Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michael Hannon' 'Guy Clarkson' 'Edyta J. Kolodziejczyk' 'Mirela Pascu' 'Gabriel I. Pascu' 'Floriana Tuna' _publ_contact_author_name 'Dr Michael Hannon' _publ_contact_author_address ; Department of Chemistry University of Warwick Gibbet Hill Road Coventry CV4 7AL UNITED KINGDOM ; _publ_contact_author_email M.J.HANNON@WARWICK.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Binding sites on the outside of metallo-supramolecular architectures; engineering coordination polymers from discrete architectures ; data_mp3 _database_code_depnum_ccdc_archive 'CCDC 233558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 N6' _chemical_formula_weight 240.28 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.4272(16) _cell_length_b 7.440(3) _cell_length_c 17.810(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.344(9) _cell_angle_gamma 90.00 _cell_volume 586.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1723 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 3516 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.91 _reflns_number_total 1411 _reflns_number_gt 849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0692P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1411 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _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 N1 N -0.0770(3) -0.12117(18) 0.32797(8) 0.0361(4) Uani 1 1 d . . . C2 C -0.2650(4) -0.2466(2) 0.30123(9) 0.0393(5) Uani 1 1 d . . . H2A H -0.3646 -0.2256 0.2547 0.047 Uiso 1 1 calc R . . C3 C -0.3199(4) -0.4052(2) 0.33871(9) 0.0371(5) Uani 1 1 d . . . H3A H -0.4581 -0.4890 0.3175 0.045 Uiso 1 1 calc R . . N4 N -0.1849(3) -0.44477(18) 0.40379(8) 0.0392(4) Uani 1 1 d . . . C5 C 0.0031(4) -0.3205(2) 0.43061(9) 0.0343(4) Uani 1 1 d . . . H5A H 0.1044 -0.3430 0.4768 0.041 Uiso 1 1 calc R . . C6 C 0.0577(3) -0.1583(2) 0.39359(8) 0.0278(4) Uani 1 1 d . . . C7 C 0.2661(3) -0.0204(2) 0.42479(9) 0.0282(4) Uani 1 1 d . . . N8 N 0.4023(3) -0.06645(17) 0.48578(7) 0.0310(4) Uani 1 1 d . . . C9 C 0.2961(4) 0.1548(2) 0.38425(10) 0.0422(5) Uani 1 1 d . . . H9A H 0.4528 0.2278 0.4086 0.063 Uiso 1 1 calc R . . H9B H 0.1031 0.2192 0.3856 0.063 Uiso 1 1 calc R . . H9C H 0.3522 0.1323 0.3319 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 N1 0.0398(9) 0.0403(8) 0.0280(7) 0.0027(6) -0.0060(6) -0.0050(7) C2 0.0444(11) 0.0464(11) 0.0270(9) -0.0015(8) -0.0071(7) -0.0058(9) C3 0.0406(11) 0.0374(10) 0.0333(10) -0.0091(8) -0.0032(8) -0.0044(8) N4 0.0459(9) 0.0322(8) 0.0393(9) -0.0009(7) -0.0058(7) -0.0041(7) C5 0.0410(10) 0.0324(9) 0.0294(9) 0.0008(7) -0.0063(7) -0.0007(8) C6 0.0294(9) 0.0315(9) 0.0225(8) -0.0007(7) 0.0009(6) 0.0034(7) C7 0.0289(9) 0.0302(9) 0.0256(8) 0.0010(7) 0.0010(7) 0.0025(7) N8 0.0352(8) 0.0300(8) 0.0277(7) 0.0018(6) -0.0048(6) -0.0033(6) C9 0.0534(12) 0.0354(10) 0.0376(10) 0.0087(8) -0.0135(8) -0.0065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.336(2) . ? N1 C6 1.3376(19) . ? C2 C3 1.378(2) . ? C2 H2A 0.9500 . ? C3 N4 1.334(2) . ? C3 H3A 0.9500 . ? N4 C5 1.331(2) . ? C5 C6 1.397(2) . ? C5 H5A 0.9500 . ? C6 C7 1.485(2) . ? C7 N8 1.2857(19) . ? C7 C9 1.497(2) . ? N8 N8 1.406(3) 3_656 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 C2 N1 C6 116.17(15) . . ? N1 C2 C3 122.44(16) . . ? N1 C2 H2A 118.8 . . ? C3 C2 H2A 118.8 . . ? N4 C3 C2 122.03(16) . . ? N4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C5 N4 C3 115.77(15) . . ? N4 C5 C6 122.72(15) . . ? N4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? N1 C6 C5 120.87(15) . . ? N1 C6 C7 117.19(14) . . ? C5 C6 C7 121.94(14) . . ? N8 C7 C6 114.78(14) . . ? N8 C7 C9 126.67(15) . . ? C6 C7 C9 118.55(14) . . ? C7 N8 N8 113.66(16) . 