5) Uani 1 1 d . . . H5A H 0.2921 0.1085 0.1816 0.044 Uiso 1 1 calc R . . H5B H 0.2964 0.1628 0.2369 0.044 Uiso 1 1 calc R . . C6 C 0.23978(9) 0.12723(9) 0.3333(3) 0.0370(5) Uani 1 1 d . . . C7 C 0.20830(11) 0.09013(11) 0.2948(4) 0.0495(7) Uani 1 1 d . . . H7 H 0.2183 0.0659 0.2267 0.059 Uiso 1 1 calc R . . C8 C 0.16236(11) 0.08857(12) 0.3562(5) 0.0560(9) Uani 1 1 d . . . H8 H 0.1409 0.0638 0.3282 0.067 Uiso 1 1 calc R . . C9 C 0.14826(10) 0.12302(11) 0.4570(4) 0.0490(7) Uani 1 1 d . . . H9 H 0.1171 0.1214 0.4995 0.059 Uiso 1 1 calc R . . C10 C 0.17855(9) 0.16034(10) 0.4985(4) 0.0410(6) Uani 1 1 d . . . H10 H 0.1684 0.1839 0.5686 0.049 Uiso 1 1 calc R . . C11 C 0.22442(9) 0.16228(9) 0.4341(3) 0.0360(5) Uani 1 1 d . . . C12 C 0.24156(9) 0.23793(9) 0.5498(4) 0.0388(6) Uani 1 1 d . . . H12A H 0.2362 0.2285 0.6559 0.047 Uiso 1 1 calc R . . H12B H 0.2113 0.2508 0.5086 0.047 Uiso 1 1 calc R . . C13 C 0.28043(9) 0.27486(9) 0.5403(3) 0.0345(5) Uani 1 1 d . . . C14 C 0.27486(10) 0.31492(10) 0.4497(4) 0.0414(6) Uani 1 1 d . . . H14 H 0.2462 0.3199 0.3946 0.050 Uiso 1 1 calc R . . C15 C 0.31226(11) 0.34762(11) 0.4414(4) 0.0496(7) Uani 1 1 d . . . H15 H 0.3098 0.3750 0.3787 0.059 Uiso 1 1 calc R . . C16 C 0.35302(10) 0.33975(10) 0.5254(4) 0.0447(6) Uani 1 1 d . . . H16 H 0.3788 0.3619 0.5226 0.054 Uiso 1 1 calc R . . C17 C 0.35582(9) 0.29885(9) 0.6144(3) 0.0362(5) Uani 1 1 d . . . C18 C 0.39989(9) 0.28960(9) 0.7052(3) 0.0390(6) Uani 1 1 d . . . H18A H 0.4183 0.3195 0.7186 0.047 Uiso 1 1 calc R . . H18B H 0.3912 0.2771 0.8059 0.047 Uiso 1 1 calc R . . C19 C 0.47485(8) 0.24907(8) 0.6659(3) 0.0308(4) Uani 1 1 d . . . C20 C 0.49727(9) 0.27516(9) 0.7795(3) 0.0365(5) Uani 1 1 d . . . H20 H 0.4797 0.2979 0.8364 0.044 Uiso 1 1 calc R . . C21 C 0.54570(9) 0.26766(9) 0.8090(3) 0.0372(5) Uani 1 1 d . . . H21 H 0.5612 0.2859 0.8849 0.045 Uiso 1 1 calc R . . C22 C 0.57146(9) 0.23389(9) 0.7288(3) 0.0342(5) Uani 1 1 d . . . H22 H 0.6043 0.2287 0.7501 0.041 Uiso 1 1 calc R . . C23 C 0.54855(8) 0.20763(9) 0.6162(3) 0.0318(5) Uani 1 1 d . . . H23 H 0.5661 0.1842 0.5619 0.038 Uiso 1 1 calc R . . C24 C 0.50062(8) 0.21495(8) 0.5819(3) 0.0278(4) Uani 1 1 d . . . C25 C 0.47683(8) 0.18702(9) 0.4571(3) 0.0304(5) Uani 1 1 d . . . H25A H 0.4651 0.2098 0.3801 0.036 Uiso 1 1 calc R . . H25B H 0.5011 0.1664 0.4085 0.036 Uiso 1 1 calc R . . C26 C 0.36066(11) 0.17059(12) 0.8450(3) 0.0466(7) Uani 1 1 d . . . H26A H 0.3920 0.1862 0.8438 0.070 Uiso 1 1 calc R . . H26B H 0.3641 0.1377 0.8810 0.070 Uiso 1 1 calc R . . H26C H 0.3391 0.1881 0.9123 0.070 Uiso 1 1 calc R . . C27 C 0.5117(4) 0.4037(4) 0.6598(12) 0.135(3) Uiso 0.80 1 d PD . . H27A H 0.5304 0.4293 0.6100 0.162 Uiso 0.80 1 calc PR . . H27B H 0.5341 0.3787 0.6957 0.162 Uiso 0.80 1 calc PR . . C28 C 0.4819(5) 0.4245(5) 0.7948(17) 0.198(6) Uiso 0.80 1 d PD . . H28A H 0.5015 0.4243 0.8864 0.297 Uiso 0.80 1 calc PR . . H28B H 0.4533 0.4049 0.8105 0.297 Uiso 0.80 1 calc PR . . H28C H 0.4723 0.4574 0.7716 0.297 Uiso 0.80 1 calc PR . . C29 C 0.4998(4) 0.3582(4) 0.4362(13) 0.153(4) Uiso 0.80 1 d PD . . H29A H 0.5180 0.3311 0.4789 0.183 Uiso 0.80 1 calc PR . . H29B H 0.5229 0.3797 0.3861 0.183 Uiso 0.80 1 calc PR . . C30 C 0.4627(4) 0.3374(4) 0.3087(13) 0.140(3) Uiso 0.80 1 d PD . . H30A H 0.4318 0.3305 0.3558 0.209 Uiso 0.80 1 calc PR . . H30B H 0.4758 0.3080 0.2651 0.209 Uiso 0.80 1 calc PR . . H30C H 0.4584 0.3613 0.2291 0.209 Uiso 0.80 1 calc PR . . 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 0.02908(14) 0.02809(13) 0.02668(12) -0.00245(10) -0.00376(10) 0.00231(10) O1 0.0284(8) 0.0353(9) 0.0550(12) -0.0075(8) -0.0028(8) 0.0040(7) O2 0.0287(8) 0.0320(8) 0.0497(10) -0.0123(8) -0.0080(7) 0.0082(7) O3 0.0322(8) 0.0481(10) 0.0335(9) -0.0074(9) 0.0000(8) -0.0091(7) O4 0.0279(8) 0.0501(11) 0.0383(9) -0.0001(8) 0.0001(7) -0.0057(7) O5 0.0528(11) 0.0426(10) 0.0330(10) -0.0090(8) 0.0080(8) -0.0078(9) O6 0.0758(15) 0.0390(10) 0.0457(11) 0.0051(10) -0.0120(12) 0.0046(9) O7 0.133(3) 0.0493(14) 0.081(2) 0.0228(14) -0.0107(19) 0.0189(16) O8 0.0651(15) 0.0592(13) 0.0713(17) -0.0145(14) 0.0073(14) 0.0118(11) O9 0.0522(11) 0.0327(9) 0.0378(10) 0.0018(8) -0.0107(8) 0.0020(8) N1 0.0282(9) 0.0305(9) 0.0270(10) -0.0027(8) -0.0018(7) 0.0030(7) N2 0.0279(9) 0.0279(9) 0.0330(10) -0.0027(8) -0.0020(8) 0.0036(7) N3 0.0305(10) 0.0337(10) 0.0316(10) -0.0065(8) -0.0051(8) 0.0057(8) N4 0.0324(10) 0.0297(10) 0.0405(11) -0.0042(8) -0.0018(9) 0.0083(8) N5 0.0348(10) 0.0274(9) 0.0313(10) -0.0007(8) 0.0040(8) -0.0018(8) N6 0.0578(16) 0.0532(15) 0.0500(16) -0.0043(12) -0.0193(13) 0.0113(12) C1 0.0464(14) 0.0351(13) 0.0338(12) 0.0045(10) -0.0099(11) -0.0041(11) C2 0.0348(12) 0.0353(13) 0.0426(14) 0.0023(11) -0.0098(11) 0.0012(10) C3 0.0332(12) 0.0357(12) 0.0338(12) 0.0022(10) 0.0044(10) 0.0035(10) C4 0.0295(11) 0.0333(12) 0.0366(13) -0.0026(9) 0.0043(9) 0.0012(9) C5 0.0346(12) 0.0430(14) 0.0332(12) -0.0042(10) -0.0080(10) 0.0058(10) C6 0.0295(11) 0.0399(12) 0.0415(14) 0.0020(12) -0.0113(11) 0.0038(9) C7 0.0407(14) 0.0457(15) 0.062(2) -0.0030(14) -0.0170(13) -0.0007(12) C8 0.0375(14) 0.0494(17) 0.081(3) 0.0069(16) -0.0189(15) -0.0098(12) C9 0.0280(12) 0.0485(16) 0.071(2) 0.0158(15) -0.0086(13) -0.0001(11) C10 0.0305(12) 0.0393(14) 0.0533(17) 0.0093(12) -0.0036(11) 0.0063(10) C11 0.0261(11) 0.0366(13) 0.0452(14) 0.0041(10) -0.0102(10) 0.0037(9) C12 0.0312(12) 0.0346(13) 0.0506(16) -0.0022(11) 0.0003(11) 0.0080(10) C13 0.0305(11) 0.0336(12) 0.0395(13) -0.0031(10) 0.0016(10) 0.0085(9) C14 0.0333(13) 0.0382(13) 0.0527(16) 0.0031(12) -0.0033(11) 0.0097(10) C15 0.0394(15) 0.0377(14) 0.072(2) 0.0138(14) -0.0011(14) 0.0073(11) C16 0.0350(13) 0.0313(13) 0.0678(19) 0.0031(13) -0.0001(13) 0.0050(10) C17 0.0315(12) 0.0311(12) 0.0460(14) -0.0081(10) -0.0011(10) 0.0081(9) C18 0.0329(12) 0.0335(12) 0.0507(16) -0.0124(11) -0.0041(11) 0.0092(9) C19 0.0285(10) 0.0275(10) 0.0363(12) -0.0001(10) -0.0035(10) 0.0014(8) C20 0.0371(13) 0.0307(12) 0.0417(14) -0.0054(10) -0.0066(10) 0.0017(10) C21 0.0397(13) 0.0299(11) 0.0420(14) 0.0004(10) -0.0106(11) -0.0068(9) C22 0.0258(11) 0.0347(12) 0.0422(13) 0.0080(10) -0.0033(9) -0.0057(9) C23 0.0252(10) 0.0348(12) 0.0355(12) 0.0040(10) 0.0027(9) 0.0003(9) C24 0.0274(10) 0.0274(10) 0.0286(11) 0.0006(8) 0.0001(8) 0.0009(8) C25 0.0306(11) 0.0326(11) 0.0281(11) -0.0019(9) 0.0015(9) 0.0004(9) C26 0.0436(14) 0.0583(17) 0.0380(15) 0.0010(13) -0.0023(12) 0.0076(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 2.059(2) . ? Zn1 N3 2.103(2) . ? Zn1 N1 2.117(2) . ? Zn1 N2 2.133(2) . ? Zn1 O3 2.284(2) . ? Zn1 O4 2.288(2) . ? O1 C11 1.368(3) . ? O1 C12 1.434(3) . ? O2 C19 1.372(3) . ? O2 C18 1.446(3) . ? O3 N5 1.277(3) . ? O4 N5 1.260(3) . ? O5 N5 1.225(3) . ? O6 N6 1.248(3) . ? O7 N6 1.263(4) . ? O8 N6 1.212(4) . ? O9 C26 1.425(4) . ? O9 H9O 0.8400 . ? O10 C27 1.432(11) . ? O10 C29 1.437(12) . ? N1 C25 1.477(3) . ? N1 C1 1.483(3) . ? N1 H1N 0.9300 . ? N2 C3 1.475(3) . ? N2 C2 1.476(3) . ? N2 H2N 0.9300 . ? N3 C4 1.485(3) . ? N3 C5 1.490(3) . ? N3 H3N 0.9300 . ? N4 C17 1.348(4) . ? N4 C13 1.348(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.523(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.396(4) . ? C6 C7 1.404(4) . ? C7 C8 1.397(5) . ? C7 H7 0.9500 . ? C8 C9 1.373(5) . ? C8 H8 0.9500 . ? C9 C10 1.394(4) . ? C9 H9 0.9500 . ? C10 C11 1.406(4) . ? C10 H10 0.9500 . ? C12 C13 1.503(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.389(4) . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C15 H15 0.9500 . ? C16 C17 1.393(4) . ? C16 H16 0.9500 . ? C17 C18 1.496(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.394(3) . ? C19 C24 1.410(3) . ? C20 C21 1.396(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.396(4) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 C25 1.511(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.573(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.642(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 N3 107.73(9) . . ? O6 Zn1 N1 99.01(9) . . ? N3 Zn1 N1 110.01(8) . . ? O6 Zn1 N2 166.13(9) . . ? N3 Zn1 N2 84.13(8) . . ? N1 Zn1 N2 83.08(8) . . ? O6 Zn1 O3 80.13(9) . . ? N3 Zn1 O3 146.09(7) . . ? N1 Zn1 O3 100.85(7) . . ? N2 Zn1 O3 86.01(8) . . ? O6 Zn1 O4 82.46(9) . . ? N3 Zn1 O4 91.40(7) . . ? N1 Zn1 O4 156.66(7) . . ? N2 Zn1 O4 90.24(8) . . ? O3 Zn1 O4 56.24(7) . . ? C11 O1 C12 117.9(2) . . ? C19 O2 C18 117.51(19) . . ? N5 O3 Zn1 93.22(13) . . ? N5 O4 Zn1 93.49(14) . . ? N6 O6 Zn1 119.1(2) . . ? C26 O9 H9O 109.5 . . ? C27 O10 C29 112.2(7) . . ? C25 N1 C1 114.39(19) . . ? C25 N1 Zn1 113.13(15) . . ? C1 N1 Zn1 109.48(15) . . ? C25 N1 H1N 106.4 . . ? C1 N1 H1N 106.4 . . ? Zn1 N1 H1N 106.4 . . ? C3 N2 C2 115.9(2) . . ? C3 N2 Zn1 106.51(14) . . ? C2 N2 Zn1 105.82(15) . . ? C3 N2 H2N 109.5 . . ? C2 N2 H2N 109.5 . . ? Zn1 N2 H2N 109.5 . . ? C4 N3 C5 112.9(2) . . ? C4 N3 Zn1 103.99(14) . . ? C5 N3 Zn1 117.98(17) . . ? C4 N3 H3N 107.1 . . ? C5 N3 H3N 107.1 . . ? Zn1 N3 H3N 107.1 . . ? C17 N4 C13 117.9(2) . . ? O5 N5 O4 122.4(2) . . ? O5 N5 O3 121.2(2) . . ? O4 N5 O3 116.3(2) . . ? O8 N6 O6 119.6(3) . . ? O8 N6 O7 122.8(3) . . ? O6 N6 O7 117.6(3) . . ? N1 C1 C2 112.1(2) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 111.0(2) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 107.6(2) . . ? N2 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? N2 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? N3 C4 C3 109.4(2) . . ? N3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 112.8(2) . . ? N3 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N3 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C11 C6 C7 118.9(3) . . ? C11 C6 C5 119.4(2) . . ? C7 C6 C5 121.8(3) . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? O1 C11 C6 115.0(2) . . ? O1 C11 C10 124.1(3) . . ? C6 C11 C10 121.0(3) . . ? O1 C12 C13 107.1(2) . . ? O1 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? O1 C12 H12B 110.3 . . ? C13 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? N4 C13 C14 122.9(2) . . ? N4 C13 C12 116.6(2) . . ? C14 C13 C12 120.4(2) . . ? C13 C14 C15 118.5(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 119.0(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N4 C17 C16 122.6(2) . . ? N4 C17 C18 117.8(2) . . ? C16 C17 C18 119.6(2) . . ? O2 C18 C17 107.2(2) . . ? O2 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? O2 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? O2 C19 C20 124.5(2) . . ? O2 C19 C24 115.0(2) . . ? C20 C19 C24 120.5(2) . . ? C19 C20 C21 119.6(2) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.7(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.2(2) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 121.5(2) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 118.5(2) . . ? C23 C24 C25 120.6(2) . . ? C19 C24 C25 120.9(2) . . ? N1 C25 C24 114.7(2) . . ? N1 C25 H25A 108.6 . . ? C24 C25 H25A 108.6 . . ? N1 C25 H25B 108.6 . . ? C24 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? O9 C26 H26A 109.5 . . ? O9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O10 C27 C28 105.8(9) . . ? O10 C27 H27A 110.6 . . ? C28 C27 H27A 110.6 . . ? O10 C27 H27B 110.6 . . ? C28 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O10 C29 C30 114.8(9) . . ? O10 C29 H29A 108.6 . . ? C30 C29 H29A 108.6 . . ? O10 C29 H29B 108.6 . . ? C30 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 O6 Zn1 O3 N5 -82.59(15) . . . . ? N3 Zn1 O3 N5 24.6(2) . . . . ? N1 Zn1 O3 N5 -179.97(14) . . . . ? N2 Zn1 O3 N5 97.86(15) . . . . ? O4 Zn1 O3 N5 4.89(13) . . . . ? O6 Zn1 O4 N5 78.17(15) . . . . ? N3 Zn1 O4 N5 -174.13(15) . . . . ? N1 Zn1 O4 N5 -17.1(3) . . . . ? N2 Zn1 O4 N5 -90.00(14) . . . . ? O3 Zn1 O4 N5 -4.96(13) . . . . ? N3 Zn1 O6 N6 53.8(2) . . . . ? N1 Zn1 O6 N6 -60.7(2) . . . . ? N2 Zn1 O6 N6 -158.4(3) . . . . ? O3 Zn1 O6 N6 -160.2(2) . . . . ? O4 Zn1 O6 N6 142.8(2) . . . . ? O6 Zn1 N1 C25 -37.24(17) . . . . ? N3 Zn1 N1 C25 -149.94(15) . . . . ? N2 Zn1 N1 C25 128.91(16) . . . . ? O3 Zn1 N1 C25 44.34(16) . . . . ? O4 Zn1 N1 C25 54.6(3) . . . . ? O6 Zn1 N1 C1 -166.10(17) . . . . ? N3 Zn1 N1 C1 81.20(17) . . . . ? N2 Zn1 N1 C1 0.05(16) . . . . ? O3 Zn1 N1 C1 -84.52(17) . . . . ? O4 Zn1 N1 C1 -74.3(3) . . . . ? O6 Zn1 N2 C3 -160.4(3) . . . . ? N3 Zn1 N2 C3 -11.00(16) . . . . ? N1 Zn1 N2 C3 100.04(16) . . . . ? O3 Zn1 N2 C3 -158.51(15) . . . . ? O4 Zn1 N2 C3 -102.38(15) . . . . ? O6 Zn1 N2 C2 75.8(4) . . . . ? N3 Zn1 N2 C2 -134.85(16) . . . . ? N1 Zn1 N2 C2 -23.81(16) . . . . ? O3 Zn1 N2 C2 77.64(16) . . . . ? O4 Zn1 N2 C2 133.77(16) . . . . ? O6 Zn1 N3 C4 153.01(15) . . . . ? N1 Zn1 N3 C4 -100.05(16) . . . . ? N2 Zn1 N3 C4 -19.62(15) . . . . ? O3 Zn1 N3 C4 54.2(2) . . . . ? O4 Zn1 N3 C4 70.48(15) . . . . ? O6 Zn1 N3 C5 27.11(19) . . . . ? N1 Zn1 N3 C5 134.05(17) . . . . ? N2 Zn1 N3 C5 -145.52(18) . . . . ? O3 Zn1 N3 C5 -71.7(2) . . . . ? O4 Zn1 N3 C5 -55.42(18) . . . . ? Zn1 O4 N5 O5 -171.1(2) . . . . ? Zn1 O4 N5 O3 8.3(2) . . . . ? Zn1 O3 N5 O5 171.1(2) . . . . ? Zn1 O3 N5 O4 -8.3(2) . . . . ? Zn1 O6 N6 O8 -1.4(4) . . . . ? Zn1 O6 N6 O7 176.5(2) . . . . ? C25 N1 C1 C2 -104.1(2) . . . . ? Zn1 N1 C1 C2 24.1(3) . . . . ? C3 N2 C2 C1 -73.9(3) . . . . ? Zn1 N2 C2 C1 43.8(3) . . . . ? N1 C1 C2 N2 -46.8(3) . . . . ? C2 N2 C3 C4 156.5(2) . . . . ? Zn1 N2 C3 C4 39.1(2) . . . . ? C5 N3 C4 C3 176.5(2) . . . . ? Zn1 N3 C4 C3 47.5(2) . . . . ? N2 C3 C4 N3 -60.4(2) . . . . ? C4 N3 C5 C6 66.5(3) . . . . ? Zn1 N3 C5 C6 -172.07(16) . . . . ? N3 C5 C6 C11 74.6(3) . . . . ? N3 C5 C6 C7 -104.3(3) . . . . ? C11 C6 C7 C8 0.3(4) . . . . ? C5 C6 C7 C8 179.2(3) . . . . ? C6 C7 C8 C9 -1.3(5) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C12 O1 C11 C6 172.0(2) . . . . ? C12 O1 C11 C10 -7.8(4) . . . . ? C7 C6 C11 O1 -178.8(3) . . . . ? C5 C6 C11 O1 2.2(4) . . . . ? C7 C6 C11 C10 1.0(4) . . . . ? C5 C6 C11 C10 -178.0(2) . . . . ? C9 C10 C11 O1 178.6(3) . . . . ? C9 C10 C11 C6 -1.3(4) . . . . ? C11 O1 C12 C13 -169.5(2) . . . . ? C17 N4 C13 C14 -1.1(4) . . . . ? C17 N4 C13 C12 178.8(2) . . . . ? O1 C12 C13 N4 -75.1(3) . . . . ? O1 C12 C13 C14 104.8(3) . . . . ? N4 C13 C14 C15 1.5(4) . . . . ? C12 C13 C14 C15 -178.4(3) . . . . ? C13 C14 C15 C16 -1.3(5) . . . . ? C14 C15 C16 C17 1.0(5) . . . . ? C13 N4 C17 C16 0.7(4) . . . . ? C13 N4 C17 C18 -179.5(2) . . . . ? C15 C16 C17 N4 -0.7(4) . . . . ? C15 C16 C17 C18 179.5(3) . . . . ? C19 O2 C18 C17 164.9(2) . . . . ? N4 C17 C18 O2 79.5(3) . . . . ? C16 C17 C18 O2 -100.6(3) . . . . ? C18 O2 C19 C20 -1.5(4) . . . . ? C18 O2 C19 C24 -179.6(2) . . . . ? O2 C19 C20 C21 -177.4(3) . . . . ? C24 C19 C20 C21 0.6(4) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? C22 C23 C24 C19 -1.4(4) . . . . ? C22 C23 C24 C25 178.5(2) . . . . ? O2 C19 C24 C23 178.9(2) . . . . ? C20 C19 C24 C23 0.7(4) . . . . ? O2 C19 C24 C25 -0.9(3) . . . . ? C20 C19 C24 C25 -179.1(2) . . . . ? C1 N1 C25 C24 -60.8(3) . . . . ? Zn1 N1 C25 C24 172.93(15) . . . . ? C23 C24 C25 N1 118.8(2) . . . . ? C19 C24 C25 N1 -61.4(3) . . . . ? C29 O10 C27 C28 -173.1(9) . . . . ? C27 O10 C29 C30 -176.2(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9O N4 0.84 2.03 2.840(3) 161.3 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.728 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.074 #===END data_lfl23 _database_code_CSD 178686 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 Co N6 O11' _chemical_formula_weight 697.61 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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.850(3) _cell_length_b 13.422(3) _cell_length_c 11.066(3) _cell_angle_alpha 112.555(4) _cell_angle_beta 86.932(4) _cell_angle_gamma 101.417(4) _cell_volume 1592.