# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p _database_code_depnum_ccdc_archive 'CCDC 940871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H132 Ag20 N14 O33 S10' _chemical_formula_weight 4043.79 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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 16.9534(18) _cell_length_b 12.6293(13) _cell_length_c 26.729(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.474(2) _cell_angle_gamma 90.00 _cell_volume 5717.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2900 _cell_measurement_theta_min 4.803 _cell_measurement_theta_max 38.014 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3896 _exptl_absorpt_coefficient_mu 3.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6726 _exptl_absorpt_correction_T_max 0.7622 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 SMART APEX II CCD area detector' _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 27333 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10019 _reflns_number_gt 5322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. Two of the tert-butyl groups (C10-C12 and C18-C20) show rotational disorder, and was refined with equal occupancies. The carbonate ion (O13, O14, O15) was disordered with equal occupancies related to the inversion centre. Due to relatively large thermal motion of the tert-butyl groups, the Ueq of C atoms on two tert-butyl groups (C20 C20A C18 C18A C19 C19A, C12 C10A C10 C11A C11 C12A and C6 C8 C7 C5) were restrained by using the command SIMU. Similarly, the nitrate ion (N7 O18 O16 O17) and carbonate ion (O15 C21 O14 O13) were also restrained by using the command SIMU. The geometry restraints such DFIX and FLAT were used to give the disordered motifs much more reasonable geometries. The Ag9 atom was disordered and refined with splitting mode. The occupancy factor of the disordered Ag atoms is Ag9:Ag9a 0.60:0.40. . ; _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^)+(0.0748P)^2^+155.9455P] 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 10019 _refine_ls_number_parameters 692 _refine_ls_number_restraints 195 _refine_ls_R_factor_all 0.1661 _refine_ls_R_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.2309 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.011 _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 0.96867(9) 0.53905(13) 0.32199(6) 0.0541(4) Uani 1 1 d . . . Ag2 Ag 0.81484(9) 0.45513(13) 0.36156(7) 0.0611(5) Uani 1 1 d . . . Ag3 Ag 0.72474(9) 0.36962(14) 0.45106(7) 0.0658(5) Uani 1 1 d . . . Ag4 Ag 0.96917(8) 0.35403(14) 0.39576(6) 0.0572(4) Uani 1 1 d . . . Ag5 Ag 1.13917(10) 0.60986(15) 0.34849(6) 0.0697(5) Uani 1 1 d . . . Ag6 Ag 1.01030(9) 0.68470(14) 0.41074(6) 0.0613(5) Uani 1 1 d . . . Ag7 Ag 0.82583(9) 0.57752(15) 0.45758(7) 0.0662(5) Uani 1 1 d . . . Ag8 Ag 0.72530(10) 0.34507(16) 0.57271(7) 0.0716(5) Uani 1 1 d . . . Ag9 Ag 1.1301(3) 0.7350(4) 0.50466(17) 0.0866(14) Uani 0.60 1 d PU . . Ag9A Ag 1.1059(5) 0.7878(5) 0.5049(2) 0.089(2) Uani 0.40 1 d PU . . Ag10 Ag 1.16485(11) 0.44017(18) 0.42369(7) 0.0881(7) Uani 1 1 d . . . S1 S 1.0805(3) 0.4212(4) 0.35031(18) 0.0510(13) Uani 1 1 d . . . S2 S 0.7330(3) 0.5092(4) 0.51672(19) 0.0535(13) Uani 1 1 d . . . S3 S 0.8795(3) 0.6329(4) 0.37872(19) 0.0483(12) Uani 1 1 d . . . S4 S 1.1452(3) 0.7513(5) 0.4161(2) 0.0612(14) Uani 1 1 d . . . S5 S 0.8376(3) 0.2865(4) 0.41017(19) 0.0523(13) Uani 1 1 d . . . C1 C 1.1166(11) 0.3243(18) 0.3042(7) 0.057(6) Uani 1 1 d . . . C2 C 1.1274(15) 0.382(2) 0.2553(8) 0.083(8) Uani 1 1 d . . . H2A H 1.1343 0.3308 0.2284 0.125 Uiso 1 1 calc R . . H2B H 1.1742 0.4278 0.2586 0.125 Uiso 1 1 calc R . . H2C H 1.0807 0.4259 0.2473 0.125 Uiso 1 1 calc R . . C3 C 1.1918(15) 0.276(2) 0.3228(11) 0.113(11) Uani 1 1 d . . . H3A H 1.2350 0.3267 0.3187 0.170 Uiso 1 1 calc R . . H3B H 1.2020 0.2118 0.3036 0.170 Uiso 1 1 calc R . . H3C H 1.1884 0.2583 0.3583 0.170 Uiso 1 1 calc R . . C4 C 1.0526(15) 0.238(2) 0.2951(8) 0.085(8) Uani 1 1 d . . . H4A H 1.0703 0.1872 0.2702 0.127 Uiso 1 1 calc R . . H4B H 1.0033 0.2712 0.2827 0.127 Uiso 1 1 calc R . . H4C H 1.0437 0.2009 0.3265 0.127 Uiso 1 1 calc R . . C5 C 0.6446(13) 0.5983(19) 0.5187(8) 0.073(7) Uani 1 1 d DU . . C6 C 0.665(3) 0.701(2) 0.5442(16) 0.199(18) Uiso 1 1 d DU . . H6A H 0.6940 0.6864 0.5761 0.299 Uiso 1 1 calc R . . H6B H 0.6168 0.7399 0.5505 0.299 Uiso 1 1 calc R . . H6C H 0.6985 0.7430 0.5227 0.299 Uiso 1 1 calc R . . C7 C 0.5899(19) 0.542(3) 0.5522(13) 0.150(13) Uiso 1 1 d DU . . H7A H 0.5500 0.5918 0.5635 0.225 Uiso 1 1 calc R . . H7B H 0.6200 0.5138 0.5814 0.225 Uiso 1 1 calc R . . H7C H 0.5639 0.4837 0.5338 0.225 Uiso 1 1 calc R . . C8 C 0.6150(13) 0.615(2) 0.4666(8) 0.080(8) Uani 1 1 d U . . H8A H 0.6547 0.6536 0.4481 0.120 Uiso 1 1 calc R . . H8B H 0.5662 0.6567 0.4665 0.120 Uiso 1 1 calc R . . H8C H 0.6044 0.5466 0.4505 0.120 Uiso 1 1 calc R . . C9 C 0.8209(9) 0.7454(12) 0.3480(6) 0.047(5) Uani 1 1 d D . . C10 C 0.8716(16) 0.842(2) 0.3554(14) 0.086(7) Uani 0.50 1 d PDU . . H10A H 0.8453 0.9026 0.3408 0.129 Uiso 0.50 1 d PR . . H10B H 0.8811 0.8537 0.3906 0.129 Uiso 0.50 1 d PR . . H10C H 0.9210 0.8316 0.3399 0.129 Uiso 0.50 1 d PR . . C10A C 0.8653(18) 0.797(3) 0.3065(11) 0.086(7) Uani 0.50 1 d PDU . . H10F H 0.8338 0.8528 0.2921 0.129 Uiso 0.50 1 d PR . . H10D H 0.9143 0.8248 0.3201 0.129 Uiso 0.50 1 d PR . . H10G H 0.8758 0.7451 0.2812 0.129 Uiso 0.50 1 d PR . . C11 C 0.7445(14) 0.753(3) 0.3746(12) 0.085(7) Uani 0.50 1 d PDU . . H11A H 0.7131 0.8096 0.3600 0.127 Uiso 0.50 1 d PR . . H11B H 0.7163 0.6877 0.3709 0.127 Uiso 0.50 1 d PR . . H11C H 0.7553 0.7675 0.4095 0.127 Uiso 0.50 1 d PR . . C11A C 0.807(2) 0.821(2) 0.3902(9) 0.086(7) Uani 0.50 1 d PDU . . H11F H 0.7777 0.8809 0.3779 0.129 Uiso 0.50 1 d PR . . H11D H 0.7786 0.7853 0.4153 0.129 Uiso 0.50 1 d PR . . H10E H 0.8574 0.8445 0.4045 0.129 Uiso 0.50 1 d PR . . C12A C 0.7457(14) 0.693(2) 0.3282(13) 0.085(7) Uani 0.50 1 d PDU . . H12A H 0.7118 0.7449 0.3119 0.128 Uiso 0.50 1 d PR . . H12B H 0.7587 0.6394 0.3046 0.128 Uiso 0.50 1 d PR . . H11E H 0.7190 0.6619 0.3554 0.128 Uiso 0.50 1 d PR . . C12 C 0.809(2) 0.712(3) 0.2944(8) 0.086(7) Uani 0.50 1 d PDU . . H12 H 0.7799 0.7651 0.2759 0.129 Uiso 0.50 1 d PR . . H10H H 0.8603 0.7037 0.2804 0.129 Uiso 0.50 1 d PR . . H12C H 0.7815 0.6461 0.2926 0.129 Uiso 0.50 1 d PR . . C13 C 1.1565(15) 0.886(2) 0.3882(9) 0.083(8) Uani 1 1 d . . . C14 C 1.207(3) 0.880(3) 0.3433(14) 0.22(3) Uani 1 1 d . . . H14A H 1.2604 0.8583 0.3538 0.328 Uiso 1 1 calc R . . H14B H 1.2085 0.9500 0.3274 0.328 Uiso 1 1 calc R . . H14C H 1.1841 0.8286 0.3193 0.328 Uiso 1 1 calc R . . C15 C 1.2129(19) 0.950(2) 0.4235(13) 0.133(13) Uani 1 1 d . . . H15A H 1.2315 1.0122 0.4059 0.200 Uiso 1 1 calc R . . H15B H 1.2581 0.9053 0.4340 0.200 Uiso 1 1 calc R . . H15C H 1.1848 0.9718 0.4530 0.200 Uiso 1 1 calc R . . C16 C 1.078(2) 0.937(2) 0.3781(14) 0.157(16) Uani 1 1 d . . . H16A H 1.0415 0.8858 0.3627 0.236 Uiso 1 1 calc R . . H16B H 1.0845 0.9972 0.3553 0.236 Uiso 1 1 calc R . . H16C H 1.0578 0.9626 0.4096 0.236 Uiso 1 1 calc R . . C17 C 0.8036(13) 0.1713(14) 0.3712(7) 0.070(7) Uani 1 1 d D . . C18A C 0.8657(19) 0.088(3) 0.3817(14) 0.122(11) Uani 0.50 1 d PDU . . H18A H 0.8522 0.0254 0.3628 0.183 Uiso 0.50 1 d PR . . H18B H 0.9164 0.1133 0.3724 0.183 Uiso 0.50 1 d PR . . H18C H 0.8677 0.0715 0.4168 0.183 Uiso 0.50 1 d PR . . C18 C 0.8653(19) 0.140(3) 0.3338(13) 0.122(11) Uani 0.50 1 d PDU . . H18F H 0.8461 0.0806 0.3143 0.183 Uiso 0.50 1 d PR . . H18G H 0.8750 0.1983 0.3120 0.183 Uiso 0.50 1 d PR . . H18D H 0.9135 0.1204 0.3516 0.183 Uiso 0.50 1 d PR . . C19 C 0.789(2) 0.077(2) 0.4060(11) 0.122(11) Uani 0.50 1 d PDU . . H19A H 0.7711 0.0175 0.3865 0.182 Uiso 0.50 1 d PR . . H18E H 0.8368 0.0596 0.4245 0.182 Uiso 0.50 1 d PR . . H19B H 0.7491 0.0968 0.4288 0.182 Uiso 0.50 1 d PR . . C19A C 0.7236(17) 0.139(3) 0.3884(13) 0.123(11) Uani 0.50 1 d PDU . . H19D H 0.7031 0.0793 0.3695 0.184 Uiso 0.50 