# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 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_Compound1 # start Validation Reply Form _vrf_PLAT232_2_G ; PROBLEM: Hirshfeld Test Diff (M-X) Ag1 -- S1 .. 31.5 su RESPONSE: The Hirshfeld value is considered as not relevant, on the basis that the refinement was not difficult, the structure was not disordered, wrong atom assignment was disregarded, data were not weak and no twinning or pseudo-symmetry was detected. The failure of the test may be related to the fact the bond involves an heavy atom and its ligand. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Ag N3 P S' _chemical_formula_sum 'C6 H12 Ag N3 P S' _chemical_formula_weight 297.09 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 '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 ORTHORHOMBIC _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.0290(2) _cell_length_b 9.8549(3) _cell_length_c 14.3776(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1137.63(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9163 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 35.39 _exptl_crystal_description octahedron _exptl_crystal_colour colourless _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6573 _exptl_absorpt_correction_T_max 0.7273 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21024 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 36.42 _reflns_number_total 5544 _reflns_number_gt 5077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983),2416 Friedel pairs' _refine_ls_abs_structure_Flack -0.002(17) _refine_ls_number_reflns 5544 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL wie117 in P 21 21 21 CELL 0.71069 8.0290 9.8549 14.3776 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N P S AG UNIT 24 48 12 4 4 4 MERG 2 OMIT 2 0 0 OMIT 1 0 1 OMIT 2 0 2 FMAP 2 PLAN 25 ACTA BOND $H LIST 4 L.S. 4 WGHT 0.025400 FVAR 1.72541 C11 1 0.218911 0.090454 -0.137011 11.00000 0.01580 0.01490 = 0.01541 0.00121 0.00024 0.00108 AFIX 23 H11A 2 0.146210 0.033942 -0.174468 11.00000 -1.20000 H11B 2 0.164803 0.177456 -0.127934 11.00000 -1.20000 AFIX 0 C12 1 0.383071 -0.134232 -0.058771 11.00000 0.01654 0.01239 = 0.01327 -0.00003 0.00238 0.00000 AFIX 23 H12A 2 0.425389 -0.179280 -0.003637 11.00000 -1.20000 H12B 2 0.315719 -0.198806 -0.093093 11.00000 -1.20000 AFIX 0 C13 1 0.413048 0.122402 0.024799 11.00000 0.02166 0.01536 = 0.01515 -0.00395 -0.00094 -0.00271 AFIX 23 H13A 2 0.364613 0.210372 0.038373 11.00000 -1.20000 H13B 2 0.455904 0.084416 0.082254 11.00000 -1.20000 AFIX 0 C14 1 0.465557 -0.019878 -0.203096 11.00000 0.01869 0.01715 = 0.01121 -0.00025 0.00163 0.00012 AFIX 23 H14A 2 0.560192 -0.003744 -0.243549 11.00000 -1.20000 H14B 2 0.389663 -0.079983 -0.235625 11.00000 -1.20000 AFIX 0 C15 1 0.631560 0.007355 -0.064355 11.00000 0.01352 0.02048 = 0.01870 0.00007 -0.00297 -0.00215 AFIX 23 H15A 2 0.664028 -0.035028 -0.006226 11.00000 -1.20000 H15B 2 0.732185 0.024858 -0.099712 11.00000 -1.20000 AFIX 0 C16 1 0.492596 0.198979 -0.130640 11.00000 0.02048 0.01571 = 0.01904 0.00287 -0.00158 -0.00558 AFIX 23 H16A 2 0.588890 0.221971 -0.168212 11.00000 -1.20000 H16B 2 0.434458 0.282654 -0.116214 11.00000 -1.20000 AFIX 0 N11 3 0.380472 0.110263 -0.185845 11.00000 0.01639 0.01437 = 0.01421 0.00131 0.00067 -0.00206 N12 3 0.524723 -0.088807 -0.117586 11.00000 0.01293 0.01606 = 0.01254 -0.00037 0.00079 0.00057 N13 3 0.549558 0.137095 -0.043952 11.00000 0.01766 0.01721 = 0.01701 -0.00110 -0.00203 -0.00425 P1 4 0.255348 0.009819 -0.024713 11.00000 0.01477 0.01170 = 0.01280 -0.00047 0.00215 -0.00062 S1 5 0.052570 -0.036132 0.045094 11.00000 0.01626 0.01966 = 0.01939 0.00054 0.00576 -0.00006 AG1 6 0.164377 -0.209321 0.163022 11.00000 0.01785 0.02458 = 0.01797 -0.00625 -0.00141 -0.00410 HKLF 4 REM wie117 in P 21 21 21 REM R1 = 0.0258 for 5078 Fo > 4sig(Fo) and 0.0294 for all 5544 data REM 109 parameters refined using 0 restraints END WGHT 0.0252 0.0000 REM Highest difference peak 0.534, deepest hole -0.574, 1-sigma level 0.091 Q1 1 0.3664 -0.1641 0.1764 11.00000 0.05 0.53 Q2 1 0.3735 -0.1344 0.1902 11.00000 0.05 0.53 Q3 1 0.0717 -0.2032 0.1846 11.00000 0.05 0.51 Q4 1 0.3357 -0.0387 -0.0163 11.00000 0.05 0.51 Q5 1 0.3752 -0.1202 0.1353 11.00000 0.05 0.48 Q6 1 0.0813 -0.1835 0.1610 11.00000 0.05 0.46 Q7 1 0.0825 -0.2360 0.1507 11.00000 0.05 0.45 Q8 1 0.1597 -0.2376 0.2022 11.00000 0.05 0.38 Q9 1 0.2235 -0.1592 0.1673 11.00000 0.05 0.38 Q10 1 0.2438 -0.2532 0.1623 11.00000 0.05 0.37 Q11 1 0.6086 0.1629 -0.2996 11.00000 0.05 0.35 Q12 1 0.3633 0.2742 0.0855 11.00000 0.05 0.35 Q13 1 0.3005 0.1219 -0.1591 11.00000 0.05 0.35 Q14 1 0.2964 -0.1469 0.2114 11.00000 0.05 0.34 Q15 1 0.1707 -0.0272 0.0015 11.00000 0.05 0.33 Q16 1 0.5621 0.0954 -0.2874 11.00000 0.05 0.33 Q17 1 0.4630 -0.1452 0.1644 11.00000 0.05 0.32 Q18 1 0.1662 -0.2208 0.1179 11.00000 0.05 0.32 Q19 1 0.6643 -0.1820 0.0153 11.00000 0.05 0.32 Q20 1 0.3271 -0.0590 -0.0597 11.00000 0.05 0.32 Q21 1 0.4090 -0.3440 0.0151 11.00000 0.05 0.31 Q22 1 0.4824 -0.1396 -0.0878 11.00000 0.05 0.31 Q23 1 0.3713 -0.1795 0.0897 11.00000 0.05 0.31 Q24 1 0.1659 0.2145 -0.0236 11.00000 0.05 0.30 Q25 1 -0.0233 -0.1406 0.1618 11.00000 0.05 0.30 ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.281 0.750 112 83 ' ' 2 0.500 0.383 0.250 112 83 ' ' _platon_squeeze_details ; ; 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 C11 C 0.2189(2) 0.09045(18) -0.13701(12) 0.0154(3) Uani 1 1 d . . . H11A H 0.1462 0.0339 -0.1745 0.018 Uiso 1 1 calc R . . H11B H 0.1648 0.1775 -0.1279 0.018 Uiso 1 1 calc R . . C12 C 0.3831(2) -0.13423(16) -0.05877(12) 0.0141(3) Uani 1 1 d . . . H12A H 0.4254 -0.1793 -0.0036 0.017 Uiso 1 1 calc R . . H12B H 0.3157 -0.1988 -0.0931 0.017 Uiso 1 1 calc R . . C13 C 0.4130(2) 0.12240(18) 0.02480(13) 0.0174(3) Uani 1 1 d . . . H13A H 0.3646 0.2104 0.0384 0.021 Uiso 1 1 calc R . . H13B H 0.4559 0.0844 0.0823 0.021 Uiso 1 1 calc R . . C14 C 0.4656(2) -0.01988(17) -0.20310(12) 0.0157(3) Uani 1 1 d . . . H14A H 0.5602 -0.0037 -0.2435 0.019 Uiso 1 1 calc R . . H14B H 0.3897 -0.0800 -0.2356 0.019 Uiso 1 1 calc R . . C15 C 0.6316(2) 0.00735(19) -0.06435(13) 0.0176(3) Uani 1 1 d . . . H15A H 0.6640 -0.0350 -0.0062 0.021 Uiso 1 1 calc R . . H15B H 0.7322 0.0249 -0.0997 0.021 Uiso 1 1 calc R . . C16 C 0.4926(2) 0.19898(19) -0.13064(12) 0.0184(3) Uani 1 1 d . . . H16A H 0.5889 0.2220 -0.1682 0.022 Uiso 1 1 calc R . . H16B H 0.4345 0.2827 -0.1162 0.022 Uiso 1 1 calc R . . N11 N 0.38047(18) 0.11026(15) -0.18585(10) 0.0150(3) Uani 1 1 d . . . N12 N 0.52472(18) -0.08881(14) -0.11759(10) 0.0138(2) Uani 1 1 d . . . N13 N 0.54956(19) 0.13710(15) -0.04395(11) 0.0173(3) Uani 1 1 d . . . P1 P 0.25535(6) 0.00982(4) -0.02471(3) 0.01309(8) Uani 1 1 d . . . S1 S 0.05257(6) -0.03613(5) 0.04509(3) 0.01844(8) Uani 1 1 d . . . Ag1 Ag 0.164377(17) -0.209321(15) 0.163022(10) 0.02013(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0158(7) 0.0149(7) 0.0154(7) 0.0012(5) 0.0002(5) 0.0011(6) C12 0.0165(6) 0.0124(6) 0.0133(7) 0.0000(5) 0.0024(5) 0.0000(5) C13 0.0217(8) 0.0154(7) 0.0151(7) -0.0040(6) -0.0009(6) -0.0027(6) C14 0.0187(7) 0.0171(7) 0.0112(7) -0.0003(6) 0.0016(5) 0.0001(6) C15 0.0135(7) 0.0205(7) 0.0187(8) 0.0001(6) -0.0030(5) -0.0021(6) C16 0.0205(7) 0.0157(7) 0.0190(7) 0.0029(6) -0.0016(6) -0.0056(7) N11 0.0164(6) 0.0144(6) 0.0142(6) 0.0013(5) 0.0007(5) -0.0021(5) N12 0.0129(6) 0.0161(6) 0.0125(6) -0.0004(5) 0.0008(5) 0.0006(5) N13 0.0177(6) 0.0172(6) 0.0170(7) -0.0011(5) -0.0020(5) -0.0043(5) P1 0.01477(17) 0.01170(16) 0.01280(19) -0.00047(14) 0.00215(14) -0.00062(14) S1 0.01626(18) 0.01966(19) 0.0194(2) 0.00054(16) 0.00576(15) -0.00006(15) Ag1 0.01785(5) 0.02458(6) 0.01797(6) -0.00625(5) -0.00141(5) -0.00410(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 C11 N11 1.488(2) . ? C11 P1 1.8232(18) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N12 1.486(2) . ? C12 P1 1.8184(17) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N13 1.483(2) . ? C13 P1 1.8278(18) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N11 1.474(2) . ? C14 N12 1.483(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N13 1.468(2) . ? C15 N12 1.490(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N13 1.461(2) . ? C16 N11 1.485(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? N11 Ag1 2.4092(15) 2_554 ? N12 Ag1 2.3753(14) 3_545 ? P1 S1 1.9655(6) . ? S1 Ag1 2.5678(5) . ? Ag1 N12 2.3753(14) 3_445 ? Ag1 N11 2.4092(15) 2 ? 