# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hongping Zhou' _publ_contact_author_email zhpzhp@263.net loop_ _publ_author_name 'Feng Jin' 'Hongping Zhou' data_jfag_1 _database_code_depnum_ccdc_archive 'CCDC 850217' #TrackingRef '- Complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H50 Ag2 N8 O6 S2' _chemical_formula_sum 'C64 H50 Ag2 N8 O6 S2' _chemical_formula_weight 1306.98 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' 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' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7310(19) _cell_length_b 11.700(2) _cell_length_c 13.496(3) _cell_angle_alpha 77.46(3) _cell_angle_beta 81.25(3) _cell_angle_gamma 68.07(3) _cell_volume 1387.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6225 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.55 _exptl_crystal_description neddle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7859 _exptl_absorpt_correction_T_max 0.8494 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9949 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4862 _reflns_number_gt 4315 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.8422P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4862 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.57631(2) 0.296315(18) 0.831877(19) 0.05505(11) Uani 0.9794(7) 1 d P . 1 Ag1' Ag -0.5437(9) 0.7036(8) 1.2413(6) 0.038(2) Uani 0.0206(7) 1 d PU . 2 C1 C 1.0243(2) 0.0811(2) 0.64876(17) 0.0427(6) Uani 1 1 d . . . C2 C 1.0740(3) -0.0317(2) 0.61566(19) 0.0505(6) Uani 1 1 d . . . H2 H 1.0293 -0.0906 0.6433 0.061 Uiso 1 1 calc R . . C3 C 1.1907(3) -0.0579(3) 0.5412(2) 0.0583(7) Uani 1 1 d . . . H3 H 1.2238 -0.1347 0.5197 0.070 Uiso 1 1 calc R . . C4 C 1.2585(3) 0.0273(3) 0.49862(19) 0.0571(7) Uani 1 1 d . . . C5 C 1.2104(3) 0.1388(3) 0.5351(2) 0.0636(8) Uani 1 1 d . . . H5 H 1.2571 0.1965 0.5089 0.076 Uiso 1 1 calc R . . C6 C 1.0943(3) 0.1662(3) 0.6096(2) 0.0557(7) Uani 1 1 d . . . H6 H 1.0635 0.2417 0.6331 0.067 Uiso 1 1 calc R . . C7 C 1.3786(3) 0.0009(4) 0.4122(2) 0.0865(11) Uani 1 1 d . . . H7A H 1.4441 -0.0846 0.4262 0.130 Uiso 1 1 calc R . . H7B H 1.4341 0.0553 0.4057 0.130 Uiso 1 1 calc R . . H7C H 1.3338 0.0153 0.3499 0.130 Uiso 1 1 calc R . . C8 C 0.7229(3) 0.0902(2) 1.02631(18) 0.0482(6) Uani 1 1 d . . . H8 H 0.8099 0.0989 0.9921 0.058 Uiso 1 1 calc R . . C9 C 0.7327(3) 0.0056(2) 1.11555(18) 0.0475(6) Uani 1 1 d . . . H9 H 0.8241 -0.0408 1.1421 0.057 Uiso 1 1 calc R . . C10 C 0.6043(3) -0.0088(2) 1.16465(18) 0.0455(6) Uani 1 1 d . . . H10 H 0.6078 -0.0649 1.2255 0.055 Uiso 1 1 calc R . . C11 C 0.4700(3) 0.0604(2) 1.12335(17) 0.0423(5) Uani 1 1 d . . . H11 H 0.3826 0.0499 1.1550 0.051 Uiso 1 1 calc R . . C12 C 0.4678(2) 0.14583(19) 1.03381(16) 0.0343(5) Uani 1 1 d . . . C13 C 0.3263(2) 0.22344(19) 0.98448(16) 0.0343(5) Uani 1 1 d . . . C14 C 0.2155(2) 0.3465(2) 0.83933(16) 0.0369(5) Uani 1 1 d . . . C15 C 0.0754(2) 0.3604(2) 0.88808(17) 0.0407(5) Uani 1 1 d . . . H15 H -0.0085 0.4042 0.8520 0.049 Uiso 1 1 calc R . . C16 C 0.0592(2) 0.3093(2) 0.99031(16) 0.0366(5) Uani 1 1 d . . . C17 C 0.1888(2) 0.2393(2) 1.03841(17) 0.0377(5) Uani 1 1 d . . . H17 H 0.1836 0.2030 1.1067 0.045 Uiso 1 1 calc R . . C18 C -0.0899(2) 0.3317(2) 1.04599(16) 0.0362(5) Uani 1 1 d . . . C19 C -0.1133(2) 0.2485(2) 1.13131(18) 0.0454(6) Uani 1 1 d . . . H19 H -0.0351 0.1758 1.1531 0.054 Uiso 1 1 calc R . . C20 C -0.2517(2) 0.2724(2) 1.18438(18) 0.0448(6) Uani 1 1 d . . . H20 H -0.2658 0.2165 1.2420 0.054 Uiso 1 1 calc R . . C21 C -0.3685(2) 0.3792(2) 1.15182(17) 0.0366(5) Uani 1 1 d . . . C22 C -0.3481(2) 0.4629(2) 1.06633(16) 0.0371(5) Uani 1 1 d . . . H22 H -0.4270 0.5347 1.0441 0.045 Uiso 1 1 calc R . . C23 C -0.2097(2) 0.4388(2) 1.01432(16) 0.0387(5) Uani 1 1 d . . . H23 H -0.1960 0.4952 0.9570 0.046 Uiso 1 1 calc R . . C24 C -0.5726(3) 0.3147(2) 1.2515(2) 0.0576(7) Uani 1 1 d . . . H24 H -0.5285 0.2286 1.2549 0.069 Uiso 1 1 calc R . . C25 C -0.7107(3) 0.3767(3) 1.2920(2) 0.0592(7) Uani 1 1 d . . . H25 H -0.7796 0.3423 1.3281 0.071 Uiso 1 1 calc R . . C26 C -0.7267(3) 0.5016(2) 1.26790(18) 0.0479(6) Uani 1 1 d . . . H26 H -0.8111 0.5664 1.2863 0.058 Uiso 1 1 calc R . . C27 C 0.2332(2) 0.4104(2) 0.73302(17) 0.0415(5) Uani 1 1 d . . . C28 C 0.1328(3) 0.5281(3) 0.6993(2) 0.0565(7) Uani 1 1 d . . . H28 H 0.0527 0.5658 0.7429 0.068 Uiso 1 1 calc R . . C29 C 0.1506(4) 0.5900(3) 0.6011(2) 0.0732(9) Uani 1 1 d . . . H29 H 0.0825 0.6691 0.5795 0.088 Uiso 1 1 calc R . . C30 C 0.2669(4) 0.5361(3) 0.5359(2) 0.0758(9) Uani 1 1 d . . . H30 H 0.2783 0.5782 0.4701 0.091 Uiso 1 1 calc R . . C31 C 0.3672(4) 0.4191(3) 0.5683(2) 0.0732(9) Uani 1 1 d . . . H31 H 0.4465 0.3818 0.5239 0.088 Uiso 1 1 calc R . . C32 C 0.3514(3) 0.3562(3) 0.66631(19) 0.0536(6) Uani 1 1 d . . . H32 H 0.4202 0.2773 0.6875 0.064 Uiso 1 1 calc R . . N1 N 0.5931(2) 0.16093(18) 0.98620(14) 0.0416(4) Uani 1 1 d . . . N2 N 0.33938(19) 0.27830(16) 0.88692(13) 0.0352(4) Uani 1 1 d . . . N3 N -0.51138(19) 0.40073(17) 1.20573(14) 0.0394(4) Uani 1 1 d . . . N4 N -0.60673(19) 0.51759(17) 1.21534(14) 0.0413(4) Uani 1 1 d U . . O1 O 0.9118(2) 0.1720(2) 0.81333(15) 0.0768(6) Uani 1 1 d . . . O2 O 0.8415(2) 0.00588(18) 0.78088(16) 0.0752(7) Uani 1 1 d . . . O3 O 0.74754(18) 0.21303(17) 0.68441(13) 0.0570(5) Uani 1 1 d . . . S1 S 0.86929(6) 0.11982(6) 0.74001(4) 0.04634(16) 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 Ag1 0.04035(12) 0.04399(12) 0.0655(2) 0.00112(9) 0.01731(10) -0.01168(8) Ag1' 0.046(5) 0.066(5) 0.008(5) -0.006(3) -0.006(3) -0.025(4) C1 0.0296(11) 0.0467(13) 0.0382(12) 0.0014(10) 0.0015(9) -0.0046(10) C2 0.0419(13) 0.0505(15) 0.0500(14) -0.0026(11) 0.0030(11) -0.0120(11) C3 0.0473(15) 0.0616(17) 0.0556(16) -0.0171(13) 0.0032(12) -0.0065(13) C4 0.0391(13) 0.083(2) 0.0420(14) -0.0111(13) 0.0050(11) -0.0160(13) C5 0.0519(16) 0.077(2) 0.0589(17) -0.0023(15) 0.0114(13) -0.0303(15) C6 0.0470(14) 0.0538(15) 0.0578(16) -0.0077(12) 0.0105(12) -0.0148(12) C7 0.0573(18) 0.139(3) 0.0604(19) -0.034(2) 0.0232(15) -0.033(2) C8 0.0343(12) 0.0598(15) 0.0475(14) -0.0097(12) -0.0002(10) -0.0140(11) C9 0.0413(13) 0.0505(14) 0.0461(14) -0.0086(11) -0.0100(10) -0.0084(11) C10 0.0516(14) 0.0382(12) 0.0382(13) -0.0037(10) -0.0022(10) -0.0085(11) C11 0.0402(12) 0.0424(13) 0.0402(12) -0.0072(10) 0.0051(10) -0.0130(10) C12 0.0334(11) 0.0350(11) 0.0330(11) -0.0087(9) 0.0028(9) -0.0109(9) C13 0.0317(11) 0.0331(11) 0.0371(12) -0.0087(9) 0.0035(9) -0.0115(9) C14 0.0359(11) 0.0387(12) 0.0369(12) -0.0095(9) 0.0015(9) -0.0142(9) C15 0.0324(11) 0.0484(13) 0.0390(12) -0.0081(10) -0.0010(9) -0.0121(10) C16 0.0339(11) 0.0366(12) 0.0390(12) -0.0099(9) 0.0035(9) -0.0128(9) C17 0.0351(11) 0.0395(12) 0.0351(12) -0.0052(9) 0.0038(9) -0.0127(9) C18 0.0312(11) 0.0396(12) 0.0378(12) -0.0097(9) 0.0034(9) -0.0133(9) C19 0.0340(12) 0.0390(12) 0.0523(14) -0.0016(10) 0.0037(10) -0.0068(10) C20 0.0392(12) 0.0417(13) 0.0460(13) 0.0005(10) 0.0068(10) -0.0140(10) C21 0.0306(11) 0.0384(12) 0.0415(12) -0.0116(9) 0.0043(9) -0.0132(9) C22 0.0312(11) 0.0378(12) 0.0397(12) -0.0072(9) -0.0009(9) -0.0096(9) C23 0.0365(11) 0.0423(12) 0.0352(12) -0.0050(9) 0.0023(9) -0.0147(10) C24 0.0492(15) 0.0424(14) 0.0791(19) -0.0095(13) 0.0157(13) -0.0222(12) C25 0.0466(14) 0.0582(16) 0.0708(18) -0.0066(14) 0.0175(13) -0.0272(13) C26 0.0322(12) 0.0551(15) 0.0490(14) -0.0087(11) 0.0076(10) -0.0113(10) C27 0.0402(12) 0.0518(14) 0.0352(12) -0.0049(10) -0.0012(9) -0.0215(11) C28 0.0503(15) 0.0621(17) 0.0473(15) 0.0002(12) -0.0043(11) -0.0141(13) C29 0.076(2) 0.076(2) 0.0564(18) 0.0158(15) -0.0187(16) -0.0240(17) C30 0.092(2) 0.096(3) 0.0420(16) 0.0148(16) -0.0078(16) -0.049(2) C31 0.080(2) 0.097(2) 0.0431(16) -0.0121(16) 0.0178(14) -0.0411(19) C32 0.0541(15) 0.0609(16) 0.0422(14) -0.0078(12) 0.0074(11) -0.0211(13) N1 0.0334(10) 0.0466(11) 0.0412(10) -0.0045(8) 0.0010(8) -0.0132(8) N2 0.0325(9) 0.0356(9) 0.0352(10) -0.0052(8) 0.0023(7) -0.0119(8) N3 0.0318(9) 0.0394(10) 0.0453(11) -0.0089(8) 0.0068(8) -0.0135(8) N4 0.0309(9) 0.0403(10) 0.0454(11) -0.0045(8) 0.0043(8) -0.0087(8) O1 0.0546(12) 0.1232(19) 0.0515(11) -0.0329(12) 0.0074(9) -0.0248(12) O2 0.0528(11) 0.0548(11) 0.0862(14) 0.0113(10) 0.0263(10) -0.0081(9) O3 0.0374(9) 0.0552(11) 0.0545(10) -0.0015(8) 0.0012(8) 0.0044(8) S1 0.0315(3) 0.0497(3) 0.0415(3) 0.0003(3) 0.0060(2) -0.0038(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 2.249(2) 2_567 ? Ag1 N1 2.313(2) . ? Ag1 N2 2.385(2) . ? Ag1 O3 2.5112(18) . ? Ag1' O3 2.065(8) 2_567 ? Ag1' C32 2.213(9) 2_567 ? Ag1' N2 2.470(8) 2_567 ? Ag1' N4 2.575(9) . ? C1 C2 1.375(4) . ? C1 C6 1.380(4) . ? C1 S1 1.778(2) . ? C2 C3 1.385(3) . ? C2 H2 0.9300 . ? C3 C4 1.374(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 C7 1.515(3) . ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.344(3) . ? C8 C9 1.373(3) . ? C8 H8 0.9300 . ? C9 C10 1.373(3) . ? C9 H9 0.9300 . ? C10 C11 1.382(3) . ? C10 H10 0.9300 . ? C11 C12 1.388(3) . ? C11 H11 0.9300 . ? C12 N1 1.344(3) . ? C12 C13 1.498(3) . ? C13 N2 1.343(3) . ? C13 C17 1.390(3) . ? C14 N2 1.341(3) . ? C14 C15 1.388(3) . ? C14 C27 1.484(3) . ? C15 C16 1.390(3) . ? C15 H15 0.9300 . ? C16 C17 1.389(3) . ? C16 C18 1.486(3) . ? C17 H17 0.9300 . ? C18 C19 1.387(3) . ? C18 C23 1.393(3) . ? C19 C20 1.384(3) . ? C19 H19 0.9300 . ? C20 C21 1.378(3) . ? C20 H20 0.9300 . ? C21 C22 1.384(3) . ? C21 N3 1.427(3) . ? C22 C23 1.379(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N3 1.348(3) . ? C24 C25 1.360(4) . ? C24 H24 0.9300 . ? C25 C26 1.380(4) . ? C25 H25 0.9300 . ? C26 N4 1.325(3) . ? C26 H26 0.9300 . ? C27 C28 1.384(3) . ? C27 C32 1.387(3) . ? C28 C29 1.385(4) . ? C28 H28 0.9300 . ? C29 C30 1.362(5) . ? C29 H29 0.9300 . ? C30 C31 1.375(5) . ? C30 H30 0.9300 . ? C31 C32 1.384(4) . ? C31 H31 0.9300 . ? C32 Ag1' 2.213(9) 2_567 ? C32 H32 0.9300 . ? N2 Ag1' 2.470(8) 2_567 ? N3 N4 1.356(3) . ? N4 Ag1 2.249(2) 2_567 ? O1 S1 1.448(2) . ? O2 S1 1.435(2) . ? O3 S1 1.4513(17) . ? O3 Ag1' 2.065(8) 2_567 ? 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 N1 132.11(7) 2_567 . ? N4 Ag1 N2 122.44(6) 2_567 . ? N1 Ag1 N2 71.05(6) . . ? N4 Ag1 O3 91.72(7) 2_567 . ? N1 Ag1 O3 117.16(6) . . ? N2 Ag1 O3 126.79(7) . . ? O3 Ag1' C32 114.9(4) 2_567 2_567 ? O3 Ag1' N2 149.6(4) 2_567 2_567 ? C32 Ag1' N2 76.8(3) 2_567 2_567 ? O3 Ag1' N4 94.4(3) 2_567 . ? C32 Ag1' N4 112.4(4) 2_567 . ? N2 Ag1' N4 107.2(3) 2_567 . ? C2 C1 C6 119.5(2) . . ? C2 C1 S1 120.92(19) . . ? C6 C1 S1 119.55(19) . . ? C1 C2 C3 120.0(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 117.9(2) . . ? C3 C4 C7 120.6(3) . . ? C5 C4 C7 121.5(3) . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.7(3) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 122.9(2) . . ? N1 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C10 C9 C8 118.4(2) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 118.8(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N1 C12 C11 121.4(2) . . ? N1 C12 C13 116.85(18) . . ? C11 C12 C13 121.71(19) . . ? N2 C13 C17 122.1(2) . . ? N2 C13 C12 116.83(17) . . ? C17 C13 C12 121.11(19) . . ? N2 C14 C15 121.6(2) . . ? N2 C14 C27 117.47(18) . . ? C15 C14 C27 120.9(2) . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 116.91(19) . . ? C17 C16 C18 121.7(2) . . ? C15 C16 C18 121.4(2) . . ? C16 C17 C13 120.0(2) . . ? C16 C17 H17 120.0 . . ? C13 C17 H17 120.0 . . ? C19 C18 C23 118.27(19) . . ? C19 C18 C16 121.35(19) . . ? C23 C18 C16 120.37(19) . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 119.9(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.27(19) . . ? C20 C21 N3 119.24(19) . . ? C22 C21 N3 120.47(19) . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C18 121.3(2) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? N3 C24 C25 107.6(2) . . ? N3 C24 H24 126.2 . . ? C25 C24 H24 126.2 . . ? C24 C25 C26 105.2(2) . . ? C24 C25 H25 127.4 . . ? C26 C25 H25 127.4 . . ? N4 C26 C25 111.5(2) . . ? N4 C26 H26 124.3 . . ? C25 C26 H26 124.3 . . ? C28 C27 C32 118.5(2) . . ? C28 C27 C14 120.1(2) . . ? C32 C27 C14 121.4(2) . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.5(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 120.6(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 120.3(3) . . ? C31 C32 Ag1' 116.1(3) . 2_567 ? C27 C32 Ag1' 102.4(3) . 2_567 ? C31 C32 H32 119.9 . . ? C27 C32 H32 119.9 . . ? Ag1' C32 H32 48.9 2_567 . ? C8 N1 C12 118.7(2) . . ? C8 N1 Ag1 123.19(15) . . ? C12 N1 Ag1 117.96(14) . . ? C14 N2 C13 118.69(17) . . ? C14 N2 Ag1 124.06(14) . . ? C13 N2 Ag1 114.51(14) . . ? C14 N2 Ag1' 104.4(2) . 2_567 ? C13 N2 Ag1' 136.8(2) . 2_567 ? Ag1 N2 Ag1' 25.69(19) . 2_567 ? C24 N3 N4 110.58(18) . . ? C24 N3 C21 127.4(2) . . ? N4 N3 C21 121.97(17) . . ? C26 N4 N3 105.17(19) . . ? C26 N4 Ag1 124.07(16) . 