# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wang Yaoyu' _publ_contact_author_email WYAOYU@NWU.EDU.CN loop_ _publ_author_name 'Wang Yaoyu' 'Jun-Cheng Jin' A.S.Lermontov E.Kh.Lermontova 'Qi-Zhen Shi' 'Wei-Hong Zhang' data_xb2462 _database_code_depnum_ccdc_archive 'CCDC 727388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H90 Ag12 O27, 5.18(H2 O)' _chemical_formula_sum 'C72 H100.36 Ag12 O32.18' _chemical_formula_weight 2775.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.480(4) _cell_length_b 13.463(3) _cell_length_c 18.374(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.220(4) _cell_angle_gamma 90.00 _cell_volume 4289.6(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2004 _cell_measurement_theta_min 2.245 _cell_measurement_theta_max 20.899 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 2.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5235 _exptl_absorpt_correction_T_max 0.6671 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23561 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.46 _reflns_number_total 8817 _reflns_number_gt 4114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0706P)^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 8817 _refine_ls_number_parameters 559 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.856 _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 0.24287(4) 0.52848(5) 0.63973(3) 0.0543(2) Uani 1 1 d . . . Ag2 Ag 0.51037(4) 0.53292(6) 0.57608(4) 0.0587(2) Uani 1 1 d . . . Ag3 Ag 0.29887(4) 0.61875(5) 0.81613(4) 0.0536(2) Uani 1 1 d . . . Ag4 Ag -0.05159(3) 0.42651(5) 0.45956(4) 0.0594(2) Uani 1 1 d . . . Ag5 Ag 0.40451(4) 0.54699(6) 0.70705(4) 0.0701(2) Uani 1 1 d . . . Ag6 Ag 0.19586(4) 0.72934(6) 0.69425(5) 0.0779(3) Uani 1 1 d . . . O1 O 0.5000 0.4021(10) 0.7500 0.147(5) Uani 1 2 d S . . H1B H 0.4956 0.3669 0.7867 0.176 Uiso 1 1 d R . . O2 O 0.4299(3) 0.4077(5) 0.5734(3) 0.0631(16) Uani 1 1 d . . . O3 O 0.1320(3) 0.4547(4) 0.5309(3) 0.0481(13) Uani 1 1 d . . . O5 O -0.1351(3) 0.2818(5) 0.4543(3) 0.0763(19) Uani 1 1 d . . . H5C H -0.1283 0.2247 0.4670 0.092 Uiso 1 1 d R . . H5D H -0.1760 0.3063 0.4494 0.092 Uiso 1 1 d R . . O6 O 0.4006(3) 0.3787(4) 0.4491(3) 0.0546(15) Uani 1 1 d . . . O8 O 0.2693(3) 0.4072(4) 0.7269(3) 0.0643(17) Uani 1 1 d . D . O9 O 0.2722(3) 0.3628(4) 1.0623(3) 0.0583(15) Uani 1 1 d . . . O10 O 0.3993(3) 0.3742(4) 1.1020(3) 0.0509(14) Uani 1 1 d . . . O11 O 0.3814(3) 0.7064(4) 0.7814(3) 0.0573(15) Uani 1 1 d . . . C1 C 0.3913(4) 0.3639(6) 0.5136(5) 0.045(2) Uani 1 1 d . . . C2 C 0.3270(4) 0.2970(5) 0.5165(4) 0.0395(18) Uani 1 1 d . . . C3 C 0.3472(4) 0.2459(6) 0.5946(4) 0.047(2) Uani 1 1 d . . . H3A H 0.3592 0.2951 0.6357 0.056 Uiso 1 1 calc R . . H3B H 0.3921 0.2039 0.6036 0.056 Uiso 1 1 calc R . . C4 C 0.3072(5) 0.2192(6) 0.4520(5) 0.053(2) Uani 1 1 d . . . H4A H 0.3511 0.1759 0.4594 0.064 Uiso 1 1 calc R . . H4B H 0.2952 0.2519 0.4021 0.064 Uiso 1 1 calc R . . C5 C 0.2567(4) 0.3645(5) 0.5041(4) 0.0379(18) Uani 1 1 d . . . H5A H 0.2444 0.3986 0.4548 0.046 Uiso 1 1 calc R . . H5B H 0.2691 0.4143 0.5447 0.046 Uiso 1 1 calc R . . C6 C 0.2377(5) 0.1579(6) 0.4532(4) 0.052(2) Uani 1 1 d . . . H6 H 0.2252 0.1078 0.4120 0.063 Uiso 1 1 calc R . . C7 C 0.1675(4) 0.2282(6) 0.4395(5) 0.049(2) Uani 1 1 d . . . H7A H 0.1561 0.2622 0.3903 0.059 Uiso 1 1 calc R . . H7B H 0.1225 0.1896 0.4377 0.059 Uiso 1 1 calc R . . C8 C 0.2585(5) 0.1061(6) 0.5319(5) 0.059(2) Uani 1 1 d . . . H8A H 0.2154 0.0660 0.5333 0.071 Uiso 1 1 calc R . . H8B H 0.3024 0.0627 0.5398 0.071 Uiso 1 1 calc R . . C9 C 0.1856(4) 0.3037(6) 0.5048(4) 0.0390(18) Uani 1 1 d . E . C10 C 0.2774(5) 0.1823(6) 0.5948(5) 0.052(2) Uani 1 1 d . . . H10 H 0.2903 0.1486 0.6450 0.063 Uiso 1 1 calc R . . C11 C 0.2069(4) 0.2486(6) 0.5827(4) 0.049(2) Uani 1 1 d . . . H11A H 0.2180 0.2964 0.6246 0.059 Uiso 1 1 calc R . . H11B H 0.1637 0.2082 0.5834 0.059 Uiso 1 1 calc R . . C12 C 0.1178(4) 0.3715(7) 0.4986(4) 0.045(2) Uani 1 1 d . . . C13 C 0.3266(5) 0.4020(6) 0.7858(5) 0.049(2) Uani 1 1 d . . . C14 C 0.3302(4) 0.3197(6) 0.8437(4) 0.046(2) Uani 1 1 d . D . C15 C 0.3305(4) 0.3692(5) 0.9191(4) 0.0401(18) Uani 1 1 d . . . H15A H 0.2832 0.4068 0.9091 0.048 Uiso 1 1 calc R D . H15B H 0.3735 0.4150 0.9373 0.048 Uiso 1 1 calc R . . C16 C 0.2628(5) 0.2477(6) 0.8146(4) 0.049(2) Uani 1 1 d . . . H16A H 0.2146 0.2839 0.8015 0.059 Uiso 1 1 calc R D . H16B H 0.2641 0.2146 0.7681 0.059 Uiso 1 1 calc R . . C17 C 0.4061(5) 0.2595(6) 0.8609(5) 0.052(2) Uani 1 1 d . . . H17A H 0.4064 0.2270 0.8139 0.062 Uiso 1 1 calc R D . H17B H 0.4500 0.3041 0.8784 0.062 Uiso 1 1 calc R . . C18 C 0.4122(5) 0.1821(7) 0.9231(5) 0.060(2) Uani 1 1 d . D . H18 H 0.4605 0.1452 0.9341 0.072 Uiso 1 1 calc R . . C19 C 0.3443(6) 0.1101(7) 0.8939(6) 0.074(3) Uani 1 1 d . . . H19A H 0.3480 0.0599 0.9328 0.089 Uiso 1 1 calc R D . H19B H 0.3448 0.0772 0.8471 0.089 Uiso 1 1 calc R . . C20 C 0.2676(5) 0.1712(6) 0.8765(5) 0.058(2) Uani 1 1 d . D . H20 H 0.2234 0.1262 0.8578 0.069 Uiso 1 1 calc R . . C21 C 0.2678(5) 0.2212(6) 0.9510(4) 0.050(2) Uani 1 1 d . . . H21A H 0.2699 0.1711 0.9896 0.060 Uiso 1 1 calc R D . H21B H 0.2206 0.2590 0.9409 0.060 Uiso 1 1 calc R . . C22 C 0.3372(4) 0.2904(6) 0.9822(4) 0.0421(19) Uani 1 1 d . D . C23 C 0.4110(4) 0.2311(6) 0.9978(5) 0.051(2) Uani 1 1 d . . . H23A H 0.4145 0.1805 1.0364 0.061 Uiso 1 1 calc R D . H23B H 0.4552 0.2748 1.0181 0.061 Uiso 1 1 calc R . . C24 C 0.3359(5) 0.3457(6) 1.0545(4) 0.0428(19) Uani 1 1 d . . . C25 C 0.1367(4) 0.5430(7) 0.7562(5) 0.051(2) Uani 1 1 d . . . C26 C 0.0696(4) 0.4750(6) 0.7536(4) 0.0437(19) Uani 1 1 d . . . C27 C 0.0473(4) 0.4079(6) 0.6816(4) 0.050(2) Uani 1 1 d . . . H27A H 0.0344 0.4484 0.6351 0.061 Uiso 1 1 calc R . . H27B H 0.0905 0.3656 0.6837 0.061 Uiso 1 1 calc R . . C28 C 0.0000 0.5411(8) 0.7500 0.046(3) Uani 1 2 d S . . H28A H 0.0137 0.5834 0.7955 0.055 Uiso 1 1 d R . . C30 C 0.0904(5) 0.4115(7) 0.8253(5) 0.059(2) Uani 1 1 d . . . H30A H 0.1045 0.4534 0.8710 0.071 Uiso 1 1 calc R . . H30B H 0.1342 0.3698 0.8286 0.071 Uiso 1 1 calc R . . C31 C -0.0200(5) 0.3458(6) 0.6787(5) 0.056(2) Uani 1 1 d . . . H31 H -0.0340 0.3035 0.6325 0.067 Uiso 1 1 calc R . . C32 C 0.0000 0.2804(9) 0.7500 0.069(4) Uani 1 2 d S . . H32A H -0.0435 0.2382 0.7470 0.082 Uiso 1 1 d R . . C33 C 0.3657(5) 0.7897(7) 0.7514(5) 0.052(2) Uani 1 1 d . . . C34 C 0.4304(4) 0.8546(5) 0.7484(4) 0.0412(18) Uani 1 1 d . . . C35 C 0.5000 0.7921(8) 0.7500 0.047(3) Uani 1 2 d S . . H35A H 0.5152 0.7496 0.7954 0.057 Uiso 1 1 d R . . C36 C 0.4575(5) 0.9229(6) 0.8218(5) 0.058(2) Uani 1 1 d . . . H36A H 0.4147 0.9633 0.8235 0.070 Uiso 1 1 calc R . . H36B H 0.4746 0.8822 0.8682 0.070 Uiso 1 1 calc R . . C37 C 0.4082(5) 0.9215(7) 0.6778(5) 0.064(2) Uani 1 1 d . . . H37A H 0.3646 0.9625 0.6766 0.076 Uiso 1 1 calc R . . H37B H 0.3929 0.8814 0.6311 0.076 Uiso 1 1 calc R . . C38 C 0.4774(6) 0.9891(7) 0.6803(6) 0.077(3) Uani 1 1 d . . . H38 H 0.4616 1.0310 0.6339 0.092 Uiso 1 1 calc R . . C39 C 0.5000 1.0546(9) 0.7500 0.093(6) Uani 1 2 d S . . H39A H 0.5427 1.0968 0.7506 0.111 Uiso 1 1 d R . . O15 O 0.0703(14) 0.0876(18) 0.960(2) 0.40(2) Uani 0.65 1 d P . . H15D H 0.0442 0.1065 0.9838 0.479 Uiso 0.65 1 d PR . . H15C H 0.1149 0.0770 0.9836 0.479 Uiso 0.65 1 d PR . . O18 O 0.039(3) -0.010(4) 0.806(3) 0.33(3) Uiso 0.35 1 d P . . H18C H 0.0459 0.0149 0.8471 0.398 Uiso 0.35 1 d PR . . H18D H 0.0205 -0.0638 0.7936 0.398 Uiso 0.35 1 d PR . . O16 O 0.9606(8) 0.8000(10) 0.8308(9) 0.137(5) Uani 0.59 1 d PU A 1 H16C H 0.9891 0.7666 0.8646 0.164 Uiso 0.59 1 d PR A 1 H16D H 0.9384 0.7485 0.8170 0.164 Uiso 0.59 1 d PR A 1 O17 O 0.8326(11) 0.9842(14) 0.8017(12) 0.281(9) Uani 0.82 1 d PU B 1 H17D H 0.8062 0.9707 0.7582 0.337 Uiso 0.82 1 d PR B 1 H17C H 0.8201 0.9681 0.8376 0.337 Uiso 0.82 1 d PR B 1 O17A O 0.889(3) 0.892(3) 0.820(3) 0.117(15) Uiso 0.18 1 d P C 2 H17E H 0.8780 0.8951 0.7740 0.140 Uiso 0.18 1 d PR C 2 H17F H 0.9035 0.9148 0.8628 0.140 Uiso 0.18 1 d PR C 2 O14A O 0.1965(12) 0.5330(12) 0.8185(12) 0.041(5) Uiso 0.45 1 d P . 2 O14 O 0.1897(8) 0.5661(11) 0.8150(9) 0.040(4) Uani 0.55 1 d PU . 1 O7 O 0.3902(10) 0.4529(13) 0.7989(10) 0.057(4) Uani 0.59 1 d P D 1 O7A O 0.3724(13) 0.4713(18) 0.8057(15) 0.036(6) Uiso 0.41 1 d P . 2 O4 O 0.0504(8) 0.3322(11) 0.4734(8) 0.067(4) Uani 0.63 1 d PU E 1 O4A O 0.0522(12) 0.3472(14) 0.4511(10) 0.024(5) Uiso 0.37 1 d P E 2 O13 O 0.1264(9) 0.6064(12) 0.6938(11) 0.053(4) Uani 0.52 1 d P . 1 O13A O 0.1342(11) 0.5719(12) 0.6909(12) 0.036(5) Uiso 0.48 1 d P . 2 O12 O 0.2962(9) 0.8282(12) 0.7329(11) 0.066(4) Uani 0.62 1 d P . 1 O12A O 0.303(2) 0.816(2) 0.7100(17) 0.058(9) Uiso 0.38 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0438(4) 0.0772(5) 0.0417(4) 0.0101(3) 0.0148(3) 0.0003(3) Ag2 0.0366(4) 0.0936(6) 0.0493(4) 0.0010(4) 0.0191(3) -0.0088(4) Ag3 0.0399(4) 0.0657(5) 0.0560(4) -0.0005(3) 0.0177(3) -0.0031(3) Ag4 0.0308(3) 0.0732(5) 0.0711(5) -0.0011(4) 0.0135(3) 0.0034(3) Ag5 0.0505(4) 0.1081(7) 0.0506(4) 0.0237(4) 0.0160(4) -0.0008(4) Ag6 0.0634(5) 0.0764(6) 0.0818(6) 0.0092(4) 0.0096(4) -0.0100(4) O1 0.173(13) 0.163(12) 0.133(11) 0.000 0.089(10) 0.000 O2 0.056(4) 0.089(5) 0.051(4) -0.008(3) 0.027(3) -0.020(3) O3 0.032(3) 0.051(4) 0.060(4) -0.006(3) 0.013(3) 0.004(3) O5 0.048(4) 0.094(5) 0.090(5) 0.014(4) 0.027(4) -0.001(3) O6 0.038(3) 0.079(4) 0.047(4) 0.006(3) 0.015(3) -0.003(3) O8 0.067(4) 0.075(4) 0.039(3) 0.006(3) 0.003(3) -0.003(3) O9 0.040(3) 0.081(4) 0.055(4) -0.025(3) 0.019(3) -0.004(3) O10 0.038(3) 0.080(4) 0.038(3) -0.004(3) 0.017(3) 0.001(3) O11 0.056(4) 0.060(4) 0.063(4) 0.012(3) 0.028(3) 0.006(3) C1 0.025(4) 0.058(6) 0.048(5) -0.005(4) 0.008(4) 0.001(4) C2 0.038(4) 0.042(5) 0.044(5) -0.002(4) 0.021(4) 0.002(4) C3 0.036(4) 0.061(5) 0.042(5) 0.003(4) 0.011(4) 0.009(4) C4 0.057(5) 0.057(6) 0.058(5) 0.012(4) 0.035(5) 0.012(4) C5 0.032(4) 0.046(5) 0.038(4) -0.003(4) 0.014(4) -0.002(3) C6 0.070(6) 0.049(5) 0.039(5) -0.004(4) 0.020(4) 0.000(5) C7 0.044(5) 0.053(5) 0.045(5) 0.001(4) 0.009(4) -0.008(4) C8 0.061(6) 0.044(5) 0.078(7) 0.005(5) 0.031(5) -0.001(4) C9 0.026(4) 0.050(5) 0.040(5) 0.002(4) 0.012(3) 0.002(3) C10 0.052(5) 0.062(6) 0.045(5) 0.009(4) 0.019(4) 0.005(4) C11 0.043(5) 0.060(5) 0.050(5) 0.010(4) 0.024(4) 0.002(4) C12 0.036(5) 0.060(6) 0.034(5) 0.014(4) 0.007(4) 0.004(4) C13 0.054(6) 0.055(6) 0.035(5) -0.002(4) 0.011(5) 0.002(5) C14 0.050(5) 0.043(5) 0.043(5) -0.003(4) 0.015(4) 0.004(4) C15 0.051(5) 0.043(5) 0.025(4) -0.005(3) 0.013(4) 0.003(4) C16 0.062(6) 0.046(5) 0.040(5) -0.009(4) 0.019(4) 0.001(4) C17 0.060(6) 0.048(5) 0.056(5) 0.000(4) 0.031(5) 0.013(4) C18 0.046(5) 0.069(6) 0.071(6) 0.013(5) 0.029(5) 0.027(5) C19 0.101(8) 0.048(6) 0.096(8) 0.010(5) 0.064(7) 0.013(6) C20 0.070(6) 0.051(5) 0.051(5) 0.000(4) 0.020(5) -0.010(5) C21 0.049(5) 0.053(5) 0.054(5) -0.002(4) 0.024(4) 0.002(4) C22 0.041(5) 0.052(5) 0.034(4) 0.002(4) 0.014(4) 0.002(4) C23 0.042(5) 0.060(5) 0.055(5) 0.006(4) 0.021(4) 0.019(4) C24 0.039(5) 0.052(5) 0.034(5) 0.005(4) 0.010(4) 0.003(4) C25 0.024(4) 0.090(7) 0.045(5) -0.008(5) 0.019(4) 0.001(4) C26 0.035(4) 0.062(5) 0.041(4) -0.007(4) 0.021(4) -0.002(4) C27 0.035(4) 0.069(6) 0.053(5) -0.001(5) 0.023(4) 0.004(4) C28 0.031(6) 0.058(8) 0.044(7) 0.000 0.009(5) 0.000 C30 0.049(5) 0.082(7) 0.052(5) 0.009(5) 0.023(4) 0.029(5) C31 0.056(5) 0.064(6) 0.052(5) -0.014(5) 0.024(5) -0.007(5) C32 0.082(10) 0.058(9) 0.071(9) 0.000 0.032(8) 0.000 C33 0.051(6) 0.053(6) 0.052(6) -0.007(5) 0.015(5) 0.002(5) C34 0.045(5) 0.033(4) 0.045(5) 0.000(4) 0.015(4) 0.006(4) C35 0.055(7) 0.037(7) 0.054(7) 0.000 0.025(6) 0.000 C36 0.070(6) 0.055(5) 0.048(5) -0.013(4) 0.018(5) 0.002(5) C37 0.052(5) 0.072(6) 0.066(6) 0.012(5) 0.018(5) 0.010(5) C38 0.077(7) 0.059(7) 0.108(9) 0.053(6) 0.049(6) 0.020(6) C39 0.132(15) 0.025(8) 0.153(16) 0.000 0.089(13) 0.000 O15 0.22(3) 0.23(2) 0.71(7) 0.25(3) 0.12(3) 0.05(2) O16 0.120(8) 0.089(7) 0.160(9) 0.010(7) -0.006(7) -0.010(7) O17 0.266(12) 0.254(12) 0.306(12) -0.009(9) 0.078(9) -0.007(9) O14 0.030(6) 0.043(7) 0.040(6) -0.002(6) 0.002(4) -0.012(6) O7 0.058(10) 0.062(10) 0.047(8) 0.014(6) 0.013(7) 0.013(8) O4 0.044(6) 0.079(8) 0.077(8) 0.005(6) 0.020(6) -0.009(5) O13 0.026(7) 0.050(10) 0.073(10) -0.004(9) 0.003(6) -0.004(8) O12 0.041(7) 0.064(9) 0.094(12) -0.010(8) 0.025(8) 0.001(5) _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 O8 2.220(6) . ? Ag1 O9 2.235(5) 4_565 ? Ag1 O3 2.520(5) . ? Ag1 O13A 2.560(18) . ? Ag1 Ag5 2.8215(11) . ? Ag1 Ag6 3.1101(12) . ? Ag1 Ag3 3.2763(11) . ? Ag2 O6 2.206(5) 3_666 ? Ag2 O2 2.237(6) . ? Ag2 O10 2.585(5) 4_565 ? Ag2 Ag2 2.8299(14) 3_666 ? Ag3 O14 2.132(14) . ? Ag3 O11 2.190(5) . ? Ag3 O14A 2.23(2) . ? Ag3 O7A 2.45(2) . ? Ag3 O6 2.516(5) 4_566 ? Ag3 Ag6 2.8123(11) . ? Ag4 O4 2.213(15) . ? Ag4 O3 2.231(5) 3_566 ? Ag4 O4A 2.25(2) . ? Ag4 O5 2.467(6) . ? Ag4 Ag4 2.7930(14) 3_566 ? Ag5 O10 2.176(5) 4_565 ? Ag5 O7 2.197(17) . ? Ag5 O7A 2.33(2) . ? Ag5 O1 2.565(10) . ? Ag5 Ag5 3.3312(15) 2_656 ? Ag6 O13 2.093(16) . ? Ag6 O12 2.192(16) . ? Ag6 O12A 2.23(3) . ? Ag6 O13A 2.397(18) . ? Ag6 O5 2.572(6) 3_566 ? O1 Ag5 2.565(10) 2_656 ? O1 H1B 0.8500 . ? O2 C1 1.233(8) . ? O3 C12 1.252(9) . ? O3 Ag4 2.231(5) 3_566 ? O5 Ag6 2.572(6) 3_566 ? O5 H5C 0.8001 . ? O5 H5D 0.7997 . ? O6 C1 1.271(9) . ? O6 Ag2 2.206(5) 3_666 ? O6 Ag3 2.516(5) 4_565 ? O8 C13 1.227(9) . ? O9 C24 1.254(8) . ? O9 Ag1 2.235(5) 4_566 ? O10 C24 1.255(8) . ? O10 Ag5 2.176(5) 4_566 ? O10 Ag2 2.585(5) 4_566 ? O11 C33 1.240(9) . ? C1 C2 1.508(10) . ? C2 C3 1.516(10) . ? C2 C4 1.529(10) . ? C2 C5 1.536(9) . ? C3 C10 1.550(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C6 1.534(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C9 1.553(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C8 1.530(10) . ? C6 C7 1.555(11) . ? C6 H6 0.9800 . ? C7 C9 1.519(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.493(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.521(10) . ? C9 C11 1.537(10) . ? C10 C11 1.531(10) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O4A 1.27(2) . ? C12 O4 1.284(15) . ? C13 O7A 1.23(3) . ? C13 O7 1.309(19) . ? C13 C14 1.522(11) . ? C14 C16 1.522(11) . ? C14 C15 1.536(9) . ? C14 C17 1.553(10) . ? C15 C22 1.544(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C20 1.515(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.521(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.529(12) . ? C18 C23 1.529(11) . ? C18 H18 0.9800 . ? C19 C20 1.573(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.524(10) . ? C20 H20 0.9800 . ? C21 C22 1.526(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.520(10) . ? C22 C24 1.531(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 O14 1.220(16) . ? C25 O13A 1.25(2) . ? C25 O14A 1.29(2) . ? C25 O13 1.389(18) . ? C25 C26 1.529(10) . ? C26 C30 1.504(11) . ? C26 C27 1.537(10) . ? C26 C28 1.547(9) . ? C27 C31 1.484(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C26 1.547(9) 2_556 ? C28 H28A 0.9701 . ? C30 C31 1.554(11) 2_556 ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.514(10) . ? C31 C30 1.554(11) 2_556 ? C31 H31 0.9800 . ? C32 C31 1.514(10) 2_556 ? C32 H32A 0.9701 . ? C33 O12A 1.20(3) . ? C33 O12 1.314(18) . ? C33 C34 1.497(11) . ? C34 C37 1.515(11) . ? C34 C35 1.528(9) . ? C34 C36 1.564(10) . ? C35 C34 1.528(9) 2_656 ? C35 H35A 0.9699 . ? C36 C38 1.509(11) 2_656 ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.557(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.490(12) . ? C38 C36 1.509(11) 2_656 ? C38 H38 0.9800 . ? C39 C38 1.490(12) 2_656 ? C39 H39A 0.9701 . ? O15 H15D 0.8002 . ? O15 H15C 0.8001 . ? O18 H18C 0.7999 . ? O18 H18D 0.8000 . ? O16 H16C 0.8001 . ? O16 H16D 0.8002 . ? O17 H17D 0.8000 . ? O17 H17C 0.8003 . ? O17A H17E 0.8002 . ? O17A H17F 0.7999 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ag1 O9 154.1(2) . 4_565 ? O8 Ag1 O3 101.46(19) . . ? O9 Ag1 O3 93.58(19) 4_565 . ? O8 Ag1 O13A 84.7(4) . . ? O9 Ag1 O13A 118.5(4) 4_565 . ? O3 Ag1 O13A 81.7(5) . . ? O8 Ag1 Ag5 79.21(15) . . ? O9 Ag1 Ag5 76.60(13) 4_565 . ? O3 Ag1 Ag5 146.08(12) . . ? O13A Ag1 Ag5 131.6(5) . . ? O8 Ag1 Ag6 115.05(15) . . ? O9 Ag1 Ag6 77.99(15) 4_565 . ? O3 Ag1 Ag6 110.94(12) . . ? O13A Ag1 Ag6 48.8(4) . . ? Ag5 Ag1 Ag6 98.81(3) . . ? O8 Ag1 Ag3 69.12(15) . . ? O9 Ag1 Ag3 108.89(15) 4_565 . ? O3 Ag1 Ag3 145.43(12) . . ? O13A Ag1 Ag3 64.7(5) . . ? Ag5 Ag1 Ag3 66.98(2) . . ? Ag6 Ag1 Ag3 52.17(2) . . ? O6 Ag2 O2 160.1(2) 3_666 . ? O6 Ag2 O10 118.36(19) 3_666 4_565 ? O2 Ag2 O10 78.75(19) . 4_565 ? O6 Ag2 Ag2 79.50(14) 3_666 3_666 ? O2 Ag2 Ag2 83.11(15) . 