# 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_[agl](pf6) _database_code_depnum_ccdc_archive 'CCDC 926373' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 Ag N12 O8 P4, F6 P, 0.37(C4 O), 0.63(C2 N)' _chemical_formula_sum 'C42.75 H32 Ag F6 N12.63 O8.37 P5' _chemical_formula_weight 1233.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.1835(3) _cell_length_b 31.5719(9) _cell_length_c 14.7373(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.6320(10) _cell_angle_gamma 90.00 _cell_volume 5201.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 78(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2450 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 78(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 'CCD Area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15541 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.39 _reflns_number_total 9377 _reflns_number_gt 8772 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The Flack parameter is reported from the penultimate cycle of refinment. In the final cycle, inversion twinning was introduced, leading to a final value of the minor twin component of 0.205(15) and to the final refinment statistics and parameters reported herein. ; _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^)+(0.0244P)^2^+13.1432P] 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 0.00 _refine_ls_number_reflns 9377 _refine_ls_number_parameters 752 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.109 _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 C74 C -0.1423(5) 0.07779(18) 0.7934(4) 0.0423(13) Uani 1 1 d . . . H74 H -0.1999 0.0577 0.8069 0.051 Uiso 1 1 calc R . . C33 C 0.5934(6) 0.03391(18) 1.0576(5) 0.0570(19) Uani 1 1 d . . . H33 H 0.6316 0.0177 1.1025 0.068 Uiso 1 1 calc R . . C53 C 0.0002(7) 0.0467(2) 1.0015(5) 0.0667(19) Uani 1 1 d U . . H53 H -0.0428 0.0320 0.9567 0.080 Uiso 1 1 calc R . . C52 C 0.1024(6) 0.0705(2) 0.9789(4) 0.0505(15) Uani 1 1 d U . . H52 H 0.1294 0.0720 0.9199 0.061 Uiso 1 1 calc R . . C54 C -0.0344(6) 0.0453(2) 1.0887(4) 0.0542(15) Uani 1 1 d U . . H54 H -0.1007 0.0294 1.1042 0.065 Uiso 1 1 calc R . . C84 C 0.0592(4) 0.34877(15) 0.7656(3) 0.0284(10) Uani 1 1 d . . . H84 H 0.0516 0.3769 0.7474 0.034 Uiso 1 1 calc R . . C83 C 0.0593(4) 0.31623(15) 0.7019(3) 0.0274(10) Uani 1 1 d . . . H83 H 0.0515 0.3224 0.6403 0.033 Uiso 1 1 calc R . . C85 C 0.0705(4) 0.33842(14) 0.8564(3) 0.0252(9) Uani 1 1 d . . . H85 H 0.0688 0.3601 0.8991 0.030 Uiso 1 1 calc R . . Ag1 Ag 0.59670(2) 0.218912(9) 0.53546(2) 0.02288(8) Uani 1 1 d . . . P1 P 0.41688(9) 0.20116(3) 0.75796(7) 0.0170(2) Uani 1 1 d . . . P4 P 0.18058(9) 0.19158(3) 0.82087(7) 0.0159(2) Uani 1 1 d . . . P2 P 0.51317(9) 0.17593(3) 0.93605(7) 0.0169(2) Uani 1 1 d . . . P3 P 0.27073(9) 0.15901(3) 0.99086(7) 0.0161(2) Uani 1 1 d . . . P5 P 0.76024(13) 0.04705(4) 0.35136(9) 0.0338(3) Uani 1 1 d . . . C24 C 0.3700(4) 0.33882(14) 0.5650(3) 0.0233(9) Uani 1 1 d . . . H24 H 0.3473 0.3608 0.5263 0.028 Uiso 1 1 calc R . . O4 O 0.6017(2) 0.21243(9) 0.97380(19) 0.0200(6) Uani 1 1 d . . . O8 O 0.0951(2) 0.22764(9) 0.86057(18) 0.0177(6) Uani 1 1 d . . . O7 O 0.1042(3) 0.16888(9) 0.74122(17) 0.0196(6) Uani 1 1 d . . . F1 F 0.6360(3) 0.06617(10) 0.3835(2) 0.0411(8) Uani 1 1 d . . . N46 N 0.4618(3) 0.26524(12) 0.9501(2) 0.0237(8) Uani 1 1 d . . . O3 O 0.6052(3) 0.13876(9) 0.9601(2) 0.0214(6) Uani 1 1 d . . . O1 O 0.4122(3) 0.17125(9) 0.66954(18) 0.0211(6) Uani 1 1 d . . . C13 C 0.5682(5) 0.06994(16) 0.6781(4) 0.0356(12) Uani 1 1 d . . . H13 H 0.5639 0.0434 0.7052 0.043 Uiso 1 1 calc R . . C21 C 0.4401(4) 0.27412(12) 0.6726(3) 0.0165(8) Uani 1 1 d . . . O5 O 0.2645(3) 0.11329(9) 1.03562(18) 0.0210(6) Uani 1 1 d . . . C42 C 0.6536(4) 0.28136(14) 1.0215(3) 0.0240(9) Uani 1 1 d . . . H42 H 0.7283 0.2716 1.0414 0.029 Uiso 1 1 calc R . . C71 C 0.0204(4) 0.13772(13) 0.7596(3) 0.0202(8) Uani 1 1 d . . . C12 C 0.4859(5) 0.10099(15) 0.6973(3) 0.0321(11) Uani 1 1 d . . . H12 H 0.4245 0.0959 0.7371 0.038 Uiso 1 1 calc R . . N16 N 0.5826(3) 0.14995(12) 0.5982(2) 0.0239(8) Uani 1 1 d . . . F3 F 0.6891(3) 0.00589(11) 0.3150(3) 0.0638(10) Uani 1 1 d . . . N1 N 0.4973(3) 0.17853(11) 0.8310(2) 0.0183(7) Uani 1 1 d . . . O2 O 0.4885(3) 0.24204(9) 0.72668(18) 0.0193(6) Uani 1 1 d . . . O6 O 0.1926(3) 0.18864(9) 1.05398(18) 0.0192(6) Uani 1 1 d . . . C64 C 0.2858(4) 0.24517(18) 1.2949(3) 0.0338(12) Uani 1 1 d . . . H64 H 0.3061 0.2595 1.3484 0.041 Uiso 1 1 calc R . . C45 C 0.4326(5) 0.30622(15) 0.9613(3) 0.0292(10) Uani 1 1 d . . . H45 H 0.3567 0.3149 0.9417 0.035 Uiso 1 1 calc R . . C22 C 0.3902(4) 0.30927(14) 0.7135(3) 0.0246(9) Uani 1 1 d . . . H22 H 0.3809 0.3105 0.7759 0.029 Uiso 1 1 calc R . . N3 N 0.2015(3) 0.15737(11) 0.8968(2) 0.0188(7) Uani 1 1 d . . . N4 N 0.2850(3) 0.21552(11) 0.7744(2) 0.0194(7) Uani 1 1 d . . . F4 F 0.8844(3) 0.02751(11) 0.3192(2) 0.0511(9) Uani 1 1 d . . . F6 F 0.8255(4) 0.08911(13) 0.3823(3) 0.0779(13) Uani 1 1 d . . . C44 C 0.5085(5) 0.33626(16) 1.0003(3) 0.0337(11) Uani 1 1 d . . . H44 H 0.4848 0.3643 1.0060 0.040 Uiso 1 1 calc R . . C11 C 0.4976(4) 0.14001(14) 0.6552(3) 0.0219(9) Uani 1 1 d . . . C25 C 0.4187(4) 0.30250(13) 0.5310(3) 0.0204(8) Uani 1 1 d . . . H25 H 0.4276 0.3003 0.4686 0.024 Uiso 1 1 calc R . . C15 C 0.6615(4) 0.11929(15) 0.5799(3) 0.0283(10) Uani 1 1 d . . . H15 H 0.7221 0.1253 0.5399 0.034 Uiso 1 1 calc R . . C23 C 0.3551(4) 0.34228(14) 0.6580(3) 0.0277(10) Uani 1 1 d . . . H23 H 0.3218 0.3666 0.6823 0.033 Uiso 1 1 calc R . . C61 C 0.2301(4) 0.20627(15) 1.1363(3) 0.0215(9) Uani 1 1 d . . . N2 N 0.4042(3) 0.17298(11) 1.0001(2) 0.0193(7) Uani 1 1 d . . . N26 N 0.4546(3) 0.26960(11) 0.5844(2) 0.0183(7) Uani 1 1 d . . . N56 N 0.1259(4) 0.09053(13) 1.1347(3) 0.0370(10) Uani 1 1 d . . . C41 C 0.5688(4) 0.25439(13) 0.9810(3) 0.0204(8) Uani 1 1 d . . . C43 C 0.6209(4) 0.32310(14) 1.0304(3) 0.0289(11) Uani 1 1 d . . . H43 H 0.6742 0.3425 1.0566 0.035 Uiso 1 1 calc R . . C62 C 0.2469(4) 0.18129(16) 1.2128(3) 0.0277(10) Uani 1 1 d . . . H62 H 0.2400 0.1520 1.2098 0.033 Uiso 1 1 calc R . . C63 C 0.2746(4) 0.20187(18) 1.2949(3) 0.0324(11) Uani 1 1 d . . . H63 H 0.2851 0.1865 1.3484 0.039 Uiso 1 1 calc R . . C14 C 0.6575(5) 0.07907(15) 0.6175(3) 0.0299(10) Uani 1 1 d . . . H14 H 0.7134 0.0586 0.6025 0.036 Uiso 1 1 calc R . . N36 N 0.4814(4) 0.08231(13) 0.9214(3) 0.0331(9) Uani 1 1 d . . . F5 F 0.7818(4) 0.02587(15) 0.4471(2) 0.0738(13) Uani 1 1 d . . . C55 C 0.0274(6) 0.0671(2) 1.1527(4) 0.0499(15) Uani 1 1 d U . . H55 H 0.0016 0.0661 1.2121 0.060 Uiso 1 1 calc R . . C35 C 0.4507(5) 0.04148(17) 0.9369(4) 0.0423(13) Uani 1 1 d . . . H35 H 0.3904 0.0295 0.9004 0.051 Uiso 1 1 calc R . . C31 C 0.5672(4) 0.09740(14) 0.9741(3) 0.0239(9) Uani 1 1 d . . . F2 F 0.7366(4) 0.06788(13) 0.2530(2) 0.0652(11) Uani 1 1 d . . . C34 C 0.5036(5) 0.01662(16) 1.0035(4) 0.0472(15) Uani 1 1 d . . . H34 H 0.4792 -0.0112 1.0118 0.057 Uiso 1 1 calc R . . C51 C 0.1587(4) 0.09116(14) 1.0493(3) 0.0271(10) Uani 1 1 d U . . C65 C 0.2668(4) 0.26742(16) 1.2146(3) 0.0295(10) Uani 1 1 d . . . H65 H 0.2746 0.2967 1.2154 0.035 Uiso 1 1 calc R . . C75 C -0.1570(5) 0.11985(18) 0.8172(3) 0.0376(12) Uani 1 1 d . . . H75 H -0.2270 0.1275 0.8456 0.045 Uiso 1 1 calc R . . N76 N -0.0759(4) 0.15024(12) 0.8018(3) 0.0279(8) Uani 1 1 d . . . C72 C 0.0437(5) 0.09723(15) 0.7315(3) 0.0362(12) Uani 1 1 d . . . H72 H 0.1135 0.0906 0.7016 0.043 Uiso 1 1 calc R . . C73 C -0.0410(6) 0.06655(17) 0.7495(4) 0.0487(15) Uani 1 1 d . . . H73 H -0.0290 0.0386 0.7319 0.058 Uiso 1 1 calc R . . C32 C 0.6259(5) 0.07564(18) 1.0442(4) 0.0440(14) Uani 1 1 d . . . H32 H 0.6846 0.0886 1.0806 0.053 Uiso 1 1 calc R . . N86 N 0.0841(3) 0.29829(11) 0.8859(2) 0.0200(7) Uani 1 1 d . . . N61 N 0.2375(3) 0.24810(13) 1.1352(2) 0.0247(8) Uani 1 1 d . . . C81 C 0.0850(4) 0.26784(13) 0.8231(3) 0.0180(8) Uani 1 1 d . . . C82 C 0.0709(4) 0.27488(14) 0.7307(3) 0.0235(9) Uani 1 1 d . . . H82 H 0.0694 0.2525 0.6895 0.028 Uiso 1 1 calc R . . C92A C 0.796(2) 0.4320(7) 0.8970(14) 0.075(4) Uani 0.373(11) 1 d PDU A 1 O9A O 0.7708(13) 0.4668(4) 0.8366(8) 0.074(4) Uani 0.373(11) 1 d PDU A 1 C93A C 0.730(2) 0.4367(8) 0.9817(15) 0.074(7) Uani 0.373(11) 1 d PDU A 1 C94A C 0.833(2) 0.4686(8) 0.7514(15) 0.074(4) Uani 0.373(11) 1 d PDU A 1 C95A C 0.787(3) 0.5036(9) 0.6950(17) 0.080(8) Uani 0.373(11) 1 d PDU A 1 N90D N 0.7605(16) 0.5150(5) 0.7103(13) 0.045(5) Uani 0.317(10) 1 d PDU B 2 C93D C 0.8916(12) 0.4488(4) 0.7265(9) 0.023(3) Uani 0.317(10) 1 d PDU B 2 C92D C 0.8173(11) 0.4862(4) 0.7222(9) 0.017(3) Uani 0.317(10) 1 d PDU B 2 C92B C 0.7375(16) 0.4252(6) 0.9438(15) 0.045(5) Uani 0.312(9) 1 d PDU C 3 C93B C 0.6385(19) 0.4526(7) 0.9591(17) 0.067(7) Uani 0.312(9) 1 d PDU C 3 N90B N 0.8131(16) 0.4022(6) 0.9455(14) 0.068(6) Uani 0.312(9) 1 d PDU C 3 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 C74 0.045(3) 0.044(3) 0.038(3) 0.005(2) -0.011(2) -0.023(3) C33 0.051(4) 0.039(3) 0.082(5) 0.027(3) 0.000(4) -0.003(3) C53 0.067(2) 0.066(2) 0.067(2) 0.0013(10) -0.0008(10) -0.0031(10) C52 0.0514(17) 0.0505(17) 0.0495(17) 0.0019(10) 0.0005(10) -0.0037(10) C54 0.0529(17) 0.0538(17) 0.0558(17) 0.0042(10) 0.0007(10) -0.0007(10) C84 0.032(3) 0.029(2) 0.024(2) 0.0060(18) 0.0018(19) -0.0018(19) C83 0.029(3) 0.036(3) 0.017(2) 0.0078(19) 0.0013(18) 0.003(2) C85 0.034(3) 0.024(2) 0.019(2) -0.0019(17) 0.0050(18) -0.0046(18) Ag1 0.03155(17) 0.02280(14) 0.01454(13) 0.00085(14) 0.00479(11) 0.00185(15) P1 0.0169(5) 0.0202(5) 0.0139(5) 0.0016(4) 0.0038(4) -0.0010(4) P4 0.0155(5) 0.0200(5) 0.0124(5) -0.0003(4) 0.0012(4) -0.0012(4) P2 0.0159(5) 0.0212(5) 0.0137(5) 0.0024(4) 0.0015(4) -0.0004(4) P3 0.0158(5) 0.0210(5) 0.0115(5) 0.0017(4) 0.0018(4) -0.0021(4) P5 0.0415(7) 0.0250(6) 0.0357(7) 0.0021(5) 0.0161(6) 0.0044(5) C24 0.021(2) 0.025(2) 0.024(2) 0.0070(17) 0.0017(18) 0.0029(18) O4 0.0159(14) 0.0230(15) 0.0211(15) 0.0009(11) 0.0001(12) -0.0010(11) O8 0.0200(15) 0.0191(14) 0.0142(14) -0.0002(11) 0.0044(11) -0.0005(11) O7 0.0219(15) 0.0263(15) 0.0107(13) -0.0019(11) -0.0005(11) -0.0038(12) F1 0.0450(19) 0.0313(16) 0.0479(19) 0.0037(14) 0.0151(15) 0.0103(14) N46 0.028(2) 0.0264(19) 0.0168(17) -0.0062(15) -0.0002(15) 0.0018(16) O3 0.0171(15) 0.0229(15) 0.0240(15) 0.0053(12) -0.0023(11) 0.0000(11) O1 0.0259(16) 0.0249(15) 0.0126(13) -0.0020(11) 0.0026(11) -0.0005(12) C13 0.053(3) 0.020(2) 0.034(3) 0.001(2) 0.009(2) 0.000(2) C21 0.0126(18) 0.021(2) 0.0165(19) 0.0010(15) 0.0027(15) -0.0039(15) O5 0.0210(15) 0.0234(15) 0.0186(14) 0.0052(12) 0.0017(12) -0.0041(12) C42 0.026(2) 0.028(2) 0.018(2) 0.0004(17) 0.0033(17) -0.0034(19) C71 0.022(2) 0.022(2) 0.016(2) 0.0019(16) -0.0048(16) -0.0047(17) C12 0.041(3) 0.027(2) 0.029(2) -0.0022(19) 0.012(2) -0.003(2) N16 0.027(2) 0.0260(19) 0.0184(17) 0.0014(14) 0.0014(15) -0.0002(15) F3 0.057(2) 0.0401(19) 0.095(3) -0.020(2) 0.012(2) 0.0008(17) N1 0.0146(17) 0.0256(18) 0.0151(16) 0.0030(14) 0.0044(13) 0.0028(14) O2 0.0168(14) 0.0255(15) 0.0160(14) 0.0020(11) 0.0045(11) -0.0007(12) O6 0.0173(15) 0.0269(15) 0.0134(13) -0.0010(11) 0.0002(11) 0.0006(12) C64 0.015(2) 0.062(4) 0.024(2) -0.012(2) 0.0006(18) 0.007(2) C45 0.034(3) 0.034(3) 0.020(2) -0.0012(19) 0.0016(19) 0.008(2) C22 0.030(2) 0.027(2) 0.017(2) -0.0010(17) 0.0059(17) 0.0017(18) N3 0.0193(18) 0.0215(17) 0.0154(16) 0.0003(14) -0.0005(14) -0.0018(14) N4 0.0180(18) 0.0241(18) 0.0162(17) 0.0046(14) -0.0008(14) -0.0011(14) F4 0.053(2) 0.0438(19) 0.058(2) 0.0075(16) 0.0325(17) 0.0107(15) F6 0.049(2) 0.056(2) 0.129(4) -0.038(3) 0.009(2) -0.0064(18) C44 0.052(3) 0.028(2) 0.022(2) -0.0030(19) 0.006(2) 0.000(2) C11 0.030(2) 0.021(2) 0.0147(19) -0.0037(16) 0.0025(17) -0.0014(17) C25 0.015(2) 0.028(2) 0.018(2) 0.0028(17) 0.0003(16) -0.0012(16) C15 0.032(3) 0.033(2) 0.020(2) 0.0004(18) 0.0007(19) 0.001(2) C23 0.029(2) 0.021(2) 0.033(3) 0.0004(19) 0.006(2) 0.0013(19) C61 0.012(2) 0.040(3) 0.0123(19) -0.0041(17) 0.0014(15) 0.0005(17) N2 0.0178(18) 0.0291(19) 0.0110(16) 0.0005(14) 0.0002(13) -0.0033(14) N26 0.0161(17) 0.0232(18) 0.0157(16) 0.0010(13) 0.0039(13) -0.0009(13) N56 0.033(2) 0.033(2) 0.046(3) 0.011(2) 0.015(2) -0.0015(18) C41 0.021(2) 0.025(2) 0.0155(19) 0.0001(16) 0.0052(16) -0.0006(17) C43 0.040(3) 0.029(2) 0.017(2) -0.004(2) 0.004(2) -0.009(2) C62 0.025(2) 0.040(3) 0.018(2) 0.0017(19) 0.0056(18) 0.001(2) C63 0.021(2) 0.058(3) 0.019(2) -0.002(2) 0.0021(18) 0.007(2) C14 0.039(3) 0.028(2) 0.023(2) -0.0091(19) 0.001(2) 0.001(2) N36 0.042(3) 0.035(2) 0.023(2) -0.0036(17) 0.0062(18) -0.0099(19) F5 0.066(3) 0.110(3) 0.046(2) 0.034(2) 0.0236(18) 0.044(2) C55 0.0494(17) 0.0495(17) 0.0510(17) 0.0033(10) 0.0038(10) -0.0001(10) C35 0.053(3) 0.038(3) 0.036(3) -0.013(2) 0.016(3) -0.016(3) C31 0.024(2) 0.022(2) 0.027(2) 0.0020(17) 0.0103(18) 0.0014(17) F2 0.078(3) 0.068(2) 0.051(2) 0.0208(19) 0.0257(19) 0.019(2) C34 0.052(4) 0.021(2) 0.069(4) 0.005(3) 0.019(3) -0.001(2) C51 0.0272(12) 0.0265(12) 0.0275(12) 0.0027(9) 0.0009(9) -0.0008(9) C65 0.017(2) 0.040(3) 0.032(3) -0.013(2) -0.0031(18) 0.0023(19) C75 0.029(3) 0.051(3) 0.032(3) 0.005(2) 0.001(2) -0.014(2) N76 0.027(2) 0.029(2) 0.027(2) 0.0009(16) 0.0024(16) -0.0019(16) C72 0.043(3) 0.029(3) 0.037(3) -0.008(2) 0.002(2) 0.000(2) C73 0.073(4) 0.023(3) 0.049(3) -0.005(2) -0.010(3) -0.013(3) C32 0.030(3) 0.045(3) 0.057(4) 0.027(3) -0.005(3) -0.007(2) N86 0.0226(18) 0.0208(17) 0.0165(17) -0.0005(14) 0.0021(14) -0.0028(14) N61 0.0186(19) 0.035(2) 0.0207(18) -0.0061(16) 0.0016(14) 0.0002(15) C81 0.016(2) 0.022(2) 0.0159(19) 0.0000(15) 0.0003(15) -0.0018(16) C82 0.023(2) 0.032(2) 0.015(2) -0.0048(17) -0.0014(17) 0.0015(18) C92A 0.075(4) 0.075(4) 0.075(4) -0.0003(8) 0.0020(8) -0.0002(8) O9A 0.074(4) 0.074(4) 0.075(4) -0.0005(7) 0.0020(7) -0.0003(7) C93A 0.074(7) 0.073(7) 0.074(7) 0.001(2) 0.003(2) -0.002(2) C94A 0.074(4) 0.074(4) 0.074(4) -0.0004(8) 0.0019(8) -0.0004(8) C95A 0.080(8) 0.081(8) 0.080(8) -0.001(2) 0.002(2) -0.002(2) N90D 0.044(5) 0.044(5) 0.048(5) -0.002(2) 0.001(2) 0.000(2) C93D 0.022(4) 0.023(4) 0.025(4) 0.0004(19) 0.0009(19) 0.0011(19) C92D 0.017(3) 0.016(3) 0.017(3) -0.0002(10) 0.0001(10) -0.0003(10) C92B 0.045(5) 0.045(5) 0.045(5) 0.0000(10) 0.0019(10) -0.0003(10) C93B 0.067(7) 0.067(7) 0.068(7) 0.000(2) 0.002(2) 0.000(2) N90B 0.068(6) 0.067(6) 0.069(6) 0.002(2) 0.004(2) 0.000(2) _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 C74 C73 1.368(9) . ? C74 C75 1.384(8) . ? C74 H74 0.9300 . ? C33 C34 1.377(9) . ? C33 C32 1.382(7) . ? C33 H33 0.9300 . ? C53 C54 1.352(9) . ? C53 C52 1.416(10) . ? C53 H53 0.9300 . ? C52 C51 1.364(8) . ? C52 H52 0.9300 . ? C54 C55 1.344(9) . ? C54 H54 0.9300 . ? C84 C85 1.380(6) . ? C84 C83 1.392(7) . ? C84 H84 0.9300 . ? C83 C82 1.377(6) . ? C83 H83 0.9300 . ? C85 N86 1.347(6) . ? C85 H85 0.9300 . ? Ag1 N86 2.270(3) 4_554 ? Ag1 N61 2.365(4) 4_554 ? Ag1 N16 2.372(4) . ? Ag1 N26 2.382(3) . ? P1 N1 1.557(3) . ? P1 N4 1.568(4) . ? P1 O2 1.594(3) . ? P1 O1 1.609(3) . ? P4 N4 1.565(3) . ? P4 N3 1.568(3) . ? P4 O7 1.602(3) . ? P4 O8 1.607(3) . ? P2 N1 1.556(3) . ? P2 N2 1.566(3) . ? P2 O3 1.594(3) . ? P2 O4 1.608(3) . ? P3 N2 1.559(4) . ? P3 N3 1.569(3) . ? P3 O5 1.589(3) . ? P3 O6 1.597(3) . ? P5 F5 1.574(4) . ? P5 F6 1.576(4) . ? P5 F1 1.599(3) . ? P5 F4 1.604(3) . ? P5 F2 1.607(4) . ? P5 F3 1.608(4) . ? C24 C25 1.370(6) . ? C24 C23 1.390(6) . ? C24 H24 0.9300 . ? O4 C41 1.380(5) . ? O8 C81 1.388(5) . ? O7 C71 1.390(5) . ? N46 C41 1.313(6) . ? N46 C45 1.346(6) . ? O3 C31 1.390(5) . ? O1 C11 1.393(5) . ? C13 C12 1.380(7) . ? C13 C14 1.389(7) . ? C13 H13 0.9300 . ? C21 N26 1.322(5) . ? C21 C22 1.388(6) . ? C21 O2 1.389(5) . ? O5 C51 1.393(5) . ? C42 C43 1.375(6) . ? C42 C41 1.396(6) . ? C42 H42 0.9300 . ? C71 N76 1.320(6) . ? C71 C72 1.371(6) . ? C12 C11 1.387(6) . ? C12 H12 0.9300 . ? N16 C11 1.325(6) . ? N16 C15 1.342(6) . ? O6 C61 1.388(5) . ? C64 C63 1.373(8) . ? C64 C65 1.388(7) . ? C64 H64 0.9300 . ? C45 C44 1.387(7) . ? C45 H45 0.9300 . ? C22 C23 1.375(6) . ? C22 H22 0.9300 . ? C44 C43 1.385(7) . ? C44 H44 0.9300 . ? C25 N26 1.357(5) . ? C25 H25 0.9300 . ? C15 C14 1.387(7) . ? C15 H15 0.9300 . ? C23 H23 0.9300 . ? C61 N61 1.323(6) . ? C61 C62 1.385(6) . ? N56 C51 1.321(6) . ? N56 C55 1.359(7) . ? C43 H43 0.9300 . ? C62 C63 1.400(6) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C14 H14 0.9300 . ? N36 C31 1.307(6) . ? N36 C35 1.355(7) . ? C55 H55 0.9300 . ? C35 C34 1.378(8) . ? C35 H35 0.9300 . ? C31 C32 1.391(7) . ? C34 H34 0.9300 . ? C65 N61 1.352(6) . ? C65 H65 0.9300 . ? C75 N76 1.344(6) . ? C75 H75 0.9300 . ? C72 C73 1.386(8) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C32 H32 0.9300 . ? N86 C81 1.335(5) . ? N86 Ag1 2.270(3) 4_455 ? N61 Ag1 2.365(4) 4_455 ? C81 C82 1.385(6) . ? C82 H82 0.9300 . ? C92A O9A 1.44(2) . ? C92A C93A 1.48(3) . ? O9A C94A 1.45(2) . ? C94A C95A 1.47(3) . ? N90D C92D 1.121(14) . ? C93D C92D 1.444(13) . ? C92B N90B 1.115(14) . ? C92B C93B 1.428(15) . ? 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 C73 C74 C75 118.4(5) . . ? C73 C74 H74 120.8 . . ? C75 C74 H74 120.8 . . ? C34 C33 C32 119.1(6) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C54 C53 C52 119.6(7) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C51 C52 C53 115.7(6) . . ? C51 C52 H52 122.1 . . ? C53 C52 H52 122.1 . . ? C55 C54 C53 119.7(7) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C85 C84 C83 118.5(4) . . ? C85 C84 H84 120.7 . . ? C83 C84 H84 120.7 . . ? C82 C83 C84 119.6(4) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? N86 C85 C84 122.8(4) . . ? N86 C85 H85 118.6 . . ? C84 C85 H85 118.6 . . ? N86 Ag1 N61 136.94(12) 4_554 4_554 ? N86 Ag1 N16 98.96(12) 4_554 . ? N61 Ag1 N16 102.26(13) 4_554 . ? N86 Ag1 N26 115.53(12) 4_554 . ? N61 Ag1 N26 87.38(12) 4_554 . ? N16 Ag1 N26 116.51(12) . . ? N1 P1 N4 123.60(18) . . ? N1 P1 O2 106.65(17) . . ? N4 P1 O2 107.04(17) . . ? N1 P1 O1 107.17(17) . . ? N4 P1 O1 106.62(18) . . ? O2 P1 O1 104.23(15) . . ? N4 P4 N3 123.15(19) . . ? N4 P4 O7 106.54(17) . . ? N3 P4 O7 106.30(17) . . ? N4 P4 O8 106.03(17) . . ? N3 P4 O8 107.83(16) . . ? O7 P4 O8 105.86(16) . . ? N1 P2 N2 122.34(19) . . ? N1 P2 O3 108.32(17) . . ? N2 P2 O3 109.32(18) . . ? N1 P2 O4 110.98(17) . . ? N2 P2 O4 108.43(17) . . ? O3 P2 O4 93.65(16) . . ? N2 P3 N3 122.27(18) . . ? N2 P3 O5 105.90(18) . . ? N3 P3 O5 108.08(17) . . ? N2 P3 O6 108.75(18) . . ? N3 P3 O6 105.64(17) . . ? O5 P3 O6 105.01(15) . . ? F5 P5 F6 92.4(3) . . ? F5 P5 F1 90.41(18) . . ? F6 P5 F1 89.7(2) . . ? F5 P5 F4 89.43(19) . . ? F6 P5 F4 90.7(2) . . ? F1 P5 F4 179.56(19) . . ? F5 P5 F2 178.9(3) . . ? F6 P5 F2 88.8(3) . . ? F1 P5 F2 89.47(19) . . ? F4 P5 F2 90.68(19) . . ? F5 P5 F3 91.0(3) . . ? F6 P5 F3 176.4(3) . . ? F1 P5 F3 88.74(19) . . ? F4 P5 F3 90.86(19) . . ? F2 P5 F3 87.9(2) . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C41 O4 P2 123.4(3) . . ? C81 O8 P4 123.1(2) . . ? C71 O7 P4 121.5(2) . . ? C41 N46 C45 115.5(4) . . ? C31 O3 P2 121.8(3) . . ? C11 O1 P1 122.1(3) . . ? C12 C13 C14 118.7(5) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N26 C21 C22 125.1(4) . . ? N26 C21 O2 115.4(3) . . ? C22 C21 O2 119.2(4) . . ? C51 O5 P3 124.3(3) . . ? C43 C42 C41 116.5(4) . . ? C43 C42 H42 121.7 . . ? C41 C42 H42 121.7 . . ? N76 C71 C72 125.9(4) . . ? N76 C71 O7 116.3(4) . . ? C72 C71 O7 117.7(4) . . ? C13 C12 C11 117.9(4) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C11 N16 C15 116.4(4) . . ? C11 N16 Ag1 121.4(3) . . ? C15 N16 Ag1 122.1(3) . . ? P2 N1 P1 139.4(2) . . ? C21 O2 P1 124.4(3) . . ? C61 O6 P3 126.0(3) . . ? C63 C64 C65 119.5(5) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? N46 C45 C44 124.1(5) . . ? N46 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C23 C22 C21 117.3(4) . . ? C23 C22 H22 121.3 . . ? C21 C22 H22 121.3 . . ? P4 N3 P3 131.9(2) . . ? P4 N4 P1 130.2(2) . . ? C43 C44 C45 117.9(4) . . ? C43 C44 H44 121.1 . . ? C45 C44 H44 121.1 . . ? N16 C11 C12 124.9(4) . . ? N16 C11 O1 115.8(4) . . ? C12 C11 O1 119.2(4) . . ? N26 C25 C24 122.9(4) . . ? N26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? N16 C15 C14 123.4(4) . . ? N16 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C22 C23 C24 119.1(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? N61 C61 C62 124.8(4) . . ? N61 C61 O6 114.0(4) . . ? C62 C61 O6 120.9(4) . . ? P3 N2 P2 136.4(2) . . ? C21 N26 C25 116.4(4) . . ? C21 N26 Ag1 118.2(3) . . ? C25 N26 Ag1 121.9(3) . . ? C51 N56 C55 116.3(5) . . ? N46 C41 O4 117.8(4) . . ? N46 C41 C42 126.2(4) . . ? O4 C41 C42 116.0(4) . . ? C42 C43 C44 119.9(4) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C61 C62 C63 117.5(5) . . ? C61 C62 H62 121.3 . . ? C63 C62 H62 121.3 . . ? C64 C63 C62 118.7(5) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C15 C14 C13 118.6(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C31 N36 C35 115.6(5) . . ? C54 C55 N56 123.0(6) . . ? C54 C55 H55 118.5 . . ? N56 C55 H55 118.5 . . ? N36 C35 C34 123.8(5) . . ? N36 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? N36 C31 O3 118.4(4) . . ? N36 C31 C32 125.8(4) . . ? O3 C31 C32 115.8(4) . . ? C33 C34 C35 118.6(5) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? N56 C51 C52 125.6(5) . . ? N56 C51 O5 113.9(4) . . ? C52 C51 O5 120.3(5) . . ? N61 C65 C64 122.5(5) . . ? N61 C65 H65 118.7 . . ? C64 C65 H65 118.7 . . ? N76 C75 C74 123.8(5) . . ? N76 C75 H75 118.1 . . ? C74 C75 H75 118.1 . . ? C71 N76 C75 115.5(4) . . ? C71 C72 C73 117.2(5) . . ? C71 C72 H72 121.4 . . ? C73 C72 H72 121.4 . . ? C74 C73 C72 119.3(5) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C33 C32 C31 117.1(5) . . ? C33 C32 H32 121.4 . . ? C31 C32 H32 121.4 . . ? C81 N86 C85 117.2(3) . . ? C81 N86 Ag1 120.0(3) . 4_455 ? C85 N86 Ag1 122.8(3) . 4_455 ? C61 N61 C65 117.0(4) . . ? C61 N61 Ag1 114.0(3) . 4_455 ? C65 N61 Ag1 118.7(3) . 4_455 ? N86 C81 C82 124.3(4) . . ? N86 C81 O8 112.7(3) . . ? C82 C81 O8 122.9(4) . . ? C83 C82 C81 117.5(4) . . ? C83 C82 H82 121.3 . . ? C81 C82 H82 121.3 . . ? O9A C92A C93A 110.6(16) . . ? C92A O9A C94A 118.4(18) . . ? O9A C94A C95A 110.7(17) . . ? N90D C92D C93D 173.5(18) . . ? N90B C92B C93B 169(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.678 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.077 data_2agtet_best _database_code_depnum_ccdc_archive 'CCDC 926374' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Ag N6 O4 P2, F6 P' _chemical_formula_sum 'C40 H32 Ag2 F12 N12 O8 P6' _chemical_formula_weight 1438.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.990(5) _cell_length_b 14.430(3) _cell_length_c 15.590(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.70(3) _cell_angle_gamma 90.00 _cell_volume 5621.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.504602 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14768 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5125 _reflns_number_gt 2456 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Atom N2 of the phosphazene is clearly disordered about the two-fold axis. Essentially in one conformation atom N2 is 'up" with respect to the phosphazene mean plane, and in the other conformation it is "down". Atom P2 of the phosphazene had markedly eccentric anisotropic displacement parmeters (ADPs) indicating a small twist of the phosphazene ring, that is amplified into clearly resolved disorder for one of the pyridyl rings. Atom N4, on the opposite side of the ring to atom N2, lies closely on the two-fold axis, as evidenced by markedly less eccentric ADPs compared to P2. The twist manifests itself into moderately eccentric ADPs for N5 and P1, and for one of the pyridyl rings attached to P1. There is disorder of the hexafluorophosphate anion. In addition there is clear evidence for a solvate species. Given this disorder, consideration was given to refinment in space group Cc, but the disorder present in space group C2/c is present in the Cc structure. A significant number of reflections of the class hkl h+k = 2n+1 have small but significant intensity as commonly observed when there is extensive disorder and the disorder may be less than fully stochastic. No evidence was found to suggest a doubling of one (or more axes). The final model adopted for the substituted tetraphosphazene moiety featured a tightly restrained tetraphosphazene core with a small twist of the ring about an axis approximately perpendicular to the crystallographic two-fold axis and passing through atom N2 and its two-fold related mate. Disorder was resolved for two of the four O-py substituents to the phosphazene phosphorus atoms. For the other two O-py substituents, as a consequence of the disorder of the phosphorus atoms, the P-O bonds are ~0.12 A shorter and longer than the expected value of 1.60 A at one phosphorus and vice versa at the other phosphorus. Coupled with disorder of the pyridyl rings is unresolved disorder of the Ag^+^ cation that leads to the illusion of slightly different environments for the Ag^+^ cations throughout the crystal. Thus, Ag is four-coordinated with N21-Ag-N41B approximately linear and Ag-N31 and Ag-N11 approximately perpendicular to each other and to the Ag-N21 and Ag-N41 bonds. An alternative coordination is constructed with N41A in place of N41B and N51 in place of N31. The final value for R1 (0.0703 for observed data) is compatible with the intrinsic quality of the data (R(int) = 0.069 and R(sigma) = 0.104), which showed quite pronounced drop off in intensity at moderate resolution (~0.95 A). The final value for wR2 (0.194) is rather high but reflects inadequacies in the model for disorder and the rather weak data that leaves R1 for all data to 0.85 A resolution with a value of 0.155. 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. ; # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.500 -0.085 0.250 184.1 46.2 2 0.500 0.084 0.750 184.0 46.1 3 1.000 0.415 0.250 184.1 46.2 4 0.000 0.584 0.750 184.0 46.1 _platon_squeeze_details ; PF6- molecules disordered over several sites and orientations were found in the unit cell. The contributions from these were removed using Platon / SQUEEZE. 46.1 electrons / cell were removed (0.66 PF6- = 46e-) and 184.0 A3 was left by the void. ; _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^)+(0.0923P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5125 _refine_ls_number_parameters 538 _refine_ls_number_restraints 909 _refine_ls_R_factor_all 0.1566 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.08776(3) 0.12828(5) 0.06165(5) 0.0783(4) Uani 1 1 d . . . P1 P 0.9618(4) -0.0474(5) 0.1733(7) 0.064(3) Uani 0.50 1 d PDU . . P2 P 0.94029(18) 0.1477(3) 0.1858(3) 0.0376(12) Uani 0.50 1 d PDU . . N1 N 0.9279(5) 0.0412(6) 0.1747(10) 0.045(3) Uani 0.50 1 d PDU . . N2 N 0.9772(3) 0.1765(7) 0.2624(7) 0.040(3) Uani 0.50 1 d PDU . . N4 N 1.0000 -0.0809(6) 0.2500 0.067(2) Uani 1 2 d SDU . . P4 P 1.0257(4) -0.0347(5) 0.3279(7) 0.054(2) Uani 0.50 1 d PDU . . P3 P 1.03297(18) 0.1548(3) 0.2995(4) 0.0410(14) Uani 0.50 1 d PDU . . N3 N 1.0561(5) 0.0587(6) 0.3143(11) 0.057(3) Uani 0.50 1 d PDU . . N21 N 1.0935(3) -0.0266(5) 0.0552(4) 0.0593(17) Uani 1 1 d U B . O2 O 1.0070(2) -0.0293(4) 0.0934(3) 0.0616(15) Uani 1 1 d U . . C15 C 0.8019(4) -0.1621(8) 0.0681(7) 0.094(3) Uani 1 1 d U . . H15 H 0.7856 -0.1794 0.0166 0.113 Uiso 1 1 calc R . . N11 N 0.8547(3) -0.1522(5) 0.0704(6) 0.075(2) Uani 1 1 d U . . O1 O 0.9305(3) -0.1220(4) 0.1403(5) 0.095(2) Uani 1 1 d U . . C23 C 1.1056(4) -0.2173(7) 0.0734(6) 0.076(2) Uani 1 1 d U . . H23 H 1.1095 -0.2811 0.0792 0.091 Uiso 1 1 calc R . . C11 C 0.8758(4) -0.1273(6) 0.1422(8) 0.075(2) Uani 1 1 d U . . C13 C 0.7944(4) -0.1199(6) 0.2148(6) 0.075(2) Uani 1 1 d U . . H13 H 0.7745 -0.1078 0.2636 0.089 Uiso 1 1 calc R . . C12 C 0.8485(4) -0.1102(6) 0.2170(6) 0.073(2) Uani 1 1 d U . . H12 H 0.8665 -0.0926 0.2670 0.088 Uiso 1 1 calc R . . C24 C 1.1474(4) -0.1639(7) 0.0463(6) 0.072(2) Uani 1 1 d U B . H24 H 1.1803 -0.1907 0.0341 0.087 Uiso 1 1 calc R . . C22 C 1.0560(4) -0.1736(7) 0.0924(6) 0.072(2) Uani 1 1 d U B . H22 H 1.0269 -0.2069 0.1125 0.087 Uiso 1 1 calc R . . O3 O 0.8870(3) 0.2093(6) 0.1933(6) 0.040(2) Uani 0.50 1 d PDU . 1 N31 N 0.8404(5) 0.1394(11) 0.3024(8) 0.039(3) Uani 0.50 1 d PDU A 1 C35 C 0.7921(6) 0.1092(12) 0.3274(9) 0.046(4) Uani 0.50 1 d PDU A 1 H35 H 0.7904 0.0812 0.3811 0.056 Uiso 0.50 1 calc PR A 1 C34 C 0.7444(6) 0.1157(11) 0.2808(10) 0.046(3) Uani 0.50 1 d PDU A 1 H34 H 0.7123 0.0934 0.3021 0.056 Uiso 0.50 1 calc PR A 1 C33 C 0.7474(6) 0.1565(11) 0.2020(9) 0.050(3) Uani 0.50 1 d PDU A 1 H33 H 0.7171 0.1596 0.1668 0.060 Uiso 0.50 1 calc PR A 1 C32 C 0.7931(7) 0.1916(14) 0.1755(13) 0.046(4) Uani 0.50 1 d PDU A 1 H32 H 0.7942 0.2249 0.1245 0.055 Uiso 0.50 1 calc PR A 1 C31 C 0.8409(7) 0.1782(11) 0.2252(10) 0.039(3) Uani 0.50 1 d PDU A 1 O5 O 1.0772(3) 0.2105(6) 0.2475(6) 0.040(2) Uani 0.50 1 d PDU . 2 N51 N 1.1450(5) 0.1443(11) 0.1736(9) 0.050(4) Uani 0.50 1 d PDU B 2 C55 C 1.1963(6) 0.1191(15) 0.1730(11) 0.059(4) Uani 0.50 1 d PDU B 2 H55 H 1.2093 0.0937 0.1225 0.070 Uiso 0.50 1 calc PR B 2 C51 C 1.1288(6) 0.1844(9) 0.2461(10) 0.043(3) Uani 0.50 1 d PDU . 2 C52 C 1.1638(6) 0.2008(11) 0.3163(10) 0.045(3) Uani 0.50 1 d PDU B 2 H52 H 1.1519 0.2333 0.3639 0.054 Uiso 0.50 1 calc PR B 2 C53 C 1.2142(8) 0.1692(14) 0.3141(14) 0.049(4) Uani 0.50 1 d PDU B 2 H53 H 1.2369 0.1754 0.3616 0.059 Uiso 0.50 1 calc PR B 2 C54 C 1.2316(7) 0.1279(12) 0.2412(10) 0.053(4) Uani 0.50 1 d PDU B 2 H54 H 1.2665 0.1062 0.2373 0.063 Uiso 0.50 1 calc PR B 2 C14 C 0.7691(5) -0.1477(7) 0.1405(7) 0.091(3) Uani 1 1 d U . . H14 H 0.7323 -0.1565 0.1378 0.110 Uiso 1 1 calc R . . C25 C 1.1400(4) -0.0717(6) 0.0375(5) 0.066(2) Uani 1 1 d U . . H25 H 1.1686 -0.0366 0.0179 0.080 Uiso 1 1 calc R B . C21 C 1.0536(4) -0.0812(7) 0.0798(5) 0.062(2) Uani 1 1 d U . . O4A O 0.9662(6) 0.2073(8) 0.1100(8) 0.037(2) Uani 0.50 1 d PDU . 1 N41A N 1.0461(6) 0.2752(9) 0.0717(11) 0.044(3) Uani 0.50 1 d PDU B 1 C41A C 0.9985(6) 0.2859(9) 0.1076(10) 0.043(2) Uani 0.50 1 d PDU B 1 C45A C 1.0777(6) 0.3521(10) 0.0676(11) 0.052(3) Uani 0.50 1 d PDU B 1 H45A H 1.1110 0.3467 0.0421 0.062 Uiso 0.50 1 calc PR B 1 C42A C 0.9802(5) 0.3665(10) 0.1386(9) 0.054(3) Uani 0.50 1 d PDU B 1 H42A H 0.9464 0.3702 0.1629 0.064 Uiso 0.50 1 calc PR B 1 C43A C 1.0117(6) 0.4420(10) 0.1338(10) 0.063(3) Uani 0.50 1 d PDU B 1 H43A H 0.9995 0.4989 0.1537 0.076 Uiso 0.50 1 calc PR B 1 C44A C 1.0634(6) 0.4348(11) 0.0984(12) 0.062(3) Uani 0.50 1 d PDU B 1 H44A H 1.0865 0.4854 0.0966 0.075 Uiso 0.50 1 calc PR B 1 O4B O 0.9650(7) 0.1789(8) 0.0967(8) 0.039(3) Uani 0.50 1 d PDU . 2 C45B C 1.0681(5) 0.3321(10) 0.0325(10) 0.047(3) Uani 0.50 1 d PDU B 2 H45B H 1.1026 0.3263 0.0113 0.056 Uiso 0.50 1 calc PR B 2 C41B C 0.9917(6) 0.2635(9) 0.0821(9) 0.043(3) Uani 0.50 1 d PDU B 2 N41B N 1.0409(6) 0.2522(9) 0.0527(11) 0.045(3) Uani 0.50 1 d PDU B 2 C42B C 0.9683(5) 0.3469(10) 0.0919(9) 0.052(3) Uani 0.50 1 d PDU B 2 H42B H 0.9335 0.3505 0.1123 0.063 Uiso 0.50 1 calc PR B 2 C43B C 0.9951(6) 0.4251(10) 0.0724(10) 0.060(3) Uani 0.50 1 d PDU B 2 H43B H 0.9791 0.4828 0.0791 0.072 Uiso 0.50 1 calc PR B 2 C44B C 1.0481(6) 0.4175(11) 0.0413(12) 0.059(3) Uani 0.50 1 d PDU B 2 H44B H 1.0681 0.4698 0.0277 0.071 Uiso 0.50 1 calc PR B 2 P90 P 0.31062(9) 0.05368(18) 0.52641(16) 0.0653(7) Uani 1 1 d DU . . F1 F 0.3318(6) -0.0441(7) 0.5402(8) 0.166(7) Uani 0.835(18) 1 d PU C 1 F2 F 0.3371(3) 0.0577(4) 0.4350(4) 0.114(2) Uani 1 1 d U C 1 F3 F 0.3629(3) 0.1019(10) 0.5673(6) 0.134(5) Uani 0.835(18) 1 d PU C 1 F4 F 0.2844(2) 0.0519(4) 0.6174(4) 0.110(2) Uani 1 1 d U C 1 F5 F 0.2563(4) 0.0221(8) 0.4828(7) 0.125(4) Uani 0.835(18) 1 d PU C 1 F6 F 0.2906(4) 0.1585(4) 0.5103(5) 0.080(3) Uani 0.835(18) 1 d PU C 1 F4A F 0.3693(9) 0.027(2) 0.550(3) 0.079(9) Uani 0.165(18) 1 d PDU C 2 F6A F 0.2996(13) -0.0538(16) 0.516(3) 0.079(9) Uani 0.165(18) 1 d PDU C 2 F3A F 0.3224(12) 0.1554(16) 0.539(3) 0.079(9) Uani 0.165(18) 1 d PDU C 2 F5A F 0.2516(9) 0.071(2) 0.506(3) 0.079(9) Uani 0.165(18) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0537(4) 0.0823(6) 0.1000(7) 0.0193(5) 0.0437(4) 0.0140(4) P1 0.081(5) 0.034(3) 0.078(4) -0.009(3) 0.059(3) -0.007(3) P2 0.040(2) 0.037(2) 0.037(3) 0.0071(19) 0.024(2) -0.008(2) N1 0.056(5) 0.024(5) 0.054(5) -0.010(5) 0.040(5) -0.012(4) N2 0.041(5) 0.046(5) 0.034(5) -0.012(4) 0.014(5) 0.006(4) N4 0.103(5) 0.041(4) 0.057(5) 0.000 0.035(4) 0.000 P4 0.075(5) 0.036(3) 0.052(4) 0.014(3) 0.048(3) 0.017(3) P3 0.036(2) 0.044(3) 0.044(3) -0.001(2) 0.028(3) 0.010(2) N3 0.065(6) 0.046(6) 0.062(6) 0.003(5) 0.035(5) 0.015(5) N21 0.069(4) 0.073(4) 0.037(3) 0.000(3) 0.024(3) 0.023(3) O2 0.071(3) 0.075(4) 0.039(3) -0.006(3) 0.025(3) 0.018(3) C15 0.094(5) 0.107(5) 0.083(5) 0.007(5) 0.032(4) 0.003(5) N11 0.078(4) 0.067(4) 0.082(5) 0.015(4) 0.045(4) 0.003(4) O1 0.092(4) 0.067(4) 0.127(5) -0.035(3) 0.048(4) 0.008(3) C23 0.088(5) 0.066(5) 0.072(5) -0.038(4) -0.002(4) 0.011(4) C11 0.082(4) 0.056(4) 0.088(5) 0.002(4) 0.042(4) 0.007(4) C13 0.088(5) 0.070(5) 0.067(5) 0.007(4) 0.037(4) 0.002(4) C12 0.086(5) 0.062(4) 0.071(5) 0.001(4) 0.032(4) 0.008(4) C24 0.076(5) 0.081(5) 0.060(4) -0.023(4) 0.011(4) 0.020(4) C22 0.085(5) 0.072(5) 0.060(5) -0.026(4) 0.003(4) 0.005(4) O3 0.033(4) 0.038(4) 0.048(5) 0.012(4) 0.014(4) 0.005(4) N31 0.037(5) 0.052(6) 0.027(6) -0.002(5) 0.011(5) -0.005(5) C35 0.040(6) 0.061(6) 0.038(6) 0.007(5) 0.013(5) -0.013(5) C34 0.044(5) 0.054(6) 0.041(6) 0.007(5) 0.009(5) -0.007(5) C33 0.049(6) 0.058(6) 0.044(6) 0.004(5) 0.008(5) -0.001(5) C32 0.047(6) 0.052(7) 0.038(6) 0.003(5) 0.010(5) 0.004(5) C31 0.040(5) 0.043(5) 0.035(5) -0.001(5) 0.013(5) 0.004(5) O5 0.037(4) 0.042(4) 0.042(5) 0.000(4) 0.011(4) 0.001(4) N51 0.046(6) 0.059(6) 0.045(6) 0.001(5) 0.004(5) 0.007(5) C55 0.057(7) 0.069(7) 0.051(7) -0.004(6) -0.003(6) 0.010(6) C51 0.042(5) 0.045(5) 0.042(5) 0.004(5) 0.006(5) -0.004(5) C52 0.045(6) 0.047(6) 0.044(6) -0.004(5) 0.002(5) -0.008(5) C53 0.049(6) 0.051(7) 0.046(6) -0.002(6) -0.003(5) 0.001(6) C54 0.048(6) 0.060(6) 0.050(6) -0.001(6) 0.000(5) 0.006(6) C14 0.092(5) 0.102(5) 0.080(5) 0.010(5) 0.037(4) 0.003(5) C25 0.076(4) 0.074(5) 0.049(4) -0.004(4) 0.022(4) 0.016(4) C21 0.075(4) 0.069(4) 0.043(4) -0.009(4) 0.012(3) 0.017(4) O4A 0.034(4) 0.044(5) 0.033(4) 0.008(4) 0.014(4) -0.001(4) N41A 0.042(4) 0.050(5) 0.040(5) 0.010(4) 0.013(4) 0.001(4) C41A 0.039(4) 0.049(4) 0.042(4) 0.010(4) 0.010(4) -0.001(4) C45A 0.046(4) 0.054(5) 0.055(5) 0.011(4) 0.008(4) -0.001(4) C42A 0.046(5) 0.058(5) 0.057(5) 0.005(5) 0.009(5) -0.001(4) C43A 0.056(5) 0.063(5) 0.070(6) -0.004(5) 0.007(5) 0.000(5) C44A 0.055(5) 0.064(5) 0.069(6) 0.002(5) 0.007(5) -0.006(5) O4B 0.038(4) 0.045(5) 0.035(4) 0.010(4) 0.013(4) 0.002(4) C45B 0.044(5) 0.046(5) 0.051(5) 0.007(5) 0.013(4) 0.003(4) C41B 0.039(4) 0.047(4) 0.043(5) 0.009(4) 0.013(4) 0.000(4) N41B 0.039(4) 0.050(5) 0.045(5) 0.011(4) 0.014(4) 0.001(4) C42B 0.046(5) 0.052(5) 0.059(5) 0.010(5) 0.018(5) 0.000(4) C43B 0.054(5) 0.057(5) 0.070(5) 0.011(5) 0.018(5) 0.008(4) C44B 0.053(5) 0.057(5) 0.067(5) 0.009(5) 0.016(5) -0.002(4) P90 0.0526(14) 0.0770(18) 0.0667(17) 0.0104(14) 0.0227(12) 0.0029(13) F1 0.191(12) 0.122(8) 0.188(11) 0.094(7) 0.119(10) 0.122(8) F2 0.140(5) 0.129(5) 0.075(4) 0.012(4) 0.055(4) 0.011(4) F3 0.074(5) 0.204(14) 0.122(7) -0.009(7) -0.022(5) -0.021(7) F4 0.122(5) 0.125(5) 0.084(4) 0.016(4) 0.061(4) 0.023(4) F5 0.094(6) 0.110(8) 0.171(9) -0.052(6) 0.009(5) -0.049(5) F6 0.089(6) 0.062(4) 0.089(6) 0.017(3) -0.002(4) -0.010(4) F4A 0.048(12) 0.085(17) 0.103(16) -0.017(11) -0.027(10) 0.013(10) F6A 0.048(12) 0.085(17) 0.103(16) -0.017(11) -0.027(10) 0.013(10) F3A 0.048(12) 0.085(17) 0.103(16) -0.017(11) -0.027(10) 0.013(10) F5A 0.048(12) 0.085(17) 0.103(16) -0.017(11) -0.027(10) 0.013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N41B 2.141(13) . ? Ag1 N21 2.242(7) . ? Ag1 N51 2.255(14) . ? Ag1 N41A 2.367(13) . ? Ag1 N11 2.549(7) 5_755 ? P1 O1 1.423(10) . ? P1 N1 1.535(10) . ? P1 N4 1.595(10) . ? P1 O2 1.712(14) . ? P2 N2 1.557(9) . ? P2 N1 1.576(9) . ? P2 O4B 1.592(11) . ? P2 O3 1.606(9) . ? P2 O4A 1.604(11) . ? N2 P3 1.534(9) . ? N4 P4 1.521(10) . ? P4 N3 1.564(10) . ? P3 N3 1.519(10) . ? P3 O5 1.597(9) . ? N21 C21 1.333(11) . ? N21 C25 1.362(10) . ? O2 C21 1.403(9) . ? C15 N11 1.328(12) . ? C15 C14 1.417(13) . ? C15 H15 0.9300 . ? N11 C11 1.282(12) . ? N11 Ag1 2.549(7) 5_755 ? O1 C11 1.370(11) . ? C23 C24 1.368(12) . ? C23 C22 1.426(12) . ? C23 H23 0.9300 . ? C11 C12 1.379(12) . ? C13 C12 1.361(13) . ? C13 C14 1.371(14) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? C24 C25 1.351(12) . ? C24 H24 0.9300 . ? C22 C21 1.348(12) . ? C22 H22 0.9300 . ? O3 C31 1.339(15) . ? N31 C31 1.329(15) . ? N31 C35 1.347(14) . ? C35 C34 1.390(16) . ? C35 H35 0.9300 . ? C34 C33 1.366(18) . ? C34 H34 0.9300 . ? C33 C32 1.32(2) . ? C33 H33 0.9300 . ? C32 C31 1.43(2) . ? C32 H32 0.9300 . ? O5 C51 1.344(15) . ? N51 C55 1.333(15) . ? N51 C51 1.336(15) . ? C55 C54 1.380(17) . ? C55 H55 0.9300 . ? C51 C52 1.41(2) . ? C52 C53 1.34(2) . ? C52 H52 0.9300 . ? C53 C54 1.360(19) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C14 H14 0.9300 . ? C25 H25 0.9300 . ? O4A C41A 1.393(13) . ? N41A C41A 1.331(16) . ? N41A C45A 1.364(15) . ? C41A C42A 1.342(15) . ? C45A C44A 1.337(17) . ? C45A H45A 0.9300 . ? C42A C43A 1.348(16) . ? C42A H42A 0.9300 . ? C43A C44A 1.415(16) . ? C43A H43A 0.9300 . ? C44A H44A 0.9300 . ? O4B C41B 1.411(13) . ? C45B C44B 1.338(17) . ? C45B N41B 1.377(15) . ? C45B H45B 0.9300 . ? C41B N41B 1.327(16) . ? C41B C42B 1.347(15) . ? C42B C43B 1.348(16) . ? C42B H42B 0.9300 . ? C43B C44B 1.422(16) . ? C43B H43B 0.9300 . ? C44B H44B 0.9300 . ? P90 F3A 1.51(2) . ? P90 F1 1.522(7) . ? P90 F5A 1.53(2) . ? P90 F4A 1.55(2) . ? P90 F4 1.570(6) . ? P90 F5 1.577(9) . ? P90 F2 1.580(6) . ? P90 F6A 1.58(2) . ? P90 F3 1.604(9) . ? P90 F6 1.611(7) . ? 