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 N11 C11 P1 109.58(12) . . ? N11 C11 H11A 109.8 . . ? P1 C11 H11A 109.8 . . ? N11 C11 H11B 109.8 . . ? P1 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? N12 C12 P1 110.46(11) . . ? N12 C12 H12A 109.6 . . ? P1 C12 H12A 109.6 . . ? N12 C12 H12B 109.6 . . ? P1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N13 C13 P1 108.16(12) . . ? N13 C13 H13A 110.1 . . ? P1 C13 H13A 110.1 . . ? N13 C13 H13B 110.1 . . ? P1 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N11 C14 N12 114.05(14) . . ? N11 C14 H14A 108.7 . . ? N12 C14 H14A 108.7 . . ? N11 C14 H14B 108.7 . . ? N12 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N13 C15 N12 113.48(14) . . ? N13 C15 H15A 108.9 . . ? N12 C15 H15A 108.9 . . ? N13 C15 H15B 108.9 . . ? N12 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N13 C16 N11 113.58(14) . . ? N13 C16 H16A 108.8 . . ? N11 C16 H16A 108.8 . . ? N13 C16 H16B 108.8 . . ? N11 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C14 N11 C16 108.74(14) . . ? C14 N11 C11 111.67(13) . . ? C16 N11 C11 110.71(14) . . ? C14 N11 Ag1 105.67(10) . 2_554 ? C16 N11 Ag1 109.52(10) . 2_554 ? C11 N11 Ag1 110.39(10) . 2_554 ? C14 N12 C12 111.38(13) . . ? C14 N12 C15 108.60(13) . . ? C12 N12 C15 109.87(13) . . ? C14 N12 Ag1 107.87(10) . 3_545 ? C12 N12 Ag1 105.39(10) . 3_545 ? C15 N12 Ag1 113.72(10) . 3_545 ? C16 N13 C15 109.48(14) . . ? C16 N13 C13 112.21(15) . . ? C15 N13 C13 112.31(14) . . ? C12 P1 C11 101.09(8) . . ? C12 P1 C13 100.84(8) . . ? C11 P1 C13 101.04(8) . . ? C12 P1 S1 115.14(6) . . ? C11 P1 S1 114.82(6) . . ? C13 P1 S1 120.98(7) . . ? P1 S1 Ag1 101.58(2) . . ? N12 Ag1 N11 121.12(5) 3_445 2 ? N12 Ag1 S1 102.13(4) 3_445 . ? N11 Ag1 S1 105.90(4) 2 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 36.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.534 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 927875' ####################################################################### # # 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_Compound2 # start Validation Reply Form _vrf_PLAT232_2_B ; PROBLEM: Hirshfeld Test Diff (M-X) Ag1 -- S1 .. 52.0 su RESPONSE: The Hirshfeld value is considered as not relevant, on the basis that the refinement was not difficult, the structure was not disordered, wrong atom assignment was disregarded, data were not weak and no twinning or pseudo-symmetry was detected. The failure of the test may be related to the fact the bond involves an heavy atom and its ligand. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 Ag4 N6 O10 P2 S4, 2(H2 O)' _chemical_formula_sum 'C12 H32 Ag4 N6 O12 P2 S4' _chemical_formula_weight 1074.10 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 '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 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5475(3) _cell_length_b 11.4400(3) _cell_length_c 13.2092(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.9740(10) _cell_angle_gamma 90.00 _cell_volume 1355.97(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 44.79 _exptl_crystal_description octahedron _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 3.