# 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_3rpua _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 Ag2 Cl2 N2 O12' _chemical_formula_weight 640.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3920(2) _cell_length_b 10.7920(3) _cell_length_c 11.6410(4) _cell_angle_alpha 80.2860(10) _cell_angle_beta 88.2720(10) _cell_angle_gamma 77.0800(10) _cell_volume 892.14(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(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 0.48 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624.0 _exptl_absorpt_coefficient_mu 2.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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_reflns_number 24007 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5164 _reflns_number_gt 4976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.9232P] 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 5214 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.081289(19) 0.810659(13) 0.025840(12) 0.02130(4) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.0000 0.01946(5) Uani 1 2 d S . . Ag3 Ag 0.0000 0.5000 0.0000 0.01973(5) Uani 1 2 d S . . Cl1 Cl -0.23113(5) 0.92652(4) -0.25352(3) 0.01548(7) Uani 1 1 d . . . Cl2 Cl 0.24501(5) 0.58447(4) 0.25636(3) 0.01527(7) Uani 1 1 d . . . O1 O -0.21940(18) 0.83699(12) 0.10017(10) 0.0175(2) Uani 1 1 d . . . O2 O 0.21752(17) 0.63894(12) -0.08557(10) 0.0157(2) Uani 1 1 d . . . O3 O -0.09221(19) 0.92389(14) -0.16740(12) 0.0240(3) Uani 1 1 d . . . O4 O -0.4065(2) 0.99944(16) -0.22004(16) 0.0323(3) Uani 1 1 d . . . O5 O -0.1762(3) 0.98335(16) -0.36508(13) 0.0343(4) Uani 1 1 d . . . O6 O -0.2469(2) 0.79585(13) -0.25710(13) 0.0251(3) Uani 1 1 d . . . O7 O 0.4192(2) 0.51537(15) 0.21601(14) 0.0297(3) Uani 1 1 d . . . O8 O 0.2004(3) 0.5219(2) 0.36764(14) 0.0468(5) Uani 1 1 d . . . O9 O 0.2550(2) 0.71477(15) 0.25999(18) 0.0361(4) Uani 1 1 d . . . O10 O 0.0987(2) 0.58863(15) 0.17401(13) 0.0271(3) Uani 1 1 d . . . O11 O 0.3326(2) 0.90657(14) 0.00146(14) 0.0225(3) Uani 1 1 d . . . O12 O 0.28567(19) 0.34048(13) 0.03046(13) 0.0202(2) Uani 1 1 d . . . N1 N -0.23151(19) 0.80841(13) 0.21697(12) 0.0135(2) Uani 1 1 d . . . N2 N 0.23150(18) 0.67777(13) -0.20121(12) 0.0129(2) Uani 1 1 d . . . C1 C -0.1549(2) 0.87327(16) 0.28416(16) 0.0177(3) Uani 1 1 d . . . H1 H -0.0912 0.9372 0.2491 0.021 Uiso 1 1 calc R . . C2 C -0.1687(3) 0.84705(18) 0.40367(16) 0.0210(3) Uani 1 1 d . . . H2 H -0.1164 0.8938 0.4510 0.025 Uiso 1 1 calc R . . C3 C -0.2592(3) 0.75236(19) 0.45470(16) 0.0233(3) Uani 1 1 d . . . H3 H -0.2683 0.7327 0.5370 0.028 Uiso 1 1 calc R . . C4 C -0.3361(3) 0.68670(18) 0.38303(17) 0.0223(3) Uani 1 1 d . . . H4 H -0.3986 0.6214 0.4162 0.027 Uiso 1 1 calc R . . C5 C -0.3217(2) 0.71661(17) 0.26349(16) 0.0182(3) Uani 1 1 d . . . H5 H -0.3752 0.6725 0.2142 0.022 Uiso 1 1 calc R . . C6 C 0.1552(2) 0.62080(16) -0.27600(16) 0.0179(3) Uani 1 1 d . . . H6 H 0.0902 0.5555 -0.2470 0.022 Uiso 1 1 calc R . . C7 C 0.1713(3) 0.65732(18) -0.39451(16) 0.0219(3) Uani 1 1 d . . . H7 H 0.1191 0.6163 -0.4471 0.026 Uiso 1 1 calc R . . C8 C 0.2636(3) 0.75383(18) -0.43687(16) 0.0222(3) Uani 1 1 d . . . H8 H 0.2746 0.7802 -0.5184 0.027 Uiso 1 1 calc R . . C9 C 0.3397(3) 0.81127(17) -0.35768(16) 0.0204(3) Uani 1 1 d . . . H9 H 0.4035 0.8777 -0.3850 0.024 Uiso 1 1 calc R . . C10 C 0.3229(2) 0.77196(16) -0.23921(15) 0.0164(3) Uani 1 1 d . . . H10 H 0.3752 0.8109 -0.1850 0.020 Uiso 1 1 calc R . . H11A H 0.362(4) 0.912(3) 0.063(3) 0.033(8) Uiso 1 1 d . . . H11B H 0.303(6) 0.979(4) -0.034(4) 0.060(11) Uiso 1 1 d . . . H12A H 0.281(4) 0.307(3) 0.098(3) 0.031(7) Uiso 1 1 d . . . H12B H 0.280(4) 0.289(3) -0.007(3) 0.035(8) 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 0.02091(7) 0.02403(7) 0.01706(7) -0.00030(5) 0.00442(5) -0.00391(5) Ag2 0.01536(8) 0.02409(9) 0.01749(9) 0.00082(6) -0.00400(6) -0.00400(6) Ag3 0.01623(9) 0.02395(9) 0.02085(9) -0.00472(7) 0.00180(6) -0.00777(6) Cl1 0.01599(17) 0.01665(16) 0.01316(16) -0.00122(12) -0.00057(13) -0.00312(13) Cl2 0.01627(17) 0.01704(16) 0.01271(16) -0.00367(12) -0.00045(13) -0.00312(13) O1 0.0210(6) 0.0205(6) 0.0113(5) -0.0022(4) 0.0000(4) -0.0055(4) O2 0.0171(5) 0.0188(5) 0.0103(5) 0.0003(4) 0.0013(4) -0.0041(4) O3 0.0198(6) 0.0307(7) 0.0209(6) -0.0006(5) -0.0068(5) -0.0063(5) O4 0.0171(6) 0.0352(8) 0.0439(9) -0.0184(7) -0.0024(6) 0.0047(6) O5 0.0561(11) 0.0351(8) 0.0142(6) 0.0021(6) 0.0039(6) -0.0208(7) O6 0.0351(8) 0.0186(6) 0.0238(7) -0.0057(5) 0.0030(6) -0.0094(5) O7 0.0202(7) 0.0327(7) 0.0331(8) -0.0123(6) 0.0011(6) 0.0056(5) O8 0.0632(13) 0.0550(11) 0.0138(7) 0.0067(7) 0.0085(7) -0.0060(9) O9 0.0273(8) 