# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Ag N8, F6 P' _chemical_formula_sum 'C28 H24 Ag F6 N8 P' _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _diffrn_ambient_temperature 294(2) _chemical_formula_weight 725.39 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.303(3) _cell_length_b 7.6263(16) _cell_length_c 15.344(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.767(4) _cell_angle_gamma 90.00 _cell_volume 1705.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3684 _cell_measurement_theta_min 2.692 _cell_measurement_theta_max 26.012 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9369 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.18 _reflns_number_total 3381 _reflns_number_gt 2298 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3381 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1911 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Ag Ag 0.5000 0.0000 0.5000 0.0771(3) Uani 1 2 d S . . P P 1.0000 0.0000 1.0000 0.1085(12) Uani 1 2 d S . . F1 F 0.9100(3) -0.0393(7) 1.0167(6) 0.158(2) Uani 1 1 d . . . F2 F 0.9546(4) -0.0620(10) 0.8966(6) 0.199(4) Uani 1 1 d . . . F3 F 0.9601(5) 0.1867(8) 0.9736(5) 0.173(2) Uani 1 1 d . . . N1 N 0.6028(3) 0.0106(3) 0.6323(3) 0.0531(8) Uani 1 1 d . . . N2 N 0.7689(2) 0.3127(4) 1.0212(2) 0.0543(8) Uani 1 1 d . . . H2A H 0.8174 0.3364 1.0656 0.065 Uiso 1 1 calc R . . N3 N 0.6110(3) 0.5953(5) 0.7404(3) 0.0793(11) Uani 1 1 d . . . N4 N 0.5680(3) -0.1751(5) 0.9606(3) 0.0862(13) Uani 1 1 d . . . C1 C 0.5854(2) 0.0986(4) 0.7020(2) 0.0468(8) Uani 1 1 d . . . H1A H 0.5295 0.1564 0.6906 0.056 Uiso 1 1 calc R . . C2 C 0.6466(2) 0.1061(4) 0.7885(2) 0.0407(7) Uani 1 1 d . . . C3 C 0.7306(3) 0.0240(4) 0.8046(3) 0.0510(9) Uani 1 1 d . . . H3A H 0.7741 0.0282 0.8621 0.061 Uiso 1 1 calc R . . C4 C 0.7485(3) -0.0648(6) 0.7331(3) 0.0595(10) Uani 1 1 d . . . H4A H 0.8047 -0.1201 0.7416 0.071 Uiso 1 1 calc R . . C5 C 0.6825(3) -0.0696(6) 0.6499(3) 0.0602(10) Uani 1 1 d . . . H5A H 0.6944 -0.1331 0.6030 0.072 Uiso 1 1 calc R . . C6 C 0.6225(2) 0.2082(4) 0.8638(2) 0.0423(7) Uani 1 1 d . . . H6A H 0.5560 0.2272 0.8449 0.051 Uiso 1 1 calc R . . C7 C 0.6703(2) 0.3862(4) 0.8762(3) 0.0475(8) Uani 1 1 d . . . C8 C 0.7430(3) 0.4261(5) 0.9485(3) 0.0515(8) Uani 1 1 d . . . C9 C 0.7213(2) 0.1643(4) 1.0261(2) 0.0488(8) Uani 1 1 d . . . C10 C 0.6504(2) 0.1140(4) 0.9540(2) 0.0461(8) Uani 1 1 d . . . C11 C 0.6396(3) 0.5058(4) 0.8011(4) 0.0555(10) Uani 1 1 d . . . C12 C 0.7992(3) 0.5891(6) 0.9563(4) 0.0726(12) Uani 1 1 d . . . H12A H 0.7627 0.6794 0.9187 0.109 Uiso 1 1 calc R . . H12B H 0.8516 0.5653 0.9362 0.109 Uiso 1 1 calc R . . H12C H 0.8193 0.6272 1.0189 0.109 Uiso 1 1 calc R . . C13 C 0.7527(3) 0.0692(7) 1.1158(3) 0.0689(11) Uani 1 1 d . . . H13A H 0.7109 -0.0247 1.1158 0.103 Uiso 1 1 calc R . . H13B H 0.7543 0.1492 1.1646 0.103 Uiso 1 1 calc R . . H13C H 0.8130 0.0223 1.1246 0.103 Uiso 1 1 calc R . . C14 C 0.6034(3) -0.0452(5) 0.9597(3) 0.0565(10) 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 Ag 0.1035(5) 0.0872(5) 0.0329(3) -0.00508(18) 0.0092(3) -0.0163(3) P 0.0571(10) 0.0844(15) 0.175(4) -0.0291(14) 0.0222(15) -0.0072(9) F1 0.091(3) 0.159(4) 0.226(7) -0.031(4) 0.051(4) -0.015(2) F2 0.121(4) 0.206(5) 0.227(8) -0.093(6) -0.009(4) 0.043(4) F3 0.193(4) 0.134(4) 0.204(5) 0.021(4) 0.079(4) 0.062(4) N1 0.077(2) 0.0451(16) 0.0380(18) -0.0013(11) 0.0185(17) 0.0001(14) N2 0.0606(17) 0.0552(17) 0.0429(16) -0.0057(14) 0.0094(14) -0.0108(14) N3 0.092(3) 0.063(2) 0.085(3) 0.023(2) 0.030(2) 0.008(2) N4 0.114(3) 0.071(2) 0.066(2) 0.0056(19) 0.015(2) -0.041(2) C1 0.0572(18) 0.0418(17) 0.0400(17) 0.0012(14) 0.0129(15) 0.0003(14) C2 0.0535(17) 0.0341(15) 0.0353(16) 0.0022(12) 0.0148(13) -0.0006(13) C3 0.057(2) 0.053(2) 0.041(2) 0.0022(14) 0.0127(17) 0.0080(15) C4 0.071(2) 0.058(2) 0.056(2) 0.003(2) 0.029(2) 0.0139(19) C5 0.093(3) 0.0466(19) 0.050(2) -0.0010(18) 0.035(2) 0.006(2) C6 0.0480(16) 0.0395(16) 0.0413(18) -0.0010(13) 0.0163(14) -0.0024(13) C7 0.0582(19) 0.0369(16) 0.053(2) -0.0005(14) 0.0248(17) -0.0015(14) C8 0.062(2) 0.0422(17) 0.056(2) -0.0044(17) 0.0261(18) -0.0076(16) C9 0.065(2) 0.0446(17) 0.0376(17) -0.0018(14) 0.0166(15) -0.0024(15) C10 0.0590(19) 0.0406(16) 0.0438(18) -0.0019(14) 0.0232(16) -0.0055(14) C11 0.067(2) 0.044(2) 0.061(3) 0.0034(17) 0.028(2) 0.0019(16) C12 0.085(3) 0.057(2) 0.082(3) -0.008(2) 0.033(3) -0.025(2) C13 0.091(3) 0.073(2) 0.041(2) 0.002(2) 0.018(2) -0.009(2) C14 0.075(2) 0.0503(19) 0.042(2) 0.0002(16) 0.0144(19) -0.0151(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.158(4) . ? Ag N1 2.158(4) 3_656 ? P F1 1.506(5) . ? P F1 1.506(5) 3_757 ? P F3 1.554(5) 3_757 ? P F3 1.554(5) . ? P F2 1.597(7) . ? P F2 1.597(7) 3_757 ? N1 C5 1.317(6) . ? N1 C1 1.354(5) . ? N2 C9 1.360(5) . ? N2 C8 1.371(5) . ? N2 H2A 0.8600 . ? N3 C11 1.130(6) . ? N4 C14 1.132(5) . ? C1 C2 1.373(5) . ? C1 H1A 0.9300 . ? C2 C3 1.382(5) . ? C2 C6 1.528(5) . ? C3 C4 1.386(6) . ? C3 H3A 0.9300 . ? C4 C5 1.366(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C10 1.502(5) . ? C6 C7 1.526(4) . ? C6 H6A 0.9800 . ? C7 C8 1.344(5) . ? C7 C11 1.432(6) . ? C8 C12 1.495(6) . ? C9 C10 1.348(5) . ? C9 C13 1.500(5) . ? C10 C14 1.427(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 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 N1 Ag N1 180 . 3_656 ? F1 P F1 180 . 3_757 ? F1 P F3 94.6(3) . 3_757 ? F1 P F3 85.4(3) 3_757 3_757 ? F1 P F3 85.4(3) . . ? F1 P F3 94.6(3) 3_757 . ? F3 P F3 180 3_757 . ? F1 P F2 88.1(4) . . ? F1 P F2 91.9(4) 3_757 . ? F3 P F2 90.3(3) 3_757 . ? F3 P F2 89.7(3) . . ? F1 P F2 91.9(4) . 3_757 ? F1 P F2 88.1(4) 3_757 3_757 ? F3 P F2 89.7(3) 3_757 3_757 ? F3 P F2 90.3(3) . 3_757 ? F2 P F2 180 . 3_757 ? C5 N1 C1 117.5(4) . . ? C5 N1 Ag 122.6(3) . . ? C1 N1 Ag 119.9(3) . . ? C9 N2 C8 122.9(3) . . ? C9 N2 H2A 118.6 . . ? C8 N2 H2A 118.6 . . ? N1 C1 C2 122.9(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 118.4(3) . . ? C1 C2 C6 120.1(3) . . ? C3 C2 C6 121.5(3) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 118.9(4) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? C10 C6 C7 108.7(3) . . ? C10 C6 C2 112.8(3) . . ? C7 C6 C2 109.3(3) . . ? C10 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C2 C6 H6A 108.7 . . ? C8 C7 C11 120.3(3) . . ? C8 C7 C6 123.3(3) . . ? C11 C7 C6 116.0(3) . . ? C7 C8 N2 119.3(3) . . ? C7 C8 C12 124.4(4) . . ? N2 C8 C12 116.3(4) . . ? C10 C9 N2 120.2(3) . . ? C10 C9 C13 124.6(3) . . ? N2 C9 C13 115.2(3) . . ? C9 C10 C14 119.1(3) . . ? C9 C10 C6 123.4(3) . . ? C14 C10 C6 117.2(3) . . ? N3 C11 C7 176.2(5) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 176.2(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.18 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.756 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 966505' ####################################################################### # # 