# Electronic Supplementary Material (ESI) for Chemical Communications # 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_global _iucr_compatibility_tag ACTA95 #============================================================================== #data Compound1 data_b011jj #TrackingRef 'GK13CC2013.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H82 Ag3 B3 F12 N2 O2 P4' _chemical_formula_weight 1859.44 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' B B 0.0013 0.0007 '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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.776(2) _cell_length_b 13.134(2) _cell_length_c 25.916(4) _cell_angle_alpha 90.704(5) _cell_angle_beta 91.621(5) _cell_angle_gamma 100.084(5) _cell_volume 3944.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 22.78 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6832 _exptl_absorpt_correction_T_max 0.9000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 42660 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13854 _reflns_number_gt 11683 _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. ; _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^)+(0.0500P)^2^+84.3257P] 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 13854 _refine_ls_number_parameters 1107 _refine_ls_number_restraints 540 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0963 _refine_ls_wR_factor_ref 0.2324 _refine_ls_wR_factor_gt 0.2254 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.91205(7) 0.43060(6) 0.28794(3) 0.0210(2) Uani 1 1 d D . . Ag2 Ag 0.79522(7) 0.61705(6) 0.32133(3) 0.0254(2) Uani 1 1 d . B . Ag3 Ag 0.61572(7) 0.96489(6) 0.00642(3) 0.0217(2) Uani 1 1 d . . . P1 P 1.0249(2) 0.54511(19) 0.23113(10) 0.0156(5) Uani 1 1 d . B . P2 P 0.8804(2) 0.7134(2) 0.25292(10) 0.0167(5) Uani 1 1 d . . . P3 P 0.5770(2) 0.85911(19) -0.07057(10) 0.0151(5) Uani 1 1 d . . . P4 P 0.6430(2) 1.05421(19) 0.08903(10) 0.0165(5) Uani 1 1 d . . . B1 B 0.6258(11) 0.3318(10) 0.2339(5) 0.025(3) Uani 1 1 d . . . F1 F 0.6722(6) 0.4210(5) 0.2618(3) 0.0322(15) Uani 1 1 d . . . F2 F 0.7159(7) 0.2795(6) 0.2226(3) 0.050(2) Uani 1 1 d . . . F3 F 0.5469(7) 0.2699(6) 0.2630(3) 0.051(2) Uani 1 1 d . . . F4 F 0.5756(6) 0.3568(6) 0.1879(3) 0.0389(17) Uani 1 1 d . . . B2 B 0.6676(13) 1.2630(11) -0.0415(6) 0.021(5) Uani 0.645(15) 1 d PDU A 1 F5 F 0.5732(7) 1.3082(6) -0.0534(4) 0.039(2) Uani 0.645(15) 1 d PD A 1 F6 F 0.7351(9) 1.2646(8) -0.0843(4) 0.039(2) Uani 0.645(15) 1 d PD A 1 F7 F 0.7315(10) 1.3173(7) -0.0015(5) 0.039(2) Uani 0.645(15) 1 d PDU A 1 F8 F 0.6311(9) 1.1623(6) -0.0273(3) 0.039(2) Uani 0.645(15) 1 d PDU A 1 B2A B 0.6980(19) 1.2457(18) -0.0333(9) 0.030(11) Uani 0.355(15) 1 d PDU A 2 F5A F 0.737(2) 1.3225(19) 0.0015(12) 0.076(6) Uani 0.355(15) 1 d PD A 2 F6A F 0.712(2) 1.282(2) -0.0821(9) 0.076(6) Uani 0.355(15) 1 d PDU A 2 F7A F 0.754(2) 1.1656(17) -0.0265(9) 0.076(6) Uani 0.355(15) 1 d PDU A 2 F8A F 0.5819(16) 1.212(2) -0.0266(9) 0.076(6) Uani 0.355(15) 1 d PDU A 2 B3 B 1.0818(11) 0.6568(11) 0.3964(5) 0.030(3) Uani 1 1 d . . . F9 F 1.0982(13) 0.6185(11) 0.4416(4) 0.114(5) Uani 1 1 d . . . F10 F 1.0083(9) 0.7250(8) 0.4020(5) 0.088(4) Uani 1 1 d . . . F11 F 1.0302(7) 0.5791(7) 0.3627(3) 0.060(2) Uani 1 1 d . . . F12 F 1.1815(9) 0.7057(9) 0.3773(5) 0.123(6) Uani 1 1 d . . . N1 N 0.8503(10) 0.3180(8) 0.3470(3) 0.0209(10) Uani 0.679(13) 1 d PGDU B 1 C1 C 0.7725(10) 0.2287(8) 0.3335(3) 0.0209(10) Uani 0.679(13) 1 d PGU B 1 H1 H 0.7469 0.2161 0.2985 0.025 Uiso 0.679(13) 1 calc PR B 1 C2 C 0.7321(9) 0.1580(7) 0.3711(4) 0.0209(10) Uani 0.679(13) 1 d PGU B 1 H2 H 0.6790 0.0970 0.3618 0.025 Uiso 0.679(13) 1 calc PR B 1 C3 C 0.7696(10) 0.1765(8) 0.4222(4) 0.0209(10) Uani 0.679(13) 1 d PGU B 1 C4 C 0.8474(10) 0.2658(8) 0.4358(3) 0.0210(10) Uani 0.679(13) 1 d PGU B 1 H4 H 0.8730 0.2784 0.4707 0.025 Uiso 0.679(13) 1 calc PR B 1 C5 C 0.8878(10) 0.3365(7) 0.3982(4) 0.0209(10) Uani 0.679(13) 1 d PGU B 1 H5 H 0.9409 0.3975 0.4074 0.025 Uiso 0.679(13) 1 calc PR B 1 C6 C 0.7192(13) 0.0991(12) 0.4612(6) 0.020(4) Uani 0.679(13) 1 d P B 1 H6 H 0.6717 0.0377 0.4480 0.024 Uiso 0.679(13) 1 calc PR B 1 C7 C 0.7342(14) 0.1073(14) 0.5119(6) 0.024(4) Uani 0.679(13) 1 d P B 1 H7 H 0.7827 0.1681 0.5250 0.029 Uiso 0.679(13) 1 calc PR B 1 C8 C 0.6828(11) 0.0312(8) 0.5509(3) 0.0220(10) Uani 0.679(13) 1 d PGU B 1 C9 C 0.7135(10) 0.0504(8) 0.6028(4) 0.0220(10) Uani 0.679(13) 1 d PGU B 1 H9 H 0.7692 0.1093 0.6128 0.026 Uiso 0.679(13) 1 calc PR B 1 C10 C 0.6628(10) -0.0165(9) 0.6400(3) 0.0221(10) Uani 0.679(13) 1 d PGU B 1 H10 H 0.6837 -0.0034 0.6755 0.027 Uiso 0.679(13) 1 calc PR B 1 C11 C 0.5813(10) -0.1027(9) 0.6255(3) 0.0221(10) Uani 0.679(13) 1 d PGU B 1 H11 H 0.5466 -0.1484 0.6509 0.027 Uiso 0.679(13) 1 calc PR B 1 C12 C 0.5506(10) -0.1219(8) 0.5736(4) 0.0221(10) Uani 0.679(13) 1 d PGU B 1 H12 H 0.4950 -0.1808 0.5636 0.027 Uiso 0.679(13) 1 calc PR B 1 C13 C 0.6014(11) -0.0549(9) 0.5363(3) 0.0220(10) Uani 0.679(13) 1 d PGU B 1 H13 H 0.5804 -0.0681 0.5009 0.026 Uiso 0.679(13) 1 calc PR B 1 N1Z N 0.869(2) 0.3252(17) 0.3521(7) 0.0209(10) Uani 0.321(13) 1 d PGDU B 2 C1Z C 0.784(2) 0.2377(18) 0.3474(6) 0.0209(10) Uani 0.321(13) 1 d PGU B 2 H1Z H 0.7484 0.2176 0.3146 0.025 Uiso 0.321(13) 1 calc PR B 2 C2Z C 0.7501(19) 0.1798(15) 0.3906(9) 0.0209(10) Uani 0.321(13) 1 d PGU B 2 H2Z H 0.6917 0.1201 0.3874 0.025 Uiso 0.321(13) 1 calc PR B 2 C3Z C 0.802(2) 0.2093(18) 0.4386(7) 0.0210(10) Uani 0.321(13) 1 d PGU B 2 C4Z C 0.887(2) 0.2968(18) 0.4434(6) 0.0210(10) Uani 0.321(13) 1 d PGU B 2 H4Z H 0.9228 0.3170 0.4762 0.025 Uiso 0.321(13) 1 calc PR B 2 C5Z C 0.921(2) 0.3547(15) 0.4001(8) 0.0209(10) Uani 0.321(13) 1 d PGU B 2 H5Z H 0.9795 0.4145 0.4034 0.025 Uiso 0.321(13) 1 calc PR B 2 C6Z C 0.773(2) 0.152(2) 0.4865(14) 0.0214(10) Uani 0.321(13) 1 d PDU B 2 H6Z H 0.8102 0.1810 0.5177 0.026 Uiso 0.321(13) 1 calc PR B 2 C7Z C 0.700(3) 0.064(2) 0.4899(16) 0.0218(10) Uani 0.321(13) 1 d PDU B 2 H7Z H 0.6641 0.0322 0.4591 0.026 Uiso 0.321(13) 1 calc PR B 2 C8Z C 0.669(2) 0.0106(18) 0.5420(6) 0.0220(10) Uani 0.321(13) 1 d PGU B 2 C9Z C 0.585(2) -0.0784(18) 0.5415(6) 0.0220(10) Uani 0.321(13) 1 d PGDU B 2 H9Z H 0.5500 -0.1061 0.5097 0.026 Uiso 0.321(13) 1 calc PR B 2 C10Z C 0.553(2) -0.1270(17) 0.5875(8) 0.0221(10) Uani 0.321(13) 1 d PGU B 2 H10Z H 0.4961 -0.1878 0.5872 0.027 Uiso 0.321(13) 1 calc PR B 2 C11Z C 0.605(2) -0.087(2) 0.6340(7) 0.0221(10) Uani 0.321(13) 1 d PGU B 2 H11Z H 0.5830 -0.1198 0.6655 0.027 Uiso 0.321(13) 1 calc PR B 2 C12Z C 0.689(2) 0.0024(19) 0.6345(6) 0.0221(10) Uani 0.321(13) 1 d PGU B 2 H12Z H 0.7238 0.0300 0.6662 0.027 Uiso 0.321(13) 1 calc PR B 2 C13Z C 0.721(2) 0.0510(17) 0.5884(8) 0.0220(10) Uani 0.321(13) 1 d PGDU B 2 H13Z H 0.7777 0.1118 0.5887 0.026 Uiso 0.321(13) 1 calc PR B 2 N2 N 0.7255(8) 0.5308(6) 0.3854(3) 0.025(2) Uani 1 1 d . . . C14 C 0.6233(10) 0.4689(8) 0.3826(4) 0.026(2) Uani 1 1 d . B . H14 H 0.5827 0.4611 0.3502 0.032 Uiso 1 1 calc R . . C15 C 0.5722(10) 0.4148(9) 0.4240(4) 0.027(2) Uani 1 1 d . . . H15 H 0.4984 0.3721 0.4203 0.032 Uiso 1 1 calc R B . C16 C 0.6339(10) 0.4255(8) 0.4719(4) 0.026(2) Uani 1 1 d . B . C17 C 0.7402(10) 0.4895(9) 0.4741(4) 0.030(3) Uani 1 1 d . . . H17 H 0.7845 0.4983 0.5056 0.036 Uiso 1 1 calc R B . C18 C 0.7820(11) 0.5409(9) 0.4305(5) 0.033(3) Uani 1 1 d . B . H18 H 0.8548 0.5855 0.4330 0.040 Uiso 1 1 calc R . . C19 C 0.5897(10) 0.3662(8) 0.5175(4) 0.027(3) Uani 1 1 d . . . H19 H 0.6433 0.3583 0.5446 0.033 Uiso 1 1 calc R B . C20 C 0.4804(10) 0.3235(8) 0.5230(4) 0.025(2) Uani 1 1 d . B . H20 H 0.4270 0.3352 0.4965 0.030 Uiso 1 1 calc R . . C21 C 0.4344(12) 0.2599(9) 0.5660(4) 0.034(3) Uani 1 1 d . . . C22 C 0.5065(12) 0.2203(11) 0.6018(5) 0.041(3) Uani 1 1 d . B . H22 H 0.5879 0.2352 0.5989 0.050 Uiso 1 1 calc R . . C23 C 0.4581(14) 0.1596(11) 0.6414(5) 0.050(4) Uani 1 1 d . . . H23A H 0.5072 0.1316 0.6649 0.060 Uiso 1 1 calc R B . C24 C 0.3400(14) 0.1383(10) 0.6477(5) 0.050(4) Uani 1 1 d . B . H24 H 0.3085 0.0979 0.6758 0.060 Uiso 1 1 calc R . . C25 C 0.2708(11) 0.1759(10) 0.6135(5) 0.039(3) Uani 1 1 d . . . H25 H 0.1898 0.1624 0.6180 0.047 Uiso 1 1 calc R B . C26 C 0.3149(12) 0.2352(9) 0.5708(5) 0.037(3) Uani 1 1 d . B . H26 H 0.2642 0.2576 0.5459 0.045 Uiso 1 1 calc R . . C27 C 1.0242(8) 0.6829(7) 0.2442(4) 0.018(2) Uani 1 1 d . B . H27A H 1.0722 0.7047 0.2757 0.021 Uiso 1 1 calc R . . H27B H 1.0602 0.7236 0.2151 0.021 Uiso 1 1 calc R . . C28 C 0.4236(8) 0.8299(7) -0.0905(4) 0.015(2) Uani 1 1 d . . . H28A H 0.4161 0.7999 -0.1259 0.018 Uiso 1 1 calc R . . H28B H 0.3824 0.7778 -0.0672 0.018 Uiso 1 1 calc R . . C1A C 0.7937(8) 1.0991(8) 0.1093(4) 0.018(2) Uani 1 1 d . . . C2A C 0.8602(10) 1.0255(10) 0.1192(5) 0.032(3) Uani 1 1 d . . . H2A H 0.8275 0.9545 0.1142 0.039 Uiso 1 1 calc R . . C3A C 0.9736(10) 1.0524(11) 0.1361(5) 0.036(3) Uani 1 1 d . . . H3A H 1.0187 1.0002 0.1422 0.043 Uiso 1 1 calc R . . C4A C 1.0206(11) 1.1528(12) 0.1441(6) 0.049(4) Uani 1 1 d . . . H4A H 1.0987 1.1719 0.1558 0.059 Uiso 1 1 calc R . . C5A C 0.9539(13) 1.2267(12) 0.1352(10) 0.095(8) Uani 1 1 d . . . H5AA H 0.9864 1.2976 0.1405 0.114 Uiso 1 1 calc R . . C6A C 0.8390(11) 1.1991(10) 0.1185(9) 0.073(6) Uani 1 1 d . . . H6A H 0.7928 1.2509 0.1136 0.088 Uiso 1 1 calc R . . C1B C 0.5829(8) 0.9776(8) 0.1429(4) 0.016(2) Uani 1 1 d . . . C2B C 0.5383(9) 0.8726(8) 0.1343(4) 0.025(2) Uani 1 1 d . . . H2B H 0.5418 0.8420 0.1011 0.030 Uiso 1 1 calc R . . C3B C 0.4889(10) 0.8131(9) 0.1747(5) 0.034(3) Uani 1 1 d . . . H3B H 0.4584 0.7418 0.1691 0.041 Uiso 1 1 calc R . . C4B C 0.4842(10) 0.8581(9) 0.2229(5) 0.034(3) Uani 1 1 d . . . H4B H 0.4500 0.8173 0.2503 0.040 Uiso 1 1 calc R . . C5B C 0.5288(9) 0.9617(9) 0.2319(4) 0.026(2) Uani 1 1 d . . . H5B H 0.5249 0.9922 0.2650 0.031 Uiso 1 1 calc R . . C6B C 0.5795(9) 1.0206(8) 0.1914(4) 0.018(2) Uani 1 1 d . . . H6B H 0.6121 1.0913 0.1974 0.022 Uiso 1 1 calc R . . C1C C 0.6208(8) 0.7328(8) -0.0640(4) 0.016(2) Uani 1 1 d . . . C2C C 0.7382(10) 0.7314(9) -0.0626(6) 0.044(4) Uani 1 1 d . . . H2C H 0.7910 0.7945 -0.0655 0.053 Uiso 1 1 calc R . . C3C C 0.7793(11) 0.6413(11) -0.0572(7) 0.058(5) Uani 1 1 d . . . H3C H 0.8602 0.6426 -0.0560 0.070 Uiso 1 1 calc R . . C4C C 0.7069(11) 0.5505(9) -0.0536(4) 0.032(3) Uani 1 1 d . . . H4C H 0.7362 0.4878 -0.0505 0.038 Uiso 1 1 calc R . . C5C C 0.5898(10) 0.5496(9) -0.0544(5) 0.034(3) Uani 1 1 d . . . H5C H 0.5379 0.4859 -0.0516 0.041 Uiso 1 1 calc R . . C6C C 0.5473(10) 0.6402(8) -0.0593(5) 0.028(3) Uani 1 1 d . . . H6C H 0.4664 0.6386 -0.0595 0.034 Uiso 1 1 calc R . . C1D C 0.6520(8) 0.9110(8) -0.1280(4) 0.018(2) Uani 1 1 d . . . C2D C 0.6516(9) 0.8512(8) -0.1721(4) 0.020(2) Uani 1 1 d . . . H2D H 0.6113 0.7819 -0.1733 0.024 Uiso 1 1 calc R . . C3D C 0.7102(10) 0.8928(10) -0.2145(4) 0.033(3) Uani 1 1 d . . . H3D H 0.7123 0.8510 -0.2445 0.040 Uiso 1 1 calc R . . C4D C 0.7657(10) 0.9947(10) -0.2138(4) 0.034(3) Uani 1 1 d . . . H4D H 0.8048 1.0232 -0.2433 0.041 Uiso 1 1 calc R . . C5D C 0.7637(9) 1.0544(9) -0.1700(5) 0.032(3) Uani 1 1 d . . . H5D H 0.8012 1.1246 -0.1695 0.038 Uiso 1 1 calc R . . C6D C 0.7079(9) 1.0139(8) -0.1266(4) 0.020(2) Uani 1 1 d . . . H6D H 0.7076 1.0555 -0.0963 0.024 Uiso 1 1 calc R . . C1E C 0.9091(8) 0.8530(8) 0.2655(4) 0.018(2) Uani 1 1 d . B . C2E C 0.8454(10) 0.9191(8) 0.2413(4) 0.026(2) Uani 1 1 d . . . H2E H 0.7875 0.8926 0.2159 0.031 Uiso 1 1 calc R B . C3E C 0.8659(10) 1.0222(9) 0.2538(5) 0.030(3) Uani 1 1 d . B . H3E H 0.8218 1.0667 0.2369 0.036 Uiso 1 1 calc R . . C4E C 0.9488(9) 1.0626(8) 0.2902(4) 0.025(2) Uani 1 1 d . . . H4E H 0.9632 1.1348 0.2979 0.030 Uiso 1 1 calc R B . C5E C 1.0114(10) 0.9975(9) 0.3159(4) 0.027(2) Uani 1 1 d . B . H5E H 1.0675 1.0245 0.3419 0.032 Uiso 1 1 calc R . . C6E C 0.9918(9) 0.8927(8) 0.3035(4) 0.020(2) Uani 1 1 d . . . H6E H 1.0348 0.8479 0.3208 0.024 Uiso 1 1 calc R B . C1F C 0.8045(9) 0.6959(7) 0.1913(4) 0.021(2) Uani 1 1 d . B . C2F C 0.8525(9) 0.7421(8) 0.1461(4) 0.020(2) Uani 1 1 d . . . H2F H 0.9274 0.7833 0.1476 0.024 Uiso 1 1 calc R B . C3F C 0.7908(10) 0.7275(8) 0.1000(4) 0.028(3) Uani 1 1 d . B . H3F H 0.8223 0.7606 0.0700 0.034 Uiso 1 1 calc R . . C4F C 0.6831(10) 0.6650(8) 0.0969(5) 0.029(3) Uani 1 1 d . . . H4F H 0.6418 0.6540 0.0648 0.035 Uiso 1 1 calc R B . C5F C 0.6358(10) 0.6186(9) 0.1411(5) 0.034(3) Uani 1 1 d . B . H5F H 0.5619 0.5756 0.1391 0.041 Uiso 1 1 calc R . . C6F C 0.6951(9) 0.6343(8) 0.1876(5) 0.027(2) Uani 1 1 d . . . H6F H 0.6613 0.6030 0.2177 0.033 Uiso 1 1 calc R B . C1G C 0.9835(8) 0.5304(8) 0.1633(4) 0.017(2) Uani 1 1 d . . . C2G C 1.0577(9) 0.5812(8) 0.1256(4) 0.022(2) Uani 1 1 d . B . H2G H 1.1314 0.6192 0.1357 0.027 Uiso 1 1 calc R . . C3G C 1.0217(10) 0.5748(9) 0.0741(4) 0.027(3) Uani 1 1 d . . . H3G H 1.0692 0.6100 0.0486 0.033 Uiso 1 1 calc R B . C4G C 0.9154(11) 0.5163(10) 0.0603(4) 0.033(3) Uani 1 1 d . B . H4G H 0.8919 0.5101 0.0249 0.039 Uiso 1 1 calc R . . C5G C 0.8429(10) 0.4667(8) 0.0964(4) 0.026(2) Uani 1 1 d . . . H5G H 0.7697 0.4283 0.0859 0.031 Uiso 1 1 calc R B . C6G C 0.8768(9) 0.4728(8) 0.1479(4) 0.021(2) Uani 1 1 d . B . H6G H 0.8274 0.4378 0.1729 0.026 Uiso 1 1 calc R . . C1H C 1.1784(9) 0.5361(8) 0.2343(4) 0.021(2) Uani 1 1 d . . . C2H C 1.2181(11) 0.4666(10) 0.2015(5) 0.038(3) Uani 1 1 d . B . H2H H 1.1662 0.4272 0.1771 0.046 Uiso 1 1 calc R . . C3H C 1.3330(10) 0.4539(9) 0.2040(5) 0.031(3) Uani 1 1 d . . . H3H H 1.3607 0.4077 0.1810 0.038 Uiso 1 1 calc R B . C4H C 1.4076(10) 0.5118(10) 0.2420(5) 0.034(3) Uani 1 1 d . B . H4H H 1.4858 0.5030 0.2452 0.041 Uiso 1 1 calc R . . C5H C 1.3671(10) 0.5809(9) 0.2743(5) 0.033(3) Uani 1 1 d . . . H5H H 1.4180 0.6205 0.2991 0.040 Uiso 1 1 calc R B . C6H C 1.2529(9) 0.5926(8) 0.2708(4) 0.023(2) Uani 1 1 d . B . H6H H 1.2252 0.6395 0.2934 0.028 Uiso 1 1 calc R . . O1S O 0.2904(10) 0.3590(8) 0.4236(4) 0.058(3) Uani 1 1 d U . . C1S C 0.2765(17) 0.4152(13) 0.3790(7) 0.073(5) Uani 1 1 d U . . H1SA H 0.2368 0.4736 0.3873 0.087 Uiso 1 1 calc R . . H1SB H 0.3529 0.4437 0.3653 0.087 Uiso 1 1 calc R . . C2S C 0.212(3) 0.3505(16) 0.3422(8) 0.133(12) Uani 1 1 d U . . H2SA H 0.2606 0.3378 0.3132 0.160 Uiso 1 1 calc R . . H2SB H 0.1476 0.3830 0.3284 0.160 Uiso 1 1 calc R . . C3S C 0.1652(15) 0.2520(12) 0.3670(8) 0.075(5) Uani 1 1 d U . . H3SA H 0.1998 0.1943 0.3531 0.090 Uiso 1 1 calc R . . H3SB H 0.0802 0.2348 0.3626 0.090 Uiso 1 1 calc R . . C4S C 0.2012(12) 0.2754(14) 0.4227(7) 0.064(4) Uani 1 1 d U . . H4SA H 0.1356 0.2921 0.4422 0.077 Uiso 1 1 calc R . . H4SB H 0.2271 0.2149 0.4386 0.077 Uiso 1 1 calc R . . O2S O 1.0072(17) 0.1040(16) 0.4711(8) 0.064(5) Uani 0.50 1 d PDU C -3 C5S C 1.056(3) 0.084(3) 0.5186(9) 0.049(4) Uani 0.50 1 d PDU C -3 H5SA H 1.0598 0.1455 0.5417 0.058 Uiso 0.50 1 calc PR C -3 H5SB H 1.1363 0.0731 0.5137 0.058 Uiso 0.50 1 calc PR C -3 C6S C 0.988(3) -0.009(3) 0.5438(12) 0.049(4) Uani 0.50 1 d PDU C -3 H6SA H 0.9274 0.0095 0.5657 0.058 Uiso 0.50 1 calc PR C -3 H6SB H 1.0391 -0.0465 0.5648 0.058 Uiso 0.50 1 calc PR C -3 C7S C 0.937(3) -0.073(3) 0.4965(11) 0.049(4) Uani 0.50 1 d PDU C -3 H7SA H 0.9676 -0.1384 0.4935 0.058 Uiso 0.50 1 calc PR C -3 H7SB H 0.8520 -0.0883 0.4969 0.058 Uiso 0.50 1 calc PR C -3 C8S C 0.980(3) 0.001(2) 0.4537(13) 0.049(4) Uani 0.50 1 d PDU C -3 H8SA H 1.0491 -0.0193 0.4388 0.058 Uiso 0.50 1 calc PR C -3 H8SB H 0.9193 -0.0044 0.4260 0.058 Uiso 0.50 1 calc PR C -3 O3S O 0.1235(16) 1.0111(15) 0.0124(7) 0.049(5) Uani 0.50 1 d PDU D -4 C9S C 0.0220(19) 1.048(2) -0.0004(9) 0.040(6) Uani 0.50 1 d PDU D -4 H9SA H 0.0314 1.0882 -0.0327 0.047 Uiso 0.50 1 calc PR D -4 H9SB H 0.0034 1.0943 0.0275 0.047 Uiso 0.50 1 calc PR D -4 C10S C -0.074(2) 0.954(2) -0.008(2) 0.093(19) Uani 0.50 1 d PDU D -4 H10C H -0.1148 0.9560 -0.0414 0.112 Uiso 0.50 1 calc PR D -4 H10D H -0.1305 0.9522 0.0201 0.112 Uiso 0.50 1 calc PR D -4 C11S C -0.0120(18) 0.8615(17) -0.0048(9) 0.034(5) Uani 0.50 1 d PDU D -4 H11C H -0.0578 0.8035 0.0136 0.041 Uiso 0.50 1 calc PR D -4 H11D H 0.0048 0.8375 -0.0397 0.041 Uiso 0.50 1 calc PR D -4 C12S C 0.097(2) 0.9060(17) 0.0251(10) 0.048(6) Uani 0.50 1 d PDU D -4 H12C H 0.0855 0.8985 0.0627 0.058 Uiso 0.50 1 calc PR D -4 H12D H 0.1606 0.8697 0.0155 0.058 Uiso 0.50 1 calc PR D -4 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 0.0238(4) 0.0183(4) 0.0207(4) 0.0068(3) 0.0050(3) 0.0019(3) Ag2 0.0260(4) 0.0234(4) 0.0271(5) 0.0086(3) 0.0124(3) 0.0030(3) Ag3 0.0288(4) 0.0187(4) 0.0177(4) -0.0038(3) 0.0005(3) 0.0047(3) P1 0.0157(12) 0.0158(13) 0.0143(12) 0.0008(10) -0.0011(10) 0.0007(10) P2 0.0163(13) 0.0174(13) 0.0154(13) 0.0014(10) 0.0027(10) -0.0002(10) P3 0.0134(12) 0.0128(12) 0.0185(13) 0.0002(10) -0.0007(10) 0.0011(10) P4 0.0151(13) 0.0154(13) 0.0190(13) 0.0016(10) -0.0003(10) 0.0028(10) B1 0.031(7) 0.021(6) 0.021(6) -0.006(5) 0.005(5) -0.003(5) F1 0.030(4) 0.033(4) 0.033(4) -0.001(3) -0.009(3) 0.007(3) F2 0.068(5) 0.044(4) 0.048(5) 0.001(4) 0.026(4) 0.033(4) F3 0.040(4) 0.057(5) 0.046(5) 0.010(4) 0.007(4) -0.021(4) F4 0.039(4) 0.051(4) 0.023(4) -0.009(3) -0.008(3) 0.000(3) B2 0.027(8) 0.016(7) 0.020(8) 0.011(6) -0.002(7) 0.004(7) F5 0.052(4) 0.024(3) 0.035(4) -0.004(2) -0.006(3) -0.007(3) F6 0.052(4) 0.024(3) 0.035(4) -0.004(2) -0.006(3) -0.007(3) F7 0.052(4) 0.024(3) 0.035(4) -0.004(2) -0.006(3) -0.007(3) F8 0.052(4) 0.024(3) 0.035(4) -0.004(2) -0.006(3) -0.007(3) B2A 0.033(14) 0.026(14) 0.032(14) 0.002(9) 0.000(9) 0.006(9) F5A 0.091(9) 0.084(9) 0.044(8) 0.007(6) 0.008(6) -0.011(7) F6A 0.091(9) 0.084(9) 0.044(8) 0.007(6) 0.008(6) -0.011(7) F7A 0.091(9) 0.084(9) 0.044(8) 0.007(6) 0.008(6) -0.011(7) F8A 0.091(9) 0.084(9) 0.044(8) 0.007(6) 0.008(6) -0.011(7) B3 0.026(7) 0.045(8) 0.018(6) 0.001(6) 0.001(5) 0.000(6) F9 0.160(13) 0.141(11) 0.050(7) 0.008(7) -0.046(7) 0.059(10) F10 0.082(7) 0.061(6) 0.131(10) 0.010(6) 0.040(7) 0.030(6) F11 