2_567 ? N3 N4 Ag1 130.59(13) . 2_567 ? C26 N4 Ag1' 116.9(2) . . ? N3 N4 Ag1' 127.8(2) . . ? Ag1 N4 Ag1' 24.77(18) 2_567 . ? S1 O3 Ag1' 121.1(3) . 2_567 ? S1 O3 Ag1 99.11(9) . . ? Ag1' O3 Ag1 25.0(2) 2_567 . ? O2 S1 O1 114.64(14) . . ? O2 S1 O3 112.25(13) . . ? O1 S1 O3 111.18(13) . . ? O2 S1 C1 106.13(11) . . ? O1 S1 C1 105.96(12) . . ? O3 S1 C1 105.96(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.9(4) . . . . ? S1 C1 C2 C3 177.1(2) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 2.4(4) . . . . ? C2 C3 C4 C7 -175.7(3) . . . . ? C3 C4 C5 C6 -2.2(4) . . . . ? C7 C4 C5 C6 175.8(3) . . . . ? C2 C1 C6 C5 2.1(4) . . . . ? S1 C1 C6 C5 -177.0(2) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? N1 C8 C9 C10 1.3(4) . . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? C10 C11 C12 N1 1.0(3) . . . . ? C10 C11 C12 C13 179.7(2) . . . . ? N1 C12 C13 N2 15.3(3) . . . . ? C11 C12 C13 N2 -163.4(2) . . . . ? N1 C12 C13 C17 -163.4(2) . . . . ? C11 C12 C13 C17 17.8(3) . . . . ? N2 C14 C15 C16 3.7(3) . . . . ? C27 C14 C15 C16 -174.3(2) . . . . ? C14 C15 C16 C17 -3.4(3) . . . . ? C14 C15 C16 C18 175.1(2) . . . . ? C15 C16 C17 C13 0.3(3) . . . . ? C18 C16 C17 C13 -178.2(2) . . . . ? N2 C13 C17 C16 2.8(3) . . . . ? C12 C13 C17 C16 -178.5(2) . . . . ? C17 C16 C18 C19 -26.5(3) . . . . ? C15 C16 C18 C19 155.1(2) . . . . ? C17 C16 C18 C23 152.4(2) . . . . ? C15 C16 C18 C23 -26.0(3) . . . . ? C23 C18 C19 C20 -0.9(4) . . . . ? C16 C18 C19 C20 178.0(2) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C19 C20 C21 N3 178.3(2) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? N3 C21 C22 C23 -178.7(2) . . . . ? C21 C22 C23 C18 0.1(3) . . . . ? C19 C18 C23 C22 0.5(3) . . . . ? C16 C18 C23 C22 -178.4(2) . . . . ? N3 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 N4 0.2(3) . . . . ? N2 C14 C27 C28 -142.9(2) . . . . ? C15 C14 C27 C28 35.1(3) . . . . ? N2 C14 C27 C32 35.4(3) . . . . ? C15 C14 C27 C32 -146.6(2) . . . . ? C32 C27 C28 C29 -0.1(4) . . . . ? C14 C27 C28 C29 178.2(3) . . . . ? C27 C28 C29 C30 0.2(5) . . . . ? C28 C29 C30 C31 0.0(5) . . . . ? C29 C30 C31 C32 -0.3(5) . . . . ? C30 C31 C32 C27 0.4(5) . . . . ? C30 C31 C32 Ag1' -123.8(4) . . . 2_567 ? C28 C27 C32 C31 -0.2(4) . . . . ? C14 C27 C32 C31 -178.5(3) . . . . ? C28 C27 C32 Ag1' 130.3(3) . . . 2_567 ? C14 C27 C32 Ag1' -48.0(3) . . . 2_567 ? C9 C8 N1 C12 -2.0(4) . . . . ? C9 C8 N1 Ag1 -176.79(19) . . . . ? C11 C12 N1 C8 0.8(3) . . . . ? C13 C12 N1 C8 -177.9(2) . . . . ? C11 C12 N1 Ag1 175.86(16) . . . . ? C13 C12 N1 Ag1 -2.9(3) . . . . ? N4 Ag1 N1 C8 -73.2(2) 2_567 . . . ? N2 Ag1 N1 C8 169.8(2) . . . . ? O3 Ag1 N1 C8 47.4(2) . . . . ? N4 Ag1 N1 C12 112.00(17) 2_567 . . . ? N2 Ag1 N1 C12 -5.01(15) . . . . ? O3 Ag1 N1 C12 -127.38(16) . . . . ? C15 C14 N2 C13 -0.6(3) . . . . ? C27 C14 N2 C13 177.43(19) . . . . ? C15 C14 N2 Ag1 -160.80(17) . . . . ? C27 C14 N2 Ag1 17.2(3) . . . . ? C15 C14 N2 Ag1' -179.1(3) . . . 2_567 ? C27 C14 N2 Ag1' -1.1(3) . . . 2_567 ? C17 C13 N2 C14 -2.6(3) . . . . ? C12 C13 N2 C14 178.64(19) . . . . ? C17 C13 N2 Ag1 159.42(17) . . . . ? C12 C13 N2 Ag1 -19.3(2) . . . . ? C17 C13 N2 Ag1' 175.3(3) . . . 2_567 ? C12 C13 N2 Ag1' -3.4(4) . . . 2_567 ? N4 Ag1 N2 C14 45.57(19) 2_567 . . . ? N1 Ag1 N2 C14 174.02(19) . . . . ? O3 Ag1 N2 C14 -75.74(18) . . . . ? N4 Ag1 N2 C13 -115.36(15) 2_567 . . . ? N1 Ag1 N2 C13 13.09(14) . . . . ? O3 Ag1 N2 C13 123.33(14) . . . . ? N4 Ag1 N2 Ag1' 90.3(5) 2_567 . . 2_567 ? N1 Ag1 N2 Ag1' -141.3(5) . . . 2_567 ? O3 Ag1 N2 Ag1' -31.0(5) . . . 2_567 ? C25 C24 N3 N4 -0.1(3) . . . . ? C25 C24 N3 C21 -179.0(2) . . . . ? C20 C21 N3 C24 -34.8(4) . . . . ? C22 C21 N3 C24 143.7(3) . . . . ? C20 C21 N3 N4 146.5(2) . . . . ? C22 C21 N3 N4 -35.1(3) . . . . ? C25 C26 N4 N3 -0.2(3) . . . . ? C25 C26 N4 Ag1 -175.92(18) . . . 2_567 ? C25 C26 N4 Ag1' -148.3(3) . . . . ? C24 N3 N4 C26 0.2(3) . . . . ? C21 N3 N4 C26 179.2(2) . . . . ? C24 N3 N4 Ag1 175.49(18) . . . 2_567 ? C21 N3 N4 Ag1 -5.5(3) . . . 2_567 ? C24 N3 N4 Ag1' 143.6(3) . . . . ? C21 N3 N4 Ag1' -37.5(4) . . . . ? O3 Ag1' N4 C26 -13.2(4) 2_567 . . . ? C32 Ag1' N4 C26 106.0(3) 2_567 . . . ? N2 Ag1' N4 C26 -171.5(2) 2_567 . . . ? O3 Ag1' N4 N3 -153.0(2) 2_567 . . . ? C32 Ag1' N4 N3 -33.7(4) 2_567 . . . ? N2 Ag1' N4 N3 48.7(4) 2_567 . . . ? O3 Ag1' N4 Ag1 100.4(5) 2_567 . . 2_567 ? C32 Ag1' N4 Ag1 -140.3(6) 2_567 . . 2_567 ? N2 Ag1' N4 Ag1 -57.8(3) 2_567 . . 2_567 ? N4 Ag1 O3 S1 112.24(11) 2_567 . . . ? N1 Ag1 O3 S1 -28.07(13) . . . . ? N2 Ag1 O3 S1 -113.93(10) . . . . ? N4 Ag1 O3 Ag1' -94.6(6) 2_567 . . 2_567 ? N1 Ag1 O3 Ag1' 125.1(6) . . . 2_567 ? N2 Ag1 O3 Ag1' 39.2(6) . . . 2_567 ? Ag1' O3 S1 O2 68.1(3) 2_567 . . . ? Ag1 O3 S1 O2 81.00(12) . . . . ? Ag1' O3 S1 O1 -61.8(3) 2_567 . . . ? Ag1 O3 S1 O1 -48.91(13) . . . . ? Ag1' O3 S1 C1 -176.5(3) 2_567 . . . ? Ag1 O3 S1 C1 -163.59(10) . . . . ? C2 C1 S1 O2 12.5(2) . . . . ? C6 C1 S1 O2 -168.4(2) . . . . ? C2 C1 S1 O1 134.8(2) . . . . ? C6 C1 S1 O1 -46.1(2) . . . . ? C2 C1 S1 O3 -107.0(2) . . . . ? C6 C1 S1 O3 72.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.314 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.044 # Attachment '- Polymorph 2.cif' data_wpp1 _database_code_depnum_ccdc_archive 'CCDC 852610' #TrackingRef '- Polymorph 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 N4' _chemical_formula_weight 374.43 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.090(2) _cell_length_b 7.422(3) _cell_length_c 22.999(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.998(4) _cell_angle_gamma 90.00 _cell_volume 1890.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2640 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 22.14 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9765 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13570 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5864 _reflns_number_gt 4256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(2) _refine_ls_number_reflns 5864 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7572(3) 0.2226(5) 0.91636(12) 0.0591(8) Uani 1 1 d . . . H1 H 0.6809 0.1704 0.9139 0.071 Uiso 1 1 calc R . . C2 C 0.8241(3) 0.2223(5) 0.96869(12) 0.0674(9) Uani 1 1 d . . . H2 H 0.7929 0.1695 1.0014 0.081 Uiso 1 1 calc R . . C3 C 0.9365(3) 0.2999(5) 0.97249(13) 0.0687(10) Uani 1 1 d . . . H3 H 0.9821 0.2974 1.0076 0.082 Uiso 1 1 calc R . . C4 C 0.9824(3) 0.3813(5) 0.92458(13) 0.0657(9) Uani 1 1 d . . . H4 H 1.0578 0.4362 0.9275 0.079 Uiso 1 1 calc R . . C5 C 0.9156(2) 0.3809(4) 0.87208(12) 0.0532(8) Uani 1 1 d . . . H5 H 0.9467 0.4355 0.8397 0.064 Uiso 1 1 calc R . . C6 C 0.8033(2) 0.3006(4) 0.86723(11) 0.0468(7) Uani 1 1 d . . . C7 C 0.7309(2) 0.3006(4) 0.81052(11) 0.0439(7) Uani 1 1 d . . . C8 C 0.7836(2) 0.3190(4) 0.75744(11) 0.0471(7) Uani 1 1 d . . . H8 H 0.8667 0.3341 0.7565 0.056 Uiso 1 1 calc R . . C9 C 0.7130(2) 0.3151(4) 0.70558(11) 0.0425(7) Uani 1 1 d . . . C10 C 0.5893(2) 0.2931(4) 0.71079(11) 0.0436(7) Uani 1 1 d . . . H10 H 0.5380 0.2911 0.6775 0.052 Uiso 1 1 calc R . . C11 C 0.5419(2) 0.2742(4) 0.76464(11) 0.0442(7) Uani 1 1 d . . . C12 C 0.4093(2) 0.2546(4) 0.77075(11) 0.0447(7) Uani 1 1 d . . . C13 C 0.3590(2) 0.2591(5) 0.82341(12) 0.0637(9) Uani 1 1 d . . . H13 H 0.4076 0.2731 0.8573 0.076 Uiso 1 1 calc R . . C14 C 0.2365(3) 0.2430(6) 0.82626(14) 0.0781(11) Uani 1 1 d . . . H14 H 0.2013 0.2450 0.8621 0.094 Uiso 1 1 calc R . . C15 C 0.1667(3) 0.2241(5) 0.77622(15) 0.0661(9) Uani 1 1 d . . . H15 H 0.0832 0.2141 0.7770 0.079 Uiso 1 1 calc R . . C16 C 0.2224(3) 0.2201(5) 0.72524(14) 0.0677(10) Uani 1 1 d . . . H16 H 0.1747 0.2065 0.6910 0.081 Uiso 1 1 calc R . . C17 C 0.7643(2) 0.3346(4) 0.64757(11) 0.0434(7) Uani 1 1 d . . . C18 C 0.7010(2) 0.2719(4) 0.59805(11) 0.0468(7) Uani 1 1 d . . . H18 H 0.6262 0.2176 0.6018 0.056 Uiso 1 1 calc R . . C19 C 0.8738(2) 0.4191(4) 0.63940(12) 0.0520(8) Uani 1 1 d . . . H19 H 0.9181 0.4653 0.6715 0.062 Uiso 1 1 calc R . . C20 C 0.7454(2) 0.2875(4) 0.54344(11) 0.0472(7) Uani 1 1 d . . . H20 H 0.7011 0.2426 0.5112 0.057 Uiso 1 1 calc R . . C21 C 0.9184(3) 0.4360(4) 0.58465(12) 0.0526(8) Uani 1 1 d . . . H21 H 0.9921 0.4931 0.5804 0.063 Uiso 1 1 calc R . . C22 C 0.8549(2) 0.3692(4) 0.53657(11) 0.0440(7) Uani 1 1 d . . . C23 C 0.8575(3) 0.3050(5) 0.43118(12) 0.0578(8) Uani 1 1 d . . . H23 H 0.7917 0.2274 0.4275 0.069 Uiso 1 1 calc R . . C24 C 0.9264(3) 0.3593(5) 0.38817(13) 0.0635(9) Uani 1 1 d . . . H24 H 0.9177 0.3270 0.3491 0.076 Uiso 1 1 calc R . . C25 C 1.0121(3) 0.4718(5) 0.41339(13) 0.0596(8) Uani 1 1 d . . . H25 H 1.0715 0.5302 0.3934 0.072 Uiso 1 1 calc R . . C26 C 0.6321(2) 0.6970(4) 0.90639(11) 0.0507(8) Uani 1 1 d . . . H26 H 0.6625 0.6367 0.8749 0.061 Uiso 1 1 calc R . . C27 C 0.7008(3) 0.7102(5) 0.95812(13) 0.0630(9) Uani 1 1 d . . . H27 H 0.7768 0.6572 0.9614 0.076 Uiso 1 1 calc R . . C28 C 0.6579(3) 0.8009(5) 1.00467(13) 0.0655(9) Uani 1 1 d . . . H28 H 0.7049 0.8111 1.0392 0.079 Uiso 1 1 calc R . . C29 C 0.5443(3) 0.8766(6) 0.99974(13) 0.0709(10) Uani 1 1 d . . . H29 H 0.5141 0.9375 1.0312 0.085 Uiso 1 1 calc R . . C30 C 0.4756(3) 0.8625(5) 0.94839(12) 0.0580(8) Uani 1 1 d . . . H30 H 0.3991 0.9141 0.9455 0.070 Uiso 1 1 calc R . . C31 C 0.5184(2) 0.7731(4) 0.90128(11) 0.0452(7) Uani 1 1 d . . . C32 C 0.4437(2) 0.7585(4) 0.84552(10) 0.0437(7) Uani 1 1 d . . . C33 C 0.4958(2) 0.7426(4) 0.79255(11) 0.0447(7) Uani 1 1 d . . . H33 H 0.5795 0.7396 0.7911 0.054 Uiso 1 1 calc R . . C34 C 0.4241(2) 0.7312(4) 0.74137(11) 0.0431(7) Uani 1 1 d . . . C35 C 0.3002(2) 0.7355(4) 0.74644(11) 0.0502(7) Uani 1 1 d . . . H35 H 0.2485 0.7249 0.7134 0.060 Uiso 1 1 calc R . . C36 C 0.2534(2) 0.7556(4) 0.80057(11) 0.0470(7) Uani 1 1 d . . . C37 C 0.1211(2) 0.7800(4) 0.80668(11) 0.0492(7) Uani 1 1 d . . . C38 C 0.0768(3) 0.8380(5) 0.85833(12) 0.0573(9) Uani 1 1 d . . . H38 H 0.1283 0.8514 0.8913 0.069 Uiso 1 1 calc R . . C39 C -0.0444(3) 0.8760(5) 0.86073(13) 0.0625(9) Uani 1 1 d . . . H39 H -0.0755 0.9165 0.8952 0.075 Uiso 1 1 calc R . . C40 C -0.1182(3) 0.8533(5) 0.81199(14) 0.0614(9) Uani 1 1 d . . . H40 H -0.2002 0.8794 0.8122 0.074 Uiso 1 1 calc R . . C41 C -0.0682(3) 0.7916(5) 0.76307(14) 0.0674(9) Uani 1 1 d . . . H41 H -0.1192 0.7748 0.7301 0.081 Uiso 1 1 calc R . . C42 C 0.4775(2) 0.7214(4) 0.68373(11) 0.0419(7) Uani 1 1 d . . . C43 C 0.4234(2) 0.6214(4) 0.63848(11) 0.0483(7) Uani 1 1 d . . . H43 H 0.3530 0.5579 0.6449 0.058 Uiso 1 1 calc R . . C44 C 0.5840(2) 0.8129(4) 0.67275(11) 0.0488(7) Uani 1 1 d . . . H44 H 0.6227 0.8802 0.7023 0.059 Uiso 1 1 calc R . . C45 C 0.4709(2) 0.6133(4) 0.58442(11) 0.0462(7) Uani 1 1 d . . . H45 H 0.4328 0.5448 0.5550 0.055 Uiso 1 1 calc R . . C46 C 0.6327(2) 0.8051(4) 0.61853(11) 0.0502(7) Uani 1 1 d . . . H46 H 0.7042 0.8656 0.6121 0.060 Uiso 1 1 calc R . . C47 C 0.5752(2) 0.7072(4) 0.57391(11) 0.0417(7) Uani 1 1 d . . . C48 C 0.7248(2) 0.7767(5) 0.50005(13) 0.0555(8) Uani 1 1 d . . . H48 H 0.7796 0.8453 0.5226 0.067 Uiso 1 1 calc R . . C49 C 0.7335(3) 0.7336(5) 0.44372(13) 0.0621(9) Uani 1 1 d . . . H49 H 0.7952 0.7651 0.4198 0.075 Uiso 1 1 calc R . . C50 C 0.6325(3) 0.6333(5) 0.42875(13) 0.0616(9) Uani 1 1 d . . . H50 H 0.6148 0.5865 0.3918 0.074 Uiso 1 1 calc R . . N1 N 0.61101(19) 0.2774(3) 0.81462(9) 0.0471(6) Uani 1 1 d . . . N2 N 0.3423(2) 0.2348(4) 0.72110(10) 0.0634(7) Uani 1 1 d . . . N3 N 0.32335(19) 0.7675(3) 0.85002(9) 0.0474(6) Uani 1 1 d . . . N4 N 0.0490(2) 0.7533(4) 0.75886(10) 0.0628(7) Uani 1 1 d . . . N5 N 0.90120(18) 0.3836(3) 0.48032(9) 0.0473(6) Uani 1 1 d . . . N6 N 0.9987(2) 0.4862(4) 0.47075(11) 0.0622(7) Uani 1 1 d . . . N7 N 0.62272(19) 0.7027(3) 0.51794(9) 0.0436(6) Uani 1 1 d . . . N8 N 0.5632(2) 0.6115(4) 0.47373(10) 0.0589(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0560(18) 0.071(2) 0.0498(18) 0.0052(17) -0.0041(14) 0.0036(17) C2 0.075(2) 0.085(3) 0.0412(17) 0.0089(18) -0.0038(16) 0.007(2) C3 0.069(2) 0.089(3) 0.0462(18) -0.0058(18) -0.0125(16) 0.013(2) C4 0.0518(18) 0.088(3) 0.057(2) -0.0070(19) -0.0052(16) 0.0033(18) C5 0.0507(18) 0.067(2) 0.0419(16) -0.0004(15) 0.0017(14) 0.0035(16) C6 0.0454(16) 0.0549(19) 0.0400(15) 0.0020(15) 0.0012(12) 0.0070(15) C7 0.0401(15) 0.0465(17) 0.0448(16) 0.0006(14) -0.0006(12) 0.0058(14) C8 0.0392(15) 0.0546(19) 0.0473(16) 0.0004(14) 0.0013(13) 0.0015(14) C9 0.0412(15) 0.0449(18) 0.0413(15) -0.0005(13) 0.0017(12) 0.0053(13) C10 0.0419(15) 0.0493(18) 0.0395(15) -0.0010(14) 0.0002(12) 0.0039(14) C11 0.0413(14) 0.0475(19) 0.0437(16) -0.0007(14) 0.0018(12) 0.0022(14) C12 0.0443(15) 0.0471(19) 0.0426(16) 0.0000(14) 0.0018(12) -0.0005(14) C13 0.0498(17) 0.096(3) 0.0462(17) -0.0085(18) 0.0059(14) -0.0014(19) C14 0.0568(19) 0.123(4) 0.056(2) -0.010(2) 0.0182(16) -0.008(2) C15 0.0429(17) 0.084(3) 0.072(2) 0.000(2) 0.0057(16) -0.0021(18) C16 