# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Ag3 N9' _chemical_formula_weight 984.36 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' 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 Cc 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 15.055(3) _cell_length_b 19.328(4) _cell_length_c 12.632(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.687(2) _cell_angle_gamma 90.00 _cell_volume 3555.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1619 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.39 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8236 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 9592 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.75 _reflns_number_total 4730 _reflns_number_gt 3810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.25(6) _refine_ls_number_reflns 4730 _refine_ls_number_parameters 488 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 Ag1 Ag 0.34761(6) 0.23377(5) 0.77511(7) 0.0365(3) Uani 1 1 d . . . Ag2 Ag 0.14604(5) 0.23413(5) 0.70729(6) 0.0308(3) Uani 1 1 d . . . Ag3 Ag 0.24834(7) 0.10628(4) 0.72104(7) 0.0311(2) Uani 1 1 d . . . N1 N 0.2588(7) 0.3310(4) 0.7508(8) 0.029(2) Uani 1 1 d . . . N2 N 0.3452(8) 0.2944(6) 0.5854(10) 0.047(3) Uani 1 1 d . . . N3 N 0.1594(7) 0.2692(5) 0.8854(8) 0.032(2) Uani 1 1 d . . . N4 N 0.4156(7) 0.1252(5) 0.7765(8) 0.033(3) Uani 1 1 d . . . N5 N 0.4056(7) 0.1956(5) 0.9667(8) 0.031(2) Uani 1 1 d . . . N6 N 0.3068(6) 0.1049(5) 0.5644(7) 0.029(2) Uani 1 1 d . . . N7 N 0.0865(7) 0.1154(5) 0.6847(8) 0.026(2) Uani 1 1 d . . . N8 N 0.0926(7) 0.2128(5) 0.5244(8) 0.029(2) Uani 1 1 d . . . N9 N 0.2025(7) 0.0691(5) 0.8778(8) 0.034(2) Uani 1 1 d . . . C1 C 0.3913(11) 0.2240(7) 1.0580(12) 0.046(4) Uani 1 1 d . . . H1A H 0.3520 0.2618 1.0512 0.055 Uiso 1 1 calc R . . C2 C 0.4325(10) 0.1994(8) 1.1619(12) 0.049(4) Uani 1 1 d . . . H2A H 0.4184 0.2179 1.2236 0.059 Uiso 1 1 calc R . . C3 C 0.4960(9) 0.1456(7) 1.1703(10) 0.040(3) Uani 1 1 d . . . H3A H 0.5273 0.1294 1.2389 0.048 Uiso 1 1 calc R . . C4 C 0.5126(9) 0.1168(6) 1.0781(11) 0.035(3) Uani 1 1 d . . . H4A H 0.5547 0.0810 1.0828 0.042 Uiso 1 1 calc R . . C5 C 0.4647(9) 0.1427(6) 0.9775(9) 0.028(3) Uani 1 1 d . . . C6 C 0.4775(10) 0.1114(6) 0.8741(11) 0.031(3) Uani 1 1 d . . . C7 C 0.5475(9) 0.0691(6) 0.8609(11) 0.035(3) Uani 1 1 d . . . H7A H 0.5959 0.0516 0.9153 0.042 Uiso 1 1 calc R . . C8 C 0.5302(9) 0.0582(6) 0.7485(10) 0.038(3) Uani 1 1 d . . . H8A H 0.5671 0.0333 0.7132 0.045 Uiso 1 1 calc R . . C9 C 0.3971(8) 0.0906(6) 0.5848(9) 0.035(3) Uani 1 1 d . . . C10 C 0.4388(9) 0.0744(7) 0.5018(11) 0.046(3) Uani 1 1 d . . . H10A H 0.5006 0.0627 0.5177 0.056 Uiso 1 1 calc R . . C11 C 0.3853(10) 0.0762(7) 0.3934(12) 0.053(4) Uani 1 1 d . . . H11A H 0.4116 0.0648 0.3365 0.064 Uiso 1 1 calc R . . C12 C 0.2938(9) 0.0948(7) 0.3707(10) 0.044(3) Uani 1 1 d . . . H12A H 0.2580 0.0990 0.2993 0.052 Uiso 1 1 calc R . . C13 C 0.2585(9) 0.1069(6) 0.4600(10) 0.036(3) Uani 1 1 d . . . H13A H 0.1962 0.1171 0.4462 0.043 Uiso 1 1 calc R . . C18 C 0.4486(9) 0.0911(6) 0.6987(9) 0.030(3) Uani 1 1 d . . . C21 C 0.2581(8) 0.0630(6) 0.9810(10) 0.037(3) Uani 1 1 d . . . H21A H 0.3210 0.0694 0.9920 0.044 Uiso 1 1 calc R . . C22 C 0.2232(10) 0.0473(6) 1.0710(10) 0.044(3) Uani 1 1 d . . . H22A H 0.2622 0.0448 1.1410 0.053 Uiso 1 1 calc R . . C23 C 0.1304(9) 0.0355(6) 1.0543(9) 0.039(3) Uani 1 1 d . . . H23A H 0.1057 0.0237 1.1123 0.046 Uiso 1 1 calc R . . C24 C 0.0751(8) 0.0417(6) 0.9498(9) 0.034(3) Uani 1 1 d . . . H24A H 0.0124 0.0335 0.9369 0.041 Uiso 1 1 calc R . . C25 C 0.1117(8) 0.0602(6) 0.8628(9) 0.031(3) Uani 1 1 d . . . C26 C 0.0547(9) 0.0722(6) 0.7533(10) 0.028(3) Uani 1 1 d . . . C27 C -0.0295(8) 0.0431(6) 0.6993(10) 0.034(3) Uani 1 1 d . . . H27A H -0.0647 0.0117 0.7269 0.041 Uiso 1 1 calc R . . C28 C -0.0489(8) 0.0723(6) 0.5933(10) 0.029(3) Uani 1 1 d . . . H28A H -0.1016 0.0640 0.5378 0.035 Uiso 1 1 calc R . . C29 C 0.0224(8) 0.1151(6) 0.5847(10) 0.025(3) Uani 1 1 d . . . C30 C 0.0360(8) 0.1575(6) 0.4973(9) 0.028(3) Uani 1 1 d . . . C31 C -0.0008(9) 0.1408(7) 0.3866(10) 0.039(3) Uani 1 1 d . . . H31A H -0.0390 0.1025 0.3675 0.047 Uiso 1 1 calc R . . C32 C 0.0197(9) 0.1811(8) 0.3068(11) 0.046(4) Uani 1 1 d . . . H32A H -0.0046 0.1703 0.2334 0.055 Uiso 1 1 calc R . . C33 C 0.0747(10) 0.2360(7) 0.3345(11) 0.043(3) Uani 1 1 d . . . H33A H 0.0879 0.2639 0.2805 0.051 Uiso 1 1 calc R . . C34 C 0.1113(9) 0.2508(7) 0.4424(11) 0.038(3) Uani 1 1 d . . . H34A H 0.1507 0.2884 0.4604 0.046 Uiso 1 1 calc R . . C41 C 0.1279(11) 0.2345(7) 0.9599(12) 0.051(4) Uani 1 1 d . . . H41A H 0.1032 0.1908 0.9414 0.061 Uiso 1 1 calc R . . C42 C 0.1300(11) 0.2596(7) 1.0613(11) 0.054(4) Uani 1 1 d . . . H42A H 0.1079 0.2333 1.1108 0.064 Uiso 1 1 calc R . . C43 C 0.1654(10) 0.3246(7) 1.0889(11) 0.051(4) Uani 1 1 d . . . H43A H 0.1658 0.3438 1.1565 0.061 Uiso 1 1 calc R . . C44 C 0.2001(9) 0.3606(7) 1.0152(11) 0.044(3) Uani 1 1 d . . . H44A H 0.2258 0.4041 1.0341 0.052 Uiso 1 1 calc R . . C45 C 0.1977(8) 0.3335(6) 0.9125(9) 0.036(3) Uani 1 1 d . . . C46 C 0.2304(8) 0.3666(6) 0.8282(9) 0.028(3) Uani 1 1 d . . . C47 C 0.2307(8) 0.4384(6) 0.8104(9) 0.034(3) Uani 1 1 d . . . H47A H 0.2145 0.4734 0.8524 0.041 Uiso 1 1 calc R . . C48 C 0.2612(8) 0.4450(6) 0.7146(12) 0.038(3) Uani 1 1 d . . . H48A H 0.2688 0.4865 0.6806 0.046 Uiso 1 1 calc R . . C49 C 0.2780(8) 0.3796(6) 0.6791(10) 0.029(3) Uani 1 1 d . . . C50 C 0.3120(7) 0.3595(6) 0.5873(9) 0.028(3) Uani 1 1 d . . . C51 C 0.3082(8) 0.4049(6) 0.5006(9) 0.037(3) Uani 1 1 d . . . H51A H 0.2855 0.4494 0.5034 0.044 Uiso 1 1 calc R . . C52 C 0.3372(10) 0.3849(7) 0.4124(11) 0.056(4) Uani 1 1 d . . . H52A H 0.3338 0.4149 0.3540 0.068 Uiso 1 1 calc R . . C53 C 0.3723(11) 0.3184(9) 0.4107(12) 0.063(5) Uani 1 1 d . . . H53A H 0.3943 0.3037 0.3519 0.076 Uiso 1 1 calc R . . C54 C 0.3741(10) 0.2744(7) 0.4982(13) 0.053(4) Uani 1 1 d . . . H54A H 0.3960 0.2295 0.4961 0.063 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 0.0264(6) 0.0293(6) 0.0491(7) 0.0009(5) 0.0010(5) 0.0036(5) Ag2 0.0301(6) 0.0304(6) 0.0293(5) -0.0073(4) 0.0027(4) 0.0009(5) Ag3 0.0273(4) 0.0317(4) 0.0369(6) -0.0005(4) 0.0131(4) -0.0002(5) N1 0.017(6) 0.040(5) 0.024(5) -0.004(5) -0.008(5) -0.003(4) N2 0.035(7) 0.053(7) 0.057(8) -0.010(6) 0.019(6) -0.010(6) N3 0.021(6) 0.049(6) 0.022(5) -0.005(5) -0.005(4) -0.008(5) N4 0.026(6) 0.040(6) 0.038(6) 0.010(5) 0.018(5) -0.005(5) N5 0.021(5) 0.025(5) 0.044(6) -0.001(4) 0.005(5) 0.000(4) N6 0.032(6) 0.031(5) 0.029(6) 0.005(4) 0.014(5) 0.008(4) N7 0.032(6) 0.023(5) 0.027(5) -0.006(4) 0.011(5) -0.002(4) N8 0.036(6) 0.025(5) 0.029(5) 0.001(4) 0.014(5) 0.003(4) N9 0.044(7) 0.034(5) 0.026(6) 0.004(4) 0.010(5) -0.003(5) C1 0.044(9) 0.051(9) 0.041(9) -0.006(7) 0.007(7) 0.018(7) C2 0.043(9) 0.064(10) 0.046(9) -0.023(8) 0.022(7) -0.014(8) C3 0.033(8) 0.052(8) 0.031(7) -0.002(6) 0.002(6) -0.006(6) C4 0.022(7) 0.039(7) 0.042(8) -0.008(6) 0.006(6) -0.007(5) C5 0.023(7) 0.026(6) 0.030(7) 0.000(5) -0.003(5) -0.009(5) C6 0.041(9) 0.018(6) 0.037(7) -0.003(6) 0.016(6) -0.007(6) C7 0.024(8) 0.039(8) 0.042(8) -0.001(6) 0.009(6) 0.006(6) C8 0.032(8) 0.025(6) 0.055(9) 0.010(6) 0.010(6) 0.004(5) C9 0.033(7) 0.039(7) 0.031(7) 0.002(5) 0.007(6) 0.005(6) C10 0.037(8) 0.065(9) 0.044(8) -0.002(7) 0.022(7) 0.010(7) C11 0.071(11) 0.044(7) 0.058(10) 0.002(7) 0.042(9) 0.000(7) C12 0.048(8) 0.056(8) 0.021(7) 0.010(6) -0.003(6) 0.021(7) C13 0.029(7) 0.044(7) 0.035(8) -0.003(6) 0.008(6) 0.004(5) C18 0.021(6) 0.037(8) 0.031(7) -0.009(5) 0.003(5) 0.001(5) C21 0.023(6) 0.040(7) 0.043(8) 0.005(6) -0.003(6) -0.003(5) C22 0.070(10) 0.030(6) 0.029(7) -0.003(5) 0.006(7) -0.009(6) C23 0.052(8) 0.040(7) 0.024(7) 0.009(5) 0.010(6) -0.003(6) C24 0.024(6) 0.042(7) 0.035(7) 0.006(6) 0.005(5) 0.000(5) C25 0.029(7) 0.031(6) 0.035(7) -0.007(5) 0.013(6) -0.002(5) C26 0.031(7) 0.027(6) 0.032(7) -0.002(5) 0.020(6) -0.003(5) C27 0.021(6) 0.038(7) 0.044(8) 0.007(6) 0.013(6) -0.005(5) C28 0.013(6) 0.033(7) 0.041(7) -0.004(5) 0.007(6) 0.004(5) C29 0.026(7) 0.022(6) 0.027(7) -0.010(5) 0.005(6) 0.000(5) C30 0.024(7) 0.036(7) 0.027(7) 0.006(5) 0.009(6) 0.011(6) C31 0.030(8) 0.055(9) 0.032(7) -0.008(6) 0.008(6) 0.007(6) C32 0.035(9) 0.067(10) 0.029(7) -0.005(7) 0.000(6) 0.009(7) C33 0.041(8) 0.052(8) 0.034(8) 0.013(6) 0.007(7) 0.010(7) C34 0.015(6) 0.046(8) 0.048(9) 0.005(7) -0.003(6) 0.010(6) C41 0.073(11) 0.035(7) 0.053(10) -0.005(6) 0.034(9) 0.009(7) C42 0.070(11) 0.055(9) 0.043(9) -0.003(7) 0.027(8) -0.010(8) C43 0.067(11) 0.055(9) 0.040(8) -0.009(7) 0.032(8) -0.008(8) C44 0.039(8) 0.045(7) 0.046(8) -0.023(6) 0.009(7) -0.011(6) C45 0.022(7) 0.047(8) 0.030(7) -0.011(6) -0.009(5) -0.001(6) C46 0.028(7) 0.018(5) 0.035(7) -0.005(5) 0.001(6) -0.003(5) C47 0.029(7) 0.039(7) 0.035(7) -0.006(6) 0.008(6) -0.009(5) C48 0.014(7) 0.037(6) 0.058(9) -0.004(7) -0.002(6) -0.004(5) C49 0.023(7) 0.022(6) 0.044(8) 0.000(5) 0.012(6) 0.005(5) C50 0.014(6) 0.032(6) 0.032(7) -0.001(5) -0.003(5) -0.005(5) C51 0.032(7) 0.044(7) 0.030(7) -0.010(6) 0.002(6) -0.003(5) C52 0.068(11) 0.055(9) 0.055(10) 0.016(7) 0.032(9) 0.005(8) C53 0.060(11) 0.085(12) 0.056(10) -0.030(9) 0.036(9) -0.021(9) C54 0.043(9) 0.047(9) 0.070(11) 0.002(7) 0.019(8) -0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.281(9) . ? Ag1 N4 2.333(11) . ? Ag1 N5 2.468(10) . ? Ag1 Ag3 2.8732(13) . ? Ag1 Ag2 2.9370(12) . ? Ag2 N8 2.283(10) . ? Ag2 N3 2.310(9) . ? Ag2 N7 2.455(10) . ? Ag2 N1 2.494(9) . ? Ag2 Ag3 2.8937(13) . ? Ag3 N6 2.361(9) . ? Ag3 N9 2.368(9) . ? Ag3 N7 2.369(11) . ? Ag3 N4 2.464(11) . ? N1 C46 1.352(14) . ? N1 C49 1.385(14) . ? N2 C54 1.340(17) . ? N2 C50 1.357(16) . ? N3 C41 1.335(16) . ? N3 C45 1.376(15) . ? N4 C6 1.370(17) . ? N4 C18 1.377(15) . ? N5 C5 1.339(16) . ? N5 C1 1.343(16) . ? N6 C13 1.336(15) . ? N6 C9 1.346(15) . ? N7 C26 1.373(15) . ? N7 C29 1.382(15) . ? N8 C34 1.356(16) . ? N8 C30 1.356(15) . ? N9 C25 1.342(15) . ? N9 C21 1.364(14) . ? C1 C2 1.39(2) . ? C1 H1A 0.9300 . ? C2 C3 1.398(19) . ? C2 H2A 0.9300 . ? C3 C4 1.370(17) . ? C3 H3A 0.9300 . ? C4 C5 1.386(17) . ? C4 H4A 0.9300 . ? C5 C6 1.495(17) . ? C6 C7 1.377(18) . ? C7 C8 1.392(17) . ? C7 H7A 0.9300 . ? C8 C18 1.385(17) . ? C8 H8A 0.9300 . ? C9 C10 1.388(16) . ? C9 C18 1.451(16) . ? C10 C11 1.401(18) . ? C10 H10A 0.9300 . ? C11 C12 1.382(19) . ? C11 H11A 0.9300 . ? C12 C13 1.383(16) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C21 C22 1.400(17) . ? C21 H21A 0.9300 . ? C22 C23 1.378(18) . ? C22 H22A 0.9300 . ? C23 C24 1.376(15) . ? C23 H23A 0.9300 . ? C24 C25 1.394(15) . ? C24 H24A 0.9300 . ? C25 C26 1.450(17) . ? C26 C27 1.397(17) . ? C27 C28 1.415(16) . ? C27 H27A 0.9300 . ? C28 C29 1.381(17) . ? C28 H28A 0.9300 . ? C29 C30 1.430(16) . ? C30 C31 1.405(17) . ? C31 C32 1.370(18) . ? C31 H31A 0.9300 . ? C32 C33 1.335(19) . ? C32 H32A 0.9300 . ? C33 C34 1.365(18) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C41 C42 1.363(19) . ? C41 H41A 0.9300 . ? C42 C43 1.375(18) . ? C42 H42A 0.9300 . ? C43 C44 1.368(17) . ? C43 H43A 0.9300 . ? C44 C45 1.391(16) . ? C44 H44A 0.9300 . ? C45 C46 1.432(16) . ? C46 C47 1.406(15) . ? C47 C48 1.405(17) . ? C47 H47A 0.9300 . ? C48 C49 1.385(15) . ? C48 H48A 0.9300 . ? C49 C50 1.435(15) . ? C50 C51 1.393(15) . ? C51 C52 1.353(17) . ? C51 H51A 0.9300 . ? C52 C53 1.39(2) . ? C52 H52A 0.9300 . ? C53 C54 1.39(2) . ? C53 H53A 0.9300 . ? C54 H54A 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 N1 Ag1 N4 169.4(4) . . ? N1 Ag1 N5 115.3(3) . . ? N4 Ag1 N5 71.2(3) . . ? N1 Ag1 Ag3 115.0(2) . . ? N4 Ag1 Ag3 55.3(3) . . ? N5 Ag1 Ag3 90.6(2) . . ? N1 Ag1 Ag2 55.4(2) . . ? N4 Ag1 Ag2 115.0(3) . . ? N5 Ag1 Ag2 111.7(2) . . ? Ag3 Ag1 Ag2 59.73(3) . . ? N8 Ag2 N3 163.8(4) . . ? N8 Ag2 N7 71.9(3) . . ? N3 Ag2 N7 109.1(3) . . ? N8 Ag2 N1 113.8(3) . . ? N3 Ag2 N1 71.3(3) . . ? N7 Ag2 N1 159.4(3) . . ? N8 Ag2 Ag3 87.3(2) . . ? N3 Ag2 Ag3 106.2(3) . . ? N7 Ag2 Ag3 51.8(2) . . ? N1 Ag2 Ag3 107.8(2) . . ? N8 Ag2 Ag1 111.6(3) . . ? N3 Ag2 Ag1 83.6(3) . . ? N7 Ag2 Ag1 110.6(3) . . ? N1 Ag2 Ag1 48.8(2) . . ? Ag3 Ag2 Ag1 59.04(3) . . ? N6 Ag3 N9 161.3(3) . . ? N6 Ag3 