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 N41B Ag1 N21 149.9(4) . . ? N41B Ag1 N51 107.8(6) . . ? N21 Ag1 N51 95.5(4) . . ? N41B Ag1 N41A 10.3(7) . . ? N21 Ag1 N41A 157.5(4) . . ? N51 Ag1 N41A 97.6(6) . . ? N41B Ag1 N11 98.5(4) . 5_755 ? N21 Ag1 N11 93.5(2) . 5_755 ? N51 Ag1 N11 104.6(4) . 5_755 ? N41A Ag1 N11 100.7(4) . 5_755 ? O1 P1 N1 109.5(8) . . ? O1 P1 N4 111.4(7) . . ? N1 P1 N4 124.6(9) . . ? O1 P1 O2 102.5(7) . . ? N1 P1 O2 104.5(8) . . ? N4 P1 O2 101.4(6) . . ? N2 P2 N1 117.3(7) . . ? N2 P2 O4B 111.2(8) . . ? N1 P2 O4B 105.0(8) . . ? N2 P2 O3 106.2(6) . . ? N1 P2 O3 112.7(6) . . ? O4B P2 O3 103.8(7) . . ? N2 P2 O4A 100.4(8) . . ? N1 P2 O4A 121.5(8) . . ? O3 P2 O4A 95.7(7) . . ? P1 N1 P2 134.9(8) . . ? P3 N2 P2 139.6(7) . . ? P4 N4 P1 135.1(6) . . ? N4 P4 N3 118.0(8) . . ? N3 P3 N2 125.9(7) . . ? N3 P3 O5 105.7(7) . . ? N2 P3 O5 109.7(6) . . ? P3 N3 P4 128.4(9) . . ? C21 N21 C25 114.8(8) . . ? C21 N21 Ag1 121.9(5) . . ? C25 N21 Ag1 122.7(6) . . ? C21 O2 P1 125.7(6) . . ? N11 C15 C14 123.1(11) . . ? N11 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C11 N11 C15 116.8(9) . . ? C11 N11 Ag1 115.9(6) . 5_755 ? C15 N11 Ag1 124.3(7) . 5_755 ? C11 O1 P1 125.4(7) . . ? C24 C23 C22 118.9(9) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? N11 C11 C12 125.9(10) . . ? N11 C11 O1 113.3(8) . . ? C12 C11 O1 120.7(11) . . ? C12 C13 C14 119.9(9) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C12 C11 117.4(10) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C25 C24 C23 118.8(9) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C21 C22 C23 116.5(9) . . ? C21 C22 H22 121.8 . . ? C23 C22 H22 121.8 . . ? C31 O3 P2 124.1(9) . . ? C31 N31 C35 114.6(13) . . ? N31 C35 C34 126.3(13) . . ? N31 C35 H35 116.8 . . ? C34 C35 H35 116.8 . . ? C33 C34 C35 116.3(14) . . ? C33 C34 H34 121.8 . . ? C35 C34 H34 121.8 . . ? C32 C33 C34 120.3(17) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C32 C31 119.9(16) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? N31 C31 O3 119.6(15) . . ? N31 C31 C32 122.2(14) . . ? O3 C31 C32 118.2(12) . . ? C51 O5 P3 122.5(8) . . ? C55 N51 C51 115.1(13) . . ? C55 N51 Ag1 124.5(9) . . ? C51 N51 Ag1 120.3(10) . . ? N51 C55 C54 125.2(14) . . ? N51 C55 H55 117.4 . . ? C54 C55 H55 117.4 . . ? N51 C51 O5 115.7(14) . . ? N51 C51 C52 122.6(14) . . ? O5 C51 C52 121.7(12) . . ? C53 C52 C51 119.8(16) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 118.7(17) . . ? C54 C53 H53 120.7 . . ? C52 C53 H53 120.7 . . ? C53 C54 C55 118.4(15) . . ? C53 C54 H54 120.8 . . ? C55 C54 H54 120.8 . . ? C13 C14 C15 116.8(11) . . ? C13 C14 H14 121.6 . . ? C15 C14 H14 121.6 . . ? C24 C25 N21 124.5(9) . . ? C24 C25 H25 117.7 . . ? N21 C25 H25 117.7 . . ? N21 C21 C22 126.4(8) . . ? N21 C21 O2 110.7(8) . . ? C22 C21 O2 122.9(9) . . ? C41A O4A P2 134.1(11) . . ? C41A N41A C45A 116.5(11) . . ? C41A N41A Ag1 121.9(9) . . ? C45A N41A Ag1 118.0(10) . . ? N41A C41A C42A 124.2(11) . . ? N41A C41A O4A 116.0(13) . . ? C42A C41A O4A 119.7(12) . . ? C44A C45A N41A 123.5(11) . . ? C44A C45A H45A 118.2 . . ? N41A C45A H45A 118.2 . . ? C41A C42A C43A 118.6(12) . . ? C41A C42A H42A 120.7 . . ? C43A C42A H42A 120.7 . . ? C42A C43A C44A 120.0(13) . . ? C42A C43A H43A 120.0 . . ? C44A C43A H43A 120.0 . . ? C45A C44A C43A 117.1(13) . . ? C45A C44A H44A 121.5 . . ? C43A C44A H44A 121.5 . . ? C41B O4B P2 125.1(10) . . ? C44B C45B N41B 124.1(11) . . ? C44B C45B H45B 117.9 . . ? N41B C45B H45B 117.9 . . ? N41B C41B C42B 123.7(11) . . ? N41B C41B O4B 113.0(12) . . ? C42B C41B O4B 123.2(12) . . ? C41B N41B C45B 116.0(11) . . ? C41B N41B Ag1 126.1(10) . . ? C45B N41B Ag1 116.3(10) . . ? C43B C42B C41B 120.3(12) . . ? C43B C42B H42B 119.8 . . ? C41B C42B H42B 119.8 . . ? C42B C43B C44B 118.7(12) . . ? C42B C43B H43B 120.7 . . ? C44B C43B H43B 120.7 . . ? C45B C44B C43B 117.2(12) . . ? C45B C44B H44B 121.4 . . ? C43B C44B H44B 121.4 . . ? F3A P90 F1 144.7(11) . . ? F3A P90 F5A 93.1(8) . . ? F1 P90 F5A 121.0(10) . . ? F3A P90 F4A 91.5(8) . . ? F1 P90 F4A 54.1(9) . . ? F5A P90 F4A 175.0(13) . . ? F3A P90 F4 88.9(15) . . ? F1 P90 F4 90.3(4) . . ? F5A P90 F4 77.2(17) . . ? F4A P90 F4 100.9(16) . . ? F3A P90 F5 120.2(12) . . ? F1 P90 F5 95.1(7) . . ? F4A P90 F5 146.5(11) . . ? F4 P90 F5 91.0(5) . . ? F3A P90 F2 89.9(15) . . ? F1 P90 F2 90.7(4) . . ? F5A P90 F2 102.7(17) . . ? F4A P90 F2 79.3(16) . . ? F4 P90 F2 178.8(4) . . ? F5 P90 F2 89.4(5) . . ? F3A P90 F6A 177.9(17) . . ? F5A P90 F6A 88.5(8) . . ? F4A P90 F6A 86.9(8) . . ? F4 P90 F6A 90.0(17) . . ? F5 P90 F6A 61.7(10) . . ? F2 P90 F6A 91.1(17) . . ? F3A P90 F3 50.9(11) . . ? F1 P90 F3 93.8(7) . . ? F5A P90 F3 142.3(11) . . ? F4 P90 F3 89.8(4) . . ? F5 P90 F3 171.1(6) . . ? F2 P90 F3 89.7(4) . . ? F6A P90 F3 127.2(9) . . ? F1 P90 F6 177.6(5) . . ? F5A P90 F6 61.1(11) . . ? F4A P90 F6 123.8(11) . . ? F4 P90 F6 91.4(4) . . ? F5 P90 F6 86.6(5) . . ? F2 P90 F6 87.6(3) . . ? F6A P90 F6 148.3(10) . . ? F3 P90 F6 84.5(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.682 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.097 data_[ag2l](otf)2 _database_code_depnum_ccdc_archive 'CCDC 926375' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 Ag2 F6 N12 O14 P4 S2' _chemical_formula_sum 'C42 H32 Ag2 F6 N12 O14 P4 S2' _chemical_formula_weight 1446.54 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8673(13) _cell_length_b 14.964(2) _cell_length_c 20.803(4) _cell_angle_alpha 103.983(6) _cell_angle_beta 96.807(6) _cell_angle_gamma 103.934(6) _cell_volume 2553.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 2826 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 29.16 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.590871 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15442 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9926 _reflns_number_gt 5823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One coordinated triflate ion is disordered, giving alternate positions for the weakly coordinated O atom. The disorder of this triflate appears to have propagated into the structure, leading to somewhat flattened atomic displacement ellipsoids. Since the disorder, except for the triflate ion, is not resolved, no attempt was made to create a disordered model. ; _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^)+(0.0852P)^2^+23.2992P] 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 9926 _refine_ls_number_parameters 861 _refine_ls_number_restraints 434 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 P1 P 0.6702(3) 0.0123(2) 0.15799(13) 0.0260(6) Uani 1 1 d . A . Ag1 Ag 0.83070(8) -0.13410(6) 0.32680(4) 0.0285(2) Uani 1 1 d . . . C72 C 0.3372(10) -0.0981(9) 0.3104(5) 0.032(3) Uani 1 1 d . . . H72 H 0.3001 -0.0449 0.3109 0.039 Uiso 1 1 calc R . . C2 C 0.7182(14) -0.4482(9) 0.3793(7) 0.047(3) Uani 1 1 d . . . C75 C 0.4568(11) -0.2499(9) 0.3075(6) 0.040(3) Uani 1 1 d . . . H75 H 0.4969 -0.3024 0.3054 0.048 Uiso 1 1 calc R . . C31 C 0.9131(10) -0.2062(8) 0.1663(5) 0.027(2) Uani 1 1 d . . . C32 C 0.9021(12) -0.2625(9) 0.1037(5) 0.036(3) Uani 1 1 d . . . H32 H 0.9630 -0.2408 0.0741 0.043 Uiso 1 1 calc R . . C33 C 0.7980(13) -0.3532(9) 0.0847(6) 0.043(3) Uani 1 1 d . . . H33 H 0.7856 -0.3939 0.0417 0.051 Uiso 1 1 calc R . . C34 C 0.7122(12) -0.3823(9) 0.1313(6) 0.040(3) Uani 1 1 d . . . H34 H 0.6418 -0.4432 0.1202 0.048 Uiso 1 1 calc R . . C35 C 0.7327(11) -0.3201(8) 0.1933(6) 0.035(3) Uani 1 1 d . . . H35 H 0.6749 -0.3404 0.2242 0.042 Uiso 1 1 calc R . . C73 C 0.2349(11) -0.1883(9) 0.3004(5) 0.039(3) Uani 1 1 d . . . H73 H 0.1262 -0.1971 0.2939 0.046 Uiso 1 1 calc R . . C55 C 1.1287(10) -0.0844(7) 0.4497(5) 0.023(2) Uani 1 1 d . . . H55 H 1.0986 -0.1507 0.4414 0.028 Uiso 1 1 calc R . . C53 C 1.3113(10) 0.0664(8) 0.5070(5) 0.027(2) Uani 1 1 d . . . H53 H 1.4041 0.1032 0.5370 0.032 Uiso 1 1 calc R . . C52 C 1.2190(10) 0.1102(8) 0.4754(5) 0.025(2) Uani 1 1 d . . . H52 H 1.2477 0.1763 0.4827 0.030 Uiso 1 1 calc R . . C51 C 1.0799(10) 0.0514(7) 0.4320(4) 0.021(2) Uani 1 1 d . . . C61 C 1.1057(11) 0.2865(8) 0.3554(6) 0.032(3) Uani 1 1 d . . . C62 C 1.0819(15) 0.3242(10) 0.4200(7) 0.051(3) Uani 1 1 d . . . H62 H 1.0605 0.2873 0.4497 0.061 Uiso 1 1 calc R . . C63 C 1.0929(16) 0.4222(11) 0.4369(8) 0.062(4) Uani 1 1 d . . . H63 H 1.0746 0.4515 0.4789 0.074 Uiso 1 1 calc R . . C65 C 1.1506(12) 0.4289(8) 0.3304(7) 0.040(3) Uani 1 1 d . . . H65 H 1.1739 0.4643 0.2999 0.048 Uiso 1 1 calc R . . N61 N 1.1391(9) 0.3342(6) 0.3108(5) 0.030(2) Uani 1 1 d . A . C71 C 0.4978(11) -0.0911(9) 0.3196(5) 0.030(3) Uani 1 1 d . . . C74 C 0.2944(11) -0.2641(9) 0.3001(6) 0.041(3) Uani 1 1 d . . . H74 H 0.2271 -0.3246 0.2950 0.049 Uiso 1 1 calc R . . C81 C 0.5371(11) 0.2020(9) 0.3720(6) 0.033(3) Uani 1 1 d . . . N81 N 0.6099(10) 0.1896(8) 0.4263(5) 0.039(2) Uani 1 1 d . . . C85 C 0.6263(12) 0.2567(9) 0.4838(6) 0.042(3) Uani 1 1 d . . . H85 H 0.6817 0.2511 0.5228 0.050 Uiso 1 1 calc R . . C84 C 0.5662(13) 0.3332(10) 0.4886(7) 0.050(3) Uani 1 1 d . . . H84 H 0.5761 0.3767 0.5302 0.060 Uiso 1 1 calc R . . C83 C 0.4906(13) 0.3451(9) 0.4308(7) 0.047(3) Uani 1 1 d . . . H83 H 0.4504 0.3975 0.4329 0.056 Uiso 1 1 calc R . . C21 C 0.6931(10) 0.1956(8) 0.1652(5) 0.028(2) Uani 1 1 d . A . N21 N 0.8135(9) 0.2720(7) 0.1921(5) 0.031(2) Uani 1 1 d . A . C25 C 0.7838(12) 0.3590(9) 0.2110(6) 0.038(3) Uani 1 1 d . . . H25 H 0.8674 0.4143 0.2294 0.046 Uiso 1 1 calc R . . C24 C 0.6307(12) 0.3654(9) 0.2030(6) 0.041(3) Uani 1 1 d . . . H24 H 0.6103 0.4247 0.2156 0.049 Uiso 1 1 calc R . . C23 C 0.5095(12) 0.2837(10) 0.1764(7) 0.048(3) Uani 1 1 d . . . H23 H 0.4057 0.2873 0.1715 0.057 Uiso 1 1 calc R . . C41 C 1.1345(10) 0.0648(8) 0.1289(5) 0.026(2) Uani 1 1 d . . . C42 C 1.1777(10) -0.0074(8) 0.0837(5) 0.029(2) Uani 1 1 d . . . H42 H 1.1851 -0.0639 0.0933 0.034 Uiso 1 1 calc R . . N41 N 1.1230(8) 0.1455(7) 0.1191(4) 0.028(2) Uani 1 1 d . A . F4 F 0.5902(8) -0.4701(6) 0.3307(4) 0.067(3) Uani 1 1 d . . . F6 F 0.7611(9) -0.5275(5) 0.3773(4) 0.062(2) Uani 1 1 d . . . F5 F 0.6734(9) -0.4214(7) 0.4380(4) 0.077(3) Uani 1 1 d . . . N2 N 0.9835(8) 0.0119(6) 0.2850(4) 0.0234(18) Uani 1 1 d . . . N31 N 0.8319(9) -0.2311(6) 0.2124(4) 0.0262(19) Uani 1 1 d . . . N51 N 1.0357(8) -0.0428(6) 0.4177(4) 0.0237(18) Uani 1 1 d . . . N4 N 0.5742(8) 0.0172(7) 0.2167(4) 0.032(2) Uani 1 1 d U . . N1 N 0.8113(8) -0.0353(7) 0.1582(4) 0.028(2) Uani 1 1 d . . . N3 N 0.8068(9) 0.1376(7) 0.3172(4) 0.029(2) Uani 1 1 d . . . C82 C 0.4750(11) 0.2788(8) 0.3699(6) 0.036(3) Uani 1 1 d . . . H82 H 0.4259 0.2847 0.3298 0.043 Uiso 1 1 calc R . . N71 N 0.5571(9) -0.1635(7) 0.3176(4) 0.033(2) Uani 1 1 d . . . C22 C 0.5383(11) 0.1976(8) 0.1571(6) 0.037(3) Uani 1 1 d . . . H22 H 0.4561 0.1415 0.1389 0.044 Uiso 1 1 calc R . . O1 O 0.5502(7) -0.0420(5) 0.0891(3) 0.0293(16) Uani 1 1 d D . . O7 O 0.6110(7) -0.0038(6) 0.3357(3) 0.0311(17) Uani 1 1 d . . . O8 O 0.5144(8) 0.1331(6) 0.3113(4) 0.039(2) Uani 1 1 d . . . O2 O 0.7388(7) 0.1129(5) 0.1447(3) 0.0280(16) Uani 1 1 d . . . O3 O 1.0199(7) -0.1146(5) 0.1863(3) 0.0253(15) Uani 1 1 d . . . O10 O 0.9188(9) -0.3973(6) 0.3063(4) 0.047(2) Uani 1 1 d . . . O6 O 1.1048(7) 0.1912(5) 0.3338(4) 0.0286(16) Uani 1 1 d . . . O5 O 0.9735(7) 0.0934(5) 0.4058(3) 0.0257(16) Uani 1 1 d . . . O4 O 1.1133(7) 0.0551(5) 0.1926(3) 0.0227(15) Uani 1 1 d . . . O9 O 0.8020(10) -0.2783(6) 0.3672(5) 0.053(2) Uani 1 1 d . . . P4 P 0.6334(3) 0.0714(2) 0.29288(14) 0.0302(6) Uani 1 1 d . . . P2 P 0.9693(3) -0.0195(2) 0.20675(12) 0.0224(6) Uani 1 1 d . . . P3 P 0.9587(3) 0.1049(2) 0.33168(13) 0.0238(6) Uani 1 1 d . . . Ag2 Ag 1.06884(8) 0.25454(6) 0.20020(4) 0.0330(2) Uani 1 1 d . . . S2 S 0.8774(3) -0.35410(19) 0.36869(15) 0.0326(6) Uani 1 1 d . . . C54 C 1.2681(11) -0.0308(9) 0.4946(5) 0.031(3) Uani 1 1 d . . . H54 H 1.3308 -0.0608 0.5159 0.037 Uiso 1 1 calc R . . C64 C 1.1296(14) 0.4765(10) 0.3936(8) 0.056(4) Uani 1 1 d . . . H64 H 1.1399 0.5420 0.4058 0.068 Uiso 1 1 calc R . . C43 C 1.2084(11) 0.0123(9) 0.0237(5) 0.037(3) Uani 1 1 d . . . H43 H 1.2388 -0.0316 -0.0083 0.044 Uiso 1 1 calc R . . C45 C 1.1530(11) 0.1635(9) 0.0604(5) 0.036(3) Uani 1 1 d . . . H45 H 1.1460 0.2212 0.0527 0.044 Uiso 1 1 calc R A . C44 C 1.1938(12) 0.0971(10) 0.0115(6) 0.041(3) Uani 1 1 d . A . H44 H 1.2112 0.1094 -0.0291 0.049 Uiso 1 1 calc R . . O11 O 0.9937(9) -0.3327(5) 0.4278(4) 0.0370(18) Uani 1 1 d . . . N11A N 0.4721(17) -0.1895(11) 0.1164(7) 0.0324(13) Uani 0.546(6) 1 d PDU A 1 C11A C 0.474(2) -0.1376(10) 0.0727(12) 0.0322(13) Uani 0.546(6) 1 d PDU A 1 C15A C 0.396(2) -0.2838(13) 0.0900(9) 0.0325(13) Uani 0.546(6) 1 d PDU A 1 H15A H 0.3925 -0.3239 0.1180 0.039 Uiso 0.546(6) 1 calc PR A 1 C14A C 0.327(2) -0.3214(12) 0.0256(8) 0.0326(13) Uani 0.546(6) 1 d PDU A 1 H14A H 0.2731 -0.3862 0.0088 0.039 Uiso 0.546(6) 1 calc PR A 1 C13A C 0.337(2) -0.2611(13) -0.0157(9) 0.0325(13) Uani 0.546(6) 1 d PDU A 1 H13A H 0.2892 -0.2861 -0.0610 0.039 Uiso 0.546(6) 1 calc PR A 1 C12A C 0.415(2) -0.1657(13) 0.0084(9) 0.0323(13) Uani 0.546(6) 1 d PDU A 1 H12A H 0.4244 -0.1243 -0.0187 0.039 Uiso 0.546(6) 1 calc PR A 1 S1A S 1.2764(10) 0.4640(7) 0.1476(5) 0.0381(14) Uani 0.546(6) 1 d PDU A 1 O7A O 1.2344(17) 0.4037(11) 0.1899(8) 0.052(3) Uani 0.546(6) 1 d PD A 1 O8A O 1.3824(16) 0.5563(11) 0.1833(8) 0.057(5) Uani 0.546(6) 1 d PDU A 1 O6A O 1.313(2) 0.4204(16) 0.0858(9) 0.089(8) Uani 0.546(6) 1 d PDU A 1 C1A C 1.084(2) 0.4909(11) 0.1223(7) 0.044(4) Uani 0.546(6) 1 d PDU A 1 F1A F 1.0350(19) 0.5267(14) 0.1751(8) 0.061(6) Uani 0.546(6) 1 d PDU A 1 F2A F 0.9751(17) 0.4097(12) 0.0989(9) 0.102(6) Uani 0.546(6) 1 d PDU A 1 F3A F 1.094(2) 0.5347(17) 0.0767(9) 0.075(7) Uani 0.546(6) 1 d PDU A 1 S1B S 1.2525(12) 0.4601(8) 0.1337(6) 0.0383(14) Uani 0.454(6) 1 d PDU A 2 C1B C 1.1343(19) 0.5494(12) 0.1297(7) 0.044(4) Uani 0.454(6) 1 d PDU A 2 O7B O 1.1364(19) 0.3732(10) 0.1238(10) 0.052(3) Uani 0.454(6) 1 d PD A 2 O8B O 1.3442(18) 0.4978(13) 0.2022(7) 0.042(4) Uani 0.454(6) 1 d PDU A 2 O6B O 1.3423(17) 0.4674(12) 0.0831(7) 0.028(4) Uani 0.454(6) 1 d PDU A 2 F1B F 1.062(2) 0.5587(16) 0.1789(9) 0.062(7) Uani 0.454(6) 1 d PDU A 2 F2B F 1.2269(19) 0.6343(10) 0.1435(9) 0.067(5) Uani 0.454(6) 1 d PDU A 2 F3B F 1.052(3) 0.5236(18) 0.0689(8) 0.056(7) Uani 0.454(6) 1 d PDU A 2 C12B C 0.517(2) -0.2179(14) 0.0745(10) 0.0325(13) Uani 0.454(6) 1 d PDU A 2 H12B H 0.6087 -0.2074 0.1056 0.039 Uiso 0.454(6) 1 calc PR A 2 C11B C 0.471(3) -0.1447(11) 0.0606(12) 0.0322(13) Uani 0.454(6) 1 d PDU A 2 C13B C 0.425(2) -0.3083(14) 0.0412(11) 0.0327(13) Uani 0.454(6) 1 d PDU A 2 H13B H 0.4543 -0.3602 0.0506 0.039 Uiso 0.454(6) 1 calc PR A 2 C14B C 0.291(2) -0.3253(13) -0.0058(11) 0.0326(13) Uani 0.454(6) 1 d PDU A 2 H14B H 0.2309 -0.3871 -0.0300 0.039 Uiso 0.454(6) 1 calc PR A 2 C15B C 0.252(2) -0.2478(14) -0.0144(10) 0.0324(13) Uani 0.454(6) 1 d PDU A 2 H15B H 0.1577 -0.2567 -0.0431 0.039 Uiso 0.454(6) 1 calc PR A 2 N11B N 0.341(2) -0.1580(12) 0.0157(9) 0.0323(13) Uani 0.454(6) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0107(10) 0.0410(17) 0.0288(13) 0.0124(12) 0.0033(9) 0.0092(11) Ag1 0.0100(3) 0.0334(5) 0.0361(4) -0.0006(4) 0.0024(3) 0.0062(3) C72 0.011(4) 0.057(8) 0.033(6) 0.016(5) 0.006(4) 0.013(5) C2 0.035(6) 0.035(7) 0.068(9) 0.000(6) 0.030(6) 0.007(6) C75 0.015(5) 0.035(7) 0.057(7) -0.011(6) 0.002(5) 0.006(5) C31 0.015(4) 0.028(6) 0.035(6) 0.002(5) 0.002(4) 0.009(4) C32 0.028(5) 0.044(7) 0.030(6) 0.000(5) 0.007(4) 0.012(5) C33 0.038(6) 0.037(7) 0.040(7) -0.011(5) 0.004(5) 0.009(5) C34 0.024(5) 0.036(7) 0.047(7) -0.006(5) 0.001(5) 0.006(5) C35 0.015(5) 0.040(7) 0.039(6) 0.003(5) 0.003(4) -0.001(5) C73 0.009(4) 0.068(9) 0.037(6) 0.010(6) 0.009(4) 0.011(5) C55 0.023(5) 0.024(5) 0.031(5) 0.014(4) 0.013(4) 0.013(4) C53 0.013(4) 0.037(6) 0.025(5) 0.004(5) 0.001(4) 0.002(4) C52 0.014(4) 0.031(6) 0.025(5) 0.001(4) 0.006(4) 0.002(4) C51 0.012(4) 0.034(6) 0.015(4) 0.004(4) 0.004(3) 0.006(4) C61 0.017(5) 0.036(6) 0.042(6) -0.001(5) 0.006(4) 0.020(4) C62 0.053(8) 0.049(8) 0.058(8) 0.004(7) 0.028(6) 0.028(7) C63 0.059(9) 0.048(9) 0.079(10) -0.004(8) 0.024(8) 0.035(7) C65 0.023(5) 0.027(6) 0.070(8) 0.011(6) -0.007(5) 0.015(5) N61 0.014(4) 0.025(5) 0.050(6) 0.008(4) 0.001(4) 0.011(3) C71 0.015(4) 0.056(8) 0.018(5) 0.006(5) 0.005(4) 0.010(5) C74 0.012(5) 0.042(7) 0.051(7) -0.009(6) 0.001(4) 0.000(5) C81 0.016(5) 0.047(7) 0.049(7) 0.021(6) 0.022(5) 0.015(5) N81 0.025(4) 0.054(7) 0.049(6) 0.012(5) 0.010(4) 0.028(4) C85 0.027(5) 0.053(8) 0.050(7) 0.015(6) 0.020(5) 0.012(5) C84 0.027(6) 0.047(8) 0.073(9) 0.006(7) 0.018(6) 0.011(6) C83 0.028(6) 0.033(7) 0.089(10) 0.028(7) 0.029(6) 0.008(5) C21 0.011(4) 0.035(6) 0.032(5) 0.007(5) 0.000(4) 0.000(4) N21 0.012(4) 0.034(5) 0.046(5) 0.012(4) 0.004(4) 0.002(4) C25 0.020(5) 0.030(6) 0.061(8) 0.014(6) 0.003(5) 0.001(5) C24 0.021(5) 0.037(7) 0.061(8) 0.006(6) 0.008(5) 0.010(5) C23 0.018(5) 0.052(8) 0.073(9) 0.012(7) 0.012(5) 0.011(5) C41 0.011(4) 0.036(6) 0.023(5) -0.001(4) -0.004(4) 0.004(4) C42 0.017(4) 0.031(6) 0.034(6) 0.005(5) 0.007(4) 0.003(4) N41 0.011(4) 0.040(6) 0.025(4) 0.005(4) -0.004(3) -0.003(4) F4 