# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Qingxiang Liu' _publ_contact_author_email QXLIU@EYOU.COM _publ_section_title ; Macrocyclic dinuclear silver(I) complexes based on bis(N-heterocyclic carbene) ligands: synthesis and structural studies ; loop_ _publ_author_name 'Qingxiang Liu.' 'Shu-Sheng Ge.' 'Jian-Hua Guo.' 'Shu-Wen Liu.' ; Hai-Bin Song ; 'Xiu-Guang Wang.' 'Xiao-Qiong Yang.' 'Yan Zang.' 'Xiao-Jun Zhao.' # Attachment 'CIF_2a.cif' data_080513a _database_code_depnum_ccdc_archive 'CCDC 704839' #TrackingRef 'CIF_2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 Ag4 Br4 N8' _chemical_formula_weight 1215.74 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' Br Br -0.2901 2.4595 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.632(2) _cell_length_b 9.769(2) _cell_length_c 10.179(3) _cell_angle_alpha 83.769(4) _cell_angle_beta 71.882(4) _cell_angle_gamma 83.372(4) _cell_volume 901.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1976 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.85 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 6.603 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.223 _exptl_absorpt_correction_T_max 0.305 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4634 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3184 _reflns_number_gt 2523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+9.9335P] 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 SHELXL _refine_ls_extinction_coef 0.0097(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3164 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.18255(8) 0.37430(8) 0.75587(8) 0.0474(3) Uani 1 1 d . . . Ag2 Ag 0.63564(16) 0.8413(2) 0.9469(2) 0.1699(11) Uani 1 1 d . . . Br1 Br 0.81000(16) 0.66368(13) 0.81636(14) 0.0707(4) Uani 1 1 d . . . Br2 Br 0.50063(15) 0.92451(16) 1.18525(12) 0.0713(4) Uani 1 1 d . . . N1 N 0.3859(8) 0.6051(8) 0.7369(7) 0.0367(17) Uani 1 1 d . . . N2 N 0.3356(8) 0.6053(8) 0.5481(8) 0.0424(18) Uani 1 1 d . . . N3 N 0.0821(9) 0.0865(9) 0.7554(9) 0.049(2) Uani 1 1 d . . . N4 N -0.0742(8) 0.1941(8) 0.9158(8) 0.0419(18) Uani 1 1 d . . . C1 C 0.1432(16) 0.6655(17) 0.4362(17) 0.091(5) Uani 1 1 d . . . H1A H 0.0722 0.6628 0.5266 0.136 Uiso 1 1 calc R . . H1B H 0.1020 0.6350 0.3710 0.136 Uiso 1 1 calc R . . H1C H 0.1696 0.7584 0.4083 0.136 Uiso 1 1 calc R . . C2 C 0.2745(13) 0.5741(13) 0.4405(11) 0.059(3) Uani 1 1 d . . . H2A H 0.2496 0.4790 0.4574 0.070 Uiso 1 1 calc R . . H2B H 0.3487 0.5829 0.3510 0.070 Uiso 1 1 calc R . . C3 C 0.4256(11) 0.7089(10) 0.5319(11) 0.049(2) Uani 1 1 d . . . H3 H 0.4579 0.7681 0.4528 0.059 Uiso 1 1 calc R . . C4 C 0.4583(11) 0.7097(10) 0.6489(10) 0.046(2) Uani 1 1 d . . . H4 H 0.5177 0.7685 0.6680 0.055 Uiso 1 1 calc R . . C5 C 0.3113(10) 0.5387(9) 0.6754(9) 0.038(2) Uani 1 1 d . . . C6 C 0.3920(11) 0.5690(11) 0.8786(9) 0.043(2) Uani 1 1 d . . . H6A H 0.4937 0.5567 0.8777 0.052 Uiso 1 1 calc R . . H6B H 0.3494 0.4820 0.9130 0.052 Uiso 1 1 calc R . . C7 C -0.3110(11) 0.3212(12) 1.0246(11) 0.049(2) Uani 1 1 d . . . H7A H -0.3225 0.3474 0.9337 0.059 Uiso 1 1 calc R . . H7B H -0.3547 0.2346 1.0586 0.059 Uiso 1 1 calc R . . C8 C -0.1491(10) 0.2995(10) 1.0111(11) 0.044(2) Uani 1 1 d . . . H8A H -0.1048 0.3860 0.9777 0.052 Uiso 1 1 calc R . . H8B H -0.1369 0.2717 1.1015 0.052 Uiso 1 1 calc R . . C9 C -0.1235(14) 0.0686(12) 0.9162(13) 0.064(3) Uani 1 1 d . . . H9 H -0.2091 0.0355 0.9765 0.076 Uiso 1 1 calc R . . C10 C -0.0258(13) 0.0019(11) 0.8138(12) 0.057(3) Uani 1 1 d . . . H10 H -0.0312 -0.0853 0.7880 0.069 Uiso 1 1 calc R . . C11 C 0.0546(10) 0.2090(10) 0.8158(10) 0.040(2) Uani 1 1 d . . . C12 C 0.2135(13) 0.0490(15) 0.6396(13) 0.069(3) Uani 1 1 d . . . H12A H 0.2936 0.0994 0.6423 0.083 Uiso 1 1 calc R . . H12B H 0.2422 -0.0488 0.6519 0.083 Uiso 1 1 calc R . . C13 C 0.1907(17) 0.078(2) 0.5069(15) 0.104(6) Uani 1 1 d . . . H13A H 0.1138 0.0264 0.5022 0.156 Uiso 1 1 calc R . . H13B H 0.2795 0.0529 0.4358 0.156 Uiso 1 1 calc R . . H13C H 0.1635 0.1753 0.4934 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0406(4) 0.0486(5) 0.0504(5) -0.0041(3) -0.0059(3) -0.0149(3) Ag2 0.0754(9) 0.1604(16) 0.255(2) -0.1480(16) 0.0356(11) -0.0512(10) Br1 0.0835(9) 0.0533(7) 0.0662(8) -0.0048(6) -0.0058(6) -0.0165(6) Br2 0.0727(8) 0.0977(10) 0.0422(6) 0.0079(6) -0.0175(6) -0.0142(7) N1 0.031(4) 0.041(4) 0.036(4) -0.003(3) -0.008(3) -0.002(3) N2 0.041(4) 0.044(5) 0.039(4) -0.007(4) -0.010(3) 0.007(4) N3 0.046(5) 0.046(5) 0.052(5) -0.012(4) -0.012(4) 0.002(4) N4 0.037(4) 0.044(5) 0.040(4) -0.004(3) -0.002(3) -0.011(3) C1 0.070(9) 0.116(12) 0.098(11) -0.021(9) -0.051(8) 0.026(9) C2 0.065(7) 0.070(7) 0.043(6) -0.011(5) -0.022(5) 0.007(6) C3 0.053(6) 0.041(6) 0.047(6) 0.010(5) -0.010(5) -0.005(5) C4 0.046(6) 0.036(5) 0.049(6) 0.003(4) -0.003(4) -0.011(4) C5 0.035(5) 0.036(5) 0.040(5) -0.007(4) -0.007(4) 0.005(4) C6 0.042(5) 0.051(6) 0.034(5) 0.001(4) -0.010(4) -0.003(4) C7 0.043(5) 0.061(6) 0.044(6) -0.006(5) -0.011(4) -0.007(5) C8 0.035(5) 0.044(5) 0.050(6) -0.013(4) -0.006(4) -0.004(4) C9 0.063(7) 0.054(7) 0.066(7) -0.008(6) 0.000(6) -0.024(6) C10 0.060(7) 0.040(6) 0.071(7) -0.008(5) -0.014(6) -0.018(5) C11 0.037(5) 0.039(5) 0.043(5) 0.000(4) -0.013(4) -0.005(4) C12 0.050(7) 0.083(9) 0.073(8) -0.030(7) -0.014(6) 0.004(6) C13 0.072(9) 0.159(17) 0.068(9) -0.023(10) -0.009(8) 0.025(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C11 2.068(9) . ? Ag1 C5 2.081(9) . ? Ag2 Br1 2.4570(19) . ? Ag2 Br2 2.542(2) . ? Ag2 Br2 2.916(3) 2_677 ? Br2 Ag2 2.916(3) 2_677 ? N1 C5 1.343(12) . ? N1 C4 1.382(12) . ? N1 C6 1.465(12) . ? N2 C5 1.350(12) . ? N2 C3 1.371(13) . ? N2 C2 1.467(13) . ? N3 C10 1.351(13) . ? N3 C11 1.366(12) . ? N3 C12 1.478(14) . ? N4 C11 1.349(12) . ? N4 C9 1.364(13) . ? N4 C8 1.460(12) . ? C1 C2 1.472(17) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.324(15) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 C7 1.513(14) 2_567 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C6 1.513(14) 2_567 ? C7 C8 1.514(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.339(16) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.429(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 C11 Ag1 C5 174.3(4) . . ? Br1 Ag2 Br2 145.88(14) . . ? Br1 Ag2 Br2 123.14(11) . 2_677 ? Br2 Ag2 Br2 90.98(6) . 2_677 ? Ag2 Br2 Ag2 89.02(6) . 2_677 ? C5 N1 C4 111.6(8) . . ? C5 N1 C6 124.1(8) . . ? C4 N1 C6 124.3(8) . . ? C5 N2 C3 110.6(8) . . ? C5 N2 C2 125.6(9) . . ? C3 N2 C2 123.8(9) . . ? C10 N3 C11 112.0(8) . . ? C10 N3 C12 123.2(9) . . ? C11 N3 C12 124.8(9) . . ? C11 N4 C9 111.2(8) . . ? C11 N4 C8 123.7(8) . . ? C9 N4 C8 125.0(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C1 112.8(10) . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 N2 107.9(9) . . ? C4 C3 H3 126.1 . . ? N2 C3 H3 126.1 . . ? C3 C4 N1 105.8(9) . . ? C3 C4 H4 127.1 . . ? N1 C4 H4 127.1 . . ? N1 C5 N2 104.1(8) . . ? N1 C5 Ag1 128.9(7) . . ? N2 C5 Ag1 127.0(7) . . ? N1 C6 C7 112.1(8) . 2_567 ? N1 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 2_567 . ? N1 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 2_567 . ? H6A C6 H6B 107.9 . . ? C6 C7 C8 113.0(8) 2_567 . ? C6 C7 H7A 109.0 2_567 . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 2_567 . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N4 C8 C7 111.5(8) . . ? N4 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N4 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 N4 107.3(9) . . ? C10 C9 H9 126.3 . . ? N4 C9 H9 126.3 . . ? C9 C10 N3 106.3(9) . . ? C9 C10 H10 126.8 . . ? N3 C10 H10 126.8 . . ? N4 C11 N3 103.1(8) . . ? N4 C11 Ag1 130.8(7) . . ? N3 C11 Ag1 126.1(7) . . ? C13 C12 N3 113.0(11) . . ? C13 C12 H12A 109.0 . . ? N3 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? N3 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Ag2 Br2 Ag2 179.68(13) . . . 2_677 ? Br2 Ag2 Br2 Ag2 0.0 2_677 . . 2_677 ? C5 N2 C2 C1 97.8(13) . . . . ? C3 N2 C2 C1 -81.7(14) . . . . ? C5 N2 C3 C4 -0.5(11) . . . . ? C2 N2 C3 C4 179.1(9) . . . . ? N2 C3 C4 N1 -0.3(11) . . . . ? C5 N1 C4 C3 1.0(11) . . . . ? C6 N1 C4 C3 179.8(9) . . . . ? C4 N1 C5 N2 -1.2(10) . . . . ? C6 N1 C5 N2 179.9(8) . . . . ? C4 N1 C5 Ag1 -179.8(7) . . . . ? C6 N1 C5 Ag1 1.4(12) . . . . ? C3 N2 C5 N1 1.0(10) . . . . ? C2 N2 C5 N1 -178.5(8) . . . . ? C3 N2 C5 Ag1 179.6(7) . . . . ? C2 N2 C5 Ag1 0.1(13) . . . . ? C11 Ag1 C5 N1 -168(3) . . . . ? C11 Ag1 C5 N2 13(4) . . . . ? C5 N1 C6 C7 -111.2(10) . . . 2_567 ? C4 N1 C6 C7 70.1(11) . . . 2_567 ? C11 N4 C8 C7 134.1(10) . . . . ? C9 N4 C8 C7 -46.5(14) . . . . ? C6 C7 C8 N4 -179.3(8) 2_567 . . . ? C11 N4 C9 C10 -0.7(14) . . . . ? C8 N4 C9 C10 179.8(10) . . . . ? N4 C9 C10 N3 1.4(14) . . . . ? C11 N3 C10 C9 -1.6(13) . . . . ? C12 N3 C10 C9 178.5(11) . . . . ? C9 N4 C11 N3 -0.2(11) . . . . ? C8 N4 C11 N3 179.3(9) . . . . ? C9 N4 C11 Ag1 177.6(8) . . . . ? C8 N4 C11 Ag1 -2.9(14) . . . . ? C10 N3 C11 N4 1.1(11) . . . . ? C12 N3 C11 N4 -179.0(10) . . . . ? C10 N3 C11 Ag1 -176.9(8) . . . . ? C12 N3 C11 Ag1 3.0(14) . . . . ? C5 Ag1 C11 N4 -129(3) . . . . ? C5 Ag1 C11 N3 49(4) . . . . ? C10 N3 C12 C13 85.2(17) . . . . ? C11 N3 C12 C13 -94.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.667 _refine_diff_density_min -3.082 _refine_diff_density_rms 0.168 # Attachment 'CIF_2b.cif' data_r071105d _database_code_depnum_ccdc_archive 'CCDC 704840' #TrackingRef 'CIF_2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H24 Ag F6 N4 P' _chemical_formula_weight 609.30 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 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 11.245(2) _cell_length_b 10.293(2) _cell_length_c 20.831(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.69(3) _cell_angle_gamma 90.00 _cell_volume 2408.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5227 _cell_measurement_theta_min 1.813 _cell_measurement_theta_max 27.900 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17733 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4256 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.5792P] 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 4244 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.622286(16) -0.062615(17) 0.615435(9) 0.01753(8) Uani 1 1 d . . . N1 N 0.87888(18) 0.0332(2) 0.59832(10) 0.0191(5) Uani 1 1 d . . . N2 N 0.76182(18) 0.12863(19) 0.52954(10) 0.0178(5) Uani 1 1 d . . . N3 N 0.53993(17) 0.30613(19) 0.37745(9) 0.0154(4) Uani 1 1 d . . . N4 N 0.54775(18) 0.19469(19) 0.29109(10) 0.0168(4) Uani 1 1 d . . . C1 C 1.0563(2) -0.2536(3) 0.64831(13) 0.0250(6) Uani 1 1 d . . . H1 H 1.1076 -0.2124 0.6781 0.030 Uiso 1 1 calc R . . C2 C 1.0813(2) -0.3792(3) 0.62807(14) 0.0289(7) Uani 1 1 d . . . H2 H 1.1496 -0.4210 0.6443 0.035 Uiso 1 1 calc R . . C3 C 1.0061(3) -0.4421(3) 0.58428(14) 0.0286(7) Uani 1 1 d . . . H3 H 1.0223 -0.5268 0.5718 0.034 Uiso 1 1 calc R . . C4 C 0.9058(2) -0.3783(3) 0.55888(13) 0.0262(6) Uani 1 1 d . . . H4 H 0.8554 -0.4198 0.5287 0.031 Uiso 1 1 calc R . . C5 C 0.8806(2) -0.2531(3) 0.57831(12) 0.0222(6) Uani 1 1 d . . . H5 H 0.8136 -0.2109 0.5607 0.027 Uiso 1 1 calc R . . C6 C 0.9543(2) -0.1893(2) 0.62395(12) 0.0196(5) Uani 1 1 d . . . C7 C 0.9242(3) -0.0559(2) 0.64874(13) 0.0247(6) Uani 1 1 d . . . H7A H 0.8648 -0.0646 0.6808 0.030 Uiso 1 1 calc R . . H7B H 0.9950 -0.0183 0.6697 0.030 Uiso 1 1 calc R . . C8 C 0.7623(2) 0.0443(2) 0.57912(12) 0.0161(5) Uani 1 1 d . . . C9 C 0.8760(2) 0.1697(3) 0.51781(13) 0.0237(6) Uani 1 1 d . . . H9 H 0.8975 0.2278 0.4861 0.028 Uiso 1 1 calc R . . C10 C 0.9499(2) 0.1100(3) 0.56084(13) 0.0240(6) Uani 1 1 d . . . H10 H 1.0323 0.1183 0.5648 0.029 Uiso 1 1 calc R . . C11 C 0.6553(2) 0.1635(2) 0.48968(13) 0.0203(6) Uani 1 1 d . . . H11A H 0.5869 0.1192 0.5061 0.024 Uiso 1 1 calc R . . H11B H 0.6651 0.1334 0.4461 0.024 Uiso 1 1 calc R . . C12 C 0.6313(2) 0.3092(2) 0.48836(12) 0.0201(6) Uani 1 1 d . . . H12A H 0.7003 0.3542 0.4731 0.024 Uiso 1 1 calc R . . H12B H 0.6184 0.3393 0.5316 0.024 Uiso 1 1 calc R . . C13 C 0.5223(2) 0.3420(2) 0.44471(12) 0.0201(6) Uani 1 1 d . . . H13A H 0.4536 0.2961 0.4597 0.024 Uiso 1 1 calc R . . H13B H 0.5064 0.4344 0.4472 0.024 Uiso 1 1 calc R . . C14 C 0.5011(2) 0.1935(2) 0.34994(12) 0.0162(5) Uani 1 1 d . . . C15 C 0.6129(2) 0.3064(2) 0.28159(13) 0.0200(5) Uani 1 1 d . . . H15 H 0.6522 0.3288 0.2449 0.024 Uiso 1 1 calc R . . C16 C 0.6080(2) 0.3764(2) 0.33622(12) 0.0186(5) Uani 1 1 d . . . H16 H 0.6437 0.4566 0.3445 0.022 Uiso 1 1 calc R . . C17 C 0.5277(2) 0.0904(2) 0.24348(13) 0.0215(6) Uani 1 1 d . . . H17A H 0.5528 0.0082 0.2625 0.026 Uiso 1 1 calc R . . H17B H 0.5762 0.1066 0.2070 0.026 Uiso 1 1 calc R . . C18 C 0.3987(2) 0.0803(2) 0.22024(12) 0.0187(5) Uani 1 1 d . . . C19 C 0.3386(2) -0.0378(3) 0.22246(13) 0.0241(6) Uani 1 1 d . . . H19 H 0.3774 -0.1108 0.2394 0.029 Uiso 1 1 calc R . . C20 C 0.2208(3) -0.0472(3) 0.19941(14) 0.0280(6) Uani 1 1 d . . . H20 H 0.1817 -0.1268 0.2002 0.034 Uiso 1 1 calc R . . C21 C 0.1617(3) 0.0613(3) 0.17532(13) 0.0277(6) Uani 1 1 d . . . H21 H 0.0825 0.0552 0.1607 0.033 Uiso 1 1 calc R . . C22 C 0.2206(3) 0.1789(3) 0.17305(13) 0.0289(6) Uani 1 1 d . . . H22 H 0.1811 0.2521 0.1568 0.035 Uiso 1 1 calc R . . C23 C 0.3389(3) 0.1880(3) 0.19503(13) 0.0264(6) Uani 1 1 d . . . H23 H 0.3784 0.2671 0.1928 0.032 Uiso 