3_656 ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3A N1 0.95 2.78 3.404(2) 124.3 2_445 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.201 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.048 data_ft32 _database_code_depnum_ccdc_archive 'CCDC 233559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Ag B F4 N6' _chemical_formula_weight 511.05 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' B B 0.0013 0.0007 '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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.3804(11) _cell_length_b 10.3804(11) _cell_length_c 16.099(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1502.3(3) _cell_formula_units_Z 3 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2025 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 7601 _diffrn_reflns_av_R_equivalents 0.1133 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1780 _reflns_number_gt 1022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0399P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1780 _refine_ls_number_parameters 164 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 1.0000 0.0000 0.0428(4) Uani 1 6 d S . . Ag2 Ag -0.3333 0.3333 0.30569(5) 0.0411(3) Uani 1 3 d S . . N1 N -0.2044(7) 0.5543(7) 0.2088(4) 0.073(2) Uani 1 1 d . . . C2 C -0.1214(10) 0.5678(9) 0.1435(5) 0.081(3) Uani 1 1 d . . . H2A H -0.0852 0.5004 0.1377 0.097 Uiso 1 1 calc R . . C3 C -0.0853(8) 0.6744(8) 0.0838(4) 0.0506(19) Uani 1 1 d . . . H3A H -0.0290 0.6767 0.0368 0.061 Uiso 1 1 calc R . . N4 N -0.1280(6) 0.7738(7) 0.0911(3) 0.0563(16) Uani 1 1 d . . . C5 C -0.2087(8) 0.7628(8) 0.1601(4) 0.056(2) Uani 1 1 d . . . H5A H -0.2405 0.8333 0.1677 0.067 Uiso 1 1 calc R . . C6 C -0.2456(7) 0.6562(8) 0.2181(4) 0.0431(18) Uani 1 1 d . . . C7 C -0.3345(7) 0.6437(8) 0.2944(4) 0.0496(18) Uani 1 1 d . . . C8 C -0.3884(9) 0.7546(9) 0.3033(5) 0.077(2) Uani 1 1 d . . . H8A H -0.4539 0.7285 0.3518 0.116 Uiso 1 1 calc R . . H8B H -0.4433 0.7523 0.2533 0.116 Uiso 1 1 calc R . . H8C H -0.3028 0.8548 0.3107 0.116 Uiso 1 1 calc R . . N9 N -0.3610(5) 0.5410(6) 0.3447(3) 0.0413(13) Uani 1 1 d . . . C10 C -0.4328(7) 0.5242(7) 0.4224(4) 0.0382(16) Uani 1 1 d . . . C11 C -0.5628(7) 0.3924(8) 0.4397(4) 0.0454(17) Uani 1 1 d . . . H11A H -0.6062 0.3173 0.3984 0.054 Uiso 1 1 calc R . . C12 C -0.3708(7) 0.6302(7) 0.4838(4) 0.0457(17) Uani 1 1 d . . . H12A H -0.2809 0.7202 0.4730 0.055 Uiso 1 1 calc R . . B20 B 0.0000 1.0000 0.5862(6) 0.21(5) Uani 0.50 3 d SPD . . F21 F 0.0000 1.0000 0.5000 0.241(13) Uani 1 6 d SD . . F22 F -0.1389(10) 0.9111(10) 0.6280(7) 0.101(3) Uani 0.50 1 d P . . B10 B -0.6667 0.6667 0.0836(17) 0.093(7) Uani 1 3 d S . . F11 F -0.623(7) 0.604(7) 0.130(2) 0.23(2) Uani 0.47(4) 1 d P . 1 F12 F -0.790(3) 0.620(4) 0.0388(19) 0.20(2) Uani 0.47(4) 1 d P . 1 F13 F -0.767(13) 0.528(4) 0.099(5) 0.25(5) Uani 0.29(6) 1 d P . 2 F14 F -0.6667 0.6667 -0.004(3) 0.15(4) Uani 0.29(6) 3 d SP . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0466(6) 0.0466(6) 0.0353(8) 0.000 0.000 0.0233(3) Ag2 0.0428(4) 0.0428(4) 0.0377(6) 0.000 0.000 0.0214(2) N1 0.098(5) 0.082(5) 0.062(4) 0.033(4) 0.041(4) 0.062(5) C2 0.120(8) 0.095(7) 0.063(6) 0.042(5) 0.052(5) 0.081(6) C3 0.058(5) 0.053(5) 0.044(5) 0.002(4) 0.012(4) 0.030(4) N4 0.066(4) 0.065(4) 0.040(4) 0.016(3) 0.012(3) 0.034(4) C5 0.079(6) 0.056(5) 0.050(5) 0.012(4) 0.014(4) 0.045(5) C6 0.055(5) 0.052(5) 0.032(4) 0.011(3) 0.003(3) 0.034(4) C7 0.051(5) 0.050(5) 0.046(4) 0.000(4) 0.008(3) 0.023(4) C8 0.114(7) 0.088(6) 0.067(5) 0.020(4) 0.029(5) 0.078(6) N9 0.047(3) 0.045(4) 0.032(3) 0.001(3) 0.006(3) 0.023(3) C10 0.048(4) 0.044(4) 0.030(4) 0.001(3) 0.007(3) 0.029(4) C11 0.049(5) 0.052(5) 0.035(4) -0.004(3) 0.000(3) 0.025(4) C12 0.044(4) 0.039(4) 0.050(4) 0.007(3) 0.016(3) 0.018(4) B20 0.017(15) 0.017(15) 0.61(15) 0.000 0.000 0.008(8) F21 0.250(18) 0.250(18) 0.22(3) 0.000 0.000 0.125(9) F22 0.062(6) 0.068(7) 0.182(10) 0.011(6) 0.006(6) 0.038(5) B10 0.102(14) 0.102(14) 0.073(17) 0.000 0.000 0.051(7) F11 0.25(5) 0.27(5) 0.24(3) 0.04(4) -0.09(4) 0.18(4) F12 0.16(3) 0.23(4) 0.25(4) -0.09(3) -0.06(3) 0.12(3) F13 0.31(10) 0.04(2) 0.28(6) 0.07(2) -0.05(6) 0.00(3) F14 0.19(6) 0.19(6) 0.05(3) 0.000 0.000 0.10(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 N4 2.511(5) 5_455 ? Ag1 N4 2.511(5) 2_675 ? Ag1 N4 2.511(5) 4_575 ? Ag1 N4 2.511(5) 6_665 ? Ag1 N4 2.511(5) . ? Ag1 N4 2.511(5) 3_465 ? Ag2 N9 2.397(5) 3_455 ? Ag2 N9 2.397(5) 2_565 ? Ag2 N9 2.397(5) . ? Ag2 N1 2.533(6) 3_455 ? Ag2 N1 2.533(6) 2_565 ? Ag2 N1 2.533(6) . ? N1 C2 1.322(8) . ? N1 C6 1.333(8) . ? C2 C3 1.369(9) . ? C3 N4 1.317(8) . ? N4 C5 1.361(8) . ? C5 C6 1.349(8) . ? C6 C7 1.502(9) . ? C7 N9 1.255(8) . ? C7 C8 1.518(9) . ? N9 C10 1.422(7) . ? C10 C12 1.375(8) . ? C10 C11 1.387(8) . ? C11 C12 1.373(8) 4_466 ? C12 C11 1.373(8) 4_466 ? B20 F21 1.388(10) . ? B20 F22 1.433(11) 3_465 ? B20 F22 1.433(11) . ? B20 F22 1.433(11) 2_675 ? F21 B20 1.388(10) 4_576 ? B10 F11 1.21(2) 2_575 ? B10 F11 1.21(2) 3_355 ? B10 F11 1.21(2) . ? B10 F13 1.31(4) 3_355 ? B10 F13 1.31(4) . ? B10 F13 1.31(4) 2_575 ? B10 F12 1.33(2) . ? B10 F12 1.33(2) 3_355 ? B10 F12 1.33(2) 2_575 ? B10 F14 1.42(5) . ? F11 F12 1.47(4) 2_575 ? F11 F11 1.66(5) 2_575 ? F11 F11 1.66(5) 3_355 ? F12 F11 1.47(4) 3_355 ? 