# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_C26H35N3O1_(2) _database_code_depnum_ccdc_archive 'CCDC 852724' #TrackingRef 'edu_eduag12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 N3 O' _chemical_formula_weight 405.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.7919(6) _cell_length_b 11.3124(12) _cell_length_c 18.4842(19) _cell_angle_alpha 83.323(2) _cell_angle_beta 87.083(2) _cell_angle_gamma 83.546(2) _cell_volume 1194.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1213 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 20.36 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 9305 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4115 _reflns_number_gt 1627 _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^)+(0.0350P)^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 4115 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 C3 C 0.5252(5) 0.7908(2) 0.20468(14) 0.0549(8) Uani 1 1 d . . . C4 C 0.6994(5) 0.8669(2) 0.20283(13) 0.0603(8) Uani 1 1 d . . . H4 H 0.8001 0.8719 0.2397 0.072 Uiso 1 1 calc R . . C5 C 0.6928(5) 0.9333(2) 0.13544(14) 0.0557(8) Uani 1 1 d . . . C6 C 0.8259(5) 1.0289(2) 0.10192(15) 0.0567(8) Uani 1 1 d . . . C10 C 1.0146(5) 1.0587(3) 0.13597(14) 0.0691(9) Uani 1 1 d . . . H10 H 1.0566 1.0188 0.1810 0.083 Uiso 1 1 calc R . . C9 C 1.1406(5) 1.1482(3) 0.10279(16) 0.0780(10) Uani 1 1 d . . . H9 H 1.2696 1.1686 0.1246 0.094 Uiso 1 1 calc R . . C8 C 1.0711(6) 1.2056(3) 0.03748(15) 0.0751(10) Uani 1 1 d . . . H8 H 1.1510 1.2669 0.0140 0.090 Uiso 1 1 calc R . . C7 C 0.8823(5) 1.1720(3) 0.00669(14) 0.0706(9) Uani 1 1 d . . . H7 H 0.8378 1.2119 -0.0381 0.085 Uiso 1 1 calc R . . C11 C 0.4530(5) 0.7011(2) 0.26395(13) 0.0540(8) Uani 1 1 d . . . C12 C 0.2663(5) 0.6383(2) 0.25779(14) 0.0674(9) Uani 1 1 d . . . H12 H 0.1824 0.6541 0.2155 0.081 Uiso 1 1 calc R . . C13 C 0.1982(5) 0.5528(2) 0.31178(14) 0.0681(9) Uani 1 1 d . . . H13 H 0.0717 0.5115 0.3057 0.082 Uiso 1 1 calc R . . C14 C 0.3218(5) 0.5295(2) 0.37533(14) 0.0561(8) Uani 1 1 d . . . C15 C 0.5057(5) 0.5931(2) 0.38329(13) 0.0595(8) Uani 1 1 d . . . H15 H 0.5865 0.5792 0.4262 0.071 Uiso 1 1 calc R . . C16 C 0.5721(5) 0.6775(2) 0.32827(13) 0.0588(8) Uani 1 1 d . . . H16 H 0.6982 0.7191 0.3344 0.071 Uiso 1 1 calc R . . C17 C 0.0861(5) 0.3763(2) 0.42764(13) 0.0627(8) Uani 1 1 d . . . H17A H 0.1140 0.3309 0.3861 0.075 Uiso 1 1 calc R . . H17B H -0.0596 0.4271 0.4216 0.075 Uiso 1 1 calc R . . C18 C 0.0764(5) 0.2933(2) 0.49702(13) 0.0592(8) Uani 1 1 d . . . H18A H 0.0550 0.3406 0.5378 0.071 Uiso 1 1 calc R . . H18B H 0.2244 0.2442 0.5020 0.071 Uiso 1 1 calc R . . C19 C -0.1147(4) 0.2124(2) 0.50106(13) 0.0597(8) Uani 1 1 d . . . H19A H -0.2632 0.2610 0.4963 0.072 Uiso 1 1 calc R . . H19B H -0.0935 0.1644 0.4605 0.072 Uiso 1 1 calc R . . C20 C -0.1196(5) 0.1295(2) 0.57211(13) 0.0607(8) Uani 1 1 d . . . H20A H -0.1363 0.1780 0.6124 0.073 Uiso 1 1 calc R . . H20B H 0.0288 0.0805 0.5762 0.073 Uiso 1 1 calc R . . C21 C -0.3100(4) 0.0482(2) 0.57978(13) 0.0630(8) Uani 1 1 d . . . H21A H -0.4589 0.0968 0.5762 0.076 Uiso 1 1 calc R . . H21B H -0.2940 -0.0006 0.5396 0.076 Uiso 1 1 calc R . . C22 C -0.3089(5) -0.0332(2) 0.65081(13) 0.0650(8) Uani 1 1 d . . . H22A H -0.3253 0.0160 0.6907 0.078 Uiso 1 1 calc R . . H22B H -0.1588 -0.0807 0.6544 0.078 Uiso 1 1 calc R . . C23 C -0.4967(5) -0.1171(2) 0.66030(13) 0.0668(9) Uani 1 1 d . . . H23A H -0.6472 -0.0700 0.6572 0.080 Uiso 1 1 calc R . . H23B H -0.4809 -0.1666 0.6205 0.080 Uiso 1 1 calc R . . C24 C -0.4902(5) -0.1974(2) 0.73157(13) 0.0701(9) Uani 1 1 d . . . H24A H -0.5111 -0.1471 0.7710 0.084 Uiso 1 1 calc R . . H24B H -0.3366 -0.2412 0.7353 0.084 Uiso 1 1 calc R . . C25 C -0.6665(5) -0.2861(2) 0.74300(14) 0.0730(9) Uani 1 1 d . . . H25A H -0.8210 -0.2433 0.7395 0.088 Uiso 1 1 calc R . . H25B H -0.6452 -0.3379 0.7043 0.088 Uiso 1 1 calc R . . C26 C -0.6508(5) -0.3633(3) 0.81623(15) 0.0820(10) Uani 1 1 d . . . H26A H -0.6705 -0.3113 0.8548 0.098 Uiso 1 1 calc R . . H26B H -0.4963 -0.4063 0.8195 0.098 Uiso 1 1 calc R . . C27 C -0.8256(6) -0.4518(3) 0.82910(17) 0.1042(12) Uani 1 1 d . . . H27A H -0.9803 -0.4091 0.8261 0.125 Uiso 1 1 calc R . . H27B H -0.8061 -0.5041 0.7907 0.125 Uiso 1 1 calc R . . C28 C -0.8063(7) -0.5277(3) 0.90243(17) 0.1510(17) Uani 1 1 d . . . H28A H -0.6549 -0.5719 0.9054 0.227 Uiso 1 1 calc R . . H28B H -0.9228 -0.5824 0.9074 0.227 Uiso 1 1 calc R . . H28C H -0.8290 -0.4767 0.9408 0.227 Uiso 1 1 calc R . . N1 N 0.5218(4) 0.8944(2) 0.10083(11) 0.0653(7) Uani 1 1 d . . . H1 H 0.4616 0.9401 0.0445 0.078 Uiso 1 1 d . . . N2 N 0.4151(4) 0.8070(2) 0.14203(12) 0.0676(7) Uani 1 1 d . . . N3 N 0.7573(4) 1.0848(2) 0.03740(11) 0.0627(7) Uani 1 1 d . . . O2 O 0.2726(3) 0.44727(16) 0.43308(9) 0.0679(6) 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 C3 0.060(2) 0.0577(19) 0.0455(17) 0.0001(15) -0.0025(15) -0.0036(17) C4 0.065(2) 0.064(2) 0.0508(18) 