1 d PR . . H19C H 0.7285 0.1198 0.4232 0.184 Uiso 0.50 1 d PR . . H19E H 0.6884 0.1976 0.3842 0.184 Uiso 0.50 1 d PR . . C20 C 0.7273(18) 0.205(3) 0.3437(13) 0.122(11) Uani 0.50 1 d PDU . . H20A H 0.7069 0.1480 0.3230 0.183 Uiso 0.50 1 d PR . . H19F H 0.6893 0.2229 0.3679 0.183 Uiso 0.50 1 d PR . . H20B H 0.7376 0.2651 0.3233 0.183 Uiso 0.50 1 d PR . . C20A C 0.801(2) 0.208(3) 0.3175(9) 0.123(11) Uani 0.50 1 d PDU . . H20D H 0.7830 0.1501 0.2962 0.184 Uiso 0.50 1 d PR . . H20C H 0.7644 0.2658 0.3135 0.184 Uiso 0.50 1 d PR . . H18H H 0.8522 0.2297 0.3084 0.184 Uiso 0.50 1 d PR . . C21 C 1.0000 0.5000 0.5000 0.059(5) Uani 1 2 d SDU . . C22 C 0.5727(15) 0.209(2) 0.5940(10) 0.087(8) Uani 1 1 d . . . H22 H 0.5878 0.1703 0.5655 0.105 Uiso 1 1 calc R . . C23 C 0.4787(16) 0.250(3) 0.6558(11) 0.109(10) Uani 1 1 d . . . H23A H 0.4364 0.2986 0.6443 0.163 Uiso 1 1 calc R . . H23B H 0.5239 0.2918 0.6690 0.163 Uiso 1 1 calc R . . H23C H 0.4596 0.2046 0.6823 0.163 Uiso 1 1 calc R . . C24 C 0.4480(17) 0.109(2) 0.5915(13) 0.127(12) Uani 1 1 d . . . H24A H 0.4740 0.0707 0.5649 0.191 Uiso 1 1 calc R . . H24B H 0.4012 0.1453 0.5774 0.191 Uiso 1 1 calc R . . H24C H 0.4322 0.0582 0.6171 0.191 Uiso 1 1 calc R . . C25 C 0.6360(17) 0.466(2) 0.3144(12) 0.096(9) Uani 1 1 d . . . H25 H 0.6673 0.4640 0.2858 0.115 Uiso 1 1 calc R . . C26 C 0.5080(17) 0.448(3) 0.3446(11) 0.113(10) Uani 1 1 d . . . H26A H 0.5274 0.4869 0.3743 0.170 Uiso 1 1 calc R . . H26B H 0.5048 0.3723 0.3525 0.170 Uiso 1 1 calc R . . H26C H 0.4554 0.4742 0.3341 0.170 Uiso 1 1 calc R . . C27 C 0.5216(16) 0.463(2) 0.2580(9) 0.096(9) Uani 1 1 d . . . H27A H 0.5207 0.3904 0.2446 0.144 Uiso 1 1 calc R . . H27B H 0.5504 0.5090 0.2357 0.144 Uiso 1 1 calc R . . H27C H 0.4674 0.4885 0.2604 0.144 Uiso 1 1 calc R . . C28 C 1.079(2) 0.664(3) 0.2308(13) 0.127(12) Uani 1 1 d . . . H28 H 1.1349 0.6691 0.2337 0.152 Uiso 1 1 calc R . . C29 C 1.097(2) 0.628(4) 0.1440(13) 0.19(2) Uani 1 1 d . . . H29A H 1.1526 0.6387 0.1547 0.278 Uiso 1 1 calc R . . H29B H 1.0834 0.6741 0.1157 0.278 Uiso 1 1 calc R . . H29C H 1.0894 0.5536 0.1339 0.278 Uiso 1 1 calc R . . C30 C 0.968(2) 0.663(3) 0.1746(13) 0.153(16) Uani 1 1 d . . . H30A H 0.9480 0.7163 0.1972 0.230 Uiso 1 1 calc R . . H30B H 0.9420 0.5950 0.1802 0.230 Uiso 1 1 calc R . . H30C H 0.9584 0.6850 0.1398 0.230 Uiso 1 1 calc R . . N1 N 0.5905(11) 0.2305(16) 0.4686(7) 0.067(5) Uani 1 1 d . . . N2 N 0.8472(11) 0.4459(15) 0.2395(7) 0.061(5) Uani 1 1 d . . . N3 N 1.2951(10) 0.5722(17) 0.3043(8) 0.072(6) Uani 1 1 d . . . N4 N 0.5595(10) 0.4628(15) 0.3059(6) 0.059(5) Uani 1 1 d . . . N5 N 1.0485(13) 0.6510(18) 0.1840(9) 0.093(7) Uani 1 1 d . . . N6 N 0.5028(12) 0.1861(19) 0.6143(8) 0.083(6) Uani 1 1 d . . . N7 N 0.9154(14) 0.7680(19) 0.5276(9) 0.198(15) Uani 1 1 d DU . . O1 O 0.6531(8) 0.2106(12) 0.4959(6) 0.069(4) Uani 1 1 d . . . O2 O 0.5936(8) 0.3065(14) 0.4386(6) 0.078(5) Uani 1 1 d . . . O3 O 0.5314(9) 0.1784(16) 0.4717(8) 0.106(7) Uani 1 1 d . . . O4 O 0.7973(13) 0.4423(18) 0.2702(7) 0.119(7) Uani 1 1 d . . . O5 O 0.9176(11) 0.4467(18) 0.2520(7) 0.118(8) Uani 1 1 d . . . O6 O 0.8266(11) 0.4504(14) 0.1958(6) 0.098(6) Uani 1 1 d . . . O7 O 1.2395(8) 0.6289(15) 0.2914(6) 0.084(5) Uani 1 1 d . . . O8 O 1.3478(11) 0.5646(19) 0.2761(7) 0.118(8) Uani 1 1 d . . . O9 O 1.2951(8) 0.5245(15) 0.3449(6) 0.085(5) Uani 1 1 d . . . O10 O 0.6722(8) 0.4716(17) 0.3555(6) 0.093(6) Uani 1 1 d . . . O11 O 0.6178(10) 0.2790(17) 0.6111(7) 0.100(6) Uani 1 1 d . . . O12 O 1.0445(11) 0.6716(16) 0.2707(7) 0.097(6) Uani 1 1 d . . . O13 O 0.9496(13) 0.472(2) 0.4674(9) 0.066(5) Uani 0.50 1 d PDU . . O14 O 1.0083(18) 0.508(2) 0.4540(4) 0.066(5) Uani 0.50 1 d PDU . . O15 O 1.0638(10) 0.537(2) 0.4858(11) 0.069(5) Uani 0.50 1 d PDU . . O16 O 0.8437(13) 0.764(3) 0.5213(13) 0.245(17) Uani 1 1 d DU . . O17 O 0.944(2) 0.815(3) 0.5643(12) 0.29(2) Uani 1 1 d DU . . O18 O 0.9568(15) 0.711(3) 0.5035(12) 0.244(18) Uani 1 1 d DU . . 