Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #=============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Sordo' _publ_contact_author_address ; Inorganic Chemistry University of Santiago de Compostela Facultad de Farmacia, Campus Sur Santiago de Compostela Galicia 15782 SPAIN ; _publ_contact_author_email QIJSORDO@USC.ES # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and antimicrobial activities of silver(I) sulfanylcarboxylates. Structural isomers with identically or unequally coordinated Ag centers in an Ag4S4 ring. ; loop_ _publ_author_name _publ_author_address E.Barreiro ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; J.S.Casas ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; M.D.Couce ; Departamento de Quimica Inorganica Facultade de Quimica Edificio Ciencias Experimentais Universidade de Vigo 36310 Vigo Galicia, Spain ; A.Sanchez ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; R.Seoane ; Departamento de Microbiologia Facultade de Medicina Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; J.Sordo ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; ; J.M.Varela ; ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; E.Vazquez-Lopez ; Departamento de Quimica Inorganica Facultade de Quimica Edificio Ciencias Experimentais Universidade de Vigo 36310 Vigo Galicia, Spain ; #=============================================================================== ################ # CCDC 637276 # ################ data_11 _database_code_depnum_ccdc_archive 'CCDC 637276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 Ag2 N2 O4 S2' _chemical_formula_weight 776.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.658(3) _cell_length_b 14.597(4) _cell_length_c 19.874(5) _cell_angle_alpha 91.661(5) _cell_angle_beta 97.236(4) _cell_angle_gamma 100.182(4) _cell_volume 3297.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737695 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12931 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.02 _reflns_number_total 12931 _reflns_number_gt 9577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP-3 (Farrugia, 1997) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12931 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.06465(2) 0.859007(17) 0.058972(13) 0.02037(7) Uani 1 1 d . . . S1 S -0.10451(8) 0.81352(6) -0.02716(4) 0.0207(2) Uani 1 1 d . . . N1 N 0.1219(3) 0.0886(2) 0.59030(15) 0.0205(7) Uani 1 1 d . . . Ag2 Ag 0.12660(2) 1.059461(17) 0.098296(13) 0.02095(7) Uani 1 1 d . . . S2 S 0.16236(7) 0.93248(6) 0.16756(4) 0.01817(19) Uani 1 1 d . . . N2 N 0.8311(3) 0.4407(2) 0.91249(15) 0.0209(7) Uani 1 1 d . . . Ag3 Ag 0.04695(2) 0.348914(17) 0.537095(13) 0.01976(7) Uani 1 1 d . . . S3 S 0.11765(7) 0.39961(6) 0.65360(4) 0.01820(19) Uani 1 1 d . . . N3 N 0.6420(3) 0.4435(2) 0.55948(15) 0.0205(7) Uani 1 1 d . . . Ag4 Ag 0.09305(2) 0.545116(18) 0.602071(14) 0.02324(7) Uani 1 1 d . . . S4 S 0.01036(7) 0.68273(6) 0.58271(4) 0.01871(19) Uani 1 1 d . . . N4 N 0.3564(3) 0.9076(2) 0.91895(15) 0.0214(7) Uani 1 1 d . . . O11 O 0.0790(2) 0.69802(15) 0.01970(12) 0.0265(6) Uani 1 1 d . . . C11 C 0.0196(3) 0.6658(2) -0.03572(18) 0.0215(8) Uani 1 1 d . . . O12 O 0.0199(2) 0.58611(16) -0.06185(12) 0.0287(6) Uani 1 1 d . . . C12 C -0.0587(3) 0.7253(2) -0.07498(17) 0.0172(7) Uani 1 1 d . . . C13 C -0.0857(3) 0.7064(2) -0.14200(17) 0.0209(8) Uani 1 1 d . . . H13 H -0.0531 0.6567 -0.1592 0.025 Uiso 1 1 calc R . . C14 C -0.1573(3) 0.7500(2) -0.19319(17) 0.0207(8) Uani 1 1 d . . . C15 C -0.1232(3) 0.7605(2) -0.25789(17) 0.0265(9) Uani 1 1 d . . . H15 H -0.0547 0.7389 -0.2680 0.032 Uiso 1 1 calc R . . C16 C -0.1878(3) 0.8020(2) -0.30719(18) 0.0293(9) Uani 1 1 d . . . H16 H -0.1628 0.8090 -0.3507 0.035 Uiso 1 1 calc R . . C17 C -0.2873(3) 0.8332(2) -0.29433(18) 0.0269(9) Uani 1 1 d . . . H17 H -0.3303 0.8628 -0.3284 0.032 Uiso 1 1 calc R . . C18 C -0.3243(3) 0.8214(2) -0.23193(18) 0.0260(9) Uani 1 1 d . . . H18 H -0.3941 0.8419 -0.2230 0.031 Uiso 1 1 calc R . . C19 C -0.2604(3) 0.7794(2) -0.18115(17) 0.0219(8) Uani 1 1 d . . . H19 H -0.2875 0.7709 -0.1382 0.026 Uiso 1 1 calc R . . O21 O 0.2803(2) 0.91236(18) 0.04132(12) 0.0303(6) Uani 1 1 d . . . C21 C 0.3564(3) 0.9286(2) 0.09277(17) 0.0187(8) Uani 1 1 d . . . O22 O 0.4652(2) 0.93927(16) 0.09104(11) 0.0244(6) Uani 1 1 d . . . C22 C 0.3136(3) 0.9349(2) 0.16215(16) 0.0158(7) Uani 1 1 d . . . C23 C 0.3959(3) 0.9435(2) 0.21686(16) 0.0180(7) Uani 1 1 d . . . H23 H 0.4729 0.9412 0.2068 0.022 Uiso 1 1 calc R . . C24 C 0.3875(3) 0.9557(2) 0.28953(17) 0.0196(8) Uani 1 1 d . . . C25 C 0.2910(3) 0.9169(2) 0.32057(17) 0.0233(8) Uani 1 1 d . . . H25 H 0.2257 0.8785 0.2941 0.028 Uiso 1 1 calc R . . C26 C 0.2883(3) 0.9335(2) 0.38957(17) 0.0268(9) Uani 1 1 d . . . H26 H 0.2221 0.9059 0.4101 0.032 Uiso 1 1 calc R . . C27 C 0.3825(3) 0.9905(2) 0.42824(18) 0.0268(9) Uani 1 1 d . . . H27 H 0.3801 1.0029 0.4752 0.032 Uiso 1 1 calc R . . C28 C 0.4797(3) 1.0292(2) 0.39927(17) 0.0250(8) Uani 1 1 d . . . H28 H 0.5441 1.0684 0.4259 0.030 Uiso 1 1 calc R . . C29 C 0.4829(3) 1.0103(2) 0.33026(17) 0.0236(8) Uani 1 1 d . . . H29 H 0.5514 1.0350 0.3107 0.028 Uiso 1 1 calc R . . O31 O 0.2757(2) 0.51191(16) 0.56081(12) 0.0258(6) Uani 1 1 d . . . C31 C 0.3257(3) 0.4533(2) 0.59336(17) 0.0228(8) Uani 1 1 d . . . O32 O 0.4164(2) 0.4268(2) 0.57932(13) 0.0411(7) Uani 1 1 d . . . C32 C 0.2713(3) 0.4094(2) 0.65339(17) 0.0189(8) Uani 1 1 d . . . C33 C 0.3440(3) 0.3790(2) 0.70166(16) 0.0201(8) Uani 1 1 d . . . H33 H 0.4224 0.3852 0.6916 0.024 Uiso 1 1 calc R . . C34 C 0.3272(3) 0.3381(2) 0.76700(17) 0.0208(8) Uani 1 1 d . . . C35 C 0.4088(3) 0.2842(3) 0.79369(19) 0.0297(9) Uani 1 1 d . . . H35 H 0.4712 0.2755 0.7691 0.036 Uiso 1 1 calc R . . C36 C 0.4000(3) 0.2433(3) 0.8555(2) 0.0386(10) Uani 1 1 d . . . H36 H 0.4552 0.2062 0.8725 0.046 Uiso 1 1 calc R . . C37 C 0.3107(3) 0.2569(3) 0.89198(19) 0.0351(10) Uani 1 1 d . . . H37 H 0.3051 0.2299 0.9346 0.042 Uiso 1 1 calc R . . C38 C 0.2293(3) 0.3098(3) 0.86643(18) 0.0300(9) Uani 1 1 d . . . H38 H 0.1673 0.3184 0.8914 0.036 Uiso 1 1 calc R . . C39 C 0.2380(3) 0.3501(2) 0.80459(17) 0.0259(8) Uani 1 1 d . . . H39 H 0.1819 0.3866 0.7877 0.031 Uiso 1 1 calc R . . O41 O 0.0511(2) 0.82910(15) 0.47943(12) 0.0236(6) Uani 1 1 d . . . C41 C 0.1226(3) 0.8497(2) 0.53239(18) 0.0198(8) Uani 1 1 d . . . O42 O 0.1889(2) 0.92774(15) 0.54705(12) 0.0268(6) Uani 1 1 d . . . C42 C 0.1334(3) 0.7745(2) 0.58455(16) 0.0173(7) Uani 1 1 d . . . C43 C 0.2330(3) 0.7831(2) 0.62744(17) 0.0203(8) Uani 1 1 d . . . H43 H 0.2887 0.8380 0.6233 0.024 Uiso 1 1 calc R . . C44 C 0.2708(3) 0.7216(2) 0.68019(17) 0.0222(8) Uani 1 1 d . . . C45 C 0.3869(3) 0.7091(2) 0.68994(18) 0.0284(9) Uani 1 1 d . . . H45 H 0.4412 0.7413 0.6630 0.034 Uiso 1 1 calc R . . C46 C 0.4250(4) 0.6510(3) 0.7378(2) 0.0354(10) Uani 1 1 d . . . H46 H 0.5046 0.6427 0.7428 0.042 Uiso 1 1 calc R . . C47 C 0.3490(4) 0.6049(3) 0.7785(2) 0.0399(11) Uani 1 1 d . . . H47 H 0.3756 0.5642 0.8109 0.048 Uiso 1 1 calc R . . C48 C 0.2343(4) 0.6181(3) 0.77185(19) 0.0368(10) Uani 1 1 d . . . H48 H 0.1820 0.5878 0.8006 0.044 Uiso 1 1 calc R . . C49 C 0.1949(3) 0.6758(2) 0.72293(18) 0.0294(9) Uani 1 1 d . . . H49 H 0.1154 0.6842 0.7184 0.035 Uiso 1 1 calc R . . C1A C 0.0018(3) -0.0165(2) 0.6581(2) 0.0330(9) Uani 1 1 d . . . H13A H -0.0682 -0.0060 0.6287 0.050 Uiso 1 1 calc R . . H11A H -0.0181 -0.0289 0.7039 0.050 Uiso 1 1 calc R . . H12A H 0.0300 -0.0702 0.6397 0.050 Uiso 1 1 calc R . . C2A C 0.0971(3) 0.0691(3) 0.66145(18) 0.0275(9) Uani 1 1 d . . . H2A H 0.172(3) 0.057(2) 0.6916(15) 0.015(8) Uiso 1 1 d . . . C3A C 0.0624(4) 0.1526(3) 0.69466(19) 0.0391(10) Uani 1 1 d . . . H33A H 0.1294 0.2045 0.7006 0.059 Uiso 1 1 calc R . . H31A H 0.0388 0.1366 0.7391 0.059 Uiso 1 1 calc R . . H32A H -0.0036 0.1709 0.6659 0.059 Uiso 1 1 calc R . . C4A C 0.3356(3) 0.1506(3) 0.6203(2) 0.0341(10) Uani 