0.0010(16) -0.0044(15) -0.0120(17) C5 0.059(2) 0.060(2) 0.0468(18) -0.0007(15) -0.0021(16) -0.0086(16) C6 0.059(2) 0.0584(19) 0.0518(18) -0.0039(16) 0.0003(17) -0.0056(17) C10 0.074(2) 0.078(2) 0.0537(19) 0.0057(16) -0.0111(18) -0.0147(19) C9 0.078(2) 0.088(3) 0.072(2) -0.0037(19) -0.0104(19) -0.031(2) C8 0.094(3) 0.075(2) 0.059(2) -0.0008(18) -0.0034(19) -0.025(2) C7 0.086(3) 0.076(2) 0.0514(19) 0.0056(17) -0.0114(18) -0.027(2) C11 0.058(2) 0.0573(19) 0.0442(17) -0.0001(14) -0.0001(15) -0.0034(16) C12 0.070(2) 0.077(2) 0.0537(19) 0.0104(16) -0.0150(17) -0.0142(19) C13 0.071(2) 0.077(2) 0.0565(19) 0.0092(16) -0.0162(17) -0.0204(17) C14 0.060(2) 0.0565(19) 0.0511(18) 0.0050(15) -0.0021(16) -0.0120(17) C15 0.060(2) 0.068(2) 0.0491(18) 0.0046(15) -0.0096(15) -0.0090(17) C16 0.061(2) 0.0639(19) 0.0509(17) 0.0063(15) -0.0077(15) -0.0134(16) C17 0.065(2) 0.0604(19) 0.0613(19) 0.0063(15) -0.0062(16) -0.0133(17) C18 0.061(2) 0.0570(18) 0.0583(18) 0.0025(15) -0.0040(15) -0.0095(16) C19 0.064(2) 0.0559(18) 0.0585(18) 0.0016(14) -0.0035(15) -0.0099(16) C20 0.059(2) 0.0626(19) 0.0589(18) 0.0044(15) -0.0018(15) -0.0128(16) C21 0.063(2) 0.0640(19) 0.0606(18) 0.0051(15) -0.0050(16) -0.0109(17) C22 0.064(2) 0.068(2) 0.0615(19) 0.0005(15) 0.0002(16) -0.0110(17) C23 0.070(2) 0.070(2) 0.0595(19) 0.0016(16) -0.0050(16) -0.0123(18) C24 0.068(2) 0.075(2) 0.066(2) 0.0022(17) 0.0000(17) -0.0133(18) C25 0.079(2) 0.071(2) 0.070(2) -0.0020(17) 0.0030(17) -0.0207(18) C26 0.091(3) 0.070(2) 0.082(2) 0.0050(18) 0.0145(19) -0.019(2) C27 0.122(3) 0.085(3) 0.106(3) -0.002(2) 0.010(2) -0.029(2) C28 0.239(5) 0.105(3) 0.097(3) 0.032(2) 0.033(3) -0.028(3) N1 0.0691(18) 0.0711(17) 0.0532(15) 0.0141(13) -0.0060(13) -0.0172(14) N2 0.0731(18) 0.0751(17) 0.0534(15) 0.0164(13) -0.0087(13) -0.0244(14) N3 0.0696(18) 0.0667(16) 0.0513(15) 0.0041(13) -0.0048(13) -0.0150(14) O2 0.0728(15) 0.0741(14) 0.0567(12) 0.0166(10) -0.0099(10) -0.0283(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C3 N2 1.334(3) . ? C3 C4 1.395(3) . ? C3 C11 1.482(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 N1 1.346(3) . ? C5 C6 1.460(3) . ? C6 N3 1.340(3) . ? C6 C10 1.381(3) . ? C10 C9 1.382(3) . ? C10 H10 0.9300 . ? C9 C8 1.360(3) . ? C9 H9 0.9300 . ? C8 C7 1.367(3) . ? C8 H8 0.9300 . ? C7 N3 1.345(3) . ? C7 H7 0.9300 . ? C11 C12 1.375(3) . ? C11 C16 1.389(3) . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C13 C14 1.390(3) . ? C13 H13 0.9300 . ? C14 C15 1.374(3) . ? C14 O2 1.373(3) . ? C15 C16 1.382(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O2 1.431(3) . ? C17 C18 1.502(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.507(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.523(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.505(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.514(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.513(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.510(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.501(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.524(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.493(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.520(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N1 N2 1.361(2) . ? N1 H1 1.1594 . ? 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 C3 C4 110.8(2) . . ? N2 C3 C11 119.5(3) . . ? C4 C3 C11 129.6(3) . . ? C5 C4 C3 106.3(2) . . ? C5 C4 H4 126.8 . . ? C3 C4 H4 126.8 . . ? N1 C5 C4 105.5(3) . . ? N1 C5 C6 122.1(2) . . ? C4 C5 C6 132.4(3) . . ? N3 C6 C10 122.3(3) . . ? N3 C6 C5 117.2(3) . . ? C10 C6 C5 120.6(3) . . ? C9 C10 C6 119.7(3) . . ? C9 C10 H10 120.2 . . ? C6 C10 H10 120.2 . . ? C10 C9 C8 118.3(3) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C7 C8 C9 119.2(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? N3 C7 C8 123.9(3) . . ? N3 C7 H7 118.1 . . ? C8 C7 H7 118.1 . . ? C12 C11 C16 117.4(2) . . ? C12 C11 C3 121.7(2) . . ? C16 C11 C3 120.9(3) . . ? C11 C12 C13 122.7(3) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 O2 115.8(2) . . ? C15 C14 C13 119.3(2) . . ? O2 C14 C13 124.9(3) . . ? C14 C15 C16 120.8(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 120.8(3) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? O2 C17 C18 106.9(2) . . ? O2 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O2 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 114.1(2) . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 112.7(2) . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 115.0(2) . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20B 108.5 . . ? C21 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 113.6(2) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 115.1(2) . . ? C21 C22 H22A 108.5 . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22B 108.5 . . ? C23 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C22 113.8(2) . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C23 C24 C25 116.4(2) . . ? C23 C24 H24A 108.2 . . ? C25 C24 H24A 108.2 . . ? C23 C24 H24B 108.2 . . ? C25 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C24 113.5(2) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C27 114.5(3) . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 113.5(3) . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C5 N1 N2 113.0(2) . . ? C5 N1 H1 121.8 . . ? N2 N1 H1 124.8 . . ? C3 N2 N1 104.4(2) . . ? C7 N3 C6 116.7(2) . . ? C14 O2 C17 118.6(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 N2 C3 C4 C5 0.4(3) . . . . ? C11 C3 C4 C5 -179.3(3) . . . . ? C3 C4 C5 N1 -0.5(3) . . . . ? C3 C4 C5 C6 178.2(3) . . . . ? N1 C5 C6 N3 6.0(4) . . . . ? C4 C5 C6 N3 -172.5(3) . . . . ? N1 C5 C6 C10 -173.7(3) . . . . ? C4 C5 C6 C10 7.7(5) . . . . ? N3 C6 C10 C9 -0.8(4) . . . . ? C5 C6 C10 C9 179.0(3) . . . . ? C6 C10 C9 C8 1.0(4) . . . . ? C10 C9 C8 C7 -0.8(5) . . . . ? C9 C8 C7 N3 0.4(5) . . . . ? N2 C3 C11 C12 -3.7(4) . . . . ? C4 C3 C11 C12 176.0(3) . . . . ? N2 C3 C11 C16 176.5(3) . . . . ? C4 C3 C11 C16 -3.8(4) . . . . ? C16 C11 C12 C13 -1.3(4) . . . . ? C3 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 0.9(4) . . . . ? C12 C13 C14 O2 179.9(3) . . . . ? O2 C14 C15 C16 179.4(2) . . . . ? C13 C14 C15 C16 -1.6(4) . . . . ? C12 C11 C16 C15 0.7(4) . . . . ? C3 C11 C16 C15 -179.5(2) . . . . ? C14 C15 C16 C11 0.7(4) . . . . ? O2 C17 C18 C19 179.1(2) . . . . ? C17 C18 C19 C20 -179.9(2) . . . . ? C18 C19 C20 C21 178.9(2) . . . . ? C19 C20 C21 C22 179.7(2) . . . . ? C20 C21 C22 C23 -179.5(2) . . . . ? C21 C22 C23 C24 179.8(2) . . . . ? C22 C23 C24 C25 -177.7(2) . . . . ? C23 C24 C25 C26 -179.5(2) . . . . ? C24 C25 C26 C27 179.6(3) . . . . ? C25 C26 C27 C28 180.0(3) . . . . ? C4 C5 N1 N2 0.5(3) . . . . ? C6 C5 N1 N2 -178.4(2) . . . . ? C4 C3 N2 N1 -0.1(3) . . . . ? C11 C3 N2 N1 179.6(2) . . . . ? C5 N1 N2 C3 -0.2(3) . . . . ? C8 C7 N3 C6 -0.1(4) . . . . ? C10 C6 N3 C7 0.3(4) . . . . ? C5 C6 N3 C7 -179.5(2) . . . . ? C15 C14 O2 C17 -178.7(2) . . . . ? C13 C14 O2 C17 2.3(4) . . . . ? C18 C17 O2 C14 178.6(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 N3 1.16 2.09 3.065(3) 139.8 2_675 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.323 _refine_diff_density_min -0.125 _refine_diff_density_rms 0.030 data_C106H144Ag2Cl4N14O10_(5) _database_code_depnum_ccdc_archive 'CCDC 852725' #TrackingRef 'edu_eduag12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H144 Ag2 Cl4 N14 O10' _chemical_formula_weight 2131.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 12.5359(17) _cell_length_b 13.0895(16) _cell_length_c 17.370(2) _cell_angle_alpha 96.276(2) _cell_angle_beta 92.882(2) _cell_angle_gamma 102.947(3) _cell_volume 2752.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 21296 _diffrn_reflns_av_R_equivalents 0.1933 _diffrn_reflns_av_sigmaI/netI 0.4734 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9437 _reflns_number_gt 2121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0500P)^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 9437 _refine_ls_number_parameters 581 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.3376 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.018 _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 N5 N 0.5568(9) 0.7629(10) 0.3274(6) 0.068(4) Uani 1 1 d . . . H5 H 0.6235 0.7611 0.3179 0.082 Uiso 1 1 d . . . N2 N 0.7156(9) 0.4900(7) 0.3552(6) 0.051(3) Uani 1 1 d . . . H2 H 0.7370 0.5565 0.3490 0.061 Uiso 1 1 d . . . Ag1 Ag 0.48400(9) 0.52076(9) 0.41268(7) 0.0753(5) Uani 1 1 d . . . N1 N 0.6177(9) 0.4462(9) 0.3860(6) 0.059(3) Uani 1 1 d . . . O1 O 1.1818(8) 0.5232(8) 0.2072(5) 0.079(3) Uani 1 1 d . . . O2 O 0.7568(7) 0.7057(8) 0.3389(6) 0.081(4) Uani 1 1 d . . . C3 C 0.7723(11) 0.4182(12) 0.3370(8) 0.053(4) Uani 1 1 d . . . N3 N 0.4548(11) 0.3191(10) 0.4463(7) 0.079(4) Uani 1 1 d . . . O3 O 0.8782(9) 0.7079(9) 0.4311(7) 0.113(4) Uani 1 1 d . . . C4 C 0.7163(11) 0.3243(11) 0.3560(7) 0.057(4) Uani 1 1 d . . . H4A H 0.7353 0.2595 0.3479 0.069 Uiso 1 1 calc R . . N4 N 0.4882(9) 0.6832(9) 0.3595(7) 0.072(4) Uani 1 1 d . . . O4 O 0.8463(8) 0.8484(9) 0.3996(6) 0.115(4) Uani 1 1 d . . . C5 C 0.6220(11) 0.3457(11) 0.3911(8) 0.053(4) Uani 1 1 d . . . O5 O 0.7325(8) 1.1731(7) 0.1592(5) 0.080(3) Uani 1 1 d . . . C6 C 0.5341(13) 0.2759(13) 0.4192(8) 0.056(4) Uani 1 1 d . . . N6 N 0.3177(8) 0.5562(9) 0.4143(6) 0.057(3) Uani 1 1 d . . . C7 C 0.5343(12) 0.1716(14) 0.4172(9) 0.083(5) Uani 1 1 d . . . H7A H 0.5911 0.1444 0.3971 0.100 Uiso 1 1 calc R . . N7 N 0.8298(13) 0.7536(11) 0.3884(10) 0.091(5) Uani 1 1 d . . . C8 C 0.4461(16) 0.1081(12) 0.4464(9) 0.088(5) Uani 1 1 d . . . H8A H 0.4452 0.0371 0.4477 0.105 Uiso 1 1 calc R . . C9 C 0.3620(14) 0.1450(14) 0.4731(9) 0.094(6) Uani 1 1 d . . . H9A H 0.3028 0.1001 0.4911 0.113 Uiso 1 1 calc R . . C10 C 0.3649(14) 0.2512(17) 0.4732(8) 0.095(6) Uani 1 1 d . . . H10A H 0.3068 0.2779 