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 0.0465(9) 0.0611(10) 0.0545(9) 0.0025(8) -0.0022(7) 0.0049(8) Ag2 0.0422(8) 0.0516(10) 0.0891(13) 0.0064(9) -0.0022(8) 0.0020(7) Ag3 0.0486(9) 0.0743(12) 0.0756(12) -0.0167(10) 0.0164(8) 0.0003(8) Ag4 0.0399(8) 0.0662(11) 0.0657(10) 0.0050(8) 0.0036(7) 0.0044(7) Ag5 0.0600(10) 0.0884(14) 0.0613(11) -0.0041(10) 0.0100(8) -0.0214(9) Ag6 0.0406(8) 0.0834(12) 0.0596(10) 0.0037(9) -0.0002(7) -0.0099(8) Ag7 0.0429(9) 0.0850(13) 0.0708(11) 0.0278(10) 0.0022(8) 0.0001(8) Ag8 0.0530(10) 0.0885(14) 0.0734(12) 0.0124(10) 0.0045(8) -0.0097(9) Ag9 0.079(2) 0.126(4) 0.054(2) 0.009(3) -0.0100(16) 0.034(3) Ag9A 0.161(6) 0.059(4) 0.046(3) 0.006(3) -0.016(4) 0.018(3) Ag10 0.0714(12) 0.1124(17) 0.0777(13) -0.0259(12) -0.0310(10) 0.0217(11) S1 0.033(2) 0.068(4) 0.052(3) -0.011(3) -0.004(2) 0.002(2) S2 0.037(3) 0.069(4) 0.055(3) -0.006(3) 0.007(2) 0.011(2) S3 0.034(2) 0.044(3) 0.066(3) 0.010(2) -0.001(2) 0.009(2) S4 0.049(3) 0.075(4) 0.059(3) 0.007(3) -0.002(2) -0.006(3) S5 0.050(3) 0.049(3) 0.058(3) -0.006(3) 0.007(2) 0.001(2) C1 0.039(11) 0.086(16) 0.046(12) -0.018(11) -0.009(9) 0.007(11) C2 0.092(18) 0.11(2) 0.050(14) -0.005(14) 0.006(13) 0.012(16) C3 0.086(19) 0.11(2) 0.14(3) -0.06(2) -0.036(18) 0.037(17) C4 0.11(2) 0.10(2) 0.042(13) -0.021(13) 0.016(13) 0.009(17) C5 0.063(14) 0.085(16) 0.069(14) -0.031(13) -0.007(11) 0.014(12) C8 0.064(14) 0.12(2) 0.060(14) 0.041(14) 0.000(11) 0.044(14) C9 0.050(11) 0.041(11) 0.050(12) 0.015(9) -0.007(9) 0.010(9) C10 0.077(14) 0.049(13) 0.13(2) 0.031(13) 0.010(14) 0.036(11) C10A 0.077(14) 0.049(13) 0.13(2) 0.031(13) 0.010(14) 0.035(11) C11 0.075(14) 0.049(13) 0.131(19) 0.031(12) 0.011(14) 0.038(11) C11A 0.077(14) 0.050(13) 0.131(19) 0.030(13) 0.010(14) 0.038(11) C12A 0.076(14) 0.049(13) 0.13(2) 0.031(13) 0.009(14) 0.036(11) C12 0.077(14) 0.049(13) 0.13(2) 0.030(13) 0.009(14) 0.035(11) C13 0.073(16) 0.10(2) 0.078(17) 0.027(15) -0.012(14) 0.005(15) C14 0.44(8) 0.08(3) 0.14(3) 0.03(2) 0.16(4) -0.01(4) C15 0.14(3) 0.08(2) 0.18(3) 0.05(2) -0.04(3) -0.03(2) C16 0.22(4) 0.08(2) 0.17(4) 0.04(2) -0.07(3) 0.04(2) C17 0.103(19) 0.026(11) 0.084(17) -0.009(11) 0.030(14) -0.009(11) C18A 0.22(3) 0.057(16) 0.092(18) -0.034(14) 0.08(2) -0.051(17) C18 0.22(3) 0.058(16) 0.092(17) -0.034(14) 0.08(2) -0.050(17) C19 0.22(3) 0.057(16) 0.092(18) -0.034(14) 0.08(2) -0.052(17) C19A 0.22(3) 0.059(16) 0.093(18) -0.035(14) 0.08(2) -0.052(17) C20 0.22(3) 0.058(16) 0.092(18) -0.034(14) 0.08(2) -0.052(17) C20A 0.22(3) 0.059(16) 0.092(18) -0.034(14) 0.08(2) -0.050(17) C21 0.060(12) 0.068(12) 0.049(10) -0.003(11) 0.001(9) 0.023(11) C22 0.060(16) 0.12(2) 0.076(18) 0.022(17) -0.001(14) -0.001(16) C23 0.09(2) 0.14(3) 0.10(2) 0.04(2) 0.017(17) -0.021(19) C24 0.10(2) 0.10(2) 0.19(4) 0.06(2) 0.03(2) -0.024(19) C25 0.09(2) 0.078(19) 0.13(3) -0.003(18) 0.046(19) 0.015(16) C26 0.09(2) 0.16(3) 0.09(2) 0.01(2) 0.002(17) -0.02(2) C27 0.10(2) 0.11(2) 0.074(18) -0.025(16) -0.001(15) 0.000(17) C28 0.16(3) 0.12(3) 0.09(2) 0.02(2) -0.04(2) -0.01(2) C29 0.18(4) 0.28(6) 0.10(3) -0.03(3) 0.06(3) -0.11(4) C30 0.16(4) 0.14(3) 0.15(3) 0.02(3) -0.08(3) -0.03(3) N1 0.047(12) 0.074(14) 0.080(14) 0.013(11) 0.013(10) -0.002(10) N2 0.050(11) 0.092(15) 0.042(11) -0.003(10) -0.002(9) -0.005(10) N3 0.030(10) 0.113(17) 0.072(14) 0.017(12) 0.007(9) 0.005(10) N4 0.043(10) 0.104(15) 0.032(9) -0.007(9) 0.005(7) 0.028(10) N5 0.081(15) 0.107(18) 0.088(16) 0.025(14) -0.035(14) -0.021(13) N6 0.069(14) 0.108(18) 0.072(14) 0.021(13) 0.014(11) -0.006(13) N7 0.18(3) 0.18(3) 0.22(3) -0.10(2) -0.15(3) 0.01(2) O1 0.034(8) 0.086(11) 0.088(11) 0.028(9) 0.009(7) -0.007(7) O2 0.057(9) 0.091(12) 0.086(12) 0.033(10) 0.009(8) 0.015(9) O3 0.038(9) 0.125(16) 0.155(18) 0.050(13) 0.000(10) -0.019(10) O4 0.128(17) 0.17(2) 0.062(12) -0.031(12) 0.003(11) -0.052(15) O5 0.071(12) 0.18(2) 0.103(14) -0.077(14) -0.012(10) 0.023(13) O6 0.126(15) 0.101(14) 0.062(11) 0.007(10) -0.040(10) -0.025(11) O7 0.034(8) 0.131(15) 0.089(12) 0.020(11) 0.007(8) 