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_formula_moiety '2(C28 H24 Ag N8), F6 P' _chemical_formula_sum 'C56 H48 Ag2 F6 N16 P' _chemical_melting_point ? _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _diffrn_ambient_temperature 150(2) _chemical_formula_weight 1305.81 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0792(4) _cell_length_b 11.0233(5) _cell_length_c 14.1410(7) _cell_angle_alpha 97.122(2) _cell_angle_beta 101.625(2) _cell_angle_gamma 92.199(2) _cell_volume 1372.62(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.4604 _cell_measurement_theta_max 26.3948 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 659 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7098 _exptl_absorpt_correction_T_max 0.8535 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 25919 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5608 _reflns_number_gt 5314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006)' _computing_data_reduction 'SAINT V7.34A (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 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^)+(0.0457P)^2^+0.9271P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5608 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 Ag Ag 0.266749(15) 0.162349(13) 0.336969(10) 0.02258(7) Uani 1 1 d . . . N1 N 0.03755(18) 0.21542(15) 0.26525(12) 0.0193(3) Uani 1 1 d . . . N2 N 0.68654(19) -0.17517(16) 0.08678(12) 0.0197(3) Uani 1 1 d . . . H2A H 0.683(3) -0.251(3) 0.0878(19) 0.027(6) Uiso 1 1 d . . . N3 N 0.4475(2) 0.14026(18) 0.24891(14) 0.0287(4) Uani 1 1 d . . . N4 N 0.8505(2) 0.08894(18) -0.12122(14) 0.0298(4) Uani 1 1 d . . . N5 N 0.2686(2) 0.01807(16) 0.43927(13) 0.0250(4) Uani 1 1 d . . . N6 N 0.6774(2) 0.44985(16) 0.76938(13) 0.0217(3) Uani 1 1 d . . . H6A H 0.651(3) 0.479(2) 0.818(2) 0.028(7) Uiso 1 1 d . . . N7 N 0.3905(2) 0.33518(17) 0.44801(13) 0.0293(4) Uani 1 1 d . . . N8 N 1.1133(2) 0.2541(2) 0.69940(18) 0.0486(6) Uani 1 1 d . . . C1 C -0.0665(2) 0.13893(17) 0.20255(14) 0.0171(4) Uani 1 1 d . . . H1A H -0.0491 0.0542 0.1938 0.020 Uiso 1 1 calc R . . C2 C 0.0108(2) 0.33427(18) 0.27826(16) 0.0241(4) Uani 1 1 d . . . H2B H 0.0830 0.3890 0.3231 0.029 Uiso 1 1 calc R . . C3 C -0.1174(2) 0.38060(19) 0.22928(18) 0.0290(5) Uani 1 1 d . . . H3B H -0.1326 0.4655 0.2401 0.035 Uiso 1 1 calc R . . C4 C -0.2234(2) 0.30151(18) 0.16411(16) 0.0236(4) Uani 1 1 d . . . H4A H -0.3122 0.3316 0.1294 0.028 Uiso 1 1 calc R . . C5 C -0.1984(2) 0.17788(17) 0.15000(13) 0.0161(3) Uani 1 1 d . . . C6 C 0.6835(2) 0.08704(17) 0.08241(13) 0.0165(4) Uani 1 1 d . . . H6C H 0.6153 0.1368 0.0456 0.020 Uiso 1 1 d R . . C7 C 0.6008(2) 0.01469(18) 0.14252(14) 0.0179(4) Uani 1 1 d . . . C8 C 0.6082(2) -0.10762(18) 0.14546(13) 0.0178(4) Uani 1 1 d . . . C9 C 0.7511(2) -0.12515(18) 0.01927(13) 0.0175(4) Uani 1 1 d . . . C10 C 0.7490(2) -0.00310(18) 0.01389(13) 0.0175(4) Uani 1 1 d . . . C11 C 0.5146(2) 0.08257(18) 0.20158(15) 0.0210(4) Uani 1 1 d . . . C12 C 0.5323(2) -0.17780(19) 0.20834(15) 0.0233(4) Uani 1 1 d . . . H12A H 0.4795 -0.1216 0.2472 0.035 Uiso 1 1 calc R . . H12B H 0.6080 -0.2173 0.2518 0.035 Uiso 1 1 calc R . . H12C H 0.4597 -0.2404 0.1671 0.035 Uiso 1 1 calc R . . C13 C 0.8193(2) -0.21407(18) -0.04553(15) 0.0224(4) Uani 1 1 d . . . H13A H 0.8622 -0.1703 -0.0910 0.034 Uiso 1 1 calc R . . H13B H 0.7414 -0.2758 -0.0823 0.034 Uiso 1 1 calc R . . H13C H 0.8990 -0.2544 -0.0058 0.034 Uiso 1 1 calc R . . C14 C 0.8075(2) 0.04587(18) -0.06115(14) 0.0207(4) Uani 1 1 d . . . C15 C 0.2703(2) -0.10001(19) 0.40344(15) 0.0239(4) Uani 1 1 d . . . H15A H 0.2868 -0.1190 0.3392 0.029 Uiso 1 1 calc R . . C16 C 0.2442(3) 0.0439(2) 0.52985(16) 0.0292(5) Uani 1 1 d . . . H16A H 0.2421 0.1273 0.5561 0.035 Uiso 1 1 calc R . . C17 C 0.2222(3) -0.0454(2) 0.58613(16) 0.0341(5) Uani 1 1 d . . . H17A H 0.2057 -0.0237 0.6501 0.041 Uiso 1 1 calc R . . C18 C 0.2245(3) -0.1672(2) 0.54881(16) 0.0292(5) Uani 1 1 d . . . H18A H 0.2094 -0.2301 0.5868 0.035 Uiso 1 1 calc R . . C19 C 0.2491(2) -0.19649(18) 0.45517(15) 0.0207(4) Uani 1 1 d . . . C20 C 0.7550(2) 0.32832(17) 0.59361(14) 0.0203(4) Uani 1 1 d . . . H20A H 0.7986 0.3832 0.5536 0.024 Uiso 1 1 calc R . . C21 C 0.5996(2) 0.36961(17) 0.60293(14) 0.0194(4) Uani 1 1 d . . . C22 C 0.5689(2) 0.43049(17) 0.68522(14) 0.0193(4) Uani 1 1 d . . . C23 C 0.8151(2) 0.40084(18) 0.77610(15) 0.0209(4) Uani 1 1 d . . . C24 C 0.8553(2) 0.34419(18) 0.69584(15) 0.0219(4) Uani 1 1 d . . . C25 C 0.4833(2) 0.35079(17) 0.51747(15) 0.0221(4) Uani 1 1 d . . . C26 C 0.4213(2) 0.4825(2) 0.69248(15) 0.0261(4) Uani 1 1 d . . . H26A H 0.3513 0.4645 0.6292 0.039 Uiso 1 1 calc R . . H26B H 0.4365 0.5714 0.7112 0.039 Uiso 1 1 calc R . . H26C H 0.3793 0.4456 0.7417 0.039 Uiso 1 1 calc R . . C27 C 0.9118(2) 0.4163(2) 0.87666(16) 0.0284(4) Uani 1 1 d . . . H27A H 1.0077 0.3792 0.8746 0.043 Uiso 1 1 calc R . . H27B H 0.8598 0.3761 0.9199 0.043 Uiso 1 1 calc R . . H27C H 0.9312 0.5038 0.9012 0.043 Uiso 1 1 calc R . . C28 C 0.9996(2) 0.2948(2) 0.70149(17) 0.0302(5) Uani 1 1 d . . . P P 0.5000 0.5000 0.0000 0.02057(15) Uani 1 2 d S . . F1 F 0.45126(14) 0.42229(11) 0.08659(8) 0.0237(2) Uani 1 1 d . . . F2 F 0.34727(13) 0.43162(11) -0.08232(8) 0.0234(2) Uani 1 1 d . . . F3 F 0.39666(14) 0.61483(11) 0.03241(9) 0.0249(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01986(10) 0.02387(10) 0.02240(10) 0.00029(6) 0.00218(6) 0.00198(6) N1 0.0177(8) 0.0196(8) 0.0199(8) -0.0002(6) 0.0042(6) 0.0008(6) N2 0.0220(8) 0.0166(8) 0.0215(8) 0.0016(6) 0.0072(6) 0.0019(6) N3 0.0266(9) 0.0303(10) 0.0302(10) -0.0027(8) 0.0119(8) 0.0028(7) N4 0.0328(10) 0.0302(10) 0.0300(10) 0.0072(8) 0.0133(8) 0.0015(8) N5 0.0327(9) 0.0199(8) 0.0227(9) 0.0003(7) 0.0075(7) 0.0031(7) N6 0.0235(8) 0.0263(9) 0.0154(8) 0.0001(7) 0.0055(7) 0.0046(7) N7 0.0356(10) 0.0234(9) 0.0239(9) -0.0038(7) -0.0009(8) -0.0014(7) N8 0.0271(11) 0.0590(15) 0.0506(14) -0.0184(11) 0.0007(9) 0.0119(10) C1 0.0185(9) 0.0148(8) 0.0186(9) 0.0013(7) 0.0062(7) 0.0013(7) C2 0.0201(9) 0.0191(9) 0.0306(11) -0.0024(8) 0.0036(8) -0.0023(7) C3 0.0271(11) 0.0143(9) 0.0437(13) -0.0004(8) 0.0051(9) 0.0031(8) C4 0.0198(9) 0.0198(9) 0.0307(11) 0.0053(8) 0.0026(8) 0.0047(7) C5 0.0153(8) 0.0183(9) 0.0153(8) 0.0021(7) 0.0048(7) 0.0003(7) C6 0.0136(8) 0.0179(9) 0.0169(9) 0.0014(7) 0.0008(7) 0.0026(7) C7 0.0135(8) 0.0213(9) 0.0174(9) -0.0026(7) 0.0034(7) -0.0007(7) C8 0.0124(8) 0.0235(9) 0.0158(9) -0.0001(7) 0.0009(7) -0.0006(7) C9 0.0142(8) 0.0214(9) 0.0157(9) 0.0006(7) 0.0018(7) 0.0009(7) C10 0.0153(8) 0.0216(9) 0.0146(9) 0.0004(7) 0.0023(7) 0.0008(7) C11 0.0163(9) 0.0227(9) 0.0225(10) 0.0002(8) 0.0023(7) -0.0018(7) C12 0.0229(10) 0.0240(10) 0.0241(10) 0.0022(8) 0.0086(8) -0.0014(8) C13 0.0228(9) 0.0216(10) 0.0235(10) -0.0007(8) 0.0089(8) 0.0017(7) C14 0.0187(9) 0.0205(9) 0.0213(10) -0.0014(7) 0.0027(7) 0.0015(7) C15 0.0308(11) 