1 1 d . . . H41A H 0.3532 0.0909 0.6048 0.051 Uiso 1 1 calc R . . H42A H 0.3283 0.1498 0.6689 0.051 Uiso 1 1 calc R . . H43A H 0.3994 0.2011 0.6126 0.051 Uiso 1 1 calc R . . C5A C 0.2211(3) 0.1663(2) 0.58096(19) 0.0226(8) Uani 1 1 d . . . H5A H 0.203(2) 0.223(2) 0.5990(14) 0.008(8) Uiso 1 1 d . . . C6A C 0.2284(3) 0.1710(3) 0.50564(19) 0.0316(9) Uani 1 1 d . . . H61A H 0.2457 0.1122 0.4882 0.047 Uiso 1 1 calc R . . H63A H 0.2911 0.2224 0.4980 0.047 Uiso 1 1 calc R . . H62A H 0.1532 0.1815 0.4820 0.047 Uiso 1 1 calc R . . C1B C 0.7460(3) 0.5068(3) 1.0047(2) 0.0396(10) Uani 1 1 d . . . H12B H 0.7944 0.4719 1.0344 0.059 Uiso 1 1 calc R . . H11B H 0.6728 0.5093 1.0235 0.059 Uiso 1 1 calc R . . H13B H 0.7891 0.5702 1.0017 0.059 Uiso 1 1 calc R . . C2B C 0.7176(3) 0.4584(3) 0.93424(19) 0.0283(9) Uani 1 1 d . . . H2B H 0.672(3) 0.395(2) 0.9371(15) 0.011(8) Uiso 1 1 d . . . C3B C 0.6537(3) 0.5149(3) 0.8838(2) 0.0399(11) Uani 1 1 d . . . H31B H 0.7063 0.5730 0.8768 0.060 Uiso 1 1 calc R . . H32B H 0.5840 0.5294 0.9018 0.060 Uiso 1 1 calc R . . H33B H 0.6295 0.4787 0.8405 0.060 Uiso 1 1 calc R . . C4B C 0.9520(3) 0.3991(3) 0.8282(2) 0.0389(10) Uani 1 1 d . . . H41B H 1.0039 0.4595 0.8396 0.058 Uiso 1 1 calc R . . H43B H 0.9523 0.3810 0.7804 0.058 Uiso 1 1 calc R . . H42B H 0.9801 0.3519 0.8569 0.058 Uiso 1 1 calc R . . C5B C 0.8289(3) 0.4063(3) 0.84014(18) 0.0269(9) Uani 1 1 d . . . H5B H 0.796(3) 0.452(2) 0.8105(16) 0.019(9) Uiso 1 1 d . . . C6B C 0.7452(3) 0.3132(2) 0.8258(2) 0.0358(10) Uani 1 1 d . . . H61B H 0.7693 0.2683 0.8579 0.054 Uiso 1 1 calc R . . H62B H 0.7473 0.2898 0.7793 0.054 Uiso 1 1 calc R . . H63B H 0.6650 0.3214 0.8309 0.054 Uiso 1 1 calc R . . C1C C 0.6603(5) 0.6078(3) 0.5872(2) 0.0564(14) Uani 1 1 d . . . H11C H 0.6715 0.6182 0.5398 0.085 Uiso 1 1 calc R . . H12C H 0.7033 0.6615 0.6162 0.085 Uiso 1 1 calc R . . H13C H 0.5763 0.5999 0.5916 0.085 Uiso 1 1 calc R . . C2C C 0.7059(4) 0.5212(3) 0.6088(2) 0.0335(10) Uani 1 1 d . . . H2C H 0.791(3) 0.529(2) 0.6041(17) 0.032(11) Uiso 1 1 d . . . C3C C 0.6887(4) 0.5012(3) 0.68115(18) 0.0420(11) Uani 1 1 d . . . H32C H 0.6045 0.4889 0.6851 0.063 Uiso 1 1 calc R . . H31C H 0.7277 0.5552 0.7111 0.063 Uiso 1 1 calc R . . H33C H 0.7227 0.4466 0.6943 0.063 Uiso 1 1 calc R . . C4C C 0.7898(3) 0.3408(3) 0.5803(2) 0.0463(12) Uani 1 1 d . . . H42C H 0.8209 0.3594 0.5382 0.069 Uiso 1 1 calc R . . H43C H 0.8000 0.2768 0.5890 0.069 Uiso 1 1 calc R . . H41C H 0.8323 0.3828 0.6182 0.069 Uiso 1 1 calc R . . C5C C 0.6608(3) 0.3460(2) 0.5734(2) 0.0253(9) Uani 1 1 d . . . H5C H 0.628(3) 0.330(2) 0.6148(16) 0.021(9) Uiso 1 1 d . . . C6C C 0.5905(3) 0.2813(3) 0.5155(2) 0.0358(10) Uani 1 1 d . . . H63C H 0.5085 0.2900 0.5101 0.054 Uiso 1 1 calc R . . H62C H 0.5939 0.2165 0.5258 0.054 Uiso 1 1 calc R . . H61C H 0.6238 0.2956 0.4734 0.054 Uiso 1 1 calc R . . C1D C 0.2022(4) 1.0014(3) 0.8981(2) 0.0589(14) Uani 1 1 d . . . H11D H 0.1946 0.9982 0.9466 0.088 Uiso 1 1 calc R . . H13D H 0.1256 1.0045 0.8724 0.088 Uiso 1 1 calc R . . H12D H 0.2590 1.0571 0.8910 0.088 Uiso 1 1 calc R . . C2D C 0.2446(4) 0.9156(3) 0.8740(2) 0.0362(11) Uani 1 1 d . . . H2D H 0.194(4) 0.873(3) 0.879(2) 0.052(15) Uiso 1 1 d . . . C3D C 0.2640(4) 0.9211(3) 0.8005(2) 0.0554(14) Uani 1 1 d . . . H31D H 0.3155 0.9801 0.7943 0.083 Uiso 1 1 calc R . . H32D H 0.1883 0.9177 0.7719 0.083 Uiso 1 1 calc R . . H33D H 0.3008 0.8690 0.7875 0.083 Uiso 1 1 calc R . . C4D C 0.5285(4) 0.8331(3) 0.9447(2) 0.0428(11) Uani 1 1 d . . . H42D H 0.5309 0.8528 0.9925 0.064 Uiso 1 1 calc R . . H43D H 0.5777 0.8813 0.9224 0.064 Uiso 1 1 calc R . . H41D H 0.5583 0.7746 0.9419 0.064 Uiso 1 1 calc R . . C5D C 0.4035(3) 0.8188(3) 0.90993(19) 0.0292(9) Uani 1 1 d . . . H5D H 0.400(3) 0.805(2) 0.8624(17) 0.020(9) Uiso 1 1 d . . . C6D C 0.3255(4) 0.7388(3) 0.9375(2) 0.0579(14) Uani 1 1 d . . . H61D H 0.3244 0.7515 0.9861 0.087 Uiso 1 1 calc R . . H62D H 0.3561 0.6813 0.9309 0.087 Uiso 1 1 calc R . . H63D H 0.2455 0.7317 0.9134 0.087 Uiso 1 1 calc R . . H1N1 H 0.141(3) 0.039(3) 0.5694(18) 0.033(11) Uiso 1 1 d . . . H2N1 H 0.059(3) 0.103(2) 0.5663(17) 0.023(10) Uiso 1 1 d . . . H1N2 H 0.886(3) 0.485(2) 0.9198(17) 0.020(11) Uiso 1 1 d . . . H2N2 H 0.861(3) 0.390(3) 0.9414(19) 0.049(12) Uiso 1 1 d . . . H1N3 H 0.662(4) 0.456(3) 0.511(2) 0.075(16) Uiso 1 1 d . . . H2N3 H 0.563(3) 0.446(2) 0.5591(16) 0.023(10) Uiso 1 1 d . . . H1N4 H 0.414(3) 0.958(2) 0.9100(16) 0.020(9) Uiso 1 1 d . . . H2N4 H 0.336(4) 0.912(3) 0.968(2) 0.065(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02228(15) 0.01900(14) 0.01820(14) -0.00069(11) -0.00225(11) 0.00309(11) S1 0.0219(5) 0.0220(5) 0.0180(5) -0.0001(4) -0.0022(4) 0.0066(4) N1 0.0194(17) 0.0149(16) 0.0270(18) 0.0011(14) -0.0019(14) 0.0056(13) Ag2 0.02119(15) 0.01856(14) 0.02364(15) 0.00126(11) 0.00002(12) 0.00711(11) S2 0.0177(5) 0.0221(5) 0.0149(4) 0.0014(4) 0.0021(4) 0.0043(4) N2 0.0218(18) 0.0165(17) 0.0223(17) 0.0015(14) -0.0038(14) 0.0026(15) Ag3 0.01605(14) 0.01980(14) 0.02325(15) 0.00038(11) 0.00034(11) 0.00454(11) S3 0.0166(4) 0.0185(4) 0.0208(5) 0.0049(4) 0.0049(4) 0.0041(4) N3 0.0172(17) 0.0251(17) 0.0200(17) 0.0036(13) 0.0029(13) 0.0049(13) Ag4 0.02282(15) 0.01676(14) 0.03119(16) 0.00498(12) 0.00367(12) 0.00575(12) S4 0.0159(4) 0.0173(4) 0.0229(5) 0.0043(4) 0.0017(4) 0.0031(4) N4 0.0216(17) 0.0245(17) 0.0175(16) 0.0011(13) 0.0045(13) 0.0015(14) O11 0.0313(15) 0.0202(13) 0.0260(14) 0.0022(11) -0.0101(12) 0.0087(11) C11 0.0187(19) 0.0211(19) 0.024(2) 0.0071(16) 0.0022(16) 0.0012(15) O12 0.0333(15) 0.0167(13) 0.0345(15) -0.0005(11) -0.0071(12) 0.0085(11) C12 0.0146(18) 0.0138(17) 0.0218(19) -0.0009(14) 0.0000(15) 0.0009(14) C13 0.0211(19) 0.0155(18) 0.026(2) -0.0016(15) -0.0002(16) 0.0049(15) C14 0.0207(19) 0.0165(18) 0.023(2) -0.0008(15) -0.0055(16) 0.0041(15) C15 0.026(2) 0.031(2) 0.023(2) -0.0026(17) 0.0013(17) 0.0085(17) C16 0.037(2) 0.029(2) 0.018(2) 0.0030(16) -0.0003(17) -0.0023(18) C17 0.036(2) 0.0150(19) 0.026(2) 0.0013(16) -0.0087(18) 0.0040(17) C18 0.020(2) 0.026(2) 0.030(2) -0.0054(17) -0.0069(17) 0.0071(16) C19 0.022(2) 0.023(2) 0.0181(19) -0.0015(15) -0.0009(15) 0.0022(16) O21 0.0238(14) 0.0500(17) 0.0150(13) -0.0050(12) 0.0014(11) 0.0030(12) C21 0.024(2) 0.0145(18) 0.0183(19) -0.0003(14) 0.0053(16) 0.0039(15) O22 0.0197(14) 0.0295(14) 0.0249(14) 0.0032(11) 0.0054(11) 0.0050(11) C22 0.0194(18) 0.0147(17) 0.0138(17) -0.0014(14) 0.0016(14) 0.0049(14) C23 0.0168(18) 0.0201(18) 0.0181(18) -0.0008(15) 0.0032(15) 0.0062(15) C24 0.023(2) 0.0206(19) 0.0172(18) 0.0022(15) 0.0010(15) 0.0107(15) C25 0.022(2) 0.023(2) 0.023(2) 0.0046(16) -0.0036(16) 0.0053(16) C26 0.025(2) 0.036(2) 0.023(2) 0.0098(17) 0.0042(17) 0.0126(18) C27 0.037(2) 0.032(2) 0.0160(19) 0.0054(16) 0.0025(17) 0.0198(19) C28 0.027(2) 0.029(2) 0.0181(19) 0.0012(16) -0.0088(16) 0.0106(17) C29 0.021(2) 0.027(2) 0.024(2) 0.0042(16) -0.0001(16) 0.0087(16) O31 0.0270(14) 0.0285(14) 0.0229(14) 0.0087(11) 0.0084(11) 0.0025(12) C31 0.0188(19) 0.028(2) 0.0196(19) -0.0006(16) 0.0028(16) 0.0002(16) O32 0.0220(15) 0.078(2) 0.0308(16) 0.0143(15) 0.0120(12) 0.0224(15) C32 0.0200(19) 0.0171(18) 0.0210(19) -0.0022(15) 0.0063(15) 0.0047(15) C33 0.0175(19) 0.0221(19) 0.0206(19) -0.0002(15) 0.0009(15) 0.0051(15) C34 0.0218(19) 0.0213(19) 0.0181(19) 0.0021(15) -0.0030(15) 0.0040(15) C35 0.024(2) 0.035(2) 0.031(2) 0.0068(18) 0.0012(17) 0.0080(18) C36 0.035(2) 0.049(3) 0.035(2) 0.016(2) -0.002(2) 0.019(2) C37 0.038(2) 0.045(3) 0.023(2) 0.0120(19) 0.0014(19) 0.010(2) C38 0.034(2) 0.039(2) 0.021(2) 0.0063(17) 0.0087(17) 0.0133(19) C39 0.028(2) 0.030(2) 0.021(2) 0.0044(16) 0.0026(17) 0.0104(17) O41 0.0225(14) 0.0206(13) 0.0271(14) 0.0073(11) -0.0017(11) 0.0048(11) C41 0.022(2) 0.0156(18) 0.025(2) 0.0030(15) 0.0086(16) 0.0095(16) O42 0.0328(15) 0.0136(13) 0.0338(15) 0.0040(11) 0.0043(12) 0.0031(11) C42 0.0181(18) 0.0139(17) 0.0203(18) -0.0025(14) 