0.052(5) 0.074(6) 0.040(5) -0.022(4) -0.001(4) -0.021(4) F12 0.079(7) 0.099(8) 0.167(12) -0.097(9) 0.085(8) -0.060(6) N1 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0016(16) C1 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0015(16) C2 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0011(18) 0.0015(16) C3 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0011(18) 0.0014(16) C4 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0011(18) 0.0014(16) C5 0.018(2) 0.024(2) 0.0203(19) 0.0049(17) 0.0012(18) 0.0014(16) C6 0.026(8) 0.025(8) 0.010(7) -0.004(7) -0.011(6) 0.007(7) C7 0.025(9) 0.027(9) 0.019(8) 0.001(7) -0.003(7) 0.001(7) C8 0.019(2) 0.026(2) 0.0198(19) 0.0056(17) 0.0003(17) -0.0001(16) C9 0.019(2) 0.026(2) 0.0198(19) 0.0056(17) 0.0004(17) -0.0003(16) C10 0.019(2) 0.026(2) 0.0197(19) 0.0057(17) 0.0004(18) -0.0004(17) C11 0.019(2) 0.026(2) 0.020(2) 0.0057(17) 0.0004(18) -0.0004(16) C12 0.019(2) 0.026(2) 0.020(2) 0.0057(17) 0.0004(18) -0.0003(16) C13 0.019(2) 0.026(2) 0.0197(19) 0.0057(17) 0.0003(17) -0.0003(16) N1Z 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0015(16) C1Z 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0015(16) C2Z 0.018(2) 0.024(2) 0.0201(19) 0.0049(17) 0.0011(18) 0.0015(16) C3Z 0.018(2) 0.024(2) 0.0201(19) 0.0050(17) 0.0011(17) 0.0013(16) C4Z 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0014(16) C5Z 0.018(2) 0.024(2) 0.0202(19) 0.0049(17) 0.0012(18) 0.0014(16) C6Z 0.019(2) 0.025(2) 0.0200(19) 0.0052(17) 0.0008(18) 0.0007(16) C7Z 0.019(2) 0.025(2) 0.0198(19) 0.0054(17) 0.0005(17) 0.0001(16) C8Z 0.019(2) 0.026(2) 0.0198(19) 0.0056(17) 0.0003(17) -0.0002(16) C9Z 0.019(2) 0.026(2) 0.0197(19) 0.0056(17) 0.0003(17) -0.0003(16) C10Z 0.019(2) 0.026(2) 0.020(2) 0.0057(17) 0.0003(18) -0.0003(16) C11Z 0.019(2) 0.026(2) 0.020(2) 0.0057(17) 0.0004(18) -0.0004(17) C12Z 0.019(2) 0.026(2) 0.0197(19) 0.0056(17) 0.0004(18) -0.0004(17) C13Z 0.019(2) 0.026(2) 0.0198(19) 0.0056(17) 0.0004(18) -0.0003(16) N2 0.036(5) 0.013(4) 0.024(5) 0.002(4) 0.013(4) -0.003(4) C14 0.033(6) 0.021(6) 0.022(6) 0.010(4) 0.006(5) -0.007(5) C15 0.035(6) 0.026(6) 0.021(6) 0.012(5) 0.007(5) 0.008(5) C16 0.039(7) 0.024(6) 0.018(5) 0.006(4) 0.009(5) 0.013(5) C17 0.034(7) 0.032(6) 0.023(6) 0.004(5) 0.001(5) 0.004(5) C18 0.031(7) 0.033(7) 0.034(7) 0.007(5) 0.006(5) -0.001(5) C19 0.040(7) 0.023(6) 0.020(6) 0.008(5) 0.004(5) 0.009(5) C20 0.028(6) 0.025(6) 0.023(6) 0.005(5) 0.012(5) 0.007(5) C21 0.063(9) 0.029(6) 0.015(6) 0.002(5) 0.018(6) 0.022(6) C22 0.051(8) 0.052(8) 0.021(6) 0.013(6) 0.008(6) 0.008(7) C23 0.076(11) 0.045(8) 0.033(8) 0.024(6) 0.017(7) 0.019(8) C24 0.081(11) 0.030(7) 0.043(8) 0.018(6) 0.028(8) 0.020(7) C25 0.035(7) 0.040(7) 0.041(8) 0.001(6) 0.014(6) -0.002(6) C26 0.059(9) 0.023(6) 0.029(7) -0.003(5) 0.019(6) 0.003(6) C27 0.015(5) 0.018(5) 0.019(5) 0.000(4) 0.003(4) 0.000(4) C28 0.013(5) 0.015(5) 0.015(5) 0.003(4) 0.003(4) -0.001(4) C1A 0.011(5) 0.021(5) 0.024(5) -0.006(4) 0.005(4) 0.004(4) C2A 0.030(6) 0.033(7) 0.036(7) 0.010(5) 0.004(5) 0.013(5) C3A 0.024(6) 0.055(8) 0.033(7) 0.014(6) 0.000(5) 0.017(6) C4A 0.015(6) 0.061(10) 0.071(10) -0.020(8) -0.010(6) 0.004(6) C5A 0.029(8) 0.033(9) 0.22(3) -0.044(12) -0.043(12) -0.001(7) C6A 0.015(6) 0.025(7) 0.18(2) -0.024(9) -0.016(9) 0.009(5) C1B 0.012(5) 0.021(5) 0.016(5) 0.005(4) -0.004(4) 0.002(4) C2B 0.023(6) 0.020(6) 0.032(6) 0.003(5) 0.001(5) 0.001(4) C3B 0.031(7) 0.024(6) 0.045(8) 0.005(5) -0.005(6) 0.000(5) C4B 0.032(7) 0.031(7) 0.038(7) 0.018(5) 0.004(5) 0.004(5) C5B 0.028(6) 0.032(6) 0.020(6) 0.006(5) 0.007(5) 0.012(5) C6B 0.021(5) 0.014(5) 0.022(5) 0.001(4) -0.006(4) 0.008(4) C1C 0.019(5) 0.023(5) 0.009(5) 0.005(4) -0.002(4) 0.010(4) C2C 0.014(6) 0.019(6) 0.100(12) 0.017(7) 0.002(6) 0.004(5) C3C 0.019(6) 0.046(9) 0.114(14) 0.033(9) 0.010(7) 0.015(6) C4C 0.043(7) 0.032(7) 0.025(6) 0.005(5) -0.005(5) 0.024(6) C5C 0.032(7) 0.022(6) 0.044(7) 0.003(5) -0.017(6) -0.003(5) C6C 0.024(6) 0.015(5) 0.047(7) 0.003(5) -0.008(5) 0.010(4) C1D 0.014(5) 0.019(5) 0.023(5) 0.003(4) 0.001(4) 0.008(4) C2D 0.020(5) 0.022(5) 0.021(5) 0.004(4) 0.000(4) 0.013(4) C3D 0.029(6) 0.057(8) 0.019(6) 0.008(5) 0.007(5) 0.020(6) C4D 0.024(6) 0.058(8) 0.022(6) 0.020(6) 0.006(5) 0.011(6) C5D 0.021(6) 0.030(6) 0.041(7) 0.017(5) -0.004(5) -0.004(5) C6D 0.020(5) 0.018(5) 0.018(5) 0.011(4) -0.010(4) -0.001(4) C1E 0.017(5) 0.023(5) 0.013(5) 0.004(4) 0.003(4) 0.002(4) C2E 0.028(6) 0.026(6) 0.023(6) 0.000(5) -0.001(5) 0.005(5) C3E 0.035(7) 0.027(6) 0.033(7) 0.001(5) 0.005(5) 0.016(5) C4E 0.029(6) 0.012(5) 0.031(6) -0.006(4) 0.003(5) -0.002(4) C5E 0.035(6) 0.029(6) 0.017(5) -0.006(4) 0.002(5) 0.007(5) C6E 0.023(5) 0.024(6) 0.014(5) 0.005(4) 0.001(4) 0.006(4) C1F 0.016(5) 0.010(5) 0.035(6) -0.005(4) -0.001(4) -0.001(4) C2F 0.024(6) 0.016(5) 0.020(5) -0.003(4) -0.004(4) 0.003(4) C3F 0.038(7) 0.017(5) 0.029(6) 0.004(5) -0.011(5) 0.005(5) C4F 0.025(6) 0.023(6) 0.038(7) -0.005(5) -0.016(5) 0.004(5) C5F 0.019(6) 0.035(7) 0.045(8) -0.010(6) -0.011(5) -0.004(5) C6F 0.022(6) 0.023(6) 0.034(6) -0.005(5) 0.001(5) -0.003(5) C1G 0.013(5) 0.020(5) 0.018(5) 0.003(4) 0.000(4) 0.006(4) C2G 0.022(5) 0.028(6) 0.019(5) 0.000(4) 0.001(4) 0.011(5) C3G 0.036(7) 0.034(6) 0.016(5) -0.001(5) 0.003(5) 0.019(5) C4G 0.041(7) 0.041(7) 0.020(6) -0.005(5) -0.002(5) 0.017(6) C5G 0.024(6) 0.025(6) 0.030(6) -0.015(5) -0.006(5) 0.008(5) C6G 0.022(5) 0.018(5) 0.025(6) 0.002(4) -0.006(4) 0.005(4) C1H 0.021(5) 0.021(5) 0.019(5) 0.009(4) 0.000(4) -0.002(4) C2H 0.032(7) 0.037(7) 0.050(8) -0.002(6) 0.004(6) 0.020(6) C3H 0.024(6) 0.039(7) 0.036(7) 0.006(5) 0.005(5) 0.016(5) C4H 0.025(6) 0.043(7) 0.040(7) 0.021(6) 0.006(5) 0.019(5) C5H 0.029(6) 0.033(7) 0.037(7) 0.010(5) 0.001(5) 0.002(5) C6H 0.023(6) 0.020(5) 0.026(6) 0.001(4) 0.000(5) 0.007(4) O1S 0.078(7) 0.048(6) 0.046(6) 0.012(4) -0.014(5) 0.006(5) C1S 0.098(14) 0.049(9) 0.063(10) 0.032(7) -0.031(9) -0.007(8) C2S 0.27(4) 0.066(12) 0.049(10) 0.012(8) -0.051(14) -0.009(15) C3S 0.059(10) 0.037(7) 0.125(13) -0.010(8) -0.042(10) 0.010(7) C4S 0.026(7) 0.083(11) 0.082(9) 0.052(9) 0.005(7) 0.005(6) O2S 0.040(11) 0.068(9) 0.087(13) 0.025(9) -0.013(10) 0.021(10) C5S 0.028(8) 0.079(8) 0.042(7) 0.004(6) 0.012(8) 0.017(6) C6S 0.028(8) 0.079(8) 0.042(7) 0.004(6) 0.012(8) 0.017(6) C7S 0.028(8) 0.079(8) 0.042(7) 0.004(6) 0.012(8) 0.017(6) C8S 0.028(8) 0.079(8) 0.042(7) 0.004(6) 0.012(8) 0.017(6) O3S 0.047(12) 0.061(11) 0.030(10) -0.010(9) 0.001(9) -0.012(9) C9S 0.073(18) 0.034(8) 0.011(12) -0.002(10) 0.022(13) 0.003(11) C10S 0.035(18) 0.058(17) 0.19(5) -0.05(3) -0.01(2) 0.019(12) C11S 0.037(12) 0.031(9) 0.033(13) 0.008(10) 0.021(9) 0.001(8) C12S 0.048(14) 0.060(12) 0.039(16) -0.005(12) 0.007(11) 0.016(11) _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 N1Z 2.191(6) . ? Ag1 N1 2.191(5) . ? Ag1 P1 2.379(3) . ? Ag1 Ag2 3.1359(12) . ? Ag2 N2 2.123(8) . ? Ag2 P2 2.337(3) . ? Ag3 P3 2.404(3) . ? Ag3 P4 2.415(3) . ? Ag3 Ag3 3.0374(17) 2_675 ? P1 C1G 1.810(10) . ? P1 C1H 1.832(11) . ? P1 C27 1.839(10) . ? P2 C1F 1.799(11) . ? P2 C27 1.827(10) . ? P2 C1E 1.830(10) . ? P3 C1C 1.830(10) . ? P3 C1D 1.830(10) . ? P3 C28 1.837(9) . ? P4 C1B 1.817(10) . ? P4 C1A 1.829(10) . ? P4 C28 1.831(10) 2_675 ? B1 F3 1.373(14) . ? B1 F4 1.384(15) . ? B1 F1 1.389(14) . ? B1 F2 1.397(15) . ? B2 F8 1.375(14) . ? B2 F7 1.377(15) . ? B2 F5 1.377(16) . ? B2 F6 1.382(15) . ? B2A F7A 1.348(19) . ? B2A F5A 1.355(19) . ? B2A F6A 1.362(19) . ? B2A F8A 1.377(19) . ? B3 F9 1.304(17) . ? B3 F12 1.346(16) . ? B3 F10 1.359(17) . ? B3 F11 1.380(16) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.501(17) . ? C4 C5 1.3900 . ? C6 C7 1.32(2) . ? C7 C8 1.495(17) . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? N1Z C1Z 1.3900 . ? N1Z C5Z 1.3900 . ? C1Z C2Z 1.3900 . ? C2Z C3Z 1.3900 . ? C3Z C4Z 1.3900 . ? C3Z C6Z 1.48(3) . ? C4Z C5Z 1.3900 . ? C6Z C7Z 1.3200(11) . ? C7Z C8Z 1.55(4) . ? C8Z C9Z 1.3900 . ? C8Z C13Z 1.3900 . ? C9Z C10Z 1.3900 . ? C10Z C11Z 1.3900 . ? C11Z C12Z 1.3900 . ? C12Z C13Z 1.3900 . ? N2 C18 1.322(15) . ? N2 C14 1.329(14) . ? C14 C15 1.386(14) . ? C15 C16 1.413(16) . ? C16 C17 1.379(16) . ? C16 C19 1.480(14) . ? C17 C18 1.383(16) . ? C19 C20 1.323(16) . ? C20 C21 1.460(15) . ? C21 C26 1.397(19) . ? C21 C22 1.406(18) . ? C22 C23 1.380(17) . ? C23 C24 1.38(2) . ? C24 C25 1.34(2) . ? C25 C26 1.419(17) . ? C28 P4 1.831(10) 2_675 ? C1A C6A 1.345(16) . ? C1A C2A 1.367(15) . ? C2A C3A 1.379(17) . ? C3A C4A 1.349(19) . ? C4A C5A 1.37(2) . ? C5A C6A 1.393(19) . ? C1B C6B 1.376(14) . ? C1B C2B 1.401(14) . ? C2B C3B 1.394(16) . ? C3B C4B 1.382(18) . ? C4B C5B 1.384(17) . ? C5B C6B 1.397(15) . ? C1C C6C 1.373(15) . ? C1C C2C 1.385(15) . ? C2C C3C 1.362(17) . ? C3C C4C 1.345(18) . ? C4C C5C 1.377(17) . ? C5C C6C 1.375(15) . ? C1D C2D 1.377(14) . ? C1D C6D 1.396(14) . ? C2D C3D 1.381(15) . ? C3D C4D 1.382(18) . ? C4D C5D 1.374(18) . ? C5D C6D 1.384(15) . ? C1E C2E 1.388(15) . ? C1E C6E 1.393(14) . ? C2E C3E 1.366(16) . ? C3E C4E 1.372(16) . ? C4E C5E 1.388(16) . ? C5E C6E 1.388(15) . ? C1F C6F 1.397(14) . ? C1F C2F 1.412(15) . ? C2F C3F 1.375(15) . ? C3F C4F 1.384(16) . ? C4F C5F 1.388(18) . ? C5F C6F 1.372(16) . ? C1G C6G 1.393(14) . ? C1G C2G 1.422(14) . ? C2G C3G 1.387(15) . ? C3G C4G 1.383(17) . ? C4G C5G 1.376(17) . ? C5G C6G 1.380(15) . ? C1H C6H 1.386(15) . ? C1H C2H 1.388(16) . ? C2H C3H 1.392(16) . ? C3H C4H 1.420(18) . ? C4H C5H 1.381(18) . ? C5H C6H 1.381(16) . ? O1S C4S 1.379(18) . ? O1S C1S 1.400(17) . ? C1S C2S 1.39(2) . ? C2S C3S 1.48(3) . ? C3S C4S 1.50(2) . ? O2S C5S 1.391(18) . ? O2S C8S 1.398(19) . ? C5S C6S 1.513(19) . ? C6S C7S 1.522(19) . ? C7S C8S 1.521(19) . ? O3S C9S 1.402(18) . ? O3S C12S 1.407(18) . ? C9S C10S 1.526(19) . ? C10S C11S 1.529(19) . ? C11S C12S 1.504(18) . ? 