0.0215(10) 0.0208(10) -0.0003(8) 0.0103(8) 0.0014(8) C16 0.0404(12) 0.0222(10) 0.0229(10) -0.0045(8) 0.0058(9) 0.0052(9) C17 0.0536(15) 0.0322(12) 0.0169(10) -0.0028(9) 0.0109(10) 0.0057(10) C18 0.0430(13) 0.0263(11) 0.0199(10) 0.0048(8) 0.0090(9) 0.0036(9) C19 0.0217(9) 0.0198(9) 0.0201(10) -0.0001(7) 0.0045(7) 0.0034(7) C20 0.0249(10) 0.0176(9) 0.0194(9) 0.0008(7) 0.0080(8) 0.0010(7) C21 0.0224(9) 0.0163(9) 0.0188(9) 0.0020(7) 0.0028(7) 0.0014(7) C22 0.0213(9) 0.0180(9) 0.0187(9) 0.0043(7) 0.0035(7) 0.0011(7) C23 0.0210(9) 0.0186(9) 0.0224(10) 0.0026(7) 0.0037(8) -0.0012(7) C24 0.0204(9) 0.0188(9) 0.0252(10) -0.0015(7) 0.0043(8) -0.0002(7) C25 0.0291(10) 0.0150(9) 0.0224(10) 0.0011(7) 0.0071(9) 0.0010(7) C26 0.0234(10) 0.0313(11) 0.0229(10) 0.0017(8) 0.0036(8) 0.0073(8) C27 0.0271(11) 0.0321(11) 0.0231(10) 0.0006(8) 0.0003(8) 0.0020(9) C28 0.0234(11) 0.0316(11) 0.0303(11) -0.0097(9) 0.0019(8) 0.0010(9) P 0.0229(3) 0.0197(3) 0.0186(3) 0.0002(3) 0.0043(3) 0.0028(3) F1 0.0279(6) 0.0236(6) 0.0205(6) 0.0040(5) 0.0068(5) 0.0010(5) F2 0.0230(6) 0.0223(6) 0.0217(6) 0.0003(4) -0.0007(4) -0.0002(4) F3 0.0283(6) 0.0232(6) 0.0231(6) -0.0010(5) 0.0064(5) 0.0090(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 Ag N1 2.2564(16) . ? Ag N3 2.2547(18) . ? Ag N5 2.2771(18) . ? Ag N7 2.3960(18) . ? N1 C2 1.339(3) . ? N1 C1 1.344(2) . ? N2 C8 1.369(2) . ? N2 C9 1.375(3) . ? N2 H2A 0.84(3) . ? N3 C11 1.145(3) . ? N4 C14 1.149(3) . ? N5 C16 1.342(3) . ? N5 C15 1.339(3) . ? N6 C23 1.372(3) . ? N6 C22 1.371(3) . ? N6 H6A 0.81(3) . ? N7 C25 1.148(3) . ? N8 C28 1.146(3) . ? C1 C5 1.389(3) . ? C1 H1A 0.9500 . ? C2 C3 1.379(3) . ? C2 H2B 0.9500 . ? C3 C4 1.384(3) . ? C3 H3B 0.9500 . ? C4 C5 1.387(3) . ? C4 H4A 0.9500 . ? C5 C6 1.528(2) 1_455 ? C6 C7 1.517(3) . ? C6 C10 1.522(3) . ? C6 C5 1.528(2) 1_655 ? C6 H6C 0.9600 . ? C7 C8 1.358(3) . ? C7 C11 1.423(3) . ? C8 C12 1.497(3) . ? C9 C10 1.358(3) . ? C9 C13 1.495(3) . ? C10 C14 1.431(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C19 1.392(3) . ? C15 H15A 0.9500 . ? C16 C17 1.374(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 C19 1.388(3) . ? C18 H18A 0.9500 . ? C19 C20 1.525(3) 2_656 ? C20 C19 1.525(3) 2_656 ? C20 C21 1.525(3) . ? C20 C24 1.531(3) . ? C20 H20A 1.0000 . ? C21 C22 1.354(3) . ? C21 C25 1.423(3) . ? C22 C26 1.495(3) . ? C23 C24 1.349(3) . ? C23 C27 1.499(3) . ? C24 C28 1.429(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? P F3 1.6772(11) 2_665 ? P F3 1.6773(11) . ? P F1 1.6965(11) 2_665 ? P F1 1.6965(11) . ? P F2 1.7023(11) 2_665 ? P F2 1.7023(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N3 119.16(7) . . ? N1 Ag N5 116.03(6) . . ? N3 Ag N5 112.47(7) . . ? N1 Ag N7 108.06(6) . . ? N3 Ag N7 96.16(7) . . ? N5 Ag N7 100.96(6) . . ? C2 N1 C1 117.98(17) . . ? C2 N1 Ag 117.06(13) . . ? C1 N1 Ag 124.55(13) . . ? C8 N2 C9 122.22(17) . . ? C8 N2 H2A 116.9(18) . . ? C9 N2 H2A 120.3(18) . . ? C11 N3 Ag 152.44(17) . . ? C16 N5 C15 117.76(18) . . ? C16 N5 Ag 122.55(14) . . ? C15 N5 Ag 118.84(14) . . ? C23 N6 C22 122.04(18) . . ? C23 N6 H6A 120.4(19) . . ? C22 N6 H6A 116.4(19) . . ? C25 N7 Ag 136.45(16) . . ? N1 C1 C5 123.08(17) . . ? N1 C1 H1A 118.5 . . ? C5 C1 H1A 118.5 . . ? N1 C2 C3 122.70(19) . . ? N1 C2 H2B 118.7 . . ? C3 C2 H2B 118.7 . . ? C2 C3 C4 119.02(19) . . ? C2 C3 H3B 120.5 . . ? C4 C3 H3B 120.5 . . ? C5 C4 C3 119.23(18) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C1 117.99(17) . . ? C4 C5 C6 120.62(17) . 1_455 ? C1 C5 C6 121.32(16) . 1_455 ? C7 C6 C10 108.35(15) . . ? C7 C6 C5 109.67(15) . 1_655 ? C10 C6 C5 113.66(15) . 1_655 ? C7 C6 H6C 110.0 . . ? C10 C6 H6C 110.1 . . ? C5 C6 H6C 105.0 1_655 . ? C8 C7 C11 119.04(17) . . ? C8 C7 C6 124.43(17) . . ? C11 C7 C6 116.49(17) . . ? C7 C8 N2 119.87(17) . . ? C7 C8 C12 124.36(17) . . ? N2 C8 C12 115.76(17) . . ? C10 C9 N2 120.35(17) . . ? C10 C9 C13 124.31(17) . . ? N2 C9 C13 115.34(17) . . ? C9 C10 C14 119.48(17) . . ? C9 C10 C6 123.76(17) . . ? C14 C10 C6 116.75(17) . . ? N3 C11 C7 178.0(2) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 177.2(2) . . ? N5 C15 C19 123.61(19) . . ? N5 C15 H15A 118.2 . . ? C19 C15 H15A 118.2 . . ? N5 C16 C17 122.6(2) . . ? N5 C16 H16A 118.7 . . ? C17 C16 H16A 118.7 . . ? C18 C17 C16 119.4(2) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 119.2(2) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C18 C19 C15 117.47(19) . . ? C18 C19 C20 122.62(18) . 2_656 ? C15 C19 C20 119.82(18) . 2_656 ? C19 C20 C21 113.04(16) 2_656 . ? C19 C20 C24 110.60(16) 2_656 . ? C21 C20 C24 107.94(16) . . ? C19 C20 H20A 108.4 2_656 . ? C21 C20 H20A 108.4 . . ? C24 C20 H20A 108.4 . . ? C22 C21 C25 118.39(18) . . ? C22 C21 C20 123.99(18) . . ? C25 C21 C20 117.44(17) . . ? C21 C22 N6 120.32(18) . . ? C21 C22 C26 124.50(18) . . ? N6 C22 C26 115.18(17) . . ? C24 C23 N6 120.32(18) . . ? C24 C23 C27 124.67(19) . . ? N6 C23 C27 115.01(18) . . ? C23 C24 C28 120.90(19) . . ? C23 C24 C20 124.14(18) . . ? C28 C24 C20 114.96(18) . . ? N7 C25 C21 179.3(2) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C24 175.5(3) . . ? F3 P F3 180.000(1) 2_665 . ? F3 P F1 89.77(6) 2_665 2_665 ? F3 P F1 90.23(6) . 2_665 ? F3 P F1 90.23(6) 2_665 . ? F3 P F1 89.77(6) . . ? F1 P F1 179.999(1) 2_665 . ? F3 P F2 90.26(6) 2_665 2_665 ? F3 P F2 89.74(6) . 2_665 ? F1 P F2 89.91(6) 2_665 2_665 ? F1 P F2 90.09(6) . 2_665 ? F3 P F2 89.74(6) 2_665 . ? F3 P F2 90.26(6) . . ? F1 P F2 90.09(6) 2_665 . ? F1 P F2 89.91(6) . . ? F2 P F2 180.0 2_665 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.548 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 966506' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C16 H15 Ag N5, B F4 ' _chemical_formula_sum 'C16 H15 Ag B F4 N5' _chemical_melting_point ? _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _diffrn_ambient_temperature 150(2) _chemical_formula_weight 472.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7672(6) _cell_length_b 19.8975(14) _cell_length_c 11.2697(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.772(7) _cell_angle_gamma 90.00 _cell_volume 1861.