0.001(9) O8 0.072(12) 0.19(2) 0.094(14) 0.055(14) 0.031(11) 0.017(13) O9 0.052(9) 0.138(16) 0.064(10) 0.032(11) -0.004(8) 0.001(9) O10 0.032(8) 0.177(19) 0.069(11) 0.008(12) -0.012(8) 0.011(10) O11 0.063(11) 0.149(18) 0.088(13) 0.000(12) 0.007(9) -0.029(12) O12 0.121(15) 0.116(16) 0.055(11) 0.042(11) 0.006(10) 0.006(12) O13 0.065(12) 0.077(12) 0.054(10) -0.012(11) -0.001(9) 0.026(11) O14 0.071(12) 0.072(12) 0.053(10) -0.005(11) 0.001(9) 0.017(11) O15 0.072(12) 0.073(12) 0.062(11) -0.003(11) 0.001(10) 0.022(11) O16 0.20(3) 0.25(3) 0.27(4) -0.10(3) -0.10(3) 0.03(3) O17 0.36(5) 0.21(4) 0.29(4) -0.01(3) -0.14(4) -0.02(3) O18 0.21(3) 0.31(4) 0.22(3) -0.14(3) -0.02(3) 0.03(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 O5 2.338(17) . ? Ag1 S3 2.487(5) . ? Ag1 S1 2.502(5) . ? Ag1 O12 2.548(18) . ? Ag1 Ag2 3.047(2) . ? Ag1 Ag4 3.057(2) . ? Ag1 Ag6 3.060(2) . ? Ag1 Ag5 3.079(2) . ? Ag2 O10 2.426(14) . ? Ag2 O4 2.452(17) . ? Ag2 S5 2.516(5) . ? Ag2 S3 2.531(5) . ? Ag2 Ag7 2.995(3) . ? Ag2 Ag4 3.018(2) . ? Ag2 Ag3 3.088(2) . ? Ag3 O2 2.371(16) . ? Ag3 S5 2.478(5) . ? Ag3 S2 2.487(5) . ? Ag3 Ag9 2.991(4) 3_766 ? Ag3 Ag7 3.136(3) . ? Ag3 Ag8 3.266(3) . ? Ag4 S5 2.434(5) . ? Ag4 S1 2.440(5) . ? Ag4 O13 2.46(2) . ? Ag4 O14 2.56(3) . ? Ag5 O7 2.346(14) . ? Ag5 S4 2.541(6) . ? Ag5 S1 2.584(6) . ? Ag5 Ag10 2.957(3) . ? Ag5 Ag6 2.958(2) . ? Ag5 Ag8 3.102(2) 3_766 ? Ag6 S3 2.432(5) . ? Ag6 S4 2.435(5) . ? Ag6 O14 2.52(3) . ? Ag6 Ag9A 3.209(7) . ? Ag6 Ag9 3.224(5) . ? Ag7 S3 2.434(5) . ? Ag7 S2 2.436(5) . ? Ag7 O13 2.49(2) . ? Ag7 Ag10 3.179(3) 3_766 ? Ag8 O11 2.287(17) . ? Ag8 S4 2.517(6) 3_766 ? Ag8 S2 2.563(6) . ? Ag8 Ag5 3.102(2) 3_766 ? Ag8 Ag10 3.289(3) 3_766 ? Ag9 Ag9A 0.783(6) . ? Ag9 S5 2.334(7) 3_766 ? Ag9 S4 2.400(7) . ? Ag9 Ag3 2.991(4) 3_766 ? Ag9A S4 2.534(9) . ? Ag9A S5 2.601(8) 3_766 ? Ag10 S2 2.388(5) 3_766 ? Ag10 S1 2.389(5) . ? Ag10 Ag7 3.179(3) 3_766 ? Ag10 Ag8 3.289(3) 3_766 ? S1 C1 1.86(2) . ? S2 C5 1.88(2) . ? S2 Ag10 2.388(5) 3_766 ? S3 C9 1.900(14) . ? S4 C13 1.87(3) . ? S4 Ag8 2.517(6) 3_766 ? S5 C17 1.866(18) . ? S5 Ag9 2.334(7) 3_766 ? S5 Ag9A 2.601(8) 3_766 ? C1 C3 1.48(3) . ? C1 C2 1.52(3) . ? C1 C4 1.55(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.48(3) . ? C5 C7 1.496(10) . ? C5 C6 1.497(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.496(9) . ? C9 C10 1.501(9) . ? C9 C11 1.508(9) . ? C9 C12A 1.511(9) . ? C9 C10A 1.511(9) . ? C10 C10A 1.427(15) . ? C10 C11A 1.485(14) . ? C10 H10A 0.9600 . ? C10 H10B 0.9599 . ? C10 H10C 0.9599 . ? C10A C12 1.452(14) . ? C10A H10F 0.9601 . ? C10A H10D 0.9600 . ? C10A H10G 0.9600 . ? C11 C11A 1.416(14) . ? C11 C12A 1.454(14) . ? C11 H11A 0.9602 . ? C11 H11B 0.9598 . ? C11 H11C 0.9599 . ? C11A H11F 0.9600 . ? C11A H11D 0.9601 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H11E 0.9599 . ? C12 H12 0.9599 . ? C12 H10H 0.9601 . ? C12 H12C 0.9600 . ? C13 C16 1.49(4) . ? C13 C14 1.50(4) . ? C13 C15 1.54(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18A 1.506(15) . ? C17 C20A 1.506(15) . ? C17 C19A 1.509(15) . ? C17 C20 1.520(15) . ? C17 C18 1.530(15) . ? C17 C19 1.533(15) . ? C18A C18 1.439(15) . ? C18A C19 1.486(15) . ? C18A H18A 0.9601 . ? C18A H18B 0.9600 . ? C18A H18C 0.9602 . ? C18 C20A 1.445(15) . ? C18 H18F 0.9600 . ? C18 H18G 0.9597 . ? C18 H18D 0.9602 . ? C19 C19A 1.411(15) . ? C19 H19A 0.9601 . ? C19 H18E 0.9601 . ? C19 H19B 0.9600 . ? C19A C20 1.461(15) . ? C19A H19D 0.9601 . ? C19A H19C 0.9599 . ? C20 C20A 1.454(15) . ? C20 H20A 0.9600 . ? C20 H19F 0.9601 . ? C20A H20D 0.9600 . ? C20A H20C 0.9600 . ? C20A H18H 0.9598 . ? C21 O13 1.243(10) . ? C21 O13 1.243(10) 3_766 ? C21 O14 1.247(10) . ? C21 O14 1.247(10) 3_766 ? C21 O15 1.251(10) . ? C21 O15 1.251(10) 3_766 ? C22 O11 1.24(3) . ? C22 N6 1.36(3) . ? C22 H22 0.9500 . ? C23 N6 1.45(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N6 1.46(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O10 1.24(3) . ? C25 N4 1.31(3) . ? C25 H25 0.9500 . ? C26 N4 1.39(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N4 1.41(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O12 1.24(4) . ? C28 N5 1.34(3) . ? C28 H28 0.9500 . ? C29 N5 1.41(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.38(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N1 O3 1.20(2) . ? N1 O2 1.25(2) . ? N1 O1 1.29(2) . ? N2 O4 1.21(2) . ? N2 O6 1.21(2) . ? N2 O5 1.23(2) . ? N3 O8 1.20(2) . ? N3 O7 1.22(2) . ? N3 O9 1.24(2) . ? N7 O18 1.215(9) . ? N7 O16 1.220(9) . ? N7 O17 1.227(9) . ? O13 O14 1.16(3) . ? O13 O15 1.29(3) 3_766 ? O14 O15 1.29(3) . ? O15 O13 1.29(3) 3_766 ? 