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 N4 180.0(4) 5_455 2_675 ? N4 Ag1 N4 89.36(19) 5_455 4_575 ? N4 Ag1 N4 90.64(19) 2_675 4_575 ? N4 Ag1 N4 89.36(19) 5_455 6_665 ? N4 Ag1 N4 90.64(19) 2_675 6_665 ? N4 Ag1 N4 89.36(19) 4_575 6_665 ? N4 Ag1 N4 90.64(19) 5_455 . ? N4 Ag1 N4 89.36(19) 2_675 . ? N4 Ag1 N4 180.0 4_575 . ? N4 Ag1 N4 90.64(19) 6_665 . ? N4 Ag1 N4 90.64(19) 5_455 3_465 ? N4 Ag1 N4 89.36(19) 2_675 3_465 ? N4 Ag1 N4 90.64(19) 4_575 3_465 ? N4 Ag1 N4 180.000(1) 6_665 3_465 ? N4 Ag1 N4 89.36(19) . 3_465 ? N9 Ag2 N9 113.38(10) 3_455 2_565 ? N9 Ag2 N9 113.38(10) 3_455 . ? N9 Ag2 N9 113.38(10) 2_565 . ? N9 Ag2 N1 66.02(19) 3_455 3_455 ? N9 Ag2 N1 90.43(19) 2_565 3_455 ? N9 Ag2 N1 152.0(2) . 3_455 ? N9 Ag2 N1 152.0(2) 3_455 2_565 ? N9 Ag2 N1 66.02(19) 2_565 2_565 ? N9 Ag2 N1 90.43(19) . 2_565 ? N1 Ag2 N1 86.1(2) 3_455 2_565 ? N9 Ag2 N1 90.4(2) 3_455 . ? N9 Ag2 N1 152.0(2) 2_565 . ? N9 Ag2 N1 66.02(19) . . ? N1 Ag2 N1 86.1(2) 3_455 . ? N1 Ag2 N1 86.1(2) 2_565 . ? C2 N1 C6 117.1(6) . . ? C2 N1 Ag2 127.4(5) . . ? C6 N1 Ag2 114.6(4) . . ? N1 C2 C3 123.0(7) . . ? N4 C3 C2 120.5(7) . . ? C3 N4 C5 116.1(6) . . ? C3 N4 Ag1 116.9(4) . . ? C5 N4 Ag1 124.8(5) . . ? C6 C5 N4 123.0(7) . . ? N1 C6 C5 120.1(6) . . ? N1 C6 C7 116.7(6) . . ? C5 C6 C7 123.2(7) . . ? N9 C7 C6 117.7(6) . . ? N9 C7 C8 125.1(6) . . ? C6 C7 C8 117.1(6) . . ? C7 N9 C10 123.5(6) . . ? C7 N9 Ag2 121.4(4) . . ? C10 N9 Ag2 114.3(4) . . ? C12 C10 C11 118.7(6) . . ? C12 C10 N9 121.8(6) . . ? C11 C10 N9 119.3(6) . . ? C12 C11 C10 120.4(6) 4_466 . ? C11 C12 C10 120.9(6) 4_466 . ? F21 B20 F22 118.0(6) . 3_465 ? F21 B20 F22 118.0(6) . . ? F22 B20 F22 99.7(7) 3_465 . ? F21 B20 F22 118.0(6) . 2_675 ? F22 B20 F22 99.7(7) 3_465 2_675 ? F22 B20 F22 99.7(7) . 2_675 ? B20 F21 B20 180.000(3) 4_576 . ? F11 B10 F11 86(3) 2_575 3_355 ? F11 B10 F11 86(3) 2_575 . ? F11 B10 F11 86(3) 3_355 . ? F11 B10 F13 53(4) 2_575 3_355 ? F11 B10 F13 67(4) 3_355 3_355 ? F11 B10 F13 131(4) . 3_355 ? F11 B10 F13 131(4) 2_575 . ? F11 B10 F13 53(4) 3_355 . ? F11 B10 F13 67(4) . . ? F13 B10 F13 117(2) 3_355 . ? F11 B10 F13 67(4) 2_575 2_575 ? F11 B10 F13 131(4) 3_355 2_575 ? F11 B10 F13 53(4) . 2_575 ? F13 B10 F13 117(2) 3_355 2_575 ? F13 B10 F13 117(2) . 2_575 ? F11 B10 F12 130(3) 2_575 . ? F11 B10 F12 70.5(18) 3_355 . ? F11 B10 F12 133(4) . . ? F13 B10 F12 77(5) 3_355 . ? F13 B10 F12 67(4) . . ? F13 B10 F12 157(4) 2_575 . ? F11 B10 F12 70.5(18) 2_575 3_355 ? F11 B10 F12 133(4) 3_355 3_355 ? F11 B10 F12 130(3) . 3_355 ? F13 B10 F12 67(4) 3_355 3_355 ? F13 B10 F12 157(4) . 3_355 ? F13 B10 F12 77(5) 2_575 3_355 ? F12 B10 F12 94(2) . 3_355 ? F11 B10 F12 133(4) 2_575 2_575 ? F11 B10 F12 130(3) 3_355 2_575 ? F11 B10 F12 70.5(18) . 2_575 ? F13 B10 F12 157(4) 3_355 2_575 ? F13 B10 F12 77(5) . 2_575 ? F13 B10 F12 67(4) 2_575 2_575 ? F12 B10 F12 94(2) . 2_575 ? F12 B10 F12 94(2) 3_355 2_575 ? F11 B10 F14 128(2) 2_575 . ? F11 B10 F14 128(2) 3_355 . ? F11 B10 F14 128(2) . . ? F13 B10 F14 101(3) 3_355 . ? F13 B10 F14 101(3) . . ? F13 B10 F14 101(3) 2_575 . ? F12 B10 F14 57.3(18) . . ? F12 B10 F14 57.3(18) 3_355 . ? F12 B10 F14 57.3(18) 2_575 . ? B10 F11 F12 58.7(14) . 2_575 ? B10 F11 F11 46.8(16) . 2_575 ? F12 F11 F11 97(2) 2_575 2_575 ? B10 F11 F11 46.8(16) . 3_355 ? F12 F11 F11 95(2) 2_575 3_355 ? F11 F11 F11 60.000(6) 2_575 3_355 ? B10 F12 F11 50.8(13) . 3_355 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C12 H12A F21 0.95 2.94 3.853(7) 161.0 . C2 H2A F13 0.95 3.23 3.96(14) 135.8 1_655 C3 H3A F12 0.95 2.81 3.45(3) 125.5 1_655 C11 H11A F22 0.95 2.56 3.309(12) 136.4 4_466 C12 H12A F22 0.95 2.65 3.477(11) 145.8 6_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.619 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.095 data_ft28 _database_code_depnum_ccdc_archive 'CCDC 233560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 Ag B F4 N4 O' _chemical_formula_weight 569.16 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.4389(13) _cell_length_b 9.8630(6) _cell_length_c 13.5869(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.578(2) _cell_angle_gamma 90.00 _cell_volume 2368.