N7 115.0(3) . . ? N9 Ag3 N7 71.4(3) . . ? N6 Ag3 N4 70.6(3) . . ? N9 Ag3 N4 107.5(3) . . ? N7 Ag3 N4 166.2(3) . . ? N6 Ag3 Ag1 85.8(2) . . ? N9 Ag3 Ag1 107.8(2) . . ? N7 Ag3 Ag1 115.5(2) . . ? N4 Ag3 Ag1 51.2(2) . . ? N6 Ag3 Ag2 105.4(2) . . ? N9 Ag3 Ag2 92.6(2) . . ? N7 Ag3 Ag2 54.5(2) . . ? N4 Ag3 Ag2 112.4(2) . . ? Ag1 Ag3 Ag2 61.23(3) . . ? C46 N1 C49 106.5(9) . . ? C46 N1 Ag1 127.2(7) . . ? C49 N1 Ag1 115.8(8) . . ? C46 N1 Ag2 102.6(7) . . ? C49 N1 Ag2 127.5(7) . . ? Ag1 N1 Ag2 75.8(2) . . ? C54 N2 C50 118.7(12) . . ? C41 N3 C45 118.6(11) . . ? C41 N3 Ag2 125.5(9) . . ? C45 N3 Ag2 115.8(8) . . ? C6 N4 C18 105.3(11) . . ? C6 N4 Ag1 112.3(8) . . ? C18 N4 Ag1 131.5(8) . . ? C6 N4 Ag3 129.8(8) . . ? C18 N4 Ag3 104.7(8) . . ? Ag1 N4 Ag3 73.5(3) . . ? C5 N5 C1 118.1(11) . . ? C5 N5 Ag1 112.9(7) . . ? C1 N5 Ag1 128.7(8) . . ? C13 N6 C9 117.8(9) . . ? C13 N6 Ag3 127.0(8) . . ? C9 N6 Ag3 114.5(7) . . ? C26 N7 C29 107.5(11) . . ? C26 N7 Ag3 109.8(8) . . ? C29 N7 Ag3 128.5(7) . . ? C26 N7 Ag2 132.1(8) . . ? C29 N7 Ag2 105.0(7) . . ? Ag3 N7 Ag2 73.7(3) . . ? C34 N8 C30 118.3(10) . . ? C34 N8 Ag2 126.0(9) . . ? C30 N8 Ag2 115.8(7) . . ? C25 N9 C21 118.6(10) . . ? C25 N9 Ag3 115.0(8) . . ? C21 N9 Ag3 126.0(8) . . ? N5 C1 C2 122.8(12) . . ? N5 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C1 C2 C3 117.4(12) . . ? C1 C2 H2A 121.3 . . ? C3 C2 H2A 121.3 . . ? C4 C3 C2 120.5(12) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 117.9(12) . . ? C3 C4 H4A 121.1 . . ? C5 C4 H4A 121.1 . . ? N5 C5 C4 123.2(11) . . ? N5 C5 C6 116.7(11) . . ? C4 C5 C6 120.1(12) . . ? N4 C6 C7 111.9(11) . . ? N4 C6 C5 119.9(12) . . ? C7 C6 C5 128.2(13) . . ? C6 C7 C8 105.2(12) . . ? C6 C7 H7A 127.4 . . ? C8 C7 H7A 127.4 . . ? C18 C8 C7 108.0(12) . . ? C18 C8 H8A 126.0 . . ? C7 C8 H8A 126.0 . . ? N6 C9 C10 122.0(11) . . ? N6 C9 C18 116.7(10) . . ? C10 C9 C18 121.3(12) . . ? C9 C10 C11 118.4(12) . . ? C9 C10 H10A 120.8 . . ? C11 C10 H10A 120.8 . . ? C12 C11 C10 120.3(12) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 116.4(12) . . ? C11 C12 H12A 121.8 . . ? C13 C12 H12A 121.8 . . ? N6 C13 C12 125.1(11) . . ? N6 C13 H13A 117.5 . . ? C12 C13 H13A 117.5 . . ? N4 C18 C8 109.5(11) . . ? N4 C18 C9 120.8(11) . . ? C8 C18 C9 129.7(12) . . ? N9 C21 C22 122.0(11) . . ? N9 C21 H21A 119.0 . . ? C22 C21 H21A 119.0 . . ? C23 C22 C21 119.0(12) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C24 C23 C22 118.4(11) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? C23 C24 C25 121.0(12) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? N9 C25 C24 120.9(11) . . ? N9 C25 C26 116.7(10) . . ? C24 C25 C26 122.4(11) . . ? N7 C26 C27 110.8(11) . . ? N7 C26 C25 118.9(12) . . ? C27 C26 C25 130.2(11) . . ? C26 C27 C28 104.2(10) . . ? C26 C27 H27A 127.9 . . ? C28 C27 H27A 127.9 . . ? C29 C28 C27 109.6(11) . . ? C29 C28 H28A 125.2 . . ? C27 C28 H28A 125.2 . . ? C28 C29 N7 107.9(11) . . ? C28 C29 C30 132.0(12) . . ? N7 C29 C30 120.1(11) . . ? N8 C30 C31 119.7(10) . . ? N8 C30 C29 117.4(10) . . ? C31 C30 C29 122.7(12) . . ? C32 C31 C30 119.7(13) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C33 C32 C31 120.0(13) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 119.6(13) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? N8 C34 C33 122.7(13) . . ? N8 C34 H34A 118.7 . . ? C33 C34 H34A 118.7 . . ? N3 C41 C42 123.8(13) . . ? N3 C41 H41A 118.1 . . ? C42 C41 H41A 118.1 . . ? C41 C42 C43 118.5(13) . . ? C41 C42 H42A 120.7 . . ? C43 C42 H42A 120.7 . . ? C44 C43 C42 118.9(12) . . ? C44 C43 H43A 120.5 . . ? C42 C43 H43A 120.5 . . ? C43 C44 C45 121.2(12) . . ? C43 C44 H44A 119.4 . . ? C45 C44 H44A 119.4 . . ? N3 C45 C44 118.9(11) . . ? N3 C45 C46 114.8(10) . . ? C44 C45 C46 126.3(12) . . ? N1 C46 C47 111.8(10) . . ? N1 C46 C45 122.9(10) . . ? C47 C46 C45 125.2(10) . . ? C48 C47 C46 104.1(11) . . ? C48 C47 H47A 127.9 . . ? C46 C47 H47A 127.9 . . ? C49 C48 C47 108.7(12) . . ? C49 C48 H48A 125.6 . . ? C47 C48 H48A 125.6 . . ? N1 C49 C48 108.8(10) . . ? N1 C49 C50 121.4(10) . . ? C48 C49 C50 129.8(11) . . ? N2 C50 C51 120.8(11) . . ? N2 C50 C49 118.3(10) . . ? C51 C50 C49 120.9(10) . . ? C52 C51 C50 120.7(12) . . ? C52 C51 H51A 119.6 . . ? C50 C51 H51A 119.6 . . ? C51 C52 C53 118.7(12) . . ? C51 C52 H52A 120.7 . . ? C53 C52 H52A 120.7 . . ? C54 C53 C52 118.9(13) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? N2 C54 C53 122.2(14) . . ? N2 C54 H54A 118.9 . . ? C53 C54 H54A 118.9 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.609 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.144 _database_code_depnum_ccdc_archive 'CCDC 963075' ####################################################################### # # 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_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H50 Ag3 F3 N6 O3 P2 S' _chemical_formula_weight 1437.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 19.8842(3) _cell_length_b 17.3938(3) _cell_length_c 17.4070(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.2390(10) _cell_angle_gamma 90.00 _cell_volume 5717.94(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9784 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6283 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 29949 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.55 _reflns_number_total 6557 _reflns_number_gt 5933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0582P)^2^+3.1937P] 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 6557 _refine_ls_number_parameters 412 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.406663(7) 0.421702(8) 0.092810(8) 0.02002(6) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.0000 0.02251(7) Uani 1 2 d S . . P1 P 0.30375(2) 0.47864(3) 0.00573(3) 0.01745(10) Uani 1 1 d . . . N1 N 0.44636(8) 0.29296(9) 0.11388(9) 0.0208(3) Uani 1 1 d . . . N2 N 0.52213(8) 0.42838(9) 0.15584(9) 0.0188(3) Uani 1 1 d . . . N3 N 0.52739(9) 0.58440(9) 0.09311(10) 0.0224(3) Uani 1 1 d . . . C1 C 0.41057(11) 0.22707(12) 0.08904(11) 0.0275(4) Uani 1 1 d . . . H1 H 0.3638 0.2305 0.0558 0.033 Uiso 1 1 calc R . . C2 C 0.43901(13) 0.15488(12) 0.10986(12) 0.0315(5) Uani 1 1 d . . . H2 H 0.4121 0.1108 0.0920 0.038 Uiso 1 1 calc R . . C3 C 0.50920(13) 0.15016(13) 0.15847(13) 0.0313(5) Uani 1 1 d . . . H3 H 0.5305 0.1025 0.1732 0.038 Uiso 1 1 calc R . . C4 C 0.54682(11) 0.21654(12) 0.18458(12) 0.0266(4) Uani 1 1 d . . . H4 H 0.5938 0.2139 0.2172 0.032 Uiso 1 1 calc R . . C5 C 0.51448(10) 0.28815(11) 0.16203(10) 0.0208(4) Uani 1 1 d . . . C6 C 0.55134(10) 0.36035(12) 0.18848(10) 0.0203(4) Uani 1 1 d . . . C7 C 0.61690(10) 0.37332(13) 0.24771(11) 0.0248(4) Uani 1 1 d . . . H7 H 0.6474 0.3362 0.2782 0.030 Uiso 1 1 calc R . . C8 C 0.62724(10) 0.45297(13) 0.25182(11) 0.0257(4) Uani 1 1 d . . . H8 H 0.6657 0.4794 0.2860 0.031 Uiso 1 1 calc R . . C9 C 0.56803(10) 0.48493(12) 0.19405(10) 0.0211(4) Uani 1 1 d . . . C10 C 0.55664(10) 0.56573(12) 0.17180(12) 0.0227(4) Uani 1 1 d . . . C11 C 0.57627(12) 0.62359(14) 0.23061(14) 0.0342(5) Uani 1 1 d . . . H11 H 0.5958 0.6107 0.2849 0.041 Uiso 1 1 calc R . . C12 C 0.56655(13) 0.69991(15) 0.20767(17) 0.0423(6) Uani 1 1 d . . . H12 H 0.5798 0.7386 0.2464 0.051 Uiso 1 1 calc R . . C13 C 0.53703(12) 0.71836(14) 0.12705(17) 0.0392(6) Uani 1 1 d . . . H13 H 0.5301 0.7693 0.1104 0.047 Uiso 1 1 calc R . . C15 C 0.51812(11) 0.65921(12) 0.07200(14) 0.0302(4) Uani 1 1 d . . . H15 H 0.4980 0.6714 0.0176 0.036 Uiso 1 1 calc R . . C21 C 0.27494(10) 0.43811(12) -0.09607(11) 0.0203(4) Uani 1 1 d . . . C22 C 0.22770(11) 0.47562(13) -0.16162(12) 0.0281(4) Uani 1 1 d . . . H22 H 0.2119 0.5248 -0.1553 0.034 Uiso 1 1 calc R . . C23 C 0.20421(12) 0.43964(15) -0.23635(13) 0.0332(5) Uani 1 1 d . . . H23 H 0.1731 0.4651 -0.2801 0.040 Uiso 1 1 calc R . . C24 C 0.22644(11) 0.36686(14) -0.24632(13) 0.0324(5) Uani 1 1 d . . . H24 H 0.2107 0.3434 -0.2968 0.039 Uiso 1 1 calc R . . C25 C 0.27226(11) 0.32820(14) -0.18138(14) 0.0326(5) Uani 1 1 d . . . H25 H 0.2863 0.2783 -0.1878 0.039 Uiso 1 1 calc R . . C26 C 0.29707(10) 0.36416(12) -0.10677(12) 0.0257(4) Uani 1 1 d . . . H26 H 0.3288 0.3386 -0.0635 0.031 Uiso 1 1 calc R . . C31 C 0.22363(9) 0.47126(11) 0.03527(10) 0.0195(4) Uani 1 1 d . . . C32 C 0.16866(10) 0.52494(12) 0.01030(12) 0.0248(4) Uani 1 1 d . . . H32 H 0.1731 0.5670 -0.0208 0.030 Uiso 1 1 calc R . . C33 C 0.10763(11) 0.51567(14) 0.03183(12) 0.0294(5) Uani 1 1 d . . . H33 H 0.0715 0.5518 0.0156 0.035 Uiso 1 1 calc R . . C34 C 0.10030(11) 0.45281(15) 0.07736(12) 0.0306(5) Uani 1 1 d . . . H34 H 0.0593 0.4467 0.0916 0.037 Uiso 1 1 calc R . . C35 C 0.15405(11) 0.39913(15) 0.10168(12) 0.0310(5) Uani 1 1 d . . . H35 H 0.1489 0.3567 0.1319 0.037 Uiso 1 1 calc R . . C36 C 0.21569(11) 0.40837(12) 0.08113(11) 0.0241(4) Uani 1 1 d . . . H36 H 0.2519 0.3723 0.0981 0.029 Uiso 1 1 calc R . . C41 C 0.31508(10) 0.58181(11) -0.00387(12) 0.0203(4) Uani 1 1 d . . . C42 C 0.33430(11) 0.61426(12) -0.06688(12) 0.0254(4) Uani 1 1 d . . . H42 H 0.3374 0.5838 -0.1095 0.030 Uiso 1 1 calc R . . C43 C 0.34888(12) 0.69246(13) -0.06588(14) 0.0315(5) Uani 1 1 d . . . H43 H 0.3607 0.7142 -0.1088 0.038 Uiso 1 1 calc R . . C44 C 0.34615(12) 0.73817(13) -0.00265(15) 0.0346(5) Uani 1 1 d . . . H44 H 0.3566 0.7903 -0.0025 0.041 Uiso 1 1 calc R . . C45 C 0.32767(12) 0.70629(13) 0.06106(14) 0.0340(5) Uani 1 1 d . . . H45 H 0.3261 0.7369 0.1043 0.041 Uiso 1 1 calc R . . C46 C 0.31160(11) 0.62918(12) 0.06000(12) 0.0263(4) Uani 1 1 d . . . H46 H 0.2983 0.6082 0.1022 0.032 Uiso 1 1 calc R . . C100 C 0.0422(8) 0.5885(5) 0.7863(8) 0.047(5) Uani 0.50 1 d PD . . F1 F 0.0938(5) 0.5796(5) 0.7534(6) 0.076(3) Uani 0.50 1 d PD . . F2 F 0.0500(4) 0.5327(3) 0.8422(3) 0.0612(14) Uani 0.50 1 d PD . . F3 F 0.0544(3) 0.6545(3) 0.8277(3) 0.0445(13) Uani 0.50 1 d PD . . S1 S -0.04358(11) 0.58365(12) 0.71030(13) 0.0156(6) Uani 0.50 1 d PD . . O1 O -0.0914(5) 0.6059(5) 0.7524(7) 0.0398(16) Uani 0.50 1 d PD . . O2 O -0.0494(4) 0.5071(3) 0.6851(3) 0.0604(17) Uani 0.50 1 d PD . . O3 O -0.0399(4) 0.6384(4) 0.6521(4) 0.0430(15) Uani 0.50 1 d PD . . 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 0.01209(9) 0.01971(9) 0.02453(9) -0.00019(5) 0.00033(6) 0.00119(5) Ag2 0.02063(11) 0.02564(12) 0.01936(10) -0.00344(7) 0.00354(8) -0.00219(8) P1 0.0124(2) 0.0179(2) 0.0202(2) -0.00005(17) 0.00246(16) 0.00091(18) N1 0.0205(8) 0.0192(8) 0.0199(7) -0.0023(6) 0.0023(6) 0.0007(6) N2 0.0138(8) 0.0237(9) 0.0171(7) -0.0029(6) 0.0025(6) -0.0016(6) N3 0.0172(8) 0.0222(8) 0.0278(8) -0.0038(6) 0.0070(6) -0.0020(6) C1 0.0308(11) 0.0220(10) 0.0243(9) -0.0041(7) 0.0010(8) -0.0009(8) C2 0.0446(13) 0.0209(10) 0.0269(10) -0.0044(8) 0.0080(9) -0.0007(9) C3 0.0427(13) 0.0236(10) 0.0312(10) 0.0047(8) 0.0165(9) 0.0120(10) C4 0.0235(10) 0.0308(11) 0.0268(9) 0.0054(8) 0.0099(8) 0.0085(9) C5 0.0204(9) 0.0255(10) 0.0178(8) 0.0015(7) 0.0078(7) 0.0048(8) C6 0.0142(8) 0.0295(10) 0.0168(8) 0.0012(7) 0.0044(6) 0.0018(8) C7 0.0146(9) 0.0397(12) 0.0183(8) 0.0028(8) 0.0027(7) 0.0021(8) C8 0.0138(9) 0.0433(13) 0.0185(8) -0.0029(8) 0.0027(7) -0.0058(9) C9 0.0141(8) 0.0315(11) 0.0170(8) -0.0058(7) 0.0037(6) -0.0052(8) C10 0.0145(9) 0.0276(10) 0.0265(9) -0.0095(8) 0.0072(7) -0.0058(8) C11 0.0255(11) 0.0411(13) 0.0359(11) -0.0188(10) 0.0095(9) -0.0108(10) C12 0.0307(12) 0.0351(13) 0.0646(16) -0.0288(12) 0.0198(11) -0.0103(10) C13 0.0266(11) 0.0246(11) 0.0697(17) -0.0095(11) 0.0197(11) -0.0014(9) C15 0.0207(10) 0.0234(10) 0.0467(12) 0.0001(9) 0.0108(9) 0.0014(8) C21 0.0142(9) 0.0232(9) 0.0226(8) -0.0015(7) 0.0046(7) -0.0020(7) C22 0.0238(10) 0.0288(11) 0.0277(10) -0.0005(8) 0.0025(8) 0.0026(9) C23 0.0266(11) 0.0427(13) 0.0251(10) 0.0003(9) 0.0004(8) -0.0038(10) C24 0.0259(11) 0.0430(13) 0.0283(10) -0.0123(9) 0.0086(8) -0.0144(10) C25 0.0261(11) 0.0306(12) 0.0413(12) -0.0119(9) 0.0108(9) -0.0036(9) C26 0.0199(9) 0.0251(10) 0.0300(10) -0.0030(8) 0.0049(7) 0.0015(8) C31 0.0146(8) 0.0241(10) 0.0180(8) -0.0037(7) 0.0023(6) -0.0015(7) C32 0.0186(9) 0.0277(11) 0.0265(9) -0.0004(8) 0.0048(7) 0.0020(8) C33 0.0177(9) 0.0413(13) 0.0279(10) -0.0057(9) 0.0051(8) 0.0059(9) C34 0.0184(9) 0.0523(14) 