1 1 calc R . . P1 P 0.32237(6) 0.22643(7) 0.61436(3) 0.02097(16) Uani 1 1 d . . . F1 F 0.3187(3) 0.1499(2) 0.54905(10) 0.0796(9) Uani 1 1 d . . . F2 F 0.2686(2) 0.10327(18) 0.64907(10) 0.0592(6) Uani 1 1 d . . . F3 F 0.1927(2) 0.2783(3) 0.59904(16) 0.1004(10) Uani 1 1 d . . . F4 F 0.3238(2) 0.30602(19) 0.67989(9) 0.0635(7) Uani 1 1 d . . . F5 F 0.3771(2) 0.35028(18) 0.58030(9) 0.0582(6) Uani 1 1 d . . . F6 F 0.4506(2) 0.1755(3) 0.63120(16) 0.0952(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01964(11) 0.01464(11) 0.01863(12) 0.00173(8) 0.00441(8) -0.00130(7) N1 0.0206(11) 0.0179(11) 0.0188(12) 0.0001(9) 0.0000(9) 0.0000(9) N2 0.0195(11) 0.0147(10) 0.0194(12) 0.0033(9) 0.0018(9) -0.0003(9) N3 0.0169(10) 0.0154(10) 0.0139(11) 0.0005(8) 0.0013(8) 0.0014(8) N4 0.0184(11) 0.0164(10) 0.0158(11) -0.0022(9) 0.0027(8) -0.0020(9) C1 0.0219(14) 0.0267(15) 0.0262(15) 0.0114(12) -0.0019(11) -0.0026(11) C2 0.0214(14) 0.0289(15) 0.0370(18) 0.0170(13) 0.0100(13) 0.0071(12) C3 0.0364(17) 0.0223(14) 0.0285(16) 0.0080(12) 0.0163(13) 0.0071(12) C4 0.0315(15) 0.0251(15) 0.0225(15) -0.0003(12) 0.0069(12) 0.0006(12) C5 0.0203(13) 0.0252(14) 0.0214(14) 0.0009(12) 0.0021(11) 0.0036(11) C6 0.0193(13) 0.0216(13) 0.0179(13) 0.0056(11) 0.0012(10) 0.0024(11) C7 0.0289(15) 0.0231(14) 0.0214(15) 0.0028(11) -0.0070(12) 0.0008(11) C8 0.0182(12) 0.0138(12) 0.0164(13) -0.0014(10) 0.0018(10) 0.0008(10) C9 0.0232(14) 0.0213(14) 0.0274(15) 0.0048(12) 0.0095(12) -0.0021(11) C10 0.0170(13) 0.0229(14) 0.0324(16) 0.0013(12) 0.0041(12) -0.0042(11) C11 0.0220(13) 0.0172(13) 0.0213(14) 0.0020(11) -0.0028(11) 0.0004(10) C12 0.0290(14) 0.0166(13) 0.0146(13) -0.0006(10) -0.0010(11) 0.0023(11) C13 0.0273(14) 0.0172(13) 0.0160(13) -0.0023(10) 0.0020(11) 0.0052(11) C14 0.0169(12) 0.0150(12) 0.0166(13) 0.0012(10) -0.0003(10) 0.0021(10) C15 0.0192(13) 0.0209(13) 0.0202(14) 0.0020(11) 0.0027(11) -0.0032(11) C16 0.0187(13) 0.0153(13) 0.0218(14) 0.0020(11) -0.0003(11) -0.0026(10) C17 0.0241(14) 0.0215(14) 0.0191(14) -0.0079(11) 0.0024(11) -0.0020(11) C18 0.0255(14) 0.0202(13) 0.0106(12) -0.0039(10) 0.0019(10) -0.0039(11) C19 0.0313(15) 0.0195(14) 0.0219(15) -0.0038(11) 0.0052(12) -0.0028(11) C20 0.0317(16) 0.0261(15) 0.0264(16) -0.0047(12) 0.0041(12) -0.0109(12) C21 0.0285(15) 0.0362(17) 0.0184(14) -0.0040(12) -0.0003(12) -0.0079(13) C22 0.0348(16) 0.0282(15) 0.0232(15) 0.0033(12) -0.0032(12) -0.0006(13) C23 0.0348(16) 0.0200(14) 0.0240(15) 0.0020(12) -0.0031(12) -0.0081(12) P1 0.0233(4) 0.0190(3) 0.0207(4) -0.0017(3) 0.0023(3) -0.0011(3) F1 0.169(3) 0.0384(12) 0.0321(11) -0.0146(9) 0.0137(14) -0.0255(14) F2 0.0938(17) 0.0327(10) 0.0537(13) 0.0005(9) 0.0296(12) -0.0219(11) F3 0.0413(14) 0.0698(17) 0.186(3) -0.0021(18) -0.0387(16) 0.0140(12) F4 0.1157(19) 0.0446(12) 0.0319(11) -0.0148(9) 0.0236(12) -0.0268(12) F5 0.1067(18) 0.0296(10) 0.0413(11) -0.0047(9) 0.0360(12) -0.0219(11) F6 0.0351(12) 0.0800(18) 0.169(3) 0.0097(18) -0.0117(15) 0.0217(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C14 2.087(2) 3_656 ? Ag1 C8 2.092(2) . ? N1 C8 1.357(3) . ? N1 C10 1.390(3) . ? N1 C7 1.467(3) . ? N2 C8 1.349(3) . ? N2 C9 1.385(3) . ? N2 C11 1.469(3) . ? N3 C14 1.356(3) . ? N3 C16 1.381(3) . ? N3 C13 1.471(3) . ? N4 C14 1.356(3) . ? N4 C15 1.382(3) . ? N4 C17 1.472(3) . ? C1 C2 1.392(4) . ? C1 C6 1.399(4) . ? C1 H1 0.9300 . ? C2 C3 1.377(4) . ? C2 H2 0.9300 . ? C3 C4 1.388(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 C6 1.396(4) . ? C5 H5 0.9300 . ? C6 C7 1.511(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.342(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.524(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.529(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 Ag1 2.087(2) 3_656 ? C15 C16 1.350(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.512(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.386(4) . ? C18 C19 1.393(4) . ? C19 C20 1.391(4) . ? C19 H19 0.9300 . ? C20 C21 1.382(4) . ? C20 H20 0.9300 . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C23 1.389(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? P1 F6 1.559(2) . ? P1 F1 1.571(2) . ? P1 F3 1.572(2) . ? P1 F4 1.5914(19) . ? P1 F2 1.5925(19) . ? P1 F5 1.5963(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 C14 Ag1 C8 171.43(9) 3_656 . ? C8 N1 C10 111.0(2) . . ? C8 N1 C7 124.2(2) . . ? C10 N1 C7 124.6(2) . . ? C8 N2 C9 111.2(2) . . ? C8 N2 C11 124.3(2) . . ? C9 N2 C11 124.3(2) . . ? C14 N3 C16 111.2(2) . . ? C14 N3 C13 124.2(2) . . ? C16 N3 C13 124.3(2) . . ? C14 N4 C15 111.5(2) . . ? C14 N4 C17 123.3(2) . . ? C15 N4 C17 125.2(2) . . ? C2 C1 C6 120.2(3) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 118.4(2) . . ? C5 C6 C7 121.7(2) . . ? C1 C6 C7 119.9(2) . . ? N1 C7 C6 113.5(2) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N2 C8 N1 104.4(2) . . ? N2 C8 Ag1 129.74(18) . . ? N1 C8 Ag1 125.59(18) . . ? C10 C9 N2 107.0(2) . . ? C10 C9 H9 126.5 . . ? N2 C9 H9 126.5 . . ? C9 C10 N1 106.4(2) . . ? C9 C10 H10 126.8 . . ? N1 C10 H10 126.8 . . ? N2 C11 C12 112.9(2) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 111.4(2) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N3 C13 C12 111.8(2) . . ? N3 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N4 C14 N3 104.1(2) . . ? N4 C14 Ag1 127.60(17) . 3_656 ? N3 C14 Ag1 127.72(17) . 3_656 ? C16 C15 N4 106.3(2) . . ? C16 C15 H15 126.9 . . ? N4 C15 H15 126.9 . . ? C15 C16 N3 106.9(2) . . ? C15 C16 H16 126.6 . . ? N3 C16 H16 126.6 . . ? N4 C17 C18 112.3(2) . . ? N4 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N4 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C23 C18 C19 118.9(3) . . ? C23 C18 C17 120.5(2) . . ? C19 C18 C17 120.6(2) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.8(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.7(3) . . ? C18 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? F6 P1 F1 90.71(17) . . ? F6 P1 F3 178.71(18) . . ? F1 P1 F3 90.49(17) . . ? F6 P1 F4 90.46(16) . . ? F1 P1 F4 178.74(15) . . ? F3 P1 F4 88.34(16) . . ? F6 P1 F2 89.84(14) . . ? F1 P1 F2 89.95(11) . . ? F3 P1 F2 89.69(15) . . ? F4 P1 F2 90.52(11) . . ? F6 P1 F5 89.81(14) . . ? F1 P1 F5 90.59(11) . . ? F3 P1 F5 90.66(14) . . ? F4 P1 F5 88.94(10) . . ? F2 P1 F5 179.36(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.4(4) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C1 1.8(4) . . . . ? C4 C5 C6 C7 -176.2(2) . . . . ? C2 C1 C6 C5 -1.3(4) . . . . ? C2 C1 C6 C7 176.7(2) . . . . ? C8 N1 C7 C6 88.5(3) . . . . ? C10 N1 C7 C6 -86.6(3) . . . . ? C5 C6 C7 N1 -42.2(3) . . . . ? C1 C6 C7 N1 139.9(2) . . . . ? C9 N2 C8 N1 0.0(3) . . . . ? C11 N2 C8 N1 175.1(2) . . . . ? C9 N2 C8 Ag1 -174.63(18) . . . . ? C11 N2 C8 Ag1 0.5(4) . . . . ? C10 N1 C8 N2 0.0(3) . . . . ? C7 N1 C8 N2 -175.7(2) . . . . ? C10 N1 C8 Ag1 174.87(18) . . . . ? C7 N1 C8 Ag1 -0.8(3) . . . . ? C14 Ag1 C8 N2 126.9(6) 3_656 . . . ? C14 Ag1 C8 N1 -46.6(7) 3_656 . . . ? C8 N2 C9 C10 0.1(3) . . . . ? C11 N2 C9 C10 -175.0(2) . . . . ? N2 C9 C10 N1 -0.1(3) . . . . ? C8 N1 C10 C9 0.1(3) . . . . ? C7 N1 C10 C9 175.7(2) . . . . ? C8 N2 C11 C12 123.6(3) . . . . ? C9 N2 C11 C12 -61.9(3) . . . . ? N2 C11 C12 C13 178.1(2) . . . . ? C14 N3 C13 C12 96.5(3) . . . . ? C16 N3 C13 C12 -76.7(3) . . . . ? C11 C12 C13 N3 -62.7(3) . . . . ? C15 N4 C14 N3 -0.8(3) . . . . ? C17 N4 C14 N3 -179.4(2) . . . . ? C15 N4 C14 Ag1 170.94(18) . . . 3_656 ? C17 N4 C14 Ag1 -7.6(3) . . . 3_656 ? C16 N3 C14 N4 0.7(3) . . . . ? C13 N3 C14 N4 -173.3(2) . . . . ? C16 N3 C14 Ag1 -171.07(17) . . . 3_656 ? C13 N3 C14 Ag1 14.9(3) . . . 3_656 ? C14 N4 C15 C16 0.7(3) . . . . ? C17 N4 C15 C16 179.2(2) . . . . ? N4 C15 C16 N3 -0.2(3) . . . . ? C14 N3 C16 C15 -0.3(3) . . . . ? C13 N3 C16 C15 173.7(2) . . . . ? C14 N4 C17 C18 65.1(3) . . . . ? C15 N4 C17 C18 -113.3(3) . . . . ? N4 C17 C18 C23 54.3(3) . . . . ? N4 C17 C18 C19 -127.1(3) . . . . ? C23 C18 C19 C20 0.3(4) . . . . ? C17 C18 C19 C20 -178.3(2) . . . . ? C18 C19 C20 C21 -1.3(4) . . . . ? C19 C20 C21 C22 1.2(4) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? C19 C18 C23 C22 0.8(4) . . . . ? C17 C18 C23 C22 179.4(2) . . . . ? C21 C22 C23 C18 -0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.612 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.071 # Attachment 'CIF_2c.cif' data_080106c _database_code_depnum_ccdc_archive 'CCDC 704841' #TrackingRef 'CIF_2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H44 Ag2 F12 N8 P2' _chemical_formula_weight 998.39 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1278(12) _cell_length_b 10.3697(12) _cell_length_c 11.5198(13) _cell_angle_alpha 87.968(2) _cell_angle_beta 64.179(2) _cell_angle_gamma 67.365(2) _cell_volume 992.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3130 _cell_measurement_theta_min 2.450 _cell_measurement_theta_max 27.378 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 1.155 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5150 _diffrn_reflns_av_R_equivalents 0.0108 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3512 _reflns_number_gt 3142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.5651P] 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 3492 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.84231(3) -0.06262(3) 0.52652(2) 0.05005(11) Uani 1 1 d . . . P1 P 0.69609(11) 0.27257(10) 0.21170(9) 0.0550(2) Uani 1 1 d . . . F1 F 0.7878(4) 0.1993(3) 0.2929(3) 0.1010(9) Uani 1 1 d . . . F2 F 0.8152(5) 0.1485(3) 0.0956(3) 0.1301(14) Uani 1 1 d . . . F3 F 0.6049(4) 0.3497(3) 0.1301(3) 0.1120(11) Uani 1 1 d . . . F4 F 0.5784(4) 0.3990(3) 0.3274(3) 0.1181(12) Uani 1 1 d . . . F5 F 0.8076(5) 0.3548(4) 0.1516(4) 0.1335(13) Uani 1 1 d . . . F6 F 0.5864(5) 0.1942(5) 0.2728(4) 0.1444(15) Uani 1 1 d . . . N1 N 0.6969(4) 0.1016(3) 0.8001(3) 0.0540(7) Uani 1 1 d . . . N2 N 0.5516(3) 0.2118(3) 0.7093(3) 0.0477(6) Uani 1 1 d . . . N3 N -0.0104(3) 0.2579(3) 0.7413(3) 0.0510(7) Uani 1 1 d . . . N4 N -0.1339(3) 0.3416(3) 0.6277(3) 0.0534(7) Uani 1 1 d . . . C1 C 0.7679(7) -0.1191(7) 0.8897(7) 0.116(2) Uani 1 1 d . . . H1A H 0.6702 -0.0757 0.9695 0.175 Uiso 1 1 calc R . . H1B H 0.8498 -0.1865 0.9083 0.175 Uiso 1 1 calc R . . H1C H 0.7492 -0.1666 0.8321 0.175 Uiso 1 1 calc R . . C2 C 0.8214(5) -0.0079(5) 0.8258(4) 0.0700(11) Uani 1 1 d . . . H2A H 0.8465 0.0359 0.8819 0.084 Uiso 1 1 calc R . . H2B H 0.9187 -0.0518 0.7441 0.084 Uiso 1 1 calc R . . C3 C 0.5779(5) 0.2216(5) 0.8857(4) 0.0645(10) Uani 1 1 d . . . H3 H 0.5638 0.2495 0.9676 0.077 Uiso 1 1 calc R . . C4 C 0.4861(5) 0.2910(4) 0.8299(4) 0.0618(9) Uani 1 1 d . . . H4 H 0.3955 0.3763 0.8652 0.074 Uiso 1 1 calc R . . C5 C 0.6829(4) 0.0944(4) 0.6894(3) 0.0449(7) Uani 1 1 d . . . C6 C 0.4824(4) 0.2482(4) 0.6174(3) 0.0533(8) Uani 1 1 d . . . H6A H 0.5688 0.2164 0.5287 0.064 Uiso 1 1 calc R . . H6B H 0.4269 0.3502 0.6289 0.064 Uiso 1 1 calc R . . C7 C 0.3659(4) 0.1825(4) 0.6362(3) 0.0536(8) Uani 1 1 d . . . H7A H 0.4249 0.0805 0.6144 0.064 Uiso 1 1 calc R . . H7B H 0.3214 0.2135 0.5756 0.064 Uiso 1 1 calc R . . C8 C 0.2288(4) 0.2185(4) 0.7731(4) 0.0586(9) Uani 1 1 d . . . H8A H 0.1770 0.3204 0.7987 0.070 Uiso 1 1 calc R . . H8B H 0.2724 0.1782 0.8326 0.070 Uiso 1 1 calc R . . C9 C 0.1033(5) 0.1655(4) 0.7873(4) 0.0593(9) Uani 1 1 d . . . H9A H 0.1568 0.0709 0.7379 0.071 Uiso 1 1 calc R . . H9B H 0.0440 0.1597 0.8785 0.071 Uiso 1 1 calc R . . C10 C -0.1374(5) 0.3843(5) 0.8120(4) 0.0669(10) Uani 1 1 d . . . H10 H -0.1643 0.4257 0.8939 0.080 Uiso 1 1 calc R . . C11 C -0.2141(5) 0.4359(4) 0.7406(4) 0.0697(11) Uani 1 1 d . . . H11 H -0.3050 0.5200 0.7633 0.084 Uiso 1 1 calc R . . C12 C -0.0067(4) 0.2302(3) 0.6265(3) 0.0455(7) Uani 1 1 d . . . C13 C -0.1799(5) 0.3590(4) 0.5219(4) 0.0641(10) Uani 1 1 d . . . H13A H -0.2961 0.4058 0.5592 0.077 Uiso 1 1 calc R . . H13B H -0.1459 0.2664 0.4763 0.077 Uiso 1 1 calc R . . C14 C -0.1082(8) 0.4427(7) 0.4266(6) 0.111(2) Uani 1 1 d . . . H14A H -0.1432 0.5353 0.4707 0.167 Uiso 1 1 calc R . . H14B H -0.1419 0.4510 0.3596 0.167 Uiso 1 1 calc R . . H14C H 0.0070 0.3958 0.3878 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04804(17) 0.05804(18) 0.04833(17) 0.01274(11) -0.02508(12) -0.02275(12) P1 0.0563(5) 0.0570(5) 0.0452(5) 0.0072(4) -0.0266(4) -0.0129(4) F1 0.102(2) 0.106(2) 0.0868(19) 0.0193(16) -0.0650(17) -0.0094(16) F2 0.156(3) 0.094(2) 0.0639(17) -0.0120(15) -0.0350(19) 0.007(2) F3 0.128(3) 0.113(2) 0.103(2) 0.0177(18) -0.088(2) -0.0168(19) F4 0.137(3) 0.0818(18) 0.0768(18) -0.0142(15) -0.0423(18) 0.0074(18) F5 0.133(3) 0.161(3) 0.148(3) 0.067(3) -0.069(3) -0.100(3) F6 0.148(3) 0.174(4) 0.164(4) 0.058(3) -0.072(3) -0.119(3) N1 0.0547(17) 0.076(2) 0.0502(16) 0.0194(15) -0.0324(14) -0.0363(15) N2 0.0489(15) 0.0576(16) 0.0459(15) 0.0127(12) -0.0243(13) -0.0283(13) N3 0.0455(15) 0.0633(17) 0.0476(16) 0.0145(13) -0.0195(13) -0.0282(14) N4 0.0412(14) 0.0596(17) 0.0658(19) 0.0176(14) -0.0278(14) -0.0237(13) C1 0.109(4) 0.136(5) 0.136(5) 0.090(4) -0.079(4) -0.059(4) C2 0.062(2) 0.103(3) 0.065(2) 0.030(2) -0.044(2) -0.038(2) C3 0.071(2) 0.090(3) 0.047(2) 0.0063(19) -0.0287(19) -0.044(2) C4 0.061(2) 0.069(2) 0.058(2) 0.0020(18) -0.0241(18) -0.0319(19) C5 0.0443(17) 0.0603(19) 0.0471(18) 0.0203(15) -0.0269(14) -0.0320(15) C6 0.0527(19) 0.065(2) 0.0490(19) 0.0230(16) -0.0283(16) -0.0258(17) C7 0.0508(19) 0.066(2) 0.0494(19) 0.0130(16) -0.0298(16) -0.0221(16) C8 0.058(2) 0.078(2) 0.050(2) 0.0152(17) -0.0297(17) -0.0323(19) C9 0.063(2) 0.081(3) 0.051(2) 0.0308(18) -0.0330(18) -0.040(2) C10 0.055(2) 0.079(3) 0.056(2) 0.0019(19) -0.0151(18) -0.028(2) C11 0.043(2) 0.065(2) 0.081(3) 0.003(2) -0.019(2) -0.0134(17) C12 0.0430(17) 0.0561(18) 0.0492(18) 0.0201(14) -0.0238(14) -0.0297(15) C13 0.059(2) 0.072(2) 0.088(3) 0.029(2) -0.051(2) -0.0343(19) C14 0.168(6) 0.147(5) 0.131(5) 0.093(4) -0.119(5) -0.120(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C5 2.081(3) . ? Ag1 C12 2.081(3) 2_656 ? P1 F6 1.537(3) . ? P1 F2 1.556(3) . ? P1 F4 1.566(3) . ? P1 F1 1.574(3) . ? P1 F5 1.582(3) . ? P1 F3 1.584(3) . ? N1 C5 1.351(4) . ? N1 C3 1.368(5) . ? N1 C2 1.472(5) . ? N2 C5 1.346(4) . ? N2 C4 1.380(5) . ? N2 C6 1.472(4) . ? N3 C12 1.345(4) . ? N3 C10 1.379(5) . ? N3 C9 1.474(4) . ? N4 C12 1.354(4) . ? N4 C11 1.366(5) . ? N4 C13 1.467(5) . ? C1 C2 1.496(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.329(6) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 C7 1.512(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.513(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.514(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.331(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 Ag1 2.081(3) 2_656 ? C13 C14 1.486(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 C5 Ag1 C12 175.44(11) . 