0.4912 0.114 Uiso 1 1 calc R . . C11 C 0.8780(11) 0.4458(12) 0.3014(8) 0.064(4) Uani 1 1 d . . . C12 C 0.9559(11) 0.3840(10) 0.3054(7) 0.065(4) Uani 1 1 d . . . H12A H 0.9407 0.3232 0.3300 0.078 Uiso 1 1 calc R . . C13 C 1.0539(13) 0.4127(13) 0.2733(9) 0.085(5) Uani 1 1 d . . . H13A H 1.1036 0.3698 0.2760 0.102 Uiso 1 1 calc R . . C14 C 1.0825(12) 0.5029(13) 0.2369(9) 0.072(5) Uani 1 1 d . . . C15 C 1.0066(11) 0.5656(10) 0.2324(7) 0.062(4) Uani 1 1 d . . . H15A H 1.0226 0.6263 0.2078 0.074 Uiso 1 1 calc R . . C16 C 0.9076(10) 0.5369(11) 0.2648(8) 0.064(4) Uani 1 1 d . . . H16A H 0.8583 0.5802 0.2621 0.077 Uiso 1 1 calc R . . C17 C 0.5130(11) 0.8421(12) 0.3109(8) 0.062(4) Uani 1 1 d . . . C18 C 0.4040(11) 0.8135(11) 0.3336(7) 0.067(4) Uani 1 1 d . . . H18A H 0.3489 0.8501 0.3286 0.080 Uiso 1 1 calc R . . C19 C 0.3971(11) 0.7188(11) 0.3650(7) 0.054(4) Uani 1 1 d . . . C20 C 0.3041(11) 0.6495(13) 0.3962(8) 0.063(4) Uani 1 1 d . . . C21 C 0.2059(10) 0.6853(11) 0.4062(8) 0.076(5) Uani 1 1 d . . . H21A H 0.1988 0.7505 0.3928 0.091 Uiso 1 1 calc R . . C22 C 0.1209(11) 0.6178(13) 0.4372(8) 0.089(5) Uani 1 1 d . . . H22A H 0.0547 0.6373 0.4436 0.107 Uiso 1 1 calc R . . C23 C 0.1336(11) 0.5218(11) 0.4587(8) 0.077(5) Uani 1 1 d . . . H23A H 0.0774 0.4762 0.4794 0.092 Uiso 1 1 calc R . . C24 C 0.2355(12) 0.4968(11) 0.4477(8) 0.073(5) Uani 1 1 d . . . H24A H 0.2469 0.4349 0.4648 0.088 Uiso 1 1 calc R . . C25 C 0.5691(11) 0.9319(11) 0.2756(8) 0.059(4) Uani 1 1 d . . . C26 C 0.5177(11) 1.0010(12) 0.2437(8) 0.065(4) Uani 1 1 d . . . H26A H 0.4428 0.9933 0.2480 0.078 Uiso 1 1 calc R . . C27 C 0.5706(11) 1.0786(11) 0.2067(9) 0.074(5) Uani 1 1 d . . . H27A H 0.5320 1.1235 0.1860 0.089 Uiso 1 1 calc R . . C28 C 0.6828(13) 1.0938(10) 0.1984(8) 0.058(4) Uani 1 1 d . . . C29 C 0.7392(11) 1.0265(13) 0.2312(9) 0.093(6) Uani 1 1 d . . . H29A H 0.8147 1.0357 0.2291 0.112 Uiso 1 1 calc R . . C30 C 0.6787(11) 0.9454(12) 0.2670(9) 0.088(5) Uani 1 1 d . . . H30A H 0.7148 0.8976 0.2863 0.105 Uiso 1 1 calc R . . C43 C 0.8443(10) 1.1785(10) 0.1431(8) 0.073(4) Uani 1 1 d . . . H43A H 0.8511 1.1127 0.1143 0.087 Uiso 1 1 calc R . . H43B H 0.8907 1.1907 0.1912 0.087 Uiso 1 1 calc R . . C44 C 0.8780(10) 1.2677(11) 0.0961(8) 0.077(4) Uani 1 1 d . . . H44A H 0.8791 1.3341 0.1274 0.092 Uiso 1 1 calc R . . H44B H 0.8255 1.2596 0.0517 0.092 Uiso 1 1 calc R . . C45 C 0.9925(10) 1.2690(10) 0.0684(7) 0.070(4) Uani 1 1 d . . . H45A H 1.0432 1.2721 0.1131 0.084 Uiso 1 1 calc R . . H45B H 0.9897 1.2036 0.0353 0.084 Uiso 1 1 calc R . . C46 C 1.0357(10) 1.3608(10) 0.0242(8) 0.079(5) Uani 1 1 d . . . H46A H 1.0363 1.4258 0.0571 0.095 Uiso 1 1 calc R . . H46B H 0.9852 1.3566 -0.0208 0.095 Uiso 1 1 calc R . . C47 C 1.1510(11) 1.3671(11) -0.0033(8) 0.079(5) Uani 1 1 d . . . H47A H 1.2017 1.3725 0.0418 0.095 Uiso 1 1 calc R . . H47B H 1.1507 1.3016 -0.0355 0.095 Uiso 1 1 calc R . . C48 C 1.1929(11) 1.4573(11) -0.0483(8) 0.086(5) Uani 1 1 d . . . H48A H 1.1974 1.5230 -0.0152 0.103 Uiso 1 1 calc R . . H48B H 1.1403 1.4542 -0.0919 0.103 Uiso 1 1 calc R . . C49 C 1.3046(11) 1.4585(11) -0.0788(8) 0.087(5) Uani 1 1 d . . . H49A H 1.2981 1.3958 -0.1157 0.104 Uiso 1 1 calc R . . H49B H 1.3553 1.4543 -0.0358 0.104 Uiso 1 1 calc R . . C50 C 1.3537(10) 1.5548(11) -0.1180(8) 0.071(4) Uani 1 1 d . . . H50A H 1.3040 1.5589 -0.1616 0.085 Uiso 1 1 calc R . . H50B H 1.3602 1.6179 -0.0814 0.085 Uiso 1 1 calc R . . C51 C 1.4651(12) 1.5532(12) -0.1467(9) 0.104(6) Uani 1 1 d . . . H51A H 1.5137 1.5467 -0.1031 0.124 Uiso 1 1 calc R . . H51B H 1.4577 1.4907 -0.1840 0.124 Uiso 1 1 calc R . . C52 C 1.5170(10) 1.6458(11) -0.1831(8) 0.075(4) Uani 1 1 d . . . H52A H 1.5238 1.7075 -0.1451 0.090 Uiso 1 1 calc R . . H52B H 1.4666 1.6524 -0.2255 0.090 Uiso 1 1 calc R . . C53 C 1.6252(10) 1.6509(13) -0.2139(9) 0.098(6) Uani 1 1 d . . . H53A H 1.6182 1.5909 -0.2534 0.118 Uiso 1 1 calc R . . H53B H 1.6756 1.6424 -0.1721 0.118 Uiso 1 1 calc R . . C54 C 1.6768(12) 1.7488(12) -0.2485(9) 0.112(6) Uani 1 1 d . . . H54A H 1.7469 1.7427 -0.2659 0.169 Uiso 1 1 calc R . . H54B H 1.6866 1.8092 -0.2099 0.169 Uiso 1 1 calc R . . H54C H 1.6300 1.7570 -0.2917 0.169 Uiso 1 1 calc R . . C31 C 1.2132(8) 0.6192(10) 0.1747(8) 0.067(4) Uani 1 1 d D . . H31A H 1.2108 0.6786 0.2126 0.081 Uiso 1 1 calc R . . H31B H 1.1639 0.6193 0.1299 0.081 Uiso 1 1 calc R . . C36 C 1.6399(8) 0.8466(10) 0.0180(7) 0.075(4) Uani 1 1 d D . . H36A H 1.6902 0.8554 0.0639 0.090 Uiso 1 1 calc R . . H36B H 1.6457 0.7828 -0.0140 0.090 Uiso 1 1 calc R . . C33 C 1.3694(8) 0.7237(10) 0.1096(7) 0.076(4) Uani 1 1 d D . . H33A H 1.3655 0.7863 0.1437 0.091 Uiso 1 1 calc R . . H33B H 1.3205 0.7193 0.0637 0.091 Uiso 1 1 calc R . . C34 C 1.4863(8) 0.7361(10) 0.0853(7) 0.072(4) Uani 1 1 d D . . H34A H 1.5358 0.7419 0.1312 0.086 Uiso 1 1 calc R . . H34B H 1.4909 0.6732 0.0517 0.086 Uiso 1 1 calc R . . C35 C 1.5236(9) 0.8319(10) 0.0432(7) 0.076(5) Uani 1 1 d