0.0026(15) 0.0048(14) C43 0.024(2) 0.0122(17) 0.025(2) -0.0032(15) 0.0030(16) 0.0037(15) C44 0.022(2) 0.0206(19) 0.0205(19) -0.0047(15) -0.0050(16) 0.0017(16) C45 0.025(2) 0.027(2) 0.030(2) -0.0029(17) -0.0034(17) 0.0033(17) C46 0.033(2) 0.034(2) 0.035(2) -0.0085(19) -0.0154(19) 0.0109(19) C47 0.049(3) 0.025(2) 0.038(3) 0.0034(19) -0.020(2) 0.005(2) C48 0.037(3) 0.035(2) 0.032(2) 0.0111(19) -0.0076(19) -0.004(2) C49 0.027(2) 0.032(2) 0.028(2) 0.0063(18) -0.0038(17) 0.0048(18) C1A 0.033(2) 0.023(2) 0.044(3) 0.0086(18) 0.0104(19) 0.0045(18) C2A 0.032(2) 0.029(2) 0.021(2) 0.0064(17) 0.0010(18) 0.0048(18) C3A 0.059(3) 0.028(2) 0.030(2) -0.0019(18) 0.010(2) 0.003(2) C4A 0.021(2) 0.033(2) 0.045(3) -0.0032(19) -0.0006(18) 0.0035(18) C5A 0.020(2) 0.0131(18) 0.035(2) -0.0003(16) 0.0025(16) 0.0037(15) C6A 0.026(2) 0.031(2) 0.041(2) 0.0147(19) 0.0098(18) 0.0097(18) C1B 0.040(3) 0.041(3) 0.043(3) -0.001(2) 0.012(2) 0.016(2) C2B 0.023(2) 0.027(2) 0.037(2) 0.0057(18) 0.0069(18) 0.0060(17) C3B 0.032(2) 0.041(3) 0.049(3) 0.011(2) -0.002(2) 0.018(2) C4B 0.035(2) 0.046(3) 0.034(2) -0.008(2) 0.0035(19) 0.007(2) C5B 0.032(2) 0.026(2) 0.022(2) 0.0025(17) -0.0049(17) 0.0099(18) C6B 0.036(2) 0.030(2) 0.036(2) -0.0072(18) -0.0125(19) 0.0054(19) C1C 0.104(4) 0.023(2) 0.033(3) -0.0029(19) -0.011(3) 0.001(3) C2C 0.032(2) 0.034(2) 0.028(2) 0.0028(18) -0.0024(19) -0.0062(19) C3C 0.052(3) 0.044(3) 0.023(2) 0.0027(19) -0.004(2) -0.003(2) C4C 0.027(2) 0.058(3) 0.059(3) 0.016(2) 0.008(2) 0.020(2) C5C 0.025(2) 0.022(2) 0.033(2) 0.0110(17) 0.0130(18) 0.0096(17) C6C 0.043(3) 0.025(2) 0.042(3) 0.0009(19) 0.010(2) 0.0130(19) C1D 0.056(3) 0.099(4) 0.040(3) 0.017(3) 0.016(2) 0.053(3) C2D 0.026(2) 0.036(3) 0.040(3) 0.012(2) -0.007(2) -0.007(2) C3D 0.081(4) 0.061(3) 0.024(2) -0.009(2) -0.017(2) 0.031(3) C4D 0.051(3) 0.044(3) 0.041(3) 0.006(2) 0.008(2) 0.029(2) C5D 0.040(2) 0.031(2) 0.022(2) 0.0009(17) 0.0122(18) 0.0128(19) C6D 0.079(4) 0.032(3) 0.075(4) 0.016(2) 0.045(3) 0.017(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 S1 2.4250(10) . ? Ag1 S2 2.4330(10) . ? Ag1 O11 2.495(2) . ? Ag1 O21 2.568(2) . ? Ag1 Ag2 2.9449(8) . ? Ag1 Ag2 3.9440(8) 2_575 ? S1 C12 1.774(3) . ? S1 Ag2 2.3941(10) 2_575 ? N1 C2A 1.504(4) . ? N1 C5A 1.504(4) . ? Ag2 S1 2.3941(10) 2_575 ? Ag2 S2 2.4044(10) . ? S2 C22 1.775(3) . ? N2 C2B 1.504(5) . ? N2 C5B 1.505(4) . ? Ag3 S4 2.3990(11) 2_566 ? Ag3 S3 2.4067(10) . ? Ag3 O41 2.641(2) 2_566 ? Ag3 Ag4 3.0373(8) . ? S3 C32 1.772(3) . ? S3 Ag4 2.4310(10) . ? N3 C2C 1.502(5) . ? N3 C5C 1.506(4) . ? Ag4 S4 2.3976(10) . ? Ag4 O31 2.494(2) . ? S4 C42 1.777(3) . ? S4 Ag3 2.3990(11) 2_566 ? N4 C5D 1.508(4) . ? N4 C2D 1.509(5) . ? O11 C11 1.256(4) . ? C11 O12 1.261(4) . ? C11 C12 1.528(4) . ? C12 C13 1.339(4) . ? C13 C14 1.465(4) . ? C14 C19 1.391(4) . ? C14 C15 1.398(5) . ? C15 C16 1.380(5) . ? C16 C17 1.369(5) . ? C17 C18 1.369(5) . ? C18 C19 1.399(5) . ? O21 C21 1.254(4) . ? C21 O22 1.255(4) . ? C21 C22 1.530(4) . ? C22 C23 1.344(4) . ? C23 C24 1.468(4) . ? C24 C25 1.392(5) . ? C24 C29 1.396(5) . ? C25 C26 1.391(5) . ? C26 C27 1.384(5) . ? C27 C28 1.375(5) . ? C28 C29 1.398(5) . ? O31 C31 1.266(4) . ? C31 O32 1.249(4) . ? C31 C32 1.526(5) . ? C32 C33 1.337(4) . ? C33 C34 1.466(4) . ? C34 C39 1.387(5) . ? C34 C35 1.403(5) . ? C35 C36 1.388(5) . ? C36 C37 1.380(5) . ? C37 C38 1.384(5) . ? C38 C39 1.385(5) . ? O41 C41 1.251(4) . ? C41 O42 1.262(4) . ? C41 C42 1.542(4) . ? C42 C43 1.335(4) . ? C43 C44 1.476(5) . ? C44 C45 1.387(5) . ? C44 C49 1.402(5) . ? C45 C46 1.377(5) . ? C46 C47 1.375(6) . ? C47 C48 1.375(5) . ? C48 C49 1.392(5) . ? C1A C2A 1.512(5) . ? C2A C3A 1.510(5) . ? C4A C5A 1.518(5) . ? C5A C6A 1.513(5) . ? C1B C2B 1.521(5) . ? C2B C3B 1.522(5) . ? C4B C5B 1.506(5) . ? C5B C6B 1.524(5) . ? C1C C2C 1.508(5) . ? C2C C3C 1.506(5) . ? C4C C5C 1.508(5) . ? C5C C6C 1.521(5) . ? C1D C2D 1.512(6) . ? C2D C3D 1.508(6) . ? C4D C5D 1.509(5) . ? C5D C6D 1.509(5) . ? 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 S1 Ag1 S2 153.25(3) . . ? S1 Ag1 O11 75.87(6) . . ? S2 Ag1 O11 123.32(6) . . ? S1 Ag1 O21 127.84(6) . . ? S2 Ag1 O21 74.81(6) . . ? O11 Ag1 O21 88.80(8) . . ? S1 Ag1 Ag2 115.64(2) . . ? S2 Ag1 Ag2 52.06(2) . . ? O11 Ag1 Ag2 161.75(6) . . ? O21 Ag1 Ag2 72.95(6) . . ? S1 Ag1 Ag2 34.82(2) . 2_575 ? S2 Ag1 Ag2 134.69(3) . 2_575 ? O11 Ag1 Ag2 101.91(5) . 2_575 ? O21 Ag1 Ag2 106.22(6) . 2_575 ? Ag2 Ag1 Ag2 84.205(15) . 2_575 ? C12 S1 Ag2 108.57(11) . 2_575 ? C12 S1 Ag1 101.24(11) . . ? Ag2 S1 Ag1 109.85(4) 2_575 . ? C2A N1 C5A 118.1(3) . . ? S1 Ag2 S2 175.99(3) 2_575 . ? S1 Ag2 Ag1 127.20(3) 2_575 . ? S2 Ag2 Ag1 52.94(3) . . ? C22 S2 Ag2 100.68(11) . . ? C22 S2 Ag1 103.53(11) . . ? Ag2 S2 Ag1 75.00(3) . . ? C2B N2 C5B 117.7(3) . . ? S4 Ag3 S3 172.68(3) 2_566 . ? S4 Ag3 O41 73.57(5) 2_566 2_566 ? S3 Ag3 O41 113.64(6) . 2_566 ? S4 Ag3 Ag4 122.27(2) 2_566 . ? S3 Ag3 Ag4 51.47(2) . . ? O41 Ag3 Ag4 155.91(5) 2_566 . ? C32 S3 Ag3 100.62(11) . . ? C32 S3 Ag4 98.50(11) . . ? Ag3 S3 Ag4 77.78(3) . . ? C2C N3 C5C 117.9(3) . . ? S4 Ag4 S3 156.52(3) . . ? S4 Ag4 O31 125.86(6) . . ? S3 Ag4 O31 77.20(6) . . ? S4 Ag4 Ag3 135.28(3) . . ? S3 Ag4 Ag3 50.75(3) . . ? O31 Ag4 Ag3 70.42(5) . . ? C42 S4 Ag4 104.96(11) . . ? C42 S4 Ag3 101.68(11) . 2_566 ? Ag4 S4 Ag3 96.02(3) . 2_566 ? C5D N4 C2D 116.5(3) . . ? C11 O11 Ag1 117.5(2) . . ? O11 C11 O12 124.0(3) . . ? O11 C11 C12 119.2(3) . . ? O12 C11 C12 116.8(3) . . ? C13 C12 C11 117.2(3) . . ? C13 C12 S1 126.2(3) . . ? C11 C12 S1 116.7(2) . . ? C12 C13 C14 130.5(3) . . ? C19 C14 C15 117.8(3) . . ? C19 C14 C13 123.0(3) . . ? C15 C14 C13 119.1(3) . . ? C16 C15 C14 120.7(3) . . ? C17 C16 C15 121.0(3) . . ? C16 C17 C18 119.3(3) . . ? C17 C18 C19 120.7(3) . . ? C14 C19 C18 120.3(3) . . ? C21 O21 Ag1 118.2(2) . . ? O21 C21 O22 124.2(3) . . ? O21 C21 C22 117.8(3) . . ? O22 C21 C22 118.0(3) . . ? C23 C22 C21 116.7(3) . . ? C23 C22 S2 123.2(3) . . ? C21 C22 S2 120.2(2) . . ? C22 C23 C24 131.2(3) . . ? C25 C24 C29 117.8(3) . . ? C25 C24 C23 124.5(3) . . ? C29 C24 C23 117.7(3) . . ? C26 C25 C24 121.3(3) . . ? C27 C26 C25 119.7(3) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 119.4(3) . . ? C24 C29 C28 121.3(3) . . ? C31 O31 Ag4 115.7(2) . . ? O32 C31 O31 124.7(3) . . ? O32 C31 C32 116.6(3) . . ? O31 C31 C32 118.7(3) . . ? C33 C32 C31 116.8(3) . . ? C33 C32 S3 124.7(3) . . ? C31 C32 S3 118.4(2) . . ? C32 C33 C34 133.0(3) . . ? C39 C34 C35 118.0(3) . . ? C39 C34 C33 124.8(3) . . ? C35 C34 C33 117.2(3) . . ? C36 C35 C34 121.1(4) . . ? C37 C36 C35 119.7(4) . . ? C36 C37 C38 120.0(4) . . ? C37 C38 C39 120.2(3) . . ? C38 C39 C34 121.1(3) . . ? O41 C41 O42 125.4(3) . . ? O41 C41 C42 118.5(3) . . ? O42 C41 C42 116.1(3) . . ? C43 C42 C41 118.2(3) . . ? C43 C42 S4 125.1(3) . . ? C41 C42 S4 116.7(2) . . ? C42 C43 C44 130.7(3) . . ? C45 C44 C49 117.4(3) . . ? C45 C44 C43 119.7(3) . . ? C49 C44 C43 122.9(3) . . ? C46 C45 C44 121.3(4) . . ? C47 C46 C45 120.6(4) . . ? C48 C47 C46 119.6(4) . . ? C47 C48 C49 120.0(4) . . ? C48 C49 C44 121.0(4) . . ? N1 C2A C3A 110.5(3) . . ? N1 C2A C1A 108.2(3) . . ? C3A C2A C1A 111.9(3) . . ? N1 C5A C6A 107.7(3) . . ? N1 C5A C4A 110.7(3) . . ? C6A C5A C4A 111.8(3) . . ? N2 C2B C1B 107.7(3) . . ? N2 C2B C3B 112.2(3) . . ? C1B C2B C3B 111.9(3) . . ? N2 C5B C4B 108.9(3) . . ? N2 C5B C6B 110.1(3) . . ? C4B C5B C6B 111.7(3) . . ? N3 C2C C3C 112.3(3) . . ? N3 C2C C1C 106.5(3) . . ? C3C C2C C1C 111.5(4) . . ? N3 C5C C4C 110.8(3) . . ? N3 C5C C6C 107.7(3) . . ? C4C C5C C6C 111.6(3) . . ? C3D C2D N4 111.3(4) . . ? C3D C2D C1D 110.7(4) . . ? N4 C2D C1D 108.2(3) . . ? N4 C5D C6D 110.0(3) . . ? N4 C5D C4D 108.8(3) . . ? C6D C5D C4D 112.1(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 S2 Ag1 S1 C12 -162.02(12) . . . . ? O11 Ag1 S1 C12 -22.65(12) . . . . ? O21 Ag1 S1 C12 54.48(14) . . . . ? Ag2 Ag1 S1 C12 142.24(11) . . . . ? Ag2 Ag1 S1 C12 114.64(12) 2_575 . . . ? S2 Ag1 S1 Ag2 83.34(8) . . . 