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1861 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 11833 _diffrn_reflns_av_R_equivalents 0.1737 _diffrn_reflns_av_sigmaI/netI 0.2300 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4151 _reflns_number_gt 1763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0435P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4151 _refine_ls_number_parameters 325 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.2064 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.985 _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 0.81027(4) 0.08278(7) -0.32345(6) 0.0415(3) Uani 1 1 d . . . N01 N 0.8197(4) 0.3014(7) 0.0281(6) 0.036(2) Uani 1 1 d . . . C02 C 0.8693(6) 0.3348(10) -0.0224(8) 0.050(3) Uani 1 1 d . . . H02A H 0.9032 0.4081 0.0017 0.060 Uiso 1 1 calc R . . C03 C 0.8724(6) 0.2637(10) -0.1103(8) 0.050(3) Uani 1 1 d . . . H03A H 0.9076 0.2912 -0.1457 0.060 Uiso 1 1 calc R . . N04 N 0.8282(5) 0.1606(8) -0.1447(6) 0.038(2) Uani 1 1 d . . . C05 C 0.7783(5) 0.1285(9) -0.0933(8) 0.037(3) Uani 1 1 d . . . H05A H 0.7440 0.0561 -0.1186 0.044 Uiso 1 1 calc R . . C06 C 0.7741(5) 0.1942(9) -0.0064(8) 0.033(3) Uani 1 1 d . . . C07 C 0.7199(5) 0.1570(9) 0.0525(7) 0.031(2) Uani 1 1 d . . . C08 C 0.6754(5) 0.0289(9) 0.0217(8) 0.044(3) Uani 1 1 d . . . H08A H 0.6398 0.0183 0.0626 0.067 Uiso 1 1 calc R . . H08B H 0.7101 -0.0487 0.0337 0.067 Uiso 1 1 calc R . . H08C H 0.6474 0.0333 -0.0513 0.067 Uiso 1 1 calc R . . N09 N 0.7154(4) 0.2374(7) 0.1248(6) 0.038(2) Uani 1 1 d . . . C10 C 0.6689(5) 0.2129(9) 0.1884(7) 0.030(2) Uani 1 1 d . . . C11 C 0.6207(5) 0.3189(9) 0.1972(7) 0.031(2) Uani 1 1 d . . . H11A H 0.6168 0.3980 0.1562 0.037 Uiso 1 1 calc R . . C12 C 0.5788(5) 0.3070(9) 0.2663(7) 0.033(2) Uani 1 1 d . . . H12A H 0.5444 0.3775 0.2695 0.039 Uiso 1 1 calc R . . C13 C 0.5848(5) 0.1959(10) 0.3315(7) 0.035(2) Uani 1 1 d . . . C14 C 0.6338(5) 0.0940(10) 0.3223(7) 0.044(3) Uani 1 1 d . . . H14A H 0.6395 0.0170 0.3658 0.052 Uiso 1 1 calc R . . C15 C 0.6749(5) 0.1008(9) 0.2518(7) 0.035(2) Uani 1 1 d . . . H15A H 0.7075 0.0282 0.2467 0.042 Uiso 1 1 calc R . . C16 C 0.5453(5) 0.1887(10) 0.4144(7) 0.049(3) Uani 1 1 d . . . H16A H 0.5598 0.2702 0.4582 0.059 Uiso 1 1 calc R . . H16B H 0.5653 0.1090 0.4579 0.059 Uiso 1 1 calc R . . C17 C 0.4594(5) 0.1793(8) 0.3810(8) 0.030(2) Uani 1 1 d . . . C18 C 0.4144(6) 0.1843(8) 0.2803(8) 0.038(3) Uani 1 1 d . . . H18A H 0.4375 0.1937 0.2265 0.046 Uiso 1 1 calc R . . C19 C 0.3363(6) 0.1759(8) 0.2566(7) 0.033(3) Uani 1 1 d . . . H19A H 0.3070 0.1797 0.1867 0.040 Uiso 1 1 calc R . . C20 C 0.2997(5) 0.1620(8) 0.3326(7) 0.026(2) Uani 1 1 d . . . C21 C 0.3453(5) 0.1599(8) 0.4331(7) 0.033(2) Uani 1 1 d . . . H21A H 0.3224 0.1511 0.4872 0.039 Uiso 1 1 calc R . . C22 C 0.4225(6) 0.1702(8) 0.4570(7) 0.037(3) Uani 1 1 d . . . H22A H 0.4516 0.1712 0.5271 0.044 Uiso 1 1 calc R . . N23 N 0.2208(4) 0.1416(6) 0.3101(5) 0.033(2) Uani 1 1 d . . . H23A H 0.1977 0.1715 0.2445 0.039 Uiso 1 1 calc R . . H23B H 0.2026 0.1925 0.3546 0.039 Uiso 1 1 calc R . . B10 B 0.1512(9) 0.2859(15) 0.0394(12) 0.062(4) Uani 1 1 d DU . . F11 F 0.1970(4) 0.2074(7) -0.0079(6) 0.084(3) Uani 0.893(13) 1 d P A 1 F12 F 0.1254(5) 0.1963(9) 0.0969(6) 0.092(4) Uani 0.893(13) 1 d P A 1 F13 F 0.2004(5) 0.3792(8) 0.1003(7) 0.093(3) Uani 0.893(13) 1 d P A 1 F14 F 0.0967(5) 0.3449(10) -0.0351(6) 0.096(4) Uani 0.893(13) 1 d P A 1 F11A F 0.195(4) 0.355(6) 0.000(5) 0.13(3) Uiso 0.107(13) 1 d PDU A 2 F12A F 0.175(4) 0.163(5) 0.064(4) 0.08(3) Uiso 0.107(13) 1 d PD A 2 F13A F 0.144(4) 0.348(5) 0.124(4) 0.07(2) Uiso 0.107(13) 1 d PD A 2 F14A F 0.082(3) 0.281(7) -0.025(5) 0.24(10) Uiso 0.107(13) 1 d PD A 2 O001 O 0.9599(4) 0.0875(8) -0.2533(6) 0.073(2) Uani 1 1 d . . . C02A C 0.9904(15) 0.041(3) -0.141(2) 0.081(8) Uiso 0.50 1 d P B 1 H02C H 0.9559 -0.0221 -0.1202 0.098 Uiso 0.50 1 calc PR B 1 H02D H 1.0037 0.1182 -0.0923 0.098 Uiso 0.50 1 calc PR B 1 C02B C 0.9786(14) -0.028(2) -0.199(2) 0.071(7) Uiso 0.50 1 d P B 2 H02E H 0.9600 -0.1077 -0.2443 0.085 Uiso 0.50 1 calc PR B 2 H02F H 0.9556 -0.0306 -0.1420 0.085 Uiso 0.50 1 calc PR B 2 C003 C 1.0636(7) -0.0327(13) -0.1587(13) 0.109(5) Uani 1 1 d . . . H03C H 1.1031 -0.0456 -0.0926 0.130 Uiso 0.50 1 calc PR B 1 H03D H 1.0498 -0.1223 -0.1917 0.130 Uiso 0.50 1 calc PR B 1 H03E H 