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3170 _cell_measurement_theta_min 2.7690 _cell_measurement_theta_max 29.1068 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94585 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8923 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 29.17 _reflns_number_total 4308 _reflns_number_gt 3624 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _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^)+(0.0362P)^2^+4.0883P] 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 4308 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Ag Ag 0.30647(4) 0.058496(18) 0.94985(3) 0.03236(12) Uani 1 1 d . . . N1 N 0.1048(4) -0.01057(16) 0.8818(3) 0.0203(6) Uani 1 1 d . . . N2 N -0.3367(4) 0.12667(18) 0.5355(3) 0.0226(7) Uani 1 1 d . . . H2A H -0.342(5) 0.165(2) 0.515(4) 0.026(13) Uiso 1 1 d . . . N3 N -0.4857(4) 0.01054(19) 0.8538(3) 0.0298(8) Uani 1 1 d . . . N4 N -0.1528(5) -0.07670(18) 0.3984(4) 0.0322(8) Uani 1 1 d . . . N5 N 0.4391(5) 0.1499(2) 1.0033(4) 0.0361(9) Uani 1 1 d . . . C1 C 0.1109(5) -0.0736(2) 0.9247(4) 0.0284(9) Uani 1 1 d . . . H1A H 0.2027 -0.0870 0.9920 0.034 Uiso 1 1 calc R . . C2 C -0.0092(6) -0.1193(2) 0.8757(4) 0.0349(10) Uani 1 1 d . . . H2B H -0.0004 -0.1637 0.9082 0.042 Uiso 1 1 calc R . . C3 C -0.1436(5) -0.1000(2) 0.7782(4) 0.0281(9) Uani 1 1 d . . . H3A H -0.2286 -0.1310 0.7431 0.034 Uiso 1 1 calc R . . C4 C -0.1534(4) -0.03533(18) 0.7322(3) 0.0180(7) Uani 1 1 d . . . C5 C -0.0263(4) 0.00785(18) 0.7872(3) 0.0172(7) Uani 1 1 d . . . H5A H -0.0321 0.0526 0.7566 0.021 Uiso 1 1 calc R . . C6 C -0.3000(4) -0.01021(18) 0.6267(3) 0.0176(7) Uani 1 1 d . . . H6A H -0.3778 -0.0483 0.5991 0.021 Uiso 1 1 calc R . . C7 C -0.3830(4) 0.04624(19) 0.6737(3) 0.0194(7) Uani 1 1 d . . . C8 C -0.3939(4) 0.11044(19) 0.6319(3) 0.0207(8) Uani 1 1 d . . . C9 C -0.2741(4) 0.0794(2) 0.4744(3) 0.0205(7) Uani 1 1 d . . . C10 C -0.2583(4) 0.01482(19) 0.5136(3) 0.0182(7) Uani 1 1 d . . . C11 C -0.4424(4) 0.0286(2) 0.7727(4) 0.0222(8) Uani 1 1 d . . . C12 C -0.4677(5) 0.1666(2) 0.6831(4) 0.0276(9) Uani 1 1 d . . . H12A H -0.5053 0.1495 0.7505 0.054(16) Uiso 1 1 calc R . . H12B H -0.5591 0.1853 0.6161 0.068(19) Uiso 1 1 calc R . . H12C H -0.3871 0.2019 0.7164 0.062(18) Uiso 1 1 calc R . . C13 C -0.2315(5) 0.1049(2) 0.3637(4) 0.0275(9) Uani 1 1 d . . . H13A H -0.1937 0.0675 0.3241 0.041 Uiso 1 1 calc R . . H13B H -0.1462 0.1387 0.3917 0.041 Uiso 1 1 calc R . . H13C H -0.3269 0.1252 0.3032 0.041 Uiso 1 1 calc R . . C14 C -0.1985(5) -0.0345(2) 0.4474(4) 0.0218(8) Uani 1 1 d . . . C15 C 0.5066(5) 0.1983(2) 1.0377(4) 0.0321(10) Uani 1 1 d . . . C16 C 0.5959(8) 0.2601(3) 1.0820(6) 0.0512(15) Uani 1 1 d . . . H16A H 0.6444 0.2758 1.0199 0.14(4) Uiso 1 1 calc R . . H16B H 0.6809 0.2515 1.1617 0.09(2) Uiso 1 1 calc R . . H16C H 0.5224 0.2945 1.0942 0.11(3) Uiso 1 1 calc R . . F1 F 0.4356(4) 0.32980(15) 1.3040(3) 0.0583(9) Uani 1 1 d . . . F2 F 0.3403(4) 0.25828(16) 1.4196(3) 0.0482(7) Uani 1 1 d . . . F3 F 0.6038(4) 0.25756(15) 1.4352(3) 0.0568(9) Uani 1 1 d . . . F4 F 0.4166(5) 0.21829(19) 1.2625(4) 0.0813(14) Uani 1 1 d . . . B B 0.4468(6) 0.2667(3) 1.3531(5) 0.0313(11) 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 Ag 0.02444(18) 0.0434(2) 0.02799(19) -0.00621(14) 0.00666(13) -0.01085(14) N1 0.0169(15) 0.0273(17) 0.0171(15) -0.0009(12) 0.0063(12) 0.0023(13) N2 0.0250(18) 0.0215(17) 0.0228(17) 0.0018(14) 0.0098(14) 0.0018(13) N3 0.0270(18) 0.042(2) 0.0217(17) 0.0049(15) 0.0094(15) 0.0074(16) N4 0.035(2) 0.0295(19) 0.039(2) 0.0004(16) 0.0212(17) 0.0045(16) N5 0.036(2) 0.037(2) 0.038(2) -0.0091(17) 0.0151(17) -0.0035(17) C1 0.028(2) 0.030(2) 0.022(2) 0.0079(16) 0.0020(16) 0.0090(17) C2 0.043(3) 0.023(2) 0.032(2) 0.0123(18) 0.003(2) 0.0018(18) C3 0.031(2) 0.025(2) 0.026(2) 0.0020(16) 0.0062(17) -0.0067(17) C4 0.0188(18) 0.0197(17) 0.0179(17) -0.0005(14) 0.0094(14) 0.0010(14) C5 0.0174(17) 0.0180(17) 0.0175(18) 0.0011(13) 0.0073(14) 0.0019(14) C6 0.0139(16) 0.0230(18) 0.0165(17) -0.0011(14) 0.0056(14) -0.0005(14) C7 0.0140(17) 0.030(2) 0.0128(16) -0.0020(14) 0.0026(13) 0.0004(14) C8 0.0147(17) 0.028(2) 0.0184(18) -0.0020(15) 0.0039(14) 0.0028(15) C9 0.0128(16) 0.0279(19) 0.0206(18) -0.0019(15) 0.0053(14) -0.0001(14) C10 0.0133(16) 0.0255(19) 0.0143(17) 0.0008(14) 0.0024(13) -0.0002(14) C11 0.0147(17) 0.030(2) 0.0199(19) -0.0001(15) 0.0031(15) 0.0041(15) C12 0.027(2) 0.030(2) 0.026(2) -0.0040(17) 0.0105(17) 0.0062(17) C13 0.031(2) 0.029(2) 0.025(2) 0.0072(16) 0.0126(17) 0.0037(17) C14 0.0180(18) 0.0264(19) 0.0212(18) 0.0019(15) 0.0066(15) 0.0006(15) C15 0.031(2) 0.036(2) 0.035(2) -0.0020(19) 0.018(2) 0.0005(19) C16 0.065(4) 0.038(3) 0.064(4) -0.016(3) 0.039(3) -0.022(3) F1 0.0514(19) 0.0385(16) 0.076(2) 0.0268(16) 0.0080(17) 0.0003(14) F2 0.0429(16) 0.071(2) 0.0364(16) 0.0034(14) 0.0210(13) -0.0040(15) F3 0.0348(16) 0.0423(17) 0.087(3) 0.0242(16) 0.0111(16) 0.0020(13) F4 0.110(3) 0.084(3) 0.073(3) -0.053(2) 0.061(2) -0.063(2) B 0.035(3) 0.029(2) 0.031(3) -0.002(2) 0.013(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N5 2.139(4) . ? Ag N1 2.175(3) . ? Ag N3 2.583(4) 1_655 ? N1 C1 1.338(5) . ? N1 C5 1.342(5) . ? N2 C8 1.374(5) . ? N2 C9 1.380(5) . ? N2 H2A 0.80(5) . ? N3 C11 1.154(5) . ? N3 Ag 2.583(4) 1_455 ? N4 C14 1.146(5) . ? N5 C15 1.130(6) . ? C1 C2 1.367(6) . ? C1 H1A 0.9500 . ? C2 C3 1.382(6) . ? C2 H2B 0.9500 . ? C3 C4 1.379(5) . ? C3 H3A 0.9500 . ? C4 C5 1.385(5) . ? C4 C6 1.527(5) . ? C5 H5A 0.9500 . ? C6 C10 1.518(5) . ? C6 C7 1.524(5) . ? C6 H6A 1.0000 . ? C7 C8 1.354(5) . ? C7 C11 1.419(5) . ? C8 C12 1.498(5) . ? C9 C10 1.352(5) . ? C9 C13 1.500(5) . ? C10 C14 1.430(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.457(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? F1 B 1.363(6) . ? F2 B 1.383(6) . ? F3 B 1.402(6) . ? F4 B 1.366(6) . ? 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 N5 Ag N1 160.63(13) . . ? N5 Ag N3 92.26(14) . 1_655 ? N1 Ag N3 102.82(12) . 1_655 ? C1 N1 C5 117.9(3) . . ? C1 N1 Ag 122.0(3) . . ? C5 N1 Ag 119.9(3) . . ? C8 N2 C9 122.7(3) . . ? C8 N2 H2A 117(3) . . ? C9 N2 H2A 121(3) . . ? C11 N3 Ag 132.3(3) . 1_455 ? C15 N5 Ag 176.0(4) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C1 C2 C3 119.0(4) . . ? C1 C2 H2B 120.5 . . ? C3 C2 H2B 120.5 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C6 122.2(3) . . ? C5 C4 C6 120.0(3) . . ? N1 C5 C4 123.1(3) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? C10 C6 C7 108.7(3) . . ? C10 C6 C4 113.0(3) . . ? C7 C6 C4 110.3(3) . . ? C10 C6 H6A 108.2 . . ? C7 C6 H6A 108.2 . . ? C4 C6 H6A 108.2 . . ? C8 C7 C11 120.3(4) . . ? C8 C7 C6 124.2(3) . . ? C11 C7 C6 115.4(3) . . ? C7 C8 N2 119.6(3) . . ? C7 C8 C12 124.1(4) . . ? N2 C8 C12 116.3(3) . . ? C10 C9 N2 120.0(3) . . ? C10 C9 C13 124.5(4) . . ? N2 C9 C13 115.5(3) . . ? C9 C10 C14 119.8(3) . . ? C9 C10 C6 124.0(3) . . ? C14 C10 C6 116.1(3) . . ? N3 C11 C7 175.8(4) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 176.1(4) . . ? N5 C15 C16 179.1(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F1 B F4 112.0(4) . . ? F1 B F2 111.0(4) . . ? F4 B F2 108.5(4) . . ? F1 B F3 108.3(4) . . ? F4 B F3 108.4(4) . . ? F2 B F3 108.5(4) . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.176 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 966507' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C30 H27 Ag N9, C F3 O3 S' _chemical_formula_sum 'C31 H27 Ag F3 N9 O3 S' _chemical_melting_point ? _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _diffrn_ambient_temperature 150(2) _chemical_formula_weight 770.