2_575 ? O11 Ag1 S1 Ag2 -137.29(7) . . . 2_575 ? O21 Ag1 S1 Ag2 -60.17(8) . . . 2_575 ? Ag2 Ag1 S1 Ag2 27.60(4) . . . 2_575 ? S1 Ag1 Ag2 S1 -33.17(5) . . . 2_575 ? S2 Ag1 Ag2 S1 174.98(4) . . . 2_575 ? O11 Ag1 Ag2 S1 93.03(17) . . . 2_575 ? O21 Ag1 Ag2 S1 91.20(6) . . . 2_575 ? Ag2 Ag1 Ag2 S1 -17.75(3) 2_575 . . 2_575 ? S1 Ag1 Ag2 S2 151.85(4) . . . . ? O11 Ag1 Ag2 S2 -81.95(17) . . . . ? O21 Ag1 Ag2 S2 -83.77(6) . . . . ? Ag2 Ag1 Ag2 S2 167.27(3) 2_575 . . . ? S1 Ag2 S2 C22 7.7(5) 2_575 . . . ? Ag1 Ag2 S2 C22 101.30(11) . . . . ? S1 Ag2 S2 Ag1 -93.6(4) 2_575 . . . ? S1 Ag1 S2 C22 -168.50(12) . . . . ? O11 Ag1 S2 C22 60.58(13) . . . . ? O21 Ag1 S2 C22 -17.62(12) . . . . ? Ag2 Ag1 S2 C22 -97.63(11) . . . . ? Ag2 Ag1 S2 C22 -115.59(11) 2_575 . . . ? S1 Ag1 S2 Ag2 -70.87(7) . . . . ? O11 Ag1 S2 Ag2 158.21(7) . . . . ? O21 Ag1 S2 Ag2 80.01(6) . . . . ? Ag2 Ag1 S2 Ag2 -17.96(4) 2_575 . . . ? S4 Ag3 S3 C32 -64.0(3) 2_566 . . . ? O41 Ag3 S3 C32 105.77(12) 2_566 . . . ? Ag4 Ag3 S3 C32 -96.51(11) . . . . ? S4 Ag3 S3 Ag4 32.5(2) 2_566 . . . ? O41 Ag3 S3 Ag4 -157.72(6) 2_566 . . . ? C32 S3 Ag4 S4 -145.91(12) . . . . ? Ag3 S3 Ag4 S4 114.98(7) . . . . ? C32 S3 Ag4 O31 24.07(12) . . . . ? Ag3 S3 Ag4 O31 -75.03(6) . . . . ? C32 S3 Ag4 Ag3 99.10(11) . . . . ? S4 Ag3 Ag4 S4 35.53(5) 2_566 . . . ? S3 Ag3 Ag4 S4 -149.12(4) . . . . ? O41 Ag3 Ag4 S4 -90.81(13) 2_566 . . . ? S4 Ag3 Ag4 S3 -175.35(4) 2_566 . . . ? O41 Ag3 Ag4 S3 58.31(13) 2_566 . . . ? S4 Ag3 Ag4 O31 -86.09(6) 2_566 . . . ? S3 Ag3 Ag4 O31 89.26(6) . . . . ? O41 Ag3 Ag4 O31 147.57(13) 2_566 . . . ? S3 Ag4 S4 C42 132.66(13) . . . . ? O31 Ag4 S4 C42 -35.26(14) . . . . ? Ag3 Ag4 S4 C42 -133.43(11) . . . . ? S3 Ag4 S4 Ag3 -123.52(7) . . . 2_566 ? O31 Ag4 S4 Ag3 68.56(8) . . . 2_566 ? Ag3 Ag4 S4 Ag3 -29.61(5) . . . 2_566 ? S1 Ag1 O11 C11 16.8(2) . . . . ? S2 Ag1 O11 C11 176.3(2) . . . . ? O21 Ag1 O11 C11 -112.8(2) . . . . ? Ag2 Ag1 O11 C11 -114.6(2) . . . . ? Ag2 Ag1 O11 C11 -6.5(2) 2_575 . . . ? Ag1 O11 C11 O12 179.0(3) . . . . ? Ag1 O11 C11 C12 -0.9(4) . . . . ? O11 C11 C12 C13 156.1(3) . . . . ? O12 C11 C12 C13 -23.9(5) . . . . ? O11 C11 C12 S1 -23.6(4) . . . . ? O12 C11 C12 S1 156.5(3) . . . . ? Ag2 S1 C12 C13 -30.7(3) 2_575 . . . ? Ag1 S1 C12 C13 -146.3(3) . . . . ? Ag2 S1 C12 C11 148.9(2) 2_575 . . . ? Ag1 S1 C12 C11 33.3(2) . . . . ? C11 C12 C13 C14 -179.9(3) . . . . ? S1 C12 C13 C14 -0.2(6) . . . . ? C12 C13 C14 C19 -38.8(6) . . . . ? C12 C13 C14 C15 143.0(4) . . . . ? C19 C14 C15 C16 2.3(5) . . . . ? C13 C14 C15 C16 -179.4(3) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 -1.3(5) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C15 C14 C19 C18 -2.4(5) . . . . ? C13 C14 C19 C18 179.4(3) . . . . ? C17 C18 C19 C14 0.7(5) . . . . ? S1 Ag1 O21 C21 -176.5(2) . . . . ? S2 Ag1 O21 C21 19.6(2) . . . . ? O11 Ag1 O21 C21 -105.5(2) . . . . ? Ag2 Ag1 O21 C21 73.9(2) . . . . ? Ag2 Ag1 O21 C21 152.4(2) 2_575 . . . ? Ag1 O21 C21 O22 167.2(2) . . . . ? Ag1 O21 C21 C22 -12.2(4) . . . . ? O21 C21 C22 C23 173.8(3) . . . . ? O22 C21 C22 C23 -5.5(4) . . . . ? O21 C21 C22 S2 -7.1(4) . . . . ? O22 C21 C22 S2 173.5(2) . . . . ? Ag2 S2 C22 C23 123.6(3) . . . . ? Ag1 S2 C22 C23 -159.4(3) . . . . ? Ag2 S2 C22 C21 -55.3(2) . . . . ? Ag1 S2 C22 C21 21.6(3) . . . . ? C21 C22 C23 C24 176.6(3) . . . . ? S2 C22 C23 C24 -2.4(5) . . . . ? C22 C23 C24 C25 33.9(6) . . . . ? C22 C23 C24 C29 -145.9(4) . . . . ? C29 C24 C25 C26 1.3(5) . . . . ? C23 C24 C25 C26 -178.4(3) . . . . ? C24 C25 C26 C27 0.8(5) . . . . ? C25 C26 C27 C28 -1.3(5) . . . . ? C26 C27 C28 C29 -0.3(5) . . . . ? C25 C24 C29 C28 -3.0(5) . . . . ? C23 C24 C29 C28 176.8(3) . . . . ? C27 C28 C29 C24 2.5(5) . . . . ? S4 Ag4 O31 C31 157.7(2) . . . . ? S3 Ag4 O31 C31 -17.4(2) . . . . ? Ag3 Ag4 O31 C31 -70.0(2) . . . . ? Ag4 O31 C31 O32 178.6(3) . . . . ? Ag4 O31 C31 C32 0.0(4) . . . . ? O32 C31 C32 C33 27.0(5) . . . . ? O31 C31 C32 C33 -154.2(3) . . . . ? O32 C31 C32 S3 -151.5(3) . . . . ? O31 C31 C32 S3 27.2(4) . . . . ? Ag3 S3 C32 C33 -136.0(3) . . . . ? Ag4 S3 C32 C33 144.9(3) . . . . ? Ag3 S3 C32 C31 42.4(3) . . . . ? Ag4 S3 C32 C31 -36.6(3) . . . . ? C31 C32 C33 C34 176.5(3) . . . . ? S3 C32 C33 C34 -5.0(6) . . . . ? C32 C33 C34 C39 -23.5(6) . . . . ? C32 C33 C34 C35 157.7(4) . . . . ? C39 C34 C35 C36 0.7(5) . . . . ? C33 C34 C35 C36 179.6(3) . . . . ? C34 C35 C36 C37 -1.0(6) . . . . ? C35 C36 C37 C38 1.1(6) . . . . ? C36 C37 C38 C39 -0.8(6) . . . . ? C37 C38 C39 C34 0.4(6) . . . . ? C35 C34 C39 C38 -0.3(5) . . . . ? C33 C34 C39 C38 -179.2(3) . . . . ? O41 C41 C42 C43 157.0(3) . . . . ? O42 C41 C42 C43 -22.3(4) . . . . ? O41 C41 C42 S4 -23.3(4) . . . . ? O42 C41 C42 S4 157.4(2) . . . . ? Ag4 S4 C42 C43 -39.6(3) . . . . ? Ag3 S4 C42 C43 -139.1(3) 2_566 . . . ? Ag4 S4 C42 C41 140.7(2) . . . . ? Ag3 S4 C42 C41 41.1(2) 2_566 . . . ? C41 C42 C43 C44 -177.2(3) . . . . ? S4 C42 C43 C44 3.1(5) . . . . ? C42 C43 C44 C45 141.3(4) . . . . ? C42 C43 C44 C49 -40.2(6) . . . . ? C49 C44 C45 C46 2.6(5) . . . . ? C43 C44 C45 C46 -178.9(3) . . . . ? C44 C45 C46 C47 -1.3(6) . . . . ? C45 C46 C47 C48 -0.9(6) . . . . ? C46 C47 C48 C49 1.8(6) . . . . ? C47 C48 C49 C44 -0.4(6) . . . . ? C45 C44 C49 C48 -1.8(5) . . . . ? C43 C44 C49 C48 179.8(3) . . . . ? C5A N1 C2A C3A 62.1(4) . . . . ? C5A N1 C2A C1A -175.1(3) . . . . ? C2A N1 C5A C6A 179.5(3) . . . . ? C2A N1 C5A C4A 56.9(4) . . . . ? C5B N2 C2B C1B -171.1(3) . . . . ? C5B N2 C2B C3B -47.5(4) . . . . ? C2B N2 C5B C4B 176.6(3) . . . . ? C2B N2 C5B C6B -60.6(4) . . . . ? C5C N3 C2C C3C -51.1(5) . . . . ? C5C N3 C2C C1C -173.5(3) . . . . ? C2C N3 C5C C4C -55.8(4) . . . . ? C2C N3 C5C C6C -178.1(3) . . . . ? C5D N4 C2D C3D -66.8(4) . . . . ? C5D N4 C2D C1D 171.3(3) . . . . ? C2D N4 C5D C6D -71.4(4) . . . . ? C2D N4 C5D C4D 165.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N1 O42 0.89(4) 1.87(4) 2.750(4) 166(3) 1_545 N2 H1N2 O12 0.82(3) 1.94(3) 2.759(4) 177(3) 1_656 N1 H2N1 O41 0.88(3) 1.91(4) 2.772(4) 163(3) 2_566 N2 H2N2 O11 1.04(4) 1.72(4) 2.751(4) 172(3) 2_666 N2 H2N2 O12 1.04(4) 2.59(4) 3.315(4) 127(3) 2_666 N3 H1N3 O31 1.02(5) 1.73(5) 2.740(4) 168(4) 2_666 N3 H2N3 O32 0.93(3) 1.78(3) 2.678(4) 162(3) . N4 H1N4 O22 0.95(3) 1.87(3) 2.802(4) 170(3) 2_676 N4 H2N4 O21 1.03(4) 1.67(4) 2.695(4) 171(4) 1_556 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.599 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.104 ################ # CCDC 637276 # ################ data_15 _database_code_depnum_ccdc_archive 'CCDC 637277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H96 Ag4 N4 O8 S4' _chemical_formula_sum 'C52 H96 Ag4 N4 O8 S4' _chemical_formula_weight 1465.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 13.115(5) _cell_length_b 17.310(5) _cell_length_c 27.739(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.078(5) _cell_angle_gamma 90.000(5) _cell_volume 6218(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 67192 _cell_measurement_theta_min 4.698 _cell_measurement_theta_max 52.728 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694006 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65382 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.48 _reflns_number_total 12808 _reflns_number_gt 10085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+54.4808P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12808 _refine_ls_number_parameters 668 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.191 _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 0.76410(4) 0.21517(3) 0.292913(18) 0.02713(14) Uani 1 1 d . . . S1 S 0.58773(12) 0.18838(10) 0.30222(6) 0.0210(3) Uani 1 1 d . A . N1 N 1.1439(4) 0.0761(3) 0.1108(2) 0.0265(13) Uani 1 1 d . . . H1A9 H 1.2136 0.0854 0.1128 0.032 Uiso 1 1 calc R . . H1B9 H 1.1367 0.0322 0.1287 0.032 Uiso 1 1 calc R . . Ag2 Ag 0.86480(4) 0.30634(3) 0.203621(18) 0.02490(13) Uani 1 1 d . A . S2 S 0.93532(12) 0.25011(10) 0.28099(6) 