0.0519(19) 0.094(3) 0.0561(19) 0.002(2) -0.0054(15) -0.0094(19) C17 0.0399(15) 0.0465(18) 0.0438(16) -0.0036(13) 0.0027(12) 0.0036(13) C18 0.0346(13) 0.059(2) 0.0470(16) 0.0010(15) 0.0014(12) -0.0027(14) C19 0.0501(17) 0.063(2) 0.0425(17) -0.0076(15) -0.0017(13) -0.0089(15) C20 0.0408(15) 0.061(2) 0.0391(15) -0.0043(14) -0.0033(12) 0.0011(15) C21 0.0509(17) 0.058(2) 0.0495(17) -0.0039(15) 0.0060(14) -0.0148(15) C22 0.0416(16) 0.0505(18) 0.0398(15) 0.0026(13) 0.0021(12) 0.0005(14) C23 0.0509(17) 0.077(2) 0.0453(17) -0.0128(17) 0.0039(14) -0.0123(17) C24 0.061(2) 0.083(3) 0.0471(18) -0.0074(17) 0.0027(16) 0.0044(19) C25 0.059(2) 0.074(2) 0.0475(19) 0.0068(16) 0.0113(15) -0.0057(17) C26 0.0482(17) 0.060(2) 0.0434(16) -0.0001(14) 0.0012(13) 0.0055(14) C27 0.0484(18) 0.079(3) 0.060(2) 0.0102(19) -0.0056(15) -0.0007(17) C28 0.065(2) 0.084(3) 0.0465(18) -0.0027(18) -0.0080(15) -0.008(2) C29 0.078(2) 0.088(3) 0.0468(19) -0.0222(18) 0.0011(17) 0.007(2) C30 0.0552(18) 0.067(2) 0.0520(19) -0.0111(16) 0.0023(15) 0.0123(16) C31 0.0463(16) 0.0471(19) 0.0425(15) 0.0010(14) 0.0047(12) 0.0016(14) C32 0.0479(16) 0.0439(18) 0.0395(15) 0.0005(13) 0.0039(12) 0.0039(14) C33 0.0397(14) 0.0493(18) 0.0453(16) 0.0019(14) 0.0040(12) 0.0055(14) C34 0.0468(16) 0.0429(17) 0.0398(15) 0.0033(14) 0.0028(12) 0.0028(14) C35 0.0449(16) 0.063(2) 0.0425(16) 0.0024(15) -0.0004(12) 0.0073(15) C36 0.0470(15) 0.054(2) 0.0403(16) 0.0015(14) 0.0023(13) 0.0070(15) C37 0.0472(16) 0.056(2) 0.0441(16) 0.0006(15) 0.0033(13) 0.0041(15) C38 0.0524(18) 0.077(2) 0.0430(17) 0.0003(16) 0.0052(14) 0.0080(16) C39 0.0538(19) 0.081(3) 0.0543(19) 0.0015(17) 0.0165(16) 0.0072(18) C40 0.0433(17) 0.073(2) 0.069(2) 0.0028(18) 0.0124(16) 0.0078(16) C41 0.0451(17) 0.092(3) 0.064(2) -0.003(2) -0.0066(15) 0.0042(18) C42 0.0436(15) 0.0443(17) 0.0379(15) 0.0022(14) 0.0026(12) 0.0046(14) C43 0.0435(16) 0.0548(19) 0.0465(17) 0.0025(14) 0.0016(13) -0.0036(14) C44 0.0536(17) 0.0520(19) 0.0409(15) -0.0040(14) 0.0034(13) -0.0035(15) C45 0.0438(16) 0.0555(19) 0.0390(16) -0.0015(14) -0.0014(12) -0.0035(14) C46 0.0488(16) 0.0536(19) 0.0486(17) -0.0028(14) 0.0078(13) -0.0069(15) C47 0.0410(15) 0.0463(17) 0.0381(15) 0.0020(13) 0.0025(12) 0.0097(13) C48 0.0455(16) 0.066(2) 0.0559(18) -0.0008(16) 0.0058(13) 0.0006(16) C49 0.0540(19) 0.081(3) 0.0527(19) 0.0103(18) 0.0159(15) 0.0166(18) C50 0.063(2) 0.079(2) 0.0430(18) -0.0058(17) 0.0054(16) 0.0142(18) N1 0.0454(13) 0.0539(16) 0.0419(13) 0.0004(12) 0.0003(10) 0.0025(12) N2 0.0473(14) 0.090(2) 0.0524(15) -0.0033(15) 0.0000(11) -0.0092(15) N3 0.0467(13) 0.0532(17) 0.0421(13) 0.0006(12) 0.0013(10) 0.0088(12) N4 0.0500(14) 0.088(2) 0.0499(15) -0.0065(15) 0.0000(12) 0.0077(15) N5 0.0429(13) 0.0543(16) 0.0447(14) 0.0029(12) 0.0031(11) -0.0040(12) N6 0.0544(15) 0.076(2) 0.0564(16) 0.0001(14) 0.0080(12) -0.0121(14) N7 0.0428(13) 0.0508(15) 0.0375(13) -0.0016(11) 0.0033(10) 0.0038(11) N8 0.0573(16) 0.074(2) 0.0450(15) -0.0101(13) -0.0016(12) 0.0058(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(4) . ? C1 C6 1.390(4) . ? C1 H1 0.9300 . ? C2 C3 1.372(4) . ? C2 H2 0.9300 . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 H4 0.9300 . ? C5 C6 1.380(4) . ? C5 H5 0.9300 . ? C6 C7 1.495(3) . ? C7 N1 1.348(3) . ? C7 C8 1.388(3) . ? C8 C9 1.392(3) . ? C8 H8 0.9300 . ? C9 C10 1.393(3) . ? C9 C17 1.485(3) . ? C10 C11 1.378(3) . ? C10 H10 0.9300 . ? C11 N1 1.348(3) . ? C11 C12 1.491(3) . ? C12 N2 1.338(3) . ? C12 C13 1.360(3) . ? C13 C14 1.369(4) . ? C13 H13 0.9300 . ? C14 C15 1.360(4) . ? C14 H14 0.9300 . ? C15 C16 1.353(4) . ? C15 H15 0.9300 . ? C16 N2 1.343(3) . ? C16 H16 0.9300 . ? C17 C18 1.387(3) . ? C17 C19 1.387(4) . ? C18 C20 1.378(3) . ? C18 H18 0.9300 . ? C19 C21 1.383(4) . ? C19 H19 0.9300 . ? C20 C22 1.374(3) . ? C20 H20 0.9300 . ? C21 C22 1.372(3) . ? C21 H21 0.9300 . ? C22 N5 1.421(3) . ? C23 N5 1.340(3) . ? C23 C24 1.343(4) . ? C23 H23 0.9300 . ? C24 C25 1.371(4) . ? C24 H24 0.9300 . ? C25 N6 1.340(3) . ? C25 H25 0.9300 . ? C26 C31 1.381(4) . ? C26 C27 1.382(4) . ? C26 H26 0.9300 . ? C27 C28 1.370(4) . ? C27 H27 0.9300 . ? C28 C29 1.379(4) . ? C28 H28 0.9300 . ? C29 C30 1.376(4) . ? C29 H29 0.9300 . ? C30 C31 1.376(4) . ? C30 H30 0.9300 . ? C31 C32 1.493(3) . ? C32 N3 1.346(3) . ? C32 C33 1.380(3) . ? C33 C34 1.388(3) . ? C33 H33 0.9300 . ? C34 C35 1.386(3) . ? C34 C42 1.482(3) . ? C35 C36 1.381(3) . ? C35 H35 0.9300 . ? C36 N3 1.346(3) . ? C36 C37 1.492(3) . ? C37 N4 1.340(3) . ? C37 C38 1.378(4) . ? C38 C39 1.377(4) . ? C38 H38 0.9300 . ? C39 C40 1.363(4) . ? C39 H39 0.9300 . ? C40 C41 1.359(4) . ? C40 H40 0.9300 . ? C41 N4 1.339(3) . ? C41 H41 0.9300 . ? C42 C43 1.389(3) . ? C42 C44 1.397(4) . ? C43 C45 1.377(3) . ? C43 H43 0.9300 . ? C44 C46 1.386(3) . ? C44 H44 0.9300 . ? C45 C47 1.382(4) . ? C45 H45 0.9300 . ? C46 C47 1.386(4) . ? C46 H46 0.9300 . ? C47 N7 1.417(3) . ? C48 N7 1.342(3) . ? C48 C49 1.343(4) . ? C48 H48 0.9300 . ? C49 C50 1.373(4) . ? C49 H49 0.9300 . ? C50 N8 1.331(3) . ? C50 H50 0.9300 . ? N5 N6 1.350(3) . ? N7 N8 1.363(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.4(3) . . ? C2 C1 H1 119.8 . . ? C6 C1 H1 119.8 . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 118.9(2) . . ? C5 C6 C7 120.8(3) . . ? C1 C6 C7 120.4(3) . . ? N1 C7 C8 122.4(2) . . ? N1 C7 C6 115.2(2) . . ? C8 C7 C6 122.4(2) . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 116.1(2) . . ? C8 C9 C17 122.9(2) . . ? C10 C9 C17 120.9(2) . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? N1 C11 C10 122.5(2) . . ? N1 C11 C12 116.2(2) . . ? C10 C11 C12 121.3(2) . . ? N2 C12 C13 121.8(2) . . ? N2 C12 C11 115.9(2) . . ? C13 C12 C11 122.3(2) . . ? C12 C13 C14 119.6(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 118.0(3) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? N2 C16 C15 123.9(3) . . ? N2 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? C18 C17 C19 116.7(2) . . ? C18 C17 C9 120.2(2) . . ? C19 C17 C9 123.0(2) . . ? C20 C18 C17 122.0(2) . . ? C20 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C21 C19 C17 121.5(3) . . ? C21 C19 H19 119.3 . . ? C17 C19 H19 119.3 . . ? C22 C20 C18 120.1(2) . . ? C22 C20 H20 119.9 . . ? C18 C20 H20 119.9 . . ? C22 C21 C19 120.5(3) . . ? C22 C21 H21 119.7 . . ? C19 C21 H21 119.7 . . ? C21 C22 C20 119.1(2) . . ? C21 C22 N5 120.8(2) . . ? C20 C22 N5 120.1(2) . . ? N5 C23 C24 107.2(3) . . ? N5 C23 H23 126.4 . . ? C24 C23 H23 126.4 . . ? C23 C24 C25 106.2(3) . . ? C23 C24 H24 126.9 . . ? C25 C24 H24 126.9 . . ? N6 C25 C24 110.8(3) . . ? N6 C25 H25 124.6 . . ? C24 C25 H25 124.6 . . ? C31 C26 C27 120.3(3) . . ? C31 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.9(3) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C26 118.8(2) . . ? C30 C31 C32 120.8(2) . . ? C26 C31 C32 120.4(2) . . ? N3 C32 C33 122.3(2) . . ? N3 C32 C31 116.0(2) . . ? C33 C32 C31 121.7(2) . . ? C32 C33 C34 120.4(2) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 117.0(2) . . ? C35 C34 C42 121.4(2) . . ? C33 C34 C42 121.6(2) . . ? C36 C35 C34 119.9(2) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? N3 C36 C35 122.8(2) . . ? N3 C36 C37 116.0(2) . . ? C35 C36 C37 121.0(2) . . ? N4 C37 C38 121.9(3) . . ? N4 C37 C36 116.9(2) . . ? C38 C37 C36 121.1(2) . . ? C39 C38 C37 119.4(3) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C40 C39 C38 119.1(3) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C41 C40 C39 118.0(3) . . ? C41 C40 H40 121.0 . . ? C39 C40 H40 121.0 . . ? N4 C41 C40 124.8(3) . . ? N4 C41 H41 117.6 . . ? C40 C41 H41 117.6 . . ? C43 C42 C44 117.4(2) . . ? C43 C42 C34 121.3(2) . . ? C44 C42 C34 121.2(2) . . ? C45 C43 C42 122.0(3) . . ? C45 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C46 C44 C42 121.0(3) . . ? C46 C44 H44 119.5 . . ? C42 C44 H44 119.5 . . ? C43 C45 C47 120.0(3) . . ? C43 C45 H45 120.0 . . ? C47 C45 H45 120.0 . . ? C47 C46 C44 120.1(3) . . ? C47 C46 H46 119.9 . . ? C44 C46 H46 119.9 . . ? C45 C47 C46 119.5(2) . . ? C45 C47 N7 120.1(2) . . ? C46 C47 N7 120.4(2) . . ? N7 C48 C49 107.6(3) . . ? N7 C48 H48 126.2 . . ? C49 C48 H48 126.2 . . ? C48 C49 C50 105.8(3) . . ? C48 C49 H49 127.1 . . ? C50 C49 H49 127.1 . . ? N8 C50 C49 111.6(3) . . ? N8 C50 H50 124.2 . . ? C49 C50 H50 124.2 . . ? C11 N1 C7 117.5(2) . . ? C12 N2 C16 117.2(2) . . ? C36 N3 C32 117.5(2) . . ? C41 N4 C37 116.7(3) . . ? C23 N5 N6 111.5(2) . . ? C23 N5 C22 127.1(2) . . ? N6 N5 C22 121.4(2) . . ? C25 N6 N5 104.3(2) . . ? C48 N7 N8 111.0(2) . . ? C48 N7 C47 129.0(2) . . ? N8 N7 C47 120.1(2) . . ? C50 N8 N7 104.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.3(5) . . . . ? C1 C2 C3 C4 1.2(6) . . . . ? C2 C3 C4 C5 -1.5(5) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? C4 C5 C6 C7 179.8(3) . . . . ? C2 C1 C6 C5 -1.4(5) . . . . ? C2 C1 C6 C7 179.9(3) . . . . ? C5 C6 C7 N1 -157.9(3) . . . . ? C1 C6 C7 N1 20.7(4) . . . . ? C5 C6 C7 C8 23.5(4) . . . . ? C1 C6 C7 C8 -157.9(3) . . . . ? N1 C7 C8 C9 0.4(4) . . . . ? C6 C7 C8 C9 178.9(3) . . . . ? C7 C8 C9 C10 0.3(4) . . . . ? C7 C8 C9 C17 179.8(3) . . . . ? C8 C9 C10 C11 -0.8(4) . . . . ? C17 C9 C10 C11 179.7(3) . . . . ? C9 C10 C11 N1 0.6(4) . . . . ? C9 C10 C11 C12 178.6(3) . . . . ? N1 C11 C12 N2 -174.1(3) . . . . ? C10 C11 C12 N2 7.8(4) . . . . ? N1 C11 C12 C13 6.9(5) . . . . ? C10 C11 C12 C13 -171.3(3) . . . . ? N2 C12 C13 C14 0.0(5) . . . . ? C11 C12 C13 C14 179.1(3) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C13 C14 C15 C16 0.7(6) . . . . ? C14 C15 C16 N2 -0.4(6) . . . . ? C8 C9 C17 C18 158.5(3) . . . . ? C10 C9 C17 C18 -22.1(4) . . . . ? C8 C9 C17 C19 -23.5(4) . . . . ? C10 C9 C17 C19 156.0(3) . . . . ? C19 C17 C18 C20 1.8(4) . . . . ? C9 C17 C18 C20 180.0(3) . . . . ? C18 C17 C19 C21 -1.4(4) . . . . ? C9 C17 C19 C21 -179.5(3) . . . . ? C17 C18 C20 C22 -0.8(4) . . . . ? C17 C19 C21 C22 0.1(5) . . . . ? C19 C21 C22 C20 0.9(5) . . . . ? C19 C21 C22 N5 -179.0(3) . . . . ? C18 C20 C22 C21 -0.6(4) . . . . ? C18 C20 C22 N5 179.4(3) . . . . ? N5 C23 C24 C25 0.1(4) . . . . ? C23 C24 C25 N6 0.8(4) . . . . ? C31 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 1.0(5) . . . . ? C27 C28 C29 C30 -0.6(6) . . . . ? C28 C29 C30 C31 0.0(5) . . . . ? C29 C30 C31 C26 0.1(5) . . . . ? C29 C30 C31 C32 -179.8(3) . . . . ? C27 C26 C31 C30 0.3(5) . . . . ? C27 C26 C31 C32 -179.8(3) . . . . ? C30 C31 C32 N3 -26.1(4) . . . . ? C26 C31 C32 N3 154.0(3) . . . . ? C30 C31 C32 C33 151.9(3) . . . . ? C26 C31 C32 C33 -28.0(4) . . . . ? N3 C32 C33 C34 -1.5(5) . . . . ? C31 C32 C33 C34 -179.3(3) . . . . ? C32 C33 C34 C35 -0.4(5) . . . . ? C32 C33 C34 C42 177.6(3) . . . . ? C33 C34 C35 C36 1.8(5) . . . . ? C42 C34 C35 C36 -176.1(3) . . . . ? C34 C35 C36 N3 -1.5(5) . . . . ? C34 C35 C36 C37 173.5(3) . . . . ? N3 C36 C37 N4 -174.5(3) . . . . ? C35 C36 C37 N4 10.2(5) . . . . ? N3 C36 C37 C38 9.4(5) . . . . ? C35 C36 C37 C38 -166.0(3) . . . . ? N4 C37 C38 C39 -2.3(5) . . . . ? C36 C37 C38 C39 173.7(3) . . . . ? C37 C38 C39 C40 0.7(5) . . . . ? C38 C39 C40 C41 0.8(5) . . . . ? C39 C40 C41 N4 -0.9(6) . . . . ? C35 C34 C42 C43 -36.4(4) . . . . ? C33 C34 C42 C43 145.7(3) . . . . ? C35 C34 C42 C44 143.3(3) . . . . ? C33 C34 C42 C44 -34.5(4) . . . . ? C44 C42 C43 C45 -0.9(4) . . . . ? C34 C42 C43 C45 178.9(3) . . . . ? C43 C42 C44 C46 0.6(4) . . . . ? C34 C42 C44 C46 -179.2(3) . . . . ? C42 C43 C45 C47 -0.2(4) . . . . ? C42 C44 C46 C47 0.8(4) . . . . ? C43 C45 C47 C46 1.6(4) . . . . ? C43 C45 C47 N7 -178.5(2) . . . . ? C44 C46 C47 C45 -1.9(4) . . . . ? C44 C46 C47 N7 178.2(3) . . . . ? N7 C48 C49 C50 0.6(4) . . . . ? C48 C49 C50 N8 -0.7(4) . . . . ? C10 C11 N1 C7 0.2(4) . . . . ? C12 C11 N1 C7 -178.0(2) . . . . ? C8 C7 N1 C11 -0.6(4) . . . . ? C6 C7 N1 C11 -179.2(3) . . . . ? C13 C12 N2 C16 0.3(5) . . . . ? C11 C12 N2 C16 -178.8(3) . . . . ? C15 C16 N2 C12 -0.1(5) . . . . ? C35 C36 N3 C32 -0.3(5) . . . . ? C37 C36 N3 C32 -175.6(2) . . . . ? C33 C32 N3 C36 1.8(4) . . . . ? C31 C32 N3 C36 179.7(2) . . . . ? C40 C41 N4 C37 -0.6(6) . . . . ? C38 C37 N4 C41 2.2(5) . . . . ? C36 C37 N4 C41 -173.9(3) . . . . ? C24 C23 N5 N6 -1.0(4) . . . . ? C24 C23 N5 C22 178.2(3) . . . . ? C21 C22 N5 C23 170.6(3) . . . . ? C20 C22 N5 C23 -9.3(4) . . . . ? C21 C22 N5 N6 -10.3(4) . . . . ? C20 C22 N5 N6 169.8(3) . . . . ? C24 C25 N6 N5 -1.4(4) . . . . ? C23 N5 N6 C25 1.5(3) . . . . ? C22 N5 N6 C25 -177.8(3) . . . . ? C49 C48 N7 N8 -0.3(3) . . . . ? C49 C48 N7 C47 178.7(3) . . . . ? C45 C47 N7 C48 -176.4(3) . . . . ? C46 C47 N7 C48 3.4(4) . . . . ? C45 C47 N7 N8 2.5(4) . . . . ? C46 C47 N7 N8 -177.6(3) . . . . ? C49 C50 N8 N7 0.5(4) . . . . ? C48 N7 N8 C50 -0.1(3) . . . . ? C47 N7 N8 C50 -179.