0.0218(9) -0.0072(9) 0.0071(7) -0.0067(10) C35 0.0258(11) 0.0431(13) 0.0230(9) 0.0017(9) 0.0061(8) -0.0107(10) C36 0.0211(10) 0.0277(10) 0.0203(9) -0.0003(7) 0.0018(7) -0.0004(8) C41 0.0142(9) 0.0191(9) 0.0259(9) -0.0002(7) 0.0039(7) 0.0009(7) C42 0.0233(10) 0.0234(10) 0.0328(10) 0.0004(8) 0.0138(8) 0.0035(8) C43 0.0292(11) 0.0245(11) 0.0477(12) 0.0073(9) 0.0221(10) 0.0037(9) C44 0.0285(11) 0.0191(10) 0.0588(14) -0.0006(10) 0.0177(10) 0.0008(9) C45 0.0353(12) 0.0247(11) 0.0417(12) -0.0104(9) 0.0117(9) -0.0006(9) C46 0.0271(10) 0.0248(10) 0.0271(9) -0.0023(8) 0.0084(8) -0.0004(8) C100 0.071(8) 0.029(7) 0.045(8) 0.014(5) 0.023(6) 0.023(5) F1 0.037(3) 0.153(8) 0.044(3) -0.003(5) 0.019(2) 0.036(5) F2 0.075(3) 0.048(3) 0.039(3) 0.022(2) -0.013(2) -0.006(3) F3 0.041(3) 0.032(2) 0.050(3) -0.0105(19) -0.0023(18) -0.0076(17) S1 0.0156(8) 0.0147(11) 0.0166(10) 0.0022(7) 0.0052(6) 0.0012(7) O1 0.024(3) 0.058(3) 0.043(3) -0.010(2) 0.018(2) 0.002(3) O2 0.083(4) 0.032(3) 0.044(3) -0.017(2) -0.012(3) -0.005(3) O3 0.036(3) 0.049(4) 0.036(3) 0.027(3) 0.0005(19) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.2163(15) . ? Ag1 P1 2.3503(5) . ? Ag1 N1 2.3645(16) . ? Ag1 Ag2 3.12827(14) . ? Ag2 N3 2.1275(16) . ? Ag2 N3 2.1275(16) 5_665 ? Ag2 Ag1 3.12827(14) 5_665 ? P1 C41 1.8227(19) . ? P1 C21 1.8248(19) . ? P1 C31 1.8254(19) . ? N1 C1 1.347(3) . ? N1 C5 1.354(2) . ? N2 C6 1.362(2) . ? N2 C9 1.365(2) . ? N3 C15 1.349(3) . ? N3 C10 1.350(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9300 . ? C2 C3 1.390(3) . ? C2 H2 0.9300 . ? C3 C4 1.373(3) . ? C3 H3 0.9300 . ? C4 C5 1.400(3) . ? C4 H4 0.9300 . ? C5 C6 1.454(3) . ? C6 C7 1.404(2) . ? C7 C8 1.399(3) . ? C7 H7 0.9300 . ? C8 C9 1.402(3) . ? C8 H8 0.9300 . ? C9 C10 1.457(3) . ? C10 C11 1.401(3) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.379(4) . ? C12 H12 0.9300 . ? C13 C15 1.376(3) . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C21 C26 1.391(3) . ? C21 C22 1.393(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 C24 1.370(3) . ? C23 H23 0.9300 . ? C24 C25 1.384(3) . ? C24 H24 0.9300 . ? C25 C26 1.386(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.392(3) . ? C31 C32 1.399(3) . ? C32 C33 1.387(3) . ? C32 H32 0.9300 . ? C33 C34 1.384(3) . ? C33 H33 0.9300 . ? C34 C35 1.382(3) . ? C34 H34 0.9300 . ? C35 C36 1.389(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.389(3) . ? C41 C46 1.403(3) . ? C42 C43 1.390(3) . ? C42 H42 0.9300 . ? C43 C44 1.372(3) . ? C43 H43 0.9300 . ? C44 C45 1.388(3) . ? C44 H44 0.9300 . ? C45 C46 1.378(3) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C100 S1 0.102(14) 2_556 ? C100 F1 1.330(11) . ? C100 F3 1.336(11) . ? C100 F2 1.349(11) . ? C100 O1 1.384(16) 2_556 ? C100 O3 1.392(13) 2_556 ? C100 O2 1.493(12) 2_556 ? C100 C100 1.76(3) 2_556 ? C100 S1 1.804(13) . ? F1 O1 0.468(14) 2_556 ? F1 S1 1.340(9) 2_556 ? F2 O2 0.649(6) 2_556 ? F2 S1 1.250(6) 2_556 ? F3 O3 0.590(7) 2_556 ? F3 S1 1.383(6) 2_556 ? S1 C100 0.102(14) 2_556 ? S1 F2 1.250(6) 2_556 ? S1 F1 1.340(9) 2_556 ? S1 F3 1.383(6) 2_556 ? S1 O2 1.395(6) . ? S1 O3 1.409(6) . ? S1 O1 1.425(8) . ? S1 S1 1.848(5) 2_556 ? O1 F1 0.468(14) 2_556 ? O1 C100 1.384(16) 2_556 ? O2 F2 0.649(6) 2_556 ? O2 C100 1.493(12) 2_556 ? O3 F3 0.590(6) 2_556 ? O3 C100 1.392(13) 2_556 ? 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 N2 Ag1 P1 148.77(4) . . ? N2 Ag1 N1 74.28(6) . . ? P1 Ag1 N1 132.85(4) . . ? N2 Ag1 Ag2 62.79(4) . . ? P1 Ag1 Ag2 91.203(12) . . ? N1 Ag1 Ag2 105.62(4) . . ? N3 Ag2 N3 180.00(6) . 5_665 ? N3 Ag2 Ag1 92.36(5) . 5_665 ? N3 Ag2 Ag1 87.64(4) 5_665 5_665 ? N3 Ag2 Ag1 87.64(5) . . ? N3 Ag2 Ag1 92.36(4) 5_665 . ? Ag1 Ag2 Ag1 180.000(3) 5_665 . ? C41 P1 C21 107.55(9) . . ? C41 P1 C31 103.81(9) . . ? C21 P1 C31 102.12(8) . . ? C41 P1 Ag1 111.49(6) . . ? C21 P1 Ag1 114.13(7) . . ? C31 P1 Ag1 116.69(6) . . ? C1 N1 C5 118.15(17) . . ? C1 N1 Ag1 129.71(13) . . ? C5 N1 Ag1 112.04(12) . . ? C6 N2 C9 106.87(16) . . ? C6 N2 Ag1 113.68(12) . . ? C9 N2 Ag1 135.24(13) . . ? C15 N3 C10 119.17(18) . . ? C15 N3 Ag2 118.52(14) . . ? C10 N3 Ag2 122.24(13) . . ? N1 C1 C2 123.97(19) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 117.7(2) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 119.4(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.01(19) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 120.73(18) . . ? N1 C5 C6 116.74(17) . . ? C4 C5 C6 122.52(17) . . ? N2 C6 C7 110.09(18) . . ? N2 C6 C5 120.76(16) . . ? C7 C6 C5 129.14(18) . . ? C8 C7 C6 106.53(18) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 106.20(17) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 110.31(18) . . ? N2 C9 C10 122.77(16) . . ? C8 C9 C10 126.80(18) . . ? N3 C10 C11 120.1(2) . . ? N3 C10 C9 118.94(16) . . ? C11 C10 C9 120.95(19) . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C15 C13 C12 118.1(2) . . ? C15 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N3 C15 C13 123.2(2) . . ? N3 C15 H15 118.4 . . ? C13 C15 H15 118.4 . . ? C26 C21 C22 118.96(18) . . ? C26 C21 P1 118.10(15) . . ? C22 C21 P1 122.75(16) . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.6(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.5(2) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C36 C31 C32 119.00(18) . . ? C36 C31 P1 118.84(15) . . ? C32 C31 P1 122.10(15) . . ? C33 C32 C31 120.20(19) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.94(19) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.4(2) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C41 C46 118.75(18) . . ? C42 C41 P1 123.01(15) . . ? C46 C41 P1 117.87(15) . . ? C41 C42 C43 119.70(19) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 121.1(2) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.7(2) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 119.8(2) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 120.91(19) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? S1 C100 F1 93(8) 2_556 . ? S1 C100 F3 115(8) 2_556 . ? F1 C100 F3 107.4(10) . . ? S1 C100 F2 15(7) 2_556 . ? F1 C100 F2 107.3(10) . . ? F3 C100 F2 105.6(9) . . ? S1 C100 O1 112(8) 2_556 2_556 ? F1 C100 O1 19.7(6) . 2_556 ? F3 C100 O1 92.2(8) . 2_556 ? F2 C100 O1 124.8(12) . 2_556 ? S1 C100 O3 98(7) 2_556 2_556 ? F1 C100 O3 128.3(11) . 2_556 ? F3 C100 O3 24.9(3) . 2_556 ? F2 C100 O3 85.2(8) . 2_556 ? O1 C100 O3 115.9(10) 2_556 2_556 ? S1 C100 O2 16(8) 2_556 2_556 ? F1 C100 O2 91.6(8) . 2_556 ? F3 C100 O2 130.7(10) . 2_556 ? F2 C100 O2 25.8(3) . 2_556 ? O1 C100 O2 111.3(9) 2_556 2_556 ? O3 C100 O2 110.9(9) 2_556 2_556 ? S1 C100 C100 116(9) 2_556 2_556 ? F1 C100 C100 112.5(12) . 2_556 ? F3 C100 C100 111.0(8) . 2_556 ? F2 C100 C100 112.7(9) . 2_556 ? O1 C100 C100 108.2(11) 2_556 2_556 ? O3 C100 C100 107.4(9) 2_556 2_556 ? O2 C100 C100 102.1(7) 2_556 2_556 ? S1 C100 S1 114(9) 2_556 . ? F1 C100 S1 111.0(9) . . ? F3 C100 S1 113.9(9) . . ? F2 C100 S1 111.3(8) . . ? O1 C100 S1 107.7(8) 2_556 . ? O3 C100 S1 110.0(9) 2_556 . ? O2 C100 S1 99.7(7) 2_556 . ? C100 C100 S1 2.9(4) 2_556 . ? O1 F1 C100 87(2) 2_556 . ? O1 F1 S1 91(2) 2_556 2_556 ? C100 F1 S1 4.4(6) . 2_556 ? O2 F2 S1 88.6(9) 2_556 2_556 ? O2 F2 C100 89.6(10) 2_556 . ? S1 F2 C100 1.2(6) 2_556 . ? O3 F3 C100 82.8(12) 2_556 . ? O3 F3 S1 80.3(11) 2_556 2_556 ? C100 F3 S1 3.8(6) . 2_556 ? C100 S1 F2 164(7) 2_556 2_556 ? C100 S1 F1 82(8) 2_556 2_556 ? F2 S1 F1 112.8(5) 2_556 2_556 ? C100 S1 F3 61(8) 2_556 2_556 ? F2 S1 F3 108.5(3) 2_556 2_556 ? F1 S1 F3 104.2(5) 2_556 2_556 ? C100 S1 O2 163(9) 2_556 . ? F2 S1 O2 27.7(3) 2_556 . ? F1 S1 O2 95.6(5) 2_556 . ? F3 S1 O2 135.6(4) 2_556 . ? C100 S1 O3 78(7) 2_556 . ? F2 S1 O3 88.3(4) 2_556 . ? F1 S1 O3 126.0(5) 2_556 . ? F3 S1 O3 24.4(3) 2_556 . ? O2 S1 O3 115.9(4) . . ? C100 S1 O1 64(8) 2_556 . ? F2 S1 O1 129.6(5) 2_556 . ? F1 S1 O1 19.2(6) 2_556 . ? F3 S1 O1 88.6(5) 2_556 . ? O2 S1 O1 114.7(5) . . ? O3 S1 O1 112.3(5) . . ? C100 S1 C100 61(9) 2_556 . ? F2 S1 C100 115.2(5) 2_556 . ? F1 S1 C100 109.3(5) 2_556 . ? F3 S1 C100 106.2(5) 2_556 . ? O2 S1 C100 103.9(4) . . ? O3 S1 C100 104.2(5) . . ? O1 S1 C100 103.9(5) . . ? C100 S1 S1 63(9) 2_556 2_556 ? F2 S1 S1 113.8(3) 2_556 2_556 ? F1 S1 S1 108.0(4) 2_556 2_556 ? F3 S1 S1 109.1(3) 2_556 2_556 ? O2 S1 S1 101.6(3) . 2_556 ? O3 S1 S1 106.9(3) . 2_556 ? O1 S1 S1 103.7(5) . 2_556 ? C100 S1 S1 2.9(4) . 2_556 ? F1 O1 C100 73.6(18) 2_556 2_556 ? F1 O1 S1 70.1(18) 2_556 . ? C100 O1 S1 3.8(6) 2_556 . ? F2 O2 S1 63.6(8) 2_556 . ? F2 O2 C100 64.6(9) 2_556 2_556 ? S1 O2 C100 1.2(7) . 2_556 ? F3 O3 C100 72.3(11) 2_556 2_556 ? F3 O3 S1 75.3(11) 2_556 . ? C100 O3 S1 4.1(6) 2_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 Ag2 N3 -62.47(6) . . . . ? P1 Ag1 Ag2 N3 99.51(5) . . . . ? N1 Ag1 Ag2 N3 -125.08(6) . . . . ? N2 Ag1 Ag2 N3 117.53(6) . . . 5_665 ? P1 Ag1 Ag2 N3 -80.49(5) . . . 5_665 ? N1 Ag1 Ag2 N3 54.92(6) . . . 5_665 ? N2 Ag1 Ag2 Ag1 -174(100) . . . 5_665 ? P1 Ag1 Ag2 Ag1 -12(100) . . . 5_665 ? N1 Ag1 Ag2 Ag1 123(100) . . . 5_665 ? N2 Ag1 P1 C41 -18.28(11) . . . . ? N1 Ag1 P1 C41 -163.08(8) . . . . ? Ag2 Ag1 P1 C41 -50.32(7) . . . . ? N2 Ag1 P1 C21 103.83(10) . . . . ? N1 Ag1 P1 C21 -40.97(9) . . . . ? Ag2 Ag1 P1 C21 71.79(7) . . . . ? N2 Ag1 P1 C31 -137.30(10) . . . . ? N1 Ag1 P1 C31 77.90(9) . . . . ? Ag2 Ag1 P1 C31 -169.35(7) . . . . ? N2 Ag1 N1 C1 -175.24(17) . . . . ? P1 Ag1 N1 C1 -13.33(19) . . . . ? Ag2 Ag1 N1 C1 -120.13(16) . . . . ? N2 Ag1 N1 C5 8.64(12) . . . . ? P1 Ag1 N1 C5 170.56(9) . . . . ? Ag2 Ag1 N1 C5 63.76(12) . . . . ? P1 Ag1 N2 C6 -167.49(9) . . . . ? N1 Ag1 N2 C6 -13.53(11) . . . . ? Ag2 Ag1 N2 C6 -130.87(13) . . . . ? P1 Ag1 N2 C9 39.4(2) . . . . ? N1 Ag1 N2 C9 -166.68(18) . . . . ? Ag2 Ag1 N2 C9 75.98(17) . . . . ? N3 Ag2 N3 C15 -72(100) 5_665 . . . ? Ag1 Ag2 N3 C15 53.05(14) 5_665 . . . ? Ag1 Ag2 N3 C15 -126.95(14) . . . . ? N3 Ag2 N3 C10 112(100) 5_665 . . . ? Ag1 Ag2 N3 C10 -123.78(15) 5_665 . . . ? Ag1 Ag2 N3 C10 56.22(15) . . . . ? C5 N1 C1 C2 0.2(3) . . . . ? Ag1 N1 C1 C2 -175.70(16) . . . . ? N1 C1 C2 C3 -1.0(3) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C1 N1 C5 C4 0.6(3) . . . . ? Ag1 N1 C5 C4 177.21(13) . . . . ? C1 N1 C5 C6 -179.34(16) . . . . ? Ag1 N1 C5 C6 -2.73(19) . . . . ? C3 C4 C5 N1 -0.6(3) . . . . ? C3 C4 C5 C6 179.31(18) . . . . ? C9 N2 C6 C7 -0.5(2) . . . . ? Ag1 N2 C6 C7 -161.10(12) . . . . ? C9 N2 C6 C5 178.53(16) . . . . ? Ag1 N2 C6 C5 17.9(2) . . . . ? N1 C5 C6 N2 -10.1(2) . . . . ? C4 C5 C6 N2 169.99(17) . . . . ? N1 C5 C6 C7 168.77(18) . . . . ? C4 C5 C6 C7 -11.2(3) . . . . ? N2 C6 C7 C8 0.9(2) . . . . ? C5 C6 C7 C8 -178.07(18) . . . . ? C6 C7 C8 C9 -0.9(2) . . . . ? C6 N2 C9 C8 0.0(2) . . . . ? Ag1 N2 C9 C8 154.34(14) . . . . ? C6 N2 C9 C10 176.27(16) . . . . ? Ag1 N2 C9 C10 -29.3(3) . . . . ? C7 C8 C9 N2 0.6(2) . . . . ? C7 C8 C9 C10 -175.55(18) . . . . ? C15 N3 C10 C11 0.7(3) . . . . ? Ag2 N3 C10 C11 177.53(14) . . . . ? C15 N3 C10 C9 -178.60(17) . . . . ? Ag2 N3 C10 C9 -1.8(2) . . . . ? N2 C9 C10 N3 -36.3(3) . . . . ? C8 C9 C10 N3 139.4(2) . . . . ? N2 C9 C10 C11 144.39(19) . . . . ? C8 C9 C10 C11 -39.9(3) . . . . ? N3 C10 C11 C12 -1.0(3) . . . . ? C9 C10 C11 C12 178.4(2) . . . . ? C10 C11 C12 C13 0.5(3) . . . . ? C11 C12 C13 C15 0.1(3) . . . . ? C10 N3 C15 C13 -0.1(3) . . . . ? Ag2 N3 C15 C13 -177.01(17) . . . . ? C12 C13 C15 N3 -0.3(3) . . . . ? C41 P1 C21 C26 146.69(15) . . . . ? C31 P1 C21 C26 -104.40(16) . . . . ? Ag1 P1 C21 C26 22.44(17) . . . . ? C41 P1 C21 C22 -38.39(19) . . . . ? C31 P1 C21 C22 70.52(19) . . . . ? Ag1 P1 C21 C22 -162.64(15) . . . . ? C26 C21 C22 C23 -0.9(3) . . . . ? P1 C21 C22 C23 -175.75(17) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C25 0.6(3) . . . . ? C23 C24 C25 C26 -1.7(3) . . . . ? C24 C25 C26 C21 1.6(3) . . . . ? C22 C21 C26 C25 -0.3(3) . . . . ? P1 C21 C26 C25 174.82(16) . . . . ? C41 P1 C31 C36 -151.92(15) . . . . ? C21 P1 C31 C36 96.34(16) . . . . ? Ag1 P1 C31 C36 -28.83(17) . . . . ? C41 P1 C31 C32 30.97(17) . . . . ? C21 P1 C31 C32 -80.78(17) . . . . ? Ag1 P1 C31 C32 154.05(14) . . . . ? C36 C31 C32 C33 0.6(3) . . . . ? P1 C31 C32 C33 177.75(15) . . . . ? C31 C32 C33 C34 -0.8(3) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? C33 C34 C35 C36 0.5(3) . . . . ? C34 C35 C36 C31 -0.6(3) . . . . ? C32 C31 C36 C35 0.0(3) . . . . ? P1 C31 C36 C35 -177.16(15) . . . . ? C21 P1 C41 C42 -29.82(19) . . . . ? C31 P1 C41 C42 -137.55(17) . . . . ? Ag1 P1 C41 C42 96.01(17) . . . . ? C21 P1 C41 C46 157.23(15) . . . . ? C31 P1 C41 C46 49.50(17) . . . . ? Ag1 P1 C41 C46 -76.93(16) . . . . ? C46 C41 C42 C43 -0.6(3) . . . . ? P1 C41 C42 C43 -173.53(16) . . . . ? C41 C42 C43 C44 1.4(3) . . . . ? C42 C43 C44 C45 -0.8(3) . . . . ? C43 C44 C45 C46 -0.6(3) . . . . ? C44 C45 C46 C41 1.4(3) . . . . ? C42 C41 C46 C45 -0.7(3) . . . . ? P1 C41 C46 C45 172.51(17) . . . . ? S1 C100 F1 O1 -159(9) 2_556 . . 