0.0206(3) Uani 1 1 d . A . N2 N 0.9251(4) -0.0109(3) 0.31612(19) 0.0233(12) Uani 1 1 d . . . H2A9 H 0.8621 0.0025 0.3243 0.028 Uiso 1 1 calc R . . H2B9 H 0.9452 -0.0562 0.3322 0.028 Uiso 1 1 calc R . . Ag3 Ag 0.71363(4) 0.21281(3) 0.140030(18) 0.02320(13) Uani 1 1 d . . . S3 S 0.77247(12) 0.33883(10) 0.12295(6) 0.0241(4) Uani 1 1 d . A . N3 N 0.7545(5) -0.1302(4) 0.4135(2) 0.0345(15) Uani 1 1 d . . . H3A9 H 0.7334 -0.0895 0.3930 0.041 Uiso 1 1 calc R . . H3B9 H 0.8211 -0.1420 0.4096 0.041 Uiso 1 1 calc R . . Ag4 Ag 0.59920(4) 0.13473(3) 0.223722(18) 0.02520(13) Uani 1 1 d . A . S4 S 0.64073(12) 0.08825(10) 0.14722(6) 0.0223(3) Uani 1 1 d . A . N4 N 0.6206(5) 0.4570(4) 0.2844(2) 0.0353(16) Uani 1 1 d . . . H4A9 H 0.6907 0.4481 0.2893 0.042 Uiso 1 1 calc R . . H4B9 H 0.6097 0.5009 0.3015 0.042 Uiso 1 1 calc R . . O11 O 0.6569(5) -0.0184(4) 0.3512(3) 0.0369(16) Uani 0.80 1 d PU A 1 C11 C 0.6771(5) 0.0484(4) 0.3424(2) 0.0201(13) Uani 1 1 d . . . O12 O 0.7650(5) 0.0724(4) 0.3346(2) 0.0323(14) Uani 0.80 1 d PU A 1 C12 C 0.5953(5) 0.1093(4) 0.3438(2) 0.0219(14) Uani 1 1 d . A . C13 C 0.5304(5) 0.1075(4) 0.3763(3) 0.0295(16) Uani 1 1 d . . . C14 C 0.5262(6) 0.0467(5) 0.4150(3) 0.040(2) Uani 1 1 d . A . H14A H 0.5961 0.0353 0.4327 0.048 Uiso 1 1 calc R . . H14B H 0.4952 -0.0017 0.4003 0.048 Uiso 1 1 calc R . . C15 C 0.4587(10) 0.0822(7) 0.4490(4) 0.089(5) Uani 1 1 d . . . H15A H 0.4185 0.0417 0.4628 0.107 Uiso 1 1 calc R A . H15B H 0.5018 0.1097 0.4763 0.107 Uiso 1 1 calc R . . C16 C 0.3895(8) 0.1364(6) 0.4194(4) 0.061(3) Uani 1 1 d . A . H16A H 0.3687 0.1785 0.4400 0.074 Uiso 1 1 calc R . . H16B H 0.3266 0.1095 0.4033 0.074 Uiso 1 1 calc R . . C17 C 0.4498(6) 0.1688(5) 0.3814(3) 0.039(2) Uani 1 1 d . A . H17A H 0.4040 0.1772 0.3499 0.047 Uiso 1 1 calc R . . H17B H 0.4831 0.2184 0.3925 0.047 Uiso 1 1 calc R . . O21 O 0.8821(6) 0.4389(5) 0.3515(3) 0.0349(18) Uani 0.70 1 d P A 1 C21 C 0.8832(5) 0.3976(4) 0.3150(2) 0.0220(14) Uani 1 1 d . . . O22 O 0.8262(5) 0.4076(4) 0.2738(3) 0.0291(15) Uani 0.70 1 d PU A 1 C22 C 0.9628(5) 0.3335(4) 0.3182(2) 0.0187(13) Uani 1 1 d . A . C23 C 1.0530(5) 0.3386(4) 0.3477(3) 0.0238(14) Uani 1 1 d . . . C24 C 1.1368(6) 0.2771(4) 0.3528(3) 0.0354(18) Uani 1 1 d . A . H24A H 1.1638 0.2702 0.3217 0.043 Uiso 1 1 calc R . . H24B H 1.1100 0.2270 0.3625 0.043 Uiso 1 1 calc R . . C25 C 1.2208(8) 0.3079(6) 0.3926(5) 0.091(5) Uani 1 1 d . . . H25A H 1.2198 0.2788 0.4233 0.109 Uiso 1 1 calc R A . H25B H 1.2895 0.3007 0.3827 0.109 Uiso 1 1 calc R . . C26 C 1.2038(7) 0.3865(7) 0.4003(4) 0.068(3) Uani 1 1 d . A . H26A H 1.2494 0.4181 0.3830 0.082 Uiso 1 1 calc R . . H26B H 1.2198 0.3984 0.4356 0.082 Uiso 1 1 calc R . . C27 C 1.0932(5) 0.4050(4) 0.3816(3) 0.0302(16) Uani 1 1 d . A . H27A H 1.0876 0.4546 0.3636 0.036 Uiso 1 1 calc R . . H27B H 1.0531 0.4090 0.4090 0.036 Uiso 1 1 calc R . . O31 O 1.0027(3) 0.3470(3) 0.15078(16) 0.0274(11) Uani 1 1 d . . . C31 C 0.9801(5) 0.3319(4) 0.1055(2) 0.0225(14) Uani 1 1 d . A . O32 O 1.0454(4) 0.3259(3) 0.07801(18) 0.0370(13) Uani 1 1 d . . . C32 C 0.8671(5) 0.3246(4) 0.0834(2) 0.0207(13) Uani 1 1 d . . . C33 C 0.8345(5) 0.3136(4) 0.0353(2) 0.0271(15) Uani 1 1 d . A . C34 C 0.7231(6) 0.3114(5) 0.0124(3) 0.040(2) Uani 1 1 d . . . H34A H 0.6879 0.3599 0.0191 0.048 Uiso 1 1 calc R A . H34B H 0.6873 0.2675 0.0254 0.048 Uiso 1 1 calc R . . C35 C 0.7236(8) 0.3017(8) -0.0421(3) 0.074(4) Uani 1 1 d . A . H35A H 0.6682 0.2658 -0.0564 0.088 Uiso 1 1 calc R . . H35B H 0.7125 0.3521 -0.0590 0.088 Uiso 1 1 calc R . . C36 C 0.8233(8) 0.2708(9) -0.0471(4) 0.088(5) Uani 1 1 d . . . H36A H 0.8433 0.2875 -0.0785 0.105 Uiso 1 1 calc R A . H36B H 0.8217 0.2136 -0.0464 0.105 Uiso 1 1 calc R . . C37 C 0.9005(6) 0.3016(5) -0.0042(3) 0.0365(18) Uani 1 1 d . A . H37A H 0.9561 0.2636 0.0061 0.044 Uiso 1 1 calc R . . H37B H 0.9317 0.3508 -0.0128 0.044 Uiso 1 1 calc R . . O41 O 0.4264(4) 0.0947(3) 0.17359(16) 0.0265(11) Uani 1 1 d . . . C41 C 0.4222(5) 0.1017(4) 0.1278(2) 0.0231(14) Uani 1 1 d . A . O42 O 0.3394(3) 0.1071(3) 0.09868(17) 0.0327(12) Uani 1 1 d . . . C42 C 0.5215(5) 0.1011(4) 0.1066(2) 0.0200(13) Uani 1 1 d . . . C43 C 0.5238(5) 0.1069(4) 0.0584(2) 0.0202(13) Uani 1 1 d . A . C44 C 0.4355(5) 0.1247(4) 0.0173(2) 0.0275(15) Uani 1 1 d . . . H44A H 0.3904 0.1658 0.0271 0.033 Uiso 1 1 calc R A . H44B H 0.3934 0.0780 0.0080 0.033 Uiso 1 1 calc R . . C45 C 0.4897(6) 0.1517(5) -0.0244(3) 0.040(2) Uani 1 1 d . A . H45A H 0.5066 0.2074 -0.0213 0.048 Uiso 1 1 calc R . . H45B H 0.4459 0.1425 -0.0564 0.048 Uiso 1 1 calc R . . C46 C 0.5877(6) 0.1030(5) -0.0193(2) 0.0361(18) Uani 1 1 d . . . H46A H 0.6409 0.1278 -0.0358 0.043 Uiso 1 1 calc R A . H46B H 0.5732 0.0506 -0.0330 0.043 Uiso 1 1 calc R . . C47 C 0.6219(5) 0.1000(4) 0.0361(2) 0.0253(15) Uani 1 1 d . A . H47A H 0.6575 0.0506 0.0457 0.030 Uiso 1 1 calc R . . H47B H 0.6696 0.1431 0.0470 0.030 Uiso 1 1 calc R . . C1A C 1.1552(7) -0.0109(6) 0.0425(4) 0.064(3) Uani 1 1 d . . . H1A1 H 1.1453 -0.0547 0.0637 0.096 Uiso 1 1 calc R . . H1A2 H 1.2291 -0.0003 0.0446 0.096 Uiso 1 1 calc R . . H1A3 H 1.1259 -0.0234 0.0087 0.096 Uiso 1 1 calc R . . C2A C 1.1012(6) 0.0600(5) 0.0589(3) 0.040(2) Uani 1 1 d . . . H2A H 1.0259 0.0482 0.0566 0.048 Uiso 1 1 calc R . . C3A C 1.1131(7) 0.1284(7) 0.0271(3) 0.056(3) Uani 1 1 d . . . H3A1 H 1.0771 0.1729 0.0384 0.084 Uiso 1 1 calc R . . H3A2 H 1.0833 0.1165 -0.0067 0.084 Uiso 1 1 calc R . . H3A3 H 1.1866 0.1406 0.0289 0.084 Uiso 1 1 calc R . . C4A C 1.1413(7) 0.1411(6) 0.1885(3) 0.047(2) Uani 1 1 d . . . H4A1 H 1.2167 0.1448 0.1922 0.071 Uiso 1 1 calc R . . H4A2 H 1.1221 0.0924 0.2027 0.071 Uiso 1 1 calc R . . H4A3 H 1.1143 0.1846 0.2053 0.071 Uiso 1 1 calc R . . C5A C 1.0962(5) 0.1433(4) 0.1348(2) 0.0267(15) Uani 1 1 d . . . H5A H 1.1171 0.1928 0.1205 0.032 Uiso 1 1 calc R . . C9A C 0.9792(5) 0.1383(4) 0.1268(3) 0.0339(17) Uani 1 1 d . . . H9A1 H 0.9528 0.1407 0.0917 0.051 Uiso 1 1 calc R . . H9A2 H 0.9511 0.1816 0.1434 0.051 Uiso 1 1 calc R . . H9A3 H 0.9581 0.0895 0.1401 0.051 Uiso 1 1 calc R . . C1B C 0.8275(6) -0.0893(5) 0.2526(3) 0.0378(19) Uani 1 1 d . . . H1B1 H 0.8507 -0.1354 0.2717 0.057 Uiso 1 1 calc R . . H1B2 H 0.8155 -0.1023 0.2177 0.057 Uiso 1 1 calc R . . H1B3 H 0.7632 -0.0703 0.2622 0.057 Uiso 1 1 calc R . . C2B C 0.9098(5) -0.0269(4) 0.2620(2) 0.0236(14) Uani 1 1 d . . . H2B H 0.9758 -0.0471 0.2531 0.028 Uiso 1 1 calc R . . C3B C 0.8797(6) 0.0466(5) 0.2335(3) 0.0353(18) Uani 1 1 d . . . H3B1 H 0.9353 0.0847 0.2408 0.053 Uiso 1 1 calc R . . H3B2 H 0.8162 0.0675 0.2429 0.053 Uiso 1 1 calc R . . H3B3 H 0.8682 0.0351 0.1985 0.053 Uiso 1 1 calc R . . C4B C 1.0044(10) 0.0556(6) 0.3908(3) 0.066(3) Uani 1 1 d . . . H4B1 H 0.9347 0.0655 0.3979 0.099 Uiso 1 1 calc R . . H4B2 H 1.0503 0.0978 0.4040 0.099 Uiso 1 1 calc R . . H4B3 H 1.0301 0.0068 0.4060 0.099 Uiso 1 1 calc R . . C5B C 1.0014(6) 0.0505(4) 0.3355(2) 0.0349(18) Uani 1 1 d . . . H5B H 0.9754 0.1010 0.3209 0.042 Uiso 1 1 calc R . . C6B C 1.1048(6) 0.0363(5) 0.3221(3) 0.043(2) Uani 1 1 d . . . H6B1 H 1.0990 0.0335 0.2865 0.065 Uiso 1 1 calc R . . H6B2 H 1.1324 -0.0126 0.3365 0.065 Uiso 1 1 calc R . . H6B3 H 1.1514 0.0786 0.3344 0.065 Uiso 1 1 calc R . . O11B O 0.703(2) 0.0081(16) 0.3821(11) 0.0369(16) Uani 0.20 1 d PU A 2 O12B O 0.7043(18) 0.0321(15) 0.3047(10) 0.0323(14) Uani 0.20 1 d PU A 2 O21B O 0.9095(11) 0.4632(8) 0.3235(7) 0.023(3) Uani 0.30 1 d P A 2 O22B O 0.7870(12) 0.3741(9) 0.3136(6) 0.0291(15) Uani 0.30 1 d PU A 2 C1C C 0.6892(6) -0.2075(5) 0.3422(3) 0.044(2) Uani 1 1 d . . . H1C1 H 0.7604 -0.2138 0.3363 0.067 Uiso 1 1 calc R . . H1C2 H 0.6586 -0.1618 0.3248 0.067 Uiso 1 1 calc R . . H1C3 H 0.6488 -0.2534 0.3304 0.067 Uiso 1 1 calc R . . C2C C 0.6886(5) -0.1977(4) 0.3968(3) 0.0312(16) Uani 1 1 d . . . H2C H 0.7196 -0.2449 0.4141 0.037 Uiso 1 1 calc R . . C3C C 0.5783(6) -0.1881(5) 0.4075(3) 0.0402(19) Uani 1 1 d . . . H3C1 H 0.5798 -0.1820 0.4427 0.060 Uiso 1 1 calc R . . H3C2 H 0.5375 -0.2339 0.3961 0.060 Uiso 1 1 calc R . . H3C3 H 0.5468 -0.1423 0.3905 0.060 Uiso 1 1 calc R . . C4C C 0.7948(7) -0.1672(6) 0.5004(3) 0.050(2) Uani 1 1 d . . . H4C1 H 0.7487 -0.2119 0.4942 0.075 Uiso 1 1 calc R . . H4C2 H 0.7958 -0.1491 0.5339 0.075 Uiso 1 1 calc R . . H4C3 H 0.8648 -0.1823 0.4959 0.075 Uiso 1 1 calc R . . C5C C 0.7566(7) -0.1030(5) 0.4650(3) 0.048(2) Uani 1 1 d . . . H5C H 0.6849 -0.0886 0.4696 0.058 Uiso 1 1 calc R . . C6C C 0.8245(7) -0.0319(6) 0.4726(5) 0.065(3) Uani 1 1 d . . . H6C1 H 0.7968 0.0081 0.4491 0.098 Uiso 1 1 calc R . . H6C2 H 0.8948 -0.0453 0.4677 0.098 Uiso 1 1 calc R . . H6C3 H 0.8259 -0.0125 0.5059 0.098 Uiso 1 1 calc R . . C1D C 0.6161(11) 0.3893(6) 0.3592(3) 0.082(4) Uani 1 1 d . . . H1D1 H 0.6914 0.3848 0.3627 0.123 Uiso 1 1 calc R . . H1D2 H 0.5881 0.3444 0.3742 0.123 Uiso 1 1 calc R . . H1D3 H 0.5979 0.4366 0.3753 0.123 Uiso 1 1 calc R . . C2D C 0.5712(8) 0.3923(5) 0.3057(3) 0.050(2) Uani 1 1 d . . . H2D H 0.5912 0.3436 0.2902 0.060 Uiso 1 1 calc R . . C3D C 0.4545(8) 0.3982(6) 0.2962(4) 0.056(3) Uani 1 1 d . . . H3D1 H 0.4303 0.3990 0.2609 0.084 Uiso 1 1 calc R . . H3D2 H 0.4330 0.4459 0.3108 0.084 Uiso 1 1 calc R . . H3D3 H 0.4246 0.3536 0.3107 0.084 Uiso 1 1 calc R . . C4D C 0.5995(7) 0.4024(7) 0.2018(3) 0.063(3) Uani 1 1 d . . . H4D1 H 0.5565 0.3608 0.2116 0.094 Uiso 1 1 calc R . . H4D2 H 0.6720 0.3861 0.2072 0.094 Uiso 1 1 calc R . . H4D3 H 0.5777 0.4140 0.1671 0.094 Uiso 1 1 calc R . . C5D C 0.5877(5) 0.4734(5) 0.2317(3) 0.0349(19) Uani 1 1 d . . . H5D H 0.5135 0.4895 0.2262 0.042 Uiso 1 1 calc R . . C6D C 0.6529(7) 0.5395(7) 0.2182(3) 0.058(3) Uani 1 1 d . . . H6D1 H 0.6435 0.5845 0.2385 0.088 Uiso 1 1 calc R . . H6D2 H 0.6318 0.5527 0.1837 0.088 Uiso 1 1 calc R . . H6D3 H 0.7258 0.5242 0.2237 0.088 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 0.0231(3) 0.0368(3) 0.0225(3) 0.0000(2) 0.0067(2) -0.0097(2) S1 0.0213(8) 0.0238(8) 0.0192(7) 0.0033(6) 0.0074(6) 0.0039(6) N1 0.016(3) 0.030(3) 0.034(3) 0.003(3) 0.005(2) -0.002(2) Ag2 0.0240(3) 0.0304(3) 0.0202(2) 0.0004(2) 0.00337(19) -0.0055(2) S2 0.0197(8) 0.0220(8) 0.0209(8) 0.0000(6) 0.0062(6) 0.0010(6) N2 0.027(3) 0.029(3) 0.017(3) 0.004(2) 0.012(2) 0.011(2) Ag3 0.0172(2) 0.0298(3) 0.0230(2) -0.0011(2) 0.00436(18) -0.0060(2) S3 0.0187(8) 0.0281(9) 0.0253(8) 0.0014(7) 0.0031(6) -0.0002(7) N3 0.028(3) 0.026(3) 0.054(4) 0.013(3) 0.020(3) 0.011(3) Ag4 0.0239(3) 0.0339(3) 0.0187(2) -0.0017(2) 0.00618(19) -0.0077(2) S4 0.0184(7) 0.0296(9) 0.0189(8) 0.0002(7) 0.0035(6) -0.0010(7) N4 0.036(3) 0.040(4) 0.024(3) -0.012(3) -0.013(3) 0.022(3) O11 0.030(4) 0.034(4) 0.049(4) 0.014(3) 0.014(3) 0.009(3) C11 0.018(3) 0.025(4) 0.019(3) 0.002(3) 0.006(2) 0.005(3) O12 0.024(3) 0.037(4) 0.040(4) 0.004(3) 0.018(3) 0.007(3) C12 0.025(3) 0.023(3) 0.018(3) 0.002(3) 0.006(3) 0.006(3) C13 0.027(4) 0.036(4) 0.028(4) 0.009(3) 0.014(3) 0.011(3) C14 0.041(4) 0.045(5) 0.041(4) 0.020(4) 0.029(4) 0.015(4) C15 0.100(9) 0.100(9) 0.089(8) 0.061(7) 0.079(8) 0.062(8) C16 0.058(6) 0.066(7) 0.073(7) 0.026(5) 0.051(5) 0.026(5) C17 0.036(4) 0.042(5) 0.046(5) 0.013(4) 0.025(4) 0.013(4) O21 0.031(4) 0.037(5) 0.037(4) -0.008(4) 0.007(4) 0.015(3) C21 0.018(3) 0.022(4) 0.027(3) -0.001(3) 0.006(3) 0.002(3) O22 0.024(3) 0.029(4) 0.031(3) -0.007(3) -0.003(3) 0.014(3) C22 0.021(3) 0.020(3) 0.017(3) 0.003(2) 0.007(2) -0.001(3) C23 0.017(3) 0.022(3) 0.032(4) 0.003(3) 0.002(3) 0.003(3) C24 0.027(4) 0.028(4) 0.048(5) 0.005(3) -0.005(3) 0.001(3) C25 0.049(6) 0.051(7) 0.147(12) -0.006(7) -0.062(7) 0.013(5) C26 0.038(5) 0.091(9) 0.067(7) -0.043(6) -0.019(5) 0.012(5) C27 0.028(4) 0.029(4) 0.032(4) 0.000(3) -0.001(3) 0.001(3) O31 0.023(2) 0.042(3) 0.016(2) -0.006(2) -0.0001(18) -0.007(2) C31 0.026(3) 0.024(4) 0.017(3) 0.000(3) 0.002(3) -0.006(3) O32 0.021(2) 0.068(4) 0.024(3) -0.007(3) 0.009(2) -0.014(2) C32 0.020(3) 0.023(3) 0.019(3) 0.004(3) 0.004(3) -0.003(3) C33 0.026(3) 0.034(4) 0.019(3) 0.001(3) -0.003(3) -0.007(3) C34 0.035(4) 0.049(5) 0.030(4) 0.011(4) -0.014(3) -0.008(4) C35 0.057(6) 0.131(11) 0.028(5) -0.002(6) -0.009(4) -0.035(7) C36 0.063(7) 0.160(13) 0.034(5) -0.054(7) -0.010(5) 0.017(8) C37 0.039(4) 0.048(5) 0.022(4) -0.002(3) 0.002(3) -0.006(4) O41 0.025(2) 0.035(3) 0.021(2) 0.000(2) 0.0084(19) -0.008(2) C41 0.013(3) 0.032(4) 0.025(3) -0.001(3) 0.006(3) -0.004(3) O42 0.017(2) 0.059(4) 0.023(2) -0.001(2) 0.0050(19) -0.008(2) C42 0.019(3) 0.025(3) 0.016(3) 0.003(3) 0.005(2) -0.002(3) C43 0.017(3) 0.022(3) 0.021(3) -0.003(3) 0.002(2) -0.002(3) C44 0.021(3) 0.038(4) 0.022(3) 0.004(3) 0.001(3) -0.004(3) C45 0.033(4) 0.063(6) 0.022(4) 0.011(4) 0.001(3) 0.007(4) C46 0.038(4) 0.056(5) 0.015(3) 0.000(3) 0.007(3) 0.005(4) C47 0.024(3) 0.035(4) 0.018(3) 0.000(3) 0.006(3) 0.000(3) C1A 0.030(4) 0.078(7) 0.083(7) -0.047(6) 0.009(5) -0.006(5) C2A 0.023(4) 0.057(6) 0.038(4) -0.019(4) 0.001(3) -0.002(4) C3A 0.043(5) 0.098(8) 0.025(4) 0.000(5) 0.001(4) 0.013(5) C4A 0.049(5) 0.076(7) 0.020(4) -0.004(4) 0.015(4) -0.005(5) C5A 0.026(3) 0.028(4) 0.028(4) 0.006(3) 0.011(3) -0.001(3) C9A 0.026(4) 0.028(4) 0.051(5) 0.006(4) 0.017(3) 0.003(3) C1B 0.036(4) 0.047(5) 0.029(4) 0.004(4) 0.001(3) -0.013(4) C2B 0.020(3) 0.037(4) 0.015(3) -0.002(3) 0.006(2) 0.004(3) C3B 0.041(4) 0.046(5) 0.018(3) 0.002(3) 0.003(3) 0.001(4) C4B 0.113(9) 0.063(7) 0.020(4) -0.004(4) 0.001(5) -0.014(6) C5B 0.058(5) 0.027(4) 0.017(3) 0.001(3) -0.004(3) 0.004(4) C6B 0.032(4) 0.038(5) 0.056(5) 0.006(4) -0.009(4) -0.007(4) O11B 0.030(4) 0.034(4) 0.049(4) 0.014(3) 0.014(3) 0.009(3) O12B 0.024(3) 0.037(4) 0.040(4) 0.004(3) 0.018(3) 0.007(3) O21B 0.016(7) 0.011(8) 0.043(10) -0.002(7) 0.010(7) 0.005(6) O22B 0.024(3) 0.029(4) 0.031(3) -0.007(3) -0.003(3) 0.014(3) C1C 0.039(4) 0.058(6) 0.038(4) 0.021(4) 0.012(4) 0.008(4) C2C 0.026(4) 0.028(4) 0.042(4) 0.012(3) 0.011(3) 0.007(3) C3C 0.029(4) 0.038(5) 0.057(5) 0.006(4) 0.015(4) 0.001(3) C4C 0.044(5) 0.070(7) 0.043(5) -0.012(5) 0.028(4) -0.011(5) C5C 0.035(4) 0.052(6) 0.064(6) -0.016(5) 0.027(4) 0.001(4) C6C 0.039(5) 0.057(7) 0.103(9) -0.022(6) 0.022(5) -0.005(5) C1D 0.161(13) 0.049(6) 0.028(5) 0.006(4) -0.007(6) 0.011(7) C2D 0.078(7) 0.035(5) 0.034(4) -0.006(4) 0.000(4) 0.016(5) C3D 0.075(7) 0.047(6) 0.052(6) -0.009(5) 0.028(5) -0.011(5) C4D 0.044(5) 0.107(9) 0.035(5) -0.030(5) 0.004(4) 0.013(6) C5D 0.022(3) 0.061(5) 0.021(3) -0.008(3) -0.001(3) 0.015(3) C6D 0.035(5) 0.098(8) 0.044(5) 0.002(5) 0.012(4) -0.005(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 S2 2.3984(18) . ? Ag1 S1 2.4126(19) . ? Ag1 O12 2.728(6) . ? Ag1 O22B 2.817(16) . ? Ag1 Ag4 2.9983(9) . ? Ag1 Ag2 3.3767(9) . ? S1 C12 1.782(7) . ? S1 Ag4 2.3937(17) . ? N1 C2A 1.487(9) . ? N1 C5A 1.523(9) . ? Ag2 S2 2.4047(17) . ? Ag2 S3 2.4361(18) . ? Ag2 O31 2.599(5) . ? Ag2 O22 2.726(7) . ? Ag2 Ag3 2.9257(9) . ? S2 C22 1.779(7) . ? N2 C5B 1.499(10) . ? N2 C2B 1.507(8) . ? Ag3 S4 2.3799(19) . ? Ag3 S3 2.3861(19) . ? Ag3 Ag4 3.2509(9) . ? S3 C32 1.799(6) . ? N3 C2C 1.483(10) . ? N3 C5C 1.499(11) . ? Ag4 S4 2.4108(17) . ? Ag4 O41 2.561(5) . ? Ag4 O12B 3.02(3) . ? S4 C42 1.792(6) . ? N4 C2D 1.465(12) . ? N4 C5D 1.485(9) . ? O11 C11 1.219(9) . ? C11 O12B 1.19(3) . ? C11 O12 1.275(8) . ? C11 O11B 1.30(3) . ? C11 C12 1.510(9) . ? C12 C13 1.334(9) . ? C13 C14 1.510(10) . ? C13 C17 1.521(10) . ? C14 C15 1.521(11) . ? C15 C16 1.465(13) . ? C16 C17 1.522(11) . ? O21 C21 1.242(10) . ? C21 O21B 1.199(16) . ? C21 O22 1.275(9) . ? C21 O22B 1.320(17) . ? C21 C22 1.515(9) . ? C22 C23 1.331(9) . ? C23 C24 1.521(10) . ? C23 C27 1.527(10) . ? C24 C25 1.528(12) . ? C25 C26 1.400(14) . ? C26 C27 1.497(11) . ? O31 C31 1.271(8) . ? C31 O32 1.238(8) . ? C31 C32 1.517(9) . ? C32 C33 1.349(9) . ? C33 C34 1.499(10) . ? C33 C37 1.513(10) . ? C34 C35 1.523(12) . ? C35 C36 1.440(15) . ? C36 C37 1.531(11) . ? O41 C41 1.268(8) . ? C41 O42 1.251(8) . ? C41 C42 1.512(8) . ? C42 C43 1.346(9) . ? C43 C47 1.518(9) . ? C43 C44 1.522(9) . ? C44 C45 1.525(10) . ? C45 C46 1.525(11) . ? C46 C47 1.532(9) . ? C1A C2A 1.522(12) . ? C2A C3A 1.500(13) . ? C4A C5A 1.514(10) . ? C5A C9A 1.518(9) . ? C1B C2B 1.520(10) . ? C2B C3B 1.518(10) . ? C4B C5B 1.531(10) . ? C5B C6B 1.483(11) . ? C1C C2C 1.525(11) . ? C2C C3C 1.532(10) . ? C4C C5C 1.515(13) . ? C5C C6C 1.515(13) . ? C1D C2D 1.507(12) . ? C2D C3D 1.516(14) . ? C4D C5D 1.504(12) . ? C5D C6D 1.511(13) . ? 