0.0224(7) 0.0635(12) -0.0190(7) -0.0020(7) -0.0068(6) O10 0.0228(7) 0.0366(8) 0.0250(7) -0.0101(6) -0.0066(5) -0.0084(6) O11 0.0254(7) 0.0204(6) 0.0225(7) -0.0053(5) -0.0010(5) -0.0055(5) O12 0.0254(7) 0.0165(5) 0.0195(6) -0.0037(5) 0.0005(5) -0.0060(5) N1 0.0120(6) 0.0148(6) 0.0135(6) -0.0030(5) 0.0003(5) -0.0021(4) N2 0.0117(6) 0.0138(6) 0.0119(6) -0.0016(4) 0.0013(4) -0.0005(4) C1 0.0166(7) 0.0187(7) 0.0194(8) -0.0053(6) -0.0007(6) -0.0056(6) C2 0.0196(8) 0.0262(8) 0.0181(8) -0.0077(6) -0.0021(6) -0.0033(6) C3 0.0208(8) 0.0301(9) 0.0156(8) -0.0021(6) 0.0032(6) -0.0004(7) C4 0.0212(8) 0.0238(8) 0.0211(8) 0.0000(6) 0.0052(6) -0.0066(6) C5 0.0172(7) 0.0194(7) 0.0198(8) -0.0037(6) 0.0025(6) -0.0074(6) C6 0.0169(7) 0.0180(7) 0.0195(8) -0.0038(6) -0.0019(6) -0.0043(6) C7 0.0220(8) 0.0264(8) 0.0165(8) -0.0069(6) -0.0043(6) -0.0005(6) C8 0.0215(8) 0.0265(8) 0.0138(7) -0.0002(6) 0.0009(6) 0.0023(6) C9 0.0201(8) 0.0201(7) 0.0189(8) 0.0004(6) 0.0048(6) -0.0036(6) C10 0.0153(7) 0.0160(7) 0.0181(7) -0.0026(6) 0.0019(6) -0.0041(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 O11 2.3091(15) . ? Ag1 O1 2.3354(13) . ? Ag1 O2 2.4552(13) . ? Ag1 O3 2.5969(13) . ? Ag2 O2 2.4129(12) 2_665 ? Ag2 O2 2.4129(12) . ? Ag2 O12 2.5650(14) . ? Ag2 O12 2.5651(14) 2_665 ? Ag2 O7 2.5909(16) 2_665 ? Ag2 O7 2.5909(16) . ? Ag3 O12 2.4004(14) . ? Ag3 O12 2.4004(14) 2_565 ? Ag3 O2 2.5107(12) . ? Ag3 O2 2.5107(12) 2_565 ? Ag3 O10 2.5701(14) 2_565 ? Ag3 O10 2.5701(14) . ? Cl1 O5 1.4278(15) . ? Cl1 O4 1.4384(15) . ? Cl1 O6 1.4483(14) . ? Cl1 O3 1.4491(13) . ? Cl2 O8 1.4220(16) . ? Cl2 O9 1.4322(15) . ? Cl2 O7 1.4449(14) . ? Cl2 O10 1.4550(14) . ? O1 N1 1.3473(18) . ? O2 N2 1.3487(17) . ? O11 H11A 0.77(3) . ? O11 H11B 0.80(4) . ? O12 H12A 0.81(3) . ? O12 H12B 0.77(3) . ? N1 C1 1.346(2) . ? N1 C5 1.346(2) . ? N2 C6 1.349(2) . ? N2 C10 1.350(2) . ? C1 C2 1.378(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(3) . ? C2 H2 0.9500 . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.379(2) . ? C6 H6 0.9500 . ? C7 C8 1.385(3) . ? C7 H7 0.9500 . ? C8 C9 1.390(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 O11 Ag1 O1 142.39(5) . . ? O11 Ag1 O2 94.40(5) . . ? O1 Ag1 O2 122.99(4) . . ? O11 Ag1 O3 98.00(5) . . ? O1 Ag1 O3 82.89(4) . . ? O2 Ag1 O3 84.73(4) . . ? O2 Ag2 O2 180.0 2_665 . ? O2 Ag2 O12 99.77(4) 2_665 . ? O2 Ag2 O12 80.23(4) . . ? O2 Ag2 O12 80.23(4) 2_665 2_665 ? O2 Ag2 O12 99.77(4) . 2_665 ? O12 Ag2 O12 180.00(6) . 2_665 ? O2 Ag2 O7 97.53(4) 2_665 2_665 ? O2 Ag2 O7 82.47(4) . 2_665 ? O12 Ag2 O7 97.57(5) . 2_665 ? O12 Ag2 O7 82.43(5) 2_665 2_665 ? O2 Ag2 O7 82.47(4) 2_665 . ? O2 Ag2 O7 97.53(4) . . ? O12 Ag2 O7 82.43(5) . . ? O12 Ag2 O7 97.57(5) 2_665 . ? O7 Ag2 O7 180.00(6) 2_665 . ? O12 Ag3 O12 180.0 . 2_565 ? O12 Ag3 O2 81.58(4) . . ? O12 Ag3 O2 98.42(4) 2_565 . ? O12 Ag3 O2 98.42(4) . 2_565 ? O12 Ag3 O2 81.58(4) 2_565 2_565 ? O2 Ag3 O2 180.0 . 2_565 ? O12 Ag3 O10 93.61(5) . 2_565 ? O12 Ag3 O10 86.39(5) 2_565 2_565 ? O2 Ag3 O10 104.41(5) . 2_565 ? O2 Ag3 O10 75.59(5) 2_565 2_565 ? O12 Ag3 O10 86.39(5) . . ? O12 Ag3 O10 93.61(5) 2_565 . ? O2 Ag3 O10 75.59(5) . . ? O2 Ag3 O10 104.41(5) 2_565 . ? O10 Ag3 O10 180.0 2_565 . ? O5 Cl1 O4 110.90(11) . . ? O5 Cl1 O6 109.60(9) . . ? O4 Cl1 O6 109.17(10) . . ? O5 Cl1 O3 109.25(10) . . ? O4 Cl1 O3 108.75(9) . . ? O6 Cl1 O3 109.14(9) . . ? O8 Cl2 O9 110.99(13) . . ? O8 Cl2 O7 110.62(11) . . ? O9 Cl2 O7 109.69(10) . . ? O8 Cl2 O10 108.86(12) . . ? O9 Cl2 O10 107.51(10) . . ? O7 Cl2 O10 109.10(9) . . ? N1 O1 Ag1 115.65(9) . . ? N2 O2 Ag2 112.84(9) . . ? N2 O2 Ag1 115.19(9) . . ? Ag2 O2 Ag1 113.39(5) . . ? N2 O2 Ag3 122.94(9) . . ? Ag2 O2 Ag3 97.28(4) . . ? Ag1 O2 Ag3 92.84(4) . . ? Cl1 O3 Ag1 148.51(9) . . ? Cl2 O7 Ag2 125.05(9) . . ? Cl2 O10 Ag3 147.06(9) . . ? Ag1 O11 H11A 106(2) . . ? Ag1 O11 H11B 111(3) . . ? H11A O11 H11B 107(4) . . ? Ag3 O12 Ag2 96.15(5) . . ? Ag3 O12 H12A 104(2) . . ? Ag2 O12 H12A 113(2) . . ? Ag3 O12 H12B 107(2) . . ? Ag2 O12 H12B 127(2) . . ? H12A O12 H12B 107(3) . . ? C1 N1 C5 121.64(15) . . ? C1 N1 O1 119.21(14) . . ? C5 N1 O1 119.14(14) . . ? O2 N2 C6 119.19(14) . . ? O2 N2 C10 119.15(14) . . ? C6 N2 C10 121.66(15) . . ? N1 C1 C2 120.06(16) . . ? N1 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C1 C2 C3 119.89(17) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.69(17) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.86(17) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 119.84(16) . . ? N1 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N2 C6 C7 120.04(16) . . ? N2 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C8 120.00(17) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 118.62(16) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 120.16(17) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 119.51(16) . . ? N2 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.531 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 965104' ####################################################################### # # 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_3rpu146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Ag2 Cl2 N4 O12' _chemical_formula_weight 795.