D . . H35A H 1.5186 0.8946 0.0770 0.091 Uiso 1 1 calc R . . H35B H 1.4736 0.8259 -0.0024 0.091 Uiso 1 1 calc R . . C32 C 1.3292(9) 0.6271(9) 0.1508(7) 0.073(4) Uani 1 1 d D . . H32A H 1.3315 0.5640 0.1166 0.087 Uiso 1 1 calc R . . H32B H 1.3781 0.6308 0.1967 0.087 Uiso 1 1 calc R . . C37 C 1.6757(10) 0.9400(11) -0.0269(8) 0.100(5) Uani 1 1 d D . . H37A H 1.6702 1.0041 0.0048 0.120 Uiso 1 1 calc R . . H37B H 1.6265 0.9311 -0.0733 0.120 Uiso 1 1 calc R . . C38 C 1.7924(9) 0.9513(10) -0.0499(8) 0.087(5) Uani 1 1 d D . . H38A H 1.8427 0.9694 -0.0035 0.105 Uiso 1 1 calc R . . H38B H 1.8005 0.8844 -0.0760 0.105 Uiso 1 1 calc R . . C40 C 1.9328(11) 1.0522(12) -0.1366(9) 0.122(6) Uiso 1 1 d D . . H40A H 1.9488 0.9845 -0.1534 0.146 Uiso 1 1 calc R . . H40B H 1.9896 1.0905 -0.0973 0.146 Uiso 1 1 calc R . . C39 C 1.8213(11) 1.0358(11) -0.1031(8) 0.107(6) Uani 1 1 d D . . H39A H 1.8163 1.1024 -0.0747 0.128 Uiso 1 1 calc R . . H39B H 1.7656 1.0197 -0.1462 0.128 Uiso 1 1 calc R . . C41 C 1.9302(17) 1.1153(18) -0.2056(12) 0.260 Uiso 1 1 d D . . H41A H 1.9039 1.0705 -0.2542 0.312 Uiso 1 1 calc R . . H41B H 1.8884 1.1690 -0.1973 0.312 Uiso 1 1 calc R . . C42 C 2.0529(17) 1.161(2) -0.2001(15) 0.320 Uiso 1 1 d D . . H42A H 2.0824 1.1646 -0.1475 0.480 Uiso 1 1 calc R . . H42B H 2.0670 1.2311 -0.2153 0.480 Uiso 1 1 calc R . . H42C H 2.0871 1.1173 -0.2338 0.480 Uiso 1 1 calc R . . C55 C 1.0100(14) 0.9049(14) -0.4322(10) 0.161(8) Uiso 1 1 d . . . H55A H 1.0189 0.9809 -0.4240 0.193 Uiso 1 1 calc R . . H55B H 0.9626 0.8780 -0.4793 0.193 Uiso 1 1 calc R . . Cl1 Cl 1.1378(5) 0.8766(5) -0.4445(4) 0.214(3) Uiso 1 1 d . . . Cl2 Cl 0.9480(5) 0.8510(5) -0.3551(4) 0.206(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N5 0.064(8) 0.068(10) 0.079(9) 0.038(8) 0.024(7) 0.012(8) N2 0.054(7) 0.038(8) 0.061(8) 0.006(6) 0.016(6) 0.008(6) Ag1 0.0572(7) 0.0734(9) 0.1044(10) 0.0194(7) 0.0143(6) 0.0282(6) N1 0.062(8) 0.056(9) 0.061(8) 0.019(7) 0.014(7) 0.013(7) O1 0.062(7) 0.112(9) 0.081(8) 0.035(7) 0.029(6) 0.045(6) O2 0.061(7) 0.062(8) 0.116(10) 0.013(7) 0.005(6) 0.004(6) C3 0.042(9) 0.054(11) 0.059(11) 0.005(9) -0.005(8) 0.009(9) N3 0.060(9) 0.100(11) 0.083(10) 0.031(9) 0.035(8) 0.016(9) O3 0.107(9) 0.114(10) 0.136(11) 0.032(8) -0.013(7) 0.058(8) C4 0.051(9) 0.059(11) 0.069(11) 0.022(9) 0.006(8) 0.020(9) N4 0.048(7) 0.081(10) 0.095(10) 0.021(8) 0.006(7) 0.028(7) O4 0.123(9) 0.078(9) 0.136(10) 0.028(9) -0.039(7) 0.012(8) C5 0.049(10) 0.031(10) 0.078(12) 0.001(9) -0.002(9) 0.009(8) O5 0.079(7) 0.074(8) 0.099(8) 0.034(7) 0.023(6) 0.027(6) C6 0.076(12) 0.033(11) 0.054(11) 0.009(9) -0.003(9) 0.003(10) N6 0.053(8) 0.042(8) 0.075(9) 0.027(7) 0.004(7) -0.001(7) C7 0.074(12) 0.068(14) 0.090(13) 0.010(11) 0.018(10) -0.023(11) N7 0.100(13) 0.023(10) 0.151(17) 0.009(11) 0.017(11) 0.013(10) C8 0.128(16) 0.049(12) 0.103(14) 0.024(10) 0.027(12) 0.042(13) C9 0.098(14) 0.051(13) 0.130(16) 0.021(12) 0.025(12) 0.001(11) C10 0.094(14) 0.120(18) 0.072(13) -0.001(13) 0.018(11) 0.030(14) C11 0.059(10) 0.071(12) 0.074(12) 0.017(10) 0.015(9) 0.032(9) C12 0.053(9) 0.066(11) 0.085(12) 0.022(9) 0.026(9) 0.024(9) C13 0.082(13) 0.094(15) 0.094(14) 0.004(12) 0.005(11) 0.055(11) C14 0.050(10) 0.081(14) 0.091(14) 0.001(11) 0.009(10) 0.029(10) C15 0.051(9) 0.075(11) 0.065(11) 0.023(9) 0.021(8) 0.017(9) C16 0.047(9) 0.066(12) 0.083(12) 0.001(10) -0.001(9) 0.025(8) C17 0.039(9) 0.072(13) 0.078(12) 0.021(10) 0.007(9) 0.015(9) C18 0.080(12) 0.067(12) 0.067(11) 0.024(9) 0.026(9) 0.034(9) C19 0.049(10) 0.059(11) 0.057(11) 0.021(9) 0.012(8) 0.014(9) C20 0.045(10) 0.089(14) 0.050(11) -0.016(10) -0.005(8) 0.016(10) C21 0.040(9) 0.102(13) 0.101(13) 0.032(10) 0.028(9) 0.035(9) C22 0.052(10) 0.115(16) 0.109(14) 0.068(12) 0.015(10) 0.013(10) C23 0.066(11) 0.066(12) 0.099(13) 0.009(10) 0.014(10) 0.014(9) C24 0.056(10) 0.069(12) 0.101(13) 0.022(10) 0.023(10) 0.019(9) C25 0.051(10) 0.053(11) 0.072(11) 0.024(9) 0.005(9) 0.006(9) C26 0.067(10) 0.073(12) 0.070(12) 0.023(10) 0.015(9) 0.037(10) C27 0.053(10) 0.063(12) 0.114(15) 0.022(11) 0.009(10) 0.024(9) C28 0.078(12) 0.030(10) 0.069(11) 0.024(8) 0.030(9) 0.007(9) C29 0.057(10) 0.084(14) 0.139(16) 0.060(12) -0.001(10) 0.000(10) C30 0.044(10) 0.074(13) 0.147(16) 0.026(11) -0.006(10) 0.017(9) C43 0.065(11) 0.045(10) 0.113(14) 0.021(10) 0.023(10) 0.016(8) C44 0.067(10) 0.076(12) 0.091(12) 0.027(10) 0.008(9) 0.013(9) C45 0.077(11) 0.083(12) 0.052(10) 0.030(9) 0.021(9) 0.008(9) C46 0.074(11) 0.093(13) 0.084(12) 0.038(10) 0.019(10) 0.032(9) C47 0.092(12) 0.081(12) 0.079(12) 0.032(10) 0.032(10) 0.035(9) C48 0.070(11) 0.107(14) 0.097(13) 0.046(11) 0.022(10) 0.035(10) C49 0.083(12) 0.101(14) 0.088(13) 0.013(11) 0.013(10) 0.042(10) C50 0.058(10) 0.088(13) 0.068(11) 0.021(10) -0.002(8) 0.015(9) C51 0.082(13) 0.102(15) 0.140(16) 0.064(13) 0.009(12) 0.026(11) C52 0.069(11) 0.090(13) 0.072(12) 0.016(10) 0.004(9) 0.025(9) C53 0.049(10) 0.151(17) 0.115(15) 