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0714(4) _cell_length_b 18.3581(8) _cell_length_c 20.8126(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.060(2) _cell_angle_gamma 90.00 _cell_volume 3389.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7332 _exptl_absorpt_correction_T_max 0.8695 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37802 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.36 _reflns_number_total 6891 _reflns_number_gt 6122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006)' _computing_data_reduction 'SAINT V7.34A (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 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^)+(0.0506P)^2^+4.5255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6891 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ag Ag 0.23471(2) 0.120560(12) 0.201790(9) 0.03294(8) Uani 1 1 d . . . N1 N 0.0242(2) 0.15520(11) 0.13467(10) 0.0226(4) Uani 1 1 d . . . N2 N -0.2949(3) -0.08202(13) 0.08723(11) 0.0289(5) Uani 1 1 d . . . H2A H -0.294(4) -0.1280(19) 0.1042(18) 0.042(9) Uiso 1 1 d . . . N3 N -0.5546(3) 0.12654(14) 0.14304(14) 0.0413(6) Uani 1 1 d . . . N4 N -0.1624(3) 0.03163(16) -0.09881(12) 0.0429(6) Uani 1 1 d . . . N5 N 0.3468(2) 0.03712(12) 0.27266(10) 0.0260(4) Uani 1 1 d . . . N6 N 0.8760(3) -0.09638(13) 0.47974(12) 0.0311(5) Uani 1 1 d . . . H6A H 0.925(4) -0.1240(18) 0.5065(18) 0.035(9) Uiso 1 1 d . . . N7 N 0.5702(3) 0.11165(15) 0.49869(15) 0.0461(6) Uani 1 1 d . . . N8 N 0.9108(3) -0.0343(2) 0.26006(14) 0.0635(10) Uani 1 1 d . . . N9 N 0.3114(4) 0.24232(18) 0.24815(17) 0.0619(8) Uani 1 1 d . A . C1 C 0.0154(3) 0.22166(13) 0.10721(13) 0.0273(5) Uani 1 1 d . . . H1B H 0.0936 0.2557 0.1228 0.033 Uiso 1 1 calc R . . C2 C -0.1016(3) 0.24248(14) 0.05767(13) 0.0305(5) Uani 1 1 d . . . H2B H -0.1043 0.2900 0.0394 0.037 Uiso 1 1 calc R . . C3 C -0.2161(3) 0.19293(14) 0.03459(12) 0.0270(5) Uani 1 1 d . . . H3A H -0.2983 0.2061 0.0003 0.032 Uiso 1 1 calc R . . C4 C -0.2090(3) 0.12398(13) 0.06223(11) 0.0208(5) Uani 1 1 d . . . C5 C -0.0873(3) 0.10791(13) 0.11255(12) 0.0215(5) Uani 1 1 d . . . H5A H -0.0828 0.0611 0.1323 0.026 Uiso 1 1 calc R . . C6 C -0.3259(3) 0.06541(14) 0.03792(12) 0.0247(5) Uani 1 1 d . . . H6B H -0.4083 0.0875 0.0040 0.030 Uiso 1 1 calc R . . C7 C -0.3954(3) 0.03524(14) 0.09340(12) 0.0260(5) Uani 1 1 d . . . C8 C -0.3757(3) -0.03306(14) 0.11583(12) 0.0264(5) Uani 1 1 d . . . C9 C -0.2422(3) -0.06552(14) 0.03170(12) 0.0250(5) Uani 1 1 d . . . C10 C -0.2580(3) 0.00225(14) 0.00650(12) 0.0248(5) Uani 1 1 d . . . C11 C -0.4840(3) 0.08520(15) 0.12150(14) 0.0317(6) Uani 1 1 d . . . C12 C -0.4415(3) -0.06337(16) 0.17036(13) 0.0336(6) Uani 1 1 d . . . H12A H -0.4965 -0.0249 0.1881 0.050 Uiso 1 1 calc R . . H12B H -0.3603 -0.0818 0.2052 0.050 Uiso 1 1 calc R . . H12C H -0.5107 -0.1032 0.1535 0.050 Uiso 1 1 calc R . . C13 C -0.1697(3) -0.12687(15) 0.00307(14) 0.0324(6) Uani 1 1 d . . . H13A H -0.0623 -0.1163 0.0068 0.050(10) Uiso 1 1 calc R . . H13B H -0.2181 -0.1328 -0.0433 0.050(10) Uiso 1 1 calc R . . H13C H -0.1809 -0.1719 0.0269 0.050(10) Uiso 1 1 calc R . . C14 C -0.2047(3) 0.01777(15) -0.05214(13) 0.0295(5) Uani 1 1 d . . . C15 C 0.2876(3) -0.02957(16) 0.27194(12) 0.0288(5) Uani 1 1 d . . . H15A H 0.1894 -0.0378 0.2463 0.035 Uiso 1 1 calc R . . C16 C 0.3636(3) -0.08709(16) 0.30700(14) 0.0330(6) Uani 1 1 d . . . H16A H 0.3183 -0.1339 0.3055 0.040 Uiso 1 1 calc R . . C17 C 0.5074(3) -0.07527(15) 0.34437(13) 0.0306(6) Uani 1 1 d . . . H17A H 0.5620 -0.1140 0.3686 0.037 Uiso 1 1 calc R . . C18 C 0.5702(3) -0.00655(14) 0.34588(11) 0.0236(5) Uani 1 1 d . . . C19 C 0.4859(3) 0.04788(14) 0.30938(12) 0.0243(5) Uani 1 1 d . . . H19A H 0.5284 0.0953 0.3103 0.029 Uiso 1 1 calc R . . C20 C 0.7265(3) 0.00975(14) 0.38670(12) 0.0262(5) Uani 1 1 d . . . H20A H 0.7573 0.0594 0.3746 0.031 Uiso 1 1 calc R . . C21 C 0.7253(3) 0.00937(14) 0.45974(12) 0.0265(5) Uani 1 1 d . . . C22 C 0.7926(3) -0.04244(14) 0.50138(12) 0.0269(5) Uani 1 1 d . . . C23 C 0.9087(3) -0.09468(16) 0.41804(13) 0.0319(6) Uani 1 1 d . . . C24 C 0.8428(3) -0.04477(16) 0.37393(13) 0.0316(6) Uani 1 1 d . . . C25 C 0.6400(3) 0.06550(16) 0.48237(13) 0.0323(6) Uani 1 1 d . . . C26 C 0.7838(3) -0.04748(17) 0.57219(13) 0.0341(6) Uani 1 1 d . . . H26A H 0.7223 -0.0073 0.5832 0.051 Uiso 1 1 calc R . . H26B H 0.8855 -0.0444 0.5996 0.051 Uiso 1 1 calc R . . H26C H 0.7378 -0.0940 0.5802 0.051 Uiso 1 1 calc R . . C27 C 1.0176(3) -0.1521(2) 0.40577(17) 0.0462(8) Uani 1 1 d . . . H27A H 1.0347 -0.1469 0.3610 0.069 Uiso 1 1 calc R . . H27B H 0.9758 -0.2004 0.4109 0.069 Uiso 1 1 calc R . . H27C H 1.1134 -0.1464 0.4374 0.069 Uiso 1 1 calc R . . C28 C 0.8812(3) -0.0406(2) 0.31066(14) 0.0425(7) Uani 1 1 d . . . C29 C 0.3519(4) 0.2601(2) 0.30005(19) 0.0511(8) Uani 1 1 d . . . C30 C 0.400(4) 0.2680(18) 0.3738(18) 0.071(5) Uani 0.44(4) 1 d P A 1 H30D H 0.4000 0.2201 0.3945 0.107 Uiso 0.44(4) 1 calc PR A 1 H30E H 0.3299 0.3004 0.3899 0.107 Uiso 0.44(4) 1 calc PR A 1 H30F H 0.5019 0.2887 0.3849 0.107 Uiso 0.44(4) 1 calc PR A 1 C30' C 0.401(3) 0.2957(16) 0.3628(14) 0.071(5) Uani 0.56(4) 1 d P A 2 H30A H 0.4751 0.2651 0.3915 0.12(2) Uiso 0.56(4) 1 calc PR A 2 H30B H 0.3138 0.3034 0.3831 0.12(2) Uiso 0.56(4) 1 calc PR A 2 H30C H 0.4463 0.3428 0.3563 0.12(2) Uiso 0.56(4) 1 calc PR A 2 S S 0.90489(7) 0.22828(3) 0.38027(3) 0.02752(14) Uani 1 1 d . . . F1 F 0.7825(3) 0.15916(14) 0.27288(10) 0.0710(7) Uani 1 1 d . . . F2 F 0.9123(3) 0.25298(13) 0.25750(10) 0.0659(6) Uani 1 1 d . . . F3 F 1.0230(3) 0.15445(15) 0.29695(12) 0.0768(7) Uani 1 1 d . . . O1 O 0.9053(2) 0.16124(11) 0.41623(10) 0.0377(5) Uani 1 1 d . . . O2 O 0.7676(2) 0.26898(12) 0.37236(11) 0.0424(5) Uani 1 1 d . . . O3 O 1.0409(3) 0.27011(13) 0.39773(11) 0.0493(6) Uani 1 1 d . . . C31 C 0.9047(4) 0.19725(19) 0.29704(15) 0.0448(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 Ag 0.02704(12) 0.04240(14) 0.02660(12) -0.00383(8) -0.00076(8) 0.01201(8) N1 0.0219(10) 0.0242(10) 0.0217(10) -0.0036(8) 0.0043(8) 0.0018(8) N2 0.0320(12) 0.0300(12) 0.0281(11) -0.0029(9) 0.0140(9) 0.0003(9) N3 0.0373(14) 0.0373(13) 0.0547(16) -0.0074(11) 0.0217(12) 0.0019(11) N4 0.0461(15) 0.0535(16) 0.0323(13) 0.0044(11) 0.0156(11) 0.0004(12) N5 0.0217(10) 0.0365(12) 0.0206(10) 0.0005(8) 0.0060(8) 0.0046(9) N6 0.0288(11) 0.0335(12) 0.0289(12) 0.0018(10) 0.0011(9) 0.0055(10) N7 0.0402(15) 0.0476(16) 0.0497(16) -0.0065(12) 0.0075(12) 0.0116(12) N8 0.0293(14) 0.127(3) 0.0365(15) 0.0041(17) 0.0114(12) 0.0044(16) N9 0.063(2) 0.0539(18) 0.063(2) -0.0240(16) 0.0019(16) 0.0015(15) C1 0.0286(13) 0.0229(12) 0.0303(13) -0.0053(10) 0.0060(10) -0.0032(10) C2 0.0374(14) 0.0209(12) 0.0330(13) 0.0037(10) 0.0070(11) 0.0009(10) C3 0.0280(12) 0.0303(13) 0.0216(11) 0.0014(10) 0.0024(10) 0.0033(10) C4 0.0191(11) 0.0258(12) 0.0191(11) -0.0036(9) 0.0074(9) 0.0000(9) C5 0.0215(11) 0.0215(11) 0.0228(11) 0.0011(9) 0.0073(9) 0.0013(9) C6 0.0195(11) 0.0300(13) 0.0240(12) -0.0035(10) 