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 21.9957(2) _cell_length_b 21.9957(2) _cell_length_c 14.0739(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5896.9(1) _cell_formula_units_Z 9 _cell_measurement_temperature 120(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 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6102 _exptl_absorpt_correction_T_max 0.8027 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 95119 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6016 _reflns_number_gt 5879 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+23.0181P] 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), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.038(18) _refine_ls_number_reflns 6016 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 0.0000 0.0000 0.58860(2) 0.01371(8) Uani 1 3 d S . . Ag2 Ag 0.070400(13) -0.015410(14) 0.319641(18) 0.02321(6) Uani 1 1 d . . . Ag3 Ag 0.0000 0.0000 0.07707(3) 0.01689(8) Uani 1 3 d S . . Ag4 Ag 0.0000 0.0000 -0.16466(3) 0.01559(7) Uani 1 3 d S . . Cl1 Cl 0.22908(4) 0.01824(5) 0.26373(6) 0.02480(16) Uani 1 1 d . . . Cl2 Cl 0.34883(4) 0.23328(4) -0.17688(6) 0.02359(16) Uani 1 1 d . . . O1 O 0.08429(12) -0.00149(13) 0.47384(15) 0.0197(5) Uani 1 1 d . . . O2 O 0.08321(12) 0.07826(12) 0.20344(18) 0.0200(5) Uani 1 1 d . . . O3 O 0.00175(12) 0.08307(11) -0.04303(16) 0.0201(5) Uani 1 1 d . . . O4 O -0.05522(11) -0.09270(12) -0.28597(16) 0.0196(5) Uani 1 1 d . . . O5 O 0.16134(16) -0.04501(15) 0.2634(3) 0.0499(9) Uani 1 1 d . . . O6 O 0.25412(16) 0.0339(2) 0.1686(2) 0.0529(9) Uani 1 1 d . . . O7 O 0.2769(2) 0.0074(2) 0.3204(2) 0.0533(9) Uani 1 1 d . . . O8 O 0.22066(14) 0.07444(13) 0.30316(19) 0.0306(6) Uani 1 1 d . . . O9 O 0.31820(17) 0.16341(14) -0.1397(2) 0.0406(7) Uani 1 1 d . . . O10 O 0.35380(15) 0.27985(14) -0.10153(18) 0.0309(6) Uani 1 1 d . . . O12 O 0.30548(18) 0.23570(18) -0.2511(2) 0.0455(8) Uani 1 1 d . . . N1 N 0.15220(13) 0.03986(15) 0.49987(18) 0.0179(5) Uani 1 1 d . . . N2 N 0.14657(14) 0.13392(14) 0.18377(19) 0.0173(5) Uani 1 1 d . . . N3 N 0.05667(15) 0.14825(14) -0.04197(19) 0.0193(5) Uani 1 1 d . . . N4 N -0.12504(14) -0.12752(14) -0.27790(18) 0.0181(5) Uani 1 1 d . . . C1 C 0.19339(17) 0.01105(18) 0.5083(2) 0.0194(6) Uani 1 1 d . . . H1 H 0.1758 -0.0371 0.4937 0.023 Uiso 1 1 calc R . . C2 C 0.26207(18) 0.05291(19) 0.5388(2) 0.0244(7) Uani 1 1 d . . . H2 H 0.2919 0.0335 0.5453 0.029 Uiso 1 1 calc R . . C3 C 0.28704(18) 0.1226(2) 0.5597(3) 0.0297(8) Uani 1 1 d . . . H3 H 0.3337 0.1511 0.5820 0.036 Uiso 1 1 calc R . . C4 C 0.24350(18) 0.15075(19) 0.5479(3) 0.0274(7) Uani 1 1 d . . . H4 H 0.2605 0.1990 0.5606 0.033 Uiso 1 1 calc R . . C5 C 0.17525(17) 0.10823(17) 0.5175(2) 0.0209(6) Uani 1 1 d . . . H5 H 0.1449 0.1269 0.5091 0.025 Uiso 1 1 calc R . . C6 C 0.17630(18) 0.18975(18) 0.2427(2) 0.0223(6) Uani 1 1 d . . . H6 H 0.1531 0.1896 0.2997 0.027 Uiso 1 1 calc R . . C7 C 0.24075(18) 0.24723(18) 0.2200(3) 0.0262(7) Uani 1 1 d . . . H7 H 0.2619 0.2868 0.2611 0.031 Uiso 1 1 calc R . . C8 C 0.27413(19) 0.24661(19) 0.1368(3) 0.0296(8) Uani 1 1 d . . . H8 H 0.3180 0.2860 0.1197 0.035 Uiso 1 1 calc R . . C9 C 0.24308(18) 0.1882(2) 0.0792(3) 0.0270(7) Uani 1 1 d . . . H9 H 0.2661 0.1868 0.0228 0.032 Uiso 1 1 calc R . . C10 C 0.17853(17) 0.13177(18) 0.1031(2) 0.0206(6) Uani 1 1 d . . . H10 H 0.1568 0.0917 0.0629 0.025 Uiso 1 1 calc R . . C11 C 0.0529(2) 0.19737(19) 0.0106(3) 0.0333(8) Uani 1 1 d . . . H11 H 0.0114 0.1854 0.0454 0.040 Uiso 1 1 calc R . . C12 C 0.1087(2) 0.2648(2) 0.0140(3) 0.0424(10) Uani 1 1 d . . . H12 H 0.1062 0.2990 0.0523 0.051 Uiso 1 1 calc R . . C13 C 0.1676(2) 0.2826(2) -0.0375(3) 0.0370(9) Uani 1 1 d . . . H13 H 0.2059 0.3294 -0.0366 0.044 Uiso 1 1 calc R . . C14 C 0.1711(2) 0.2322(2) -0.0908(3) 0.0341(9) Uani 1 1 d . . . H14 H 0.2120 0.2437 -0.1268 0.041 Uiso 1 1 calc R . . C15 C 0.11484(19) 0.16449(19) -0.0915(3) 0.0256(7) Uani 1 1 d . . . H15 H 0.1174 0.1292 -0.1274 0.031 Uiso 1 1 calc R . . C16 C -0.16248(18) -0.09798(19) -0.3091(2) 0.0235(7) Uani 1 1 d . . . H16 H -0.1390 -0.0523 -0.3361 0.028 Uiso 1 1 calc R . . C17 C -0.2343(2) -0.1338(2) -0.3018(3) 