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.148 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.042 # Attachment '- Polymorph 1.cif' data_jf_Polymorph_1 _database_code_depnum_ccdc_archive 'CCDC 852655' #TrackingRef '- Polymorph 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 N4' _chemical_formula_weight 374.43 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.434(5) _cell_length_b 5.479(5) _cell_length_c 17.999(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 92.686(5) _cell_angle_gamma 90.000(5) _cell_volume 1914.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4935 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.41 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9767 _exptl_absorpt_correction_T_max 0.9844 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10979 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3375 _reflns_number_gt 2649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+0.2540P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0073(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3375 _refine_ls_number_parameters 313 _refine_ls_number_restraints 287 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.008 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N3 N 0.51112(6) 0.1349(2) 0.37474(7) 0.0505(3) Uani 1 1 d U . . N1 N 0.83297(7) 0.2396(3) 0.07141(8) 0.0633(4) Uani 1 1 d U . . C20 C 0.56629(8) 0.1457(3) 0.32655(8) 0.0484(4) Uani 1 1 d U . . C17 C 0.67368(8) 0.1774(3) 0.22802(9) 0.0510(4) Uani 1 1 d U . . C7 C 0.83220(9) 0.3833(3) 0.13127(10) 0.0601(4) Uani 1 1 d U C . N4 N 0.49688(8) 0.3318(2) 0.41726(8) 0.0622(4) Uani 1 1 d U . . C11 C 0.78231(8) 0.0746(3) 0.06198(9) 0.0584(4) Uani 1 1 d U B . C8 C 0.78206(8) 0.3672(3) 0.18302(10) 0.0601(5) Uani 1 1 d U . . H8 H 0.7838 0.4704 0.2241 0.072 Uiso 1 1 calc R . . C12 C 0.78499(9) -0.0841(3) -0.00498(10) 0.0615(5) Uani 1 1 d U . . C10 C 0.73018(8) 0.0513(3) 0.11125(9) 0.0595(4) Uani 1 1 d U . . H10 H 0.6956 -0.0636 0.1022 0.071 Uiso 1 1 calc R B . C9 C 0.72907(8) 0.1977(3) 0.17414(9) 0.0545(4) Uani 1 1 d U B . C19 C 0.57604(8) -0.0367(3) 0.27513(9) 0.0561(4) Uani 1 1 d U . . H19 H 0.5466 -0.1706 0.2728 0.067 Uiso 1 1 calc R . . C18 C 0.62906(9) -0.0211(3) 0.22739(9) 0.0566(4) Uani 1 1 d U . . H18 H 0.6353 -0.1469 0.1937 0.068 Uiso 1 1 calc R . . C21 C 0.61079(9) 0.3423(3) 0.32939(10) 0.0599(5) Uani 1 1 d U . . H21 H 0.6054 0.4653 0.3643 0.072 Uiso 1 1 calc R . . C22 C 0.66307(9) 0.3565(3) 0.28074(10) 0.0609(5) Uani 1 1 d U . . H22 H 0.6923 0.4909 0.2832 0.073 Uiso 1 1 calc R . . C23 C 0.46625(9) -0.0485(3) 0.38583(10) 0.0625(5) Uani 1 1 d U . . H23 H 0.4659 -0.2005 0.3629 0.075 Uiso 1 1 calc R . . C1 C 0.88915(9) 0.5654(4) 0.14001(10) 0.0660(5) Uani 1 1 d U . . C24 C 0.42204(9) 0.0292(4) 0.43620(10) 0.0658(5) Uani 1 1 d U . . H24 H 0.3853 -0.0564 0.4548 0.079 Uiso 1 1 calc R . . C25 C 0.44324(9) 0.2643(3) 0.45434(10) 0.0644(5) Uani 1 1 d U . . H25 H 0.4221 0.3626 0.4886 0.077 Uiso 1 1 calc R . . C15 C 0.78907(13) -0.3828(5) -0.12730(14) 0.0973(8) Uani 1 1 d U . . H15 H 0.7969 -0.5053 -0.1617 0.117 Uiso 1 1 calc R A 1 C14 C 0.8279(3) -0.1611(18) -0.1240(3) 0.0857(19) Uani 0.510(10) 1 d PU B 1 H14 H 0.8546 -0.1163 -0.1633 0.103 Uiso 0.510(10) 1 calc PR B 1 C13 C 0.8254(3) -0.0142(16) -0.0619(3) 0.0729(16) Uani 0.510(10) 1 d PU B 1 H13 H 0.8507 0.1299 -0.0587 0.088 Uiso 0.510(10) 1 calc PR B 1 C16 C 0.7446(7) -0.399(4) -0.0811(9) 0.112(2) Uani 0.510(10) 1 d PU B 1 H16 H 0.7125 -0.5220 -0.0910 0.134 Uiso 0.510(10) 1 calc PR B 1 N2 N 0.7330(7) -0.261(4) -0.0142(9) 0.117(2) Uani 0.510(10) 1 d PRU B 1 C13' C 0.8463(5) -0.1208(15) -0.0413(5) 0.087(2) Uani 0.490(10) 1 d PU B 2 H13' H 0.8860 -0.0384 -0.0251 0.104 Uiso 0.490(10) 1 calc PR B 2 C14' C 0.8481(5) -0.2781(17) -0.1009(5) 0.102(3) Uani 0.490(10) 1 d PU B 2 H14' H 0.8895 -0.3118 -0.1226 0.123 Uiso 0.490(10) 1 calc PR B 2 C16' C 0.7355(7) -0.398(4) -0.0782(9) 0.109(2) Uani 0.490(10) 1 d PU B 2 H16' H 0.7004 -0.5130 -0.0842 0.131 Uiso 0.490(10) 1 calc PR B 2 N2' N 0.7379(7) -0.239(4) -0.0225(9) 0.109(2) Uani 0.490(10) 1 d PRU B 2 C2 C 0.9328(9) 0.608(3) 0.0837(12) 0.086(3) Uani 0.43(3) 1 d PU C 1 H2 H 0.9280 0.5181 0.0399 0.103 Uiso 0.43(3) 1 calc PR C 1 C3 C 0.9835(8) 0.782(3) 0.0909(11) 0.102(3) Uani 0.43(3) 1 d PU C 1 H3 H 1.0114 0.8175 0.0516 0.123 Uiso 0.43(3) 1 calc PR C 1 C2' C 0.9490(6) 0.529(3) 0.1007(6) 0.084(2) Uani 0.57(3) 1 d PU C 2 H2' H 0.9526 0.3968 0.0688 0.101 Uiso 0.57(3) 1 calc PR C 2 C3' C 1.0031(8) 0.696(3) 0.1103(5) 0.104(3) Uani 0.57(3) 1 d PU C 2 H3' H 1.0445 0.6730 0.0874 0.125 Uiso 0.57(3) 1 calc PR C 2 C4 C 0.99202(14) 0.9024(5) 0.15685(17) 0.1111(9) Uani 1 1 d U . . H4 H 1.0328 0.9837 0.1702 0.133 Uiso 1 1 calc R C 1 C5 C 0.93887(13) 0.8980(4) 0.20172(14) 0.0933(7) Uani 1 1 d U C . H5 H 0.9372 1.0132 0.2395 0.112 Uiso 1 1 calc R . . C6 C 0.88781(10) 0.7323(4) 0.19397(11) 0.0695(5) Uani 1 1 d U C . H6 H 0.8517 0.7342 0.2261 0.083 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 N3 0.0552(7) 0.0407(7) 0.0553(7) -0.0036(6) -0.0017(6) 0.0011(5) N1 0.0627(8) 0.0651(9) 0.0616(9) 0.0016(7) -0.0007(7) -0.0085(7) C20 0.0503(8) 0.0400(8) 0.0541(9) 0.0004(7) -0.0062(7) 0.0025(6) C17 0.0521(8) 0.0440(8) 0.0560(9) 0.0004(7) -0.0051(7) 0.0025(6) C7 0.0610(10) 0.0588(10) 0.0598(10) 0.0030(8) -0.0051(8) -0.0072(8) N4 0.0689(9) 0.0508(8) 0.0669(9) -0.0144(7) 0.0040(7) -0.0014(7) C11 0.0564(9) 0.0607(10) 0.0575(9) 0.0008(8) -0.0039(7) -0.0042(8) C8 0.0633(10) 0.0570(10) 0.0596(10) -0.0033(8) -0.0010(8) -0.0061(8) C12 0.0565(9) 0.0688(11) 0.0590(10) -0.0044(8) 0.0000(8) -0.0064(8) C10 0.0556(9) 0.0592(10) 0.0634(10) -0.0038(8) -0.0024(8) -0.0061(7) C9 0.0542(9) 0.0504(9) 0.0583(9) 0.0029(7) -0.0056(7) 0.0008(7) C19 0.0620(10) 0.0444(9) 0.0615(9) -0.0060(7) -0.0004(8) -0.0078(7) C18 0.0644(9) 0.0478(9) 0.0576(9) -0.0095(7) 0.0010(8) -0.0030(7) C21 0.0669(10) 0.0424(9) 0.0705(11) -0.0125(8) 0.0044(8) -0.0032(7) C22 0.0617(10) 0.0446(9) 0.0767(11) -0.0060(8) 0.0045(8) -0.0093(7) C23 0.0659(10) 0.0466(9) 0.0751(11) -0.0061(8) 0.0046(9) -0.0079(8) C1 0.0646(10) 0.0675(11) 0.0655(11) 0.0091(9) -0.0011(8) -0.0128(9) C24 0.0610(10) 0.0653(11) 0.0713(11) -0.0026(9) 0.0072(8) -0.0062(8) C25 0.0630(10) 0.0671(11) 0.0633(10) -0.0099(9) 0.0046(8) 0.0017(8) C15 0.0980(17) 0.113(2) 0.0815(15) -0.0369(14) 0.0043(13) -0.0084(14) C14 0.075(3) 0.123(6) 0.059(3) -0.015(3) 0.002(2) -0.002(3) C13 0.067(3) 0.089(4) 0.063(3) -0.004(3) 0.002(2) -0.008(3) C16 0.108(4) 0.123(4) 0.105(4) -0.044(3) 0.012(4) -0.040(4) N2 0.117(4) 0.128(4) 0.105(4) -0.041(4) 0.003(4) -0.044(3) C13' 0.083(4) 0.085(5) 0.093(5) -0.023(4) 0.026(4) -0.030(3) C14' 0.105(5) 0.110(6) 0.095(5) -0.029(4) 0.039(4) -0.026(4) C16' 0.102(4) 0.124(4) 0.101(4) -0.043(3) 0.000(3) -0.044(4) N2' 0.094(3) 0.136(5) 0.099(4) -0.040(3) 0.032(3) -0.040(3) C2 0.084(7) 0.085(7) 0.091(7) -0.011(6) 0.025(5) -0.023(5) C3 0.088(5) 0.113(7) 0.108(6) -0.002(5) 0.028(5) -0.039(4) C2' 0.082(5) 0.090(6) 0.082(4) -0.001(4) 0.005(3) -0.027(4) C3' 0.094(5) 0.125(7) 0.095(4) 0.008(4) 0.011(4) -0.048(5) C4 0.1028(17) 0.114(2) 0.116(2) -0.0042(17) 0.0057(16) -0.0577(16) C5 0.1047(16) 0.0831(15) 0.0905(15) -0.0077(12) -0.0116(13) -0.0211(13) C6 0.0719(11) 0.0687(11) 0.0675(11) -0.0054(9) -0.0005(9) -0.0204(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C23 1.351(2) . ? N3 N4 1.3586(19) . ? N3 C20 1.412(2) . ? N1 C7 1.335(2) . ? N1 C11 1.342(2) . ? C20 C21 1.381(2) . ? C20 C19 1.381(2) . ? C17 C22 1.387(2) . ? C17 C18 1.391(2) . ? C17 C9 1.486(2) . ? C7 C8 1.382(2) . ? C7 C1 1.493(2) . ? N4 C25 1.317(2) . ? C11 C10 1.383(2) . ? C11 C12 1.489(3) . ? C8 C9 1.390(2) . ? C8 H8 0.9300 . ? C12 N2' 1.277(16) . ? C12 C13 1.375(6) . ? C12 C13' 1.400(7) . ? C12 N2 1.405(16) . ? C10 C9 1.389(2) . ? C10 H10 0.9300 . ? C19 C18 1.375(2) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C21 C22 1.374(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.347(2) . ? C23 H23 0.9300 . ? C1 C6 1.335(3) . ? C1 C2 1.373(16) . ? C1 C2' 1.404(13) . ? C24 C25 1.387(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C15 C16 1.231(13) . ? C15 C14' 1.349(9) . ? C15 C16' 1.400(12) . ? C15 C14 1.429(9) . ? C15 H15 0.9300 . ? C14 C13 1.379(8) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C16 N2 1.4470 . ? C16 H16 0.9300 . ? C13' C14' 1.377(9) . ? C13' H13' 0.9300 . ? C14' H14' 0.9300 . ? C16' N2' 1.3286 . ? C16' H16' 0.9300 . ? C2 C3 1.374(18) . ? C2 H2 0.9300 . ? C3 C4 1.360(16) . ? C3 H3 0.9300 . ? C2' C3' 1.395(14) . ? C2' H2' 0.9300 . ? C3' C4 1.432(14) . ? C3' H3' 0.9300 . ? C4 C5 1.341(4) . ? C4 H4 0.9300 . ? C5 C6 1.347(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 N3 N4 110.93(14) . . ? C23 N3 C20 129.49(13) . . ? N4 N3 C20 119.57(12) . . ? C7 N1 C11 117.62(15) . . ? C21 C20 C19 118.95(16) . . ? C21 C20 N3 120.15(14) . . ? C19 C20 N3 120.89(13) . . ? C22 C17 C18 116.50(16) . . ? C22 C17 C9 121.90(15) . . ? C18 C17 C9 121.59(15) . . ? N1 C7 C8 122.75(15) . . ? N1 C7 C1 116.29(16) . . ? C8 C7 C1 120.97(16) . . ? C25 N4 N3 104.44(14) . . ? N1 C11 C10 122.44(16) . . ? N1 C11 C12 116.26(15) . . ? C10 C11 C12 121.30(15) . . ? C7 C8 C9 120.47(16) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N2' C12 C13 115.4(7) . . ? N2' C12 C13' 113.9(7) . . ? C13 C12 C13' 33.2(3) . . ? N2' C12 N2 7.5(14) . . ? C13 C12 N2 122.5(6) . . ? C13' C12 N2 117.9(7) . . ? N2' C12 C11 122.4(6) . . ? C13 C12 C11 118.9(3) . . ? C13' C12 C11 121.7(3) . . ? N2 C12 C11 116.6(6) . . ? C11 C10 C9 120.60(16) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C9 C8 116.11(16) . . ? C10 C9 C17 121.86(15) . . ? C8 C9 C17 122.02(15) . . ? C18 C19 C20 120.27(15) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C18 C17 121.94(15) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C22 C21 C20 120.07(15) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 122.26(15) . . ? C21 C22 H22 118.9 . . ? C17 C22 H22 118.9 . . ? C24 C23 N3 107.52(16) . . ? C24 C23 H23 126.2 . . ? N3 C23 H23 126.2 . . ? C6 C1 C2 117.0(6) . . ? C6 C1 C2' 120.5(5) . . ? C2 C1 C2' 25.3(6) . . ? C6 C1 C7 119.65(17) . . ? C2 C1 C7 121.2(7) . . ? C2' C1 C7 118.7(6) . . ? C23 C24 C25 105.07(16) . . ? C23 C24 H24 127.5 . . ? C25 C24 H24 127.5 . . ? N4 C25 C24 112.03(16) . . ? N4 C25 H25 124.0 . . ? C24 C25 H25 124.0 . . ? C16 C15 C14' 113.9(8) . . ? C16 C15 C16' 3.4(15) . . ? C14' C15 C16' 116.7(7) . . ? C16 C15 C14 114.8(9) . . ? C14' C15 C14 35.5(4) . . ? C16' C15 C14 115.6(8) . . ? C16 C15 H15 122.6 . . ? C14' C15 H15 112.3 . . ? C16' C15 H15 121.7 . . ? C14 C15 H15 122.6 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C12 C13 C14 118.9(6) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C16 N2 131.8(8) . . ? C15 C16 H16 114.1 . . ? N2 C16 H16 114.1 . . ? C12 N2 C16 108.7(6) . . ? C14' C13' C12 120.5(6) . . ? C14' C13' H13' 119.8 . . ? C12 C13' H13' 119.8 . . ? C15 C14' C13' 119.2(6) . . ? C15 C14' H14' 120.4 . . ? C13' C14' H14' 120.4 . . ? N2' C16' C15 115.8(7) . . ? N2' C16' H16' 122.1 . . ? C15 C16' H16' 122.1 . . ? C12 N2' C16' 128.5(6) . . ? C1 C2 C3 121.0(12) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 118.4(11) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3' C2' C1 118.8(9) . . ? C3' C2' H2' 120.6 . . ? C1 C2' H2' 120.6 . . ? C2' C3' C4 117.2(9) . . ? C2' C3' H3' 121.4 . . ? C4 C3' H3' 121.4 . . ? C5 C4 C3 116.9(5) . . ? C5 C4 C3' 118.6(4) . . ? C3 C4 C3' 28.6(5) . . ? C5 C4 H4 121.6 . . ? C3 C4 H4 121.6 . . ? C3' C4 H4 112.4 . . ? C4 C5 C6 122.3(2) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C1 C6 C5 119.8(2) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? 