0.034(4) 0.058(5) 0.090(6) -0.008(5) 0.027(4) -0.001(4) F6 0.060(5) 0.031(4) 0.099(6) 0.020(4) 0.044(5) 0.003(4) F5 0.054(5) 0.094(7) 0.075(6) 0.006(5) 0.052(4) 0.004(4) N2 0.015(4) 0.024(5) 0.028(4) 0.003(4) -0.004(3) 0.008(3) N31 0.016(4) 0.028(5) 0.033(5) 0.002(4) 0.002(3) 0.010(3) N51 0.010(3) 0.031(5) 0.028(4) 0.004(4) 0.004(3) 0.006(3) N4 0.011(3) 0.056(6) 0.036(4) 0.022(4) 0.010(3) 0.013(4) N1 0.008(3) 0.047(6) 0.028(4) 0.010(4) 0.003(3) 0.010(4) N3 0.016(4) 0.040(5) 0.040(5) 0.015(4) 0.012(3) 0.019(4) C82 0.015(5) 0.042(7) 0.063(8) 0.031(6) 0.018(5) 0.009(5) N71 0.009(4) 0.043(6) 0.038(5) -0.002(4) 0.003(3) 0.004(4) C22 0.013(4) 0.032(7) 0.056(7) 0.006(6) 0.002(5) -0.001(4) O1 0.016(3) 0.038(4) 0.035(4) 0.019(3) 0.001(3) 0.004(3) O7 0.009(3) 0.054(5) 0.034(4) 0.020(4) 0.003(3) 0.007(3) O8 0.019(3) 0.070(6) 0.042(4) 0.023(4) 0.013(3) 0.031(4) O2 0.012(3) 0.035(4) 0.037(4) 0.010(3) 0.006(3) 0.006(3) O3 0.012(3) 0.031(4) 0.028(4) 0.003(3) -0.001(3) 0.004(3) O10 0.038(4) 0.052(6) 0.048(5) 0.011(4) 0.020(4) 0.005(4) O6 0.015(3) 0.031(4) 0.040(4) 0.003(3) 0.012(3) 0.011(3) O5 0.017(3) 0.034(4) 0.027(4) 0.001(3) 0.006(3) 0.017(3) O4 0.011(3) 0.030(4) 0.023(3) 0.003(3) 0.002(2) 0.004(3) O9 0.050(5) 0.031(5) 0.083(7) 0.015(5) 0.013(5) 0.021(4) P4 0.0144(11) 0.0514(19) 0.0351(15) 0.0168(13) 0.0094(10) 0.0212(12) P2 0.0108(10) 0.0326(15) 0.0237(12) 0.0054(11) 0.0034(9) 0.0086(10) P3 0.0124(11) 0.0311(15) 0.0284(13) 0.0042(11) 0.0056(9) 0.0106(10) Ag2 0.0133(3) 0.0342(5) 0.0498(5) 0.0115(4) 0.0060(3) 0.0038(3) S2 0.0303(13) 0.0217(14) 0.0473(16) 0.0085(12) 0.0138(12) 0.0079(11) C54 0.016(5) 0.056(8) 0.029(5) 0.013(5) 0.010(4) 0.020(5) C64 0.034(7) 0.038(8) 0.086(11) -0.002(8) -0.003(7) 0.018(6) C43 0.018(5) 0.058(8) 0.022(5) 0.000(5) 0.004(4) -0.002(5) C45 0.019(5) 0.050(8) 0.035(6) 0.015(6) 0.001(4) -0.003(5) C44 0.020(5) 0.062(9) 0.031(6) 0.013(6) 0.002(4) -0.004(5) O11 0.039(4) 0.023(4) 0.052(5) 0.012(4) 0.011(4) 0.011(3) N11A 0.0325(18) 0.0313(17) 0.0329(18) 0.0120(13) 0.0042(14) 0.0062(13) C11A 0.0324(17) 0.0312(17) 0.0328(18) 0.0119(13) 0.0043(14) 0.0063(13) C15A 0.0327(18) 0.0313(17) 0.0330(18) 0.0119(13) 0.0041(14) 0.0061(13) C14A 0.0328(18) 0.0314(17) 0.0330(18) 0.0119(13) 0.0040(14) 0.0061(13) C13A 0.0328(18) 0.0314(17) 0.0329(18) 0.0118(13) 0.0041(14) 0.0062(13) C12A 0.0325(18) 0.0312(17) 0.0327(18) 0.0119(13) 0.0042(14) 0.0063(13) S1A 0.039(2) 0.0394(18) 0.043(3) 0.0165(19) 0.017(2) 0.0149(17) O7A 0.051(8) 0.041(8) 0.076(9) 0.030(7) 0.029(6) 0.012(6) O8A 0.053(6) 0.054(6) 0.061(6) 0.018(4) 0.010(4) 0.011(4) O6A 0.092(9) 0.092(9) 0.083(9) 0.021(5) 0.021(5) 0.026(5) C1A 0.043(5) 0.046(5) 0.042(5) 0.015(3) 0.011(3) 0.005(3) F1A 0.058(7) 0.061(7) 0.069(7) 0.016(4) 0.018(4) 0.024(5) F2A 0.102(8) 0.102(8) 0.101(8) 0.038(5) 0.012(5) 0.020(5) F3A 0.073(9) 0.078(9) 0.078(8) 0.033(5) 0.015(5) 0.019(5) S1B 0.039(2) 0.0396(18) 0.044(3) 0.0170(19) 0.017(2) 0.0154(17) C1B 0.043(5) 0.046(5) 0.042(5) 0.015(4) 0.011(3) 0.005(3) O7B 0.051(8) 0.041(8) 0.076(9) 0.030(7) 0.029(6) 0.012(6) O8B 0.044(6) 0.045(6) 0.038(6) 0.015(4) 0.008(4) 0.011(4) O6B 0.027(5) 0.024(5) 0.031(5) 0.009(4) 0.007(4) 0.005(4) F1B 0.056(8) 0.061(8) 0.066(8) 0.006(5) 0.012(5) 0.025(5) F2B 0.071(6) 0.065(7) 0.066(6) 0.015(5) 0.012(5) 0.022(5) F3B 0.054(8) 0.057(8) 0.060(8) 0.020(5) 0.011(5) 0.018(5) C12B 0.0326(17) 0.0314(17) 0.0330(18) 0.0118(13) 0.0041(14) 0.0062(13) C11B 0.0324(17) 0.0312(17) 0.0328(18) 0.0119(13) 0.0043(14) 0.0063(13) C13B 0.0328(18) 0.0315(17) 0.0331(18) 0.0118(13) 0.0040(14) 0.0062(13) C14B 0.0328(18) 0.0314(17) 0.0330(18) 0.0118(13) 0.0041(14) 0.0062(13) C15B 0.0327(18) 0.0313(17) 0.0328(18) 0.0118(13) 0.0042(14) 0.0063(14) N11B 0.0326(18) 0.0313(17) 0.0328(18) 0.0118(13) 0.0042(14) 0.0064(13) _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 P1 N4 1.567(8) . ? P1 O1 1.583(7) . ? P1 N1 1.582(8) . ? P1 O2 1.585(8) . ? Ag1 N71 2.334(7) . ? Ag1 N51 2.343(7) . ? Ag1 O9 2.467(9) . ? Ag1 N31 2.473(8) . ? C72 C71 1.389(12) . ? C72 C73 1.385(17) . ? C72 H72 0.9300 . ? C2 F6 1.323(15) . ? C2 F5 1.329(13) . ? C2 F4 1.344(15) . ? C2 S2 1.814(12) . ? C75 N71 1.333(15) . ? C75 C74 1.389(13) . ? C75 H75 0.9300 . ? C31 N31 1.335(13) . ? C31 C32 1.348(14) . ? C31 O3 1.398(12) . ? C32 C33 1.378(17) . ? C32 H32 0.9300 . ? C33 C34 1.387(17) . ? C33 H33 0.9300 . ? C34 C35 1.359(15) . ? C34 H34 0.9300 . ? C35 N31 1.342(14) . ? C35 H35 0.9300 . ? C73 C74 1.359(17) . ? C73 H73 0.9300 . ? C55 N51 1.352(12) . ? C55 C54 1.389(13) . ? C55 H55 0.9300 . ? C53 C54 1.363(16) . ? C53 C52 1.366(15) . ? C53 H53 0.9300 . ? C52 C51 1.393(12) . ? C52 H52 0.9300 . ? C51 N51 1.315(13) . ? C51 O5 1.383(11) . ? C61 N61 1.318(15) . ? C61 O6 1.385(13) . ? C61 C62 1.389(16) . ? C62 C63 1.400(19) . ? C62 H62 0.9300 . ? C63 C64 1.37(2) . ? C63 H63 0.9300 . ? C65 N61 1.352(14) . ? C65 C64 1.393(19) . ? C65 H65 0.9300 . ? N61 Ag2 2.253(9) . ? C71 N71 1.309(15) . ? C71 O7 1.379(13) . ? C74 H74 0.9300 . ? C81 N81 1.309(14) . ? C81 O8 1.382(13) . ? C81 C82 1.395(16) . ? N81 C85 1.330(15) . ? C85 C84 1.362(18) . ? C85 H85 0.9300 . ? C84 C83 1.377(19) . ? C84 H84 0.9300 . ? C83 C82 1.375(17) . ? C83 H83 0.9300 . ? C21 N21 1.312(12) . ? C21 C22 1.371(13) . ? C21 O2 1.381(13) . ? N21 C25 1.363(14) . ? N21 Ag2 2.332(8) . ? C25 C24 1.378(14) . ? C25 H25 0.9300 . ? C24 C23 1.362(16) . ? C24 H24 0.9300 . ? C23 C22 1.349(17) . ? C23 H23 0.9300 . ? C41 N41 1.297(14) . ? C41 O4 1.398(12) . ? C41 C42 1.411(14) . ? C42 C43 1.393(15) . ? C42 H42 0.9300 . ? N41 C45 1.356(13) . ? N41 Ag2 2.231(9) . ? N2 P2 1.563(8) . ? N2 P3 1.571(8) . ? N4 P4 1.556(9) . ? N1 P2 1.558(7) . ? N3 P3 1.561(8) . ? N3 P4 1.563(8) . ? C82 H82 0.9300 . ? C22 H22 0.9300 . ? O1 C11A 1.363(15) . ? O1 C11B 1.465(16) . ? O7 P4 1.587(8) . ? O8 P4 1.583(7) . ? O3 P2 1.571(7) . ? O10 S2 1.435(8) . ? O6 P3 1.582(7) . ? O5 P3 1.586(7) . ? O4 P2 1.588(7) . ? O9 S2 1.454(9) . ? Ag2 O7A 2.431(13) . ? S2 O11 1.423(8) . ? C54 H54 0.9300 . ? C64 H64 0.9300 . ? C43 C44 1.384(18) . ? C43 H43 0.9300 . ? C45 C44 1.387(17) . ? C45 H45 0.9300 . ? C44 H44 0.9300 . ? N11A C11A 1.33(3) . ? N11A C15A 1.35(2) . ? C11A C12A 1.30(3) . ? C15A C14A 1.33(2) . ? C15A H15A 0.9300 . ? C14A C13A 1.38(2) . ? C14A H14A 0.9300 . ? C13A C12A 1.36(2) . ? C13A H13A 0.9300 . ? C12A H12A 0.9300 . ? S1A O6A 1.407(14) . ? S1A O7A 1.423(13) . ? S1A O8A 1.434(14) . ? S1A C1A 1.890(19) . ? C1A F3A 1.276(14) . ? C1A F1A 1.274(14) . ? C1A F2A 1.297(14) . ? S1B O7B 1.403(14) . ? S1B O6B 1.401(14) . ? S1B O8B 1.459(14) . ? S1B C1B 1.90(2) . ? C1B F1B 1.265(14) . ? C1B F2B 1.280(15) . ? C1B F3B 1.299(14) . ? C12B C11B 1.34(3) . ? C12B C13B 1.36(2) . ? C12B H12B 0.9300 . ? C11B N11B 1.34(3) . ? C13B C14B 1.38(2) . ? C13B H13B 0.9300 . ? C14B C15B 1.33(2) . ? C14B H14B 0.9300 . ? C15B N11B 1.34(2) . ? C15B H15B 0.9300 . ? 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 N4 P1 O1 108.3(4) . . ? N4 P1 N1 120.3(5) . . ? O1 P1 N1 107.0(4) . . ? N4 P1 O2 113.8(5) . . ? O1 P1 O2 99.9(4) . . ? N1 P1 O2 105.5(4) . . ? N71 Ag1 N51 130.2(3) . . ? N71 Ag1 O9 86.6(3) . . ? N51 Ag1 O9 92.1(3) . . ? N71 Ag1 N31 97.8(3) . . ? N51 Ag1 N31 132.0(2) . . ? O9 Ag1 N31 89.7(3) . . ? C71 C72 C73 116.6(11) . . ? C71 C72 H72 121.7 . . ? C73 C72 H72 121.7 . . ? F6 C2 F5 107.5(12) . . ? F6 C2 F4 108.0(10) . . ? F5 C2 F4 107.1(9) . . ? F6 C2 S2 111.6(7) . . ? F5 C2 S2 111.3(8) . . ? F4 C2 S2 111.1(10) . . ? N71 C75 C74 122.0(11) . . ? N71 C75 H75 119.0 . . ? C74 C75 H75 119.0 . . ? N31 C31 C32 125.4(10) . . ? N31 C31 O3 116.2(8) . . ? C32 C31 O3 118.5(10) . . ? C31 C32 C33 118.0(11) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? C32 C33 C34 118.5(10) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C35 C34 C33 118.9(11) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N31 C35 C34 123.5(11) . . ? N31 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? C74 C73 C72 119.6(9) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? N51 C55 C54 121.9(10) . . ? N51 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C54 C53 C52 120.4(9) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C52 C51 117.1(10) . . ? C53 C52 H52 121.4 . . ? C51 C52 H52 121.4 . . ? N51 C51 O5 116.6(7) . . ? N51 C51 C52 124.3(9) . . ? O5 C51 C52 118.9(9) . . ? N61 C61 O6 113.5(9) . . ? N61 C61 C62 126.5(11) . . ? O6 C61 C62 120.0(11) . . ? C61 C62 C63 114.5(14) . . ? C61 C62 H62 122.7 . . ? C63 C62 H62 122.7 . . ? C64 C63 C62 122.2(13) . . ? C64 C63 H63 118.9 . . ? C62 C63 H63 118.9 . . ? N61 C65 C64 123.7(13) . . ? N61 C65 H65 118.1 . . ? C64 C65 H65 118.1 . . ? C61 N61 C65 116.2(10) . . ? C61 N61 Ag2 118.8(7) . . ? C65 N61 Ag2 119.2(8) . . ? N71 C71 C72 124.6(11) . . ? N71 C71 O7 113.5(8) . . ? C72 C71 O7 121.8(11) . . ? C73 C74 C75 119.1(11) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? N81 C81 O8 118.6(10) . . ? N81 C81 C82 125.4(11) . . ? O8 C81 C82 116.0(10) . . ? C81 N81 C85 116.6(11) . . ? N81 C85 C84 123.4(13) . . ? N81 C85 H85 118.3 . . ? C84 C85 H85 118.3 . . ? C85 C84 C83 119.0(13) . . ? C85 C84 H84 120.5 . . ? C83 C84 H84 120.5 . . ? C82 C83 C84 119.4(12) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? N21 C21 C22 123.8(11) . . ? N21 C21 O2 112.8(8) . . ? C22 C21 O2 123.4(9) . . ? C21 N21 C25 118.3(9) . . ? C21 N21 Ag2 118.8(7) . . ? C25 N21 Ag2 122.9(6) . . ? N21 C25 C24 120.4(10) . . ? N21 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C23 C24 C25 119.1(12) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C22 C23 C24 120.7(10) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? N41 C41 O4 114.7(8) . . ? N41 C41 C42 125.8(10) . . ? O4 C41 C42 119.3(10) . . ? C43 C42 C41 115.0(11) . . ? C43 C42 H42 122.5 . . ? C41 C42 H42 122.5 . . ? C41 N41 C45 118.4(10) . . ? C41 N41 Ag2 120.1(7) . . ? C45 N41 Ag2 121.4(8) . . ? P2 N2 P3 129.4(6) . . ? C31 N31 C35 115.7(9) . . ? C31 N31 Ag1 129.0(7) . . ? C35 N31 Ag1 115.2(7) . . ? C51 N51 C55 117.4(8) . . ? C51 N51 Ag1 120.4(6) . . ? C55 N51 Ag1 121.3(7) . . ? P4 N4 P1 128.6(5) . . ? P2 N1 P1 136.3(6) . . ? P3 N3 P4 126.5(6) . . ? C83 C82 C81 116.2(12) . . ? C83 C82 H82 121.9 . . ? C81 C82 H82 121.9 . . ? C71 N71 C75 117.8(8) . . ? C71 N71 Ag1 117.8(7) . . ? C75 N71 Ag1 124.3(7) . . ? C23 C22 C21 117.7(10) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C11A O1 P1 122.2(12) . . ? C11B O1 P1 129.4(13) . . ? C71 O7 P4 127.2(6) . . ? C81 O8 P4 123.6(6) . . ? C21 O2 P1 128.0(6) . . ? C31 O3 P2 123.7(6) . . ? C61 O6 P3 123.3(6) . . ? C51 O5 P3 123.4(5) . . ? C41 O4 P2 124.9(5) . . ? S2 O9 Ag1 140.4(6) . . ? N4 P4 N3 119.3(4) . . ? N4 P4 O8 105.0(4) . . ? N3 P4 O8 109.2(5) . . ? N4 P4 O7 109.2(5) . . ? N3 P4 O7 107.1(4) . . ? O8 P4 O7 106.3(4) . . ? N1 P2 N2 121.5(4) . . ? N1 P2 O3 106.8(4) . . ? N2 P2 O3 108.6(4) . . ? N1 P2 O4 112.5(4) . . ? N2 P2 O4 104.5(4) . . ? O3 P2 O4 101.1(3) . . ? N3 P3 N2 121.9(4) . . ? N3 P3 O6 106.8(5) . . ? N2 P3 O6 107.0(4) . . ? N3 P3 O5 107.4(4) . . ? N2 P3 O5 106.9(4) . . ? O6 P3 O5 105.9(4) . . ? N41 Ag2 N61 143.3(3) . . ? N41 Ag2 N21 119.4(3) . . ? N61 Ag2 N21 93.8(3) . . ? N41 Ag2 O7A 102.0(4) . . ? N61 Ag2 O7A 82.0(4) . . ? N21 Ag2 O7A 105.3(4) . . ? O11 S2 O10 115.9(5) . . ? O11 S2 O9 113.6(5) . . ? O10 S2 O9 115.4(6) . . ? O11 S2 C2 103.4(6) . . ? O10 S2 C2 103.8(5) . . ? O9 S2 C2 102.3(6) . . ? C53 C54 C55 118.8(10) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? C63 C64 C65 116.8(13) . . ? C63 C64 H64 121.6 . . ? C65 C64 H64 121.6 . . ? C44 C43 C42 120.2(11) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? N41 C45 C44 121.0(12) . . ? N41 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C44 C43 119.5(11) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C11A N11A C15A 114.8(14) . . ? C12A C11A N11A 128.7(14) . . ? C12A C11A O1 107.7(18) . . ? N11A C11A O1 123.6(18) . . ? C14A C15A N11A 122.6(16) . . ? C14A C15A H15A 118.7 . . ? N11A C15A H15A 118.7 . . ? C15A C14A C13A 117.9(16) . . ? C15A C14A H14A 121.0 . . ? C13A C14A H14A 121.0 . . ? C12A C13A C14A 121.6(16) . . ? C12A C13A H13A 119.2 . . ? C14A C13A H13A 119.2 . . ? C11A C12A C13A 114.3(16) . . ? C11A C12A H12A 122.8 . . ? C13A C12A H12A 122.8 . . ? O6A S1A O7A 116.2(12) . . ? O6A S1A O8A 114.9(12) . . ? O7A S1A O8A 113.4(11) . . ? O6A S1A C1A 103.9(9) . . ? O7A S1A C1A 102.2(7) . . ? O8A S1A C1A 103.9(8) . . ? S1A O7A Ag2 147.3(10) . . ? F3A C1A F1A 118.8(16) . . ? F3A C1A F2A 109.3(17) . . ? F1A C1A F2A 99.9(15) . . ? F3A C1A S1A 110.9(12) . . ? F1A C1A S1A 109.3(11) . . ? F2A C1A S1A 107.6(12) . . ? O7B S1B O6B 117.3(12) . . ? O7B S1B O8B 113.0(12) . . ? O6B S1B O8B 114.5(11) . . ? O7B S1B C1B 103.8(8) . . ? O6B S1B C1B 103.3(9) . . ? O8B S1B C1B 102.5(8) . . ? F1B C1B F2B 100.2(16) . . ? F1B C1B F3B 118.7(16) . . ? F2B C1B F3B 110.7(18) . . ? F1B C1B S1B 109.6(12) . . ? F2B C1B S1B 110.5(12) . . ? F3B C1B S1B 107.1(12) . . ? C11B C12B C13B 117.3(18) . . ? C11B C12B H12B 121.4 . . ? C13B C12B H12B 121.4 . . ? N11B C11B C12B 122.4(14) . . ? N11B C11B O1 110.3(19) . . ? C12B C11B O1 127(2) . . ? C12B C13B C14B 122.2(18) . . ? C12B C13B H13B 118.9 . . ? C14B C13B H13B 118.9 . . ? C15B C14B C13B 115.8(16) . . ? C15B C14B H14B 122.1 . . ? C13B C14B H14B 122.1 . . ? C14B C15B N11B 123.9(17) . . ? C14B C15B H15B 118.0 . . ? N11B C15B H15B 118.0 . . ? C11B N11B C15B 118.2(16) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.154 _refine_diff_density_min -1.315 _refine_diff_density_rms 0.177 data_ag2otf2n _database_code_depnum_ccdc_archive 'CCDC 926376' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H16 Ag F3 N6 O7 P2 S), 2(C2), 0.5(O2)' _chemical_formula_sum 'C46 H32 Ag2 F6 N12 O15 P4 S2 ' _chemical_formula_weight 1510.60 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8370(18) _cell_length_b 12.822(3) _cell_length_c 13.162(3) _cell_angle_alpha 110.32(3) _cell_angle_beta 91.58(3) _cell_angle_gamma 92.00(3) _cell_volume 1396.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(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 0.67 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.733145 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24098 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0433 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5114 _reflns_number_gt 4964 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One diethylether solvate species is disordered. ; _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^)+(0.0301P)^2^+1.2154P] 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 5114 _refine_ls_number_parameters 425 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.066 _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 1.105597(16) 0.261324(11) 0.787552(12) 0.01536(7) Uani 1 1 d . . . N31 N 0.84808(19) 0.20351(14) 0.71560(15) 0.0151(4) Uani 1 1 d . . . C31 C 0.7398(2) 0.26162(15) 0.77340(17) 0.0125(4) Uani 1 1 d . . . O3 O 0.79695(15) 0.36049(11) 0.84997(12) 0.0135(3) Uani 1 1 d . . . N2 N 0.62223(19) 0.40699(13) 1.00930(14) 0.0125(3) Uani 1 1 d . . . C32 C 0.5871(2) 0.22877(17) 0.76008(18) 0.0155(4) Uani 1 1 d . . . C33 C 0.5464(2) 0.12829(17) 0.67836(19) 0.0179(4) Uani 1 1 d . . . C34 C 0.6572(3) 0.06683(17) 0.61534(19) 0.0208(5) Uani 1 1 d . . . C35 C 0.8064(3) 0.10686(17) 0.63618(18) 0.0193(5) Uani 1 1 d . . . O9A O 1.011(2) 0.4842(13) 0.4884(19) 0.063(3) Uani 0.235(5) 1 d PDU . 1 P2 P 0.69968(6) 0.45533(4) 0.92931(4) 0.01018(11) Uani 1 1 d . . . P1 P 0.44008(6) 0.55176(4) 0.87401(4) 0.01067(12) Uani 1 1 d . . . S1 S 0.87682(6) 0.04297(4) 0.29899(4) 0.01545(12) Uani 1 1 d . . . N21 N 0.6363(2) 0.73279(16) 0.77725(16) 0.0205(4) Uani 1 1 d . . . C21 C 0.5430(2) 0.73540(16) 0.85358(18) 0.0140(4) Uani 1 1 d . . . C22 C 0.5423(3) 0.81590(18) 0.95531(19) 0.0221(5) Uani 1 1 d . . . H22 H 0.4709 0.8131 1.0051 0.027 Uiso 1 1 calc R . . C24 C 0.7549(3) 0.9013(2) 0.9025(2) 0.0308(6) Uani 1 1 d . . . H24 H 0.8303 0.9576 0.9172 0.037 Uiso 1 1 calc R . . C25 C 0.7431(3) 0.8166(2) 0.8031(2) 0.0261(5) Uani 1 1 d . . . H25 H 0.8122 0.8174 0.7512 0.031 Uiso 1 1 calc R . . C23 C 0.6529(3) 0.90108(19) 0.9799(2) 0.0308(6) Uani 1 1 d . . . H23 H 0.6583 0.9573 1.0475 0.037 Uiso 1 1 calc R . . N41 N 0.9423(2) 0.71343(14) 1.03904(14) 0.0138(4) Uani 1 1 d . . . C41 C 0.9139(2) 0.61611(16) 0.96083(17) 0.0125(4) Uani 1 1 d . . . C42 C 0.9658(2) 0.58771(17) 0.85739(18) 0.0183(4) Uani 1 1 d . . . H42 H 0.9419 0.5182 0.8052 0.022 Uiso 1 1 calc R . . C43 C 1.0546(3) 0.66663(18) 0.83428(19) 0.0195(5) Uani 1 1 d . . . H43 H 1.0920 0.6512 0.7655 0.023 Uiso 1 1 calc R . . C44 C 1.0876(3) 0.76921(18) 0.9146(2) 0.0204(5) Uani 1 1 d . . . H44 H 1.1481 0.8232 0.9008 0.025 Uiso 1 1 calc R . . C45 C 1.0293(3) 0.78950(17) 1.01479(19) 0.0196(5) Uani 1 1 d . . . H45 H 1.0507 0.8586 1.0683 0.024 Uiso 1 1 calc R . . O10 O 0.91230(19) 0.02448(13) 0.18838(14) 0.0266(4) Uani 1 1 d . . . O11 O 0.98271(19) 0.11547(13) 0.37964(15) 0.0295(4) Uani 1 1 d . . . O12 O 0.82454(18) -0.05593(12) 0.31966(14) 0.0228(4) Uani 1 1 d . . . C1 C 0.7056(3) 0.12305(18) 0.31598(19) 0.0196(5) Uani 1 1 d . . . F3 F 0.73345(17) 0.22115(11) 0.30424(13) 0.0302(3) Uani 1 1 d . . . F2 F 0.65026(18) 0.14282(12) 0.41359(12) 0.0331(3) Uani 1 1 d . . . F1 F 0.59564(16) 0.06868(12) 0.24331(13) 0.0320(3) Uani 1 1 d . . . O2 O 0.43171(16) 0.64742(11) 0.82411(12) 0.0136(3) Uani 1 1 d . . . O4 O 0.83245(16) 0.54093(11) 0.99549(12) 0.0135(3) Uani 1 1 d . . . N1 N 0.60323(19) 0.50516(13) 0.85641(14) 0.0131(4) Uani 1 1 d . . . O1 O 0.31609(16) 0.46359(11) 0.79827(12) 0.0139(3) Uani 1 1 d . . . N11 N 0.2404(2) 0.30446(14) 0.66566(15) 0.0147(4) Uani 1 1 d . . . C11 C 0.3291(2) 0.39635(16) 0.69137(17) 0.0137(4) Uani 1 1 d . . . C14 C 0.3245(3) 0.25363(19) 0.48508(19) 0.0239(5) Uani 1 1 d . . . H14 H 0.3202 0.2037 0.4141 0.029 Uiso 1 1 calc R . . C12 C 0.4211(3) 0.42342(18) 0.62022(19) 0.0223(5) Uani 1 1 d . . . H12 H 0.4822 0.4885 0.6424 0.027 Uiso 1 1 calc R . . C13 C 0.4185(3) 0.3496(2) 0.5146(2) 0.0269(5) Uani 1 1 d . . . H13 H 0.4789 0.3641 0.4638 0.032 Uiso 1 1 calc R . . H32 H 0.5152 0.2720 0.8039 0.032 Uiso 1 1 d R . . C15 C 0.2386(3) 0.23358(18) 0.56165(18) 0.0196(5) Uani 1 1 d . . . H15 H 0.1767 0.1689 0.5416 0.024 Uiso 1 1 calc R . . H33 H 0.4455 0.1025 0.6661 0.024 Uiso 1 1 d R . . H34 H 0.6318 -0.0003 0.5598 0.024 Uiso 1 1 d R . . H35 H 0.8809 0.0655 0.5937 0.024 Uiso 1 1 d R . . C92A C 0.8554(9) 0.4689(6) 0.5318(8) 0.058(2) Uani 0.471(9) 1 d PDU . 