2_556 ? F3 C100 F1 O1 -41(3) . . . 2_556 ? F2 C100 F1 O1 -154(3) . . . 2_556 ? O3 C100 F1 O1 -57(3) 2_556 . . 2_556 ? O2 C100 F1 O1 -175(3) 2_556 . . 2_556 ? C100 C100 F1 O1 81(3) 2_556 . . 2_556 ? S1 C100 F1 O1 84(3) . . . 2_556 ? F3 C100 F1 S1 118(9) . . . 2_556 ? F2 C100 F1 S1 5(8) . . . 2_556 ? O1 C100 F1 S1 159(9) 2_556 . . 2_556 ? O3 C100 F1 S1 102(9) 2_556 . . 2_556 ? O2 C100 F1 S1 -16(8) 2_556 . . 2_556 ? C100 C100 F1 S1 -120(9) 2_556 . . 2_556 ? S1 C100 F1 S1 -117(9) . . . 2_556 ? S1 C100 F2 O2 -36(37) 2_556 . . 2_556 ? F1 C100 F2 O2 -54.7(16) . . . 2_556 ? F3 C100 F2 O2 -168.9(14) . . . 2_556 ? O1 C100 F2 O2 -64.9(17) 2_556 . . 2_556 ? O3 C100 F2 O2 176.6(14) 2_556 . . 2_556 ? C100 C100 F2 O2 69.8(15) 2_556 . . 2_556 ? S1 C100 F2 O2 67.0(14) . . . 2_556 ? F1 C100 F2 S1 -19(36) . . . 2_556 ? F3 C100 F2 S1 -133(38) . . . 2_556 ? O1 C100 F2 S1 -29(36) 2_556 . . 2_556 ? O3 C100 F2 S1 -148(38) 2_556 . . 2_556 ? O2 C100 F2 S1 36(37) 2_556 . . 2_556 ? C100 C100 F2 S1 105(37) 2_556 . . 2_556 ? S1 C100 F2 S1 103(37) . . . 2_556 ? S1 C100 F3 O3 -48(10) 2_556 . . 2_556 ? F1 C100 F3 O3 -150.4(16) . . . 2_556 ? F2 C100 F3 O3 -36.2(17) . . . 2_556 ? O1 C100 F3 O3 -163.3(16) 2_556 . . 2_556 ? O2 C100 F3 O3 -42(2) 2_556 . . 2_556 ? C100 C100 F3 O3 86.3(16) 2_556 . . 2_556 ? S1 C100 F3 O3 86.3(14) . . . 2_556 ? F1 C100 F3 S1 -103(10) . . . 2_556 ? F2 C100 F3 S1 12(9) . . . 2_556 ? O1 C100 F3 S1 -115(10) 2_556 . . 2_556 ? O3 C100 F3 S1 48(10) 2_556 . . 2_556 ? O2 C100 F3 S1 5(8) 2_556 . . 2_556 ? C100 C100 F3 S1 134(10) 2_556 . . 2_556 ? S1 C100 F3 S1 134(10) . . . 2_556 ? S1 C100 S1 C100 135(16) 2_556 . . 2_556 ? F1 C100 S1 C100 -121(8) . . . 2_556 ? F3 C100 S1 C100 0(8) . . . 2_556 ? F2 C100 S1 C100 119(9) . . . 2_556 ? O1 C100 S1 C100 -101(8) 2_556 . . 2_556 ? O3 C100 S1 C100 27(8) 2_556 . . 2_556 ? O2 C100 S1 C100 143(9) 2_556 . . 2_556 ? S1 C100 S1 F2 -62(8) 2_556 . . 2_556 ? F1 C100 S1 F2 41.5(9) . . . 2_556 ? F3 C100 S1 F2 162.7(7) . . . 2_556 ? F2 C100 S1 F2 -78.1(8) . . . 2_556 ? O1 C100 S1 F2 62.1(8) 2_556 . . 2_556 ? O3 C100 S1 F2 -170.7(6) 2_556 . . 2_556 ? O2 C100 S1 F2 -54.1(7) 2_556 . . 2_556 ? C100 C100 S1 F2 163(8) 2_556 . . 2_556 ? S1 C100 S1 F1 66(8) 2_556 . . 2_556 ? F1 C100 S1 F1 169.6(9) . . . 2_556 ? F3 C100 S1 F1 -69.1(8) . . . 2_556 ? F2 C100 S1 F1 50.1(9) . . . 2_556 ? O1 C100 S1 F1 -169.8(6) 2_556 . . 2_556 ? O3 C100 S1 F1 -42.6(9) 2_556 . . 2_556 ? O2 C100 S1 F1 74.1(7) 2_556 . . 2_556 ? C100 C100 S1 F1 -69(8) 2_556 . . 2_556 ? S1 C100 S1 F3 177(8) 2_556 . . 2_556 ? F1 C100 S1 F3 -78.6(8) . . . 2_556 ? F3 C100 S1 F3 42.7(7) . . . 2_556 ? F2 C100 S1 F3 161.9(7) . . . 2_556 ? O1 C100 S1 F3 -58.0(8) 2_556 . . 2_556 ? O3 C100 S1 F3 69.2(7) 2_556 . . 2_556 ? O2 C100 S1 F3 -174.2(6) 2_556 . . 2_556 ? C100 C100 S1 F3 43(8) 2_556 . . 2_556 ? S1 C100 S1 O2 -35(8) 2_556 . . . ? F1 C100 S1 O2 68.4(8) . . . . ? F3 C100 S1 O2 -170.3(7) . . . . ? F2 C100 S1 O2 -51.1(7) . . . . ? O1 C100 S1 O2 89.0(8) 2_556 . . . ? O3 C100 S1 O2 -143.8(7) 2_556 . . . ? O2 C100 S1 O2 -27.1(8) 2_556 . . . ? C100 C100 S1 O2 -170(8) 2_556 . . . ? S1 C100 S1 O3 -157(8) 2_556 . . . ? F1 C100 S1 O3 -53.4(8) . . . . ? F3 C100 S1 O3 67.9(7) . . . . ? F2 C100 S1 O3 -172.9(7) . . . . ? O1 C100 S1 O3 -32.8(8) 2_556 . . . ? O3 C100 S1 O3 94.4(7) 2_556 . . . ? O2 C100 S1 O3 -149.0(6) 2_556 . . . ? C100 C100 S1 O3 68(8) 2_556 . . . ? S1 C100 S1 O1 85(8) 2_556 . . . ? F1 C100 S1 O1 -171.2(6) . . . . ? F3 C100 S1 O1 -49.9(8) . . . . ? F2 C100 S1 O1 69.3(8) . . . . ? O1 C100 S1 O1 -150.6(9) 2_556 . . . ? O3 C100 S1 O1 -23.4(9) 2_556 . . . ? O2 C100 S1 O1 93.3(7) 2_556 . . . ? C100 C100 S1 O1 -50(8) 2_556 . . . ? F1 C100 S1 S1 104(8) . . . 2_556 ? F3 C100 S1 S1 -135(8) . . . 2_556 ? F2 C100 S1 S1 -16(7) . . . 2_556 ? O1 C100 S1 S1 125(8) 2_556 . . 2_556 ? O3 C100 S1 S1 -108(8) 2_556 . . 2_556 ? O2 C100 S1 S1 8(7) 2_556 . . 2_556 ? C100 C100 S1 S1 -135(16) 2_556 . . 2_556 ? C100 S1 O1 F1 -157(10) 2_556 . . 2_556 ? F2 S1 O1 F1 32(3) 2_556 . . 2_556 ? F3 S1 O1 F1 145(3) 2_556 . . 2_556 ? O2 S1 O1 F1 4(3) . . . 2_556 ? O3 S1 O1 F1 139(2) . . . 2_556 ? C100 S1 O1 F1 -109(3) . . . 2_556 ? S1 S1 O1 F1 -106(3) 2_556 . . 2_556 ? F2 S1 O1 C100 -171(9) 2_556 . . 2_556 ? F1 S1 O1 C100 157(10) 2_556 . . 2_556 ? F3 S1 O1 C100 -58(9) 2_556 . . 2_556 ? O2 S1 O1 C100 161(9) . . . 2_556 ? O3 S1 O1 C100 -64(9) . . . 2_556 ? C100 S1 O1 C100 48(9) . . . 2_556 ? S1 S1 O1 C100 51(9) 2_556 . . 2_556 ? C100 S1 O2 F2 -148(28) 2_556 . . 2_556 ? F1 S1 O2 F2 130.5(13) 2_556 . . 2_556 ? F3 S1 O2 F2 13.5(16) 2_556 . . 2_556 ? O3 S1 O2 F2 -4.4(15) . . . 2_556 ? O1 S1 O2 F2 129.1(12) . . . 2_556 ? C100 S1 O2 F2 -118.1(12) . . . 2_556 ? S1 S1 O2 F2 -119.8(12) 2_556 . . 2_556 ? F2 S1 O2 C100 148(27) 2_556 . . 2_556 ? F1 S1 O2 C100 -82(27) 2_556 . . 2_556 ? F3 S1 O2 C100 161(28) 2_556 . . 2_556 ? O3 S1 O2 C100 143(28) . . . 2_556 ? O1 S1 O2 C100 -83(27) . . . 2_556 ? C100 S1 O2 C100 30(28) . . . 2_556 ? S1 S1 O2 C100 28(27) 2_556 . . 2_556 ? C100 S1 O3 F3 -42(9) 2_556 . . 2_556 ? F2 S1 O3 F3 146.6(14) 2_556 . . 2_556 ? F1 S1 O3 F3 29.4(16) 2_556 . . 2_556 ? O2 S1 O3 F3 148.6(13) . . . 2_556 ? O1 S1 O3 F3 14.0(16) . . . 2_556 ? C100 S1 O3 F3 -97.8(14) . . . 2_556 ? S1 S1 O3 F3 -99.0(13) 2_556 . . 2_556 ? F2 S1 O3 C100 -172(9) 2_556 . . 2_556 ? F1 S1 O3 C100 71(9) 2_556 . . 2_556 ? F3 S1 O3 C100 42(9) 2_556 . . 2_556 ? O2 S1 O3 C100 -170(9) . . . 2_556 ? O1 S1 O3 C100 56(9) . . . 2_556 ? C100 S1 O3 C100 -56(9) . . . 2_556 ? S1 S1 O3 C100 -57(9) 2_556 . . 2_556 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.684 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.190 _database_code_depnum_ccdc_archive 'CCDC 963076' ####################################################################### # # 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_complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H76 Ag4 F6 Li4 N6 O20 P4 S2' _chemical_formula_weight 1890.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 12.4463(2) _cell_length_b 12.9013(2) _cell_length_c 14.0856(2) _cell_angle_alpha 66.1580(10) _cell_angle_beta 69.5560(10) _cell_angle_gamma 74.9330(10) _cell_volume 1919.76(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6599 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22224 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_unetI/netI 0.0180 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7469 _reflns_number_gt 6290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0711P)^2^+1.5184P] 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 7469 _refine_ls_number_parameters 520 _refine_ls_number_restraints 291 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.010 _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 S1 S 1.23515(10) 0.87452(11) 0.13333(10) 0.0692(3) Uani 1 1 d U . . O7 O 1.2812(4) 0.7641(4) 0.1922(5) 0.138(2) Uani 1 1 d U . . O8 O 1.2777(3) 0.9053(4) 0.0195(3) 0.0937(11) Uani 1 1 d U . . O9 O 1.1155(3) 0.9094(4) 0.1717(3) 0.0951(12) Uani 1 1 d U . . C40 C 1.3050(8) 0.9610(10) 0.1612(9) 0.139(3) Uani 1 1 d U . . F1 F 1.4176(4) 0.9323(5) 0.1349(5) 0.163(2) Uani 1 1 d U . . F2 F 1.2708(6) 0.9453(7) 0.2649(5) 0.202(3) Uani 1 1 d U . . F3 F 1.2768(7) 1.0701(5) 0.1067(7) 0.225(3) Uani 1 1 d U . . O1S O 0.6159(15) 1.159(5) 0.187(3) 0.085(3) Uani 0.474(11) 1 d PDU A 3 C1S C 0.6037(12) 1.1577(17) 0.2946(14) 0.100(3) Uani 0.474(11) 1 d PDU A 3 H1S1 H 0.6586 1.2002 0.2929 0.120 Uiso 0.474(11) 1 calc PR A 3 H1S2 H 0.6130 1.0801 0.3450 0.120 Uiso 0.474(11) 1 calc PR A 3 C2S C 0.4820(11) 1.2156(15) 0.3220(14) 0.111(3) Uani 0.474(11) 1 d PDU A 3 H2S1 H 0.4696 1.2922 0.2710 0.133 Uiso 0.474(11) 1 calc PR A 3 H2S2 H 0.4544 1.2159 0.3953 0.133 Uiso 0.474(11) 1 calc PR A 3 C3S C 0.4324(12) 1.1234(16) 0.3063(14) 0.122(4) Uani 0.474(11) 1 d PDU A 3 H3S1 H 0.4389 1.0491 0.3623 0.146 Uiso 0.474(11) 1 calc PR A 3 H3S2 H 0.3524 1.1478 0.3041 0.146 Uiso 0.474(11) 1 calc PR A 3 C4S C 0.5123(13) 1.1229(16) 0.1988(13) 0.099(3) Uani 0.474(11) 1 d PDU A 3 H4S1 H 0.5284 1.0466 0.1954 0.119 Uiso 0.474(11) 1 calc PR A 3 H4S2 H 0.4775 1.1745 0.1415 0.119 Uiso 0.474(11) 1 calc PR A 3 O1S' O 0.6199(13) 1.151(4) 0.183(2) 0.083(3) Uani 0.526(11) 1 d PDU A 4 C1S' C 0.6071(11) 1.1925(16) 0.2659(12) 0.102(3) Uani 0.526(11) 1 d PDU A 4 H1S3 H 0.5959 1.2755 0.2405 0.123 Uiso 0.526(11) 1 calc PR A 4 H1S4 H 0.6735 1.1635 0.2949 0.123 Uiso 0.526(11) 1 calc PR A 4 C2S' C 0.4985(11) 1.1442(15) 0.3493(10) 0.122(3) Uani 0.526(11) 1 d PDU A 4 H2S3 H 0.4673 1.1775 0.4057 0.146 Uiso 0.526(11) 1 calc PR A 4 H2S4 H 0.5102 1.0614 0.3807 0.146 Uiso 0.526(11) 1 calc PR A 4 C3S' C 0.4222(9) 1.1906(16) 0.2648(11) 0.115(3) Uani 0.526(11) 1 d PDU A 4 H3S3 H 0.3583 1.1474 0.2905 0.139 Uiso 0.526(11) 1 calc PR A 4 H3S4 H 0.3924 1.2711 0.2505 0.139 Uiso 0.526(11) 1 calc PR A 4 C4S' C 0.5077(11) 1.1710(15) 0.1691(11) 0.098(3) Uani 0.526(11) 1 d PDU A 4 H4S3 H 0.4939 1.1053 0.1602 0.117 Uiso 0.526(11) 1 calc PR A 4 H4S4 H 0.5015 1.2373 0.1050 0.117 Uiso 0.526(11) 1 calc PR A 4 C21 C 1.2184(7) 0.6066(7) -0.0140(8) 0.089(2) Uani 0.653(11) 1 d PDU A 1 H21A H 1.2662 0.6025 -0.0839 0.107 Uiso 0.653(11) 1 calc PR A 1 H21B H 1.1555 0.5624 0.0106 0.107 Uiso 0.653(11) 1 calc PR A 1 C22 C 1.2892(13) 0.5576(14) 0.0647(11) 0.137(4) Uani 0.653(11) 1 d PDU A 1 H22A H 1.3518 0.6011 0.0398 0.205 Uiso 0.653(11) 1 calc PR A 1 H22B H 1.3198 0.4794 0.0710 0.205 Uiso 0.653(11) 1 calc PR A 1 H22C H 1.2414 0.5608 0.1340 0.205 Uiso 0.653(11) 1 calc PR A 1 C21' C 1.2142(14) 0.6244(15) 0.0594(13) 0.099(4) Uani 0.347(11) 1 d PDU A 2 H21C H 1.1566 0.5725 0.0981 0.118 Uiso 0.347(11) 1 calc PR A 2 H21D H 1.2249 0.6506 0.1107 0.118 Uiso 0.347(11) 1 calc PR A 2 C22' C 1.3274(19) 0.562(3) 0.011(2) 0.125(7) Uani 0.347(11) 1 d PDU A 2 H22D H 1.3160 0.5324 -0.0370 0.188 Uiso 0.347(11) 1 calc PR A 2 H22E H 1.3540 0.4993 0.0677 0.188 Uiso 0.347(11) 1 calc PR A 2 H22F H 1.3841 0.6133 -0.0284 0.188 Uiso 0.347(11) 1 calc PR A 2 C23 C 1.0062(7) 0.6994(6) -0.1437(5) 0.112(2) Uani 1 1 d DU A . H23A H 0.9926 0.6318 -0.0793 0.134 Uiso 1 1 calc R . . H23B H 1.0779 0.6807 -0.1940 0.134 Uiso 1 1 calc R . . C24 C 0.9112(7) 0.7307(9) -0.1925(8) 0.159(3) Uani 1 1 d DU . . H24A H 0.8446 0.7672 -0.1517 0.238 Uiso 1 1 calc R . . H24B H 0.8924 0.6631 -0.1925 0.238 Uiso 1 1 calc R . . H24C H 0.9341 0.7823 -0.2655 0.238 Uiso 1 1 calc R . . Ag1 Ag 0.91841(3) 0.64269(2) 0.14249(2) 0.05225(11) Uani 1 1 d . . . Ag2 Ag 0.91978(3) 0.69174(2) 0.32453(2) 0.05752(12) Uani 1 1 d . . . P1 P 1.03654(8) 0.76757(7) -0.00163(7) 0.0454(2) Uani 1 1 d U . . P2 P 0.80281(8) 0.86877(8) 0.30558(7) 0.0469(2) Uani 1 1 d . . . Li1 Li 0.7677(6) 1.1005(6) 0.0968(6) 0.0608(16) Uani 1 1 d . . . Li2 Li 0.9894(5) 0.9596(5) 0.1045(5) 0.0469(13) Uani 1 1 d . . . N1 N 0.8705(3) 0.5042(2) 0.3013(2) 0.0512(7) Uani 1 1 d . . . N2 N 0.7306(3) 0.6129(3) 0.1633(3) 0.0618(8) Uani 1 1 d . . . N3 N 1.0535(3) 0.5464(3) 0.3581(2) 0.0547(8) Uani 1 1 d . . . O1 O 1.0319(3) 0.8862(2) -0.0031(2) 0.0579(7) Uani 1 1 d . . . O2 O 1.1728(3) 0.7222(3) -0.0241(3) 0.0818(9) Uani 1 1 d DU . . O3 O 1.0178(4) 0.7896(3) -0.1155(2) 0.0833(10) Uani 1 1 d DU . . O4 O 0.8319(2) 0.9602(2) 0.1958(2) 0.0515(6) Uani 1 1 d . A . O5 O 0.7936(3) 0.9192(2) 0.3958(2) 0.0674(8) Uani 1 1 d . . . O6 O 0.6674(2) 0.8585(3) 0.3461(3) 0.0675(8) Uani 1 1 d . . . C1 C 0.6594(4) 0.6740(5) 0.1013(4) 0.0792(13) Uani 1 1 d . . . H1A H 0.6853 