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 963 _cell_measurement_theta_min 2.522 _cell_measurement_theta_max 28.188 _exptl_crystal_description plate _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type 'numerical and empirical' _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ; Gaussian (XPREP, Bruker 1995) and SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 180 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.002 _diffrn_reflns_number 16660 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.26 _reflns_number_total 7351 _reflns_number_gt 6368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _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^)+(0.0476P)^2^+0.5208P] 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 7351 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Co1 Co 0.353073(16) 0.103046(16) 0.223627(17) 0.01730(6) Uani 1 1 d . . . O1 O -0.00500(9) 0.16697(9) 0.42244(11) 0.0249(2) Uani 1 1 d . . . O2 O 0.32864(10) 0.47521(9) 0.36582(11) 0.0271(2) Uani 1 1 d . . . O3 O 0.36899(10) -0.04594(10) 0.23452(11) 0.0248(2) Uani 1 1 d . . . H3O H 0.3392(18) -0.1087(19) 0.185(2) 0.036(6) Uiso 1 1 d . . . O4 O 0.37481(10) 0.18715(9) 0.42823(10) 0.0233(2) Uani 1 1 d . . . H4O H 0.441(2) 0.1990(18) 0.440(2) 0.039(6) Uiso 1 1 d . . . O5 O 0.53935(9) 0.11800(9) 0.20458(10) 0.0228(2) Uani 1 1 d . . . O6 O 0.60546(10) 0.20674(10) 0.40676(11) 0.0322(3) Uani 1 1 d . . . O7 O 0.72080(10) 0.18620(10) 0.24363(12) 0.0320(3) Uani 1 1 d . . . O8 O 0.29185(14) -0.24822(11) 0.06121(13) 0.0457(3) Uani 1 1 d . . . O9 O 0.18153(18) -0.39987(14) 0.05487(17) 0.0725(6) Uani 1 1 d . . . O10 O 0.19960(13) -0.25465(11) 0.23319(13) 0.0449(3) Uani 1 1 d . . . O11 O 0.11334(12) 0.26365(11) 0.19429(13) 0.0372(3) Uani 1 1 d . . . H11O H 0.101(2) 0.300(2) 0.266(2) 0.048(7) Uiso 1 1 d . . . N1 N 0.37574(11) 0.25579(10) 0.18752(12) 0.0201(2) Uani 1 1 d . . . H1N H 0.3189(16) 0.2880(15) 0.2211(18) 0.023(4) Uiso 1 1 d . . . N2 N 0.32326(11) 0.03354(11) 0.01708(12) 0.0203(3) Uani 1 1 d . . . H2N H 0.3448(16) -0.0247(16) -0.0189(17) 0.021(4) Uiso 1 1 d . . . N3 N 0.16963(11) 0.05581(11) 0.22542(12) 0.0192(2) Uani 1 1 d . . . H3N H 0.1401(16) 0.1086(16) 0.2375(17) 0.022(5) Uiso 1 1 d . . . N4 N 0.08726(11) 0.39782(11) 0.45773(13) 0.0230(3) Uani 1 1 d . . . N5 N 0.62310(11) 0.17077(10) 0.28551(12) 0.0223(3) Uani 1 1 d . . . N6 N 0.22156(14) -0.30167(13) 0.11576(15) 0.0365(3) Uani 1 1 d . . . C1 C 0.36566(14) 0.22754(13) 0.04373(15) 0.0255(3) Uani 1 1 d . . . H1A H 0.4205 0.2825 0.0196 0.031 Uiso 1 1 calc R . . H1B H 0.2869 0.2303 0.0213 0.031 Uiso 1 1 calc R . . C2 C 0.39076(13) 0.11375(13) -0.03382(14) 0.0245(3) Uani 1 1 d . . . H2A H 0.3704 0.0915 -0.1274 0.029 Uiso 1 1 calc R . . H2B H 0.4740 0.1149 -0.0267 0.029 Uiso 1 1 calc R . . C3 C 0.19704(13) 0.01329(13) -0.00839(14) 0.0239(3) Uani 1 1 d . . . H3A H 0.1769 -0.0427 -0.0975 0.029 Uiso 1 1 calc R . . H3B H 0.1741 0.0820 -0.0025 0.029 Uiso 1 1 calc R . . C4 C 0.13404(13) -0.02667(13) 0.09227(14) 0.0236(3) Uani 1 1 d . . . H4A H 0.0499 -0.0371 0.0793 0.028 Uiso 1 1 calc R . . H4B H 0.1527 -0.0982 0.0820 0.028 Uiso 1 1 calc R . . C5 C 0.12810(12) 0.01163(13) 0.32820(14) 0.0213(3) Uani 1 1 d . . . H5A H 0.1560 0.0679 0.4149 0.026 Uiso 1 1 calc R . . H5B H 0.1620 -0.0536 0.3138 0.026 Uiso 1 1 calc R . . C6 C -0.00137(13) -0.02033(13) 0.32978(14) 0.0212(3) Uani 1 1 d . . . C7 C -0.05673(14) -0.12993(13) 0.28251(15) 0.0250(3) Uani 1 1 d . . . H7 H -0.0124 -0.1860 0.2482 0.030 Uiso 1 1 calc R . . C8 C -0.17639(15) -0.15878(14) 0.28475(15) 0.0283(3) Uani 1 1 d . . . H8 H -0.2135 -0.2339 0.2511 0.034 Uiso 1 1 calc R . . C9 C -0.24020(14) -0.07678(14) 0.33649(15) 0.0272(3) Uani 1 1 d . . . H9 H -0.3215 -0.0962 0.3402 0.033 Uiso 1 1 calc R . . C10 C -0.18730(13) 0.03426(13) 0.38343(14) 0.0238(3) Uani 1 1 d . . . H10 H -0.2320 0.0901 0.4175 0.029 Uiso 1 1 calc R . . C11 C -0.06802(13) 0.06140(12) 0.37921(14) 0.0211(3) Uani 1 1 d . . . C12 C -0.06589(13) 0.25611(13) 0.48030(16) 0.0257(3) Uani 1 1 d . . . H12A H -0.1182 0.2437 0.5481 0.031 Uiso 1 1 calc R . . H12B H -0.1121 0.2628 0.4128 0.031 Uiso 1 1 calc R . . C13 C 0.02429(13) 0.35840(13) 0.54039(15) 0.0235(3) Uani 1 1 d . . . C14 C 0.04079(14) 0.40780(14) 0.67590(16) 0.0272(3) Uani 1 1 d . . . H14 H -0.0058 0.3784 0.7315 0.033 Uiso 1 1 calc R . . C15 C 0.12635(15) 0.50051(15) 0.72817(16) 0.0314(4) Uani 1 1 d . . . H15 H 0.1403 0.5353 0.8201 0.038 Uiso 1 1 calc R . . C16 C 0.19109(14) 0.54136(14) 0.64337(17) 0.0296(3) Uani 1 1 d . . . H16 H 0.2500 0.6049 0.6767 0.036 Uiso 1 1 calc R . . C17 C 0.16928(13) 0.48879(13) 0.50951(16) 0.0248(3) Uani 1 1 d . . . C18 C 0.23593(14) 0.53407(13) 0.41604(17) 0.0274(3) Uani 1 1 d . . . H18A H 0.1847 0.5248 0.3432 0.033 Uiso 1 1 calc R . . H18B H 0.2673 0.6135 0.4619 0.033 Uiso 1 1 calc R . . C19 C 0.40844(13) 0.51367(12) 0.29033(15) 0.0227(3) Uani 1 1 d . . . C20 C 0.41155(14) 0.61081(13) 0.27088(16) 0.0268(3) Uani 1 1 d . . . H20 H 0.3558 0.6551 0.3092 0.032 Uiso 1 1 calc R . . C21 C 0.49757(15) 0.64214(13) 0.19448(16) 0.0287(3) Uani 1 1 d . . . H21 H 0.4998 0.7081 0.1806 0.034 Uiso 1 1 calc R . . C22 C 0.57980(14) 0.57890(13) 0.13853(15) 0.0264(3) Uani 1 1 d . . . H22 H 0.6391 0.6020 0.0883 0.032 Uiso 1 1 calc R . . C23 C 0.57475(13) 0.48114(13) 0.15652(14) 0.0235(3) Uani 1 1 d . . . H23 H 0.6304 0.4370 0.1170 0.028 Uiso 1 1 calc R . . C24 C 0.48956(13) 0.44681(12) 0.23144(14) 0.0212(3) Uani 1 1 d . . . C25 C 0.48289(13) 0.33814(12) 0.24567(15) 0.0212(3) Uani 1 1 d . . . H25A H 0.5503 0.3065 0.2034 0.025 Uiso 1 1 calc R . . H25B H 0.4878 0.3518 0.3399 0.025 Uiso 1 1 calc R . . C26 C 0.42053(15) -0.05453(14) 0.34297(17) 0.0302(3) Uani 1 1 d . . . H26A H 0.4960 -0.0054 0.3643 0.045 Uiso 1 1 calc R . . H26B H 0.4300 -0.1305 0.3202 0.045 Uiso 1 1 calc R . . H26C H 0.3709 -0.0337 0.4188 0.045 Uiso 1 1 calc R . . C27 C 0.32164(15) 0.27938(13) 0.50324(15) 0.0267(3) Uani 1 1 d . . . H27A H 0.3453 0.3381 0.4699 0.040 Uiso 1 1 calc R . . H27B H 0.3458 0.3066 0.5954 0.040 Uiso 1 1 calc R . . H27C H 0.2377 0.2561 0.4953 0.040 Uiso 1 1 calc R . . C28 C 0.0583(2) 0.2955(2) 0.1072(2) 0.0594(7) Uani 1 1 d . . . H28A H -0.0244 0.2880 0.1238 0.089 Uiso 1 1 calc R . . H28B H 0.0703 0.2483 0.0166 0.089 Uiso 1 1 calc R . . H28C H 0.0911 0.3722 0.1213 0.089 Uiso 1 1 calc R . . 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 0.01770(10) 0.01800(11) 0.01703(10) 0.00699(7) 0.00107(7) 0.00480(7) O1 0.0193(5) 0.0203(5) 0.0335(6) 0.0086(5) 0.0050(4) 0.0044(4) O2 0.0255(6) 0.0241(6) 0.0376(6) 0.0168(5) 0.0117(5) 0.0108(5) O3 0.0256(6) 0.0216(6) 0.0296(6) 0.0116(5) -0.0017(4) 0.0051(5) O4 0.0227(6) 0.0255(6) 0.0209(5) 0.0068(4) 0.0004(4) 0.0069(5) O5 0.0192(5) 0.0228(5) 0.0231(5) 0.0046(4) -0.0025(4) 0.0045(4) O6 0.0291(6) 0.0394(7) 0.0225(5) 0.0032(5) -0.0039(5) 0.0101(5) O7 0.0196(5) 0.0334(7) 0.0389(6) 0.0108(5) 0.0002(5) 0.0016(5) O8 0.0628(9) 0.0361(8) 0.0387(7) 0.0161(6) 0.0132(7) 0.0103(7) O9 0.0959(15) 0.0439(10) 0.0507(9) 0.0044(8) -0.0105(9) -0.0224(9) O10 0.0500(8) 0.0379(8) 0.0405(7) 0.0090(6) 0.0166(6) 0.0106(6) O11 0.0439(8) 0.0362(7) 0.0313(7) 0.0075(6) 0.0069(6) 0.0197(6) N1 0.0200(6) 0.0215(6) 0.0203(6) 0.0087(5) 0.0027(5) 0.0060(5) N2 0.0211(6) 0.0204(6) 0.0200(6) 0.0069(5) 0.0027(5) 0.0075(5) N3 0.0200(6) 0.0186(6) 0.0199(6) 0.0074(5) 0.0017(5) 0.0062(5) N4 0.0207(6) 0.0206(6) 0.0269(6) 0.0069(5) 0.0036(5) 0.0076(5) N5 0.0221(6) 0.0180(6) 0.0267(6) 0.0068(5) -0.0013(5) 0.0063(5) N6 0.0388(9) 0.0340(8) 0.0331(8) 0.0101(6) -0.0016(6) 0.0033(7) C1 0.0306(8) 0.0267(8) 0.0225(7) 0.0134(6) -0.0001(6) 0.0047(6) C2 0.0239(7) 0.0316(8) 0.0188(7) 0.0108(6) 0.0035(6) 0.0052(6) C3 0.0213(7) 0.0297(8) 0.0202(7) 0.0083(6) -0.0015(6) 0.0056(6) C4 0.0214(7) 0.0253(8) 0.0217(7) 0.0071(6) -0.0015(6) 0.0025(6) C5 0.0199(7) 0.0236(7) 0.0222(7) 0.0107(6) 0.0015(5) 0.0048(6) C6 0.0211(7) 0.0243(8) 0.0191(6) 0.0101(6) 0.0011(5) 0.0029(6) C7 0.0292(8) 0.0230(8) 0.0221(7) 0.0090(6) 0.0028(6) 0.0031(6) C8 0.0308(8) 0.0267(8) 0.0232(7) 0.0098(6) -0.0016(6) -0.0049(7) C9 0.0209(7) 0.0376(9) 0.0239(7) 0.0162(7) -0.0013(6) -0.0026(6) C10 0.0212(7) 0.0303(8) 0.0230(7) 0.0137(6) 0.0015(6) 0.0047(6) C11 0.0219(7) 0.0231(7) 0.0191(6) 0.0103(6) 0.0006(5) 0.0017(6) C12 0.0205(7) 0.0243(8) 0.0314(8) 0.0087(6) 0.0045(6) 0.0073(6) C13 0.0181(7) 0.0232(8) 0.0294(8) 0.0083(6) 0.0036(6) 0.0090(6) C14 0.0253(8) 0.0299(8) 0.0280(8) 0.0113(7) 0.0057(6) 0.0098(7) C15 0.0323(9) 0.0317(9) 0.0255(8) 0.0038(7) -0.0007(6) 0.0100(7) C16 0.0256(8) 0.0218(8) 0.0360(9) 0.0047(7) -0.0020(7) 0.0045(6) C17 0.0214(7) 0.0200(7) 0.0336(8) 0.0089(6) 0.0039(6) 0.0089(6) C18 0.0232(7) 0.0229(8) 0.0381(9) 0.0125(7) 0.0073(6) 0.0091(6) C19 0.0228(7) 0.0216(7) 0.0249(7) 0.0108(6) 0.0019(6) 0.0031(6) C20 0.0301(8) 0.0229(8) 0.0295(8) 0.0107(6) 0.0013(6) 0.0085(6) C21 0.0390(9) 0.0211(8) 0.0281(8) 0.0128(6) -0.0013(7) 0.0028(7) C22 0.0303(8) 0.0249(8) 0.0226(7) 0.0105(6) 0.0007(6) -0.0008(6) C23 0.0227(7) 0.0249(8) 0.0224(7) 0.0091(6) -0.0010(6) 0.0028(6) C24 0.0223(7) 0.0196(7) 0.0224(7) 0.0087(6) -0.0016(5) 0.0031(6) C25 0.0193(7) 0.0210(7) 0.0256(7) 0.0109(6) 0.0014(5) 0.0048(6) C26 0.0314(9) 0.0310(9) 0.0343(8) 0.0172(7) -0.0005(7) 0.0097(7) C27 0.0315(8) 0.0253(8) 0.0235(7) 0.0082(6) 0.0058(6) 0.0096(7) C28 0.0774(17) 0.0590(15) 0.0391(11) 0.0031(10) -0.0100(11) 0.0357(13) _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 O3 2.0941(12) . ? Co1 O4 2.1103(12) . ? Co1 N2 2.1306(14) . ? Co1 N3 2.1418(13) . ? Co1 O5 2.1828(12) . ? Co1 N1 2.1985(13) . ? O1 C11 1.3760(18) . ? O1 C12 1.4376(18) . ? O2 C19 1.3825(18) . ? O2 C18 1.4427(18) . ? O3 C26 1.4279(19) . ? O3 H3O 0.83(2) . ? O4 C27 1.4433(19) . ? O4 H4O 0.78(2) . ? O5 N5 1.2724(16) . ? O6 N5 1.2610(17) . ? O7 N5 1.2327(17) . ? O8 N6 1.271(2) . ? O9 N6 1.234(2) . ? O10 N6 1.247(2) . ? O11 C28 1.425(3) . ? O11 H11O 0.78(2) . ? N1 C1 1.4931(19) . ? N1 C25 1.4947(19) . ? N1 H1N 0.862(19) . ? N2 C2 1.4805(19) . ? N2 C3 1.4886(19) . ? N2 H2N 0.815(19) . ? N3 C4 1.4849(19) . ? N3 C5 1.4931(18) . ? N3 H3N 0.814(19) . ? N4 C13 1.347(2) . ? N4 C17 1.348(2) . ? C1 C2 1.518(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.515(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.390(2) . ? C6 C11 1.401(2) . ? C7 C8 1.395(2) . ? C7 H7 0.9500 . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.398(2) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C12 C13 1.505(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.394(2) . ? C14 C15 1.386(2) . ? C14 H14 0.9500 . ? C15 C16 1.386(2) . ? C15 H15 0.9500 . ? C16 C17 1.388(2) . ? C16 H16 0.9500 . ? C17 C18 1.506(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.394(2) . ? C19 C24 1.407(2) . ? C20 C21 1.393(2) . ? C20 H20 0.9500 . ? C21 C22 1.383(2) . ? C21 H21 0.9500 . ? C22 C23 1.390(2) . ? C22 H22 0.9500 . ? C23 C24 1.392(2) . ? C23 H23 0.9500 . ? C24 C25 1.513(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O4 92.16(5) . . ? O3 Co1 N2 94.07(5) . . ? O4 Co1 N2 173.46(5) . . ? O3 Co1 N3 89.31(5) . . ? O4 Co1 N3 95.51(5) . . ? N2 Co1 N3 82.63(5) . . ? O3 Co1 O5 81.23(4) . . ? O4 Co1 O5 90.05(4) . . ? N2 Co1 O5 92.82(4) . . ? N3 Co1 O5 169.21(5) . . ? O3 Co1 N1 166.18(5) . . ? O4 Co1 N1 93.29(5) . . ? N2 Co1 N1 81.06(5) . . ? N3 Co1 N1 102.78(5) . . ? O5 Co1 N1 86.07(4) . . ? C11 O1 C12 117.97(12) . . ? C19 O2 C18 117.17(12) . . ? C26 O3 Co1 124.15(10) . . ? C26 O3 H3O 107.7(15) . . ? Co1 O3 H3O 127.6(15) . . ? C27 O4 Co1 123.77(9) . . ? C27 O4 H4O 113.5(17) . . ? Co1 O4 H4O 103.6(16) . . ? N5 O5 Co1 132.55(9) . . ? C28 O11 H11O 108.9(18) . . ? C1 N1 C25 111.48(11) . . ? C1 N1 Co1 108.98(9) . . ? C25 N1 Co1 115.63(9) . . ? C1 N1 H1N 105.4(12) . . ? C25 N1 H1N 106.3(12) . . ? Co1 N1 H1N 108.5(12) . . ? C2 N2 C3 113.47(12) . . ? C2 N2 Co1 106.17(9) . . ? C3 N2 Co1 108.00(9) . . ? C2 N2 H2N 108.0(12) . . ? C3 N2 H2N 107.9(13) . . ? Co1 N2 H2N 113.4(12) . . ? C4 N3 C5 111.38(12) . . ? C4 N3 Co1 106.08(9) . . ? C5 N3 Co1 113.98(9) . . ? C4 N3 H3N 107.8(13) . . ? C5 N3 H3N 107.8(12) . . ? Co1 N3 H3N 109.7(13) . . ? C13 N4 C17 117.99(14) . . ? O7 N5 O6 120.91(13) . . ? O7 N5 O5 119.12(13) . . ? O6 N5 O5 119.97(12) . . ? O9 N6 O10 121.17(16) . . ? O9 N6 O8 120.00(16) . . ? O10 N6 O8 118.70(15) . . ? N1 C1 C2 111.17(12) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.92(12) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 108.87(12) . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 109.13(12) . . ? N3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N3 C5 C6 113.65(12) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C11 118.77(14) . . ? C7 C6 C5 121.35(14) . . ? C11 C6 C5 119.88(13) . . ? C6 C7 C8 120.99(15) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 119.21(15) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.22(15) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 118.71(15) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? O1 C11 C10 124.78(14) . . ? O1 C11 C6 114.14(13) . . ? C10 C11 C6 121.07(14) . . ? O1 C12 C13 106.35(12) . . ? O1 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? O1 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.6 . . ? N4 C13 C14 122.70(15) . . ? N4 C13 C12 117.04(14) . . ? C14 C13 C12 120.25(14) . . ? C15 C14 C13 118.90(15) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 118.52(15) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 119.60(16) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N4 C17 C16 122.29(15) . . ? N4 C17 C18 117.28(14) . . ? C16 C17 C18 120.41(15) . . ? O2 C18 C17 108.40(12) . . ? O2 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O2 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? O2 C19 C20 124.36(14) . . ? O2 C19 C24 115.11(13) . . ? C20 C19 C24 120.53(14) . . ? C21 C20 C19 119.14(15) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 121.14(15) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.29(14) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 121.15(15) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 118.71(14) . . ? C23 C24 C25 120.33(14) . . ? C19 C24 C25 120.95(13) . . ? N1 C25 C24 114.18(12) . . ? N1 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? N1 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 H28A 109.5 . . ? O11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 Co1 O3 C26 -19.54(12) . . . . ? N2 Co1 O3 C26 162.41(12) . . . . ? N3 Co1 O3 C26 -115.03(12) . . . . ? O5 Co1 O3 C26 70.17(12) . . . . ? N1 Co1 O3 C26 93.7(2) . . . . ? O3 Co1 O4 C27 -148.58(11) . . . . ? N2 Co1 O4 C27 14.1(5) . . . . ? N3 Co1 O4 C27 -59.06(12) . . . . ? O5 Co1 O4 C27 130.20(11) . . . . ? N1 Co1 O4 C27 44.13(12) . . . . ? O3 Co1 O5 N5 -100.68(13) . . . . ? O4 Co1 O5 N5 -8.50(12) . . . . ? N2 Co1 O5 N5 165.63(12) . . . . ? N3 Co1 O5 N5 -129.7(2) . . . . ? N1 Co1 O5 N5 84.79(12) . . . . ? O3 Co1 N1 C1 66.8(2) . . . . ? O4 Co1 N1 C1 179.85(10) . . . . ? N2 Co1 N1 C1 -3.46(10) . . . . ? N3 Co1 N1 C1 -83.74(10) . . . . ? O5 Co1 N1 C1 90.02(10) . . . . ? O3 Co1 N1 C25 -59.7(2) . . . . ? O4 Co1 N1 C25 53.37(10) . . . . ? N2 Co1 N1 C25 -129.94(10) . . . . ? N3 Co1 N1 C25 149.78(10) . . . . ? O5 Co1 N1 C25 -36.45(10) . . . . ? O3 Co1 N2 C2 -138.20(9) . . . . ? O4 Co1 N2 C2 59.2(4) . . . . ? N3 Co1 N2 C2 133.02(10) . . . . ? O5 Co1 N2 C2 -56.80(10) . . . . ? N1 Co1 N2 C2 28.77(9) . . . . ? O3 Co1 N2 C3 99.78(10) . . . . ? O4 Co1 N2 C3 -62.8(4) . . . . ? N3 Co1 N2 C3 11.01(10) . . . . ? O5 Co1 N2 C3 -178.82(9) . . . . ? N1 Co1 N2 C3 -93.24(10) . . . . ? O3 Co1 N3 C4 -75.98(10) . . . . ? O4 Co1 N3 C4 -168.09(9) . . . . ? N2 Co1 N3 C4 18.22(9) . . . . ? O5 Co1 N3 C4 -47.4(3) . . . . ? N1 Co1 N3 C4 97.27(10) . . . . ? O3 Co1 N3 C5 46.94(10) . . . . ? O4 Co1 N3 C5 -45.16(10) . . . . ? N2 Co1 N3 C5 141.14(11) . . . . ? O5 Co1 N3 C5 75.5(2) . . . . ? N1 Co1 N3 C5 -139.81(10) . . . . ? Co1 O5 N5 O7 -163.19(10) . . . . ? Co1 O5 N5 O6 16.6(2) . . . . ? C25 N1 C1 C2 106.26(14) . . . . ? Co1 N1 C1 C2 -22.57(15) . . . . ? C3 N2 C2 C1 68.28(16) . . . . ? Co1 N2 C2 C1 -50.18(13) . . . . ? N1 C1 C2 N2 49.43(17) . . . . ? C2 N2 C3 C4 -155.68(13) . . . . ? Co1 N2 C3 C4 -38.27(14) . . . . ? C5 N3 C4 C3 -169.10(12) . . . . ? Co1 N3 C4 C3 -44.55(13) . . . . ? N2 C3 C4 N3 56.81(16) . . . . ? C4 N3 C5 C6 -60.65(16) . . . . ? Co1 N3 C5 C6 179.37(10) . . . . ? N3 C5 C6 C7 105.85(16) . . . . ? N3 C5 C6 C11 -73.92(17) . . . . ? C11 C6 C7 C8 -0.5(2) . . . . ? C5 C6 C7 C8 179.77(13) . . . . ? C6 C7 C8 C9 -0.9(2) . . . . ? C7 C8 C9 C10 1.6(2) . . . . ? C8 C9 C10 C11 -1.0(2) . . . . ? C12 O1 C11 C10 2.2(2) . . . . ? C12 O1 C11 C6 -177.22(13) . . . . ? C9 C10 C11 O1 -179.73(13) . . . . ? C9 C10 C11 C6 -0.4(2) . . . . ? C7 C6 C11 O1 -179.49(13) . . . . ? C5 C6 C11 O1 0.30(19) . . . . ? C7 C6 C11 C10 1.1(2) . . . . ? C5 C6 C11 C10 -179.14(13) . . . . ? C11 O1 C12 C13 169.63(12) . . . . ? C17 N4 C13 C14 0.0(2) . . . . ? C17 N4 C13 C12 -179.37(13) . . . . ? O1 C12 C13 N4 72.81(17) . . . . ? O1 C12 C13 C14 -106.59(16) . . . . ? N4 C13 C14 C15 -0.8(2) . . . . ? C12 C13 C14 C15 178.52(15) . . . . ? C13 C14 C15 C16 0.9(2) . . . . ? C14 C15 C16 C17 -0.2(2) . . . . ? C13 N4 C17 C16 0.7(2) . . . . ? C13 N4 C17 C18 -177.85(13) . . . . ? C15 C16 C17 N4 -0.6(2) . . . . ? C15 C16 C17 C18 177.92(15) . . . . ? C19 O2 C18 C17 -172.35(13) . . . . ? N4 C17 C18 O2 -84.00(17) . . . . ? C16 C17 C18 O2 97.40(17) . . . . ? C18 O2 C19 C20 6.7(2) . . . . ? C18 O2 C19 C24 -173.14(13) . . . . ? O2 C19 C20 C21 178.84(15) . . . . ? C24 C19 C20 C21 -1.3(2) . . . . ? C19 C20 C21 C22 -0.3(2) . . . . ? C20 C21 C22 C23 1.5(2) . . . . ? C21 C22 C23 C24 -1.0(2) . . . . ? C22 C23 C24 C19 -0.6(2) . . . . ? C22 C23 C24 C25 177.71(14) . . . . ? O2 C19 C24 C23 -178.37(13) . . . . ? C20 C19 C24 C23 1.8(2) . . . . ? O2 C19 C24 C25 3.3(2) . . . . ? C20 C19 C24 C25 -176.53(14) . . . . ? C1 N1 C25 C24 61.02(16) . . . . ? Co1 N1 C25 C24 -173.78(9) . . . . ? C23 C24 C25 N1 -115.55(15) . . . . ? C19 C24 C25 N1 62.72(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O8 0.83(2) 1.84(2) 2.6638(19) 172(2) . O3 H3O O10 0.83(2) 2.51(2) 3.1021(19) 129.9(18) . O3 H3O N6 0.83(2) 2.53(2) 3.312(2) 158.4(19) . O4 H4O O6 0.78(2) 1.95(2) 2.7000(18) 162(2) . O4 H4O N5 0.78(2) 2.67(2) 3.2698(18) 135(2) . O11 H11O N4 0.78(2) 2.04(2) 2.817(2) 174(2) . N1 H1N O2 0.862(19) 2.390(19) 2.9922(18) 127.3(15) . N1 H1N O11 0.862(19) 2.412(19) 3.128(2) 140.8(16) . N2 H2N O5 0.815(19) 2.465(19) 3.1401(17) 140.9(16) 2_655 N2 H2N O7 0.815(19) 2.626(18) 3.2122(19) 130.2(15) 2_655 N3 H3N O11 0.814(19) 2.388(19) 3.138(2) 153.5(16) . N3 H3N O1 0.814(19) 2.586(18) 3.0831(17) 120.9(15) . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.598 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.054 #===END data_lfl33 _database_code_CSD 178687 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.80 H41.20 N6 Ni O11' _chemical_formula_weight 694.18 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 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7459(16) _cell_length_b 13.4578(18) _cell_length_c 11.0282(15) _cell_angle_alpha 111.944(2) _cell_angle_beta 87.059(2) _cell_angle_gamma 101.493(2) _cell_volume 1584.