1.0831 -0.1257 -0.1617 0.130 Uiso 0.50 1 d PR B 2 H03F H 1.0802 -0.0006 -0.0867 0.130 Uiso 0.50 1 d PR B 2 C004 C 1.0897(7) 0.0577(14) -0.2253(11) 0.095(5) Uani 1 1 d . B . H04C H 1.1294 0.0159 -0.2514 0.114 Uiso 0.50 1 calc PR C 1 H04D H 1.1079 0.1453 -0.1917 0.114 Uiso 0.50 1 calc PR C 1 H04E H 1.1356 0.1071 -0.1860 0.114 Uiso 0.50 1 d PR C 2 H04F H 1.1015 0.0066 -0.2815 0.114 Uiso 0.50 1 d PR C 2 C05A C 1.0146(10) 0.072(2) -0.3083(14) 0.036(5) Uiso 0.50 1 d P B 1 H05C H 1.0151 0.1515 -0.3521 0.043 Uiso 0.50 1 calc PR B 1 H05D H 1.0039 -0.0105 -0.3521 0.043 Uiso 0.50 1 calc PR B 1 C05B C 1.026(2) 0.149(3) -0.266(3) 0.130(13) Uiso 0.50 1 d P B 2 H05E H 1.0357 0.2366 -0.2289 0.156 Uiso 0.50 1 calc PR B 2 H05F H 1.0201 0.1665 -0.3397 0.156 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0446(5) 0.0381(5) 0.0450(5) 0.0056(5) 0.0180(4) 0.0043(5) N01 0.039(6) 0.035(5) 0.043(6) 0.003(4) 0.024(5) 0.001(4) C02 0.055(8) 0.043(7) 0.059(9) -0.009(6) 0.028(7) -0.009(6) C03 0.055(8) 0.044(7) 0.064(9) 0.006(6) 0.038(7) -0.012(6) N04 0.035(6) 0.049(6) 0.025(5) -0.001(4) 0.002(5) -0.005(5) C05 0.031(7) 0.038(7) 0.042(7) 0.001(5) 0.011(6) -0.005(5) C06 0.034(7) 0.021(6) 0.044(7) -0.001(5) 0.014(6) 0.004(5) C07 0.029(6) 0.034(6) 0.032(7) 0.009(5) 0.012(5) 0.009(5) C08 0.040(7) 0.040(6) 0.055(7) -0.007(5) 0.017(6) -0.002(5) N09 0.042(6) 0.042(5) 0.032(5) -0.001(4) 0.015(5) 0.000(4) C10 0.027(6) 0.036(6) 0.032(6) 0.003(5) 0.017(5) -0.009(5) C11 0.035(6) 0.031(6) 0.029(6) 0.009(5) 0.014(5) 0.001(5) C12 0.021(6) 0.032(6) 0.036(7) -0.001(5) -0.005(5) -0.004(5) C13 0.028(6) 0.049(7) 0.028(6) 0.003(5) 0.005(5) -0.003(5) C14 0.042(7) 0.045(7) 0.043(7) 0.021(6) 0.012(6) -0.009(6) C15 0.038(6) 0.032(6) 0.036(6) 0.010(5) 0.011(5) -0.002(5) C16 0.051(8) 0.068(8) 0.028(7) 0.008(5) 0.009(6) -0.011(6) C17 0.033(7) 0.028(6) 0.031(7) 0.002(5) 0.010(6) -0.003(5) C18 0.050(8) 0.036(6) 0.031(7) -0.001(5) 0.015(6) -0.008(5) C19 0.041(7) 0.027(6) 0.037(7) -0.008(5) 0.018(6) -0.004(5) C20 0.022(6) 0.030(6) 0.029(7) 0.001(5) 0.010(6) 0.002(4) C21 0.026(7) 0.041(6) 0.032(7) 0.004(5) 0.010(6) 0.002(5) C22 0.057(8) 0.040(6) 0.014(6) -0.003(5) 0.010(6) -0.006(6) N23 0.042(6) 0.028(5) 0.031(5) -0.003(3) 0.016(4) 0.005(4) B10 0.051(11) 0.067(11) 0.076(13) -0.012(10) 0.033(10) 0.008(9) F11 0.094(7) 0.080(6) 0.096(7) 0.012(5) 0.058(6) 0.004(5) F12 0.092(7) 0.125(8) 0.069(6) 0.037(5) 0.038(5) -0.018(5) F13 0.090(7) 0.064(6) 0.104(8) -0.011(5) -0.007(6) 0.009(5) F14 0.109(8) 0.049(6) 0.084(7) -0.001(4) -0.045(5) 0.028(5) O001 0.060(5) 0.084(6) 0.079(6) 0.021(5) 0.024(5) 0.005(5) C003 0.060(11) 0.074(10) 0.172(17) 0.042(10) 0.002(10) 0.007(8) C004 0.061(10) 0.085(11) 0.139(14) -0.020(10) 0.029(10) 0.005(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 N23 2.306(6) 3_655 ? Ag1 N01 2.368(7) 4_565 ? Ag1 N09 2.449(7) 4_565 ? Ag1 N04 2.477(7) . ? N01 C02 1.332(10) . ? N01 C06 1.349(10) . ? N01 Ag1 2.368(7) 4_566 ? C02 C03 1.401(12) . ? C03 N04 1.304(11) . ? N04 C05 1.343(10) . ? C05 C06 1.368(11) . ? C06 C07 1.493(11) . ? C07 N09 1.283(10) . ? C07 C08 1.499(11) . ? N09 C10 1.400(10) . ? N09 Ag1 2.449(7) 4_566 ? C10 C15 1.386(11) . ? C10 C11 1.400(11) . ? C11 C12 1.380(10) . ? C12 C13 1.394(11) . ? C13 C14 1.381(12) . ? C13 C16 1.507(11) . ? C14 C15 1.382(11) . ? C16 C17 1.522(12) . ? C17 C18 1.383(12) . ? C17 C22 1.392(10) . ? C18 C19 1.385(12) . ? C19 C20 1.392(10) . ? C20 C21 1.385(11) . ? C20 N23 1.412(10) . ? C21 C22 1.372(11) . ? N23 Ag1 2.306(6) 3_655 ? B10 F11A 1.28(4) . ? B10 F12A 1.30(4) . ? B10 F14A 1.33(5) . ? B10 F14 1.339(16) . ? B10 F13A 1.35(4) . ? B10 F12 1.354(15) . ? B10 F13 1.387(15) . ? B10 F11 1.426(13) . ? O001 C02B 1.35(2) . ? O001 C05B 1.42(3) . ? O001 C05A 1.425(18) . ? O001 C02A 1.53(3) . ? C02A C003 1.61(2) . ? C02B C003 1.51(3) . ? C003 C004 1.447(14) . ? C004 C05B 1.45(3) . ? C004 C05A 1.52(2) . ? 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 N23 Ag1 N01 127.6(2) 3_655 4_565 ? N23 Ag1 N09 123.0(3) 3_655 4_565 ? N01 Ag1 N09 68.0(3) 4_565 4_565 ? N23 Ag1 N04 100.8(3) 3_655 . ? N01 Ag1 N04 131.6(3) 4_565 . ? N09 Ag1 N04 86.6(2) 4_565 . ? C02 N01 C06 117.9(8) . . ? C02 N01 Ag1 123.2(7) . 4_566 ? C06 N01 Ag1 118.9(6) . 