0.7356 0.0400 0.095 Uiso 1 1 calc R . . C2 C 0.5494(5) 0.6501(6) 0.1236(5) 0.0949(17) Uani 1 1 d . . . H2A H 0.5026 0.6947 0.0783 0.114 Uiso 1 1 calc R . . C3 C 0.5116(5) 0.5621(7) 0.2112(5) 0.1015(19) Uani 1 1 d . . . H3A H 0.4379 0.5443 0.2277 0.122 Uiso 1 1 calc R . . C4 C 0.5828(5) 0.4969(5) 0.2777(5) 0.0878(16) Uani 1 1 d . . . H4A H 0.5572 0.4351 0.3390 0.105 Uiso 1 1 calc R . . C5 C 0.6943(4) 0.5248(4) 0.2517(4) 0.0611(10) Uani 1 1 d . . . C6 C 0.7721(4) 0.4627(3) 0.3185(3) 0.0596(10) Uani 1 1 d . . . C7 C 0.7683(5) 0.3568(4) 0.4007(4) 0.0781(14) Uani 1 1 d . . . H7A H 0.7097 0.3114 0.4284 0.094 Uiso 1 1 calc R . . C8 C 0.8649(5) 0.3315(4) 0.4331(4) 0.0780(14) Uani 1 1 d . . . H8B H 0.8858 0.2651 0.4862 0.094 Uiso 1 1 calc R . . C9 C 0.9278(4) 0.4239(3) 0.3718(3) 0.0569(10) Uani 1 1 d . . . C10 C 1.0343(4) 0.4394(3) 0.3808(3) 0.0578(10) Uani 1 1 d . . . C11 C 1.1172(5) 0.3464(4) 0.4158(3) 0.0761(15) Uani 1 1 d . . . H11A H 1.1052 0.2728 0.4299 0.091 Uiso 1 1 calc R . . C12 C 1.2121(5) 0.3609(5) 0.4294(4) 0.0866(17) Uani 1 1 d . . . H12A H 1.2652 0.2980 0.4534 0.104 Uiso 1 1 calc R . . C13 C 1.2310(4) 0.4700(6) 0.4076(4) 0.0885(17) Uani 1 1 d . . . H13A H 1.2963 0.4823 0.4171 0.106 Uiso 1 1 calc R . . C14 C 1.1492(4) 0.5610(5) 0.3708(3) 0.0726(12) Uani 1 1 d . . . H14A H 1.1618 0.6350 0.3545 0.087 Uiso 1 1 calc R . . C25 C 0.8822(5) 0.9760(5) 0.3842(5) 0.0882(16) Uani 1 1 d . . . H25A H 0.8942 1.0391 0.3158 0.106 Uiso 1 1 calc R . . H25B H 0.9539 0.9236 0.3846 0.106 Uiso 1 1 calc R . . C26 C 0.8502(8) 1.0198(7) 0.4735(6) 0.126(3) Uani 1 1 d . . . H26A H 0.9111 1.0579 0.4657 0.189 Uiso 1 1 calc R . . H26B H 0.8385 0.9572 0.5411 0.189 Uiso 1 1 calc R . . H26C H 0.7800 1.0728 0.4721 0.189 Uiso 1 1 calc R . . C27 C 0.6251(5) 0.8019(6) 0.3034(5) 0.0914(16) Uani 1 1 d . . . H27A H 0.6835 0.7402 0.2875 0.110 Uiso 1 1 calc R . . H27B H 0.6087 0.8548 0.2364 0.110 Uiso 1 1 calc R . . C28 C 0.5196(6) 0.7553(7) 0.3796(7) 0.130(3) Uani 1 1 d . . . H28A H 0.4919 0.7168 0.3488 0.195 Uiso 1 1 calc R . . H28B H 0.4614 0.8165 0.3945 0.195 Uiso 1 1 calc R . . H28C H 0.5362 0.7020 0.4456 0.195 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 S1 0.0534(6) 0.0791(7) 0.0717(7) -0.0229(6) -0.0175(5) -0.0086(5) O7 0.097(3) 0.074(3) 0.175(5) 0.015(3) -0.034(3) -0.002(2) O8 0.067(2) 0.149(3) 0.072(2) -0.048(2) -0.0065(17) -0.028(2) O9 0.0514(17) 0.158(4) 0.072(2) -0.049(2) -0.0200(16) 0.012(2) C40 0.123(6) 0.182(7) 0.162(7) -0.095(6) -0.054(5) -0.024(5) F1 0.107(3) 0.221(5) 0.209(5) -0.096(4) -0.050(3) -0.059(3) F2 0.192(5) 0.323(8) 0.176(5) -0.160(6) -0.064(4) -0.035(5) F3 0.260(7) 0.093(3) 0.334(9) -0.087(5) -0.076(7) -0.030(4) O1S 0.056(4) 0.111(6) 0.095(4) -0.056(4) -0.014(4) 0.002(4) C1S 0.083(4) 0.117(6) 0.104(5) -0.058(5) -0.026(4) 0.011(4) C2S 0.088(5) 0.121(6) 0.113(5) -0.062(5) -0.013(4) 0.016(5) C3S 0.079(5) 0.125(7) 0.126(6) -0.043(6) -0.004(5) 0.006(6) C4S 0.062(4) 0.118(6) 0.110(5) -0.045(5) -0.014(4) -0.003(5) O1S' 0.054(3) 0.107(6) 0.098(4) -0.055(3) -0.015(3) -0.003(4) C1S' 0.086(4) 0.118(6) 0.107(5) -0.062(4) -0.023(4) 0.011(4) C2S' 0.099(5) 0.132(6) 0.112(5) -0.054(5) -0.013(4) 0.018(5) C3S' 0.072(4) 0.127(6) 0.121(6) -0.045(5) -0.012(4) 0.011(5) C4S' 0.058(4) 0.124(7) 0.104(5) -0.043(5) -0.022(4) 0.004(5) C21 0.065(4) 0.092(4) 0.121(5) -0.065(4) -0.014(4) 0.003(3) C22 0.119(9) 0.137(8) 0.127(9) -0.051(8) -0.019(8) 0.016(7) C21' 0.067(6) 0.103(6) 0.114(7) -0.047(6) -0.009(6) 0.003(5) C22' 0.091(10) 0.130(10) 0.119(11) -0.041(11) -0.015(9) 0.020(9) C23 0.170(6) 0.103(4) 0.079(3) -0.050(3) -0.033(4) -0.015(4) C24 0.151(7) 0.222(9) 0.172(8) -0.147(7) -0.028(6) -0.031(7) Ag1 0.06035(19) 0.04437(17) 0.04294(17) -0.01128(12) 0.00237(13) -0.02194(13) Ag2 0.0714(2) 0.04103(17) 0.04848(18) -0.01565(13) -0.01019(14) 0.00250(13) P1 0.0528(5) 0.0388(4) 0.0381(4) -0.0111(4) -0.0004(4) -0.0166(4) P2 0.0493(5) 0.0383(4) 0.0420(5) -0.0145(4) 0.0026(4) -0.0082(4) Li1 0.053(4) 0.064(4) 0.061(4) -0.019(3) -0.009(3) -0.011(3) Li2 0.040(3) 0.051(3) 0.040(3) -0.011(2) -0.006(2) -0.006(2) N1 0.0594(18) 0.0345(14) 0.0440(16) -0.0090(12) 0.0012(14) -0.0099(13) N2 0.0554(19) 0.062(2) 0.061(2) -0.0176(17) -0.0039(16) -0.0202(16) N3 0.0550(19) 0.0530(18) 0.0418(16) -0.0111(14) -0.0070(14) -0.0020(14) O1 0.0845(19) 0.0391(13) 0.0450(14) -0.0098(11) -0.0095(13) -0.0196(12) O2 0.0484(16) 0.082(2) 0.107(2) -0.0443(19) 0.0047(16) -0.0126(14) O3 0.141(3) 0.0681(19) 0.0442(15) -0.0132(14) -0.0195(17) -0.0378(19) O4 0.0453(13) 0.0437(13) 0.0466(13) -0.0082(11) -0.0006(11) -0.0044(10) O5 0.088(2) 0.0588(17) 0.0526(16) -0.0286(14) 0.0039(14) -0.0228(15) O6 0.0532(16) 0.0635(17) 0.0735(19) -0.0296(15) 0.0114(14) -0.0186(13) C1 0.070(3) 0.090(4) 0.070(3) -0.017(3) -0.016(2) -0.021(3) C2 0.060(3) 0.131(5) 0.094(4) -0.039(4) -0.018(3) -0.017(3) C3 0.066(3) 0.139(6) 0.098(4) -0.039(4) -0.004(3) -0.041(4) C4 0.070(3) 0.099(4) 0.085(4) -0.028(3) 0.010(3) -0.047(3) C5 0.059(2) 0.058(2) 0.061(2) -0.027(2) 0.0061(19) -0.0200(19) C6 0.066(2) 0.048(2) 0.054(2) -0.0195(18) 0.0101(19) -0.0251(18) C7 0.097(4) 0.051(2) 0.070(3) -0.007(2) -0.002(3) -0.036(2) C8 0.118(4) 0.040(2) 0.054(3) 0.0019(18) -0.010(3) -0.024(2) C9 0.075(3) 0.0394(18) 0.0397(19) -0.0086(15) -0.0040(18) -0.0057(17) C10 0.071(3) 0.046(2) 0.0327(17) -0.0076(15) -0.0019(17) 0.0031(18) C11 0.096(4) 0.055(3) 0.044(2) -0.0068(19) -0.013(2) 0.018(2) C12 0.077(3) 0.094(4) 0.046(2) -0.011(3) -0.010(2) 0.027(3) C13 0.053(3) 0.131(5) 0.053(3) -0.016(3) -0.008(2) -0.002(3) C14 0.064(3) 0.085(3) 0.049(2) -0.011(2) -0.007(2) -0.011(2) C25 0.106(4) 0.094(4) 0.076(3) -0.033(3) -0.017(3) -0.039(3) C26 0.173(7) 0.116(5) 0.131(6) -0.068(5) -0.056(6) -0.029(5) C27 0.072(3) 0.118(5) 0.097(4) -0.055(4) -0.012(3) -0.020(3) C28 0.110(5) 0.153(7) 0.135(6) -0.055(5) 0.005(4) -0.079(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 S1 O9 1.413(3) . ? S1 O7 1.413(4) . ? S1 O8 1.418(4) . ? S1 C40 1.804(8) . ? O8 Li1 1.943(8) 2_775 ? O9 Li2 1.948(6) . ? C40 F1 1.310(10) . ? C40 F2 1.314(11) . ? C40 F3 1.323(12) . ? O1S C4S 1.417(18) . ? O1S C1S 1.464(17) . ? O1S Li1 2.03(2) . ? C1S C2S 1.496(12) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.591(13) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.495(11) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? O1S' C1S' 1.414(16) . ? O1S' C4S' 1.421(17) . ? O1S' Li1 1.935(18) . ? C1S' C2S' 1.527(12) . ? C1S' H1S3 0.9700 . ? C1S' H1S4 0.9700 . ? C2S' C3S' 1.611(12) . ? C2S' H2S3 0.9700 . ? C2S' H2S4 0.9700 . ? C3S' C4S' 1.465(11) . ? C3S' H3S3 0.9700 . ? C3S' H3S4 0.9700 . ? C4S' H4S3 0.9700 . ? C4S' H4S4 0.9700 . ? C21 O2 1.419(8) . ? C21 C22 1.495(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21' O2 1.458(14) . ? C21' C22' 1.513(10) . ? C21' H21C 0.9700 . ? C21' H21D 0.9700 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23 O3 1.426(6) . ? C23 C24 1.460(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Ag1 N1 2.223(3) . ? Ag1 P1 2.3196(9) . ? Ag1 N2 2.366(3) . ? Ag1 Ag2 2.8851(4) . ? Ag2 N3 2.172(3) . ? Ag2 P2 2.3360(9) . ? P1 O1 1.508(3) . ? P1 O3 1.602(3) . ? P1 O2 1.606(3) . ? P1 Li1 2.943(7) 2_775 ? P2 O4 1.506(3) . ? P2 O6 1.602(3) . ? P2 O5 1.605(3) . ? P2 Li2 2.987(6) . ? Li1 O8 1.943(8) 2_775 ? Li1 O4 1.961(8) . ? Li1 O2 2.299(8) 2_775 ? Li1 O1 2.395(7) 2_775 ? Li1 Li2 2.893(9) . ? Li1 P1 2.943(7) 2_775 ? Li1 Li2 3.515(9) 2_775 ? Li2 O4 1.933(6) . ? Li2 O1 1.939(6) 2_775 ? Li2 O1 1.954(7) . ? Li2 Li2 2.635(11) 2_775 ? Li2 Li1 3.515(9) 2_775 ? N1 C9 1.358(5) . ? N1 C6 1.368(5) . ? N2 C5 1.333(5) . ? N2 C1 1.337(6) . ? N3 C14 1.335(6) . ? N3 C10 1.350(5) . ? O1 Li2 1.939(6) 2_775 ? O1 Li1 2.395(7) 2_775 ? O2 Li1 2.299(8) 2_775 ? O5 C25 1.407(6) . ? O6 C27 1.396(6) . ? C1 C2 1.382(7) . ? C1 H1A 0.9300 . ? C2 C3 1.332(9) . ? C2 H2A 0.9300 . ? C3 C4 1.387(9) . ? C3 H3A 0.9300 . ? C4 C5 1.410(6) . ? C4 H4A 0.9300 . ? C5 C6 1.446(7) . ? C6 C7 1.389(6) . ? C7 C8 1.348(8) . ? C7 H7A 0.9300 . ? C8 C9 1.400(6) . ? C8 H8B 0.9300 . ? C9 C10 1.446(6) . ? C10 C11 1.407(6) . ? C11 C12 1.330(8) . ? C11 H11A 0.9300 . ? C12 C13 1.379(9) . ? C12 H12A 0.9300 . ? C13 C14 1.392(7) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C25 C26 1.472(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.464(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 O9 S1 O7 117.1(3) . . ? O9 S1 O8 114.8(2) . . ? O7 S1 O8 114.7(3) . . ? O9 S1 C40 104.5(4) . . ? O7 S1 C40 100.0(4) . . ? O8 S1 C40 102.6(4) . . ? S1 O8 Li1 137.4(3) . 2_775 ? S1 O9 Li2 132.2(3) . . ? F1 C40 F2 107.4(7) . . ? F1 C40 F3 110.6(9) . . ? F2 C40 F3 109.0(9) . . ? F1 C40 S1 110.7(7) . . ? F2 C40 S1 110.2(8) . . ? F3 C40 S1 109.0(6) . . ? C4S O1S C1S 103.8(17) . . ? C4S O1S Li1 119.1(19) . . ? C1S O1S Li1 122(2) . . ? O1S C1S C2S 100.8(15) . . ? O1S C1S H1S1 111.6 . . ? C2S C1S H1S1 111.6 . . ? O1S C1S H1S2 111.6 . . ? C2S C1S H1S2 111.6 . . ? H1S1 C1S H1S2 109.4 . . ? C1S C2S C3S 92.2(11) . . ? C1S C2S H2S1 113.2 . . ? C3S C2S H2S1 113.2 . . ? C1S C2S H2S2 113.2 . . ? C3S C2S H2S2 113.2 . . ? H2S1 C2S H2S2 110.6 . . ? C4S C3S C2S 99.7(10) . . ? C4S C3S H3S1 111.8 . . ? C2S C3S H3S1 111.8 . . ? C4S C3S H3S2 111.8 . . ? C2S C3S H3S2 111.8 . . ? H3S1 C3S H3S2 109.6 . . ? O1S C4S C3S 107.2(11) . . ? O1S C4S H4S1 110.3 . . ? C3S C4S H4S1 110.3 . . ? O1S C4S H4S2 110.3 . . ? C3S C4S H4S2 110.3 . . ? H4S1 C4S H4S2 108.5 . . ? C1S' O1S' C4S' 106.1(16) . . ? C1S' O1S' Li1 124.0(11) . . ? C4S' O1S' Li1 129.3(11) . . ? O1S' C1S' C2S' 101.6(16) . . ? O1S' C1S' H1S3 111.4 . . ? C2S' C1S' H1S3 111.4 . . ? O1S' C1S' H1S4 111.4 . . ? C2S' C1S' H1S4 111.4 . . ? H1S3 C1S' H1S4 109.3 . . ? C1S' C2S' C3S' 95.0(10) . . ? C1S' C2S' H2S3 112.7 . . ? C3S' C2S' H2S3 112.7 . . ? C1S' C2S' H2S4 112.7 . . ? C3S' C2S' H2S4 112.7 . . ? H2S3 C2S' H2S4 110.2 . . ? C4S' C3S' C2S' 101.5(8) . . ? C4S' C3S' H3S3 111.5 . . ? C2S' C3S' H3S3 111.5 . . ? C4S' C3S' H3S4 111.5 . . ? C2S' C3S' H3S4 111.5 . . ? H3S3 C3S' H3S4 109.3 . . ? O1S' C4S' C3S' 108.3(10) . . ? O1S' C4S' H4S3 110.0 . . ? C3S' C4S' H4S3 110.0 . . ? O1S' C4S' H4S4 110.0 . . ? C3S' C4S' H4S4 110.0 . . ? H4S3 C4S' H4S4 108.4 . . ? O2 C21 C22 109.9(8) . . ? O2 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? O2 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? O2 C21' C22' 111.1(15) . . ? O2 C21' H21C 109.4 . . ? C22' C21' H21C 109.4 . . ? O2 C21' H21D 109.4 . . ? C22' C21' H21D 109.4 . . ? H21C C21' H21D 108.0 . . ? C21' C22' H22D 109.5 . . ? C21' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? O3 C23 C24 111.8(6) . . ? O3 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? O3 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 Ag1 P1 156.64(9) . . ? N1 Ag1 N2 74.19(12) . . ? P1 Ag1 N2 129.11(9) . . ? N1 Ag1 Ag2 65.22(8) . . ? P1 Ag1 Ag2 102.57(3) . . ? N2 Ag1 Ag2 109.99(9) . . ? N3 Ag2 P2 164.53(10) . . ? N3 Ag2 Ag1 89.90(9) . . ? P2 Ag2 Ag1 102.86(3) . . ? O1 P1 O3 103.76(16) . . ? O1 P1 O2 101.90(18) . . ? O3 P1 O2 100.7(2) . . ? O1 P1 Ag1 119.92(11) . . ? O3 P1 Ag1 112.93(13) . . ? O2 P1 Ag1 115.25(14) . . ? O1 P1 Li1 54.12(18) . 2_775 ? O3 P1 Li1 94.5(2) . 2_775 ? O2 P1 Li1 50.94(19) . 2_775 ? Ag1 P1 Li1 152.06(15) . 2_775 ? O4 P2 O6 110.40(16) . . ? O4 P2 O5 109.11(15) . . ? O6 P2 O5 93.05(17) . . ? O4 P2 Ag2 116.04(10) . . ? O6 P2 Ag2 112.90(12) . . ? O5 P2 Ag2 113.01(13) . . ? O4 P2 Li2 34.03(14) . . ? O6 P2 Li2 141.15(17) . . ? O5 P2 Li2 111.31(17) . . ? Ag2 P2 Li2 85.65(12) . . ? O1S' Li1 O8 101.0(7) . 2_775 ? O1S' Li1 O4 105.9(14) . . ? O8 Li1 O4 120.4(4) 2_775 . ? O1S' Li1 O1S 2(2) . . ? O8 Li1 O1S 102.5(7) 2_775 . ? O4 Li1 O1S 106.6(15) . . ? O1S' Li1 O2 93.2(14) . 2_775 ? O8 Li1 O2 102.5(3) 2_775 2_775 ? O4 Li1 O2 127.4(4) . 2_775 ? O1S Li1 O2 91.0(14) . 2_775 ? O1S' Li1 O1 152.1(10) . 2_775 ? O8 Li1 O1 97.1(3) 2_775 2_775 ? O4 Li1 O1 82.5(3) . 2_775 ? O1S Li1 O1 149.6(11) . 2_775 ? O2 Li1 O1 62.0(2) 2_775 2_775 ? O1S' Li1 Li2 144.5(12) . . ? O8 Li1 Li2 108.6(3) 2_775 . ? O4 Li1 Li2 41.63(19) . . ? O1S Li1 Li2 144.3(13) . . ? O2 Li1 Li2 99.0(3) 2_775 . ? O1 Li1 Li2 41.70(17) 2_775 . ? O1S' Li1 P1 122.0(12) . 