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 O5 Ag1 S3 120.8(4) . . ? O5 Ag1 S1 101.2(5) . . ? S3 Ag1 S1 124.86(17) . . ? O5 Ag1 O12 94.3(7) . . ? S3 Ag1 O12 110.4(5) . . ? S1 Ag1 O12 99.2(4) . . ? O5 Ag1 Ag2 79.1(5) . . ? S3 Ag1 Ag2 53.29(12) . . ? S1 Ag1 Ag2 109.69(14) . . ? O12 Ag1 Ag2 151.1(4) . . ? O5 Ag1 Ag4 97.2(6) . . ? S3 Ag1 Ag4 87.47(12) . . ? S1 Ag1 Ag4 50.89(13) . . ? O12 Ag1 Ag4 149.6(4) . . ? Ag2 Ag1 Ag4 59.26(5) . . ? O5 Ag1 Ag6 170.0(5) . . ? S3 Ag1 Ag6 50.72(12) . . ? S1 Ag1 Ag6 88.67(12) . . ? O12 Ag1 Ag6 85.3(5) . . ? Ag2 Ag1 Ag6 96.44(6) . . ? Ag4 Ag1 Ag6 88.01(6) . . ? O5 Ag1 Ag5 129.8(5) . . ? S3 Ag1 Ag5 108.09(13) . . ? S1 Ag1 Ag5 53.96(13) . . ? O12 Ag1 Ag5 56.1(4) . . ? Ag2 Ag1 Ag5 146.14(7) . . ? Ag4 Ag1 Ag5 95.58(6) . . ? Ag6 Ag1 Ag5 57.61(5) . . ? O10 Ag2 O4 82.0(7) . . ? O10 Ag2 S5 103.7(5) . . ? O4 Ag2 S5 117.9(6) . . ? O10 Ag2 S3 111.0(5) . . ? O4 Ag2 S3 105.8(5) . . ? S5 Ag2 S3 126.97(17) . . ? O10 Ag2 Ag7 92.2(4) . . ? O4 Ag2 Ag7 152.6(6) . . ? S5 Ag2 Ag7 89.54(13) . . ? S3 Ag2 Ag7 51.44(12) . . ? O10 Ag2 Ag4 154.9(5) . . ? O4 Ag2 Ag4 109.9(6) . . ? S5 Ag2 Ag4 51.20(12) . . ? S3 Ag2 Ag4 87.54(11) . . ? Ag7 Ag2 Ag4 86.43(6) . . ? O10 Ag2 Ag1 144.4(5) . . ? O4 Ag2 Ag1 75.3(5) . . ? S5 Ag2 Ag1 111.04(13) . . ? S3 Ag2 Ag1 51.96(12) . . ? Ag7 Ag2 Ag1 95.48(6) . . ? Ag4 Ag2 Ag1 60.55(5) . . ? O10 Ag2 Ag3 63.7(4) . . ? O4 Ag2 Ag3 134.8(5) . . ? S5 Ag2 Ag3 51.25(12) . . ? S3 Ag2 Ag3 113.25(14) . . ? Ag7 Ag2 Ag3 62.05(6) . . ? Ag4 Ag2 Ag3 93.94(6) . . ? Ag1 Ag2 Ag3 148.21(7) . . ? O2 Ag3 S5 122.2(4) . . ? O2 Ag3 S2 111.2(4) . . ? S5 Ag3 S2 126.18(17) . . ? O2 Ag3 Ag9 131.1(4) . 3_766 ? S5 Ag3 Ag9 49.43(15) . 3_766 ? S2 Ag3 Ag9 90.76(16) . 3_766 ? O2 Ag3 Ag2 120.1(4) . . ? S5 Ag3 Ag2 52.36(13) . . ? S2 Ag3 Ag2 106.49(14) . . ? Ag9 Ag3 Ag2 92.01(11) 3_766 . ? O2 Ag3 Ag7 142.7(4) . . ? S5 Ag3 Ag7 87.06(13) . . ? S2 Ag3 Ag7 49.71(13) . . ? Ag9 Ag3 Ag7 84.82(12) 3_766 . ? Ag2 Ag3 Ag7 57.51(5) . . ? O2 Ag3 Ag8 94.0(4) . . ? S5 Ag3 Ag8 115.45(14) . . ? S2 Ag3 Ag8 50.74(13) . . ? Ag9 Ag3 Ag8 66.24(10) 3_766 . ? Ag2 Ag3 Ag8 145.50(7) . . ? Ag7 Ag3 Ag8 92.64(6) . . ? S5 Ag4 S1 159.11(18) . . ? S5 Ag4 O13 86.3(6) . . ? S1 Ag4 O13 108.0(7) . . ? S5 Ag4 O14 112.6(6) . . ? S1 Ag4 O14 81.6(5) . . ? O13 Ag4 O14 26.6(7) . . ? S5 Ag4 Ag2 53.69(13) . . ? S1 Ag4 Ag2 112.42(13) . . ? O13 Ag4 Ag2 80.5(4) . . ? O14 Ag4 Ag2 93.6(7) . . ? S5 Ag4 Ag1 113.14(14) . . ? S1 Ag4 Ag1 52.71(12) . . ? O13 Ag4 Ag1 92.3(7) . . ? O14 Ag4 Ag1 78.8(4) . . ? Ag2 Ag4 Ag1 60.20(5) . . ? O7 Ag5 S4 112.5(5) . . ? O7 Ag5 S1 113.4(5) . . ? S4 Ag5 S1 129.71(18) . . ? O7 Ag5 Ag10 115.3(4) . . ? S4 Ag5 Ag10 91.48(14) . . ? S1 Ag5 Ag10 50.52(12) . . ? O7 Ag5 Ag6 155.1(5) . . ? S4 Ag5 Ag6 51.89(13) . . ? S1 Ag5 Ag6 89.42(12) . . ? Ag10 Ag5 Ag6 86.55(7) . . ? O7 Ag5 Ag1 125.4(4) . . ? S4 Ag5 Ag1 112.10(14) . . ? S1 Ag5 Ag1 51.55(11) . . ? Ag10 Ag5 Ag1 93.15(7) . . ? Ag6 Ag5 Ag1 60.88(5) . . ? O7 Ag5 Ag8 83.5(4) . 3_766 ? S4 Ag5 Ag8 51.83(13) . 3_766 ? S1 Ag5 Ag8 115.52(13) . 3_766 ? Ag10 Ag5 Ag8 65.70(6) . 3_766 ? Ag6 Ag5 Ag8 95.90(7) . 3_766 ? Ag1 Ag5 Ag8 150.46(7) . 