3_666 ? O10 Ag2 Ag2 119.25(12) 4_565 3_666 ? O14 Ag3 O11 158.2(4) . . ? O14 Ag3 O14A 11.9(7) . . ? O11 Ag3 O14A 164.9(6) . . ? O14 Ag3 O7A 106.2(7) . . ? O11 Ag3 O7A 87.3(6) . . ? O14A Ag3 O7A 94.5(7) . . ? O14 Ag3 O6 113.6(4) . 4_566 ? O11 Ag3 O6 85.04(19) . 4_566 ? O14A Ag3 O6 110.0(6) . 4_566 ? O7A Ag3 O6 80.7(6) . 4_566 ? O14 Ag3 Ag6 77.9(4) . . ? O11 Ag3 Ag6 80.26(15) . . ? O14A Ag3 Ag6 86.8(5) . . ? O7A Ag3 Ag6 127.4(6) . . ? O6 Ag3 Ag6 147.03(13) 4_566 . ? O14 Ag3 Ag1 83.8(4) . . ? O11 Ag3 Ag1 85.71(15) . . ? O14A Ag3 Ag1 81.2(5) . . ? O7A Ag3 Ag1 67.4(6) . . ? O6 Ag3 Ag1 147.18(12) 4_566 . ? Ag6 Ag3 Ag1 60.87(3) . . ? O4 Ag4 O3 165.1(4) . 3_566 ? O4 Ag4 O4A 12.0(6) . . ? O3 Ag4 O4A 162.5(5) 3_566 . ? O4 Ag4 O5 92.7(4) . . ? O3 Ag4 O5 98.3(2) 3_566 . ? O4A Ag4 O5 99.2(5) . . ? O4 Ag4 Ag4 87.0(4) . 3_566 ? O3 Ag4 Ag4 78.53(14) 3_566 3_566 ? O4A Ag4 Ag4 86.1(5) . 3_566 ? O5 Ag4 Ag4 152.03(14) . 3_566 ? O10 Ag5 O7 169.2(5) 4_565 . ? O10 Ag5 O7A 163.6(6) 4_565 . ? O7 Ag5 O7A 11.3(8) . . ? O10 Ag5 O1 117.31(15) 4_565 . ? O7 Ag5 O1 65.0(4) . . ? O7A Ag5 O1 76.2(5) . . ? O10 Ag5 Ag1 86.48(14) 4_565 . ? O7 Ag5 Ag1 84.0(4) . . ? O7A Ag5 Ag1 77.7(6) . . ? O1 Ag5 Ag1 125.4(2) . . ? O10 Ag5 Ag5 97.76(14) 4_565 2_656 ? O7 Ag5 Ag5 91.4(4) . 2_656 ? O7A Ag5 Ag5 98.3(6) . 2_656 ? O1 Ag5 Ag5 49.5(2) . 2_656 ? Ag1 Ag5 Ag5 174.55(2) . 2_656 ? O13 Ag6 O12 158.5(7) . . ? O13 Ag6 O12A 158.5(10) . . ? O12 Ag6 O12A 13.1(8) . . ? O13 Ag6 O13A 10.0(7) . . ? O12 Ag6 O13A 152.4(6) . . ? O12A Ag6 O13A 149.2(9) . . ? O13 Ag6 O5 84.7(5) . 3_566 ? O12 Ag6 O5 112.9(5) . 3_566 ? O12A Ag6 O5 102.1(7) . 3_566 ? O13A Ag6 O5 83.8(5) . 3_566 ? O13 Ag6 Ag3 80.2(5) . . ? O12 Ag6 Ag3 78.4(5) . . ? O12A Ag6 Ag3 81.2(9) . . ? O13A Ag6 Ag3 74.8(5) . . ? O5 Ag6 Ag3 137.84(15) 3_566 . ? O13 Ag6 Ag1 63.2(5) . . ? O12 Ag6 Ag1 109.4(4) . . ? O12A Ag6 Ag1 99.3(7) . . ? O13A Ag6 Ag1 53.5(4) . . ? O5 Ag6 Ag1 71.07(14) 3_566 . ? Ag3 Ag6 Ag1 66.96(3) . . ? Ag5 O1 Ag5 81.0(4) 2_656 . ? Ag5 O1 H1B 115.1 2_656 . ? Ag5 O1 H1B 115.1 . . ? C1 O2 Ag2 123.8(5) . . ? C12 O3 Ag4 130.0(5) . 3_566 ? C12 O3 Ag1 135.1(5) . . ? Ag4 O3 Ag1 92.1(2) 3_566 . ? Ag4 O5 Ag6 97.2(2) . 3_566 ? Ag4 O5 H5C 135.4 . . ? Ag6 O5 H5C 102.7 3_566 . ? Ag4 O5 H5D 103.4 . . ? Ag6 O5 H5D 81.7 3_566 . ? H5C O5 H5D 118.6 . . ? C1 O6 Ag2 129.1(5) . 3_666 ? C1 O6 Ag3 127.7(5) . 4_565 ? Ag2 O6 Ag3 98.62(19) 3_666 4_565 ? C13 O8 Ag1 125.9(6) . . ? C24 O9 Ag1 129.5(5) . 4_566 ? C24 O10 Ag5 120.7(5) . 4_566 ? C24 O10 Ag2 129.0(5) . 4_566 ? Ag5 O10 Ag2 97.6(2) 4_566 4_566 ? C33 O11 Ag3 122.5(5) . . ? O2 C1 O6 122.2(7) . . ? O2 C1 C2 118.4(7) . . ? O6 C1 C2 119.3(7) . . ? C1 C2 C3 111.4(6) . . ? C1 C2 C4 111.2(6) . . ? C3 C2 C4 109.8(6) . . ? C1 C2 C5 106.1(6) . . ? C3 C2 C5 109.2(6) . . ? C4 C2 C5 109.1(6) . . ? C2 C3 C10 108.6(6) . . ? C2 C3 H3A 110.0 . . ? C10 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? C10 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C2 C4 C6 109.5(6) . . ? C2 C4 H4A 109.8 . . ? C6 C4 H4A 109.8 . . ? C2 C4 H4B 109.8 . . ? C6 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C2 C5 C9 111.2(6) . . ? C2 C5 H5A 109.4 . . ? C9 C5 H5A 109.4 . . ? C2 C5 H5B 109.4 . . ? C9 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C8 C6 C4 108.8(7) . . ? C8 C6 C7 110.6(6) . . ? C4 C6 C7 109.0(6) . . ? C8 C6 H6 109.5 . . ? C4 C6 H6 109.5 . . ? C7 C6 H6 109.5 . . ? C9 C7 C6 109.7(6) . . ? C9 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C9 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C10 C8 C6 109.5(7) . . ? C10 C8 H8A 109.8 . . ? C6 C8 H8A 109.8 . . ? C10 C8 H8B 109.8 . . ? C6 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C7 C9 C12 113.0(6) . . ? C7 C9 C11 109.1(6) . . ? C12 C9 C11 107.4(6) . . ? C7 C9 C5 107.6(6) . . ? C12 C9 C5 111.1(6) . . ? C11 C9 C5 108.5(6) . . ? C8 C10 C11 109.1(7) . . ? C8 C10 C3 110.5(6) . . ? C11 C10 C3 110.2(7) . . ? C8 C10 H10 109.0 . . ? C11 C10 H10 109.0 . . ? C3 C10 H10 109.0 . . ? C10 C11 C9 110.4(6) . . ? C10 C11 H11A 109.6 . . ? C9 C11 H11A 109.6 . . ? C10 C11 H11B 109.6 . . ? C9 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O3 C12 O4A 123.4(11) . . ? O3 C12 O4 123.9(10) . . ? O4A C12 O4 21.1(10) . . ? O3 C12 C9 118.0(7) . . ? O4A C12 C9 117.7(11) . . ? O4 C12 C9 116.8(10) . . ? O7A C13 O8 121.0(14) . . ? O7A C13 O7 20.7(13) . . ? O8 C13 O7 125.3(10) . . ? O7A C13 C14 119.1(14) . . ? O8 C13 C14 118.3(8) . . ? O7 C13 C14 115.7(10) . . ? C16 C14 C13 112.6(7) . . ? C16 C14 C15 109.9(6) . . ? C13 C14 C15 107.4(6) . . ? C16 C14 C17 108.1(6) . . ? C13 C14 C17 109.9(6) . . ? C15 C14 C17 108.8(6) . . ? C14 C15 C22 110.7(6) . . ? C14 C15 H15A 109.5 . . ? C22 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C22 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C20 C16 C14 109.9(7) . . ? C20 C16 H16A 109.7 . . ? C14 C16 H16A 109.7 . . ? C20 C16 H16B 109.7 . . ? C14 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C14 109.7(6) . . ? C18 C17 H17A 109.7 . . ? C14 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? C14 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C17 C18 C19 109.4(7) . . ? C17 C18 C23 111.0(7) . . ? C19 C18 C23 108.9(7) . . ? C17 C18 H18 109.2 . . ? C19 C18 H18 109.2 . . ? C23 C18 H18 109.2 . . ? C18 C19 C20 108.2(7) . . ? C18 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? C18 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C16 C20 C21 110.9(7) . . ? C16 C20 C19 108.8(7) . . ? C21 C20 C19 109.1(7) . . ? C16 C20 H20 109.4 . . ? C21 C20 H20 109.4 . . ? C19 C20 H20 109.4 . . ? C20 C21 C22 110.3(6) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 109.5(7) . . ? C23 C22 C24 112.0(6) . . ? C21 C22 C24 111.0(6) . . ? C23 C22 C15 109.7(6) . . ? C21 C22 C15 107.4(6) . . ? C24 C22 C15 107.2(6) . . ? C22 C23 C18 110.3(6) . . ? C22 C23 H23A 109.6 . . ? C18 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C18 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? O9 C24 O10 123.5(7) . . ? O9 C24 C22 119.0(7) . . ? O10 C24 C22 117.5(7) . . ? O14 C25 O13A 121.6(13) . . ? O14 C25 O14A 20.9(11) . . ? O13A C25 O14A 128.3(14) . . ? O14 C25 O13 114.4(12) . . ? O13A C25 O13 20.7(11) . . ? O14A C25 O13 128.7(13) . . ? O14 C25 C26 125.0(10) . . ? O13A C25 C26 113.4(11) . . ? O14A C25 C26 113.6(11) . . ? O13 C25 C26 117.6(9) . . ? C30 C26 C25 110.7(7) . . ? C30 C26 C27 109.3(7) . . ? C25 C26 C27 110.7(6) . . ? C30 C26 C28 108.8(5) . . ? C25 C26 C28 108.1(6) . . ? C27 C26 C28 109.2(6) . . ? C31 C27 C26 109.5(6) . . ? C31 C27 H27A 109.8 . . ? C26 C27 H27A 109.8 . . ? C31 C27 H27B 109.8 . . ? C26 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? C26 C28 C26 109.8(9) . 2_556 ? C26 C28 H28A 109.5 . . ? C26 C28 H28A 109.9 2_556 . ? C26 C30 C31 109.0(7) . 2_556 ? C26 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 2_556 . ? C26 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 2_556 . ? H30A C30 H30B 108.3 . . ? C27 C31 C32 110.2(7) . . ? C27 C31 C30 111.0(7) . 2_556 ? C32 C31 C30 108.8(6) . 2_556 ? C27 C31 H31 108.9 . . ? C32 C31 H31 108.9 . . ? C30 C31 H31 108.9 2_556 . ? C31 C32 C31 108.9(10) 2_556 . ? C31 C32 H32A 109.8 2_556 . ? C31 C32 H32A 110.0 . . ? O12A C33 O11 125.3(17) . . ? O12A C33 O12 22.7(15) . . ? O11 C33 O12 121.9(10) . . ? O12A C33 C34 114.3(17) . . ? O11 C33 C34 118.4(8) . . ? O12 C33 C34 118.8(10) . . ? C33 C34 C37 113.2(7) . . ? C33 C34 C35 110.9(6) . . ? C37 C34 C35 108.7(6) . . ? C33 C34 C36 109.5(6) . . ? C37 C34 C36 107.4(6) . . ? C35 C34 C36 106.9(6) . . ? C34 C35 C34 113.3(9) 2_656 . ? C34 C35 H35A 108.5 2_656 . ? C34 C35 H35A 109.4 . . ? C38 C36 C34 110.2(7) 2_656 . ? C38 C36 H36A 109.6 2_656 . ? C34 C36 H36A 109.6 . . ? C38 C36 H36B 109.6 2_656 . ? C34 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C34 C37 C38 110.2(7) . . ? C34 C37 H37A 109.6 . . ? C38 C37 H37A 109.6 . . ? C34 C37 H37B 109.6 . . ? C38 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C36 112.5(8) . 2_656 ? C39 C38 C37 110.8(7) . . ? C36 C38 C37 108.0(7) 2_656 . ? C39 C38 H38 108.5 . . ? C36 C38 H38 108.5 2_656 . ? C37 C38 H38 108.5 . . ? C38 C39 C38 107.4(10) . 2_656 ? C38 C39 H39A 110.0 . . ? C38 C39 H39A 110.6 2_656 . ? H15D O15 H15C 117.4 . . ? H18C O18 H18D 123.9 . . ? H16C O16 H16D 83.4 . . ? H17D O17 H17C 120.8 . . ? H17E O17A H17F 153.5 . . ? C25 O14A Ag3 113.5(12) . . ? C25 O14 Ag3 124.0(10) . . ? C13 O7 Ag5 120.0(11) . . ? C13 O7A Ag5 115.9(16) . . ? C13 O7A Ag3 107.2(13) . . ? Ag5 O7A Ag3 90.2(9) . . ? C12 O4 Ag4 119.1(10) . . ? C12 O4A Ag4 117.8(12) . . ? C25 O13 Ag6 125.0(11) . . ? C25 O13A Ag6 113.0(11) . . ? C25 O13A Ag1 120.6(11) . . ? Ag6 O13A Ag1 77.6(6) . . ? C33 O12 Ag6 119.1(10) . . ? C33 O12A Ag6 123(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 O8 Ag1 Ag3 O14 -70.9(4) . . . . ? O9 Ag1 Ag3 O14 136.6(4) 4_565 . . . ? O3 Ag1 Ag3 O14 8.8(5) . . . . ? O13A Ag1 Ag3 O14 23.2(6) . . . . ? Ag5 Ag1 Ag3 O14 -157.7(4) . . . . ? Ag6 Ag1 Ag3 O14 79.5(4) . . . . ? O8 Ag1 Ag3 O11 128.3(2) . . . . ? O9 Ag1 Ag3 O11 -24.2(2) 4_565 . . . ? O3 Ag1 Ag3 O11 -152.0(3) . . . . ? O13A Ag1 Ag3 O11 -137.6(4) . . . . ? Ag5 Ag1 Ag3 O11 41.49(15) . . . . ? Ag6 Ag1 Ag3 O11 -81.23(15) . . . . ? O8 Ag1 Ag3 O14A -59.2(5) . . . . ? O9 Ag1 Ag3 O14A 148.3(5) 4_565 . . . ? O3 Ag1 Ag3 O14A 20.5(5) . . . . ? O13A Ag1 Ag3 O14A 34.9(6) . . . . ? Ag5 Ag1 Ag3 O14A -146.0(5) . . . . ? Ag6 Ag1 Ag3 O14A 91.2(5) . . . . ? O8 Ag1 Ag3 O7A 39.5(7) . . . . ? O9 Ag1 Ag3 O7A -113.1(7) 4_565 . . . ? O3 Ag1 Ag3 O7A 119.1(7) . . . . ? O13A Ag1 Ag3 O7A 133.6(8) . . . . ? Ag5 Ag1 Ag3 O7A -47.4(6) . . . . ? Ag6 Ag1 Ag3 O7A -170.1(6) . . . . ? O8 Ag1 Ag3 O6 54.3(3) . . . 4_566 ? O9 Ag1 Ag3 O6 -98.2(3) 4_565 . . 4_566 ? O3 Ag1 Ag3 O6 134.0(3) . . . 4_566 ? O13A Ag1 Ag3 O6 148.5(5) . . . 4_566 ? Ag5 Ag1 Ag3 O6 -32.5(2) . . . 4_566 ? Ag6 Ag1 Ag3 O6 -155.2(2) . . . 4_566 ? O8 Ag1 Ag3 Ag6 -150.46(17) . . . . ? O9 Ag1 Ag3 Ag6 57.03(14) 4_565 . . . ? O3 Ag1 Ag3 Ag6 -70.8(2) . . . . ? O13A Ag1 Ag3 Ag6 -56.3(4) . . . . ? Ag5 Ag1 Ag3 Ag6 122.73(3) . . . . ? O8 Ag1 Ag5 O10 159.5(2) . . . 4_565 ? O9 Ag1 Ag5 O10 -11.2(2) 4_565 . . 4_565 ? O3 Ag1 Ag5 O10 65.0(3) . . . 4_565 ? O13A Ag1 Ag5 O10 -127.6(5) . . . 4_565 ? Ag6 Ag1 Ag5 O10 -86.47(15) . . . 4_565 ? Ag3 Ag1 Ag5 O10 -128.73(15) . . . 4_565 ? O8 Ag1 Ag5 O7 -15.3(5) . . . . ? O9 Ag1 Ag5 O7 174.0(5) 4_565 . . . ? O3 Ag1 Ag5 O7 -109.8(5) . . . . ? O13A Ag1 Ag5 O7 57.6(7) . . . . ? Ag6 Ag1 Ag5 O7 98.7(5) . . . . ? Ag3 Ag1 Ag5 O7 56.5(5) . . . . ? O8 Ag1 Ag5 O7A -24.7(6) . . . . ? O9 Ag1 Ag5 O7A 164.6(6) 4_565 . . . ? O3 Ag1 Ag5 O7A -119.2(6) . . . . ? O13A Ag1 Ag5 O7A 48.2(8) . . . . ? Ag6 Ag1 Ag5 O7A 89.3(6) . . . . ? Ag3 Ag1 Ag5 O7A 47.0(6) . . . . ? O8 Ag1 Ag5 O1 38.19(16) . . . . ? O9 Ag1 Ag5 O1 -132.50(16) 4_565 . . . ? O3 Ag1 Ag5 O1 -56.3(2) . . . . ? O13A Ag1 Ag5 O1 111.1(5) . . . . ? Ag6 Ag1 Ag5 O1 152.19(3) . . . . ? Ag3 Ag1 Ag5 O1 109.93(4) . . . . ? O8 Ag1 Ag5 Ag5 18.2(4) . . . 2_656 ? O9 Ag1 Ag5 Ag5 -152.5(4) 4_565 . . 2_656 ? O3 Ag1 Ag5 Ag5 -76.3(5) . . . 2_656 ? O13A Ag1 Ag5 Ag5 91.1(6) . . . 2_656 ? Ag6 Ag1 Ag5 Ag5 132.2(4) . . . 2_656 ? Ag3 Ag1 Ag5 Ag5 89.9(4) . . . 2_656 ? O14 Ag3 Ag6 O13 -24.7(7) . . . . ? O11 Ag3 Ag6 O13 155.5(5) . . . . ? O14A Ag3 Ag6 O13 -16.8(7) . . . . ? O7A Ag3 Ag6 O13 76.5(9) . . . . ? O6 Ag3 Ag6 O13 -139.7(6) 4_566 . . . ? Ag1 Ag3 Ag6 O13 65.0(5) . . . . ? O14 Ag3 Ag6 O12 153.2(6) . . . . ? O11 Ag3 Ag6 O12 -26.7(5) . . . . ? O14A Ag3 Ag6 O12 161.1(7) . . . . ? O7A Ag3 Ag6 O12 -105.6(9) . . . . ? O6 Ag3 Ag6 O12 38.2(5) 4_566 . . . ? Ag1 Ag3 Ag6 O12 -117.2(4) . . . . ? O14 Ag3 Ag6 O12A 166.2(7) . . . . ? O11 Ag3 Ag6 O12A -13.6(6) . . . . ? O14A Ag3 Ag6 O12A 174.1(8) . . . . ? O7A Ag3 Ag6 O12A -92.6(10) . . . . ? O6 Ag3 Ag6 O12A 51.2(7) 4_566 . . . ? Ag1 Ag3 Ag6 O12A -104.1(6) . . . . ? O14 Ag3 Ag6 O13A -33.3(6) . . . . ? O11 Ag3 Ag6 O13A 146.9(5) . . . . ? O14A Ag3 Ag6 O13A -25.3(7) . . . . ? O7A Ag3 Ag6 O13A 67.9(9) . . . . ? O6 Ag3 Ag6 O13A -148.3(5) 4_566 . . . ? Ag1 Ag3 Ag6 O13A 56.4(4) . . . . ? O14 Ag3 Ag6 O5 -95.4(4) . . . 3_566 ? O11 Ag3 Ag6 O5 84.8(2) . . . 3_566 ? O14A Ag3 Ag6 O5 -87.5(5) . . . 3_566 ? O7A Ag3 Ag6 O5 5.8(8) . . . 3_566 ? O6 Ag3 Ag6 O5 149.6(3) 4_566 . . 3_566 ? Ag1 Ag3 Ag6 O5 -5.73(19) . . . 3_566 ? O14 Ag3 Ag6 Ag1 -89.7(4) . . . . ? O11 Ag3 Ag6 Ag1 90.51(15) . . . . ? O14A Ag3 Ag6 Ag1 -81.7(5) . . . . ? O7A Ag3 Ag6 Ag1 11.5(7) . . . . ? O6 Ag3 Ag6 Ag1 155.3(2) 4_566 . . . ? O8 Ag1 Ag6 O13 -59.9(6) . . . . ? O9 Ag1 Ag6 O13 143.8(6) 4_565 . . . ? O3 Ag1 Ag6 O13 54.6(6) . . . . ? O13A Ag1 Ag6 O13 -2.8(11) . . . . ? Ag5 Ag1 Ag6 O13 -142.0(5) . . . . ? Ag3 Ag1 Ag6 O13 -90.4(5) . . . . ? O8 Ag1 Ag6 O12 98.1(6) . . . . ? O9 Ag1 Ag6 O12 -58.2(5) 4_565 . . . ? O3 Ag1 Ag6 O12 -147.4(5) . . . . ? O13A Ag1 Ag6 O12 155.2(8) . . . . ? Ag5 Ag1 Ag6 O12 16.0(5) . . . . ? Ag3 Ag1 Ag6 O12 67.6(5) . . . . ? O8 Ag1 Ag6 O12A 106.8(8) . . . . ? O9 Ag1 Ag6 O12A -49.5(8) 4_565 . . . ? O3 Ag1 Ag6 O12A -138.8(8) . . . . ? O13A Ag1 Ag6 O12A 163.9(10) . . . . ? Ag5 Ag1 Ag6 O12A 24.6(8) . . . . ? Ag3 Ag1 Ag6 O12A 76.2(8) . . . . ? O8 Ag1 Ag6 O13A -57.1(6) . . . . ? O9 Ag1 Ag6 O13A 146.6(6) 4_565 . . . ? O3 Ag1 Ag6 O13A 57.3(6) . . . . ? Ag5 Ag1 Ag6 O13A -139.2(6) . . . . ? Ag3 Ag1 Ag6 O13A -87.7(6) . . . . ? O8 Ag1 Ag6 O5 -153.5(2) . . . 3_566 ? O9 Ag1 Ag6 O5 50.19(19) 4_565 . . 3_566 ? O3 Ag1 Ag6 O5 -39.07(19) . . . 3_566 ? O13A Ag1 Ag6 O5 -96.4(6) . . . 3_566 ? Ag5 Ag1 Ag6 O5 124.35(13) . . . 3_566 ? Ag3 Ag1 Ag6 O5 175.94(13) . . . 3_566 ? O8 Ag1 Ag6 Ag3 30.56(17) . . . . ? O9 Ag1 Ag6 Ag3 -125.75(14) 4_565 . . . ? O3 Ag1 Ag6 Ag3 145.00(13) . . . . ? O13A Ag1 Ag6 Ag3 87.7(6) . . . . ? Ag5 Ag1 Ag6 Ag3 -51.58(3) . . . . ? O10 Ag5 O1 Ag5 76.06(19) 4_565 . . 2_656 ? O7 Ag5 O1 Ag5 -115.7(5) . . . 2_656 ? O7A Ag5 O1 Ag5 -114.0(7) . . . 2_656 ? Ag1 Ag5 O1 Ag5 -177.55(5) . . . 2_656 ? O6 Ag2 O2 C1 -42.9(10) 3_666 . . . ? O10 Ag2 O2 C1 108.0(6) 4_565 . . . ? Ag2 Ag2 O2 C1 -13.8(6) 3_666 . . . ? O8 Ag1 O3 C12 -43.9(7) . . . . ? O9 Ag1 O3 C12 114.9(7) 4_565 . . . ? O13A Ag1 O3 C12 -126.8(8) . . . . ? Ag5 Ag1 O3 C12 43.8(8) . . . . ? Ag6 Ag1 O3 C12 -166.6(7) . . . . ? Ag3 Ag1 O3 C12 -113.6(7) . . . . ? O8 Ag1 O3 Ag4 117.3(2) . . . 3_566 ? O9 Ag1 O3 Ag4 -83.8(2) 4_565 . . 3_566 ? O13A Ag1 O3 Ag4 34.5(4) . . . 3_566 ? Ag5 Ag1 O3 Ag4 -155.00(9) . . . 3_566 ? Ag6 Ag1 O3 Ag4 -5.35(19) . . . 3_566 ? Ag3 Ag1 O3 Ag4 47.6(3) . . . 3_566 ? O4 Ag4 O5 Ag6 -97.2(4) . . . 3_566 ? O3 Ag4 O5 Ag6 92.9(2) 3_566 . . 3_566 ? O4A Ag4 O5 Ag6 -87.0(5) . . . 3_566 ? Ag4 Ag4 O5 Ag6 174.00(14) 3_566 . . 