0.0027(9) -0.0007(9) C7 0.0192(11) 0.0338(13) 0.0258(12) -0.0088(10) 0.0064(9) -0.0048(10) C8 0.0211(11) 0.0344(13) 0.0245(12) -0.0072(10) 0.0064(9) -0.0058(10) C9 0.0195(11) 0.0332(13) 0.0227(11) -0.0063(10) 0.0049(9) -0.0024(10) C10 0.0201(11) 0.0327(13) 0.0222(11) -0.0064(10) 0.0061(9) -0.0035(10) C11 0.0262(13) 0.0333(14) 0.0374(14) -0.0053(11) 0.0106(11) -0.0068(11) C12 0.0359(14) 0.0372(15) 0.0317(14) -0.0066(11) 0.0163(12) -0.0038(12) C13 0.0359(15) 0.0350(14) 0.0289(13) -0.0025(11) 0.0125(11) 0.0049(11) C14 0.0283(13) 0.0339(14) 0.0262(13) -0.0046(10) 0.0054(10) -0.0006(11) C15 0.0195(11) 0.0456(15) 0.0214(12) -0.0012(11) 0.0049(9) -0.0037(11) C16 0.0281(13) 0.0368(15) 0.0334(14) 0.0040(11) 0.0047(11) -0.0104(11) C17 0.0278(13) 0.0324(14) 0.0294(13) 0.0088(11) 0.0007(10) -0.0020(11) C18 0.0193(11) 0.0321(13) 0.0200(11) 0.0014(9) 0.0051(9) -0.0006(9) C19 0.0226(11) 0.0282(12) 0.0229(11) 0.0001(9) 0.0064(9) 0.0007(10) C20 0.0206(11) 0.0318(13) 0.0251(12) 0.0030(10) 0.0020(9) -0.0038(10) C21 0.0211(12) 0.0314(13) 0.0253(12) -0.0037(10) 0.0011(9) -0.0009(10) C22 0.0226(12) 0.0316(13) 0.0251(12) -0.0031(10) 0.0015(9) -0.0029(10) C23 0.0205(12) 0.0427(15) 0.0311(14) -0.0070(11) 0.0019(10) 0.0011(11) C24 0.0208(12) 0.0483(16) 0.0253(13) -0.0029(11) 0.0040(10) -0.0014(11) C25 0.0264(13) 0.0378(15) 0.0305(13) -0.0026(11) 0.0009(11) -0.0005(11) C26 0.0303(14) 0.0444(16) 0.0255(13) 0.0002(11) 0.0009(11) 0.0015(12) C27 0.0299(15) 0.061(2) 0.0461(18) -0.0101(15) 0.0044(13) 0.0143(14) C28 0.0180(12) 0.077(2) 0.0328(15) 0.0004(14) 0.0046(11) 0.0029(13) C29 0.0382(17) 0.0494(19) 0.063(2) -0.0225(17) 0.0044(16) 0.0028(14) C30 0.054(3) 0.096(14) 0.058(9) -0.031(10) -0.001(5) 0.019(11) C30' 0.054(3) 0.096(14) 0.058(9) -0.031(10) -0.001(5) 0.019(11) S 0.0276(3) 0.0293(3) 0.0239(3) -0.0006(2) 0.0014(2) 0.0005(2) F1 0.0903(17) 0.0766(16) 0.0397(11) -0.0188(11) -0.0010(11) -0.0290(13) F2 0.0958(17) 0.0692(14) 0.0356(10) 0.0124(10) 0.0200(11) -0.0050(12) F3 0.0955(18) 0.0819(17) 0.0658(15) 0.0001(12) 0.0466(14) 0.0301(14) O1 0.0440(11) 0.0344(11) 0.0334(10) 0.0043(8) 0.0052(9) 0.0043(9) O2 0.0397(11) 0.0391(11) 0.0483(12) -0.0009(9) 0.0092(10) 0.0102(9) O3 0.0388(12) 0.0561(14) 0.0461(12) 0.0022(10) -0.0066(10) -0.0146(10) C31 0.0544(19) 0.0495(18) 0.0314(15) 0.0025(13) 0.0114(14) -0.0049(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.211(2) . ? Ag N5 2.220(2) . ? Ag N9 2.476(3) . ? Ag N3 2.477(3) 1_655 ? N1 C5 1.340(3) . ? N1 C1 1.343(3) . ? N2 C8 1.372(3) . ? N2 C9 1.373(3) . ? N2 H2A 0.91(4) . ? N3 C11 1.143(4) . ? N3 Ag 2.477(3) 1_455 ? N4 C14 1.145(4) . ? N5 C15 1.336(4) . ? N5 C19 1.346(3) . ? N6 C23 1.377(4) . ? N6 C22 1.378(3) . ? N6 H6A 0.82(4) . ? N7 C25 1.151(4) . ? N8 C28 1.146(4) . ? N9 C29 1.115(5) . ? C1 C2 1.371(4) . ? C1 H1B 0.9500 . ? C2 C3 1.389(4) . ? C2 H2B 0.9500 . ? C3 C4 1.386(3) . ? C3 H3A 0.9500 . ? C4 C5 1.385(3) . ? C4 C6 1.521(3) . ? C5 H5A 0.9500 . ? C6 C10 1.523(3) . ? C6 C7 1.530(3) . ? C6 H6B 1.0000 . ? C7 C8 1.337(4) . ? C7 C11 1.423(4) . ? C8 C12 1.495(4) . ? C9 C10 1.346(4) . ? C9 C13 1.490(3) . ? C10 C14 1.432(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.383(4) . ? C15 H15A 0.9500 . ? C16 C17 1.389(4) . ? C16 H16A 0.9500 . ? C17 C18 1.382(4) . ? C17 H17A 0.9500 . ? C18 C19 1.385(3) . ? C18 C20 1.522(3) . ? C19 H19A 0.9500 . ? C20 C24 1.518(4) . ? C20 C21 1.523(3) . ? C20 H20A 1.0000 . ? C21 C22 1.345(4) . ? C21 C25 1.426(4) . ? C22 C26 1.495(4) . ? C23 C24 1.345(4) . ? C23 C27 1.502(4) . ? C24 C28 1.433(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30' 1.44(3) . ? C29 C30 1.51(4) . ? C30 H30D 0.9800 . ? C30 H30E 0.9800 . ? C30 H30F 0.9800 . ? C30' H30A 0.9800 . ? C30' H30B 0.9800 . ? C30' H30C 0.9800 . ? S O2 1.432(2) . ? S O3 1.434(2) . ? S O1 1.440(2) . ? S C31 1.823(3) . ? F1 C31 1.318(4) . ? F2 C31 1.324(4) . ? F3 C31 1.331(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 N1 Ag N5 146.45(8) . . ? N1 Ag N9 96.99(9) . . ? N5 Ag N9 108.16(10) . . ? N1 Ag N3 109.21(9) . 1_655 ? N5 Ag N3 93.73(8) . 1_655 ? N9 Ag N3 88.25(10) . 1_655 ? C5 N1 C1 118.0(2) . . ? C5 N1 Ag 121.42(16) . . ? C1 N1 Ag 119.80(16) . . ? C8 N2 C9 122.1(2) . . ? C8 N2 H2A 113(2) . . ? C9 N2 H2A 124(2) . . ? C11 N3 Ag 135.8(2) . 1_455 ? C15 N5 C19 117.9(2) . . ? C15 N5 Ag 119.86(16) . . ? C19 N5 Ag 121.38(17) . . ? C23 N6 C22 121.9(2) . . ? C23 N6 H6A 117(2) . . ? C22 N6 H6A 119(2) . . ? C29 N9 Ag 130.6(3) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1B 118.6 . . ? C2 C1 H1B 118.6 . . ? C1 C2 C3 118.9(2) . . ? C1 C2 H2B 120.5 . . ? C3 C2 H2B 120.5 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C5 C4 C3 118.0(2) . . ? C5 C4 C6 119.4(2) . . ? C3 C4 C6 122.6(2) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? C4 C6 C10 111.38(19) . . ? C4 C6 C7 111.93(19) . . ? C10 C6 C7 108.4(2) . . ? C4 C6 H6B 108.3 . . ? C10 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? C8 C7 C11 120.4(2) . . ? C8 C7 C6 123.9(2) . . ? C11 C7 C6 115.7(2) . . ? C7 C8 N2 120.5(2) . . ? C7 C8 C12 124.7(2) . . ? N2 C8 C12 114.8(2) . . ? C10 C9 N2 120.3(2) . . ? C10 C9 C13 124.2(2) . . ? N2 C9 C13 115.5(2) . . ? C9 C10 C14 119.2(2) . . ? C9 C10 C6 123.8(2) . . ? C14 C10 C6 117.0(2) . . ? N3 C11 C7 178.4(3) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 178.6(3) . . ? N5 C15 C16 122.6(2) . . ? N5 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C15 C16 C17 118.9(2) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 117.9(2) . . ? C17 C18 C20 121.6(2) . . ? C19 C18 C20 120.5(2) . . ? N5 C19 C18 123.4(2) . . ? N5 C19 H19A 118.3 . . ? C18 C19 H19A 118.3 . . ? C24 C20 C18 111.9(2) . . ? C24 C20 C21 108.8(2) . . ? C18 C20 C21 110.9(2) . . ? C24 C20 H20A 108.4 . . ? C18 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? C22 C21 C25 120.2(2) . . ? C22 C21 C20 123.3(2) . . ? C25 C21 C20 116.4(2) . . ? C21 C22 N6 120.3(2) . . ? C21 C22 C26 124.6(2) . . ? N6 C22 C26 115.1(2) . . ? C24 C23 N6 120.0(2) . . ? C24 C23 C27 125.2(3) . . ? N6 C23 C27 114.8(3) . . ? C23 C24 C28 120.3(3) . . ? C23 C24 C20 123.8(2) . . ? C28 C24 C20 115.9(2) . . ? N7 C25 C21 177.9(3) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C24 177.3(4) . . ? N9 C29 C30' 170.1(13) . . ? N9 C29 C30 168.1(14) . . ? C30' C29 C30 21.6(14) . . ? C29 C30 H30D 109.5 . . ? C29 C30 H30E 109.5 . . ? C29 C30 H30F 109.5 . . ? C29 C30' H30A 109.5 . . ? C29 C30' H30B 109.5 . . ? H30A C30' H30B 109.5 . . ? C29 C30' H30C 109.5 . . ? H30A C30' H30C 109.5 . . ? H30B C30' H30C 109.5 . . ? O2 S O3 115.53(14) . . ? O2 S O1 114.42(13) . . ? O3 S O1 114.67(13) . . ? O2 S C31 103.03(15) . . ? O3 S C31 103.79(15) . . ? O1 S C31 103.07(14) . . ? F1 C31 F2 108.8(3) . . ? F1 C31 F3 107.5(3) . . ? F2 C31 F3 107.9(3) . . ? F1 C31 S 111.2(2) . . ? F2 C31 S 111.1(2) . . ? F3 C31 S 110.