3_766 ? S3 Ag6 S4 162.45(19) . . ? S3 Ag6 O14 83.8(7) . . ? S4 Ag6 O14 108.1(7) . . ? S3 Ag6 Ag5 113.60(14) . . ? S4 Ag6 Ag5 55.19(15) . . ? O14 Ag6 Ag5 90.0(5) . . ? S3 Ag6 Ag1 52.34(13) . . ? S4 Ag6 Ag1 115.99(15) . . ? O14 Ag6 Ag1 79.3(5) . . ? Ag5 Ag6 Ag1 61.52(5) . . ? S3 Ag6 Ag9A 143.8(2) . . ? S4 Ag6 Ag9A 51.1(2) . . ? O14 Ag6 Ag9A 90.9(6) . . ? Ag5 Ag6 Ag9A 102.15(17) . . ? Ag1 Ag6 Ag9A 160.62(15) . . ? S3 Ag6 Ag9 149.49(16) . . ? S4 Ag6 Ag9 47.72(16) . . ? O14 Ag6 Ag9 80.7(6) . . ? Ag5 Ag6 Ag9 92.58(9) . . ? Ag1 Ag6 Ag9 147.00(10) . . ? Ag9A Ag6 Ag9 13.98(10) . . ? S3 Ag7 S2 160.03(18) . . ? S3 Ag7 O13 84.2(7) . . ? S2 Ag7 O13 108.0(8) . . ? S3 Ag7 Ag2 54.41(13) . . ? S2 Ag7 Ag2 110.82(14) . . ? O13 Ag7 Ag2 80.6(4) . . ? S3 Ag7 Ag3 114.60(14) . . ? S2 Ag7 Ag3 51.16(13) . . ? O13 Ag7 Ag3 90.9(6) . . ? Ag2 Ag7 Ag3 60.44(6) . . ? S3 Ag7 Ag10 151.68(14) . 3_766 ? S2 Ag7 Ag10 48.14(13) . 3_766 ? O13 Ag7 Ag10 81.5(6) . 3_766 ? Ag2 Ag7 Ag10 144.88(8) . 3_766 ? Ag3 Ag7 Ag10 90.01(7) . 3_766 ? O11 Ag8 S4 118.6(5) . 3_766 ? O11 Ag8 S2 128.2(5) . . ? S4 Ag8 S2 113.21(17) 3_766 . ? O11 Ag8 Ag5 110.1(5) . 3_766 ? S4 Ag8 Ag5 52.52(14) 3_766 3_766 ? S2 Ag8 Ag5 101.12(13) . 3_766 ? O11 Ag8 Ag3 120.9(5) . . ? S4 Ag8 Ag3 97.42(14) 3_766 . ? S2 Ag8 Ag3 48.70(12) . . ? Ag5 Ag8 Ag3 128.97(7) 3_766 . ? O11 Ag8 Ag10 138.5(5) . 3_766 ? S4 Ag8 Ag10 84.58(14) 3_766 3_766 ? S2 Ag8 Ag10 46.13(12) . 3_766 ? Ag5 Ag8 Ag10 55.03(6) 3_766 3_766 ? Ag3 Ag8 Ag10 85.88(6) . 3_766 ? Ag9A Ag9 S5 101.1(8) . 3_766 ? Ag9A Ag9 S4 90.7(8) . . ? S5 Ag9 S4 160.3(3) 3_766 . ? Ag9A Ag9 Ag3 142.8(9) . 3_766 ? S5 Ag9 Ag3 53.77(15) 3_766 3_766 ? S4 Ag9 Ag3 107.9(2) . 3_766 ? Ag9A Ag9 Ag6 82.0(8) . . ? S5 Ag9 Ag6 148.2(3) 3_766 . ? S4 Ag9 Ag6 48.65(15) . . ? Ag3 Ag9 Ag6 134.50(18) 3_766 . ? Ag9 Ag9A S4 71.3(8) . . ? Ag9 Ag9A S5 61.7(7) . 3_766 ? S4 Ag9A S5 130.6(3) . 3_766 ? Ag9 Ag9A Ag6 84.1(8) . . ? S4 Ag9A Ag6 48.44(17) . . ? S5 Ag9A Ag6 133.8(3) 3_766 . ? S2 Ag10 S1 164.9(2) 3_766 . ? S2 Ag10 Ag5 109.90(16) 3_766 . ? S1 Ag10 Ag5 56.60(14) . . ? S2 Ag10 Ag7 49.43(13) 3_766 3_766 ? S1 Ag10 Ag7 144.58(15) . 3_766 ? Ag5 Ag10 Ag7 136.80(9) . 3_766 ? S2 Ag10 Ag8 50.69(14) 3_766 3_766 ? S1 Ag10 Ag8 115.15(16) . 3_766 ? Ag5 Ag10 Ag8 59.26(6) . 3_766 ? Ag7 Ag10 Ag8 91.43(6) 3_766 3_766 ? C1 S1 Ag10 114.1(6) . . ? C1 S1 Ag4 112.7(7) . . ? Ag10 S1 Ag4 94.28(19) . . ? C1 S1 Ag1 117.2(6) . . ? Ag10 S1 Ag1 127.4(2) . . ? Ag4 S1 Ag1 76.40(14) . . ? C1 S1 Ag5 117.2(7) . . ? Ag10 S1 Ag5 72.87(15) . . ? Ag4 S1 Ag5 129.5(2) . . ? Ag1 S1 Ag5 74.49(16) . . ? C5 S2 Ag10 112.2(7) . 3_766 ? C5 S2 Ag7 110.2(8) . . ? Ag10 S2 Ag7 82.43(17) 3_766 . ? C5 S2 Ag3 115.1(7) . . ? Ag10 S2 Ag3 132.7(2) 3_766 . ? Ag7 S2 Ag3 79.14(16) . . ? C5 S2 Ag8 114.0(8) . . ? Ag10 S2 Ag8 83.17(17) 3_766 . ? Ag7 S2 Ag8 135.7(2) . . ? Ag3 S2 Ag8 80.56(17) . . ? C9 S3 Ag6 113.7(5) . . ? C9 S3 Ag7 112.4(5) . . ? Ag6 S3 Ag7 98.16(18) . . ? C9 S3 Ag1 114.4(6) . . ? Ag6 S3 Ag1 76.94(14) . . ? Ag7 S3 Ag1 130.6(2) . . ? C9 S3 Ag2 111.8(5) . . ? Ag6 S3 Ag2 133.1(2) . . ? Ag7 S3 Ag2 74.15(15) . . ? Ag1 S3 Ag2 74.75(15) . . ? C13 S4 Ag9 119.3(9) . . ? C13 S4 Ag6 113.8(8) . . ? Ag9 S4 Ag6 83.6(2) . . ? C13 S4 Ag8 112.5(8) . 3_766 ? Ag9 S4 Ag8 88.3(2) . 3_766 ? Ag6 S4 Ag8 130.7(3) . 3_766 ? C13 S4 Ag9A 104.2(9) . . ? Ag6 S4 Ag9A 80.4(3) . . ? Ag8 S4 Ag9A 103.9(3) 3_766 . ? C13 S4 Ag5 110.8(9) . . ? Ag9 S4 Ag5 129.7(3) . . ? Ag6 S4 Ag5 72.92(16) . . ? Ag8 S4 Ag5 75.65(18) 3_766 . ? Ag9A S4 Ag5 142.2(3) . . ? C17 S5 Ag9 120.5(7) . 3_766 ? C17 S5 Ag4 116.6(6) . . ? Ag9 S5 Ag4 91.0(2) 3_766 . ? C17 S5 Ag3 110.5(7) . . ? Ag9 S5 Ag3 76.80(18) 3_766 . ? Ag4 S5 Ag3 130.7(2) . . ? C17 S5 Ag2 109.6(7) . . ? Ag9 S5 Ag2 128.8(3) 3_766 . ? Ag4 S5 Ag2 75.10(15) . . ? Ag3 S5 Ag2 76.38(15) . . ? C17 S5 Ag9A 107.4(7) . 3_766 ? Ag4 S5 Ag9A 87.7(3) . 3_766 ? Ag3 S5 Ag9A 91.7(2) . 3_766 ? Ag2 S5 Ag9A 143.0(3) . 3_766 ? C3 C1 C2 111(2) . . ? C3 C1 C4 111(2) . . ? C2 C1 C4 108.3(17) . . ? C3 C1 S1 110.6(15) . . ? C2 C1 S1 108.0(16) . . ? C4 C1 S1 108.6(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 116(2) . . ? C8 C5 C6 112(3) . . ? C7 C5 C6 106(3) . . ? C8 C5 S2 107.4(14) . . ? C7 C5 S2 104(2) . . ? C6 C5 S2 111(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? O13 C21 O13 180 . 