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_T_max 0.8312 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11641 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.33 _reflns_number_total 4740 _reflns_number_gt 4704 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0189P)^2^+0.8565P] 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_abs_structure_details 'Flack (1983), 2200 Friedel pairs' _refine_ls_abs_structure_Flack 0.352(14) _refine_ls_number_reflns 4740 _refine_ls_number_parameters 374 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0161 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL wie193a in P 21 CELL 0.71069 9.5475 11.4400 13.2092 90.000 109.974 90.000 ZERR 2.00 0.0003 0.0003 0.0004 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O P S AG UNIT 24 64 12 24 4 8 8 MERG 2 TWIN shel 8 0.83 DFIX 0.950 0.020 O2 H2A FMAP 2 PLAN 50 ACTA HTAB 2.00000 LIST 4 L.S. 16 TEMP -123.00 WGHT 0.018900 0.856500 BASF 0.35161 FVAR 0.11722 C11 1 0.855298 0.437004 0.215848 11.00000 0.01685 0.01057 = 0.01005 0.00030 0.00416 0.00015 AFIX 23 H11A 2 0.958388 0.449785 0.265599 11.00000 -1.20000 H11B 2 0.787502 0.437389 0.258237 11.00000 -1.20000 AFIX 0 C12 1 0.624219 0.499321 0.021017 11.00000 0.00996 0.01227 = 0.01382 0.00082 0.00479 0.00069 AFIX 23 H12A 2 0.547780 0.501036 0.056168 11.00000 -1.20000 H12B 2 0.590393 0.549920 -0.043627 11.00000 -1.20000 AFIX 0 C13 1 0.929740 0.522902 0.040264 11.00000 0.01176 0.01031 = 0.01513 -0.00034 0.00568 -0.00286 AFIX 23 H13A 2 0.905390 0.574667 -0.023487 11.00000 -1.20000 H13B 2 1.033712 0.538629 0.086984 11.00000 -1.20000 AFIX 0 C14 1 0.757600 0.372249 -0.065827 11.00000 0.01236 0.01294 = 0.01206 -0.00208 0.00529 -0.00214 AFIX 23 H14A 2 0.728908 0.429494 -0.125630 11.00000 -1.20000 H14B 2 0.754480 0.293511 -0.097623 11.00000 -1.20000 AFIX 0 C15 1 0.949294 0.318014 0.100096 11.00000 0.01297 0.01177 = 0.01857 0.00226 0.00534 0.00217 AFIX 23 H15A 2 0.951865 0.236648 0.075268 11.00000 -1.20000 H15B 2 1.050250 0.337275 0.150233 11.00000 -1.20000 AFIX 0 C16 1 0.694252 0.300003 0.085710 11.00000 0.01420 0.01197 = 0.01200 -0.00164 0.00209 -0.00120 AFIX 23 H16A 2 0.623665 0.309157 0.125335 11.00000 -1.20000 H16B 2 0.689121 0.217730 0.061466 11.00000 -1.20000 AFIX 0 C21 1 0.912755 0.545966 0.522948 11.00000 0.01198 0.01115 = 0.01145 0.00229 0.00468 0.00204 AFIX 23 H21A 2 1.020165 0.529650 0.559140 11.00000 -1.20000 H21B 2 0.874680 0.493945 0.459525 11.00000 -1.20000 AFIX 0 C22 1 0.624103 0.570693 0.536686 11.00000 0.01116 0.01033 = 0.01718 0.00201 0.00507 0.00151 AFIX 23 H22A 2 0.579364 0.518930 0.473835 11.00000 -1.20000 H22B 2 0.559499 0.569747 0.581484 11.00000 -1.20000 AFIX 0 C23 1 0.879918 0.636482 0.712098 11.00000 0.01663 0.01309 = 0.01231 -0.00038 0.00493 0.00071 AFIX 23 H23A 2 0.824494 0.637432 0.763213 11.00000 -1.20000 H23B 2 0.986874 0.624319 0.753581 11.00000 -1.20000 AFIX 0 C24 1 0.730102 0.695952 0.430477 11.00000 0.01238 0.01264 = 0.01012 0.00157 0.00082 0.00054 AFIX 23 H24A 2 0.720967 0.774302 0.397009 11.00000 -1.20000 H24B 2 0.690879 0.638158 0.371784 11.00000 -1.20000 AFIX 0 C25 1 0.945964 0.752722 0.581262 11.00000 0.01314 0.01084 = 0.01828 0.00080 0.00413 -0.00266 AFIX 23 H25A 2 1.051020 0.733414 0.622836 11.00000 -1.20000 H25B 2 0.943508 0.833408 0.553613 11.00000 -1.20000 AFIX 0 C26 1 0.703271 0.772378 0.593518 11.00000 0.01591 0.01235 = 0.01444 -0.00227 0.00491 0.00179 AFIX 23 H26A 2 0.693720 0.854012 0.567149 11.00000 -1.20000 H26B 2 0.645540 0.765260 0.642834 11.00000 -1.20000 AFIX 0 N11 3 0.844633 0.324117 0.158936 11.00000 0.01195 0.00903 = 0.01378 0.00001 0.00269 0.00053 N12 3 0.646724 0.377110 -0.010035 11.00000 0.01063 0.00983 = 0.01252 -0.00123 0.00469 -0.00176 N13 3 0.913240 0.397249 0.005480 11.00000 0.00908 0.01016 = 0.01626 -0.00057 0.00552 -0.00009 N21 3 0.890666 0.670967 0.488219 11.00000 0.01246 0.00953 = 0.01226 0.00077 0.00357 -0.00145 N22 3 0.637231 0.692512 0.499742 11.00000 0.01362 0.00982 = 0.01350 0.00136 0.00274 0.00149 N23 3 0.859095 0.748519 0.653413 11.00000 0.01354 0.01077 = 0.01556 -0.00279 0.00410 -0.00234 O1 4 1.157189 0.544603 0.399828 11.00000 0.01788 0.01754 = 0.02556 -0.00312 0.00604 -0.00047 O2 4 0.809425 1.030093 0.080296 11.00000 0.02667 0.01834 = 0.01864 0.00132 0.00751 0.00589 O10 4 0.671466 0.318394 0.409919 11.00000 0.03950 0.02237 = 0.02160 -0.00238 -0.00305 0.00263 O20 4 0.332927 0.199151 