3_566 ? O9 Ag1 O8 C13 44.3(9) 4_565 . . . ? O3 Ag1 O8 C13 168.5(7) . . . . ? O13A Ag1 O8 C13 -111.0(8) . . . . ? Ag5 Ag1 O8 C13 23.1(6) . . . . ? Ag6 Ag1 O8 C13 -71.6(7) . . . . ? Ag3 Ag1 O8 C13 -46.2(6) . . . . ? O14 Ag3 O11 C33 27.7(14) . . . . ? O14A Ag3 O11 C33 59(2) . . . . ? O7A Ag3 O11 C33 156.9(9) . . . . ? O6 Ag3 O11 C33 -122.2(6) 4_566 . . . ? Ag6 Ag3 O11 C33 28.2(6) . . . . ? Ag1 Ag3 O11 C33 89.3(6) . . . . ? Ag2 O2 C1 O6 8.4(11) . . . . ? Ag2 O2 C1 C2 -166.7(5) . . . . ? Ag2 O6 C1 O2 7.0(11) 3_666 . . . ? Ag3 O6 C1 O2 -143.8(6) 4_565 . . . ? Ag2 O6 C1 C2 -177.9(5) 3_666 . . . ? Ag3 O6 C1 C2 31.3(10) 4_565 . . . ? O2 C1 C2 C3 -34.3(9) . . . . ? O6 C1 C2 C3 150.4(7) . . . . ? O2 C1 C2 C4 -157.2(7) . . . . ? O6 C1 C2 C4 27.6(10) . . . . ? O2 C1 C2 C5 84.4(8) . . . . ? O6 C1 C2 C5 -90.9(8) . . . . ? C1 C2 C3 C10 177.5(6) . . . . ? C4 C2 C3 C10 -58.9(8) . . . . ? C5 C2 C3 C10 60.7(8) . . . . ? C1 C2 C4 C6 -175.8(6) . . . . ? C3 C2 C4 C6 60.5(8) . . . . ? C5 C2 C4 C6 -59.2(8) . . . . ? C1 C2 C5 C9 179.3(6) . . . . ? C3 C2 C5 C9 -60.5(8) . . . . ? C4 C2 C5 C9 59.5(7) . . . . ? C2 C4 C6 C8 -60.2(8) . . . . ? C2 C4 C6 C7 60.6(8) . . . . ? C8 C6 C7 C9 57.4(8) . . . . ? C4 C6 C7 C9 -62.2(8) . . . . ? C4 C6 C8 C10 60.5(8) . . . . ? C7 C6 C8 C10 -59.3(9) . . . . ? C6 C7 C9 C12 -176.4(6) . . . . ? C6 C7 C9 C11 -56.9(8) . . . . ? C6 C7 C9 C5 60.5(8) . . . . ? C2 C5 C9 C7 -60.1(7) . . . . ? C2 C5 C9 C12 175.7(6) . . . . ? C2 C5 C9 C11 57.8(8) . . . . ? C6 C8 C10 C11 60.8(8) . . . . ? C6 C8 C10 C3 -60.5(9) . . . . ? C2 C3 C10 C8 59.7(8) . . . . ? C2 C3 C10 C11 -61.0(8) . . . . ? C8 C10 C11 C9 -61.8(8) . . . . ? C3 C10 C11 C9 59.8(8) . . . . ? C7 C9 C11 C10 59.8(8) . . . . ? C12 C9 C11 C10 -177.3(7) . . . . ? C5 C9 C11 C10 -57.1(8) . . . . ? Ag4 O3 C12 O4A 14.4(14) 3_566 . . . ? Ag1 O3 C12 O4A 169.6(10) . . . . ? Ag4 O3 C12 O4 -11.0(14) 3_566 . . . ? Ag1 O3 C12 O4 144.2(9) . . . . ? Ag4 O3 C12 C9 -177.3(4) 3_566 . . . ? Ag1 O3 C12 C9 -22.1(10) . . . . ? C7 C9 C12 O3 -156.0(7) . . . . ? C11 C9 C12 O3 83.6(8) . . . . ? C5 C9 C12 O3 -35.0(9) . . . . ? C7 C9 C12 O4A 13.0(13) . . . . ? C11 C9 C12 O4A -107.5(11) . . . . ? C5 C9 C12 O4A 134.0(11) . . . . ? C7 C9 C12 O4 36.8(12) . . . . ? C11 C9 C12 O4 -83.7(11) . . . . ? C5 C9 C12 O4 157.8(9) . . . . ? Ag1 O8 C13 O7A 7.1(15) . . . . ? Ag1 O8 C13 O7 -17.2(16) . . . . ? Ag1 O8 C13 C14 172.7(5) . . . . ? O7A C13 C14 C16 171.6(12) . . . . ? O8 C13 C14 C16 5.7(10) . . . . ? O7 C13 C14 C16 -165.3(11) . . . . ? O7A C13 C14 C15 50.4(14) . . . . ? O8 C13 C14 C15 -115.5(8) . . . . ? O7 C13 C14 C15 73.5(12) . . . . ? O7A C13 C14 C17 -67.8(13) . . . . ? O8 C13 C14 C17 126.3(8) . . . . ? O7 C13 C14 C17 -44.7(13) . . . . ? C16 C14 C15 C22 59.3(8) . . . . ? C13 C14 C15 C22 -177.9(6) . . . . ? C17 C14 C15 C22 -58.9(8) . . . . ? C13 C14 C16 C20 -176.9(6) . . . . ? C15 C14 C16 C20 -57.1(8) . . . . ? C17 C14 C16 C20 61.5(8) . . . . ? C16 C14 C17 C18 -60.8(8) . . . . ? C13 C14 C17 C18 175.9(7) . . . . ? C15 C14 C17 C18 58.6(9) . . . . ? C14 C17 C18 C19 61.3(8) . . . . ? C14 C17 C18 C23 -58.8(9) . . . . ? C17 C18 C19 C20 -60.4(8) . . . . ? C23 C18 C19 C20 61.0(9) . . . . ? C14 C16 C20 C21 57.9(9) . . . . ? C14 C16 C20 C19 -62.0(8) . . . . ? C18 C19 C20 C16 60.7(9) . . . . ? C18 C19 C20 C21 -60.3(9) . . . . ? C16 C20 C21 C22 -60.4(9) . . . . ? C19 C20 C21 C22 59.4(8) . . . . ? C20 C21 C22 C23 -59.1(8) . . . . ? C20 C21 C22 C24 176.8(6) . . . . ? C20 C21 C22 C15 59.9(8) . . . . ? C14 C15 C22 C23 59.0(8) . . . . ? C14 C15 C22 C21 -59.9(8) . . . . ? C14 C15 C22 C24 -179.2(6) . . . . ? C21 C22 C23 C18 59.8(8) . . . . ? C24 C22 C23 C18 -176.6(7) . . . . ? C15 C22 C23 C18 -57.7(9) . . . . ? C17 C18 C23 C22 58.7(9) . . . . ? C19 C18 C23 C22 -61.7(9) . . . . ? Ag1 O9 C24 O10 15.4(12) 4_566 . . . ? Ag1 O9 C24 C22 -162.3(5) 4_566 . . . ? Ag5 O10 C24 O9 2.4(10) 4_566 . . . ? Ag2 O10 C24 O9 -130.5(7) 4_566 . . . ? Ag5 O10 C24 C22 -179.8(5) 4_566 . . . ? Ag2 O10 C24 C22 47.3(9) 4_566 . . . ? C23 C22 C24 O9 -151.0(7) . . . . ? C21 C22 C24 O9 -28.4(10) . . . . ? C15 C22 C24 O9 88.6(8) . . . . ? C23 C22 C24 O10 31.1(10) . . . . ? C21 C22 C24 O10 153.8(7) . . . . ? C15 C22 C24 O10 -89.3(8) . . . . ? O14 C25 C26 C30 -20.6(14) . . . . ? O13A C25 C26 C30 157.3(10) . . . . ? O14A C25 C26 C30 -0.4(13) . . . . ? O13 C25 C26 C30 179.9(11) . . . . ? O14 C25 C26 C27 -142.0(12) . . . . ? O13A C25 C26 C27 35.9(12) . . . . ? O14A C25 C26 C27 -121.8(11) . . . . ? O13 C25 C26 C27 58.5(13) . . . . ? O14 C25 C26 C28 98.4(12) . . . . ? O13A C25 C26 C28 -83.6(10) . . . . ? O14A C25 C26 C28 118.6(11) . . . . ? O13 C25 C26 C28 -61.1(12) . . . . ? C30 C26 C27 C31 60.2(9) . . . . ? C25 C26 C27 C31 -177.6(7) . . . . ? C28 C26 C27 C31 -58.7(9) . . . . ? C30 C26 C28 C26 -60.3(5) . . . 2_556 ? C25 C26 C28 C26 179.4(7) . . . 2_556 ? C27 C26 C28 C26 58.9(5) . . . 2_556 ? C25 C26 C30 C31 178.5(6) . . . 2_556 ? C27 C26 C30 C31 -59.4(8) . . . 2_556 ? C28 C26 C30 C31 59.9(8) . . . 2_556 ? C26 C27 C31 C32 -60.8(9) . . . . ? C26 C27 C31 C30 59.8(9) . . . 2_556 ? C27 C31 C32 C31 61.7(5) . . . 2_556 ? C30 C31 C32 C31 -60.2(5) 2_556 . . 2_556 ? Ag3 O11 C33 O12A -32.2(18) . . . . ? Ag3 O11 C33 O12 -5.2(15) . . . . ? Ag3 O11 C33 C34 164.4(5) . . . . ? O12A C33 C34 C37 -17.3(16) . . . . ? O11 C33 C34 C37 147.9(8) . . . . ? O12 C33 C34 C37 -42.2(14) . . . . ? O12A C33 C34 C35 -139.8(14) . . . . ? O11 C33 C34 C35 25.4(10) . . . . ? O12 C33 C34 C35 -164.7(11) . . . . ? O12A C33 C34 C36 102.6(15) . . . . ? O11 C33 C34 C36 -92.3(9) . . . . ? O12 C33 C34 C36 77.7(14) . . . . ? C33 C34 C35 C34 -176.9(7) . . . 2_656 ? C37 C34 C35 C34 58.1(5) . . . 2_656 ? C36 C34 C35 C34 -57.6(5) . . . 2_656 ? C33 C34 C36 C38 -179.8(8) . . . 2_656 ? C37 C34 C36 C38 -56.5(9) . . . 2_656 ? C35 C34 C36 C38 60.0(9) . . . 2_656 ? C33 C34 C37 C38 178.0(7) . . . . ? C35 C34 C37 C38 -58.3(9) . . . . ? C36 C34 C37 C38 57.0(9) . . . . ? C34 C37 C38 C39 -61.5(9) . . . . ? C34 C37 C38 C36 62.0(10) . . . 2_656 ? C36 C38 C39 C38 -60.7(6) 2_656 . . 2_656 ? C37 C38 C39 C38 60.2(5) . . . 2_656 ? O14 C25 O14A Ag3 -59(4) . . . . ? O13A C25 O14A Ag3 19(2) . . . . ? O13 C25 O14A Ag3 -7(2) . . . . ? C26 C25 O14A Ag3 173.2(7) . . . . ? O14 Ag3 O14A C25 58(4) . . . . ? O11 Ag3 O14A C25 -13(3) . . . . ? O7A Ag3 O14A C25 -109.9(13) . . . . ? O6 Ag3 O14A C25 168.4(10) 4_566 . . . ? Ag6 Ag3 O14A C25 17.4(11) . . . . ? Ag1 Ag3 O14A C25 -43.6(11) . . . . ? O13A C25 O14 Ag3 -19.0(19) . . . . ? O14A C25 O14 Ag3 96(5) . . . . ? O13 C25 O14 Ag3 -41.1(17) . . . . ? C26 C25 O14 Ag3 158.8(7) . . . . ? O11 Ag3 O14 C25 46(2) . . . . ? O14A Ag3 O14 C25 -92(4) . . . . ? O7A Ag3 O14 C25 -80.2(15) . . . . ? O6 Ag3 O14 C25 -167.0(11) 4_566 . . . ? Ag6 Ag3 O14 C25 45.6(12) . . . . ? Ag1 Ag3 O14 C25 -15.9(12) . . . . ? O7A C13 O7 Ag5 -91(5) . . . . ? O8 C13 O7 Ag5 -5.9(19) . . . . ? C14 C13 O7 Ag5 164.5(7) . . . . ? O10 Ag5 O7 C13 -11(4) 4_565 . . . ? O7A Ag5 O7 C13 72(5) . . . . ? O1 Ag5 O7 C13 -116.3(14) . . . . ? Ag1 Ag5 O7 C13 17.4(12) . . . . ? Ag5 Ag5 O7 C13 -159.6(13) 2_656 . . . ? O8 C13 O7A Ag5 -43.2(16) . . . . ? O7 C13 O7A Ag5 65(5) . . . . ? C14 C13 O7A Ag5 151.3(9) . . . . ? O8 C13 O7A Ag3 55.7(16) . . . . ? O7 C13 O7A Ag3 164(6) . . . . ? C14 C13 O7A Ag3 -109.9(12) . . . . ? O10 Ag5 O7A C13 60(3) 4_565 . . . ? O7 Ag5 O7A C13 -78(5) . . . . ? O1 Ag5 O7A C13 -86.6(14) . . . . ? Ag1 Ag5 O7A C13 45.1(13) . . . . ? Ag5 Ag5 O7A C13 -131.2(13) 2_656 . . . ? O10 Ag5 O7A Ag3 -49(3) 4_565 . . . ? O7 Ag5 O7A Ag3 172(6) . . . . ? O1 Ag5 O7A Ag3 164.1(8) . . . . ? Ag1 Ag5 O7A Ag3 -64.2(6) . . . . ? Ag5 Ag5 O7A Ag3 119.5(6) 2_656 . . . ? O14 Ag3 O7A C13 13.9(17) . . . . ? O11 Ag3 O7A C13 -148.6(15) . . . . ? O14A Ag3 O7A C13 16.4(16) . . . . ? O6 Ag3 O7A C13 126.0(15) 4_566 . . . ? Ag6 Ag3 O7A C13 -73.0(16) . . . . ? Ag1 Ag3 O7A C13 -62.1(14) . . . . ? O14 Ag3 O7A Ag5 131.2(7) . . . . ? O11 Ag3 O7A Ag5 -31.3(6) . . . . ? O14A Ag3 O7A Ag5 133.7(8) . . . . ? O6 Ag3 O7A Ag5 -116.8(7) 4_566 . . . ? Ag6 Ag3 O7A Ag5 44.2(10) . . . . ? Ag1 Ag3 O7A Ag5 55.1(6) . . . . ? O3 C12 O4 Ag4 15.2(15) . . . . ? O4A C12 O4 Ag4 -81(4) . . . . ? C9 C12 O4 Ag4 -178.4(6) . . . . ? O3 Ag4 O4 C12 -25(2) 3_566 . . . ? O4A Ag4 O4 C12 74(4) . . . . ? O5 Ag4 O4 C12 -162.6(10) . . . . ? Ag4 Ag4 O4 C12 -10.6(10) 3_566 . . . ? O3 C12 O4A Ag4 -24.7(17) . . . . ? O4 C12 O4A Ag4 74(4) . . . . ? C9 C12 O4A Ag4 166.9(7) . . . . ? O4 Ag4 O4A C12 -75(4) . . . . ? O3 Ag4 O4A C12 48(2) 3_566 . . . ? O5 Ag4 O4A C12 -132.8(12) . . . . ? Ag4 Ag4 O4A C12 19.6(12) 3_566 . . . ? O14 C25 O13 Ag6 2.3(19) . . . . ? O13A C25 O13 Ag6 -113(4) . . . . ? O14A C25 O13 Ag6 -16(2) . . . . ? C26 C25 O13 Ag6 163.9(8) . . . . ? O12 Ag6 O13 C25 17(3) . . . . ? O12A Ag6 O13 C25 53(3) . . . . ? O13A Ag6 O13 C25 78(5) . . . . ? O5 Ag6 O13 C25 162.8(14) 3_566 . . . ? Ag3 Ag6 O13 C25 22.3(12) . . . . ? Ag1 Ag6 O13 C25 91.3(13) . . . . ? O14 C25 O13A Ag6 -29.6(17) . . . . ? O14A C25 O13A Ag6 -53.9(18) . . . . ? O13 C25 O13A Ag6 46(3) . . . . ? C26 C25 O13A Ag6 152.3(7) . . . . ? O14 C25 O13A Ag1 59.3(17) . . . . ? O14A C25 O13A Ag1 35(2) . . . . ? O13 C25 O13A Ag1 135(5) . . . . ? C26 C25 O13A Ag1 -118.7(11) . . . . ? O13 Ag6 O13A C25 -76(5) . . . . ? O12 Ag6 O13A C25 59.7(18) . . . . ? O12A Ag6 O13A C25 85.9(18) . . . . ? O5 Ag6 O13A C25 -170.7(12) 3_566 . . . ? Ag3 Ag6 O13A C25 45.9(11) . . . . ? Ag1 Ag6 O13A C25 118.3(13) . . . . ? O13 Ag6 O13A Ag1 166(6) . . . . ? O12 Ag6 O13A Ag1 -58.6(15) . . . . ? O12A Ag6 O13A Ag1 -32.3(17) . . . . ? O5 Ag6 O13A Ag1 71.0(4) 3_566 . . . ? Ag3 Ag6 O13A Ag1 -72.4(3) . . . . ? O8 Ag1 O13A C25 20.6(12) . . . . ? O9 Ag1 O13A C25 -147.4(11) 4_565 . . . ? O3 Ag1 O13A C25 123.0(13) . . . . ? Ag5 Ag1 O13A C25 -49.9(15) . . . . ? Ag6 Ag1 O13A C25 -109.6(15) . . . . ? Ag3 Ag1 O13A C25 -48.8(12) . . . . ? O8 Ag1 O13A Ag6 130.2(5) . . . . ? O9 Ag1 O13A Ag6 -37.8(6) 4_565 . . . ? O3 Ag1 O13A Ag6 -127.4(4) . . . . ? Ag5 Ag1 O13A Ag6 59.7(6) . . . . ? Ag3 Ag1 O13A Ag6 60.8(3) . . . . ? O12A C33 O12 Ag6 73(5) . . . . ? O11 C33 O12 Ag6 -33.3(19) . . . . ? C34 C33 O12 Ag6 157.1(7) . . . . ? O13 Ag6 O12 C33 47(3) . . . . ? O12A Ag6 O12 C33 -60(5) . . . . ? O13A Ag6 O12 C33 27(2) . . . . ? O5 Ag6 O12 C33 -96.5(14) 3_566 . . . ? Ag3 Ag6 O12 C33 40.8(13) . . . . ? Ag1 Ag6 O12 C33 -19.4(15) . . . . ? O11 C33 O12A Ag6 11(3) . . . . ? O12 C33 O12A Ag6 -78(5) . . . . ? C34 C33 O12A Ag6 175.2(10) . . . . ? O13 Ag6 O12A C33 -22(4) . . . . ? O12 Ag6 O12A C33 85(6) . . . . ? O13A Ag6 O12A C33 -30(3) . . . . ? O5 Ag6 O12A C33 -128.8(18) 3_566 . . . ? Ag3 Ag6 O12A C33 8.4(18) . . . . ? Ag1 Ag6 O12A C33 -56.3(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.136 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.139 # Attachment '2.cif.cif' data_xb2560m _database_code_depnum_ccdc_archive 'CCDC 727389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Ag N2, C12 H15 O4' _chemical_formula_sum 'C24 H27 Ag N2 O4' _chemical_formula_weight 515.35 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.288(2) _cell_length_b 13.706(2) _cell_length_c 13.376(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.697(3) _cell_angle_gamma 90.00 _cell_volume 2133.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1586 _cell_measurement_theta_min 2.189 _cell_measurement_theta_max 21.259 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7919 _exptl_absorpt_correction_T_max 0.8512 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11914 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.66 _reflns_number_total 4460 _reflns_number_gt 2655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0900P)^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 4460 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N2 N 0.9317(3) 0.8803(2) 1.0950(3) 0.0330(9) Uani 1 1 d . . . C24 C 1.0216(4) 0.8214(3) 1.1312(4) 0.0374(11) Uani 1 1 d . . . H24 H 1.0947 0.8488 1.1535 0.045 Uiso 1 1 calc R . . C22 C 0.8277(4) 0.8383(3) 1.0658(4) 0.0401(11) Uani 1 1 d . . . H22 H 0.7629 0.8779 1.0428 0.048 Uiso 1 1 calc R . . Ag1 Ag 0.94326(3) 0.03828(2) 1.07911(3) 0.04438(17) Uani 1 1 d . . . O1 O 0.7404(3) 0.0564(2) 0.9252(3) 0.0471(9) Uani 1 1 d . . . O2 O 0.8152(3) -0.0235(3) 0.8223(3) 0.0564(10) Uani 1 1 d . . . O3 O 0.3732(3) -0.1072(3) 0.9513(3) 0.0495(9) Uani 1 1 d . . . H3 H 0.3345 -0.0878 0.9872 0.074 Uiso 1 1 calc R . . O4 O 0.2421(3) -0.0279(4) 0.8250(3) 0.0791(14) Uani 1 1 d . . . N1 N 0.9584(3) 0.1962(3) 1.1036(3) 0.0382(9) Uani 1 1 d . . . C15 C 0.9791(4) 0.4000(3) 1.1270(4) 0.0328(10) Uani 1 1 d . . . C11 C 0.5296(3) -0.0377(3) 0.8519(4) 0.0344(10) Uani 1 1 d . . . H11A H 0.5196 0.0306 0.8659 0.041 Uiso 1 1 calc R . . H11B H 0.5602 -0.0709 0.9192 0.041 Uiso 1 1 calc R . . C19 C 0.8868(4) 0.5693(3) 1.1026(4) 0.0352(11) Uani 1 1 d . . . H19A H 0.8428 0.5502 1.0312 0.042 Uiso 1 1 calc R . . H19B H 0.8406 0.5547 1.1475 0.042 Uiso 1 1 calc R . . C20 C 0.9068(4) 0.6770(3) 1.1044(3) 0.0322(10) Uani 1 1 d . . . C14 C 0.8728(4) 0.3543(3) 1.0895(4) 0.0388(11) Uani 1 1 d . . . H14 H 0.8059 0.3914 1.0717 0.047 Uiso 1 1 calc R . . C16 C 1.0735(4) 0.3387(3) 1.1524(4) 0.0386(11) Uani 1 1 d . . . H16 H 1.1469 0.3651 1.1777 0.046 Uiso 1 1 calc R . . C2 C 0.6143(4) -0.0470(3) 0.7899(4) 0.0339(10) Uani 1 1 d . . . C17 C 1.0606(4) 0.2401(3) 1.1410(4) 0.0392(11) Uani 1 1 d . . . H17 H 1.1262 0.2014 1.1602 0.047 Uiso 1 1 calc R . . C21 C 0.8128(4) 0.7392(3) 1.0685(4) 0.0362(10) Uani 1 1 d . . . H21 H 0.7390 0.7133 1.0459 0.043 Uiso 1 1 calc R . . C10 C 0.4126(4) -0.0823(3) 0.7894(4) 0.0386(11) Uani 1 1 d . . . C18 C 0.9954(4) 0.5078(3) 1.1386(4) 0.0393(11) Uani 1 1 d . . . H18A H 1.0453 0.5280 1.0991 0.047 Uiso 1 1 calc R . . H18B H 1.0350 0.5221 1.2124 0.047 Uiso 1 1 calc R . . C1 C 0.7325(4) -0.0016(3) 0.8499(4) 0.0367(11) Uani 1 1 d . . . C9 C 0.3640(4) -0.0294(4) 0.6853(4) 0.0519(14) Uani 1 1 d . . . H9A H 0.3534 0.0391 0.6979 0.062 Uiso 1 1 calc R . . H9B H 0.2899 -0.0568 0.6459 0.062 Uiso 1 1 calc R . . C4 C 0.6274(4) -0.1553(3) 0.7682(4) 0.0378(11) Uani 1 1 d . . . H4A H 0.6796 -0.1625 0.7276 0.045 Uiso 1 1 calc R . . H4B H 0.6601 -0.1895 0.8346 0.045 Uiso 1 1 calc R . . C8 C 0.4480(4) -0.0402(4) 0.6216(4) 0.0523(13) Uani 1 1 d . . . H8 H 0.4168 -0.0056 0.5543 0.063 Uiso 1 1 calc R . . C23 C 1.0120(4) 0.7218(3) 1.1373(4) 0.0378(11) Uani 1 1 d . . . H23 H 1.0779 0.6842 1.1641 0.045 Uiso 1 1 calc R . . C7 C 0.4293(4) -0.1909(3) 0.7704(4) 0.0443(12) Uani 1 1 d . . . H7A H 0.4598 -0.2245 0.8374 0.053 Uiso 1 1 calc R . . H7B H 0.3561 -0.2203 0.7316 0.053 Uiso 1 1 calc R . . C12 C 0.3325(4) -0.0696(4) 0.8548(4) 0.0437(12) Uani 1 1 d . . . C13 C 0.8659(4) 0.2544(3) 1.0785(4) 0.0424(12) Uani 1 1 d . . . H13 H 0.7936 0.2260 1.0523 0.051 Uiso 1 1 calc R . . C5 C 0.5120(4) -0.2002(4) 0.7079(4) 0.0461(12) Uani 1 1 d . . . H5 H 0.5229 -0.2694 0.6955 0.055 Uiso 1 1 calc R . . C3 C 0.5644(4) 0.0053(4) 0.6845(4) 0.0503(13) Uani 1 1 d . . . H3A H 0.6173 0.0000 0.6442 0.060 Uiso 1 1 calc R . . H3B H 0.5541 0.0739 0.6966 0.060 Uiso 1 1 calc R . . C6 C 0.4640(4) -0.1470(5) 0.5998(4) 0.0621(17) Uani 1 1 d . . . H6A H 0.5173 -0.1534 0.5602 0.074 Uiso 1 1 calc R . . H6B H 0.3911 -0.1755 0.5588 0.074 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 N2 0.035(2) 0.0162(17) 0.042(2) 0.0003(14) 0.0038(18) -0.0011(15) C24 0.036(3) 0.023(2) 0.047(3) -0.0008(19) 0.005(2) -0.0015(19) C22 0.046(3) 0.032(2) 0.044(3) 0.004(2) 0.016(2) 0.006(2) Ag1 0.0588(3) 0.0204(2) 0.0559(3) -0.00100(16) 0.0211(2) -0.00170(16) O1 0.0396(19) 0.061(2) 0.044(2) -0.0153(17) 0.0184(17) -0.0161(16) O2 0.0308(19) 0.060(2) 0.081(3) -0.0224(19) 0.022(2) -0.0058(16) O3 0.040(2) 0.056(2) 0.055(3) -0.0059(18) 0.0196(18) -0.0019(16) O4 0.038(2) 0.133(4) 0.067(3) 0.010(3) 0.018(2) 0.032(2) N1 0.035(2) 0.0218(18) 0.053(3) 0.0007(16) 0.008(2) -0.0007(16) C15 0.037(3) 0.025(2) 0.033(3) 0.0005(18) 0.008(2) 0.0004(18) C11 0.025(2) 0.030(2) 0.042(3) -0.0024(19) 0.003(2) -0.0024(18) C19 0.044(3) 0.026(2) 0.039(3) -0.0012(19) 0.019(2) -0.0005(19) C20 0.045(3) 0.027(2) 0.029(3) 0.0014(17) 0.018(2) -0.0030(19) C14 0.031(2) 0.027(2) 0.057(3) 0.002(2) 0.011(2) 0.0007(19) C16 0.029(2) 0.030(2) 0.049(3) 0.004(2) 0.001(2) -0.0039(19) C2 0.025(2) 0.034(2) 0.042(3) -0.0023(19) 0.010(2) 0.0006(18) C17 0.034(3) 0.029(2) 0.052(3) 0.001(2) 0.010(2) 0.0047(19) C21 0.036(3) 0.034(2) 0.040(3) -0.004(2) 0.014(2) -0.005(2) C10 0.025(2) 0.036(2) 0.054(3) -0.010(2) 0.011(2) -0.0027(19) C18 0.043(3) 0.024(2) 0.045(3) -0.002(2) 0.008(2) -0.006(2) C1 0.033(3) 0.031(2) 0.046(3) 0.000(2) 0.013(2) -0.0038(19) C9 0.024(3) 0.065(4) 0.056(4) -0.002(3) -0.003(2) 0.009(2) C4 0.039(3) 0.045(3) 0.033(3) -0.007(2) 0.016(2) 0.003(2) C8 0.037(3) 0.071(4) 0.041(3) 0.003(3) 0.002(2) 0.004(3) C23 0.038(3) 0.025(2) 0.050(3) -0.003(2) 0.013(2) 0.0017(19) C7 0.043(3) 0.045(3) 0.048(3) -0.010(2) 0.018(3) -0.012(2) C12 0.031(3) 0.044(3) 0.051(4) -0.009(2) 0.007(3) -0.005(2) C13 0.036(3) 0.030(2) 0.056(3) -0.001(2) 0.009(2) -0.004(2) C5 0.045(3) 0.044(3) 0.054(3) -0.021(2) 0.021(3) -0.004(2) C3 0.035(3) 0.052(3) 0.058(4) 0.010(3) 0.007(3) 0.003(2) C6 0.043(3) 0.097(5) 0.046(4) -0.030(3) 0.014(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N2 C24 1.329(5) . ? N2 C22 1.342(5) . ? N2 Ag1 2.184(3) 1_565 ? C24 C23 1.374(6) . ? C24 H24 0.9300 . ? C22 C21 1.372(6) . ? C22 H22 0.9300 . ? Ag1 N2 2.184(3) 1_545 ? Ag1 N1 2.188(4) . ? Ag1 O1 2.688(3) . ? Ag1 Ag1 3.0685(8) 3_757 ? O1 C1 1.262(6) . ? O2 C1 1.225(5) . ? O3 C12 1.329(6) . ? O3 H3 0.8200 . ? O4 C12 1.197(6) . ? N1 C17 1.337(5) . ? N1 C13 1.340(6) . ? C15 C16 1.383(6) . ? C15 C14 1.389(6) . ? C15 C18 1.492(6) . ? C11 C2 1.530(6) . ? C11 C10 1.539(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C19 C20 1.497(6) . ? C19 C18 1.520(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C23 1.370(6) . ? C20 C21 1.391(6) . ? C14 C13 1.377(6) . ? C14 H14 0.9300 . ? C16 C17 1.363(6) . ? C16 H16 0.9300 . ? C2 C3 1.525(7) . ? C2 C4 1.530(6) . ? C2 C1 1.548(6) . ? C17 H17 0.9300 . ? C21 H21 0.9300 . ? C10 C9 1.511(7) . ? C10 C12 1.523(7) . ? C10 C7 1.535(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C9 C8 1.542(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C4 C5 1.518(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C8 C6 1.517(8) . ? C8 C3 1.540(7) . ? C8 H8 0.9800 . ? C23 H23 0.9300 . ? C7 C5 1.515(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C13 H13 0.9300 . ? C5 C6 1.556(7) . ? C5 H5 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 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 C24 N2 C22 116.7(4) . . ? C24 N2 Ag1 124.5(3) . 