1 C91A C 0.8722(10) 0.3789(6) 0.5769(6) 0.042(2) Uani 0.471(9) 1 d PDU . 1 O9B O 0.9429(11) 0.5026(8) 0.4530(9) 0.044(2) Uani 0.265(5) 1 d PDU . 2 C92B C 0.9539(8) 0.4233(6) 0.5140(7) 0.060(2) Uani 0.529(9) 1 d PDU . 2 C91B C 0.8203(12) 0.4145(9) 0.5693(8) 0.074(3) Uani 0.529(9) 1 d PDU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01326(10) 0.01403(9) 0.01525(11) 0.00075(7) 0.00277(7) -0.00226(6) N31 0.0118(8) 0.0149(8) 0.0149(9) 0.0005(7) 0.0004(7) 0.0014(7) C31 0.0140(10) 0.0091(8) 0.0125(10) 0.0016(7) -0.0003(8) -0.0001(7) O3 0.0097(7) 0.0097(6) 0.0160(8) -0.0020(5) 0.0011(6) -0.0007(5) N2 0.0118(8) 0.0103(7) 0.0136(9) 0.0022(6) -0.0001(7) -0.0006(6) C32 0.0128(10) 0.0137(9) 0.0181(11) 0.0030(8) 0.0026(8) 0.0007(8) C33 0.0147(10) 0.0167(10) 0.0210(12) 0.0057(9) -0.0034(9) -0.0034(8) C34 0.0244(12) 0.0132(9) 0.0193(11) -0.0007(8) -0.0056(10) -0.0010(8) C35 0.0185(11) 0.0161(10) 0.0174(11) -0.0021(8) 0.0004(9) 0.0049(8) O9A 0.046(5) 0.053(5) 0.077(5) 0.007(5) 0.013(4) -0.004(4) P2 0.0087(2) 0.0083(2) 0.0111(3) 0.00027(19) 0.0010(2) -0.00020(18) P1 0.0101(2) 0.0091(2) 0.0114(3) 0.00202(19) -0.0001(2) -0.00112(18) S1 0.0132(2) 0.0126(2) 0.0185(3) 0.00282(19) 0.0009(2) -0.00006(19) N21 0.0171(9) 0.0251(9) 0.0212(10) 0.0106(8) 0.0010(8) -0.0005(8) C21 0.0133(10) 0.0119(9) 0.0187(11) 0.0079(8) -0.0020(8) -0.0005(8) C22 0.0252(12) 0.0181(10) 0.0213(12) 0.0047(9) 0.0023(10) -0.0006(9) C24 0.0271(13) 0.0256(12) 0.0428(16) 0.0181(11) -0.0118(12) -0.0118(10) C25 0.0174(11) 0.0360(13) 0.0323(14) 0.0221(11) -0.0007(10) -0.0055(10) C23 0.0386(15) 0.0183(11) 0.0293(14) 0.0017(10) -0.0084(12) -0.0070(10) N41 0.0135(8) 0.0120(8) 0.0147(9) 0.0031(7) 0.0019(7) 0.0000(6) C41 0.0076(9) 0.0125(9) 0.0169(11) 0.0050(8) -0.0007(8) -0.0011(7) C42 0.0183(11) 0.0182(10) 0.0145(11) 0.0013(8) 0.0011(9) -0.0031(8) C43 0.0178(11) 0.0247(11) 0.0168(11) 0.0083(9) 0.0044(9) -0.0007(9) C44 0.0189(11) 0.0180(10) 0.0262(12) 0.0105(9) 0.0016(9) -0.0037(8) C45 0.0220(11) 0.0127(9) 0.0221(12) 0.0038(8) 0.0008(9) -0.0034(8) O10 0.0284(9) 0.0266(8) 0.0245(9) 0.0072(7) 0.0115(7) 0.0045(7) O11 0.0230(9) 0.0238(8) 0.0346(10) 0.0025(7) -0.0104(8) -0.0044(7) O12 0.0189(8) 0.0173(7) 0.0338(10) 0.0107(7) 0.0048(7) 0.0020(6) C1 0.0199(11) 0.0188(10) 0.0215(12) 0.0083(9) 0.0048(9) 0.0034(9) F3 0.0341(8) 0.0200(6) 0.0418(9) 0.0165(6) 0.0088(7) 0.0070(6) F2 0.0369(8) 0.0379(8) 0.0295(8) 0.0152(7) 0.0193(7) 0.0165(7) F1 0.0192(7) 0.0357(8) 0.0409(9) 0.0137(7) -0.0077(6) 0.0020(6) O2 0.0129(7) 0.0123(6) 0.0152(7) 0.0049(6) -0.0023(6) -0.0026(5) O4 0.0137(7) 0.0116(6) 0.0127(7) 0.0015(5) -0.0006(6) -0.0048(5) N1 0.0123(8) 0.0134(8) 0.0129(9) 0.0036(7) 0.0020(7) 0.0003(7) O1 0.0125(7) 0.0137(7) 0.0119(7) 0.0002(6) 0.0012(6) -0.0036(5) N11 0.0133(8) 0.0147(8) 0.0132(9) 0.0013(7) -0.0014(7) -0.0011(7) C11 0.0144(10) 0.0139(9) 0.0105(10) 0.0017(8) -0.0017(8) 0.0009(8) C14 0.0339(13) 0.0205(11) 0.0130(11) 0.0005(9) -0.0006(10) 0.0000(9) C12 0.0270(12) 0.0190(10) 0.0194(12) 0.0056(9) 0.0029(10) -0.0059(9) C13 0.0359(14) 0.0284(12) 0.0175(12) 0.0091(10) 0.0080(10) -0.0023(10) C15 0.0219(11) 0.0183(10) 0.0147(11) 0.0013(8) -0.0020(9) -0.0027(9) C92A 0.058(4) 0.041(3) 0.077(4) 0.021(3) 0.026(3) 0.001(3) C91A 0.055(5) 0.030(3) 0.031(3) 0.000(3) -0.022(3) 0.019(3) O9B 0.051(4) 0.036(3) 0.057(5) 0.028(3) 0.019(4) 0.015(3) C92B 0.049(3) 0.044(3) 0.082(4) 0.014(3) 0.018(3) 0.004(3) C91B 0.079(6) 0.079(6) 0.056(5) 0.017(5) -0.002(5) -0.028(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 N11 2.231(2) 1_655 ? Ag1 N41 2.2456(19) 2_767 ? Ag1 N31 2.4292(19) . ? Ag1 O12 2.6246(17) 2_756 ? N31 C31 1.321(3) . ? N31 C35 1.346(3) . ? C31 O3 1.385(2) . ? C31 C32 1.387(3) . ? O3 P2 1.5965(15) . ? N2 P2 1.5571(19) . ? N2 P1 1.5635(19) 2_667 ? C32 C33 1.389(3) . ? C32 H32 0.9308 . ? C33 C34 1.383(3) . ? C33 H33 0.9297 . ? C34 C35 1.383(3) . ? C34 H34 0.9305 . ? C35 H35 0.9307 . ? O9A O9A 0.47(3) 2_766 ? O9A C92A 1.382(19) 2_766 ? O9A C92A 1.533(15) . ? P2 N1 1.5729(18) . ? P2 O4 1.5904(15) . ? P1 N2 1.5635(19) 2_667 ? P1 N1 1.5722(18) . ? P1 O2 1.5826(15) . ? P1 O1 1.5946(16) . ? S1 O10 1.4369(18) . ? S1 O11 1.4372(18) . ? S1 O12 1.4495(16) . ? S1 C1 1.833(2) . ? N21 C21 1.310(3) . ? N21 C25 1.349(3) . ? C21 C22 1.378(3) . ? C21 O2 1.410(2) . ? C22 C23 1.384(3) . ? C22 H22 0.9300 . ? C24 C25 1.378(4) . ? C24 C23 1.379(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C23 H23 0.9300 . ? N41 C41 1.323(3) . ? N41 C45 1.350(3) . ? N41 Ag1 2.2456(19) 2_767 ? C41 C42 1.378(3) . ? C41 O4 1.390(2) . ? C41 Ag1 3.147(2) 2_767 ? C42 C43 1.380(3) . ? C42 H42 0.9300 . ? C43 C44 1.387(3) . ? C43 H43 0.9300 . ? C44 C45 1.371(3) . ? C44 H44 0.9300 . ? C45 Ag1 3.148(2) 2_767 ? C45 H45 0.9300 . ? O12 Ag1 2.6246(17) 2_756 ? C1 F2 1.331(3) . ? C1 F3 1.335(3) . ? C1 F1 1.336(3) . ? O4 Ag1 3.1098(19) 2_767 ? O1 C11 1.382(2) . ? O1 Ag1 3.0985(17) 1_455 ? N11 C11 1.327(3) . ? N11 C15 1.354(3) . ? N11 Ag1 2.231(2) 1_455 ? C11 C12 1.381(3) . ? C11 Ag1 3.150(2) 1_455 ? C14 C15 1.366(4) . ? C14 C13 1.391(3) . ? C14 H14 0.9300 . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 Ag1 3.136(2) 1_455 ? C15 H15 0.9300 . ? C92A O9A 1.38(2) 2_766 ? C92A C91A 1.478(9) . ? O9B C92B 1.246(13) 2_766 ? O9B C92B 1.503(11) . ? O9B O9B 1.60(2) 2_766 ? C92B O9B 1.246(13) 2_766 ? C92B C91B 1.426(11) . ? 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 Ag1 N41 150.14(7) 1_655 2_767 ? N11 Ag1 N31 109.72(7) 1_655 . ? N41 Ag1 N31 96.29(7) 2_767 . ? N11 Ag1 O12 84.92(6) 1_655 2_756 ? N41 Ag1 O12 111.81(6) 2_767 2_756 ? N31 Ag1 O12 86.51(6) . 2_756 ? C31 N31 C35 117.45(18) . . ? C31 N31 Ag1 115.92(13) . . ? C35 N31 Ag1 125.26(14) . . ? N31 C31 O3 111.73(17) . . ? N31 C31 C32 124.77(18) . . ? O3 C31 C32 123.50(18) . . ? O3 C31 Ag1 70.43(10) . . ? C32 C31 Ag1 163.29(14) . . ? C31 O3 P2 126.03(13) . . ? C31 O3 Ag1 84.34(11) . . ? P2 O3 Ag1 149.08(8) . . ? P2 N2 P1 139.42(11) . 2_667 ? C31 C32 C33 116.92(19) . . ? C31 C32 H32 121.5 . . ? C33 C32 H32 121.6 . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 118.87(19) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.5 . . ? N31 C35 C34 122.5(2) . . ? N31 C35 H35 118.7 . . ? C34 C35 H35 118.8 . . ? O9A O9A C92A 100(4) 2_766 2_766 ? O9A O9A C92A 63(4) 2_766 . ? C92A O9A C92A 162.6(11) 2_766 . ? N2 P2 N1 120.95(9) . . ? N2 P2 O4 107.54(9) . . ? N1 P2 O4 111.19(9) . . ? N2 P2 O3 108.03(9) . . ? N1 P2 O3 107.10(9) . . ? O4 P2 O3 99.97(8) . . ? N2 P1 N1 119.41(10) 2_667 . ? N2 P1 O2 109.72(9) 2_667 . ? N1 P1 O2 107.84(9) . . ? N2 P1 O1 106.54(9) 2_667 . ? N1 P1 O1 111.15(9) . . ? O2 P1 O1 100.55(8) . . ? O10 S1 O11 115.50(11) . . ? O10 S1 O12 114.69(10) . . ? O11 S1 O12 114.98(11) . . ? O10 S1 C1 102.99(11) . . ? O11 S1 C1 103.62(10) . . ? O12 S1 C1 102.54(10) . . ? C21 N21 C25 115.8(2) . . ? N21 C21 C22 126.3(2) . . ? N21 C21 O2 114.61(18) . . ? C22 C21 O2 119.0(2) . . ? C21 C22 C23 116.8(2) . . ? C21 C22 H22 121.6 . . ? C23 C22 H22 121.6 . . ? C25 C24 C23 118.9(2) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N21 C25 C24 123.2(2) . . ? N21 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C24 C23 C22 119.0(2) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C41 N41 C45 116.92(19) . . ? C41 N41 Ag1 121.55(14) . 2_767 ? C45 N41 Ag1 120.13(14) . 2_767 ? N41 C41 C42 124.84(19) . . ? N41 C41 O4 112.69(18) . . ? C42 C41 O4 122.36(18) . . ? C42 C41 Ag1 160.01(15) . 2_767 ? O4 C41 Ag1 75.68(11) . 2_767 ? C41 C42 C43 117.3(2) . . ? C41 C42 H42 121.3 . . ? C43 C42 H42 121.3 . . ? C42 C43 C44 119.4(2) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C45 C44 C43 118.7(2) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? N41 C45 C44 122.8(2) . . ? C44 C45 Ag1 158.57(15) . 2_767 ? N41 C45 H45 118.6 . . ? C44 C45 H45 118.6 . . ? Ag1 C45 H45 81.4 2_767 . ? S1 O12 Ag1 126.45(10) . 2_756 ? F2 C1 F3 107.66(18) . . ? F2 C1 F1 106.88(19) . . ? F3 C1 F1 107.51(19) . . ? F2 C1 S1 111.59(16) . . ? F3 C1 S1 111.39(16) . . ? F1 C1 S1 111.57(15) . . ? C21 O2 P1 120.37(13) . . ? C41 O4 P2 126.62(13) . . ? C41 O4 Ag1 78.66(10) . 2_767 ? P2 O4 Ag1 140.68(8) . 2_767 ? P1 N1 P2 128.91(12) . . ? C11 O1 P1 127.23(14) . . ? C11 O1 Ag1 79.31(11) . 1_455 ? P1 O1 Ag1 142.68(8) . 1_455 ? C11 N11 C15 117.31(19) . . ? C11 N11 Ag1 122.56(14) . 1_455 ? C15 N11 Ag1 120.07(14) . 1_455 ? N11 C11 C12 124.62(19) . . ? N11 C11 O1 111.67(18) . . ? C12 C11 O1 123.70(18) . . ? C12 C11 Ag1 161.07(15) . 1_455 ? O1 C11 Ag1 75.15(11) . 1_455 ? C15 C14 C13 119.2(2) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C11 C12 C13 117.2(2) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? N11 C15 C14 122.4(2) . . ? C14 C15 Ag1 160.23(16) . 1_455 ? N11 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? Ag1 C15 H15 80.9 1_455 . ? O9A C92A C91A 115.5(14) 2_766 . ? C91A C92A O9A 105.3(10) . . ? C92B O9B C92B 109.7(8) 2_766 . ? C92B O9B O9B 62.4(8) 2_766 2_766 ? C92B O9B O9B 47.3(5) . 2_766 ? O9B C92B C91B 126.3(9) 2_766 . ? O9B C92B O9B 70.3(9) 2_766 . ? C91B C92B O9B 113.5(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.629 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.166 data_[ag3mel](pf6)3 _database_code_depnum_ccdc_archive 'CCDC 926377' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H54 Ag3 N14 O8 P4, 3(F6 P), 2(C2 H3 N)7' _chemical_formula_sum 'C56 H60 Ag3 F18 N16 O8 P7' _chemical_formula_weight 1967.60 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' F F 0.0171 0.0103 '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' 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 Pna2(1) _space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 36.803(2) _cell_length_b 7.3345(4) _cell_length_c 27.2815(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7364.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.504602 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; Two large unit-cell axes have led to partial overlap of reflections resulting in the unusually high R(int), and also in a number of apparent systematic absence violations. ; _diffrn_ambient_temperature 198(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91850 _diffrn_reflns_av_R_equivalents 0.1970 _diffrn_reflns_av_sigmaI/netI 0.1197 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13002 _reflns_number_gt 8352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 'Because of weak data ( = 3.1), moderately tight restraints on ADPs were applied. The orientations of the ellipsoids are generally chemically sensible, not elongated along sigma bonds.' ; _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^)+(0.0567P)^2^+65.8352P] 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 -0.05(4) _refine_ls_number_reflns 13002 _refine_ls_number_parameters 985 _refine_ls_number_restraints 211 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.001 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 N94 N 0.1457(4) 0.818(2) 0.3160(5) 0.055(4) Uani 1 1 d U . . Ag1 Ag 0.93970(3) 0.39189(14) 0.41888(3) 0.0278(2) Uani 1 1 d . . . Ag2 Ag 0.77426(2) 0.60332(15) 0.53015(3) 0.0255(2) Uani 1 1 d . . . Ag3 Ag 0.76487(3) 1.10264(16) 0.48471(3) 0.0284(2) Uani 1 1 d . . . C11 C 0.8917(3) 0.5798(16) 0.3399(4) 0.017(3) Uani 1 1 d . . . C12 C 0.8804(4) 0.6530(17) 0.2968(4) 0.022(3) Uani 1 1 d . . . H12 H 0.8560 0.6784 0.2911 0.027 Uiso 1 1 calc R . . C13 C 0.9068(3) 0.6886(18) 0.2613(4) 0.022(3) Uani 1 1 d U . . C14 C 0.9418(4) 0.6432(16) 0.2725(5) 0.024(3) Uani 1 1 d . . . H14 H 0.9598 0.6632 0.2491 0.029 Uiso 1 1 calc R . . C15 C 0.9513(3) 0.5706(17) 0.3158(4) 0.019(3) Uani 1 1 d U . . H15 H 0.9756 0.5462 0.3222 0.023 Uiso 1 1 calc R . . C16 C 0.8955(4) 0.7699(18) 0.2127(4) 0.028(3) Uani 1 1 d . . . H16A H 0.9156 0.8357 0.1988 0.041 Uiso 1 1 calc R . . H16B H 0.8755 0.8514 0.2176 0.041 Uiso 1 1 calc R . . H16C H 0.8884 0.6740 0.1907 0.041 Uiso 1 1 calc R . . C21 C 0.7849(3) 0.5577(14) 0.4189(4) 0.012(2) Uani 1 1 d U . . C22 C 0.7776(3) 0.5386(17) 0.3701(5) 0.021(3) Uani 1 1 d . . . H22 H 0.7964 0.5421 0.3474 0.026 Uiso 1 1 calc R . . C23 C 0.7424(3) 0.5142(16) 0.3545(4) 0.016(3) Uani 1 1 d . . . C24 C 0.7155(3) 0.5107(18) 0.3912(5) 0.023(3) Uani 1 1 d . . . H24 H 0.6913 0.4928 0.3827 0.028 Uiso 1 1 calc R . . C25 C 0.7246(3) 0.5330(18) 0.4388(4) 0.023(3) Uani 1 1 d . . . H25 H 0.7064 0.5303 0.4624 0.027 Uiso 1 1 calc R . . C26 C 0.7326(4) 0.496(2) 0.3015(5) 0.035(4) Uani 1 1 d . . . H26A H 0.7539 0.5132 0.2818 0.052 Uiso 1 1 calc R . . H26B H 0.7147 0.5859 0.2931 0.052 Uiso 1 1 calc R . . H26C H 0.7228 0.3763 0.2957 0.052 Uiso 1 1 calc R . . C31 C 0.9010(3) 1.1106(17) 0.3238(4) 0.017(3) Uani 1 1 d . . . C32 C 0.9043(4) 1.1806(19) 0.2771(5) 0.025(3) Uani 1 1 d U . . H32 H 0.8844 1.2297 0.2608 0.030 Uiso 1 1 calc R . . C33 C 0.9389(4) 1.1752(18) 0.2550(5) 0.025(3) Uani 1 1 d . . . C34 C 0.9664(4) 1.0932(18) 0.2817(5) 0.033(3) Uani 1 1 d . . . H34 H 0.9896 1.0833 0.2685 0.040 Uiso 1 1 calc R . . C35 C 0.9593(4) 1.026(2) 0.3277(5) 0.036(4) Uani 1 1 d U . . H35 H 0.9784 0.9728 0.3448 0.043 Uiso 1 1 calc R . . C36 C 0.9445(5) 1.245(2) 0.2045(5) 0.049(5) Uani 1 1 d . . . H36A H 0.9677 1.2053 0.1925 0.073 Uiso 1 1 calc R . . H36B H 0.9438 1.3762 0.2049 0.073 Uiso 1 1 calc R . . H36C H 0.9256 1.2001 0.1835 0.073 Uiso 1 1 calc R . . C41 C 0.7849(3) 1.0890(16) 0.3759(4) 0.013(2) Uani 1 1 d U . . C42 C 0.7831(3) 1.0614(17) 0.3263(4) 0.021(3) Uani 1 1 d . . . H42 H 0.8034 1.0831 0.3067 0.025 Uiso 1 1 calc R . . C43 C 0.7512(4) 1.0014(19) 0.3058(4) 0.027(3) Uani 1 1 d . . . C44 C 0.7221(4) 0.9723(18) 0.3374(4) 0.024(3) Uani 1 1 d U . . H44 H 0.7003 0.9269 0.3252 0.029 Uiso 1 1 calc R . . C45 C 0.7253(3) 1.0099(19) 0.3858(5) 0.025(3) Uani 1 1 d . . . H45 H 0.7050 0.9971 0.4057 0.030 Uiso 1 1 calc R . . C46 C 0.7485(5) 0.961(2) 0.2517(5) 0.047(4) Uani 1 1 d . . . H46A H 0.7552 1.0669 0.2333 0.071 Uiso 1 1 calc R . . H46B H 0.7240 0.9268 0.2438 0.071 Uiso 1 1 calc R . . H46C H 0.7646 0.8620 0.2436 0.071 Uiso 1 1 calc R . . C51 C 0.9428(3) 1.2117(15) 0.5212(4) 0.017(3) Uani 1 1 d . . . C52 C 0.9547(3) 1.1379(16) 0.5641(5) 0.023(3) Uani 1 1 d . . . H52 H 0.9388 1.1140 0.5898 0.028 Uiso 1 1 calc R . . C53 C 0.9921(4) 1.0992(18) 0.5677(5) 0.027(3) Uani 1 1 d . . . C54 C 1.0137(3) 1.1362(19) 0.5273(5) 0.034(3) Uani 1 1 d . . . H54 H 1.0384 1.1089 0.5280 0.041 Uiso 1 1 calc R . . C55 C 0.9984(3) 1.2138(16) 0.4859(5) 0.021(3) Uani 1 1 d U . . H55 H 1.0134 1.2392 0.4594 0.025 Uiso 1 1 calc R . . C56 C 1.0074(4) 1.022(2) 0.6146(5) 0.040(4) Uani 1 1 d . . . H56A H 1.0291 0.9543 0.6076 0.059 Uiso 1 1 calc R . . H56B H 0.9897 0.9423 0.6294 0.059 Uiso 1 1 calc R . . H56C H 1.0129 1.1194 0.6368 0.059 Uiso 1 1 calc R . . C61 C 0.8250(3) 1.2085(16) 0.5572(4) 0.019(3) Uani 1 1 d . . . C62 C 0.8437(3) 1.2442(18) 0.6006(4) 0.020(3) Uani 1 1 d . . . H62 H 0.8682 1.2751 0.6003 0.024 Uiso 1 1 calc R . . C63 C 0.8244(4) 1.2321(17) 0.6443(4) 0.021(3) Uani 1 1 d . . . C64 C 0.7875(3) 1.184(2) 0.6423(5) 0.032(3) Uani 1 1 d . . . H64 H 0.7742 1.1702 0.6710 0.038 Uiso 1 1 calc R . . C65 C 0.7714(4) 1.158(2) 0.5983(5) 0.035(4) Uani 1 1 d . . . H65 H 0.7465 1.1350 0.5977 0.042 Uiso 1 1 calc R . . C66 C 0.8434(4) 1.2690(19) 0.6918(4) 0.028(3) Uani 1 1 d . . . H66A H 0.8689 1.2454 0.6881 0.043 Uiso 1 1 calc R . . H66B H 0.8336 1.1911 0.7168 0.043 Uiso 1 1 calc R . . H66C H 0.8398 1.3941 0.7009 0.043 Uiso 1 1 calc R . . C71 C 0.9576(3) 0.6795(16) 0.5241(4) 0.016(3) Uani 1 1 d . . . C72 C 0.9831(3) 0.6096(17) 0.5577(4) 0.020(3) Uani 1 1 d . . . H72 H 0.9766 0.5627 0.5882 0.024 Uiso 1 1 calc R . . C73 C 1.0194(3) 0.6167(18) 0.5413(5) 0.025(3) Uani 1 1 d U . . C74 C 1.0259(4) 0.683(2) 0.4962(5) 0.037(4) Uani 1 1 d . . . H74 H 1.0496 0.6813 0.4844 0.044 Uiso 1 1 calc R . . C75 C 0.9989(4) 0.751(2) 0.4670(5) 0.037(4) Uani 1 1 d . . . H75 H 1.0049 0.8030 0.4370 0.044 Uiso 1 1 calc R . . C76 C 1.0484(4) 0.547(3) 0.5764(6) 0.050(5) Uani 1 1 d . . . H76A H 1.0620 0.4515 0.5609 0.075 Uiso 1 1 calc R . . H76B H 1.0370 0.5009 0.6055 0.075 Uiso 1 1 calc R . . H76C H 1.0645 0.6453 0.5849 0.075 Uiso 1 1 calc R . . C81 C 0.8439(3) 0.6873(16) 0.5895(4) 0.018(3) Uani 1 1 d U . . C82 C 0.8663(4) 0.7275(18) 0.6285(4) 0.024(3) Uani 1 1 d . . . H82 H 0.8913 0.7266 0.6242 0.029 Uiso 1 1 calc R . . C83 C 0.8519(4) 0.7692(18) 0.6741(4) 0.025(3) Uani 1 1 d . . . C84 C 0.8136(4) 0.762(2) 0.6767(5) 0.035(4) Uani 1 1 d . . . H84 H 0.8021 0.7839 0.7065 0.042 Uiso 1 1 calc R . . C85 C 0.7933(4) 0.722(2) 0.6361(5) 0.030(3) Uani 1 1 d . . . H85 H 0.7681 0.7239 0.6388 0.035 Uiso 1 1 calc R . . C86 C 0.8744(4) 0.812(2) 0.7164(5) 0.035(4) Uani 1 1 d . . . H86A H 0.8918 0.7167 0.7214 0.053 Uiso 1 1 calc R . . H86B H 0.8593 0.8237 0.7450 0.053 Uiso 1 1 calc R . . H86C H 0.8869 0.9253 0.7108 0.053 Uiso 1 1 calc R . . C90 C 0.6833(4) 0.907(2) 0.5241(6) 0.047(3) Uani 1 1 d U . . C91 C 0.6466(4) 0.863(2) 0.5383(6) 0.040(4) Uani 1 1 d U . . H91A H 0.6386 0.7565 0.5210 0.060 Uiso 1 1 calc R . . H91B H 0.6309 0.9637 0.5305 0.060 Uiso 1 1 calc R . . H91C H 0.6458 0.8402 0.5729 0.060 Uiso 1 1 calc R . . C92 C 0.6922(4) 0.4413(19) 0.5822(5) 0.027(3) Uani 1 1 d U . . C93 C 0.6591(4) 0.384(2) 0.6085(5) 0.041(4) Uani 1 1 d U . . H93A H 0.6655 0.3015 0.6344 0.061 Uiso 1 1 calc R . . H93B H 0.6428 0.3250 0.5861 0.061 Uiso 1 1 calc R . . H93C H 0.6474 0.4896 0.6222 0.061 Uiso 1 1 calc R . . C94 C 0.1219(5) 0.754(2) 0.3370(6) 0.044(4) Uani 1 1 d U . . C95 C 0.0907(6) 0.674(3) 0.3650(8) 0.078(6) Uani 1 1 d U . . H95A H 0.0997 0.5961 0.3904 0.116 Uiso 1 1 calc R . . H95B H 0.0756 0.6053 0.3431 0.116 Uiso 1 1 calc R . . H95C H 0.0767 0.7711 0.3793 0.116 Uiso 1 1 calc R . . C96 C 0.0377(5) 0.280(3) 0.3517(6) 0.049(4) Uani 1 1 d U . . C97 C 0.0645(5) 0.181(3) 0.3205(7) 0.067(5) Uani 1 1 d U . . H97A H 0.0602 0.2094 0.2866 0.100 Uiso 1 1 calc R . . H97B H 0.0620 0.0521 0.3255 0.100 Uiso 1 1 calc R . . H97C H 0.0887 0.2180 0.3293 0.100 Uiso 1 1 calc R . . F1 F 0.0596(4) 0.471(3) 0.1747(6) 0.196(12) Uani 1 1 d . . . F2 F 0.0287(4) 0.744(2) 0.2501(6) 0.121(6) Uani 1 1 d . . . F3 F 0.0609(3) 0.773(3) 0.1846(7) 0.171(10) Uani 1 1 d . . . F4 F 0.0083(2) 0.6215(13) 0.1793(3) 0.054(3) Uani 1 1 d . . . F5 F 0.0812(2) 0.5846(14) 0.2426(3) 0.055(3) Uani 1 1 d . . . F6 F 0.0258(3) 