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 942 _cell_measurement_theta_min 3.130 _cell_measurement_theta_max 28.020 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.384 _exptl_crystal_size_mid 0.281 _exptl_crystal_size_min 0.241 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 226 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 16203 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7153 _reflns_number_gt 6584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _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^)+(0.0569P)^2^+0.5762P] 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 7153 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.143972(15) 0.393784(14) 0.778172(16) 0.01606(7) Uani 1 1 d . . . O1 O 0.50457(9) 0.33246(9) 0.57706(11) 0.0240(2) Uani 1 1 d . . . O2 O 0.17248(10) 0.02469(9) 0.63120(11) 0.0257(2) Uani 1 1 d . . . O3 O 0.12820(9) 0.54145(9) 0.76426(11) 0.0237(2) Uani 1 1 d . . . H3O H 0.1582 0.6040 0.8165 0.036 Uiso 1 1 d R . . O4 O 0.12355(9) 0.31507(8) 0.57645(10) 0.0212(2) Uani 1 1 d . . . H4O H 0.0515 0.2976 0.5614 0.032 Uiso 1 1 d R . . O5 O -0.04001(9) 0.38108(9) 0.80082(10) 0.0218(2) Uani 1 1 d . . . O6 O -0.10805(10) 0.29334(10) 0.59927(11) 0.0302(3) Uani 1 1 d . . . O7 O -0.22329(10) 0.31414(10) 0.76280(12) 0.0306(3) Uani 1 1 d . . . O8 O 0.20036(14) 0.74298(11) 0.93869(14) 0.0450(3) Uani 1 1 d . . . O9 O 0.31435(18) 0.89324(14) 0.94697(17) 0.0662(5) Uani 1 1 d . . . O10 O 0.29876(13) 0.75005(11) 0.77038(14) 0.0450(3) Uani 1 1 d . . . O11 O 0.38631(11) 0.23487(10) 0.80202(12) 0.0202(3) Uani 0.80 1 d P . . H11O H 0.3970 0.1932 0.7255 0.030 Uiso 0.80 1 calc PR . . O12 O 0.4070(6) 0.1289(6) 0.9343(7) 0.0393(15) Uiso 0.20 1 d P . . N1 N 0.12501(11) 0.24271(10) 0.81020(12) 0.0186(2) Uani 1 1 d . . . H1N H 0.1840(17) 0.2124(15) 0.7776(18) 0.022 Uiso 1 1 d . . . N2 N 0.17090(11) 0.46169(10) 0.97931(12) 0.0193(2) Uani 1 1 d . . . H2N H 0.1492(16) 0.5242(16) 1.0176(18) 0.023 Uiso 1 1 d . . . N3 N 0.32515(11) 0.43904(10) 0.77225(11) 0.0181(2) Uani 1 1 d . . . H3N H 0.3570(17) 0.3877(16) 0.7622(18) 0.022 Uiso 1 1 d . . . N4 N 0.41388(11) 0.10248(10) 0.53946(12) 0.0218(2) Uani 1 1 d . . . N5 N -0.12507(11) 0.32887(10) 0.72025(12) 0.0208(2) Uani 1 1 d . . . N6 N 0.27395(14) 0.79643(12) 0.88642(15) 0.0330(3) Uani 1 1 d . . . C1 C 0.13260(14) 0.26899(13) 0.95393(14) 0.0244(3) Uani 1 1 d . . . H1A H 0.2120 0.2677 0.9785 0.029 Uiso 1 1 calc R . . H1B H 0.0775 0.2129 0.9766 0.029 Uiso 1 1 calc R . . C2 C 0.10427(13) 0.38083(13) 1.03033(14) 0.0233(3) Uani 1 1 d . . . H2A H 0.0200 0.3778 1.0221 0.028 Uiso 1 1 calc R . . H2B H 0.1243 0.4030 1.1241 0.028 Uiso 1 1 calc R . . C3 C 0.29806(13) 0.48352(13) 1.00660(14) 0.0230(3) Uani 1 1 d . . . H3A H 0.3218 0.4162 1.0040 0.028 Uiso 1 1 calc R . . H3B H 0.3174 0.5404 1.0948 0.028 Uiso 1 1 calc R . . C4 C 0.36193(13) 0.52170(12) 0.90426(14) 0.0219(3) Uani 1 1 d . . . H4A H 0.3440 0.5928 0.9126 0.026 Uiso 1 1 calc R . . H4B H 0.4468 0.5315 0.9172 0.026 Uiso 1 1 calc R . . C5 C 0.36737(12) 0.48356(12) 0.66899(14) 0.0198(3) Uani 1 1 d . . . H5A H 0.3319 0.5474 0.6815 0.024 Uiso 1 1 calc R . . H5B H 0.3409 0.4273 0.5823 0.024 Uiso 1 1 calc R . . C6 C 0.49756(12) 0.51764(12) 0.66986(13) 0.0199(3) Uani 1 1 d . . . C7 C 0.55172(14) 0.62709(13) 0.71765(14) 0.0239(3) Uani 1 1 d . . . H7 H 0.5060 0.6819 0.7512 0.029 Uiso 1 1 calc R . . C8 C 0.67252(14) 0.65755(13) 0.71692(15) 0.0266(3) Uani 1 1 d . . . H8 H 0.7089 0.7325 0.7507 0.032 Uiso 1 1 calc R . . C9 C 0.73877(13) 0.57770(14) 0.66661(15) 0.0253(3) Uani 1 1 d . . . H9 H 0.8208 0.5984 0.6642 0.030 Uiso 1 1 calc R . . C10 C 0.68686(13) 0.46675(13) 0.61912(14) 0.0227(3) Uani 1 1 d . . . H10 H 0.7330 0.4123 0.5859 0.027 Uiso 1 1 calc R . . C11 C 0.56645(12) 0.43771(12) 0.62144(13) 0.0196(3) Uani 1 1 d . . . C12 C 0.56744(13) 0.24531(12) 0.51913(16) 0.0242(3) Uani 1 1 d . . . H12A H 0.6140 0.2380 0.5866 0.029 Uiso 1 1 calc R . . H12B H 0.6204 0.2595 0.4522 0.029 Uiso 1 1 calc R . . C13 C 0.47742(13) 0.14338(12) 0.45769(15) 0.0219(3) Uani 1 1 d . . . C14 C 0.46186(14) 0.09569(13) 0.32237(16) 0.0264(3) Uani 1 1 d . . . H14 H 0.5089 0.1263 0.2675 0.032 Uiso 1 1 calc R . . C15 C 0.37650(15) 0.00275(14) 0.26900(16) 0.0304(3) Uani 1 1 d . . . H15 H 0.3632 -0.0309 0.1771 0.036 Uiso 1 1 calc R . . C16 C 0.31126(14) -0.03975(13) 0.35285(17) 0.0284(3) Uani 1 1 d . . . H16 H 0.2527 -0.1036 0.3190 0.034 Uiso 1 1 calc R . . C17 C 0.33218(13) 0.01179(12) 0.48686(15) 0.0234(3) Uani 1 1 d . . . C18 C 0.26426(14) -0.03511(13) 0.57924(17) 0.0266(3) Uani 1 1 d . . . H18A H 0.2310 -0.1134 0.5322 0.032 Uiso 1 1 calc R . . H18B H 0.3159 -0.0285 0.6512 0.032 Uiso 1 1 calc R . . C19 C 0.09247(13) -0.01413(12) 0.70695(14) 0.0214(3) Uani 1 1 d . . . C20 C 0.08987(14) -0.11081(13) 0.72663(16) 0.0254(3) Uani 1 1 d . . . H20 H 0.1462 -0.1544 0.6882 0.031 Uiso 1 1 calc R . . C21 C 0.00336(15) -0.14289(13) 0.80351(16) 0.0270(3) Uani 1 1 d . . . H21 H 0.0012 -0.2088 0.8174 0.032 Uiso 1 1 calc R . . C22 C -0.07936(14) -0.07995(13) 0.85985(15) 0.0250(3) Uani 1 1 d . . . H22 H -0.1388 -0.1031 0.9107 0.030 Uiso 1 1 calc R . . C23 C -0.07459(13) 0.01739(12) 0.84133(14) 0.0223(3) Uani 1 1 d . . . H23 H -0.1306 0.0611 0.8809 0.027 Uiso 1 1 calc R . . C24 C 0.01092(13) 0.05197(12) 0.76580(14) 0.0198(3) Uani 1 1 d . . . C25 C 0.01738(13) 0.16035(12) 0.75108(14) 0.0207(3) Uani 1 1 d . . . H25A H 0.0131 0.1474 0.6568 0.025 Uiso 1 1 calc R . . H25B H -0.0511 0.1911 0.7924 0.025 Uiso 1 1 calc R . . C26 C 0.07946(15) 0.55009(14) 0.65355(16) 0.0292(3) Uani 1 1 d . . . H26A H 0.0019 0.5036 0.6328 0.044 Uiso 1 1 calc R . . H26B H 0.1295 0.5264 0.5784 0.044 Uiso 1 1 calc R . . H26C H 0.0735 0.6262 0.6734 0.044 Uiso 1 1 calc R . . C27 C 0.17739(14) 0.22422(13) 0.50075(15) 0.0246(3) Uani 1 1 d . . . H27A H 0.1544 0.1652 0.5340 0.037 Uiso 1 1 calc R . . H27B H 0.2621 0.2479 0.5080 0.037 Uiso 1 1 calc R . . H27C H 0.1522 0.1979 0.4089 0.037 Uiso 1 1 calc R . . C28 C 0.4513(2) 0.2137(2) 0.8921(2) 0.0378(5) Uani 0.80 1 d P . . H28A H 0.5325 0.2170 0.8658 0.057 Uiso 0.80 1 calc PR . . H28B H 0.4188 0.1409 0.8926 0.057 Uiso 0.80 1 calc PR . . H28C H 0.4474 0.2687 0.9799 0.057 Uiso 0.80 1 calc PR . . 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 0.01668(10) 0.01668(10) 0.01562(10) 0.00618(7) 0.00116(6) 0.00486(7) O1 0.0185(5) 0.0192(5) 0.0326(6) 0.0080(4) 0.0046(4) 0.0044(4) O2 0.0246(5) 0.0226(5) 0.0353(6) 0.0152(5) 0.0110(4) 0.0103(4) O3 0.0265(5) 0.0205(5) 0.0266(5) 0.0108(4) -0.0015(4) 0.0057(4) O4 0.0215(5) 0.0227(5) 0.0192(5) 0.0063(4) 0.0004(4) 0.0068(4) O5 0.0187(5) 0.0221(5) 0.0222(5) 0.0045(4) -0.0018(4) 0.0049(4) O6 0.0275(6) 0.0366(6) 0.0216(5) 0.0031(5) -0.0033(4) 0.0097(5) O7 0.0187(5) 0.0334(6) 0.0369(6) 0.0113(5) 0.0009(4) 0.0025(5) O8 0.0616(9) 0.0367(7) 0.0394(7) 0.0177(6) 0.0148(7) 0.0119(7) O9 0.0882(13) 0.0392(8) 0.0482(9) 0.0036(7) -0.0129(9) -0.0180(8) O10 0.0498(8) 0.0351(7) 0.0425(8) 0.0071(6) 0.0178(6) 0.0097(6) O11 0.0256(7) 0.0201(6) 0.0166(6) 0.0043(5) 0.0045(5) 0.0140(5) N1 0.0187(6) 0.0200(6) 0.0191(6) 0.0088(5) 0.0029(4) 0.0061(5) N2 0.0196(6) 0.0201(6) 0.0184(6) 0.0060(5) 0.0021(4) 0.0071(5) N3 0.0193(6) 0.0179(6) 0.0188(6) 0.0078(5) 0.0013(4) 0.0058(5) N4 0.0195(6) 0.0204(6) 0.0249(6) 0.0065(5) 0.0036(5) 0.0074(5) N5 0.0210(6) 0.0167(6) 0.0247(6) 0.0061(5) -0.0018(5) 0.0060(5) N6 0.0364(8) 0.0283(7) 0.0324(7) 0.0093(6) -0.0022(6) 0.0054(6) C1 0.0299(8) 0.0253(7) 0.0211(7) 0.0125(6) -0.0011(6) 0.0043(6) C2 0.0240(7) 0.0296(8) 0.0175(6) 0.0105(6) 0.0033(5) 0.0052(6) C3 0.0212(7) 0.0285(7) 0.0189(6) 0.0080(6) -0.0013(5) 0.0054(6) C4 0.0202(7) 0.0230(7) 0.0202(7) 0.0062(6) -0.0015(5) 0.0024(5) C5 0.0193(7) 0.0221(7) 0.0200(6) 0.0099(5) 0.0015(5) 0.0043(5) C6 0.0200(7) 0.0232(7) 0.0178(6) 0.0095(5) 0.0008(5) 0.0032(5) C7 0.0273(8) 0.0231(7) 0.0213(7) 0.0088(6) 0.0033(6) 0.0043(6) C8 0.0286(8) 0.0249(7) 0.0227(7) 0.0087(6) -0.0013(6) -0.0034(6) C9 0.0196(7) 0.0336(8) 0.0225(7) 0.0132(6) -0.0008(5) -0.0014(6) C10 0.0206(7) 0.0283(8) 0.0216(7) 0.0122(6) 0.0014(5) 0.0047(6) C11 0.0204(7) 0.0214(7) 0.0178(6) 0.0091(5) 0.0011(5) 0.0024(5) C12 0.0194(7) 0.0219(7) 0.0298(8) 0.0071(6) 0.0035(6) 0.0062(6) C13 0.0182(7) 0.0210(7) 0.0269(7) 0.0073(6) 0.0034(5) 0.0082(5) C14 0.0258(8) 0.0278(8) 0.0265(7) 0.0097(6) 0.0050(6) 0.0090(6) C15 0.0309(8) 0.0312(8) 0.0247(7) 0.0036(6) -0.0009(6) 0.0097(7) C16 0.0235(8) 0.0222(7) 0.0337(8) 0.0039(6) -0.0014(6) 0.0040(6) C17 0.0196(7) 0.0195(7) 0.0315(8) 0.0081(6) 0.0043(6) 0.0083(5) C18 0.0238(7) 0.0220(7) 0.0372(8) 0.0127(6) 0.0084(6) 0.0099(6) C19 0.0205(7) 0.0204(7) 0.0239(7) 0.0092(6) 0.0010(5) 0.0036(5) C20 0.0282(8) 0.0217(7) 0.0286(7) 0.0104(6) 0.0012(6) 0.0076(6) C21 0.0355(9) 0.0203(7) 0.0279(8) 0.0126(6) -0.0003(6) 0.0037(6) C22 0.0282(8) 0.0245(7) 0.0218(7) 0.0106(6) 0.0008(6) 0.0000(6) C23 0.0208(7) 0.0227(7) 0.0231(7) 0.0087(6) 0.0003(5) 0.0032(6) C24 0.0204(7) 0.0186(6) 0.0213(6) 0.0086(5) -0.0008(5) 0.0032(5) C25 0.0192(7) 0.0202(7) 0.0247(7) 0.0103(6) 0.0011(5) 0.0046(5) C26 0.0329(9) 0.0291(8) 0.0315(8) 0.0152(7) -0.0005(6) 0.0112(7) C27 0.0288(8) 0.0231(7) 0.0214(7) 0.0067(6) 0.0052(6) 0.0084(6) C28 0.0425(13) 0.0401(12) 0.0283(10) 0.0024(9) -0.0103(9) 0.0201(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.0730(12) . ? Ni1 O4 2.0787(10) . ? Ni1 O3 2.0940(11) . ? Ni1 N3 2.0983(13) . ? Ni1 O5 2.1427(11) . ? Ni1 N1 2.1578(12) . ? O1 C11 1.3720(18) . ? O1 C12 1.4373(18) . ? O2 C19 1.3798(17) . ? O2 C18 1.4408(18) . ? O3 C26 1.4269(19) . ? O3 H3O 0.8400 . ? O4 C27 1.4432(17) . ? O4 H4O 0.8400 . ? O5 N5 1.2752(16) . ? O6 N5 1.2580(17) . ? O7 N5 1.2301(17) . ? O8 N6 1.268(2) . ? O9 N6 1.227(2) . ? O10 N6 1.245(2) . ? O11 C28 1.424(2) . ? O11 H11O 0.8400 . ? N1 C1 1.4928(18) . ? N1 C25 1.4960(19) . ? N1 H1N 0.87(2) . ? N2 C2 1.4786(19) . ? N2 C3 1.4875(19) . ? N2 H2N 0.87(2) . ? N3 C4 1.4853(18) . ? N3 C5 1.4951(17) . ? N3 H3N 0.82(2) . ? N4 C17 1.345(2) . ? N4 C13 1.3458(19) . ? C1 C2 1.519(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.506(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.390(2) . ? C6 C11 1.404(2) . ? C7 C8 1.397(2) . ? C7 H7 0.9500 . ? C8 C9 1.383(2) . ? C8 H8 0.9500 . ? C9 C10 1.400(2) . ? C9 H9 0.9500 . ? C10 C11 1.392(2) . ? C10 H10 0.9500 . ? C12 C13 1.503(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.392(2) . ? C14 C15 1.388(2) . ? C14 H14 0.9500 . ? C15 C16 1.385(2) . ? C15 H15 0.9500 . ? C16 C17 1.389(2) . ? C16 H16 0.9500 . ? C17 C18 1.506(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.391(2) . ? C19 C24 1.405(2) . ? C20 C21 1.396(2) . ? C20 H20 0.9500 . ? C21 C22 1.386(2) . ? C21 H21 0.9500 . ? C22 C23 1.389(2) . ? C22 H22 0.9500 . ? C23 C24 1.392(2) . ? C23 H23 0.9500 . ? C24 C25 1.514(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 N2 Ni1 O4 175.16(4) . . ? N2 Ni1 O3 93.87(5) . . ? O4 Ni1 O3 90.64(4) . . ? N2 Ni1 N3 84.49(5) . . ? O4 Ni1 N3 93.86(4) . . ? O3 Ni1 N3 89.04(5) . . ? N2 Ni1 O5 90.86(4) . . ? O4 Ni1 O5 91.55(4) . . ? O3 Ni1 O5 81.14(4) . . ? N3 Ni1 O5 168.85(5) . . ? N2 Ni1 N1 82.69(5) . . ? O4 Ni1 N1 93.23(4) . . ? O3 Ni1 N1 168.06(5) . . ? N3 Ni1 N1 101.94(5) . . ? O5 Ni1 N1 87.46(4) . . ? C11 O1 C12 118.09(11) . . ? C19 O2 C18 116.81(11) . . ? C26 O3 Ni1 124.32(10) . . ? C26 O3 H3O 109.5 . . ? Ni1 O3 H3O 125.6 . . ? C27 O4 Ni1 123.75(9) . . ? C27 O4 H4O 109.5 . . ? Ni1 O4 H4O 105.6 . . ? N5 O5 Ni1 131.64(9) . . ? C28 O11 H11O 109.5 . . ? C1 N1 C25 110.78(11) . . ? C1 N1 Ni1 108.35(9) . . ? C25 N1 Ni1 115.29(9) . . ? C1 N1 H1N 105.6(12) . . ? C25 N1 H1N 107.4(12) . . ? Ni1 N1 H1N 108.9(12) . . ? C2 N2 C3 112.96(12) . . ? C2 N2 Ni1 106.04(9) . . ? C3 N2 Ni1 107.88(9) . . ? C2 N2 H2N 109.6(12) . . ? C3 N2 H2N 105.8(13) . . ? Ni1 N2 H2N 114.7(12) . . ? C4 N3 C5 110.55(11) . . ? C4 N3 Ni1 105.47(9) . . ? C5 N3 Ni1 115.05(9) . . ? C4 N3 H3N 106.5(13) . . ? C5 N3 H3N 107.7(13) . . ? Ni1 N3 H3N 111.3(13) . . ? C17 N4 C13 117.94(13) . . ? O7 N5 O6 120.92(13) . . ? O7 N5 O5 118.98(12) . . ? O6 N5 O5 120.11(12) . . ? O9 N6 O10 121.09(16) . . ? O9 N6 O8 120.39(16) . . ? O10 N6 O8 118.39(15) . . ? N1 C1 C2 110.89(12) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 109.72(12) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 108.81(12) . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 109.13(12) . . ? N3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N3 C5 C6 113.52(11) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C11 118.86(13) . . ? C7 C6 C5 121.46(13) . . ? C11 C6 C5 119.68(13) . . ? C6 C7 C8 120.85(15) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 119.45(15) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 121.03(14) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 118.81(14) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? O1 C11 C10 124.80(14) . . ? O1 C11 C6 114.21(12) . . ? C10 C11 C6 120.99(14) . . ? O1 C12 C13 106.13(12) . . ? O1 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? O1 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? N4 C13 C14 122.75(14) . . ? N4 C13 C12 116.83(13) . . ? C14 C13 C12 120.42(14) . . ? C15 C14 C13 118.91(15) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 118.47(15) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C17 119.44(15) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N4 C17 C16 122.48(14) . . ? N4 C17 C18 117.38(14) . . ? C16 C17 C18 120.12(14) . . ? O2 C18 C17 108.18(12) . . ? O2 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O2 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? O2 C19 C20 124.22(13) . . ? O2 C19 C24 115.06(12) . . ? C20 C19 C24 120.72(13) . . ? C19 C20 C21 119.13(15) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.91(14) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.39(14) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 121.11(14) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 118.72(13) . . ? C23 C24 C25 120.27(13) . . ? C19 C24 C25 120.99(13) . . ? N1 C25 C24 114.15(12) . . ? N1 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? N1 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 H28A 109.5 . . ? O11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 N2 Ni1 O3 C26 -163.58(12) . . . . ? O4 Ni1 O3 C26 18.15(12) . . . . ? N3 Ni1 O3 C26 112.00(12) . . . . ? O5 Ni1 O3 C26 -73.31(11) . . . . ? N1 Ni1 O3 C26 -90.8(2) . . . . ? N2 Ni1 O4 C27 -10.5(6) . . . . ? O3 Ni1 O4 C27 148.52(11) . . . . ? N3 Ni1 O4 C27 59.43(11) . . . . ? O5 Ni1 O4 C27 -130.33(11) . . . . ? N1 Ni1 O4 C27 -42.78(11) . . . . ? N2 Ni1 O5 N5 -166.21(12) . . . . ? O4 Ni1 O5 N5 9.59(12) . . . . ? O3 Ni1 O5 N5 100.00(12) . . . . ? N3 Ni1 O5 N5 128.6(2) . . . . ? N1 Ni1 O5 N5 -83.57(12) . . . . ? N2 Ni1 N1 C1 3.98(9) . . . . ? O4 Ni1 N1 C1 -178.62(9) . . . . ? O3 Ni1 N1 C1 -69.9(2) . . . . ? N3 Ni1 N1 C1 86.74(10) . . . . ? O5 Ni1 N1 C1 -87.22(9) . . . . ? N2 Ni1 N1 C25 128.74(10) . . . . ? O4 Ni1 N1 C25 -53.86(10) . . . . ? O3 Ni1 N1 C25 54.9(2) . . . . ? N3 Ni1 N1 C25 -148.50(9) . . . . ? O5 Ni1 N1 C25 37.54(9) . . . . ? O4 Ni1 N2 C2 -61.6(5) . . . . ? O3 Ni1 N2 C2 139.45(9) . . . . ? N3 Ni1 N2 C2 -131.89(10) . . . . ? O5 Ni1 N2 C2 58.27(9) . . . . ? N1 Ni1 N2 C2 -29.06(9) . . . . ? O4 Ni1 N2 C3 59.7(6) . . . . ? O3 Ni1 N2 C3 -99.26(10) . . . . ? N3 Ni1 N2 C3 -10.60(10) . . . . ? O5 Ni1 N2 C3 179.56(9) . . . . ? N1 Ni1 N2 C3 92.23(10) . . . . ? N2 Ni1 N3 C4 -18.05(9) . . . . ? O4 Ni1 N3 C4 166.51(9) . . . . ? O3 Ni1 N3 C4 75.93(9) . . . . ? O5 Ni1 N3 C4 47.7(3) . . . . ? N1 Ni1 N3 C4 -99.37(9) . . . . ? N2 Ni1 N3 C5 -140.15(10) . . . . ? O4 Ni1 N3 C5 44.42(10) . . . . ? O3 Ni1 N3 C5 -46.17(10) . . . . ? O5 Ni1 N3 C5 -74.4(2) . . . . ? N1 Ni1 N3 C5 138.54(9) . . . . ? Ni1 O5 N5 O7 163.55(10) . . . . ? Ni1 O5 N5 O6 -16.51(19) . . . . ? C25 N1 C1 C2 -105.53(14) . . . . ? Ni1 N1 C1 C2 21.86(14) . . . . ? C3 N2 C2 C1 -68.14(15) . . . . ? Ni1 N2 C2 C1 49.81(13) . . . . ? N1 C1 C2 N2 -48.50(16) . . . . ? C2 N2 C3 C4 154.18(12) . . . . ? Ni1 N2 C3 C4 37.30(14) . . . . ? C5 N3 C4 C3 168.54(12) . . . . ? Ni1 N3 C4 C3 43.59(13) . . . . ? N2 C3 C4 N3 -55.44(16) . . . . ? C4 N3 C5 C6 59.29(16) . . . . ? Ni1 N3 C5 C6 178.60(9) . . . . ? N3 C5 C6 C7 -105.28(15) . . . . ? N3 C5 C6 C11 74.78(16) . . . . ? C11 C6 C7 C8 0.5(2) . . . . ? C5 C6 C7 C8 -179.50(13) . . . . ? C6 C7 C8 C9 0.7(2) . . . . ? C7 C8 C9 C10 -1.5(2) . . . . ? C8 C9 C10 C11 1.0(2) . . . . ? C12 O1 C11 C10 -2.5(2) . . . . ? C12 O1 C11 C6 176.68(12) . . . . ? C9 C10 C11 O1 179.40(13) . . . . ? C9 C10 C11 C6 0.2(2) . . . . ? C7 C6 C11 O1 179.82(13) . . . . ? C5 C6 C11 O1 -0.23(18) . . . . ? C7 C6 C11 C10 -0.9(2) . . . . ? C5 C6 C11 C10 179.01(13) . . . . ? C11 O1 C12 C13 -169.51(12) . . . . ? C17 N4 C13 C14 -0.1(2) . . . . ? C17 N4 C13 C12 179.50(13) . . . . ? O1 C12 C13 N4 -72.63(16) . . . . ? O1 C12 C13 C14 106.95(15) . . . . ? N4 C13 C14 C15 0.7(2) . . . . ? C12 C13 C14 C15 -178.83(14) . . . . ? C13 C14 C15 C16 -0.9(2) . . . . ? C14 C15 C16 C17 0.5(2) . . . . ? C13 N4 C17 C16 -0.4(2) . . . . ? C13 N4 C17 C18 178.13(13) . . . . ? C15 C16 C17 N4 0.2(2) . . . . ? C15 C16 C17 C18 -178.31(15) . . . . ? C19 O2 C18 C17 173.00(13) . . . . ? N4 C17 C18 O2 82.03(17) . . . . ? C16 C17 C18 O2 -99.41(16) . . . . ? C18 O2 C19 C20 -5.5(2) . . . . ? C18 O2 C19 C24 174.28(13) . . . . ? O2 C19 C20 C21 -178.84(14) . . . . ? C24 C19 C20 C21 1.4(2) . . . . ? C19 C20 C21 C22 0.1(2) . . . . ? C20 C21 C22 C23 -1.2(2) . . . . ? C21 C22 C23 C24 0.8(2) . . . . ? C22 C23 C24 C19 0.6(2) . . . . ? C22 C23 C24 C25 -177.66(14) . . . . ? O2 C19 C24 C23 178.48(13) . . . . ? C20 C19 C24 C23 -1.8(2) . . . . ? O2 C19 C24 C25 -3.3(2) . . . . ? C20 C19 C24 C25 176.50(14) . . . . ? C1 N1 C25 C24 -61.12(16) . . . . ? Ni1 N1 C25 C24 175.40(9) . . . . ? C23 C24 C25 N1 114.69(15) . . . . ? C19 C24 C25 N1 -63.54(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O8 0.84 1.84 2.6695(19) 171.0 . O3 H3O O10 0.84 2.49 3.0871(18) 128.5 . O3 H3O N6 0.84 2.52 3.3108(19) 156.9 . O4 H4O O6 0.84 1.89 2.6865(16) 157.0 . O4 H4O N5 0.84 2.64 3.2555(16) 131.2 . O11 H11O N4 0.84 1.98 2.8180(18) 174.8 . N1 H1N O11 0.87(2) 2.35(2) 3.0876(18) 142.8(16) . N1 H1N O2 0.87(2) 2.418(19) 3.0044(16) 125.3(15) . N2 H2N O5 0.87(2) 2.40(2) 3.1305(16) 141.6(16) 2_567 N2 H2N O7 0.87(2) 2.623(19) 3.2551(18) 130.3(15) 2_567 N3 H3N O11 0.82(2) 2.35(2) 3.1079(18) 154.5(17) . N3 H3N O1 0.82(2) 2.596(19) 3.0926(16) 120.4(15) . O12 H28B O11 0.55 1.98 2.439(7) 143.6 . _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.738 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.059 #===END data_lfl44 _database_code_CSD 178688 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Cu N6 O9' _chemical_formula_weight 638.13 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? 