1_565 ? C22 N2 Ag1 118.9(3) . 1_565 ? N2 C24 C23 123.2(4) . . ? N2 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? N2 C22 C21 122.7(4) . . ? N2 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N2 Ag1 N1 166.15(14) 1_545 . ? N2 Ag1 O1 95.32(11) 1_545 . ? N1 Ag1 O1 92.10(12) . . ? N2 Ag1 Ag1 77.66(10) 1_545 3_757 ? N1 Ag1 Ag1 113.94(10) . 3_757 ? O1 Ag1 Ag1 91.06(7) . 3_757 ? C1 O1 Ag1 111.6(3) . . ? C12 O3 H3 109.5 . . ? C17 N1 C13 116.5(4) . . ? C17 N1 Ag1 121.7(3) . . ? C13 N1 Ag1 121.8(3) . . ? C16 C15 C14 115.6(4) . . ? C16 C15 C18 120.1(4) . . ? C14 C15 C18 124.3(4) . . ? C2 C11 C10 110.6(4) . . ? C2 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C20 C19 C18 114.8(4) . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C18 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C23 C20 C21 115.5(4) . . ? C23 C20 C19 125.5(4) . . ? C21 C20 C19 119.0(4) . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C3 C2 C4 108.4(4) . . ? C3 C2 C11 108.7(4) . . ? C4 C2 C11 108.3(3) . . ? C3 C2 C1 108.8(4) . . ? C4 C2 C1 110.5(4) . . ? C11 C2 C1 112.0(4) . . ? N1 C17 C16 123.3(4) . . ? N1 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C22 C21 C20 120.8(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C9 C10 C12 109.7(4) . . ? C9 C10 C7 110.3(4) . . ? C12 C10 C7 110.6(4) . . ? C9 C10 C11 109.5(4) . . ? C12 C10 C11 107.8(4) . . ? C7 C10 C11 108.9(4) . . ? C15 C18 C19 116.1(4) . . ? C15 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? C15 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? O2 C1 O1 122.5(4) . . ? O2 C1 C2 118.5(4) . . ? O1 C1 C2 119.1(4) . . ? C10 C9 C8 109.1(4) . . ? C10 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C5 C4 C2 110.9(4) . . ? C5 C4 H4A 109.5 . . ? C2 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C6 C8 C3 109.9(4) . . ? C6 C8 C9 110.4(4) . . ? C3 C8 C9 109.1(5) . . ? C6 C8 H8 109.1 . . ? C3 C8 H8 109.1 . . ? C9 C8 H8 109.1 . . ? C20 C23 C24 121.1(4) . . ? C20 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C5 C7 C10 108.8(4) . . ? C5 C7 H7A 109.9 . . ? C10 C7 H7A 109.9 . . ? C5 C7 H7B 109.9 . . ? C10 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O4 C12 O3 121.9(5) . . ? O4 C12 C10 124.4(5) . . ? O3 C12 C10 113.7(4) . . ? N1 C13 C14 123.2(4) . . ? N1 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C7 C5 C4 110.5(4) . . ? C7 C5 C6 110.6(4) . . ? C4 C5 C6 108.4(4) . . ? C7 C5 H5 109.1 . . ? C4 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? C2 C3 C8 110.0(4) . . ? C2 C3 H3A 109.7 . . ? C8 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C8 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C8 C6 C5 107.9(4) . . ? C8 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? C8 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 N2 C24 C23 1.5(7) . . . . ? Ag1 N2 C24 C23 -177.9(3) 1_565 . . . ? C24 N2 C22 C21 -2.5(7) . . . . ? Ag1 N2 C22 C21 176.9(4) 1_565 . . . ? N2 Ag1 O1 C1 -51.9(3) 1_545 . . . ? N1 Ag1 O1 C1 139.8(3) . . . . ? Ag1 Ag1 O1 C1 25.8(3) 3_757 . . . ? N2 Ag1 N1 C17 84.8(7) 1_545 . . . ? O1 Ag1 N1 C17 -152.7(4) . . . . ? Ag1 Ag1 N1 C17 -60.6(4) 3_757 . . . ? N2 Ag1 N1 C13 -97.5(6) 1_545 . . . ? O1 Ag1 N1 C13 24.9(4) . . . . ? Ag1 Ag1 N1 C13 117.0(4) 3_757 . . . ? C18 C19 C20 C23 -1.5(6) . . . . ? C18 C19 C20 C21 177.2(4) . . . . ? C16 C15 C14 C13 -0.7(7) . . . . ? C18 C15 C14 C13 178.1(5) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C18 C15 C16 C17 -179.1(4) . . . . ? C10 C11 C2 C3 59.0(5) . . . . ? C10 C11 C2 C4 -58.7(5) . . . . ? C10 C11 C2 C1 179.2(4) . . . . ? C13 N1 C17 C16 -1.1(7) . . . . ? Ag1 N1 C17 C16 176.7(4) . . . . ? C15 C16 C17 N1 1.2(8) . . . . ? N2 C22 C21 C20 1.4(7) . . . . ? C23 C20 C21 C22 0.8(7) . . . . ? C19 C20 C21 C22 -178.0(4) . . . . ? C2 C11 C10 C9 -60.1(5) . . . . ? C2 C11 C10 C12 -179.4(4) . . . . ? C2 C11 C10 C7 60.6(5) . . . . ? C16 C15 C18 C19 176.5(4) . . . . ? C14 C15 C18 C19 -2.2(7) . . . . ? C20 C19 C18 C15 -173.8(4) . . . . ? Ag1 O1 C1 O2 -34.7(6) . . . . ? Ag1 O1 C1 C2 145.2(3) . . . . ? C3 C2 C1 O2 -76.7(5) . . . . ? C4 C2 C1 O2 42.2(6) . . . . ? C11 C2 C1 O2 163.1(4) . . . . ? C3 C2 C1 O1 103.3(5) . . . . ? C4 C2 C1 O1 -137.7(4) . . . . ? C11 C2 C1 O1 -16.8(6) . . . . ? C12 C10 C9 C8 178.2(4) . . . . ? C7 C10 C9 C8 -59.8(5) . . . . ? C11 C10 C9 C8 60.1(5) . . . . ? C3 C2 C4 C5 -59.9(5) . . . . ? C11 C2 C4 C5 57.9(5) . . . . ? C1 C2 C4 C5 -179.1(4) . . . . ? C10 C9 C8 C6 60.4(5) . . . . ? C10 C9 C8 C3 -60.5(5) . . . . ? C21 C20 C23 C24 -1.9(7) . . . . ? C19 C20 C23 C24 176.8(4) . . . . ? N2 C24 C23 C20 0.8(7) . . . . ? C9 C10 C7 C5 60.1(5) . . . . ? C12 C10 C7 C5 -178.4(4) . . . . ? C11 C10 C7 C5 -60.1(5) . . . . ? C9 C10 C12 O4 3.5(7) . . . . ? C7 C10 C12 O4 -118.4(6) . . . . ? C11 C10 C12 O4 122.7(6) . . . . ? C9 C10 C12 O3 -174.9(4) . . . . ? C7 C10 C12 O3 63.2(5) . . . . ? C11 C10 C12 O3 -55.7(5) . . . . ? C17 N1 C13 C14 0.1(7) . . . . ? Ag1 N1 C13 C14 -177.7(4) . . . . ? C15 C14 C13 N1 0.8(8) . . . . ? C10 C7 C5 C4 60.1(5) . . . . ? C10 C7 C5 C6 -59.9(5) . . . . ? C2 C4 C5 C7 -59.8(5) . . . . ? C2 C4 C5 C6 61.5(5) . . . . ? C4 C2 C3 C8 58.3(5) . . . . ? C11 C2 C3 C8 -59.3(5) . . . . ? C1 C2 C3 C8 178.5(4) . . . . ? C6 C8 C3 C2 -60.8(6) . . . . ? C9 C8 C3 C2 60.5(5) . . . . ? C3 C8 C6 C5 61.1(6) . . . . ? C9 C8 C6 C5 -59.4(5) . . . . ? C7 C5 C6 C8 60.0(5) . . . . ? C4 C5 C6 C8 -61.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.66 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.600 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.119 # Attachment '3.cif.cif' data_081006bjin _database_code_depnum_ccdc_archive 'CCDC 727390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 Ag N2 O4, C H4 O' _chemical_formula_sum 'C26 H33 Ag N2 O5' _chemical_formula_weight 561.41 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4101(10) _cell_length_b 9.9258(10) _cell_length_c 24.483(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.159(2) _cell_angle_gamma 90.00 _cell_volume 2490.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4468 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7730 _exptl_absorpt_correction_T_max 0.8353 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 12516 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4468 _reflns_number_gt 3698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^+0.6221P] 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 4468 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.820 _refine_ls_restrained_S_all 0.820 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.62163(2) 0.41524(2) 1.008420(9) 0.05126(13) Uani 1 1 d . . . O3 O 0.5646(2) 0.6545(2) 0.72855(8) 0.0510(5) Uani 1 1 d . . . O2 O 0.8034(2) 0.4587(2) 0.94793(10) 0.0612(6) Uani 1 1 d . . . O1 O 0.6597(2) 0.6158(2) 0.95169(10) 0.0592(6) Uani 1 1 d . . . O4 O 0.7260(2) 0.7324(3) 0.68974(8) 0.0552(6) Uani 1 1 d . . . H4 H 0.6687 0.7354 0.6621 0.083 Uiso 1 1 calc R . . C3 C 0.7210(2) 0.6289(3) 0.83343(10) 0.0330(5) Uani 1 1 d . . . H3A H 0.6322 0.6547 0.8356 0.040 Uiso 1 1 calc R . . H3B H 0.7214 0.5337 0.8245 0.040 Uiso 1 1 calc R . . C4 C 0.7687(2) 0.7107(3) 0.78753(10) 0.0345(6) Uani 1 1 d . . . C2 C 0.8095(2) 0.6540(3) 0.88971(10) 0.0344(6) Uani 1 1 d . . . C1 C 0.7549(3) 0.5704(3) 0.93355(11) 0.0373(6) Uani 1 1 d . . . C6 C 0.9093(3) 0.6712(3) 0.78435(12) 0.0406(6) Uani 1 1 d . . . H6A H 0.9397 0.7232 0.7556 0.049 Uiso 1 1 calc R . . H6B H 0.9129 0.5765 0.7749 0.049 Uiso 1 1 calc R . . C7 C 0.7663(3) 0.8620(3) 0.80230(12) 0.0414(6) Uani 1 1 d . . . H7A H 0.7970 0.9149 0.7738 0.050 Uiso 1 1 calc R . . H7B H 0.6776 0.8895 0.8038 0.050 Uiso 1 1 calc R . . C5 C 0.6746(3) 0.6941(3) 0.73312(11) 0.0372(6) Uani 1 1 d . . . C12 C 0.9494(3) 0.6145(3) 0.88561(12) 0.0411(6) Uani 1 1 d . . . H12A H 0.9527 0.5195 0.8768 0.049 Uiso 1 1 calc R . . H12B H 1.0059 0.6297 0.9210 0.049 Uiso 1 1 calc R . . C10 C 0.8529(3) 0.8876(3) 0.85803(13) 0.0460(7) Uani 1 1 d . . . H10 H 0.8504 0.9837 0.8671 0.055 Uiso 1 1 calc R . . C11 C 0.8045(3) 0.8055(3) 0.90305(11) 0.0426(6) Uani 1 1 d . . . H11A H 0.7156 0.8313 0.9051 0.051 Uiso 1 1 calc R . . H11B H 0.8587 0.8237 0.9387 0.051 Uiso 1 1 calc R . . C8 C 0.9975(3) 0.6979(3) 0.84057(13) 0.0448(7) Uani 1 1 d . . . H8 H 1.0873 0.6719 0.8385 0.054 Uiso 1 1 calc R . . C9 C 0.9934(3) 0.8472(3) 0.85470(14) 0.0525(8) Uani 1 1 d . . . H9A H 1.0246 0.9001 0.8264 0.063 Uiso 1 1 calc R . . H9B H 1.0497 0.8646 0.8900 0.063 Uiso 1 1 calc R . . N1 N 0.6729(2) 0.5060(2) 1.09190(9) 0.0412(5) Uani 1 1 d . . . C13 C 0.7745(3) 0.5872(3) 1.10606(14) 0.0458(7) Uani 1 1 d . . . H13 H 0.8246 0.6080 1.0793 0.055 Uiso 1 1 calc R . . C15 C 0.7382(3) 0.6135(3) 1.19853(12) 0.0409(6) Uani 1 1 d . . . C14 C 0.8097(3) 0.6420(3) 1.15768(12) 0.0453(7) Uani 1 1 d . . . H14 H 0.8820 0.6985 1.1653 0.054 Uiso 1 1 calc R . . C18 C 0.7780(3) 0.6631(3) 1.25709(12) 0.0476(7) Uani 1 1 d . . . H18A H 0.7037 0.7047 1.2693 0.057 Uiso 1 1 calc R . . H18B H 0.8456 0.7308 1.2583 0.057 Uiso 1 1 calc R . . C17 C 0.6022(3) 0.4798(3) 1.13107(13) 0.0498(7) Uani 1 1 d . . . H17 H 0.5297 0.4241 1.1221 0.060 Uiso 1 1 calc R . . C16 C 0.6304(3) 0.5304(3) 1.18366(12) 0.0501(7) Uani 1 1 d . . . H16 H 0.5777 0.5093 1.2094 0.060 Uiso 1 1 calc R . . N2 N 0.5359(2) 0.2401(2) 0.95938(10) 0.0464(6) Uani 1 1 d . . . C26 C 0.4349(3) 0.0232(3) 0.89198(12) 0.0431(6) Uani 1 1 d . . . C25 C 0.3830(3) 0.0619(3) 0.93770(13) 0.0495(7) Uani 1 1 d . . . H25 H 0.3123 0.0152 0.9469 0.059 Uiso 1 1 calc R . . C27 C 0.5382(4) 0.0983(3) 0.88092(16) 0.0589(9) Uani 1 1 d . . . H27 H 0.5760 0.0778 0.8502 0.071 Uiso 1 1 calc R . . C24 C 0.4352(3) 0.1687(3) 0.96973(13) 0.0522(8) Uani 1 1 d . . . H24 H 0.3980 0.1923 1.0003 0.063 Uiso 1 1 calc R . . C28 C 0.5858(3) 0.2034(4) 0.91494(14) 0.0595(9) Uani 1 1 d . . . H28 H 0.6565 0.2517 0.9066 0.071 Uiso 1 1 calc R . . C30 C 0.8807(3) 0.5925(3) 1.35534(13) 0.0485(7) Uani 1 1 d . . . H30A H 0.9488 0.6591 1.3550 0.058 Uiso 1 1 calc R . . H30B H 0.8109 0.6348 1.3706 0.058 Uiso 1 1 calc R . . C29 C 0.8286(3) 0.5478(3) 1.29612(13) 0.0508(7) Uani 1 1 d . . . H29A H 0.7584 0.4838 1.2966 0.061 Uiso 1 1 calc R . . H29B H 0.8977 0.5017 1.2817 0.061 Uiso 1 1 calc R . . O5 O 0.9245(2) 0.2652(2) 0.90691(9) 0.0579(6) Uani 1 1 d . . . H5 H 0.8897 0.3302 0.9189 0.087 Uiso 1 1 calc R . . C31 C 0.9778(6) 0.1832(5) 0.95020(19) 0.1007(17) Uani 1 1 d . . . H31A H 1.0347 0.2352 0.9774 0.151 Uiso 1 1 calc R . . H31B H 1.0267 0.1125 0.9367 0.151 Uiso 1 1 calc R . . H31C H 0.9093 0.1447 0.9668 0.151 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 0.0665(2) 0.04965(19) 0.03898(17) -0.00412(9) 0.01292(12) -0.00362(10) O3 0.0424(12) 0.0689(15) 0.0401(11) 0.0048(10) 0.0027(9) -0.0045(10) O2 0.0764(16) 0.0507(13) 0.0652(15) 0.0200(11) 0.0363(12) 0.0132(11) O1 0.0679(15) 0.0600(14) 0.0587(14) 0.0072(11) 0.0355(12) 0.0094(11) O4 0.0594(13) 0.0765(16) 0.0300(10) 0.0045(10) 0.0088(9) -0.0131(11) C3 0.0354(14) 0.0346(13) 0.0307(13) -0.0023(11) 0.0105(10) -0.0015(10) C4 0.0393(14) 0.0355(14) 0.0296(13) 0.0007(10) 0.0087(11) 0.0004(11) C2 0.0365(14) 0.0367(14) 0.0306(13) 0.0010(11) 0.0078(11) 0.0010(10) C1 0.0434(15) 0.0410(15) 0.0279(13) -0.0043(11) 0.0070(12) -0.0026(11) C6 0.0423(15) 0.0433(16) 0.0396(15) 0.0039(12) 0.0159(12) -0.0009(12) C7 0.0527(17) 0.0339(14) 0.0377(15) 0.0033(12) 0.0080(12) 0.0014(12) C5 0.0457(16) 0.0331(14) 0.0338(14) -0.0015(11) 0.0093(11) 0.0026(11) C12 0.0399(15) 0.0453(16) 0.0383(15) 0.0031(12) 0.0071(12) 0.0012(12) C10 0.0611(19) 0.0307(14) 0.0441(17) -0.0014(12) 0.0036(14) -0.0087(12) C11 0.0548(17) 0.0393(15) 0.0312(14) -0.0058(11) 0.0010(12) -0.0002(12) C8 0.0338(14) 0.0533(17) 0.0484(17) 0.0088(14) 0.0106(12) -0.0003(12) C9 0.0504(17) 0.0555(19) 0.0484(18) 0.0058(14) -0.0004(14) -0.0213(14) N1 0.0450(13) 0.0446(13) 0.0341(12) 0.0038(10) 0.0075(10) -0.0026(10) C13 0.0459(16) 0.0506(18) 0.0440(17) 0.0054(13) 0.0167(13) -0.0056(13) C15 0.0440(16) 0.0390(14) 0.0400(15) 0.0050(12) 0.0084(12) 0.0053(12) C14 0.0427(15) 0.0493(17) 0.0444(17) 0.0036(13) 0.0093(13) -0.0065(13) C18 0.0586(18) 0.0453(17) 0.0384(16) -0.0018(13) 0.0077(13) 0.0048(14) C17 0.0483(17) 0.0604(19) 0.0421(17) 0.0022(14) 0.0120(13) -0.0151(14) C16 0.0507(18) 0.064(2) 0.0381(16) 0.0057(14) 0.0149(13) -0.0080(15) N2 0.0526(14) 0.0458(14) 0.0429(14) -0.0056(11) 0.0137(11) -0.0004(11) C26 0.0450(16) 0.0448(16) 0.0388(15) 0.0013(12) 0.0053(12) 0.0052(12) C25 0.0523(18) 0.0540(18) 0.0441(17) 0.0015(14) 0.0139(14) -0.0058(14) C27 0.061(2) 0.065(2) 0.056(2) -0.0200(16) 0.0270(17) -0.0120(16) C24 0.067(2) 0.0520(18) 0.0424(17) -0.0050(14) 0.0226(15) -0.0001(15) C28 0.061(2) 0.067(2) 0.057(2) -0.0205(17) 0.0277(16) -0.0192(16) C30 0.0564(19) 0.0454(17) 0.0424(17) -0.0008(12) 0.0052(14) 0.0014(13) C29 0.062(2) 0.0475(17) 0.0418(17) 0.0005(14) 0.0054(14) 0.0073(14) O5 0.0689(15) 0.0583(14) 0.0435(12) -0.0040(10) 0.0020(10) 0.0094(11) C31 0.149(4) 0.068(3) 0.066(3) 0.003(2) -0.032(3) 0.021(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 2.210(2) . ? Ag1 N1 2.211(2) . ? Ag1 O1 2.499(2) . ? Ag1 Ag1 3.0076(5) 3_667 ? O3 C5 1.198(3) . ? O2 C1 1.243(4) . ? O1 C1 1.240(4) . ? O4 C5 1.326(3) . ? O4 H4 0.8200 . ? C3 C2 1.537(4) . ? C3 C4 1.537(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.517(4) . ? C4 C6 1.531(4) . ? C4 C7 1.546(4) . ? C2 C12 1.528(4) . ? C2 C11 1.541(4) . ? C2 C1 1.543(4) . ? C6 C8 1.537(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C10 1.518(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C8 1.531(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 C11 1.527(4) . ? C10 C9 1.532(5) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C8 C9 1.524(5) . ? C8 H8 0.9800 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N1 C13 1.327(4) . ? N1 C17 1.334(4) . ? C13 C14 1.365(4) . ? C13 H13 0.9300 . ? C15 C14 1.377(4) . ? C15 C16 1.388(4) . ? C15 C18 1.503(4) . ? C14 H14 0.9300 . ? C18 C29 1.524(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 C16 1.365(4) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? N2 C24 1.326(4) . ? N2 C28 1.336(4) . ? C26 C27 1.374(5) . ? C26 C25 1.380(4) . ? C26 C30 1.504(4) 4_565 ? C25 C24 1.373(5) . ? C25 H25 0.9300 . ? C27 C28 1.372(5) . ? C27 H27 0.9300 . ? C24 H24 0.9300 . ? C28 H28 0.9300 . ? C30 C26 1.504(4) 4_666 ? C30 C29 1.522(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? O5 C31 1.373(5) . ? O5 H5 0.8200 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 N1 146.22(9) . . ? N2 Ag1 O1 114.41(9) . . ? N1 Ag1 O1 98.82(9) . . ? N2 Ag1 Ag1 96.66(7) . 3_667 ? N1 Ag1 Ag1 87.65(6) . 3_667 ? O1 Ag1 Ag1 71.95(5) . 3_667 ? C1 O1 Ag1 97.15(18) . . ? C5 O4 H4 109.5 . . ? C2 C3 C4 110.5(2) . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C6 113.7(2) . . ? C5 C4 C3 110.1(2) . . ? C6 C4 C3 109.7(2) . . ? C5 C4 C7 106.1(2) . . ? C6 C4 C7 108.4(2) . . ? C3 C4 C7 108.7(2) . . ? C12 C2 C3 109.1(2) . . ? C12 C2 C11 109.4(2) . . ? C3 C2 C11 108.1(2) . . ? C12 C2 C1 112.3(2) . . ? C3 C2 C1 107.5(2) . . ? C11 C2 C1 110.3(2) . . ? O1 C1 O2 122.2(3) . . ? O1 C1 C2 118.0(2) . . ? O2 C1 C2 119.7(2) . . ? C4 C6 C8 109.6(2) . . ? C4 C6 H6A 109.7 . . ? C8 C6 H6A 109.7 . . ? C4 C6 H6B 109.7 . . ? C8 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C10 C7 C4 110.0(2) . . ? C10 C7 H7A 109.7 . . ? C4 C7 H7A 109.7 . . ? C10 C7 H7B 109.7 . . ? C4 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O3 C5 O4 122.2(3) . . ? O3 C5 C4 125.2(2) . . ? O4 C5 C4 112.6(2) . . ? C2 C12 C8 110.2(2) . . ? C2 C12 H12A 109.6 . . ? C8 C12 H12A 109.6 . . ? C2 C12 H12B 109.6 . . ? C8 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C7 C10 C11 109.9(2) . . ? C7 C10 C9 109.2(3) . . ? C11 C10 C9 109.8(3) . . ? C7 C10 H10 109.3 . . ? C11 C10 H10 109.3 . . ? C9 C10 H10 109.3 . . ? C10 C11 C2 109.9(2) . . ? C10 C11 H11A 109.7 . . ? C2 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C2 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C9 C8 C12 109.6(3) . . ? C9 C8 C6 109.6(2) . . ? C12 C8 C6 109.4(2) . . ? C9 C8 H8 109.4 . . ? C12 C8 H8 109.4 . . ? C6 C8 H8 109.4 . . ? C8 C9 C10 109.4(2) . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C13 N1 C17 116.5(3) . . ? C13 N1 Ag1 122.7(2) . . ? C17 N1 Ag1 120.8(2) . . ? N1 C13 C14 123.7(3) . . ? N1 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C14 C15 C16 116.5(3) . . ? C14 C15 C18 122.1(3) . . ? C16 C15 C18 121.2(3) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C15 C18 C29 111.1(2) . . ? C15 C18 H18A 109.4 . . ? C29 C18 H18A 109.4 . . ? C15 C18 H18B 109.4 . . ? C29 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N1 C17 C16 123.5(3) . . ? N1 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C24 N2 C28 116.4(3) . . ? C24 N2 Ag1 125.0(2) . . ? C28 N2 Ag1 118.6(2) . . ? C27 C26 C25 116.2(3) . . ? C27 C26 C30 121.4(3) . 