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 N1Z Ag1 N1 6.8(8) . . ? N1Z Ag1 P1 159.6(7) . . ? N1 Ag1 P1 165.7(3) . . ? N1Z Ag1 Ag2 101.2(8) . . ? N1 Ag1 Ag2 100.9(4) . . ? P1 Ag1 Ag2 87.61(7) . . ? N2 Ag2 P2 177.3(3) . . ? N2 Ag2 Ag1 89.3(2) . . ? P2 Ag2 Ag1 90.03(7) . . ? P3 Ag3 P4 173.37(9) . . ? P3 Ag3 Ag3 90.82(7) . 2_675 ? P4 Ag3 Ag3 88.83(7) . 2_675 ? C1G P1 C1H 105.1(5) . . ? C1G P1 C27 102.9(5) . . ? C1H P1 C27 103.6(5) . . ? C1G P1 Ag1 116.1(3) . . ? C1H P1 Ag1 113.3(3) . . ? C27 P1 Ag1 114.4(3) . . ? C1F P2 C27 107.6(5) . . ? C1F P2 C1E 105.6(5) . . ? C27 P2 C1E 103.2(4) . . ? C1F P2 Ag2 116.9(3) . . ? C27 P2 Ag2 108.8(3) . . ? C1E P2 Ag2 113.8(3) . . ? C1C P3 C1D 102.9(4) . . ? C1C P3 C28 104.9(4) . . ? C1D P3 C28 105.1(4) . . ? C1C P3 Ag3 112.9(3) . . ? C1D P3 Ag3 115.8(3) . . ? C28 P3 Ag3 113.9(3) . . ? C1B P4 C1A 103.8(5) . . ? C1B P4 C28 105.1(4) . 2_675 ? C1A P4 C28 105.0(4) . 2_675 ? C1B P4 Ag3 114.5(3) . . ? C1A P4 Ag3 114.8(3) . . ? C28 P4 Ag3 112.6(3) 2_675 . ? F3 B1 F4 111.0(10) . . ? F3 B1 F1 109.7(9) . . ? F4 B1 F1 110.3(10) . . ? F3 B1 F2 109.4(10) . . ? F4 B1 F2 108.5(9) . . ? F1 B1 F2 107.9(10) . . ? F8 B2 F7 109.7(10) . . ? F8 B2 F5 109.5(10) . . ? F7 B2 F5 109.7(10) . . ? F8 B2 F6 109.4(10) . . ? F7 B2 F6 109.3(10) . . ? F5 B2 F6 109.2(10) . . ? F7A B2A F5A 110.5(12) . . ? F7A B2A F6A 110.3(12) . . ? F5A B2A F6A 109.7(12) . . ? F7A B2A F8A 109.1(12) . . ? F5A B2A F8A 108.8(12) . . ? F6A B2A F8A 108.3(12) . . ? F9 B3 F12 111.4(14) . . ? F9 B3 F10 107.7(12) . . ? F12 B3 F10 109.6(13) . . ? F9 B3 F11 109.8(13) . . ? F12 B3 F11 110.1(11) . . ? F10 B3 F11 108.1(11) . . ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 120.0(5) . . ? C5 N1 Ag1 120.0(5) . . ? C2 C1 N1 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 122.7(9) . . ? C2 C3 C6 117.3(9) . . ? C5 C4 C3 120.0 . . ? C4 C5 N1 120.0 . . ? C7 C6 C3 126.7(15) . . ? C6 C7 C8 127.0(16) . . ? C9 C8 C13 120.0 . . ? C9 C8 C7 118.9(9) . . ? C13 C8 C7 121.0(9) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C1Z N1Z C5Z 120.0 . . ? C1Z N1Z Ag1 122.0(11) . . ? C5Z N1Z Ag1 117.6(11) . . ? C2Z C1Z N1Z 120.0 . . ? C1Z C2Z C3Z 120.0 . . ? C4Z C3Z C2Z 120.0 . . ? C4Z C3Z C6Z 116(2) . . ? C2Z C3Z C6Z 124(2) . . ? C5Z C4Z C3Z 120.0 . . ? C4Z C5Z N1Z 120.0 . . ? C7Z C6Z C3Z 126(3) . . ? C6Z C7Z C8Z 123(3) . . ? C9Z C8Z C13Z 120.0 . . ? C9Z C8Z C7Z 118.4(14) . . ? C13Z C8Z C7Z 121.6(14) . . ? C8Z C9Z C10Z 120.0 . . ? C9Z C10Z C11Z 120.0 . . ? C12Z C11Z C10Z 120.0 . . ? C11Z C12Z C13Z 120.0 . . ? C12Z C13Z C8Z 120.0 . . ? C18 N2 C14 117.6(9) . . ? C18 N2 Ag2 120.0(7) . . ? C14 N2 Ag2 122.3(7) . . ? N2 C14 C15 124.2(11) . . ? C14 C15 C16 117.6(11) . . ? C17 C16 C15 117.6(10) . . ? C17 C16 C19 120.7(10) . . ? C15 C16 C19 121.6(11) . . ? C16 C17 C18 119.8(11) . . ? N2 C18 C17 123.1(11) . . ? C20 C19 C16 124.3(11) . . ? C19 C20 C21 125.9(11) . . ? C26 C21 C22 119.0(11) . . ? C26 C21 C20 118.9(11) . . ? C22 C21 C20 122.0(12) . . ? C23 C22 C21 119.5(13) . . ? C22 C23 C24 122.0(14) . . ? C25 C24 C23 118.6(12) . . ? C24 C25 C26 122.1(13) . . ? C21 C26 C25 118.7(13) . . ? P2 C27 P1 113.9(5) . . ? P4 C28 P3 111.7(5) 2_675 . ? C6A C1A C2A 119.0(11) . . ? C6A C1A P4 123.4(9) . . ? C2A C1A P4 117.5(8) . . ? C1A C2A C3A 121.3(12) . . ? C4A C3A C2A 120.0(12) . . ? C3A C4A C5A 119.0(12) . . ? C4A C5A C6A 120.8(13) . . ? C1A C6A C5A 119.8(13) . . ? C6B C1B C2B 119.7(9) . . ? C6B C1B P4 121.6(8) . . ? C2B C1B P4 118.7(8) . . ? C3B C2B C1B 119.6(11) . . ? C4B C3B C2B 119.8(11) . . ? C3B C4B C5B 120.9(11) . . ? C4B C5B C6B 119.0(10) . . ? C1B C6B C5B 120.9(10) . . ? C6C C1C C2C 117.6(10) . . ? C6C C1C P3 125.5(8) . . ? C2C C1C P3 116.9(8) . . ? C3C C2C C1C 121.2(11) . . ? C4C C3C C2C 121.0(12) . . ? C3C C4C C5C 119.1(11) . . ? C6C C5C C4C 120.4(11) . . ? C1C C6C C5C 120.7(10) . . ? C2D C1D C6D 120.5(10) . . ? C2D C1D P3 121.2(8) . . ? C6D C1D P3 118.3(8) . . ? C1D C2D C3D 119.5(11) . . ? C2D C3D C4D 120.7(11) . . ? C5D C4D C3D 119.3(10) . . ? C4D C5D C6D 121.1(11) . . ? C5D C6D C1D 118.8(10) . . ? C2E C1E C6E 119.3(10) . . ? C2E C1E P2 122.0(8) . . ? C6E C1E P2 118.5(8) . . ? C3E C2E C1E 120.0(11) . . ? C2E C3E C4E 121.3(11) . . ? C3E C4E C5E 119.6(10) . . ? C4E C5E C6E 119.7(10) . . ? C5E C6E C1E 120.1(10) . . ? C6F C1F C2F 118.5(10) . . ? C6F C1F P2 119.4(8) . . ? C2F C1F P2 122.0(8) . . ? C3F C2F C1F 120.0(10) . . ? C2F C3F C4F 120.7(11) . . ? C3F C4F C5F 119.7(10) . . ? C6F C5F C4F 120.4(11) . . ? C5F C6F C1F 120.8(11) . . ? C6G C1G C2G 119.7(9) . . ? C6G C1G P1 120.2(8) . . ? C2G C1G P1 120.0(8) . . ? C3G C2G C1G 119.4(10) . . ? C4G C3G C2G 119.1(11) . . ? C5G C4G C3G 121.9(11) . . ? C4G C5G C6G 119.9(11) . . ? C5G C6G C1G 119.9(10) . . ? C6H C1H C2H 120.1(10) . . ? C6H C1H P1 121.0(8) . . ? C2H C1H P1 118.8(9) . . ? C1H C2H C3H 120.8(12) . . ? C2H C3H C4H 118.2(11) . . ? C5H C4H C3H 120.4(11) . . ? C4H C5H C6H 120.2(12) . . ? C5H C6H C1H 120.3(11) . . ? C4S O1S C1S 106.7(12) . . ? C2S C1S O1S 109.2(14) . . ? C1S C2S C3S 108.2(16) . . ? C2S C3S C4S 101.9(13) . . ? O1S C4S C3S 107.3(13) . . ? C5S O2S C8S 97(3) . . ? O2S C5S C6S 112(3) . . ? C5S C6S C7S 100.9(19) . . ? C8S C7S C6S 100.5(18) . . ? O2S C8S C7S 113(2) . . ? C9S O3S C12S 110.1(19) . . ? O3S C9S C10S 107(2) . . ? C9S C10S C11S 105(2) . . ? C12S C11S C10S 102(2) . . ? O3S C12S C11S 106.5(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.463 _refine_diff_density_min -2.191 _refine_diff_density_rms 0.176 _database_code_depnum_ccdc_archive 'CCDC 934071' ####################################################################### # # 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_global _iucr_compatibility_tag ACTA95 #===#END #data_compound2 data_D057jj #TrackingRef 'GK13CC2013.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H82 Ag3 B3 F12 N2 O2 P4' _chemical_formula_weight 1859.44 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' B B 0.0013 0.0007 '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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9171(9) _cell_length_b 13.1457(10) _cell_length_c 25.686(2) _cell_angle_alpha 90.637(2) _cell_angle_beta 89.989(2) _cell_angle_gamma 99.454(2) _cell_volume 3969.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2197 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 17.45 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type Multi_scan _exptl_absorpt_correction_T_min 0.4684 _exptl_absorpt_correction_T_max 0.5633 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 43405 _diffrn_reflns_av_R_equivalents 0.1141 _diffrn_reflns_av_sigmaI/netI 0.1301 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13994 _reflns_number_gt 7210 _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. ; _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^)+(0.1385P)^2^+0.2639P] 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 13994 _refine_ls_number_parameters 864 _refine_ls_number_restraints 278 _refine_ls_R_factor_all 0.1775 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.2778 _refine_ls_wR_factor_gt 0.2360 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _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 O1S O 0.309(2) 0.334(2) 0.4108(11) 0.323(15) Uiso 1 1 d D . . C1S C 0.264(3) 0.3961(18) 0.3702(13) 0.260(9) Uiso 1 1 d D . . H1S1 H 0.2044 0.4340 0.3835 0.312 Uiso 1 1 calc R . . H1S2 H 0.3247 0.4439 0.3525 0.312 Uiso 1 1 calc R . . C2S C 0.217(3) 0.305(3) 0.3374(8) 0.260(9) Uiso 1 1 d D . . H2S1 H 0.1617 0.3225 0.3117 0.312 Uiso 1 1 calc R . . H2S2 H 0.2786 0.2770 0.3190 0.312 Uiso 1 1 calc R . . C3S C 0.162(2) 0.233(2) 0.3769(13) 0.260(9) Uiso 1 1 d D . . H3S1 H 0.1877 0.1654 0.3740 0.312 Uiso 1 1 calc R . . H3S2 H 0.0782 0.2231 0.3736 0.312 Uiso 1 1 calc R . . C4S C 0.201(3) 0.287(2) 0.4275(9) 0.260(9) Uiso 1 1 d D . . H4S1 H 0.1530 0.3384 0.4381 0.312 Uiso 1 1 calc R . . H4S2 H 0.2054 0.2381 0.4561 0.312 Uiso 1 1 calc R . . O2S O 0.922(6) -0.101(3) 0.494(3) 0.57(7) Uiso 0.50 1 d PD A -1 C7S C 0.992(5) 0.049(4) 0.4622(19) 0.199(14) Uiso 0.50 