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 28.340(8) _cell_length_b 8.324(2) _cell_length_c 24.685(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.890(5) _cell_angle_gamma 90.00 _cell_volume 5719(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 918 _cell_measurement_theta_min 3.494 _cell_measurement_theta_max 27.951 _exptl_crystal_description tabular _exptl_crystal_colour blue _exptl_crystal_size_max 0.510 _exptl_crystal_size_mid 0.241 _exptl_crystal_size_min 0.123 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details ; Gaussian (XPREP, Bruker 1995; Coppens et al., 1965) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 280 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 24727 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.21 _reflns_number_total 6545 _reflns_number_gt 5636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997), XSHELL (Bruker, 2000) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _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^)+(0.0300P)^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 6545 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.749 _refine_ls_restrained_S_all 1.749 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.362783(7) 0.13275(2) 0.115856(8) 0.02079(8) Uani 1 1 d . . . O1 O 0.33319(4) 0.38690(13) 0.13371(5) 0.0240(3) Uani 1 1 d . . . O2 O 0.42690(4) -0.03552(14) 0.10908(5) 0.0246(3) Uani 1 1 d . . . O3 O 0.40231(7) -0.2282(2) 0.24793(7) 0.0686(6) Uani 1 1 d . . . O4 O 0.42239(8) -0.0056(2) 0.28431(11) 0.1084(10) Uani 1 1 d . . . O5 O 0.43240(6) -0.2151(2) 0.33437(6) 0.0523(4) Uani 1 1 d . . . O6 O 0.33331(6) 0.68098(19) 0.05152(6) 0.0494(4) Uani 1 1 d . . . O7 O 0.33639(6) 0.52148(16) -0.01656(7) 0.0514(4) Uani 1 1 d . . . O8 O 0.31374(6) 0.76687(16) -0.03146(6) 0.0490(4) Uani 1 1 d . . . O9 O 0.37211(9) -0.5287(3) 0.30268(8) 0.0796(6) Uani 1 1 d . . . H9O H 0.3878 -0.4426 0.3046 0.119 Uiso 1 1 calc R . . N1 N 0.36786(5) 0.22091(18) 0.03949(6) 0.0228(3) Uani 1 1 d . . . H1N H 0.3605(7) 0.327(2) 0.0408(7) 0.024(5) Uiso 1 1 d . . . N2 N 0.30760(5) 0.00756(18) 0.07481(6) 0.0225(3) Uani 1 1 d . . . H2N H 0.3169(7) -0.074(2) 0.0646(8) 0.022(5) Uiso 1 1 d . . . N3 N 0.34127(6) 0.04757(18) 0.18464(6) 0.0257(3) Uani 1 1 d . . . H3N H 0.3635(7) 0.003(2) 0.2030(8) 0.029(6) Uiso 1 1 d . . . N4 N 0.42150(5) 0.26141(17) 0.15483(6) 0.0226(3) Uani 1 1 d . . . N5 N 0.41957(5) -0.14994(19) 0.28914(7) 0.0323(4) Uani 1 1 d . . . N6 N 0.32771(6) 0.65655(18) 0.00078(7) 0.0311(4) Uani 1 1 d . . . C1 C 0.32853(6) 0.1484(2) -0.00233(7) 0.0246(4) Uani 1 1 d . . . H1A H 0.3404 0.0512 -0.0185 0.030 Uiso 1 1 calc R . . H1B H 0.3175 0.2262 -0.0324 0.030 Uiso 1 1 calc R . . C2 C 0.28741(6) 0.1047(2) 0.02605(7) 0.0250(4) Uani 1 1 d . . . H2A H 0.2722 0.2031 0.0374 0.030 Uiso 1 1 calc R . . H2B H 0.2628 0.0425 0.0008 0.030 Uiso 1 1 calc R . . C3 C 0.27346(6) -0.0316(2) 0.11140(7) 0.0267(4) Uani 1 1 d . . . H3A H 0.2527 -0.1229 0.0962 0.032 Uiso 1 1 calc R . . H3B H 0.2528 0.0621 0.1150 0.032 Uiso 1 1 calc R . . C4 C 0.30342(7) -0.0757(2) 0.16716(7) 0.0277(4) Uani 1 1 d . . . H4A H 0.2824 -0.0830 0.1949 0.033 Uiso 1 1 calc R . . H4B H 0.3186 -0.1819 0.1647 0.033 Uiso 1 1 calc R . . C5 C 0.32689(7) 0.1740(2) 0.22172(7) 0.0307(4) Uani 1 1 d . . . H5A H 0.3547 0.2452 0.2346 0.037 Uiso 1 1 calc R . . H5B H 0.3185 0.1212 0.2546 0.037 Uiso 1 1 calc R . . C6 C 0.28493(7) 0.2748(2) 0.19430(8) 0.0291(4) Uani 1 1 d . . . C7 C 0.23993(8) 0.2616(3) 0.20842(9) 0.0396(5) Uani 1 1 d . . . H7 H 0.2352 0.1871 0.2361 0.047 Uiso 1 1 calc R . . C8 C 0.20152(8) 0.3562(3) 0.18263(10) 0.0460(6) Uani 1 1 d . . . H8 H 0.1709 0.3447 0.1925 0.055 Uiso 1 1 calc R . . C9 C 0.20786(7) 0.4666(3) 0.14276(9) 0.0409(5) Uani 1 1 d . . . H9 H 0.1818 0.5324 0.1259 0.049 Uiso 1 1 calc R . . C10 C 0.25238(7) 0.4813(2) 0.12734(8) 0.0319(4) Uani 1 1 d . . . H10 H 0.2570 0.5562 0.0998 0.038 Uiso 1 1 calc R . . C11 C 0.28995(6) 0.3848(2) 0.15298(7) 0.0256(4) Uani 1 1 d . . . C12 C 0.36952(6) 0.4932(2) 0.16215(8) 0.0273(4) Uani 1 1 d . . . H12A H 0.3639 0.5134 0.2000 0.033 Uiso 1 1 calc R . . H12B H 0.3679 0.5974 0.1425 0.033 Uiso 1 1 calc R . . C13 C 0.41811(6) 0.4188(2) 0.16474(7) 0.0229(4) Uani 1 1 d . . . C14 C 0.45891(7) 0.5153(2) 0.17892(7) 0.0292(4) Uani 1 1 d . . . H14 H 0.4557 0.6272 0.1850 0.035 Uiso 1 1 calc R . . C15 C 0.50387(7) 0.4468(2) 0.18399(8) 0.0339(4) Uani 1 1 d . . . H15 H 0.5320 0.5109 0.1932 0.041 Uiso 1 1 calc R . . C16 C 0.50745(6) 0.2827(2) 0.17542(7) 0.0294(4) Uani 1 1 d . . . H16 H 0.5380 0.2322 0.1798 0.035 Uiso 1 1 calc R . . C17 C 0.46580(6) 0.1941(2) 0.16046(7) 0.0247(4) Uani 1 1 d . . . C18 C 0.46743(6) 0.0149(2) 0.15044(8) 0.0293(4) Uani 1 1 d . . . H18A H 0.4977 -0.0126 0.1380 0.035 Uiso 1 1 calc R . . H18B H 0.4670 -0.0432 0.1853 0.035 Uiso 1 1 calc R . . C19 C 0.43656(6) -0.0756(2) 0.05714(7) 0.0245(4) Uani 1 1 d . . . C20 C 0.44934(7) -0.2328(2) 0.04873(8) 0.0324(4) Uani 1 1 d . . . H20 H 0.4539 -0.3073 0.0784 0.039 Uiso 1 1 calc R . . C21 C 0.45553(7) -0.2810(3) -0.00348(9) 0.0395(5) Uani 1 1 d . . . H21 H 0.4642 -0.3888 -0.0096 0.047 Uiso 1 1 calc R . . C22 C 0.44905(7) -0.1720(3) -0.04621(9) 0.0385(5) Uani 1 1 d . . . H22 H 0.4532 -0.2050 -0.0819 0.046 Uiso 1 1 calc R . . C23 C 0.43653(7) -0.0150(2) -0.03752(8) 0.0322(4) Uani 1 1 d . . . H23 H 0.4322 0.0588 -0.0674 0.039 Uiso 1 1 calc R . . C24 C 0.43005(6) 0.0372(2) 0.01465(7) 0.0257(4) Uani 1 1 d . . . C25 C 0.41536(6) 0.2089(2) 0.02219(8) 0.0265(4) Uani 1 1 d . . . H25A H 0.4401 0.2611 0.0504 0.032 Uiso 1 1 calc R . . H25B H 0.4139 0.2678 -0.0129 0.032 Uiso 1 1 calc R . . C26 C 0.35849(12) -0.5576(4) 0.35272(12) 0.0870(10) Uani 1 1 d . . . H26A H 0.3852 -0.5311 0.3828 0.131 Uiso 1 1 calc R . . H26B H 0.3501 -0.6712 0.3551 0.131 Uiso 1 1 calc R . . H26C H 0.3306 -0.4909 0.3557 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02060(12) 0.02058(12) 0.02045(12) 0.00001(8) 0.00198(8) 0.00166(8) O1 0.0235(6) 0.0234(6) 0.0253(6) -0.0019(5) 0.0049(5) 0.0027(5) O2 0.0246(6) 0.0263(6) 0.0226(6) -0.0010(5) 0.0039(5) 0.0042(5) O3 0.0837(13) 0.0671(12) 0.0449(10) -0.0225(9) -0.0138(9) 0.0227(10) O4 0.1018(17) 0.0375(11) 0.144(2) 0.0269(12) -0.0826(15) -0.0210(10) O5 0.0578(10) 0.0577(10) 0.0363(9) 0.0093(8) -0.0043(7) 0.0006(8) O6 0.0698(11) 0.0457(9) 0.0340(9) 0.0047(7) 0.0132(8) 0.0079(8) O7 0.0728(11) 0.0225(7) 0.0553(10) -0.0049(7) 0.0032(8) 0.0092(7) O8 0.0684(11) 0.0227(7) 0.0474(9) 0.0057(6) -0.0107(8) 0.0028(7) O9 0.1010(17) 0.0701(14) 0.0734(14) -0.0125(11) 0.0306(12) -0.0260(12) N1 0.0237(7) 0.0199(8) 0.0238(8) -0.0004(6) 0.0022(6) 0.0004(6) N2 0.0223(8) 0.0214(8) 0.0235(8) 0.0009(6) 0.0037(6) 0.0038(6) N3 0.0278(8) 0.0230(8) 0.0248(8) 0.0026(6) 0.0015(7) 0.0032(6) N4 0.0230(7) 0.0254(8) 0.0187(7) 0.0004(6) 0.0021(6) 0.0016(6) N5 0.0214(8) 0.0309(9) 0.0422(10) 0.0028(7) -0.0001(7) -0.0020(6) N6 0.0308(9) 0.0234(8) 0.0375(10) 0.0021(7) 0.0027(7) -0.0026(6) C1 0.0259(9) 0.0249(9) 0.0215(9) -0.0004(7) 0.0007(7) 0.0027(7) C2 0.0242(9) 0.0251(9) 0.0239(9) 0.0013(7) -0.0003(7) 0.0031(7) C3 0.0243(9) 0.0275(9) 0.0285(10) -0.0001(7) 0.0052(7) -0.0015(7) C4 0.0321(10) 0.0238(9) 0.0280(10) 0.0032(7) 0.0078(8) 0.0001(8) C5 0.0431(11) 0.0285(10) 0.0217(9) 0.0004(7) 0.0092(8) 0.0008(8) C6 0.0340(10) 0.0284(10) 0.0265(9) -0.0076(8) 0.0095(8) 0.0000(8) C7 0.0454(12) 0.0379(12) 0.0411(12) -0.0138(9) 0.0227(10) -0.0052(10) C8 0.0294(11) 0.0560(14) 0.0567(15) -0.0298(12) 0.0188(10) -0.0042(10) C9 0.0298(11) 0.0466(13) 0.0442(12) -0.0199(10) 0.0018(9) 0.0093(9) C10 0.0323(10) 0.0318(10) 0.0294(10) -0.0093(8) 0.0004(8) 0.0084(8) C11 0.0261(9) 0.0268(9) 0.0242(9) -0.0075(7) 0.0052(7) 0.0030(7) C12 0.0310(10) 0.0218(9) 0.0287(10) -0.0038(7) 0.0050(8) 0.0007(7) C13 0.0282(9) 0.0242(8) 0.0167(8) 0.0008(7) 0.0050(7) 0.0016(7) C14 0.0357(10) 0.0253(9) 0.0265(9) -0.0017(7) 0.0059(8) -0.0029(8) C15 0.0307(10) 0.0421(12) 0.0288(10) -0.0029(9) 0.0053(8) -0.0095(9) C16 0.0228(9) 0.0420(11) 0.0229(9) -0.0010(8) 0.0029(7) 0.0010(8) C17 0.0261(9) 0.0302(9) 0.0176(8) 0.0011(7) 0.0034(7) 0.0041(7) C18 0.0267(10) 0.0320(10) 0.0266(9) -0.0020(8) -0.0016(7) 0.0073(8) C19 0.0192(8) 0.0287(9) 0.0263(9) -0.0034(7) 0.0063(7) 0.0007(7) C20 0.0326(10) 0.0288(10) 0.0368(11) -0.0020(8) 0.0095(8) 0.0047(8) C21 0.0386(11) 0.0361(11) 0.0470(13) -0.0125(10) 0.0164(10) 0.0040(9) C22 0.0335(11) 0.0508(13) 0.0342(11) -0.0119(10) 0.0142(9) -0.0013(9) C23 0.0268(10) 0.0446(12) 0.0272(10) 0.0006(8) 0.0103(8) -0.0025(8) C24 0.0200(9) 0.0290(9) 0.0288(9) -0.0008(7) 0.0064(7) -0.0020(7) C25 0.0264(9) 0.0273(9) 0.0262(9) 0.0021(7) 0.0062(7) -0.0022(7) C26 0.101(3) 0.105(3) 0.064(2) 0.0240(18) 0.0367(18) 0.043(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.9898(15) . ? Cu1 N3 2.0368(16) . ? Cu1 N1 2.0531(15) . ? Cu1 N4 2.0584(15) . ? Cu1 O2 2.3252(13) . ? Cu1 O1 2.3480(13) . ? O1 C11 1.396(2) . ? O1 C12 1.436(2) . ? O2 C19 1.401(2) . ? O2 C18 1.447(2) . ? O3 N5 1.229(2) . ? O4 N5 1.211(2) . ? O5 N5 1.233(2) . ? O6 N6 1.249(2) . ? O7 N6 1.244(2) . ? O8 N6 1.231(2) . ? O9 C26 1.383(3) . ? O9 H9O 0.8400 . ? N1 C25 1.491(2) . ? N1 C1 1.496(2) . ? N1 H1N 0.91(2) . ? N2 C2 1.473(2) . ? N2 C3 1.479(2) . ? N2 H2N 0.79(2) . ? N3 C4 1.488(2) . ? N3 C5 1.501(2) . ? N3 H3N 0.79(2) . ? N4 C13 1.340(2) . ? N4 C17 1.358(2) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.519(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.507(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.389(3) . ? C6 C11 1.398(3) . ? C7 C8 1.396(3) . ? C7 H7 0.9500 . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C12 C13 1.500(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.397(2) . ? C14 C15 1.380(3) . ? C14 H14 0.9500 . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.514(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.384(3) . ? C19 C24 1.394(2) . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 C22 1.377(3) . ? C21 H21 0.9500 . ? C22 C23 1.381(3) . ? C22 H22 0.9500 . ? C23 C24 1.404(3) . ? C23 H23 0.9500 . ? C24 C25 1.510(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 N2 Cu1 N3 84.95(6) . . ? N2 Cu1 N1 84.51(6) . . ? N3 Cu1 N1 166.85(6) . . ? N2 Cu1 N4 177.07(6) . . ? N3 Cu1 N4 97.72(6) . . ? N1 Cu1 N4 93.01(6) . . ? N2 Cu1 O2 101.39(6) . . ? N3 Cu1 O2 102.20(5) . . ? N1 Cu1 O2 87.59(5) . . ? N4 Cu1 O2 76.90(5) . . ? N2 Cu1 O1 107.05(6) . . ? N3 Cu1 O1 89.05(5) . . ? N1 Cu1 O1 86.54(5) . . ? N4 Cu1 O1 74.30(5) . . ? O2 Cu1 O1 150.22(4) . . ? C11 O1 C12 115.82(13) . . ? C11 O1 Cu1 114.84(9) . . ? C12 O1 Cu1 113.49(10) . . ? C19 O2 C18 116.64(13) . . ? C19 O2 Cu1 119.98(10) . . ? C18 O2 Cu1 107.54(10) . . ? C26 O9 H9O 109.5 . . ? C25 N1 C1 111.77(14) . . ? C25 N1 Cu1 117.57(11) . . ? C1 N1 Cu1 108.49(10) . . ? C25 N1 H1N 107.4(12) . . ? C1 N1 H1N 105.7(11) . . ? Cu1 N1 H1N 105.0(12) . . ? C2 N2 C3 114.96(14) . . ? C2 N2 Cu1 105.96(11) . . ? C3 N2 Cu1 110.27(11) . . ? C2 N2 H2N 108.4(14) . . ? C3 N2 H2N 107.5(14) . . ? Cu1 N2 H2N 109.7(14) . . ? C4 N3 C5 113.34(15) . . ? C4 N3 Cu1 108.13(11) . . ? C5 N3 Cu1 115.02(11) . . ? C4 N3 H3N 107.3(14) . . ? C5 N3 H3N 104.7(15) . . ? Cu1 N3 H3N 107.9(15) . . ? C13 N4 C17 118.80(15) . . ? C13 N4 Cu1 120.98(11) . . ? C17 N4 Cu1 118.90(12) . . ? O4 N5 O3 117.9(2) . . ? O4 N5 O5 120.8(2) . . ? O3 N5 O5 121.33(18) . . ? O8 N6 O7 120.82(18) . . ? O8 N6 O6 119.43(16) . . ? O7 N6 O6 119.75(17) . . ? N1 C1 C2 108.42(14) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 107.22(14) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? N2 C3 C4 106.75(14) . . ? N2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? N2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N3 C4 C3 110.18(14) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 113.49(15) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C11 117.38(18) . . ? C7 C6 C5 121.82(18) . . ? C11 C6 C5 120.80(16) . . ? C6 C7 C8 121.0(2) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.3(2) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.0(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 118.8(2) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 O1 118.97(17) . . ? C10 C11 C6 122.50(18) . . ? O1 C11 C6 118.29(15) . . ? O1 C12 C13 109.50(14) . . ? O1 C12 H12A 109.8 . . ? C13 C12 H12A 109.8 . . ? O1 C12 H12B 109.8 . . ? C13 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? N4 C13 C14 121.58(16) . . ? N4 C13 C12 119.53(15) . . ? C14 C13 C12 118.87(16) . . ? C15 C14 C13 119.41(17) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.06(17) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 118.83(17) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? N4 C17 C16 122.27(17) . . ? N4 C17 C18 116.48(15) . . ? C16 C17 C18 121.24(16) . . ? O2 C18 C17 110.88(14) . . ? O2 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C24 121.69(17) . . ? C20 C19 O2 117.66(16) . . ? C24 C19 O2 120.50(15) . . ? C19 C20 C21 119.58(19) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 119.85(19) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.34(19) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 121.16(18) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 117.38(17) . . ? C19 C24 C25 123.03(16) . . ? C23 C24 C25 119.57(16) . . ? N1 C25 C24 112.56(14) . . ? N1 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? N1 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? O9 C26 H26A 109.5 . . ? O9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 N2 Cu1 O1 C11 45.10(12) . . . . ? N3 Cu1 O1 C11 -39.33(12) . . . . ? N1 Cu1 O1 C11 128.28(11) . . . . ? N4 Cu1 O1 C11 -137.62(12) . . . . ? O2 Cu1 O1 C11 -152.69(11) . . . . ? N2 Cu1 O1 C12 -178.48(11) . . . . ? N3 Cu1 O1 C12 97.10(12) . . . . ? N1 Cu1 O1 C12 -95.30(11) . . . . ? N4 Cu1 O1 C12 -1.19(11) . . . . ? O2 Cu1 O1 C12 -16.27(16) . . . . ? N2 Cu1 O2 C19 60.46(12) . . . . ? N3 Cu1 O2 C19 147.69(12) . . . . ? N1 Cu1 O2 C19 -23.45(12) . . . . ? N4 Cu1 O2 C19 -117.10(12) . . . . ? O1 Cu1 O2 C19 -102.21(13) . . . . ? N2 Cu1 O2 C18 -163.06(11) . . . . ? N3 Cu1 O2 C18 -75.84(11) . . . . ? N1 Cu1 O2 C18 113.03(11) . . . . ? N4 Cu1 O2 C18 19.37(10) . . . . ? O1 Cu1 O2 C18 34.27(15) . . . . ? N2 Cu1 N1 C25 -126.83(13) . . . . ? N3 Cu1 N1 C25 -163.7(2) . . . . ? N4 Cu1 N1 C25 51.60(12) . . . . ? O2 Cu1 N1 C25 -25.13(12) . . . . ? O1 Cu1 N1 C25 125.66(12) . . . . ? N2 Cu1 N1 C1 1.18(11) . . . . ? N3 Cu1 N1 C1 -35.7(3) . . . . ? N4 Cu1 N1 C1 179.61(11) . . . . ? O2 Cu1 N1 C1 102.88(11) . . . . ? O1 Cu1 N1 C1 -106.33(11) . . . . ? N3 Cu1 N2 C2 143.04(12) . . . . ? N1 Cu1 N2 C2 -29.08(11) . . . . ? N4 Cu1 N2 C2 -61.4(12) . . . . ? O2 Cu1 N2 C2 -115.51(11) . . . . ? O1 Cu1 N2 C2 55.59(12) . . . . ? N3 Cu1 N2 C3 18.05(12) . . . . ? N1 Cu1 N2 C3 -154.08(12) . . . . ? N4 Cu1 N2 C3 173.6(11) . . . . ? O2 Cu1 N2 C3 119.50(11) . . . . ? O1 Cu1 N2 C3 -69.40(12) . . . . ? N2 Cu1 N3 C4 8.84(12) . . . . ? N1 Cu1 N3 C4 45.7(3) . . . . ? N4 Cu1 N3 C4 -169.93(11) . . . . ? O2 Cu1 N3 C4 -91.75(12) . . . . ? O1 Cu1 N3 C4 116.05(11) . . . . ? N2 Cu1 N3 C5 -118.96(13) . . . . ? N1 Cu1 N3 C5 -82.1(3) . . . . ? N4 Cu1 N3 C5 62.27(13) . . . . ? O2 Cu1 N3 C5 140.45(12) . . . . ? O1 Cu1 N3 C5 -11.75(12) . . . . ? N2 Cu1 N4 C13 109.5(11) . . . . ? N3 Cu1 N4 C13 -95.14(13) . . . . ? N1 Cu1 N4 C13 77.24(13) . . . . ? O2 Cu1 N4 C13 164.06(13) . . . . ? O1 Cu1 N4 C13 -8.31(12) . . . . ? N2 Cu1 N4 C17 -57.3(12) . . . . ? N3 Cu1 N4 C17 98.14(13) . . . . ? N1 Cu1 N4 C17 -89.49(13) . . . . ? O2 Cu1 N4 C17 -2.66(12) . . . . ? O1 Cu1 N4 C17 -175.04(13) . . . . ? C25 N1 C1 C2 157.77(14) . . . . ? Cu1 N1 C1 C2 26.55(15) . . . . ? C3 N2 C2 C1 173.57(15) . . . . ? Cu1 N2 C2 C1 51.52(15) . . . . ? N1 C1 C2 N2 -51.86(17) . . . . ? C2 N2 C3 C4 -159.93(14) . . . . ? Cu1 N2 C3 C4 -40.25(16) . . . . ? C5 N3 C4 C3 95.11(18) . . . . ? Cu1 N3 C4 C3 -33.64(17) . . . . ? N2 C3 C4 N3 48.69(19) . . . . ? C4 N3 C5 C6 -64.0(2) . . . . ? Cu1 N3 C5 C6 61.09(19) . . . . ? N3 C5 C6 C7 109.2(2) . . . . ? N3 C5 C6 C11 -70.2(2) . . . . ? C11 C6 C7 C8 -0.7(3) . . . . ? C5 C6 C7 C8 179.89(18) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C7 C8 C9 C10 1.4(3) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 O1 173.35(16) . . . . ? C9 C10 C11 C6 -0.9(3) . . . . ? C12 O1 C11 C10 95.26(19) . . . . ? Cu1 O1 C11 C10 -129.35(14) . . . . ? C12 O1 C11 C6 -90.21(18) . . . . ? Cu1 O1 C11 C6 45.18(18) . . . . ? C7 C6 C11 C10 1.6(3) . . . . ? C5 C6 C11 C10 -179.03(16) . . . . ? C7 C6 C11 O1 -172.76(16) . . . . ? C5 C6 C11 O1 6.6(2) . . . . ? C11 O1 C12 C13 144.71(14) . . . . ? Cu1 O1 C12 C13 8.73(17) . . . . ? C17 N4 C13 C14 2.1(2) . . . . ? Cu1 N4 C13 C14 -164.69(13) . . . . ? C17 N4 C13 C12 -176.24(15) . . . . ? Cu1 N4 C13 C12 17.0(2) . . . . ? O1 C12 C13 N4 -16.4(2) . . . . ? O1 C12 C13 C14 165.30(15) . . . . ? N4 C13 C14 C15 -1.3(3) . . . . ? C12 C13 C14 C15 176.97(17) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C14 C15 C16 C17 1.9(3) . . . . ? C13 N4 C17 C16 -0.7(2) . . . . ? Cu1 N4 C17 C16 166.27(13) . . . . ? C13 N4 C17 C18 178.18(15) . . . . ? Cu1 N4 C17 C18 -14.8(2) . . . . ? C15 C16 C17 N4 -1.3(3) . . . . ? C15 C16 C17 C18 179.87(16) . . . . ? C19 O2 C18 C17 106.80(17) . . . . ? Cu1 O2 C18 C17 -31.34(16) . . . . ? N4 C17 C18 O2 32.3(2) . . . . ? C16 C17 C18 O2 -148.72(16) . . . . ? C18 O2 C19 C20 88.31(19) . . . . ? Cu1 O2 C19 C20 -138.96(13) . . . . ? C18 O2 C19 C24 -96.15(18) . . . . ? Cu1 O2 C19 C24 36.6(2) . . . . ? C24 C19 C20 C21 -0.6(3) . . . . ? O2 C19 C20 C21 174.92(17) . . . . ? C19 C20 C21 C22 0.2(3) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C21 C22 C23 C24 -0.1(3) . . . . ? C20 C19 C24 C23 0.6(3) . . . . ? O2 C19 C24 C23 -174.78(15) . . . . ? C20 C19 C24 C25 179.01(16) . . . . ? O2 C19 C24 C25 3.7(3) . . . . ? C22 C23 C24 C19 -0.2(3) . . . . ? C22 C23 C24 C25 -178.73(17) . . . . ? C1 N1 C25 C24 -60.49(18) . . . . ? Cu1 N1 C25 C24 65.93(17) . . . . ? C19 C24 C25 N1 -60.5(2) . . . . ? C23 C24 C25 N1 117.91(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9O O5 0.84 2.32 3.137(3) 164.9 . O9 H9O O3 0.84 2.35 3.042(3) 139.9 . O9 H9O N5 0.84 2.65 3.469(3) 165.3 . N1 H1N O7 0.91(2) 2.171(19) 2.916(2) 138.2(16) . N2 H2N O6 0.79(2) 2.13(2) 2.900(2) 166.3(19) 1_545 N3 H3N O4 0.79(2) 2.36(2) 3.066(2) 149.3(19) . N3 H3N O3 0.79(2) 2.39(2) 3.111(2) 152.3(19) . N3 H3N N5 0.79(2) 2.72(2) 3.481(2) 161.4(19) . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.790 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.061 #===END data_lfl49 _database_code_CSD 178689 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H30 Cd1.50 N7 O11' _chemical_formula_weight 773.16 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 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 29.273(6) _cell_length_b 8.4920(17) _cell_length_c 23.673(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.575(3) _cell_angle_gamma 90.00 _cell_volume 5833(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.808 _cell_measurement_theta_max 26.099 _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_size_max 0.476 _exptl_crystal_size_mid 0.206 _exptl_crystal_size_min 0.086 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.59862 _exptl_absorpt_correction_T_max 0.90834 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 -1.00 0.0400 -1.00 0.00 1.00 0.0460 1.00 0.00 0.00 0.0980 -1.00 0.00 0.00 0.1080 1.00 1.00 0.00 0.2610 -1.00 1.00 -2.00 0.2170 2.00 -1.00 0.00 0.2590 -2.00 -1.00 0.00 0.2390 _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not determined' _diffrn_reflns_number 26575 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6928 _reflns_number_gt 6006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997), XSHELL (Bruker, 2000) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _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^)+(0.0200P)^2^+2.0000P] 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 6928 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_restrained_S_all 1.291 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.344978(4) 0.411131(14) 0.071902(5) 0.02092(4) Uani 1 1 d . . . O1 O 0.37473(4) 0.46809(18) 0.17469(5) 0.0327(3) Uani 1 1 d . . . O2 O 0.38576(5) 0.40886(14) -0.01193(6) 0.0330(3) Uani 1 1 d . . . O3 O 0.28736(5) 0.46120(16) -0.01408(6) 0.0343(3) Uani 1 1 d . . . O4 O 0.32635(5) 0.67346(16) 0.00980(6) 0.0338(3) Uani 1 1 d . . . O5 O 0.27609(6) 0.67197(19) -0.06586(6) 0.0513(4) Uani 1 1 d . . . N1 N 0.28410(6) 0.55067(19) 0.10778(7) 0.0281(3) Uani 1 1 d . . . H1N H 0.2769(7) 0.621(2) 0.0809(9) 0.032(6) Uiso 1 1 d . . . N2 N 0.29006(5) 0.21642(18) 0.08790(6) 0.0242(3) Uani 1 1 d . . . H2N H 0.2735(7) 0.190(2) 0.0549(9) 0.030(5) Uiso 1 1 d . . . N3 N 0.38515(5) 0.15860(19) 0.07639(7) 0.0260(3) Uani 1 1 d . . . H3N H 0.3992(6) 0.159(2) 0.1071(8) 0.018(5) Uiso 1 1 d . . . N4 N 0.41849(5) 0.54162(17) 0.08603(6) 0.0217(3) Uani 1 1 d . . . N5 N 0.29637(5) 0.60408(18) -0.02397(6) 0.0274(3) Uani 1 1 d . . . C1 C 0.24352(7) 0.4459(2) 0.10651(9) 0.0341(4) Uani 1 1 d . . . H1A H 0.2266 0.4438 0.0674 0.041 Uiso 1 1 calc R . . H1B H 0.2225 0.4883 0.1323 0.041 Uiso 1 1 calc R . . C2 C 0.25746(6) 0.2800(2) 0.12461(8) 0.0291(4) Uani 1 1 d . . . H2A H 0.2721 0.2803 0.1648 0.035 Uiso 1 1 calc R . . H2B H 0.2298 0.2121 0.1219 0.035 Uiso 1 1 calc R . . C3 C 0.31422(7) 0.0742(2) 0.11142(8) 0.0302(4) Uani 1 1 d . . . H3A H 0.2920 -0.0137 0.1117 0.036 Uiso 1 1 calc R . . H3B H 0.3283 0.0941 0.1511 0.036 Uiso 1 1 calc R . . C4 C 0.35125(7) 0.0302(2) 0.07531(8) 0.0309(4) Uani 1 1 d . . . H4A H 0.3668 -0.0676 0.0902 0.037 Uiso 1 1 calc R . . H4B H 0.3371 0.0107 0.0356 0.037 Uiso 1 1 calc R . . C5 C 0.42047(7) 0.1295(3) 0.03836(8) 0.0356(5) Uani 1 1 d . . . H5A H 0.4338 0.0235 0.0465 0.043 Uiso 1 1 calc R . . H5B H 0.4456 0.2073 0.0470 0.043 Uiso 1 1 calc R . . C6 C 0.40221(6) 0.1399(2) -0.02412(8) 0.0272(4) Uani 1 1 d . . . C7 C 0.40270(8) 0.0124(3) -0.06072(11) 0.0476(6) Uani 1 1 d . . . H7 H 0.4123 -0.0876 -0.0456 0.057 Uiso 1 1 calc R . . C8 C 0.38959(9) 0.0277(3) -0.11868(11) 0.0543(7) Uani 1 1 d . . . H8 H 0.3904 -0.0613 -0.1429 0.065 Uiso 1 1 calc R . . C9 C 0.37546(7) 0.1698(4) -0.14135(9) 0.0504(7) Uani 1 1 d . . . H9 H 0.3665 0.1798 -0.1812 0.061 Uiso 1 1 calc R . . C10 C 0.37422(7) 0.2994(3) -0.10624(8) 0.0372(5) Uani 1 1 d . . . H10 H 0.3643 0.3987 -0.1217 0.045 Uiso 1 1 calc R . . C11 C 0.38765(6) 0.2824(2) -0.04838(7) 0.0231(4) Uani 1 1 d . . . C12 C 0.41523(6) 0.5402(2) -0.01798(8) 0.0278(4) Uani 1 1 d . . . H12A H 0.3971 0.6279 -0.0373 0.033 Uiso 1 1 calc R . . H12B H 0.4394 0.5101 -0.0415 0.033 Uiso 1 1 calc R . . C13 C 0.43721(6) 0.59213(19) 0.04014(7) 0.0232(4) Uani 1 1 d . . . C14 C 0.47591(6) 0.6877(2) 0.04500(8) 0.0288(4) Uani 1 1 d . . . H14 H 0.4880 0.7231 0.0119 0.035 Uiso 1 1 calc R . . C15 C 0.49669(6) 0.7308(2) 0.09857(9) 0.0323(4) Uani 1 1 d . . . H15 H 0.5228 0.7982 0.1029 0.039 Uiso 1 1 calc R . . C16 C 0.47881(6) 0.6743(2) 0.14580(8) 0.0302(4) Uani 1 1 d . . . H16 H 0.4931 0.6995 0.1831 0.036 Uiso 1 1 calc R . . C17 C 0.43969(6) 0.5801(2) 0.13801(7) 0.0236(4) Uani 1 1 d . . . C18 C 0.42126(6) 0.5128(2) 0.18940(8) 0.0290(4) Uani 1 1 d . . . H18A H 0.4398 0.4200 0.2036 0.035 Uiso 1 1 calc R . . H18B H 0.4236 0.5924 0.2202 0.035 Uiso 1 1 calc R . . C19 C 0.34846(6) 0.4574(2) 0.21949(7) 0.0248(4) Uani 1 1 d . . . C20 C 0.36168(7) 0.3650(2) 0.26669(8) 0.0343(4) Uani 1 1 d . . . H20 H 0.3899 0.3082 0.2704 0.041 Uiso 1 1 calc R . . C21 C 0.33282(7) 0.3566(2) 0.30887(8) 0.0346(4) Uani 1 1 d . . . H21 H 0.3413 0.2928 0.3415 0.041 Uiso 1 1 calc R . . C22 C 0.29239(7) 0.4394(2) 0.30379(8) 0.0308(4) Uani 1 1 d . . . H22 H 0.2732 0.4341 0.3331 0.037 Uiso 1 1 calc R . . C23 C 0.27959(7) 0.5305(2) 0.25604(8) 0.0311(4) Uani 1 1 d . . . H23 H 0.2513 0.5869 0.2526 0.037 Uiso 1 1 calc R . . C24 C 0.30742(6) 0.5410(2) 0.21296(7) 0.0254(4) Uani 1 1 d . . . C25 C 0.29388(8) 0.6422(2) 0.16118(8) 0.0350(5) Uani 1 1 d . . . H25A H 0.2661 0.7039 0.1668 0.042 Uiso 1 1 calc R . . H25B H 0.3191 0.7176 0.1574 0.042 Uiso 1 1 calc R . . Cd2 Cd 0.5000 0.09160(2) 0.2500 0.02503(5) Uani 1 2 d S . . O6 O 0.41913(5) 0.08720(17) 0.20883(7) 0.0477(4) Uani 1 1 d . . . O7 O 0.44855(5) -0.11932(17) 0.25204(6) 0.0378(3) Uani 1 1 d . . . O8 O 0.37742(5) -0.1229(2) 0.21297(7) 0.0513(4) Uani 1 1 d . . . O9 O 0.47860(5) 0.30083(18) 0.30525(6) 0.0421(4) Uani 1 1 d . . . O10 O 0.49656(8) 0.09208(19) 0.35309(7) 0.0655(6) Uani 1 1 d . . . O11 O 0.47586(6) 0.29793(19) 0.39660(6) 0.0485(4) Uani 1 1 d . . . N6 N 0.41397(5) -0.0527(2) 0.22430(7) 0.0310(4) Uani 1 1 d . . . N7 N 0.48365(5) 0.2315(2) 0.35273(7) 0.0318(4) 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 Cd1 0.02295(7) 0.02014(7) 0.01997(7) 0.00078(5) 0.00393(5) -0.00475(5) O1 0.0224(6) 0.0554(9) 0.0215(6) -0.0063(6) 0.0076(5) -0.0120(6) O2 0.0498(9) 0.0222(7) 0.0313(7) -0.0046(5) 0.0215(6) -0.0106(6) O3 0.0427(8) 0.0305(7) 0.0283(7) 0.0005(6) -0.0006(6) -0.0064(6) O4 0.0372(8) 0.0315(8) 0.0327(7) -0.0047(6) 0.0042(6) -0.0058(6) O5 0.0668(11) 0.0543(10) 0.0290(8) 0.0102(7) -0.0082(7) 0.0219(8) N1 0.0340(9) 0.0260(8) 0.0242(8) 0.0045(6) 0.0033(7) 0.0056(7) N2 0.0235(7) 0.0250(8) 0.0236(8) 0.0033(6) 0.0014(6) -0.0034(6) N3 0.0260(8) 0.0311(9) 0.0198(8) 0.0064(6) -0.0006(6) -0.0022(7) N4 0.0200(7) 0.0205(7) 0.0252(8) 0.0026(6) 0.0057(6) -0.0001(6) N5 0.0307(8) 0.0308(9) 0.0208(8) 0.0016(6) 0.0039(6) 0.0059(7) C1 0.0250(9) 0.0423(12) 0.0350(11) 0.0016(9) 0.0043(8) 0.0050(8) C2 0.0220(9) 0.0351(10) 0.0307(10) 0.0021(8) 0.0053(7) -0.0058(8) C3 0.0314(10) 0.0246(10) 0.0356(10) 0.0099(8) 0.0079(8) -0.0037(8) C4 0.0369(11) 0.0207(9) 0.0353(11) 0.0032(8) 0.0054(8) -0.0014(8) C5 0.0271(10) 0.0430(12) 0.0378(11) 0.0156(9) 0.0083(8) 0.0120(9) C6 0.0251(9) 0.0263(9) 0.0322(10) 0.0012(7) 0.0111(7) 0.0003(7) C7 0.0620(15) 0.0239(11) 0.0647(16) -0.0059(10) 0.0373(13) -0.0044(10) C8 0.0585(15) 0.0555(16) 0.0552(15) -0.0341(13) 0.0316(12) -0.0302(13) C9 0.0308(11) 0.095(2) 0.0260(11) -0.0193(12) 0.0068(9) -0.0141(12) C10 0.0314(10) 0.0557(14) 0.0250(10) 0.0052(9) 0.0055(8) 0.0090(10) C11 0.0218(8) 0.0259(9) 0.0225(9) -0.0026(7) 0.0063(7) -0.0023(7) C12 0.0330(10) 0.0227(9) 0.0295(10) 0.0055(7) 0.0108(8) -0.0048(8) C13 0.0226(8) 0.0195(8) 0.0289(9) 0.0036(7) 0.0082(7) 0.0032(7) C14 0.0257(9) 0.0256(10) 0.0377(11) 0.0044(8) 0.0144(8) -0.0013(7) C15 0.0206(9) 0.0311(10) 0.0468(12) -0.0026(9) 0.0098(8) -0.0054(8) C16 0.0209(9) 0.0342(11) 0.0359(11) -0.0063(8) 0.0046(7) -0.0037(8) C17 0.0190(8) 0.0243(9) 0.0278(9) -0.0006(7) 0.0041(7) 0.0016(7) C18 0.0197(8) 0.0397(11) 0.0270(9) 0.0041(8) 0.0007(7) -0.0026(8) C19 0.0234(9) 0.0312(10) 0.0208(9) -0.0045(7) 0.0065(7) -0.0043(7) C20 0.0334(10) 0.0440(12) 0.0255(10) 0.0015(8) 0.0042(8) 0.0122(9) C21 0.0495(12) 0.0319(10) 0.0237(10) 0.0032(8) 0.0101(9) 0.0021(9) C22 0.0374(11) 0.0293(10) 0.0289(10) -0.0070(8) 0.0158(8) -0.0094(8) C23 0.0302(10) 0.0334(10) 0.0313(10) -0.0077(8) 0.0103(8) 0.0032(8) C24 0.0321(10) 0.0208(9) 0.0240(9) -0.0042(7) 0.0060(7) -0.0001(7) C25 0.0499(12) 0.0242(10) 0.0314(10) -0.0002(8) 0.0068(9) 0.0096(9) Cd2 0.03065(10) 0.02334(10) 0.02143(9) 0.000 0.00463(7) 0.000 O6 0.0454(9) 0.0326(8) 0.0591(10) 0.0021(7) -0.0149(8) 0.0018(7) O7 0.0295(7) 0.0425(8) 0.0395(8) 0.0121(6) -0.0025(6) 0.0000(6) O8 0.0337(8) 0.0675(11) 0.0490(10) 0.0094(8) -0.0093(7) -0.0156(8) O9 0.0534(9) 0.0464(9) 0.0256(7) -0.0020(6) 0.0017(6) 0.0130(7) O10 0.1262(18) 0.0376(10) 0.0353(9) -0.0013(7) 0.0207(10) 0.0167(10) O11 0.0613(10) 0.0563(10) 0.0307(8) -0.0147(7) 0.0162(7) 0.0042(8) N6 0.0281(8) 0.0414(10) 0.0228(8) -0.0023(7) 0.0006(6) -0.0004(7) N7 0.0309(8) 0.0385(10) 0.0272(8) -0.0067(7) 0.0075(7) -0.0028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.3710(15) . ? Cd1 N1 2.3875(16) . ? Cd1 N4 2.4043(14) . ? Cd1 N3 2.4413(16) . ? Cd1 O2 2.4472(13) . ? Cd1 O3 2.5026(14) . ? Cd1 O1 2.5208(13) . ? Cd1 O4 2.6851(14) . ? O1 C19 1.393(2) . ? O1 C18 1.413(2) . ? O2 C11 1.383(2) . ? O2 C12 1.429(2) . ? O3 N5 1.270(2) . ? O4 N5 1.2536(19) . ? O5 N5 1.2300(19) . ? N1 C25 1.480(2) . ? N1 C1 1.481(3) . ? N1 H1N 0.87(2) . ? N2 C3 1.472(2) . ? N2 C2 1.475(2) . ? N2 H2N 0.89(2) . ? N3 C4 1.472(2) . ? N3 C5 1.478(2) . ? N3 H3N 0.788(19) . ? N4 C17 1.343(2) . ? N4 C13 1.350(2) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.507(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.383(3) . ? C6 C7 1.388(3) . ? C7 C8 1.381(4) . ? C7 H7 0.9500 . ? C8 C9 1.363(4) . ? C8 H8 0.9500 . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 C11 1.382(2) . ? C10 H10 0.9500 . ? C12 C13 1.506(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.386(2) . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.389(2) . ? C16 H16 0.9500 . ? C17 C18 1.507(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.378(3) . ? C19 C24 1.386(3) . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 C22 1.368(3) . ? C21 H21 0.9500 . ? C22 C23 1.380(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(2) . ? C23 H23 0.9500 . ? C24 C25 1.507(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Cd2 O9 2.3402(14) 2_655 ? Cd2 O9 2.3402(14) . ? Cd2 O7 2.3448(14) . ? Cd2 O7 2.3448(14) 2_655 ? Cd2 O6 2.4386(15) . ? Cd2 O6 2.4386(15) 2_655 ? Cd2 O10 2.4558(17) 2_655 ? Cd2 O10 2.4558(17) . ? O6 N6 1.258(2) . ? O7 N6 1.265(2) . ? O8 N6 1.223(2) . ? O9 N7 1.260(2) . ? O10 N7 1.243(2) . ? O11 N7 1.229(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 N2 Cd1 N1 74.68(6) . . ? N2 Cd1 N4 155.84(5) . . ? N1 Cd1 N4 114.71(5) . . ? N2 Cd1 N3 73.34(5) . . ? N1 Cd1 N3 142.97(5) . . ? N4 Cd1 N3 88.95(5) . . ? N2 Cd1 O2 122.51(5) . . ? N1 Cd1 O2 139.39(5) . . ? N4 Cd1 O2 65.99(5) . . ? N3 Cd1 O2 75.21(5) . . ? N2 Cd1 O3 81.37(5) . . ? N1 Cd1 O3 75.54(5) . . ? N4 Cd1 O3 121.98(5) . . ? N3 Cd1 O3 116.99(5) . . ? O2 Cd1 O3 71.96(5) . . ? N2 Cd1 O1 97.75(5) . . ? N1 Cd1 O1 74.96(5) . . ? N4 Cd1 O1 65.69(4) . . ? N3 Cd1 O1 91.34(5) . . ? O2 Cd1 O1 129.86(4) . . ? O3 Cd1 O1 149.60(5) . . ? N2 Cd1 O4 124.96(5) . . ? N1 Cd1 O4 71.08(5) . . ? N4 Cd1 O4 78.88(4) . . ? N3 Cd1 O4 144.54(5) . . ? O2 Cd1 O4 69.39(4) . . ? O3 Cd1 O4 49.25(4) . . ? O1 Cd1 O4 112.87(5) . . ? C19 O1 C18 116.17(14) . . ? C19 O1 Cd1 124.56(10) . . ? C18 O1 Cd1 119.26(10) . . ? C11 O2 C12 117.99(13) . . ? C11 O2 Cd1 125.16(10) . . ? C12 O2 Cd1 116.14(10) . . ? N5 O3 Cd1 100.27(10) . . ? N5 O4 Cd1 91.94(10) . . ? C25 N1 C1 113.41(16) . . ? C25 N1 Cd1 119.69(12) . . ? C1 N1 Cd1 109.20(11) . . ? C25 N1 H1N 105.4(14) . . ? C1 N1 H1N 106.1(13) . . ? Cd1 N1 H1N 101.4(14) . . ? C3 N2 C2 113.16(14) . . ? C3 N2 Cd1 109.32(11) . . ? C2 N2 Cd1 110.11(11) . . ? C3 N2 H2N 107.4(13) . . ? C2 N2 H2N 106.9(13) . . ? Cd1 N2 H2N 109.9(13) . . ? C4 N3 C5 112.93(16) . . ? C4 N3 Cd1 109.27(11) . . ? C5 N3 Cd1 119.45(11) . . ? C4 N3 H3N 106.9(14) . . ? C5 N3 H3N 104.0(13) . . ? Cd1 N3 H3N 103.0(14) . . ? C17 N4 C13 118.19(15) . . ? C17 N4 Cd1 122.44(11) . . ? C13 N4 Cd1 119.05(11) . . ? O5 N5 O4 121.12(16) . . ? O5 N5 O3 120.43(16) . . ? O4 N5 O3 118.45(14) . . ? N1 C1 C2 111.59(15) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 110.18(15) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C4 109.45(15) . . ? N2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N3 C4 C3 109.83(15) . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 113.69(15) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C11 C6 C7 116.82(18) . . ? C11 C6 C5 120.57(17) . . ? C7 C6 C5 122.40(19) . . ? C8 C7 C6 121.5(2) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 120.3(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.1(2) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C6 122.34(18) . . ? C10 C11 O2 120.51(17) . . ? C6 C11 O2 117.13(15) . . ? O2 C12 C13 109.14(14) . . ? O2 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? O2 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 C14 122.24(17) . . ? N4 C13 C12 118.19(15) . . ? C14 C13 C12 119.57(16) . . ? C15 C14 C13 119.18(17) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 118.88(17) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.09(18) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N4 C17 C16 122.33(16) . . ? N4 C17 C18 118.42(15) . . ? C16 C17 C18 119.20(16) . . ? O1 C18 C17 109.81(14) . . ? O1 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O1 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C24 121.90(17) . . ? C20 C19 O1 122.03(17) . . ? C24 C19 O1 116.04(16) . . ? C19 C20 C21 118.57(18) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 120.70(18) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.89(17) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.99(18) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 117.95(17) . . ? C19 C24 C25 120.93(16) . . ? C23 C24 C25 121.11(17) . . ? N1 C25 C24 113.30(15) . . ? N1 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N1 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O9 Cd2 O9 81.20(8) 2_655 . ? O9 Cd2 O7 144.24(5) 2_655 . ? O9 Cd2 O7 110.39(5) . . ? O9 Cd2 O7 110.39(5) 2_655 2_655 ? O9 Cd2 O7 144.24(5) . 2_655 ? O7 Cd2 O7 80.39(7) . 2_655 ? O9 Cd2 O6 96.05(5) 2_655 . ? O9 Cd2 O6 85.29(5) . . ? O7 Cd2 O6 53.43(5) . . ? O7 Cd2 O6 124.91(5) 2_655 . ? O9 Cd2 O6 85.29(5) 2_655 2_655 ? O9 Cd2 O6 96.05(5) . 2_655 ? O7 Cd2 O6 124.91(5) . 2_655 ? O7 Cd2 O6 53.43(5) 2_655 2_655 ? O6 Cd2 O6 178.24(7) . 2_655 ? O9 Cd2 O10 52.71(5) 2_655 2_655 ? O9 Cd2 O10 127.10(5) . 2_655 ? O7 Cd2 O10 97.61(6) . 2_655 ? O7 Cd2 O10 82.54(6) 2_655 2_655 ? O6 Cd2 O10 76.56(7) . 2_655 ? O6 Cd2 O10 103.44(7) 2_655 2_655 ? O9 Cd2 O10 127.10(5) 2_655 . ? O9 Cd2 O10 52.71(5) . . ? O7 Cd2 O10 82.54(6) . . ? O7 Cd2 O10 97.61(6) 2_655 . ? O6 Cd2 O10 103.44(7) . . ? O6 Cd2 O10 76.56(7) 2_655 . ? O10 Cd2 O10 179.81(9) 2_655 . ? N6 O6 Cd2 92.62(11) . . ? N6 O7 Cd2 96.88(11) . . ? N7 O9 Cd2 97.79(11) . . ? N7 O10 Cd2 92.70(11) . . ? O8 N6 O6 122.11(17) . . ? O8 N6 O7 120.84(17) . . ? O6 N6 O7 117.04(16) . . ? O11 N7 O10 121.43(18) . . ? O11 N7 O9 121.77(18) . . ? O10 N7 O9 116.80(16) . . ? 