4_565 ? C25 C26 C30 122.5(3) . 4_565 ? C24 C25 C26 120.4(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? N2 C24 C25 123.4(3) . . ? N2 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? N2 C28 C27 123.4(3) . . ? N2 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C26 C30 C29 112.3(2) 4_666 . ? C26 C30 H30A 109.2 4_666 . ? C29 C30 H30A 109.2 . . ? C26 C30 H30B 109.2 4_666 . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C29 C18 113.9(3) . . ? C30 C29 H29A 108.8 . . ? C18 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C18 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C31 O5 H5 109.5 . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.621 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.058 # Attachment '4.cif.cif' data_xb2706 _database_code_depnum_ccdc_archive 'CCDC 727391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H48 Ag3 N4 O8, C12 H10 Ag N2, 2(H2 O)' _chemical_formula_sum 'C60 H62 Ag4 N6 O10' _chemical_formula_weight 1458.64 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 21.570(11) _cell_length_b 13.665(11) _cell_length_c 21.803(14) _cell_angle_alpha 90.00 _cell_angle_beta 118.245(19) _cell_angle_gamma 90.00 _cell_volume 5661(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 309 _cell_measurement_theta_min 2.982 _cell_measurement_theta_max 14.156 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7632 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14231 _diffrn_reflns_av_R_equivalents 0.1506 _diffrn_reflns_av_sigmaI/netI 0.2929 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.48 _reflns_number_total 5244 _reflns_number_gt 1551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0535P)^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 5244 _refine_ls_number_parameters 349 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1898 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 0.713 _refine_ls_restrained_S_all 0.713 _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 Ag1 Ag 1.0000 1.03340(8) 0.2500 0.0595(4) Uani 1 2 d S . . Ag2 Ag 1.08449(4) 1.02748(5) 0.17861(4) 0.0624(3) Uani 1 1 d . . . Ag3 Ag 1.0000 1.0000 0.0000 0.0667(4) Uani 1 2 d S . . O2 O 0.8458(4) 1.0326(6) 0.1758(4) 0.093(3) Uani 1 1 d . . . O3 O 0.9253(4) 1.0278(5) 0.1409(3) 0.063(2) Uani 1 1 d . . . O4 O 0.8657(4) 0.9895(6) -0.1048(4) 0.075(2) Uani 1 1 d . . . O5 O 0.7678(15) 1.011(2) -0.1802(15) 0.078(9) Uani 0.34 1 d P A 1 O5A O 0.7668(8) 0.9304(11) -0.1783(8) 0.091(5) Uani 0.66 1 d P A 2 C1 C 0.8641(6) 1.0267(7) 0.1293(5) 0.054(3) Uani 1 1 d . . . C2 C 0.8080(7) 0.9744(8) -0.1208(6) 0.054(3) Uani 1 1 d . . . N1 N 1.0720(4) 0.1889(3) 0.1868(3) 0.060(2) Uani 1 1 d G . . C11 C 1.1354(3) 0.2396(6) 0.2175(3) 0.085(4) Uani 1 1 d G . . H11A H 1.1777 0.2058 0.2331 0.102 Uiso 1 1 calc R . . C12 C 1.1357(4) 0.3406(6) 0.2248(4) 0.101(5) Uani 1 1 d G B . H12A H 1.1782 0.3745 0.2454 0.121 Uiso 1 1 calc R . . C13 C 1.0726(6) 0.3910(3) 0.2015(4) 0.082(4) Uani 1 1 d GD . . C14 C 1.0092(4) 0.3404(5) 0.1709(4) 0.084(4) Uani 1 1 d G B . H14A H 0.9670 0.3741 0.1553 0.101 Uiso 1 1 calc R . . C15 C 1.0089(3) 0.2393(5) 0.1635(3) 0.073(3) Uani 1 1 d G . . H15A H 0.9664 0.2055 0.1430 0.087 Uiso 1 1 calc R B . C16A C 1.0944(11) 0.4961(12) 0.2145(10) 0.037(5) Uiso 0.49 1 d PD B 2 H16B H 1.1413 0.5154 0.2356 0.045 Uiso 0.49 1 calc PR B 2 C16 C 1.0424(12) 0.4961(14) 0.1929(10) 0.069(7) Uani 0.51 1 d PDU B 1 H16A H 0.9946 0.5104 0.1698 0.083 Uiso 0.51 1 calc PR B 1 N2 N 1.0691(4) 0.8711(3) 0.1971(3) 0.059(2) Uani 1 1 d G . . C21 C 1.0049(3) 0.8227(6) 0.1644(3) 0.068(3) Uani 1 1 d G . . H21A H 0.9635 0.8581 0.1395 0.081 Uiso 1 1 calc R . . C22 C 1.0023(4) 0.7214(6) 0.1689(4) 0.082(4) Uani 1 1 d G B . H22A H 0.9593 0.6891 0.1470 0.098 Uiso 1 1 calc R . . C23 C 1.0641(6) 0.6686(3) 0.2062(4) 0.088(5) Uani 1 1 d GD . . C24 C 1.1284(4) 0.7170(6) 0.2389(3) 0.096(5) Uani 1 1 d G B . H24A H 1.1697 0.6816 0.2639 0.116 Uiso 1 1 calc R . . C25 C 1.1309(3) 0.8182(6) 0.2344(3) 0.073(3) Uani 1 1 d G . . H25A H 1.1739 0.8506 0.2563 0.088 Uiso 1 1 calc R B . C26A C 1.0408(11) 0.5607(13) 0.1934(10) 0.034(6) Uiso 0.48 1 d PD B 2 H26B H 0.9938 0.5417 0.1728 0.041 Uiso 0.48 1 calc PR B 2 C26 C 1.0915(12) 0.5622(14) 0.2218(11) 0.069(7) Uani 0.52 1 d PD B 1 H26A H 1.1388 0.5467 0.2492 0.083 Uiso 0.52 1 calc PR B 1 C30 C 0.8055(5) 1.0103(7) 0.0563(4) 0.047(3) Uani 1 1 d . A . C31 C 0.7550(5) 1.0991(7) 0.0326(5) 0.066(3) Uani 1 1 d . . . H31A H 0.7357 1.1088 0.0642 0.079 Uiso 1 1 calc R . . H31B H 0.7804 1.1578 0.0328 0.079 Uiso 1 1 calc R . . C32 C 0.6951(6) 1.0793(9) -0.0416(5) 0.071(4) Uani 1 1 d . A . H32A H 0.6627 1.1350 -0.0559 0.086 Uiso 1 1 calc R . . C33 C 0.6554(6) 0.9897(11) -0.0422(6) 0.101(5) Uani 1 1 d . . . H33A H 0.6159 0.9798 -0.0882 0.122 Uiso 1 1 calc R . . H33B H 0.6373 0.9967 -0.0093 0.122 Uiso 1 1 calc R . . C34 C 0.7052(6) 0.9031(8) -0.0223(6) 0.077(4) Uani 1 1 d . A . H34A H 0.6794 0.8432 -0.0240 0.093 Uiso 1 1 calc R . . C35 C 0.7662(5) 0.9166(7) 0.0520(5) 0.064(3) Uani 1 1 d . . . H35A H 0.7478 0.9192 0.0848 0.077 Uiso 1 1 calc R . . H35B H 0.7981 0.8614 0.0641 0.077 Uiso 1 1 calc R . . C36 C 0.8339(4) 1.0001(6) 0.0042(4) 0.054(3) Uani 1 1 d . . . H36A H 0.8663 0.9453 0.0180 0.065 Uiso 1 1 calc R A . H36B H 0.8603 1.0587 0.0063 0.065 Uiso 1 1 calc R . . C37 C 0.7768(5) 0.9846(7) -0.0715(5) 0.053(3) Uani 1 1 d . A . C38 C 0.7263(5) 1.0724(7) -0.0903(5) 0.063(3) Uani 1 1 d . . . H38A H 0.7517 1.1322 -0.0877 0.075 Uiso 1 1 calc R A . H38B H 0.6888 1.0653 -0.1378 0.075 Uiso 1 1 calc R . . C39 C 0.7358(5) 0.8930(8) -0.0724(5) 0.069(3) Uani 1 1 d . . . H39A H 0.7669 0.8367 -0.0592 0.083 Uiso 1 1 calc R A . H39B H 0.6980 0.8821 -0.1192 0.083 Uiso 1 1 calc R . . N3 N 1.0058(3) 0.8426(3) 0.0076(3) 0.051(2) Uani 1 1 d G . . C41 C 0.9460(2) 0.7859(4) -0.0297(3) 0.059(3) Uani 1 1 d G . . H41A H 0.9028 0.8159 -0.0571 0.071 Uiso 1 1 calc R . . C42 C 0.9507(3) 0.6845(4) -0.0261(3) 0.057(3) Uani 1 1 d G . . H42A H 0.9107 0.6465 -0.0510 0.069 Uiso 1 1 calc R . . C43 C 1.0152(3) 0.6397(3) 0.0149(3) 0.042(3) Uani 1 1 d G . . C44 C 1.0750(3) 0.6963(4) 0.0522(3) 0.051(3) Uani 1 1 d G . . H44A H 1.1181 0.6664 0.0797 0.061 Uiso 1 1 calc R . . C45 C 1.0703(3) 0.7978(4) 0.0486(3) 0.053(3) Uani 1 1 d G . . H45A H 1.1103 0.8357 0.0736 0.064 Uiso 1 1 calc R . . C46 C 1.0243(5) 0.5314(6) 0.0218(5) 0.057(3) Uani 1 1 d . . . H46A H 1.0655 0.5063 0.0579 0.068 Uiso 1 1 calc R . . O11 O 0.7202(7) 1.0644(12) 0.1789(7) 0.078(5) Uani 0.55 1 d P C 1 H11B H 0.7569 1.0568 0.1788 0.093 Uiso 0.55 1 d PR C 1 H11C H 0.7342 1.0557 0.2197 0.093 Uiso 0.55 1 d PR C 1 O11A O 0.7278(14) 1.0091(16) 0.1850(14) 0.120(12) Uiso 0.45 1 d P D 2 H11D H 0.7616 1.0127 0.1790 0.144 Uiso 0.45 1 d PR D 2 H11E H 0.7371 1.0114 0.2251 0.144 Uiso 0.45 1 d PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0505(8) 0.0749(9) 0.0429(7) 0.000 0.0137(6) 0.000 Ag2 0.0734(6) 0.0471(5) 0.0746(6) 0.0003(4) 0.0413(5) 0.0010(4) Ag3 0.0763(9) 0.0412(7) 0.0756(9) 0.0008(6) 0.0301(7) -0.0006(6) O2 0.059(5) 0.171(9) 0.037(5) -0.014(5) 0.014(4) 0.006(5) O3 0.041(4) 0.087(6) 0.051(5) 0.000(4) 0.013(4) 0.002(4) O4 0.070(6) 0.100(6) 0.082(6) -0.016(5) 0.058(5) -0.015(5) O5 0.054(16) 0.15(3) 0.039(15) 0.024(19) 0.028(13) 0.06(2) O5A 0.080(10) 0.137(13) 0.054(9) -0.040(11) 0.029(8) -0.051(11) C1 0.056(8) 0.061(7) 0.041(7) 0.002(6) 0.020(7) -0.004(6) C2 0.068(9) 0.065(8) 0.041(7) -0.020(7) 0.035(7) -0.014(8) N1 0.084(7) 0.041(5) 0.049(6) 0.009(4) 0.027(5) 0.011(5) C11 0.073(9) 0.069(9) 0.083(9) -0.023(7) 0.013(7) -0.012(7) C12 0.143(13) 0.061(9) 0.069(9) -0.014(7) 0.026(9) -0.008(9) C13 0.144(12) 0.033(6) 0.076(9) -0.018(6) 0.057(9) -0.006(8) C14 0.124(11) 0.032(6) 0.103(10) 0.020(7) 0.059(9) 0.027(7) C15 0.081(9) 0.070(8) 0.075(8) 0.023(7) 0.044(7) 0.024(7) C16 0.068(10) 0.052(9) 0.070(10) -0.013(8) 0.018(8) 0.014(8) N2 0.056(6) 0.054(5) 0.047(6) -0.004(4) 0.009(5) -0.003(5) C21 0.068(9) 0.071(8) 0.068(8) -0.011(7) 0.036(7) 0.000(7) C22 0.126(11) 0.054(7) 0.090(10) -0.010(7) 0.070(9) -0.019(8) C23 0.183(15) 0.038(7) 0.070(9) 0.011(7) 0.081(10) 0.010(9) C24 0.168(14) 0.053(8) 0.077(10) 0.025(7) 0.065(10) 0.019(8) C25 0.082(9) 0.076(9) 0.051(7) 0.007(6) 0.023(7) 0.007(7) C26 0.066(18) 0.061(16) 0.076(17) 0.028(14) 0.031(14) 0.015(14) C30 0.044(6) 0.052(6) 0.027(5) -0.003(5) 0.003(5) -0.001(5) C31 0.080(8) 0.056(7) 0.070(8) 0.007(6) 0.042(7) 0.014(6) C32 0.039(8) 0.117(11) 0.037(7) 0.006(7) 0.001(6) 0.034(7) C33 0.035(7) 0.176(15) 0.071(9) -0.015(10) 0.007(7) -0.010(10) C34 0.069(9) 0.083(9) 0.072(9) -0.008(7) 0.027(8) -0.037(7) C35 0.077(8) 0.062(8) 0.066(8) -0.006(6) 0.043(7) -0.018(6) C36 0.035(6) 0.052(6) 0.048(7) 0.015(5) -0.002(5) 0.005(5) C37 0.047(7) 0.063(7) 0.053(7) -0.011(6) 0.026(6) 0.009(6) C38 0.059(8) 0.075(8) 0.057(7) 0.008(6) 0.030(7) 0.010(6) C39 0.062(8) 0.093(10) 0.050(7) -0.017(6) 0.026(7) -0.008(7) N3 0.069(6) 0.033(4) 0.047(5) -0.002(4) 0.023(5) 0.009(4) C41 0.071(8) 0.038(6) 0.058(7) -0.005(5) 0.024(6) -0.007(6) C42 0.066(8) 0.038(6) 0.087(8) 0.003(6) 0.051(7) -0.004(5) C43 0.061(8) 0.030(5) 0.050(7) -0.003(5) 0.039(6) 0.006(5) C44 0.041(6) 0.029(5) 0.075(8) 0.002(5) 0.020(6) 0.006(5) C45 0.040(7) 0.054(7) 0.075(8) 0.002(6) 0.035(6) 0.007(5) C46 0.088(8) 0.023(5) 0.065(8) 0.001(5) 0.041(7) 0.007(5) O11 0.065(10) 0.127(16) 0.056(10) 0.029(10) 0.040(8) 0.044(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 Ag1 O3 2.152(6) 2_755 ? Ag1 O3 2.152(6) . ? Ag1 Ag2 2.9042(15) 2_755 ? Ag1 Ag2 2.9042(15) . ? Ag2 N2 2.229(5) . ? Ag2 N1 2.240(5) 1_565 ? Ag2 O4 2.333(7) 5_775 ? Ag3 N3 2.156(4) . ? Ag3 N3 2.156(4) 5_775 ? Ag3 O4 2.715(8) . ? O2 C1 1.254(11) . ? O3 C1 1.221(11) . ? O4 C2 1.140(11) . ? O4 Ag2 2.333(7) 5_775 ? O5 C2 1.27(2) . ? O5A C2 1.293(16) . ? C1 C30 1.509(12) . ? C2 C37 1.521(13) . ? N1 C11 1.3900 . ? N1 C15 1.3900 . ? N1 Ag2 2.240(5) 1_545 ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 C16A 1.494(18) . ? C13 C16 1.55(2) . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16A C26A 1.35(2) . ? C16A H16B 0.9300 . ? C16 C26 1.30(2) . ? C16 H16A 0.9300 . ? N2 C21 1.3900 . ? N2 C25 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.3900 . ? C23 C26A 1.539(19) . ? C23 C26 1.545(19) . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26A H26B 0.9300 . ? C26 H26A 0.9300 . ? C30 C35 1.514(11) . ? C30 C36 1.532(12) . ? C30 C31 1.547(11) . ? C31 C32 1.542(12) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.491(14) . ? C32 C38 1.506(12) . ? C32 H32A 0.9800 . ? C33 C34 1.517(14) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C39 1.528(12) . ? C34 C35 1.539(12) . ? C34 H34A 0.9800 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.537(11) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C39 1.527(12) . ? C37 C38 1.541(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? N3 C41 1.3900 . ? N3 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 C43 1.3900 . ? C42 H42A 0.9300 . ? C43 C44 1.3900 . ? C43 C46 1.491(9) . ? C44 C45 1.3900 . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C46 1.340(16) 5_765 ? C46 H46A 0.9300 . ? O11 H11B 0.8000 . ? O11 H11C 0.8000 . ? O11 H11D 1.1385 . ? O11 H11E 1.1497 . ? O11A H11B 0.9570 . ? O11A H11C 0.9485 . ? O11A H11D 0.7998 . ? O11A H11E 0.7999 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ag1 O3 176.0(3) 2_755 . ? O3 Ag1 Ag2 74.8(2) 2_755 2_755 ? O3 Ag1 Ag2 105.1(2) . 2_755 ? O3 Ag1 Ag2 105.1(2) 2_755 . ? O3 Ag1 Ag2 74.8(2) . . ? Ag2 Ag1 Ag2 176.80(5) 2_755 . ? N2 Ag2 N1 153.7(2) . 1_565 ? N2 Ag2 O4 100.7(2) . 5_775 ? N1 Ag2 O4 105.4(2) 1_565 5_775 ? N2 Ag2 Ag1 75.22(16) . . ? N1 Ag2 Ag1 78.46(17) 1_565 . ? O4 Ag2 Ag1 169.7(2) 5_775 . ? N3 Ag3 N3 180.0 . 5_775 ? N3 Ag3 O4 90.7(2) . . ? N3 Ag3 O4 89.3(2) 5_775 . ? C1 O3 Ag1 113.6(7) . . ? C2 O4 Ag2 124.2(8) . 5_775 ? C2 O4 Ag3 147.4(8) . . ? Ag2 O4 Ag3 85.9(3) 5_775 . ? O3 C1 O2 123.8(10) . . ? O3 C1 C30 120.3(10) . . ? O2 C1 C30 115.8(10) . . ? O4 C2 O5 111.0(18) . . ? O4 C2 O5A 122.1(13) . . ? O5 C2 O5A 51.1(12) . . ? O4 C2 C37 123.4(10) . . ? O5 C2 C37 111.5(15) . . ? O5A C2 C37 113.4(11) . . ? C11 N1 C15 120.0 . . ? C11 N1 Ag2 113.6(4) . 1_545 ? C15 N1 Ag2 126.4(4) . 1_545 ? N1 C11 C12 120.0 . . ? N1 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 C16A 104.0(10) . . ? C14 C13 C16A 135.9(10) . . ? C12 C13 C16 141.8(10) . . ? C14 C13 C16 98.1(10) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 N1 120.0 . . ? C14 C15 H15A 120.0 . . ? N1 C15 H15A 120.0 . . ? C26A C16A C13 115.0(17) . . ? C26A C16A H16B 122.5 . . ? C13 C16A H16B 122.5 . . ? C26 C16 C13 113(2) . . ? C26 C16 H16A 123.7 . . ? C13 C16 H16A 123.7 . . ? C21 N2 C25 120.0 . . ? C21 N2 Ag2 124.1(4) . . ? C25 N2 Ag2 114.9(5) . . ? C22 C21 N2 120.0 . . ? C22 C21 H21A 120.0 . . ? N2 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 C26A 135.2(10) . . ? C22 C23 C26A 104.6(10) . . ? C24 C23 C26 98.6(10) . . ? C22 C23 C26 141.1(10) . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 N2 120.0 . . ? C24 C25 H25A 120.0 . . ? N2 C25 H25A 120.0 . . ? C16A C26A C23 114.3(18) . . ? C16A C26A H26B 122.8 . . ? C23 C26A H26B 122.8 . . ? C16 C26 C23 114(2) . . ? C16 C26 H26A 123.0 . . ? C23 C26 H26A 123.0 . . ? C1 C30 C35 110.9(8) . . ? C1 C30 C36 111.5(8) . . ? C35 C30 C36 106.7(8) . . ? C1 C30 C31 110.0(8) . . ? C35 C30 C31 110.9(8) . . ? C36 C30 C31 106.8(7) . . ? C32 C31 C30 108.7(8) . . ? C32 C31 H31A 109.9 . . ? C30 C31 H31A 109.9 . . ? C32 C31 H31B 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? C33 C32 C38 112.9(10) . . ? C33 C32 C31 110.3(9) . . ? C38 C32 C31 108.5(9) . . ? C33 C32 H32A 108.3 . . ? C38 C32 H32A 108.3 . . ? C31 C32 H32A 108.3 . . ? C32 C33 C34 108.2(9) . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C33 C34 C39 110.7(10) . . ? C33 C34 C35 110.1(9) . . ? C39 C34 C35 108.6(9) . . ? C33 C34 H34A 109.1 . . ? C39 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C30 C35 C34 110.0(8) . . ? C30 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? C30 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C30 C36 C37 114.2(7) . . ? C30 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? C30 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C2 C37 C39 111.3(8) . . ? C2 C37 C36 111.9(8) . . ? C39 C37 C36 107.0(8) . . ? C2 C37 C38 112.1(9) . . ? C39 C37 C38 107.7(8) . . ? C36 C37 C38 106.5(7) . . ? C32 C38 C37 110.9(8) . . ? C32 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C37 C39 C34 111.1(8) . . ? C37 C39 H39A 109.4 . . ? C34 C39 H39A 109.4 . . ? C37 C39 H39B 109.4 . . ? C34 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C41 N3 C45 120.0 . . ? C41 N3 Ag3 120.5(3) . . ? C45 N3 Ag3 119.5(3) . . ? C42 C41 N3 120.0 . . ? C42 C41 H41A 120.0 . . ? N3 C41 H41A 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 C46 116.9(6) . . ? C42 C43 C46 123.1(6) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 N3 120.0 . . ? C44 C45 H45A 120.0 . . ? N3 C45 H45A 120.0 . . ? C46 C46 C43 122.8(11) 5_765 . ? C46 C46 H46A 118.6 5_765 . ? C43 C46 H46A 118.6 . . ? H11B O11 H11C 97.5 . . ? H11D O11A H11E 113.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.736 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.130 # Attachment '5.cif' data_j2 _database_code_depnum_ccdc_archive 'CCDC 727392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H23 Ag N2 O4, H2 O' _chemical_formula_sum 'C22 H25 Ag N2 O5' _chemical_formula_weight 505.31 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.498(2) _cell_length_b 6.9069(14) _cell_length_c 13.575(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.800(3) _cell_angle_gamma 90.00 _cell_volume 986.