4_566 ? N01 C02 C03 121.1(9) . . ? N04 C03 C02 121.6(9) . . ? C03 N04 C05 116.7(8) . . ? C03 N04 Ag1 119.2(7) . . ? C05 N04 Ag1 121.2(7) . . ? N04 C05 C06 123.6(9) . . ? N01 C06 C05 119.2(8) . . ? N01 C06 C07 117.0(9) . . ? C05 C06 C07 123.8(9) . . ? N09 C07 C06 117.2(9) . . ? N09 C07 C08 125.8(8) . . ? C06 C07 C08 117.0(8) . . ? C07 N09 C10 123.3(8) . . ? C07 N09 Ag1 118.1(6) . 4_566 ? C10 N09 Ag1 117.4(6) . 4_566 ? C15 C10 C11 118.8(8) . . ? C15 C10 N09 124.5(8) . . ? C11 C10 N09 116.1(8) . . ? C12 C11 C10 119.2(8) . . ? C11 C12 C13 122.7(9) . . ? C14 C13 C12 116.7(8) . . ? C14 C13 C16 120.1(9) . . ? C12 C13 C16 123.0(9) . . ? C13 C14 C15 122.0(9) . . ? C14 C15 C10 120.5(9) . . ? C13 C16 C17 117.6(8) . . ? C18 C17 C22 117.0(9) . . ? C18 C17 C16 124.9(9) . . ? C22 C17 C16 118.0(9) . . ? C17 C18 C19 121.2(9) . . ? C18 C19 C20 121.7(9) . . ? C21 C20 C19 116.5(9) . . ? C21 C20 N23 120.6(8) . . ? C19 C20 N23 122.8(9) . . ? C22 C21 C20 122.0(9) . . ? C21 C22 C17 121.5(9) . . ? C20 N23 Ag1 112.6(5) . 3_655 ? F11A B10 F12A 113.5(19) . . ? F11A B10 F14A 110.1(18) . . ? F12A B10 F14A 108.9(18) . . ? F11A B10 F14 83(3) . . ? F12A B10 F14 136(3) . . ? F14A B10 F14 31(3) . . ? F11A B10 F13A 110.0(18) . . ? F12A B10 F13A 108.2(17) . . ? F14A B10 F13A 105.7(18) . . ? F14 B10 F13A 102(3) . . ? F11A B10 F12 163(3) . . ? F12A B10 F12 52(3) . . ? F14A B10 F12 86(3) . . ? F14 B10 F12 114.1(12) . . ? F13A B10 F12 70(2) . . ? F11A B10 F13 61(3) . . ? F12A B10 F13 111(3) . . ? F14A B10 F13 139(3) . . ? F14 B10 F13 112.6(13) . . ? F13A B10 F13 53(3) . . ? F12 B10 F13 111.5(13) . . ? F11A B10 F11 65(3) . . ? F12A B10 F11 54(3) . . ? F14A B10 F11 105(3) . . ? F14 B10 F11 108.0(12) . . ? F13A B10 F11 148(3) . . ? F12 B10 F11 104.9(11) . . ? F13 B10 F11 105.0(11) . . ? C02B O001 C05B 109.4(18) . . ? C02B O001 C05A 94.7(14) . . ? C05B O001 C05A 38.7(14) . . ? C02B O001 C02A 41.0(12) . . ? C05B O001 C02A 99.4(18) . . ? C05A O001 C02A 112.0(13) . . ? O001 C02A C003 94.1(14) . . ? O001 C02B C003 107.5(16) . . ? C004 C003 C02B 104.5(14) . . ? C004 C003 C02A 104.8(12) . . ? C02B C003 C02A 38.2(12) . . ? C003 C004 C05B 104.2(16) . . ? C003 C004 C05A 97.1(12) . . ? C05B C004 C05A 36.9(14) . . ? O001 C05A C004 104.6(13) . . ? O001 C05B C004 108(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N23 H23A F12 0.92 2.08 2.979(10) 164.4 . N23 H23A F12A 0.92 2.37 3.21(6) 152.6 . N23 H23A F13A 0.92 2.40 3.24(5) 151.6 . C03 H03A O001 0.95 2.81 3.344(12) 116.4 . N23 H23B F11 0.92 2.14 3.024(10) 160.4 4_566 N23 H23B F11A 0.92 2.07 2.75(6) 129.7 4_566 N23 H23B F14A 0.92 3.12 3.93(8) 146.8 4_566 C02A H02D F14A 0.99 2.18 3.06(7) 148.4 1_655 C05 H05A F12A 0.95 2.61 2.99(5) 104.5 3_655 C02 H02A F13 0.95 2.91 3.154(12) 96.1 3_665 C02 H02A F14 0.95 2.48 3.271(14) 141.0 3_665 C02B H02E F14 0.99 2.92 3.69(3) 136.0 2_644 C02B H02E F14A 0.99 3.20 4.05(8) 144.9 2_644 C05A H05C F12 0.99 2.77 3.55(2) 135.6 4_665 C05A H05C F13A 0.99 2.49 2.90(6) 104.5 4_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.653 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.120 data_mp2 _database_code_depnum_ccdc_archive 'CCDC 233561' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H27 Ag2 F12 N13 P2' _chemical_formula_weight 1027.29 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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.1092(4) _cell_length_b 15.3225(4) _cell_length_c 15.7434(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3644.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6402 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 17193 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 29.04 _reflns_number_total 4507 _reflns_number_gt 2117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0449P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00068(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4507 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _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 -0.5000 0.78110(3) 0.7500 0.07733(16) Uani 1 2 d S . . Ag2 Ag -0.5000 0.49231(3) 0.7500 0.07566(15) Uani 1 2 d S . . N1 N -0.53372(15) 0.82675(16) 0.61605(14) 0.0549(6) Uani 1 1 d . . . C2 C -0.5680(2) 0.9044(2) 0.5975(2) 0.0669(8) Uani 1 1 d . . . H2A H -0.5825 0.9431 0.6425 0.080 Uiso 1 1 calc R . . C3 C -0.5831(2) 0.9304(2) 0.5156(2) 0.0710(9) Uani 1 1 d . . . H3A H -0.6080 0.9864 0.5057 0.085 Uiso 1 1 calc R . . N4 N -0.56424(19) 0.88044(18) 0.45007(16) 0.0735(8) Uani 1 1 d . . . C5 C -0.5300(2) 0.8033(2) 0.46902(19) 0.0689(9) Uani 1 1 d . . . H5A H -0.5153 0.7652 0.4235 0.083 Uiso 1 1 calc R . . C6 C -0.51445(16) 0.77480(18) 0.55079(17) 0.0513(7) Uani 1 1 d . . . C7 C -0.47421(18) 0.68845(19) 0.56861(19) 0.0563(7) Uani 1 1 d . . . N8 N -0.44927(15) 0.67628(16) 0.64449(15) 0.0573(6) Uani 1 1 d . . . N9 N -0.41616(15) 0.59508(16) 0.66656(14) 0.0600(6) Uani 1 1 d . . . C10 C -0.33220(19) 0.5852(2) 0.66841(17) 0.0571(7) Uani 1 1 d . . . C11 C -0.29933(18) 0.5014(2) 0.70110(19) 0.0569(8) Uani 1 1 d . . . N12 N -0.35506(16) 0.45057(17) 0.74396(15) 0.0649(7) Uani 1 1 d . . . C13 C -0.3223(2) 0.3771(2) 0.7763(2) 0.0762(10) Uani 1 1 d . . . H13A H -0.3601 0.3390 0.8071 0.091 Uiso 1 1 calc R . . C14 C -0.2343(3) 0.3554(2) 0.7660(2) 0.0802(11) Uani 1 1 d . . . H14A H -0.2128 0.3037 0.7921 0.096 Uiso 1 1 calc R . . N15 N -0.17925(19) 0.4030(2) 0.72161(19) 0.0785(8) Uani 1 1 d . . . C16 C -0.21287(19) 0.4751(2) 0.68911(19) 0.0701(9) Uani 1 1 d . . . H16A H -0.1754 0.5109 0.6555 0.084 Uiso 1 1 calc R . . C17 C -0.2685(2) 0.6536(2) 0.6403(3) 0.0911(12) Uani 1 1 d . . . H17A H -0.2969 0.7110 0.6435 0.137 Uiso 1 1 calc R . . H17B H -0.2504 0.6421 0.5815 0.137 Uiso 1 1 calc R . . H17C H -0.2163 0.6528 0.6772 0.137 Uiso 1 1 calc R . . C18 C -0.4647(3) 0.6226(2) 0.4983(2) 0.0893(12) Uani 1 1 d . . . H18A H -0.4459 0.5666 0.5221 0.134 Uiso 1 1 calc R . . H18B H -0.4204 0.6431 0.4575 0.134 Uiso 1 1 calc R . . H18C H -0.5217 0.6154 0.4694 0.134 Uiso 1 1 calc R . . P1 P -0.24962(7) 0.86316(6) 0.43558(8) 0.0843(3) Uani 1 1 d . . . F1 F -0.32562(18) 0.87133(15) 0.50389(17) 0.1239(9) Uani 1 1 d . A . F2 F -0.17428(18) 0.85212(18) 0.36760(19) 0.1475(11) Uani 1 1 d . A . F3 F -0.3116(9) 0.9134(13) 0.3753(5) 0.151(6) Uani 0.530(17) 1 d P A 1 F4 F -0.1891(7) 0.8232(12) 0.5116(9) 0.157(5) Uani 0.530(17) 1 d P A 1 F5 F -0.2155(8) 0.9534(7) 0.4687(9) 0.153(4) Uani 0.530(17) 1 d P A 1 F6 F -0.2909(11) 0.7721(8) 0.4203(10) 0.162(7) Uani 0.530(17) 1 d P A 1 F3A F -0.2594(12) 0.9595(7) 0.4068(16) 0.159(8) Uani 0.470(17) 1 d P A 2 F4A F -0.2288(11) 0.7655(8) 0.4523(9) 0.135(5) Uani 0.470(17) 1 d P A 2 F5A F -0.1821(7) 0.8867(16) 0.4987(10) 0.187(7) Uani 0.470(17) 1 d P A 2 F6A F -0.3151(6) 0.8354(15) 0.3610(6) 0.161(5) Uani 0.470(17) 1 d P A 2 N01 N -0.5000 0.2661(5) 0.7500 0.1130(18) Uani 1 2 d S . . C02 C -0.5000 0.1917(6) 0.7500 0.0847(17) Uani 1 2 d S . . C03 C -0.5000 0.0987(5) 0.7500 0.113(2) Uani 1 2 d S . . H03C H -0.4489 0.0774 0.7822 0.170 Uiso 0.50 1 calc PR . . H03B H -0.4964 0.0774 0.6914 0.170 Uiso 0.50 1 calc PR . . H03A H -0.5546 0.0774 0.7763 0.170 Uiso 0.50 1 calc PR . . 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 0.0975(3) 0.0911(3) 0.0434(2) 0.000 -0.00517(19) 0.000 Ag2 0.0528(2) 0.0771(3) 0.0971(3) 0.000 0.01876(19) 0.000 N1 0.0568(13) 0.0613(15) 0.0468(14) -0.0014(13) -0.0022(12) -0.0014(13) C2 0.073(2) 0.063(2) 0.064(2) -0.0080(17) 0.0006(17) 0.0002(18) C3 0.072(2) 0.066(2) 0.075(2) 0.0119(19) 0.0020(19) 0.0135(17) N4 0.0771(19) 0.084(2) 0.0592(18) 0.0075(15) -0.0016(15) 0.0126(16) C5 0.079(2) 0.079(2) 0.0483(19) -0.0027(16) 0.0048(17) 0.0103(18) C6 0.0460(17) 0.0577(17) 0.0501(16) 0.0012(14) -0.0003(13) -0.0035(13) C7 0.0557(17) 0.0619(19) 0.0514(18) -0.0027(15) 0.0037(14) -0.0044(14) N8 0.0540(14) 0.0624(16) 0.0555(15) 0.0060(12) 0.0062(12) 0.0021(13) N9 0.0569(15) 0.0665(16) 0.0566(15) 0.0059(12) 0.0070(12) 0.0056(13) C10 0.0536(18) 0.067(2) 0.0510(17) 0.0041(15) 0.0046(14) 0.0002(16) C11 0.0487(16) 0.070(2) 0.0522(18) -0.0030(15) 0.0021(14) 0.0022(16) N12 0.0587(15) 0.0596(16) 0.0763(17) 0.0034(14) 0.0099(14) 0.0013(13) C13 0.070(2) 0.068(2) 0.091(3) 0.0052(18) 0.0031(19) 0.0018(18) C14 0.077(3) 0.071(2) 0.092(3) 0.0062(18) -0.007(2) 0.0155(19) N15 0.0631(17) 0.094(2) 0.0785(19) 0.0047(17) 0.0074(15) 0.0182(18) C16 0.0559(18) 0.092(3) 0.063(2) 0.0083(18) 0.0047(16) 0.0123(17) C17 0.060(2) 0.084(3) 0.129(3) 0.030(2) 0.003(2) -0.0067(18) C18 0.121(3) 0.079(3) 0.068(3) -0.0187(18) -0.012(2) 0.021(2) P1 0.0778(7) 0.0811(7) 0.0940(8) 0.0034(6) -0.0001(7) 0.0148(6) F1 0.1130(19) 0.124(2) 0.135(2) 0.0081(14) 0.0307(16) 0.0153(15) F2 0.128(2) 0.160(3) 0.155(2) 0.0295(18) 0.0583(19) 0.0460(17) F3 0.154(8) 0.203(16) 0.095(5) 0.020(6) -0.018(5) 0.084(8) F4 0.122(6) 0.176(11) 0.173(8) 0.063(9) -0.005(6) 0.061(7) F5 0.146(9) 0.097(7) 0.215(9) -0.005(6) -0.019(7) -0.037(5) F6 0.171(10) 0.101(7) 0.213(12) -0.079(7) 