2_775 ? O8 Li1 P1 108.6(3) 2_775 2_775 ? O4 Li1 P1 100.4(3) . 2_775 ? O1S Li1 P1 119.6(12) . 2_775 ? O2 Li1 P1 32.85(12) 2_775 2_775 ? O1 Li1 P1 30.69(11) 2_775 2_775 ? Li2 Li1 P1 66.36(19) . 2_775 ? O1S' Li1 Li2 168.1(11) . 2_775 ? O8 Li1 Li2 68.7(2) 2_775 2_775 ? O4 Li1 Li2 85.0(3) . 2_775 ? O1S Li1 Li2 168.2(14) . 2_775 ? O2 Li1 Li2 83.6(2) 2_775 2_775 ? O1 Li1 Li2 32.02(15) 2_775 2_775 ? Li2 Li1 Li2 47.3(2) . 2_775 ? P1 Li1 Li2 58.96(16) 2_775 2_775 ? O4 Li2 O1 96.6(3) . 2_775 ? O4 Li2 O9 118.7(3) . . ? O1 Li2 O9 120.8(4) 2_775 . ? O4 Li2 O1 117.3(3) . . ? O1 Li2 O1 94.8(3) 2_775 . ? O9 Li2 O1 106.6(3) . . ? O4 Li2 Li2 115.1(4) . 2_775 ? O1 Li2 Li2 47.6(2) 2_775 2_775 ? O9 Li2 Li2 126.1(4) . 2_775 ? O1 Li2 Li2 47.2(2) . 2_775 ? O4 Li2 Li1 42.39(19) . . ? O1 Li2 Li1 55.2(2) 2_775 . ? O9 Li2 Li1 145.7(3) . . ? O1 Li2 Li1 107.7(3) . . ? Li2 Li2 Li1 78.8(3) 2_775 . ? O4 Li2 P2 25.86(11) . . ? O1 Li2 P2 121.6(3) 2_775 . ? O9 Li2 P2 96.9(2) . . ? O1 Li2 P2 116.6(3) . . ? Li2 Li2 P2 135.8(3) 2_775 . ? Li1 Li2 P2 68.24(19) . . ? O4 Li2 Li1 157.8(3) . 2_775 ? O1 Li2 Li1 87.9(2) 2_775 2_775 ? O9 Li2 Li1 76.2(2) . 2_775 ? O1 Li2 Li1 40.54(18) . 2_775 ? Li2 Li2 Li1 53.9(2) 2_775 2_775 ? Li1 Li2 Li1 132.7(2) . 2_775 ? P2 Li2 Li1 147.4(2) . 2_775 ? C9 N1 C6 106.5(3) . . ? C9 N1 Ag1 136.0(3) . . ? C6 N1 Ag1 113.5(3) . . ? C5 N2 C1 118.9(4) . . ? C5 N2 Ag1 112.4(3) . . ? C1 N2 Ag1 128.6(3) . . ? C14 N3 C10 119.3(4) . . ? C14 N3 Ag2 119.2(3) . . ? C10 N3 Ag2 120.8(3) . . ? P1 O1 Li2 135.5(2) . 2_775 ? P1 O1 Li2 136.2(2) . . ? Li2 O1 Li2 85.2(3) 2_775 . ? P1 O1 Li1 95.2(2) . 2_775 ? Li2 O1 Li1 83.1(3) 2_775 2_775 ? Li2 O1 Li1 107.4(3) . 2_775 ? C21 O2 C21' 46.2(8) . . ? C21 O2 P1 122.5(4) . . ? C21' O2 P1 118.8(7) . . ? C21 O2 Li1 140.2(4) . 2_775 ? C21' O2 Li1 124.9(9) . 2_775 ? P1 O2 Li1 96.2(2) . 2_775 ? C23 O3 P1 122.3(3) . . ? P2 O4 Li2 120.1(2) . . ? P2 O4 Li1 143.9(3) . . ? Li2 O4 Li1 96.0(3) . . ? C25 O5 P2 120.3(3) . . ? C27 O6 P2 119.2(3) . . ? N2 C1 C2 123.4(5) . . ? N2 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.7(6) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 119.5(5) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N2 C5 C4 119.8(5) . . ? N2 C5 C6 117.5(4) . . ? C4 C5 C6 122.7(4) . . ? N1 C6 C7 109.3(4) . . ? N1 C6 C5 120.8(3) . . ? C7 C6 C5 129.8(4) . . ? C8 C7 C6 107.6(4) . . ? C8 C7 H7A 126.2 . . ? C6 C7 H7A 126.2 . . ? C7 C8 C9 107.3(4) . . ? C7 C8 H8B 126.3 . . ? C9 C8 H8B 126.3 . . ? N1 C9 C8 109.2(4) . . ? N1 C9 C10 122.7(3) . . ? C8 C9 C10 128.0(4) . . ? N3 C10 C11 118.9(5) . . ? N3 C10 C9 119.0(3) . . ? C11 C10 C9 122.1(4) . . ? C12 C11 C10 121.8(5) . . ? C12 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C12 C13 C14 117.9(5) . . ? C12 C13 H13A 121.1 . . ? C14 C13 H13A 121.1 . . ? N3 C14 C13 122.7(5) . . ? N3 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? O5 C25 C26 109.7(5) . . ? O5 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? O5 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C28 110.7(5) . . ? O6 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O6 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.936 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.172 _database_code_depnum_ccdc_archive 'CCDC 963077' ####################################################################### # # 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_complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cu N6 Na O2' _chemical_formula_weight 671.24 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' Cu Cu 0.3201 1.2651 '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' Na Na 0.0362 0.0249 '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 Orthorhombic _symmetry_space_group_name_H-M 'Fdd2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 11.6882(3) _cell_length_b 30.6434(8) _cell_length_c 18.0484(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6464.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7123 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.55 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6596 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7241 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2976 _reflns_number_gt 2949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0242P)^2^+3.9959P] 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 0.023(9) _refine_ls_number_reflns 2976 _refine_ls_number_parameters 210 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0530 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Cu1 Cu -0.2500 -0.2500 0.221725(15) 0.01557(6) Uani 1 2 d S . . Na1 Na -0.2500 -0.2500 0.06145(5) 0.01707(18) Uani 1 2 d S . . O1 O -0.37965(9) -0.26146(4) -0.03788(7) 0.0268(2) Uani 1 1 d . . . N1 N -0.09464(10) -0.25736(4) 0.16953(7) 0.0136(2) Uani 1 1 d . . . N2 N -0.17698(9) -0.19514(4) 0.25938(6) 0.0155(2) Uani 1 1 d . . . N3 N -0.18803(10) -0.32503(4) 0.08111(7) 0.0172(2) Uani 1 1 d . . . C1 C -0.22580(14) -0.16267(5) 0.29811(8) 0.0212(3) Uani 1 1 d . . . H1A H -0.3009 -0.1663 0.3140 0.025 Uiso 1 1 calc R . . C2 C -0.17097(15) -0.12442(5) 0.31559(9) 0.0261(3) Uani 1 1 d . . . H2A H -0.2081 -0.1027 0.3425 0.031 Uiso 1 1 calc R . . C3 C -0.05876(15) -0.11888(5) 0.29210(10) 0.0284(3) Uani 1 1 d . . . H3A H -0.0193 -0.0933 0.3031 0.034 Uiso 1 1 calc R . . C4 C -0.00673(13) -0.15165(6) 0.25227(10) 0.0247(3) Uani 1 1 d . . . H4A H 0.0684 -0.1484 0.2363 0.030 Uiso 1 1 calc R . . C5 C -0.06722(11) -0.18988(5) 0.23590(7) 0.0159(3) Uani 1 1 d . . . C6 C -0.02040(11) -0.22595(5) 0.19450(8) 0.0158(3) Uani 1 1 d . . . C7 C 0.09299(12) -0.23756(6) 0.17873(9) 0.0214(3) Uani 1 1 d . . . H7A H 0.1584 -0.2216 0.1897 0.026 Uiso 1 1 calc R . . C8 C 0.08790(11) -0.27784(5) 0.14334(9) 0.0205(3) Uani 1 1 d . . . H8A H 0.1496 -0.2941 0.1261 0.025 Uiso 1 1 calc R . . C9 C -0.02854(11) -0.28924(5) 0.13863(8) 0.0154(3) Uani 1 1 d . . . C10 C -0.07966(11) -0.32847(5) 0.10686(7) 0.0153(3) Uani 1 1 d . . . C11 C -0.01967(13) -0.36780(5) 0.10292(9) 0.0218(3) Uani 1 1 d . . . H11A H 0.0550 -0.3695 0.1205 0.026 Uiso 1 1 calc R . . C12 C -0.07169(14) -0.40415(5) 0.07286(9) 0.0262(3) Uani 1 1 d . . . H12A H -0.0323 -0.4304 0.0696 0.031 Uiso 1 1 calc R . . C13 C -0.18346(14) -0.40102(5) 0.04759(9) 0.0248(3) Uani 1 1 d . . . H13A H -0.2211 -0.4251 0.0278 0.030 Uiso 1 1 calc R . . C14 C -0.23680(12) -0.36100(5) 0.05285(10) 0.0222(3) Uani 1 1 d . . . H14A H -0.3116 -0.3588 0.0357 0.027 Uiso 1 1 calc R . . C15 C -0.40549(17) -0.22530(6) -0.08456(10) 0.0369(4) Uani 1 1 d . . . H15A H -0.3955 -0.2330 -0.1363 0.044 Uiso 1 1 calc R . . H15B H -0.3564 -0.2007 -0.0731 0.044 Uiso 1 1 calc R . . C16 C -0.5287(2) -0.21457(7) -0.06842(11) 0.0441(5) Uani 1 1 d . . . H16A H -0.5364 -0.1978 -0.0231 0.053 Uiso 1 1 calc R . . H16B H -0.5637 -0.1987 -0.1090 0.053 Uiso 1 1 calc R . . C17 C -0.57920(18) -0.25933(8) -0.06035(15) 0.0507(6) Uani 1 1 d . . . H17A H -0.5980 -0.2718 -0.1082 0.061 Uiso 1 1 calc R . . H17B H -0.6474 -0.2587 -0.0298 0.061 Uiso 1 1 calc R . . C18 C -0.48356(13) -0.28465(6) -0.02294(13) 0.0303(4) Uani 1 1 d . . . H18A H -0.4968 -0.2864 0.0300 0.036 Uiso 1 1 calc R . . H18B H -0.4794 -0.3140 -0.0427 0.036 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 Cu1 0.01068(10) 0.01797(12) 0.01808(11) 0.000 0.000 -0.00078(9) Na1 0.0166(4) 0.0172(4) 0.0174(4) 0.000 0.000 0.0030(3) O1 0.0224(5) 0.0301(6) 0.0280(6) 0.0077(5) -0.0063(5) -0.0054(5) N1 0.0118(5) 0.0157(6) 0.0133(5) -0.0011(4) -0.0012(4) 0.0002(4) N2 0.0169(5) 0.0162(6) 0.0135(5) -0.0009(4) -0.0025(4) 0.0028(4) N3 0.0162(5) 0.0159(6) 0.0195(6) -0.0005(5) -0.0023(4) 0.0009(4) C1 0.0249(7) 0.0200(8) 0.0186(7) 0.0003(6) -0.0008(5) 0.0077(6) C2 0.0403(9) 0.0177(8) 0.0205(8) -0.0045(6) -0.0062(6) 0.0092(6) C3 0.0391(9) 0.0180(8) 0.0281(8) -0.0042(6) -0.0093(7) -0.0047(7) C4 0.0257(8) 0.0238(9) 0.0246(8) -0.0015(7) -0.0050(5) -0.0071(5) C5 0.0168(6) 0.0177(7) 0.0133(6) 0.0008(5) -0.0039(5) -0.0008(5) C6 0.0133(5) 0.0189(7) 0.0151(6) 0.0000(5) -0.0025(5) -0.0023(5) C7 0.0128(6) 0.0293(8) 0.0220(7) -0.0028(6) -0.0001(5) -0.0047(6) C8 0.0110(6) 0.0286(8) 0.0220(7) -0.0030(6) 0.0000(5) 0.0030(5) C9 0.0129(5) 0.0191(7) 0.0140(6) -0.0004(5) -0.0006(5) 0.0025(5) C10 0.0165(6) 0.0179(7) 0.0116(6) 0.0001(5) 0.0019(5) 0.0021(5) C11 0.0215(6) 0.0225(8) 0.0215(7) -0.0027(6) -0.0032(6) 0.0067(6) C12 0.0334(8) 0.0196(8) 0.0256(8) -0.0036(6) -0.0013(6) 0.0102(6) C13 0.0321(8) 0.0199(8) 0.0224(7) -0.0042(6) -0.0024(6) -0.0028(6) C14 0.0216(7) 0.0201(8) 0.0250(8) -0.0007(6) -0.0057(6) -0.0024(6) C15 0.0516(11) 0.0375(10) 0.0216(8) 0.0136(7) -0.0088(7) -0.0140(8) C16 0.0638(12) 0.0436(12) 0.0251(9) -0.0022(8) -0.0204(9) 0.0222(10) C17 0.0253(10) 0.0720(15) 0.0547(14) -0.0031(12) -0.0121(9) -0.0039(10) C18 0.0322(8) 0.0276(8) 0.0312(9) -0.0004(9) 0.0027(8) -0.0099(6) _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 Cu1 N2 2.0041(12) . ? Cu1 N2 2.0041(12) 14_445 ? Cu1 N1 2.0581(12) 14_445 ? Cu1 N1 2.0581(12) . ? Cu1 Na1 2.8927(9) . ? Na1 O1 2.3736(13) . ? Na1 O1 2.3736(13) 14_445 ? Na1 N3 2.4365(12) 14_445 ? Na1 N3 2.4365(12) . ? Na1 N1 2.6745(13) . ? Na1 N1 2.6745(13) 14_445 ? O1 C15 1.424(2) . ? O1 C18 1.4328(19) . ? N1 C9 1.3646(17) . ? N1 C6 1.3720(17) . ? N2 C1 1.3433(19) . ? N2 C5 1.3607(17) . ? N3 C14 1.3417(19) . ? N3 C10 1.3534(17) . ? C1 C2 1.372(2) . ? C1 H1A 0.9300 . ? C2 C3 1.389(2) . ? C2 H2A 0.9300 . ? C3 C4 1.377(2) . ? C3 H3A 0.9300 . ? C4 C5 1.400(2) . ? C4 H4A 0.9300 . ? C5 C6 1.442(2) . ? C6 C7 1.4015(19) . ? C7 C8 1.391(2) . ? C7 H7A 0.9300 . ? C8 C9 1.4076(17) . ? C8 H8A 0.9300 . ? C9 C10 1.4599(19) . ? C10 C11 1.396(2) . ? C11 C12 1.380(2) . ? C11 H11A 0.9300 . ? C12 C13 1.387(2) . ? C12 H12A 0.9300 . ? C13 C14 1.379(2) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.506(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.500(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.519(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? 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 N2 Cu1 N2 140.35(7) . 14_445 ? N2 Cu1 N1 116.04(5) . 14_445 ? N2 Cu1 N1 82.61(5) 14_445 14_445 ? N2 Cu1 N1 82.61(5) . . ? N2 Cu1 N1 116.04(5) 14_445 . ? N1 Cu1 N1 125.52(7) 14_445 . ? N2 Cu1 Na1 109.82(4) . . ? N2 Cu1 Na1 109.82(4) 14_445 . ? N1 Cu1 Na1 62.76(3) 14_445 . ? N1 Cu1 Na1 62.76(3) . . ? O1 Na1 O1 81.89(6) . 14_445 ? O1 Na1 N3 93.43(4) . 14_445 ? O1 Na1 N3 99.21(4) 14_445 14_445 ? O1 Na1 N3 99.21(4) . . ? O1 Na1 N3 93.43(4) 14_445 . ? N3 Na1 N3 163.26(7) 14_445 . ? O1 Na1 N1 166.37(4) . . ? O1 Na1 N1 97.46(4) 14_445 . ? N3 Na1 N1 100.09(4) 14_445 . ? N3 Na1 N1 67.19(4) . . ? O1 Na1 N1 97.46(4) . 14_445 ? O1 Na1 N1 166.37(4) 14_445 14_445 ? N3 Na1 N1 67.19(4) 14_445 14_445 ? N3 Na1 N1 100.09(4) . 14_445 ? N1 Na1 N1 86.34(6) . 14_445 ? O1 Na1 Cu1 139.05(3) . . ? O1 Na1 Cu1 139.05(3) 14_445 . ? N3 Na1 Cu1 81.63(3) 14_445 . ? N3 Na1 Cu1 81.63(3) . . ? N1 Na1 Cu1 43.17(3) . . ? N1 Na1 Cu1 43.17(3) 14_445 . ? C15 O1 C18 108.51(13) . . ? C15 O1 Na1 117.84(10) . . ? C18 O1 Na1 118.19(11) . . ? C9 N1 C6 106.16(11) . . ? C9 N1 Cu1 139.92(10) . . ? C6 N1 Cu1 109.32(9) . . ? C9 N1 Na1 98.44(8) . . ? C6 N1 Na1 127.58(9) . . ? Cu1 N1 Na1 74.07(4) . . ? C1 N2 C5 118.35(13) . . ? C1 N2 Cu1 128.09(10) . . ? C5 N2 Cu1 113.28(9) . . ? C14 N3 C10 117.66(13) . . ? C14 N3 Na1 126.41(10) . . ? C10 N3 Na1 113.69(9) . . ? N2 C1 C2 123.63(15) . . ? N2 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 C2 C3 118.38(15) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 119.17(15) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 119.84(14) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N2 C5 C4 120.63(13) . . ? N2 C5 C6 115.37(12) . . ? C4 C5 C6 124.00(13) . . ? N1 C6 C7 110.69(13) . . ? N1 C6 C5 117.90(12) . . ? C7 C6 C5 131.20(13) . . ? C8 C7 C6 106.15(13) . . ? C8 C7 H7A 126.9 . . ? C6 C7 H7A 126.9 . . ? C7 C8 C9 106.81(12) . . ? C7 C8 H8A 126.6 . . ? C9 C8 H8A 126.6 . . ? N1 C9 C8 110.20(12) . . ? N1 C9 C10 121.21(12) . . ? C8 C9 C10 128.59(13) . . ? N3 C10 C11 121.32(13) . . ? N3 C10 C9 116.99(12) . . ? C11 C10 C9 121.70(12) . . ? C12 C11 C10 119.71(14) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 119.24(14) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 117.68(15) . . ? C14 C13 H13A 121.2 . . ? C12 C13 H13A 121.2 . . ? N3 C14 C13 124.38(14) . . ? N3 C14 H14A 117.8 . . ? C13 C14 H14A 117.8 . . ? O1 C15 C16 104.97(14) . . ? O1 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? O1 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.8 . . ? C17 C16 C15 101.25(16) . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16B 111.5 . . ? C15 C16 H16B 111.5 . . ? H16A C16 H16B 109.3 . . ? C16 C17 C18 102.77(15) . . ? C16 C17 H17A 111.2 . . ? C18 C17 H17A 111.2 . . ? C16 C17 H17B 111.2 . . ? C18 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? O1 C18 C17 106.66(16) . . ? O1 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O1 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 Na1 O1 -129.97(6) . . . . ? N2 Cu1 Na1 O1 50.03(6) 14_445 . . . ? N1 Cu1 Na1 O1 -20.13(6) 14_445 . . . ? N1 Cu1 Na1 O1 159.87(6) . . . . ? N2 Cu1 Na1 O1 50.03(6) . . . 14_445 ? N2 Cu1 Na1 O1 -129.97(6) 14_445 . . 14_445 ? N1 Cu1 Na1 O1 159.87(6) 14_445 . . 14_445 ? N1 Cu1 Na1 O1 -20.13(6) . . . 14_445 ? N2 Cu1 Na1 N3 -44.40(4) . . . 14_445 ? N2 Cu1 Na1 N3 135.60(4) 14_445 . . 14_445 ? N1 Cu1 Na1 N3 65.43(5) 14_445 . . 14_445 ? N1 Cu1 Na1 N3 -114.57(5) . . . 14_445 ? N2 Cu1 Na1 N3 135.60(4) . . . . ? N2 Cu1 Na1 N3 -44.40(4) 14_445 . . . ? N1 Cu1 Na1 N3 -114.57(5) 14_445 . . . ? N1 Cu1 Na1 N3 65.43(5) . . . . ? N2 Cu1 Na1 N1 70.16(5) . . . . ? N2 Cu1 Na1 N1 -109.84(5) 14_445 . . . ? N1 Cu1 Na1 N1 180.0 14_445 . . . ? N2 Cu1 Na1 N1 -109.84(5) . . . 14_445 ? N2 Cu1 Na1 N1 70.16(5) 14_445 . . 14_445 ? N1 Cu1 Na1 N1 180.0 . . . 14_445 ? O1 Na1 O1 C15 -65.67(11) 14_445 . . . ? N3 Na1 O1 C15 33.16(13) 14_445 . . . ? N3 Na1 O1 C15 -157.86(12) . . . . ? N1 Na1 O1 C15 -153.92(18) . . . . ? N1 Na1 O1 C15 100.59(12) 14_445 . . . ? Cu1 Na1 O1 C15 114.33(11) . . . . ? O1 Na1 O1 C18 160.67(14) 14_445 . . . ? N3 Na1 O1 C18 -100.50(12) 14_445 . . . ? N3 Na1 O1 C18 68.49(12) . . . . ? N1 Na1 O1 C18 72.4(2) . . . . ? N1 Na1 O1 C18 -33.07(12) 14_445 . . . ? Cu1 Na1 O1 C18 -19.33(14) . . . . ? N2 Cu1 N1 C9 159.02(15) . . . . ? N2 Cu1 N1 C9 15.82(16) 14_445 . . . ? N1 Cu1 N1 C9 -84.14(14) 14_445 . . . ? Na1 Cu1 N1 C9 -84.14(14) . . . . ? N2 Cu1 N1 C6 8.05(9) . . . . ? N2 Cu1 N1 C6 -135.15(9) 14_445 . . . ? N1 Cu1 N1 C6 124.89(10) 14_445 . . . ? Na1 Cu1 N1 C6 124.89(10) . . . . ? N2 Cu1 N1 Na1 -116.83(4) . . . . ? N2 Cu1 N1 Na1 99.96(4) 14_445 . . . ? N1 Cu1 N1 Na1 0.0 14_445 . . . ? O1 Na1 N1 C9 32.9(2) . . . . ? O1 Na1 N1 C9 -53.51(9) 14_445 . . . ? N3 Na1 N1 C9 -154.31(9) 14_445 . . . ? N3 Na1 N1 C9 37.09(8) . . . . ? N1 Na1 N1 C9 139.64(10) 14_445 . . . ? Cu1 Na1 N1 C9 139.64(10) . . . . ? O1 Na1 N1 C6 150.84(18) . . . . ? O1 Na1 N1 C6 64.47(11) 14_445 . . . ? N3 Na1 N1 C6 -36.33(12) 14_445 . . . ? N3 Na1 N1 C6 155.06(12) . . . . ? N1 Na1 N1 C6 -102.38(12) 14_445 . . . ? Cu1 Na1 N1 C6 -102.38(12) . . . . ? O1 Na1 N1 Cu1 -106.77(19) . . . . ? O1 Na1 N1 Cu1 166.85(4) 14_445 . . . ? N3 Na1 N1 Cu1 66.05(4) 14_445 . . . ? N3 Na1 N1 Cu1 -102.56(4) . . . . ? N1 Na1 N1 Cu1 0.0 14_445 . . . ? N2 Cu1 N2 C1 -65.15(12) 14_445 . . . ? N1 Cu1 N2 C1 46.28(13) 14_445 . . . ? N1 Cu1 N2 C1 172.34(13) . . . . ? Na1 Cu1 N2 C1 114.85(12) . . . . ? N2 Cu1 N2 C5 121.04(9) 14_445 . . . ? N1 Cu1 N2 C5 -127.53(9) 14_445 . . . ? N1 Cu1 N2 C5 -1.47(9) . . . . ? Na1 Cu1 N2 C5 -58.96(9) . . . . ? O1 Na1 N3 C14 -12.68(13) . . . . ? O1 Na1 N3 C14 -95.01(13) 14_445 . . . ? N3 Na1 N3 C14 125.87(13) 14_445 . . . ? N1 Na1 N3 C14 168.33(14) . . . . ? N1 Na1 N3 C14 86.67(13) 14_445 . . . ? Cu1 Na1 N3 C14 125.87(13) . . . . ? O1 Na1 N3 C10 149.78(9) . . . . ? O1 Na1 N3 C10 67.45(9) 14_445 . . . ? N3 Na1 N3 C10 -71.66(9) 14_445 . . . ? N1 Na1 N3 C10 -29.21(8) . . . . ? N1 Na1 N3 C10 -110.86(9) 14_445 . . . ? Cu1 Na1 N3 C10 -71.66(9) . . . . ? C5 N2 C1 C2 -0.2(2) . . . . ? Cu1 N2 C1 C2 -173.75(11) . . . . ? N2 C1 C2 C3 -0.1(2) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C2 C3 C4 C5 0.1(2) . . . . ? C1 N2 C5 C4 0.45(19) . . . . ? Cu1 N2 C5 C4 174.92(11) . . . . ? C1 N2 C5 C6 -179.83(13) . . . . ? Cu1 N2 C5 C6 -5.36(14) . . . . ? C3 C4 C5 N2 -0.4(2) . . . . ? C3 C4 C5 C6 179.88(15) . . . . ? C9 N1 C6 C7 0.70(16) . . . . ? Cu1 N1 C6 C7 161.72(10) . . . . ? Na1 N1 C6 C7 -113.86(13) . . . . ? C9 N1 C6 C5 -174.58(12) . . . . ? Cu1 N1 C6 C5 -13.57(15) . . . . ? Na1 N1 C6 C5 70.86(15) . . . . ? N2 C5 C6 N1 13.19(18) . . . . ? C4 C5 C6 N1 -167.10(14) . . . . ? N2 C5 C6 C7 -160.94(15) . . . . ? C4 C5 C6 C7 18.8(3) . . . . ? N1 C6 C7 C8 -0.55(18) . . . . ? C5 C6 C7 C8 173.90(15) . . . . ? C6 C7 C8 C9 0.18(18) . . . . ? C6 N1 C9 C8 -0.58(15) . . . . ? Cu1 N1 C9 C8 -152.10(12) . . . . ? Na1 N1 C9 C8 132.64(11) . . . . ? C6 N1 C9 C10 179.22(13) . . . . ? Cu1 N1 C9 C10 27.7(2) . . . . ? Na1 N1 C9 C10 -47.56(13) . . . . ? C7 C8 C9 N1 0.25(17) . . . . ? C7 C8 C9 C10 -179.54(15) . . . . ? C14 N3 C10 C11 1.2(2) . . . . ? Na1 N3 C10 C11 -162.87(12) . . . . ? C14 N3 C10 C9 -178.95(13) . . . . ? Na1 N3 C10 C9 16.94(14) . . . . ? N1 C9 C10 N3 26.75(19) . . . . ? C8 C9 C10 N3 -153.49(14) . . . . ? N1 C9 C10 C11 -153.43(14) . . . . ? C8 C9 C10 C11 26.3(2) . . . . ? N3 C10 C11 C12 -0.6(2) . . . . ? C9 C10 C11 C12 179.58(14) . . . . ? C10 C11 C12 C13 -0.6(2) . . . . ? C11 C12 C13 C14 1.0(2) . . . . ? C10 N3 C14 C13 -0.7(2) . . . . ? Na1 N3 C14 C13 161.10(13) . . . . ? C12 C13 C14 N3 -0.4(3) . . . . ? C18 O1 C15 C16 26.4(2) . . . . ? Na1 O1 C15 C16 -111.39(13) . . . . ? O1 C15 C16 C17 -39.1(2) . . . . ? C15 C16 C17 C18 36.1(2) . . . . ? C15 O1 C18 C17 -2.8(2) . . . . ? Na1 O1 C18 C17 134.75(15) . . . . ? C16 C17 C18 O1 -21.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.209 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.046 _database_code_depnum_ccdc_archive 'CCDC 963078' ####################################################################### # # 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_complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Ag2 Br4 F6 N6 O6 S2' _chemical_formula_weight 1272.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8073(16) _cell_length_b 15.310(3) _cell_length_c 16.630(3) _cell_angle_alpha 110.57(3) _cell_angle_beta 98.30(3) _cell_angle_gamma 96.19(3) _cell_volume 1814.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7027 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.63 _exptl_crystal_description layer _exptl_crystal_colour 'slightly yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 5.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5111 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 15452 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.65 _reflns_number_total 8113 _reflns_number_gt 6909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0280P)^2^+1.9851P] 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 8113 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.51379(3) 0.212947(16) -0.025930(15) 0.01677(6) Uani 1 1 d . . . Br1 Br 0.60686(4) 0.44200(2) 0.07428(2) 0.02023(8) Uani 1 1 d . . . Br2 Br 0.53977(5) -0.31650(2) 0.16514(2) 0.02178(8) Uani 1 1 d . . . S1 S 0.98560(10) 0.23794(5) -0.02888(5) 0.01450(15) Uani 1 1 d . . . F1 F 0.9195(3) 0.40074(13) -0.03169(14) 0.0275(5) Uani 1 1 d . . . F2 F 1.1032(3) 0.41074(14) 0.08262(14) 0.0338(5) Uani 1 1 d . . . F3 F 1.1839(3) 0.38038(14) -0.04099(15) 0.0328(5) Uani 1 1 d . . . O1 O 0.8533(3) 0.23666(16) 0.02314(15) 0.0206(5) Uani 1 1 d . . . O2 O 1.1440(3) 0.20736(17) -0.00276(17) 0.0290(6) Uani 1 1 d . . . O3 O 0.9190(3) 0.20087(15) -0.12237(14) 0.0175(5) Uani 1 1 d . . . N1 N 0.4454(3) 0.10189(17) 0.19971(17) 0.0144(5) Uani 1 1 d . . . H1A H 0.4798 0.1309 0.2554 0.017 Uiso 1 1 calc R . . N2 N 0.4956(3) 0.29005(17) 0.11670(17) 0.0135(5) Uani 1 1 d . . . N3 N 0.4720(3) -0.14190(17) 0.16964(16) 0.0129(5) Uani 1 1 d . . . C1 C 0.5207(4) 0.3844(2) 0.1477(2) 0.0150(6) Uani 1 1 d . . . C2 C 0.4925(4) 0.4420(2) 0.2274(2) 0.0204(7) Uani 1 1 d . . . H2A H 0.5126 0.5076 0.2448 0.025 Uiso 1 1 calc R . . C3 C 0.4331(5) 0.3983(2) 0.2803(2) 0.0222(7) Uani 1 1 d . . . H3A H 0.4103 0.4341 0.3345 0.027 Uiso 1 1 calc R . . C4 C 0.4078(4) 0.3006(2) 0.2520(2) 0.0193(7) Uani 1 1 d . . . H4A H 0.3696 0.2704 0.2875 0.023 Uiso 1 1 calc R . . C5 C 0.4398(4) 0.2476(2) 0.1700(2) 0.0141(6) Uani 1 1 d . . . C6 C 0.4161(4) 0.1450(2) 0.1401(2) 0.0139(6) Uani 1 1 d . . . C7 C 0.3593(4) 0.0744(2) 0.0583(2) 0.0159(6) Uani 1 1 d . . . H7A H 0.3283 0.0828 0.0058 0.019 Uiso 1 1 calc R . . C8 C 0.3568(4) -0.0132(2) 0.0692(2) 0.0148(6) Uani 1 1 d . . . H8A H 0.3239 -0.0729 0.0250 0.018 Uiso 1 1 calc R . . C9 C 0.4112(4) 0.0054(2) 0.1563(2) 0.0137(6) Uani 1 1 d . . . C10 C 0.4257(4) -0.0561(2) 0.2069(2) 0.0136(6) Uani 1 1 d . . . C11 C 0.3878(4) -0.0260(2) 0.2907(2) 0.0142(6) Uani 1 1 d . . . H11A H 0.3558 0.0332 0.3147 0.017 Uiso 1 1 calc R . . C12 C 0.3979(4) -0.0840(2) 0.3384(2) 0.0171(6) Uani 1 1 d . . . H12A H 0.3740 -0.0642 0.3946 0.020 Uiso 1 1 calc R . . C13 C 0.4438(4) -0.1715(2) 0.3012(2) 0.0173(6) Uani 1 1 d . . . H13A H 0.4510 -0.2126 0.3310 0.021 Uiso 1 1 calc R . . C14 C 0.4787(4) -0.1958(2) 0.2178(2) 0.0143(6) Uani 1 1 d . . . C71 C 1.0509(4) 0.3641(2) -0.0032(2) 0.0193(7) Uani 1 1 d . . . Ag3 Ag 0.02388(3) 0.208909(16) 0.467736(15) 0.01772(6) Uani 1 1 d . . . Br5 Br 0.14690(4) 0.44724(2) 0.56351(2) 0.02074(8) Uani 1 1 d . . . Br6 Br 0.04377(5) -0.32163(2) 0.66370(2) 0.02724(9) Uani 1 1 d . . . N21 N 0.0315(3) 0.10908(17) 0.70559(17) 0.0144(5) Uani 1 1 d . . . H21A H -0.0128 0.1320 0.7515 0.017 Uiso 1 1 calc R . . N22 N 0.0443(3) -0.13663(17) 0.67873(16) 0.0123(5) Uani 1 1 d . . . N23 N 0.0785(3) 0.29471(17) 0.61320(16) 0.0131(5) Uani 1 1 d . . . C29 C 0.0446(4) -0.1916(2) 0.7260(2) 0.0155(6) Uani 1 1 d . . . C30 C 0.0454(4) -0.1618(2) 0.8144(2) 0.0209(7) Uani 1 1 d . . . H30A H 0.0420 -0.2041 0.8431 0.025 Uiso 1 1 calc R . . C31 C 0.0514(4) -0.0664(2) 0.8582(2) 0.0211(7) Uani 1 1 d . . . H31A H 0.0481 -0.0429 0.9176 0.025 Uiso 1 1 calc R . . C32 C 0.0623(4) -0.0057(2) 0.8136(2) 0.0208(7) Uani 1 1 d . . . H32A H 0.0722 0.0593 0.8433 0.025 Uiso 1 1 calc R . . C33 C 0.0583(4) -0.0423(2) 0.7237(2) 0.0132(6) Uani 1 1 d . . . C34 C 0.0751(4) 0.0209(2) 0.6754(2) 0.0133(6) Uani 1 1 d . . . C35 C 0.1448(4) 0.0108(2) 0.6013(2) 0.0149(6) Uani 1 1 d . . . H35A H 0.1860 -0.0421 0.5676 0.018 Uiso 1 1 calc R . . C36 C 0.1418(4) 0.0957(2) 0.5867(2) 0.0146(6) Uani 1 1 d . . . H36A H 0.1816 0.1091 0.5415 0.018 Uiso 1 1 calc R . . C37 C 0.0693(4) 0.1560(2) 0.6512(2) 0.0132(6) Uani 1 1 d . . . C38 C 0.0416(4) 0.2531(2) 0.6705(2) 0.0144(6) Uani 1 1 d . . . C39 C -0.0149(5) 0.3039(2) 0.7467(2) 0.0208(7) Uani 1 1 d . . . H39A H -0.0462 0.2739 0.7836 0.025 Uiso 1 1 calc R . . C40 C -0.0244(5) 0.3985(2) 0.7673(2) 0.0262(8) Uani 1 1 d . . . H40A H -0.0654 0.4321 0.8171 0.031 Uiso 1 1 calc R . . C41 C 0.0275(5) 0.4430(2) 0.7132(2) 0.0229(7) Uani 1 1 d . . . H41A H 0.0294 0.5076 0.7271 0.027 Uiso 1 1 calc R . . C42 C 0.0759(4) 0.3877(2) 0.6383(2) 0.0161(6) Uani 1 1 d . . . S3 S 0.55197(10) 0.20988(6) 0.46348(5) 0.01635(16) Uani 1 1 d . . . F7 F 0.7302(3) 0.38287(15) 0.52436(16) 0.0395(6) Uani 1 1 d . . . F8 F 0.5299(3) 0.36130(15) 0.59567(13) 0.0359(5) Uani 1 1 d . . . F9 F 0.4600(3) 0.37094(15) 0.46897(14) 0.0335(5) Uani 1 1 d . . . O7 O 0.3716(3) 0.17443(18) 0.45905(18) 0.0345(6) Uani 1 1 d . . . O8 O 0.5992(3) 0.19889(16) 0.38031(14) 0.0211(5) Uani 1 1 d . . . O9 O 0.6799(4) 0.18729(18) 0.52129(16) 0.0315(6) Uani 1 1 d . . . C73 C 0.5682(4) 0.3375(2) 0.5159(2) 0.0231(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02534(13) 0.01221(12) 0.01254(12) 0.00319(10) 0.00670(10) 0.00319(9) Br1 0.03002(18) 0.01234(16) 0.02013(17) 0.00716(14) 0.00969(14) 0.00087(13) Br2 0.03283(19) 0.01445(17) 0.02015(18) 0.00639(14) 0.00688(14) 0.01070(13) S1 0.0174(4) 0.0099(4) 0.0144(4) 0.0034(3) 0.0011(3) 0.0019(3) F1 0.0314(11) 0.0173(10) 0.0409(13) 0.0149(10) 0.0149(10) 0.0097(8) F2 0.0462(13) 0.0185(11) 0.0219(12) -0.0068(9) 0.0039(10) -0.0030(10) F3 0.0269(11) 0.0238(11) 0.0443(14) 0.0062(10) 0.0198(10) -0.0049(9) O1 