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4307 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1877 _reflns_number_gt 1583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0457P)^2^+3.7521P] 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 1877 _refine_ls_number_parameters 170 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 1.02285(5) 0.7500 0.94523(5) 0.0461(3) Uani 1 2 d S . . N1 N 0.8398(5) 0.7500 0.9617(5) 0.0370(14) Uani 1 2 d S . . N2 N 0.2205(5) 0.7500 0.9568(4) 0.0349(14) Uani 1 2 d S . . O1 O 0.9336(4) 0.5939(9) 0.7545(3) 0.0783(16) Uani 1 1 d . . . O2 O 0.4271(5) 0.7500 0.4669(5) 0.067(2) Uani 1 2 d S . . O3 O 0.4085(6) 0.7500 0.3001(5) 0.122(4) Uani 1 2 d S . . H3 H 0.3328 0.7500 0.2883 0.183 Uiso 1 2 calc SR . . O4 O 0.8352(5) 0.2500 0.7782(5) 0.082(2) Uani 1 2 d S . . H4WA H 0.8764 0.1650 0.7647 0.098 Uiso 1 1 d R . . C1 C 0.7362(7) 0.7500 0.8711(7) 0.071(3) Uani 1 2 d S . . H1 H 0.7459 0.7500 0.8063 0.085 Uiso 1 2 calc SR . . C2 C 0.6150(7) 0.7500 0.8673(7) 0.071(3) Uani 1 2 d S . . H2 H 0.5458 0.7500 0.8010 0.086 Uiso 1 2 calc SR . . C3 C 0.5954(6) 0.7500 0.9600(5) 0.0281(14) Uani 1 2 d S . . C4 C 0.7026(7) 0.7500 1.0532(6) 0.050(2) Uani 1 2 d S . . H4 H 0.6955 0.7500 1.1191 0.060 Uiso 1 2 calc SR . . C5 C 0.8216(6) 0.7500 1.0507(6) 0.050(2) Uani 1 2 d S . . H5 H 0.8925 0.7500 1.1159 0.060 Uiso 1 2 calc SR . . C6 C 0.3230(6) 0.7500 1.0475(6) 0.0395(17) Uani 1 2 d S . . H6 H 0.3122 0.7500 1.1118 0.047 Uiso 1 2 calc SR . . C7 C 0.4450(6) 0.7500 1.0529(5) 0.0384(17) Uani 1 2 d S . . H7 H 0.5138 0.7500 1.1194 0.046 Uiso 1 2 calc SR . . C8 C 0.4651(6) 0.7500 0.9592(5) 0.0264(13) Uani 1 2 d S . . C9 C 0.3585(6) 0.7500 0.8648(6) 0.044(2) Uani 1 2 d S . . H9 H 0.3668 0.7500 0.7994 0.053 Uiso 1 2 calc SR . . C10 C 0.2396(7) 0.7500 0.8659(6) 0.057(2) Uani 1 2 d S . . H10 H 0.1691 0.7500 0.8004 0.068 Uiso 1 2 calc SR . . C11 C 0.9036(7) 0.7500 0.7046(7) 0.069(3) Uani 1 2 d S . . C12 C 0.8317(7) 0.7500 0.5831(6) 0.070(3) Uani 1 2 d SD . . C13 C 0.6901(6) 0.7500 0.5551(5) 0.0296(14) Uani 1 2 d S . . H13A H 0.6676 0.8637 0.5856 0.035 Uiso 0.50 1 calc PR . . H13B H 0.6676 0.6363 0.5856 0.035 Uiso 0.50 1 calc PR . . C14 C 0.6164(6) 0.7500 0.4327(5) 0.0321(15) Uani 1 2 d S . . C15 C 0.4759(7) 0.7500 0.4035(6) 0.051(2) Uani 1 2 d S . . C16 C 0.6510(6) 0.9288(11) 0.3849(4) 0.069(2) Uani 1 1 d D . . H16A H 0.6036 0.9299 0.3074 0.082 Uiso 1 1 calc R . . H16B H 0.6293 1.0446 0.4142 0.082 Uiso 1 1 calc R . . C17 C 0.7914(7) 0.926(2) 0.4117(5) 0.152(6) Uani 1 1 d D . . H17 H 0.8136 1.0414 0.3813 0.182 Uiso 1 1 calc R . . C18 C 0.8636(7) 0.9304(18) 0.5357(5) 0.158(6) Uani 1 1 d D . . H18A H 0.9544 0.9362 0.5549 0.189 Uiso 1 1 calc R . . H18B H 0.8392 1.0446 0.5644 0.189 Uiso 1 1 calc R . . C19 C 0.8248(11) 0.7500 0.3639(9) 0.218(16) Uani 1 2 d S . . H19A H 0.9149 0.7500 0.3797 0.261 Uiso 1 2 calc SR . . H19B H 0.7780 0.7500 0.2864 0.261 Uiso 1 2 calc SR . . 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 0.0207(3) 0.0763(5) 0.0447(4) 0.000 0.0165(2) 0.000 N1 0.023(3) 0.052(4) 0.039(3) 0.000 0.015(3) 0.000 N2 0.023(3) 0.052(4) 0.031(3) 0.000 0.012(2) 0.000 O1 0.051(3) 0.137(5) 0.033(2) -0.006(3) 0.002(2) -0.006(3) O2 0.034(3) 0.131(6) 0.042(3) 0.000 0.020(3) 0.000 O3 0.030(3) 0.301(14) 0.031(3) 0.000 0.007(3) 0.000 O4 0.033(3) 0.146(7) 0.065(4) 0.000 0.017(3) 0.000 C1 0.026(4) 0.152(11) 0.036(4) 0.000 0.015(3) 0.000 C2 0.025(4) 0.156(11) 0.035(4) 0.000 0.015(3) 0.000 C3 0.019(3) 0.036(4) 0.029(3) 0.000 0.010(3) 0.000 C4 0.028(4) 0.096(7) 0.026(4) 0.000 0.011(3) 0.000 C5 0.017(3) 0.092(7) 0.035(4) 0.000 0.005(3) 0.000 C6 0.031(4) 0.059(5) 0.032(4) 0.000 0.016(3) 0.000 C7 0.025(3) 0.060(5) 0.028(4) 0.000 0.010(3) 0.000 C8 0.019(3) 0.029(3) 0.033(3) 0.000 0.013(3) 0.000 C9 0.019(3) 0.081(6) 0.031(4) 0.000 0.009(3) 0.000 C10 0.024(4) 0.107(8) 0.038(4) 0.000 0.010(3) 0.000 C11 0.021(4) 0.160(12) 0.023(4) 0.000 0.007(3) 0.000 C12 0.021(4) 0.162(11) 0.027(4) 0.000 0.009(3) 0.000 C13 0.027(3) 0.037(4) 0.027(3) 0.000 0.013(3) 0.000 C14 0.027(3) 0.040(4) 0.031(3) 0.000 0.014(3) 0.000 C15 0.031(4) 0.090(7) 0.026(4) 0.000 0.006(3) 0.000 C16 0.085(4) 0.075(5) 0.028(3) 0.011(3) 0.004(3) -0.035(4) C17 0.091(6) 0.312(16) 0.031(3) 0.031(6) 0.003(4) -0.132(9) C18 0.085(5) 0.336(16) 0.033(3) 0.022(6) 0.004(3) -0.136(8) C19 0.044(6) 0.59(5) 0.027(6) 0.000 0.017(5) 0.000 _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 N1 2.204(5) . ? Ag1 N2 2.214(5) 1_655 ? Ag1 O1 2.603(4) . ? N1 C5 1.308(9) . ? N1 C1 1.323(10) . ? N2 C6 1.316(9) . ? N2 C10 1.338(9) . ? N2 Ag1 2.214(5) 1_455 ? O1 C11 1.245(6) . ? O2 C15 1.203(9) . ? O3 C15 1.301(9) . ? O3 H3 0.8200 . ? O4 H4WA 0.8199 . ? C1 C2 1.373(11) . ? C1 H1 0.9300 . ? C2 C3 1.365(10) . ? C2 H2 0.9300 . ? C3 C4 1.364(9) . ? C3 C8 1.495(8) . ? C4 C5 1.382(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.375(9) . ? C6 H6 0.9300 . ? C7 C8 1.381(9) . ? C7 H7 0.9300 . ? C8 C9 1.370(9) . ? C9 C10 1.374(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O1 1.245(6) 4_575 ? C11 C12 1.517(11) . ? C12 C13 1.515(9) . ? C12 C18 1.514(9) 4_575 ? C12 C18 1.514(9) . ? C13 C14 1.531(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.500(9) . ? C14 C16 1.521(7) 4_575 ? C14 C16 1.521(7) . ? C16 C17 1.505(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C19 1.497(14) . ? C17 C18 1.549(8) . ? C17 H17 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C17 1.497(14) 4_575 ? C19 H19A 0.9700 . ? C19 H19B 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 N1 Ag1 N2 171.0(2) . 1_655 ? N1 Ag1 O1 95.24(17) . . ? N2 Ag1 O1 93.00(16) 1_655 . ? C5 N1 C1 116.0(6) . . ? C5 N1 Ag1 127.6(5) . . ? C1 N1 Ag1 116.4(5) . . ? C6 N2 C10 116.4(6) . . ? C6 N2 Ag1 124.9(5) . 1_455 ? C10 N2 Ag1 118.7(5) . 1_455 ? C11 O1 Ag1 95.4(5) . . ? C15 O3 H3 109.5 . . ? N1 C1 C2 123.7(7) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 120.5(7) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 115.6(6) . . ? C4 C3 C8 122.3(6) . . ? C2 C3 C8 122.1(6) . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 123.5(7) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 124.0(6) . . ? N2 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C6 C7 C8 119.8(6) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 116.3(6) . . ? C9 C8 C3 121.4(6) . . ? C7 C8 C3 122.2(6) . . ? C8 C9 C10 120.5(7) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N2 C10 C9 123.0(7) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? O1 C11 O1 119.9(8) 4_575 . ? O1 C11 C12 120.0(4) 4_575 . ? O1 C11 C12 120.0(4) . . ? C13 C12 C18 108.3(5) . 4_575 ? C13 C12 C18 108.3(5) . . ? C18 C12 C18 110.8(10) 4_575 . ? C13 C12 C11 109.4(6) . . ? C18 C12 C11 110.0(4) 4_575 . ? C18 C12 C11 110.0(4) . . ? C12 C13 C14 109.9(5) . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C16 109.1(4) . 4_575 ? C15 C14 C16 109.1(4) . . ? C16 C14 C16 108.6(7) 4_575 . ? C15 C14 C13 110.6(5) . . ? C16 C14 C13 109.8(4) 4_575 . ? C16 C14 C13 109.8(4) . . ? O2 C15 O3 121.8(7) . . ? O2 C15 C14 125.1(7) . . ? O3 C15 C14 113.2(6) . . ? C17 C16 C14 108.9(6) . . ? C17 C16 H16A 109.9 . . ? C14 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? C14 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C19 C17 C16 110.2(8) . . ? C19 C17 C18 111.7(11) . . ? C16 C17 C18 108.4(6) . . ? C19 C17 H17 108.9 . . ? C16 C17 H17 108.9 . . ? C18 C17 H17 108.9 . . ? C12 C18 C17 109.2(7) . . ? C12 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? C12 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? C17 C19 C17 108.3(9) . 4_575 ? C17 C19 H19A 110.0 . . ? C17 C19 H19A 110.0 4_575 . ? C17 C19 H19B 110.0 . . ? C17 C19 H19B 110.0 4_575 . ? H19A C19 H19B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.761 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.108 # Attachment '6.cif' data_xb2417 _database_code_depnum_ccdc_archive 'CCDC 727393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C10 H8 Ag N2), C12 H13 O4, 6(H2 O)' _chemical_formula_sum 'C32 H41 Ag2 N4 O10' _chemical_formula_weight 857.43 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 14.281(9) _cell_length_b 6.811(4) _cell_length_c 21.032(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.541(10) _cell_angle_gamma 90.00 _cell_volume 2011(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7552 _exptl_absorpt_correction_T_max 0.8289 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9376 _diffrn_reflns_av_R_equivalents 0.1211 _diffrn_reflns_av_sigmaI/netI 0.2325 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3793 _reflns_number_gt 1208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics APEX2 _computing_publication_material APEX2 _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^)+(0.0027P)^2^+0.0500P] 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 3793 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1606 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 0.82010(6) 0.2500 0.26078(3) 0.0865(4) Uani 1 2 d S . . Ag2 Ag 1.29309(6) 0.2500 0.77015(3) 0.1049(5) Uani 1 2 d S . . N1 N 0.9039(7) 0.2500 0.3591(4) 0.076(3) Uani 1 2 d S . . N2 N 0.7150(6) 0.2500 0.1688(4) 0.069(3) Uani 1 2 d S . . N3 N 0.3931(6) 0.2500 -0.1366(4) 0.065(3) Uani 1 2 d S . . N4 N 1.1996(8) 0.2500 0.6750(4) 0.090(3) Uani 1 2 d S . . C1 C 0.7490(7) 0.2500 0.1130(5) 0.082(4) Uani 1 2 d S . . H1A H 0.8144 0.2500 0.1145 0.098 Uiso 1 2 calc SR . . C2 C 0.6215(7) 0.2500 0.1658(4) 0.055(3) Uani 1 2 d S . . H2A H 0.5979 0.2500 0.2042 0.065 Uiso 1 2 calc SR . . C3 C 0.5570(7) 0.2500 0.1072(4) 0.065(3) Uani 1 2 d S . . H3A H 0.4920 0.2500 0.1077 0.077 Uiso 1 2 calc SR . . C4 C 0.6884(7) 0.2500 0.0538(4) 0.082(4) Uani 1 2 d S . . H4A H 0.7146 0.2500 0.0165 0.099 Uiso 1 2 calc SR . . C5 C 0.5882(7) 0.2500 0.0478(5) 0.059(3) Uani 1 2 d S . . C6 C 0.5190(6) 0.2500 -0.0167(4) 0.053(3) Uani 1 2 d S . . C7 C 0.4211(6) 0.2500 -0.0209(4) 0.072(4) Uani 1 2 d S . . H7A H 0.3955 0.2500 0.0167 0.086 Uiso 1 2 calc SR . . C8 C 0.3613(7) 0.2500 -0.0802(5) 0.071(4) Uani 1 2 d S . . H8A H 0.2959 0.2500 -0.0814 0.085 Uiso 1 2 calc SR . . C9 C 0.4908(9) 0.2500 -0.1325(4) 0.079(4) Uani 1 2 d S . . H9A H 0.5148 0.2500 -0.1708 0.095 Uiso 1 2 calc SR . . C10 C 0.5544(7) 0.2500 -0.0748(4) 0.069(3) Uani 1 2 d S . . H10A H 0.6197 0.2500 -0.0743 0.083 Uiso 1 2 calc SR . . C11 C 1.0604(7) 0.2500 0.4284(5) 0.081(4) Uani 1 2 d S . . H11A H 1.1260 0.2500 0.4304 0.097 Uiso 1 2 calc SR . . C12 C 0.9988(9) 0.2500 0.3683(4) 0.096(4) Uani 1 2 d S . . H12A H 1.0266 0.2500 0.3316 0.115 Uiso 1 2 calc SR . . C13 C 0.8647(7) 0.2500 0.4132(5) 0.070(4) Uani 1 2 d S . . H13A H 0.7987 0.2500 0.4091 0.084 Uiso 1 2 calc SR . . C14 C 0.9214(8) 0.2500 0.4751(4) 0.079(4) Uani 1 2 d S . . H14A H 0.8920 0.2500 0.5111 0.095 Uiso 1 2 calc SR . . C15 C 1.0233(7) 0.2500 0.4845(5) 0.065(4) Uani 1 2 d S . . C16 C 1.0820(7) 0.2500 0.5514(5) 0.066(4) Uani 1 2 d S . . C17 C 1.1812(7) 0.2500 0.5596(4) 0.082(4) Uani 1 2 d S . . H17A H 1.2101 0.2500 0.5234 0.099 Uiso 1 2 calc SR . . C18 C 1.2367(8) 0.2500 0.6197(6) 0.097(5) Uani 1 2 d S . . H18A H 1.3025 0.2500 0.6231 0.116 Uiso 1 2 calc SR . . C19 C 1.0463(7) 0.2500 0.6081(4) 0.074(4) Uani 1 2 d S . . H19A H 0.9806 0.2500 0.6058 0.088 Uiso 1 2 calc SR . . C20 C 1.1036(7) 0.2500 0.6671(4) 0.074(4) Uani 1 2 d S . . H20A H 1.0756 0.2500 0.7037 0.088 Uiso 1 2 calc SR . . O1 O -0.0385(4) 0.4131(9) 0.2091(3) 0.095(2) Uani 1 1 d . . . O2 O 0.3842(6) 0.4048(13) 0.2141(4) 0.202(4) Uani 1 1 d . . . C21 C 0.3427(11) 0.2500 0.1935(6) 0.122(6) Uani 1 2 d S . . C22 C 0.2457(8) 0.2500 0.1517(7) 0.102(5) Uani 1 2 d S . . C23 C 0.1686(6) 0.2500 0.1977(4) 0.090(4) Uani 1 2 d S . . H23A H 0.1752 0.3650 0.2246 0.107 Uiso 0.50 1 d PR . . C24 C 0.0687(7) 0.2500 0.1484(5) 0.060(3) Uani 1 2 d S . . C25 C -0.0102(9) 0.2500 0.1921(6) 0.076(5) Uani 1 2 d S . . C26 C 0.0573(5) 0.0681(13) 0.1068(3) 0.093(3) Uani 1 1 d . . . H26A H -0.0052 0.0671 0.0794 0.112 Uiso 1 1 calc R . . H26B H 0.0631 -0.0480 0.1340 0.112 Uiso 1 1 calc R . . C27 C 0.1373(6) 0.0661(14) 0.0634(4) 0.099(3) Uani 1 1 d . . . H27A H 0.1302 -0.0523 0.0365 0.119 Uiso 1 1 calc R . . C28 C 0.2352(5) 0.0642(14) 0.1077(3) 0.095(3) Uani 1 1 d . . . H28A H 0.2849 0.0632 0.0818 0.114 Uiso 1 1 calc R . . H28B H 0.2419 -0.0532 0.1342 0.114 Uiso 1 1 calc R . . C29 C 0.1248(9) 0.2500 0.0193(6) 0.104(4) Uani 1 2 d S . . H29A H 0.0621 0.2500 -0.0078 0.125 Uiso 1 2 calc SR . . H29B H 0.1721 0.2500 -0.0085 0.125 Uiso 1 2 calc SR . . O11 O 0.8583(5) 0.7500 0.1598(3) 0.097(3) Uani 1 2 d S . . O12 O 0.6326(19) 0.2500 0.372(3) 0.32(3) Uani 0.42 2 d SP A 1 O12A O 0.641(3) 0.2500 0.3440(18) 0.40(4) Uani 0.58 2 d SP B 2 O13 O 0.5419(5) 0.5534(12) 0.2930(3) 0.179(3) Uani 1 1 d . . . O14 O 0.2951(8) 0.7500 0.2606(6) 0.251(6) Uani 1 2 d S . . O15 O 0.1097(9) 0.7500 0.2832(5) 0.291(7) Uani 1 2 d S . . H11C H 0.8945 0.6542 0.1790 0.349 Uiso 1 1 d R . . H14C H 0.3260 0.6539 0.2489 0.349 Uiso 1 1 d R . . H15C H 0.0748 0.6658 0.2662 0.349 Uiso 1 1 d R . . H12B H 0.6128 0.3390 0.3436 0.349 Uiso 0.42 1 d PR C 1 H12D H 0.6447 0.3349 0.3086 0.349 Uiso 0.58 1 d PR D 2 H13C H 0.4967 0.5017 0.2730 0.349 Uiso 1 1 d R . . H13D H 0.5186 0.5493 0.3257 0.349 Uiso 1 1 d 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 0.0755(6) 0.1195(11) 0.0520(5) 0.000 -0.0218(4) 0.000 Ag2 0.1134(8) 0.1135(11) 0.0646(6) 0.000 -0.0453(5) 0.000 N1 0.075(7) 0.097(9) 0.049(5) 0.000 -0.010(5) 0.000 N2 0.053(6) 0.083(9) 0.057(6) 0.000 -0.023(5) 0.000 N3 0.064(6) 0.060(8) 0.064(6) 0.000 -0.009(5) 0.000 N4 0.104(8) 0.080(10) 0.069(7) 0.000 -0.025(6) 0.000 C1 0.053(7) 0.125(13) 0.053(7) 0.000 -0.033(6) 0.000 C2 0.052(7) 0.047(9) 0.058(7) 0.000 -0.007(5) 0.000 C3 0.092(8) 0.056(10) 0.038(6) 0.000 -0.009(6) 0.000 C4 0.065(8) 0.117(12) 0.066(7) 0.000 0.016(6) 0.000 C5 0.054(7) 0.054(10) 0.060(7) 0.000 -0.012(6) 0.000 C6 0.050(6) 0.053(9) 0.046(6) 0.000 -0.023(5) 0.000 C7 0.057(7) 0.113(12) 0.037(6) 0.000 -0.012(5) 0.000 C8 0.046(6) 0.110(12) 0.050(6) 0.000 -0.008(5) 0.000 C9 0.102(10) 0.097(11) 0.032(6) 0.000 -0.005(6) 0.000 C10 0.073(7) 0.076(11) 0.050(6) 0.000 -0.010(6) 0.000 C11 0.057(7) 0.119(13) 0.061(7) 0.000 -0.005(6) 0.000 C12 0.087(9) 0.152(14) 0.040(6) 0.000 -0.009(6) 0.000 C13 0.056(7) 0.063(10) 0.076(7) 0.000 -0.027(6) 0.000 C14 0.111(10) 0.076(11) 0.045(7) 0.000 0.004(7) 0.000 C15 0.057(7) 0.078(11) 0.048(7) 0.000 -0.020(6) 0.000 C16 0.050(7) 0.067(10) 0.067(7) 0.000 -0.027(6) 0.000 C17 0.077(8) 0.093(11) 0.063(7) 0.000 -0.025(6) 0.000 C18 0.080(9) 0.110(14) 0.087(9) 0.000 -0.022(8) 0.000 C19 0.070(7) 0.112(12) 0.030(6) 0.000 -0.013(5) 0.000 C20 0.059(7) 0.098(11) 0.055(7) 0.000 -0.014(5) 0.000 O1 0.113(4) 0.075(7) 0.102(4) 0.010(4) 0.031(3) 0.013(4) O2 0.160(7) 0.181(10) 0.220(8) -0.030(6) -0.087(6) -0.017(6) C21 0.099(13) 0.18(2) 0.080(9) 0.000 -0.006(8) 0.000 C22 0.068(9) 0.114(16) 0.114(10) 0.000 -0.012(8) 0.000 C23 0.024(6) 0.172(14) 0.069(6) 0.000 0.001(5) 0.000 C24 0.061(7) 0.077(12) 0.042(6) 0.000 0.007(6) 0.000 C25 0.074(10) 0.051(15) 0.084(10) 0.000 -0.035(9) 0.000 C26 0.078(6) 0.134(10) 0.072(5) -0.003(6) 0.024(4) -0.006(6) C27 0.104(7) 0.083(9) 0.108(7) -0.008(6) 0.014(6) 0.012(6) C28 0.087(6) 0.094(9) 0.104(6) -0.021(6) 0.020(5) 0.006(6) C29 0.131(11) 0.085(14) 0.097(9) 0.000 0.025(8) 0.000 O11 0.084(5) 0.116(8) 0.081(5) 0.000 -0.013(4) 0.000 O12 0.046(15) 0.42(8) 0.46(7) 0.000 -0.07(3) 0.000 O12A 0.58(7) 0.028(17) 0.40(4) 0.000 -0.39(4) 0.000 O13 0.159(6) 0.210(8) 0.143(5) 0.011(5) -0.040(4) -0.033(6) O14 0.154(11) 0.302(18) 0.311(15) 0.000 0.075(10) 0.000 O15 0.226(14) 0.39(2) 0.284(14) 0.000 0.106(12) 0.000 _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 N1 2.191(8) . ? Ag1 N2 2.221(7) . ? Ag2 N4 2.193(8) . ? Ag2 N3 2.205(8) 1_656 ? N1 C12 1.334(12) . ? N1 C13 1.357(11) . ? N2 C2 1.327(10) . ? N2 C1 1.348(10) . ? N3 C8 1.345(10) . ? N3 C9 1.382(12) . ? N3 Ag2 2.205(8) 1_454 ? N4 C20 1.351(12) . ? N4 C18 1.362(12) . ? C1 C4 1.380(11) . ? C1 H1A 0.9300 . ? C2 C3 1.397(10) . ? C2 H2A 0.9300 . ? C3 C5 1.402(11) . ? C3 H3A 0.9300 . ? C4 C5 1.414(12) . ? C4 H4A 0.9300 . ? C5 C6 1.525(10) . ? C6 C7 1.386(12) . ? C6 C10 1.405(11) . ? C7 C8 1.377(10) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.377(11) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C15 1.380(11) . ? C11 C12 1.402(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.402(11) . ? C13 H13A 0.9300 . ? C14 C15 1.432(13) . ? C14 H14A 0.9300 . ? C15 C16 1.501(10) . ? C16 C19 1.379(11) . ? C16 C17 1.396(12) . ? C17 C18 1.363(12) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.355(10) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? O1 C25 1.256(8) . ? O2 C21 1.248(8) . ? C21 O2 1.248(8) 4_565 ? C21 C22 1.499(16) . ? C22 C28 1.559(8) . ? C22 C28 1.559(8) 4_565 ? C22 C23 1.593(14) . ? C23 C24 1.604(11) . ? C23 H23A 0.9600 . ? C24 C26 1.508(8) . ? C24 C26 1.508(8) 4_565 ? C24 C25 1.579(17) . ? C25 O1 1.256(8) 4_565 ? C26 C27 1.587(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.532(9) . ? C27 C29 1.550(9) . ? C27 H27A 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C27 1.550(9) 4_565 ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? O11 H11C 0.8835 . ? O12 H12B 0.8651 . ? O12A H12B 0.7295 . ? O12A H12D 0.9508 . ? O13 H13C 0.7850 . ? O13 H13D 0.8188 . ? O14 H14C 0.8501 . ? O15 H15C 0.8000 . ? 