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 C23 N3 C20 C21 -173.10(16) . . . . ? N4 N3 C20 C21 8.2(2) . . . . ? C23 N3 C20 C19 8.0(2) . . . . ? N4 N3 C20 C19 -170.71(14) . . . . ? C11 N1 C7 C8 0.3(3) . . . . ? C11 N1 C7 C1 -179.84(15) . . . . ? C23 N3 N4 C25 0.36(18) . . . . ? C20 N3 N4 C25 179.32(13) . . . . ? C7 N1 C11 C10 0.5(3) . . . . ? C7 N1 C11 C12 -179.55(15) . . . . ? N1 C7 C8 C9 -0.5(3) . . . . ? C1 C7 C8 C9 179.70(15) . . . . ? N1 C11 C12 N2' -176.0(11) . . . . ? C10 C11 C12 N2' 4.0(11) . . . . ? N1 C11 C12 C13 -17.3(4) . . . . ? C10 C11 C12 C13 162.6(4) . . . . ? N1 C11 C12 C13' 21.2(6) . . . . ? C10 C11 C12 C13' -158.8(5) . . . . ? N1 C11 C12 N2 178.5(9) . . . . ? C10 C11 C12 N2 -1.5(9) . . . . ? N1 C11 C10 C9 -1.2(3) . . . . ? C12 C11 C10 C9 178.87(16) . . . . ? C11 C10 C9 C8 1.0(2) . . . . ? C11 C10 C9 C17 179.87(15) . . . . ? C7 C8 C9 C10 -0.2(2) . . . . ? C7 C8 C9 C17 -179.10(15) . . . . ? C22 C17 C9 C10 -164.85(16) . . . . ? C18 C17 C9 C10 14.1(2) . . . . ? C22 C17 C9 C8 14.0(2) . . . . ? C18 C17 C9 C8 -167.02(15) . . . . ? C21 C20 C19 C18 -0.4(2) . . . . ? N3 C20 C19 C18 178.52(14) . . . . ? C20 C19 C18 C17 -1.0(3) . . . . ? C22 C17 C18 C19 1.6(2) . . . . ? C9 C17 C18 C19 -177.43(15) . . . . ? C19 C20 C21 C22 1.1(2) . . . . ? N3 C20 C21 C22 -177.81(14) . . . . ? C20 C21 C22 C17 -0.4(3) . . . . ? C18 C17 C22 C21 -0.9(2) . . . . ? C9 C17 C22 C21 178.16(15) . . . . ? N4 N3 C23 C24 0.02(19) . . . . ? C20 N3 C23 C24 -178.80(15) . . . . ? N1 C7 C1 C6 172.91(17) . . . . ? C8 C7 C1 C6 -7.2(3) . . . . ? N1 C7 C1 C2 10.3(12) . . . . ? C8 C7 C1 C2 -169.9(11) . . . . ? N1 C7 C1 C2' -18.9(7) . . . . ? C8 C7 C1 C2' 160.9(7) . . . . ? N3 C23 C24 C25 -0.4(2) . . . . ? N3 N4 C25 C24 -0.6(2) . . . . ? C23 C24 C25 N4 0.6(2) . . . . ? C16 C15 C14 C13 15.2(11) . . . . ? C14' C15 C14 C13 -81.8(8) . . . . ? C16' C15 C14 C13 18.9(10) . . . . ? N2' C12 C13 C14 -19.9(12) . . . . ? C13' C12 C13 C14 75.5(10) . . . . ? N2 C12 C13 C14 -16.8(11) . . . . ? C11 C12 C13 C14 -180.0(4) . . . . ? C15 C14 C13 C12 -0.6(7) . . . . ? C14' C15 C16 N2 24.1(14) . . . . ? C16' C15 C16 N2 -120(30) . . . . ? C14 C15 C16 N2 -14.9(13) . . . . ? N2' C12 N2 C16 39(11) . . . . ? C13 C12 N2 C16 17.3(9) . . . . ? C13' C12 N2 C16 -21.0(8) . . . . ? C11 C12 N2 C16 -179.17(17) . . . . ? C15 C16 N2 C12 -0.7(4) . . . . ? N2' C12 C13' C14' 12.6(13) . . . . ? C13 C12 C13' C14' -87.8(12) . . . . ? N2 C12 C13' C14' 19.7(12) . . . . ? C11 C12 C13' C14' 176.7(5) . . . . ? C16 C15 C14' C13' -25.0(14) . . . . ? C16' C15 C14' C13' -22.7(13) . . . . ? C14 C15 C14' C13' 74.6(9) . . . . ? C12 C13' C14' C15 4.8(10) . . . . ? C16 C15 C16' N2' 60(29) . . . . ? C14' C15 C16' N2' 23.1(10) . . . . ? C14 C15 C16' N2' -16.6(8) . . . . ? C13 C12 N2' C16' 24.1(12) . . . . ? C13' C12 N2' C16' -12.5(12) . . . . ? N2 C12 N2' C16' -136(12) . . . . ? C11 C12 N2' C16' -176.49(18) . . . . ? C15 C16' N2' C12 -5.2(3) . . . . ? C6 C1 C2 C3 14.4(14) . . . . ? C2' C1 C2 C3 -90(3) . . . . ? C7 C1 C2 C3 177.5(7) . . . . ? C1 C2 C3 C4 3.6(14) . . . . ? C6 C1 C2' C3' -10.3(8) . . . . ? C2 C1 C2' C3' 79(3) . . . . ? C7 C1 C2' C3' -178.3(5) . . . . ? C1 C2' C3' C4 -3.6(9) . . . . ? C2 C3 C4 C5 -19.5(15) . . . . ? C2 C3 C4 C3' 81.6(19) . . . . ? C2' C3' C4 C5 15.4(11) . . . . ? C2' C3' C4 C3 -78.9(19) . . . . ? C3 C4 C5 C6 18.4(12) . . . . ? C3' C4 C5 C6 -14.0(9) . . . . ? C2 C1 C6 C5 -16.2(12) . . . . ? C2' C1 C6 C5 12.5(8) . . . . ? C7 C1 C6 C5 -179.54(18) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.262 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.042 # Attachment '- Complex 2.cif' data_jf_2 _database_code_depnum_ccdc_archive 'CCDC 853515' #TrackingRef '- Complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H36 Ag2 Cl2 N8 O8' _chemical_formula_weight 1163.51 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' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.667(5) _cell_length_b 22.086(5) _cell_length_c 14.712(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 119.395(5) _cell_angle_gamma 90.000(5) _cell_volume 4718(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1877 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 18.88 _exptl_crystal_description Columnar _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7519 _exptl_absorpt_correction_T_max 0.8238 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16594 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4174 _reflns_number_gt 2198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+4.2797P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4174 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.18895(3) 0.79239(2) 0.84465(4) 0.0811(2) Uani 1 1 d . . . Cl1 Cl 0.68728(11) 0.67759(8) 0.67792(12) 0.0815(5) Uani 1 1 d . . . N3 N -0.1075(3) 0.87444(19) 0.8114(3) 0.0520(10) Uani 1 1 d . . . C10 C -0.1330(3) 0.9329(2) 0.7960(4) 0.0524(12) Uani 1 1 d . . . C6 C -0.0174(3) 0.8614(2) 0.8614(4) 0.0506(12) Uani 1 1 d . . . C8 C 0.0246(3) 0.9666(2) 0.8830(3) 0.0497(12) Uani 1 1 d . . . C11 C -0.2338(3) 0.9452(2) 0.7417(4) 0.0577(14) Uani 1 1 d . . . O2 O 0.7167(3) 0.63890(18) 0.6223(3) 0.1080(15) Uani 1 1 d . . . N4 N -0.0534(3) 0.7567(2) 0.8693(3) 0.0629(12) Uani 1 1 d . . . C5 C 0.0094(4) 0.7963(2) 0.8748(4) 0.0576(13) Uani 1 1 d . . . C4 C 0.0937(4) 0.7770(3) 0.8880(4) 0.0689(15) Uani 1 1 d . . . H4 H 0.1362 0.8053 0.8907 0.083 Uiso 1 1 calc R . . C9 C -0.0693(3) 0.9794(2) 0.8284(4) 0.0559(13) Uani 1 1 d . . . H9 H -0.0893 1.0193 0.8137 0.067 Uiso 1 1 calc R . . C7 C 0.0488(3) 0.9060(2) 0.8986(3) 0.0565(13) Uani 1 1 d . . . H7 H 0.1107 0.8953 0.9347 0.068 Uiso 1 1 calc R . . C12 C -0.2662(4) 1.0000(3) 0.7564(5) 0.0835(18) Uani 1 1 d . . . H12 H -0.2252 1.0295 0.7991 0.100 Uiso 1 1 calc R . . O4 O 0.7035(3) 0.73823(19) 0.6606(3) 0.1153(16) Uani 1 1 d . . . O1 O 0.7391(3) 0.6655(2) 0.7862(3) 0.1188(16) Uani 1 1 d . . . C2 C 0.0492(5) 0.6766(3) 0.8901(5) 0.0840(19) Uani 1 1 d . . . H2 H 0.0613 0.6353 0.8953 0.101 Uiso 1 1 calc R . . C16 C -0.2972(4) 0.9023(3) 0.6777(4) 0.0755(17) Uani 1 1 d . . . H16 H -0.2766 0.8653 0.6669 0.091 Uiso 1 1 calc R . . C1 C -0.0326(5) 0.6971(3) 0.8760(4) 0.0801(18) Uani 1 1 d . . . H1 H -0.0764 0.6691 0.8705 0.096 Uiso 1 1 calc R . . O3 O 0.5930(4) 0.6698(3) 0.6397(5) 0.179(3) Uani 1 1 d . . . C13 C -0.3601(5) 1.0106(3) 0.7073(6) 0.109(2) Uani 1 1 d . . . H13 H -0.3815 1.0476 0.7170 0.131 Uiso 1 1 calc R . . C3 C 0.1142(4) 0.7171(3) 0.8969(4) 0.0817(18) Uani 1 1 d . . . H3 H 0.1711 0.7039 0.9074 0.098 Uiso 1 1 calc R . . C15 C -0.3903(4) 0.9139(3) 0.6298(5) 0.103(2) Uani 1 1 d . . . H15 H -0.4320 0.8847 0.5869 0.123 Uiso 1 1 calc R . . C14 C -0.4217(5) 0.9680(4) 0.6450(6) 0.122(3) Uani 1 1 d . . . H14 H -0.4846 0.9756 0.6132 0.146 Uiso 1 1 calc R . . C17 C 0.0956(3) 1.0153(2) 0.9236(3) 0.0488(12) Uani 1 1 d . . . C22 C 0.0716(3) 1.0749(2) 0.9251(4) 0.0644(15) Uani 1 1 d . . . H22 H 0.0099 1.0847 0.8992 0.077 Uiso 1 1 calc R . . C18 C 0.1878(4) 1.0033(2) 0.9609(5) 0.0789(17) Uani 1 1 d . . . H18 H 0.2061 0.9638 0.9584 0.095 Uiso 1 1 calc R . . C20 C 0.2281(3) 1.1063(2) 1.0041(4) 0.0515(13) Uani 1 1 d . . . C19 C 0.2534(3) 1.0482(3) 1.0016(4) 0.0786(18) Uani 1 1 d . . . H19 H 0.3152 1.0388 1.0275 0.094 Uiso 1 1 calc R . . C21 C 0.1373(3) 1.1205(2) 0.9643(4) 0.0636(14) Uani 1 1 d . . . H21 H 0.1196 1.1605 0.9635 0.076 Uiso 1 1 calc R . . N1 N 0.2971(3) 1.15204(19) 1.0475(3) 0.0564(11) Uani 1 1 d . . . C23 C 0.3740(4) 1.1575(3) 1.0402(4) 0.0713(16) Uani 1 1 d . . . H23 H 0.3915 1.1319 1.0027 0.086 Uiso 1 1 calc R . . C24 C 0.4219(4) 1.2064(3) 1.0963(4) 0.0715(16) Uani 1 1 d . . . H24 H 0.4775 1.2212 1.1050 0.086 Uiso 1 1 calc R . . N2 N 0.2934(3) 1.19669(19) 1.1085(3) 0.0603(11) Uani 1 1 d . . . C25 C 0.3695(4) 1.2294(2) 1.1376(4) 0.0678(15) Uani 1 1 d . . . H25 H 0.3853 1.2634 1.1803 0.081 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 Ag1 0.0771(4) 0.0765(3) 0.1096(4) -0.0205(3) 0.0612(3) -0.0215(3) Cl1 0.0808(12) 0.0822(12) 0.0732(12) -0.0166(9) 0.0314(10) -0.0252(9) N3 0.042(3) 0.061(3) 0.047(2) -0.004(2) 0.017(2) -0.010(2) C10 0.050(3) 0.054(3) 0.052(3) -0.006(3) 0.024(3) -0.006(3) C6 0.050(3) 0.056(3) 0.046(3) 0.001(3) 0.024(3) -0.005(3) C8 0.046(3) 0.059(3) 0.042(3) -0.004(2) 0.019(3) -0.011(3) C11 0.042(3) 0.061(4) 0.062(3) 0.004(3) 0.020(3) -0.004(3) O2 0.149(4) 0.076(3) 0.098(3) -0.018(2) 0.060(3) -0.009(3) N4 0.070(3) 0.061(3) 0.069(3) 0.003(2) 0.043(3) -0.003(3) C5 0.059(4) 0.067(4) 0.052(3) 0.001(3) 0.031(3) -0.003(3) C4 0.070(4) 0.072(4) 0.062(4) 0.003(3) 0.030(3) 0.002(3) C9 0.045(3) 0.062(4) 0.052(3) 0.000(3) 0.017(3) -0.006(3) C7 0.043(3) 0.066(4) 0.050(3) 0.009(3) 0.015(3) 0.001(3) C12 0.047(4) 0.084(5) 0.102(5) -0.009(4) 0.024(3) -0.002(3) O4 0.166(5) 0.067(3) 0.097(3) -0.009(2) 0.052(3) -0.021(3) O1 0.152(4) 0.118(4) 0.066(3) 0.003(3) 0.037(3) -0.008(3) C2 0.117(6) 0.059(4) 0.093(5) 0.010(3) 0.065(5) 0.019(4) C16 0.051(4) 0.076(4) 0.085(4) -0.008(3) 0.023(3) -0.012(3) C1 0.106(5) 0.065(5) 0.090(5) 0.004(3) 0.064(4) -0.001(4) O3 0.091(4) 0.260(7) 0.177(6) -0.055(5) 0.058(4) -0.078(4) C13 0.067(5) 0.093(5) 0.151(7) -0.005(5) 0.040(5) 0.017(4) C3 0.078(4) 0.085(5) 0.082(4) 0.007(4) 0.039(4) 0.021(4) C15 0.048(4) 0.115(6) 0.119(6) -0.027(5) 0.021(4) -0.014(4) C14 0.045(4) 0.133(7) 0.154(8) -0.012(6) 0.022(5) 0.003(5) C17 0.044(3) 0.060(3) 0.039(3) -0.001(2) 0.018(2) -0.007(3) C22 0.036(3) 0.060(4) 0.077(4) 0.008(3) 0.012(3) -0.001(3) C18 0.049(4) 0.064(4) 0.117(5) -0.017(3) 0.036(4) -0.004(3) C20 0.045(3) 0.061(4) 0.046(3) -0.008(3) 0.021(3) -0.013(3) C19 0.036(3) 0.076(4) 0.109(5) -0.025(4) 0.024(3) -0.008(3) C21 0.046(3) 0.056(3) 0.076(4) 0.003(3) 0.020(3) -0.002(3) N1 0.043(3) 0.074(3) 0.054(3) -0.003(2) 0.025(2) -0.013(2) C23 0.057(4) 0.092(4) 0.082(4) -0.013(3) 0.047(3) -0.016(3) C24 0.050(3) 0.086(4) 0.076(4) -0.009(3) 0.030(3) -0.026(3) N2 0.055(3) 0.065(3) 0.063(3) -0.005(2) 0.031(2) -0.014(2) C25 0.059(4) 0.072(4) 0.067(4) -0.010(3) 0.026(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.178(4) 5_577 ? Ag1 N4 2.249(4) . ? Ag1 N3 2.453(4) . ? Cl1 O3 1.395(5) . ? Cl1 O4 1.414(4) . ? Cl1 O1 1.415(4) . ? Cl1 O2 1.426(4) . ? N3 C6 1.340(5) . ? N3 C10 1.343(6) . ? C10 C9 1.382(6) . ? C10 C11 1.489(6) . ? C6 C7 1.378(6) . ? C6 C5 1.489(6) . ? C8 C7 1.384(6) . ? C8 C9 1.393(6) . ? C8 C17 1.488(6) . ? C11 C12 1.385(7) . ? C11 C16 1.388(6) . ? N4 C5 1.335(6) . ? N4 C1 1.351(6) . ? C5 C4 1.387(7) . ? C4 C3 1.357(7) . ? C4 H4 0.9300 . ? C9 H9 0.9300 . ? C7 H7 0.9300 . ? C12 C13 1.383(8) . ? C12 H12 0.9300 . ? C2 C1 1.352(8) . ? C2 C3 1.371(8) . ? C2 H2 0.9300 . ? C16 C15 1.377(7) . ? C16 H16 0.9300 . ? C1 H1 0.9300 . ? C13 C14 1.364(9) . ? C13 H13 0.9300 . ? C3 H3 0.9300 . ? C15 C14 1.366(9) . ? C15 H15 0.9300 . ? C14 H14 0.9300 . ? C17 C22 1.380(6) . ? C17 C18 1.379(6) . ? C22 C21 1.389(6) . ? C22 H22 0.9300 . ? C18 C19 1.378(7) . ? C18 H18 0.9300 . ? C20 C19 1.356(6) . ? C20 C21 1.365(6) . ? C20 N1 1.424(6) . ? C19 H19 0.9300 . ? C21 H21 0.9300 . ? N1 C23 1.344(6) . ? N1 N2 1.355(5) . ? C23 C24 1.356(7) . ? C23 H23 0.9300 . ? C24 C25 1.383(7) . ? C24 H24 0.9300 . ? N2 C25 1.334(6) . ? N2 Ag1 2.178(4) 5_577 ? C25 H25 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N4 152.14(15) 5_577 . ? N2 Ag1 N3 125.99(15) 5_577 . ? N4 Ag1 N3 71.39(15) . . ? O3 Cl1 O4 108.7(4) . . ? O3 Cl1 O1 112.0(4) . . ? O4 Cl1 O1 108.4(3) . . ? O3 Cl1 O2 109.3(3) . . ? O4 Cl1 O2 108.3(3) . . ? O1 Cl1 O2 109.9(3) . . ? C6 N3 C10 118.4(4) . . ? C6 N3 Ag1 108.2(3) . . ? C10 N3 Ag1 125.7(3) . . ? N3 C10 C9 122.0(4) . . ? N3 C10 C11 116.5(4) . . ? C9 C10 C11 121.5(5) . . ? N3 C6 C7 121.8(5) . . ? N3 C6 C5 117.6(4) . . ? C7 C6 C5 120.6(5) . . ? C7 C8 C9 116.4(4) . . ? C7 C8 C17 121.4(5) . . ? C9 C8 C17 122.2(5) . . ? C12 C11 C16 118.5(5) . . ? C12 C11 C10 120.0(5) . . ? C16 C11 C10 121.5(5) . . ? C5 N4 C1 118.0(5) . . ? C5 N4 Ag1 118.3(4) . . ? C1 N4 Ag1 123.7(4) . . ? N4 C5 C4 121.1(5) . . ? N4 C5 C6 116.7(5) . . ? C4 C5 C6 122.1(5) . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C6 C7 C8 121.0(5) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C13 C12 C11 119.7(6) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C1 C2 C3 119.6(6) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C15 C16 C11 120.8(6) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? N4 C1 C2 122.7(6) . . ? N4 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C14 C13 C12 121.3(6) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C4 C3 C2 118.5(6) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C13 C14 C15 119.4(6) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C22 C17 C18 116.9(5) . . ? C22 C17 C8 121.0(5) . . ? C18 C17 C8 122.1(5) . . ? C17 C22 C21 121.6(5) . . ? C17 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C19 C18 C17 121.7(5) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 N1 119.3(5) . . ? C21 C20 N1 120.7(5) . . ? C20 C19 C18 120.1(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C20 C21 C22 119.6(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 N1 N2 110.1(4) . . ? C23 N1 C20 128.3(5) . . ? N2 N1 C20 121.6(4) . . ? N1 C23 C24 108.8(5) . . ? N1 C23 H23 125.6 . . ? C24 C23 H23 125.6 . . ? C23 C24 C25 104.5(5) . . ? C23 C24 H24 127.7 . . ? C25 C24 H24 127.7 . . ? C25 N2 N1 105.2(4) . . ? C25 N2 Ag1 128.3(4) . 5_577 ? N1 N2 Ag1 126.4(3) . 5_577 ? N2 C25 C24 111.5(5) . . ? N2 C25 H25 124.3 . . ? C24 C25 H25 124.