0.0263(12) 0.0176(12) 0.0171(12) 0.0072(10) 0.0049(10) -0.0024(9) O2 0.0281(13) 0.0234(14) 0.0304(15) 0.0057(12) -0.0041(11) 0.0119(11) O3 0.0219(11) 0.0143(11) 0.0129(11) 0.0018(9) 0.0031(9) 0.0013(9) N1 0.0219(13) 0.0087(13) 0.0110(13) 0.0025(11) 0.0023(11) 0.0008(10) N2 0.0141(12) 0.0094(12) 0.0162(14) 0.0043(11) 0.0021(10) 0.0009(10) N3 0.0142(12) 0.0107(13) 0.0137(13) 0.0048(11) 0.0032(10) 0.0009(10) C1 0.0168(15) 0.0124(15) 0.0160(16) 0.0060(13) 0.0030(12) 0.0013(12) C2 0.0296(18) 0.0087(15) 0.0189(17) 0.0009(14) 0.0041(14) 0.0021(13) C3 0.0344(19) 0.0151(17) 0.0142(17) 0.0012(14) 0.0079(14) 0.0029(14) C4 0.0281(17) 0.0138(16) 0.0172(17) 0.0058(14) 0.0086(14) 0.0019(13) C5 0.0152(14) 0.0109(15) 0.0129(15) 0.0023(13) 0.0007(12) -0.0009(11) C6 0.0193(15) 0.0106(15) 0.0136(15) 0.0055(13) 0.0056(12) 0.0033(12) C7 0.0195(15) 0.0136(16) 0.0159(16) 0.0071(13) 0.0040(12) 0.0026(12) C8 0.0192(15) 0.0090(15) 0.0140(16) 0.0025(13) 0.0023(12) 0.0002(12) C9 0.0145(14) 0.0109(15) 0.0160(16) 0.0055(13) 0.0033(12) 0.0013(11) C10 0.0131(14) 0.0110(15) 0.0132(15) 0.0026(13) -0.0003(12) -0.0022(11) C11 0.0140(14) 0.0117(15) 0.0149(16) 0.0028(13) 0.0025(12) 0.0013(11) C12 0.0198(15) 0.0201(17) 0.0093(15) 0.0034(13) 0.0043(12) 0.0007(13) C13 0.0217(16) 0.0155(16) 0.0159(16) 0.0087(14) 0.0022(13) 0.0003(12) C14 0.0120(14) 0.0122(15) 0.0172(16) 0.0044(13) 0.0014(12) 0.0023(11) C71 0.0188(16) 0.0154(16) 0.0205(18) 0.0027(14) 0.0054(13) 0.0014(13) Ag3 0.02941(13) 0.01170(12) 0.01119(12) 0.00284(10) 0.00454(10) 0.00410(10) Br5 0.02881(17) 0.01413(16) 0.02304(18) 0.01025(14) 0.00815(14) 0.00375(13) Br6 0.0522(2) 0.00946(16) 0.02301(19) 0.00638(14) 0.01478(17) 0.00641(15) N21 0.0197(13) 0.0113(13) 0.0126(13) 0.0034(11) 0.0052(11) 0.0044(10) N22 0.0152(12) 0.0103(13) 0.0107(13) 0.0026(11) 0.0021(10) 0.0037(10) N23 0.0153(12) 0.0102(13) 0.0121(13) 0.0028(11) 0.0009(10) 0.0014(10) C29 0.0218(16) 0.0087(15) 0.0149(16) 0.0034(13) 0.0032(13) 0.0024(12) C30 0.0315(18) 0.0172(17) 0.0169(17) 0.0096(14) 0.0053(14) 0.0038(14) C31 0.0302(18) 0.0208(18) 0.0097(16) 0.0034(14) 0.0028(13) 0.0032(14) C32 0.0283(18) 0.0156(17) 0.0183(17) 0.0053(14) 0.0045(14) 0.0062(13) C33 0.0144(14) 0.0112(15) 0.0129(15) 0.0036(13) 0.0020(12) 0.0020(11) C34 0.0133(14) 0.0106(15) 0.0141(16) 0.0033(13) 0.0005(12) 0.0020(11) C35 0.0165(15) 0.0108(15) 0.0161(16) 0.0026(13) 0.0038(12) 0.0046(12) C36 0.0185(15) 0.0109(15) 0.0146(16) 0.0047(13) 0.0040(12) 0.0027(12) C37 0.0142(14) 0.0106(15) 0.0147(16) 0.0062(13) 0.0004(12) 0.0003(11) C38 0.0154(14) 0.0124(15) 0.0138(16) 0.0048(13) -0.0005(12) 0.0010(12) C39 0.0332(19) 0.0159(17) 0.0151(17) 0.0062(14) 0.0072(14) 0.0069(14) C40 0.047(2) 0.0192(18) 0.0173(18) 0.0072(15) 0.0135(16) 0.0135(16) C41 0.040(2) 0.0086(16) 0.0188(18) 0.0031(14) 0.0061(15) 0.0071(14) C42 0.0186(15) 0.0148(16) 0.0164(16) 0.0081(14) 0.0016(12) 0.0031(12) S3 0.0195(4) 0.0153(4) 0.0140(4) 0.0040(3) 0.0057(3) 0.0032(3) F7 0.0337(12) 0.0238(12) 0.0474(15) 0.0023(11) 0.0038(11) -0.0079(10) F8 0.0561(15) 0.0331(13) 0.0179(11) 0.0034(10) 0.0125(10) 0.0195(11) F9 0.0447(13) 0.0331(13) 0.0308(12) 0.0159(10) 0.0106(10) 0.0223(10) O7 0.0262(13) 0.0285(15) 0.0430(17) 0.0042(13) 0.0190(12) -0.0039(11) O8 0.0248(12) 0.0221(13) 0.0136(12) 0.0033(10) 0.0062(9) 0.0013(10) O9 0.0455(16) 0.0293(15) 0.0210(14) 0.0093(12) 0.0023(12) 0.0170(12) C73 0.0258(17) 0.0236(19) 0.0182(18) 0.0046(15) 0.0058(14) 0.0058(14) _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 N3 2.276(3) 2_655 ? Ag1 N2 2.282(3) . ? Br1 C1 1.894(3) . ? Br2 C14 1.893(3) . ? S1 O2 1.432(2) . ? S1 O1 1.443(2) . ? S1 O3 1.447(2) . ? S1 C71 1.821(3) . ? F1 C71 1.328(4) . ? F2 C71 1.329(4) . ? F3 C71 1.333(4) . ? N1 C9 1.373(4) . ? N1 C6 1.377(4) . ? N1 H1A 0.8600 . ? N2 C1 1.333(4) . ? N2 C5 1.362(4) . ? N3 C14 1.336(4) . ? N3 C10 1.355(4) . ? N3 Ag1 2.276(3) 2_655 ? C1 C2 1.374(4) . ? C2 C3 1.380(4) . ? C2 H2A 0.9300 . ? C3 C4 1.383(4) . ? C3 H3A 0.9300 . ? C4 C5 1.394(4) . ? C4 H4A 0.9300 . ? C5 C6 1.453(4) . ? C6 C7 1.380(4) . ? C7 C8 1.413(4) . ? C7 H7A 0.9300 . ? C8 C9 1.366(4) . ? C8 H8A 0.9300 . ? C9 C10 1.469(4) . ? C10 C11 1.393(4) . ? C11 C12 1.384(4) . ? C11 H11A 0.9300 . ? C12 C13 1.374(4) . ? C12 H12A 0.9300 . ? C13 C14 1.381(4) . ? C13 H13A 0.9300 . ? Ag3 N22 2.246(3) 2_556 ? Ag3 N23 2.260(3) . ? Br5 C42 1.889(3) . ? Br6 C29 1.892(3) . ? N21 C34 1.364(4) . ? N21 C37 1.382(4) . ? N21 H21A 0.8600 . ? N22 C29 1.338(4) . ? N22 C33 1.356(4) . ? N22 Ag3 2.246(3) 2_556 ? N23 C42 1.339(4) . ? N23 C38 1.364(4) . ? C29 C30 1.377(4) . ? C30 C31 1.377(5) . ? C30 H30A 0.9300 . ? C31 C32 1.381(4) . ? C31 H31A 0.9300 . ? C32 C33 1.395(4) . ? C32 H32A 0.9300 . ? C33 C34 1.465(4) . ? C34 C35 1.384(4) . ? C35 C36 1.406(4) . ? C35 H35A 0.9300 . ? C36 C37 1.384(4) . ? C36 H36A 0.9300 . ? C37 C38 1.455(4) . ? C38 C39 1.395(4) . ? C39 C40 1.380(4) . ? C39 H39A 0.9300 . ? C40 C41 1.383(4) . ? C40 H40A 0.9300 . ? C41 C42 1.371(4) . ? C41 H41A 0.9300 . ? S3 O7 1.435(2) . ? S3 O9 1.440(3) . ? S3 O8 1.440(2) . ? S3 C73 1.820(4) . ? F7 C73 1.339(4) . ? F8 C73 1.334(4) . ? F9 C73 1.329(4) . ? 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 N3 Ag1 N2 177.30(9) 2_655 . ? O2 S1 O1 115.42(15) . . ? O2 S1 O3 114.61(15) . . ? O1 S1 O3 114.50(14) . . ? O2 S1 C71 104.50(15) . . ? O1 S1 C71 102.38(14) . . ? O3 S1 C71 103.13(14) . . ? C9 N1 C6 109.3(2) . . ? C9 N1 H1A 125.3 . . ? C6 N1 H1A 125.3 . . ? C1 N2 C5 116.5(3) . . ? C1 N2 Ag1 117.88(19) . . ? C5 N2 Ag1 125.1(2) . . ? C14 N3 C10 116.2(3) . . ? C14 N3 Ag1 116.9(2) . 2_655 ? C10 N3 Ag1 125.8(2) . 2_655 ? N2 C1 C2 126.0(3) . . ? N2 C1 Br1 115.8(2) . . ? C2 C1 Br1 118.2(2) . . ? C1 C2 C3 117.0(3) . . ? C1 C2 H2A 121.5 . . ? C3 C2 H2A 121.5 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N2 C5 C4 121.3(3) . . ? N2 C5 C6 118.4(3) . . ? C4 C5 C6 120.3(3) . . ? N1 C6 C7 107.5(3) . . ? N1 C6 C5 120.0(3) . . ? C7 C6 C5 132.4(3) . . ? C6 C7 C8 107.3(3) . . ? C6 C7 H7A 126.3 . . ? C8 C7 H7A 126.3 . . ? C9 C8 C7 107.8(3) . . ? C9 C8 H8A 126.1 . . ? C7 C8 H8A 126.1 . . ? C8 C9 N1 108.0(3) . . ? C8 C9 C10 132.5(3) . . ? N1 C9 C10 119.3(3) . . ? N3 C10 C11 121.7(3) . . ? N3 C10 C9 118.8(3) . . ? C11 C10 C9 119.5(3) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C14 117.3(3) . . ? C12 C13 H13A 121.4 . . ? C14 C13 H13A 121.4 . . ? N3 C14 C13 125.9(3) . . ? N3 C14 Br2 116.3(2) . . ? C13 C14 Br2 117.8(2) . . ? F1 C71 F2 108.6(3) . . ? F1 C71 F3 107.1(3) . . ? F2 C71 F3 107.4(3) . . ? F1 C71 S1 111.3(2) . . ? F2 C71 S1 111.0(2) . . ? F3 C71 S1 111.4(2) . . ? N22 Ag3 N23 173.72(9) 2_556 . ? C34 N21 C37 109.7(2) . . ? C34 N21 H21A 125.2 . . ? C37 N21 H21A 125.2 . . ? C29 N22 C33 116.5(3) . . ? C29 N22 Ag3 117.4(2) . 2_556 ? C33 N22 Ag3 125.23(19) . 2_556 ? C42 N23 C38 116.8(3) . . ? C42 N23 Ag3 117.3(2) . . ? C38 N23 Ag3 120.4(2) . . ? N22 C29 C30 125.9(3) . . ? N22 C29 Br6 115.9(2) . . ? C30 C29 Br6 118.2(2) . . ? C31 C30 C29 116.8(3) . . ? C31 C30 H30A 121.6 . . ? C29 C30 H30A 121.6 . . ? C30 C31 C32 119.7(3) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C31 C32 C33 119.6(3) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? N22 C33 C32 121.4(3) . . ? N22 C33 C34 118.0(3) . . ? C32 C33 C34 120.5(3) . . ? N21 C34 C35 108.1(3) . . ? N21 C34 C33 121.2(3) . . ? C35 C34 C33 130.5(3) . . ? C34 C35 C36 107.2(3) . . ? C34 C35 H35A 126.4 . . ? C36 C35 H35A 126.4 . . ? C37 C36 C35 108.1(3) . . ? C37 C36 H36A 125.9 . . ? C35 C36 H36A 125.9 . . ? N21 C37 C36 107.0(3) . . ? N21 C37 C38 120.9(3) . . ? C36 C37 C38 132.0(3) . . ? N23 C38 C39 120.6(3) . . ? N23 C38 C37 118.0(3) . . ? C39 C38 C37 121.4(3) . . ? C40 C39 C38 120.1(3) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C41 119.4(3) . . ? C39 C40 H40A 120.3 . . ? C41 C40 H40A 120.3 . . ? C42 C41 C40 116.9(3) . . ? C42 C41 H41A 121.5 . . ? C40 C41 H41A 121.5 . . ? N23 C42 C41 125.8(3) . . ? N23 C42 Br5 116.7(2) . . ? C41 C42 Br5 117.6(2) . . ? O7 S3 O9 115.93(17) . . ? O7 S3 O8 115.06(16) . . ? O9 S3 O8 113.71(15) . . ? O7 S3 C73 103.36(16) . . ? O9 S3 C73 103.57(16) . . ? O8 S3 C73 102.86(15) . . ? F9 C73 F8 108.3(3) . . ? F9 C73 F7 106.4(3) . . ? F8 C73 F7 107.7(3) . . ? F9 C73 S3 111.4(2) . . ? F8 C73 S3 111.2(2) . . ? F7 C73 S3 111.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ag1 N2 C1 -27.6(19) 2_655 . . . ? N3 Ag1 N2 C5 143.8(17) 2_655 . . . ? C5 N2 C1 C2 -1.2(5) . . . . ? Ag1 N2 C1 C2 170.9(3) . . . . ? C5 N2 C1 Br1 177.7(2) . . . . ? Ag1 N2 C1 Br1 -10.2(3) . . . . ? N2 C1 C2 C3 0.1(5) . . . . ? Br1 C1 C2 C3 -178.7(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C1 N2 C5 C4 1.1(4) . . . . ? Ag1 N2 C5 C4 -170.4(2) . . . . ? C1 N2 C5 C6 -178.1(3) . . . . ? Ag1 N2 C5 C6 10.4(4) . . . . ? C3 C4 C5 N2 -0.1(5) . . . . ? C3 C4 C5 C6 179.1(3) . . . . ? C9 N1 C6 C7 1.2(3) . . . . ? C9 N1 C6 C5 178.7(3) . . . . ? N2 C5 C6 N1 148.0(3) . . . . ? C4 C5 C6 N1 -31.2(4) . . . . ? N2 C5 C6 C7 -35.2(5) . . . . ? C4 C5 C6 C7 145.6(3) . . . . ? N1 C6 C7 C8 -0.8(3) . . . . ? C5 C6 C7 C8 -177.9(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 N1 0.6(3) . . . . ? C7 C8 C9 C10 176.0(3) . . . . ? C6 N1 C9 C8 -1.2(3) . . . . ? C6 N1 C9 C10 -177.2(3) . . . . ? C14 N3 C10 C11 0.2(4) . . . . ? Ag1 N3 C10 C11 167.4(2) 2_655 . . . ? C14 N3 C10 C9 -178.3(3) . . . . ? Ag1 N3 C10 C9 -11.1(4) 2_655 . . . ? C8 C9 C10 N3 35.0(5) . . . . ? N1 C9 C10 N3 -150.0(3) . . . . ? C8 C9 C10 C11 -143.6(3) . . . . ? N1 C9 C10 C11 31.4(4) . . . . ? N3 C10 C11 C12 0.3(4) . . . . ? C9 C10 C11 C12 178.8(3) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C10 N3 C14 C13 -0.4(4) . . . . ? Ag1 N3 C14 C13 -168.8(2) 2_655 . . . ? C10 N3 C14 Br2 179.0(2) . . . . ? Ag1 N3 C14 Br2 10.6(3) 2_655 . . . ? C12 C13 C14 N3 0.0(5) . . . . ? C12 C13 C14 Br2 -179.4(2) . . . . ? O2 S1 C71 F1 174.1(2) . . . . ? O1 S1 C71 F1 -65.1(2) . . . . ? O3 S1 C71 F1 54.0(2) . . . . ? O2 S1 C71 F2 -64.8(3) . . . . ? O1 S1 C71 F2 55.9(3) . . . . ? O3 S1 C71 F2 175.0(2) . . . . ? O2 S1 C71 F3 54.8(3) . . . . ? O1 S1 C71 F3 175.5(2) . . . . ? O3 S1 C71 F3 -65.4(3) . . . . ? N22 Ag3 N23 C42 -20.2(9) 2_556 . . . ? N22 Ag3 N23 C38 132.7(7) 2_556 . . . ? C33 N22 C29 C30 4.8(5) . . . . ? Ag3 N22 C29 C30 -165.2(3) 2_556 . . . ? C33 N22 C29 Br6 -175.2(2) . . . . ? Ag3 N22 C29 Br6 14.8(3) 2_556 . . . ? N22 C29 C30 C31 -1.9(5) . . . . ? Br6 C29 C30 C31 178.1(2) . . . . ? C29 C30 C31 C32 -2.2(5) . . . . ? C30 C31 C32 C33 3.2(5) . . . . ? C29 N22 C33 C32 -3.7(4) . . . . ? Ag3 N22 C33 C32 165.5(2) 2_556 . . . ? C29 N22 C33 C34 174.4(3) . . . . ? Ag3 N22 C33 C34 -16.4(4) 2_556 . . . ? C31 C32 C33 N22 -0.1(5) . . . . ? C31 C32 C33 C34 -178.2(3) . . . . ? C37 N21 C34 C35 1.0(3) . . . . ? C37 N21 C34 C33 176.4(3) . . . . ? N22 C33 C34 N21 157.7(3) . . . . ? C32 C33 C34 N21 -24.2(4) . . . . ? N22 C33 C34 C35 -28.1(5) . . . . ? C32 C33 C34 C35 150.0(3) . . . . ? N21 C34 C35 C36 -0.3(3) . . . . ? C33 C34 C35 C36 -175.1(3) . . . . ? C34 C35 C36 C37 -0.5(4) . . . . ? C34 N21 C37 C36 -1.3(3) . . . . ? C34 N21 C37 C38 -177.6(3) . . . . ? C35 C36 C37 N21 1.1(3) . . . . ? C35 C36 C37 C38 176.8(3) . . . . ? C42 N23 C38 C39 6.9(4) . . . . ? Ag3 N23 C38 C39 -146.1(2) . . . . ? C42 N23 C38 C37 -170.9(3) . . . . ? Ag3 N23 C38 C37 36.1(3) . . . . ? N21 C37 C38 N23 -178.8(3) . . . . ? C36 C37 C38 N23 6.0(5) . . . . ? N21 C37 C38 C39 3.4(5) . . . . ? C36 C37 C38 C39 -171.8(3) . . . . ? N23 C38 C39 C40 -3.7(5) . . . . ? C37 C38 C39 C40 174.0(3) . . . . ? C38 C39 C40 C41 -1.9(6) . . . . ? C39 C40 C41 C42 3.9(5) . . . . ? C38 N23 C42 C41 -5.0(5) . . . . ? Ag3 N23 C42 C41 148.9(3) . . . . ? C38 N23 C42 Br5 174.6(2) . . . . ? Ag3 N23 C42 Br5 -31.5(3) . . . . ? C40 C41 C42 N23 -0.5(5) . . . . ? C40 C41 C42 Br5 179.9(3) . . . . ? O7 S3 C73 F9 -60.4(3) . . . . ? O9 S3 C73 F9 178.3(2) . . . . ? O8 S3 C73 F9 59.7(3) . . . . ? O7 S3 C73 F8 60.6(3) . . . . ? O9 S3 C73 F8 -60.7(3) . . . . ? O8 S3 C73 F8 -179.3(2) . . . . ? O7 S3 C73 F7 -179.1(2) . . . . ? O9 S3 C73 F7 59.6(3) . . . . ? O8 S3 C73 F7 -59.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.888 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 963079'