0.046(13) 0.031(10) 0.045(10) C54 0.119(14) 0.114(15) 0.114(15) 0.051(13) 0.031(12) 0.024(12) C31 0.052(9) 0.055(11) 0.091(12) 0.024(9) 0.005(9) -0.002(8) C36 0.057(10) 0.094(13) 0.078(12) 0.009(10) -0.004(9) 0.028(9) C33 0.051(9) 0.090(12) 0.100(13) 0.028(10) 0.016(9) 0.034(8) C34 0.039(9) 0.097(13) 0.075(12) -0.001(10) 0.012(8) 0.010(8) C35 0.057(10) 0.095(13) 0.083(12) 0.014(10) 0.013(9) 0.028(9) C32 0.068(10) 0.075(12) 0.074(12) -0.008(9) 0.026(9) 0.018(9) C37 0.090(13) 0.106(14) 0.119(15) 0.061(12) 0.022(11) 0.027(11) C38 0.059(10) 0.089(13) 0.128(15) 0.055(11) 0.037(10) 0.020(9) C39 0.098(13) 0.098(14) 0.125(15) 0.037(12) 0.036(11) 0.007(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N5 C17 1.329(14) . ? N5 N4 1.383(12) . ? N5 H5 0.8646 . ? N2 C3 1.322(13) . ? N2 N1 1.393(11) . ? N2 H2 0.8715 . ? Ag1 N1 2.165(10) . ? Ag1 N6 2.236(10) . ? Ag1 N4 2.400(12) . ? Ag1 N3 2.714(12) . ? Ag1 Ag1 3.162(2) 2_666 ? N1 C5 1.340(13) . ? O1 C14 1.354(14) . ? O1 C31 1.417(12) . ? O2 N7 1.232(15) . ? C3 C4 1.356(14) . ? C3 C11 1.478(16) . ? N3 C6 1.330(15) . ? N3 C10 1.405(17) . ? O3 N7 1.220(15) . ? C4 C5 1.425(15) . ? C4 H4A 0.9300 . ? N4 C19 1.331(13) . ? O4 N7 1.204(13) . ? C5 C6 1.410(16) . ? O5 C28 1.355(13) . ? O5 C43 1.432(12) . ? C6 C7 1.363(16) . ? N6 C20 1.338(15) . ? N6 C24 1.342(14) . ? C7 C8 1.381(16) . ? C7 H7A 0.9300 . ? C8 C9 1.336(17) . ? C8 H8A 0.9300 . ? C9 C10 1.382(17) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C16 1.399(15) . ? C11 C12 1.405(15) . ? C12 C13 1.368(16) . ? C12 H12A 0.9300 . ? C13 C14 1.385(17) . ? C13 H13A 0.9300 . ? C14 C15 1.394(15) . ? C15 C16 1.380(14) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.421(15) . ? C17 C25 1.443(16) . ? C18 C19 1.394(15) . ? C18 H18A 0.9300 . ? C19 C20 1.474(16) . ? C20 C21 1.424(14) . ? C21 C22 1.396(15) . ? C21 H21A 0.9300 . ? C22 C23 1.389(15) . ? C22 H22A 0.9300 . ? C23 C24 1.404(15) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C30 1.364(15) . ? C25 C26 1.369(15) . ? C26 C27 1.329(14) . ? C26 H26A 0.9300 . ? C27 C28 1.394(15) . ? C27 H27A 0.9300 . ? C28 C29 1.396(16) . ? C29 C30 1.385(16) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C43 C44 1.493(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.534(14) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.510(14) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.532(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.499(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.520(15) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.521(15) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.510(15) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.465(15) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.474(14) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.502(15) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C31 C32 1.516(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C36 C37 1.517(5) . ? C36 C35 1.521(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C33 C32 1.521(5) . ? C33 C34 1.523(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.517(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C37 C38 1.516(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.512(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C40 C39 1.520(5) . ? C40 C41 1.532(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C42 1.515(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C55 Cl2 1.721(16) . ? C55 Cl1 1.741(16) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? 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 C17 N5 N4 115.5(11) . . ? C17 N5 H5 121.9 . . ? N4 N5 H5 122.6 . . ? C3 N2 N1 111.4(11) . . ? C3 N2 H2 124.2 . . ? N1 N2 H2 124.4 . . ? N1 Ag1 N6 162.4(4) . . ? N1 Ag1 N4 115.8(4) . . ? N6 Ag1 N4 70.6(4) . . ? N1 Ag1 N3 65.1(4) . . ? N6 Ag1 N3 105.3(4) . . ? N4 Ag1 N3 168.6(4) . . ? N1 Ag1 Ag1 88.8(3) . 2_666 ? N6 Ag1 Ag1 99.2(3) . 2_666 ? N4 Ag1 Ag1 129.9(3) . 2_666 ? N3 Ag1 Ag1 60.6(3) . 2_666 ? C5 N1 N2 104.5(11) . . ? C5 N1 Ag1 127.7(10) . . ? N2 N1 Ag1 127.7(9) . . ? C14 O1 C31 117.1(11) . . ? N2 C3 C4 108.5(12) . . ? N2 C3 C11 121.2(14) . . ? C4 C3 C11 130.3(14) . . ? C6 N3 C10 117.0(14) . . ? C6 N3 Ag1 110.4(10) . . ? C10 N3 Ag1 131.5(12) . . ? C3 C4 C5 105.6(12) . . ? C3 C4 H4A 127.2 . . ? C5 C4 H4A 127.2 . . ? C19 N4 N5 102.3(11) . . ? C19 N4 Ag1 115.1(10) . . ? N5 N4 Ag1 142.5(9) . . ? N1 C5 C4 109.7(13) . . ? N1 C5 C6 120.3(13) . . ? C4 C5 C6 129.5(14) . . ? C28 O5 C43 117.5(11) . . ? N3 C6 C7 124.5(15) . . ? N3 C6 C5 115.6(14) . . ? C7 C6 C5 119.9(16) . . ? C20 N6 C24 117.2(13) . . ? C20 N6 Ag1 119.6(9) . . ? C24 N6 Ag1 121.8(9) . . ? C6 C7 C8 116.7(16) . . ? C6 C7 H7A 121.6 . . ? C8 C7 H7A 121.6 . . ? O3 N7 O4 119.1(18) . . ? O3 N7 O2 122.2(15) . . ? O4 N7 O2 118.4(17) . . ? C9 C8 C7 122.5(15) . . ? C9 C8 H8A 118.8 . . ? C7 C8 H8A 118.8 . . ? C8 C9 C10 118.7(16) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C9 