0.054(9) -0.043(7) F3A 0.140(12) 0.092(6) 0.246(19) 0.045(9) 0.100(12) 0.044(7) F4A 0.152(10) 0.109(7) 0.143(8) 0.037(6) 0.030(7) 0.054(7) F5A 0.166(8) 0.216(18) 0.178(11) -0.064(11) -0.081(7) 0.030(11) F6A 0.130(6) 0.206(14) 0.148(7) -0.019(9) -0.056(5) 0.028(7) N01 0.106(4) 0.134(5) 0.100(4) 0.000 -0.011(3) 0.000 C02 0.067(3) 0.138(6) 0.049(3) 0.000 0.001(2) 0.000 C03 0.138(6) 0.119(5) 0.083(4) 0.000 0.022(4) 0.000 _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 2.280(2) 3_456 ? Ag1 N1 2.280(2) . ? Ag1 N8 2.434(2) . ? Ag1 N8 2.434(2) 3_456 ? Ag2 N12 2.283(2) . ? Ag2 N12 2.283(2) 3_456 ? Ag2 N9 2.410(2) . ? Ag2 N9 2.410(2) 3_456 ? N1 C2 1.331(4) . ? N1 C6 1.332(3) . ? C2 C3 1.368(4) . ? C3 N4 1.316(4) . ? N4 C5 1.324(4) . ? C5 C6 1.380(4) . ? C6 C7 1.483(4) . ? C7 N8 1.266(3) . ? C7 C18 1.504(4) . ? N8 N9 1.385(3) . ? N9 C10 1.278(3) . ? C10 C11 1.469(4) . ? C10 C17 1.491(4) . ? C11 N12 1.331(3) . ? C11 C16 1.380(4) . ? N12 C13 1.331(4) . ? C13 C14 1.380(5) . ? C14 N15 1.308(4) . ? N15 C16 1.319(4) . ? P1 F5A 1.469(10) . ? P1 F3 1.539(7) . ? P1 F6 1.547(6) . ? P1 F3A 1.551(8) . ? P1 F4A 1.551(9) . ? P1 F5 1.565(8) . ? P1 F2 1.572(3) . ? P1 F1 1.578(3) . ? P1 F6A 1.593(8) . ? P1 F4 1.625(9) . ? N01 C02 1.139(8) . ? C02 C03 1.425(9) . ? 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 N1 144.26(12) 3_456 . ? N1 Ag1 N8 139.76(8) 3_456 . ? N1 Ag1 N8 69.00(9) . . ? N1 Ag1 N8 69.00(9) 3_456 3_456 ? N1 Ag1 N8 139.76(8) . 3_456 ? N8 Ag1 N8 97.43(11) . 3_456 ? N12 Ag2 N12 147.47(13) . 3_456 ? N12 Ag2 N9 69.89(9) . . ? N12 Ag2 N9 135.21(8) 3_456 . ? N12 Ag2 N9 135.21(8) . 3_456 ? N12 Ag2 N9 69.89(9) 3_456 3_456 ? N9 Ag2 N9 98.42(11) . 3_456 ? C2 N1 C6 116.8(2) . . ? C2 N1 Ag1 124.39(19) . . ? C6 N1 Ag1 118.77(19) . . ? N1 C2 C3 122.1(3) . . ? N4 C3 C2 122.3(3) . . ? C3 N4 C5 115.3(3) . . ? N4 C5 C6 124.0(3) . . ? N1 C6 C5 119.6(3) . . ? N1 C6 C7 118.5(2) . . ? C5 C6 C7 121.9(3) . . ? N8 C7 C6 115.6(3) . . ? N8 C7 C18 124.6(3) . . ? C6 C7 C18 119.9(3) . . ? C7 N8 N9 118.5(2) . . ? C7 N8 Ag1 116.9(2) . . ? N9 N8 Ag1 122.35(16) . . ? C10 N9 N8 118.1(3) . . ? C10 N9 Ag2 115.6(2) . . ? N8 N9 Ag2 122.25(16) . . ? N9 C10 C11 116.6(3) . . ? N9 C10 C17 123.4(3) . . ? C11 C10 C17 120.0(3) . . ? N12 C11 C16 119.8(3) . . ? N12 C11 C10 118.4(2) . . ? C16 C11 C10 121.9(3) . . ? C13 N12 C11 117.0(3) . . ? C13 N12 Ag2 125.3(2) . . ? C11 N12 Ag2 117.63(19) . . ? N12 C13 C14 121.1(3) . . ? N15 C14 C13 122.8(3) . . ? C14 N15 C16 115.4(3) . . ? N15 C16 C11 123.8(3) . . ? F5A P1 F3 135.8(6) . . ? F5A P1 F6 127.4(7) . . ? F3 P1 F6 96.3(6) . . ? F5A P1 F3A 91.7(6) . . ? F3 P1 F3A 44.4(5) . . ? F6 P1 F3A 140.7(8) . . ? F5A P1 F4A 88.9(6) . . ? F3 P1 F4A 135.3(6) . . ? F6 P1 F4A 40.4(4) . . ? F3A P1 F4A 170.6(5) . . ? F5A P1 F5 47.8(5) . . ? F3 P1 F5 88.0(5) . . ? F6 P1 F5 168.9(5) . . ? F3A P1 F5 44.6(6) . . ? F4A P1 F5 136.7(6) . . ? F5A P1 F2 89.1(6) . . ? F3 P1 F2 94.3(4) . . ? F6 P1 F2 95.1(3) . . ? F3A P1 F2 88.4(3) . . ? F4A P1 F2 82.2(4) . . ? F5 P1 F2 94.8(4) . . ? F5A P1 F1 91.4(6) . . ? F3 P1 F1 86.4(4) . . ? F6 P1 F1 83.4(3) . . ? F3A P1 F1 93.1(3) . . ? F4A P1 F1 96.2(4) . . ? F5 P1 F1 86.7(3) . . ? F2 P1 F1 178.36(15) . . ? F5A P1 F6A 174.4(7) . . ? F3 P1 F6A 45.7(4) . . ? F6 P1 F6A 52.7(4) . . ? F3A P1 F6A 88.8(7) . . ? F4A P1 F6A 89.6(5) . . ? F5 P1 F6A 133.3(5) . . ? F2 P1 F6A 85.3(4) . . ? F1 P1 F6A 94.1(4) . . ? F5A P1 F4 37.3(7) . . ? F3 P1 F4 169.8(5) . . ? F6 P1 F4 90.1(6) . . ? F3A P1 F4 128.9(8) . . ? F4A P1 F4 52.9(4) . . ? F5 P1 F4 84.4(5) . . ? F2 P1 F4 93.1(4) . . ? F1 P1 F4 86.4(4) . . ? F6A P1 F4 142.3(6) . . ? N01 C02 C03 180.000(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2A F3 0.95 2.73 3.359(13) 124.0 5_476 C3 H3A F1 0.95 2.40 3.351(4) 174.1 5_476 C5 H5A N01 0.95 2.78 3.637(4) 149.9 5_466 C13 H13A F6 0.95 2.68 3.254(9) 119.7 7_566 C14 H14A F6 0.95 2.61 3.233(8) 123.5 7_566 C03 H03A N4 0.98 2.81 3.311(3) 112.2 7_566 C03 H03C F6A 0.98 2.72 3.447(11) 131.1 7_566 C03 H03C F3 0.98 2.54 3.468(13) 157.3 7_566 C2 H2A N15 0.95 2.66 3.307(4) 125.6 6_567 C14 H14A F2 0.95 2.73 3.674(5) 172.2 7_566 C16 H16A N4 0.95 2.89 3.840(4) 178.7 4_566 C03 H03A C16 0.98 2.91 3.854(5) 161.9 6_557 _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 29.04 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.473 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.058