0.454(2) 0.2424(5) 0.118(6) Uani 1 1 d . . . F7 F 0.1363(2) -0.0458(14) 0.4478(4) 0.059(3) Uani 1 1 d . . . F8 F 0.0948(3) 0.3177(14) 0.4752(4) 0.072(3) Uani 1 1 d . . . F9 F 0.1519(2) 0.2150(16) 0.4855(4) 0.071(3) Uani 1 1 d . . . F10 F 0.1278(3) 0.2166(15) 0.4094(4) 0.068(3) Uani 1 1 d . . . F11 F 0.0793(2) 0.0628(12) 0.4368(3) 0.050(2) Uani 1 1 d . . . F12 F 0.1032(2) 0.0503(17) 0.5120(3) 0.072(3) Uani 1 1 d . . . F13 F 0.1886(4) 0.3948(15) 0.6989(6) 0.117(6) Uani 1 1 d . . . F14 F 0.1873(4) 0.8126(18) 0.6843(7) 0.128(6) Uani 1 1 d . . . F15 F 0.2304(2) 0.6132(16) 0.7005(3) 0.059(3) Uani 1 1 d . . . F16 F 0.1959(3) 0.577(3) 0.6346(4) 0.145(8) Uani 1 1 d . . . F17 F 0.1461(2) 0.6007(15) 0.6774(4) 0.065(3) Uani 1 1 d . . . F18 F 0.1813(3) 0.633(2) 0.7453(4) 0.095(5) Uani 1 1 d . . . N1 N 0.8847(2) 0.6462(13) 0.4596(3) 0.015(2) Uani 1 1 d U . . N2 N 0.8454(3) 0.8523(14) 0.3954(4) 0.022(2) Uani 1 1 d U . . N3 N 0.8784(2) 1.1426(12) 0.4365(3) 0.011(2) Uani 1 1 d U . . N4 N 0.8806(3) 0.9399(14) 0.5206(4) 0.024(2) Uani 1 1 d U . . N11 N 0.9257(3) 0.5320(14) 0.3510(4) 0.021(2) Uani 1 1 d . . . N21 N 0.7600(3) 0.5596(15) 0.4535(4) 0.024(3) Uani 1 1 d U . . N31 N 0.9266(3) 1.0328(15) 0.3498(4) 0.025(3) Uani 1 1 d . . . N41 N 0.7566(3) 1.0649(13) 0.4062(3) 0.021(3) Uani 1 1 d . . . N51 N 0.9627(2) 1.2544(13) 0.4822(4) 0.017(2) Uani 1 1 d . . . N61 N 0.7899(3) 1.1631(13) 0.5542(3) 0.019(2) Uani 1 1 d U . . N71 N 0.9637(3) 0.7455(15) 0.4811(4) 0.028(3) Uani 1 1 d . . . N81 N 0.8077(3) 0.6816(15) 0.5932(4) 0.024(2) Uani 1 1 d U . . N90 N 0.7121(4) 0.9407(18) 0.5123(5) 0.047(3) Uani 1 1 d U . . N92 N 0.7176(4) 0.488(2) 0.5637(5) 0.047(4) Uani 1 1 d . . . N96 N 0.0188(4) 0.361(2) 0.3747(5) 0.053(4) Uani 1 1 d U . . O1 O 0.8659(2) 0.5273(11) 0.3754(3) 0.0159(18) Uani 1 1 d . . . O2 O 0.82014(19) 0.5633(10) 0.4385(3) 0.0153(18) Uani 1 1 d . . . O3 O 0.8663(2) 1.1241(12) 0.3451(3) 0.021(2) Uani 1 1 d . . . O4 O 0.8159(2) 1.1580(10) 0.3991(3) 0.0152(18) Uani 1 1 d U . . O5 O 0.9058(2) 1.2643(10) 0.5170(3) 0.0164(18) Uani 1 1 d . . . O6 O 0.8408(2) 1.2234(10) 0.5119(3) 0.0164(18) Uani 1 1 d . . . O7 O 0.9213(2) 0.6633(11) 0.5400(3) 0.022(2) Uani 1 1 d . . . O8 O 0.8568(2) 0.6296(11) 0.5440(3) 0.0159(18) Uani 1 1 d . . . P1 P 0.85520(8) 0.6622(4) 0.41834(12) 0.0157(7) Uani 1 1 d . . . P2 P 0.85407(8) 1.0579(4) 0.39673(11) 0.0165(7) Uani 1 1 d . . . P3 P 0.87698(8) 1.1277(4) 0.49448(10) 0.0130(7) Uani 1 1 d . . . P4 P 0.88623(8) 0.7319(4) 0.51223(11) 0.0139(7) Uani 1 1 d . . . P5 P 0.04487(10) 0.6037(7) 0.21139(14) 0.0383(10) Uani 1 1 d . . . P6 P 0.11559(10) 0.1386(6) 0.46049(14) 0.0407(11) Uani 1 1 d . . . P7 P 0.18834(9) 0.6048(6) 0.68914(13) 0.0327(9) 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 N94 0.043(7) 0.078(8) 0.045(7) -0.007(6) 0.000(6) -0.009(6) Ag1 0.0268(5) 0.0368(6) 0.0197(5) 0.0068(6) -0.0041(4) 0.0026(5) Ag2 0.0209(5) 0.0392(6) 0.0163(5) -0.0019(6) -0.0015(4) 0.0004(5) Ag3 0.0221(5) 0.0443(6) 0.0189(5) -0.0008(6) 0.0000(4) -0.0034(5) C11 0.017(6) 0.020(7) 0.013(6) -0.002(5) 0.003(5) 0.006(5) C12 0.026(7) 0.025(8) 0.016(6) 0.002(6) -0.001(5) -0.008(6) C13 0.024(5) 0.023(5) 0.018(4) 0.007(4) -0.001(4) -0.004(4) C14 0.033(8) 0.009(7) 0.030(7) 0.001(5) 0.024(6) -0.004(6) C15 0.019(4) 0.022(5) 0.018(4) -0.004(4) 0.006(4) 0.003(4) C16 0.048(9) 0.021(8) 0.013(6) 0.005(6) -0.004(6) -0.001(7) C21 0.015(4) 0.012(4) 0.010(4) 0.002(4) -0.005(4) 0.002(3) C22 0.024(7) 0.020(7) 0.020(7) -0.010(6) -0.011(6) 0.009(6) C23 0.019(6) 0.010(6) 0.018(6) -0.001(5) 0.000(5) -0.003(5) C24 0.017(7) 0.031(8) 0.022(7) 0.001(6) -0.001(5) -0.004(6) C25 0.018(7) 0.033(8) 0.018(6) -0.007(6) 0.003(5) -0.010(6) C26 0.027(8) 0.049(10) 0.027(8) -0.011(7) -0.005(6) 0.003(7) C31 0.022(6) 0.014(6) 0.015(6) -0.007(6) 0.007(5) 0.005(6) C32 0.024(5) 0.030(5) 0.020(5) 0.001(4) 0.006(4) -0.005(4) C33 0.032(8) 0.020(7) 0.023(7) -0.009(6) 0.017(6) -0.002(6) C34 0.030(8) 0.017(7) 0.053(9) 0.005(7) 0.022(7) -0.001(7) C35 0.030(5) 0.038(5) 0.039(5) -0.007(4) 0.003(4) 0.009(4) C36 0.067(12) 0.039(9) 0.040(9) -0.001(8) 0.034(9) -0.003(9) C41 0.011(4) 0.012(4) 0.016(4) 0.003(4) -0.005(3) -0.005(4) C42 0.026(7) 0.023(8) 0.014(6) 0.008(5) -0.006(5) -0.007(6) C43 0.041(8) 0.025(8) 0.014(7) 0.000(6) -0.013(6) 0.003(6) C44 0.024(5) 0.028(5) 0.020(5) -0.001(4) -0.010(4) -0.004(4) C45 0.011(6) 0.043(9) 0.022(7) 0.004(6) 0.005(5) -0.006(6) C46 0.055(10) 0.067(11) 0.019(8) -0.001(8) -0.018(7) -0.005(9) C51 0.022(7) 0.013(6) 0.017(7) -0.003(5) -0.010(5) 0.011(5) C52 0.023(7) 0.020(7) 0.026(7) -0.002(6) 0.002(5) 0.007(6) C53 0.033(8) 0.019(7) 0.031(7) -0.004(7) -0.010(6) 0.014(7) C54 0.022(7) 0.047(10) 0.034(8) 0.011(8) -0.008(7) 0.004(7) C55 0.023(5) 0.015(5) 0.025(6) -0.007(5) 0.001(5) 0.010(5) C56 0.037(9) 0.044(9) 0.037(9) -0.006(8) -0.023(7) 0.018(7) C61 0.031(8) 0.008(6) 0.016(7) 0.001(5) 0.005(6) 0.001(6) C62 0.014(6) 0.035(8) 0.010(6) 0.003(6) -0.002(5) 0.000(6) C63 0.034(8) 0.013(7) 0.017(6) 0.008(5) -0.004(6) 0.001(6) C64 0.019(7) 0.054(10) 0.022(7) -0.011(7) 0.001(6) -0.005(7) C65 0.033(8) 0.043(10) 0.030(8) 0.025(7) 0.012(6) 0.000(7) C66 0.041(9) 0.030(8) 0.014(6) -0.006(6) -0.004(6) 0.001(7) C71 0.012(6) 0.016(6) 0.019(7) -0.001(6) -0.002(5) -0.001(5) C72 0.021(6) 0.020(7) 0.019(6) 0.009(6) -0.004(5) 0.010(6) C73 0.015(5) 0.025(6) 0.035(6) -0.010(6) -0.007(5) 0.011(5) C74 0.015(7) 0.062(10) 0.034(9) 0.002(8) 0.000(6) -0.001(7) C75 0.023(8) 0.052(10) 0.036(9) 0.018(8) 0.012(6) 0.005(7) C76 0.024(8) 0.087(14) 0.039(9) -0.008(9) -0.006(7) 0.013(9) C81 0.023(6) 0.011(5) 0.019(6) 0.007(5) -0.004(5) -0.004(5) C82 0.027(7) 0.027(8) 0.019(7) 0.003(6) -0.004(6) 0.002(6) C83 0.030(8) 0.031(8) 0.015(7) -0.012(6) 0.006(6) -0.002(6) C84 0.036(8) 0.060(10) 0.010(6) 0.000(7) 0.007(6) 0.021(8) C85 0.020(7) 0.045(9) 0.024(8) 0.000(7) 0.002(6) 0.012(7) C86 0.038(9) 0.045(9) 0.023(7) -0.001(7) -0.001(6) 0.005(7) C90 0.047(3) 0.047(3) 0.047(3) 0.0002(8) 0.0001(8) -0.0002(8) C91 0.040(4) 0.040(4) 0.040(4) 0.0002(10) 0.0002(10) -0.0002(10) C92 0.033(7) 0.030(7) 0.019(6) 0.005(5) -0.001(5) 0.006(6) C93 0.031(6) 0.050(6) 0.042(6) 0.010(5) 0.003(5) -0.012(5) C94 0.045(7) 0.047(8) 0.041(7) -0.008(6) -0.006(6) -0.001(7) C95 0.077(9) 0.081(10) 0.075(9) -0.005(8) 0.002(8) -0.026(8) C96 0.043(7) 0.059(8) 0.043(8) 0.004(7) -0.003(7) 0.006(7) C97 0.060(8) 0.081(9) 0.059(8) 0.003(8) 0.003(7) 0.010(8) F1 0.109(12) 0.36(3) 0.120(12) -0.166(16) -0.070(10) 0.148(15) F2 0.066(8) 0.142(13) 0.155(14) -0.059(11) -0.016(9) 0.038(9) F3 0.060(8) 0.24(2) 0.213(18) 0.177(17) -0.054(10) -0.051(11) F4 0.032(5) 0.069(7) 0.060(6) 0.034(5) -0.005(4) 0.003(5) F5 0.035(5) 0.084(7) 0.044(5) 0.017(5) -0.005(4) 0.005(5) F6 0.072(8) 0.163(14) 0.118(11) 0.091(11) -0.045(8) -0.042(9) F7 0.032(5) 0.086(8) 0.059(6) 0.008(6) 0.004(4) 0.007(5) F8 0.054(6) 0.061(6) 0.102(9) -0.015(6) -0.012(6) 0.022(5) F9 0.031(5) 0.106(8) 0.074(7) -0.046(7) -0.013(5) -0.002(5) F10 0.060(7) 0.087(8) 0.057(7) 0.016(6) 0.006(5) 0.001(6) F11 0.037(5) 0.067(6) 0.046(5) -0.018(5) -0.009(4) 0.011(5) F12 0.038(5) 0.146(10) 0.032(5) 0.012(6) 0.000(4) 0.022(6) F13 0.111(10) 0.044(7) 0.196(16) 0.001(9) -0.082(11) -0.012(7) F14 0.090(10) 0.070(9) 0.225(18) 0.045(10) -0.080(11) -0.027(8) F15 0.025(5) 0.121(9) 0.030(5) 0.016(6) -0.001(4) -0.020(6) F16 0.067(8) 0.34(2) 0.031(6) -0.047(10) -0.016(5) 0.070(12) F17 0.029(5) 0.084(8) 0.082(7) 0.005(6) -0.016(5) 0.004(5) F18 0.047(6) 0.188(14) 0.050(6) -0.038(8) 0.009(5) 0.008(8) N1 0.014(4) 0.017(4) 0.014(4) 0.005(3) -0.004(3) -0.001(3) N2 0.021(3) 0.022(3) 0.022(3) -0.0009(10) 0.0004(10) 0.0002(10) N3 0.012(4) 0.009(4) 0.011(4) 0.003(3) 0.001(3) 0.002(3) N4 0.022(4) 0.033(4) 0.017(4) -0.002(4) 0.002(3) -0.001(4) N11 0.021(6) 0.027(6) 0.015(5) 0.000(5) 0.000(4) 0.005(5) N21 0.019(4) 0.033(5) 0.020(4) -0.003(4) -0.002(3) -0.003(4) N31 0.032(6) 0.027(6) 0.016(5) 0.004(5) -0.004(5) -0.004(5) N41 0.025(6) 0.022(6) 0.017(6) -0.004(4) 0.000(4) -0.006(5) N51 0.018(5) 0.016(5) 0.018(5) 0.001(5) -0.004(5) -0.003(4) N61 0.022(4) 0.019(4) 0.015(4) -0.006(3) 0.004(3) -0.004(3) N71 0.022(6) 0.039(7) 0.023(6) -0.002(6) -0.002(5) -0.003(5) N81 0.023(4) 0.030(4) 0.018(4) 0.005(4) -0.001(3) 0.000(4) N90 0.047(3) 0.047(3) 0.047(3) 0.0001(8) 0.0002(8) -0.0002(8) N92 0.031(8) 0.072(10) 0.039(8) 0.013(7) -0.001(6) -0.006(7) N96 0.044(7) 0.063(8) 0.051(7) 0.002(6) -0.001(6) 0.010(6) O1 0.012(4) 0.011(4) 0.025(5) 0.005(4) 0.002(4) -0.003(3) O2 0.013(4) 0.022(5) 0.012(4) 0.002(3) -0.002(3) 0.002(3) O3 0.021(4) 0.032(5) 0.009(4) 0.003(4) 0.007(3) 0.009(4) O4 0.020(3) 0.009(3) 0.017(3) -0.007(3) -0.005(3) 0.004(3) O5 0.018(4) 0.016(4) 0.015(4) 0.002(3) -0.001(3) 0.008(4) O6 0.017(4) 0.016(4) 0.017(4) -0.006(4) 0.000(3) 0.011(4) O7 0.020(4) 0.027(5) 0.020(5) 0.003(4) 0.000(4) -0.001(4) O8 0.018(4) 0.019(5) 0.011(4) -0.010(4) 0.002(3) 0.001(4) P1 0.0163(15) 0.0194(17) 0.0113(14) 0.0009(15) -0.0005(14) 0.0028(13) P2 0.0171(16) 0.0230(19) 0.0093(15) 0.0063(13) 0.0013(13) 0.0011(14) P3 0.0152(15) 0.0126(16) 0.0113(16) -0.0003(13) -0.0011(11) 0.0029(13) P4 0.0158(16) 0.0164(16) 0.0095(15) 0.0008(13) -0.0007(13) 0.0007(14) P5 0.0266(19) 0.055(3) 0.033(2) 0.015(2) 0.0049(16) 0.005(2) P6 0.027(2) 0.062(3) 0.033(2) -0.008(2) -0.0049(17) 0.011(2) P7 0.0249(18) 0.045(2) 0.0283(19) -0.002(2) 0.0017(15) -0.0037(19) _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 N94 C94 1.15(2) . ? Ag1 N51 2.172(10) 1_545 ? Ag1 N11 2.180(10) . ? Ag2 N21 2.181(10) . ? Ag2 N81 2.190(10) . ? Ag2 N92 2.428(13) . ? Ag3 N61 2.153(10) . ? Ag3 N41 2.181(9) . ? Ag3 N90 2.397(14) . ? C11 N11 1.331(14) . ? C11 C12 1.360(16) . ? C11 O1 1.409(13) . ? C12 C13 1.395(17) . ? C12 H12 0.9300 . ? C13 C14 1.367(18) . ? C13 C16 1.511(16) . ? C14 C15 1.343(17) . ? C14 H14 0.9300 . ? C15 N11 1.375(14) . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 N21 1.314(15) . ? C21 C22 1.364(16) . ? C21 O2 1.403(12) . ? C22 C23 1.376(16) . ? C22 H22 0.9300 . ? C23 C24 1.408(16) . ? C23 C26 1.494(17) . ? C24 C25 1.350(16) . ? C24 H24 0.9300 . ? C25 N21 1.378(15) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C31 N31 1.309(15) . ? C31 C32 1.377(16) . ? C31 O3 1.405(13) . ? C32 C33 1.411(18) . ? C32 H32 0.9300 . ? C33 C34 1.38(2) . ? C33 C36 1.484(19) . ? C34 C35 1.374(19) . ? C34 H34 0.9300 . ? C35 N31 1.348(17) . ? C35 H35 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C41 N41 1.342(14) . ? C41 C42 1.369(16) . ? C41 O4 1.402(13) . ? C42 C43 1.373(17) . ? C42 H42 0.9300 . ? C43 C44 1.393(18) . ? C43 C46 1.509(18) . ? C44 C45 1.353(17) . ? C44 H44 0.9300 . ? C45 N41 1.341(15) . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C51 N51 1.330(15) . ? C51 C52 1.362(16) . ? C51 O5 1.419(13) . ? C52 C53 1.411(18) . ? C52 H52 0.9300 . ? C53 C54 1.385(19) . ? C53 C56 1.509(17) . ? C54 C55 1.384(18) . ? C54 H54 0.9300 . ? C55 N51 1.350(14) . ? C55 H55 0.9300 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C61 N61 1.335(15) . ? C61 O6 1.369(13) . ? C61 C62 1.396(16) . ? C62 C63 1.390(17) . ? C62 H62 0.9300 . ? C63 C64 1.405(17) . ? C63 C66 1.495(16) . ? C64 C65 1.352(19) . ? C64 H64 0.9300 . ? C65 N61 1.384(16) . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C71 N71 1.289(16) . ? C71 O7 1.409(13) . ? C71 C72 1.409(15) . ? C72 C73 1.411(16) . ? C72 H72 0.9300 . ? C73 C74 1.343(19) . ? C73 C76 1.521(18) . ? C74 C75 1.369(18) . ? C74 H74 0.9300 . ? C75 N71 1.352(16) . ? C75 H75 0.9300 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C81 N81 1.339(16) . ? C81 C82 1.377(16) . ? C81 O8 1.394(14) . ? C82 C83 1.386(17) . ? C82 H82 0.9300 . ? C83 C84 1.412(18) . ? C83 C86 1.455(17) . ? C84 C85 1.369(18) . ? C84 H84 0.9300 . ? C85 N81 1.318(16) . ? C85 H85 0.9300 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C90 N90 1.138(18) . ? C90 C91 1.44(2) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 N92 1.116(17) . ? C92 C93 1.476(19) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 C95 1.50(2) . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 N96 1.109(19) . ? C96 C97 1.49(2) . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 0.9600 . ? F1 P5 1.497(13) . ? F2 P5 1.593(14) . ? F3 P5 1.559(14) . ? F4 P5 1.610(9) . ? F5 P5 1.589(9) . ? F6 P5 1.555(12) . ? F7 P6 1.591(11) . ? F8 P6 1.571(10) . ? F9 P6 1.601(9) . ? F10 P6 1.571(10) . ? F11 P6 1.584(9) . ? F12 P6 1.614(10) . ? F13 P7 1.563(12) . ? F14 P7 1.530(13) . ? F15 P7 1.578(8) . ? F16 P7 1.529(11) . ? F17 P7 1.588(9) . ? F18 P7 1.567(10) . ? N1 P1 1.567(9) . ? N1 P4 1.569(10) . ? N2 P2 1.542(11) . ? N2 P1 1.570(11) . ? N3 P2 1.537(9) . ? N3 P3 1.587(9) . ? N4 P4 1.556(11) . ? N4 P3 1.557(11) . ? N51 Ag1 2.172(10) 1_565 ? O1 P1 1.584(9) . ? O2 P1 1.579(8) . ? O3 P2 1.557(8) . ? O4 P2 1.586(8) . ? O5 P3 1.583(8) . ? O6 P3 1.580(8) . ? O7 P4 1.581(8) . ? O8 P4 1.577(8) . ? 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 N51 Ag1 N11 170.6(4) 1_545 . ? N21 Ag2 N81 157.9(4) . . ? N21 Ag2 N92 96.0(4) . . ? N81 Ag2 N92 106.1(4) . . ? N61 Ag3 N41 161.9(4) . . ? N61 Ag3 N90 99.9(4) . . ? N41 Ag3 N90 97.6(4) . . ? N11 C11 C12 126.0(11) . . ? N11 C11 O1 113.8(10) . . ? C12 C11 O1 119.7(10) . . ? C11 C12 C13 117.5(12) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C14 C13 C12 117.1(11) . . ? C14 C13 C16 123.4(11) . . ? C12 C13 C16 119.5(12) . . ? C15 C14 C13 122.6(11) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 N11 121.2(11) . . ? C14 C15 H15 119.4 . . ? N11 C15 H15 119.4 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N21 C21 C22 124.2(11) . . ? N21 C21 O2 111.7(10) . . ? C22 C21 O2 123.9(11) . . ? C21 C22 C23 120.2(12) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 116.2(11) . . ? C22 C23 C26 122.7(11) . . ? C24 C23 C26 121.2(11) . . ? C25 C24 C23 120.6(12) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 N21 122.0(11) . . ? C24 C25 H25 119.0 . . ? N21 C25 H25 119.0 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N31 C31 C32 126.9(11) . . ? N31 C31 O3 117.3(10) . . ? C32 C31 O3 115.8(10) . . ? C31 C32 C33 117.7(13) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 116.5(12) . . ? C34 C33 C36 122.6(13) . . ? C32 C33 C36 120.8(14) . . ? C35 C34 C33 119.9(13) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N31 C35 C34 124.4(13) . . ? N31 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N41 C41 C42 123.6(10) . . ? N41 C41 O4 113.6(9) . . ? C42 C41 O4 122.6(10) . . ? C41 C42 C43 119.3(12) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C44 117.2(11) . . ? C42 C43 C46 121.2(13) . . ? C44 C43 C46 121.6(13) . . ? C45 C44 C43 120.3(12) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? N41 C45 C44 122.8(12) . . ? N41 C45 H45 118.6 . . ? C44 C45 H45 118.6 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N51 C51 C52 127.1(11) . . ? N51 C51 O5 113.7(9) . . ? C52 C51 O5 119.0(11) . . ? C51 C52 C53 117.0(12) . . ? C51 C52 H52 121.5 . . ? C53 C52 H52 121.5 . . ? C54 C53 C52 117.8(12) . . ? C54 C53 C56 122.4(12) . . ? C52 C53 C56 119.9(12) . . ? C55 C54 C53 119.7(12) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? N51 C55 C54 123.3(12) . . ? N51 C55 H55 118.4 . . ? C54 C55 H55 118.4 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N61 C61 O6 112.1(10) . . ? N61 C61 C62 125.2(11) . . ? O6 C61 C62 122.7(11) . . ? C63 C62 C61 117.7(11) . . ? C63 C62 H62 121.2 . . ? C61 C62 H62 121.2 . . ? C62 C63 C64 118.3(11) . . ? C62 C63 C66 119.6(12) . . ? C64 C63 C66 122.1(12) . . ? C65 C64 C63 119.8(13) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 N61 123.4(13) . . ? C64 C65 H65 118.3 . . ? N61 C65 H65 118.3 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N71 C71 O7 118.5(10) . . ? N71 C71 C72 127.8(11) . . ? O7 C71 C72 113.5(10) . . ? C71 C72 C73 114.3(11) . . ? C71 C72 H72 122.9 . . ? C73 C72 H72 122.9 . . ? C74 C73 C72 118.2(11) . . ? C74 C73 C76 124.9(12) . . ? C72 C73 C76 116.9(12) . . ? C73 C74 C75 122.4(12) . . ? C73 C74 H74 118.8 . . ? C75 C74 H74 118.8 . . ? N71 C75 C74 121.2(13) . . ? N71 C75 H75 119.4 . . ? C74 C75 H75 119.4 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N81 C81 C82 122.9(11) . . ? N81 C81 O8 113.4(10) . . ? C82 C81 O8 123.4(11) . . ? C81 C82 C83 120.9(12) . . ? C81 C82 H82 119.5 . . ? C83 C82 H82 119.5 . . ? C82 C83 C84 114.6(12) . . ? C82 C83 C86 122.9(12) . . ? C84 C83 C86 122.4(12) . . ? C85 C84 C83 120.8(12) . . ? C85 C84 H84 119.6 . . ? C83 C84 H84 119.6 . . ? N81 C85 C84 123.3(12) . . ? N81 C85 H85 118.4 . . ? C84 C85 H85 118.4 . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N90 C90 C91 179.2(18) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N92 C92 C93 177.4(16) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N94 C94 C95 179(2) . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? N96 C96 C97 177(2) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? P1 N1 P4 130.7(6) . . ? P2 N2 P1 144.3(7) . . ? P2 N3 P3 131.0(6) . . ? P4 N4 P3 144.3(7) . . ? C11 N11 C15 115.6(10) . . ? C11 N11 Ag1 122.6(8) . . ? C15 N11 Ag1 121.8(8) . . ? C21 N21 C25 116.7(10) . . ? C21 N21 Ag2 121.5(8) . . ? C25 N21 Ag2 121.7(8) . . ? C31 N31 C35 114.6(11) . . ? C45 N41 C41 116.7(10) . . ? C45 N41 Ag3 124.5(8) . . ? C41 N41 Ag3 118.7(8) . . ? C51 N51 C55 115.1(10) . . ? C51 N51 Ag1 122.0(7) . 1_565 ? C55 N51 Ag1 122.9(8) . 