2_656 ? F6 P1 F2 90.9(2) . . ? F6 P1 F4 90.2(2) . . ? F2 P1 F4 178.9(2) . . ? F6 P1 F1 88.4(2) . . ? F2 P1 F1 90.49(17) . . ? F4 P1 F1 89.49(17) . . ? F6 P1 F5 178.9(2) . . ? F2 P1 F5 90.1(2) . . ? F4 P1 F5 88.8(2) . . ? F1 P1 F5 91.0(2) . . ? F6 P1 F3 92.9(2) . . ? F2 P1 F3 90.20(18) . . ? F4 P1 F3 89.79(17) . . ? F1 P1 F3 178.52(19) . . ? F5 P1 F3 87.7(2) . . ? C5 N1 C3 111.0(3) . . ? C5 N1 C2 124.1(3) . . ? C3 N1 C2 124.9(3) . . ? C5 N2 C4 111.0(3) . . ? C5 N2 C6 124.7(3) . . ? C4 N2 C6 124.3(3) . . ? C12 N3 C10 110.7(3) . . ? C12 N3 C9 125.1(3) . . ? C10 N3 C9 124.2(3) . . ? C12 N4 C11 111.2(3) . . ? C12 N4 C13 124.5(3) . . ? C11 N4 C13 124.3(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 111.7(3) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C4 C3 N1 107.2(3) . . ? C4 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? C3 C4 N2 106.6(4) . . ? C3 C4 H4 126.7 . . ? N2 C4 H4 126.7 . . ? N2 C5 N1 104.2(3) . . ? N2 C5 Ag1 130.4(2) . . ? N1 C5 Ag1 125.3(2) . . ? N2 C6 C7 112.7(3) . . ? N2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C8 114.4(3) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 113.9(3) . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N3 C9 C8 112.4(3) . . ? N3 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? N3 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 N3 107.0(4) . . ? C11 C10 H10 126.5 . . ? N3 C10 H10 126.5 . . ? C10 C11 N4 106.9(4) . . ? C10 C11 H11 126.6 . . ? N4 C11 H11 126.6 . . ? N3 C12 N4 104.2(3) . . ? N3 C12 Ag1 129.9(2) . 2_656 ? N4 C12 Ag1 125.8(2) . 2_656 ? N4 C13 C14 112.8(3) . . ? N4 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N4 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 C1 -88.9(5) . . . . ? C3 N1 C2 C1 89.1(5) . . . . ? C5 N1 C3 C4 0.5(4) . . . . ? C2 N1 C3 C4 -177.7(3) . . . . ? N1 C3 C4 N2 -0.3(4) . . . . ? C5 N2 C4 C3 -0.1(4) . . . . ? C6 N2 C4 C3 177.3(3) . . . . ? C4 N2 C5 N1 0.4(4) . . . . ? C6 N2 C5 N1 -177.0(3) . . . . ? C4 N2 C5 Ag1 -176.5(2) . . . . ? C6 N2 C5 Ag1 6.1(5) . . . . ? C3 N1 C5 N2 -0.6(4) . . . . ? C2 N1 C5 N2 177.7(3) . . . . ? C3 N1 C5 Ag1 176.6(2) . . . . ? C2 N1 C5 Ag1 -5.2(4) . . . . ? C12 Ag1 C5 N2 -158.0(12) 2_656 . . . ? C12 Ag1 C5 N1 25.7(15) 2_656 . . . ? C5 N2 C6 C7 86.2(4) . . . . ? C4 N2 C6 C7 -90.9(4) . . . . ? N2 C6 C7 C8 56.1(4) . . . . ? C6 C7 C8 C9 173.7(3) . . . . ? C12 N3 C9 C8 102.7(4) . . . . ? C10 N3 C9 C8 -78.4(4) . . . . ? C7 C8 C9 N3 -80.0(4) . . . . ? C12 N3 C10 C11 0.2(4) . . . . ? C9 N3 C10 C11 -178.8(3) . . . . ? N3 C10 C11 N4 -0.2(4) . . . . ? C12 N4 C11 C10 0.1(4) . . . . ? C13 N4 C11 C10 -180.0(3) . . . . ? C10 N3 C12 N4 -0.1(4) . . . . ? C9 N3 C12 N4 178.9(3) . . . . ? C10 N3 C12 Ag1 177.3(2) . . . 2_656 ? C9 N3 C12 Ag1 -3.7(5) . . . 2_656 ? C11 N4 C12 N3 0.0(4) . . . . ? C13 N4 C12 N3 -179.9(3) . . . . ? C11 N4 C12 Ag1 -177.6(2) . . . 2_656 ? C13 N4 C12 Ag1 2.5(4) . . . 2_656 ? C12 N4 C13 C14 -92.9(5) . . . . ? C11 N4 C13 C14 87.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.713 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.073 # Attachment 'CIF_2d.cif' data_080314a _database_code_depnum_ccdc_archive 'CCDC 704842' #TrackingRef 'CIF_2d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Ag2 F12 N8 P2' _chemical_formula_weight 1246.66 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.531(3) _cell_length_b 12.021(3) _cell_length_c 14.501(6) _cell_angle_alpha 110.703(7) _cell_angle_beta 92.506(7) _cell_angle_gamma 108.340(5) _cell_volume 1300.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2967 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 24.57 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6608 _diffrn_reflns_av_R_equivalents 0.0125 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4585 _reflns_number_gt 3792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+1.3958P] 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 4543 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.38845(5) 0.33068(3) 0.68629(3) 0.06230(17) Uani 1 1 d . . . N1 N 0.5492(5) 0.1263(4) 0.6520(3) 0.0632(10) Uani 1 1 d . . . N2 N 0.6797(5) 0.2567(4) 0.5895(3) 0.0626(10) Uani 1 1 d . . . N3 N 0.8001(6) 0.4758(4) 0.2612(3) 0.0671(11) Uani 1 1 d . . . N4 N 0.9146(6) 0.6308(4) 0.2180(3) 0.0700(11) Uani 1 1 d . . . C1 C 0.5535(11) 0.2077(7) 0.8889(6) 0.113(2) Uani 1 1 d . . . H1 H 0.5153 0.2680 0.8794 0.135 Uiso 1 1 calc R . . C2 C 0.6370(15) 0.2339(9) 0.9811(7) 0.139(4) Uani 1 1 d . . . H2 H 0.6597 0.3130 1.0323 0.166 Uiso 1 1 calc R . . C3 C 0.6852(14) 0.1485(11) 0.9980(7) 0.140(3) Uani 1 1 d . . . H3 H 0.7373 0.1648 1.0614 0.169 Uiso 1 1 calc R . . C4 C 0.6579(16) 0.0362(11) 0.9214(8) 0.160(4) Uani 1 1 d . . . H4 H 0.6931 -0.0243 0.9328 0.192 Uiso 1 1 calc R . . C5 C 0.5801(12) 0.0093(7) 0.8280(6) 0.118(3) Uani 1 1 d . . . H5 H 0.5649 -0.0680 0.7763 0.142 Uiso 1 1 calc R . . C6 C 0.5251(7) 0.0948(5) 0.8104(4) 0.0690(13) Uani 1 1 d . . . C7 C 0.4360(7) 0.0665(5) 0.7086(5) 0.0789(15) Uani 1 1 d . . . H7A H 0.3905 -0.0248 0.6714 0.095 Uiso 1 1 calc R . . H7B H 0.3431 0.0973 0.7160 0.095 Uiso 1 1 calc R . . C8 C 0.6707(8) 0.0845(6) 0.6107(4) 0.0761(14) Uani 1 1 d . . . H8 H 0.6923 0.0133 0.6106 0.091 Uiso 1 1 calc R . . C9 C 0.7534(7) 0.1656(6) 0.5702(4) 0.0767(15) Uani 1 1 d . . . H9 H 0.8424 0.1612 0.5360 0.092 Uiso 1 1 calc R . . C10 C 0.5538(6) 0.2334(4) 0.6397(3) 0.0589(11) Uani 1 1 d . . . C11 C 0.7335(7) 0.3633(5) 0.5576(4) 0.0719(14) Uani 1 1 d . . . H11A H 0.8550 0.3959 0.5670 0.086 Uiso 1 1 calc R . . H11B H 0.6982 0.4308 0.5996 0.086 Uiso 1 1 calc R . . C12 C 0.6632(6) 0.3270(5) 0.4498(4) 0.0645(12) Uani 1 1 d . . . H12A H 0.5448 0.3149 0.4434 0.077 Uiso 1 1 calc R . . H12B H 0.6744 0.2471 0.4092 0.077 Uiso 1 1 calc R . . C13 C 0.7532(7) 0.4286(5) 0.4113(4) 0.0652(12) Uani 1 1 d . . . H13A H 0.7371 0.5072 0.4500 0.078 Uiso 1 1 calc R . . H13B H 0.8725 0.4439 0.4214 0.078 Uiso 1 1 calc R . . C14 C 0.6924(7) 0.3924(5) 0.3028(4) 0.0747(14) Uani 1 1 d . . . H14A H 0.6862 0.3059 0.2657 0.090 Uiso 1 1 calc R . . H14B H 0.5802 0.3947 0.2947 0.090 Uiso 1 1 calc R . . C15 C 0.9362(8) 0.4566(7) 0.2201(4) 0.0845(17) Uani 1 1 d . . . H15 H 0.9724 0.3892 0.2131 0.101 Uiso 1 1 calc R . . C16 C 1.0067(8) 0.5525(7) 0.1919(4) 0.0865(18) Uani 1 1 d . . . H16 H 1.1000 0.5642 0.1607 0.104 Uiso 1 1 calc R . . C17 C 0.7846(6) 0.5832(5) 0.2602(3) 0.0608(11) Uani 1 1 d . . . C18 C 0.9426(7) 0.7423(6) 0.1942(4) 0.0789(15) Uani 1 1 d . . . H18A H 1.0624 0.7847 0.2011 0.095 Uiso 1 1 calc R . . H18B H 0.9010 0.8007 0.2426 0.095 Uiso 1 1 calc R . . C19 C 0.8602(6) 0.7148(5) 0.0905(4) 0.0659(12) Uani 1 1 d . . . C20 C 0.9030(12) 0.8114(8) 0.0564(6) 0.126(3) Uani 1 1 d . . . H20 H 0.9745 0.8923 0.0985 0.151 Uiso 1 1 calc R . . C21 C 0.8388(15) 0.7881(11) -0.0419(8) 0.150(4) Uani 1 1 d . . . H21 H 0.8742 0.8515 -0.0669 0.180 Uiso 1 1 calc R . . C22 C 0.7232(11) 0.6709(10) -0.1012(6) 0.115(3) Uani 1 1 d . . . H22 H 0.6713 0.6572 -0.1640 0.138 Uiso 1 1 calc R . . C23 C 0.6869(9) 0.5791(7) -0.0684(5) 0.0936(18) Uani 1 1 d . . . H23 H 0.6137 0.4986 -0.1100 0.112 Uiso 1 1 calc R . . C24 C 0.7556(8) 0.5994(6) 0.0271(4) 0.0854(16) Uani 1 1 d . . . H24 H 0.7288 0.5318 0.0479 0.103 Uiso 1 1 calc R . . P1 P 0.08988(18) 0.18897(14) 0.34093(12) 0.0719(4) Uani 1 1 d . . . F1 F 0.1927(13) 0.3184(5) 0.3435(5) 0.237(4) Uani 1 1 d . . . F2 F 0.0255(12) 0.2530(7) 0.4322(6) 0.230(4) Uani 1 1 d . . . F3 F -0.0199(10) 0.0601(6) 0.3436(6) 0.212(3) Uani 1 1 d . . . F4 F 0.1543(14) 0.1266(9) 0.2544(7) 0.271(5) Uani 1 1 d . . . F5 F -0.0510(13) 0.1757(10) 0.2673(8) 0.277(5) Uani 1 1 d . . . F6 F 0.2243(9) 0.1945(9) 0.4149(8) 0.247(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 0.0673(3) 0.0604(2) 0.0594(2) 0.02407(18) 0.01093(17) 0.02190(18) N1 0.062(2) 0.054(2) 0.067(2) 0.0215(19) 0.0029(19) 0.0152(19) N2 0.064(2) 0.062(2) 0.054(2) 0.0194(18) 0.0093(18) 0.0149(19) N3 0.081(3) 0.072(3) 0.053(2) 0.025(2) 0.001(2) 0.033(2) N4 0.070(3) 0.087(3) 0.053(2) 0.029(2) 0.009(2) 0.025(2) C1 0.158(7) 0.081(4) 0.107(6) 0.033(4) 0.014(5) 0.057(5) C2 0.217(11) 0.104(6) 0.091(6) 0.021(5) 0.015(6) 0.072(7) C3 0.186(10) 0.163(9) 0.089(5) 0.052(6) 0.013(6) 0.082(8) C4 0.229(13) 0.162(9) 0.134(8) 0.061(7) 0.003(8) 0.127(10) C5 0.188(9) 0.094(5) 0.095(5) 0.033(4) 0.018(5) 0.084(6) C6 0.073(3) 0.059(3) 0.085(4) 0.038(3) 0.030(3) 0.024(2) C7 0.072(3) 0.058(3) 0.099(4) 0.037(3) 0.011(3) 0.006(3) C8 0.085(4) 0.072(3) 0.072(3) 0.022(3) 0.008(3) 0.036(3) C9 0.074(3) 0.093(4) 0.064(3) 0.024(3) 0.017(3) 0.039(3) C10 0.059(3) 0.050(2) 0.054(2) 0.015(2) 0.005(2) 0.009(2) C11 0.077(3) 0.066(3) 0.061(3) 0.024(2) 0.013(2) 0.009(3) C12 0.058(3) 0.061(3) 0.070(3) 0.025(2) 0.001(2) 0.017(2) C13 0.069(3) 0.059(3) 0.058(3) 0.021(2) 0.006(2) 0.015(2) C14 0.083(4) 0.069(3) 0.066(3) 0.029(3) -0.009(3) 0.020(3) C15 0.095(4) 0.105(5) 0.065(3) 0.026(3) 0.004(3) 0.059(4) C16 0.074(4) 0.127(5) 0.070(4) 0.035(4) 0.019(3) 0.053(4) C17 0.064(3) 0.069(3) 0.045(2) 0.019(2) 0.001(2) 0.022(2) C18 0.074(3) 0.087(4) 0.065(3) 0.032(3) 0.014(3) 0.012(3) C19 0.059(3) 0.081(3) 0.066(3) 0.036(3) 0.019(2) 0.024(3) C20 0.146(7) 0.100(5) 0.112(6) 0.056(5) -0.019(5) 0.008(5) C21 0.178(10) 0.157(9) 0.138(8) 0.098(7) 0.002(7) 0.047(8) C22 0.117(6) 0.150(7) 0.092(5) 0.057(5) -0.003(4) 0.055(6) C23 0.099(5) 0.104(5) 0.072(4) 0.029(4) -0.001(3) 0.036(4) C24 0.095(4) 0.084(4) 0.071(4) 0.031(3) 0.005(3) 0.024(3) P1 0.0652(8) 0.0667(8) 0.0814(9) 0.0201(7) 0.0168(7) 0.0293(7) F1 0.373(12) 0.094(4) 0.191(6) 0.067(4) 0.070(7) -0.002(5) F2 0.286(10) 0.207(7) 0.213(7) 0.059(6) 0.164(7) 0.117(7) F3 0.193(6) 0.121(4) 0.257(8) 0.078(5) -0.005(6) -0.028(4) F4 0.350(13) 0.245(9) 0.231(9) 0.041(7) 0.176(9) 0.164(9) F5 0.256(10) 0.264(10) 0.277(10) 0.088(8) -0.119(9) 0.089(8) F6 0.129(5) 0.304(10) 0.319(11) 0.195(9) -0.061(6) 0.017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C17 2.085(5) 2_666 ? Ag1 C10 2.092(5) . ? N1 C10 1.349(6) . ? N1 C8 1.362(7) . ? N1 C7 1.474(7) . ? N2 C10 1.336(6) . ? N2 C9 1.381(7) . ? N2 C11 1.461(7) . ? N3 C17 1.344(6) . ? N3 C15 1.374(8) . ? N3 C14 1.452(7) . ? N4 C17 1.355(7) . ? N4 C16 1.372(7) . ? N4 C18 1.453(7) . ? C1 C2 1.368(11) . ? C1 C6 1.368(9) . ? C1 H1 0.9300 . ? C2 C3 1.311(12) . ? C2 H2 0.9300 . ? C3 C4 1.352(12) . ? C3 H3 0.9300 . ? C4 C5 1.363(12) . ? C4 H4 0.9300 . ? C5 C6 1.349(9) . ? C5 H5 0.9300 . ? C6 C7 1.503(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.342(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.505(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.523(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.495(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.332(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 Ag1 2.085(5) 2_666 ? C18 C19 1.508(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.347(8) . ? C19 C20 1.371(9) . ? C20 C21 1.400(11) . ? C20 H20 0.9300 . ? C21 C22 1.375(13) . ? C21 H21 0.9300 . ? C22 C23 1.307(10) . ? C22 H22 0.9300 . ? C23 C24 1.386(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? P1 F4 1.447(6) . ? P1 F2 1.501(6) . ? P1 F5 1.503(7) . ? P1 F6 1.505(6) . ? P1 F1 1.513(6) . ? P1 F3 1.552(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 C17 Ag1 C10 174.70(18) 2_666 . ? C10 N1 C8 111.1(4) . . ? C10 N1 C7 124.9(4) . . ? C8 N1 C7 123.9(5) . . ? C10 N2 C9 111.2(5) . . ? C10 N2 C11 125.3(5) . . ? C9 N2 C11 123.5(5) . . ? C17 N3 C15 110.7(5) . . ? C17 N3 C14 125.3(5) . . ? C15 N3 C14 123.9(5) . . ? C17 N4 C16 110.9(5) . . ? C17 N4 C18 124.5(5) . . ? C16 N4 C18 124.3(5) . . ? C2 C1 C6 121.4(7) . . ? C2 C1 H1 119.3 . . ? C6 C1 H1 119.3 . . ? C3 C2 C1 120.6(8) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 118.8(9) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 121.8(8) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 120.0(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 117.4(6) . . ? C5 C6 C7 121.0(6) . . ? C1 C6 C7 121.6(6) . . ? N1 C7 C6 111.7(4) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C9 C8 N1 107.0(5) . . ? C9 C8 H8 126.5 . . ? N1 C8 H8 126.5 . . ? C8 C9 N2 106.1(5) . . ? C8 C9 H9 126.9 . . ? N2 C9 H9 126.9 . . ? N2 C10 N1 104.6(4) . . ? N2 C10 Ag1 129.9(4) . . ? N1 C10 Ag1 125.5(4) . . ? N2 C11 C12 112.8(4) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 111.6(4) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 112.9(4) . . ? C14 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? C14 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N3 C14 C13 112.8(4) . . ? N3 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N3 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 N3 107.3(5) . . ? C16 C15 H15 126.3 . . ? N3 C15 H15 126.3 . . ? C15 C16 N4 106.6(5) . . ? C15 C16 H16 126.7 . . ? N4 C16 H16 126.7 . . ? N3 C17 N4 104.4(4) . . ? N3 C17 Ag1 130.4(4) . 