0.144435 11.00000 0.03689 0.02130 = 0.05094 -0.01254 0.02412 -0.00479 O31 4 0.382414 0.614386 0.121662 11.00000 0.02353 0.01854 = 0.02781 0.00702 0.00735 -0.00104 O32 4 0.537700 0.481294 0.252796 11.00000 0.01779 0.03025 = 0.03130 0.00995 0.00254 0.00207 O33 4 0.279071 0.435549 0.157847 11.00000 0.01943 0.01782 = 0.03258 -0.00242 0.00404 -0.00522 O34 4 0.343781 0.587941 0.290621 11.00000 0.05557 0.02971 = 0.04597 -0.01748 0.03680 -0.01346 O41 4 0.534969 0.913079 0.280667 11.00000 0.01834 0.01882 = 0.02210 0.00268 0.00729 -0.00289 O42 4 0.667605 1.074067 0.391290 11.00000 0.03467 0.02885 = 0.02531 -0.00409 0.01247 -0.00104 O43 4 0.617246 1.078488 0.199864 11.00000 0.03840 0.03768 = 0.02516 0.00642 0.00598 -0.00802 P1 5 0.802639 0.551021 0.114057 11.00000 0.00975 0.00799 = 0.01027 -0.00066 0.00280 -0.00021 P2 5 0.811712 0.519592 0.615593 11.00000 0.00948 0.00918 = 0.01061 0.00135 0.00322 0.00060 S1 6 0.809549 0.714036 0.172808 11.00000 0.01272 0.00927 = 0.01419 -0.00204 0.00550 -0.00155 S2 6 0.830028 0.364113 0.688888 11.00000 0.01052 0.01067 = 0.01227 0.00216 0.00380 0.00010 S3 6 0.386238 0.528551 0.206943 11.00000 0.01320 0.01291 = 0.01733 -0.00063 0.00735 -0.00098 S4 6 0.654043 1.002586 0.296308 11.00000 0.01582 0.01517 = 0.01247 -0.00138 0.00355 -0.00174 AG1 7 1.016750 0.721642 0.372718 11.00000 0.02357 0.01938 = 0.02542 0.00592 0.01537 0.00119 AG2 7 0.552594 0.779916 0.144526 11.00000 0.01326 0.01887 = 0.02736 -0.00160 -0.00053 0.00468 AG3 7 0.586317 0.270201 0.606260 11.00000 0.01358 0.01918 = 0.03365 -0.00070 -0.00067 -0.00615 AG4 7 0.929183 0.852976 0.086169 11.00000 0.03516 0.01746 = 0.05447 0.01215 0.03512 0.00609 O44 4 0.796819 0.942371 0.310575 11.00000 0.02222 0.03376 = 0.04803 -0.01438 0.01370 -0.00183 H1A 2 1.206627 0.552810 0.454181 11.00000 -1.50000 H1B 2 1.215579 0.559279 0.360296 11.00000 -1.50000 H2A 2 0.739248 1.032443 0.009312 11.00000 -1.20000 H2B 2 0.761952 1.037769 0.122599 11.00000 -1.50000 H10A 2 10.740390 10.322570 10.471478 11.00000 -1.50000 H10B 2 10.642550 10.247220 10.401240 11.00000 -1.50000 H20A 2 10.317902 10.269280 10.157950 11.00000 -1.50000 H20B 2 10.406099 10.154700 10.178801 11.00000 -1.50000 HKLF 4 REM wie193a in P 21 REM R1 = 0.0160 for 4704 Fo > 4sig(Fo) and 0.0161 for all 4740 data REM 374 parameters refined using 2 restraints END WGHT 0.0159 0.8117 REM Highest difference peak 0.503, deepest hole -0.375, 1-sigma level 0.076 Q1 1 0.7416 0.9828 0.2428 11.00000 0.05 0.50 Q2 1 0.7259 0.9938 0.4151 11.00000 0.05 0.49 Q3 1 0.6081 0.3642 0.3567 11.00000 0.05 0.43 Q4 1 0.5682 1.1157 0.2767 11.00000 0.05 0.42 Q5 1 0.8549 0.8628 0.0363 11.00000 0.05 0.40 Q6 1 0.9498 0.8992 0.1365 11.00000 0.05 0.32 Q7 1 0.9508 0.7184 0.2596 11.00000 0.05 0.31 Q8 1 0.6213 0.2620 0.5386 11.00000 0.05 0.30 Q9 1 0.8146 0.6866 0.4551 11.00000 0.05 0.29 Q10 1 1.0205 0.7205 0.3041 11.00000 0.05 0.29 Q11 1 0.8585 0.5461 0.5630 11.00000 0.05 0.27 Q12 1 0.7146 0.6555 0.3948 11.00000 0.05 0.27 Q13 1 0.8342 0.5047 0.1624 11.00000 0.05 0.27 Q14 1 0.6582 0.8986 0.3659 11.00000 0.05 0.26 Q15 1 1.1052 0.4246 0.1394 11.00000 0.05 0.26 Q16 1 1.1418 0.6138 0.3601 11.00000 0.05 0.26 Q17 1 0.8383 0.3753 -0.0363 11.00000 0.05 0.25 Q18 1 0.7535 0.4227 0.4215 11.00000 0.05 0.25 Q19 1 0.3856 0.2083 0.1044 11.00000 0.05 0.25 Q20 1 0.9147 0.3533 0.0407 11.00000 0.05 0.25 Q21 1 0.8514 0.3857 0.4612 11.00000 0.05 0.24 Q22 1 0.5538 0.5765 0.6240 11.00000 0.05 0.23 Q23 1 0.9054 0.8577 0.3429 11.00000 0.05 0.23 Q24 1 0.8571 0.6829 0.8735 11.00000 0.05 0.22 Q25 1 0.5888 0.2613 0.4844 11.00000 0.05 0.22 Q26 1 0.6629 0.3203 -0.2390 11.00000 0.05 0.22 Q27 1 0.5218 0.7758 0.2211 11.00000 0.05 0.22 Q28 1 0.5490 0.8952 0.3563 11.00000 0.05 0.21 Q29 1 0.8768 0.2867 0.2240 11.00000 0.05 0.21 Q30 1 0.6418 1.1333 0.4553 11.00000 0.05 0.21 Q31 1 0.7663 0.3088 0.1217 11.00000 0.05 0.21 Q32 1 0.9806 0.7957 0.2643 11.00000 0.05 0.21 Q33 1 0.7611 1.1527 0.4419 11.00000 0.05 0.21 Q34 1 0.2676 0.6118 0.2408 11.00000 0.05 0.21 Q35 1 0.8505 0.5669 0.6853 