1_565 ? C61 N61 C65 115.5(11) . . ? C61 N61 Ag3 121.2(8) . . ? C65 N61 Ag3 123.3(9) . . ? C71 N71 C75 116.0(11) . . ? C85 N81 C81 117.4(11) . . ? C85 N81 Ag2 122.1(9) . . ? C81 N81 Ag2 120.5(8) . . ? C90 N90 Ag3 162.5(13) . . ? C92 N92 Ag2 175.1(13) . . ? C11 O1 P1 120.4(7) . . ? C21 O2 P1 129.5(7) . . ? C31 O3 P2 128.0(7) . . ? C41 O4 P2 122.4(7) . . ? C51 O5 P3 120.1(7) . . ? C61 O6 P3 126.5(7) . . ? C71 O7 P4 126.9(7) . . ? C81 O8 P4 125.3(7) . . ? N1 P1 N2 120.8(5) . . ? N1 P1 O2 106.4(5) . . ? N2 P1 O2 111.0(5) . . ? N1 P1 O1 108.1(5) . . ? N2 P1 O1 108.5(5) . . ? O2 P1 O1 100.0(4) . . ? N3 P2 N2 122.1(5) . . ? N3 P2 O3 110.1(5) . . ? N2 P2 O3 110.1(5) . . ? N3 P2 O4 107.4(5) . . ? N2 P2 O4 105.7(5) . . ? O3 P2 O4 98.6(4) . . ? N4 P3 O6 109.1(5) . . ? N4 P3 O5 108.9(5) . . ? O6 P3 O5 99.6(4) . . ? N4 P3 N3 120.9(5) . . ? O6 P3 N3 107.3(4) . . ? O5 P3 N3 108.8(5) . . ? N4 P4 N1 121.5(5) . . ? N4 P4 O8 107.2(5) . . ? N1 P4 O8 106.7(5) . . ? N4 P4 O7 110.5(5) . . ? N1 P4 O7 109.9(5) . . ? O8 P4 O7 98.4(4) . . ? F1 P5 F6 93.9(13) . . ? F1 P5 F3 93.9(13) . . ? F6 P5 F3 172.0(12) . . ? F1 P5 F5 89.7(6) . . ? F6 P5 F5 91.5(6) . . ? F3 P5 F5 90.2(6) . . ? F1 P5 F2 179.3(8) . . ? F6 P5 F2 85.9(9) . . ? F3 P5 F2 86.3(11) . . ? F5 P5 F2 90.9(6) . . ? F1 P5 F4 89.6(6) . . ? F6 P5 F4 88.6(5) . . ? F3 P5 F4 89.8(6) . . ? F5 P5 F4 179.3(6) . . ? F2 P5 F4 89.8(6) . . ? F8 P6 F10 93.5(6) . . ? F8 P6 F11 89.3(5) . . ? F10 P6 F11 90.4(5) . . ? F8 P6 F7 177.7(6) . . ? F10 P6 F7 88.9(6) . . ? F11 P6 F7 91.0(5) . . ? F8 P6 F9 90.2(6) . . ? F10 P6 F9 90.7(6) . . ? F11 P6 F9 178.8(6) . . ? F7 P6 F9 89.4(5) . . ? F8 P6 F12 88.6(6) . . ? F10 P6 F12 177.7(7) . . ? F11 P6 F12 88.6(5) . . ? F7 P6 F12 89.1(6) . . ? F9 P6 F12 90.3(6) . . ? F16 P7 F14 93.1(11) . . ? F16 P7 F13 91.8(10) . . ? F14 P7 F13 175.1(10) . . ? F16 P7 F18 179.0(6) . . ? F14 P7 F18 87.0(9) . . ? F13 P7 F18 88.1(9) . . ? F16 P7 F15 91.0(6) . . ? F14 P7 F15 90.2(7) . . ? F13 P7 F15 90.0(7) . . ? F18 P7 F15 88.0(5) . . ? F16 P7 F17 88.9(6) . . ? F14 P7 F17 88.7(6) . . ? F13 P7 F17 91.2(6) . . ? F18 P7 F17 92.2(6) . . ? F15 P7 F17 178.8(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.021 _refine_diff_density_min -1.595 _refine_diff_density_rms 0.153 data_[ag4mel](cf3so3)4 _database_code_depnum_ccdc_archive 'CCDC 926378' #TrackingRef 'Revised Brodie Ag combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H51 Ag4 F3 N15 O11 P4 S, C F3 O4 S, 2(C F3 O3 S), C2 N, O' _chemical_formula_sum 'C60 H51 Ag4 F12 N16 O22 P4 S4' _chemical_formula_weight 2259.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 '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 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9201(12) _cell_length_b 17.4130(14) _cell_length_c 17.8452(14) _cell_angle_alpha 100.983(4) _cell_angle_beta 92.204(4) _cell_angle_gamma 102.358(4) _cell_volume 4430.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 198(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 0.280 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2238 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780589 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63468 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 21808 _reflns_number_gt 12795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two triflate ions are well ordered and coordinated to silver ions, one through a single oxygen atoms and the other in a mu-1,3 bridging a pair of solver ions. For the other two triflate ions, one is disordered in a single site and the other is disordered along with solvent species over several sites. ; _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^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21808 _refine_ls_number_parameters 1346 _refine_ls_number_restraints 1310 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.013 _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 O11 O 0.3828(4) 1.0029(4) 0.4261(3) 0.0711(15) Uani 1 1 d U . . Ag1 Ag 0.48561(3) 0.14903(3) 0.72246(3) 0.04171(13) Uani 1 1 d . . . Ag2 Ag 0.20626(3) 0.29534(3) 1.06552(3) 0.03850(12) Uani 1 1 d . . . Ag3 Ag 0.09030(3) 0.07286(3) 0.98585(2) 0.03475(12) Uani 1 1 d . . . Ag4 Ag 0.28792(3) 0.21318(3) 0.63260(3) 0.04186(13) Uani 1 1 d . . . N11 N 0.5580(3) 0.2629(3) 0.7951(3) 0.0321(10) Uani 1 1 d U . . N21 N 0.3193(3) 0.2479(3) 1.1067(2) 0.0312(10) Uani 1 1 d U A . N31 N 0.3937(3) 0.0303(3) 0.6852(2) 0.0314(10) Uani 1 1 d U . . N41 N 0.2060(3) 0.0253(3) 1.0177(2) 0.0277(9) Uani 1 1 d U . . N51 N 0.1878(3) 0.0962(3) 0.6072(2) 0.0316(10) Uani 1 1 d U A . N61 N -0.0106(3) 0.1260(3) 0.9367(2) 0.0273(9) Uani 1 1 d U . . N71 N 0.3655(3) 0.3338(3) 0.6911(3) 0.0359(11) Uani 1 1 d U A . N81 N 0.1200(3) 0.3468(3) 0.9961(2) 0.0297(10) Uani 1 1 d U A . P1 P 0.38518(8) 0.22869(8) 0.91881(7) 0.0223(3) Uani 1 1 d . . . P2 P 0.28116(8) 0.07249(8) 0.85179(7) 0.0218(3) Uani 1 1 d . . . P3 P 0.14242(8) 0.14057(8) 0.79433(7) 0.0220(3) Uani 1 1 d . . . P4 P 0.25348(8) 0.29656(8) 0.85149(7) 0.0231(3) Uani 1 1 d . . . N1 N 0.3304(3) 0.1410(2) 0.9200(2) 0.0236(9) Uani 1 1 d U . . N2 N 0.2145(3) 0.0866(2) 0.7885(2) 0.0231(9) Uani 1 1 d U . . N3 N 0.1645(3) 0.2283(2) 0.8432(2) 0.0236(9) Uani 1 1 d U . . N4 N 0.3520(3) 0.2820(2) 0.8665(2) 0.0254(9) Uani 1 1 d U . . O1 O 0.4859(2) 0.2223(2) 0.89676(19) 0.0263(8) Uani 1 1 d U . . O2 O 0.3968(2) 0.2787(2) 1.00494(19) 0.0276(8) Uani 1 1 d U A . O3 O 0.3597(2) 0.0355(2) 0.80913(18) 0.0266(8) Uani 1 1 d U . . O4 O 0.2253(2) 0.0023(2) 0.88975(19) 0.0259(8) Uani 1 1 d U . . O5 O 0.1138(2) 0.1455(2) 0.70887(19) 0.0274(8) Uani 1 1 d U A . O6 O 0.0516(2) 0.0926(2) 0.8237(2) 0.0276(8) Uani 1 1 d U . . O7 O 0.2561(2) 0.3335(2) 0.7767(2) 0.0289(8) Uani 1 1 d U A . O8 O 0.2393(2) 0.3658(2) 0.91921(19) 0.0274(8) Uani 1 1 d U A . C11 C 0.5448(3) 0.2825(3) 0.8684(3) 0.0259(11) Uani 1 1 d U . . C12 C 0.5870(4) 0.3529(3) 0.9170(3) 0.0353(12) Uani 1 1 d U . . H12 H 0.5751 0.3627 0.9683 0.042 Uiso 1 1 calc R . . C13 C 0.6481(4) 0.4096(4) 0.8874(4) 0.0444(15) Uani 1 1 d U . . C14 C 0.6627(4) 0.3906(4) 0.8104(4) 0.0450(15) Uani 1 1 d U . . H14 H 0.7032 0.4267 0.7883 0.054 Uiso 1 1 calc R . . C15 C 0.6167(4) 0.3183(4) 0.7673(3) 0.0405(14) Uani 1 1 d U . . H15 H 0.6268 0.3068 0.7157 0.049 Uiso 1 1 calc R . . C16 C 0.6968(6) 0.4876(5) 0.9386(4) 0.073(2) Uani 1 1 d U . . H16A H 0.7365 0.5194 0.9095 0.110 Uiso 1 1 calc R . . H16B H 0.7328 0.4768 0.9795 0.110 Uiso 1 1 calc R . . H16C H 0.6522 0.5162 0.9596 0.110 Uiso 1 1 calc R . . C21 C 0.3940(3) 0.2453(3) 1.0694(3) 0.0268(11) Uani 1 1 d U . . C22 C 0.4683(4) 0.2187(3) 1.0959(3) 0.0324(12) Uani 1 1 d U A . H22 H 0.5202 0.2195 1.0685 0.039 Uiso 1 1 calc R . . C23 C 0.4641(4) 0.1910(4) 1.1632(3) 0.0371(13) Uani 1 1 d U . . C24 C 0.3853(4) 0.1937(4) 1.2021(3) 0.0376(13) Uani 1 1 d U A . H24 H 0.3803 0.1758 1.2479 0.045 Uiso 1 1 calc R . . C25 C 0.3162(4) 0.2218(4) 1.1742(3) 0.0377(13) Uani 1 1 d U . . H25 H 0.2648 0.2235 1.2018 0.045 Uiso 1 1 calc R A . C26 C 0.5424(5) 0.1613(5) 1.1940(4) 0.0574(19) Uani 1 1 d U A . H26A H 0.5275 0.1037 1.1832 0.086 Uiso 1 1 calc R . . H26B H 0.5527 0.1810 1.2483 0.086 Uiso 1 1 calc R . . H26C H 0.5970 0.1803 1.1700 0.086 Uiso 1 1 calc R . . C31 C 0.3464(3) -0.0079(3) 0.7336(3) 0.0266(11) Uani 1 1 d U . . C32 C 0.2928(3) -0.0845(3) 0.7153(3) 0.0319(12) Uani 1 1 d U . . H32 H 0.2624 -0.1080 0.7527 0.038 Uiso 1 1 calc R . . C33 C 0.2846(4) -0.1262(3) 0.6402(3) 0.0358(12) Uani 1 1 d U . . C34 C 0.3328(4) -0.0877(4) 0.5878(3) 0.0375(13) Uani 1 1 d U . . H34 H 0.3294 -0.1134 0.5368 0.045 Uiso 1 1 calc R . . C35 C 0.3857(4) -0.0112(4) 0.6119(3) 0.0379(13) Uani 1 1 d U . . H35 H 0.4179 0.0134 0.5759 0.046 Uiso 1 1 calc R . . C36 C 0.2261(5) -0.2098(4) 0.6160(4) 0.0579(19) Uani 1 1 d U . . H36A H 0.1884 -0.2135 0.5701 0.087 Uiso 1 1 calc R . . H36B H 0.1875 -0.2221 0.6560 0.087 Uiso 1 1 calc R . . H36C H 0.2650 -0.2474 0.6065 0.087 Uiso 1 1 calc R . . C41 C 0.2539(3) -0.0047(3) 0.9636(3) 0.0242(10) Uani 1 1 d U . . C42 C 0.3248(4) -0.0414(3) 0.9744(3) 0.0304(11) Uani 1 1 d U . . H42 H 0.3540 -0.0632 0.9332 0.037 Uiso 1 1 calc R . . C43 C 0.3516(4) -0.0451(3) 1.0485(3) 0.0342(12) Uani 1 1 d U . . C44 C 0.3042(4) -0.0121(3) 1.1062(3) 0.0355(12) Uani 1 1 d U . . H44 H 0.3211 -0.0123 1.1569 0.043 Uiso 1 1 calc R . . C45 C 0.2321(4) 0.0210(3) 1.0896(3) 0.0322(12) Uani 1 1 d U . . H45 H 0.2001 0.0414 1.1296 0.039 Uiso 1 1 calc R . . C46 C 0.4270(5) -0.0855(4) 1.0649(4) 0.0540(18) Uani 1 1 d U . . H46A H 0.4045 -0.1427 1.0515 0.081 Uiso 1 1 calc R . . H46B H 0.4474 -0.0699 1.1184 0.081 Uiso 1 1 calc R . . H46C H 0.4776 -0.0698 1.0353 0.081 Uiso 1 1 calc R . . C51 C 0.1154(3) 0.0827(3) 0.6482(3) 0.0280(11) Uani 1 1 d U . . C52 C 0.0459(4) 0.0147(3) 0.6343(3) 0.0321(12) Uani 1 1 d U A . H52 H -0.0031 0.0096 0.6650 0.039 Uiso 1 1 calc R . . C53 C 0.0508(4) -0.0461(3) 0.5733(3) 0.0358(12) Uani 1 1 d U . . C54 C 0.1252(4) -0.0348(4) 0.5295(3) 0.0424(14) Uani 1 1 d U A . H54 H 0.1305 -0.0748 0.4883 0.051 Uiso 1 1 calc R . . C55 C 0.1917(4) 0.0363(4) 0.5473(3) 0.0397(14) Uani 1 1 d U . . H55 H 0.2410 0.0433 0.5170 0.048 Uiso 1 1 calc R A . C56 C -0.0232(5) -0.1231(4) 0.5572(4) 0.0522(17) Uani 1 1 d U A . H56A H -0.0484 -0.1326 0.6042 0.078 Uiso 1 1 calc R . . H56B H 0.0030 -0.1672 0.5351 0.078 Uiso 1 1 calc R . . H56C H -0.0712 -0.1185 0.5221 0.078 Uiso 1 1 calc R . . C61 C -0.0116(3) 0.1303(3) 0.8637(3) 0.0270(11) Uani 1 1 d U . . C62 C -0.0708(3) 0.1638(3) 0.8264(3) 0.0328(12) Uani 1 1 d U . . H62 H -0.0682 0.1650 0.7747 0.039 Uiso 1 1 calc R . . C63 C -0.1357(4) 0.1963(3) 0.8697(4) 0.0370(13) Uani 1 1 d U . . C64 C -0.1369(4) 0.1908(3) 0.9453(3) 0.0355(12) Uani 1 1 d U . . H64 H -0.1804 0.2102 0.9748 0.043 Uiso 1 1 calc R . . C65 C -0.0745(4) 0.1571(3) 0.9774(3) 0.0336(12) Uani 1 1 d U . . H65 H -0.0756 0.1553 1.0292 0.040 Uiso 1 1 calc R . . C66 C -0.2035(5) 0.2334(4) 0.8322(4) 0.0562(18) Uani 1 1 d U . . H66A H -0.2554 0.1921 0.8081 0.084 Uiso 1 1 calc R . . H66B H -0.1742 0.2604 0.7944 0.084 Uiso 1 1 calc R . . H66C H -0.2238 0.2714 0.8703 0.084 Uiso 1 1 calc R . . C71 C 0.3385(3) 0.3742(3) 0.7538(3) 0.0283(11) Uani 1 1 d U . . C72 C 0.3834(4) 0.4482(3) 0.7934(4) 0.0391(13) Uani 1 1 d U A . H72 H 0.3598 0.4732 0.8365 0.047 Uiso 1 1 calc R . . C73 C 0.4659(4) 0.4859(4) 0.7678(4) 0.0482(15) Uani 1 1 d U . . C74 C 0.4946(4) 0.4458(4) 0.7017(4) 0.0497(16) Uani 1 1 d U A . H74 H 0.5480 0.4694 0.6820 0.060 Uiso 1 1 calc R . . C75 C 0.4450(4) 0.3719(4) 0.6653(4) 0.0469(15) Uani 1 1 d U . . H75 H 0.4660 0.3463 0.6211 0.056 Uiso 1 1 calc R A . C76 C 0.5203(5) 0.5666(4) 0.8121(5) 0.075(2) Uani 1 1 d U A . H76A H 0.5850 0.5689 0.8095 0.113 Uiso 1 1 calc R . . H76B H 0.5060 0.5734 0.8646 0.113 Uiso 1 1 calc R . . H76C H 0.5044 0.6086 0.7902 0.113 Uiso 1 1 calc R . . C81 C 0.1498(3) 0.3747(3) 0.9343(3) 0.0264(11) Uani 1 1 d U . . C82 C 0.1035(4) 0.4105(3) 0.8892(3) 0.0346(12) Uani 1 1 d U A . H82 H 0.1297 0.4292 0.8478 0.041 Uiso 1 1 calc R . . C83 C 0.0152(4) 0.4182(4) 0.9073(4) 0.0434(14) Uani 1 1 d U . . C84 C -0.0169(4) 0.3902(4) 0.9705(4) 0.0491(16) Uani 1 1 d U A . H84 H -0.0752 0.3948 0.9846 0.059 Uiso 1 1 calc R . . C85 C 0.0352(4) 0.3557(4) 1.0131(4) 0.0416(14) Uani 1 1 d U . . H85 H 0.0111 0.3377 1.0556 0.050 Uiso 1 1 calc R A . C86 C -0.0408(5) 0.4540(5) 0.8577(5) 0.067(2) Uani 1 1 d U A . H86A H -0.0057 0.5053 0.8518 0.100 Uiso 1 1 calc R . . H86B H -0.0961 0.4608 0.8813 0.100 Uiso 1 1 calc R . . H86C H -0.0564 0.4189 0.8084 0.100 Uiso 1 1 calc R . . C90 C 0.4788(5) 0.1889(4) 0.5318(4) 0.0536(17) Uani 1 1 d U . . C91 C 0.4959(6) 0.2034(5) 0.4550(4) 0.069(2) Uani 1 1 d U . . H91A H 0.4995 0.1540 0.4217 0.104 Uiso 1 1 calc R . . H91B H 0.5528 0.2421 0.4572 0.104 Uiso 1 1 calc R . . H91C H 0.4465 0.2234 0.4356 0.104 Uiso 1 1 calc R . . N90 N 0.4632(5) 0.1789(4) 0.5910(4) 0.0704(18) Uani 1 1 d U . . C92A C 0.242(2) 0.2731(19) 0.4589(15) 0.059(6) Uani 0.450(3) 1 d PDU A 1 C93A C 0.1939(18) 0.3065(16) 0.4042(15) 0.098(8) Uani 0.450(3) 1 d PDU A 1 N92A N 0.277(3) 0.2587(18) 0.5092(16) 0.074(10) Uani 0.450(3) 1 d PDU A 1 C92B C 0.2538(19) 0.2551(15) 0.4476(11) 0.059(5) Uani 0.550(3) 1 d PDU A 2 C93B C 0.2232(14) 0.2692(12) 0.3731(9) 0.085(5) Uani 0.550(3) 1 d PDU A 2 N92B N 0.2795(15) 0.2380(14) 0.5002(10) 0.047(4) Uani 0.550(3) 1 d PDU A 2 C94A C 0.1685(17) 0.412(2) 1.2438(16) 0.068(5) Uani 0.550(3) 1 d PDU A 1 C95A C 0.0842(12) 0.4216(11) 1.2877(10) 0.069(4) Uani 0.550(3) 1 d PDU A 1 N91A N 0.2158(13) 0.3917(15) 1.2023(12) 0.073(7) Uani 0.550(3) 1 d PDU A 1 C94B C 0.147(2) 0.412(3) 1.2348(19) 0.068(6) Uani 0.450(3) 1 d PDU A 2 C95B C 0.117(3) 0.452(2) 1.3085(18) 0.158(17) Uani 0.450(3) 1 d PDU A 2 N91B N 0.1918(18) 0.3989(17) 1.1882(14) 0.062(6) Uani 0.450(3) 1 d PDU A 2 C100 C 0.2461(5) 0.9992(5) 0.3331(4) 0.0560(18) Uani 1 1 d U . . F11 F 0.1880(3) 0.9431(4) 0.3606(3) 0.0966(17) Uani 1 1 d U . . F12 F 0.2362(4) 1.0679(3) 0.3714(3) 0.1019(18) Uani 1 1 d U . . F13 F 0.2172(3) 0.9898(3) 0.2606(2) 0.0784(14) Uani 1 1 d U . . S1 S 0.36456(12) 0.98740(11) 0.34492(9) 0.0499(4) Uani 1 1 d . . . O12 O 0.3603(4) 0.9068(3) 0.3069(3) 0.0778(17) Uani 1 1 d U . . O13 O 0.4148(4) 1.0472(3) 0.3071(3) 0.0745(16) Uani 1 1 d U . . C200 C -0.0449(4) 0.1646(4) 1.2239(3) 0.0417(14) Uani 1 1 d U . . F21 F -0.0219(3) 0.2317(3) 1.2758(3) 0.0773(13) Uani 1 1 d U . . F22 F -0.0783(2) 0.1047(2) 1.2588(2) 0.0576(10) Uani 1 1 d U . . F23 F -0.1145(2) 0.1707(2) 1.1767(2) 0.0550(10) Uani 1 1 d U . . S2 S 0.05216(10) 0.14539(10) 1.17085(9) 0.0403(4) Uani 1 1 d . . . O21 O 0.0786(3) 0.2147(3) 1.1365(3) 0.0593(13) Uani 1 1 d U . . O22 O 0.1171(3) 0.1378(4) 1.2288(3) 0.0715(16) Uani 1 1 d U . . O23 O 0.0133(3) 0.0733(3) 1.1160(2) 0.0511(11) Uani 1 1 d U . . C30A C 0.7670(12) 0.3636(11) 0.2064(11) 0.075(5) Uani 0.450(3) 1 d PDU A 1 F31A F 0.7953(11) 0.4420(8) 0.2291(10) 0.094(5) Uani 0.450(3) 1 d PDU A 1 F32A F 0.8317(14) 0.3280(11) 0.2207(13) 0.165(8) Uani 0.450(3) 1 d PDU A 1 F33A F 0.6940(11) 0.3407(9) 0.2408(8) 0.128(5) Uani 0.450(3) 1 d PDU A 1 S3A S 0.7362(11) 0.3444(9) 0.1017(9) 0.052(3) Uani 0.450(3) 1 d PDU A 1 O31A O 0.7058(16) 0.2571(8) 0.0836(11) 0.063(5) Uani 0.450(3) 1 d PDU A 1 O32A O 0.8191(11) 0.3739(11) 0.0677(11) 0.113(6) Uani 0.450(3) 1 d PDU A 1 O33A O 0.6685(13) 0.3894(12) 0.0977(13) 0.084(7) Uani 0.450(3) 1 d PDU A 1 C30B C 0.8016(10) 0.3530(8) 0.1724(8) 0.067(4) Uani 0.550(3) 1 d PDU A 2 F31B F 0.8265(9) 0.4297(7) 0.2054(9) 0.101(5) Uani 0.550(3) 1 d PDU A 2 F32B F 0.8797(6) 0.3306(6) 0.1545(6) 0.096(3) Uani 0.550(3) 1 d PDU A 2 F33B F 0.7658(8) 0.3100(7) 0.2231(6) 0.096(3) Uani 0.550(3) 1 d PDU A 2 S3B S 0.7242(9) 0.3352(8) 0.0856(7) 0.056(2) Uani 0.550(3) 1 d PDU A 2 O31B O 0.7001(15) 0.2509(8) 0.0582(10) 0.080(6) Uani 0.550(3) 1 d PDU A 2 O32B O 0.7783(8) 0.3786(8) 0.0355(7) 0.082(4) Uani 0.550(3) 1 d PDU A 2 O33B O 0.6473(9) 0.3697(9) 0.1134(10) 0.063(4) Uani 0.550(3) 1 d PDU A 2 C40B C 0.7118(15) 0.5124(16) 0.5234(12) 0.244(8) Uani 0.450(3) 1 d PDU A 1 S4B S 0.6810(5) 0.4133(6) 0.5491(4) 0.137(3) Uani 0.450(3) 1 d PDU A 1 O41B O 0.7172(17) 0.4285(15) 0.6226(10) 0.218(12) Uani 0.450(3) 1 d PDU A 1 O42B O 0.7176(13) 0.3673(10) 0.4887(10) 0.152(7) Uani 0.450(3) 1 d PDU A 1 O43B O 0.5787(11) 0.4003(14) 0.5327(15) 0.232(13) Uani 0.450(3) 1 d PDU A 1 F42B F 0.7964(12) 0.5146(13) 0.5176(14) 0.250(8) Uani 0.450(3) 1 d PDU A 1 F41B F 0.6806(18) 0.5511(10) 0.5828(13) 0.264(8) Uani 0.450(3) 1 d PDU A 1 F43B F 0.6541(17) 0.4966(13) 0.4620(12) 0.258(8) Uani 0.450(3) 1 d PDU A 1 O203 O 0.067(2) 0.786(2) 0.3618(19) 0.299(15) Uani 0.550(3) 1 d PU A 1 N400 N 0.5452(18) 0.6352(14) 0.6358(13) 0.171(9) Uani 0.550(3) 1 d PDU A 1 C401 C 0.463(2) 0.618(3) 0.623(2) 0.29(2) Uani 0.550(3) 1 d PDU A 1 C402 C 0.3879(19) 0.632(2) 0.6741(19) 0.198(13) Uani 0.550(3) 1 d PDU A 1 C302 C 0.0927(13) 0.5567(11) 0.5835(11) 0.074(5) Uani 0.450(3) 1 d PDU A 1 C301 C 0.0469(19) 0.6126(18) 0.5731(18) 0.133(10) Uani 0.450(3) 1 d PDU A 1 N300 N -0.0029(15) 0.6519(13) 0.5532(12) 0.119(7) Uani 0.450(3) 1 d PDU A 1 C40A C -0.0554(10) 0.6801(8) 0.3535(8) 0.074(4) Uani 0.550(3) 1 d PDU A 2 S4A S 0.0485(3) 0.6798(3) 0.4098(4) 0.0976(17) Uani 0.550(3) 1 d PD A 2 O41A O 0.0105(11) 0.6652(9) 0.4828(8) 0.139(6) Uani 0.550(3) 1 d PDU A 2 O42A O 0.1066(8) 0.7604(6) 0.4175(8) 0.100(4) Uani 0.550(3) 1 d PDU A 2 O43A O 0.0839(12) 0.6199(9) 0.3648(9) 0.154(6) Uani 0.550(3) 1 d PDU A 2 F43A F -0.0307(7) 0.7008(6) 0.2862(5) 0.092(3) Uani 0.550(3) 1 d PDU A 2 F41A F -0.0991(6) 0.7280(6) 0.3861(5) 0.093(3) Uani 0.550(3) 1 d PDU A 2 F42A F -0.1030(8) 0.6080(6) 0.3397(6) 0.121(4) Uani 0.550(3) 1 d PDU A 2 O202 O 0.6451(10) 0.3615(8) 0.5858(8) 0.085(4) Uani 0.450(3) 1 d PU A 2 O100 O 0.2862(8) 0.7774(6) 0.3998(6) 0.172(4) Uani 1 1 d U . . 