2_666 ? N4 C17 Ag1 125.1(4) . 2_666 ? N4 C18 C19 114.5(5) . . ? N4 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? N4 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C24 C19 C20 118.0(6) . . ? C24 C19 C18 124.0(5) . . ? C20 C19 C18 117.8(6) . . ? C19 C20 C21 119.9(8) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.7(8) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 119.4(7) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.3(7) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 121.4(6) . . ? C19 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? F4 P1 F2 178.7(6) . . ? F4 P1 F5 86.1(7) . . ? F2 P1 F5 95.2(7) . . ? F4 P1 F6 94.1(7) . . ? F2 P1 F6 84.6(6) . . ? F5 P1 F6 176.4(5) . . ? F4 P1 F1 91.2(5) . . ? F2 P1 F1 89.1(5) . . ? F5 P1 F1 91.9(6) . . ? F6 P1 F1 91.6(5) . . ? F4 P1 F3 92.1(6) . . ? F2 P1 F3 87.5(5) . . ? F5 P1 F3 88.2(5) . . ? F6 P1 F3 88.2(5) . . ? F1 P1 F3 176.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -3.2(17) . . . . ? C1 C2 C3 C4 3.0(19) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 -1.3(18) . . . . ? C4 C5 C6 C1 1.1(13) . . . . ? C4 C5 C6 C7 -178.8(9) . . . . ? C2 C1 C6 C5 1.1(12) . . . . ? C2 C1 C6 C7 -179.0(8) . . . . ? C10 N1 C7 C6 -102.1(6) . . . . ? C8 N1 C7 C6 73.4(6) . . . . ? C5 C6 C7 N1 -99.7(7) . . . . ? C1 C6 C7 N1 80.4(7) . . . . ? C10 N1 C8 C9 -0.7(6) . . . . ? C7 N1 C8 C9 -176.8(5) . . . . ? N1 C8 C9 N2 0.8(6) . . . . ? C10 N2 C9 C8 -0.6(6) . . . . ? C11 N2 C9 C8 -180.0(5) . . . . ? C9 N2 C10 N1 0.1(5) . . . . ? C11 N2 C10 N1 179.5(4) . . . . ? C9 N2 C10 Ag1 -177.5(4) . . . . ? C11 N2 C10 Ag1 1.9(7) . . . . ? C8 N1 C10 N2 0.4(5) . . . . ? C7 N1 C10 N2 176.4(4) . . . . ? C8 N1 C10 Ag1 178.1(3) . . . . ? C7 N1 C10 Ag1 -5.9(7) . . . . ? C17 Ag1 C10 N2 -172.9(16) 2_666 . . . ? C17 Ag1 C10 N1 10(2) 2_666 . . . ? C10 N2 C11 C12 -98.3(6) . . . . ? C9 N2 C11 C12 81.0(6) . . . . ? N2 C11 C12 C13 -166.0(5) . . . . ? C11 C12 C13 C14 177.0(5) . . . . ? C17 N3 C14 C13 -89.3(6) . . . . ? C15 N3 C14 C13 88.6(6) . . . . ? C12 C13 C14 N3 -168.0(5) . . . . ? C17 N3 C15 C16 -0.5(6) . . . . ? C14 N3 C15 C16 -178.6(5) . . . . ? N3 C15 C16 N4 1.1(6) . . . . ? C17 N4 C16 C15 -1.4(6) . . . . ? C18 N4 C16 C15 -175.5(5) . . . . ? C15 N3 C17 N4 -0.4(5) . . . . ? C14 N3 C17 N4 177.7(4) . . . . ? C15 N3 C17 Ag1 -178.2(4) . . . 2_666 ? C14 N3 C17 Ag1 -0.2(7) . . . 2_666 ? C16 N4 C17 N3 1.1(5) . . . . ? C18 N4 C17 N3 175.1(4) . . . . ? C16 N4 C17 Ag1 179.1(4) . . . 2_666 ? C18 N4 C17 Ag1 -6.9(7) . . . 2_666 ? C17 N4 C18 C19 -89.9(6) . . . . ? C16 N4 C18 C19 83.3(7) . . . . ? N4 C18 C19 C24 6.1(8) . . . . ? N4 C18 C19 C20 -169.4(6) . . . . ? C24 C19 C20 C21 -0.3(13) . . . . ? C18 C19 C20 C21 175.5(8) . . . . ? C19 C20 C21 C22 5.0(16) . . . . ? C20 C21 C22 C23 -6.6(16) . . . . ? C21 C22 C23 C24 3.7(13) . . . . ? C20 C19 C24 C23 -2.7(10) . . . . ? C18 C19 C24 C23 -178.3(6) . . . . ? C22 C23 C24 C19 1.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.802 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.073 # Attachment 'CIF_2e_.cif' data_80628c _database_code_depnum_ccdc_archive 'CCDC 704843' #TrackingRef 'CIF_2e_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Ag2 F12 N8 P2' _chemical_formula_weight 1026.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2803(10) _cell_length_b 21.4577(11) _cell_length_c 11.6771(6) _cell_angle_alpha 90.00 _cell_angle_beta 123.7450(10) _cell_angle_gamma 90.00 _cell_volume 4225.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7318 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.90 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10713 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3734 _reflns_number_gt 3205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 14 restraints were used while dealing with disordered -CH2-CH2-CH2-. -CH2-CH2-CH2- are disordered in two positions with the occupancy factors of 0.554 and 0.446. The C-C and C-H distances were restrained to 1.50 \%A and 0.97 \%A, respectively. The thermal parameters of disordered atoms were refined with isotropy. DFIX 1.50 0.005 C6 C7' C7' C8' C8' C9' C9' C10 DFIX 1.50 0.005 C6 C7 C7 C8 C8 C9 C9 C10 ISOR 0.005 C7' ; _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^)+(0.0552P)^2^+13.1045P] 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 3732 _refine_ls_number_parameters 274 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.041 _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 0.35886(2) 0.246514(15) 0.62922(3) 0.06598(16) Uani 1 1 d . . . N1 N 0.3620(2) 0.38747(18) 0.6933(4) 0.0679(9) Uani 1 1 d . . . N2 N 0.3841(2) 0.33080(17) 0.8612(3) 0.0631(9) Uani 1 1 d . B . N3 N 0.65964(19) 0.15450(16) 1.0896(3) 0.0585(8) Uani 1 1 d . B . N4 N 0.6430(3) 0.10424(19) 0.9178(4) 0.0719(10) Uani 1 1 d . B . C1 C 0.3693(2) 0.3278(2) 0.7335(4) 0.0609(10) Uani 1 1 d . . . C2 C 0.3857(3) 0.3917(2) 0.8990(5) 0.0778(14) Uani 1 1 d . . . H2 H 0.3946 0.4056 0.9819 0.093 Uiso 1 1 calc R . . C3 C 0.3724(3) 0.4269(2) 0.7951(5) 0.0809(14) Uani 1 1 d . . . H3 H 0.3703 0.4702 0.7915 0.097 Uiso 1 1 calc R . . C4 C 0.3448(3) 0.4076(3) 0.5582(5) 0.0856(15) Uani 1 1 d . . . H4A H 0.3187 0.3738 0.4926 0.103 Uiso 1 1 calc R . . H4B H 0.3086 0.4426 0.5254 0.103 Uiso 1 1 calc R . . C5 C 0.4163(4) 0.4257(4) 0.5634(6) 0.122(2) Uani 1 1 d . . . H5A H 0.4391 0.4622 0.6197 0.183 Uiso 1 1 calc R . . H5B H 0.4024 0.4344 0.4720 0.183 Uiso 1 1 calc R . . H5C H 0.4540 0.3922 0.6021 0.183 Uiso 1 1 calc R . . C6 C 0.3950(3) 0.2769(3) 0.9449(5) 0.0879(16) Uani 1 1 d D . . H6A H 0.3841 0.2409 0.8865 0.105 Uiso 1 1 calc R A 1 H6B H 0.3525 0.2787 0.9597 0.105 Uiso 1 1 calc R A 1 C7 C 0.4670(4) 0.2611(5) 1.0796(6) 0.070(3) Uani 0.554(10) 1 d PD B 1 H7A H 0.4579 0.2252 1.1194 0.084 Uiso 0.554(10) 1 calc PR B 1 H7B H 0.4835 0.2959 1.1429 0.084 Uiso 0.554(10) 1 calc PR B 1 C8 C 0.5284(4) 0.2469(4) 1.0499(7) 0.057(2) Uani 0.554(10) 1 d PD B 1 H8A H 0.5422 0.2842 1.0208 0.069 Uiso 0.554(10) 1 calc PR B 1 H8B H 0.5092 0.2157 0.9781 0.069 Uiso 0.554(10) 1 calc PR B 1 C9 C 0.5991(5) 0.2228(6) 1.1841(10) 0.067(3) Uani 0.554(10) 1 d PD B 1 H9A H 0.6151 0.2545 1.2540 0.080 Uiso 0.554(10) 1 calc PR B 1 H9B H 0.5825 0.1866 1.2116 0.080 Uiso 0.554(10) 1 calc PR B 1 C7' C 0.4845(4) 0.2676(5) 1.0319(17) 0.096(5) Uani 0.446(10) 1 d PDU B 2 H7'A H 0.5032 0.2755 0.9727 0.115 Uiso 0.446(10) 1 calc PR B 2 H7'B H 0.5068 0.3000 1.1016 0.115 Uiso 0.446(10) 1 calc PR B 2 C8' C 0.5203(5) 0.2068(5) 1.1044(10) 0.069(3) Uani 0.446(10) 1 d PD B 2 H8'A H 0.5075 0.1764 1.0335 0.083 Uiso 0.446(10) 1 calc PR B 2 H8'B H 0.4921 0.1943 1.1458 0.083 Uiso 0.446(10) 1 calc PR B 2 C9' C 0.6077(5) 0.1996(7) 1.2142(11) 0.067(4) Uani 0.446(10) 1 d PD B 2 H9'A H 0.6207 0.2301 1.2851 0.081 Uiso 0.446(10) 1 calc PR B 2 H9'B H 0.6144 0.1589 1.2555 0.081 Uiso 0.446(10) 1 calc PR B 2 C10 C 0.6701(2) 0.2051(2) 1.1822(4) 0.0659(11) Uani 1 1 d D . . H10A H 0.6875 0.2418 1.1576 0.079 Uiso 1 1 calc R B 1 H10B H 0.7124 0.1935 1.2751 0.079 Uiso 1 1 calc R B 1 C11 C 0.6482(2) 0.1625(2) 0.9651(4) 0.0612(10) Uani 1 1 d . . . C12 C 0.6517(3) 0.0614(2) 1.0115(6) 0.0817(14) Uani 1 1 d . . . H12 H 0.6503 0.0183 1.0019 0.098 Uiso 1 1 calc R B . C13 C 0.6625(3) 0.0925(2) 1.1190(5) 0.0749(13) Uani 1 1 d . B . H13 H 0.6704 0.0753 1.1989 0.090 Uiso 1 1 calc R . . C14 C 0.6355(4) 0.0894(3) 0.7870(6) 0.104(2) Uani 1 1 d . . . H14A H 0.6421 0.1278 0.7505 0.125 Uiso 1 1 calc R B . H14B H 0.6788 0.0620 0.8078 0.125 Uiso 1 1 calc R . . C15 C 0.5659(5) 0.0621(5) 0.6856(8) 0.178(5) Uani 1 1 d . B . H15A H 0.5606 0.0222 0.7168 0.268 Uiso 1 1 calc R . . H15B H 0.5665 0.0568 0.6045 0.268 Uiso 1 1 calc R . . H15C H 0.5221 0.0882 0.6646 0.268 Uiso 1 1 calc R . . P1 P 0.23744(8) 0.11217(5) 0.89451(12) 0.0664(3) Uani 1 1 d . . . F1 F 0.2388(3) 0.1695(2) 0.9759(4) 0.161(2) Uani 1 1 d . . . F2 F 0.2264(3) 0.15438(17) 0.7758(4) 0.1452(17) Uani 1 1 d . . . F3 F 0.3290(2) 0.1142(2) 0.9654(5) 0.1511(17) Uani 1 1 d . . . F4 F 0.2374(2) 0.05435(14) 0.8112(4) 0.1143(12) Uani 1 1 d . . . F5 F 0.2514(3) 0.0693(3) 1.0130(4) 0.159(2) Uani 1 1 d . . . F6 F 0.1468(2) 0.1090(3) 0.8226(5) 0.178(2) 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 0.0771(3) 0.0699(3) 0.0533(2) -0.00629(14) 0.03771(19) 0.00361(16) N1 0.070(2) 0.074(2) 0.057(2) 0.0037(18) 0.0333(18) 0.0137(18) N2 0.060(2) 0.078(2) 0.0533(19) -0.0007(17) 0.0327(17) 0.0178(17) N3 0.0594(19) 0.066(2) 0.0526(18) 0.0102(15) 0.0326(16) 0.0147(16) N4 0.084(3) 0.075(3) 0.068(2) -0.002(2) 0.050(2) 0.006(2) C1 0.055(2) 0.077(3) 0.048(2) -0.0009(19) 0.0267(19) 0.015(2) C2 0.085(3) 0.085(3) 0.067(3) -0.009(2) 0.045(3) 0.024(3) C3 0.092(4) 0.068(3) 0.083(3) -0.005(3) 0.048(3) 0.019(3) C4 0.089(4) 0.094(4) 0.060(3) 0.013(3) 0.033(3) 0.010(3) C5 0.112(5) 0.174(7) 0.075(4) 0.019(4) 0.049(4) -0.017(5) C6 0.110(4) 0.094(4) 0.065(3) 0.018(3) 0.052(3) 0.033(3) C7 0.078(6) 0.101(7) 0.054(5) 0.011(4) 0.052(5) 0.013(5) C8 0.067(5) 0.079(6) 0.037(4) 0.002(3) 0.036(4) -0.017(4) C9 0.063(6) 0.066(8) 0.069(7) 0.005(5) 0.035(5) 0.024(5) C7' 0.102(6) 0.085(6) 0.083(6) 0.002(4) 0.041(4) 0.007(4) C8' 0.059(6) 0.091(8) 0.059(6) -0.003(5) 0.033(5) 0.004(5) C9' 0.046(6) 0.078(11) 0.051(6) -0.013(6) 0.009(5) 0.025(6) C10 0.062(2) 0.081(3) 0.048(2) -0.001(2) 0.026(2) 0.006(2) C11 0.062(2) 0.069(3) 0.054(2) 0.0053(19) 0.033(2) 0.006(2) C12 0.095(4) 0.059(3) 0.093(4) 0.014(3) 0.053(3) 0.016(2) C13 0.084(3) 0.074(3) 0.069(3) 0.027(2) 0.044(3) 0.024(2) C14 0.130(5) 0.113(5) 0.086(4) -0.028(3) 0.071(4) -0.012(4) C15 0.139(7) 0.305(14) 0.112(6) -0.086(7) 0.083(6) -0.083(8) P1 0.0873(8) 0.0573(6) 0.0648(7) 0.0001(5) 0.0487(6) 0.0064(6) F1 0.230(6) 0.122(3) 0.126(3) -0.039(3) 0.095(4) 0.045(3) F2 0.256(5) 0.087(2) 0.144(3) 0.042(2) 0.143(4) 0.043(3) F3 0.090(3) 0.207(5) 0.144(3) -0.042(3) 0.057(3) -0.019(3) F4 0.174(3) 0.0658(18) 0.119(3) -0.0220(17) 0.091(3) -0.007(2) F5 0.232(6) 0.162(4) 0.139(4) 0.074(3) 0.137(4) 0.066(3) F6 0.087(3) 0.278(7) 0.155(4) -0.017(4) 0.059(3) -0.002(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 C1 2.069(4) . ? Ag1 C11 2.075(4) 2_656 ? N1 C1 1.344(6) . ? N1 C3 1.377(6) . ? N1 C4 1.479(6) . ? N2 C1 1.350(5) . ? N2 C2 1.375(6) . ? N2 C6 1.449(6) . ? N3 C11 1.349(5) . ? N3 C13 1.368(6) . ? N3 C10 1.464(5) . ? N4 C11 1.348(6) . ? N4 C12 1.363(6) . ? N4 C14 1.483(7) . ? C2 C3 1.322(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.468(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.473(5) . ? C6 C7' 1.523(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.497(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.511(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.501(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C7' C8' 1.504(5) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8' C9' 1.511(5) . ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? C9' C10 1.509(5) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 Ag1 2.075(4) 2_656 ? C12 C13 1.328(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.371(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? P1 F6 1.541(4) . ? P1 F1 1.545(4) . ? P1 F5 1.551(4) . ? P1 F3 1.558(4) . ? P1 F2 1.564(4) . ? P1 F4 1.576(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag1 C11 176.90(16) . 2_656 ? C1 N1 C3 110.5(4) . . ? C1 N1 C4 124.5(4) . . ? C3 N1 C4 125.1(4) . . ? C1 N2 C2 110.5(4) . . ? C1 N2 C6 124.3(4) . . ? C2 N2 C6 125.1(4) . . ? C11 N3 C13 110.7(4) . . ? C11 N3 C10 124.7(4) . . ? C13 N3 C10 124.6(4) . . ? C11 N4 C12 110.6(4) . . ? C11 N4 C14 124.1(4) . . ? C12 N4 C14 125.1(5) . . ? N1 C1 N2 104.7(4) . . ? N1 C1 Ag1 130.0(3) . . ? N2 C1 Ag1 125.3(3) . . ? C3 C2 N2 107.0(4) . . ? C3 C2 H2 126.5 . . ? N2 C2 H2 126.5 . . ? C2 C3 N1 107.3(4) . . ? C2 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? C5 C4 N1 113.0(4) . . ? C5 C4 H4A 109.0 . . ? N1 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? N1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 126.3(6) . . ? N2 C6 C7' 103.5(6) . . ? C7 C6 C7' 31.8(6) . . ? N2 C6 H6A 105.7 . . ? C7 C6 H6A 105.7 . . ? C7' C6 H6A 95.0 . . ? N2 C6 H6B 105.7 . . ? C7 C6 H6B 105.7 . . ? C7' C6 H6B 137.3 . . ? H6A C6 H6B 106.2 . . ? C6 C7 C8 105.0(5) . . ? C6 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? C6 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C8 C9 105.1(4) . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C10 C9 C8 115.9(6) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C8' C7' C6 120.9(8) . . ? C8' C7' H7'A 107.1 . . ? C6 C7' H7'A 107.1 . . ? C8' C7' H7'B 107.1 . . ? C6 C7' H7'B 107.1 . . ? H7'A C7' H7'B 106.8 . . ? C7' C8' C9' 122.6(9) . . ? C7' C8' H8'A 106.7 . . ? C9' C8' H8'A 106.7 . . ? C7' C8' H8'B 106.7 . . ? C9' C8' H8'B 106.7 . . ? H8'A C8' H8'B 106.6 . . ? C10 C9' C8' 122.1(8) . . ? C10 C9' H9'A 106.8 . . ? C8' C9' H9'A 106.8 . . ? C10 C9' H9'B 106.8 . . ? C8' C9' H9'B 106.8 . . ? H9'A C9' H9'B 106.7 . . ? N3 C10 C9 116.9(6) . . ? N3 C10 C9' 109.1(7) . . ? C9 C10 C9' 22.2(6) . . ? N3 C10 H10A 108.1 . . ? C9 C10 H10A 108.1 . . ? C9' C10 H10A 129.2 . . ? N3 C10 H10B 108.1 . . ? C9 C10 H10B 108.1 . . ? C9' C10 H10B 92.7 . . ? H10A C10 H10B 107.3 . . ? N4 C11 N3 104.5(4) . . ? N4 C11 Ag1 128.4(3) . 2_656 ? N3 C11 Ag1 127.1(3) . 2_656 ? C13 C12 N4 107.4(4) . . ? C13 C12 H12 126.3 . . ? N4 C12 H12 126.3 . . ? C12 C13 N3 106.8(4) . . ? C12 C13 H13 126.6 . . ? N3 C13 H13 126.6 . . ? C15 C14 N4 116.7(6) . . ? C15 C14 H14A 108.1 . . ? N4 C14 H14A 108.1 . . ? C15 C14 H14B 108.1 . . ? N4 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? F6 P1 F1 88.8(3) . . ? F6 P1 F5 91.8(3) . . ? F1 P1 F5 89.5(3) . . ? F6 P1 F3 178.8(3) . . ? F1 P1 F3 92.4(3) . . ? F5 P1 F3 88.2(3) . . ? F6 P1 F2 90.1(3) . . ? F1 P1 F2 91.7(2) . . ? F5 P1 F2 177.8(3) . . ? F3 P1 F2 89.8(3) . . ? F6 P1 F4 92.2(3) . . ? F1 P1 F4 178.8(3) . . ? F5 P1 F4 91.2(2) . . ? F3 P1 F4 86.6(2) . . ? F2 P1 F4 87.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C1 N2 0.1(5) . . . . ? C4 N1 C1 N2 -179.5(4) . . . . ? C3 N1 C1 Ag1 178.9(3) . . . . ? C4 N1 C1 Ag1 -0.6(7) . . . . ? C2 N2 C1 N1 0.2(5) . . . . ? C6 N2 C1 N1 178.9(4) . . . . ? C2 N2 C1 Ag1 -178.8(3) . . . . ? C6 N2 C1 Ag1 0.0(6) . . . . ? C11 Ag1 C1 N1 160(3) 2_656 . . . ? C11 Ag1 C1 N2 -21(3) 2_656 . . . ? C1 N2 C2 C3 -0.3(6) . . . . ? C6 N2 C2 C3 -179.1(5) . . . . ? N2 C2 C3 N1 0.4(6) . . . . ? C1 N1 C3 C2 -0.3(6) . . . . ? C4 N1 C3 C2 179.3(5) . . . . ? C1 N1 C4 C5 -97.8(7) . . . . ? C3 N1 C4 C5 82.7(7) . . . . ? C1 N2 C6 C7 118.2(6) . . . . ? C2 N2 C6 C7 -63.1(7) . . . . ? C1 N2 C6 C7' 93.6(9) . . . . ? C2 N2 C6 C7' -87.7(9) . . . . ? N2 C6 C7 C8 -66.4(9) . . . . ? C7' C6 C7 C8 -16.1(10) . . . . ? C6 C7 C8 C9 -173.0(8) . . . . ? C7 C8 C9 C10 -179.8(9) . . . . ? N2 C6 C7' C8' -162.7(13) . . . . ? C7 C6 C7' C8' 56.9(12) . . . . ? C6 C7' C8' C9' -167.0(11) . . . . ? C7' C8' C9' C10 -66.5(19) . . . . ? C11 N3 C10 C9 100.4(6) . . . . ? C13 N3 C10 C9 -81.5(6) . . . . ? C11 N3 C10 C9' 123.0(6) . . . . ? C13 N3 C10 C9' -58.9(7) . . . . ? C8 C9 C10 N3 -62.2(11) . . . . ? C8 C9 C10 C9' -136(3) . . . . ? C8' C9' C10 N3 -64.6(13) . . . . ? C8' C9' C10 C9 50.2(18) . . . . ? C12 N4 C11 N3 -0.5(5) . . . . ? C14 N4 C11 N3 -175.8(5) . . . . ? C12 N4 C11 Ag1 179.1(4) . . . 2_656 ? C14 N4 C11 Ag1 3.8(7) . . . 2_656 ? C13 N3 C11 N4 0.8(5) . . . . ? C10 N3 C11 N4 179.0(4) . . . . ? C13 N3 C11 Ag1 -178.8(3) . . . 2_656 ? C10 N3 C11 Ag1 -0.6(6) . . . 2_656 ? C11 N4 C12 C13 0.0(6) . . . . ? C14 N4 C12 C13 175.3(5) . . . . ? N4 C12 C13 N3 0.5(6) . . . . ? C11 N3 C13 C12 -0.8(5) . . . . ? C10 N3 C13 C12 -179.1(4) . . . . ? C11 N4 C14 C15 -114.6(8) . . . . ? C12 N4 C14 C15 70.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.651 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.085 # Attachment 'CIF_2f.cif' data_80615c _database_code_depnum_ccdc_archive 'CCDC 704844' #TrackingRef 'CIF_2f.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H112 Ag4 F24 N16 O P4 ' _chemical_formula_weight 2565.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 24.699(5) _cell_length_b 18.113(4) _cell_length_c 12.594(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5634(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9724 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.64 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592.0 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27078 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5132 _reflns_number_gt 3855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+99.5815P] 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 cosntr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5131 _refine_ls_number_parameters 417 _refine_ls_number_restraints 218 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.2122 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.067 _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 0.16259(3) 0.00934(4) 0.87588(6) 0.0525(3) Uani 1 1 d . . . F1 F 0.1614(6) 0.2500 0.5027(8) 0.101(4) Uani 1 2 d S . . F2 F 0.1154(3) 0.1880(4) 0.3768(7) 0.099(2) Uani 1 1 d . . . F3 F 0.2061(3) 0.1877(4) 0.3779(7) 0.088(2) Uani 1 1 d . . . F4 F 0.1613(6) 0.2500 0.2540(7) 0.116(5) Uani 1 2 d S . . F5 F 0.2026(5) 0.7500 0.3761(14) 0.152(6) Uani 1 2 d S . . F6 F 0.2672(5) 0.8069(8) 0.2908(11) 0.208(7) Uani 1 1 d . . . F7 F 0.2640(5) 0.8090(9) 0.4619(11) 0.219(8) Uani 1 1 d . . . F8 F 0.3308(4) 0.7500 0.3947(6) 0.072(3) Uani 1 2 d S . . N1 N 0.1431(4) 0.0603(5) 0.6440(8) 0.063(3) Uani 1 1 d . A . N2 N 0.1815(4) -0.0448(5) 0.6474(7) 0.059(2) Uani 1 1 d . . . N3 N 0.1495(4) 0.0623(5) 1.1097(8) 0.061(2) Uani 1 1 d . . . N4 N 0.1872(4) -0.0434(5) 1.1050(7) 0.057(2) Uani 1 1 d . . . P1 P 0.16052(17) 0.2500 0.3851(3) 0.0466(8) Uani 1 2 d S . . P2 P 0.26463(19) 0.7500 0.3755(4) 0.0634(11) Uani 1 2 d S . . C1 C 0.1609(5) 0.0091(9) 0.7102(9) 0.078(4) Uani 1 1 d . . . C2 C 0.1516(8) 0.0377(11) 0.5343(12) 0.112(7) Uani 1 1 d . . . H2 H 0.1423 0.0620 0.4719 0.134 Uiso 1 1 calc R . . C3 C 0.1738(7) -0.0207(11) 0.5461(10) 0.102(6) Uani 1 1 d . . . H3 H 0.1854 -0.0483 0.4882 0.122 Uiso 1 1 calc R . . C4 C 0.2053(5) -0.1148(7) 0.6820(10) 0.068(3) Uani 1 1 d . . . H4A H 0.2120 -0.1127 0.7578 0.082 Uiso 1 1 calc R . . H4B H 0.2398 -0.1218 0.6465 0.082 Uiso 1 1 calc R . . C5 C 0.1687(5) -0.1803(6) 0.6580(9) 0.064(3) Uani 1 1 d . . . H5A H 0.1340 -0.1738 0.6926 0.077 Uiso 1 1 calc R . . H5B H 0.1627 -0.1840 0.5821 0.077 Uiso 1 1 calc R . . C6 C 0.1960(8) -0.2500 0.6986(14) 0.075(5) Uani 1 2 d S . . H6A H 0.2336 -0.2500 0.6764 0.090 Uiso 1 2 calc SR . . H6B H 0.1952 -0.2500 0.7756 0.090 Uiso 1 2 calc SR . . C8 C 0.0531(4) 0.1334(10) 0.6679(15) 0.079(11) Uani 0.520(15) 1 d PGDU A 1 C9 C 0.0304(6) 0.1829(11) 0.5964(16) 0.136(14) Uani 0.520(15) 1 d PGDU A 1 H9 H 0.0524 0.2153 0.5588 0.164 Uiso 0.520(15) 1 calc PR A 1 C10 C -0.0254(6) 0.1839(14) 0.5809(19) 0.20(2) Uani 0.520(15) 1 d PGU A 1 H10 H -0.0406 0.2170 0.5330 0.241 Uiso 0.520(15) 1 calc PR A 1 C11 C -0.0583(4) 0.1354(15) 0.637(2) 0.162(18) Uani 0.520(15) 1 d PGU A 1 H11 H -0.0956 0.1361 0.6267 0.195 Uiso 0.520(15) 1 calc PR A 1 C12 C -0.0355(5) 0.0859(13) 0.7086(19) 0.109(11) Uani 0.520(15) 1 d PGU A 1 H12 H -0.0575 0.0535 0.7461 0.131 Uiso 0.520(15) 1 calc PR A 1 C13 C 0.0202(5) 0.0849(11) 0.7240(15) 0.104(10) Uani 0.520(15) 1 d PGDU A 1 H13 H 0.0355 0.0518 0.7719 0.124 Uiso 0.520(15) 1 calc PR A 1 C7 C 0.1136(4) 0.1291(6) 0.6797(10) 0.079(4) Uani 1 1 d D . . H7A H 0.1220 0.1366 0.7542 0.094 Uiso 1 1 calc R A 1 H7B H 0.1290 0.1705 0.6412 0.094 Uiso 1 1 calc R A 1 C8' C 0.0541(4) 0.1132(12) 0.6752(14) 0.053(7) Uani 0.480(15) 1 d PGDU A 2 C9' C 0.0332(6) 0.0705(13) 0.5932(16) 0.133(15) Uani 0.480(15) 1 d PGDU A 2 H9' H 0.0563 0.0490 0.5438 0.159 Uiso 0.480(15) 1 calc PR A 2 C10' C -0.0224(7) 0.0598(16) 0.585(2) 0.21(3) Uani 0.480(15) 1 d PGU A 2 H10' H -0.0364 0.0312 0.5302 0.255 Uiso 0.480(15) 1 calc PR A 2 C12' C -0.0570(4) 0.0919(16) 0.659(2) 0.119(13) Uani 0.480(15) 1 d PGU A 2 H12' H -0.0942 0.0847 0.6534 0.143 Uiso 0.480(15) 1 calc PR A 2 C11' C -0.0361(5) 0.1346(16) 0.741(2) 0.136(16) Uani 0.480(15) 1 d PGU A 2 H11' H -0.0592 0.1561 0.7901 0.163 Uiso 0.480(15) 1 calc PR A 2 C13' C 0.0195(6) 0.1453(14) 0.7489(17) 0.21(3) Uani 0.480(15) 1 d PGDU A 2 H13' H 0.0335 0.1739 0.8038 0.246 Uiso 0.480(15) 1 calc PR A 2 C14 C 0.1656(4) 0.0085(4) 1.0401(7) 0.042(2) Uani 1 1 d . . . C15 C 0.1613(6) 0.0446(6) 1.2068(9) 0.066(3) Uani 1 1 d . B . H15 H 0.1548 0.0743 1.2656 0.080 Uiso 1 1 calc R . . C16 C 0.1847(5) -0.0237(7) 1.2107(9) 0.066(3) Uani 1 1 d . B . H16 H 0.1962 -0.0503 1.2698 0.079 Uiso 1 1 calc R . . C17 C 0.2088(5) -0.1142(6) 1.0675(9) 0.062(3) Uani 1 1 d . . . H17A H 0.2441 -0.1221 1.0994 0.075 Uiso 1 1 calc R . . H17B H 0.2138 -0.1116 0.9912 0.075 Uiso 1 1 calc R . . C18 C 0.1735(4) -0.1786(6) 1.0925(9) 0.061(3) Uani 1 1 d . . . H18A H 0.1388 -0.1725 1.0578 0.073 Uiso 1 1 calc R B . H18B H 0.1674 -0.1809 1.1685 0.073 Uiso 1 1 calc R . . C19 C 0.1998(7) -0.2500 1.0553(14) 0.065(4) Uani 1 2 d S . . H19A H 0.2001 -0.2500 0.9783 0.077 Uiso 1 2 calc SR . . H19B H 0.2372 -0.2500 1.0789 0.077 Uiso 1 2 calc SR . . C21 C 0.0619(4) 0.1235(10) 1.0930(17) 0.10(2) Uani 0.460(14) 1 d PGDU B 1 C22 C 0.0324(5) 0.0691(10) 1.0411(16) 0.093(10) Uani 0.460(14) 1 d PGDU B 1 H22 H 0.0499 0.0355 0.9970 0.111 Uiso 0.460(14) 1 calc PR B 1 C23 C -0.0234(5) 0.0648(11) 1.0549(17) 0.095(10) Uani 0.460(14) 1 d PGU B 1 H23 H -0.0431 0.0284 1.0202 0.114 Uiso 0.460(14) 1 calc PR B 1 C24 C -0.0496(4) 0.1150(13) 1.1208(19) 0.107(14) Uani 0.460(14) 1 d PGU B 1 H24 H -0.0869 0.1121 1.1301 0.128 Uiso 0.460(14) 1 calc PR B 1 C25 C -0.0200(5) 0.1694(12) 1.1728(17) 0.096(11) Uani 0.460(14) 1 d PGU B 1 H25 H -0.0376 0.2030 1.2168 0.115 Uiso 0.460(14) 1 calc PR B 1 C26 C 0.0357(5) 0.1736(10) 1.1589(15) 0.077(8) Uani 0.460(14) 1 d PGDU B 1 H26 H 0.0555 0.2100 1.1936 0.092 Uiso 0.460(14) 1 calc PR B 1 C20 C 0.1223(3) 0.1284(6) 1.0783(10) 0.073(3) Uani 1 1 d DU B 1 H20A H 0.1302 0.1384 1.0042 0.088 Uiso 1 1 calc R B 1 H20B H 0.1361 0.1694 1.1199 0.088 Uiso 1 1 calc R B 1 C21' C 0.0619(3) 0.1275(8) 1.0826(9) 0.048(9) Uani 0.540(14) 1 d PGDU B 2 C22' C 0.0321(5) 0.1502(12) 0.9948(11) 0.137(14) Uani 0.540(14) 1 d PGDU B 2 H22' H 0.0498 0.1655 0.9335 0.164 Uiso 0.540(14) 1 calc PR B 2 C23' C -0.0241(5) 0.1501(15) 0.9987(16) 0.23(3) Uani 0.540(14) 1 d PGU B 2 H23' H -0.0440 0.1653 0.9400 0.280 Uiso 0.540(14) 1 calc PR B 2 C24' C -0.0506(3) 0.1272(13) 1.0904(19) 0.107(13) Uani 0.540(14) 1 d PGU B 2 H24' H -0.0882 0.1271 1.0931 0.128 Uiso 0.540(14) 1 calc PR B 2 C25' C -0.0208(5) 0.1045(11) 1.1782(15) 0.101(9) Uani 0.540(14) 1 d PGU B 2 H25' H -0.0385 0.0892 1.2395 0.121 Uiso 0.540(14) 1 calc PR B 2 C26' C 0.0354(5) 0.1046(10) 1.1743(11) 0.103(10) Uani 0.540(14) 1 d PGDU B 2 H26' H 0.0553 0.0894 1.2330 0.123 Uiso 0.540(14) 1 calc PR B 2 O1 O 0.1641(11) 0.005(2) 0.359(2) 0.087(12) Uani 0.25 1 d P . . 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 0.0645(5) 0.0468(4) 0.0463(4) -0.0011(4) 0.0014(4) -0.0017(4) F1 0.140(11) 0.103(9) 0.059(6) 0.000 0.002(7) 0.000 F2 0.089(5) 0.082(5) 0.125(7) 0.006(5) -0.008(5) -0.030(4) F3 0.102(6) 0.057(4) 0.103(6) 0.005(4) -0.009(5) 0.013(4) F4 0.132(11) 0.188(13) 0.028(5) 0.000 -0.010(6) 0.000 F5 0.060(7) 0.234(18) 0.161(14) 0.000 0.007(9) 0.000 F6 0.162(11) 0.249(15) 0.213(14) 0.159(12) 0.000(10) -0.002(10) F7 0.148(10) 0.298(18) 0.212(13) -0.182(13) -0.003(9) 0.016(11) F8 0.086(7) 0.108(7) 0.022(4) 0.000 0.017(4) 0.000 N1 0.075(6) 0.054(5) 0.059(6) 0.009(5) -0.010(5) -0.016(5) N2 0.064(6) 0.059(5) 0.054(5) 0.005(5) -0.001(4) -0.008(5) N3 0.072(6) 0.050(5) 0.062(6) -0.022(5) 0.020(5) -0.012(4) N4 0.059(5) 0.062(6) 0.049(5) 0.001(4) 0.006(4) -0.007(4) P1 0.073(2) 0.0420(18) 0.0251(16) 0.000 0.0020(18) 0.000 P2 0.068(3) 0.075(3) 0.047(2) 0.000 -0.007(2) 0.000 C1 0.060(7) 0.123(12) 0.053(6) -0.052(8) 0.006(6) -0.032(8) C2 0.145(17) 0.134(15) 0.056(8) 0.047(10) -0.043(9) -0.069(14) C3 0.132(15) 0.144(16) 0.030(6) 0.017(8) -0.012(7) -0.056(13) C4 0.069(8) 0.071(8) 0.063(7) -0.021(6) -0.008(6) 0.002(6) C5 0.060(7) 0.069(7) 0.063(7) -0.008(6) -0.004(6) 0.006(6) C6 0.080(13) 0.085(13) 0.060(11) 0.000 0.007(10) 0.000 C8 0.086(14) 0.071(13) 0.082(14) 0.008(9) 0.001(9) 0.001(8) C9 0.130(16) 0.137(16) 0.142(17) -0.009(10) -0.005(10) 0.003(10) C10 0.20(2) 0.20(3) 0.20(3) -0.005(10) -0.001(10) 0.001(10) C11 0.16(2) 0.16(2) 0.16(2) 0.000(10) 0.003(10) -0.002(10) C12 0.098(13) 0.112(14) 0.117(14) 0.000(9) -0.004(9) -0.007(9) C13 0.097(13) 0.105(13) 0.109(13) 0.006(9) 0.005(9) 0.008(9) C7 0.107(11) 0.048(7) 0.081(9) 0.013(6) -0.021(8) -0.007(7) C8' 0.064(11) 0.035(8) 0.060(10) 0.015(8) 0.006(8) -0.007(7) C9' 0.125(17) 0.136(17) 0.138(17) 0.011(10) -0.008(10) -0.001(10) C10' 0.21(3) 0.21(3) 0.22(3) 0.009(10) 0.000(10) 0.002(10) C12' 0.120(16) 0.121(16) 0.117(16) 0.010(10) -0.002(10) -0.001(10) C11' 0.130(18) 0.139(18) 0.139(18) -0.005(10) 0.010(10) 0.006(10) C13' 0.21(3) 0.20(3) 0.20(3) -0.002(10) 0.000(10) -0.001(10) C14 0.050(5) 0.019(4) 0.057(5) -0.028(4) 0.010(5) -0.007(4) C15 0.107(10) 0.047(6) 0.046(6) -0.002(5) 0.015(6) -0.020(7) C16 0.084(9) 0.063(7) 0.050(6) 0.009(6) -0.010(6) -0.012(6) C17 0.059(7) 0.063(7) 0.065(7) 0.008(6) -0.004(6) 0.009(6) C18 0.054(7) 0.062(7) 0.066(7) 0.000(6) -0.003(5) 0.002(5) C19 0.062(11) 0.068(11) 0.064(11) 0.000 0.008(8) 0.000 C21 0.10(2) 0.10(2) 0.10(2) -0.002(7) -0.003(7) 0.001(7) C22 0.090(12) 0.091(12) 0.097(12) -0.004(7) 0.004(7) 0.000(7) C23 0.094(12) 0.092(12) 0.098(12) -0.001(7) 0.001(7) -0.004(7) C24 0.102(15) 0.108(15) 0.110(15) 0.003(7) -0.001(7) -0.004(7) C25 0.094(12) 0.094(12) 0.099(12) -0.010(7) 0.003(7) -0.002(7) C26 0.072(10) 0.080(10) 0.079(10) -0.011(7) 0.003(7) -0.003(7) C20 0.088(7) 0.054(6) 0.078(7) -0.014(5) 0.017(6) -0.003(6) C21' 0.054(12) 0.037(10) 0.053(11) -0.006(7) -0.005(7) -0.004(7) C22' 0.137(16) 0.143(16) 0.131(16) -0.001(10) 0.002(10) -0.001(10) C23' 0.23(3) 0.24(3) 0.23(3) 0.000(10) -0.004(10) 0.004(10) C24' 0.095(15) 0.114(15) 0.112(15) 0.011(9) -0.005(9) 0.001(9) C25' 0.099(12) 0.097(12) 0.107(12) 0.018(9) -0.001(9) 0.001(9) C26' 0.099(12) 0.105(13) 0.104(13) 0.010(9) -0.009(9) 0.002(9) O1 0.042(15) 0.18(4) 0.035(14) -0.05(2) -0.015(13) -0.01(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 Ag1 C14 2.070(9) . ? Ag1 C1 2.087(11) . ? F1 P1 1.481(11) . ? F2 P1 1.586(7) . ? F3 P1 1.597(7) . ? F4 P1 1.652(10) . ? F5 P2 1.533(13) . ? F6 P2 1.485(11) . ? F7 P2 1.525(11) . ? F8 P2 1.652(11) . ? N1 C1 1.323(17) . ? N1 C2 1.455(19) . ? N1 C7 1.513(15) . ? N2 C1 1.356(15) . ? N2 C3 1.361(15) . ? N2 C4 1.464(14) . ? N3 C15 1.297(14) . ? N3 C14 1.370(11) . ? N3 C20 1.430(14) . ? N4 C14 1.355(13) . ? N4 C16 1.379(14) . ? N4 C17 1.468(14) . ? P1 F2 1.586(7) 7_565 ? P1 F3 1.597(7) 7_565 ? P2 F6 1.485(11) 7_575 ? P2 F7 1.525(11) 7_575 ? C2 C3 1.20(2) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.521(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.520(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.520(15) 7 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C8 C7 1.502(6) . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C7 C8' 1.498(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8' C9' 1.3900 . ? C8' C13' 1.3900 . ? C9' C10' 1.3900 . ? C9' H9' 0.9300 . ? C10' C12' 1.3900 . ? C10' H10' 0.9300 . ? C12' C11' 1.3900 . ? C12' H12' 0.9300 . ? C11' C13' 1.3900 . ? C11' H11' 0.9300 . ? C13' H13' 0.9300 . ? C15 C16 1.366(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.489(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.521(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C18 1.521(13) 7 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 C20 1.506(6) . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21' C22' 1.3900 . ? C21' C26' 1.3900 . ? C22' C23' 1.3900 . ? C22' H22' 0.9300 . ? C23' C24' 1.3900 . ? C23' H23' 0.9300 . ? C24' C25' 1.3900 . ? C24' H24' 0.9300 . ? C25' C26' 1.3900 . ? C25' H25' 0.9300 . ? C26' H26' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ag1 C1 178.9(5) . . ? C1 N1 C2 110.7(12) . . ? C1 N1 C7 123.4(10) . . ? C2 N1 C7 125.7(12) . . ? C1 N2 C3 105.2(13) . . ? C1 N2 C4 126.9(11) . . ? C3 N2 C4 127.8(12) . . ? C15 N3 C14 111.2(10) . . ? C15 N3 C20 125.0(10) . . ? C14 N3 C20 123.8(10) . . ? C14 N4 C16 112.7(9) . . ? C14 N4 C17 123.7(8) . . ? C16 N4 C17 123.5(10) . . ? F1 P1 F2 94.4(5) . 7_565 ? F1 P1 F2 94.4(5) . . ? F2 P1 F2 90.1(6) 7_565 . ? F1 P1 F3 92.6(5) . . ? F2 P1 F3 172.9(5) 7_565 . ? F2 P1 F3 89.5(4) . . ? F1 P1 F3 92.6(5) . 7_565 ? F2 P1 F3 89.5(4) 7_565 7_565 ? F2 P1 F3 172.9(5) . 7_565 ? F3 P1 F3 90.0(6) . 7_565 ? F1 P1 F4 178.5(8) . . ? F2 P1 F4 86.6(5) 7_565 . ? F2 P1 F4 86.6(5) . . ? F3 P1 F4 86.3(5) . . ? F3 P1 F4 86.3(5) 7_565 . ? F6 P2 F6 87.9(14) 7_575 . ? F6 P2 F7 178.1(8) 7_575 . ? F6 P2 F7 91.6(9) . . ? F6 P2 F7 91.6(9) 7_575 7_575 ? F6 P2 F7 178.1(8) . 7_575 ? F7 P2 F7 88.9(14) . 7_575 ? F6 P2 F5 92.7(7) 7_575 . ? F6 P2 F5 92.7(7) . . ? F7 P2 F5 89.2(7) . . ? F7 P2 F5 89.2(7) 7_575 . ? F6 P2 F8 93.6(6) 7_575 . ? F6 P2 F8 93.6(6) . . ? F7 P2 F8 84.6(5) . . ? F7 P2 F8 84.6(5) 7_575 . ? F5 P2 F8 171.3(8) . . ? N1 C1 N2 105.2(10) . . ? N1 C1 Ag1 129.5(10) . . ? N2 C1 Ag1 125.3(11) . . ? C3 C2 N1 101.3(13) . . ? C3 C2 H2 129.3 . . ? N1 C2 H2 129.3 . . ? C2 C3 N2 117.5(18) . . ? C2 C3 H3 121.2 . . ? N2 C3 H3 121.2 . . ? N2 C4 C5 112.2(9) . . ? N2 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 108.5(10) . . ? C6 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C5 C6 C5 112.4(15) 7 . ? C5 C6 H6A 109.1 7 . ? C5 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 7 . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C9 C8 C13 120.0 . . ? C9 C8 C7 120.0(4) . . ? C13 C8 C7 119.9(4) . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C8' C7 C8 14.5(11) . . ? C8' C7 N1 107.6(9) . . ? C8 C7 N1 119.5(12) . . ? C8' C7 H7A 105.8 . . ? C8 C7 H7A 107.4 . . ? N1 C7 H7A 107.4 . . ? C8' C7 H7B 120.9 . . ? C8 C7 H7B 107.4 . . ? N1 C7 H7B 107.4 . . ? H7A C7 H7B 107.0 . . ? C9' C8' C13' 120.0 . . ? C9' C8' C7 120.1(4) . . ? C13' C8' C7 119.8(4) . . ? C8' C9' C10' 120.0 . . ? C8' C9' H9' 120.0 . . ? C10' C9' H9' 120.0 . . ? C12' C10' C9' 120.0 . . ? C12' C10' H10' 120.0 . . ? C9' C10' H10' 120.0 . . ? C10' C12' C11' 120.0 . . ? C10' C12' H12' 120.0 . . ? C11' C12' H12' 120.0 . . ? C13' C11' C12' 120.0 . . ? C13' C11' H11' 120.0 . . ? C12' C11' H11' 120.0 . . ? C11' C13' C8' 120.0 . . ? C11' C13' H13' 120.0 . . ? C8' C13' H13' 120.0 . . ? N4 C14 N3 102.8(9) . . ? N4 C14 Ag1 128.5(6) . . ? N3 C14 Ag1 128.6(8) . . ? N3 C15 C16 110.7(11) . . ? N3 C15 H15 124.7 . . ? C16 C15 H15 124.7 . . ? C15 C16 N4 102.6(10) . . ? C15 C16 H16 128.7 . . ? N4 C16 H16 128.7 . . ? N4 C17 C18 113.8(9) . . ? N4 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? N4 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 110.6(10) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C18 116.5(14) 7 . ? C18 C19 H19A 108.2 7 . ? C18 C19 H19A 108.2 . . ? C18 C19 H19B 108.2 7 . ? C18 C19 H19B 108.2 . . ? H19A C19 H19B 107.3 . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 120.3(4) . . ? C26 C21 C20 119.7(4) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? N3 C20 C21 112.4(12) . . ? N3 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N3 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22' C21' C26' 120.0 . . ? C21' C22' C23' 120.0 . . ? C21' C22' H22' 120.0 . . ? C23' C22' H22' 120.0 . . ? C22' C23' C24' 120.0 . . ? C22' C23' H23' 120.0 . . ? C24' C23' H23' 120.0 . . ? C25' C24' C23' 120.0 . . ? C25' C24' H24' 120.0 . . ? C23' C24' H24' 120.0 . . ? C26' C25' C24' 120.0 . . ? C26' C25' H25' 120.0 . . ? C24' C25' H25' 120.0 . . ? C25' C26' C21' 120.0 . . ? C25' C26' H26' 120.0 . . ? C21' C26' H26' 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 1.2(14) . . . . ? C7 N1 C1 N2 176.1(8) . . . . ? C2 N1 C1 Ag1 178.0(10) . . . . ? C7 N1 C1 Ag1 -7.1(17) . . . . ? C3 N2 C1 N1 -0.3(13) . . . . ? C4 N2 C1 N1 -178.5(10) . . . . ? C3 N2 C1 Ag1 -177.2(10) . . . . ? C4 N2 C1 Ag1 4.5(16) . . . . ? C14 Ag1 C1 N1 -145(22) . . . . ? C14 Ag1 C1 N2 31(24) . . . . ? C1 N1 C2 C3 -1.8(18) . . . . ? C7 N1 C2 C3 -176.5(13) . . . . ? N1 C2 C3 N2 2(2) . . . . ? C1 N2 C3 C2 -1(2) . . . . ? C4 N2 C3 C2 177.2(15) . . . . ? C1 N2 C4 C5 107.9(12) . . . . ? C3 N2 C4 C5 -70.0(16) . . . . ? N2 C4 C5 C6 -178.8(11) . . . . ? C4 C5 C6 C5 -167.8(10) . . . 7 ? C13 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 176(2) . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C8 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? C7 C8 C13 C12 -176(2) . . . . ? C9 C8 C7 C8' -149(5) . . . . ? C13 C8 C7 C8' 27(4) . . . . ? C9 C8 C7 N1 -112.4(14) . . . . ? C13 C8 C7 N1 63.8(18) . . . . ? C1 N1 C7 C8' -93.5(14) . . . . ? C2 N1 C7 C8' 80.6(16) . . . . ? C1 N1 C7 C8 -102.5(13) . . . . ? C2 N1 C7 C8 71.6(15) . . . . ? C8 C7 C8' C9' 109(5) . . . . ? N1 C7 C8' C9' -38(2) . . . . ? C8 C7 C8' C13' -67(4) . . . . ? N1 C7 C8' C13' 146.5(14) . . . . ? C13' C8' C9' C10' 0.0 . . . . ? C7 C8' C9' C10' -176(2) . . . . ? C8' C9' C10' C12' 0.0 . . . . ? C9' C10' C12' C11' 0.0 . . . . ? C10' C12' C11' C13' 0.0 . . . . ? C12' C11' C13' C8' 0.0 . . . . ? C9' C8' C13' C11' 0.0 . . . . ? C7 C8' C13' C11' 176(2) . . . . ? C16 N4 C14 N3 0.2(12) . . . . ? C17 N4 C14 N3 177.9(9) . . . . ? C16 N4 C14 Ag1 176.5(8) . . . . ? C17 N4 C14 Ag1 -5.8(14) . . . . ? C15 N3 C14 N4 1.1(12) . . . . ? C20 N3 C14 N4 -177.8(8) . . . . ? C15 N3 C14 Ag1 -175.2(8) . . . . ? C20 N3 C14 Ag1 5.9(14) . . . . ? C1 Ag1 C14 N4 -31(23) . . . . ? C1 Ag1 C14 N3 144(23) . . . . ? C14 N3 C15 C16 -2.0(14) . . . . ? C20 N3 C15 C16 176.8(10) . . . . ? N3 C15 C16 N4 2.0(14) . . . . ? C14 N4 C16 C15 -1.3(13) . . . . ? C17 N4 C16 C15 -179.0(10) . . . . ? C14 N4 C17 C18 -106.6(11) . . . . ? C16 N4 C17 C18 70.9(14) . . . . ? N4 C17 C18 C19 -177.6(11) . . . . ? C17 C18 C19 C18 169.5(10) . . . 7 ? C26 C21 C22 C23 0.0 . . . . ? C20 C21 C22 C23 -180(2) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? C20 C21 C26 C25 180(2) . . . . ? C15 N3 C20 C21 -80.4(14) . . . . ? C14 N3 C20 C21 98.4(12) . . . . ? C22 C21 C20 N3 -59.1(18) . . . . ? C26 C21 C20 N3 120.9(13) . . . . ? C26' C21' C22' C23' 0.0 . . . . ? C21' C22' C23' C24' 0.0 . . . . ? C22' C23' C24' C25' 0.0 . . . . ? C23' C24' C25' C26' 0.0 . . . . ? C24' C25' C26' C21' 0.0 . . . . ? C22' C21' C26' C25' 0.0 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.768 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.130 # Attachment 'CIF_2g.cif' data_80121b _database_code_depnum_ccdc_archive 'CCDC 704845' #TrackingRef 'CIF_2g.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H134 Ag4 F24 N16 O P4 S' _chemical_formula_weight 2643.68 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' 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 P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.8837(10) _cell_length_b 16.5498(15) _cell_length_c 17.1589(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.671(2) _cell_angle_gamma 90.00 _cell_volume 3344.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6506 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1346 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20815 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.02 _reflns_number_total 8372 _reflns_number_gt 4624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^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 0.0097(11) _refine_ls_number_reflns 8079 _refine_ls_number_parameters 400 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.82908(3) 0.44467(2) 0.230324(17) 0.06943(16) Uani 1 1 d . . . C1 C 0.8328(4) 0.4501(3) 0.3521(3) 0.0669(11) Uani 1 1 d . . . N1 N 0.7925(3) 0.5089(2) 0.3942(2) 0.0702(9) Uani 1 1 d . A . N2 N 0.8878(3) 0.3984(2) 0.40538(18) 0.0634(8) Uani 1 1 d . . . C2 C 0.8211(4) 0.4963(3) 0.4738(2) 0.0684(11) Uani 1 1 d . . . N3 N 0.7956(3) 0.5126(2) 0.06263(19) 0.0640(9) Uani 1 1 d . . . C3 C 0.8832(4) 0.4259(3) 0.4821(2) 0.0650(11) Uani 1 1 d . . . N4 N 0.8839(3) 0.39886(19) 0.06440(18) 0.0587(8) Uani 1 1 d . . . C4 C 0.9296(5) 0.3959(3) 0.5540(3) 0.0812(13) Uani 1 1 d . . . H4 H 0.9706 0.3479 0.5584 0.097 Uiso 1 1 calc R . . C5 C 0.9126(6) 0.4396(4) 0.6177(3) 0.0993(18) Uani 1 1 d . . . H5 H 0.9432 0.4221 0.6676 0.119 Uiso 1 1 calc R . . C6 C 0.8484(6) 0.5121(5) 0.6093(3) 0.105(2) Uani 1 1 d . . . H6 H 0.8373 0.5406 0.6543 0.126 Uiso 1 1 calc R . . C7 C 0.8030(5) 0.5412(3) 0.5392(3) 0.0839(14) Uani 1 1 d . . . H7 H 0.7616 0.5891 0.5347 0.101 Uiso 1 1 calc R . . C8 C 0.9472(4) 0.3256(2) 0.3869(3) 0.0683(11) Uani 1 1 d . . . H8A H 1.0212 0.3240 0.4185 0.082 Uiso 1 1 calc R . . H8B H 0.9587 0.3267 0.3320 0.082 Uiso 1 1 calc R . . C9 C 0.8809(5) 0.2500 0.4027(4) 0.0671(15) Uani 1 2 d S . . H9A H 0.8662 0.2500 0.4569 0.081 Uiso 1 2 calc SR . . H9B H 0.8084 0.2500 0.3691 0.081 Uiso 1 2 calc SR . . C10 C 0.7279(5) 0.5772(3) 0.3596(3) 0.0953(16) Uani 1 1 d D . . H10A H 0.7375 0.5829 0.3052 0.114 Uiso 0.705(10) 1 d PR A 1 H10B H 0.7523 0.6263 0.3866 0.114 Uiso 0.705(10) 1 d PR A 1 H10C H 0.7322 0.5780 0.3041 0.114 Uiso 0.295(10) 1 d PR A 2 H10D H 0.7618 0.6262 0.3816 0.114 Uiso 0.295(10) 1 d PR A 2 C11 C 0.6028(7) 0.5710(8) 0.3716(8) 0.146(4) Uani 0.705(10) 1 d PDU A 1 H11A H 0.5636 0.6211 0.3563 0.176 Uiso 0.705(10) 1 calc PR A 1 H11B H 0.5964 0.5605 0.4265 0.176 Uiso 0.705(10) 1 calc PR A 1 C12 C 0.5503(8) 0.5005(8) 0.3197(9) 0.162(4) Uani 0.705(10) 1 d PDU A 1 H12A H 0.5761 0.5030 0.2685 0.195 Uiso 0.705(10) 1 calc PR A 1 H12B H 0.5745 0.4493 0.3439 0.195 Uiso 0.705(10) 1 calc PR A 1 C13 C 0.4216(9) 0.5066(13) 0.3105(12) 0.231(6) Uani 0.705(10) 1 d PDU A 1 H13A H 0.3890 0.4576 0.2876 0.346 Uiso 0.705(10) 1 calc PR A 1 H13B H 0.3972 0.5514 0.2769 0.346 Uiso 0.705(10) 1 calc PR A 1 H13C H 0.3975 0.5146 0.3611 0.346 Uiso 0.705(10) 1 calc PR A 1 C11' C 0.6007(13) 0.560(2) 0.3338(15) 0.156(4) Uani 0.295(10) 1 d PDU A 2 H11C H 0.5587 0.6098 0.3260 0.187 Uiso 0.295(10) 1 calc PR A 2 H11D H 0.5910 0.5298 0.2847 0.187 Uiso 0.295(10) 1 calc PR A 2 C12' C 0.5564(16) 0.509(2) 0.3988(13) 0.160(4) Uani 0.295(10) 1 d PDU A 2 H12C H 0.6112 0.4678 0.4171 0.192 Uiso 0.295(10) 1 calc PR A 2 H12D H 0.5465 0.5439 0.4430 0.192 Uiso 0.295(10) 1 calc PR A 2 C13' C 0.443(2) 0.470(2) 0.367(2) 0.192(7) Uani 0.295(10) 1 d PDU A 2 H13D H 0.4409 0.4607 0.3115 0.287 Uiso 0.295(10) 1 calc PR A 2 H13E H 0.3822 0.5057 0.3756 0.287 Uiso 0.295(10) 1 calc PR A 2 H13F H 0.4355 0.4199 0.3933 0.287 Uiso 0.295(10) 1 calc PR A 2 C14 C 0.8352(4) 0.4515(2) 0.1097(2) 0.0613(10) Uani 1 1 d . . . C15 C 0.8209(4) 0.4999(3) -0.0134(2) 0.0648(10) Uani 1 1 d . . . C16 C 0.8785(4) 0.4273(3) -0.0119(2) 0.0616(10) Uani 1 1 d . . . C17 C 0.9199(4) 0.3979(3) -0.0782(3) 0.0790(13) Uani 1 1 d . . . H17 H 0.9589 0.3491 -0.0778 0.095 Uiso 1 1 calc R . . C18 C 0.8998(6) 0.4448(4) -0.1440(3) 0.1007(19) Uani 1 1 d . . . H18 H 0.9284 