0.0357(9) Uani 1 1 d . . . H17 H -0.2605 -0.1131 -0.3242 0.043 Uiso 1 1 calc R . . C18 C -0.2683(2) -0.1998(3) -0.2620(3) 0.0477(13) Uani 1 1 d . . . H18 H -0.3180 -0.2251 -0.2568 0.057 Uiso 1 1 calc R . . C19 C -0.2294(2) -0.2282(2) -0.2301(3) 0.0448(11) Uani 1 1 d . . . H19 H -0.2524 -0.2735 -0.2020 0.054 Uiso 1 1 calc R . . C20 C -0.1572(2) -0.19216(18) -0.2380(3) 0.0293(8) Uani 1 1 d . . . H20 H -0.1305 -0.2124 -0.2158 0.035 Uiso 1 1 calc R . . O11 O 0.41771(16) 0.25402(17) -0.2128(2) 0.0435(7) 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 Ag1 0.01460(11) 0.01460(11) 0.01192(17) 0.000 0.000 0.00730(6) Ag2 0.02201(12) 0.03216(14) 0.01777(11) -0.00547(10) -0.00481(10) 0.01526(11) Ag3 0.01908(12) 0.01908(12) 0.01251(18) 0.000 0.000 0.00954(6) Ag4 0.01750(10) 0.01750(10) 0.01179(16) 0.000 0.000 0.00875(5) Cl1 0.0214(4) 0.0317(4) 0.0214(4) -0.0010(3) 0.0044(3) 0.0134(3) Cl2 0.0265(4) 0.0235(4) 0.0213(4) -0.0009(3) -0.0002(3) 0.0129(3) O1 0.0124(11) 0.0307(13) 0.0125(11) -0.0029(9) -0.0018(8) 0.0081(10) O2 0.0139(11) 0.0173(11) 0.0222(11) -0.0004(9) 0.0013(9) 0.0029(10) O3 0.0204(11) 0.0153(11) 0.0192(10) -0.0005(8) 0.0015(9) 0.0049(9) O4 0.0134(10) 0.0181(11) 0.0207(11) 0.0012(9) 0.0014(8) 0.0028(9) O5 0.0288(15) 0.0240(14) 0.091(3) 0.0039(15) 0.0250(16) 0.0085(13) O6 0.0343(16) 0.072(2) 0.0244(15) -0.0085(14) 0.0095(12) 0.0058(16) O7 0.066(2) 0.080(2) 0.0464(19) -0.0211(17) -0.0191(16) 0.061(2) O8 0.0381(15) 0.0274(13) 0.0328(14) 0.0023(11) -0.0013(11) 0.0213(12) O9 0.0465(17) 0.0215(13) 0.0403(17) 0.0007(12) -0.0072(13) 0.0068(13) O10 0.0358(14) 0.0308(14) 0.0252(13) -0.0067(10) -0.0001(11) 0.0159(12) O12 0.063(2) 0.0543(19) 0.0344(16) -0.0114(14) -0.0181(14) 0.0403(17) N1 0.0121(12) 0.0245(14) 0.0141(12) -0.0025(10) -0.0002(9) 0.0069(11) N2 0.0151(12) 0.0161(12) 0.0199(13) 0.0013(10) -0.0008(10) 0.0072(11) N3 0.0219(14) 0.0161(13) 0.0169(13) -0.0022(10) -0.0027(10) 0.0073(11) N4 0.0167(13) 0.0183(13) 0.0140(12) -0.0028(10) -0.0008(10) 0.0047(11) C1 0.0198(15) 0.0258(16) 0.0141(14) -0.0014(12) 0.0009(12) 0.0126(13) C2 0.0195(16) 0.0336(19) 0.0226(17) 0.0000(14) -0.0006(13) 0.0152(15) C3 0.0169(16) 0.036(2) 0.0282(18) -0.0052(15) -0.0027(13) 0.0076(15) C4 0.0233(17) 0.0225(17) 0.0306(18) -0.0030(14) 0.0009(14) 0.0071(14) C5 0.0211(15) 0.0223(16) 0.0181(15) -0.0006(12) 0.0006(12) 0.0099(13) C6 0.0240(16) 0.0227(16) 0.0217(16) -0.0063(13) -0.0053(13) 0.0128(13) C7 0.0227(16) 0.0186(16) 0.0346(19) -0.0038(13) -0.0109(14) 0.0083(14) C8 0.0180(16) 0.0257(18) 0.036(2) 0.0102(15) -0.0017(14) 0.0038(14) C9 0.0220(17) 0.0310(19) 0.0214(16) 0.0060(14) 0.0027(13) 0.0083(15) C10 0.0192(15) 0.0244(16) 0.0184(15) 0.0015(13) 0.0012(12) 0.0110(14) C11 0.040(2) 0.0216(17) 0.0303(19) -0.0065(14) 0.0112(16) 0.0096(16) C12 0.051(3) 0.0207(18) 0.040(2) -0.0076(16) 0.002(2) 0.0056(18) C13 0.035(2) 0.0208(18) 0.037(2) 0.0020(15) -0.0036(17) 0.0008(16) C14 0.0236(19) 0.0293(19) 0.045(2) 0.0093(17) 0.0013(16) 0.0098(16) C15 0.0220(17) 0.0260(18) 0.0294(19) 0.0031(14) -0.0012(14) 0.0124(15) C16 0.0221(17) 0.0307(18) 0.0170(15) -0.0011(13) 0.0018(12) 0.0128(15) C17 0.0226(18) 0.053(3) 0.0256(19) -0.0071(17) -0.0018(14) 0.0149(18) C18 0.0194(19) 0.061(3) 0.034(2) -0.006(2) 0.0026(16) -0.001(2) C19 0.032(2) 0.034(2) 0.036(2) 0.0068(17) 0.0085(18) -0.0077(18) C20 0.0289(19) 0.0203(17) 0.0247(17) 0.0056(13) 0.0011(14) 0.0019(15) O11 0.0361(16) 0.0476(18) 0.0461(18) 0.0000(14) 0.0147(13) 0.0204(15) _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 O1 2.471(2) . ? Ag1 O1 2.471(2) 3 ? Ag1 O1 2.472(2) 2 ? Ag1 O4 2.504(2) 2_556 ? Ag1 O4 2.504(2) 3_556 ? Ag1 O4 2.504(2) 1_556 ? Ag2 O1 2.192(2) . ? Ag2 O2 2.275(2) 3 ? Ag2 O5 2.521(3) . ? Ag2 O2 2.534(2) . ? Ag2 Ag2 3.0187(4) 2 ? Ag2 Ag2 3.0187(4) 3 ? Ag3 O3 2.475(2) 3 ? Ag3 O3 2.475(2) . ? Ag3 O3 2.475(2) 2 ? Ag3 O2 2.515(2) . ? Ag3 O2 2.515(2) 3 ? Ag3 O2 2.515(2) 2 ? Ag4 O4 2.464(2) 3 ? Ag4 O4 2.464(2) 2 ? Ag4 O4 2.464(2) . ? Ag4 O3 2.490(2) 3 ? Ag4 O3 2.490(2) 2 ? Ag4 O3 2.490(2) . ? Cl1 O6 1.422(3) . ? Cl1 O7 1.432(3) . ? Cl1 O5 1.443(3) . ? Cl1 O8 1.449(3) . ? Cl2 O12 1.433(3) . ? Cl2 O9 1.433(3) . ? Cl2 O11 1.438(3) . ? Cl2 O10 1.440(3) . ? O1 N1 1.354(3) . ? O2 N2 1.346(3) . ? O2 Ag2 2.275(2) 2 ? O3 N3 1.335(3) . ? O4 N4 1.335(3) . ? O4 Ag1 2.504(2) 1_554 ? N1 C1 1.346(4) . ? N1 C5 1.348(4) . ? N2 C10 1.349(4) . ? N2 C6 1.349(4) . ? N3 C15 1.339(5) . ? N3 C11 1.346(4) . ? N4 C16 1.352(4) . ? N4 C20 1.353(4) . ? C1 C2 1.387(5) . ? C1 H1 0.9500 . ? C2 C3 1.377(5) . ? C2 H2 0.9500 . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 C9 1.377(5) . ? C8 H8 0.9500 . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.374(5) . ? C11 H11 0.9500 . ? C12 C13 1.360(6) . ? C12 H12 0.9500 . ? C13 C14 1.372(6) . ? C13 H13 0.9500 . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.371(5) . ? C16 H16 0.9500 . ? C17 C18 1.375(7) . ? C17 H17 0.9500 . ? C18 C19 1.364(7) . ? C18 H18 0.9500 . ? C19 C20 1.380(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? 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 O1 Ag1 O1 81.92(8) . 3 ? O1 Ag1 O1 81.92(8) . 2 ? O1 Ag1 O1 81.92(8) 3 2 ? O1 Ag1 O4 88.41(7) . 2_556 ? O1 Ag1 O4 153.91(8) 3 2_556 ? O1 Ag1 O4 120.76(8) 2 2_556 ? O1 Ag1 O4 153.91(8) . 3_556 ? O1 Ag1 O4 120.76(8) 3 3_556 ? O1 Ag1 O4 88.41(7) 2 3_556 ? O4 Ag1 O4 75.80(8) 2_556 3_556 ? O1 Ag1 O4 120.76(8) . 1_556 ? O1 Ag1 O4 88.42(7) 3 1_556 ? O1 Ag1 O4 153.91(8) 2 1_556 ? O4 Ag1 O4 75.80(8) 2_556 1_556 ? O4 Ag1 O4 75.80(8) 3_556 1_556 ? O1 Ag2 O2 143.95(9) . 3 ? O1 Ag2 O5 105.90(11) . . ? O2 Ag2 O5 90.97(10) 3 . ? O1 Ag2 O2 125.07(9) . . ? O2 Ag2 O2 79.48(11) 3 . ? O5 Ag2 O2 103.14(9) . . ? O1 Ag2 Ag2 88.64(7) . 2 ? O2 Ag2 Ag2 93.11(6) 3 2 ? O5 Ag2 Ag2 148.52(7) . 2 ? O2 Ag2 Ag2 47.38(5) . 2 ? O1 Ag2 Ag2 96.16(6) . 3 ? O2 Ag2 Ag2 55.04(6) 3 3 ? O5 Ag2 Ag2 141.97(7) . 3 ? O2 Ag2 Ag2 88.13(5) . 3 ? Ag2 Ag2 Ag2 60.0 2 3 ? O3 Ag3 O3 78.50(8) 3 . ? O3 Ag3 O3 78.50(8) 3 2 ? O3 Ag3 O3 78.50(8) . 2 ? O3 Ag3 O2 102.08(8) 3 . ? O3 Ag3 O2 103.90(7) . . ? O3 Ag3 O2 177.60(8) 2 . ? O3 Ag3 O2 103.90(7) 3 3 ? O3 Ag3 O2 177.60(8) . 3 ? O3 Ag3 O2 102.08(7) 2 3 ? O2 Ag3 O2 75.52(8) . 3 ? O3 Ag3 O2 177.60(8) 3 2 ? O3 Ag3 O2 102.08(7) . 2 ? O3 Ag3 O2 103.90(7) 2 2 ? O2 Ag3 O2 75.52(8) . 2 ? O2 Ag3 O2 75.52(8) 3 2 ? O4 Ag4 O4 77.28(8) 3 2 ? O4 Ag4 O4 77.28(8) 3 . ? O4 Ag4 O4 77.28(8) 2 . ? O4 Ag4 O3 154.69(8) 3 3 ? O4 Ag4 O3 90.05(7) 2 3 ? O4 Ag4 O3 121.62(8) . 3 ? O4 Ag4 O3 121.61(8) 3 2 ? O4 Ag4 O3 154.69(8) 2 2 ? O4 Ag4 O3 90.05(7) . 2 ? O3 Ag4 O3 77.94(8) 3 2 ? O4 Ag4 O3 90.05(7) 3 . ? O4 Ag4 O3 121.62(8) 2 . ? O4 Ag4 O3 154.69(8) . . ? O3 Ag4 O3 77.94(8) 3 . ? O3 Ag4 O3 77.94(8) 2 . ? O6 Cl1 O7 109.7(2) . . ? O6 Cl1 O5 108.6(2) . . ? O7 Cl1 O5 109.4(2) . . ? O6 Cl1 O8 110.6(2) . . ? O7 Cl1 O8 110.28(18) . . ? O5 Cl1 O8 108.24(16) . . ? O12 Cl2 O9 109.94(19) . . ? O12 Cl2 O11 110.3(2) . . ? O9 Cl2 O11 108.9(2) . . ? O12 Cl2 O10 109.00(18) . . ? O9 Cl2 O10 108.78(17) . . ? O11 Cl2 O10 109.88(18) . . ? N1 O1 Ag2 113.05(17) . . ? N1 O1 Ag1 113.40(17) . . ? Ag2 O1 Ag1 126.57(10) . . ? N2 O2 Ag2 120.00(18) . 2 ? N2 O2 Ag3 123.05(19) . . ? Ag2 O2 Ag3 106.20(9) 2 . ? N2 O2 Ag2 121.07(18) . . ? Ag2 O2 Ag2 77.57(7) 2 . ? Ag3 O2 Ag2 98.79(8) . . ? N3 O3 Ag3 117.18(18) . . ? N3 O3 Ag4 117.99(18) . . ? Ag3 O3 Ag4 86.50(7) . . ? N4 O4 Ag4 111.44(17) . . ? N4 O4 Ag1 118.53(18) . 1_554 ? Ag4 O4 Ag1 88.68(7) . 1_554 ? Cl1 O5 Ag2 108.66(15) . . ? C1 N1 C5 122.9(3) . . ? C1 N1 O1 118.9(3) . . ? C5 N1 O1 118.2(3) . . ? O2 N2 C10 117.5(3) . . ? O2 N2 C6 120.8(3) . . ? C10 N2 C6 121.7(3) . . ? O3 N3 C15 120.8(3) . . ? O3 N3 C11 118.8(3) . . ? C15 N3 C11 120.4(3) . . ? O4 N4 C16 119.9(3) . . ? O4 N4 C20 119.0(3) . . ? C16 N4 C20 121.1(3) . . ? N1 C1 C2 118.8(3) . . ? N1 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 119.2(3) . . ? N1 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N2 C6 C7 119.9(3) . . ? N2 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 119.5(3) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 119.5(3) . . ? N2 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N3 C11 C12 120.3(4) . . ? N3 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.5(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N3 C15 C14 120.4(4) . . ? N3 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N4 C16 C17 120.2(4) . . ? N4 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 118.8(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.1(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? N4 C20 C19 118.9(4) . . ? N4 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.763 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 965105' ####################################################################### # # 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_3rpu156-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 Ag Cl N3 O8' _chemical_formula_weight 508.62 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' Cl Cl 0.1484 0.1585 '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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' _cell_length_a 13.3014(3) _cell_length_b 13.3014(3) _cell_length_c 5.9918(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 918.09(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(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 