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 O11 0.071(3) 0.101(4) 0.041(3) 0.024(3) -0.004(2) 0.014(3) Ag1 0.0441(3) 0.0375(3) 0.0361(2) 0.0014(2) 0.0076(2) -0.0025(2) Ag2 0.0325(2) 0.0458(3) 0.0420(3) 0.0191(2) 0.00601(19) 0.00963(19) Ag3 0.0320(2) 0.0471(3) 0.0330(2) 0.0155(2) 0.00738(17) 0.01872(19) Ag4 0.0432(3) 0.0395(3) 0.0389(2) 0.0077(2) 0.0098(2) -0.0004(2) N11 0.028(2) 0.033(3) 0.034(2) 0.008(2) 0.0065(19) 0.0023(19) N21 0.025(2) 0.038(3) 0.031(2) 0.010(2) 0.0023(18) 0.0048(19) N31 0.036(2) 0.031(2) 0.026(2) 0.0043(19) 0.0063(19) 0.0067(19) N41 0.028(2) 0.032(2) 0.027(2) 0.0119(19) 0.0066(18) 0.0086(18) N51 0.035(2) 0.038(3) 0.024(2) 0.010(2) 0.0027(19) 0.010(2) N61 0.022(2) 0.031(2) 0.029(2) 0.0083(19) 0.0041(17) 0.0047(17) N71 0.037(2) 0.034(3) 0.037(3) 0.013(2) 0.009(2) 0.002(2) N81 0.027(2) 0.029(2) 0.033(2) 0.0079(19) 0.0072(18) 0.0035(18) P1 0.0209(6) 0.0252(7) 0.0210(6) 0.0066(5) 0.0019(5) 0.0042(5) P2 0.0214(6) 0.0246(7) 0.0202(6) 0.0066(5) 0.0034(5) 0.0050(5) P3 0.0204(6) 0.0257(7) 0.0206(6) 0.0071(5) 0.0021(5) 0.0044(5) P4 0.0221(6) 0.0242(7) 0.0245(6) 0.0086(5) 0.0029(5) 0.0049(5) N1 0.024(2) 0.026(2) 0.020(2) 0.0057(17) 0.0045(16) 0.0047(17) N2 0.025(2) 0.025(2) 0.0202(19) 0.0051(17) 0.0039(16) 0.0060(17) N3 0.022(2) 0.022(2) 0.027(2) 0.0067(17) 0.0051(17) 0.0038(16) N4 0.024(2) 0.027(2) 0.027(2) 0.0129(18) 0.0059(17) 0.0030(17) O1 0.0212(17) 0.0273(19) 0.0307(18) 0.0080(15) 0.0032(14) 0.0037(14) O2 0.0336(19) 0.0267(19) 0.0216(17) 0.0066(15) 0.0029(15) 0.0030(15) O3 0.0236(17) 0.036(2) 0.0226(17) 0.0069(15) 0.0039(14) 0.0108(15) O4 0.0273(18) 0.0266(19) 0.0235(17) 0.0097(15) 0.0016(14) 0.0016(14) O5 0.0326(19) 0.029(2) 0.0238(17) 0.0086(15) 0.0021(15) 0.0106(15) O6 0.0232(17) 0.0248(19) 0.0340(19) 0.0080(16) 0.0072(15) 0.0011(14) O7 0.0249(17) 0.035(2) 0.0292(18) 0.0128(16) 0.0018(15) 0.0056(15) O8 0.0228(17) 0.0272(19) 0.0301(18) 0.0026(15) 0.0037(14) 0.0040(14) C11 0.017(2) 0.031(3) 0.028(2) 0.006(2) 0.0005(19) 0.0031(19) C12 0.032(3) 0.038(3) 0.032(3) 0.005(2) 0.003(2) 0.001(2) C13 0.042(3) 0.036(3) 0.048(3) 0.010(3) 0.001(3) -0.008(2) C14 0.040(3) 0.040(3) 0.049(3) 0.012(3) 0.008(3) -0.008(3) C15 0.037(3) 0.043(3) 0.038(3) 0.009(3) 0.010(2) -0.002(3) C16 0.079(5) 0.060(5) 0.064(5) 0.012(4) 0.001(4) -0.018(4) C21 0.031(3) 0.028(3) 0.019(2) 0.004(2) 0.001(2) 0.001(2) C22 0.031(3) 0.034(3) 0.032(3) 0.005(2) 0.007(2) 0.006(2) C23 0.036(3) 0.040(3) 0.038(3) 0.015(2) 0.001(2) 0.009(2) C24 0.040(3) 0.046(3) 0.028(3) 0.015(2) 0.002(2) 0.004(2) C25 0.037(3) 0.045(3) 0.031(3) 0.013(3) 0.006(2) 0.004(2) C26 0.050(4) 0.078(5) 0.060(4) 0.035(4) 0.008(3) 0.029(3) C31 0.025(2) 0.033(3) 0.025(2) 0.006(2) 0.002(2) 0.012(2) C32 0.026(2) 0.033(3) 0.037(3) 0.007(2) 0.004(2) 0.007(2) C33 0.030(3) 0.036(3) 0.039(3) 0.001(2) -0.002(2) 0.008(2) C34 0.037(3) 0.040(3) 0.030(3) -0.002(2) 0.001(2) 0.008(2) C35 0.040(3) 0.043(3) 0.028(3) 0.004(2) 0.009(2) 0.007(3) C36 0.059(4) 0.055(4) 0.048(4) -0.001(3) 0.006(3) -0.003(3) C41 0.025(2) 0.023(3) 0.025(2) 0.010(2) 0.0021(19) 0.0016(19) C42 0.033(3) 0.030(3) 0.031(3) 0.007(2) 0.009(2) 0.011(2) C43 0.032(3) 0.035(3) 0.041(3) 0.018(2) 0.003(2) 0.010(2) C44 0.039(3) 0.044(3) 0.030(3) 0.017(2) 0.004(2) 0.012(2) C45 0.035(3) 0.042(3) 0.027(3) 0.014(2) 0.010(2) 0.017(2) C46 0.054(4) 0.067(4) 0.054(4) 0.021(3) 0.002(3) 0.038(3) C51 0.030(3) 0.035(3) 0.022(2) 0.009(2) -0.003(2) 0.012(2) C52 0.030(3) 0.038(3) 0.029(3) 0.011(2) -0.002(2) 0.007(2) C53 0.038(3) 0.038(3) 0.029(3) 0.005(2) -0.007(2) 0.007(2) C54 0.054(3) 0.045(3) 0.026(3) 0.001(2) 0.001(2) 0.010(3) C55 0.048(3) 0.050(3) 0.022(3) 0.006(2) 0.007(2) 0.013(3) C56 0.052(4) 0.043(4) 0.051(4) 0.001(3) -0.005(3) -0.001(3) C61 0.022(2) 0.023(3) 0.034(3) 0.006(2) 0.005(2) 0.0006(19) C62 0.027(2) 0.036(3) 0.034(3) 0.009(2) -0.003(2) 0.004(2) C63 0.029(3) 0.033(3) 0.048(3) 0.007(2) -0.001(2) 0.006(2) C64 0.025(2) 0.035(3) 0.047(3) 0.006(2) 0.008(2) 0.010(2) C65 0.030(3) 0.036(3) 0.035(3) 0.005(2) 0.011(2) 0.007(2) C66 0.045(4) 0.061(4) 0.070(4) 0.013(4) -0.002(3) 0.028(3) C71 0.030(3) 0.028(3) 0.032(3) 0.017(2) 0.006(2) 0.008(2) C72 0.044(3) 0.033(3) 0.043(3) 0.012(2) 0.010(2) 0.009(2) C73 0.047(3) 0.035(3) 0.061(4) 0.012(3) 0.014(3) 0.002(3) C74 0.048(3) 0.037(3) 0.062(4) 0.013(3) 0.024(3) 0.000(3) C75 0.048(3) 0.043(3) 0.049(3) 0.011(3) 0.023(3) 0.004(3) C76 0.063(5) 0.048(4) 0.097(6) 0.000(4) 0.018(4) -0.015(4) C81 0.021(2) 0.020(2) 0.035(3) 0.000(2) 0.002(2) 0.0032(19) C82 0.032(3) 0.031(3) 0.040(3) 0.006(2) -0.001(2) 0.009(2) C83 0.039(3) 0.034(3) 0.053(3) -0.006(3) -0.005(3) 0.013(2) C84 0.033(3) 0.048(3) 0.062(4) -0.005(3) 0.006(3) 0.014(3) C85 0.032(3) 0.039(3) 0.052(3) 0.004(3) 0.015(3) 0.007(2) C86 0.061(4) 0.070(5) 0.076(5) 0.012(4) -0.010(4) 0.036(4) C90 0.060(4) 0.046(4) 0.057(4) 0.013(3) 0.006(3) 0.017(3) C91 0.080(5) 0.073(5) 0.057(4) 0.016(4) 0.024(4) 0.015(4) N90 0.096(5) 0.064(4) 0.057(4) 0.024(3) 0.013(4) 0.020(4) C92A 0.060(8) 0.062(10) 0.054(8) 0.012(7) 0.004(7) 0.008(7) C93A 0.103(11) 0.099(11) 0.099(11) 0.045(9) -0.014(9) 0.022(9) N92A 0.089(13) 0.071(14) 0.071(13) 0.031(10) 0.010(9) 0.020(9) C92B 0.063(7) 0.061(9) 0.051(7) 0.013(7) 0.004(6) 0.011(6) C93B 0.102(10) 0.098(10) 0.062(8) 0.035(7) -0.011(7) 0.021(8) N92B 0.053(7) 0.058(9) 0.028(6) 0.008(6) 0.003(5) 0.011(6) C94A 0.083(10) 0.062(7) 0.066(8) 0.022(6) 0.009(8) 0.020(8) C95A 0.082(9) 0.066(8) 0.067(8) 0.026(7) 0.013(7) 0.027(7) N91A 0.079(10) 0.076(10) 0.063(9) 0.012(7) 0.007(7) 0.017(7) C94B 0.081(10) 0.059(7) 0.067(8) 0.022(7) 0.002(8) 0.014(8) C95B 0.165(19) 0.16(2) 0.150(19) 0.017(11) 0.028(11) 0.058(11) N91B 0.080(11) 0.052(9) 0.059(10) 0.014(7) 0.010(8) 0.022(8) C100 0.061(4) 0.075(5) 0.035(3) 0.009(3) 0.010(3) 0.022(4) F11 0.065(3) 0.150(5) 0.080(3) 0.043(3) 0.036(3) 0.013(3) F12 0.116(4) 0.114(4) 0.082(3) -0.013(3) 0.003(3) 0.072(4) F13 0.064(3) 0.133(4) 0.040(2) 0.017(2) 0.005(2) 0.029(3) S1 0.0461(9) 0.0623(12) 0.0389(9) 0.0088(8) 0.0038(7) 0.0082(8) O12 0.064(3) 0.070(4) 0.091(4) -0.014(3) 0.015(3) 0.023(3) O13 0.067(3) 0.086(4) 0.071(3) 0.037(3) 0.011(3) 0.000(3) C200 0.041(3) 0.048(4) 0.034(3) 0.006(3) 0.009(3) 0.008(3) F21 0.076(3) 0.074(3) 0.066(3) -0.018(2) 0.016(2) 0.010(2) F22 0.049(2) 0.078(3) 0.058(2) 0.036(2) 0.0244(18) 0.018(2) F23 0.042(2) 0.072(3) 0.061(2) 0.026(2) 0.0116(18) 0.0216(19) S2 0.0290(7) 0.0561(10) 0.0381(8) 0.0154(7) 0.0118(6) 0.0078(7) O21 0.049(3) 0.057(3) 0.066(3) 0.022(2) 0.014(2) -0.010(2) O22 0.037(2) 0.127(5) 0.059(3) 0.032(3) 0.006(2) 0.025(3) O23 0.064(3) 0.048(3) 0.041(2) 0.006(2) 0.018(2) 0.013(2) C30A 0.073(8) 0.073(8) 0.080(9) 0.017(7) 0.000(7) 0.019(7) F31A 0.090(9) 0.081(8) 0.094(9) -0.011(6) -0.001(7) 0.009(7) F32A 0.177(12) 0.163(11) 0.167(12) 0.036(9) -0.025(10) 0.066(10) F33A 0.149(10) 0.141(9) 0.086(7) 0.029(7) 0.025(7) 0.005(8) S3A 0.059(6) 0.046(4) 0.049(5) 0.008(4) 0.026(4) 0.006(3) O31A 0.061(8) 0.055(8) 0.059(9) -0.015(6) 0.015(7) 0.004(6) O32A 0.102(10) 0.111(10) 0.114(10) 0.007(8) 0.062(8) 0.001(8) O33A 0.094(11) 0.086(10) 0.076(10) -0.001(8) -0.004(8) 0.048(8) C30B 0.067(7) 0.065(7) 0.075(8) 0.029(6) 0.007(6) 0.015(6) F31B 0.092(8) 0.086(8) 0.106(9) 0.004(6) -0.014(6) -0.005(6) F32B 0.059(5) 0.121(7) 0.127(7) 0.066(6) 0.003(5) 0.025(5) F33B 0.094(7) 0.115(7) 0.091(6) 0.066(6) 0.021(6) 0.008(6) S3B 0.038(3) 0.063(4) 0.059(5) -0.004(3) 0.014(3) 0.008(3) O31B 0.065(7) 0.078(8) 0.078(10) -0.023(6) 0.018(7) 0.004(6) O32B 0.059(6) 0.120(8) 0.079(7) 0.053(6) 0.008(5) 0.019(6) O33B 0.050(6) 0.065(7) 0.074(8) 0.007(6) 0.013(5) 0.020(5) C40B 0.246(10) 0.233(10) 0.249(11) 0.049(8) 0.024(8) 0.044(8) S4B 0.127(6) 0.189(7) 0.086(4) -0.005(5) 0.059(5) 0.040(5) O41B 0.219(15) 0.221(15) 0.212(15) 0.032(10) 0.020(10) 0.056(10) O42B 0.161(11) 0.155(11) 0.153(11) 0.013(9) 0.043(9) 0.078(9) O43B 0.209(15) 0.234(16) 0.234(16) 0.014(10) 0.045(11) 0.032(10) F42B 0.218(9) 0.259(11) 0.256(12) 0.070(9) 0.033(8) 0.001(8) F41B 0.276(12) 0.232(10) 0.274(11) 0.025(9) 0.033(9) 0.053(9) F43B 0.283(12) 0.254(12) 0.248(10) 0.078(8) -0.010(9) 0.071(9) O203 0.311(18) 0.300(18) 0.283(18) 0.073(11) 0.037(11) 0.047(11) N400 0.202(13) 0.146(12) 0.174(12) 0.074(10) 0.005(10) 0.023(9) C401 0.29(3) 0.28(3) 0.31(3) 0.096(12) 0.033(11) 0.062(12) C402 0.203(16) 0.191(16) 0.208(17) 0.053(11) 0.020(11) 0.053(11) C302 0.076(9) 0.068(9) 0.079(9) 0.017(8) -0.006(8) 0.017(7) C301 0.128(13) 0.131(14) 0.127(13) 0.025(10) 0.027(10) -0.003(10) N300 0.130(11) 0.125(11) 0.083(10) 0.022(9) 0.016(9) -0.011(9) C40A 0.085(8) 0.075(8) 0.065(8) 0.020(7) -0.021(7) 0.021(7) S4A 0.083(3) 0.065(3) 0.142(5) 0.020(3) -0.024(3) 0.014(2) O41A 0.177(10) 0.131(9) 0.129(9) 0.068(8) 0.014(8) 0.040(8) O42A 0.079(7) 0.074(7) 0.130(8) 0.002(6) -0.002(6) 0.002(5) O43A 0.164(10) 0.151(10) 0.161(10) 0.000(8) 0.019(8) 0.094(8) F43A 0.110(6) 0.090(6) 0.077(5) 0.013(5) 0.004(5) 0.031(5) F41A 0.077(5) 0.144(7) 0.066(5) 0.019(5) 0.007(4) 0.041(5) F42A 0.133(7) 0.093(7) 0.120(7) 0.038(6) -0.033(6) -0.014(6) O202 0.088(8) 0.090(8) 0.090(8) 0.044(7) 0.049(7) 0.019(6) O100 0.217(8) 0.177(7) 0.144(7) 0.035(6) 0.059(6) 0.082(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 O11 S1 1.427(5) . ? Ag1 N11 2.185(4) . ? Ag1 N31 2.189(4) . ? Ag1 N90 2.523(6) . ? Ag2 N81 2.188(4) . ? Ag2 N21 2.190(4) . ? Ag2 N91B 2.61(2) . ? Ag2 N91A 2.66(2) . ? Ag3 N61 2.167(4) . ? Ag3 N41 2.169(4) . ? Ag4 N71 2.208(5) . ? Ag4 N51 2.209(5) . ? Ag4 N92B 2.486(15) . ? Ag4 N92A 2.49(2) . ? N11 C11 1.321(6) . ? N11 C15 1.341(7) . ? N21 C21 1.324(6) . ? N21 C25 1.365(7) . ? N31 C31 1.323(6) . ? N31 C35 1.357(7) . ? N41 C41 1.318(6) . ? N41 C45 1.347(6) . ? N51 C51 1.332(7) . ? N51 C55 1.356(7) . ? N61 C61 1.319(6) . ? N61 C65 1.362(6) . ? N71 C71 1.327(7) . ? N71 C75 1.371(7) . ? N81 C81 1.341(7) . ? N81 C85 1.346(7) . ? P1 N4 1.571(4) . ? P1 N1 1.575(4) . ? P1 O1 1.590(3) . ? P1 O2 1.599(4) . ? P2 N1 1.564(4) . ? P2 N2 1.565(4) . ? P2 O4 1.603(3) . ? P2 O3 1.605(3) . ? P3 N2 1.566(4) . ? P3 N3 1.568(4) . ? P3 O5 1.591(3) . ? P3 O6 1.595(3) . ? P4 N3 1.562(4) . ? P4 N4 1.566(4) . ? P4 O7 1.587(4) . ? P4 O8 1.592(4) . ? O1 C11 1.403(6) . ? O2 C21 1.383(6) . ? O3 C31 1.398(6) . ? O4 C41 1.406(6) . ? O5 C51 1.389(6) . ? O6 C61 1.402(6) . ? O7 C71 1.400(6) . ? O8 C81 1.406(6) . ? C11 C12 1.369(7) . ? C12 C13 1.391(8) . ? C12 H12 0.9300 . ? C13 C14 1.387(9) . ? C13 C16 1.504(9) . ? C14 C15 1.367(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 C22 1.390(7) . ? C22 C23 1.375(8) . ? C22 H22 0.9300 . ? C23 C24 1.392(8) . ? C23 C26 1.501(8) . ? C24 C25 1.350(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C31 C32 1.372(7) . ? C32 C33 1.384(8) . ? C32 H32 0.9300 . ? C33 C34 1.388(8) . ? C33 C36 1.502(8) . ? C34 C35 1.373(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C41 C42 1.372(7) . ? C42 C43 1.384(7) . ? C42 H42 0.9300 . ? C43 C44 1.376(8) . ? C43 C46 1.496(8) . ? C44 C45 1.372(7) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C51 C52 1.372(7) . ? C52 C53 1.383(8) . ? C52 H52 0.9300 . ? C53 C54 1.383(8) . ? C53 C56 1.516(8) . ? C54 C55 1.385(8) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C61 C62 1.375(7) . ? C62 C63 1.407(8) . ? C62 H62 0.9300 . ? C63 C64 1.371(8) . ? C63 C66 1.510(8) . ? C64 C65 1.364(8) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C71 C72 1.363(8) . ? C72 C73 1.401(8) . ? C72 H72 0.9300 . ? C73 C74 1.384(9) . ? C73 C76 1.516(9) . ? C74 C75 1.365(9) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C81 C82 1.358(7) . ? C82 C83 1.397(8) . ? C82 H82 0.9300 . ? C83 C84 1.375(9) . ? C83 C86 1.497(9) . ? C84 C85 1.369(9) . ? C84 H84 0.9300 . ? C85 H85 0.9300 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C90 N90 1.128(8) . ? C90 C91 1.461(10) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92A N92A 1.118(16) . ? C92A C93A 1.463(17) . ? C92B N92B 1.114(14) . ? C92B C93B 1.471(15) . ? C94A N91A 1.107(15) . ? C94A C95A 1.527(16) . ? C94B N91B 1.112(17) . ? C94B C95B 1.492(18) . ? C100 F12 1.301(8) . ? C100 F13 1.317(7) . ? C100 F11 1.341(9) . ? C100 S1 1.830(7) . ? S1 O12 1.424(5) . ? S1 O13 1.440(5) . ? C200 F21 1.316(7) . ? C200 F22 1.331(7) . ? C200 F23 1.346(7) . ? C200 S2 1.816(6) . ? S2 O23 1.430(5) . ? S2 O22 1.434(5) . ? S2 O21 1.444(5) . ? C30A F32A 1.294(17) . ? C30A F33A 1.297(17) . ? C30A F31A 1.317(17) . ? C30A S3A 1.856(19) . ? S3A O33A 1.41(2) . ? S3A O32A 1.437(15) . ? S3A O31A 1.459(13) . ? C30B F31B 1.319(14) . ? C30B F32B 1.337(14) . ? C30B F33B 1.338(14) . ? C30B S3B 1.832(16) . ? S3B O31B 1.419(13) . ? S3B O32B 1.440(13) . ? S3B O33B 1.466(15) . ? C40B F42B 1.264(18) . ? C40B F41B 1.302(18) . ? C40B F43B 1.313(19) . ? C40B S4B 1.84(3) . ? S4B O41B 1.355(15) . ? S4B O42B 1.416(13) . ? S4B O43B 1.502(16) . ? N400 C401 1.20(2) . ? C401 C402 1.50(2) . ? C302 C301 1.34(3) . ? C301 N300 1.199(19) . ? C40A F41A 1.239(14) . ? C40A F42A 1.277(14) . ? C40A F43A 1.359(14) . ? C40A S4A 1.816(13) . ? S4A O43A 1.401(12) . ? S4A O42A 1.462(10) . ? S4A O41A 1.485(12) . ? 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 Ag1 N31 161.10(16) . . ? N11 Ag1 N90 105.57(19) . . ? N31 Ag1 N90 90.43(19) . . ? N81 Ag2 N21 162.62(16) . . ? N81 Ag2 N91B 91.3(6) . . ? N21 Ag2 N91B 99.9(6) . . ? N81 Ag2 N91A 101.5(5) . . ? N21 Ag2 N91A 89.5(5) . . ? N91B Ag2 N91A 10.4(8) . . ? N61 Ag3 N41 169.40(15) . . ? N71 Ag4 N51 162.01(16) . . ? N71 Ag4 N92B 98.2(5) . . ? N51 Ag4 N92B 95.8(5) . . ? N71 Ag4 N92A 91.2(8) . . ? N51 Ag4 N92A 101.6(8) . . ? N92B Ag4 N92A 8.7(11) . . ? C11 N11 C15 115.8(5) . . ? C11 N11 Ag1 122.3(3) . . ? C15 N11 Ag1 121.9(4) . . ? C21 N21 C25 117.1(5) . . ? C21 N21 Ag2 122.4(3) . . ? C25 N21 Ag2 120.4(4) . . ? C31 N31 C35 115.4(5) . . ? C31 N31 Ag1 122.3(3) . . ? C35 N31 Ag1 122.2(4) . . ? C41 N41 C45 115.8(4) . . ? C41 N41 Ag3 119.1(3) . . ? C45 N41 Ag3 125.0(3) . . ? C51 N51 C55 115.8(5) . . ? C51 N51 Ag4 120.7(4) . . ? C55 N51 Ag4 123.4(4) . . ? C61 N61 C65 116.5(5) . . ? C61 N61 Ag3 119.9(3) . . ? C65 N61 Ag3 123.6(4) . . ? C71 N71 C75 115.5(5) . . ? C71 N71 Ag4 122.3(3) . . ? C75 N71 Ag4 122.2(4) . . ? C81 N81 C85 114.9(5) . . ? C81 N81 Ag2 121.9(3) . . ? C85 N81 Ag2 123.2(4) . . ? N4 P1 N1 122.7(2) . . ? N4 P1 O1 106.1(2) . . ? N1 P1 O1 106.7(2) . . ? N4 P1 O2 107.0(2) . . ? N1 P1 O2 107.1(2) . . ? O1 P1 O2 106.14(19) . . ? N1 P2 N2 122.6(2) . . ? N1 P2 O4 106.0(2) . . ? N2 P2 O4 107.6(2) . . ? N1 P2 O3 107.2(2) . . ? N2 P2 O3 107.3(2) . . ? O4 P2 O3 104.92(19) . . ? N2 P3 N3 122.1(2) . . ? N2 P3 O5 106.3(2) . . ? N3 P3 O5 107.3(2) . . ? N2 P3 O6 107.6(2) . . ? N3 P3 O6 107.2(2) . . ? O5 P3 O6 105.17(19) . . ? N3 P4 N4 122.5(2) . . ? N3 P4 O7 108.3(2) . . ? N4 P4 O7 106.1(2) . . ? N3 P4 O8 105.7(2) . . ? N4 P4 O8 107.6(2) . . ? O7 P4 O8 105.63(19) . . ? P2 N1 P1 129.3(3) . . ? P2 N2 P3 130.6(3) . . ? P4 N3 P3 130.1(3) . . ? P4 N4 P1 129.6(3) . . ? C11 O1 P1 122.4(3) . . ? C21 O2 P1 124.7(3) . . ? C31 O3 P2 123.0(3) . . ? C41 O4 P2 120.1(3) . . ? C51 O5 P3 120.7(3) . . ? C61 O6 P3 123.4(3) . . ? C71 O7 P4 121.7(3) . . ? C81 O8 P4 119.8(3) . . ? N11 C11 C12 125.4(5) . . ? N11 C11 O1 114.7(4) . . ? C12 C11 O1 119.9(5) . . ? C11 C12 C13 118.1(5) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 117.6(6) . . ? C14 C13 C16 122.3(6) . . ? C12 C13 C16 120.0(6) . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N11 C15 C14 123.9(6) . . ? N11 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N21 C21 O2 114.5(5) . . ? N21 C21 C22 123.6(5) . . ? O2 C21 C22 121.6(4) . . ? C23 C22 C21 119.0(5) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 117.1(5) . . ? C22 C23 C26 121.1(5) . . ? C24 C23 C26 121.8(5) . . ? C25 C24 C23 121.0(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 N21 122.1(5) . . ? C24 C25 H25 119.0 . . ? N21 C25 H25 119.0 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N31 C31 C32 125.4(5) . . ? N31 C31 O3 113.6(4) . . ? C32 C31 O3 121.0(5) . . ? C31 C32 C33 118.8(5) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C32 C33 C34 117.3(5) . . ? C32 C33 C36 121.6(5) . . ? C34 C33 C36 121.1(5) . . ? C35 C34 C33 119.6(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N31 C35 C34 123.5(5) . . ? N31 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N41 C41 C42 125.7(5) . . ? N41 C41 O4 113.8(4) . . ? C42 C41 O4 120.5(4) . . ? C41 C42 C43 118.1(5) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C44 C43 C42 117.2(5) . . ? C44 C43 C46 121.5(5) . . ? C42 C43 C46 121.3(5) . . ? C45 C44 C43 120.6(5) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? N41 C45 C44 122.5(5) . . ? N41 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N51 C51 C52 125.6(5) . . ? N51 C51 O5 114.1(4) . . ? C52 C51 O5 120.4(5) . . ? C51 C52 C53 118.1(5) . . ? C51 C52 H52 121.0 . . ? C53 C52 H52 121.0 . . ? C54 C53 C52 118.2(5) . . ? C54 C53 C56 122.0(5) . . ? C52 C53 C56 119.8(5) . . ? C53 C54 C55 119.7(5) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? N51 C55 C54 122.6(5) . . ? N51 C55 H55 118.7 . . ? C54 C55 H55 118.7 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N61 C61 C62 125.3(5) . . ? N61 C61 O6 113.8(4) . . ? C62 C61 O6 120.8(5) . . ? C61 C62 C63 117.3(5) . . ? C61 C62 H62 121.3 . . ? C63 C62 H62 121.3 . . ? C64 C63 C62 118.1(5) . . ? C64 C63 C66 121.8(6) . . ? C62 C63 C66 120.1(6) . . ? C65 C64 C63 120.3(5) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? N61 C65 C64 122.5(5) . . ? N61 C65 H65 118.7 . . ? C64 C65 H65 118.7 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N71 C71 C72 125.5(5) . . ? N71 C71 O7 113.3(5) . . ? C72 C71 O7 121.2(5) . . ? C71 C72 C73 118.7(6) . . ? C71 C72 H72 120.7 . . ? C73 C72 H72 120.7 . . ? C74 C73 C72 117.0(6) . . ? C74 C73 C76 122.5(6) . . ? C72 C73 C76 120.5(6) . . ? C75 C74 C73 120.4(6) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 N71 122.9(6) . . ? C74 C75 H75 118.6 . . ? N71 C75 H75 118.6 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N81 C81 C82 126.6(5) . . ? N81 C81 O8 113.2(4) . . ? C82 C81 O8 120.2(5) . . ? C81 C82 C83 117.7(6) . . ? C81 C82 H82 121.2 . . ? C83 C82 H82 121.2 . . ? C84 C83 C82 116.9(6) . . ? C84 C83 C86 123.0(6) . . ? C82 C83 C86 120.1(6) . . ? C85 C84 C83 121.3(6) . . ? C85 C84 H84 119.3 . . ? C83 C84 H84 119.3 . . ? N81 C85 C84 122.7(6) . . ? N81 C85 H85 118.7 . . ? C84 C85 H85 118.7 . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N90 C90 C91 177.7(8) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 N90 Ag1 159.6(7) . . ? N92A C92A C93A 168(3) . . ? C92A N92A Ag4 156(3) . . ? N92B C92B C93B 173(3) . . ? C92B N92B Ag4 160(2) . . ? N91A C94A C95A 164(3) . . ? C94A N91A Ag2 139(2) . . ? N91B C94B C95B 159(4) . . ? C94B N91B Ag2 144(3) . . ? F12 C100 F13 110.1(7) . . ? F12 C100 F11 105.8(6) . . ? F13 C100 F11 105.8(6) . . ? F12 C100 S1 111.9(5) . . ? F13 C100 S1 112.2(5) . . ? F11 C100 S1 110.7(5) . . ? O12 S1 O11 115.0(4) . . ? O12 S1 O13 114.2(4) . . ? O11 S1 O13 115.5(3) . . ? O12 S1 C100 104.1(3) . . ? O11 S1 C100 103.0(3) . . ? O13 S1 C100 102.7(3) . . ? F21 C200 F22 108.5(5) . . ? F21 C200 F23 107.9(5) . . ? F22 C200 F23 106.6(5) . . ? F21 C200 S2 111.5(4) . . ? F22 C200 S2 111.2(4) . . ? F23 C200 S2 111.0(4) . . ? O23 S2 O22 115.5(3) . . ? O23 S2 O21 113.0(3) . . ? O22 S2 O21 115.7(3) . . ? O23 S2 C200 103.3(3) . . ? O22 S2 C200 103.3(3) . . ? O21 S2 C200 103.9(3) . . ? F32A C30A F33A 112.1(18) . . ? F32A C30A F31A 110.5(16) . . ? F33A C30A F31A 107.8(15) . . ? F32A C30A S3A 110.4(17) . . ? F33A C30A S3A 109.5(13) . . ? F31A C30A S3A 106.4(14) . . ? O33A S3A O32A 114.0(13) . . ? O33A S3A O31A 117.5(15) . . ? O32A S3A O31A 113.4(14) . . ? O33A S3A C30A 101.9(14) . . ? O32A S3A C30A 106.4(14) . . ? O31A S3A C30A 101.4(12) . . ? F31B C30B F32B 105.6(12) . . ? F31B C30B F33B 110.0(13) . . ? F32B C30B F33B 106.3(12) . . ? F31B C30B S3B 112.4(12) . . ? F32B C30B S3B 109.7(11) . . ? F33B C30B S3B 112.4(11) . . ? O31B S3B O32B 113.9(11) . . ? O31B S3B O33B 114.0(11) . . ? O32B S3B O33B 114.0(11) . . ? O31B S3B C30B 106.5(12) . . ? O32B S3B C30B 104.0(9) . . ? O33B S3B C30B 103.0(11) . . ? F42B C40B F41B 123(2) . . ? F42B C40B F43B 120.8(19) . . ? F41B C40B F43B 111.9(18) . . ? F42B C40B S4B 97.0(17) . . ? F41B C40B S4B 96.0(16) . . ? F43B C40B S4B 97.5(17) . . ? O41B S4B O42B 122.2(14) . . ? O41B S4B O43B 119.5(13) . . ? O42B S4B O43B 109.8(12) . . ? O41B S4B C40B 102.6(11) . . ? O42B S4B C40B 99.8(9) . . ? O43B S4B C40B 96.6(10) . . ? N400 C401 C402 131(3) . . ? N300 C301 C302 168(3) . . ? F41A C40A F42A 111.7(13) . . ? F41A C40A F43A 108.8(11) . . ? F42A C40A F43A 109.0(12) . . ? F41A C40A S4A 112.9(10) . . ? F42A C40A S4A 106.1(10) . . ? F43A C40A S4A 108.2(10) . . ? O43A S4A O42A 113.4(9) . . ? O43A S4A O41A 118.7(9) . . ? O42A S4A O41A 112.6(8) . . ? O43A S4A C40A 103.4(9) . . ? O42A S4A C40A 105.3(7) . . ? O41A S4A C40A 101.0(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.053 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.118 #===END