11.00000 0.05 0.21 Q36 1 1.1869 0.5167 0.2729 11.00000 0.05 0.21 Q37 1 0.8808 0.7990 -0.0199 11.00000 0.05 0.21 Q38 1 0.4605 0.2016 0.1806 11.00000 0.05 0.20 Q39 1 0.7243 0.3778 -0.0246 11.00000 0.05 0.20 Q40 1 0.9226 0.3735 0.7521 11.00000 0.05 0.20 Q41 1 0.7194 0.6354 0.7994 11.00000 0.05 0.20 Q42 1 0.3625 0.2217 0.1932 11.00000 0.05 0.19 Q43 1 0.9733 0.7240 0.4485 11.00000 0.05 0.19 Q44 1 0.3301 0.6196 0.1741 11.00000 0.05 0.19 Q45 1 0.5906 0.6308 -0.0784 11.00000 0.05 0.19 Q46 1 0.5497 0.4386 0.3038 11.00000 0.05 0.19 Q47 1 0.4931 0.4514 -0.0175 11.00000 0.05 0.19 Q48 1 0.2942 0.1509 0.0467 11.00000 0.05 0.19 Q49 1 0.9018 0.7128 0.5306 11.00000 0.05 0.19 Q50 1 0.9262 0.4198 0.3736 11.00000 0.05 0.19 ; 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 C11 C 0.8553(3) 0.4370(3) 0.2158(2) 0.0126(6) Uani 1 1 d . . . H11A H 0.9584 0.4498 0.2656 0.015 Uiso 1 1 calc R . . H11B H 0.7875 0.4374 0.2582 0.015 Uiso 1 1 calc R . . C12 C 0.6242(3) 0.4993(3) 0.0210(2) 0.0118(6) Uani 1 1 d . . . H12A H 0.5478 0.5010 0.0562 0.014 Uiso 1 1 calc R . . H12B H 0.5904 0.5499 -0.0436 0.014 Uiso 1 1 calc R . . C13 C 0.9297(3) 0.5229(3) 0.0403(2) 0.0121(6) Uani 1 1 d . . . H13A H 0.9054 0.5747 -0.0235 0.015 Uiso 1 1 calc R . . H13B H 1.0337 0.5386 0.0870 0.015 Uiso 1 1 calc R . . C14 C 0.7576(3) 0.3722(3) -0.0658(2) 0.0122(6) Uani 1 1 d . . . H14A H 0.7289 0.4295 -0.1256 0.015 Uiso 1 1 calc R . . H14B H 0.7545 0.2935 -0.0976 0.015 Uiso 1 1 calc R . . C15 C 0.9493(3) 0.3180(3) 0.1001(2) 0.0144(6) Uani 1 1 d . . . H15A H 0.9519 0.2366 0.0753 0.017 Uiso 1 1 calc R . . H15B H 1.0503 0.3373 0.1502 0.017 Uiso 1 1 calc R . . C16 C 0.6943(3) 0.3000(3) 0.0857(2) 0.0133(6) Uani 1 1 d . . . H16A H 0.6237 0.3092 0.1253 0.016 Uiso 1 1 calc R . . H16B H 0.6891 0.2177 0.0615 0.016 Uiso 1 1 calc R . . C21 C 0.9128(3) 0.5460(3) 0.5229(2) 0.0113(6) Uani 1 1 d . . . H21A H 1.0202 0.5296 0.5591 0.014 Uiso 1 1 calc R . . H21B H 0.8747 0.4939 0.4595 0.014 Uiso 1 1 calc R . . C22 C 0.6241(3) 0.5707(3) 0.5367(3) 0.0128(6) Uani 1 1 d . . . H22A H 0.5794 0.5189 0.4738 0.015 Uiso 1 1 calc R . . H22B H 0.5595 0.5697 0.5815 0.015 Uiso 1 1 calc R . . C23 C 0.8799(4) 0.6365(3) 0.7121(2) 0.0140(6) Uani 1 1 d . . . H23A H 0.8245 0.6374 0.7632 0.017 Uiso 1 1 calc R . . H23B H 0.9869 0.6243 0.7536 0.017 Uiso 1 1 calc R . . C24 C 0.7301(3) 0.6960(3) 0.4305(2) 0.0125(6) Uani 1 1 d . . . H24A H 0.7210 0.7743 0.3970 0.015 Uiso 1 1 calc R . . H24B H 0.6909 0.6382 0.3718 0.015 Uiso 1 1 calc R . . C25 C 0.9460(3) 0.7527(3) 0.5813(2) 0.0144(6) Uani 1 1 d . . . H25A H 1.0510 0.7334 0.6228 0.017 Uiso 1 1 calc R . . H25B H 0.9435 0.8334 0.5536 0.017 Uiso 1 1 calc R . . C26 C 0.7033(3) 0.7724(3) 0.5935(2) 0.0143(6) Uani 1 1 d . . . H26A H 0.6937 0.8540 0.5671 0.017 Uiso 1 1 calc R . . H26B H 0.6455 0.7653 0.6428 0.017 Uiso 1 1 calc R . . N11 N 0.8446(3) 0.3241(2) 0.1589(2) 0.0120(5) Uani 1 1 d . . . N12 N 0.6467(3) 0.3771(2) -0.01003(19) 0.0108(5) Uani 1 1 d . . . N13 N 0.9132(3) 0.3972(2) 0.0055(2) 0.0115(5) Uani 1 1 d . . . N21 N 0.8907(3) 0.6710(2) 0.48822(19) 0.0116(5) Uani 1 1 d . . . N22 N 0.6372(3) 0.6925(2) 0.4997(2) 0.0128(5) Uani 1 1 d . . . N23 N 0.8591(3) 0.7485(2) 0.6534(2) 0.0135(5) Uani 1 1 d . . . O1 O 1.1572(3) 0.5446(2) 0.3998(2) 0.0207(5) Uani 1 1 d . . . O2 O 0.8094(3) 1.0301(2) 0.0803(2) 0.0213(5) Uani 1 1 d D . . O10 O 0.6715(3) 0.3184(2) 0.4099(2) 0.0313(6) Uani 1 1 d . . . O20 O 0.3329(3) 0.1992(2) 0.1444(2) 0.0340(6) Uani 1 1 d . . . O31 O 0.3824(3) 0.6144(2) 0.1217(2) 0.0237(5) Uani 1 1 d . . . O32 O 0.5377(3) 0.4813(2) 0.2528(2) 0.0280(6) Uani 1 1 d . . . O33 O 0.2791(3) 0.4355(2) 0.1578(2) 0.0245(5) Uani 1 1 d . . . O34 O 0.3438(4) 0.5879(3) 0.2906(2) 0.0387(7) Uani 1 1 d . . . O41 O 0.5350(3) 0.9131(2) 0.28067(19) 0.0197(5) Uani 1 1 d . . . O42 O 0.6676(3) 1.0741(2) 0.3913(2) 0.0290(6) Uani 1 1 d . . . O43 O 0.6172(3) 1.0785(3) 0.1999(2) 0.0350(6) Uani 1 1 d . . . P1 P 0.80264(8) 0.55102(6) 0.11406(6) 0.00950(15) Uani 1 1 d . . . P2 P 0.81171(8) 0.51959(7) 