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 N2 Cd1 O1 C19 -31.22(14) . . . . ? N1 Cd1 O1 C19 40.56(14) . . . . ? N4 Cd1 O1 C19 167.17(15) . . . . ? N3 Cd1 O1 C19 -104.59(14) . . . . ? O2 Cd1 O1 C19 -176.34(12) . . . . ? O3 Cd1 O1 C19 54.93(18) . . . . ? O4 Cd1 O1 C19 102.02(14) . . . . ? N2 Cd1 O1 C18 148.11(13) . . . . ? N1 Cd1 O1 C18 -140.11(14) . . . . ? N4 Cd1 O1 C18 -13.49(13) . . . . ? N3 Cd1 O1 C18 74.75(14) . . . . ? O2 Cd1 O1 C18 2.99(16) . . . . ? O3 Cd1 O1 C18 -125.74(13) . . . . ? O4 Cd1 O1 C18 -78.65(14) . . . . ? N2 Cd1 O2 C11 -14.46(15) . . . . ? N1 Cd1 O2 C11 -119.64(14) . . . . ? N4 Cd1 O2 C11 139.77(15) . . . . ? N3 Cd1 O2 C11 44.22(13) . . . . ? O3 Cd1 O2 C11 -81.21(14) . . . . ? O1 Cd1 O2 C11 123.32(13) . . . . ? O4 Cd1 O2 C11 -133.55(14) . . . . ? N2 Cd1 O2 C12 175.43(11) . . . . ? N1 Cd1 O2 C12 70.25(15) . . . . ? N4 Cd1 O2 C12 -30.34(12) . . . . ? N3 Cd1 O2 C12 -125.89(13) . . . . ? O3 Cd1 O2 C12 108.68(13) . . . . ? O1 Cd1 O2 C12 -46.79(14) . . . . ? O4 Cd1 O2 C12 56.34(12) . . . . ? N2 Cd1 O3 N5 155.33(11) . . . . ? N1 Cd1 O3 N5 79.04(11) . . . . ? N4 Cd1 O3 N5 -31.33(12) . . . . ? N3 Cd1 O3 N5 -138.41(10) . . . . ? O2 Cd1 O3 N5 -76.26(10) . . . . ? O1 Cd1 O3 N5 64.70(14) . . . . ? O4 Cd1 O3 N5 1.74(9) . . . . ? N2 Cd1 O4 N5 -34.18(12) . . . . ? N1 Cd1 O4 N5 -88.69(10) . . . . ? N4 Cd1 O4 N5 150.12(10) . . . . ? N3 Cd1 O4 N5 78.07(13) . . . . ? O2 Cd1 O4 N5 81.78(10) . . . . ? O3 Cd1 O4 N5 -1.73(9) . . . . ? O1 Cd1 O4 N5 -152.45(9) . . . . ? N2 Cd1 N1 C25 120.07(14) . . . . ? N4 Cd1 N1 C25 -36.18(15) . . . . ? N3 Cd1 N1 C25 89.03(16) . . . . ? O2 Cd1 N1 C25 -117.48(13) . . . . ? O3 Cd1 N1 C25 -155.09(14) . . . . ? O1 Cd1 N1 C25 17.45(13) . . . . ? O4 Cd1 N1 C25 -103.71(14) . . . . ? N2 Cd1 N1 C1 -12.99(11) . . . . ? N4 Cd1 N1 C1 -169.25(11) . . . . ? N3 Cd1 N1 C1 -44.03(16) . . . . ? O2 Cd1 N1 C1 109.46(12) . . . . ? O3 Cd1 N1 C1 71.84(12) . . . . ? O1 Cd1 N1 C1 -115.61(12) . . . . ? O4 Cd1 N1 C1 123.22(12) . . . . ? N1 Cd1 N2 C3 -140.69(13) . . . . ? N4 Cd1 N2 C3 -24.0(2) . . . . ? N3 Cd1 N2 C3 20.40(11) . . . . ? O2 Cd1 N2 C3 79.95(13) . . . . ? O3 Cd1 N2 C3 142.03(12) . . . . ? O1 Cd1 N2 C3 -68.68(12) . . . . ? O4 Cd1 N2 C3 166.31(10) . . . . ? N1 Cd1 N2 C2 -15.79(11) . . . . ? N4 Cd1 N2 C2 100.85(15) . . . . ? N3 Cd1 N2 C2 145.30(12) . . . . ? O2 Cd1 N2 C2 -155.14(10) . . . . ? O3 Cd1 N2 C2 -93.06(11) . . . . ? O1 Cd1 N2 C2 56.23(11) . . . . ? O4 Cd1 N2 C2 -68.79(12) . . . . ? N2 Cd1 N3 C4 10.68(11) . . . . ? N1 Cd1 N3 C4 41.95(16) . . . . ? N4 Cd1 N3 C4 174.02(12) . . . . ? O2 Cd1 N3 C4 -120.56(12) . . . . ? O3 Cd1 N3 C4 -60.16(12) . . . . ? O1 Cd1 N3 C4 108.38(12) . . . . ? O4 Cd1 N3 C4 -116.96(12) . . . . ? N2 Cd1 N3 C5 142.85(15) . . . . ? N1 Cd1 N3 C5 174.12(12) . . . . ? N4 Cd1 N3 C5 -53.80(14) . . . . ? O2 Cd1 N3 C5 11.61(13) . . . . ? O3 Cd1 N3 C5 72.01(14) . . . . ? O1 Cd1 N3 C5 -119.45(14) . . . . ? O4 Cd1 N3 C5 15.21(18) . . . . ? N2 Cd1 N4 C17 -49.3(2) . . . . ? N1 Cd1 N4 C17 59.03(14) . . . . ? N3 Cd1 N4 C17 -91.49(13) . . . . ? O2 Cd1 N4 C17 -165.75(14) . . . . ? O3 Cd1 N4 C17 146.93(12) . . . . ? O1 Cd1 N4 C17 0.45(12) . . . . ? O4 Cd1 N4 C17 122.02(13) . . . . ? N2 Cd1 N4 C13 137.30(14) . . . . ? N1 Cd1 N4 C13 -114.32(12) . . . . ? N3 Cd1 N4 C13 95.16(13) . . . . ? O2 Cd1 N4 C13 20.90(11) . . . . ? O3 Cd1 N4 C13 -26.41(14) . . . . ? O1 Cd1 N4 C13 -172.89(14) . . . . ? O4 Cd1 N4 C13 -51.33(12) . . . . ? Cd1 O4 N5 O5 -176.90(16) . . . . ? Cd1 O4 N5 O3 2.95(16) . . . . ? Cd1 O3 N5 O5 176.64(15) . . . . ? Cd1 O3 N5 O4 -3.21(17) . . . . ? C25 N1 C1 C2 -95.82(19) . . . . ? Cd1 N1 C1 C2 40.42(18) . . . . ? C3 N2 C2 C1 165.15(15) . . . . ? Cd1 N2 C2 C1 42.47(17) . . . . ? N1 C1 C2 N2 -57.1(2) . . . . ? C2 N2 C3 C4 -172.46(15) . . . . ? Cd1 N2 C3 C4 -49.34(17) . . . . ? C5 N3 C4 C3 -175.46(15) . . . . ? Cd1 N3 C4 C3 -39.95(17) . . . . ? N2 C3 C4 N3 61.4(2) . . . . ? C4 N3 C5 C6 70.5(2) . . . . ? Cd1 N3 C5 C6 -60.1(2) . . . . ? N3 C5 C6 C11 67.7(2) . . . . ? N3 C5 C6 C7 -117.8(2) . . . . ? C11 C6 C7 C8 0.5(3) . . . . ? C5 C6 C7 C8 -174.22(19) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C9 C10 C11 C6 -0.2(3) . . . . ? C9 C10 C11 O2 -178.44(17) . . . . ? C7 C6 C11 C10 -0.1(3) . . . . ? C5 C6 C11 C10 174.64(17) . . . . ? C7 C6 C11 O2 178.12(16) . . . . ? C5 C6 C11 O2 -7.1(2) . . . . ? C12 O2 C11 C10 -64.9(2) . . . . ? Cd1 O2 C11 C10 125.12(15) . . . . ? C12 O2 C11 C6 116.77(18) . . . . ? Cd1 O2 C11 C6 -53.2(2) . . . . ? C11 O2 C12 C13 -135.57(16) . . . . ? Cd1 O2 C12 C13 35.29(18) . . . . ? C17 N4 C13 C14 -3.2(2) . . . . ? Cd1 N4 C13 C14 170.47(13) . . . . ? C17 N4 C13 C12 176.09(15) . . . . ? Cd1 N4 C13 C12 -10.3(2) . . . . ? O2 C12 C13 N4 -16.5(2) . . . . ? O2 C12 C13 C14 162.74(15) . . . . ? N4 C13 C14 C15 1.2(3) . . . . ? C12 C13 C14 C15 -178.05(17) . . . . ? C13 C14 C15 C16 1.5(3) . . . . ? C14 C15 C16 C17 -2.0(3) . . . . ? C13 N4 C17 C16 2.5(3) . . . . ? Cd1 N4 C17 C16 -170.87(13) . . . . ? C13 N4 C17 C18 -174.92(15) . . . . ? Cd1 N4 C17 C18 11.7(2) . . . . ? C15 C16 C17 N4 0.0(3) . . . . ? C15 C16 C17 C18 177.48(17) . . . . ? C19 O1 C18 C17 -157.92(16) . . . . ? Cd1 O1 C18 C17 22.7(2) . . . . ? N4 C17 C18 O1 -22.1(2) . . . . ? C16 C17 C18 O1 160.33(16) . . . . ? C18 O1 C19 C20 -54.7(2) . . . . ? Cd1 O1 C19 C20 124.62(17) . . . . ? C18 O1 C19 C24 127.38(18) . . . . ? Cd1 O1 C19 C24 -53.3(2) . . . . ? C24 C19 C20 C21 -0.2(3) . . . . ? O1 C19 C20 C21 -178.01(18) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C20 C21 C22 C23 0.9(3) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C20 C19 C24 C23 0.6(3) . . . . ? O1 C19 C24 C23 178.46(16) . . . . ? C20 C19 C24 C25 179.52(18) . . . . ? O1 C19 C24 C25 -2.6(3) . . . . ? C22 C23 C24 C19 -0.1(3) . . . . ? C22 C23 C24 C25 -179.09(18) . . . . ? C1 N1 C25 C24 64.8(2) . . . . ? Cd1 N1 C25 C24 -66.5(2) . . . . ? C19 C24 C25 N1 66.8(2) . . . . ? C23 C24 C25 N1 -114.3(2) . . . . ? O9 Cd2 O6 N6 158.80(11) 2_655 . . . ? O9 Cd2 O6 N6 -120.59(12) . . . . ? O7 Cd2 O6 N6 -0.82(10) . . . . ? O7 Cd2 O6 N6 38.71(14) 2_655 . . . ? O6 Cd2 O6 N6 19.16(11) 2_655 . . . ? O10 Cd2 O6 N6 109.47(12) 2_655 . . . ? O10 Cd2 O6 N6 -70.73(12) . . . . ? O9 Cd2 O7 N6 -35.53(16) 2_655 . . . ? O9 Cd2 O7 N6 68.18(11) . . . . ? O7 Cd2 O7 N6 -147.22(13) 2_655 . . . ? O6 Cd2 O7 N6 0.82(10) . . . . ? O6 Cd2 O7 N6 -178.45(10) 2_655 . . . ? O10 Cd2 O7 N6 -66.17(12) 2_655 . . . ? O10 Cd2 O7 N6 113.71(12) . . . . ? O9 Cd2 O9 N7 -152.10(14) 2_655 . . . ? O7 Cd2 O9 N7 62.96(12) . . . . ? O7 Cd2 O9 N7 -39.25(16) 2_655 . . . ? O6 Cd2 O9 N7 111.01(11) . . . . ? O6 Cd2 O9 N7 -67.85(11) 2_655 . . . ? O10 Cd2 O9 N7 -179.77(11) 2_655 . . . ? O10 Cd2 O9 N7 0.16(11) . . . . ? O9 Cd2 O10 N7 35.05(17) 2_655 . . . ? O9 Cd2 O10 N7 -0.16(11) . . . . ? O7 Cd2 O10 N7 -122.94(14) . . . . ? O7 Cd2 O10 N7 157.86(13) 2_655 . . . ? O6 Cd2 O10 N7 -73.41(14) . . . . ? O6 Cd2 O10 N7 108.39(14) 2_655 . . . ? O10 Cd2 O10 N7 17.5(2) 2_655 . . . ? Cd2 O6 N6 O8 -178.13(16) . . . . ? Cd2 O6 N6 O7 1.36(17) . . . . ? Cd2 O7 N6 O8 178.07(15) . . . . ? Cd2 O7 N6 O6 -1.43(18) . . . . ? Cd2 O10 N7 O11 179.71(15) . . . . ? Cd2 O10 N7 O9 0.27(18) . . . . ? Cd2 O9 N7 O11 -179.73(15) . . . . ? Cd2 O9 N7 O10 -0.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N O6 0.788(19) 2.478(19) 3.219(2) 157.5(17) . N2 H2N O3 0.89(2) 2.30(2) 3.069(2) 144.2(17) 7 N1 H1N O5 0.87(2) 2.34(2) 3.029(2) 135.4(18) 7_565 N1 H1N O4 0.87(2) 2.40(2) 2.958(2) 121.8(17) . N1 H1N N5 0.87(2) 2.62(2) 3.218(2) 126.2(17) . _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.762 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.062 #===END data_lfl51 _database_code_CSD 178690 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H62 Ag3 N11 O14' _chemical_formula_weight 1364.72 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.470(3) _cell_length_b 20.354(5) _cell_length_c 10.173(2) _cell_angle_alpha 79.900(4) _cell_angle_beta 108.100(4) _cell_angle_gamma 100.973(4) _cell_volume 2774.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 2.640 _cell_measurement_theta_max 25.783 _exptl_crystal_description blade _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.202 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.063 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8130 _exptl_absorpt_correction_T_max 0.9367 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 171 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 27139 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12729 _reflns_number_gt 8768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997), XSHELL (Bruker, 2000) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _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^)+(0.0300P)^2^+2.0000P] 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 12729 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.73227(2) 0.135228(17) 0.82150(3) 0.03681(9) Uani 1 1 d . . . Ag2 Ag 0.5000 0.0000 0.5000 0.03166(11) Uani 1 2 d S . . O1 O 0.89332(19) 0.21480(13) 0.9608(3) 0.0356(6) Uani 1 1 d . . . O2 O 0.49204(19) 0.12266(13) 0.8052(3) 0.0351(6) Uani 1 1 d . . . O3 O 0.6287(3) 0.01920(17) 0.8145(4) 0.0674(10) Uani 1 1 d . . . O4 O 0.7333(3) -0.03797(18) 0.7920(5) 0.0821(13) Uani 1 1 d . . . O5 O 0.5921(2) -0.08759(16) 0.8098(3) 0.0568(9) Uani 1 1 d . . . N1 N 0.8744(2) 0.08479(15) 0.8380(3) 0.0305(7) Uani 1 1 d . . . H1 H 0.8604 0.0392 0.8682 0.037 Uiso 1 1 calc R . . N2 N 0.7489(2) 0.16723(16) 0.5966(3) 0.0319(7) Uani 1 1 d . . . H2 H 0.7473 0.2135 0.5780 0.038 Uiso 1 1 calc R . . N3 N 0.5225(2) 0.10509(14) 0.5327(3) 0.0282(7) Uani 1 1 d . . . H3 H 0.5608 0.1073 0.6245 0.034 Uiso 1 1 calc R . . N4 N 0.6909(2) 0.19249(16) 0.9603(3) 0.0314(7) Uani 1 1 d . . . N5 N 0.6517(3) -0.03509(19) 0.8041(3) 0.0419(9) Uani 1 1 d . . . C1 C 0.8739(3) 0.0897(2) 0.6918(4) 0.0338(9) Uani 1 1 d . . . H1A H 0.8236 0.0541 0.6457 0.041 Uiso 1 1 calc R . . H1B H 0.9387 0.0824 0.6881 0.041 Uiso 1 1 calc R . . C2 C 0.8517(3) 0.1585(2) 0.6147(4) 0.0370(10) Uani 1 1 d . . . H2A H 0.8971 0.1941 0.6675 0.044 Uiso 1 1 calc R . . H2B H 0.8630 0.1637 0.5221 0.044 Uiso 1 1 calc R . . C3 C 0.6805(3) 0.1380(2) 0.4723(4) 0.0355(9) Uani 1 1 d . . . H3A H 0.6802 0.0886 0.4862 0.043 Uiso 1 1 calc R . . H3B H 0.7039 0.1570 0.3899 0.043 Uiso 1 1 calc R . . C4 C 0.5776(3) 0.1523(2) 0.4451(4) 0.0359(10) Uani 1 1 d . . . H4A H 0.5804 0.1990 0.4632 0.043 Uiso 1 1 calc R . . H4B H 0.5417 0.1493 0.3456 0.043 Uiso 1 1 calc R . . C5 C 0.4299(3) 0.13061(19) 0.5205(4) 0.0312(9) Uani 1 1 d . . . H5A H 0.3896 0.1341 0.4217 0.037 Uiso 1 1 calc R . . H5B H 0.4461 0.1763 0.5497 0.037 Uiso 1 1 calc R . . C6 C 0.3713(3) 0.08533(19) 0.6083(4) 0.0299(9) Uani 1 1 d . . . C7 C 0.2824(3) 0.0477(2) 0.5488(4) 0.0372(10) Uani 1 1 d . . . H7 H 0.2568 0.0518 0.4501 0.045 Uiso 1 1 calc R . . C8 C 0.2295(3) 0.0039(2) 0.6304(5) 0.0424(11) Uani 1 1 d . . . H8 H 0.1682 -0.0213 0.5880 0.051 Uiso 1 1 calc R . . C9 C 0.2672(3) -0.0023(2) 0.7728(5) 0.0450(11) Uani 1 1 d . . . H9 H 0.2323 -0.0329 0.8288 0.054 Uiso 1 1 calc R . . C10 C 0.3551(3) 0.0355(2) 0.8361(4) 0.0400(10) Uani 1 1 d . . . H10 H 0.3802 0.0311 0.9349 0.048 Uiso 1 1 calc R . . C11 C 0.4062(3) 0.07965(19) 0.7542(4) 0.0321(9) Uani 1 1 d . . . C12 C 0.5409(3) 0.1121(2) 0.9524(4) 0.0419(11) Uani 1 1 d . . . H12A H 0.5805 0.0749 0.9728 0.050 Uiso 1 1 calc R . . H12B H 0.4916 0.0995 1.0051 0.050 Uiso 1 1 calc R . . C13 C 0.6059(3) 0.1755(2) 0.9956(4) 0.0347(9) Uani 1 1 d . . . C14 C 0.5802(3) 0.2146(2) 1.0748(4) 0.0424(11) Uani 1 1 d . . . H14 H 0.5194 0.2023 1.0966 0.051 Uiso 1 1 calc R . . C15 C 0.6424(3) 0.2706(2) 1.1209(4) 0.0478(12) Uani 1 1 d . . . H15 H 0.6261 0.2973 1.1760 0.057 Uiso 1 1 calc R . . C16 C 0.7284(3) 0.2875(2) 1.0863(4) 0.0428(11) Uani 1 1 d . . . H16 H 0.7729 0.3261 1.1176 0.051 Uiso 1 1 calc R . . C17 C 0.7508(3) 0.2481(2) 1.0055(4) 0.0344(9) Uani 1 1 d . . . C18 C 0.8455(3) 0.2691(2) 0.9644(5) 0.0404(10) Uani 1 1 d . . . H18A H 0.8308 0.2959 0.8711 0.048 Uiso 1 1 calc R . . H18B H 0.8915 0.2989 1.0311 0.048 Uiso 1 1 calc R . . C19 C 0.9331(3) 0.1764(2) 1.0837(4) 0.0328(9) Uani 1 1 d . . . C20 C 0.9381(3) 0.1904(2) 1.2136(4) 0.0409(10) Uani 1 1 d . . . H20 H 0.9115 0.2280 1.2229 0.049 Uiso 1 1 calc R . . C21 C 0.9831(3) 0.1483(3) 1.3321(5) 0.0486(12) Uani 1 1 d . . . H21 H 0.9874 0.1579 1.4221 0.058 Uiso 1 1 calc R . . C22 C 1.0212(3) 0.0934(2) 1.3198(5) 0.0482(12) Uani 1 1 d . . . H22 H 1.0508 0.0648 1.4003 0.058 Uiso 1 1 calc R . . C23 C 1.0157(3) 0.0803(2) 1.1876(4) 0.0414(10) Uani 1 1 d . . . H23 H 1.0423 0.0425 1.1791 0.050 Uiso 1 1 calc R . . C24 C 0.9727(3) 0.12072(19) 1.0681(4) 0.0330(9) Uani 1 1 d . . . C25 C 0.9730(3) 0.1089(2) 0.9278(4) 0.0342(9) Uani 1 1 d . . . H25A H 1.0002 0.1515 0.8804 0.041 Uiso 1 1 calc R . . H25B H 1.0170 0.0752 0.9395 0.041 Uiso 1 1 calc R . . Ag3 Ag 0.73696(3) 0.619329(18) 0.86691(4) 0.05604(12) Uani 1 1 d . . . Ag4 Ag 0.5000 0.5000 0.5000 0.03656(12) Uani 1 2 d S . . O6 O 0.8910(2) 0.69698(16) 1.0191(3) 0.0478(8) Uani 1 1 d . . . O7 O 0.6442(2) 0.44985(16) 0.9407(3) 0.0505(8) Uani 1 1 d . . . O8 O 0.5421(3) 0.5905(2) 0.7430(6) 0.0921(15) Uani 1 1 d . . . O9 O 0.4988(3) 0.6909(2) 0.6957(5) 0.0802(12) Uani 1 1 d . . . O10 O 0.3969(4) 0.6080(2) 0.6265(5) 0.127(2) Uani 1 1 d . . . N6 N 0.7144(2) 0.73216(17) 0.7762(3) 0.0431(9) Uani 1 1 d . . . H6 H 0.6513 0.7370 0.7741 0.052 Uiso 1 1 calc R . . N7 N 0.7838(2) 0.62714(17) 0.6636(4) 0.0440(9) Uani 1 1 d . . . H7A H 0.8465 0.6150 0.6932 0.053 Uiso 1 1 calc R . . N8 N 0.6456(2) 0.48604(16) 0.6415(3) 0.0366(8) Uani 1 1 d . . . H8A H 0.6548 0.5098 0.7158 0.044 Uiso 1 1 calc R . . N9 N 0.7913(3) 0.56560(18) 1.0816(4) 0.0444(9) Uani 1 1 d . . . N10 N 0.4811(3) 0.6300(2) 0.6877(4) 0.0505(10) Uani 1 1 d . . . C26 C 0.7151(3) 0.7339(2) 0.6315(4) 0.0483(12) Uani 1 1 d . . . H26A H 0.7217 0.7813 0.5879 0.058 Uiso 1 1 calc R . . H26B H 0.6517 0.7101 0.5785 0.058 Uiso 1 1 calc R . . C27 C 0.7981(3) 0.7012(2) 0.6230(5) 0.0515(13) Uani 1 1 d . . . H27A H 0.8032 0.7106 0.5265 0.062 Uiso 1 1 calc R . . H27B H 0.8607 0.7213 0.6850 0.062 Uiso 1 1 calc R . . C28 C 0.7312(3) 0.5916(2) 0.5418(5) 0.0470(12) Uani 1 1 d . . . H28A H 0.7654 0.6066 0.4688 0.056 Uiso 1 1 calc R . . H28B H 0.6640 0.6036 0.5035 0.056 Uiso 1 1 calc R . . C29 C 0.7248(3) 0.5159(2) 0.5769(5) 0.0454(11) Uani 1 1 d . . . H29A H 0.7134 0.4956 0.4907 0.055 Uiso 1 1 calc R . . H29B H 0.7884 0.5048 0.6417 0.055 Uiso 1 1 calc R . . C30 C 0.6562(3) 0.4147(2) 0.7026(5) 0.0445(11) Uani 1 1 d . . . H30A H 0.7192 0.4135 0.7773 0.053 Uiso 1 1 calc R . . H30B H 0.6576 0.3888 0.6296 0.053 Uiso 1 1 calc R . . C31 C 0.5731(3) 0.3824(2) 0.7616(5) 0.0435(11) Uani 1 1 d . . . C32 C 0.5036(3) 0.3318(2) 0.7017(5) 0.0563(13) Uani 1 1 d . . . H32 H 0.5096 0.3157 0.6229 0.068 Uiso 1 1 calc R . . C33 C 0.4252(4) 0.3038(3) 0.7533(6) 0.0666(16) Uani 1 1 d . . . H33 H 0.3779 0.2688 0.7109 0.080 Uiso 1 1 calc R . . C34 C 0.4166(3) 0.3272(3) 0.8668(6) 0.0642(17) Uani 1 1 d . . . H34 H 0.3619 0.3088 0.9012 0.077 Uiso 1 1 calc R . . C35 C 0.4862(3) 0.3775(2) 0.9327(5) 0.0549(14) Uani 1 1 d . . . H35 H 0.4797 0.3934 1.0113 0.066 Uiso 1 1 calc R . . C36 C 0.5659(3) 0.4038(2) 0.8800(5) 0.0461(12) Uani 1 1 d . . . C37 C 0.6372(4) 0.4876(2) 1.0425(6) 0.0643(16) Uani 1 1 d . . . H37A H 0.5981 0.4593 1.1017 0.077 Uiso 1 1 calc R . . H37B H 0.6042 0.5274 0.9958 0.077 Uiso 1 1 calc R . . C38 C 0.7396(4) 0.5099(2) 1.1305(5) 0.0498(13) Uani 1 1 d . . . C39 C 0.7801(6) 0.4730(2) 1.2569(5) 0.088(2) Uani 1 1 d . . . H39 H 0.7432 0.4330 1.2888 0.105 Uiso 1 1 calc R . . C40 C 0.8727(7) 0.4941(3) 1.3355(5) 0.109(3) Uani 1 1 d . . . H40 H 0.9007 0.4692 1.4226 0.131 Uiso 1 1 calc R . . C41 C 0.9244(5) 0.5512(3) 1.2872(5) 0.0695(17) Uani 1 1 d . . . H41 H 0.9888 0.5671 1.3412 0.083 Uiso 1 1 calc R . . C42 C 0.8831(4) 0.5860(2) 1.1599(4) 0.0461(11) Uani 1 1 d . . . C43 C 0.9436(3) 0.6444(3) 1.1007(5) 0.0589(14) Uani 1 1 d . . . H43A H 0.9964 0.6635 1.1784 0.071 Uiso 1 1 calc R . . H43B H 0.9753 0.6277 1.0422 0.071 Uiso 1 1 calc R . . C44 C 0.8585(3) 0.7372(2) 1.0862(5) 0.0481(12) Uani 1 1 d . . . C45 C 0.8825(3) 0.7355(3) 1.2310(5) 0.0553(14) Uani 1 1 d . . . H45 H 0.9205 0.7031 1.2914 0.066 Uiso 1 1 calc R . . C46 C 0.8502(4) 0.7815(3) 1.2844(6) 0.0632(15) Uani 1 1 d . . . H46 H 0.8674 0.7810 1.3826 0.076 Uiso 1 1 calc R . . C47 C 0.7940(4) 0.8279(3) 1.1996(6) 0.0647(15) Uani 1 1 d . . . H47 H 0.7723 0.8592 1.2385 0.078 Uiso 1 1 calc R . . C48 C 0.7690(3) 0.8288(3) 1.0570(5) 0.0565(13) Uani 1 1 d . . . H48 H 0.7289 0.8606 0.9985 0.068 Uiso 1 1 calc R . . C49 C 0.8010(3) 0.7846(2) 0.9963(5) 0.0495(12) Uani 1 1 d . . . C50 C 0.7829(3) 0.7899(2) 0.8409(4) 0.0515(13) Uani 1 1 d . . . H50A H 0.7556 0.8321 0.7967 0.062 Uiso 1 1 calc R . . H50B H 0.8465 0.7929 0.8212 0.062 Uiso 1 1 calc R . . N11 N 0.9454(4) 0.3490(3) 0.4461(6) 0.025(3) Uiso 0.25 1 d PG . . O11 O 1.0319(5) 0.3671(7) 0.4504(10) 0.037(4) Uiso 0.25 1 d PG . . O12 O 0.8916(6) 0.3216(5) 0.3468(9) 0.030(3) Uiso 0.25 1 d PG . . O13 O 0.9188(6) 0.3483(5) 0.5500(8) 0.032(2) Uiso 0.25 1 d PG . . N12 N 0.9738(3) 0.35378(19) 0.3598(4) 0.0284(14) Uiso 0.50 1 d PG . . O14A O 0.9074(5) 0.3102(3) 0.3819(6) 0.033(3) Uiso 0.30 1 d PG . . O14B O 0.8957(3) 0.3556(4) 0.3172(6) 0.047(3) Uiso 0.20 1 d PG . . O15A O 1.0334(4) 0.3781(4) 0.4590(5) 0.033(3) Uiso 0.30 1 d PG . . O15B O 1.0383(4) 0.3371(5) 0.4656(4) 0.047(3) Uiso 0.20 1 d PG . . O16 O 0.9884(3) 0.3637(2) 0.2448(4) 0.0350(13) Uiso 0.50 1 d PG . . N13 N 0.9988(6) 0.4583(4) 0.0658(8) 0.067(5) Uiso 0.25 1 d PG . . O17 O 1.0200(8) 0.4067(4) 0.1432(10) 0.048(2) Uiso 0.25 1 d PG . . O18 O 1.0640(7) 0.5058(4) 0.0638(12) 0.048(2) Uiso 0.25 1 d PG . . O19 O 0.9187(7) 0.4575(6) -0.0231(13) 0.093(5) Uiso 0.25 1 d PG . . O20 O 0.7330(7) 0.3127(5) 0.5320(9) 0.075(2) Uiso 0.50 1 d PG . . H20A H 0.7146 0.3059 0.6189 0.113 Uiso 0.50 1 d PG . . H20B H 0.6769 0.3246 0.4533 0.113 Uiso 0.50 1 d PG . . O21 O 0.7937(5) 0.3234(3) 0.5521(6) 0.0469(16) Uiso 0.50 1 d PG . . H21A H 0.7472 0.3139 0.4619 0.070 Uiso 0.50 1 d PG . . H21B H 0.8606 0.3340 0.5431 0.070 Uiso 0.50 1 d PG . . 