C10 N3 120.6(15) . . ? C9 C10 H10A 119.7 . . ? N3 C10 H10A 119.7 . . ? C16 C11 C12 116.4(13) . . ? C16 C11 C3 121.9(13) . . ? C12 C11 C3 121.6(14) . . ? C13 C12 C11 120.3(14) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 122.9(14) . . ? C12 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? O1 C14 C13 117.6(14) . . ? O1 C14 C15 124.5(16) . . ? C13 C14 C15 117.8(14) . . ? C16 C15 C14 119.5(13) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C11 123.1(13) . . ? C15 C16 H16A 118.5 . . ? C11 C16 H16A 118.5 . . ? N5 C17 C18 103.9(13) . . ? N5 C17 C25 124.6(13) . . ? C18 C17 C25 131.4(14) . . ? C19 C18 C17 105.4(12) . . ? C19 C18 H18A 127.3 . . ? C17 C18 H18A 127.3 . . ? N4 C19 C18 112.8(12) . . ? N4 C19 C20 116.3(14) . . ? C18 C19 C20 130.8(14) . . ? N6 C20 C21 123.7(14) . . ? N6 C20 C19 117.6(13) . . ? C21 C20 C19 118.7(15) . . ? C22 C21 C20 116.6(14) . . ? C22 C21 H21A 121.7 . . ? C20 C21 H21A 121.7 . . ? C23 C22 C21 121.0(14) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 116.8(14) . . ? C22 C23 H23A 121.6 . . ? C24 C23 H23A 121.6 . . ? N6 C24 C23 124.5(13) . . ? N6 C24 H24A 117.8 . . ? C23 C24 H24A 117.8 . . ? C30 C25 C26 116.6(14) . . ? C30 C25 C17 119.0(14) . . ? C26 C25 C17 124.2(14) . . ? C27 C26 C25 122.7(14) . . ? C27 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C26 C27 C28 121.1(14) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? O5 C28 C27 118.7(14) . . ? O5 C28 C29 122.9(14) . . ? C27 C28 C29 118.3(13) . . ? C30 C29 C28 117.7(14) . . ? C30 C29 H29A 121.2 . . ? C28 C29 H29A 121.2 . . ? C25 C30 C29 123.5(14) . . ? C25 C30 H30A 118.2 . . ? C29 C30 H30A 118.2 . . ? O5 C43 C44 107.3(11) . . ? O5 C43 H43A 110.3 . . ? C44 C43 H43A 110.3 . . ? O5 C43 H43B 110.3 . . ? C44 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? C43 C44 C45 109.7(11) . . ? C43 C44 H44A 109.7 . . ? C45 C44 H44A 109.7 . . ? C43 C44 H44B 109.7 . . ? C45 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? C46 C45 C44 113.2(11) . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? C44 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C47 115.3(11) . . ? C45 C46 H46A 108.5 . . ? C47 C46 H46A 108.5 . . ? C45 C46 H46B 108.5 . . ? C47 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C48 C47 C46 115.1(11) . . ? C48 C47 H47A 108.5 . . ? C46 C47 H47A 108.5 . . ? C48 C47 H47B 108.5 . . ? C46 C47 H47B 108.5 . . ? H47A C47 H47B 107.5 . . ? C47 C48 C49 114.2(12) . . ? C47 C48 H48A 108.7 . . ? C49 C48 H48A 108.7 . . ? C47 C48 H48B 108.7 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C48 C49 C50 115.1(12) . . ? C48 C49 H49A 108.5 . . ? C50 C49 H49A 108.5 . . ? C48 C49 H49B 108.5 . . ? C50 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C51 C50 C49 113.3(12) . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50B 108.9 . . ? C49 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 115.3(12) . . ? C52 C51 H51A 108.5 . . ? C50 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? C50 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C51 C52 C53 119.4(13) . . ? C51 C52 H52A 107.5 . . ? C53 C52 H52A 107.5 . . ? C51 C52 H52B 107.5 . . ? C53 C52 H52B 107.5 . . ? H52A C52 H52B 107.0 . . ? C52 C53 C54 117.5(13) . . ? C52 C53 H53A 107.9 . . ? C54 C53 H53A 107.9 . . ? C52 C53 H53B 107.9 . . ? C54 C53 H53B 107.9 . . ? H53A C53 H53B 107.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1 C31 C32 107.1(10) . . ? O1 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? O1 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? C37 C36 C35 114.4(10) . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C32 C33 C34 114.1(9) . . ? C32 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? C32 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C35 C34 C33 113.0(9) . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C34 C35 C36 114.3(9) . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C31 C32 C33 112.1(10) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C36 C37 C38 112.1(10) . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C39 C38 C37 111.2(10) . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C39 C40 C41 108.5(13) . . ? C39 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? C39 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? C38 C39 C40 118.2(12) . . ? C38 C39 H39A 107.8 . . ? C40 C39 H39A 107.8 . . ? C38 C39 H39B 107.8 . . ? C40 C39 H39B 107.8 . . ? H39A C39 H39B 107.1 . . ? C42 C41 C40 95.3(15) . . ? C42 C41 H41A 112.7 . . ? C40 C41 H41A 112.7 . . ? C42 C41 H41B 112.7 . . ? C40 C41 H41B 112.7 . . ? H41A C41 H41B 110.2 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Cl2 C55 Cl1 112.8(10) . . ? Cl2 C55 H55A 109.0 . . ? Cl1 C55 H55A 109.0 . . ? Cl2 C55 H55B 109.0 . . ? Cl1 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 N1 C5 4.6(14) . . . . ? C3 N2 N1 Ag1 -171.8(8) . . . . ? N6 Ag1 N1 C5 -54(2) . . . . ? N4 Ag1 N1 C5 -162.1(10) . . . . ? N3 Ag1 