0.61559(6) 0.00981(15) Uani 1 1 d . . . S1 S 0.80955(8) 0.71404(7) 0.17281(5) 0.01183(14) Uani 1 1 d . . . S2 S 0.83003(8) 0.36411(7) 0.68889(5) 0.01117(14) Uani 1 1 d . . . S3 S 0.38624(8) 0.52855(7) 0.20694(6) 0.01393(15) Uani 1 1 d . . . S4 S 0.65404(9) 1.00259(7) 0.29631(6) 0.01482(15) Uani 1 1 d . . . Ag1 Ag 1.01675(3) 0.72164(2) 0.37272(2) 0.02099(6) Uani 1 1 d . . . Ag2 Ag 0.55259(2) 0.77992(2) 0.14453(2) 0.02176(6) Uani 1 1 d . . . Ag3 Ag 0.58632(3) 0.27020(2) 0.60626(2) 0.02439(7) Uani 1 1 d . . . Ag4 Ag 0.92918(3) 0.85298(2) 0.08617(3) 0.03059(8) Uani 1 1 d . . . O44 O 0.7968(3) 0.9424(3) 0.3106(2) 0.0342(6) Uani 1 1 d . . . H1A H 1.207(7) 0.553(6) 0.454(5) 0.051 Uiso 1 1 d . . . H1B H 1.216(7) 0.559(5) 0.360(5) 0.051 Uiso 1 1 d . . . H2A H 0.739(5) 1.032(5) 0.009(2) 0.041 Uiso 1 1 d D . . H2B H 0.762(7) 1.038(5) 0.123(5) 0.051 Uiso 1 1 d . . . H10A H 0.7404 0.3226 0.4715 0.051 Uiso 1 1 d . . . H10B H 0.6425 0.2472 0.4012 0.051 Uiso 1 1 d . . . H20A H 0.3179 0.2693 0.1580 0.051 Uiso 1 1 d . . . H20B H 0.4061 0.1547 0.1788 0.051 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 C11 0.0169(14) 0.0106(15) 0.0100(13) 0.0003(11) 0.0042(11) 0.0002(12) C12 0.0100(13) 0.0123(14) 0.0138(14) 0.0008(11) 0.0048(11) 0.0007(11) C13 0.0118(14) 0.0103(15) 0.0151(14) -0.0003(11) 0.0057(11) -0.0029(12) C14 0.0124(14) 0.0129(15) 0.0121(13) -0.0021(11) 0.0053(11) -0.0021(11) C15 0.0130(14) 0.0118(15) 0.0186(16) 0.0023(11) 0.0053(12) 0.0022(11) C16 0.0142(14) 0.0120(16) 0.0120(14) -0.0016(11) 0.0021(11) -0.0012(11) C21 0.0120(14) 0.0111(15) 0.0114(14) 0.0023(11) 0.0047(11) 0.0020(11) C22 0.0112(14) 0.0103(14) 0.0172(14) 0.0020(11) 0.0051(11) 0.0015(12) C23 0.0166(15) 0.0131(15) 0.0123(14) -0.0004(11) 0.0049(12) 0.0007(12) C24 0.0124(14) 0.0126(15) 0.0101(13) 0.0016(11) 0.0008(11) 0.0005(11) C25 0.0131(14) 0.0108(16) 0.0183(15) 0.0008(11) 0.0041(11) -0.0027(11) C26 0.0159(14) 0.0123(14) 0.0144(14) -0.0023(12) 0.0049(11) 0.0018(13) N11 0.0120(12) 0.0090(12) 0.0138(12) 0.0000(9) 0.0027(10) 0.0005(9) N12 0.0106(11) 0.0098(13) 0.0125(12) -0.0012(9) 0.0047(10) -0.0018(9) N13 0.0091(12) 0.0102(13) 0.0163(13) -0.0006(10) 0.0055(10) -0.0001(9) N21 0.0125(12) 0.0095(12) 0.0123(12) 0.0008(9) 0.0036(10) -0.0015(10) N22 0.0136(12) 0.0098(13) 0.0135(12) 0.0014(9) 0.0027(10) 0.0015(10) N23 0.0135(12) 0.0108(14) 0.0156(12) -0.0028(9) 0.0041(10) -0.0023(10) O1 0.0179(12) 0.0175(13) 0.0256(12) -0.0031(10) 0.0060(10) -0.0005(10) O2 0.0267(13) 0.0183(13) 0.0186(12) 0.0013(9) 0.0075(10) 0.0059(10) O10 0.0395(15) 0.0224(13) 0.0216(13) -0.0024(10) -0.0031(11) 0.0026(11) O20 0.0369(15) 0.0213(14) 0.0509(16) -0.0125(12) 0.0241(13) -0.0048(11) O31 0.0235(12) 0.0185(13) 0.0278(13) 0.0070(10) 0.0074(10) -0.0010(10) O32 0.0178(12) 0.0302(15) 0.0313(14) 0.0099(11) 0.0025(10) 0.0021(10) O33 0.0194(12) 0.0178(13) 0.0326(13) -0.0024(10) 0.0040(10) -0.0052(10) O34 0.0556(19) 0.0297(15) 0.0460(17) -0.0175(13) 0.0368(15) -0.0135(14) O41 0.0183(11) 0.0188(12) 0.0221(12) 0.0027(9) 0.0073(9) -0.0029(10) O42 0.0347(14) 0.0289(14) 0.0253(13) -0.0041(11) 0.0125(11) -0.0010(12) O43 0.0384(16) 0.0377(16) 0.0252(14) 0.0064(12) 0.0060(12) -0.0080(13) P1 0.0098(3) 0.0080(4) 0.0103(3) -0.0007(3) 0.0028(3) -0.0002(3) P2 0.0095(3) 0.0092(4) 0.0106(3) 0.0014(3) 0.0032(3) 0.0006(3) S1 0.0127(3) 0.0093(3) 0.0142(3) -0.0020(3) 0.0055(3) -0.0016(3) S2 0.0105(3) 0.0107(3) 0.0123(3) 0.0022(3) 0.0038(3) 0.0001(3) S3 0.0132(4) 0.0129(4) 0.0173(4) -0.0006(3) 0.0073(3) -0.0010(3) S4 0.0158(4) 0.0152(4) 0.0125(3) -0.0014(3) 0.0035(3) -0.0017(3) Ag1 0.02357(12) 0.01938(13) 0.02542(12) 0.00592(10) 0.01537(10) 0.00119(10) Ag2 0.01326(11) 0.01887(13) 0.02736(13) -0.00160(11) -0.00053(9) 0.00468(10) Ag3 0.01358(11) 0.01918(12) 0.03365(14) -0.00070(11) -0.00067(9) -0.00615(10) Ag4 0.03516(15) 0.01746(13) 0.05447(18) 0.01215(13) 0.03512(14) 0.00609(12) O44 0.0222(13) 0.0338(16) 0.0480(17) -0.0144(13) 0.0137(12) -0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 N11 1.480(4) . ? C11 P1 