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 Ag1 0.02660(17) 0.0497(2) 0.03733(18) -0.01582(14) 0.00849(13) 0.00482(14) Ag2 0.0300(2) 0.0286(2) 0.0352(2) -0.00191(18) 0.00758(18) 0.00623(18) O1 0.0281(15) 0.0363(15) 0.0417(16) -0.0077(13) 0.0065(12) 0.0060(12) O2 0.0317(16) 0.0398(16) 0.0269(14) -0.0017(12) 0.0045(12) -0.0025(13) O3 0.059(2) 0.041(2) 0.089(3) 0.0048(18) 0.009(2) 0.0090(18) O4 0.088(3) 0.055(2) 0.132(4) -0.033(2) 0.079(3) -0.023(2) O5 0.050(2) 0.053(2) 0.059(2) -0.0107(16) 0.0159(16) -0.0177(17) N1 0.0257(18) 0.0299(17) 0.0359(18) -0.0063(14) 0.0076(14) 0.0040(14) N2 0.0265(18) 0.0288(17) 0.0391(19) -0.0013(14) 0.0094(14) 0.0029(14) N3 0.0252(17) 0.0291(17) 0.0262(16) -0.0011(13) 0.0033(13) 0.0033(14) N4 0.0251(18) 0.0391(19) 0.0291(17) -0.0046(14) 0.0049(14) 0.0069(15) N5 0.050(2) 0.039(2) 0.0286(19) -0.0013(16) 0.0087(17) -0.0055(19) C1 0.026(2) 0.041(2) 0.037(2) -0.0097(18) 0.0089(17) 0.0051(18) C2 0.031(2) 0.040(2) 0.041(2) -0.0035(19) 0.0166(19) -0.0016(18) C3 0.037(2) 0.038(2) 0.032(2) -0.0033(18) 0.0131(18) 0.0005(19) C4 0.035(2) 0.034(2) 0.033(2) 0.0020(17) 0.0080(18) 0.0009(18) C5 0.027(2) 0.030(2) 0.032(2) 0.0001(16) 0.0017(16) 0.0081(17) C6 0.024(2) 0.032(2) 0.034(2) -0.0027(17) 0.0049(16) 0.0095(17) C7 0.030(2) 0.039(2) 0.041(2) -0.0113(19) 0.0048(18) 0.0054(19) C8 0.028(2) 0.041(2) 0.056(3) -0.012(2) 0.012(2) -0.0029(19) C9 0.037(3) 0.039(2) 0.057(3) 0.001(2) 0.018(2) 0.000(2) C10 0.033(2) 0.044(2) 0.038(2) 0.0014(19) 0.0086(19) 0.002(2) C11 0.025(2) 0.031(2) 0.038(2) -0.0027(17) 0.0065(17) 0.0059(17) C12 0.031(2) 0.056(3) 0.031(2) 0.002(2) 0.0054(18) -0.001(2) C13 0.028(2) 0.052(3) 0.0213(19) -0.0016(18) 0.0016(16) 0.0111(19) C14 0.034(2) 0.069(3) 0.028(2) -0.001(2) 0.0091(18) 0.020(2) C15 0.048(3) 0.065(3) 0.037(2) -0.013(2) 0.005(2) 0.031(3) C16 0.043(3) 0.042(3) 0.045(3) -0.017(2) 0.002(2) 0.017(2) C17 0.032(2) 0.036(2) 0.034(2) -0.0075(18) 0.0037(18) 0.0078(18) C18 0.035(2) 0.034(2) 0.053(3) -0.011(2) 0.011(2) 0.0040(19) C19 0.019(2) 0.039(2) 0.038(2) -0.0105(18) 0.0062(17) -0.0041(17) C20 0.020(2) 0.058(3) 0.047(3) -0.018(2) 0.0054(18) 0.0058(19) C21 0.030(2) 0.080(4) 0.037(3) -0.016(2) 0.010(2) 0.002(2) C22 0.029(2) 0.066(3) 0.042(3) 0.006(2) 0.008(2) 0.005(2) C23 0.028(2) 0.042(2) 0.050(3) -0.003(2) 0.008(2) 0.0034(19) C24 0.021(2) 0.035(2) 0.042(2) -0.0091(18) 0.0071(17) -0.0015(17) C25 0.024(2) 0.039(2) 0.041(2) -0.0118(18) 0.0102(17) 0.0004(18) Ag3 0.0433(2) 0.0479(2) 0.0496(2) 0.02024(17) -0.00194(16) -0.00906(17) Ag4 0.0288(2) 0.0373(2) 0.0398(3) 0.00209(19) 0.00889(19) 0.00344(19) O6 0.0307(17) 0.055(2) 0.0413(17) 0.0098(15) 0.0016(13) -0.0035(15) O7 0.0391(19) 0.062(2) 0.055(2) 0.0013(16) 0.0252(16) 0.0062(16) O8 0.054(3) 0.060(3) 0.183(5) -0.049(3) 0.052(3) -0.003(2) O9 0.042(2) 0.066(3) 0.134(4) -0.044(2) 0.010(2) 0.0073(19) O10 0.118(4) 0.087(3) 0.087(3) 0.017(3) -0.049(3) -0.047(3) N6 0.0255(19) 0.047(2) 0.041(2) 0.0096(17) 0.0003(15) -0.0029(16) N7 0.0265(19) 0.043(2) 0.051(2) 0.0116(18) 0.0068(17) 0.0007(16) N8 0.0293(19) 0.040(2) 0.0362(19) 0.0024(15) 0.0091(15) 0.0026(15) N9 0.050(2) 0.043(2) 0.047(2) 0.0149(17) 0.0264(19) 0.0184(18) N10 0.044(3) 0.062(3) 0.047(2) -0.019(2) 0.026(2) -0.022(2) C26 0.040(3) 0.048(3) 0.043(3) 0.018(2) 0.004(2) 0.007(2) C27 0.041(3) 0.041(3) 0.062(3) 0.018(2) 0.016(2) 0.004(2) C28 0.035(3) 0.057(3) 0.044(3) 0.011(2) 0.016(2) 0.000(2) C29 0.033(2) 0.055(3) 0.048(3) 0.003(2) 0.018(2) 0.003(2) C30 0.037(3) 0.046(3) 0.049(3) 0.008(2) 0.013(2) 0.012(2) C31 0.030(2) 0.049(3) 0.045(3) 0.018(2) 0.010(2) 0.013(2) C32 0.043(3) 0.057(3) 0.055(3) 0.017(2) 0.008(2) 0.005(2) C33 0.048(3) 0.067(4) 0.060(4) 0.021(3) 0.004(3) -0.006(3) C34 0.030(3) 0.062(3) 0.085(4) 0.038(3) 0.021(3) 0.006(2) C35 0.044(3) 0.054(3) 0.067(3) 0.024(3) 0.029(3) 0.016(2) C36 0.030(2) 0.044(3) 0.058(3) 0.018(2) 0.013(2) 0.011(2) C37 0.074(4) 0.032(3) 0.111(5) 0.005(3) 0.069(4) 0.006(3) C38 0.082(4) 0.032(2) 0.053(3) 0.002(2) 0.046(3) 0.010(2) C39 0.200(8) 0.031(3) 0.037(3) -0.001(2) 0.053(4) -0.001(4) C40 0.232(9) 0.044(3) 0.022(3) -0.003(2) -0.002(4) 0.016(5) C41 0.120(5) 0.047(3) 0.032(3) -0.007(2) -0.002(3) 0.029(3) C42 0.056(3) 0.050(3) 0.037(2) 0.006(2) 0.017(2) 0.025(2) C43 0.032(3) 0.084(4) 0.049(3) 0.014(3) 0.004(2) 0.014(3) C44 0.034(3) 0.050(3) 0.045(3) 0.010(2) 0.008(2) -0.011(2) C45 0.041(3) 0.058(3) 0.044(3) 0.017(2) 0.004(2) -0.011(2) C46 0.064(4) 0.068(4) 0.051(3) 0.001(3) 0.025(3) -0.013(3) C47 0.061(4) 0.065(3) 0.067(4) 0.007(3) 0.032(3) -0.002(3) C48 0.039(3) 0.054(3) 0.064(3) 0.010(3) 0.011(2) 0.000(2) C49 0.033(3) 0.050(3) 0.047(3) 0.011(2) 0.005(2) -0.013(2) C50 0.039(3) 0.050(3) 0.045(3) 0.014(2) 0.001(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.254(3) . ? Ag1 N2 2.340(3) . ? Ag1 N1 2.417(3) . ? Ag1 O3 2.544(3) . ? Ag1 O1 2.716(3) . ? Ag2 N3 2.170(3) 2_656 ? Ag2 N3 2.170(3) . ? O1 C19 1.374(4) . ? O1 C18 1.423(5) . ? O2 C11 1.387(4) . ? O2 C12 1.440(4) . ? O3 N5 1.244(5) . ? O4 N5 1.237(5) . ? O5 N5 1.244(4) . ? N1 C1 1.470(5) . ? N1 C25 1.481(5) . ? N1 H1 0.9300 . ? N2 C3 1.481(5) . ? N2 C2 1.482(5) . ? N2 H2 0.9300 . ? N3 C4 1.485(4) . ? N3 C5 1.490(4) . ? N3 H3 0.9300 . ? N4 C17 1.344(5) . ? N4 C13 1.353(5) . ? C1 C2 1.519(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.503(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.382(5) . ? C6 C11 1.403(5) . ? C7 C8 1.395(6) . ? C7 H7 0.9500 . ? C8 C9 1.372(6) . ? C8 H8 0.9500 . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C12 C13 1.491(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.395(6) . ? C14 C15 1.366(6) . ? C14 H14 0.9500 . ? C15 C16 1.362(6) . ? C15 H15 0.9500 . ? C16 C17 1.385(5) . ? C16 H16 0.9500 . ? C17 C18 1.519(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.377(6) . ? C19 C24 1.416(5) . ? C20 C21 1.406(6) . ? C20 H20 0.9500 . ? C21 C22 1.377(6) . ? C21 H21 0.9500 . ? C22 C23 1.392(6) . ? C22 H22 0.9500 . ? C23 C24 1.385(5) . ? C23 H23 0.9500 . ? C24 C25 1.490(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Ag3 N9 2.237(3) . ? Ag3 N7 2.340(4) . ? Ag3 N6 2.364(3) . ? Ag3 O6 2.690(3) . ? Ag3 O8 2.703(4) . ? Ag4 N8 2.188(3) . ? Ag4 N8 2.188(3) 2_666 ? O6 C44 1.379(6) . ? O6 C43 1.421(5) . ? O7 C36 1.382(5) . ? O7 C37 1.430(6) . ? O8 N10 1.243(5) . ? O9 N10 1.228(5) . ? O10 N10 1.221(5) . ? N6 C26 1.469(5) . ? N6 C50 1.489(5) . ? N6 H6 0.9300 . ? N7 C28 1.469(6) . ? N7 C27 1.483(5) . ? N7 H7A 0.9300 . ? N8 C29 1.476(5) . ? N8 C30 1.494(5) . ? N8 H8A 0.9300 . ? N9 C38 1.343(5) . ? N9 C42 1.350(6) . ? C26 C27 1.511(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.510(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.500(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.374(6) . ? C31 C36 1.389(6) . ? C32 C33 1.381(7) . ? C32 H32 0.9500 . ? C33 C34 1.371(8) . ? C33 H33 0.9500 . ? C34 C35 1.392(7) . ? C34 H34 0.9500 . ? C35 C36 1.397(6) . ? C35 H35 0.9500 . ? C37 C38 1.505(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.386(7) . ? C39 C40 1.361(9) . ? C39 H39 0.9500 . ? C40 C41 1.361(8) . ? C40 H40 0.9500 . ? C41 C42 1.376(6) . ? C41 H41 0.9500 . ? C42 C43 1.490(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.400(6) . ? C44 C49 1.408(6) . ? C45 C46 1.375(7) . ? C45 H45 0.9500 . ? C46 C47 1.367(7) . ? C46 H46 0.9500 . ? C47 C48 1.379(7) . ? C47 H47 0.9500 . ? C48 C49 1.393(7) . ? C48 H48 0.9500 . ? C49 C50 1.507(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N11 N12 1.063(8) . ? N11 O14A 1.070(9) . ? N11 O12 1.2169 . ? N11 O11 1.2249 . ? N11 O13 1.2284 . ? N11 O15A 1.276(9) . ? N11 O14B 1.282(8) . ? N11 O15B 1.358(10) . ? O11 O15B 0.62(2) . ? O11 N12 1.072(9) . ? O12 O14B 0.703(13) . ? O12 N12 1.223(9) . ? O13 H21B 0.8222 . ? N12 O14B 1.0828 . ? N12 O15A 1.2169 . ? N12 O14A 1.2249 . ? N12 O16 1.2284 . ? N12 O15B 1.2299 . ? O14A O14B 1.0459 . ? O14B O16 1.6909 . ? O15A O15B 0.8391 . ? O16 O17 1.366(9) . ? N13 O18 1.2168 . ? N13 O17 1.2249 . ? N13 O19 1.2283 . ? N13 O18 1.506(15) 2_765 ? O18 O19 0.822(15) 2_765 ? O18 N13 1.506(16) 2_765 ? O19 O18 0.82(2) 2_765 ? O20 H20A 0.9800 . ? O20 H20B 0.9800 . ? O20 H21A 0.7962 . ? O21 H20A 1.4632 . ? O21 H21A 0.9800 . ? O21 H21B 0.9800 . ? 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 N4 Ag1 N2 130.60(11) . . ? N4 Ag1 N1 135.07(11) . . ? N2 Ag1 N1 78.64(10) . . ? N4 Ag1 O3 108.78(12) . . ? N2 Ag1 O3 105.22(12) . . ? N1 Ag1 O3 89.73(11) . . ? N4 Ag1 O1 70.02(10) . . ? N2 Ag1 O1 98.38(10) . . ? N1 Ag1 O1 72.68(9) . . ? O3 Ag1 O1 147.13(10) . . ? N3 Ag2 N3 180.0 2_656 . ? C19 O1 C18 118.8(3) . . ? C19 O1 Ag1 105.8(2) . . ? C18 O1 Ag1 97.7(2) . . ? C11 O2 C12 117.4(3) . . ? N5 O3 Ag1 128.5(3) . . ? C1 N1 C25 111.5(3) . . ? C1 N1 Ag1 103.2(2) . . ? C25 N1 Ag1 121.4(2) . . ? C1 N1 H1 106.6 . . ? C25 N1 H1 106.6 . . ? Ag1 N1 H1 106.6 . . ? C3 N2 C2 111.5(3) . . ? C3 N2 Ag1 123.3(2) . . ? C2 N2 Ag1 103.0(2) . . ? C3 N2 H2 106.0 . . ? C2 N2 H2 106.0 . . ? Ag1 N2 H2 106.0 . . ? C4 N3 C5 109.4(3) . . ? C4 N3 Ag2 115.1(2) . . ? C5 N3 Ag2 113.4(2) . . ? C4 N3 H3 106.1 . . ? C5 N3 H3 106.1 . . ? Ag2 N3 H3 106.1 . . ? C17 N4 C13 117.8(3) . . ? C17 N4 Ag1 118.9(3) . . ? C13 N4 Ag1 123.2(3) . . ? O4 N5 O3 121.3(4) . . ? O4 N5 O5 119.8(4) . . ? O3 N5 O5 118.9(4) . . ? N1 C1 C2 110.7(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 111.6(3) . . ? N2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 111.9(3) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 112.9(3) . . ? N3 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N3 C5 C6 111.9(3) . . ? N3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C11 118.1(4) . . ? C7 C6 C5 121.4(3) . . ? C11 C6 C5 120.5(3) . . ? C6 C7 C8 121.4(4) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.0(4) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.3(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 O2 124.7(4) . . ? C10 C11 C6 120.9(4) . . ? O2 C11 C6 114.4(3) . . ? O2 C12 C13 109.0(3) . . ? O2 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? O2 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 C14 121.4(4) . . ? N4 C13 C12 118.6(4) . . ? C14 C13 C12 120.0(4) . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 119.9(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N4 C17 C16 122.3(4) . . ? N4 C17 C18 118.8(4) . . ? C16 C17 C18 118.9(4) . . ? O1 C18 C17 114.8(3) . . ? O1 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? O1 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? O1 C19 C20 124.3(4) . . ? O1 C19 C24 114.4(3) . . ? C20 C19 C24 121.2(4) . . ? C19 C20 C21 119.0(4) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 121.0(4) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.1(4) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 121.8(4) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C19 117.9(4) . . ? C23 C24 C25 121.4(4) . . ? C19 C24 C25 120.6(4) . . ? N1 C25 C24 113.5(3) . . ? N1 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N1 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N9 Ag3 N7 132.51(12) . . ? N9 Ag3 N6 134.26(13) . . ? N7 Ag3 N6 80.73(12) . . ? N9 Ag3 O6 70.09(12) . . ? N7 Ag3 O6 100.39(11) . . ? N6 Ag3 O6 73.93(10) . . ? N9 Ag3 O8 115.35(15) . . ? N7 Ag3 O8 95.49(13) . . ? N6 Ag3 O8 84.74(12) . . ? O6 Ag3 O8 150.79(11) . . ? N8 Ag4 N8 180.000(1) . 2_666 ? C44 O6 C43 118.4(4) . . ? C44 O6 Ag3 109.9(2) . . ? C43 O6 Ag3 97.7(3) . . ? C36 O7 C37 120.6(4) . . ? N10 O8 Ag3 128.8(3) . . ? C26 N6 C50 110.7(3) . . ? C26 N6 Ag3 101.4(3) . . ? C50 N6 Ag3 121.4(2) . . ? C26 N6 H6 107.5 . . ? C50 N6 H6 107.5 . . ? Ag3 N6 H6 107.5 . . ? C28 N7 C27 111.1(3) . . ? C28 N7 Ag3 126.6(3) . . ? C27 N7 Ag3 101.5(3) . . ? C28 N7 H7A 105.3 . . ? C27 N7 H7A 105.3 . . ? Ag3 N7 H7A 105.3 . . ? C29 N8 C30 110.5(3) . . ? C29 N8 Ag4 112.2(2) . . ? C30 N8 Ag4 114.4(2) . . ? C29 N8 H8A 106.4 . . ? C30 N8 H8A 106.4 . . ? Ag4 N8 H8A 106.4 . . ? C38 N9 C42 118.5(4) . . ? C38 N9 Ag3 122.4(3) . . ? C42 N9 Ag3 118.8(3) . . ? O10 N10 O9 116.5(5) . . ? O10 N10 O8 119.6(5) . . ? O9 N10 O8 123.8(4) . . ? N6 C26 C27 112.0(3) . . ? N6 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? N6 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N7 C27 C26 112.3(3) . . ? N7 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? N7 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? N7 C28 C29 112.4(4) . . ? N7 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? N7 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? N8 C29 C28 112.7(4) . . ? N8 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? N8 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? N8 C30 C31 111.1(3) . . ? N8 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? N8 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C36 118.9(4) . . ? C32 C31 C30 121.6(5) . . ? C36 C31 C30 119.5(4) . . ? C31 C32 C33 121.5(5) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.1(5) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 121.5(5) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C36 118.1(5) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? O7 C36 C31 114.6(4) . . ? O7 C36 C35 124.5(5) . . ? C31 C36 C35 120.8(5) . . ? O7 C37 C38 108.2(4) . . ? O7 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O7 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? N9 C38 C39 121.0(5) . . ? N9 C38 C37 118.1(4) . . ? C39 C38 C37 120.9(5) . . ? C40 C39 C38 120.1(5) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 118.9(5) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 119.7(6) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? N9 C42 C41 121.7(5) . . ? N9 C42 C43 118.5(4) . . ? C41 C42 C43 119.5(5) . . ? O6 C43 C42 115.1(4) . . ? O6 C43 H43A 108.5 . . ? C42 C43 H43A 108.5 . . ? O6 C43 H43B 108.5 . . ? C42 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? O6 C44 C45 125.0(4) . . ? O6 C44 C49 114.3(4) . . ? C45 C44 C49 120.6(5) . . ? C46 C45 C44 119.1(5) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C47 C46 C45 121.5(5) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C46 C47 C48 119.4(6) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C47 C48 C49 121.9(5) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C48 C49 C44 117.5(5) . . ? C48 C49 C50 122.2(4) . . ? C44 C49 C50 120.2(5) . . ? N6 C50 C49 113.9(3) . . ? N6 C50 H50A 108.8 . . ? C49 C50 H50A 108.8 . . ? N6 C50 H50B 108.8 . . ? C49 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? N12 N11 O14A 70.1(5) . . ? N12 N11 O12 64.5(5) . . ? O14A N11 O12 19.8(7) . . ? N12 N11 O11 55.3(5) . . ? O14A N11 O11 115.6(7) . . ? O12 N11 O11 118.1 . . ? N12 N11 O13 174.2(5) . . ? O14A N11 O13 115.7(5) . . ? O12 N11 O13 121.0 . . ? O11 N11 O13 119.8 . . ? N12 N11 O15A 61.9(4) . . ? O14A N11 O15A 126.1(8) . . ? O12 N11 O15A 126.2(5) . . ? O11 N11 O15A 11.2(8) . . ? O13 N11 O15A 112.8(5) . . ? N12 N11 O14B 54.0(4) . . ? O14A N11 O14B 51.8(4) . . ? O12 N11 O14B 32.5(6) . . ? O11 N11 O14B 106.8(5) . . ? O13 N11 O14B 129.2(5) . . ? O15A N11 O14B 109.4(6) . . ? N12 N11 O15B 59.6(5) . . ? O14A N11 O15B 97.6(7) . . ? O12 N11 O15B 108.0(7) . . ? O11 N11 O15B 27.1(9) . . ? O13 N11 O15B 117.9(5) . . ? O15A N11 O15B 37.0(3) . . ? O14B N11 O15B 112.8(6) . . ? O15B O11 N12 89.1(13) . . ? O15B O11 N11 88.6(10) . . ? N12 O11 N11 54.6(4) . . ? O14B O12 N11 78.9(8) . . ? O14B O12 N12 61.6(6) . . ? N11 O12 N12 51.7(4) . . ? N11 O13 H21B 116.2 . . ? N11 N12 O11 70.0(5) . . ? N11 N12 O14B 73.4(5) . . ? O11 N12 O14B 138.2(8) . . ? N11 N12 O15A 67.7(5) . . ? O11 N12 O15A 10.2(10) . . ? O14B N12 O15A 130.4 . . ? N11 N12 O12 63.9(4) . . ? O11 N12 O12 131.5(7) . . ? O14B N12 O12 34.8(7) . . ? O15A N12 O12 131.3(4) . . ? N11 N12 O14A 55.2(5) . . ? O11 N12 O14A 115.4(7) . . ? O14B N12 O14A 53.5 . . ? O15A N12 O14A 118.1 . . ? O12 N12 O14A 19.7(6) . . ? N11 N12 O16 166.8(5) . . ? O11 N12 O16 120.4(6) . . ? O14B N12 O16 93.8 . . ? O15A N12 O16 121.0 . . ? O12 N12 O16 107.5(4) . . ? O14A N12 O16 119.8 . . ? N11 N12 O15B 72.2(5) . . ? O11 N12 O15B 30.2(11) . . ? O14B N12 O15B 143.9 . . ? O15A N12 O15B 40.1 . . ? O12 N12 O15B 116.4(6) . . ? O14A N12 O15B 96.9 . . ? O16 N12 O15B 120.9 . . ? O14B O14A N11 74.6(5) . . ? O14B O14A N12 56.3 . . ? N11 O14A N12 54.7(4) . . ? O12 O14B O14A 16.0(7) . . ? O12 O14B N12 83.5(9) . . ? O14A O14B N12 70.2 . . ? O12 O14B N11 68.6(6) . . ? O14A O14B N11 53.6(4) . . ? N12 O14B N11 52.6(4) . . ? O12 O14B O16 103.5(10) . . ? O14A O14B O16 99.0 . . ? N12 O14B O16 46.5 . . ? N11 O14B O16 99.0(4) . . ? O15B O15A N12 70.8 . . ? O15B O15A N11 76.8(5) . . ? N12 O15A N11 50.4(4) . . ? O11 O15B O15A 9.4(10) . . ? O11 O15B N12 60.6(9) . . ? O15A O15B N12 69.1 . . ? O11 O15B N11 64.3(8) . . ? O15A O15B N11 66.2(4) . . ? N12 O15B N11 48.2(3) . . ? N12 O16 O17 149.6(6) . . ? N12 O16 O14B 39.7 . . ? O17 O16 O14B 136.4(6) . . ? O18 N13 O17 118.1 . . ? O18 N13 O19 121.0 . . ? O17 N13 O19 119.8 . . ? O18 N13 O18 88.0(10) . 2_765 ? O17 N13 O18 151.2(11) . 2_765 ? O19 N13 O18 33.0(10) . 2_765 ? N13 O17 O16 138.6(9) . . ? O19 O18 N13 147(2) 2_765 . ? O19 O18 N13 54.6(16) 2_765 2_765 ? N13 O18 N13 92.0(7) . 2_765 ? O18 O19 N13 92.4(14) 2_765 . ? H20A O20 H20B 109.5 . . ? H20A O20 H21A 173.8 . . ? H20B O20 H21A 72.0 . . ? H20A O21 H21A 90.9 . . ? H20A O21 H21B 159.1 . . ? H21A O21 H21B 109.5 . . ? 