1 d PD A -1 H7S1 H 1.0566 0.1070 0.4609 0.238 Uiso 0.50 1 calc PR A -1 H7S2 H 0.9528 0.0423 0.4280 0.238 Uiso 0.50 1 calc PR A -1 C8S C 1.030(4) -0.049(4) 0.478(2) 0.199(14) Uiso 0.50 1 d PD A -1 H8S1 H 1.0605 -0.0845 0.4477 0.238 Uiso 0.50 1 calc PR A -1 H8S2 H 1.0859 -0.0394 0.5064 0.238 Uiso 0.50 1 calc PR A -1 C5S C 0.901(4) -0.030(4) 0.533(2) 0.199(14) Uiso 0.50 1 d PD A -1 H5S1 H 0.9571 -0.0261 0.5621 0.238 Uiso 0.50 1 calc PR A -1 H5S2 H 0.8230 -0.0485 0.5478 0.238 Uiso 0.50 1 calc PR A -1 C6S C 0.914(4) 0.065(4) 0.503(2) 0.199(14) Uiso 0.50 1 d PD A -1 H6S1 H 0.8402 0.0767 0.4888 0.238 Uiso 0.50 1 calc PR A -1 H6S2 H 0.9459 0.1256 0.5252 0.238 Uiso 0.50 1 calc PR A -1 O3S O 1.106(2) 1.010(2) 0.0118(13) 0.120(11) Uiso 0.50 1 d PD B -1 C9S C 1.010(3) 1.054(3) -0.0036(18) 0.123(15) Uiso 0.50 1 d PD B -1 H9S1 H 1.0181 1.0804 -0.0396 0.148 Uiso 0.50 1 calc PR B -1 H9S2 H 0.9962 1.1096 0.0205 0.148 Uiso 0.50 1 calc PR B -1 C10S C 0.917(4) 0.957(3) 0.001(2) 0.118(16) Uiso 0.50 1 d PD B -1 H10A H 0.8691 0.9656 0.0313 0.142 Uiso 0.50 1 calc PR B -1 H10B H 0.8670 0.9540 -0.0305 0.142 Uiso 0.50 1 calc PR B -1 C11S C 0.956(4) 0.854(4) 0.005(2) 0.18(2) Uiso 0.50 1 d PD B -1 H11A H 0.9157 0.8098 0.0320 0.220 Uiso 0.50 1 calc PR B -1 H11B H 0.9545 0.8164 -0.0288 0.220 Uiso 0.50 1 calc PR B -1 C12S C 1.074(4) 0.903(3) 0.0209(19) 0.149(17) Uiso 0.50 1 d PD B -1 H12A H 1.0822 0.8919 0.0587 0.179 Uiso 0.50 1 calc PR B -1 H12B H 1.1289 0.8665 0.0027 0.179 Uiso 0.50 1 calc PR B -1 Ag1 Ag 0.89199(8) 0.41502(7) 0.28226(4) 0.0579(3) Uani 1 1 d . . . Ag2 Ag 0.76803(9) 0.62229(8) 0.32767(4) 0.0684(4) Uani 1 1 d . . . Ag3 Ag 0.60922(8) 0.96054(6) 0.00968(3) 0.0495(3) Uani 1 1 d . . . P1 P 1.0030(2) 0.5367(2) 0.22840(11) 0.0441(7) Uani 1 1 d . . . P2 P 0.8658(2) 0.7095(2) 0.25748(12) 0.0456(7) Uani 1 1 d . . . P3 P 0.5816(2) 0.8581(2) -0.06964(10) 0.0340(6) Uani 1 1 d . . . P4 P 0.6345(2) 1.0553(2) 0.09188(11) 0.0378(7) Uani 1 1 d . . . N1 N 0.8487(7) 0.3133(6) 0.3478(3) 0.066(3) Uani 1 1 d G . . C1 C 0.7529(7) 0.2375(7) 0.3508(3) 0.080(4) Uani 1 1 d GU . . H1 H 0.7150 0.2103 0.3199 0.096 Uiso 1 1 calc R . . C2 C 0.7124(9) 0.2015(7) 0.3991(5) 0.106(6) Uani 1 1 d GU . . H2 H 0.6469 0.1496 0.4012 0.128 Uiso 1 1 calc R . . C3 C 0.7678(12) 0.2413(9) 0.4443(3) 0.127(7) Uani 1 1 d GU . . C4 C 0.8636(11) 0.3171(9) 0.4413(3) 0.132(7) Uani 1 1 d GU . . H4 H 0.9015 0.3443 0.4722 0.159 Uiso 1 1 calc R . . C5 C 0.9041(8) 0.3531(7) 0.3930(4) 0.111(6) Uani 1 1 d GU . . H5 H 0.9696 0.4049 0.3909 0.133 Uiso 1 1 calc R . . C6 C 0.7317(14) 0.2377(13) 0.5056(8) 0.122(7) Uani 1 1 d DU . . H6 H 0.7985 0.2431 0.5296 0.147 Uiso 1 1 calc R . . C7 C 0.6424(15) 0.1497(12) 0.5173(8) 0.123(7) Uani 1 1 d DU . . H7 H 0.6308 0.1009 0.4869 0.147 Uiso 1 1 calc R . . C8 C 0.6557(6) 0.0931(6) 0.5655(3) 0.105(4) Uani 1 1 d G . . C9 C 0.7045(7) 0.1349(7) 0.6117(3) 0.105(4) Uani 1 1 d G . . H9 H 0.7406 0.2048 0.6132 0.125 Uiso 1 1 calc R . . C10 C 0.7003(9) 0.0743(8) 0.6559(3) 0.163(7) Uani 1 1 d G . . H10 H 0.7336 0.1028 0.6875 0.195 Uiso 1 1 calc R . . C11 C 0.6473(8) -0.0281(8) 0.6538(4) 0.178(9) Uani 1 1 d G . . H11 H 0.6445 -0.0696 0.6840 0.213 Uiso 1 1 calc R . . C12 C 0.5986(9) -0.0699(7) 0.6076(4) 0.178(9) Uani 1 1 d G . . H12 H 0.5624 -0.1399 0.6062 0.213 Uiso 1 1 calc R . . C13 C 0.6028(9) -0.0093(6) 0.5634(4) 0.163(7) Uani 1 1 d G . . H13 H 0.5695 -0.0379 0.5318 0.195 Uiso 1 1 calc R . . N2 N 0.6866(8) 0.5400(6) 0.3941(3) 0.096(4) Uani 1 1 d G . . C14 C 0.6016(8) 0.4547(6) 0.3899(3) 0.111(6) Uani 1 1 d GU . . H14 H 0.5581 0.4428 0.3588 0.133 Uiso 1 1 calc R . . C15 C 0.5798(7) 0.3863(6) 0.4311(3) 0.106(6) Uani 1 1 d GU . . H15 H 0.5214 0.3279 0.4280 0.127 Uiso 1 1 calc R . . C16 C 0.6429(7) 0.4032(5) 0.4764(3) 0.148(8) Uani 1 1 d GU . . C17 C 0.7279(9) 0.4886(5) 0.4806(3) 0.175(9) Uani 1 1 d GU . . H17 H 0.7715 0.5005 0.5117 0.210 Uiso 1 1 calc R . . C18 C 0.7498(9) 0.5570(5) 0.4395(4) 0.162(10) Uani 1 1 d GU . . H18 H 0.8082 0.6154 0.4425 0.195 Uiso 1 1 calc R . . C19 C 0.6509(15) 0.3095(12) 0.5204(8) 0.123(7) Uani 1 1 d DU . . H19 H 0.6623 0.3367 0.5569 0.148 Uiso 1 1 calc R . . C20 C 0.5580(13) 0.2223(14) 0.5157(9) 0.130(7) Uani 1 1 d DU . . H20 H 0.5255 0.2211 0.4798 0.157 Uiso 1 1 calc R . . C21 C 0.4580(15) 0.2130(14) 0.5562(7) 0.154(8) Uani 1 1 d GU . . C22 C 0.4735(14) 0.2375(12) 0.6088(8) 0.162(8) Uani 1 1 d GU . . H22 H 0.5426 0.2779 0.6204 0.195 Uiso 1 1 calc R . . C23 C 0.388(2) 0.2031(15) 0.6442(5) 0.182(7) Uani 1 1 d GU . . H23 H 0.3986 0.2198 0.6802 0.218 Uiso 1 1 calc R . . C24 C 0.2868(16) 0.1441(16) 0.6271(8) 0.247(9) Uani 1 1 d GU . . H24 H 0.2284 0.1205 0.6514 0.296 Uiso 1 1 calc R . . C25 C 0.2713(14) 0.1195(14) 0.5746(10) 0.247(9) Uani 1 1 d GU . . H25 H 0.2022 0.0792 0.5629 0.296 Uiso 1 1 calc R . . C26 C 0.3569(19) 0.1540(15) 0.5391(6) 0.182(7) Uani 1 1 d GU . . H26 H 0.3462 0.1373 0.5032 0.218 Uiso 1 1 calc R . . C27 C 1.0056(9) 0.6729(9) 0.2464(4) 0.045(3) Uani 1 1 d . . . H27A H 1.0516 0.6883 0.2784 0.055 Uiso 1 1 calc R . . H27B H 1.0443 0.7164 0.2184 0.055 Uiso 1 1 calc R . . C28 C 0.4336(8) 0.8300(7) -0.0914(4) 0.029(2) Uani 1 1 d . . . H28A H 0.4309 0.7998 -0.1270 0.035 Uiso 1 1 calc R . . H28B H 0.3905 0.7782 -0.0681 0.035 Uiso 1 1 calc R . . C1Q C 0.7797(8) 1.1044(8) 0.1108(4) 0.038(2) Uani 1 1 d . . . C2Q C 0.8501(10) 1.0331(10) 0.1236(5) 0.061(3) Uani 1 1 d . . . H2Q H 0.8207 0.9615 0.1214 0.073 Uiso 1 1 calc R . . C3Q C 0.9608(11) 1.0643(12) 0.1393(5) 0.063(4) Uani 1 1 d . . . H3Q H 1.0064 1.0142 0.1482 0.076 Uiso 1 1 calc R . . C4Q C 1.0031(11) 1.1611(12) 0.1419(5) 0.067(4) Uani 1 1 d U . . H4Q H 1.0790 1.1815 0.1538 0.081 Uiso 1 1 calc R . . C5Q C 0.9410(13) 1.2342(13) 0.1280(8) 0.102(5) Uani 1 1 d U . . H5Q H 0.9747 1.3049 0.1277 0.123 Uiso 1 1 calc R . . C6Q C 0.8264(11) 1.2041(11) 0.1140(7) 0.089(5) Uani 1 1 d U . . H6Q H 0.7812 1.2554 0.1067 0.107 Uiso 1 1 calc R . . C1R C 0.5768(8) 0.9835(8) 0.1484(4) 0.040(3) Uani 1 1 d . . . C2R C 0.5224(9) 0.8822(8) 0.1423(5) 0.048(3) Uani 1 1 d . . . H2R H 0.5188 0.8501 0.1089 0.057 Uiso 1 1 calc R . . C3R C 0.4739(10) 0.8286(10) 0.1840(6) 0.062(4) Uani 1 1 d . . . H3R H 0.4349 0.7599 0.1796 0.075 Uiso 1 1 calc R . . C4R C 0.4817(11) 0.8745(11) 0.2329(5) 0.061(3) Uani 1 1 d . . . H4R H 0.4485 0.8371 0.2621 0.073 Uiso 1 1 calc R . . C5R C 0.5356(12) 0.9709(13) 0.2394(6) 0.073(4) Uani 1 1 d . . . H5R H 0.5416 1.0009 0.2733 0.088 Uiso 1 1 calc R . . C6R C 0.5831(9) 1.0287(9) 0.1974(5) 0.050(3) Uani 1 1 d . . . H6R H 0.6193 1.0981 0.2023 0.060 Uiso 1 1 calc R . . C1U C 0.6248(8) 0.7339(7) -0.0645(4) 0.034(2) Uani 1 1 d . . . C2U C 0.7407(10) 0.7300(9) -0.0631(5) 0.061(3) Uani 1 1 d U . . H2U H 0.7938 0.7919 -0.0659 0.073 Uiso 1 1 calc R . . C3U C 0.7798(11) 0.6368(10) -0.0575(6) 0.080(4) Uani 1 1 d U . . H3U H 0.8593 0.6358 -0.0559 0.096 Uiso 1 1 calc R . . C4U C 0.7065(10) 0.5487(9) -0.0543(5) 0.060(3) Uani 1 1 d U . . H4U H 0.7342 0.4853 -0.0511 0.072 Uiso 1 1 calc R . . C5U C 0.5937(10) 0.5491(8) -0.0555(5) 0.051(3) Uani 1 1 d . . . H5U H 0.5426 0.4857 -0.0531 0.061 Uiso 1 1 calc R . . C6U C 0.5512(8) 0.6397(8) -0.0603(4) 0.044(3) Uani 1 1 d . . . H6U H 0.4712 0.6384 -0.0606 0.052 Uiso 1 1 calc R . . C1V C 0.6602(8) 0.9117(8) -0.1260(4) 0.038(3) Uani 1 1 d . . . C2V C 0.6644(10) 0.8553(10) -0.1694(4) 0.054(3) Uani 1 1 d . . . H2V H 0.6223 0.7874 -0.1717 0.065 Uiso 1 1 calc R . . C3V C 0.7313(12) 0.8963(14) -0.2119(5) 0.078(4) Uani 1 1 d . . . H3V H 0.7362 0.8556 -0.2423 0.094 Uiso 1 1 calc R . . C4V C 0.7895(12) 0.9959(16) -0.2090(6) 0.083(6) Uani 1 1 d . . . H4V H 0.8351 1.0229 -0.2375 0.099 Uiso 1 1 calc R . . C5V C 0.7831(10) 1.0554(11) -0.1667(6) 0.070(4) Uani 1 1 d . . . H5V H 0.8218 1.1246 -0.1656 0.084 Uiso 1 1 calc R . . C6V C 0.7174(9) 1.0133(9) -0.1237(5) 0.056(3) Uani 1 1 d . . . H6V H 0.7122 1.0542 -0.0934 0.068 Uiso 1 1 calc R . . C1W C 0.9023(10) 0.8482(9) 0.2717(4) 0.049(3) Uani 1 1 d . . . C2W C 0.8439(12) 0.9173(10) 0.2499(5) 0.064(4) Uani 1 1 d . . . H2W H 0.7874 0.8940 0.2244 0.077 Uiso 1 1 calc R . . C3W C 0.8647(13) 1.0227(12) 0.2641(6) 0.077(4) Uani 1 1 d . . . H3W H 0.8235 1.0705 0.2486 0.092 Uiso 1 1 calc R . . C4W C 0.9452(14) 1.0530(11) 0.3004(6) 0.075(4) Uani 1 1 d . . . H4W H 0.9606 1.1234 0.3110 0.090 Uiso 1 1 calc R . . C5W C 1.0042(12) 0.9849(14) 0.3220(6) 0.085(5) Uani 1 1 d . . . H5W H 1.0619 1.0090 0.3467 0.103 Uiso 1 1 calc R . . C6W C 0.9834(10) 0.8810(10) 0.3092(5) 0.062(4) Uani 1 1 d . . . H6W H 1.0237 0.8337 0.3257 0.074 Uiso 1 1 calc R . . C1X C 0.7914(9) 0.6984(8) 0.1957(5) 0.047(3) Uani 1 1 d . . . C2X C 0.8391(10) 0.7468(9) 0.1509(5) 0.053(3) Uani 1 1 d . . . H2X H 0.9122 0.7883 0.1528 0.064 Uiso 1 1 calc R . . C3X C 0.7829(12) 0.7358(9) 0.1047(5) 0.059(3) Uani 1 1 d . . . H3X H 0.8179 0.7676 0.0745 0.071 Uiso 1 1 calc R . . C4X C 0.6768(13) 0.6796(11) 0.1017(6) 0.070(4) Uani 1 1 d . . . H4X H 0.6373 0.6730 