0.4275 -0.1891 0.121 Uiso 1 1 calc R . . C19 C 0.8407(6) 0.5150(4) -0.1476(3) 0.1019(19) Uani 1 1 d . . . H19 H 0.8268 0.5424 -0.1952 0.122 Uiso 1 1 calc R . . C20 C 0.8004(5) 0.5469(3) -0.0821(3) 0.0816(14) Uani 1 1 d . . . H20 H 0.7624 0.5961 -0.0835 0.098 Uiso 1 1 calc R . . C21 C 0.9403(4) 0.3243(2) 0.0923(3) 0.0654(10) Uani 1 1 d . . . H21A H 0.9524 0.3248 0.1494 0.078 Uiso 1 1 calc R . . H21B H 1.0141 0.3219 0.0742 0.078 Uiso 1 1 calc R . . C22 C 0.8735(5) 0.2500 0.0646(4) 0.0632(14) Uani 1 2 d S . . H22A H 0.8015 0.2500 0.0853 0.076 Uiso 1 2 calc SR . . H22B H 0.8582 0.2500 0.0077 0.076 Uiso 1 2 calc SR . . C23 C 0.7322(5) 0.5816(3) 0.0874(3) 0.0824(14) Uani 1 1 d . . . H23A H 0.7527 0.6297 0.0602 0.099 Uiso 1 1 calc R . . H23B H 0.7531 0.5903 0.1434 0.099 Uiso 1 1 calc R . . C24 C 0.6062(5) 0.5688(4) 0.0703(4) 0.1039(19) Uani 1 1 d . . . H24A H 0.5855 0.5598 0.0144 0.125 Uiso 1 1 calc R . . H24B H 0.5858 0.5207 0.0977 0.125 Uiso 1 1 calc R . . C25 C 0.5413(7) 0.6387(5) 0.0950(6) 0.157(3) Uani 1 1 d . . . H25A H 0.5625 0.6870 0.0684 0.189 Uiso 1 1 calc R . . H25B H 0.5607 0.6470 0.1512 0.189 Uiso 1 1 calc R . . C26 C 0.4152(7) 0.6258(7) 0.0763(8) 0.231(6) Uani 1 1 d . . . H26A H 0.3952 0.6205 0.0204 0.346 Uiso 1 1 calc R . . H26B H 0.3758 0.6711 0.0947 0.346 Uiso 1 1 calc R . . H26C H 0.3942 0.5774 0.1017 0.346 Uiso 1 1 calc R . . P1 P 0.90492(19) 0.7500 0.23934(15) 0.0928(6) Uani 1 2 d S . . F1 F 0.9021(6) 0.7500 0.1471(3) 0.146(2) Uani 1 2 d S . . F2 F 0.7741(4) 0.7500 0.2285(4) 0.1260(17) Uani 1 2 d S . . P2 P 0.22483(18) 0.2500 0.26692(14) 0.0853(5) Uani 1 2 d S . . F3 F 0.9122(6) 0.7500 0.3307(3) 0.152(2) Uani 1 2 d S . . F4 F 1.0357(5) 0.7500 0.2442(6) 0.203(4) Uani 1 2 d S . . F5 F 0.9043(3) 0.65509(19) 0.2391(2) 0.1213(12) Uani 1 1 d . . . F6 F 0.3142(5) 0.3140(4) 0.2738(5) 0.247(3) Uani 1 1 d . . . F7 F 0.1264(5) 0.3124(3) 0.2571(3) 0.174(2) Uani 1 1 d . . . F8 F 0.2166(6) 0.2500 0.3591(3) 0.165(3) Uani 1 2 d S . . F9 F 0.2258(7) 0.2500 0.1766(4) 0.175(3) Uani 1 2 d S . . S1 S 0.6207(6) 0.2500 0.2233(3) 0.159(3) Uani 0.50 2 d SPD . . O1 O 0.7296(11) 0.2500 0.2127(6) 0.115(4) Uani 0.50 2 d SP . . C27 C 0.5532(12) 0.3276(3) 0.1714(10) 0.168(7) Uani 0.50 1 d PD . . H27A H 0.6072 0.3581 0.1465 0.252 Uiso 0.50 1 calc PR . . H27B H 0.5185 0.3621 0.2063 0.252 Uiso 0.50 1 calc PR . . H27C H 0.4959 0.3064 0.1320 0.252 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 0.0909(3) 0.0701(2) 0.0468(2) -0.00178(14) 0.00736(16) 0.00245(17) C1 0.084(3) 0.063(2) 0.055(2) -0.0019(19) 0.012(2) -0.002(2) N1 0.088(3) 0.063(2) 0.060(2) -0.0015(17) 0.0114(18) 0.0079(19) N2 0.080(2) 0.062(2) 0.0493(17) -0.0008(15) 0.0132(16) 0.0011(17) C2 0.088(3) 0.065(3) 0.055(2) -0.005(2) 0.018(2) -0.007(2) N3 0.076(2) 0.059(2) 0.0551(19) -0.0012(16) 0.0010(16) 0.0020(17) C3 0.079(3) 0.068(3) 0.050(2) -0.0008(18) 0.013(2) -0.007(2) N4 0.070(2) 0.0551(19) 0.0494(16) 0.0012(14) 0.0026(15) 0.0020(15) C4 0.108(4) 0.077(3) 0.058(3) 0.004(2) 0.008(2) -0.007(3) C5 0.131(5) 0.118(5) 0.048(2) 0.001(3) 0.010(3) -0.011(4) C6 0.131(5) 0.128(5) 0.059(3) -0.032(3) 0.028(3) -0.024(4) C7 0.112(4) 0.078(3) 0.067(3) -0.010(2) 0.031(3) -0.002(3) C8 0.084(3) 0.060(2) 0.062(2) -0.0049(19) 0.015(2) 0.002(2) C9 0.071(4) 0.060(3) 0.072(4) 0.000 0.013(3) 0.000 C10 0.125(5) 0.074(3) 0.086(4) -0.003(3) 0.011(3) 0.019(3) C11 0.132(5) 0.142(6) 0.164(6) 0.002(5) 0.014(5) 0.021(5) C12 0.140(5) 0.158(6) 0.185(6) -0.004(5) 0.008(5) 0.005(5) C13 0.209(9) 0.232(9) 0.248(9) -0.001(8) 0.020(7) -0.009(8) C11' 0.143(6) 0.151(6) 0.172(7) 0.003(6) 0.015(6) 0.013(5) C12' 0.147(6) 0.156(6) 0.176(7) 0.000(6) 0.018(6) 0.009(5) C13' 0.182(9) 0.192(9) 0.198(10) 0.004(8) 0.017(8) -0.001(8) C14 0.078(3) 0.054(2) 0.051(2) 0.0010(17) 0.0047(19) -0.0009(19) C15 0.068(3) 0.062(2) 0.062(2) 0.002(2) -0.002(2) -0.007(2) C16 0.064(2) 0.066(3) 0.054(2) 0.0039(18) 0.0043(18) -0.0082(19) C17 0.093(3) 0.082(3) 0.067(3) -0.001(2) 0.026(2) -0.006(3) C18 0.134(5) 0.113(5) 0.060(3) 0.004(3) 0.031(3) -0.012(4) C19 0.146(6) 0.105(5) 0.056(3) 0.027(3) 0.017(3) -0.013(4) C20 0.095(4) 0.073(3) 0.073(3) 0.021(2) -0.004(3) -0.010(2) C21 0.070(3) 0.058(2) 0.066(2) 0.0040(19) 0.002(2) 0.0020(19) C22 0.062(3) 0.054(3) 0.073(4) 0.000 0.005(3) 0.000 C23 0.106(4) 0.058(2) 0.081(3) -0.007(2) 0.004(3) 0.012(2) C24 0.102(4) 0.083(4) 0.126(5) -0.017(3) 0.011(4) 0.013(3) C25 0.139(7) 0.103(5) 0.226(10) -0.032(6) 0.010(6) 0.024(5) C26 0.101(6) 0.163(9) 0.43(2) -0.054(11) 0.040(8) 0.015(6) P1 0.0938(15) 0.0704(11) 0.1101(17) 0.000 -0.0017(12) 0.000 F1 0.211(7) 0.112(4) 0.125(4) 0.000 0.057(4) 0.000 F2 0.088(3) 0.132(4) 0.156(5) 0.000 0.009(3) 0.000 P2 0.0787(12) 0.0688(11) 0.1086(16) 0.000 0.0135(11) 0.000 F3 0.227(7) 0.109(4) 0.104(4) 0.000 -0.037(4) 0.000 F4 0.103(4) 0.130(5) 0.375(13) 0.000 0.030(6) 0.000 F5 0.140(3) 0.0679(19) 0.152(3) 0.0013(19) 0.003(2) 0.0023(19) F6 0.181(5) 0.207(6) 0.353(9) -0.042(6) 0.030(5) -0.123(5) F7 0.171(4) 0.204(5) 0.152(4) 0.032(3) 0.039(3) 0.087(4) F8 0.148(5) 0.242(8) 0.097(4) 0.000 -0.009(4) 0.000 F9 0.216(7) 0.193(7) 0.133(5) 0.000 0.088(5) 0.000 S1 0.108(4) 0.270(10) 0.099(4) 0.000 0.010(3) 0.000 O1 0.127(10) 0.166(12) 0.058(6) 0.000 0.033(6) 0.000 C27 0.123(12) 0.170(17) 0.22(2) 0.009(14) 0.044(13) -0.046(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C14 2.085(4) . ? Ag1 C1 2.086(4) . ? C1 N1 1.338(5) . ? C1 N2 1.355(5) . ? N1 C2 1.378(5) . ? N1 C10 1.448(6) . ? N2 C3 1.401(5) . ? N2 C8 1.454(5) . ? C2 C3 1.376(6) . ? C2 C7 1.388(6) . ? N3 C14 1.338(5) . ? N3 C15 1.392(5) . ? N3 C23 1.462(6) . ? C3 C4 1.374(6) . ? N4 C14 1.349(5) . ? N4 C16 1.384(5) . ? N4 C21 1.454(5) . ? C4 C5 1.349(7) . ? C4 H4 0.9300 . ? C5 C6 1.418(9) . ? C5 H5 0.9300 . ? C6 C7 1.339(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.522(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C8 1.521(5) 4_565 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.531(8) . ? C10 C11' 1.545(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9599 . ? C10 H10C 0.9600 . ? C10 H10D 0.9599 . ? C11 C12 1.547(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.520(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C11' C12' 1.538(10) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' C13' 1.527(10) . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C15 C16 1.381(6) . ? C15 C20 1.407(6) . ? C16 C17 1.387(6) . ? C17 C18 1.366(7) . ? C17 H17 0.9300 . ? C18 C19 1.355(9) . ? C18 H18 0.9300 . ? C19 C20 1.383(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.506(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C21 1.506(5) 4_565 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.502(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.484(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.505(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? P1 F2 1.541(6) . ? P1 F4 1.546(7) . ? P1 F3 1.558(6) . ? P1 F5 1.571(3) . ? P1 F5 1.571(3) 4_575 ? P1 F1 1.578(6) . ? P2 F6 1.494(5) 4_565 ? P2 F6 1.494(5) . ? P2 F9 1.552(7) . ? P2 F7 1.553(5) 4_565 ? P2 F7 1.553(5) . ? P2 F8 1.598(6) . ? S1 O1 1.330(12) . ? S1 C27 1.702(8) 4_565 ? S1 C27 1.702(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 C14 Ag1 C1 173.57(17) . . ? N1 C1 N2 105.7(4) . . ? N1 C1 Ag1 127.7(3) . . ? N2 C1 Ag1 126.3(3) . . ? C1 N1 C2 111.5(4) . . ? C1 N1 C10 123.7(4) . . ? C2 N1 C10 124.9(4) . . ? C1 N2 C3 110.7(4) . . ? C1 N2 C8 125.6(3) . . ? C3 N2 C8 123.7(4) . . ? C3 C2 N1 106.8(4) . . ? C3 C2 C7 120.6(4) . . ? N1 C2 C7 132.5(5) . . ? C14 N3 C15 110.4(4) . . ? C14 N3 C23 124.6(4) . . ? C15 N3 C23 125.0(4) . . ? C4 C3 C2 123.0(4) . . ? C4 C3 N2 131.6(4) . . ? C2 C3 N2 105.3(4) . . ? C14 N4 C16 110.8(3) . . ? C14 N4 C21 125.0(3) . . ? C16 N4 C21 124.2(3) . . ? C5 C4 C3 116.6(5) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 122.9(5) . . ? C7 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C6 C7 C2 116.5(5) . . ? C6 C7 H7 121.8 . . ? C2 C7 H7 121.8 . . ? N2 C8 C9 111.4(4) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C8 110.5(5) 4_565 . ? C8 C9 H9A 109.5 4_565 . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 4_565 . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C11 111.3(7) . . ? N1 C10 C11' 114.4(12) . . ? C11 C10 C11' 25.3(12) . . ? N1 C10 H10A 110.4 . . ? C11 C10 H10A 112.4 . . ? C11' C10 H10A 88.8 . . ? N1 C10 H10B 110.6 . . ? C11 C10 H10B 103.2 . . ? C11' C10 H10B 121.3 . . ? H10A C10 H10B 108.6 . . ? N1 C10 H10C 108.8 . . ? C11 C10 H10C 108.4 . . ? C11' C10 H10C 84.2 . . ? H10A C10 H10C 6.1 . . ? H10B C10 H10C 114.4 . . ? N1 C10 H10D 109.1 . . ? C11 C10 H10D 111.6 . . ? C11' C10 H10D 128.0 . . ? H10A C10 H10D 101.6 . . ? H10B C10 H10D 8.9 . . ? H10C C10 H10D 107.6 . . ? C10 C11 C12 107.3(7) . . ? C10 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? C10 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? C13 C12 C11 109.4(8) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12' C11' C10 108.2(9) . . ? C12' C11' H11C 110.1 . . ? C10 C11' H11C 110.1 . . ? C12' C11' H11D 110.1 . . ? C10 C11' H11D 110.1 . . ? H11C C11' H11D 108.4 . . ? C13' C12' C11' 109.8(10) . . ? C13' C12' H12C 109.7 . . ? C11' C12' H12C 109.7 . . ? C13' C12' H12D 109.7 . . ? C11' C12' H12D 109.7 . . ? H12C C12' H12D 108.2 . . ? C12' C13' H13D 109.5 . . ? C12' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C12' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? N3 C14 N4 106.5(3) . . ? N3 C14 Ag1 125.7(3) . . ? N4 C14 Ag1 127.7(3) . . ? C16 C15 N3 106.4(4) . . ? C16 C15 C20 121.7(4) . . ? N3 C15 C20 131.8(4) . . ? C15 C16 N4 105.9(4) . . ? C15 C16 C17 121.3(4) . . ? N4 C16 C17 132.8(4) . . ? C18 C17 C16 115.9(5) . . ? C18 C17 H17 122.0 . . ? C16 C17 H17 122.0 . . ? C19 C18 C17 123.9(5) . . ? C19 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C18 C19 C20 121.6(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C15 115.5(5) . . ? C19 C20 H20 122.3 . . ? C15 C20 H20 122.3 . . ? N4 C21 C22 112.9(3) . . ? N4 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N4 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C21 109.6(5) 4_565 . ? C21 C22 H22A 109.8 4_565 . ? C21 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 4_565 . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N3 C23 C24 111.8(4) . . ? N3 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N3 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 112.1(6) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 111.6(7) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F2 P1 F4 176.2(5) . . ? F2 P1 F3 92.4(4) . . ? F4 P1 F3 91.4(5) . . ? F2 P1 F5 89.76(17) . . ? F4 P1 F5 90.23(17) . . ? F3 P1 F5 90.15(17) . . ? F2 P1 F5 89.75(17) . 4_575 ? F4 P1 F5 90.24(17) . 4_575 ? F3 P1 F5 90.15(17) . 4_575 ? F5 P1 F5 179.4(4) . 4_575 ? F2 P1 F1 89.6(4) . . ? F4 P1 F1 86.6(5) . . ? F3 P1 F1 178.0(4) . . ? F5 P1 F1 89.86(17) . . ? F5 P1 F1 89.85(17) 4_575 . ? F6 P2 F6 90.3(6) 4_565 . ? F6 P2 F9 88.8(4) 4_565 . ? F6 P2 F9 88.8(4) . . ? F6 P2 F7 93.1(4) 4_565 4_565 ? F6 P2 F7 176.3(4) . 4_565 ? F9 P2 F7 89.8(3) . 4_565 ? F6 P2 F7 176.3(4) 4_565 . ? F6 P2 F7 93.1(4) . . ? F9 P2 F7 89.8(3) . . ? F7 P2 F7 83.4(5) 4_565 . ? F6 P2 F8 93.4(4) 4_565 . ? F6 P2 F8 93.4(4) . . ? F9 P2 F8 177.0(4) . . ? F7 P2 F8 87.9(3) 4_565 . ? F7 P2 F8 87.9(3) . . ? O1 S1 C27 109.1(7) . 4_565 ? O1 S1 C27 109.1(7) . . ? C27 S1 C27 98.0(7) 4_565 . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Ag1 C1 N1 57.1(17) . . . . ? C14 Ag1 C1 N2 -115.2(15) . . . . ? N2 C1 N1 C2 0.3(5) . . . . ? Ag1 C1 N1 C2 -173.2(3) . . . . ? N2 C1 N1 C10 179.8(4) . . . . ? Ag1 C1 N1 C10 6.2(7) . . . . ? N1 C1 N2 C3 -0.8(5) . . . . ? Ag1 C1 N2 C3 172.8(3) . . . . ? N1 C1 N2 C8 -178.9(4) . . . . ? Ag1 C1 N2 C8 -5.3(6) . . . . ? C1 N1 C2 C3 0.3(5) . . . . ? C10 N1 C2 C3 -179.2(4) . . . . ? C1 N1 C2 C7 177.0(5) . . . . ? C10 N1 C2 C7 -2.5(8) . . . . ? N1 C2 C3 C4 177.7(4) . . . . ? C7 C2 C3 C4 0.5(7) . . . . ? N1 C2 C3 N2 -0.8(5) . . . . ? C7 C2 C3 N2 -178.0(4) . . . . ? C1 N2 C3 C4 -177.3(5) . . . . ? C8 N2 C3 C4 0.9(7) . . . . ? C1 N2 C3 C2 1.0(5) . . . . ? C8 N2 C3 C2 179.2(4) . . . . ? C2 C3 C4 C5 -0.7(8) . . . . ? N2 C3 C4 C5 177.3(5) . . . . ? C3 C4 C5 C6 0.8(9) . . . . ? C4 C5 C6 C7 -0.8(10) . . . . ? C5 C6 C7 C2 0.5(9) . . . . ? C3 C2 C7 C6 -0.4(8) . . . . ? N1 C2 C7 C6 -176.7(5) . . . . ? C1 N2 C8 C9 -106.2(5) . . . . ? C3 N2 C8 C9 75.9(5) . . . . ? N2 C8 C9 C8 -177.2(3) . . . 4_565 ? C1 N1 C10 C11 108.5(7) . . . . ? C2 N1 C10 C11 -72.1(7) . . . . ? C1 N1 C10 C11' 81.3(15) . . . . ? C2 N1 C10 C11' -99.3(15) . . . . ? N1 C10 C11 C12 -69.7(13) . . . . ? C11' C10 C11 C12 33(3) . . . . ? C10 C11 C12 C13 -163.7(13) . . . . ? N1 C10 C11' C12' 43(3) . . . . ? C11 C10 C11' C12' -45(2) . . . . ? C10 C11' C12' C13' -164(3) . . . . ? C15 N3 C14 N4 -1.0(5) . . . . ? C23 N3 C14 N4 177.4(4) . . . . ? C15 N3 C14 Ag1 175.8(3) . . . . ? C23 N3 C14 Ag1 -5.8(6) . . . . ? C16 N4 C14 N3 1.7(5) . . . . ? C21 N4 C14 N3 178.5(4) . . . . ? C16 N4 C14 Ag1 -175.1(3) . . . . ? C21 N4 C14 Ag1 1.7(6) . . . . ? C1 Ag1 C14 N3 -56.3(17) . . . . ? C1 Ag1 C14 N4 119.8(15) . . . . ? C14 N3 C15 C16 0.0(5) . . . . ? C23 N3 C15 C16 -178.4(4) . . . . ? C14 N3 C15 C20 -178.1(5) . . . . ? C23 N3 C15 C20 3.5(8) . . . . ? N3 C15 C16 N4 0.9(5) . . . . ? C20 C15 C16 N4 179.3(4) . . . . ? N3 C15 C16 C17 -177.7(4) . . . . ? C20 C15 C16 C17 0.6(7) . . . . ? C14 N4 C16 C15 -1.6(5) . . . . ? C21 N4 C16 C15 -178.5(4) . . . . ? C14 N4 C16 C17 176.8(5) . . . . ? C21 N4 C16 C17 -0.1(7) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? N4 C16 C17 C18 -178.3(5) . . . . ? C16 C17 C18 C19 -1.9(9) . . . . ? C17 C18 C19 C20 3.4(11) . . . . ? C18 C19 C20 C15 -2.6(9) . . . . ? C16 C15 C20 C19 0.7(7) . . . . ? N3 C15 C20 C19 178.6(5) . . . . ? C14 N4 C21 C22 108.4(5) . . . . ? C16 N4 C21 C22 -75.2(5) . . . . ? N4 C21 C22 C21 177.0(3) . . . 