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 S2 Ag1 S1 176.01(6) . . ? S2 Ag1 O12 110.20(13) . . ? S1 Ag1 O12 73.78(13) . . ? S2 Ag1 O22B 73.1(3) . . ? S1 Ag1 O22B 103.8(3) . . ? O12 Ag1 O22B 143.6(4) . . ? S2 Ag1 Ag4 128.71(5) . . ? S1 Ag1 Ag4 51.12(4) . . ? O12 Ag1 Ag4 78.77(14) . . ? O22B Ag1 Ag4 128.8(3) . . ? S2 Ag1 Ag2 45.41(4) . . ? S1 Ag1 Ag2 131.37(4) . . ? O12 Ag1 Ag2 139.33(12) . . ? O22B Ag1 Ag2 69.6(3) . . ? Ag4 Ag1 Ag2 94.22(3) . . ? C12 S1 Ag4 106.6(2) . . ? C12 S1 Ag1 105.1(2) . . ? Ag4 S1 Ag1 77.19(5) . . ? C2A N1 C5A 116.6(6) . . ? S2 Ag2 S3 168.15(6) . . ? S2 Ag2 O31 114.15(11) . . ? S3 Ag2 O31 73.07(11) . . ? S2 Ag2 O22 73.22(15) . . ? S3 Ag2 O22 112.72(14) . . ? O31 Ag2 O22 116.94(19) . . ? S2 Ag2 Ag3 116.28(5) . . ? S3 Ag2 Ag3 51.87(4) . . ? O31 Ag2 Ag3 106.00(10) . . ? O22 Ag2 Ag3 127.00(15) . . ? S2 Ag2 Ag1 45.25(4) . . ? S3 Ag2 Ag1 125.90(5) . . ? O31 Ag2 Ag1 158.13(11) . . ? O22 Ag2 Ag1 68.79(16) . . ? Ag3 Ag2 Ag1 82.96(2) . . ? C22 S2 Ag1 103.5(2) . . ? C22 S2 Ag2 101.7(2) . . ? Ag1 S2 Ag2 89.34(6) . . ? C5B N2 C2B 117.7(5) . . ? S4 Ag3 S3 172.63(6) . . ? S4 Ag3 Ag2 133.94(4) . . ? S3 Ag3 Ag2 53.43(4) . . ? S4 Ag3 Ag4 47.67(4) . . ? S3 Ag3 Ag4 136.22(5) . . ? Ag2 Ag3 Ag4 98.32(3) . . ? C32 S3 Ag3 105.8(2) . . ? C32 S3 Ag2 103.8(2) . . ? Ag3 S3 Ag2 74.70(5) . . ? C2C N3 C5C 117.9(6) . . ? S1 Ag4 S4 170.25(6) . . ? S1 Ag4 O41 114.95(11) . . ? S4 Ag4 O41 74.64(11) . . ? S1 Ag4 Ag1 51.69(4) . . ? S4 Ag4 Ag1 118.56(5) . . ? O41 Ag4 Ag1 163.87(11) . . ? S1 Ag4 O12B 68.8(5) . . ? S4 Ag4 O12B 108.6(5) . . ? O41 Ag4 O12B 120.4(5) . . ? Ag1 Ag4 O12B 66.3(5) . . ? S1 Ag4 Ag3 126.20(5) . . ? S4 Ag4 Ag3 46.87(4) . . ? O41 Ag4 Ag3 101.16(10) . . ? Ag1 Ag4 Ag3 84.05(3) . . ? O12B Ag4 Ag3 124.6(4) . . ? C42 S4 Ag3 99.0(2) . . ? C42 S4 Ag4 102.5(2) . . ? Ag3 S4 Ag4 85.46(6) . . ? C2D N4 C5D 117.7(6) . . ? O12B C11 O11 93.2(14) . . ? O12B C11 O12 61.6(13) . . ? O11 C11 O12 125.0(7) . . ? O12B C11 O11B 122.7(18) . . ? O11 C11 O11B 50.1(13) . . ? O12 C11 O11B 101.2(13) . . ? O12B C11 C12 120.0(13) . . ? O11 C11 C12 118.7(6) . . ? O12 C11 C12 116.2(6) . . ? O11B C11 C12 116.5(13) . . ? C11 O12 Ag1 115.0(5) . . ? C13 C12 C11 122.1(6) . . ? C13 C12 S1 118.6(5) . . ? C11 C12 S1 119.2(5) . . ? C12 C13 C14 126.6(6) . . ? C12 C13 C17 124.9(6) . . ? C14 C13 C17 108.4(6) . . ? C13 C14 C15 104.5(7) . . ? C16 C15 C14 106.3(8) . . ? C15 C16 C17 106.3(7) . . ? C13 C17 C16 104.6(6) . . ? O21B C21 O21 48.4(9) . . ? O21B C21 O22 99.0(10) . . ? O21 C21 O22 124.9(7) . . ? O21B C21 O22B 122.8(11) . . ? O21 C21 O22B 93.9(9) . . ? O22 C21 O22B 65.9(8) . . ? O21B C21 C22 120.5(9) . . ? O21 C21 C22 118.0(6) . . ? O22 C21 C22 117.0(6) . . ? O22B C21 C22 115.0(9) . . ? C21 O22 Ag2 113.8(5) . . ? C23 C22 C21 121.7(6) . . ? C23 C22 S2 119.2(5) . . ? C21 C22 S2 119.1(5) . . ? C22 C23 C24 124.8(6) . . ? C22 C23 C27 127.9(6) . . ? C24 C23 C27 107.2(6) . . ? C23 C24 C25 104.6(7) . . ? C26 C25 C24 109.6(7) . . ? C25 C26 C27 109.0(8) . . ? C26 C27 C23 105.8(6) . . ? C31 O31 Ag2 115.2(4) . . ? O32 C31 O31 123.3(6) . . ? O32 C31 C32 118.1(6) . . ? O31 C31 C32 118.6(6) . . ? C33 C32 C31 123.3(6) . . ? C33 C32 S3 118.8(5) . . ? C31 C32 S3 117.7(5) . . ? C32 C33 C34 123.8(7) . . ? C32 C33 C37 127.4(6) . . ? C34 C33 C37 108.8(6) . . ? C33 C34 C35 105.4(7) . . ? C36 C35 C34 106.4(8) . . ? C35 C36 C37 107.1(8) . . ? C33 C37 C36 103.1(7) . . ? C41 O41 Ag4 114.4(4) . . ? O42 C41 O41 123.4(6) . . ? O42 C41 C42 117.5(6) . . ? O41 C41 C42 119.0(6) . . ? C43 C42 C41 122.9(6) . . ? C43 C42 S4 118.7(5) . . ? C41 C42 S4 118.4(4) . . ? C42 C43 C47 123.5(6) . . ? C42 C43 C44 128.7(6) . . ? C47 C43 C44 107.7(5) . . ? C43 C44 C45 103.9(5) . . ? C44 C45 C46 104.3(6) . . ? C45 C46 C47 102.8(6) . . ? C43 C47 C46 105.8(5) . . ? N1 C2A C3A 111.2(7) . . ? N1 C2A C1A 108.6(7) . . ? C3A C2A C1A 111.4(8) . . ? C4A C5A C9A 111.8(6) . . ? C4A C5A N1 106.7(6) . . ? C9A C5A N1 111.6(6) . . ? N2 C2B C3B 110.3(6) . . ? N2 C2B C1B 106.4(5) . . ? C3B C2B C1B 112.7(6) . . ? C6B C5B N2 112.2(6) . . ? C6B C5B C4B 112.4(8) . . ? N2 C5B C4B 108.1(7) . . ? C11 O12B Ag4 110.5(14) . . ? C21 O22B Ag1 112.2(9) . . ? N3 C2C C1C 107.8(6) . . ? N3 C2C C3C 112.0(6) . . ? C1C C2C C3C 110.9(7) . . ? N3 C5C C6C 108.1(8) . . ? N3 C5C C4C 109.9(7) . . ? C6C C5C C4C 112.3(8) . . ? N4 C2D C1D 107.2(8) . . ? N4 C2D C3D 112.1(7) . . ? C1D C2D C3D 113.6(9) . . ? N4 C5D C4D 110.3(7) . . ? N4 C5D C6D 107.4(7) . . ? C4D C5D C6D 111.8(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 S2 Ag1 S1 C12 -166.9(9) . . . . ? O12 Ag1 S1 C12 15.5(3) . . . . ? O22B Ag1 S1 C12 -126.9(4) . . . . ? Ag4 Ag1 S1 C12 104.0(2) . . . . ? Ag2 Ag1 S1 C12 158.3(2) . . . . ? S2 Ag1 S1 Ag4 89.2(9) . . . . ? O12 Ag1 S1 Ag4 -88.51(15) . . . . ? O22B Ag1 S1 Ag4 129.1(3) . . . . ? Ag2 Ag1 S1 Ag4 54.27(7) . . . . ? S1 Ag1 Ag2 S2 176.80(8) . . . . ? O12 Ag1 Ag2 S2 -66.2(2) . . . . ? O22B Ag1 Ag2 S2 86.1(3) . . . . ? Ag4 Ag1 Ag2 S2 -143.88(6) . . . . ? S2 Ag1 Ag2 S3 169.61(8) . . . . ? S1 Ag1 Ag2 S3 -13.59(9) . . . . ? O12 Ag1 Ag2 S3 103.4(2) . . . . ? O22B Ag1 Ag2 S3 -104.3(3) . . . . ? Ag4 Ag1 Ag2 S3 25.73(6) . . . . ? S2 Ag1 Ag2 O31 22.7(3) . . . . ? S1 Ag1 Ag2 O31 -160.5(3) . . . . ? O12 Ag1 Ag2 O31 -43.5(4) . . . . ? O22B Ag1 Ag2 O31 108.8(4) . . . . ? Ag4 Ag1 Ag2 O31 -121.2(3) . . . . ? S2 Ag1 Ag2 O22 -87.06(15) . . . . ? S1 Ag1 Ag2 O22 89.74(16) . . . . ? O12 Ag1 Ag2 O22 -153.3(3) . . . . ? O22B Ag1 Ag2 O22 -1.0(4) . . . . ? Ag4 Ag1 Ag2 O22 129.06(15) . . . . ? S2 Ag1 Ag2 Ag3 138.64(6) . . . . ? S1 Ag1 Ag2 Ag3 -44.56(6) . . . . ? O12 Ag1 Ag2 Ag3 72.4(2) . . . . ? O22B Ag1 Ag2 Ag3 -135.3(3) . . . . ? Ag4 Ag1 Ag2 Ag3 -5.24(2) . . . . ? S1 Ag1 S2 C22 64.8(9) . . . . ? O12 Ag1 S2 C22 -117.5(3) . . . . ? O22B Ag1 S2 C22 24.2(4) . . . . ? Ag4 Ag1 S2 C22 150.8(2) . . . . ? Ag2 Ag1 S2 C22 101.9(2) . . . . ? S1 Ag1 S2 Ag2 -37.1(9) . . . . ? O12 Ag1 S2 Ag2 140.54(15) . . . . ? O22B Ag1 S2 Ag2 -77.7(3) . . . . ? Ag4 Ag1 S2 Ag2 48.88(7) . . . . ? S3 Ag2 S2 C22 -148.9(3) . . . . ? O31 Ag2 S2 C22 85.4(2) . . . . ? O22 Ag2 S2 C22 -27.1(3) . . . . ? Ag3 Ag2 S2 C22 -150.6(2) . . . . ? Ag1 Ag2 S2 C22 -103.6(2) . . . . ? S3 Ag2 S2 Ag1 -45.3(3) . . . . ? O31 Ag2 S2 Ag1 -170.94(12) . . . . ? O22 Ag2 S2 Ag1 76.51(16) . . . . ? Ag3 Ag2 S2 Ag1 -47.00(6) . . . . ? S2 Ag2 Ag3 S4 -0.05(8) . . . . ? S3 Ag2 Ag3 S4 -179.61(8) . . . . ? O31 Ag2 Ag3 S4 128.00(13) . . . . ? O22 Ag2 Ag3 S4 -88.3(2) . . . . ? Ag1 Ag2 Ag3 S4 -31.61(6) . . . . ? S2 Ag2 Ag3 S3 179.57(7) . . . . ? O31 Ag2 Ag3 S3 -52.39(13) . . . . ? O22 Ag2 Ag3 S3 91.3(2) . . . . ? Ag1 Ag2 Ag3 S3 148.01(5) . . . . ? S2 Ag2 Ag3 Ag4 36.43(5) . . . . ? S3 Ag2 Ag3 Ag4 -143.14(5) . . . . ? O31 Ag2 Ag3 Ag4 164.48(12) . . . . ? O22 Ag2 Ag3 Ag4 -51.79(19) . . . . ? Ag1 Ag2 Ag3 Ag4 4.87(2) . . . . ? S4 Ag3 S3 C32 -81.8(5) . . . . ? Ag2 Ag3 S3 C32 100.3(2) . . . . ? Ag4 Ag3 S3 C32 159.4(2) . . . . ? S4 Ag3 S3 Ag2 177.8(5) . . . . ? Ag4 Ag3 S3 Ag2 59.09(7) . . . . ? S2 Ag2 S3 C32 -104.8(4) . . . . ? O31 Ag2 S3 C32 24.4(2) . . . . ? O22 Ag2 S3 C32 137.1(3) . . . . ? Ag3 Ag2 S3 C32 -102.9(2) . . . . ? Ag1 Ag2 S3 C32 -143.4(2) . . . . ? S2 Ag2 S3 Ag3 -1.9(3) . . . . ? O31 Ag2 S3 Ag3 127.25(12) . . . . ? O22 Ag2 S3 Ag3 -120.05(17) . . . . ? Ag1 Ag2 S3 Ag3 -40.48(6) . . . . ? C12 S1 Ag4 S4 -102.3(4) . . . . ? Ag1 S1 Ag4 S4 -0.1(4) . . . . ? C12 S1 Ag4 O41 88.5(3) . . . . ? Ag1 S1 Ag4 O41 -169.34(12) . . . . ? C12 S1 Ag4 Ag1 -102.2(2) . . . . ? C12 S1 Ag4 O12B -26.2(6) . . . . ? Ag1 S1 Ag4 O12B 76.0(5) . . . . ? C12 S1 Ag4 Ag3 -144.3(2) . . . . ? Ag1 S1 Ag4 Ag3 -42.10(6) . . . . ? S2 Ag1 Ag4 S1 -174.89(8) . . . . ? O12 Ag1 Ag4 S1 78.13(13) . . . . ? O22B Ag1 Ag4 S1 -75.3(4) . . . . ? Ag2 Ag1 Ag4 S1 -142.35(5) . . . . ? S2 Ag1 Ag4 S4 5.09(8) . . . . ? S1 Ag1 Ag4 S4 179.98(7) . . . . ? O12 Ag1 Ag4 S4 -101.89(13) . . . . ? O22B Ag1 Ag4 S4 104.7(4) . . . . ? Ag2 Ag1 Ag4 S4 37.63(6) . . . . ? S2 Ag1 Ag4 O41 -137.7(4) . . . . ? S1 Ag1 Ag4 O41 37.1(4) . . . . ? O12 Ag1 Ag4 O41 115.3(4) . . . . ? O22B Ag1 Ag4 O41 -38.1(6) . . . . ? Ag2 Ag1 Ag4 O41 -105.2(4) . . . . ? S2 Ag1 Ag4 O12B 104.2(5) . . . . ? S1 Ag1 Ag4 O12B -81.0(5) . . . . ? O12 Ag1 Ag4 O12B -2.8(5) . . . . ? O22B Ag1 Ag4 O12B -156.2(6) . . . . ? Ag2 Ag1 Ag4 O12B 136.7(5) . . . . ? S2 Ag1 Ag4 Ag3 -27.84(6) . . . . ? S1 Ag1 Ag4 Ag3 147.05(5) . . . . ? O12 Ag1 Ag4 Ag3 -134.82(12) . . . . ? O22B Ag1 Ag4 Ag3 71.8(4) . . . . ? Ag2 Ag1 Ag4 Ag3 4.704(19) . . . . ? S4 Ag3 Ag4 S1 171.07(8) . . . . ? S3 Ag3 Ag4 S1 -17.68(9) . . . . ? Ag2 Ag3 Ag4 S1 26.46(6) . . . . ? S3 Ag3 Ag4 S4 171.25(8) . . . . ? Ag2 Ag3 Ag4 S4 -144.61(6) . . . . ? S4 Ag3 Ag4 O41 -56.30(13) . . . . ? S3 Ag3 Ag4 O41 114.95(13) . . . . ? Ag2 Ag3 Ag4 O41 159.08(12) . . . . ? S4 Ag3 Ag4 Ag1 139.14(6) . . . . ? S3 Ag3 Ag4 Ag1 -49.61(7) . . . . ? Ag2 Ag3 Ag4 Ag1 -5.47(2) . . . . ? S4 Ag3 Ag4 O12B 83.4(6) . . . . ? S3 Ag3 Ag4 O12B -105.4(6) . . . . ? Ag2 Ag3 Ag4 O12B -61.3(6) . . . . ? S3 Ag3 S4 C42 -22.9(5) . . . . ? Ag2 Ag3 S4 C42 154.7(2) . . . . ? Ag4 Ag3 S4 C42 102.0(2) . . . . ? S3 Ag3 S4 Ag4 -124.9(5) . . . . ? Ag2 Ag3 S4 Ag4 52.72(7) . . . . ? S1 Ag4 S4 C42 -146.0(4) . . . . ? O41 Ag4 S4 C42 23.9(2) . . . . ? Ag1 Ag4 S4 C42 -146.1(2) . . . . ? O12B Ag4 S4 C42 141.3(6) . . . . ? Ag3 Ag4 S4 C42 -98.3(2) . . . . ? S1 Ag4 S4 Ag3 -47.7(4) . . . . ? O41 Ag4 S4 Ag3 122.17(12) . . . . ? Ag1 Ag4 S4 Ag3 -47.81(6) . . . . ? O12B Ag4 S4 Ag3 -120.4(5) . . . . ? O12B C11 O12 Ag1 91.8(15) . . . . ? O11 C11 O12 Ag1 164.3(6) . . . . ? O11B C11 O12 Ag1 -146.9(14) . . . . ? C12 C11 O12 Ag1 -19.7(7) . . . . ? S2 Ag1 O12 C11 -179.9(5) . . . . ? S1 Ag1 O12 C11 0.0(5) . . . . ? O22B Ag1 O12 C11 91.4(8) . . . . ? Ag4 Ag1 O12 C11 -52.6(5) . . . . ? Ag2 Ag1 O12 C11 -135.9(4) . . . . ? O12B C11 C12 C13 149.7(16) . . . . ? O11 C11 C12 C13 36.8(10) . . . . ? O12 C11 C12 C13 -139.5(7) . . . . ? O11B C11 C12 C13 -20.3(18) . . . . ? O12B C11 C12 S1 -32.7(17) . . . . ? O11 C11 C12 S1 -145.6(6) . . . . ? O12 C11 C12 S1 38.2(8) . . . . ? O11B C11 C12 S1 157.4(16) . . . . ? Ag4 S1 C12 C13 -136.2(6) . . . . ? Ag1 S1 C12 C13 143.0(6) . . . . ? Ag4 S1 C12 C11 46.1(5) . . . . ? Ag1 S1 C12 C11 -34.7(5) . . . . ? C11 C12 C13 C14 -1.0(12) . . . . ? S1 C12 C13 C14 -178.6(7) . . . . ? C11 C12 C13 C17 176.9(7) . . . . ? S1 C12 C13 C17 -0.8(11) . . . . ? C12 C13 C14 C15 166.4(10) . . . . ? C17 C13 C14 C15 -11.7(11) . . . . ? C13 C14 C15 C16 27.3(13) . . . . ? C14 C15 C16 C17 -32.6(14) . . . . ? C12 C13 C17 C16 174.5(8) . . . . ? C14 C13 C17 C16 -7.4(10) . . . . ? C15 C16 C17 C13 24.6(12) . . . . ? O21B C21 O22 Ag2 132.1(9) . . . . ? O21 C21 O22 Ag2 176.8(7) . . . . ? O22B C21 O22 Ag2 -106.0(9) . . . . ? C22 C21 O22 Ag2 1.0(8) . . . . ? S2 Ag2 O22 C21 19.2(5) . . . . ? S3 Ag2 O22 C21 -171.7(5) . . . . ? O31 Ag2 O22 C21 -89.8(6) . . . . ? Ag3 Ag2 O22 C21 129.8(5) . . . . ? Ag1 Ag2 O22 C21 67.0(5) . . . . ? O21B C21 C22 C23 27.7(14) . . . . ? O21 C21 C22 C23 -28.2(10) . . . . ? O22 C21 C22 C23 148.0(7) . . . . ? O22B C21 C22 C23 -137.6(10) . . . . ? O21B C21 C22 S2 -151.4(11) . . . . ? O21 C21 C22 S2 152.6(7) . . . . ? O22 C21 C22 S2 -31.2(8) . . . . ? O22B C21 C22 S2 43.2(10) . . . . ? Ag1 S2 C22 C23 133.0(5) . . . . ? Ag2 S2 C22 C23 -134.8(5) . . . . ? Ag1 S2 C22 C21 -47.8(5) . . . . ? Ag2 S2 C22 C21 44.4(5) . . . . ? C21 C22 C23 C24 -179.7(6) . . . . ? S2 C22 C23 C24 -0.5(10) . . . . ? C21 C22 C23 C27 -0.6(11) . . . . ? S2 C22 C23 C27 178.6(6) . . . . ? C22 C23 C24 C25 -176.9(9) . . . . ? C27 C23 C24 C25 3.8(10) . . . . ? C23 C24 C25 C26 -15.1(14) . . . . ? C24 C25 C26 C27 20.7(15) . . . . ? C25 C26 C27 C23 -17.6(13) . . . . ? C22 C23 C27 C26 -171.5(8) . . . . ? C24 C23 C27 C26 7.7(9) . . . . ? S2 Ag2 O31 C31 138.8(4) . . . . ? S3 Ag2 O31 C31 -31.2(4) . . . . ? O22 Ag2 O31 C31 -138.5(5) . . . . ? Ag3 Ag2 O31 C31 9.5(5) . . . . ? Ag1 Ag2 O31 C31 121.3(4) . . . . ? Ag2 O31 C31 O32 -158.1(6) . . . . ? Ag2 O31 C31 C32 24.9(7) . . . . ? O32 C31 C32 C33 -1.5(10) . . . . ? O31 C31 C32 C33 175.7(7) . . . . ? O32 C31 C32 S3 -176.6(5) . . . . ? O31 C31 C32 S3 0.6(8) . . . . ? Ag3 S3 C32 C33 81.4(6) . . . . ? Ag2 S3 C32 C33 159.1(5) . . . . ? Ag3 S3 C32 C31 -103.3(5) . . . . ? Ag2 S3 C32 C31 -25.6(5) . . . . ? C31 C32 C33 C34 -175.8(7) . . . . ? S3 C32 C33 C34 -0.8(10) . . . . ? C31 C32 C33 C37 4.2(12) . . . . ? S3 C32 C33 C37 179.2(6) . . . . ? C32 C33 C34 C35 177.3(8) . . . . ? C37 C33 C34 C35 -2.7(10) . . . . ? C33 C34 C35 C36 20.7(12) . . . . ? C34 C35 C36 C37 -30.7(14) . . . . ? C32 C33 C37 C36 165.1(9) . . . . ? C34 C33 C37 C36 -14.9(10) . . . . ? C35 C36 C37 C33 28.3(13) . . . . ? S1 Ag4 O41 C41 148.0(4) . . . . ? S4 Ag4 O41 C41 -30.1(5) . . . . ? Ag1 Ag4 O41 C41 116.5(5) . . . . ? O12B Ag4 O41 C41 -133.0(7) . . . . ? Ag3 Ag4 O41 C41 8.9(5) . . . . ? Ag4 O41 C41 O42 -158.5(6) . . . . ? Ag4 O41 C41 C42 23.6(8) . . . . ? O42 C41 C42 C43 0.8(10) . . . . ? O41 C41 C42 C43 178.8(7) . . . . ? O42 C41 C42 S4 -176.7(5) . . . . ? O41 C41 C42 S4 1.4(9) . . . . ? Ag3 S4 C42 C43 69.8(6) . . . . ? Ag4 S4 C42 C43 157.2(5) . . . . ? Ag3 S4 C42 C41 -112.6(5) . . . . ? Ag4 S4 C42 C41 -25.3(5) . . . . ? C41 C42 C43 C47 -174.9(6) . . . . ? S4 C42 C43 C47 2.5(9) . . . . ? C41 C42 C43 C44 8.3(11) . . . . ? S4 C42 C43 C44 -174.3(6) . . . . ? C42 C43 C44 C45 160.4(7) . . . . ? C47 C43 C44 C45 -16.8(8) . . . . ? C43 C44 C45 C46 34.9(8) . . . . ? C44 C45 C46 C47 -39.5(8) . . . . ? C42 C43 C47 C46 175.1(7) . . . . ? C44 C43 C47 C46 -7.5(8) . . . . ? C45 C46 C47 C43 28.7(8) . . . . ? C5A N1 C2A C3A 59.6(8) . . . . ? C5A N1 C2A C1A -177.4(6) . . . . ? C2A N1 C5A C4A 172.3(6) . . . . ? C2A N1 C5A C9A 49.9(8) . . . . ? C5B N2 C2B C3B -56.0(7) . . . . ? C5B N2 C2B C1B -178.5(6) . . . . ? C2B N2 C5B C6B -54.8(8) . . . . ? C2B N2 C5B C4B -179.3(7) . . . . ? O11 C11 O12B Ag4 129.8(10) . . . . ? O12 C11 O12B Ag4 -101.7(14) . . . . ? O11B C11 O12B Ag4 173.1(16) . . . . ? C12 C11 O12B Ag4 3.8(19) . . . . ? S1 Ag4 O12B C11 17.1(14) . . . . ? S4 Ag4 O12B C11 -172.9(14) . . . . ? O41 Ag4 O12B C11 -90.2(17) . . . . ? Ag1 Ag4 O12B C11 73.3(16) . . . . ? Ag3 Ag4 O12B C11 137.2(13) . . . . ? O21B C21 O22B Ag1 -179.7(12) . . . . ? O21 C21 O22B Ag1 -138.1(8) . . . . ? O22 C21 O22B Ag1 95.1(8) . . . . ? C22 C21 O22B Ag1 -14.7(11) . . . . ? S2 Ag1 O22B C21 -9.0(9) . . . . ? S1 Ag1 O22B C21 173.6(9) . . . . ? O12 Ag1 O22B C21 92.3(11) . . . . ? Ag4 Ag1 O22B C21 -135.5(8) . . . . ? Ag2 Ag1 O22B C21 -57.0(9) . . . . ? C5C N3 C2C C1C 173.1(6) . . . . ? C5C N3 C2C C3C 50.8(9) . . . . ? C2C N3 C5C C6C -177.3(7) . . . . ? C2C N3 C5C C4C 59.8(9) . . . . ? C5D N4 C2D C1D -178.7(8) . . . . ? C5D N4 C2D C3D -53.4(9) . . . . ? C2D N4 C5D C4D -55.3(9) . . . . ? C2D N4 C5D C6D -177.4(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A9 O42 0.92 1.79 2.691(7) 163.9 1_655 N1 H1B9 O21 0.92 1.74 2.639(9) 166.0 2_745 N1 H1B9 O21B 0.92 1.95 2.835(17) 160.2 2_745 N2 H2A9 O12 0.92 1.81 2.663(8) 152.6 . N2 H2A9 O12B 0.92 2.12 2.96(2) 151.3 . N2 H2B9 O31 0.92 1.84 2.741(7) 165.0 2_745 N3 H3A9 O11B 0.92 1.75 2.60(3) 152.1 . N3 H3A9 O11 0.92 1.87 2.771(9) 165.2 . N3 H3B9 O32 0.92 1.82 2.706(7) 161.8 2_745 N4 H4A9 O22B 0.92 1.85 2.630(16) 141.1 . N4 H4A9 O22 0.92 2.02 2.886(9) 156.7 . N4 H4B9 O41 0.92 1.85 2.765(8) 170.3 2_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.560 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.148 #### END