0.0694 0.084 Uiso 1 1 calc R . . C5X C 0.6278(11) 0.6334(11) 0.1439(6) 0.068(4) Uani 1 1 d . . . H5X H 0.5538 0.5938 0.1411 0.082 Uiso 1 1 calc R . . C6X C 0.6831(10) 0.6424(10) 0.1920(5) 0.059(3) Uani 1 1 d . . . H6X H 0.6466 0.6102 0.2218 0.070 Uiso 1 1 calc R . . C1Y C 0.9689(9) 0.5314(8) 0.1600(4) 0.040(3) Uani 1 1 d . . . C2Y C 1.0417(10) 0.5830(9) 0.1233(4) 0.049(3) Uani 1 1 d . . . H2Y H 1.1126 0.6213 0.1341 0.058 Uiso 1 1 calc R . . C3Y C 1.0126(11) 0.5792(10) 0.0711(5) 0.058(3) Uani 1 1 d . . . H3Y H 1.0638 0.6134 0.0461 0.070 Uiso 1 1 calc R . . C4Y C 0.9078(12) 0.5250(10) 0.0558(5) 0.060(3) Uani 1 1 d . . . H4Y H 0.8863 0.5227 0.0201 0.072 Uiso 1 1 calc R . . C5Y C 0.8366(11) 0.4759(9) 0.0914(5) 0.061(3) Uani 1 1 d . . . H5Y H 0.7654 0.4387 0.0802 0.073 Uiso 1 1 calc R . . C6Y C 0.8638(10) 0.4779(9) 0.1437(5) 0.051(3) Uani 1 1 d . . . H6Y H 0.8117 0.4432 0.1682 0.061 Uiso 1 1 calc R . . C1Z C 1.1544(11) 0.5244(11) 0.2297(5) 0.056(3) Uani 1 1 d . . . C2Z C 1.1978(13) 0.4634(14) 0.1978(7) 0.100(6) Uani 1 1 d . . . H2Z H 1.1510 0.4284 0.1710 0.119 Uiso 1 1 calc R . . C3Z C 1.3132(16) 0.4475(14) 0.2016(7) 0.091(5) Uani 1 1 d . . . H3Z H 1.3396 0.3988 0.1790 0.109 Uiso 1 1 calc R . . C4Z C 1.3819(16) 0.4970(17) 0.2347(8) 0.106(6) Uani 1 1 d . . . H4Z H 1.4575 0.4830 0.2367 0.128 Uiso 1 1 calc R . . C5Z C 1.3481(15) 0.5726(17) 0.2689(11) 0.137(8) Uani 1 1 d . . . H5Z H 1.3996 0.6131 0.2921 0.164 Uiso 1 1 calc R . . C6Z C 1.2288(16) 0.5829(15) 0.2654(9) 0.123(7) Uani 1 1 d . . . H6Z H 1.2003 0.6306 0.2878 0.147 Uiso 1 1 calc R . . B1 B 0.6173(13) 0.3304(13) 0.2392(7) 0.066(4) Uani 1 1 d . . . F1 F 0.5398(7) 0.2731(7) 0.2688(4) 0.107(3) Uani 1 1 d . . . F2 F 0.5723(7) 0.3467(8) 0.1921(4) 0.109(3) Uani 1 1 d . . . F3 F 0.6554(7) 0.4222(6) 0.2638(3) 0.078(2) Uani 1 1 d . . . F4 F 0.7129(7) 0.2822(6) 0.2315(3) 0.087(2) Uani 1 1 d . . . B2 B 0.3242(10) 0.7413(8) 0.0386(5) 0.055(4) Uani 1 1 d D . . F5 F 0.2768(6) 0.6780(5) 0.0009(2) 0.067(2) Uani 1 1 d D . . F6 F 0.2522(10) 0.7395(10) 0.0810(4) 0.057(2) Uiso 0.50 1 d PD . . F7 F 0.3726(10) 0.8360(7) 0.0279(5) 0.057(2) Uiso 0.50 1 d PD . . F8 F 0.4152(9) 0.6946(9) 0.0603(5) 0.057(2) Uiso 0.50 1 d PD . . F6X F 0.2919(12) 0.7201(11) 0.0857(4) 0.080(3) Uiso 0.50 1 d PD . . F8X F 0.4437(9) 0.7487(11) 0.0351(6) 0.080(3) Uiso 0.50 1 d PD . . F7X F 0.3104(13) 0.8409(8) 0.0233(5) 0.080(3) Uiso 0.50 1 d PD . . B3 B 0.945(3) 0.381(2) 0.6032(10) 0.121(8) Uani 1 1 d U . . F9 F 0.9352(15) 0.4334(13) 0.5627(6) 0.210(7) Uani 1 1 d U . . F10 F 0.9872(16) 0.2952(13) 0.5839(7) 0.220(7) Uani 1 1 d U . . F11 F 1.0173(11) 0.4271(9) 0.6376(4) 0.135(4) Uani 1 1 d U . . F12 F 0.8467(16) 0.3443(16) 0.6244(7) 0.237(8) 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 Ag1 0.0642(7) 0.0592(6) 0.0508(6) 0.0163(4) 0.0209(5) 0.0108(5) Ag2 0.0654(7) 0.0737(7) 0.0650(7) 0.0214(5) 0.0239(5) 0.0066(5) Ag3 0.0633(6) 0.0371(5) 0.0482(5) -0.0013(4) -0.0035(4) 0.0086(4) P1 0.0441(17) 0.0533(19) 0.0364(16) 0.0082(13) 0.0065(13) 0.0126(14) P2 0.0408(17) 0.0517(19) 0.0442(17) 0.0036(14) 0.0066(13) 0.0067(14) P3 0.0307(15) 0.0313(14) 0.0407(15) 0.0081(12) 0.0007(12) 0.0066(11) P4 0.0353(16) 0.0297(15) 0.0506(17) 0.0049(12) 0.0012(13) 0.0119(12) N1 0.069(8) 0.063(7) 0.066(7) 0.018(6) 0.015(6) 0.005(6) C1 0.079(10) 0.079(10) 0.079(10) 0.004(8) 0.044(8) 0.004(8) C2 0.134(14) 0.070(10) 0.111(13) 0.000(9) 0.062(12) 0.005(10) C3 0.21(2) 0.082(12) 0.088(12) 0.033(10) 0.071(13) 0.024(12) C4 0.23(2) 0.099(13) 0.065(10) 0.020(10) 0.016(12) 0.013(13) C5 0.165(17) 0.101(13) 0.054(9) 0.019(9) 0.007(11) -0.017(12) C6 0.121(10) 0.115(10) 0.128(10) 0.005(8) 0.005(8) 0.010(8) C7 0.105(9) 0.134(10) 0.127(10) 0.009(8) 0.020(8) 0.010(8) C8 0.068(8) 0.161(13) 0.080(8) 0.046(9) -0.002(6) 0.002(8) C9 0.068(8) 0.161(13) 0.080(8) 0.046(9) -0.002(6) 0.002(8) C10 0.132(13) 0.24(2) 0.115(12) 0.043(13) -0.050(10) 0.032(13) C11 0.131(15) 0.185(18) 0.21(2) 0.070(16) -0.074(13) 0.015(13) C12 0.131(15) 0.185(18) 0.21(2) 0.070(16) -0.074(13) 0.015(13) C13 0.132(13) 0.24(2) 0.115(12) 0.043(13) -0.050(10) 0.032(13) N2 0.140(13) 0.069(9) 0.080(9) 0.012(7) 0.059(9) 0.026(8) C14 0.084(12) 0.095(13) 0.152(17) 0.009(12) 0.056(11) 0.008(10) C15 0.093(12) 0.072(10) 0.152(16) 0.026(11) 0.046(11) 0.009(9) C16 0.22(2) 0.123(15) 0.099(14) 0.019(13) 0.082(14) 0.016(15) C17 0.33(3) 0.101(15) 0.092(13) 0.003(12) 0.076(16) 0.012(16) C18 0.35(3) 0.076(12) 0.055(11) 0.008(9) 0.053(15) 0.005(16) C19 0.116(10) 0.124(10) 0.129(10) -0.002(8) 0.013(8) 0.016(8) C20 0.117(10) 0.134(10) 0.141(11) 0.026(8) 0.010(8) 0.021(8) C21 0.144(11) 0.157(11) 0.163(11) 0.009(9) -0.006(9) 0.035(8) C22 0.165(11) 0.174(11) 0.160(11) 0.020(9) -0.015(9) 0.059(9) C23 0.171(9) 0.191(9) 0.186(9) 0.012(6) 0.007(6) 0.036(6) C24 0.247(11) 0.250(11) 0.239(11) 0.000(7) 0.019(7) 0.028(7) C25 0.247(11) 0.250(11) 0.239(11) 0.000(7) 0.019(7) 0.028(7) C26 0.171(9) 0.191(9) 0.186(9) 0.012(6) 0.007(6) 0.036(6) C27 0.033(6) 0.065(8) 0.036(6) 0.006(5) 0.002(5) -0.001(5) C28 0.031(5) 0.027(5) 0.034(5) 0.010(4) -0.004(4) 0.014(4) C1Q 0.032(6) 0.039(6) 0.048(6) 0.005(5) -0.008(5) 0.013(5) C2Q 0.051(8) 0.061(8) 0.073(9) 0.024(7) 0.000(7) 0.014(6) C3Q 0.042(8) 0.084(11) 0.071(9) 0.017(8) 0.002(6) 0.029(7) C4Q 0.034(7) 0.086(10) 0.085(9) -0.012(8) -0.007(6) 0.019(7) C5Q 0.055(9) 0.074(10) 0.179(15) -0.026(10) -0.018(9) 0.015(8) C6Q 0.043(8) 0.055(8) 0.172(14) -0.019(8) -0.027(8) 0.018(6) C1R 0.034(6) 0.034(6) 0.055(7) 0.008(5) -0.006(5) 0.018(5) C2R 0.038(6) 0.042(7) 0.067(8) 0.023(6) 0.010(6) 0.019(5) C3R 0.048(8) 0.041(7) 0.099(11) 0.023(7) -0.004(7) 0.009(6) C4R 0.060(9) 0.057(9) 0.068(9) 0.021(7) 0.011(7) 0.017(7) C5R 0.063(9) 0.097(12) 0.070(10) 0.007(8) -0.006(7) 0.046(9) C6R 0.047(7) 0.050(7) 0.053(8) 0.024(6) 0.010(6) 0.008(6) C1U 0.030(6) 0.039(6) 0.036(6) 0.010(5) -0.002(4) 0.013(5) C2U 0.036(7) 0.046(7) 0.098(9) 0.014(6) -0.004(6) 0.005(5) C3U 0.043(7) 0.052(8) 0.148(12) 0.037(8) -0.016(8) 0.012(6) C4U 0.048(7) 0.049(7) 0.085(9) 0.023(6) -0.016(6) 0.012(6) C5U 0.049(8) 0.030(6) 0.070(8) 0.005(5) -0.019(6) -0.002(5) C6U 0.023(6) 0.045(7) 0.062(7) 0.010(5) -0.015(5) 0.002(5) C1V 0.026(6) 0.042(6) 0.049(7) 0.022(5) 0.011(5) 0.011(5) C2V 0.057(8) 0.070(8) 0.039(7) 0.007(6) 0.001(6) 0.018(6) C3V 0.067(10) 0.123(14) 0.054(9) 0.024(9) 0.009(7) 0.040(10) C4V 0.048(9) 0.148(16) 0.066(10) 0.070(11) 0.033(7) 0.052(10) C5V 0.036(7) 0.076(10) 0.103(12) 0.060(9) 0.029(7) 0.019(6) C6V 0.039(7) 0.058(8) 0.077(9) 0.024(7) 0.006(6) 0.021(6) C1W 0.047(7) 0.056(8) 0.042(7) 0.001(6) 0.013(6) 0.007(6) C2W 0.075(9) 0.067(9) 0.055(8) -0.010(7) -0.006(7) 0.026(7) C3W 0.093(11) 0.076(11) 0.069(10) -0.012(8) -0.007(9) 0.036(9) C4W 0.089(11) 0.056(9) 0.080(11) -0.018(8) 0.014(9) 0.015(8) C5W 0.064(10) 0.112(14) 0.077(11) -0.048(10) -0.007(8) 0.005(9) C6W 0.055(8) 0.059(8) 0.070(9) -0.035(7) 0.001(7) 0.008(6) C1X 0.040(7) 0.045(7) 0.058(7) 0.002(6) 0.004(6) 0.014(5) C2X 0.051(7) 0.040(7) 0.067(8) 0.010(6) -0.005(6) 0.002(6) C3X 0.084(10) 0.034(7) 0.056(8) 0.000(6) -0.014(7) -0.002(7) C4X 0.072(10) 0.074(10) 0.065(9) 0.003(8) -0.015(8) 0.018(8) C5X 0.033(7) 0.090(11) 0.081(10) -0.027(9) -0.005(7) 0.010(7) C6X 0.037(7) 0.063(8) 0.074(9) -0.007(7) 0.012(6) 0.003(6) C1Y 0.040(6) 0.043(6) 0.039(6) -0.002(5) 0.012(5) 0.012(5) C2Y 0.047(7) 0.061(8) 0.041(7) 0.005(6) 0.013(5) 0.018(6) C3Y 0.063(9) 0.071(9) 0.043(7) 0.006(6) 0.012(6) 0.022(7) C4Y 0.070(9) 0.068(9) 0.043(7) -0.007(6) 0.003(7) 0.011(7) C5Y 0.058(8) 0.048(8) 0.075(10) -0.018(7) -0.012(7) 0.003(6) C6Y 0.057(8) 0.046(7) 0.050(7) -0.013(6) 0.011(6) 0.010(6) C1Z 0.045(7) 0.094(10) 0.037(7) 0.006(6) -0.003(6) 0.032(7) C2Z 0.058(10) 0.132(15) 0.115(14) -0.041(12) -0.023(9) 0.039(10) C3Z 0.096(14) 0.109(14) 0.082(12) 0.004(10) 0.000(10) 0.054(11) C4Z 0.066(12) 0.140(18) 0.122(16) 0.038(14) 0.017(11) 0.041(12) C5Z 0.052(11) 0.121(17) 0.24(3) 0.005(17) -0.018(14) 0.014(11) C6Z 0.095(15) 0.103(15) 0.18(2) 0.011(14) 0.010(14) 0.052(12) B1 0.045(9) 0.070(11) 0.081(12) -0.012(9) 0.013(9) 0.004(8) F1 0.071(6) 0.117(8) 0.123(8) -0.025(6) 0.027(5) -0.014(5) F2 0.073(6) 0.152(9) 0.099(7) -0.053(6) -0.024(5) 0.011(6) F3 0.080(5) 0.066(5) 0.087(6) -0.024(4) -0.018(4) 0.012(4) F4 0.076(6) 0.075(5) 0.107(7) -0.017(5) 0.022(5) 0.008(4) B2 0.077(11) 0.024(7) 0.058(9) 0.002(6) 0.018(8) -0.009(7) F5 0.097(6) 0.042(4) 0.054(4) 0.002(3) -0.009(4) -0.011(4) B3 0.145(16) 0.107(14) 0.087(13) -0.021(12) -0.001(13) -0.048(13) F9 0.268(15) 0.213(13) 0.141(10) 0.037(10) -0.098(10) 0.016(11) F10 0.245(15) 0.165(12) 0.245(14) -0.061(11) -0.012(12) 0.028(11) F11 0.183(10) 0.123(8) 0.087(7) 0.012(6) -0.028(7) -0.012(7) F12 0.210(13) 0.278(15) 0.190(13) -0.066(12) 0.048(11) -0.049(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1S C4S 1.394(18) . ? O1S C1S 1.486(18) . ? C1S C2S 1.484(18) . ? C2S C3S 1.476(17) . ? C3S C4S 1.510(17) . ? O2S C8S 1.41(2) . ? O2S C5S 1.42(2) . ? C7S C6S 1.436(18) . ? C7S C8S 1.503(19) . ? C5S C6S 1.473(18) . ? O3S C12S 1.409(19) . ? O3S C9S 1.420(19) . ? C9S C10S 1.558(19) . ? C10S C11S 1.50(2) . ? C11S C12S 1.50(2) . ? Ag1 N1 2.170(6) . ? Ag1 P1 2.361(3) . ? Ag2 N2 2.172(6) . ? Ag2 P2 2.351(3) . ? Ag3 P3 2.422(3) . ? Ag3 P4 2.433(3) . ? Ag3 Ag3 2.9999(18) 2_675 ? P1 C1Y 1.800(11) . ? P1 C1Z 1.838(12) . ? P1 C27 1.840(12) . ? P2 C1X 1.810(12) . ? P2 C27 1.829(11) . ? P2 C1W 1.837(12) . ? P3 C1U 1.797(10) . ? P3 C1V 1.810(10) . ? P3 C28 1.828(9) . ? P4 C1Q 1.810(10) . ? P4 C1R 1.812(11) . ? P4 C28 1.826(9) 2_675 ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.63(2) . ? C4 C5 1.3900 . ? C6 C7 1.472(16) . ? C6 C19 1.500(17) . ? C7 C8 1.47(2) . ? C7 C20 1.496(17) . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? N2 C18 1.3834 . ? N2 C14 1.3859 . ? C14 C15 1.3926 . ? C15 C16 1.3834 . ? C16 C17 1.3860 . ? C16 C19 1.69(2) . ? C17 C18 1.3926 . ? C19 C20 1.461(17) . ? C20 C21 1.57(2) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C28 P4 1.826(9) 2_675 ? C1Q C6Q 1.339(16) . ? C1Q C2Q 1.398(15) . ? C2Q C3Q 1.374(17) . ? C3Q C4Q 1.291(18) . ? C4Q C5Q 1.356(19) . ? C5Q C6Q 1.404(19) . ? C1R C6R 1.382(15) . ? C1R C2R 1.390(15) . ? C2R C3R 1.366(16) . ? C3R C4R 1.384(18) . ? C4R C5R 1.331(18) . ? C5R C6R 1.393(17) . ? C1U C2U 1.390(14) . ? C1U C6U 1.401(14) . ? C2U C3U 1.389(16) . ? C3U C4U 1.334(16) . ? C4U C5U 1.346(16) . ? C5U C6U 1.376(14) . ? C1V C2V 1.338(15) . ? C1V C6V 1.397(15) . ? C2V C3V 1.409(18) . ? C3V C4V 1.38(2) . ? C4V C5V 1.34(2) . ? C5V C6V 1.418(16) . ? C1W C2W 1.357(16) . ? C1W C6W 1.378(16) . ? C2W C3W 1.411(18) . ? C3W C4W 1.347(19) . ? C4W C5W 1.35(2) . ? C5W C6W 1.383(19) . ? C1X C6X 1.380(15) . ? C1X C2X 1.397(16) . ? C2X C3X 1.357(16) . ? C3X C4X 1.358(18) . ? C4X C5X 1.335(19) . ? C5X C6X 1.396(18) . ? C1Y C2Y 1.388(14) . ? C1Y C6Y 1.393(15) . ? C2Y C3Y 1.382(16) . ? C3Y C4Y 1.388(17) . ? C4Y C5Y 1.344(17) . ? C5Y C6Y 1.382(16) . ? C1Z C2Z 1.305(18) . ? C1Z C6Z 1.41(2) . ? C2Z C3Z 1.43(2) . ? C3Z C4Z 1.28(2) . ? C4Z C5Z 1.42(3) . ? C5Z C6Z 1.45(2) . ? B1 F1 1.334(18) . ? B1 F2 1.357(19) . ? B1 F3 1.366(17) . ? B1 F4 1.404(17) . ? B2 F6X 1.290(12) . ? B2 F7 1.315(12) . ? B2 F5 1.334(14) . ? B2 F6 1.385(12) . ? B2 F7X 1.406(12) . ? B2 F8X 1.414(13) . ? B2 F8 1.446(13) . ? F6 F6X 0.586(18) . ? F7 F7X 0.764(16) . ? F7 F8X 1.547(16) . ? F8 F8X 0.985(16) . ? F8 F6X 1.690(17) . ? B3 F9 1.27(3) . ? B3 F11 1.31(2) . ? B3 F12 1.31(3) . ? B3 F10 1.39(3) . ? 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 C4S O1S C1S 94.4(14) . . ? C2S C1S O1S 94.1(13) . . ? C3S C2S C1S 101.4(12) . . ? C2S C3S C4S 102.7(11) . . ? O1S C4S C3S 97.5(14) . . ? C8S O2S C5S 98.5(18) . . ? C6S C7S C8S 102.7(13) . . ? O2S C8S C7S 96.5(16) . . ? O2S C5S C6S 99.7(16) . . ? C7S C6S C5S 104.5(11) . . ? C12S O3S C9S 111(3) . . ? O3S C9S C10S 99(3) . . ? C11S C10S C9S 117(4) . . ? C12S C11S C10S 93(4) . . ? O3S C12S C11S 117(4) . . ? N1 Ag1 P1 158.7(3) . . ? N2 Ag2 P2 176.8(3) . . ? P3 Ag3 P4 177.04(10) . . ? P3 Ag3 Ag3 90.23(7) . 2_675 ? P4 Ag3 Ag3 90.61(7) . 2_675 ? C1Y P1 C1Z 103.5(5) . . ? C1Y P1 C27 103.9(5) . . ? C1Z P1 C27 102.8(6) . . ? C1Y P1 Ag1 117.0(4) . . ? C1Z P1 Ag1 112.2(4) . . ? C27 P1 Ag1 115.8(3) . . ? C1X P2 C27 107.5(5) . . ? C1X P2 C1W 106.1(5) . . ? C27 P2 C1W 102.2(5) . . ? C1X P2 Ag2 116.1(4) . . ? C27 P2 Ag2 112.9(4) . . ? C1W P2 Ag2 110.9(4) . . ? C1U P3 C1V 102.3(5) . . ? C1U P3 C28 104.7(4) . . ? C1V P3 C28 104.7(5) . . ? C1U P3 Ag3 113.7(3) . . ? C1V P3 Ag3 116.1(4) . . ? C28 P3 Ag3 113.9(3) . . ? C1Q P4 C1R 103.3(5) . . ? C1Q P4 C28 103.8(5) . 2_675 ? C1R P4 C28 105.1(4) . 2_675 ? C1Q P4 Ag3 116.2(4) . . ? C1R P4 Ag3 115.1(4) . . ? C28 P4 Ag3 112.0(3) 2_675 . ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 125.2(5) . . ? C5 N1 Ag1 111.6(5) . . ? N1 C1 C2 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 105.3(10) . . ? C2 C3 C6 133.3(10) . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C7 C6 C19 89.2(8) . . ? C7 C6 C3 112.4(16) . . ? C19 C6 C3 114.4(16) . . ? C6 C7 C8 117.0(17) . . ? C6 C7 C20 88.0(8) . . ? C8 C7 C20 119.4(16) . . ? C9 C8 C13 120.0 . . ? C9 C8 C7 126.3(8) . . ? C13 C8 C7 113.4(8) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C8 120.0 . . ? C18 N2 C14 119.6 . . ? C18 N2 Ag2 113.5(4) . . ? C14 N2 Ag2 123.8(4) . . ? N2 C14 C15 120.3 . . ? C16 C15 C14 120.1 . . ? C15 C16 C17 119.6 . . ? C15 C16 C19 123.0(7) . . ? C17 C16 C19 114.9(7) . . ? C16 C17 C18 120.3 . . ? N2 C18 C17 120.1 . . ? C20 C19 C6 88.3(8) . . ? C20 C19 C16 113.3(16) . . ? C6 C19 C16 114.2(15) . . ? C19 C20 C7 89.8(8) . . ? C19 C20 C21 118.6(18) . . ? C7 C20 C21 120.5(17) . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 123.6(17) . . ? C26 C21 C20 114.5(17) . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? P2 C27 P1 114.9(6) . . ? P4 C28 P3 112.5(5) 2_675 . ? C6Q C1Q C2Q 116.4(11) . . ? C6Q C1Q P4 125.6(9) . . ? C2Q C1Q P4 118.0(9) . . ? C3Q C2Q C1Q 121.5(12) . . ? C4Q C3Q C2Q 120.4(12) . . ? C3Q C4Q C5Q 121.1(13) . . ? C4Q C5Q C6Q 119.2(15) . . ? C1Q C6Q C5Q 121.2(13) . . ? C6R C1R C2R 119.2(10) . . ? C6R C1R P4 121.2(8) . . ? C2R C1R P4 119.6(9) . . ? C3R C2R C1R 120.3(12) . . ? C2R C3R C4R 119.7(12) . . ? C5R C4R C3R 120.4(13) . . ? C4R C5R C6R 121.3(14) . . ? C1R C6R C5R 118.9(12) . . ? C2U C1U C6U 116.6(9) . . ? C2U C1U P3 118.1(8) . . ? C6U C1U P3 125.3(7) . . ? C3U C2U C1U 121.0(11) . . ? C4U C3U C2U 120.4(12) . . ? C3U C4U C5U 120.5(11) . . ? C4U C5U C6U 121.0(10) . . ? C5U C6U C1U 120.5(10) . . ? C2V C1V C6V 120.0(10) . . ? C2V C1V P3 120.9(9) . . ? C6V C1V P3 119.1(9) . . ? C1V C2V C3V 120.1(13) . . ? C4V C3V C2V 119.6(14) . . ? C5V C4V C3V 121.5(12) . . ? C4V C5V C6V 118.8(14) . . ? C1V C6V C5V 120.0(13) . . ? C2W C1W C6W 119.5(12) . . ? C2W C1W P2 121.4(10) . . ? C6W C1W P2 118.7(10) . . ? C1W C2W C3W 121.7(13) . . ? C4W C3W C2W 117.6(13) . . ? C3W C4W C5W 120.9(14) . . ? C4W C5W C6W 122.2(14) . . ? C1W C6W C5W 118.0(13) . . ? C6X C1X C2X 117.7(11) . . ? C6X C1X P2 120.1(9) . . ? C2X C1X P2 122.2(9) . . ? C3X C2X C1X 121.3(12) . . ? C2X C3X C4X 120.2(13) . . ? C5X C4X C3X 120.2(13) . . ? C4X C5X C6X 121.3(13) . . ? C1X C6X C5X 119.3(12) . . ? C2Y C1Y C6Y 118.8(10) . . ? C2Y C1Y P1 122.0(9) . . ? C6Y C1Y P1 119.1(8) . . ? C3Y C2Y C1Y 120.9(12) . . ? C2Y C3Y C4Y 119.2(12) . . ? C5Y C4Y C3Y 119.9(12) . . ? C4Y C5Y C6Y 122.1(12) . . ? C5Y C6Y C1Y 119.0(11) . . ? C2Z C1Z C6Z 117.3(13) . . ? C2Z C1Z P1 122.4(11) . . ? C6Z C1Z P1 120.3(11) . . ? C1Z C2Z C3Z 122.3(15) . . ? C4Z C3Z C2Z 121.6(17) . . ? C3Z C4Z C5Z 121.7(18) . . ? C4Z C5Z C6Z 114.8(19) . . ? C1Z C6Z C5Z 121.9(18) . . ? F1 B1 F2 110.4(13) . . ? F1 B1 F3 109.7(13) . . ? F2 B1 F3 110.4(14) . . ? F1 B1 F4 111.1(14) . . ? F2 B1 F4 108.7(13) . . ? F3 B1 F4 106.4(12) . . ? F6X B2 F7 118.8(13) . . ? F6X B2 F5 117.4(10) . . ? F7 B2 F5 120.5(10) . . ? F6X B2 F6 25.0(8) . . ? F7 B2 F6 111.3(10) . . ? F5 B2 F6 110.9(9) . . ? F6X B2 F7X 113.5(11) . . ? F7 B2 F7X 32.4(7) . . ? F5 B2 F7X 105.6(10) . . ? F6 B2 F7X 94.5(10) . . ? F6X B2 F8X 109.7(11) . . ? F7 B2 F8X 69.0(9) . . ? F5 B2 F8X 108.4(9) . . ? F6 B2 F8X 131.8(12) . . ? F7X B2 F8X 100.8(9) . . ? F6X B2 F8 76.1(10) . . ? F7 B2 F8 104.2(10) . . ? F5 B2 F8 106.7(9) . . ? F6 B2 F8 101.1(9) . . ? F7X B2 F8 136.0(11) . . ? F8X B2 F8 40.3(7) . . ? F6X F6 B2 68.3(13) . . ? F7X F7 B2 80.4(11) . . ? F7X F7 F8X 137.7(13) . . ? B2 F7 F8X 58.5(7) . . ? F8X F8 B2 68.1(8) . . ? F8X F8 F6X 108.7(10) . . ? B2 F8 F6X 47.8(6) . . ? F6 F6X B2 86.7(15) . . ? F6 F6X F8 142.7(17) . . ? B2 F6X F8 56.1(7) . . ? F8 F8X B2 71.6(8) . . ? F8 F8X F7 117.0(11) . . ? B2 F8X F7 52.5(6) . . ? F7 F7X B2 67.2(10) . . ? F9 B3 F11 114(2) . . ? F9 B3 F12 113(3) . . ? F11 B3 F12 112(2) . . ? F9 B3 F10 103(2) . . ? F11 B3 F10 108(3) . . ? F12 B3 F10 106(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.544 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 934072' ####################################################################### # # 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_global _iucr_compatibility_tag ACTA95 #===#END # data_compound3 data_a789jj #TrackingRef 'GK13CC2013.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H46 Ag2 F6 N2 O4 P2' _chemical_formula_weight 1202.63 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.550(2) _cell_length_b 13.733(2) _cell_length_c 14.479(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.245(5) _cell_angle_gamma 90.00 _cell_volume 2495.