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 N1 Ag1 N2 170.9(4) . . ? N4 Ag2 N3 177.2(4) . 1_656 ? C12 N1 C13 116.2(9) . . ? C12 N1 Ag1 120.2(7) . . ? C13 N1 Ag1 123.6(7) . . ? C2 N2 C1 118.6(8) . . ? C2 N2 Ag1 123.7(7) . . ? C1 N2 Ag1 117.7(6) . . ? C8 N3 C9 116.4(8) . . ? C8 N3 Ag2 121.1(7) . 1_454 ? C9 N3 Ag2 122.5(7) . 1_454 ? C20 N4 C18 116.0(10) . . ? C20 N4 Ag2 123.2(8) . . ? C18 N4 Ag2 120.8(8) . . ? N2 C1 C4 121.3(9) . . ? N2 C1 H1A 119.4 . . ? C4 C1 H1A 119.4 . . ? N2 C2 C3 122.5(9) . . ? N2 C2 H2A 118.7 . . ? C3 C2 H2A 118.7 . . ? C2 C3 C5 121.3(9) . . ? C2 C3 H3A 119.3 . . ? C5 C3 H3A 119.3 . . ? C1 C4 C5 122.6(10) . . ? C1 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? C3 C5 C4 113.7(9) . . ? C3 C5 C6 122.2(8) . . ? C4 C5 C6 124.1(9) . . ? C7 C6 C10 117.7(8) . . ? C7 C6 C5 122.6(9) . . ? C10 C6 C5 119.7(8) . . ? C8 C7 C6 120.6(9) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? N3 C8 C7 123.0(9) . . ? N3 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? C10 C9 N3 123.4(9) . . ? C10 C9 H9A 118.3 . . ? N3 C9 H9A 118.3 . . ? C9 C10 C6 118.9(9) . . ? C9 C10 H10A 120.6 . . ? C6 C10 H10A 120.6 . . ? C15 C11 C12 119.7(10) . . ? C15 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? N1 C12 C11 125.8(10) . . ? N1 C12 H12A 117.1 . . ? C11 C12 H12A 117.1 . . ? N1 C13 C14 121.5(10) . . ? N1 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C13 C14 C15 121.9(10) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C11 C15 C14 114.9(9) . . ? C11 C15 C16 124.5(9) . . ? C14 C15 C16 120.6(9) . . ? C19 C16 C17 114.9(9) . . ? C19 C16 C15 125.4(9) . . ? C17 C16 C15 119.7(10) . . ? C18 C17 C16 121.3(11) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? N4 C18 C17 122.7(11) . . ? N4 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C20 C19 C16 122.3(10) . . ? C20 C19 H19A 118.9 . . ? C16 C19 H19A 118.9 . . ? N4 C20 C19 122.8(10) . . ? N4 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? O2 C21 O2 115.3(15) . 4_565 ? O2 C21 C22 122.3(8) . . ? O2 C21 C22 122.3(8) 4_565 . ? C21 C22 C28 109.0(7) . . ? C21 C22 C28 109.0(7) . 4_565 ? C28 C22 C28 108.5(11) . 4_565 ? C21 C22 C23 108.1(10) . . ? C28 C22 C23 111.1(6) . . ? C28 C22 C23 111.1(6) 4_565 . ? C22 C23 C24 103.8(8) . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23A 111.2 . . ? C26 C24 C26 110.5(8) . 4_565 ? C26 C24 C25 109.0(6) . . ? C26 C24 C25 109.0(6) 4_565 . ? C26 C24 C23 111.3(6) . . ? C26 C24 C23 111.3(6) 4_565 . ? C25 C24 C23 105.6(8) . . ? O1 C25 O1 124.3(16) 4_565 . ? O1 C25 C24 117.8(8) 4_565 . ? O1 C25 C24 117.8(8) . . ? C24 C26 C27 109.2(8) . . ? C24 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? C24 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C28 C27 C29 111.3(8) . . ? C28 C27 C26 108.9(6) . . ? C29 C27 C26 108.8(8) . . ? C28 C27 H27A 109.3 . . ? C29 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C27 C28 C22 109.3(8) . . ? C27 C28 H28A 109.8 . . ? C22 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? C22 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? C27 C29 C27 107.8(10) . 4_565 ? C27 C29 H29A 110.1 . . ? C27 C29 H29A 110.1 4_565 . ? C27 C29 H29B 110.1 . . ? C27 C29 H29B 110.1 4_565 . ? H29A C29 H29B 108.5 . . ? H12B O12A H12D 66.1 . . ? H13C O13 H13D 90.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C12 180.000(4) . . . . ? N2 Ag1 N1 C13 0.000(4) . . . . ? N1 Ag1 N2 C2 0.000(2) . . . . ? N1 Ag1 N2 C1 180.000(1) . . . . ? N3 Ag2 N4 C20 180.00(3) 1_656 . . . ? N3 Ag2 N4 C18 0.00(3) 1_656 . . . ? C2 N2 C1 C4 0.0 . . . . ? Ag1 N2 C1 C4 180.0 . . . . ? C1 N2 C2 C3 0.0 . . . . ? Ag1 N2 C2 C3 180.0 . . . . ? N2 C2 C3 C5 0.0 . . . . ? N2 C1 C4 C5 0.0 . . . . ? C2 C3 C5 C4 0.0 . . . . ? C2 C3 C5 C6 180.0 . . . . ? C1 C4 C5 C3 0.0 . . . . ? C1 C4 C5 C6 180.0 . . . . ? C3 C5 C6 C7 0.0 . . . . ? C4 C5 C6 C7 180.0 . . . . ? C3 C5 C6 C10 180.0 . . . . ? C4 C5 C6 C10 0.0 . . . . ? C10 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C8 180.0 . . . . ? C9 N3 C8 C7 0.0 . . . . ? Ag2 N3 C8 C7 180.0 1_454 . . . ? C6 C7 C8 N3 0.0 . . . . ? C8 N3 C9 C10 0.0 . . . . ? Ag2 N3 C9 C10 180.0 1_454 . . . ? N3 C9 C10 C6 0.0 . . . . ? C7 C6 C10 C9 0.0 . . . . ? C5 C6 C10 C9 180.0 . . . . ? C13 N1 C12 C11 0.000(2) . . . . ? Ag1 N1 C12 C11 180.000(2) . . . . ? C15 C11 C12 N1 0.000(2) . . . . ? C12 N1 C13 C14 0.000(2) . . . . ? Ag1 N1 C13 C14 180.000(2) . . . . ? N1 C13 C14 C15 0.000(3) . . . . ? C12 C11 C15 C14 0.000(2) . . . . ? C12 C11 C15 C16 180.000(2) . . . . ? C13 C14 C15 C11 0.000(3) . . . . ? C13 C14 C15 C16 180.000(2) . . . . ? C11 C15 C16 C19 180.000(3) . . . . ? C14 C15 C16 C19 0.000(3) . . . . ? C11 C15 C16 C17 0.000(3) . . . . ? C14 C15 C16 C17 180.000(3) . . . . ? C19 C16 C17 C18 0.000(4) . . . . ? C15 C16 C17 C18 180.000(3) . . . . ? C20 N4 C18 C17 0.000(4) . . . . ? Ag2 N4 C18 C17 180.000(3) . . . . ? C16 C17 C18 N4 0.000(4) . . . . ? C17 C16 C19 C20 0.000(3) . . . . ? C15 C16 C19 C20 180.000(3) . . . . ? C18 N4 C20 C19 0.000(4) . . . . ? Ag2 N4 C20 C19 180.000(3) . . . . ? C16 C19 C20 N4 0.000(4) . . . . ? O2 C21 C22 C28 152.0(14) . . . . ? O2 C21 C22 C28 -34(2) 4_565 . . . ? O2 C21 C22 C28 34(2) . . . 4_565 ? O2 C21 C22 C28 -152.0(14) 4_565 . . 4_565 ? O2 C21 C22 C23 -87.2(15) . . . . ? O2 C21 C22 C23 87.2(15) 4_565 . . . ? C21 C22 C23 C24 180.0 . . . . ? C28 C22 C23 C24 -60.4(7) . . . . ? C28 C22 C23 C24 60.4(7) 4_565 . . . ? C22 C23 C24 C26 61.9(7) . . . . ? C22 C23 C24 C26 -61.9(7) . . . 4_565 ? C22 C23 C24 C25 180.0 . . . . ? C26 C24 C25 O1 30.7(11) . . . 4_565 ? C26 C24 C25 O1 151.3(8) 4_565 . . 4_565 ? C23 C24 C25 O1 -89.0(8) . . . 4_565 ? C26 C24 C25 O1 -151.3(8) . . . . ? C26 C24 C25 O1 -30.7(11) 4_565 . . . ? C23 C24 C25 O1 89.0(8) . . . . ? C26 C24 C26 C27 61.0(10) 4_565 . . . ? C25 C24 C26 C27 -179.3(6) . . . . ? C23 C24 C26 C27 -63.3(9) . . . . ? C24 C26 C27 C28 60.5(9) . . . . ? C24 C26 C27 C29 -61.0(8) . . . . ? C29 C27 C28 C22 60.5(10) . . . . ? C26 C27 C28 C22 -59.4(10) . . . . ? C21 C22 C28 C27 -178.4(8) . . . . ? C28 C22 C28 C27 -59.8(11) 4_565 . . . ? C23 C22 C28 C27 62.6(10) . . . . ? C28 C27 C29 C27 -58.7(11) . . . 4_565 ? C26 C27 C29 C27 61.2(11) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.203 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.093 # Attachment '7.cif' data_xb2552 _database_code_depnum_ccdc_archive 'CCDC 727394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H108 Ag8 N20 O16, 2(C2 H6 O), 6(H2 O)' _chemical_formula_sum 'C112 H132 Ag8 N20 O24' _chemical_formula_weight 3005.34 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' _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 14.555(3) _cell_length_b 14.801(3) _cell_length_c 15.930(5) _cell_angle_alpha 110.220(5) _cell_angle_beta 104.945(5) _cell_angle_gamma 106.456(3) _cell_volume 2836.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1540 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 18.243 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6815 _exptl_absorpt_correction_T_max 0.7928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15535 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.1529 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10898 _reflns_number_gt 4413 _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^)+(0.0878P)^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 10898 _refine_ls_number_parameters 745 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_restrained_S_all 0.826 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.60297(5) 0.51470(6) 0.55596(6) 0.0585(2) Uani 1 1 d . . . Ag2 Ag 0.75197(5) 0.15501(5) 0.84295(5) 0.0548(2) Uani 1 1 d . . . Ag3 Ag 0.88253(6) 0.05556(6) 0.76986(5) 0.0586(2) Uani 1 1 d . . . Ag4 Ag 0.59646(6) 0.19989(7) 0.92772(6) 0.0753(3) Uani 1 1 d . . . O1 O 0.9291(5) 0.1679(5) 0.7170(5) 0.075(2) Uani 1 1 d . . . O2 O 0.7925(6) 0.2026(6) 0.7163(5) 0.087(2) Uani 1 1 d . . . O3 O 0.6966(5) 0.4099(5) 0.4957(5) 0.084(2) Uani 1 1 d . . . O4 O 0.7939(5) 0.5394(5) 0.6396(5) 0.085(2) Uani 1 1 d . . . O5 O 0.5321(7) 0.2328(6) 0.8121(5) 0.087(2) Uani 1 1 d . A . O6 O 0.4040(9) 0.0989(8) 0.7941(7) 0.077(3) Uani 0.61 1 d PD A 1 O6A O 0.3735(17) 0.2002(18) 0.8418(17) 0.124(8) Uiso 0.39 1 d PD A 2 O7 O 0.4999(5) 0.4205(6) 0.6090(5) 0.080(2) Uani 1 1 d . . . O8 O 0.3677(6) 0.3418(5) 0.4667(5) 0.087(2) Uani 1 1 d . . . O9 O 0.3122(14) 0.4241(13) 1.0133(12) 0.235(8) Uani 1 1 d . C . H9C H 0.3257 0.4472 1.0705 0.282 Uiso 1 1 d R . . N1 N 0.8911(5) 0.2613(5) 0.9691(5) 0.051(2) Uani 1 1 d . . . N2 N 0.8309(5) -0.0570(6) 0.8210(5) 0.0472(18) Uani 1 1 d . . . N3 N 0.8656(6) -0.0839(6) 1.0502(5) 0.059(2) Uani 1 1 d . . . H3C H 0.8481 -0.1388 1.0598 0.071 Uiso 1 1 calc R . . N4 N 0.9490(5) 0.0995(7) 1.1268(5) 0.0505(19) Uani 1 1 d . . . N5 N 1.0435(6) 0.2817(7) 1.2013(6) 0.066(2) Uani 1 1 d . . . H5C H 1.0914 0.3353 1.2536 0.079 Uiso 1 1 calc R . . N6 N 0.6129(5) 0.0201(6) 0.7333(5) 0.0479(18) Uani 1 1 d . . . N7 N 0.6539(6) 0.1502(8) 1.0325(6) 0.069(2) Uani 1 1 d . . . N8 N 0.6133(7) -0.1050(11) 1.0312(8) 0.090(3) Uani 1 1 d . . . H8C H 0.6310 -0.1220 1.0774 0.107 Uiso 1 1 calc R . . N9 N 0.4563(6) -0.2478(6) 0.6920(6) 0.068(2) Uani 1 1 d . . . H9D H 0.4106 -0.3037 0.6403 0.082 Uiso 1 1 calc R . . N10 N 0.5337(6) -0.1769(7) 0.8592(7) 0.068(2) Uani 1 1 d . . . C1 C 0.8709(8) 0.2115(7) 0.6970(6) 0.050(2) Uani 1 1 d . . . C2 C 0.9033(6) 0.2836(6) 0.6476(6) 0.043(2) Uani 1 1 d . . . C3 C 1.0133(6) 0.3668(7) 0.7070(6) 0.048(2) Uani 1 1 d . . . H3A H 1.0613 0.3335 0.7148 0.057 Uiso 1 1 calc R . . H3B H 1.0193 0.4113 0.7712 0.057 Uiso 1 1 calc R . . C4 C 1.0402(6) 0.4330(7) 0.6559(7) 0.052(2) Uani 1 1 d . . . H4A H 1.1122 0.4863 0.6940 0.062 Uiso 1 1 calc R . . C5 C 1.0309(7) 0.3620(8) 0.5564(8) 0.073(3) Uani 1 1 d . . . H5A H 1.0784 0.3280 0.5635 0.088 Uiso 1 1 calc R . . H5B H 1.0500 0.4040 0.5235 0.088 Uiso 1 1 calc R . . C6 C 0.8932(6) 0.2131(6) 0.5458(6) 0.047(2) Uani 1 1 d . . . H6A H 0.9399 0.1780 0.5515 0.056 Uiso 1 1 calc R . . H6B H 0.8224 0.1595 0.5080 0.056 Uiso 1 1 calc R . . C7 C 0.9198(7) 0.2787(7) 0.4959(7) 0.054(2) Uani 1 1 d . . . H7A H 0.9153 0.2334 0.4319 0.064 Uiso 1 1 calc R . . C8 C 0.9667(6) 0.4880(6) 0.6457(6) 0.047(2) Uani 1 1 d . . . H8A H 0.9703 0.5303 0.7094 0.056 Uiso 1 1 calc R . . H8B H 0.9879 0.5347 0.6174 0.056 Uiso 1 1 calc R . . C9 C 0.8463(7) 0.3335(6) 0.4823(6) 0.050(2) Uani 1 1 d . . . H9A H 0.8643 0.3738 0.4476 0.060 Uiso 1 1 calc R . . H9B H 0.7750 0.2812 0.4441 0.060 Uiso 1 1 calc R . . C10 C 0.8557(6) 0.4066(6) 0.5812(6) 0.0373(19) Uani 1 1 d . . . C11 C 0.8290(6) 0.3398(6) 0.6346(5) 0.049(2) Uani 1 1 d . . . H11A H 0.7576 0.2872 0.5977 0.059 Uiso 1 1 calc R . . H11B H 0.8342 0.3851 0.6981 0.059 Uiso 1 1 calc R . . C12 C 0.7788(7) 0.4568(7) 0.5704(7) 0.049(2) Uani 1 1 d . . . C13 C 0.4129(9) 0.3505(8) 0.5489(8) 0.062(3) Uani 1 1 d . . . C14 C 0.3578(6) 0.2719(7) 0.5767(6) 0.049(2) Uani 1 1 d D . . C15 C 0.2987(10) 0.1636(9) 0.4944(8) 0.118(5) Uani 1 1 d DU . . H15A H 0.3470 0.1337 0.4790 0.141 Uiso 1 1 calc R . . H15B H 0.2591 0.1669 0.4372 0.141 Uiso 1 1 calc R . . C16 C 0.4283(7) 0.2665(7) 0.6616(6) 0.062(3) Uani 1 1 d D . . H16A H 0.4651 0.3363 0.7167 0.075 Uiso 1 1 calc R . . H16B H 0.4798 0.2438 0.6437 0.075 Uiso 1 1 calc R . . C17 C 0.2865(11) 0.3174(12) 0.6179(12) 0.151(6) Uani 1 1 d DU . . H17A H 0.2344 0.3178 0.5660 0.181 Uiso 1 1 calc R . . H17B H 0.3282 0.3899 0.6675 0.181 Uiso 1 1 calc R . . C18 C 0.2280(11) 0.2492(12) 0.6650(11) 0.129(5) Uani 1 1 d DU . . H18A H 0.1843 0.2795 0.6919 0.155 Uiso 1 1 calc R . . C19 C 0.1659(10) 0.1511(12) 0.5771(9) 0.129(5) Uani 1 1 d D . . H19A H 0.1238 0.1667 0.5306 0.155 Uiso 1 1 calc R . . H19B H 0.1180 0.1054 0.5925 0.155 Uiso 1 1 calc R . . C20 C 0.2168(10) 0.0857(10) 0.5237(9) 0.116(5) Uani 1 1 d DU . . H20A H 0.1675 0.0168 0.4692 0.139 Uiso 1 1 calc R . . C21 C 0.3042(9) 0.0806(7) 0.6081(7) 0.084(3) Uani 1 1 d D . . H21A H 0.2702 0.0320 0.6299 0.100 Uiso 1 1 calc R . . H21B H 0.3506 0.0556 0.5823 0.100 Uiso 1 1 calc R . . C23 C 0.2941(14) 0.2265(13) 0.7334(12) 0.158(7) Uani 1 1 d D . . H23A H 0.2513 0.1727 0.7453 0.190 Uiso 1 1 calc R . . H23B H 0.3352 0.2898 0.7950 0.190 Uiso 1 1 calc R . . C22 C 0.3649(7) 0.1886(7) 0.6914(6) 0.054(2) Uani 1 1 d D A . C24 C 0.4359(11) 0.1829(11) 0.7779(8) 0.095(4) Uani 1 1 d D . . C25 C 0.9605(8) 0.3423(8) 0.9673(7) 0.079(3) Uani 1 1 d . . . H25A H 0.9440 0.3552 0.9134 0.095 Uiso 1 1 calc R . . C26 C 1.0551(9) 0.4060(9) 1.0440(9) 0.092(4) Uani 1 1 d . . . H26A H 1.1004 0.4650 1.0444 0.110 Uiso 1 1 calc R . . C27 C 1.0827(8) 0.3819(9) 1.1206(8) 0.080(3) Uani 1 1 d . . . H27A H 1.1485 0.4223 1.1709 0.096 Uiso 1 1 calc R . . C28 C 1.0136(7) 0.2985(8) 1.1228(7) 0.055(2) Uani 1 1 d . . . C29 C 0.9205(7) 0.2423(7) 1.0442(6) 0.051(2) Uani 1 1 d . . . H29A H 0.8729 0.1847 1.0436 0.061 Uiso 1 1 calc R . . C30 C 1.0077(8) 0.1917(10) 1.2078(7) 0.070(3) Uani 1 1 d . . . C31 C 1.0294(8) 0.1950(10) 1.3006(7) 0.083(4) Uani 1 1 d . . . H31A H 1.0664 0.2589 1.3569 0.099 Uiso 1 1 calc R . . C32 C 0.9946(9) 0.1020(11) 1.3058(8) 0.086(3) Uani 1 1 d U . . H32A H 1.0109 0.1030 1.3666 0.103 Uiso 1 1 calc R . . C33 C 0.9362(8) 0.0067(9) 1.2237(8) 0.073(3) Uani 1 1 d . . . H33A H 0.9096 -0.0566 1.2269 0.087 Uiso 1 1 calc R . . C34 C 0.9195(7) 0.0118(9) 1.1336(6) 0.052(2) Uani 1 1 d . . . C35 C 0.8620(7) -0.0307(7) 0.9160(6) 0.047(2) Uani 1 1 d . . . H35A H 0.9034 0.0396 0.9608 0.057 Uiso 1 1 calc R . . C36 C 0.8346(6) -0.1044(7) 0.9499(6) 0.045(2) Uani 1 1 d . . . C37 C 0.7695(7) -0.1576(8) 0.7559(7) 0.058(3) Uani 1 1 d . . . H37A H 0.7483 -0.1759 0.6899 0.070 Uiso 1 1 calc R . . C38 C 0.7369(7) -0.2348(8) 0.7848(7) 0.064(3) Uani 1 1 d . . . H38A H 0.6932 -0.3040 0.7384 0.077 Uiso 1 1 calc R . . C39 C 0.7692(7) -0.2092(7) 0.8812(8) 0.058(3) Uani 1 1 d . . . H39A H 0.7480 -0.2607 0.9013 0.069 Uiso 1 1 calc R . . C40 C 0.5645(8) 0.0161(8) 0.6509(7) 0.067(3) Uani 1 1 d . . . H40A H 0.5844 0.0779 0.6442 0.081 Uiso 1 1 calc R . . C41 C 0.4881(9) -0.0704(10) 0.5750(8) 0.089(4) Uani 1 1 d . . . H41A H 0.4618 -0.0717 0.5146 0.107 Uiso 1 1 calc R . . C42 C 0.4491(8) -0.1583(9) 0.5890(7) 0.087(4) Uani 1 1 d . . . H42A H 0.3931 -0.2186 0.5381 0.105 Uiso 1 1 calc R . . C43 C 0.4925(7) -0.1584(7) 0.6786(6) 0.052(2) Uani 1 1 d . . . C44 C 0.5818(6) -0.0625(7) 0.7473(6) 0.053(2) Uani 1 1 d . . . H44A H 0.6200 -0.0593 0.8057 0.064 Uiso 1 1 calc R . . C45 C 0.4825(8) -0.2608(10) 0.7755(10) 0.070(3) Uani 1 1 d . . . C46 C 0.4502(11) -0.3619(10) 0.7668(11) 0.110(4) Uani 1 1 d U . . H46A H 0.4094 -0.4208 0.7068 0.132 Uiso 1 1 calc R . . C47 C 0.4813(12) -0.3708(12) 0.8509(13) 0.118(5) Uani 1 1 d . . . H47A H 0.4635 -0.4376 0.8481 0.142 Uiso 1 1 calc R . . C48 C 0.5377(11) -0.2842(13) 0.9385(11) 0.107(4) Uani 1 1 d U . . H48A H 0.5615 -0.2911 0.9951 0.129 Uiso 1 1 calc R . . C49 C 0.5582(9) -0.1892(11) 0.9417(11) 0.072(3) Uani 1 1 d . . . C50 C 0.6463(9) 0.0020(13) 1.0623(8) 0.080(4) Uani 1 1 d . . . C51 C 0.7062(8) 0.0702(12) 1.1600(8) 0.095(4) Uani 1 1 d . . . H51A H 0.7235 0.0432 1.2036 0.114 Uiso 1 1 calc R . . C52 C 0.7396(9) 0.1751(12) 1.1921(9) 0.097(4) Uani 1 1 d U . . H52A H 0.7810 0.2208 1.2575 0.116 Uiso 1 1 calc R . . C53 C 0.6220(7) 0.0458(10) 1.0012(7) 0.064(3) Uani 1 1 d . . . H53A H 0.5817 0.0012 0.9353 0.077 Uiso 1 1 calc R . . C54 C 0.7116(9) 0.2149(10) 1.1266(8) 0.092(4) Uani 1 1 d . . . H54A H 0.7336 0.2874 1.1489 0.110 Uiso 1 1 calc R . . C55 C 0.340(2) 0.4983(17) 0.9902(19) 0.212(11) Uani 1 1 d D . . H55C H 0.3971 0.4936 0.9705 0.255 Uiso 0.25 1 calc PR B 2 H55D H 0.3698 0.5638 1.0497 0.255 Uiso 0.25 1 calc PR B 2 H55A H 0.3675 0.4759 0.9408 0.255 Uiso 0.75 1 d PR B 1 H55B H 0.3991 0.5547 1.0484 0.255 Uiso 0.75 1 d PR B 1 C56 C 0.266(2) 0.553(2) 0.960(2) 0.192(12) Uiso 0.75 1 d PD C 1 H56A H 0.2666 0.6028 1.0179 0.289 Uiso 0.75 1 calc PR C 1 H56B H 0.1967 0.4996 0.9199 0.289 Uiso 0.75 1 calc PR C 1 H56C H 0.2913 0.5879 0.9250 0.289 Uiso 0.75 1 calc PR C 1 C56A C 0.269(3) 0.511(3) 0.915(2) 0.050(10) Uiso 0.25 1 d PD C 2 H56D H 0.2459 0.5641 0.9462 0.075 Uiso 0.25 1 calc PR C 2 H56E H 0.2092 0.4456 0.8728 0.075 Uiso 0.25 1 calc PR C 2 H56F H 0.3042 0.5334 0.8780 0.075 Uiso 0.25 1 calc PR C 2 O10 O 0.3450(5) 0.4945(6) 0.2052(6) 0.110(3) Uani 1 1 d . . . H10A H 0.3896 0.5183 0.2582 0.132 Uiso 1 1 d R . . H10B H 0.3277 0.5400 0.2011 0.132 Uiso 1 1 d R . . O11 O 0.8395(10) 0.7498(8) 