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.588 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 966508' ####################################################################### # # 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_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H24 Ag2 Cl N8 O4, Cl O4 ' _chemical_formula_sum 'C28 H24 Ag2 Cl2 N8 O8' _chemical_melting_point ? _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _diffrn_ambient_temperature 150(2) _chemical_formula_weight 887.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5452(4) _cell_length_b 12.2962(4) _cell_length_c 15.9721(6) _cell_angle_alpha 84.345(3) _cell_angle_beta 80.885(3) _cell_angle_gamma 71.359(4) _cell_volume 1568.06(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6890 _cell_measurement_theta_min 3.0422 _cell_measurement_theta_max 29.1152 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95373 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13813 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 29.18 _reflns_number_total 7187 _reflns_number_gt 6416 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _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^)+(0.0202P)^2^+0.7575P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7187 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.377085(19) 0.107382(14) 0.306681(10) 0.02137(5) Uani 1 1 d . . . Ag2 Ag -0.19888(2) 0.509941(14) 0.791266(10) 0.02023(5) Uani 1 1 d . . . N1 N 0.3453(2) 0.42531(14) 0.08529(11) 0.0173(4) Uani 1 1 d . . . N2 N 0.8286(2) -0.00375(15) -0.08336(11) 0.0189(4) Uani 1 1 d . . . H2A H 0.836(3) -0.056(2) -0.1116(15) 0.019(6) Uiso 1 1 d . . . N3 N 0.9746(2) 0.34213(15) -0.13952(12) 0.0267(4) Uani 1 1 d . . . N4 N 0.5580(2) 0.09601(16) 0.19562(12) 0.0246(4) Uani 1 1 d . . . N5 N 0.1811(2) 0.13033(14) 0.41518(10) 0.0175(4) Uani 1 1 d . . . N6 N -0.2933(2) 0.52259(15) 0.37280(12) 0.0191(4) Uani 1 1 d . . . H6A H -0.304(3) 0.577(2) 0.3396(15) 0.021(7) Uiso 1 1 d . . . N7 N -0.4245(3) 0.16936(17) 0.39163(13) 0.0301(5) Uani 1 1 d . . . N8 N -0.1754(2) 0.47683(17) 0.65722(12) 0.0261(4) Uani 1 1 d . . . C1 C 0.2663(3) 0.44555(17) 0.01599(13) 0.0185(4) Uani 1 1 d . . . H1B H 0.1588 0.4968 0.0191 0.022 Uiso 1 1 calc R . . C2 C 0.3387(3) 0.39329(17) -0.05936(13) 0.0196(4) Uani 1 1 d . . . H2B H 0.2810 0.4098 -0.1061 0.023 Uiso 1 1 calc R . . C3 C 0.4982(3) 0.31603(17) -0.06453(13) 0.0173(4) Uani 1 1 d . . . H3A H 0.5484 0.2797 -0.1147 0.021 Uiso 1 1 calc R . . C4 C 0.5820(2) 0.29347(16) 0.00579(12) 0.0143(4) Uani 1 1 d . . . C5 C 0.5005(3) 0.35167(17) 0.07864(13) 0.0173(4) Uani 1 1 d . . . H5A H 0.5573 0.3387 0.1256 0.021 Uiso 1 1 calc R . . C6 C 0.7490(2) 0.20065(17) 0.01029(12) 0.0150(4) Uani 1 1 d . . . H6B H 0.8094 0.2233 0.0493 0.018 Uiso 1 1 calc R . . C7 C 0.8579(2) 0.17890(17) -0.07540(13) 0.0168(4) Uani 1 1 d . . . C8 C 0.8876(2) 0.08416(17) -0.11908(13) 0.0168(4) Uani 1 1 d . . . C9 C 0.7488(2) -0.00416(17) -0.00180(12) 0.0162(4) Uani 1 1 d . . . C10 C 0.7178(2) 0.08760(17) 0.04507(12) 0.0159(4) Uani 1 1 d . . . C11 C 0.9240(2) 0.26822(18) -0.11192(13) 0.0191(4) Uani 1 1 d . . . C12 C 0.9826(3) 0.06559(19) -0.20626(13) 0.0237(5) Uani 1 1 d . . . H12A H 1.0246 0.1289 -0.2245 0.035 Uiso 1 1 calc R . . H12B H 0.9101 0.0603 -0.2448 0.035 Uiso 1 1 calc R . . H12C H 1.0740 -0.0044 -0.2054 0.035 Uiso 1 1 calc R . . C13 C 0.7026(3) -0.11050(18) 0.02838(14) 0.0223(5) Uani 1 1 d . . . H13A H 0.6511 -0.1038 0.0864 0.033 Uiso 1 1 calc R . . H13B H 0.8011 -0.1761 0.0244 0.033 Uiso 1 1 calc R . . H13C H 0.6262 -0.1198 -0.0063 0.033 Uiso 1 1 calc R . . C14 C 0.6312(2) 0.08878(17) 0.12899(13) 0.0176(4) Uani 1 1 d . . . C15 C 0.2194(3) 0.06404(18) 0.48568(13) 0.0225(5) Uani 1 1 d . . . H15A H 0.3221 0.0071 0.4838 0.027 Uiso 1 1 calc R . . C16 C 0.1120(3) 0.0774(2) 0.56070(14) 0.0282(5) Uani 1 1 d . . . H16A H 0.1418 0.0298 0.6084 0.034 Uiso 1 1 calc R . . C17 C -0.0406(3) 0.16234(19) 0.56420(14) 0.0238(5) Uani 1 1 d . . . H17A H -0.1148 0.1722 0.6143 0.029 Uiso 1 1 calc R . . C18 C -0.0822(2) 0.23269(17) 0.49242(12) 0.0152(4) Uani 1 1 d . . . C19 C 0.0333(2) 0.21278(17) 0.41946(12) 0.0163(4) Uani 1 1 d . . . H19A H 0.0066 0.2592 0.3709 0.020 Uiso 1 1 calc R . . C20 C -0.2481(2) 0.32902(17) 0.49519(12) 0.0156(4) Uani 1 1 d . . . H20A H -0.3249 0.3106 0.5426 0.019 Uiso 1 1 calc R . . C21 C -0.3266(2) 0.34081(17) 0.41384(13) 0.0162(4) Uani 1 1 d . . . C22 C -0.3414(2) 0.43075(17) 0.35691(13) 0.0171(4) Uani 1 1 d . . . C23 C -0.2499(2) 0.53389(18) 0.44966(13) 0.0186(4) Uani 1 1 d . . . C24 C -0.2320(2) 0.44606(18) 0.50925(13) 0.0173(4) Uani 1 1 d . . . C25 C -0.3814(3) 0.24697(18) 0.39894(13) 0.0197(4) Uani 1 1 d . . . C26 C -0.4119(3) 0.44287(19) 0.27542(13) 0.0220(5) Uani 1 1 d . . . H26A H -0.4497 0.3783 0.2711 0.033 Uiso 1 1 calc R . . H26B H -0.3274 0.4457 0.2286 0.033 Uiso 1 1 calc R . . H26C H -0.5039 0.5124 0.2742 0.033 Uiso 1 1 calc R . . C27 C -0.2315(3) 0.64834(18) 0.46083(15) 0.0262(5) Uani 1 1 d . . . H27A H -0.1944 0.6474 0.5146 0.039 Uiso 1 1 calc R . . H27B H -0.3370 0.7069 0.4590 0.039 Uiso 1 1 calc R . . H27C H -0.1513 0.6642 0.4161 0.039 Uiso 1 1 calc R . . C28 C -0.1996(3) 0.46363(18) 0.59094(14) 0.0207(4) Uani 1 1 d . . . Cl1 Cl -0.00825(6) 0.71439(4) 0.82465(3) 0.01908(10) Uani 1 1 d . . . O1 O 0.0236(2) 0.66087(15) 0.90642(11) 0.0368(4) Uani 1 1 d . . . O2 O 0.1113(2) 0.77359(14) 0.79313(11) 0.0332(4) Uani 1 1 d . . . O3 O 0.0033(2) 0.62814(13) 0.76649(10) 0.0293(4) Uani 1 1 d . . . O4 O -0.1740(2) 0.79580(14) 0.83083(12) 0.0361(4) Uani 1 1 d . . . Cl2 Cl 0.52411(7) 0.19572(4) 0.71717(3) 0.02363(11) Uani 1 1 d . . . O5 O 0.5763(2) 0.10946(14) 0.78289(11) 0.0337(4) Uani 1 1 d . . . O6 O 0.3532(2) 0.26299(15) 0.74000(11) 0.0380(4) Uani 1 1 d . . . O7 O 0.5450(3) 0.14243(17) 0.63865(11) 0.0457(5) Uani 1 1 d . . . O8 O 0.6264(2) 0.27122(14) 0.70781(12) 0.0395(5) 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 0.02010(8) 0.02564(9) 0.01560(9) -0.00389(6) 0.00570(6) -0.00626(7) Ag2 0.02381(9) 0.02276(9) 0.01355(8) -0.00629(6) -0.00039(6) -0.00586(7) N1 0.0203(9) 0.0156(8) 0.0147(9) -0.0048(7) -0.0004(7) -0.0034(7) N2 0.0252(10) 0.0159(9) 0.0140(9) -0.0040(7) 0.0009(7) -0.0050(8) N3 0.0245(10) 0.0200(9) 0.0305(11) 0.0011(8) 0.0032(8) -0.0037(8) N4 0.0247(10) 0.0282(10) 0.0197(10) -0.0019(8) 0.0022(8) -0.0088(8) N5 0.0161(8) 0.0206(9) 0.0137(8) -0.0038(7) 0.0011(7) -0.0035(7) N6 0.0234(9) 0.0164(9) 0.0177(9) -0.0003(7) -0.0065(7) -0.0049(8) N7 0.0344(11) 0.0319(11) 0.0300(11) -0.0021(9) -0.0110(9) -0.0154(10) N8 0.0256(10) 0.0333(11) 0.0197(10) -0.0105(8) -0.0015(8) -0.0074(9) C1 0.0181(10) 0.0155(10) 0.0195(11) -0.0010(8) -0.0012(8) -0.0026(8) C2 0.0243(11) 0.0201(10) 0.0147(10) 0.0014(8) -0.0049(8) -0.0071(9) C3 0.0206(10) 0.0173(10) 0.0134(10) -0.0030(8) -0.0003(8) -0.0055(8) C4 0.0167(9) 0.0145(9) 0.0131(10) -0.0027(7) -0.0003(7) -0.0072(8) C5 0.0211(10) 0.0190(10) 0.0132(10) -0.0025(8) -0.0038(8) -0.0071(9) C6 