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N3 C6 132.7(3) 5_577 . . . ? N4 Ag1 N3 C6 -22.5(3) . . . . ? N2 Ag1 N3 C10 -15.9(4) 5_577 . . . ? N4 Ag1 N3 C10 -171.2(4) . . . . ? C6 N3 C10 C9 1.1(7) . . . . ? Ag1 N3 C10 C9 146.9(4) . . . . ? C6 N3 C10 C11 -179.0(4) . . . . ? Ag1 N3 C10 C11 -33.3(6) . . . . ? C10 N3 C6 C7 1.2(7) . . . . ? Ag1 N3 C6 C7 -150.1(4) . . . . ? C10 N3 C6 C5 -178.1(4) . . . . ? Ag1 N3 C6 C5 30.6(5) . . . . ? N3 C10 C11 C12 155.5(5) . . . . ? C9 C10 C11 C12 -24.7(8) . . . . ? N3 C10 C11 C16 -23.0(7) . . . . ? C9 C10 C11 C16 156.9(5) . . . . ? N2 Ag1 N4 C5 -121.1(4) 5_577 . . . ? N3 Ag1 N4 C5 12.5(3) . . . . ? N2 Ag1 N4 C1 60.9(6) 5_577 . . . ? N3 Ag1 N4 C1 -165.5(4) . . . . ? C1 N4 C5 C4 -0.7(7) . . . . ? Ag1 N4 C5 C4 -178.8(4) . . . . ? C1 N4 C5 C6 176.7(4) . . . . ? Ag1 N4 C5 C6 -1.4(5) . . . . ? N3 C6 C5 N4 -22.1(6) . . . . ? C7 C6 C5 N4 158.5(4) . . . . ? N3 C6 C5 C4 155.3(5) . . . . ? C7 C6 C5 C4 -24.1(7) . . . . ? N4 C5 C4 C3 -0.8(8) . . . . ? C6 C5 C4 C3 -178.1(5) . . . . ? N3 C10 C9 C8 -2.9(7) . . . . ? C11 C10 C9 C8 177.3(4) . . . . ? C7 C8 C9 C10 2.2(7) . . . . ? C17 C8 C9 C10 -177.1(4) . . . . ? N3 C6 C7 C8 -1.9(7) . . . . ? C5 C6 C7 C8 177.5(4) . . . . ? C9 C8 C7 C6 0.1(7) . . . . ? C17 C8 C7 C6 179.4(4) . . . . ? C16 C11 C12 C13 -0.2(9) . . . . ? C10 C11 C12 C13 -178.7(5) . . . . ? C12 C11 C16 C15 0.0(9) . . . . ? C10 C11 C16 C15 178.5(5) . . . . ? C5 N4 C1 C2 1.5(8) . . . . ? Ag1 N4 C1 C2 179.5(4) . . . . ? C3 C2 C1 N4 -0.9(9) . . . . ? C11 C12 C13 C14 0.5(11) . . . . ? C5 C4 C3 C2 1.5(8) . . . . ? C1 C2 C3 C4 -0.7(9) . . . . ? C11 C16 C15 C14 -0.3(11) . . . . ? C12 C13 C14 C15 -0.7(13) . . . . ? C16 C15 C14 C13 0.6(12) . . . . ? C7 C8 C17 C22 -167.8(5) . . . . ? C9 C8 C17 C22 11.4(7) . . . . ? C7 C8 C17 C18 12.6(7) . . . . ? C9 C8 C17 C18 -168.2(5) . . . . ? C18 C17 C22 C21 -1.4(8) . . . . ? C8 C17 C22 C21 179.0(5) . . . . ? C22 C17 C18 C19 2.6(8) . . . . ? C8 C17 C18 C19 -177.8(5) . . . . ? C21 C20 C19 C18 -1.3(9) . . . . ? N1 C20 C19 C18 179.4(5) . . . . ? C17 C18 C19 C20 -1.3(9) . . . . ? C19 C20 C21 C22 2.5(8) . . . . ? N1 C20 C21 C22 -178.2(4) . . . . ? C17 C22 C21 C20 -1.1(8) . . . . ? C19 C20 N1 C23 37.6(8) . . . . ? C21 C20 N1 C23 -141.7(5) . . . . ? C19 C20 N1 N2 -139.6(5) . . . . ? C21 C20 N1 N2 41.1(7) . . . . ? N2 N1 C23 C24 -0.3(6) . . . . ? C20 N1 C23 C24 -177.8(5) . . . . ? N1 C23 C24 C25 0.3(6) . . . . ? C23 N1 N2 C25 0.2(5) . . . . ? C20 N1 N2 C25 177.9(4) . . . . ? C23 N1 N2 Ag1 -176.2(3) . . . 5_577 ? C20 N1 N2 Ag1 1.4(6) . . . 5_577 ? N1 N2 C25 C24 0.0(6) . . . . ? Ag1 N2 C25 C24 176.3(4) 5_577 . . . ? C23 C24 C25 N2 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.362 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.065 # Attachment '- Complex 3.cif' data_jf_3 _database_code_depnum_ccdc_archive 'CCDC 871212' #TrackingRef '- Complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C150 H108 Ag4 N28 O16' _chemical_formula_weight 2990.12 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' 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.745(5) _cell_length_b 13.971(5) _cell_length_c 21.091(5) _cell_angle_alpha 101.276(5) _cell_angle_beta 93.521(5) _cell_angle_gamma 114.371(5) _cell_volume 3312.1(19) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4263 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 20.91 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8263 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23791 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11581 _reflns_number_gt 6916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11581 _refine_ls_number_parameters 920 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.10635(4) 0.18982(4) 0.65896(2) 0.05873(18) Uani 1 1 d . . . Ag2 Ag 0.65508(5) 0.38587(4) 0.79218(3) 0.0754(2) Uani 1 1 d . . . C1 C -0.3075(5) 0.0639(6) 0.7327(3) 0.0658(18) Uani 1 1 d . . . H1 H -0.3546 0.0655 0.6978 0.079 Uiso 1 1 calc R . . C2 C -0.3594(5) -0.0007(6) 0.7738(3) 0.0670(19) Uani 1 1 d . . . H2 H -0.4396 -0.0431 0.7666 0.080 Uiso 1 1 calc R . . C3 C -0.2898(5) -0.0009(5) 0.8257(3) 0.0644(18) Uani 1 1 d . . . H3 H -0.3227 -0.0438 0.8543 0.077 Uiso 1 1 calc R . . C4 C -0.1723(5) 0.0617(5) 0.8356(3) 0.0552(15) Uani 1 1 d . . . H4 H -0.1247 0.0625 0.8711 0.066 Uiso 1 1 calc R . . C5 C -0.1241(4) 0.1248(4) 0.7914(3) 0.0424(13) Uani 1 1 d . . . C6 C 0.0051(4) 0.1937(4) 0.7996(2) 0.0394(12) Uani 1 1 d . . . C7 C 0.0811(4) 0.2011(4) 0.8511(3) 0.0421(13) Uani 1 1 d . . . H7 H 0.0527 0.1640 0.8831 0.051 Uiso 1 1 calc R . . C8 C 0.2015(5) 0.2641(4) 0.8561(2) 0.0411(12) Uani 1 1 d . . . C9 C 0.2384(5) 0.3161(5) 0.8065(3) 0.0465(14) Uani 1 1 d . . . H9 H 0.3176 0.3577 0.8075 0.056 Uiso 1 1 calc R . . C10 C 0.1582(4) 0.3065(4) 0.7555(2) 0.0414(13) Uani 1 1 d . . . C11 C 0.1975(5) 0.3622(4) 0.7021(3) 0.0462(14) Uani 1 1 d . . . C12 C 0.2938(5) 0.3609(5) 0.6744(3) 0.0551(15) Uani 1 1 d . . . H12 H 0.3333 0.3243 0.6891 0.066 Uiso 1 1 calc R . . C13 C 0.3308(6) 0.4134(6) 0.6253(3) 0.0693(19) Uani 1 1 d . . . H13 H 0.3942 0.4112 0.6066 0.083 Uiso 1 1 calc R . . C14 C 0.2742(7) 0.4688(6) 0.6041(4) 0.081(2) Uani 1 1 d . . . H14 H 0.3005 0.5053 0.5716 0.097 Uiso 1 1 calc R . . C15 C 0.1793(7) 0.4709(6) 0.6304(4) 0.079(2) Uani 1 1 d . . . H15 H 0.1409 0.5083 0.6155 0.094 Uiso 1 1 calc R . . C16 C 0.1407(6) 0.4176(5) 0.6788(3) 0.0590(16) Uani 1 1 d . . . H16 H 0.0758 0.4187 0.6962 0.071 Uiso 1 1 calc R . . C17 C 0.2854(4) 0.2731(4) 0.9122(3) 0.0431(13) Uani 1 1 d . . . C18 C 0.2556(5) 0.1940(5) 0.9479(3) 0.0495(14) Uani 1 1 d . . . H18 H 0.1823 0.1354 0.9370 0.059 Uiso 1 1 calc R . . C19 C 0.3330(5) 0.2013(5) 0.9992(3) 0.0508(15) Uani 1 1 d . . . H19 H 0.3112 0.1478 1.0224 0.061 Uiso 1 1 calc R . . C20 C 0.4417(4) 0.2865(4) 1.0164(3) 0.0439(13) Uani 1 1 d . . . C21 C 0.4730(5) 0.3671(5) 0.9820(3) 0.0506(14) Uani 1 1 d . . . H21 H 0.5459 0.4263 0.9940 0.061 Uiso 1 1 calc R . . C22 C 0.3960(5) 0.3592(5) 0.9303(3) 0.0503(15) Uani 1 1 d . . . H22 H 0.4185 0.4126 0.9069 0.060 Uiso 1 1 calc R . . C23 C 0.5291(6) 0.2118(6) 1.0893(3) 0.073(2) Uani 1 1 d . . . H23 H 0.4820 0.1384 1.0721 0.088 Uiso 1 1 calc R . . C24 C 0.6177(8) 0.2560(8) 1.1403(4) 0.093(3) Uani 1 1 d . . . H24 H 0.6430 0.2196 1.1656 0.111 Uiso 1 1 calc R . . C25 C 0.6620(6) 0.3653(8) 1.1468(4) 0.087(2) Uani 1 1 d . . . H25 H 0.7260 0.4158 1.1775 0.104 Uiso 1 1 calc R . . C26 C -0.1822(6) 0.2860(6) 0.5505(3) 0.0674(18) Uani 1 1 d . . . H26 H -0.2312 0.2947 0.5797 0.081 Uiso 1 1 calc R . . C27 C -0.1833(7) 0.3212(6) 0.4949(4) 0.082(2) Uani 1 1 d . . . H27 H -0.2311 0.3542 0.4863 0.098 Uiso 1 1 calc R . . C28 C -0.1107(8) 0.3063(7) 0.4511(4) 0.091(2) Uani 1 1 d . . . H28 H -0.1084 0.3302 0.4128 0.110 Uiso 1 1 calc R . . C29 C -0.0418(6) 0.2555(6) 0.4652(3) 0.075(2) Uani 1 1 d . . . H29 H 0.0053 0.2432 0.4358 0.090 Uiso 1 1 calc R . . C30 C -0.0437(5) 0.2238(5) 0.5226(3) 0.0483(14) Uani 1 1 d . . . C31 C 0.0314(5) 0.1718(4) 0.5413(3) 0.0449(13) Uani 1 1 d . . . C32 C 0.1285(5) 0.1817(5) 0.5114(3) 0.0523(15) Uani 1 1 d . . . H32 H 0.1483 0.2222 0.4802 0.063 Uiso 1 1 calc R . . C33 C 0.1966(5) 0.1306(5) 0.5285(3) 0.0471(14) Uani 1 1 d . . . C34 C 0.1660(5) 0.0763(5) 0.5771(3) 0.0480(14) Uani 1 1 d . . . H34 H 0.2106 0.0436 0.5908 0.058 Uiso 1 1 calc R . . C35 C 0.0686(5) 0.0699(4) 0.6058(3) 0.0427(13) Uani 1 1 d . . . C36 C 0.0320(5) 0.0096(5) 0.6578(3) 0.0486(14) Uani 1 1 d . . . C37 C 0.1135(6) 0.0136(6) 0.7056(3) 0.0636(17) Uani 1 1 d . . . H37 H 0.1925 0.0541 0.7054 0.076 Uiso 1 1 calc R . . C38 C 0.0783(8) -0.0427(7) 0.7543(3) 0.081(2) Uani 1 1 d . . . H38 H 0.1332 -0.0369 0.7877 0.098 Uiso 1 1 calc R . . C39 C -0.0380(8) -0.1066(6) 0.7522(4) 0.082(2) Uani 1 1 d . . . H39 H -0.0615 -0.1463 0.7836 0.099 Uiso 1 1 calc R . . C40 C -0.1195(7) -0.1126(6) 0.7047(3) 0.0718(19) Uani 1 1 d . . . H40 H -0.1982 -0.1560 0.7039 0.086 Uiso 1 1 calc R . . C41 C -0.0855(6) -0.0543(5) 0.6580(3) 0.0581(16) Uani 1 1 d . . . H41 H -0.1417 -0.0576 0.6262 0.070 Uiso 1 1 calc R . . C42 C 0.2972(5) 0.1378(5) 0.4949(3) 0.0499(14) Uani 1 1 d . . . C43 C 0.3272(5) 0.0529(5) 0.4804(3) 0.0545(15) Uani 1 1 d . . . H43 H 0.2886 -0.0083 0.4961 0.065 Uiso 1 1 calc R . . C44 C 0.4129(5) 0.0565(5) 0.4432(3) 0.0607(16) Uani 1 1 d . . . H44 H 0.4302 -0.0028 0.4332 0.073 Uiso 1 1 calc R . . C45 C 0.4733(5) 0.1464(5) 0.4208(3) 0.0561(16) Uani 1 1 d . . . C46 C 0.4472(6) 0.2336(5) 0.4356(4) 0.072(2) Uani 1 1 d . . . H46 H 0.4878 0.2952 0.4207 0.087 Uiso 1 1 calc R . . C47 C 0.3615(6) 0.2297(5) 0.4723(3) 0.0680(19) Uani 1 1 d . . . H47 H 0.3454 0.2895 0.4825 0.082 Uiso 1 1 calc R . . C48 C 0.6012(6) 0.0772(7) 0.3602(4) 0.083(2) Uani 1 1 d . . . H48 H 0.5829 0.0128 0.3729 0.099 Uiso 1 1 calc R . . C49 C 0.6753(6) 0.1163(8) 0.3184(4) 0.095(3) Uani 1 1 d . . . H49 H 0.7183 0.0838 0.2971 0.114 Uiso 1 1 calc R . . C50 C 0.6754(6) 0.2125(8) 0.3133(4) 0.089(2) Uani 1 1 d . . . H50 H 0.7187 0.2559 0.2873 0.107 Uiso 1 1 calc R . . C51 C 0.8937(6) 0.4637(6) 0.7415(3) 0.0629(17) Uani 1 1 d . . . H51 H 0.8376 0.3923 0.7272 0.076 Uiso 1 1 calc R . . C52 C 0.9149(7) 0.5319(7) 0.6994(4) 0.080(2) Uani 1 1 d . . . H52 H 0.8730 0.5062 0.6571 0.096 Uiso 1 1 calc R . . C53 C 0.9995(7) 0.6399(7) 0.7205(4) 0.082(2) Uani 1 1 d . . . H53 H 1.0134 0.6865 0.6927 0.098 Uiso 1 1 calc R . . C54 C 1.0618(6) 0.6757(6) 0.7830(4) 0.0716(19) Uani 1 1 d . . . H54 H 1.1184 0.7469 0.7973 0.086 Uiso 1 1 calc R . . C55 C 1.0409(5) 0.6069(5) 0.8243(3) 0.0595(16) Uani 1 1 d . . . H55 H 1.0850 0.6323 0.8659 0.071 Uiso 1 1 calc R . . C56 C 0.9558(5) 0.5008(5) 0.8056(3) 0.0492(14) Uani 1 1 d . A . C57 C 0.9264(5) 0.4301(5) 0.8513(3) 0.0475(14) Uani 1 1 d . . . C58 C 0.7790(5) 0.3007(4) 0.8899(3) 0.0483(14) Uani 1 1 d . . . C59 C 0.6516(5) 0.2290(5) 0.8825(3) 0.0526(15) Uani 1 1 d . A . C60 C 0.6092(5) 0.1548(5) 0.9195(3) 0.0663(18) Uani 1 1 d . . . H60 H 0.6591 0.1527 0.9527 0.080 Uiso 1 1 calc R A . C61 C 0.4928(6) 0.0835(6) 0.9074(4) 0.076(2) Uani 1 1 d . A . H61 H 0.4639 0.0317 0.9315 0.092 Uiso 1 1 calc R . . C62 C 0.4195(6) 0.0897(6) 0.8592(4) 0.080(2) Uani 1 1 d . . . H62 H 0.3405 0.0426 0.8498 0.096 Uiso 1 1 calc R A . C63 C 0.4681(6) 0.1685(6) 0.8252(4) 0.077(2) Uani 1 1 d . A . H63 H 0.4194 0.1729 0.7923 0.092 Uiso 1 1 calc R . . C64 C 1.0106(5) 0.4325(4) 0.8977(3) 0.0484(14) Uani 1 1 d . A . H64 H 1.0889 0.4777 0.8990 0.058 Uiso 1 1 calc R . . C65 C 0.8590(5) 0.3024(5) 0.9380(3) 0.0510(14) Uani 1 1 d . A . H65 H 0.8335 0.2598 0.9677 0.061 Uiso 1 1 calc R . . C66 C 0.9787(5) 0.3682(4) 0.9421(3) 0.0454(13) Uani 1 1 d . . . C67 C 1.0640(5) 0.3670(4) 0.9937(3) 0.0430(13) Uani 1 1 d . A . C68 C 1.1765(5) 0.4509(4) 1.0137(3) 0.0467(14) Uani 1 1 d . . . H68 H 1.2018 0.5077 0.9931 0.056 Uiso 1 1 calc R A . C69 C 1.0333(5) 0.2805(5) 1.0224(3) 0.0567(16) Uani 1 1 d . . . H69 H 0.9611 0.2213 1.0071 0.068 Uiso 1 1 calc R A . C70 C 1.2501(5) 0.4499(4) 1.0641(3) 0.0488(14) Uani 1 1 d . A . H70 H 1.3243 0.5067 1.0771 0.059 Uiso 1 1 calc R . . C71 C 1.1063(5) 0.2791(5) 1.0730(3) 0.0573(16) Uani 1 1 d . A . H71 H 1.0823 0.2203 1.0919 0.069 Uiso 1 1 calc R . . C72 C 1.2159(5) 0.3658(4) 1.0957(3) 0.0456(13) Uani 1 1 d . . . C73 C 1.3000(6) 0.2806(6) 1.1638(3) 0.0649(18) Uani 1 1 d . . . H73 H 1.2590 0.2087 1.1406 0.078 Uiso 1 1 calc R A . C74 C 1.3798(6) 0.3169(7) 1.2186(4) 0.078(2) Uani 1 1 d . A . H74 H 1.4045 0.2771 1.2412 0.093 Uiso 1 1 calc R . . C75 C 1.4158(6) 0.4279(6) 1.2331(4) 0.076(2) Uani 1 1 d . . . H75 H 1.4729 0.4759 1.2682 0.092 Uiso 1 1 calc R A . N1 N 0.0009(4) 0.1165(4) 0.5874(2) 0.0421(11) Uani 1 1 d . . . N2 N -0.1125(4) 0.2384(4) 0.5653(2) 0.0506(12) Uani 1 1 d . . . N3 N 0.5591(4) 0.1507(5) 0.3798(3) 0.0631(14) Uani 1 1 d . . . N4 N 0.6040(5) 0.2352(5) 0.3513(3) 0.0815(18) Uani 1 1 d . . . N5 N 0.0428(4) 0.2471(3) 0.7521(2) 0.0417(10) Uani 1 1 d . . . N6 N -0.1915(4) 0.1249(4) 0.7404(2) 0.0507(12) Uani 1 1 d . . . N7 N 0.5219(4) 0.2931(4) 1.0682(2) 0.0520(12) Uani 1 1 d . . . N8 N 0.6037(5) 0.3912(5) 1.1046(3) 0.0767(17) Uani 1 1 d . . . N9 N 0.5803(4) 0.2386(4) 0.8367(3) 0.0602(14) Uani 1 1 d . A . N10 N 0.8118(4) 0.3651(4) 0.8474(2) 0.0486(11) Uani 1 1 d . A . N11 N 1.2896(4) 0.3656(4) 1.1483(2) 0.0501(12) Uani 1 1 d . A . N12 N 1.3611(4) 0.4584(4) 1.1923(3) 0.0614(14) Uani 1 1 d . . . N13 N 0.5351(7) 0.2355(7) 0.6535(4) 0.0896(18) Uani 1 1 d U . . N14 N 0.8017(8) 0.0774(6) 0.0498(7) 0.108(3) Uani 1 1 d . . . O1 O 0.6177(18) 0.3319(12) 0.6676(8) 0.104(4) Uani 0.49(2) 1 d PU A 1 O2 O 0.5429(17) 0.1806(14) 0.6015(9) 0.123(5) Uani 0.49(2) 1 d PU A 1 O3 O 0.460(2) 0.214(2) 0.6866(11) 0.136(6) Uani 0.49(2) 1 d PU A 1 O1' O 0.5594(16) 0.3334(12) 0.6750(7) 0.094(3) Uani 0.51(2) 1 d PU A 2 O2' O 0.5917(18) 0.1925(16) 0.6320(11) 0.128(5) Uani 0.51(2) 1 d PU A 2 O3' O 0.4316(15) 0.1694(15) 0.6606(10) 0.114(5) Uani 0.51(2) 1 d PU A 2 O4 O 0.7884(15) 0.0468(6) -0.0015(4) 0.308(13) Uani 1 1 d . . . O5 O 0.8618(9) 0.0714(6) 0.0884(4) 0.169(5) Uani 1 1 d . . . O6 O 0.7471(12) 0.1173(12) 0.0723(12) 0.378(14) Uani 1 1 d . . . O7 O 0.6666(8) 0.4902(15) 0.5790(5) 0.319(10) Uani 1 1 d . . . O8 O 0.9420(9) 0.9805(9) 0.9407(6) 0.217(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 Ag1 0.0625(3) 0.0799(4) 0.0429(3) 0.0207(2) 0.0115(2) 0.0366(3) Ag2 0.0798(4) 0.0650(4) 0.0737(4) 0.0065(3) -0.0134(3) 0.0320(3) C1 0.052(4) 0.086(5) 0.049(4) 0.010(4) 0.008(3) 0.022(4) C2 0.044(3) 0.082(5) 