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6120 _exptl_absorpt_correction_T_max 0.7899 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22378 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0094 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.43 _reflns_number_total 767 _reflns_number_gt 680 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+3.0616P] 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 767 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _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 0.0000 0.0000 0.5000 0.0287(2) Uani 1 6 d S . . Cl1 Cl -0.3333 0.3333 0.7500 0.0587(8) Uani 1 6 d S . . O1 O -0.0713(3) 0.0997(3) 0.7500 0.0369(9) Uani 1 2 d S . . O2 O -0.3333 0.3333 0.522(3) 0.245(12) Uani 1 3 d S . . O3 O -0.3283(10) 0.2269(9) 0.7500 0.152(4) Uani 1 2 d S . . N1 N -0.0132(5) 0.2150(4) 0.7500 0.0394(11) Uani 1 2 d S . . C1 C -0.0756(8) 0.2705(6) 0.7500 0.0536(18) Uani 1 2 d S . . H1 H -0.1580 0.2267 0.7500 0.064 Uiso 1 2 calc SR . . C2 C -0.0207(10) 0.3882(7) 0.7500 0.071(3) Uani 1 2 d S . . H2 H -0.0642 0.4271 0.7500 0.085 Uiso 1 2 calc SR . . C3 C 0.0972(12) 0.4500(7) 0.7500 0.082(3) Uani 1 2 d S . . H3 H 0.1361 0.5324 0.7500 0.098 Uiso 1 2 calc SR . . C4 C 0.1618(8) 0.3932(6) 0.7500 0.063(2) Uani 1 2 d S . . H4 H 0.2442 0.4362 0.7500 0.075 Uiso 1 2 calc SR . . C5 C 0.1029(6) 0.2731(5) 0.7500 0.0447(14) Uani 1 2 d S . . H5 H 0.1446 0.2323 0.7500 0.054 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0218(2) 0.0218(2) 0.0424(4) 0.000 0.000 0.01092(12) Cl1 0.0549(10) 0.0549(10) 0.066(2) 0.000 0.000 0.0274(5) O1 0.038(2) 0.0255(17) 0.052(2) 0.000 0.000 0.0192(16) O2 0.304(19) 0.304(19) 0.126(15) 0.000 0.000 0.152(9) O3 0.177(10) 0.117(7) 0.207(12) 0.000 0.000 0.106(8) N1 0.060(3) 0.027(2) 0.039(3) 0.000 0.000 0.028(2) C1 0.095(6) 0.053(4) 0.040(3) 0.000 0.000 0.058(4) C2 0.128(8) 0.048(4) 0.058(5) 0.000 0.000 0.061(5) C3 0.177(11) 0.031(3) 0.047(4) 0.000 0.000 0.060(6) C4 0.093(6) 0.028(3) 0.045(4) 0.000 0.000 0.013(3) C5 0.061(4) 0.026(3) 0.043(3) 0.000 0.000 0.018(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 O1 2.482(3) 7_556 ? Ag1 O1 2.482(3) . ? Ag1 O1 2.482(3) 9_556 ? Ag1 O1 2.482(3) 3 ? Ag1 O1 2.482(3) 8_557 ? Ag1 O1 2.482(3) 2_554 ? Ag1 Ag1 2.99589(10) 2 ? Ag1 Ag1 2.99589(10) 2_554 ? Cl1 O2 1.366(17) 8_457 ? Cl1 O2 1.366(17) . ? Cl1 O3 1.451(9) . ? Cl1 O3 1.451(9) 3_565 ? Cl1 O3 1.451(9) 8_457 ? O1 N1 1.328(6) . ? O1 Ag1 2.482(3) 2 ? N1 C5 1.337(9) . ? N1 C1 1.359(8) . ? C1 C2 1.357(11) . ? C1 H1 0.9500 . ? C2 C3 1.359(15) . ? C2 H2 0.9500 . ? C3 C4 1.398(13) . ? C3 H3 0.9500 . ? C4 C5 1.384(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? 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 O1 Ag1 O1 180.00(16) 7_556 . ? O1 Ag1 O1 87.33(7) 7_556 9_556 ? O1 Ag1 O1 92.67(7) . 9_556 ? O1 Ag1 O1 92.67(7) 7_556 3 ? O1 Ag1 O1 87.33(7) . 3 ? O1 Ag1 O1 180.00(15) 9_556 3 ? O1 Ag1 O1 92.67(7) 7_556 8_557 ? O1 Ag1 O1 87.33(7) . 8_557 ? O1 Ag1 O1 92.67(7) 9_556 8_557 ? O1 Ag1 O1 87.33(7) 3 8_557 ? O1 Ag1 O1 87.33(7) 7_556 2_554 ? O1 Ag1 O1 92.67(7) . 2_554 ? O1 Ag1 O1 87.33(7) 9_556 2_554 ? O1 Ag1 O1 92.67(7) 3 2_554 ? O1 Ag1 O1 180.00(13) 8_557 2_554 ? O1 Ag1 Ag1 127.13(5) 7_556 2 ? O1 Ag1 Ag1 52.87(5) . 2 ? O1 Ag1 Ag1 127.13(5) 9_556 2 ? O1 Ag1 Ag1 52.87(5) 3 2 ? O1 Ag1 Ag1 52.87(5) 8_557 2 ? O1 Ag1 Ag1 127.13(5) 2_554 2 ? O1 Ag1 Ag1 52.87(5) 7_556 2_554 ? O1 Ag1 Ag1 127.13(5) . 2_554 ? O1 Ag1 Ag1 52.87(5) 9_556 2_554 ? O1 Ag1 Ag1 127.13(5) 3 2_554 ? O1 Ag1 Ag1 127.13(5) 8_557 2_554 ? O1 Ag1 Ag1 52.87(5) 2_554 2_554 ? Ag1 Ag1 Ag1 180.0 2 2_554 ? O2 Cl1 O2 179.998(1) 8_457 . ? O2 Cl1 O3 90.002(2) 8_457 . ? O2 Cl1 O3 90.000(2) . . ? O2 Cl1 O3 90.000(5) 8_457 3_565 ? O2 Cl1 O3 90.000(6) . 3_565 ? O3 Cl1 O3 120.001(2) . 3_565 ? O2 Cl1 O3 89.998(4) 8_457 8_457 ? O2 Cl1 O3 90.000(4) . 8_457 ? O3 Cl1 O3 119.999(1) . 8_457 ? O3 Cl1 O3 120.000(1) 3_565 8_457 ? N1 O1 Ag1 117.4(2) . . ? N1 O1 Ag1 117.4(2) . 2 ? Ag1 O1 Ag1 74.26(10) . 2 ? O1 N1 C5 120.3(5) . . ? O1 N1 C1 117.8(6) . . ? C5 N1 C1 121.9(6) . . ? C2 C1 N1 120.3(9) . . ? C2 C1 H1 119.9 . . ? N1 C1 H1 119.9 . . ? C1 C2 C3 119.4(8) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 120.6(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.5(9) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 119.4(7) . . ? N1 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.874 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 965106' ####################################################################### # # 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_3rpu142 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Ag2 F6 N2 O8 S2' _chemical_formula_weight 704.10 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.26718(8) _cell_length_b 10.26639(13) _cell_length_c 11.74637(13) _cell_angle_alpha 86.5046(10) _cell_angle_beta 81.1991(9) _cell_angle_gamma 88.2690(9) _cell_volume 983.172(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.901 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 148021 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _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 2.