0.0152(9) 0.0180(10) 0.0117(9) -0.0021(8) -0.0017(7) -0.0044(8) C7 0.0142(9) 0.0188(10) 0.0151(10) 0.0008(8) 0.0009(8) -0.0037(8) C8 0.0156(9) 0.0174(10) 0.0140(10) 0.0021(8) -0.0020(8) -0.0015(8) C9 0.0130(9) 0.0180(10) 0.0157(10) 0.0008(8) -0.0024(7) -0.0026(8) C10 0.0129(9) 0.0210(10) 0.0118(10) 0.0019(8) -0.0023(7) -0.0029(8) C11 0.0159(10) 0.0183(10) 0.0184(11) -0.0024(8) 0.0013(8) 0.0001(8) C12 0.0256(11) 0.0227(11) 0.0165(11) -0.0014(9) 0.0038(9) -0.0018(9) C13 0.0216(11) 0.0211(11) 0.0236(12) 0.0017(9) -0.0016(9) -0.0073(9) C14 0.0163(10) 0.0166(10) 0.0175(11) 0.0005(8) -0.0025(8) -0.0021(8) C15 0.0214(11) 0.0210(11) 0.0200(11) -0.0003(9) -0.0025(9) 0.0003(9) C16 0.0306(12) 0.0293(12) 0.0161(11) 0.0056(9) -0.0012(9) -0.0003(10) C17 0.0234(11) 0.0282(12) 0.0136(10) -0.0007(9) 0.0042(8) -0.0027(9) C18 0.0167(9) 0.0161(10) 0.0137(10) -0.0037(8) -0.0001(8) -0.0064(8) C19 0.0180(10) 0.0195(10) 0.0120(10) -0.0014(8) -0.0028(8) -0.0064(8) C20 0.0146(9) 0.0206(10) 0.0116(9) -0.0042(8) -0.0002(7) -0.0055(8) C21 0.0125(9) 0.0205(10) 0.0155(10) -0.0061(8) -0.0016(7) -0.0038(8) C22 0.0136(9) 0.0208(10) 0.0152(10) -0.0072(8) -0.0015(8) -0.0015(8) C23 0.0136(9) 0.0203(10) 0.0209(11) -0.0091(8) -0.0008(8) -0.0022(8) C24 0.0141(9) 0.0214(10) 0.0160(10) -0.0089(8) -0.0020(8) -0.0025(8) C25 0.0191(10) 0.0240(11) 0.0162(10) -0.0044(8) -0.0025(8) -0.0059(9) C26 0.0217(11) 0.0252(11) 0.0186(11) -0.0038(9) -0.0057(8) -0.0042(9) C27 0.0248(12) 0.0209(11) 0.0341(13) -0.0086(10) -0.0080(10) -0.0048(10) C28 0.0172(10) 0.0234(11) 0.0204(11) -0.0095(9) 0.0008(8) -0.0039(9) Cl1 0.0213(2) 0.0185(2) 0.0178(2) -0.00367(19) -0.00283(19) -0.0058(2) O1 0.0463(11) 0.0440(11) 0.0266(9) 0.0101(8) -0.0166(8) -0.0208(9) O2 0.0398(10) 0.0283(9) 0.0376(10) -0.0061(7) 0.0029(8) -0.0217(8) O3 0.0366(9) 0.0282(9) 0.0271(9) -0.0140(7) 0.0061(7) -0.0168(8) O4 0.0254(9) 0.0305(9) 0.0497(11) -0.0155(8) -0.0136(8) 0.0034(7) Cl2 0.0280(3) 0.0200(3) 0.0170(3) -0.0014(2) 0.0028(2) -0.0019(2) O5 0.0396(10) 0.0291(9) 0.0300(9) 0.0109(7) -0.0071(8) -0.0099(8) O6 0.0269(9) 0.0373(10) 0.0374(10) -0.0013(8) 0.0063(8) 0.0020(8) O7 0.0544(13) 0.0485(12) 0.0282(10) -0.0177(9) -0.0063(9) -0.0027(10) O8 0.0432(11) 0.0286(9) 0.0430(11) -0.0021(8) 0.0152(9) -0.0157(8) _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 N4 2.1445(17) . ? Ag1 N5 2.1820(16) . ? Ag2 N8 2.1848(18) . ? Ag2 N1 2.2312(16) 2_566 ? Ag2 N3 2.4067(19) 1_456 ? Ag2 O3 2.5555(15) . ? N1 C5 1.340(3) . ? N1 C1 1.348(3) . ? N1 Ag2 2.2312(16) 2_566 ? N2 C9 1.372(3) . ? N2 C8 1.373(3) . ? N2 H2A 0.80(2) . ? N3 C11 1.149(3) . ? N3 Ag2 2.4067(19) 1_654 ? N4 C14 1.142(3) . ? N5 C19 1.340(3) . ? N5 C15 1.343(3) . ? N6 C23 1.369(3) . ? N6 C22 1.376(3) . ? N6 H6A 0.80(2) . ? N7 C25 1.149(3) . ? N8 C28 1.147(3) . ? C1 C2 1.381(3) . ? C1 H1B 0.9300 . ? C2 C3 1.385(3) . ? C2 H2B 0.9300 . ? C3 C4 1.385(3) . ? C3 H3A 0.9300 . ? C4 C5 1.393(3) . ? C4 C6 1.523(3) . ? C5 H5A 0.9300 . ? C6 C7 1.523(3) . ? C6 C10 1.533(3) . ? C6 H6B 0.9800 . ? C7 C8 1.350(3) . ? C7 C11 1.425(3) . ? C8 C12 1.495(3) . ? C9 C10 1.348(3) . ? C9 C13 1.498(3) . ? C10 C14 1.424(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C16 1.378(3) . ? C15 H15A 0.9300 . ? C16 C17 1.383(3) . ? C16 H16A 0.9300 . ? C17 C18 1.388(3) . ? C17 H17A 0.9300 . ? C18 C19 1.389(3) . ? C18 C20 1.527(3) . ? C19 H19A 0.9300 . ? C20 C21 1.529(3) . ? C20 C24 1.530(3) . ? C20 H20A 0.9800 . ? C21 C22 1.347(3) . ? C21 C25 1.429(3) . ? C22 C26 1.494(3) . ? C23 C24 1.354(3) . ? C23 C27 1.496(3) . ? C24 C28 1.426(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? Cl1 O1 1.4288(17) . ? Cl1 O2 1.4379(16) . ? Cl1 O4 1.4446(17) . ? Cl1 O3 1.4476(16) . ? Cl2 O7 1.4318(18) . ? Cl2 O5 1.4326(16) . ? Cl2 O6 1.4385(17) . ? Cl2 O8 1.4488(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N5 175.75(7) . . ? N8 Ag2 N1 152.98(7) . 2_566 ? N8 Ag2 N3 108.07(7) . 1_456 ? N1 Ag2 N3 91.99(6) 2_566 1_456 ? N8 Ag2 O3 94.31(6) . . ? N1 Ag2 O3 100.69(6) 2_566 . ? N3 Ag2 O3 98.20(6) 1_456 . ? C5 N1 C1 117.25(17) . . ? C5 N1 Ag2 123.23(13) . 2_566 ? C1 N1 Ag2 118.61(13) . 2_566 ? C9 N2 C8 122.96(18) . . ? C9 N2 H2A 117.7(16) . . ? C8 N2 H2A 119.2(16) . . ? C11 N3 Ag2 120.77(17) . 1_654 ? C14 N4 Ag1 167.32(18) . . ? C19 N5 C15 117.88(17) . . ? C19 N5 Ag1 124.91(13) . . ? C15 N5 Ag1 116.83(14) . . ? C23 N6 C22 122.33(19) . . ? C23 N6 H6A 116.5(17) . . ? C22 N6 H6A 120.5(17) . . ? C28 N8 Ag2 165.11(18) . . ? N1 C1 C2 122.61(19) . . ? N1 C1 H1B 118.7 . . ? C2 C1 H1B 118.7 . . ? C1 C2 C3 119.26(19) . . ? C1 C2 H2B 120.4 . . ? C3 C2 H2B 120.4 . . ? C4 C3 C2 119.31(19) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 117.51(18) . . ? C3 C4 C6 123.54(17) . . ? C5 C4 C6 118.65(17) . . ? N1 C5 C4 124.04(19) . . ? N1 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? C4 C6 C7 113.55(16) . . ? C4 C6 C10 109.00(15) . . ? C7 C6 C10 107.82(16) . . ? C4 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? C10 C6 H6B 108.8 . . ? C8 C7 C11 119.40(18) . . ? C8 C7 C6 124.07(17) . . ? C11 C7 C6 116.46(17) . . ? C7 C8 N2 119.79(18) . . ? C7 C8 C12 124.81(18) . . ? N2 C8 C12 115.40(18) . . ? C10 C9 N2 119.61(18) . . ? C10 C9 C13 124.79(18) . . ? N2 C9 C13 115.60(18) . . ? C9 C10 C14 119.80(18) . . ? C9 C10 C6 124.04(17) . . ? C14 C10 C6 115.64(17) . . ? N3 C11 C7 178.1(2) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 176.3(2) . . ? N5 C15 C16 122.4(2) . . ? N5 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C18 119.46(19) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C18 C19 117.46(19) . . ? C17 C18 C20 120.51(17) . . ? C19 C18 C20 122.02(17) . . ? N5 C19 C18 123.60(18) . . ? N5 C19 H19A 118.2 . . ? C18 C19 H19A 118.2 . . ? C18 C20 C21 112.20(16) . . ? C18 C20 C24 112.73(16) . . ? C21 C20 C24 107.71(16) . . ? C18 C20 H20A 108.0 . . ? C21 C20 H20A 108.0 . . ? C24 C20 H20A 108.0 . . ? C22 C21 C25 120.26(19) . . ? C22 C21 C20 123.99(18) . . ? C25 C21 C20 115.72(18) . . ? C21 C22 N6 120.04(19) . . ? C21 C22 C26 125.30(19) . . ? N6 C22 C26 114.64(18) . . ? C24 C23 N6 119.82(19) . . ? C24 C23 C27 125.3(2) . . ? N6 C23 C27 114.86(19) . . ? C23 C24 C28 118.49(19) . . ? C23 C24 C20 124.02(18) . . ? C28 C24 C20 117.48(18) . . ? N7 C25 C21 176.1(2) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C24 178.9(2) . . ? O1 Cl1 O2 109.75(11) . . ? O1 Cl1 O4 109.73(11) . . ? O2 Cl1 O4 109.24(10) . . ? O1 Cl1 O3 109.70(10) . . ? O2 Cl1 O3 109.61(9) . . ? O4 Cl1 O3 108.79(10) . . ? Cl1 O3 Ag2 120.81(8) . . ? O7 Cl2 O5 109.70(11) . . ? O7 Cl2 O6 110.82(12) . . ? O5 Cl2 O6 109.93(10) . . ? O7 Cl2 O8 109.08(12) . . ? O5 Cl2 O8 108.82(11) . . ? O6 Cl2 O8 108.45(11) . . ? _diffrn_measured_fraction_theta_max 0.848 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.451 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.070 #===END _database_code_depnum_ccdc_archive 'CCDC 966509'