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 N4 Ag1 O1 C19 89.0(2) . . . . ? N2 Ag1 O1 C19 -140.7(2) . . . . ? N1 Ag1 O1 C19 -65.5(2) . . . . ? O3 Ag1 O1 C19 -4.9(3) . . . . ? N4 Ag1 O1 C18 -33.9(2) . . . . ? N2 Ag1 O1 C18 96.4(2) . . . . ? N1 Ag1 O1 C18 171.7(2) . . . . ? O3 Ag1 O1 C18 -127.8(3) . . . . ? N4 Ag1 O3 N5 -146.7(3) . . . . ? N2 Ag1 O3 N5 69.7(4) . . . . ? N1 Ag1 O3 N5 -8.5(4) . . . . ? O1 Ag1 O3 N5 -64.7(4) . . . . ? N4 Ag1 N1 C1 -150.4(2) . . . . ? N2 Ag1 N1 C1 -12.8(2) . . . . ? O3 Ag1 N1 C1 92.8(2) . . . . ? O1 Ag1 N1 C1 -115.4(2) . . . . ? N4 Ag1 N1 C25 -24.7(3) . . . . ? N2 Ag1 N1 C25 112.9(3) . . . . ? O3 Ag1 N1 C25 -141.5(3) . . . . ? O1 Ag1 N1 C25 10.3(2) . . . . ? N4 Ag1 N2 C3 -110.7(3) . . . . ? N1 Ag1 N2 C3 108.2(3) . . . . ? O3 Ag1 N2 C3 21.6(3) . . . . ? O1 Ag1 N2 C3 178.5(3) . . . . ? N4 Ag1 N2 C2 122.4(2) . . . . ? N1 Ag1 N2 C2 -18.7(2) . . . . ? O3 Ag1 N2 C2 -105.3(2) . . . . ? O1 Ag1 N2 C2 51.6(2) . . . . ? N3 Ag2 N3 C4 -93(100) 2_656 . . . ? N3 Ag2 N3 C5 33(100) 2_656 . . . ? N2 Ag1 N4 C17 -64.3(3) . . . . ? N1 Ag1 N4 C17 55.1(3) . . . . ? O3 Ag1 N4 C17 164.6(3) . . . . ? O1 Ag1 N4 C17 19.5(2) . . . . ? N2 Ag1 N4 C13 112.4(3) . . . . ? N1 Ag1 N4 C13 -128.1(3) . . . . ? O3 Ag1 N4 C13 -18.6(3) . . . . ? O1 Ag1 N4 C13 -163.7(3) . . . . ? Ag1 O3 N5 O4 -1.8(6) . . . . ? Ag1 O3 N5 O5 176.3(3) . . . . ? C25 N1 C1 C2 -88.6(4) . . . . ? Ag1 N1 C1 C2 43.2(3) . . . . ? C3 N2 C2 C1 -84.3(4) . . . . ? Ag1 N2 C2 C1 49.8(3) . . . . ? N1 C1 C2 N2 -68.7(4) . . . . ? C2 N2 C3 C4 -174.6(3) . . . . ? Ag1 N2 C3 C4 62.2(4) . . . . ? C5 N3 C4 C3 168.8(3) . . . . ? Ag2 N3 C4 C3 -62.2(4) . . . . ? N2 C3 C4 N3 -81.6(4) . . . . ? C4 N3 C5 C6 -179.3(3) . . . . ? Ag2 N3 C5 C6 50.8(4) . . . . ? N3 C5 C6 C7 -111.3(4) . . . . ? N3 C5 C6 C11 68.2(5) . . . . ? C11 C6 C7 C8 -1.6(6) . . . . ? C5 C6 C7 C8 177.9(4) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C7 C8 C9 C10 1.7(7) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 O2 176.4(4) . . . . ? C9 C10 C11 C6 -1.7(6) . . . . ? C12 O2 C11 C10 11.9(5) . . . . ? C12 O2 C11 C6 -170.0(3) . . . . ? C7 C6 C11 C10 2.7(6) . . . . ? C5 C6 C11 C10 -176.8(4) . . . . ? C7 C6 C11 O2 -175.5(3) . . . . ? C5 C6 C11 O2 5.0(5) . . . . ? C11 O2 C12 C13 -158.8(3) . . . . ? C17 N4 C13 C14 0.8(5) . . . . ? Ag1 N4 C13 C14 -176.0(3) . . . . ? C17 N4 C13 C12 -177.0(3) . . . . ? Ag1 N4 C13 C12 6.2(5) . . . . ? O2 C12 C13 N4 -74.6(4) . . . . ? O2 C12 C13 C14 107.6(4) . . . . ? N4 C13 C14 C15 -1.4(6) . . . . ? C12 C13 C14 C15 176.3(4) . . . . ? C13 C14 C15 C16 0.9(6) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? C13 N4 C17 C16 0.4(5) . . . . ? Ag1 N4 C17 C16 177.3(3) . . . . ? C13 N4 C17 C18 -178.6(3) . . . . ? Ag1 N4 C17 C18 -1.6(4) . . . . ? C15 C16 C17 N4 -0.9(6) . . . . ? C15 C16 C17 C18 178.1(4) . . . . ? C19 O1 C18 C17 -67.3(4) . . . . ? Ag1 O1 C18 C17 45.5(4) . . . . ? N4 C17 C18 O1 -37.5(5) . . . . ? C16 C17 C18 O1 143.6(4) . . . . ? C18 O1 C19 C20 -6.3(5) . . . . ? Ag1 O1 C19 C20 -114.6(4) . . . . ? C18 O1 C19 C24 175.7(3) . . . . ? Ag1 O1 C19 C24 67.3(3) . . . . ? O1 C19 C20 C21 -178.2(4) . . . . ? C24 C19 C20 C21 -0.2(6) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C20 C21 C22 C23 0.8(7) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C19 -0.4(6) . . . . ? C22 C23 C24 C25 175.9(4) . . . . ? O1 C19 C24 C23 178.8(3) . . . . ? C20 C19 C24 C23 0.7(6) . . . . ? O1 C19 C24 C25 2.5(5) . . . . ? C20 C19 C24 C25 -175.7(4) . . . . ? C1 N1 C25 C24 166.0(3) . . . . ? Ag1 N1 C25 C24 44.2(4) . . . . ? C23 C24 C25 N1 111.6(4) . . . . ? C19 C24 C25 N1 -72.1(5) . . . . ? N9 Ag3 O6 C44 -90.3(3) . . . . ? N7 Ag3 O6 C44 138.0(2) . . . . ? N6 Ag3 O6 C44 60.9(2) . . . . ? O8 Ag3 O6 C44 16.2(4) . . . . ? N9 Ag3 O6 C43 33.6(3) . . . . ? N7 Ag3 O6 C43 -98.0(3) . . . . ? N6 Ag3 O6 C43 -175.1(3) . . . . ? O8 Ag3 O6 C43 140.2(3) . . . . ? N9 Ag3 O8 N10 128.1(4) . . . . ? N7 Ag3 O8 N10 -89.1(4) . . . . ? N6 Ag3 O8 N10 -9.0(4) . . . . ? O6 Ag3 O8 N10 33.8(6) . . . . ? N9 Ag3 N6 C26 158.4(2) . . . . ? N7 Ag3 N6 C26 15.5(2) . . . . ? O6 Ag3 N6 C26 119.2(3) . . . . ? O8 Ag3 N6 C26 -80.9(3) . . . . ? N9 Ag3 N6 C50 35.3(4) . . . . ? N7 Ag3 N6 C50 -107.5(3) . . . . ? O6 Ag3 N6 C50 -3.8(3) . . . . ? O8 Ag3 N6 C50 156.0(3) . . . . ? N9 Ag3 N7 C28 103.7(3) . . . . ? N6 Ag3 N7 C28 -112.3(3) . . . . ? O6 Ag3 N7 C28 176.1(3) . . . . ? O8 Ag3 N7 C28 -28.5(3) . . . . ? N9 Ag3 N7 C27 -128.8(3) . . . . ? N6 Ag3 N7 C27 15.2(2) . . . . ? O6 Ag3 N7 C27 -56.4(3) . . . . ? O8 Ag3 N7 C27 99.0(3) . . . . ? N8 Ag4 N8 C29 -65(100) 2_666 . . . ? N8 Ag4 N8 C30 168(100) 2_666 . . . ? N7 Ag3 N9 C38 -107.0(3) . . . . ? N6 Ag3 N9 C38 127.0(3) . . . . ? O6 Ag3 N9 C38 167.2(4) . . . . ? O8 Ag3 N9 C38 18.3(4) . . . . ? N7 Ag3 N9 C42 66.6(4) . . . . ? N6 Ag3 N9 C42 -59.4(4) . . . . ? O6 Ag3 N9 C42 -19.3(3) . . . . ? O8 Ag3 N9 C42 -168.1(3) . . . . ? Ag3 O8 N10 O10 174.1(4) . . . . ? Ag3 O8 N10 O9 -9.4(7) . . . . ? C50 N6 C26 C27 84.3(4) . . . . ? Ag3 N6 C26 C27 -45.8(4) . . . . ? C28 N7 C27 C26 91.2(5) . . . . ? Ag3 N7 C27 C26 -45.8(4) . . . . ? N6 C26 C27 N7 68.9(5) . . . . ? C27 N7 C28 C29 173.9(3) . . . . ? Ag3 N7 C28 C29 -62.5(5) . . . . ? C30 N8 C29 C28 -167.4(4) . . . . ? Ag4 N8 C29 C28 63.7(4) . . . . ? N7 C28 C29 N8 80.6(5) . . . . ? C29 N8 C30 C31 -176.9(4) . . . . ? Ag4 N8 C30 C31 -49.1(4) . . . . ? N8 C30 C31 C32 111.3(5) . . . . ? N8 C30 C31 C36 -68.9(5) . . . . ? C36 C31 C32 C33 2.5(6) . . . . ? C30 C31 C32 C33 -177.7(4) . . . . ? C31 C32 C33 C34 0.2(7) . . . . ? C32 C33 C34 C35 -1.5(7) . . . . ? C33 C34 C35 C36 0.0(7) . . . . ? C37 O7 C36 C31 165.7(4) . . . . ? C37 O7 C36 C35 -16.7(6) . . . . ? C32 C31 C36 O7 173.8(4) . . . . ? C30 C31 C36 O7 -6.0(5) . . . . ? C32 C31 C36 C35 -3.9(6) . . . . ? C30 C31 C36 C35 176.3(4) . . . . ? C34 C35 C36 O7 -174.8(4) . . . . ? C34 C35 C36 C31 2.7(6) . . . . ? C36 O7 C37 C38 156.7(3) . . . . ? C42 N9 C38 C39 -1.6(7) . . . . ? Ag3 N9 C38 C39 172.0(4) . . . . ? C42 N9 C38 C37 179.9(4) . . . . ? Ag3 N9 C38 C37 -6.5(5) . . . . ? O7 C37 C38 N9 82.6(5) . . . . ? O7 C37 C38 C39 -95.9(5) . . . . ? N9 C38 C39 C40 1.8(8) . . . . ? C37 C38 C39 C40 -179.7(5) . . . . ? C38 C39 C40 C41 -0.5(10) . . . . ? C39 C40 C41 C42 -0.9(9) . . . . ? C38 N9 C42 C41 0.2(7) . . . . ? Ag3 N9 C42 C41 -173.7(4) . . . . ? C38 N9 C42 C43 175.0(4) . . . . ? Ag3 N9 C42 C43 1.2(6) . . . . ? C40 C41 C42 N9 1.1(8) . . . . ? C40 C41 C42 C43 -173.7(5) . . . . ? C44 O6 C43 C42 71.8(5) . . . . ? Ag3 O6 C43 C42 -45.8(4) . . . . ? N9 C42 C43 O6 37.8(6) . . . . ? C41 C42 C43 O6 -147.3(4) . . . . ? C43 O6 C44 C45 7.6(6) . . . . ? Ag3 O6 C44 C45 118.6(4) . . . . ? C43 O6 C44 C49 -175.5(4) . . . . ? Ag3 O6 C44 C49 -64.6(4) . . . . ? O6 C44 C45 C46 175.8(4) . . . . ? C49 C44 C45 C46 -0.9(7) . . . . ? C44 C45 C46 C47 1.1(7) . . . . ? C45 C46 C47 C48 -0.1(8) . . . . ? C46 C47 C48 C49 -1.2(7) . . . . ? C47 C48 C49 C44 1.4(7) . . . . ? C47 C48 C49 C50 -173.6(4) . . . . ? O6 C44 C49 C48 -177.4(4) . . . . ? C45 C44 C49 C48 -0.4(6) . . . . ? O6 C44 C49 C50 -2.2(6) . . . . ? C45 C44 C49 C50 174.8(4) . . . . ? C26 N6 C50 C49 -169.0(4) . . . . ? Ag3 N6 C50 C49 -50.4(5) . . . . ? C48 C49 C50 N6 -113.0(5) . . . . ? C44 C49 C50 N6 72.0(5) . . . . ? N12 N11 O11 O15B -90.0(13) . . . . ? O14A N11 O11 O15B -52.2(10) . . . . ? O12 N11 O11 O15B -74.2(11) . . . . ? O13 N11 O11 O15B 93.7(11) . . . . ? O15A N11 O11 O15B 147(4) . . . . ? O14B N11 O11 O15B -107.3(11) . . . . ? O14A N11 O11 N12 37.8(9) . . . . ? O12 N11 O11 N12 15.8(8) . . . . ? O13 N11 O11 N12 -176.3(8) . . . . ? O15A N11 O11 N12 -123(4) . . . . ? O14B N11 O11 N12 -17.4(8) . . . . ? O15B N11 O11 N12 90.0(13) . . . . ? N12 N11 O12 O14B -62.5(7) . . . . ? O14A N11 O12 O14B -165(3) . . . . ? O11 N11 O12 O14B -76.8(9) . . . . ? O13 N11 O12 O14B 115.4(9) . . . . ? O15A N11 O12 O14B -67.7(13) . . . . ? O15B N11 O12 O14B -104.3(11) . . . . ? O14A N11 O12 N12 -102.3(19) . . . . ? O11 N11 O12 N12 -14.4(7) . . . . ? O13 N11 O12 N12 177.9(7) . . . . ? O15A N11 O12 N12 -5.2(8) . . . . ? O14B N11 O12 N12 62.5(8) . . . . ? O15B N11 O12 N12 -41.8(5) . . . . ? O14A N11 N12 O11 -144.0(9) . . . . ? O12 N11 N12 O11 -164.6(7) . . . . ? O13 N11 N12 O11 33(7) . . . . ? O15A N11 N12 O11 10.7(11) . . . . ? O14B N11 N12 O11 159.3(10) . . . . ? O15B N11 N12 O11 -31.9(11) . . . . ? O14A N11 N12 O14B 56.7(3) . . . . ? O12 N11 N12 O14B 36.1(7) . . . . ? O11 N11 N12 O14B -159.3(10) . . . . ? O13 N11 N12 O14B -126(6) . . . . ? O15A N11 N12 O14B -148.7(4) . . . . ? O15B N11 N12 O14B 168.8(3) . . . . ? O14A N11 N12 O15A -154.7(6) . . . . ? O12 N11 N12 O15A -175.2(7) . . . . ? O11 N11 N12 O15A -10.7(11) . . . . ? O13 N11 N12 O15A 23(6) . . . . ? O14B N11 N12 O15A 148.7(4) . . . . ? O15B N11 N12 O15A -42.55(15) . . . . ? O14A N11 N12 O12 20.6(8) . . . . ? O11 N11 N12 O12 164.6(7) . . . . ? O13 N11 N12 O12 -162(6) . . . . ? O15A N11 N12 O12 175.2(7) . . . . ? O14B N11 N12 O12 -36.1(7) . . . . ? O15B N11 N12 O12 132.7(7) . . . . ? O12 N11 N12 O14A -20.6(8) . . . . ? O11 N11 N12 O14A 144.0(9) . . . . ? O13 N11 N12 O14A 177(100) . . . . ? O15A N11 N12 O14A 154.7(6) . . . . ? O14B N11 N12 O14A -56.7(3) . . . . ? O15B N11 N12 O14A 112.1(5) . . . . ? O14A N11 N12 O16 72(2) . . . . ? O12 N11 N12 O16 51(2) . . . . ? O11 N11 N12 O16 -144(3) . . . . ? O13 N11 N12 O16 -111(6) . . . . ? O15A N11 N12 O16 -133(2) . . . . ? O14B N11 N12 O16 15(2) . . . . ? O15B N11 N12 O16 -176(2) . . . . ? O14A N11 N12 O15B -112.1(5) . . . . ? O12 N11 N12 O15B -132.7(7) . . . . ? O11 N11 N12 O15B 31.9(11) . . . . ? O13 N11 N12 O15B 65(6) . . . . ? O15A N11 N12 O15B 42.55(15) . . . . ? O14B N11 N12 O15B -168.8(3) . . . . ? O15B O11 N12 N11 88.8(11) . . . . ? O15B O11 N12 O14B 119.3(13) . . . . ? N11 O11 N12 O14B 30.5(11) . . . . ? O15B O11 N12 O15A 164(4) . . . . ? N11 O11 N12 O15A 75(3) . . . . ? O15B O11 N12 O12 70.2(16) . . . . ? N11 O11 N12 O12 -18.6(9) . . . . ? O15B O11 N12 O14A 56.5(13) . . . . ? N11 O11 N12 O14A -32.3(7) . . . . ? O15B O11 N12 O16 -100.1(10) . . . . ? N11 O11 N12 O16 171.0(7) . . . . ? N11 O11 N12 O15B -88.8(11) . . . . ? O14B O12 N12 N11 98.5(9) . . . . ? O14B O12 N12 O11 118.0(14) . . . . ? N11 O12 N12 O11 19.5(9) . . . . ? N11 O12 N12 O14B -98.5(9) . . . . ? O14B O12 N12 O15A 104.4(7) . . . . ? N11 O12 N12 O15A 5.9(9) . . . . ? O14B O12 N12 O14A 158(2) . . . . ? N11 O12 N12 O14A 59.0(16) . . . . ? O14B O12 N12 O16 -70.7(8) . . . . ? N11 O12 N12 O16 -169.2(6) . . . . ? O14B O12 N12 O15B 149.9(5) . . . . ? N11 O12 N12 O15B 51.4(7) . . . . ? N12 N11 O14A O14B -59.3(3) . . . . ? O12 N11 O14A O14B 10.3(17) . . . . ? O11 N11 O14A O14B -91.7(7) . . . . ? O13 N11 O14A O14B 121.0(5) . . . . ? O15A N11 O14A O14B -87.2(9) . . . . ? O15B N11 O14A O14B -113.0(5) . . . . ? O12 N11 O14A N12 69.7(17) . . . . ? O11 N11 O14A N12 -32.4(7) . . . . ? O13 N11 O14A N12 -179.7(7) . . . . ? O15A N11 O14A N12 -27.9(5) . . . . ? O14B N11 O14A N12 59.3(3) . . . . ? O15B N11 O14A N12 -53.7(3) . . . . ? N11 N12 O14A O14B 94.7(7) . . . . ? O11 N12 O14A O14B 132.4(11) . . . . ? O15A N12 O14A O14B 121.3 . . . . ? O12 N12 O14A O14B -15.8(17) . . . . ? O16 N12 O14A O14B -70.8 . . . . ? O15B N12 O14A O14B 157.4 . . . . ? O11 N12 O14A N11 37.7(8) . . . . ? O14B N12 O14A N11 -94.7(7) . . . . ? O15A N12 O14A N11 26.7(7) . . . . ? O12 N12 O14A N11 -110.4(19) . . . . ? O16 N12 O14A N11 -165.5(7) . . . . ? O15B N12 O14A N11 62.7(7) . . . . ? N11 O12 O14B O14A 19(3) . . . . ? N12 O12 O14B O14A -33(3) . . . . ? N11 O12 O14B N12 52.2(4) . . . . ? N12 O12 O14B N11 -52.2(4) . . . . ? N11 O12 O14B O16 94.5(5) . . . . ? N12 O12 O14B O16 42.3(2) . . . . ? N11 O14A O14B O12 -158(4) . . . . ? N12 O14A O14B O12 145(4) . . . . ? N11 O14A O14B N12 57.5(5) . . . . ? N12 O14A O14B N11 -57.5(5) . . . . ? N11 O14A O14B O16 94.6(5) . . . . ? N12 O14A O14B O16 37.1 . . . . ? N11 N12 O14B O12 -67.9(8) . . . . ? O11 N12 O14B O12 -97.8(17) . . . . ? O15A N12 O14B O12 -107.1(8) . . . . ? O14A N12 O14B O12 -9.2(8) . . . . ? O16 N12 O14B O12 115.6(8) . . . . ? O15B N12 O14B O12 -49.6(8) . . . . ? N11 N12 O14B O14A -58.7(5) . . . . ? O11 N12 O14B O14A -88.5(14) . . . . ? O15A N12 O14B O14A -97.9 . . . . ? O12 N12 O14B O14A 9.2(8) . . . . ? O16 N12 O14B O14A 124.8 . . . . ? O15B N12 O14B O14A -40.4 . . . . ? O11 N12 O14B N11 -29.8(11) . . . . ? O15A N12 O14B N11 -39.2(5) . . . . ? O12 N12 O14B N11 67.9(8) . . . . ? O14A N12 O14B N11 58.7(5) . . . . ? O16 N12 O14B N11 -176.5(5) . . . . ? O15B N12 O14B N11 18.3(5) . . . . ? N11 N12 O14B O16 176.5(5) . . . . ? O11 N12 O14B O16 146.7(14) . . . . ? O15A N12 O14B O16 137.3 . . . . ? O12 N12 O14B O16 -115.6(8) . . . . ? O14A N12 O14B O16 -124.8 . . . . ? O15B N12 O14B O16 -165.2 . . . . ? N12 N11 O14B O12 98.5(10) . . . . ? O14A N11 O14B O12 6.5(11) . . . . ? O11 N11 O14B O12 116.2(7) . . . . ? O13 N11 O14B O12 -87.5(10) . . . . ? O15A N11 O14B O12 127.6(10) . . . . ? O15B N11 O14B O12 88.0(11) . . . . ? N12 N11 O14B O14A 92.0(5) . . . . ? O12 N11 O14B O14A -6.5(11) . . . . ? O11 N11 O14B O14A 109.7(8) . . . . ? O13 N11 O14B O14A -94.0(6) . . . . ? O15A N11 O14B O14A 121.1(8) . . . . ? O15B N11 O14B O14A 81.6(7) . . . . ? O14A N11 O14B N12 -92.0(5) . . . . ? O12 N11 O14B N12 -98.5(10) . . . . ? O11 N11 O14B N12 17.7(8) . . . . ? O13 N11 O14B N12 174.0(8) . . . . ? O15A N11 O14B N12 29.1(4) . . . . ? O15B N11 O14B N12 -10.5(3) . . . . ? N12 N11 O14B O16 -2.5(4) . . . . ? O14A N11 O14B O16 -94.6(3) . . . . ? O12 N11 O14B O16 -101.1(10) . . . . ? O11 N11 O14B O16 15.1(8) . . . . ? O13 N11 O14B O16 171.4(6) . . . . ? O15A N11 O14B O16 26.6(7) . . . . ? O15B N11 O14B O16 -13.0(7) . . . . ? N11 N12 O15A O15B 88.6(6) . . . . ? O11 N12 O15A O15B -13(3) . . . . ? O14B N12 O15A O15B 129.5 . . . . ? O12 N12 O15A O15B 82.9(9) . . . . ? O14A N12 O15A O15B 65.1 . . . . ? O16 N12 O15A O15B -102.6 . . . . ? O11 N12 O15A N11 -101(3) . . . . ? O14B N12 O15A N11 40.9(6) . . . . ? O12 N12 O15A N11 -5.7(9) . . . . ? O14A N12 O15A N11 -23.5(6) . . . . ? O16 N12 O15A N11 168.8(6) . . . . ? O15B N12 O15A N11 -88.6(6) . . . . ? N12 N11 O15A O15B -75.8(4) . . . . ? O14A N11 O15A O15B -45.9(9) . . . . ? O12 N11 O15A O15B -70.5(10) . . . . ? O11 N11 O15A O15B -24(3) . . . . ? O13 N11 O15A O15B 106.6(5) . . . . ? O14B N11 O15A O15B -102.3(6) . . . . ? O14A N11 O15A N12 29.9(6) . . . . ? O12 N11 O15A N12 5.3(8) . . . . ? O11 N11 O15A N12 52(4) . . . . ? O13 N11 O15A N12 -177.6(7) . . . . ? O14B N11 O15A N12 -26.5(3) . . . . ? O15B N11 O15A N12 75.8(4) . . . . ? N12 O11 O15B O15A -154(6) . . . . ? N11 O11 O15B O15A -99(6) . . . . ? N11 O11 O15B N12 54.6(4) . . . . ? N12 O11 O15B N11 -54.6(4) . . . . ? N12 O15A O15B O11 24(5) . . . . ? N11 O15A O15B O11 77(5) . . . . ? N11 O15A O15B N12 52.3(4) . . . . ? N12 O15A O15B N11 -52.3(4) . . . . ? N11 N12 O15B O11 -80.6(12) . . . . ? O14B N12 O15B O11 -99.0(11) . . . . ? O15A N12 O15B O11 -4.4(11) . . . . ? O12 N12 O15B O11 -128.1(13) . . . . ? O14A N12 O15B O11 -130.7(11) . . . . ? O16 N12 O15B O11 98.3(11) . . . . ? N11 N12 O15B O15A -76.2(5) . . . . ? O11 N12 O15B O15A 4.4(11) . . . . ? O14B N12 O15B O15A -94.6 . . . . ? O12 N12 O15B O15A -123.7(7) . . . . ? O14A N12 O15B O15A -126.3 . . . . ? O16 N12 O15B O15A 102.7 . . . . ? O11 N12 O15B N11 80.6(12) . . . . ? O14B N12 O15B N11 -18.4(5) . . . . ? O15A N12 O15B N11 76.2(5) . . . . ? O12 N12 O15B N11 -47.5(6) . . . . ? O14A N12 O15B N11 -50.1(5) . . . . ? O16 N12 O15B N11 178.9(5) . . . . ? N12 N11 O15B O11 72.5(11) . . . . ? O14A N11 O15B O11 134.1(9) . . . . ? O12 N11 O15B O11 116.8(10) . . . . ? O13 N11 O15B O11 -101.5(10) . . . . ? O15A N11 O15B O11 -10.1(11) . . . . ? O14B N11 O15B O11 82.4(11) . . . . ? N12 N11 O15B O15A 82.6(4) . . . . ? O14A N11 O15B O15A 144.2(6) . . . . ? O12 N11 O15B O15A 126.9(6) . . . . ? O11 N11 O15B O15A 10.1(11) . . . . ? O13 N11 O15B O15A -91.4(5) . . . . ? O14B N11 O15B O15A 92.5(6) . . . . ? O14A N11 O15B N12 61.5(4) . . . . ? O12 N11 O15B N12 44.2(5) . . . . ? O11 N11 O15B N12 -72.5(11) . . . . ? O13 N11 O15B N12 -174.1(6) . . . . ? O15A N11 O15B N12 -82.6(4) . . . . ? O14B N11 O15B N12 9.8(3) . . . . ? N11 N12 O16 O17 86(2) . . . . ? O11 N12 O16 O17 -53.9(16) . . . . ? O14B N12 O16 O17 100.9(12) . . . . ? O15A N12 O16 O17 -42.1(12) . . . . ? O12 N12 O16 O17 133.6(13) . . . . ? O14A N12 O16 O17 150.4(12) . . . . ? O15B N12 O16 O17 -89.2(12) . . . . ? N11 N12 O16 O14B -15(2) . . . . ? O11 N12 O16 O14B -154.9(12) . . . . ? O15A N12 O16 O14B -143.0 . . . . ? O12 N12 O16 O14B 32.7(7) . . . . ? O14A N12 O16 O14B 49.5 . . . . ? O15B N12 O16 O14B 169.9 . . . . ? O12 O14B O16 N12 -67.2(7) . . . . ? O14A O14B O16 N12 -51.5 . . . . ? N11 O14B O16 N12 2.8(4) . . . . ? O12 O14B O16 O17 159.0(11) . . . . ? O14A O14B O16 O17 174.7(9) . . . . ? N12 O14B O16 O17 -133.8(9) . . . . ? N11 O14B O16 O17 -131.1(9) . . . . ? O18 N13 O17 O16 128.0(12) . . . . ? O19 N13 O17 O16 -64.2(12) . . . . ? O18 N13 O17 O16 -80(3) 2_765 . . . ? N12 O16 O17 N13 -61.8(18) . . . . ? O14B O16 O17 N13 3.8(17) . . . . ? O17 N13 O18 O19 166(4) . . . 2_765 ? O19 N13 O18 O19 -2(4) . . . 2_765 ? O18 N13 O18 O19 -1(4) 2_765 . . 2_765 ? O17 N13 O18 N13 167.1(10) . . . 2_765 ? O19 N13 O18 N13 -0.6(10) . . . 2_765 ? O18 N13 O18 N13 0.0(7) 2_765 . . 2_765 ? O18 N13 O19 O18 1(3) . . . 2_765 ? O17 N13 O19 O18 -166(3) . . . 2_765 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O4 0.93 2.21 2.917(5) 132.0 . N2 H2 O20 0.93 2.03 2.955(9) 175.8 . N2 H2 O21 0.93 2.20 3.102(7) 162.0 . N3 H3 O2 0.93 2.43 3.029(4) 121.8 . N3 H3 O3 0.93 2.49 3.188(4) 132.2 . N6 H6 O9 0.93 2.18 2.960(5) 140.4 . N8 H8A O7 0.93 2.43 3.009(4) 120.2 . N8 H8A O8 0.93 2.63 3.283(5) 128.2 . O20 H20B O10 0.98 1.82 2.664(10) 142.4 2_666 O20 H20B O9 0.98 2.52 3.429(10) 154.9 2_666 O20 H20B N10 0.98 2.54 3.480(10) 161.2 2_666 O20 H21A O12 0.80 2.66 3.355(12) 146.4 . O13 H21B O20 0.82 1.79 2.605(12) 173.3 . _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.100 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.097