1.817(3) . ? C12 N12 1.493(4) . ? C12 P1 1.825(3) . ? C13 N13 1.501(4) . ? C13 P1 1.826(3) . ? C14 N12 1.483(4) . ? C14 N13 1.490(4) . ? C15 N11 1.462(4) . ? C15 N13 1.486(4) . ? C16 N11 1.458(4) . ? C16 N12 1.480(4) . ? C21 N21 1.495(4) . ? C21 P2 1.824(3) . ? C22 N22 1.496(4) . ? C22 P2 1.833(3) . ? C23 N23 1.476(4) . ? C23 P2 1.808(3) . ? C24 N22 1.476(4) . ? C24 N21 1.488(4) . ? C25 N23 1.462(4) . ? C25 N21 1.490(4) . ? C26 N23 1.452(4) . ? C26 N22 1.494(4) . ? N12 Ag2 2.388(2) 2_645 ? N13 Ag4 2.287(3) 2_745 ? N21 Ag1 2.317(3) . ? N22 Ag3 2.294(2) 2_656 ? O1 Ag1 2.387(2) . ? O2 Ag4 2.315(2) . ? O31 S3 1.485(2) . ? O31 Ag2 2.446(2) . ? O32 S3 1.467(3) . ? O33 S3 1.465(2) . ? O34 S3 1.468(3) . ? O34 Ag3 2.455(3) 2_656 ? O41 S4 1.491(2) . ? O41 Ag2 2.406(2) . ? O42 S4 1.466(3) . ? O43 S4 1.481(3) . ? P1 S1 2.0123(11) . ? P2 S2 2.0040(11) . ? S1 Ag4 2.4564(8) . ? S1 Ag2 2.4698(7) . ? S1 Ag1 2.7065(7) . ? S2 Ag3 2.4545(7) . ? S2 Ag1 2.5044(8) 2_746 ? S4 O44 1.481(3) . ? Ag1 S2 2.5044(8) 2_756 ? Ag2 N12 2.388(2) 2_655 ? Ag3 N22 2.294(2) 2_646 ? Ag3 O34 2.455(3) 2_646 ? Ag4 N13 2.287(3) 2_755 ? 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 N11 C11 P1 107.27(19) . . ? N12 C12 P1 107.4(2) . . ? N13 C13 P1 108.2(2) . . ? N12 C14 N13 113.9(2) . . ? N11 C15 N13 114.4(2) . . ? N11 C16 N12 113.5(2) . . ? N21 C21 P2 108.2(2) . . ? N22 C22 P2 107.9(2) . . ? N23 C23 P2 108.7(2) . . ? N22 C24 N21 114.1(2) . . ? N23 C25 N21 113.4(2) . . ? N23 C26 N22 113.6(3) . . ? C16 N11 C15 109.6(2) . . ? C16 N11 C11 112.5(2) . . ? C15 N11 C11 111.8(2) . . ? C16 N12 C14 109.9(2) . . ? C16 N12 C12 110.7(2) . . ? C14 N12 C12 111.5(2) . . ? C16 N12 Ag2 106.97(17) . 2_645 ? C14 N12 Ag2 97.79(17) . 2_645 ? C12 N12 Ag2 119.17(18) . 2_645 ? C15 N13 C14 108.0(2) . . ? C15 N13 C13 110.9(2) . . ? C14 N13 C13 110.8(2) . . ? C15 N13 Ag4 107.75(17) . 2_745 ? C14 N13 Ag4 108.49(17) . 2_745 ? C13 N13 Ag4 110.79(18) . 2_745 ? C25 N21 C24 108.4(2) . . ? C25 N21 C21 112.0(2) . . ? C24 N21 C21 110.7(2) . . ? C25 N21 Ag1 105.59(18) . . ? C24 N21 Ag1 106.88(18) . . ? C21 N21 Ag1 113.01(18) . . ? C24 N22 C26 109.0(2) . . ? C24 N22 C22 111.2(2) . . ? C26 N22 C22 111.0(2) . . ? C24 N22 Ag3 104.00(17) . 2_656 ? C26 N22 Ag3 108.07(18) . 2_656 ? C22 N22 Ag3 113.32(18) . 2_656 ? C26 N23 C25 110.0(2) . . ? C26 N23 C23 112.2(2) . . ? C25 N23 C23 111.5(2) . . ? S3 O31 Ag2 125.10(14) . . ? S3 O34 Ag3 135.92(18) . 2_656 ? S4 O41 Ag2 107.08(12) . . ? C11 P1 C12 102.97(14) . . ? C11 P1 C13 101.67(14) . . ? C12 P1 C13 102.77(14) . . ? C11 P1 S1 114.56(10) . . ? C12 P1 S1 117.39(11) . . ? C13 P1 S1 115.40(10) . . ? C23 P2 C21 101.83(15) . . ? C23 P2 C22 102.22(15) . . ? C21 P2 C22 101.76(14) . . ? C23 P2 S2 111.39(10) . . ? C21 P2 S2 119.48(10) . . ? C22 P2 S2 117.69(11) . . ? P1 S1 Ag4 112.28(4) . . ? P1 S1 Ag2 108.93(4) . . ? Ag4 S1 Ag2 109.15(3) . . ? P1 S1 Ag1 108.83(4) . . ? Ag4 S1 Ag1 97.62(3) . . ? Ag2 S1 Ag1 119.67(3) . . ? P2 S2 Ag3 105.11(4) . . ? P2 S2 Ag1 112.64(4) . 2_746 ? Ag3 S2 Ag1 98.10(3) . 2_746 ? O33 S3 O32 110.86(15) . . ? O33 S3 O34 109.80(17) . . ? O32 S3 O34 110.28(19) . . ? O33 S3 O31 108.17(15) . . ? O32 S3 O31 108.79(15) . . ? O34 S3 O31 108.88(17) . . ? O42 S4 O44 110.02(16) . . ? O42 S4 O43 109.56(17) . . ? O44 S4 O43 108.65(19) . . ? O42 S4 O41 110.00(15) . . ? O44 S4 O41 108.86(16) . . ? O43 S4 O41 109.74(15) . . ? N21 Ag1 O1 94.62(9) . . ? N21 Ag1 S2 150.39(7) . 2_756 ? O1 Ag1 S2 103.91(7) . 2_756 ? N21 Ag1 S1 105.27(6) . . ? O1 Ag1 S1 107.75(7) . . ? S2 Ag1 S1 90.99(2) 2_756 . ? N12 Ag2 O41 91.14(8) 2_655 . ? N12 Ag2 O31 86.66(8) 2_655 . ? O41 Ag2 O31 111.68(9) . . ? N12 Ag2 S1 138.80(6) 2_655 . ? O41 Ag2 S1 113.55(6) . . ? O31 Ag2 S1 111.47(6) . . ? N22 Ag3 O34 91.69(11) 2_646 2_646 ? N22 Ag3 S2 169.69(7) 2_646 . ? O34 Ag3 S2 95.06(9) 2_646 . ? N13 Ag4 O2 101.25(10) 2_755 . ? N13 Ag4 S1 152.21(7) 2_755 . ? O2 Ag4 S1 106.20(7) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.503 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 927876'