N1 C5 5.4(10) . . . . ? Ag1 Ag1 N1 C5 63.3(11) 2_666 . . . ? N6 Ag1 N1 N2 121.2(15) . . . . ? N4 Ag1 N1 N2 13.5(11) . . . . ? N3 Ag1 N1 N2 -179.0(11) . . . . ? Ag1 Ag1 N1 N2 -121.1(9) 2_666 . . . ? N1 N2 C3 C4 -1.1(15) . . . . ? N1 N2 C3 C11 178.5(10) . . . . ? N1 Ag1 N3 C6 -7.8(9) . . . . ? N6 Ag1 N3 C6 156.5(9) . . . . ? N4 Ag1 N3 C6 89(2) . . . . ? Ag1 Ag1 N3 C6 -111.4(10) 2_666 . . . ? N1 Ag1 N3 C10 -174.9(14) . . . . ? N6 Ag1 N3 C10 -10.7(13) . . . . ? N4 Ag1 N3 C10 -78(3) . . . . ? Ag1 Ag1 N3 C10 81.4(12) 2_666 . . . ? N2 C3 C4 C5 -2.7(15) . . . . ? C11 C3 C4 C5 177.8(13) . . . . ? C17 N5 N4 C19 -2.0(16) . . . . ? C17 N5 N4 Ag1 -176.3(11) . . . . ? N1 Ag1 N4 C19 169.1(9) . . . . ? N6 Ag1 N4 C19 6.9(9) . . . . ? N3 Ag1 N4 C19 77(2) . . . . ? Ag1 Ag1 N4 C19 -78.9(10) 2_666 . . . ? N1 Ag1 N4 N5 -16.9(15) . . . . ? N6 Ag1 N4 N5 -179.2(15) . . . . ? N3 Ag1 N4 N5 -109(2) . . . . ? Ag1 Ag1 N4 N5 95.0(14) 2_666 . . . ? N2 N1 C5 C4 -6.2(13) . . . . ? Ag1 N1 C5 C4 170.3(8) . . . . ? N2 N1 C5 C6 -178.9(11) . . . . ? Ag1 N1 C5 C6 -2.5(18) . . . . ? C3 C4 C5 N1 5.7(15) . . . . ? C3 C4 C5 C6 177.6(14) . . . . ? C10 N3 C6 C7 -1(2) . . . . ? Ag1 N3 C6 C7 -170.5(11) . . . . ? C10 N3 C6 C5 178.6(12) . . . . ? Ag1 N3 C6 C5 9.4(15) . . . . ? N1 C5 C6 N3 -6.2(19) . . . . ? C4 C5 C6 N3 -177.3(13) . . . . ? N1 C5 C6 C7 173.7(13) . . . . ? C4 C5 C6 C7 3(2) . . . . ? N1 Ag1 N6 C20 -122.6(15) . . . . ? N4 Ag1 N6 C20 -8.1(9) . . . . ? N3 Ag1 N6 C20 -177.0(10) . . . . ? Ag1 Ag1 N6 C20 121.1(10) 2_666 . . . ? N1 Ag1 N6 C24 71.1(19) . . . . ? N4 Ag1 N6 C24 -174.3(11) . . . . ? N3 Ag1 N6 C24 16.8(11) . . . . ? Ag1 Ag1 N6 C24 -45.1(11) 2_666 . . . ? N3 C6 C7 C8 -1(2) . . . . ? C5 C6 C7 C8 179.3(13) . . . . ? C6 C7 C8 C9 2(2) . . . . ? C7 C8 C9 C10 -2(3) . . . . ? C8 C9 C10 N3 0(2) . . . . ? C6 N3 C10 C9 2(2) . . . . ? Ag1 N3 C10 C9 168.4(11) . . . . ? N2 C3 C11 C16 -19(2) . . . . ? C4 C3 C11 C16 160.4(14) . . . . ? N2 C3 C11 C12 158.3(13) . . . . ? C4 C3 C11 C12 -22(2) . . . . ? C16 C11 C12 C13 -1(2) . . . . ? C3 C11 C12 C13 -178.7(12) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C31 O1 C14 C13 -175.9(13) . . . . ? C31 O1 C14 C15 5(2) . . . . ? C12 C13 C14 O1 -180.0(12) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? O1 C14 C15 C16 179.9(12) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C11 -1(2) . . . . ? C12 C11 C16 C15 1(2) . . . . ? C3 C11 C16 C15 178.7(12) . . . . ? N4 N5 C17 C18 -0.3(16) . . . . ? N4 N5 C17 C25 -178.6(12) . . . . ? N5 C17 C18 C19 2.4(15) . . . . ? C25 C17 C18 C19 -179.5(14) . . . . ? N5 N4 C19 C18 3.5(15) . . . . ? Ag1 N4 C19 C18 179.7(8) . . . . ? N5 N4 C19 C20 178.6(10) . . . . ? Ag1 N4 C19 C20 -5.2(15) . . . . ? C17 C18 C19 N4 -3.9(16) . . . . ? C17 C18 C19 C20 -178.0(13) . . . . ? C24 N6 C20 C21 -4(2) . . . . ? Ag1 N6 C20 C21 -170.7(9) . . . . ? C24 N6 C20 C19 175.4(12) . . . . ? Ag1 N6 C20 C19 8.6(16) . . . . ? N4 C19 C20 N6 -1.7(18) . . . . ? C18 C19 C20 N6 172.2(13) . . . . ? N4 C19 C20 C21 177.5(12) . . . . ? C18 C19 C20 C21 -8(2) . . . . ? N6 C20 C21 C22 0(2) . . . . ? C19 C20 C21 C22 -178.9(12) . . . . ? C20 C21 C22 C23 2(2) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C20 N6 C24 C23 6(2) . . . . ? Ag1 N6 C24 C23 172.2(10) . . . . ? C22 C23 C24 N6 -4(2) . . . . ? N5 C17 C25 C30 -9(2) . . . . ? C18 C17 C25 C30 173.3(14) . . . . ? N5 C17 C25 C26 165.3(14) . . . . ? C18 C17 C25 C26 -12(2) . . . . ? C30 C25 C26 C27 -1(2) . . . . ? C17 C25 C26 C27 -175.1(14) . . . . ? C25 C26 C27 C28 0(2) . . . . ? C43 O5 C28 C27 -172.2(12) . . . . ? C43 O5 C28 C29 8.0(19) . . . . ? C26 C27 C28 O5 179.0(13) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? O5 C28 C29 C30 -177.3(13) . . . . ? C27 C28 C29 C30 3(2) . . . . ? C26 C25 C30 C29 3(2) . . . . ? C17 C25 C30 C29 177.4(14) . . . . ? C28 C29 C30 C25 -4(2) . . . . ? C28 O5 C43 C44 176.9(11) . . . . ? O5 C43 C44 C45 -173.0(10) . . . . ? C43 C44 C45 C46 -176.7(11) . . . . ? C44 C45 C46 C47 178.7(11) . . . . ? C45 C46 C47 C48 179.0(12) . . . . ? C46 C47 C48 C49 -176.8(12) . . . . ? C47 C48 C49 C50 -174.4(12) . . . . ? C48 C49 C50 C51 179.4(12) . . . . ? C49 C50 C51 C52 -178.5(13) . . . . ? C50 C51 C52 C53 -179.2(12) . . . . ? C51 C52 C53 C54 -178.1(14) . . . . ? C14 O1 C31 C32 176.2(11) . . . . ? C32 C33 C34 C35 179.1(11) . . . . ? C33 C34 C35 C36 -179.9(10) . . . . ? C37 C36 C35 C34 177.7(12) . . . . ? O1 C31 C32 C33 175.9(11) . . . . ? C34 C33 C32 C31 179.2(10) . . . . ? C35 C36 C37 C38 179.5(11) . . . . ? C36 C37 C38 C39 172.7(13) . . . . ? C37 C38 C39 C40 -175.7(13) . . . . ? C41 C40 C39 C38 163.2(15) . . . . ? C39 C40 C41 C42 154.7(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O2 0.87 1.94 2.802(13) 169.3 . N5 H5 O2 0.86 2.00 2.777(14) 149.2 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.810 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.093 #=======================================================================END