0.061(4) 0.009(4) 0.012(3) 0.018(3) C3 0.051(4) 0.063(4) 0.082(5) 0.026(4) 0.023(3) 0.021(3) C4 0.049(3) 0.061(4) 0.055(4) 0.017(3) 0.008(3) 0.022(3) C5 0.041(3) 0.045(3) 0.038(3) 0.006(3) 0.007(2) 0.017(3) C6 0.047(3) 0.038(3) 0.034(3) 0.007(2) 0.007(2) 0.020(3) C7 0.045(3) 0.041(3) 0.040(3) 0.014(2) 0.011(2) 0.016(3) C8 0.049(3) 0.038(3) 0.038(3) 0.008(2) 0.005(2) 0.021(3) C9 0.042(3) 0.049(3) 0.044(3) 0.011(3) 0.007(3) 0.015(3) C10 0.045(3) 0.040(3) 0.036(3) 0.009(2) 0.007(2) 0.017(3) C11 0.045(3) 0.043(3) 0.041(3) 0.012(3) 0.004(2) 0.010(3) C12 0.047(3) 0.061(4) 0.049(4) 0.013(3) 0.002(3) 0.016(3) C13 0.066(4) 0.068(5) 0.054(4) 0.019(4) 0.013(3) 0.008(4) C14 0.089(6) 0.074(5) 0.058(5) 0.029(4) 0.017(4) 0.008(4) C15 0.109(6) 0.064(5) 0.068(5) 0.031(4) 0.003(4) 0.037(4) C16 0.074(4) 0.049(4) 0.059(4) 0.022(3) 0.013(3) 0.028(3) C17 0.044(3) 0.043(3) 0.042(3) 0.012(3) 0.005(2) 0.017(3) C18 0.044(3) 0.048(3) 0.053(4) 0.015(3) 0.004(3) 0.014(3) C19 0.055(4) 0.043(3) 0.053(4) 0.022(3) 0.003(3) 0.016(3) C20 0.041(3) 0.050(3) 0.042(3) 0.013(3) 0.002(2) 0.020(3) C21 0.044(3) 0.049(4) 0.049(4) 0.015(3) 0.002(3) 0.012(3) C22 0.052(3) 0.051(4) 0.045(3) 0.021(3) 0.006(3) 0.015(3) C23 0.086(5) 0.069(5) 0.073(5) 0.027(4) -0.007(4) 0.041(4) C24 0.108(6) 0.104(7) 0.089(6) 0.032(5) -0.018(5) 0.068(6) C25 0.067(5) 0.113(7) 0.078(5) 0.028(5) -0.017(4) 0.038(5) C26 0.071(4) 0.081(5) 0.061(4) 0.017(4) 0.007(3) 0.044(4) C27 0.103(6) 0.107(6) 0.075(5) 0.038(5) 0.009(4) 0.078(5) C28 0.119(7) 0.124(7) 0.068(5) 0.044(5) 0.019(5) 0.078(6) C29 0.090(5) 0.108(6) 0.058(4) 0.039(4) 0.022(4) 0.063(5) C30 0.054(3) 0.052(4) 0.042(3) 0.014(3) 0.002(3) 0.026(3) C31 0.051(3) 0.041(3) 0.036(3) 0.003(3) 0.000(3) 0.018(3) C32 0.056(4) 0.049(4) 0.049(4) 0.012(3) 0.010(3) 0.020(3) C33 0.050(3) 0.045(3) 0.043(3) 0.004(3) 0.007(3) 0.020(3) C34 0.049(3) 0.049(3) 0.048(3) 0.008(3) 0.003(3) 0.026(3) C35 0.050(3) 0.039(3) 0.037(3) 0.001(2) 0.002(2) 0.021(3) C36 0.063(4) 0.051(4) 0.043(3) 0.015(3) 0.011(3) 0.034(3) C37 0.076(4) 0.088(5) 0.052(4) 0.030(4) 0.015(3) 0.054(4) C38 0.110(6) 0.114(7) 0.060(5) 0.039(5) 0.016(4) 0.080(6) C39 0.111(7) 0.088(6) 0.084(6) 0.054(5) 0.047(5) 0.060(5) C40 0.081(5) 0.073(5) 0.067(5) 0.028(4) 0.028(4) 0.033(4) C41 0.067(4) 0.063(4) 0.051(4) 0.021(3) 0.017(3) 0.031(3) C42 0.052(3) 0.053(4) 0.047(3) 0.011(3) 0.009(3) 0.025(3) C43 0.061(4) 0.051(4) 0.054(4) 0.012(3) 0.016(3) 0.026(3) C44 0.069(4) 0.059(4) 0.061(4) 0.011(3) 0.010(3) 0.037(4) C45 0.047(3) 0.058(4) 0.061(4) 0.008(3) 0.013(3) 0.022(3) C46 0.062(4) 0.053(4) 0.101(6) 0.017(4) 0.035(4) 0.020(3) C47 0.074(4) 0.053(4) 0.082(5) 0.013(4) 0.033(4) 0.031(4) C48 0.057(4) 0.092(6) 0.089(6) -0.003(4) 0.012(4) 0.034(4) C49 0.061(5) 0.129(8) 0.091(6) 0.013(6) 0.031(4) 0.040(5) C50 0.071(5) 0.108(7) 0.090(6) 0.028(5) 0.034(4) 0.034(5) C51 0.064(4) 0.072(5) 0.054(4) 0.008(3) 0.005(3) 0.035(4) C52 0.095(6) 0.101(7) 0.065(5) 0.032(5) 0.018(4) 0.059(5) C53 0.106(6) 0.099(6) 0.081(6) 0.053(5) 0.037(5) 0.066(6) C54 0.077(5) 0.072(5) 0.081(5) 0.036(4) 0.029(4) 0.037(4) C55 0.061(4) 0.068(5) 0.056(4) 0.017(3) 0.013(3) 0.033(4) C56 0.049(3) 0.056(4) 0.053(4) 0.013(3) 0.015(3) 0.031(3) C57 0.049(3) 0.054(4) 0.045(3) 0.007(3) 0.012(3) 0.029(3) C58 0.045(3) 0.042(3) 0.052(4) 0.003(3) 0.006(3) 0.017(3) C59 0.048(3) 0.044(4) 0.059(4) 0.001(3) 0.010(3) 0.018(3) C60 0.050(4) 0.066(4) 0.073(5) 0.011(4) 0.010(3) 0.018(3) C61 0.056(4) 0.068(5) 0.097(6) 0.014(4) 0.025(4) 0.020(4) C62 0.043(4) 0.072(5) 0.100(6) 0.003(4) 0.017(4) 0.008(4) C63 0.054(4) 0.071(5) 0.093(6) 0.010(4) 0.003(4) 0.021(4) C64 0.046(3) 0.042(3) 0.055(4) 0.011(3) 0.013(3) 0.017(3) C65 0.053(4) 0.044(3) 0.053(4) 0.009(3) 0.009(3) 0.020(3) C66 0.045(3) 0.043(3) 0.048(3) 0.006(3) 0.009(3) 0.021(3) C67 0.044(3) 0.038(3) 0.044(3) 0.008(3) 0.009(2) 0.015(3) C68 0.053(3) 0.040(3) 0.048(3) 0.013(3) 0.012(3) 0.020(3) C69 0.048(3) 0.044(4) 0.064(4) 0.016(3) 0.003(3) 0.006(3) C70 0.040(3) 0.041(3) 0.049(3) 0.010(3) 0.007(3) 0.003(3) C71 0.063(4) 0.040(3) 0.063(4) 0.022(3) 0.004(3) 0.013(3) C72 0.049(3) 0.043(3) 0.046(3) 0.006(3) 0.013(3) 0.022(3) C73 0.089(5) 0.062(4) 0.057(4) 0.026(3) 0.018(4) 0.040(4) C74 0.084(5) 0.077(5) 0.078(5) 0.036(4) 0.006(4) 0.035(4) C75 0.059(4) 0.083(6) 0.070(5) 0.019(4) -0.012(4) 0.017(4) N1 0.049(3) 0.047(3) 0.033(2) 0.009(2) 0.004(2) 0.024(2) N2 0.053(3) 0.055(3) 0.050(3) 0.018(2) 0.005(2) 0.028(3) N3 0.052(3) 0.069(4) 0.069(4) 0.013(3) 0.019(3) 0.028(3) N4 0.073(4) 0.087(5) 0.082(4) 0.024(4) 0.033(3) 0.028(3) N5 0.046(3) 0.043(3) 0.036(2) 0.009(2) 0.006(2) 0.020(2) N6 0.040(3) 0.063(3) 0.045(3) 0.011(2) 0.007(2) 0.020(2) N7 0.047(3) 0.055(3) 0.052(3) 0.018(3) 0.000(2) 0.020(3) N8 0.066(4) 0.070(4) 0.075(4) 0.019(3) -0.016(3) 0.015(3) N9 0.047(3) 0.051(3) 0.072(4) 0.007(3) -0.002(3) 0.016(3) N10 0.053(3) 0.047(3) 0.047(3) 0.005(2) 0.009(2) 0.025(2) N11 0.051(3) 0.048(3) 0.047(3) 0.013(2) 0.006(2) 0.018(2) N12 0.052(3) 0.057(3) 0.067(4) 0.015(3) -0.006(3) 0.017(3) N13 0.097(4) 0.091(4) 0.081(4) 0.000(4) 0.009(4) 0.051(4) N14 0.077(6) 0.056(5) 0.192(11) 0.048(7) 0.064(6) 0.015(4) O1 0.109(6) 0.090(5) 0.092(5) 0.007(5) 0.012(6) 0.031(5) O2 0.127(8) 0.125(7) 0.103(8) -0.009(6) 0.009(7) 0.058(6) O3 0.126(8) 0.141(9) 0.128(9) 0.016(7) 0.022(7) 0.052(7) O1' 0.098(6) 0.085(5) 0.092(5) -0.002(4) 0.012(5) 0.045(5) O2' 0.126(8) 0.132(7) 0.137(9) 0.026(7) 0.029(7) 0.068(6) O3' 0.105(7) 0.111(8) 0.121(8) 0.022(6) 0.008(6) 0.047(6) O4 0.57(3) 0.057(5) 0.088(6) 0.021(4) -0.043(9) -0.058(9) O5 0.187(9) 0.083(5) 0.161(7) 0.061(5) -0.061(7) -0.016(5) O6 0.166(11) 0.216(14) 0.77(4) 0.122(19) 0.212(19) 0.085(11) O7 0.142(8) 0.64(3) 0.193(10) 0.249(15) 0.054(7) 0.123(12) O8 0.225(11) 0.231(11) 0.226(11) 0.094(9) 0.052(9) 0.108(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.217(5) . ? Ag1 N6 2.231(4) . ? Ag1 N5 2.404(4) . ? Ag1 N1 2.450(4) . ? Ag2 N12 2.232(5) 2_767 ? Ag2 N9 2.297(5) . ? Ag2 N10 2.399(5) . ? Ag2 O1' 2.514(15) . ? Ag2 O1 2.545(16) . ? C1 N6 1.347(7) . ? C1 C2 1.375(9) . ? C1 H1 0.9300 . ? C2 C3 1.366(9) . ? C2 H2 0.9300 . ? C3 C4 1.365(8) . ? C3 H3 0.9300 . ? C4 C5 1.401(8) . ? C4 H4 0.9300 . ? C5 N6 1.335(7) . ? C5 C6 1.504(7) . ? C6 N5 1.360(6) . ? C6 C7 1.368(7) . ? C7 C8 1.404(7) . ? C7 H7 0.9300 . ? C8 C9 1.383(7) . ? C8 C17 1.494(7) . ? C9 C10 1.384(7) . ? C9 H9 0.9300 . ? C10 N5 1.347(6) . ? C10 C11 1.489(7) . ? C11 C16 1.390(8) . ? C11 C12 1.397(8) . ? C12 C13 1.379(8) . ? C12 H12 0.9300 . ? C13 C14 1.370(10) . ? C13 H13 0.9300 . ? C14 C15 1.370(11) . ? C14 H14 0.9300 . ? C15 C16 1.378(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.391(7) . ? C17 C18 1.397(7) . ? C18 C19 1.376(7) . ? C18 H18 0.9300 . ? C19 C20 1.370(7) . ? C19 H19 0.9300 . ? C20 C21 1.392(7) . ? C20 N7 1.411(7) . ? C21 C22 1.378(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N7 1.333(8) . ? C23 C24 1.352(10) . ? C23 H23 0.9300 . ? C24 C25 1.366(11) . ? C24 H24 0.9300 . ? C25 N8 1.320(8) . ? C25 H25 0.9300 . ? C26 C27 1.359(9) . ? C26 N2 1.366(7) . ? C26 H26 0.9300 . ? C27 C28 1.393(10) . ? C27 H27 0.9300 . ? C28 C29 1.389(10) . ? C28 H28 0.9300 . ? C29 C30 1.367(8) . ? C29 H29 0.9300 . ? C30 N2 1.339(7) . ? C30 C31 1.496(8) . ? C31 N1 1.337(7) . ? C31 C32 1.392(8) . ? C32 C33 1.402(8) . ? C32 H32 0.9300 . ? C33 C34 1.373(7) . ? C33 C42 1.480(8) . ? C34 C35 1.392(7) . ? C34 H34 0.9300 . ? C35 N1 1.356(6) . ? C35 C36 1.493(7) . ? C36 C37 1.378(8) . ? C36 C41 1.392(8) . ? C37 C38 1.399(9) . ? C37 H37 0.9300 . ? C38 C39 1.371(10) . ? C38 H38 0.9300 . ? C39 C40 1.364(10) . ? C39 H39 0.9300 . ? C40 C41 1.377(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.377(8) . ? C42 C47 1.402(8) . ? C43 C44 1.372(8) . ? C43 H43 0.9300 . ? C44 C45 1.369(8) . ? C44 H44 0.9300 . ? C45 C46 1.375(9) . ? C45 N3 1.425(7) . ? C46 C47 1.365(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 N3 1.351(9) . ? C48 C49 1.355(10) . ? C48 H48 0.9300 . ? C49 C50 1.369(11) . ? C49 H49 0.9300 . ? C50 N4 1.341(9) . ? C50 H50 0.9300 . ? C51 C52 1.385(9) . ? C51 C56 1.405(8) . ? C51 H51 0.9300 . ? C52 C53 1.405(11) . ? C52 H52 0.9300 . ? C53 C54 1.380(10) . ? C53 H53 0.9300 . ? C54 C55 1.379(9) . ? C54 H54 0.9300 . ? C55 C56 1.386(8) . ? C55 H55 0.9300 . ? C56 C57 1.469(8) . ? C57 N10 1.352(7) . ? C57 C64 1.393(8) . ? C58 N10 1.355(7) . ? C58 C65 1.384(8) . ? C58 C59 1.494(8) . ? C59 N9 1.347(8) . ? C59 C60 1.372(9) . ? C60 C61 1.376(9) . ? C60 H60 0.9300 . ? C61 C62 1.377(10) . ? C61 H61 0.9300 . ? C62 C63 1.382(10) . ? C62 H62 0.9300 . ? C63 N9 1.331(8) . ? C63 H63 0.9300 . ? C64 C66 1.387(7) . ? C64 H64 0.9300 . ? C65 C66 1.405(7) . ? C65 H65 0.9300 . ? C66 C67 1.498(8) . ? C67 C69 1.380(8) . ? C67 C68 1.397(7) . ? C68 C70 1.379(8) . ? C68 H68 0.9300 . ? C69 C71 1.381(8) . ? C69 H69 0.9300 . ? C70 C72 1.391(7) . ? C70 H70 0.9300 . ? C71 C72 1.394(8) . ? C71 H71 0.9300 . ? C72 N11 1.412(7) . ? C73 N11 1.345(7) . ? C73 C74 1.353(9) . ? C73 H73 0.9300 . ? C74 C75 1.385(10) . ? C74 H74 0.9300 . ? C75 N12 1.313(8) . ? C75 H75 0.9300 . ? N3 N4 1.359(8) . ? N7 N8 1.366(7) . ? N11 N12 1.350(7) . ? N12 Ag2 2.232(5) 2_767 ? N13 O2' 1.173(18) . ? N13 O3 1.20(2) . ? N13 O2 1.244(17) . ? N13 O1' 1.250(15) . ? N13 O1 1.282(16) . ? N13 O3' 1.300(18) . ? N14 O4 1.058(12) . ? N14 O5 1.121(11) . ? N14 O6 1.131(14) . ? 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 Ag1 N6 151.59(17) . . ? N2 Ag1 N5 133.98(16) . . ? N6 Ag1 N5 71.90(15) . . ? N2 Ag1 N1 71.49(16) . . ? N6 Ag1 N1 126.65(16) . . ? N5 Ag1 N1 91.86(14) . . ? N12 Ag2 N9 133.50(19) 2_767 . ? N12 Ag2 N10 123.83(17) 2_767 . ? N9 Ag2 N10 70.43(17) . . ? N12 Ag2 O1' 90.3(4) 2_767 . ? N9 Ag2 O1' 109.3(4) . . ? N10 Ag2 O1' 134.5(4) . . ? N12 Ag2 O1 99.1(5) 2_767 . ? N9 Ag2 O1 112.2(4) . . ? N10 Ag2 O1 117.8(5) . . ? O1' Ag2 O1 17.6(4) . . ? N6 C1 C2 123.1(6) . . ? N6 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.1(6) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C4 C3 C2 120.2(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N6 C5 C4 121.1(5) . . ? N6 C5 C6 117.8(5) . . ? C4 C5 C6 121.1(5) . . ? N5 C6 C7 121.7(5) . . ? N5 C6 C5 116.0(4) . . ? C7 C6 C5 122.2(5) . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 117.0(5) . . ? C9 C8 C17 122.0(5) . . ? C7 C8 C17 121.0(5) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N5 C10 C9 121.9(5) . . ? N5 C10 C11 117.5(5) . . ? C9 C10 C11 120.6(5) . . ? C16 C11 C12 118.1(5) . . ? C16 C11 C10 121.3(5) . . ? C12 C11 C10 120.5(5) . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.5(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.9(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.9(6) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C22 C17 C18 117.4(5) . . ? C22 C17 C8 121.7(5) . . ? C18 C17 C8 120.9(5) . . ? C19 C18 C17 121.1(5) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.3(5) . . ? C19 C20 N7 120.8(5) . . ? C21 C20 N7 119.9(5) . . ? C22 C21 C20 120.0(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 121.4(5) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? N7 C23 C24 107.3(7) . . ? N7 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? C23 C24 C25 105.3(7) . . ? C23 C24 H24 127.4 . . ? C25 C24 H24 127.4 . . ? N8 C25 C24 112.4(7) . . ? N8 C25 H25 123.8 . . ? C24 C25 H25 123.8 . . ? C27 C26 N2 123.0(6) . . ? C27 C26 H26 118.5 . . ? N2 C26 H26 118.5 . . ? C26 C27 C28 117.8(7) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C29 C28 C27 119.4(7) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 119.6(7) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N2 C30 C29 121.6(6) . . ? N2 C30 C31 116.6(5) . . ? C29 C30 C31 121.8(5) . . ? N1 C31 C32 122.3(5) . . ? N1 C31 C30 117.1(5) . . ? C32 C31 C30 120.6(5) . . ? C31 C32 C33 119.8(5) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 117.2(5) . . ? C34 C33 C42 123.0(5) . . ? C32 C33 C42 119.7(5) . . ? C33 C34 C35 120.5(5) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? N1 C35 C34 121.8(5) . . ? N1 C35 C36 116.5(5) . . ? C34 C35 C36 121.7(5) . . ? C37 C36 C41 118.6(6) . . ? C37 C36 C35 120.9(5) . . ? C41 C36 C35 120.5(5) . . ? C36 C37 C38 120.5(7) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 119.4(7) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C40 C39 C38 120.7(7) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.1(7) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C36 120.7(6) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C43 C42 C47 116.8(5) . . ? C43 C42 C33 122.1(5) . . ? C47 C42 C33 120.9(5) . . ? C44 C43 C42 121.5(6) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C45 C44 C43 120.6(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 119.4(6) . . ? C44 C45 N3 121.9(6) . . ? C46 C45 N3 118.7(6) . . ? C47 C46 C45 119.8(6) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C42 