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4516 _reflns_number_gt 4140 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+1.6210P] 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 4520 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _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 0.11033(2) 0.885213(16) 0.089435(14) 0.01608(5) Uani 1 1 d . . . Ag2 Ag 0.38475(2) 1.072407(16) -0.085811(14) 0.01883(5) Uani 1 1 d . . . F1 F -0.2939(2) 0.74049(17) 0.51287(12) 0.0325(4) Uani 1 1 d . . . F2 F -0.2996(2) 0.58429(16) 0.40056(15) 0.0368(4) Uani 1 1 d . . . F3 F -0.07575(19) 0.62545(16) 0.46127(12) 0.0299(3) Uani 1 1 d . . . F4 F 0.2964(2) 0.58396(18) -0.21747(16) 0.0406(4) Uani 1 1 d . . . F5 F 0.4904(2) 0.51091(15) -0.12739(14) 0.0372(4) Uani 1 1 d . . . F6 F 0.5407(2) 0.64993(19) -0.27028(14) 0.0419(4) Uani 1 1 d . . . O1 O 0.11326(19) 1.11106(15) 0.01791(13) 0.0168(3) Uani 1 1 d . . . O2 O 0.6611(2) 1.07046(16) -0.17961(14) 0.0212(3) Uani 1 1 d . . . O3 O -0.3108(2) 0.8343(2) 0.27111(17) 0.0352(5) Uani 1 1 d . . . O4 O -0.0665(3) 0.89278(19) 0.3458(2) 0.0395(5) Uani 1 1 d . . . O5 O -0.0530(2) 0.71491(19) 0.21916(15) 0.0300(4) Uani 1 1 d . . . O6 O 0.5446(2) 0.76760(19) -0.04478(17) 0.0293(4) Uani 1 1 d . . . O7 O 0.3333(3) 0.85499(18) -0.15225(19) 0.0355(5) Uani 1 1 d . . . N1 N 0.0982(2) 1.20540(17) 0.09417(16) 0.0140(3) Uani 1 1 d . . . N2 N 0.6701(2) 1.1256(2) -0.28636(17) 0.0212(4) Uani 1 1 d . . . S1 S -0.15413(7) 0.79360(6) 0.30104(5) 0.01985(12) Uani 1 1 d . . . S2 S 0.38975(7) 0.74813(5) -0.08160(5) 0.01864(11) Uani 1 1 d . . . C1 C 0.0605(3) 1.1727(2) 0.20780(19) 0.0184(4) Uani 1 1 d . . . H1 H 0.0435 1.0840 0.2337 0.022 Uiso 1 1 calc R . . C2 C 0.0466(3) 1.2680(2) 0.2861(2) 0.0223(5) Uani 1 1 d . . . H2 H 0.0214 1.2453 0.3663 0.027 Uiso 1 1 calc R . . C3 C 0.0695(3) 1.3974(2) 0.2476(2) 0.0235(5) Uani 1 1 d . . . H3 H 0.0604 1.4640 0.3010 0.028 Uiso 1 1 calc R . . C4 C 0.1057(3) 1.4283(2) 0.1305(2) 0.0227(5) Uani 1 1 d . . . H4 H 0.1204 1.5166 0.1027 0.027 Uiso 1 1 calc R . . C5 C 0.1203(3) 1.3300(2) 0.0543(2) 0.0185(4) Uani 1 1 d . . . H5 H 0.1459 1.3504 -0.0263 0.022 Uiso 1 1 calc R . . C6 C 0.6746(4) 1.0492(4) -0.3748(3) 0.0421(8) Uani 1 1 d . . . H6 H 0.6709 0.9570 -0.3624 0.050 Uiso 1 1 calc R . . C7 C 0.6850(4) 1.1084(6) -0.4862(3) 0.0698(15) Uani 1 1 d . . . H7 H 0.6905 1.0566 -0.5511 0.084 Uiso 1 1 calc R . . C8 C 0.6871(4) 1.2431(6) -0.5008(3) 0.0682(15) Uani 1 1 d . . . H8 H 0.6922 1.2844 -0.5758 0.082 Uiso 1 1 calc R . . C9 C 0.6820(4) 1.3161(4) -0.4080(3) 0.0529(10) Uani 1 1 d . . . H9 H 0.6843 1.4086 -0.4179 0.063 Uiso 1 1 calc R . . C10 C 0.6733(3) 1.2562(3) -0.2999(3) 0.0303(6) Uani 1 1 d . . . H10 H 0.6696 1.3071 -0.2346 0.036 Uiso 1 1 calc R . . C11 C -0.2094(3) 0.6799(2) 0.42525(19) 0.0194(4) Uani 1 1 d . . . C12 C 0.4314(3) 0.6157(2) -0.1790(2) 0.0224(5) Uani 1 1 d . . . O8 O 0.2645(2) 0.69530(17) 0.00674(16) 0.0295(4) 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 Ag1 0.01575(9) 0.01619(8) 0.01671(8) -0.00080(6) -0.00386(6) -0.00016(6) Ag2 0.01785(9) 0.01994(9) 0.01822(9) 0.00015(6) -0.00167(7) -0.00063(6) F1 0.0316(8) 0.0462(10) 0.0171(7) -0.0018(6) 0.0030(6) 0.0081(7) F2 0.0449(10) 0.0285(8) 0.0377(9) 0.0072(7) -0.0082(8) -0.0180(7) F3 0.0314(8) 0.0366(8) 0.0217(7) 0.0043(6) -0.0086(6) 0.0115(7) F4 0.0280(8) 0.0479(10) 0.0518(11) -0.0235(8) -0.0165(8) 0.0002(7) F5 0.0533(11) 0.0242(8) 0.0351(9) -0.0078(6) -0.0110(8) 0.0168(7) F6 0.0394(10) 0.0589(12) 0.0243(8) -0.0069(8) 0.0073(7) -0.0040(8) O1 0.0191(8) 0.0161(7) 0.0159(7) -0.0043(6) -0.0035(6) -0.0015(6) O2 0.0187(8) 0.0249(8) 0.0205(8) 0.0037(6) -0.0063(7) -0.0025(6) O3 0.0204(9) 0.0514(12) 0.0300(10) 0.0200(9) -0.0021(8) 0.0073(8) O4 0.0350(11) 0.0246(10) 0.0571(14) -0.0017(9) 0.0000(10) -0.0110(8) O5 0.0319(10) 0.0356(10) 0.0191(8) 0.0031(7) 0.0032(7) 0.0087(8) O6 0.0191(9) 0.0343(10) 0.0372(10) -0.0140(8) -0.0082(8) 0.0003(7) O7 0.0402(11) 0.0190(9) 0.0497(12) 0.0046(8) -0.0178(10) 0.0012(8) N1 0.0124(8) 0.0141(8) 0.0166(9) -0.0032(7) -0.0039(7) -0.0016(6) N2 0.0133(9) 0.0306(11) 0.0192(9) 0.0006(8) -0.0031(8) 0.0031(8) S1 