0.1130(8) 0.191(5) Uani 1 1 d . . . H11C H 0.8408 0.7234 0.1491 0.230 Uiso 1 1 d R . . H11D H 0.7930 0.6952 0.0712 0.230 Uiso 1 1 d R . . O12 O 0.7153(6) 0.3450(6) 0.8088(6) 0.113(3) Uani 1 1 d . . . H12A H 0.7370 0.3043 0.7825 0.136 Uiso 1 1 d R . . H12B H 0.6618 0.3128 0.8101 0.136 Uiso 1 1 d 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 0.0535(4) 0.0612(5) 0.0763(5) 0.0451(4) 0.0243(4) 0.0279(4) Ag2 0.0519(4) 0.0569(5) 0.0482(4) 0.0240(4) 0.0160(3) 0.0158(4) Ag3 0.0812(5) 0.0622(5) 0.0583(5) 0.0408(4) 0.0364(4) 0.0389(4) Ag4 0.0735(5) 0.0989(7) 0.0530(5) 0.0361(5) 0.0196(4) 0.0375(5) O1 0.097(5) 0.094(5) 0.093(5) 0.073(5) 0.053(4) 0.066(5) O2 0.110(6) 0.106(6) 0.106(6) 0.081(5) 0.058(5) 0.068(5) O3 0.081(5) 0.056(4) 0.065(5) -0.004(4) -0.017(4) 0.041(4) O4 0.069(4) 0.074(5) 0.069(5) -0.007(4) -0.004(4) 0.048(4) O5 0.098(6) 0.111(6) 0.074(5) 0.060(5) 0.030(5) 0.053(5) O6 0.098(9) 0.068(8) 0.056(7) 0.047(6) 0.010(6) 0.014(7) O7 0.060(4) 0.094(6) 0.074(5) 0.061(5) 0.010(4) 0.004(4) O8 0.121(6) 0.055(4) 0.065(5) 0.040(4) 0.011(4) 0.015(4) O9 0.28(2) 0.212(17) 0.228(16) 0.130(14) 0.071(14) 0.105(15) N1 0.030(4) 0.045(5) 0.066(5) 0.022(4) 0.028(4) -0.006(4) N2 0.064(5) 0.052(5) 0.037(4) 0.024(4) 0.023(4) 0.031(4) N3 0.082(6) 0.064(5) 0.051(5) 0.043(5) 0.029(4) 0.034(5) N4 0.047(4) 0.065(5) 0.043(5) 0.022(5) 0.018(4) 0.030(4) N5 0.051(5) 0.065(6) 0.053(6) 0.014(5) 0.009(4) 0.013(5) N6 0.044(4) 0.053(5) 0.059(5) 0.037(4) 0.023(4) 0.017(4) N7 0.063(5) 0.111(8) 0.036(5) 0.026(5) 0.020(4) 0.047(6) N8 0.085(7) 0.159(11) 0.078(8) 0.088(9) 0.040(6) 0.071(8) N9 0.076(6) 0.049(5) 0.065(6) 0.029(5) 0.020(5) 0.010(4) N10 0.077(6) 0.078(7) 0.076(6) 0.054(6) 0.038(5) 0.038(5) C1 0.061(6) 0.049(6) 0.045(6) 0.023(5) 0.027(5) 0.023(5) C2 0.046(5) 0.047(5) 0.048(5) 0.031(5) 0.025(4) 0.020(4) C3 0.033(5) 0.068(6) 0.054(6) 0.037(5) 0.019(4) 0.023(5) C4 0.043(5) 0.052(6) 0.059(6) 0.027(5) 0.017(5) 0.019(5) C5 0.075(7) 0.102(9) 0.115(9) 0.080(8) 0.068(7) 0.064(7) C6 0.060(6) 0.044(5) 0.057(6) 0.030(5) 0.041(5) 0.026(5) C7 0.069(6) 0.065(6) 0.060(6) 0.039(5) 0.046(5) 0.041(6) C8 0.037(5) 0.047(5) 0.063(6) 0.035(5) 0.021(4) 0.012(4) C9 0.063(6) 0.047(6) 0.046(5) 0.023(5) 0.026(5) 0.023(5) C10 0.041(5) 0.038(5) 0.039(5) 0.021(4) 0.020(4) 0.016(4) C11 0.053(5) 0.044(5) 0.025(5) 0.003(4) -0.003(4) 0.018(5) C12 0.052(6) 0.033(5) 0.053(6) 0.019(5) 0.010(5) 0.016(5) C13 0.091(8) 0.056(7) 0.059(7) 0.038(6) 0.025(6) 0.046(6) C14 0.054(5) 0.044(6) 0.076(7) 0.041(5) 0.033(5) 0.031(5) C15 0.145(9) 0.097(8) 0.083(7) 0.068(6) 0.009(6) 0.010(6) C16 0.082(7) 0.063(7) 0.042(6) 0.032(5) 0.031(5) 0.013(6) C17 0.146(9) 0.146(9) 0.203(10) 0.112(8) 0.084(8) 0.060(7) C18 0.106(8) 0.168(10) 0.132(9) 0.074(7) 0.068(7) 0.054(7) C19 0.102(10) 0.157(14) 0.085(10) 0.060(10) -0.020(8) 0.039(10) C20 0.165(9) 0.089(7) 0.087(7) 0.065(6) 0.039(7) 0.023(6) C21 0.143(10) 0.054(7) 0.058(7) 0.038(6) 0.034(7) 0.036(7) C23 0.25(2) 0.166(15) 0.180(17) 0.121(14) 0.130(16) 0.150(16) C22 0.058(6) 0.057(6) 0.051(6) 0.026(5) 0.024(5) 0.026(5) C24 0.108(10) 0.115(11) 0.054(7) 0.056(8) 0.026(8) 0.019(9) C25 0.080(8) 0.073(8) 0.050(7) 0.022(6) 0.015(6) 0.004(7) C26 0.090(9) 0.056(7) 0.089(9) 0.021(7) 0.028(8) -0.003(7) C27 0.058(7) 0.086(9) 0.070(8) 0.015(7) 0.031(6) 0.017(7) C28 0.046(6) 0.053(6) 0.045(6) 0.009(5) 0.013(5) 0.015(5) C29 0.057(6) 0.054(6) 0.047(6) 0.028(5) 0.023(5) 0.022(5) C30 0.069(7) 0.095(9) 0.028(6) 0.007(6) 0.003(5) 0.052(7) C31 0.076(7) 0.105(10) 0.044(7) 0.008(7) 0.023(6) 0.040(7) C32 0.089(7) 0.116(8) 0.047(6) 0.026(6) 0.021(5) 0.054(6) C33 0.082(7) 0.109(9) 0.067(7) 0.056(7) 0.041(6) 0.062(7) C34 0.051(6) 0.070(7) 0.039(6) 0.022(6) 0.022(5) 0.031(6) C35 0.063(6) 0.045(6) 0.048(6) 0.022(5) 0.029(5) 0.034(5) C36 0.055(5) 0.047(6) 0.045(5) 0.024(5) 0.025(5) 0.028(5) C37 0.070(6) 0.057(7) 0.050(6) 0.027(6) 0.028(5) 0.023(6) C38 0.072(7) 0.050(7) 0.046(6) 0.011(5) 0.020(5) 0.009(5) C39 0.058(6) 0.042(6) 0.087(8) 0.037(6) 0.039(6) 0.020(5) C40 0.069(7) 0.062(7) 0.052(6) 0.035(6) 0.008(6) 0.006(6) C41 0.088(8) 0.097(10) 0.069(8) 0.059(8) 0.013(7) 0.007(8) C42 0.076(7) 0.082(9) 0.045(6) 0.008(6) -0.016(6) 0.015(7) C43 0.051(5) 0.055(6) 0.046(6) 0.020(5) 0.016(5) 0.024(5) C44 0.047(5) 0.062(7) 0.034(5) 0.011(5) 0.003(4) 0.024(5) C45 0.072(7) 0.072(8) 0.097(10) 0.056(8) 0.045(7) 0.038(7) C46 0.137(8) 0.082(7) 0.128(9) 0.058(7) 0.064(7) 0.043(6) C47 0.150(13) 0.118(12) 0.170(15) 0.124(13) 0.099(12) 0.062(11) C48 0.118(8) 0.116(9) 0.119(8) 0.073(7) 0.068(7) 0.044(7) C49 0.081(8) 0.094(10) 0.109(10) 0.079(9) 0.069(8) 0.057(8) C50 0.079(8) 0.154(13) 0.057(8) 0.073(9) 0.037(6) 0.073(9) C51 0.075(8) 0.192(15) 0.056(8) 0.078(10) 0.034(7) 0.070(10) C52 0.086(7) 0.140(9) 0.062(7) 0.044(7) 0.022(5) 0.049(7) C53 0.057(6) 0.103(9) 0.047(6) 0.038(7) 0.029(5) 0.040(7) C54 0.096(9) 0.129(11) 0.061(8) 0.036(8) 0.033(7) 0.067(8) C55 0.26(3) 0.17(2) 0.24(3) 0.08(2) 0.17(2) 0.09(2) O10 0.065(5) 0.109(6) 0.131(7) 0.073(6) 0.011(5) 0.005(4) O11 0.347(17) 0.129(8) 0.169(10) 0.103(8) 0.157(12) 0.099(10) O12 0.092(6) 0.130(7) 0.144(8) 0.070(6) 0.073(6) 0.045(5) _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 O8 2.218(6) 2_666 ? Ag1 O7 2.279(6) . ? Ag1 O3 2.455(6) . ? Ag1 Ag1 2.8847(14) 2_666 ? Ag2 N1 2.127(7) . ? Ag2 N6 2.148(7) . ? Ag2 O2 2.505(7) . ? Ag2 Ag3 2.9452(10) . ? Ag2 Ag4 3.0326(11) . ? Ag3 O1 2.135(6) . ? Ag3 N2 2.133(7) . ? Ag4 O5 2.120(7) . ? Ag4 N7 2.122(8) . ? O1 C1 1.244(10) . ? O2 C1 1.240(10) . ? O3 C12 1.246(9) . ? O4 C12 1.245(9) . ? O5 C24 1.243(13) . ? O6 C24 1.337(13) . ? O6A C24 1.53(2) . ? O7 C13 1.240(11) . ? O8 C13 1.247(10) . ? O8 Ag1 2.218(6) 2_666 ? O9 C55 1.27(2) . ? O9 H9C 0.7999 . ? N1 C29 1.315(10) . ? N1 C25 1.345(11) . ? N2 C35 1.336(10) . ? N2 C37 1.338(10) . ? N3 C34 1.385(11) . ? N3 C36 1.435(10) . ? N3 H3C 0.8600 . ? N4 C34 1.298(10) . ? N4 C30 1.347(11) . ? N5 C30 1.336(12) . ? N5 C28 1.346(11) . ? N5 H5C 0.8600 . ? N6 C40 1.292(10) . ? N6 C44 1.294(10) . ? N7 C54 1.331(12) . ? N7 C53 1.339(12) . ? N8 C49 1.357(14) . ? N8 C50 1.375(14) . ? N8 H8C 0.8600 . ? N9 C45 1.382(12) . ? N9 C43 1.389(10) . ? N9 H9D 0.8600 . ? N10 C45 1.301(12) . ? N10 C49 1.360(13) . ? C1 C2 1.571(11) . ? C2 C3 1.507(10) . ? C2 C6 1.536(11) . ? C2 C11 1.554(10) . ? C3 C4 1.508(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.515(12) . ? C4 C8 1.527(11) . ? C4 H4A 0.9800 . ? C5 C7 1.520(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.484(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.532(11) . ? C7 H7A 0.9800 . ? C8 C10 1.517(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.517(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.514(11) . ? C10 C11 1.545(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.485(12) . ? C14 C15 1.488(12) . ? C14 C16 1.515(10) . ? C14 C17 1.550(13) . ? C15 C20 1.687(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C22 1.552(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.635(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.444(14) . ? C18 C23 1.457(14) . ? C18 H18A 0.9800 . ? C19 C20 1.541(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.636(13) . ? C20 H20A 0.9800 . ? C21 C22 1.492(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 C22 1.498(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C22 C24 1.540(14) . ? C25 C26 1.371(13) . ? C25 H25A 0.9300 . ? C26 C27 1.381(14) . ? C26 H26A 0.9300 . ? C27 C28 1.372(13) . ? C27 H27A 0.9300 . ? C28 C29 1.365(11) . ? C29 H29A 0.9300 . ? C30 C31 1.410(14) . ? C31 C32 1.365(15) . ? C31 H31A 0.9300 . ? C32 C33 1.376(14) . ? C32 H32A 0.9300 . ? C33 C34 1.426(12) . ? C33 H33A 0.9300 . ? C35 C36 1.383(11) . ? C35 H35A 0.9300 . ? C36 C39 1.401(12) . ? C37 C38 1.382(12) . ? C37 H37A 0.9300 . ? C38 C39 1.360(12) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.329(13) . ? C40 H40A 0.9300 . ? C41 C42 1.384(14) . ? C41 H41A 0.9300 . ? C42 C43 1.405(13) . ? C42 H42A 0.9300 . ? C43 C44 1.432(11) . ? C44 H44A 0.9300 . ? C45 C46 1.380(14) . ? C46 C47 1.363(17) . ? C46 H46A 0.9300 . ? C47 C48 1.357(17) . ? C47 H47A 0.9300 . ? C48 C49 1.332(15) . ? C48 H48A 0.9300 . ? C50 C53 1.372(13) . ? C50 C51 1.384(15) . ? C51 C52 1.343(16) . ? C51 H51A 0.9300 . ? C52 C54 1.393(15) . ? C52 H52A 0.9300 . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C55 C56A 1.48(3) . ? C55 C56 1.58(3) . ? C55 H55C 0.9700 . ? C55 H55D 0.9700 . ? C55 H55A 0.9699 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C56A H56D 0.9600 . ? C56A H56E 0.9600 . ? C56A H56F 0.9600 . ? O10 H10A 0.8001 . ? O10 H10B 0.8002 . ? O11 H11C 0.8000 . ? O11 H11D 0.8000 . ? O12 H12A 0.8000 . ? O12 H12B 0.8001 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ag1 O7 139.9(3) 2_666 . ? O8 Ag1 O3 114.4(3) 2_666 . ? O7 Ag1 O3 105.5(3) . . ? O8 Ag1 Ag1 76.8(2) 2_666 2_666 ? O7 Ag1 Ag1 77.17(17) . 2_666 ? O3 Ag1 Ag1 125.01(15) . 2_666 ? N1 Ag2 N6 164.7(3) . . ? N1 Ag2 O2 101.5(3) . . ? N6 Ag2 O2 91.0(3) . . ? N1 Ag2 Ag3 85.71(18) . . ? N6 Ag2 Ag3 90.78(18) . . ? O2 Ag2 Ag3 68.33(16) . . ? N1 Ag2 Ag4 98.25(18) . . ? N6 Ag2 Ag4 81.04(18) . . ? O2 Ag2 Ag4 126.33(16) . . ? Ag3 Ag2 Ag4 162.97(3) . . ? O1 Ag3 N2 178.1(3) . . ? O1 Ag3 Ag2 90.59(17) . . ? N2 Ag3 Ag2 87.99(18) . . ? O5 Ag4 N7 174.0(4) . . ? O5 Ag4 Ag2 89.0(2) . . ? N7 Ag4 Ag2 89.0(2) . . ? C1 O1 Ag3 119.0(6) . . ? C1 O2 Ag2 128.8(6) . . ? C12 O3 Ag1 97.8(5) . . ? C24 O5 Ag4 107.2(7) . . ? C13 O7 Ag1 118.2(6) . . ? C13 O8 Ag1 119.4(6) . 2_666 ? C55 O9 H9C 110.8 . . ? C29 N1 C25 117.3(8) . . ? C29 N1 Ag2 122.3(6) . . ? C25 N1 Ag2 119.5(7) . . ? C35 N2 C37 119.3(8) . . ? C35 N2 Ag3 121.8(6) . . ? C37 N2 Ag3 118.8(6) . . ? C34 N3 C36 129.3(8) . . ? C34 N3 H3C 115.4 . . ? C36 N3 H3C 115.4 . . ? C34 N4 C30 119.9(9) . . ? C30 N5 C28 127.8(9) . . ? C30 N5 H5C 116.1 . . ? C28 N5 H5C 116.1 . . ? C40 N6 C44 119.2(8) . . ? C40 N6 Ag2 121.8(7) . . ? C44 N6 Ag2 118.8(6) . . ? C54 N7 C53 119.3(10) . . ? C54 N7 Ag4 124.3(9) . . ? C53 N7 Ag4 116.2(7) . . ? C49 N8 C50 132.6(10) . . ? C49 N8 H8C 113.7 . . ? C50 N8 H8C 113.7 . . ? C45 N9 C43 130.0(9) . . ? C45 N9 H9D 115.0 . . ? C43 N9 H9D 115.0 . . ? C45 N10 C49 118.7(10) . . ? O2 C1 O1 123.4(9) . . ? O2 C1 C2 120.1(8) . . ? O1 C1 C2 116.4(8) . . ? C3 C2 C6 110.1(7) . . ? C3 C2 C11 108.3(7) . . ? C6 C2 C11 107.7(6) . . ? C3 C2 C1 111.6(7) . . ? C6 C2 C1 108.3(6) . . ? C11 C2 C1 110.7(7) . . ? C2 C3 C4 109.2(7) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 C5 108.8(7) . . ? C3 C4 C8 110.2(7) . . ? C5 C4 C8 110.1(7) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C8 C4 H4A 109.2 . . ? C4 C5 C7 110.1(7) . . ? C4 C5 H5A 109.6 . . ? C7 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C7 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C2 109.6(7) . . ? C7 C6 H6A 109.8 . . ? C2 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? C2 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C5 108.9(8) . . ? C6 C7 C9 111.9(7) . . ? C5 C7 C9 109.0(7) . . ? C6 C7 H7A 109.0 . . ? C5 C7 H7A 109.0 . . ? C9 C7 H7A 109.0 . . ? C10 C8 C4 110.0(7) . . ? C10 C8 H8A 109.7 . . ? C4 C8 H8A 109.7 . . ? C10 C8 H8B 109.7 . . ? C4 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C7 109.3(7) . . ? C10 C9 H9A 109.8 . . ? C7 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C7 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? C12 C10 C9 110.8(7) . . ? C12 C10 C8 112.3(7) . . ? C9 C10 C8 112.2(7) . . ? C12 C10 C11 108.1(6) . . ? C9 C10 C11 108.0(6) . . ? C8 C10 C11 105.2(6) . . ? C10 C11 C2 111.7(7) . . ? C10 C11 H11A 109.3 . . ? C2 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C2 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? O4 C12 O3 120.7(8) . . ? O4 C12 C10 119.6(8) . . ? O3 C12 C10 119.4(8) . . ? O7 C13 O8 124.8(10) . . ? O7 C13 C14 117.9(9) . . ? O8 C13 C14 117.3(10) . . ? C13 C14 C15 113.2(8) . . ? C13 C14 C16 113.8(8) . . ? C15 C14 C16 108.7(7) . . ? C13 C14 C17 104.2(8) . . ? C15 C14 C17 112.7(10) . . ? C16 C14 C17 103.8(9) . . ? C14 C15 C20 110.4(9) . . ? C14 C15 H15A 109.6 . . ? C20 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C20 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C14 C16 C22 111.1(7) . . ? C14 C16 H16A 109.4 . . ? C22 C16 H16A 109.4 . . ? C14 C16 H16B 109.4 . . ? C22 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C14 C17 C18 112.3(10) . . ? C14 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C14 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C23 107.0(14) . . ? C19 C18 C17 98.1(12) . . ? C23 C18 C17 116.2(12) . . ? C19 C18 H18A 111.6 . . ? C23 C18 H18A 111.6 . . ? C17 C18 H18A 111.6 . . ? C18 C19 C20 121.3(12) . . ? C18 C19 H19A 107.0 . . ? C20 C19 H19A 107.0 . . ? C18 C19 H19B 107.0 . . ? C20 C19 H19B 107.0 . . ? H19A C19 H19B 106.7 . . ? C19 C20 C21 105.8(9) . . ? C19 C20 C15 107.6(10) . . ? C21 C20 C15 98.3(9) . . ? C19 C20 H20A 114.5 . . ? C21 C20 H20A 114.5 . . ? C15 C20 H20A 114.5 . . ? C22 C21 C20 108.6(8) . . ? C22 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? C22 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C18 C23 C22 109.0(12) . . ? C18 C23 H23A 109.9 . . ? C22 C23 H23A 109.9 . . ? C18 C23 H23B 109.9 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C21 C22 C23 110.3(10) . . ? C21 C22 C24 109.5(8) . . ? C23 C22 C24 100.9(9) . . ? C21 C22 C16 111.5(8) . . ? C23 C22 C16 112.6(9) . . ? C24 C22 C16 111.5(8) . . ? O5 C24 O6 114.8(12) . . ? O5 C24 O6A 121.2(13) . . ? O6 C24 O6A 70.7(11) . . ? O5 C24 C22 120.6(10) . . ? O6 C24 C22 120.0(11) . . ? O6A C24 C22 97.4(13) . . ? N1 C25 C26 120.8(10) . . ? N1 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C27 119.5(11) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C28 C27 C26 120.3(11) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? N5 C28 C29 127.3(10) . . ? N5 C28 C27 117.5(10) . . ? C29 C28 C27 115.3(10) . . ? N1 C29 C28 126.7(9) . . ? N1 C29 H29A 116.7 . . ? C28 C29 H29A 116.7 . . ? N5 C30 N4 120.4(9) . . ? N5 C30 C31 119.2(10) . . ? N4 C30 C31 120.4(12) . . ? C32 C31 C30 118.3(11) . . ? C32 C31 H31A 120.8 . . ? C30 C31 H31A 120.8 . . ? C31 C32 C33 122.1(11) . . ? C31 C32 H32A 119.0 . . ? C33 C32 H32A 119.0 . . ? C32 C33 C34 115.2(11) . . ? C32 C33 H33A 122.4 . . ? C34 C33 H33A 122.4 . . ? N4 C34 N3 120.1(8) . . ? N4 C34 C33 123.8(9) . . ? N3 C34 C33 116.1(10) . . ? N2 C35 C36 122.3(8) . . ? N2 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C35 C36 C39 117.9(8) . . ? C35 C36 N3 126.2(8) . . ? C39 C36 N3 115.9(8) . . ? N2 C37 C38 121.5(9) . . ? N2 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C39 C38 C37 119.7(9) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C38 C39 C36 119.3(9) . . ? C38 C39 H39A 120.4 . . ? C36 C39 H39A 120.4 . . ? N6 C40 C41 124.4(10) . . ? N6 C40 H40A 117.8 . . ? C41 C40 H40A 117.8 . . ? C40 C41 C42 117.6(10) . . ? C40 C41 H41A 121.2 . . ? C42 C41 H41A 121.2 . . ? C41 C42 C43 121.3(9) . . ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? N9 C43 C42 121.6(9) . . ? N9 C43 C44 125.6(8) . . ? C42 C43 C44 112.5(9) . . ? N6 C44 C43 124.2(8) . . ? N6 C44 H44A 117.9 . . ? C43 C44 H44A 117.9 . . ? N10 C45 C46 122.8(12) . . ? N10 C45 N9 118.5(10) . . ? C46 C45 N9 118.6(12) . . ? C47 C46 C45 116.5(14) . . ? C47 C46 H46A 121.8 . . ? C45 C46 H46A 121.8 . . ? C48 C47 C46 121.3(13) . . ? C48 C47 H47A 119.3 . . ? C46 C47 H47A 119.3 . . ? C49 C48 C47 118.6(14) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C48 C49 N8 116.4(13) . . ? C48 C49 N10 121.6(14) . . ? N8 C49 N10 121.7(11) . . ? C53 C50 N8 123.2(11) . . ? C53 C50 C51 117.6(14) . . ? N8 C50 C51 119.3(11) . . ? C52 C51 C50 120.3(12) . . ? C52 C51 H51A 119.8 . . ? C50 C51 H51A 119.8 . . ? C51 C52 C54 119.5(12) . . ? C51 C52 H52A 120.2 . . ? C54 C52 H52A 120.2 . . ? N7 C53 C50 122.6(11) . . ? N7 C53 H53A 118.7 . . ? C50 C53 H53A 118.7 . . ? N7 C54 C52 120.7(12) . . ? N7 C54 H54A 119.6 . . ? C52 C54 H54A 119.6 . . ? O9 C55 C56A 124(3) . . ? O9 C55 C56 123(2) . . ? O9 C55 H55C 106.4 . . ? C56A C55 H55C 106.4 . . ? O9 C55 H55D 106.4 . . ? C56A C55 H55D 106.5 . . ? H55C C55 H55D 106.5 . . ? O9 C55 H55A 107.9 . . ? C56 C55 H55A 109.6 . . ? O9 C55 H55B 104.0 . . ? C56 C55 H55B 104.8 . . ? H55A C55 H55B 106.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? C55 C56A H56D 109.5 . . ? C55 C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C55 C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? H10A O10 H10B 108.4 . . ? H11C O11 H11D 87.8 . . ? H12A O12 H12B 109.1 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.401 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.123