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 937 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6080 _exptl_absorpt_correction_T_max 0.7957 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17401 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5718 _reflns_number_gt 5424 _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. ; _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^)+(0.0406P)^2^+3.3057P] 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 5718 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.480989(14) 0.493237(12) 0.243394(11) 0.01738(7) Uani 1 1 d . . . P1 P 0.55419(4) 0.58717(4) 0.12199(4) 0.01297(12) Uani 1 1 d . . . N1 N 0.41437(15) 0.52703(14) 0.38241(13) 0.0160(4) Uani 1 1 d . . . O1 O 0.37802(15) 0.36062(13) 0.19344(12) 0.0268(4) Uani 1 1 d . . . O2 O 0.41863(14) 0.27241(14) 0.31970(12) 0.0248(4) Uani 1 1 d . . . F1 F 0.40456(13) 0.15225(11) 0.14174(12) 0.0326(4) Uani 1 1 d . . . F2 F 0.24806(13) 0.21651(12) 0.14068(11) 0.0316(4) Uani 1 1 d . . . F3 F 0.29688(14) 0.12780(12) 0.25508(12) 0.0358(4) Uani 1 1 d . . . C1 C 0.45538(18) 0.59957(16) 0.43383(15) 0.0160(4) Uani 1 1 d . . . H1 H 0.5129 0.6360 0.4090 0.019 Uiso 1 1 calc R . . C2 C 0.41895(18) 0.62431(16) 0.52064(15) 0.0166(4) Uani 1 1 d . . . H2 H 0.4508 0.6763 0.5541 0.020 Uiso 1 1 calc R . . C3 C 0.33417(18) 0.57144(16) 0.55861(15) 0.0157(4) Uani 1 1 d . . . C4 C 0.29061(19) 0.49695(16) 0.50443(17) 0.0182(5) Uani 1 1 d . . . H4 H 0.2321 0.4601 0.5269 0.022 Uiso 1 1 calc R . . C5 C 0.33242(18) 0.47690(17) 0.41841(16) 0.0182(4) Uani 1 1 d . . . H5 H 0.3020 0.4255 0.3832 0.022 Uiso 1 1 calc R . . C6 C 0.29031(18) 0.59047(16) 0.65056(16) 0.0178(4) Uani 1 1 d . . . H6 H 0.2275 0.5562 0.6671 0.021 Uiso 1 1 calc R . . C7 C 0.33099(18) 0.65171(16) 0.71307(15) 0.0169(4) Uani 1 1 d . . . H7 H 0.3966 0.6826 0.6988 0.020 Uiso 1 1 calc R . . C8 C 0.28163(18) 0.67489(16) 0.80250(15) 0.0160(4) Uani 1 1 d . . . C9 C 0.34193(18) 0.72051(17) 0.87157(16) 0.0184(4) Uani 1 1 d . . . H9 H 0.4142 0.7368 0.8599 0.022 Uiso 1 1 calc R . . C10 C 0.29793(19) 0.74238(17) 0.95671(16) 0.0206(5) Uani 1 1 d . . . H10 H 0.3404 0.7725 1.0031 0.025 Uiso 1 1 calc R . . C11 C 0.1921(2) 0.72044(18) 0.97437(16) 0.0228(5) Uani 1 1 d . . . H11 H 0.1620 0.7348 1.0329 0.027 Uiso 1 1 calc R . . C12 C 0.1304(2) 0.67719(18) 0.90562(17) 0.0231(5) Uani 1 1 d . . . H12 H 0.0576 0.6628 0.9171 0.028 Uiso 1 1 calc R . . C13 C 0.17428(19) 0.65486(17) 0.82037(16) 0.0201(5) Uani 1 1 d . . . H13 H 0.1312 0.6258 0.7738 0.024 Uiso 1 1 calc R . . C14 C 0.37986(17) 0.28616(17) 0.24265(15) 0.0173(4) Uani 1 1 d . . . C15 C 0.3305(2) 0.19532(17) 0.19568(17) 0.0215(5) Uani 1 1 d . . . C16 C 0.49445(17) 0.55437(15) 0.01067(14) 0.0139(4) Uani 1 1 d . . . H16A H 0.4179 0.5719 0.0111 0.017 Uiso 1 1 calc R . . H16B H 0.5292 0.5924 -0.0389 0.017 Uiso 1 1 calc R . . C1A C 0.69753(17) 0.58798(15) 0.10449(16) 0.0159(4) Uani 1 1 d . . . C2A C 0.76220(19) 0.59868(16) 0.18286(16) 0.0195(5) Uani 1 1 d . . . H2A H 0.7306 0.6034 0.2422 0.023 Uiso 1 1 calc R . . C3A C 0.8719(2) 0.60242(18) 0.17449(19) 0.0255(5) Uani 1 1 d . . . H3A H 0.9151 0.6108 0.2280 0.031 Uiso 1 1 calc R . . C4A C 0.9193(2) 0.59399(19) 0.0884(2) 0.0275(5) Uani 1 1 d . . . H4A H 0.9946 0.5960 0.0828 0.033 Uiso 1 1 calc R . . C5A C 0.8558(2) 0.58269(19) 0.01047(19) 0.0275(5) Uani 1 1 d . . . H5A H 0.8880 0.5765 -0.0485 0.033 Uiso 1 1 calc R . . C6A C 0.74504(19) 0.58038(18) 0.01803(17) 0.0221(5) Uani 1 1 d . . . H6A H 0.7021 0.5736 -0.0358 0.026 Uiso 1 1 calc R . . C1B C 0.51865(17) 0.71583(15) 0.13099(15) 0.0152(4) Uani 1 1 d . . . C2B C 0.44182(18) 0.74389(16) 0.19518(16) 0.0178(4) Uani 1 1 d . . . H2B H 0.4126 0.6970 0.2361 0.021 Uiso 1 1 calc R . . C3B C 0.4077(2) 0.84052(18) 0.19959(18) 0.0234(5) Uani 1 1 d . . . H3B H 0.3554 0.8594 0.2433 0.028 Uiso 1 1 calc R . . C4B C 0.4507(2) 0.90861(17) 0.13986(19) 0.0247(5) Uani 1 1 d . . . H4B H 0.4277 0.9744 0.1426 0.030 Uiso 1 1 calc R . . C5B C 0.5273(2) 0.88124(17) 0.07589(18) 0.0227(5) Uani 1 1 d . . . H5B H 0.5561 0.9283 0.0350 0.027 Uiso 1 1 calc R . . C6B C 0.56187(19) 0.78522(17) 0.07159(16) 0.0197(5) Uani 1 1 d . . . H6B H 0.6148 0.7669 0.0283 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02221(11) 0.01653(10) 0.01343(10) 0.00003(6) 0.00279(7) -0.00315(6) P1 0.0141(3) 0.0132(2) 0.0116(2) -0.00077(19) 0.00030(19) -0.00026(19) N1 0.0156(9) 0.0176(9) 0.0148(9) -0.0002(7) -0.0001(7) 0.0024(7) O1 0.0363(10) 0.0206(8) 0.0234(9) 0.0030(7) -0.0037(7) -0.0090(7) O2 0.0213(9) 0.0329(10) 0.0201(8) -0.0011(7) -0.0015(7) -0.0011(7) F1 0.0375(9) 0.0233(7) 0.0371(9) -0.0102(7) 0.0102(7) -0.0003(6) F2 0.0288(8) 0.0328(8) 0.0329(8) -0.0034(7) -0.0112(6) -0.0094(7) F3 0.0436(10) 0.0290(8) 0.0348(9) 0.0081(7) 0.0039(7) -0.0159(7) C1 0.0163(10) 0.0155(10) 0.0164(10) 0.0023(8) -0.0004(8) 0.0005(8) C2 0.0185(11) 0.0166(10) 0.0147(10) -0.0008(8) -0.0023(8) 0.0006(8) C3 0.0161(10) 0.0166(10) 0.0143(10) 0.0007(8) -0.0002(8) 0.0046(8) C4 0.0151(11) 0.0176(11) 0.0219(12) -0.0001(8) 0.0006(9) -0.0003(8) C5 0.0164(11) 0.0185(10) 0.0198(11) -0.0033(9) -0.0010(9) 0.0001(9) C6 0.0179(11) 0.0181(10) 0.0176(11) 0.0024(8) 0.0021(8) 0.0010(8) C7 0.0149(10) 0.0189(10) 0.0171(10) 0.0017(8) 0.0002(8) 0.0016(8) C8 0.0192(11) 0.0138(10) 0.0150(10) -0.0001(8) 0.0007(8) 0.0033(8) C9 0.0164(11) 0.0194(11) 0.0194(11) -0.0002(9) -0.0010(8) 0.0016(8) C10 0.0218(12) 0.0226(11) 0.0174(11) -0.0032(9) -0.0044(9) 0.0047(9) C11 0.0273(13) 0.0243(12) 0.0169(11) -0.0017(9) 0.0053(9) 0.0043(10) C12 0.0194(11) 0.0246(12) 0.0253(12) -0.0016(10) 0.0064(9) -0.0013(9) C13 0.0194(11) 0.0212(11) 0.0196(11) -0.0018(9) -0.0010(9) -0.0002(9) C14 0.0130(10) 0.0220(11) 0.0169(10) -0.0047(9) 0.0043(8) -0.0016(8) C15 0.0236(12) 0.0200(11) 0.0209(11) 0.0015(9) 0.0029(9) -0.0027(9) C16 0.0150(10) 0.0138(10) 0.0131(10) -0.0004(8) -0.0004(8) -0.0003(8) C1A 0.0145(10) 0.0133(9) 0.0200(11) -0.0001(8) 0.0004(8) -0.0008(8) C2A 0.0215(12) 0.0166(10) 0.0204(11) -0.0020(9) -0.0016(9) 0.0019(9) C3A 0.0210(12) 0.0215(12) 0.0339(14) -0.0011(10) -0.0099(10) -0.0009(9) C4A 0.0152(11) 0.0232(12) 0.0441(16) -0.0011(11) 0.0019(10) 0.0003(9) C5A 0.0201(12) 0.0311(13) 0.0313(14) -0.0026(11) 0.0095(10) -0.0026(10) C6A 0.0193(11) 0.0260(12) 0.0209(12) -0.0012(9) 0.0010(9) -0.0024(9) C1B 0.0151(10) 0.0141(10) 0.0162(10) -0.0026(8) -0.0027(8) -0.0006(8) C2B 0.0184(11) 0.0180(10) 0.0171(10) -0.0013(8) 0.0000(8) 0.0013(8) C3B 0.0193(11) 0.0250(12) 0.0257(12) -0.0064(10) -0.0019(9) 0.0054(9) C4B 0.0252(12) 0.0152(10) 0.0335(14) -0.0031(10) -0.0079(10) 0.0028(9) C5B 0.0231(12) 0.0169(11) 0.0280(13) 0.0034(9) -0.0045(10) -0.0017(9) C6B 0.0187(11) 0.0200(11) 0.0205(11) -0.0001(9) -0.0016(9) 0.0002(9) _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 N1 2.2316(19) . ? Ag1 O1 2.3456(18) . ? Ag1 P1 2.3688(6) . ? P1 C1A 1.818(2) . ? P1 C1B 1.827(2) . ? P1 C16 1.831(2) . ? N1 C5 1.345(3) . ? N1 C1 1.345(3) . ? O1 C14 1.246(3) . ? O2 C14 1.230(3) . ? F1 C15 1.353(3) . ? F2 C15 1.335(3) . ? F3 C15 1.334(3) . ? C1 C2 1.382(3) . ? C2 C3 1.402(3) . ? C3 C4 1.399(3) . ? C3 C6 1.466(3) . ? C4 C5 1.381(3) . ? C6 C7 1.335(3) . ? C7 C8 1.473(3) . ? C8 C9 1.400(3) . ? C8 C13 1.400(3) . ? C9 C10 1.386(3) . ? C10 C11 1.387(4) . ? C11 C12 1.392(4) . ? C12 C13 1.388(3) . ? C14 C15 1.549(3) . ? C16 C16 1.532(4) 3_665 ? C1A C6A 1.393(3) . ? C1A C2A 1.400(3) . ? C2A C3A 1.384(3) . ? C3A C4A 1.389(4) . ? C4A C5A 1.387(4) . ? C5A C6A 1.395(3) . ? C1B C6B 1.395(3) . ? C1B C2B 1.396(3) . ? C2B C3B 1.396(3) . ? C3B C4B 1.385(4) . ? C4B C5B 1.390(4) . ? C5B C6B 1.390(3) . ? 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 N1 Ag1 O1 103.39(7) . . ? N1 Ag1 P1 134.75(5) . . ? O1 Ag1 P1 114.14(5) . . ? C1A P1 C1B 104.24(10) . . ? C1A P1 C16 106.29(10) . . ? C1B P1 C16 101.63(10) . . ? C1A P1 Ag1 119.60(8) . . ? C1B P1 Ag1 112.22(7) . . ? C16 P1 Ag1 111.14(7) . . ? C5 N1 C1 117.2(2) . . ? C5 N1 Ag1 122.23(15) . . ? C1 N1 Ag1 120.62(15) . . ? C14 O1 Ag1 116.86(15) . . ? N1 C1 C2 123.9(2) . . ? C1 C2 C3 118.9(2) . . ? C4 C3 C2 117.0(2) . . ? C4 C3 C6 119.5(2) . . ? C2 C3 C6 123.5(2) . . ? C5 C4 C3 120.2(2) . . ? N1 C5 C4 122.8(2) . . ? C7 C6 C3 125.7(2) . . ? C6 C7 C8 124.8(2) . . ? C9 C8 C13 118.3(2) . . ? C9 C8 C7 119.8(2) . . ? C13 C8 C7 121.9(2) . . ? C10 C9 C8 121.1(2) . . ? C9 C10 C11 120.2(2) . . ? C10 C11 C12 119.4(2) . . ? C13 C12 C11 120.6(2) . . ? C12 C13 C8 120.4(2) . . ? O2 C14 O1 130.6(2) . . ? O2 C14 C15 115.5(2) . . ? O1 C14 C15 113.8(2) . . ? F3 C15 F2 106.8(2) . . ? F3 C15 F1 106.7(2) . . ? F2 C15 F1 106.5(2) . . ? F3 C15 C14 113.8(2) . . ? F2 C15 C14 113.2(2) . . ? F1 C15 C14 109.34(19) . . ? C16 C16 P1 112.35(19) 3_665 . ? C6A C1A C2A 119.2(2) . . ? C6A C1A P1 123.54(18) . . ? C2A C1A P1 117.28(17) . . ? C3A C2A C1A 120.4(2) . . ? C2A C3A C4A 120.4(2) . . ? C5A C4A C3A 119.5(2) . . ? C4A C5A C6A 120.5(2) . . ? C1A C6A C5A 120.0(2) . . ? C6B C1B C2B 119.6(2) . . ? C6B C1B P1 121.39(17) . . ? C2B C1B P1 118.94(17) . . ? C3B C2B C1B 120.4(2) . . ? C4B C3B C2B 119.5(2) . . ? C3B C4B C5B 120.4(2) . . ? C4B C5B C6B 120.2(2) . . ? C5B C6B C1B 119.9(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.255 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.092 #===#END _database_code_depnum_ccdc_archive 'CCDC 934073'