0.0165(3) 0.0204(3) 0.0205(3) 0.0068(2) 0.0004(2) 0.0012(2) S2 0.0150(3) 0.0154(2) 0.0256(3) -0.0019(2) -0.0029(2) -0.00045(19) C1 0.0168(11) 0.0194(11) 0.0189(11) -0.0004(8) -0.0021(9) -0.0023(8) C2 0.0194(11) 0.0264(12) 0.0215(11) -0.0053(9) -0.0026(9) 0.0001(9) C3 0.0182(11) 0.0232(12) 0.0307(13) -0.0120(10) -0.0055(10) 0.0015(9) C4 0.0196(11) 0.0151(10) 0.0346(13) -0.0026(9) -0.0078(10) -0.0001(8) C5 0.0161(10) 0.0184(10) 0.0210(11) 0.0014(8) -0.0035(9) -0.0011(8) C6 0.0341(16) 0.062(2) 0.0343(15) -0.0230(14) -0.0151(13) 0.0247(14) C7 0.0342(18) 0.150(5) 0.0272(16) -0.031(2) -0.0092(14) 0.039(2) C8 0.0215(16) 0.134(4) 0.040(2) 0.041(2) 0.0032(14) 0.015(2) C9 0.0266(16) 0.075(3) 0.054(2) 0.0401(19) -0.0112(15) -0.0091(15) C10 0.0191(12) 0.0284(13) 0.0430(15) 0.0138(11) -0.0087(11) -0.0054(10) C11 0.0205(11) 0.0220(11) 0.0154(10) 0.0012(8) -0.0030(9) -0.0005(9) C12 0.0204(11) 0.0277(12) 0.0201(11) -0.0031(9) -0.0059(9) 0.0015(9) O8 0.0275(10) 0.0220(9) 0.0352(10) -0.0080(7) 0.0100(8) -0.0034(7) _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 O2 2.3714(16) 2_675 ? Ag1 O1 2.3899(15) 2_575 ? Ag1 O1 2.4170(15) . ? Ag1 O8 2.4639(17) . ? Ag1 O5 2.5279(19) . ? Ag2 O2 2.3798(17) . ? Ag2 O1 2.4182(16) . ? Ag2 O6 2.4558(18) 2_675 ? Ag2 O7 2.4787(19) . ? Ag2 O3 2.4794(18) 2_575 ? Ag2 Ag2 3.2472(3) 2_675 ? F1 C11 1.329(3) . ? F2 C11 1.323(3) . ? F3 C11 1.337(3) . ? F4 C12 1.323(3) . ? F5 C12 1.320(3) . ? F6 C12 1.329(3) . ? O1 N1 1.349(2) . ? O1 Ag1 2.3898(15) 2_575 ? O2 N2 1.336(2) . ? O2 Ag1 2.3714(16) 2_675 ? O3 S1 1.4366(18) . ? O3 Ag2 2.4794(18) 2_575 ? O4 S1 1.437(2) . ? O5 S1 1.4438(19) . ? O6 S2 1.4360(18) . ? O6 Ag2 2.4558(17) 2_675 ? O7 S2 1.4445(19) . ? N1 C5 1.343(3) . ? N1 C1 1.347(3) . ? N2 C6 1.335(3) . ? N2 C10 1.341(3) . ? S1 C11 1.822(2) . ? S2 O8 1.4422(19) . ? S2 C12 1.821(2) . ? C1 C2 1.373(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.401(5) . ? C6 H6 0.9500 . ? C7 C8 1.384(7) . ? C7 H7 0.9500 . ? C8 C9 1.354(7) . ? C8 H8 0.9500 . ? C9 C10 1.370(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 O2 Ag1 O1 167.42(5) 2_675 2_575 ? O2 Ag1 O1 87.69(5) 2_675 . ? O1 Ag1 O1 79.76(6) 2_575 . ? O2 Ag1 O8 88.32(6) 2_675 . ? O1 Ag1 O8 98.97(6) 2_575 . ? O1 Ag1 O8 129.53(6) . . ? O2 Ag1 O5 106.48(6) 2_675 . ? O1 Ag1 O5 84.58(6) 2_575 . ? O1 Ag1 O5 144.57(6) . . ? O8 Ag1 O5 84.10(6) . . ? O2 Ag2 O1 170.33(5) . . ? O2 Ag2 O6 89.52(6) . 2_675 ? O1 Ag2 O6 81.80(5) . 2_675 ? O2 Ag2 O7 92.63(7) . . ? O1 Ag2 O7 97.01(6) . . ? O6 Ag2 O7 157.62(7) 2_675 . ? O2 Ag2 O3 86.80(6) . 2_575 ? O1 Ag2 O3 93.06(6) . 2_575 ? O6 Ag2 O3 115.29(7) 2_675 2_575 ? O7 Ag2 O3 87.07(7) . 2_575 ? O2 Ag2 Ag2 70.82(4) . 2_675 ? O1 Ag2 Ag2 110.00(4) . 2_675 ? O6 Ag2 Ag2 71.57(5) 2_675 2_675 ? O7 Ag2 Ag2 88.13(4) . 2_675 ? O3 Ag2 Ag2 156.86(4) 2_575 2_675 ? N1 O1 Ag1 112.19(11) . 2_575 ? N1 O1 Ag1 118.95(12) . . ? Ag1 O1 Ag1 100.24(6) 2_575 . ? N1 O1 Ag2 116.41(12) . . ? Ag1 O1 Ag2 117.45(6) 2_575 . ? Ag1 O1 Ag2 88.73(5) . . ? N2 O2 Ag1 113.14(13) . 2_675 ? N2 O2 Ag2 110.07(12) . . ? Ag1 O2 Ag2 124.44(7) 2_675 . ? S1 O3 Ag2 130.22(11) . 2_575 ? S1 O5 Ag1 102.21(10) . . ? S2 O6 Ag2 128.75(11) . 2_675 ? S2 O7 Ag2 113.27(11) . . ? C5 N1 C1 121.72(19) . . ? C5 N1 O1 118.82(18) . . ? C1 N1 O1 119.46(18) . . ? C6 N2 O2 119.0(2) . . ? C6 N2 C10 122.7(3) . . ? O2 N2 C10 118.3(2) . . ? O3 S1 O4 115.24(13) . . ? O3 S1 O5 115.76(12) . . ? O4 S1 O5 113.86(13) . . ? O3 S1 C11 102.61(11) . . ? O4 S1 C11 103.56(12) . . ? O5 S1 C11 103.41(11) . . ? O6 S2 O8 115.14(12) . . ? O6 S2 O7 114.87(12) . . ? O8 S2 O7 113.94(12) . . ? O6 S2 C12 103.89(11) . . ? O8 S2 C12 102.79(11) . . ? O7 S2 C12 104.12(12) . . ? N1 C1 C2 119.8(2) . . ? N1 C1 H1 120.1 . . ? C2 C1 H1 120.1 . . ? C1 C2 C3 119.8(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 119.9(2) . . ? N1 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? N2 C6 C7 118.4(4) . . ? N2 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C8 C7 C6 119.2(4) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 120.0(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 119.9(3) . . ? N2 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? F2 C11 F1 107.9(2) . . ? F2 C11 F3 107.46(19) . . ? F1 C11 F3 107.77(18) . . ? F2 C11 S1 111.67(16) . . ? F1 C11 S1 110.94(16) . . ? F3 C11 S1 110.96(16) . . ? F5 C12 F4 108.6(2) . . ? F5 C12 F6 107.4(2) . . ? F4 C12 F6 107.4(2) . . ? F5 C12 S2 111.41(16) . . ? F4 C12 S2 110.68(17) . . ? F6 C12 S2 111.22(18) . . ? S2 O8 Ag1 105.76(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.717 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.085 #===END _database_code_depnum_ccdc_archive 'CCDC 965107'