3_766 ? O13 C21 O14 55.5(17) . . ? O13 C21 O14 124.5(17) 3_766 . ? O13 C21 O14 124.5(17) . 3_766 ? O13 C21 O14 55.5(17) 3_766 3_766 ? O14 C21 O14 180 . 3_766 ? O13 C21 O15 117.9(17) . . ? O13 C21 O15 62.1(17) 3_766 . ? O14 C21 O15 62.4(17) . . ? O14 C21 O15 117.6(17) 3_766 . ? O13 C21 O15 62.1(17) . 3_766 ? O13 C21 O15 117.9(17) 3_766 3_766 ? O14 C21 O15 117.6(17) . 3_766 ? O14 C21 O15 62.4(17) 3_766 3_766 ? O15 C21 O15 180 . 3_766 ? O11 C22 N6 123(3) . . ? O11 C22 H22 118.7 . . ? N6 C22 H22 118.7 . . ? N6 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O10 C25 N4 127(2) . . ? O10 C25 H25 116.3 . . ? N4 C25 H25 116.3 . . ? N4 C26 H26A 109.5 . . ? N4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O12 C28 N5 129(4) . . ? O12 C28 H28 115.4 . . ? N5 C28 H28 115.4 . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 N1 O2 121(2) . . ? O3 N1 O1 122(2) . . ? O2 N1 O1 117.1(17) . . ? O4 N2 O6 119(2) . . ? O4 N2 O5 121(2) . . ? O6 N2 O5 120(2) . . ? O8 N3 O7 117(2) . . ? O8 N3 O9 123(2) . . ? O7 N3 O9 120.2(18) . . ? C25 N4 C26 122(2) . . ? C25 N4 C27 125(2) . . ? C26 N4 C27 113(2) . . ? C28 N5 C30 120(3) . . ? C28 N5 C29 121(3) . . ? C30 N5 C29 119(3) . . ? C22 N6 C23 118(2) . . ? C22 N6 C24 122(3) . . ? C23 N6 C24 120(2) . . ? N1 O2 Ag3 103.5(12) . . ? N2 O4 Ag2 128.1(15) . . ? N2 O5 Ag1 123.0(14) . . ? N3 O7 Ag5 109.2(14) . . ? C25 O10 Ag2 120.6(16) . . ? C22 O11 Ag8 125.7(18) . . ? C28 O12 Ag1 133(2) . . ? O14 O13 C21 62.4(10) . . ? O14 O13 O15 121.6(13) . 3_766 ? C21 O13 O15 59.2(10) . 3_766 ? O14 O13 Ag4 81.2(19) . . ? C21 O13 Ag4 127.1(16) . . ? O15 O13 Ag4 137(2) 3_766 . ? O14 O13 Ag7 120(3) . . ? C21 O13 Ag7 118.4(16) . . ? O15 O13 Ag7 88.2(18) 3_766 . ? Ag4 O13 Ag7 112.5(5) . . ? O13 O14 C21 62.1(10) . . ? O13 O14 O15 121.1(13) . . ? C21 O14 O15 59.0(10) . . ? O13 O14 Ag6 121(2) . . ? C21 O14 Ag6 121.7(17) . . ? O15 O14 Ag6 91(2) . . ? O13 O14 Ag4 72.2(19) . . ? C21 O14 Ag4 120.3(18) . . ? O15 O14 Ag4 141(2) . . ? Ag6 O14 Ag4 113.7(5) . . ? C21 O15 O13 58.7(10) . 3_766 ? C21 O15 O14 58.7(10) . . ? O13 O15 O14 117.3(12) 3_766 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.214 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.206 # start Validation Reply Form _vrf_PLAT234_p ; PROBLEM: Large Hirshfeld Difference O10 -- C25 .. 0.32 Ang. RESPONSE: We ensured the correct atom was assigned. Terminal coordinated DMF molecule shows increased atomic motions but no model could be found to refine this motif as disordered. ; _vrf_PLAT241_p ; PROBLEM: Check High Ueq as Compared to Neighbors for O4 RESPONSE: We ensured the correct atom was assigned. Terminal coordinated nitrate ion show increased atomic motions but no model could be found to refine this motif as disordered. ; _vrf_PLAT201_p ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 2 RESPONSE: Duo to rotation disorder of tert-butyl group. ; _vrf_PLAT213_p ; PROBLEM: Atom N7 has ADP max/min Ratio ..... 4.2 prola RESPONSE: Duo to disorder of nitrate ion. We have tried to resolve this disorder by assigning alternative positions with partial occupancies for it but some of the atoms continue to have high ADP max/min ratio. This is could be indicative of the dynamic nature of the disorder in this ion. ; _vrf_PLAT220_p ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.7 Ratio RESPONSE: Duo to rotation disorder of perpheral tert-butyl group. ; _vrf_PLAT242_p ; PROBLEM: Check Low Ueq as Compared to Neighbors for N2 RESPONSE: Duo to disorder of nitrate ion. We have tried to resolve this disorder by assigning alternative positions with partial occupancies for it but some of the atoms continue to have high ADP max/min ratio. This is could be indicative of the dynamic nature of the disorder in this ion. ; _vrf_PLAT342_p ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0367 Ang. RESPONSE: This alert is generated because there is many disordered motifs in the structure. ; # end Validation Reply Form