121.8(6) . . ? C46 C47 H47 119.1 . . ? C42 C47 H47 119.1 . . ? N3 C48 C49 106.2(8) . . ? N3 C48 H48 126.9 . . ? C49 C48 H48 126.9 . . ? C48 C49 C50 107.4(8) . . ? C48 C49 H49 126.3 . . ? C50 C49 H49 126.3 . . ? N4 C50 C49 110.2(7) . . ? N4 C50 H50 124.9 . . ? C49 C50 H50 124.9 . . ? C52 C51 C56 121.0(7) . . ? C52 C51 H51 119.5 . . ? C56 C51 H51 119.5 . . ? C51 C52 C53 119.9(7) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 119.0(7) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C55 C54 C53 120.6(7) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 121.7(6) . . ? C54 C55 H55 119.1 . . ? C56 C55 H55 119.1 . . ? C55 C56 C51 117.7(6) . . ? C55 C56 C57 121.9(6) . . ? C51 C56 C57 120.4(6) . . ? N10 C57 C64 121.7(5) . . ? N10 C57 C56 115.9(5) . . ? C64 C57 C56 122.3(5) . . ? N10 C58 C65 121.8(5) . . ? N10 C58 C59 116.4(5) . . ? C65 C58 C59 121.8(5) . . ? N9 C59 C60 121.5(6) . . ? N9 C59 C58 117.0(5) . . ? C60 C59 C58 121.5(6) . . ? C59 C60 C61 119.8(7) . . ? C59 C60 H60 120.1 . . ? C61 C60 H60 120.1 . . ? C60 C61 C62 119.4(7) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? C61 C62 C63 117.4(6) . . ? C61 C62 H62 121.3 . . ? C63 C62 H62 121.3 . . ? N9 C63 C62 124.0(7) . . ? N9 C63 H63 118.0 . . ? C62 C63 H63 118.0 . . ? C66 C64 C57 120.6(5) . . ? C66 C64 H64 119.7 . . ? C57 C64 H64 119.7 . . ? C58 C65 C66 120.3(5) . . ? C58 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C64 C66 C65 116.9(5) . . ? C64 C66 C67 123.7(5) . . ? C65 C66 C67 119.4(5) . . ? C69 C67 C68 117.9(5) . . ? C69 C67 C66 120.1(5) . . ? C68 C67 C66 122.0(5) . . ? C70 C68 C67 120.2(5) . . ? C70 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C67 C69 C71 122.0(5) . . ? C67 C69 H69 119.0 . . ? C71 C69 H69 119.0 . . ? C68 C70 C72 121.6(5) . . ? C68 C70 H70 119.2 . . ? C72 C70 H70 119.2 . . ? C69 C71 C72 120.0(5) . . ? C69 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C72 C71 118.0(5) . . ? C70 C72 N11 121.9(5) . . ? C71 C72 N11 120.1(5) . . ? N11 C73 C74 108.8(6) . . ? N11 C73 H73 125.6 . . ? C74 C73 H73 125.6 . . ? C73 C74 C75 103.2(6) . . ? C73 C74 H74 128.4 . . ? C75 C74 H74 128.4 . . ? N12 C75 C74 113.2(6) . . ? N12 C75 H75 123.4 . . ? C74 C75 H75 123.4 . . ? C31 N1 C35 118.2(4) . . ? C31 N1 Ag1 109.3(3) . . ? C35 N1 Ag1 125.4(3) . . ? C30 N2 C26 118.6(5) . . ? C30 N2 Ag1 119.5(4) . . ? C26 N2 Ag1 121.9(4) . . ? C48 N3 N4 111.3(6) . . ? C48 N3 C45 129.3(6) . . ? N4 N3 C45 119.3(5) . . ? C50 N4 N3 104.9(7) . . ? C10 N5 C6 118.5(4) . . ? C10 N5 Ag1 127.1(3) . . ? C6 N5 Ag1 113.0(3) . . ? C5 N6 C1 118.5(5) . . ? C5 N6 Ag1 118.3(3) . . ? C1 N6 Ag1 121.3(4) . . ? C23 N7 N8 111.3(5) . . ? C23 N7 C20 127.7(5) . . ? N8 N7 C20 120.9(5) . . ? C25 N8 N7 103.6(6) . . ? C63 N9 C59 117.9(6) . . ? C63 N9 Ag2 123.8(5) . . ? C59 N9 Ag2 118.0(4) . . ? C57 N10 C58 118.6(5) . . ? C57 N10 Ag2 125.0(4) . . ? C58 N10 Ag2 114.3(4) . . ? C73 N11 N12 110.5(5) . . ? C73 N11 C72 128.5(5) . . ? N12 N11 C72 121.0(5) . . ? C75 N12 N11 104.3(5) . . ? C75 N12 Ag2 127.7(5) . 2_767 ? N11 N12 Ag2 125.4(4) . 2_767 ? O2' N13 O3 134.2(17) . . ? O2' N13 O2 38.8(10) . . ? O3 N13 O2 129.6(16) . . ? O2' N13 O1' 131.5(14) . . ? O3 N13 O1' 88.6(13) . . ? O2 N13 O1' 134.8(15) . . ? O2' N13 O1 95.9(14) . . ? O3 N13 O1 119.0(14) . . ? O2 N13 O1 111.1(13) . . ? O1' N13 O1 35.7(8) . . ? O2' N13 O3' 114.1(14) . . ? O3 N13 O3' 31.6(11) . . ? O2 N13 O3' 98.2(13) . . ? O1' N13 O3' 114.2(12) . . ? O1 N13 O3' 148.8(13) . . ? O4 N14 O5 128.3(16) . . ? O4 N14 O6 120(2) . . ? O5 N14 O6 111.4(19) . . ? N13 O1 Ag2 104.0(10) . . ? N13 O1' Ag2 106.8(10) . . ? 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 N6 C1 C2 C3 1.4(11) . . . . ? C1 C2 C3 C4 -0.1(10) . . . . ? C2 C3 C4 C5 -0.8(10) . . . . ? C3 C4 C5 N6 0.5(9) . . . . ? C3 C4 C5 C6 -179.0(5) . . . . ? N6 C5 C6 N5 -2.8(7) . . . . ? C4 C5 C6 N5 176.7(5) . . . . ? N6 C5 C6 C7 178.4(5) . . . . ? C4 C5 C6 C7 -2.1(8) . . . . ? N5 C6 C7 C8 -0.4(8) . . . . ? C5 C6 C7 C8 178.3(5) . . . . ? C6 C7 C8 C9 -0.8(8) . . . . ? C6 C7 C8 C17 179.8(5) . . . . ? C7 C8 C9 C10 1.0(8) . . . . ? C17 C8 C9 C10 -179.6(5) . . . . ? C8 C9 C10 N5 0.0(9) . . . . ? C8 C9 C10 C11 -180.0(5) . . . . ? N5 C10 C11 C16 44.3(8) . . . . ? C9 C10 C11 C16 -135.7(6) . . . . ? N5 C10 C11 C12 -136.3(5) . . . . ? C9 C10 C11 C12 43.7(8) . . . . ? C16 C11 C12 C13 0.1(9) . . . . ? C10 C11 C12 C13 -179.4(5) . . . . ? C11 C12 C13 C14 1.0(10) . . . . ? C12 C13 C14 C15 -1.3(11) . . . . ? C13 C14 C15 C16 0.5(11) . . . . ? C14 C15 C16 C11 0.6(11) . . . . ? C12 C11 C16 C15 -0.9(9) . . . . ? C10 C11 C16 C15 178.6(6) . . . . ? C9 C8 C17 C22 22.2(8) . . . . ? C7 C8 C17 C22 -158.5(5) . . . . ? C9 C8 C17 C18 -157.0(5) . . . . ? C7 C8 C17 C18 22.4(8) . . . . ? C22 C17 C18 C19 0.1(9) . . . . ? C8 C17 C18 C19 179.3(5) . . . . ? C17 C18 C19 C20 -0.2(9) . . . . ? C18 C19 C20 C21 1.0(9) . . . . ? C18 C19 C20 N7 -178.9(5) . . . . ? C19 C20 C21 C22 -1.7(9) . . . . ? N7 C20 C21 C22 178.3(5) . . . . ? C20 C21 C22 C17 1.6(9) . . . . ? C18 C17 C22 C21 -0.8(9) . . . . ? C8 C17 C22 C21 -180.0(5) . . . . ? N7 C23 C24 C25 -1.1(9) . . . . ? C23 C24 C25 N8 2.3(10) . . . . ? N2 C26 C27 C28 0.8(12) . . . . ? C26 C27 C28 C29 0.8(13) . . . . ? C27 C28 C29 C30 -1.9(13) . . . . ? C28 C29 C30 N2 1.4(11) . . . . ? C28 C29 C30 C31 -178.1(7) . . . . ? N2 C30 C31 N1 19.0(7) . . . . ? C29 C30 C31 N1 -161.4(6) . . . . ? N2 C30 C31 C32 -160.8(5) . . . . ? C29 C30 C31 C32 18.7(9) . . . . ? N1 C31 C32 C33 1.4(8) . . . . ? C30 C31 C32 C33 -178.7(5) . . . . ? C31 C32 C33 C34 -2.9(8) . . . . ? C31 C32 C33 C42 177.7(5) . . . . ? C32 C33 C34 C35 2.2(8) . . . . ? C42 C33 C34 C35 -178.4(5) . . . . ? C33 C34 C35 N1 0.0(8) . . . . ? C33 C34 C35 C36 178.8(5) . . . . ? N1 C35 C36 C37 -141.8(6) . . . . ? C34 C35 C36 C37 39.3(8) . . . . ? N1 C35 C36 C41 39.8(8) . . . . ? C34 C35 C36 C41 -139.1(6) . . . . ? C41 C36 C37 C38 -2.0(10) . . . . ? C35 C36 C37 C38 179.6(6) . . . . ? C36 C37 C38 C39 3.3(11) . . . . ? C37 C38 C39 C40 -2.4(12) . . . . ? C38 C39 C40 C41 0.1(12) . . . . ? C39 C40 C41 C36 1.2(10) . . . . ? C37 C36 C41 C40 -0.3(9) . . . . ? C35 C36 C41 C40 178.1(6) . . . . ? C34 C33 C42 C43 36.8(9) . . . . ? C32 C33 C42 C43 -143.8(6) . . . . ? C34 C33 C42 C47 -147.7(6) . . . . ? C32 C33 C42 C47 31.6(8) . . . . ? C47 C42 C43 C44 -2.5(9) . . . . ? C33 C42 C43 C44 173.1(6) . . . . ? C42 C43 C44 C45 1.6(10) . . . . ? C43 C44 C45 C46 -0.2(10) . . . . ? C43 C44 C45 N3 -177.2(6) . . . . ? C44 C45 C46 C47 -0.2(11) . . . . ? N3 C45 C46 C47 177.0(6) . . . . ? C45 C46 C47 C42 -0.9(11) . . . . ? C43 C42 C47 C46 2.2(10) . . . . ? C33 C42 C47 C46 -173.5(6) . . . . ? N3 C48 C49 C50 -0.5(9) . . . . ? C48 C49 C50 N4 0.5(10) . . . . ? C56 C51 C52 C53 0.1(10) . . . . ? C51 C52 C53 C54 1.0(11) . . . . ? C52 C53 C54 C55 -0.4(11) . . . . ? C53 C54 C55 C56 -1.3(10) . . . . ? C54 C55 C56 C51 2.4(9) . . . . ? C54 C55 C56 C57 -174.7(6) . . . . ? C52 C51 C56 C55 -1.8(9) . . . . ? C52 C51 C56 C57 175.4(6) . . . . ? C55 C56 C57 N10 140.0(6) . . . . ? C51 C56 C57 N10 -37.1(7) . . . . ? C55 C56 C57 C64 -37.5(8) . . . . ? C51 C56 C57 C64 145.4(6) . . . . ? N10 C58 C59 N9 -3.3(8) . . . . ? C65 C58 C59 N9 175.9(5) . . . . ? N10 C58 C59 C60 175.2(6) . . . . ? C65 C58 C59 C60 -5.6(9) . . . . ? N9 C59 C60 C61 4.1(10) . . . . ? C58 C59 C60 C61 -174.2(6) . . . . ? C59 C60 C61 C62 -1.7(10) . . . . ? C60 C61 C62 C63 0.0(11) . . . . ? C61 C62 C63 N9 -0.5(11) . . . . ? N10 C57 C64 C66 -0.5(8) . . . . ? C56 C57 C64 C66 176.9(5) . . . . ? N10 C58 C65 C66 -3.0(9) . . . . ? C59 C58 C65 C66 177.8(5) . . . . ? C57 C64 C66 C65 -0.4(8) . . . . ? C57 C64 C66 C67 -179.6(5) . . . . ? C58 C65 C66 C64 2.1(8) . . . . ? C58 C65 C66 C67 -178.7(5) . . . . ? C64 C66 C67 C69 -160.2(6) . . . . ? C65 C66 C67 C69 20.7(8) . . . . ? C64 C66 C67 C68 18.9(8) . . . . ? C65 C66 C67 C68 -160.3(5) . . . . ? C69 C67 C68 C70 -4.8(8) . . . . ? C66 C67 C68 C70 176.2(5) . . . . ? C68 C67 C69 C71 5.1(9) . . . . ? C66 C67 C69 C71 -175.8(5) . . . . ? C67 C68 C70 C72 0.7(9) . . . . ? C67 C69 C71 C72 -1.4(10) . . . . ? C68 C70 C72 C71 3.1(8) . . . . ? C68 C70 C72 N11 -178.4(5) . . . . ? C69 C71 C72 C70 -2.7(9) . . . . ? C69 C71 C72 N11 178.7(5) . . . . ? N11 C73 C74 C75 -0.9(8) . . . . ? C73 C74 C75 N12 1.8(9) . . . . ? C32 C31 N1 C35 0.8(8) . . . . ? C30 C31 N1 C35 -179.1(5) . . . . ? C32 C31 N1 Ag1 153.1(4) . . . . ? C30 C31 N1 Ag1 -26.8(5) . . . . ? C34 C35 N1 C31 -1.5(7) . . . . ? C36 C35 N1 C31 179.6(5) . . . . ? C34 C35 N1 Ag1 -149.0(4) . . . . ? C36 C35 N1 Ag1 32.2(6) . . . . ? N2 Ag1 N1 C31 20.1(3) . . . . ? N6 Ag1 N1 C31 175.2(3) . . . . ? N5 Ag1 N1 C31 -116.1(3) . . . . ? N2 Ag1 N1 C35 169.9(4) . . . . ? N6 Ag1 N1 C35 -35.0(5) . . . . ? N5 Ag1 N1 C35 33.7(4) . . . . ? C29 C30 N2 C26 0.2(9) . . . . ? C31 C30 N2 C26 179.7(5) . . . . ? C29 C30 N2 Ag1 -177.9(5) . . . . ? C31 C30 N2 Ag1 1.6(7) . . . . ? C27 C26 N2 C30 -1.4(10) . . . . ? C27 C26 N2 Ag1 176.7(6) . . . . ? N6 Ag1 N2 C30 -146.0(4) . . . . ? N5 Ag1 N2 C30 62.7(5) . . . . ? N1 Ag1 N2 C30 -11.3(4) . . . . ? N6 Ag1 N2 C26 35.9(7) . . . . ? N5 Ag1 N2 C26 -115.3(5) . . . . ? N1 Ag1 N2 C26 170.6(5) . . . . ? C49 C48 N3 N4 0.3(8) . . . . ? C49 C48 N3 C45 176.1(6) . . . . ? C44 C45 N3 C48 -4.9(11) . . . . ? C46 C45 N3 C48 178.0(7) . . . . ? C44 C45 N3 N4 170.5(6) . . . . ? C46 C45 N3 N4 -6.6(9) . . . . ? C49 C50 N4 N3 -0.3(9) . . . . ? C48 N3 N4 C50 0.0(8) . . . . ? C45 N3 N4 C50 -176.2(6) . . . . ? C9 C10 N5 C6 -1.3(8) . . . . ? C11 C10 N5 C6 178.7(5) . . . . ? C9 C10 N5 Ag1 -166.5(4) . . . . ? C11 C10 N5 Ag1 13.5(7) . . . . ? C7 C6 N5 C10 1.5(8) . . . . ? C5 C6 N5 C10 -177.3(5) . . . . ? C7 C6 N5 Ag1 168.7(4) . . . . ? C5 C6 N5 Ag1 -10.2(5) . . . . ? N2 Ag1 N5 C10 -14.9(5) . . . . ? N6 Ag1 N5 C10 179.1(5) . . . . ? N1 Ag1 N5 C10 50.9(4) . . . . ? N2 Ag1 N5 C6 179.3(3) . . . . ? N6 Ag1 N5 C6 13.2(3) . . . . ? N1 Ag1 N5 C6 -114.9(4) . . . . ? C4 C5 N6 C1 0.8(9) . . . . ? C6 C5 N6 C1 -179.7(5) . . . . ? C4 C5 N6 Ag1 -163.7(4) . . . . ? C6 C5 N6 Ag1 15.8(6) . . . . ? C2 C1 N6 C5 -1.7(10) . . . . ? C2 C1 N6 Ag1 162.2(5) . . . . ? N2 Ag1 N6 C5 -174.0(4) . . . . ? N5 Ag1 N6 C5 -15.4(4) . . . . ? N1 Ag1 N6 C5 63.1(5) . . . . ? N2 Ag1 N6 C1 22.0(7) . . . . ? N5 Ag1 N6 C1 -179.3(5) . . . . ? N1 Ag1 N6 C1 -100.9(5) . . . . ? C24 C23 N7 N8 -0.5(8) . . . . ? C24 C23 N7 C20 -179.3(6) . . . . ? C19 C20 N7 C23 28.1(9) . . . . ? C21 C20 N7 C23 -151.8(6) . . . . ? C19 C20 N7 N8 -150.6(6) . . . . ? C21 C20 N7 N8 29.5(8) . . . . ? C24 C25 N8 N7 -2.5(9) . . . . ? C23 N7 N8 C25 1.8(8) . . . . ? C20 N7 N8 C25 -179.3(6) . . . . ? C62 C63 N9 C59 2.8(10) . . . . ? C62 C63 N9 Ag2 -169.8(6) . . . . ? C60 C59 N9 C63 -4.6(9) . . . . ? C58 C59 N9 C63 173.9(6) . . . . ? C60 C59 N9 Ag2 168.5(5) . . . . ? C58 C59 N9 Ag2 -13.1(7) . . . . ? N12 Ag2 N9 C63 69.9(6) 2_767 . . . ? N10 Ag2 N9 C63 -171.6(6) . . . . ? O1' Ag2 N9 C63 -40.0(7) . . . . ? O1 Ag2 N9 C63 -58.7(8) . . . . ? N12 Ag2 N9 C59 -102.7(5) 2_767 . . . ? N10 Ag2 N9 C59 15.8(4) . . . . ? O1' Ag2 N9 C59 147.4(6) . . . . ? O1 Ag2 N9 C59 128.7(7) . . . . ? C64 C57 N10 C58 -0.2(8) . . . . ? C56 C57 N10 C58 -177.8(5) . . . . ? C64 C57 N10 Ag2 162.3(4) . . . . ? C56 C57 N10 Ag2 -15.2(7) . . . . ? C65 C58 N10 C57 2.0(8) . . . . ? C59 C58 N10 C57 -178.8(5) . . . . ? C65 C58 N10 Ag2 -162.4(4) . . . . ? C59 C58 N10 Ag2 16.8(6) . . . . ? N12 Ag2 N10 C57 -50.4(5) 2_767 . . . ? N9 Ag2 N10 C57 179.7(5) . . . . ? O1' Ag2 N10 C57 81.5(7) . . . . ? O1 Ag2 N10 C57 74.3(6) . . . . ? N12 Ag2 N10 C58 112.8(4) 2_767 . . . ? N9 Ag2 N10 C58 -17.1(4) . . . . ? O1' Ag2 N10 C58 -115.3(6) . . . . ? O1 Ag2 N10 C58 -122.5(5) . . . . ? C74 C73 N11 N12 -0.3(7) . . . . ? C74 C73 N11 C72 -179.1(6) . . . . ? C70 C72 N11 C73 -145.4(6) . . . . ? C71 C72 N11 C73 33.2(9) . . . . ? C70 C72 N11 N12 35.8(8) . . . . ? C71 C72 N11 N12 -145.6(6) . . . . ? C74 C75 N12 N11 -2.0(8) . . . . ? C74 C75 N12 Ag2 160.5(5) . . . 2_767 ? C73 N11 N12 C75 1.4(7) . . . . ? C72 N11 N12 C75 -179.7(5) . . . . ? C73 N11 N12 Ag2 -161.6(4) . . . 2_767 ? C72 N11 N12 Ag2 17.3(7) . . . 2_767 ? O2' N13 O1 Ag2 -111.6(17) . . . . ? O3 N13 O1 Ag2 37(2) . . . . ? O2 N13 O1 Ag2 -148.5(15) . . . . ? O1' N13 O1 Ag2 72.4(19) . . . . ? O3' N13 O1 Ag2 53(3) . . . . ? N12 Ag2 O1 N13 -126.7(12) 2_767 . . . ? N9 Ag2 O1 N13 18.2(15) . . . . ? N10 Ag2 O1 N13 97.0(13) . . . . ? O1' Ag2 O1 N13 -65.8(18) . . . . ? O2' N13 O1' Ag2 -83(2) . . . . ? O3 N13 O1' Ag2 71.9(15) . . . . ? O2 N13 O1' Ag2 -137.3(18) . . . . ? O1 N13 O1' Ag2 -78(2) . . . . ? O3' N13 O1' Ag2 91.0(15) . . . . ? N12 Ag2 O1' N13 -168.2(11) 2_767 . . . ? N9 Ag2 O1' N13 -31.2(13) . . . . ? N10 Ag2 O1' N13 50.0(14) . . . . ? O1 Ag2 O1' N13 71.5(19) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.072 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.082