4_565 ? C14 N3 C23 C24 -94.5(6) . . . . ? C15 N3 C23 C24 83.7(6) . . . . ? N3 C23 C24 C25 -179.8(6) . . . . ? C23 C24 C25 C26 178.9(8) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.573 0.250 0.582 235.5 42.5 2 0.262 0.250 0.028 20.9 0.4 3 0.427 0.750 0.418 235.6 42.1 4 0.737 0.750 0.972 20.9 0.4 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.204 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.086 # Attachment 'CIF_2h.cif' data_090313c _database_code_depnum_ccdc_archive 'CCDC 726813' #TrackingRef 'CIF_2h.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.50 H30 Ag F6 N4 O0.50 P' _chemical_formula_weight 725.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.2792(17) _cell_length_b 26.712(3) _cell_length_c 17.4205(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7575.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4532 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 20.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920.0 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19180 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3588 _reflns_number_gt 2308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3586 _refine_ls_number_parameters 216 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.3366 _refine_ls_wR_factor_gt 0.2807 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.270 _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 0.80477(6) 0.18427(3) 0.2500 0.0792(5) Uani 1 2 d S . . N1 N 0.7388(4) 0.1624(2) 0.0885(3) 0.0692(15) Uani 1 1 d . A . N2 N 0.8495(4) 0.2069(2) 0.0808(4) 0.0727(16) Uani 1 1 d . . . C1 C 0.7982(4) 0.1840(2) 0.1301(5) 0.0669(19) Uani 1 1 d . . . C2 C 0.7514(5) 0.1713(3) 0.0101(4) 0.0725(19) Uani 1 1 d . . . C3 C 0.8217(5) 0.1998(3) 0.0053(5) 0.079(2) Uani 1 1 d . . . C4 C 0.8524(6) 0.2161(4) -0.0649(5) 0.091(2) Uani 1 1 d . . . H4A H 0.8999 0.2353 -0.0687 0.109 Uiso 1 1 calc R . . C5 C 0.8072(7) 0.2018(5) -0.1294(7) 0.111(4) Uani 1 1 d . . . H5A H 0.8252 0.2116 -0.1778 0.133 Uiso 1 1 calc R . . C6 C 0.7357(8) 0.1732(4) -0.1234(6) 0.103(3) Uani 1 1 d . . . H6A H 0.7070 0.1652 -0.1679 0.124 Uiso 1 1 calc R . . C7 C 0.7063(5) 0.1565(4) -0.0537(6) 0.092(3) Uani 1 1 d . . . H7A H 0.6594 0.1368 -0.0498 0.110 Uiso 1 1 calc R . . C9 C 0.6748(9) 0.0805(3) 0.1230(10) 0.109(3) Uani 0.561(15) 1 d PGDU A 1 C10 C 0.7387(12) 0.0554(5) 0.0868(11) 0.146(7) Uani 0.561(15) 1 d PGDU A 1 H10A H 0.7741 0.0731 0.0519 0.175 Uiso 0.561(15) 1 d PR A 1 C11 C 0.7515(16) 0.0048(5) 0.1009(16) 0.302(18) Uani 0.561(15) 1 d PGU A 1 H11A H 0.7957 -0.0125 0.0759 0.362 Uiso 0.561(15) 1 d PR A 1 C12 C 0.7003(18) -0.0207(4) 0.1514(17) 0.212(12) Uani 0.561(15) 1 d PGU A 1 H12A H 0.7092 -0.0557 0.1611 0.255 Uiso 0.561(15) 1 d PR A 1 C13 C 0.6364(16) 0.0043(5) 0.1876(15) 0.204(10) Uani 0.561(15) 1 d PGU A 1 H13A H 0.5996 -0.0133 0.2269 0.245 Uiso 0.561(15) 1 d PR A 1 C14 C 0.6236(12) 0.0550(5) 0.1735(13) 0.187(10) Uani 0.561(15) 1 d PGDU A 1 H14A H 0.5794 0.0723 0.1985 0.225 Uiso 0.561(15) 1 d PR A 1 C8 C 0.6702(5) 0.1360(3) 0.1190(6) 0.095(3) Uani 1 1 d DU . . H8A H 0.6241 0.1448 0.0874 0.114 Uiso 0.561(15) 1 d PR A 1 H8B H 0.6592 0.1487 0.1695 0.114 Uiso 0.561(15) 1 d PR A 1 H8C H 0.6234 0.1415 0.0865 0.114 Uiso 0.439(15) 1 d PR A 2 H8D H 0.6572 0.1472 0.1699 0.114 Uiso 0.439(15) 1 d PR A 2 C9' C 0.6887(9) 0.0813(3) 0.1199(17) 0.109(3) Uani 0.439(15) 1 d PGDU A 2 C10' C 0.7695(10) 0.0646(6) 0.1221(18) 0.146(7) Uani 0.439(15) 1 d PGDU A 2 H10B H 0.8137 0.0883 0.1251 0.175 Uiso 0.439(15) 1 d PR A 2 C11' C 0.7863(17) 0.0136(7) 0.120(2) 0.302(18) Uani 0.439(15) 1 d PGU A 2 H11B H 0.8422 0.0021 0.1216 0.362 Uiso 0.439(15) 1 d PR A 2 C12' C 0.722(2) -0.0207(4) 0.116(2) 0.212(12) Uani 0.439(15) 1 d PGU A 2 H12B H 0.7339 -0.0559 0.1144 0.255 Uiso 0.439(15) 1 d PR A 2 C13' C 0.6415(19) -0.0040(4) 0.114(2) 0.204(10) Uani 0.439(15) 1 d PGU A 2 H13B H 0.5973 -0.0277 0.1106 0.245 Uiso 0.439(15) 1 d PR A 2 C14' C 0.6246(12) 0.0470(5) 0.1156(19) 0.187(10) Uani 0.439(15) 1 d PGDU A 2 H14B H 0.5688 0.0585 0.1141 0.225 Uiso 0.439(15) 1 d PR A 2 C15 C 0.9228(4) 0.2345(3) 0.1006(5) 0.079(2) Uani 1 1 d . . . H15A H 0.9214 0.2430 0.1548 0.095 Uiso 1 1 calc R . . H15B H 0.9243 0.2655 0.0716 0.095 Uiso 1 1 calc R . . C16 C 1.0000 0.2041(4) 0.0836(7) 0.077(3) Uani 1 2 d S . . H16A H 1.0000 0.1740 0.1147 0.092 Uiso 1 2 calc SR . . H16B H 1.0000 0.1942 0.0300 0.092 Uiso 1 2 calc SR . . C17 C 0.5000 0.3589(12) 0.7500 0.167(11) Uani 1 4 d S . . O1 O 0.5000 0.4097(6) 0.7500 0.203(11) Uani 1 4 d S . . P1 P 0.0000 0.28447(18) 0.7500 0.0869(13) Uani 1 4 d S . . P2 P 0.5000 0.14147(19) 0.7500 0.116(2) Uani 1 4 d S . . F1 F 0.0000 0.3440(4) 0.7500 0.119(4) Uani 1 4 d S . . F2 F 0.0974(5) 0.2845(3) 0.7500 0.112(2) Uani 1 2 d S . . F3 F 0.0000 0.2841(4) 0.6597(5) 0.137(3) Uani 1 2 d S . . F4 F 0.0000 0.2249(5) 0.7500 0.167(6) Uani 1 4 d S . . F5 F 0.4348(12) 0.1826(7) 0.7500 0.250(10) Uani 1 2 d S . . F6 F 0.5000 0.1472(7) 0.6603(10) 0.241(7) Uani 1 2 d S . . F7 F 0.4261(13) 0.1110(10) 0.7500 0.353(15) Uani 1 2 d S . . 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 0.0802(8) 0.0812(7) 0.0762(7) 0.000 0.000 0.0012(4) N1 0.066(4) 0.061(3) 0.081(4) -0.003(3) 0.009(3) -0.004(3) N2 0.067(4) 0.067(3) 0.084(4) 0.007(3) 0.006(3) -0.008(3) C1 0.061(4) 0.059(4) 0.081(5) -0.001(3) 0.001(3) 0.011(3) C2 0.068(5) 0.078(4) 0.071(4) 0.001(3) 0.006(4) 0.008(4) C3 0.073(5) 0.078(5) 0.086(6) 0.012(4) -0.002(4) 0.008(4) C4 0.085(6) 0.105(6) 0.083(6) 0.029(5) 0.005(4) 0.009(5) C5 0.126(10) 0.119(8) 0.087(7) 0.034(6) 0.019(6) 0.015(6) C6 0.106(8) 0.126(8) 0.077(6) -0.002(5) -0.014(6) 0.023(7) C7 0.086(6) 0.080(6) 0.109(7) -0.008(5) -0.005(5) 0.007(4) C9 0.126(6) 0.101(5) 0.100(5) -0.004(4) 0.022(5) -0.034(5) C10 0.163(9) 0.121(8) 0.155(9) 0.008(6) -0.010(7) 0.001(6) C11 0.303(19) 0.298(19) 0.305(19) -0.002(7) -0.002(7) 0.002(7) C12 0.218(13) 0.206(13) 0.213(14) -0.003(7) 0.013(7) -0.003(7) C13 0.211(12) 0.194(12) 0.208(12) 0.005(7) 0.001(7) -0.008(7) C14 0.189(11) 0.185(11) 0.189(12) 0.002(7) 0.005(7) -0.009(7) C8 0.088(5) 0.101(6) 0.096(5) -0.006(4) 0.021(4) -0.019(4) C9' 0.126(6) 0.101(5) 0.100(5) -0.004(4) 0.022(5) -0.034(5) C10' 0.163(9) 0.121(8) 0.155(9) 0.008(6) -0.010(7) 0.001(6) C11' 0.303(19) 0.298(19) 0.305(19) -0.002(7) -0.002(7) 0.002(7) C12' 0.218(13) 0.206(13) 0.213(14) -0.003(7) 0.013(7) -0.003(7) C13' 0.211(12) 0.194(12) 0.208(12) 0.005(7) 0.001(7) -0.008(7) C14' 0.189(11) 0.185(11) 0.189(12) 0.002(7) 0.005(7) -0.009(7) C15 0.064(5) 0.075(5) 0.099(5) 0.000(4) -0.001(4) -0.008(3) C16 0.063(6) 0.068(6) 0.099(8) 0.009(6) 0.000 0.000 C17 0.22(3) 0.15(3) 0.13(2) 0.000 0.000 0.000 O1 0.23(2) 0.052(9) 0.33(3) 0.000 0.000 0.000 P1 0.084(3) 0.078(3) 0.099(3) 0.000 0.000 0.000 P2 0.079(3) 0.072(3) 0.198(7) 0.000 0.000 0.000 F1 0.125(9) 0.075(7) 0.158(10) 0.000 0.000 0.000 F2 0.081(5) 0.124(6) 0.131(6) 0.000 0.000 0.003(4) F3 0.124(7) 0.184(9) 0.103(6) -0.042(6) 0.000 0.000 F4 0.155(13) 0.081(8) 0.27(2) 0.000 0.000 0.000 F5 0.230(16) 0.27(2) 0.245(18) 0.000 0.000 0.153(15) F6 0.33(2) 0.198(15) 0.192(14) -0.061(12) 0.000 0.000 F7 0.25(2) 0.29(3) 0.51(4) 0.000 0.000 -0.16(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 Ag1 C1 2.091(9) . ? Ag1 C1 2.091(9) 10_556 ? N1 C1 1.340(10) . ? N1 C2 1.401(10) . ? N1 C8 1.423(10) . ? N2 C1 1.345(10) . ? N2 C3 1.404(11) . ? N2 C15 1.445(9) . ? C2 C3 1.379(12) . ? C2 C7 1.390(12) . ? C3 C4 1.391(12) . ? C4 C5 1.398(16) . ? C4 H4A 0.9300 . ? C5 C6 1.395(16) . ? C5 H5A 0.9300 . ? C6 C7 1.379(14) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C9 C8 1.486(7) . ? C10 C11 1.3900 . ? C10 H10A 0.9600 . ? C11 C12 1.3900 . ? C11 H11A 0.9599 . ? C11 H11B 1.5208 . ? C12 C13 1.3900 . ? C12 H12A 0.9600 . ? C12 H12B 1.2637 . ? C13 C14 1.3900 . ? C13 H13A 1.0245 . ? C14 H14A 0.9600 . ? C14 H14B 1.3696 . ? C8 C9' 1.491(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9599 . ? C8 H8C 0.9599 . ? C8 H8D 0.9600 . ? C9' C10' 1.3900 . ? C9' C14' 1.3900 . ? C10' C11' 1.3900 . ? C10' H10A 1.2460 . ? C10' H10B 0.9599 . ? C11' C12' 1.3900 . ? C11' H11A 1.0507 . ? C11' H11B 0.9599 . ? C12' C13' 1.3900 . ? C12' H11A 1.3994 . ? C12' H12A 1.2428 . ? C12' H12B 0.9600 . ? C13' C14' 1.3900 . ? C13' H13B 0.9601 . ? C14' H14B 0.9600 . ? C15 C16 1.525(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C15 1.525(10) 12_755 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O1 1.36(3) . ? P1 F3 1.573(9) . ? P1 F3 1.573(9) 10_557 ? P1 F2 1.586(7) 3_556 ? P1 F2 1.586(7) . ? P1 F1 1.589(13) . ? P1 F4 1.591(14) . ? P2 F7 1.452(15) . ? P2 F7 1.452(15) 3_656 ? P2 F5 1.528(13) . ? P2 F5 1.528(13) 3_656 ? P2 F6 1.571(17) . ? P2 F6 1.571(17) 10_557 ? 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 C1 Ag1 C1 174.1(4) . 10_556 ? C1 N1 C2 110.5(6) . . ? C1 N1 C8 125.3(7) . . ? C2 N1 C8 124.2(7) . . ? C1 N2 C3 109.8(7) . . ? C1 N2 C15 126.3(7) . . ? C3 N2 C15 123.9(7) . . ? N1 C1 N2 107.3(7) . . ? N1 C1 Ag1 125.4(5) . . ? N2 C1 Ag1 127.2(6) . . ? C3 C2 C7 123.1(8) . . ? C3 C2 N1 105.9(7) . . ? C7 C2 N1 130.9(8) . . ? C2 C3 C4 121.7(8) . . ? C2 C3 N2 106.5(7) . . ? C4 C3 N2 131.8(8) . . ? C3 C4 C5 115.6(9) . . ? C3 C4 H4A 122.2 . . ? C5 C4 H4A 122.2 . . ? C6 C5 C4 122.0(9) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C7 C6 C5 122.2(10) . . ? C7 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C6 C7 C2 115.4(9) . . ? C6 C7 H7A 122.3 . . ? C2 C7 H7A 122.3 . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 119.8(4) . . ? C14 C9 C8 119.3(4) . . ? C11 C10 C9 120.0 . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11B 103.5 . . ? C12 C11 H11B 114.1 . . ? H11A C11 H11B 50.1 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12B 77.5 . . ? C13 C12 H12B 156.1 . . ? H12A C12 H12B 45.8 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 121.3 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C9 120.0 . . ? C13 C14 H14A 120.0 . . ? C9 C14 H14A 120.0 . . ? C13 C14 H14B 107.4 . . ? C9 C14 H14B 83.0 . . ? H14A C14 H14B 79.8 . . ? N1 C8 C9 118.2(7) . . ? N1 C8 C9' 109.4(8) . . ? C9 C8 C9' 9.0(9) . . ? N1 C8 H8A 106.1 . . ? C9 C8 H8A 108.1 . . ? C9' C8 H8A 113.8 . . ? N1 C8 H8B 108.3 . . ? C9 C8 H8B 108.5 . . ? C9' C8 H8B 111.9 . . ? H8A C8 H8B 107.1 . . ? N1 C8 H8C 109.1 . . ? C9 C8 H8C 102.7 . . ? C9' C8 H8C 108.4 . . ? H8A C8 H8C 5.5 . . ? H8B C8 H8C 109.8 . . ? N1 C8 H8D 111.3 . . ? C9 C8 H8D 106.2 . . ? C9' C8 H8D 109.9 . . ? H8A C8 H8D 106.3 . . ? H8B C8 H8D 3.0 . . ? H8C C8 H8D 108.8 . . ? C10' C9' C14' 120.0 . . ? C10' C9' C8 120.3(4) . . ? C14' C9' C8 119.6(4) . . ? C11' C10' C9' 120.0 . . ? C11' C10' H10A 98.1 . . ? C9' C10' H10A 88.4 . . ? C11' C10' H10B 120.0 . . ? C9' C10' H10B 120.0 . . ? H10A C10' H10B 83.6 . . ? C10' C11' C12' 120.0 . . ? C10' C11' H11A 134.3 . . ? C12' C11' H11A 68.3 . . ? C10' C11' H11B 120.0 . . ? C12' C11' H11B 120.0 . . ? H11A C11' H11B 70.8 . . ? C13' C12' C11' 120.0 . . ? C13' C12' H11A 138.1 . . ? C11' C12' H11A 44.3 . . ? C13' C12' H12A 95.5 . . ? C11' C12' H12A 126.2 . . ? H11A C12' H12A 125.5 . . ? C13' C12' H12B 120.0 . . ? C11' C12' H12B 120.0 . . ? H11A C12' H12B 88.4 . . ? H12A C12' H12B 46.6 . . ? C12' C13' C14' 120.0 . . ? C12' C13' H13B 120.0 . . ? C14' C13' H13B 120.0 . . ? C13' C14' C9' 120.0 . . ? C13' C14' H14B 120.0 . . ? C9' C14' H14B 120.0 . . ? N2 C15 C16 111.2(7) . . ? N2 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N2 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C15 110.9(9) 12_755 . ? C15 C16 H16A 109.5 12_755 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 12_755 . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.0 . . ? F3 P1 F3 179.4(9) . 10_557 ? F3 P1 F2 90.002(4) . 3_556 ? F3 P1 F2 89.999(4) 10_557 3_556 ? F3 P1 F2 90.000(4) . . ? F3 P1 F2 90.000(4) 10_557 . ? F2 P1 F2 179.9(7) 3_556 . ? F3 P1 F1 90.3(5) . . ? F3 P1 F1 90.3(5) 10_557 . ? F2 P1 F1 89.9(4) 3_556 . ? F2 P1 F1 89.9(4) . . ? F3 P1 F4 89.7(5) . . ? F3 P1 F4 89.7(5) 10_557 . ? F2 P1 F4 90.1(4) 3_556 . ? F2 P1 F4 90.1(4) . . ? F1 P1 F4 180.000(3) . . ? F7 P2 F7 112(3) . 3_656 ? F7 P2 F5 80.0(14) . . ? F7 P2 F5 168.1(18) 3_656 . ? F7 P2 F5 168.1(17) . 3_656 ? F7 P2 F5 80.0(14) 3_656 3_656 ? F5 P2 F5 88.0(18) . 3_656 ? F7 P2 F6 93.1(4) . . ? F7 P2 F6 93.1(4) 3_656 . ? F5 P2 F6 86.0(5) . . ? F5 P2 F6 86.0(5) 3_656 . ? F7 P2 F6 93.1(4) . 10_557 ? F7 P2 F6 93.1(4) 3_656 10_557 ? F5 P2 F6 86.0(5) . 10_557 ? F5 P2 F6 86.0(5) 3_656 10_557 ? F6 P2 F6 168.8(13) . 10_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 0.1(7) . . . . ? C8 N1 C1 N2 -177.4(7) . . . . ? C2 N1 C1 Ag1 177.3(5) . . . . ? C8 N1 C1 Ag1 -0.2(10) . . . . ? C3 N2 C1 N1 0.2(8) . . . . ? C15 N2 C1 N1 -179.4(6) . . . . ? C3 N2 C1 Ag1 -176.9(5) . . . . ? C15 N2 C1 Ag1 3.4(10) . . . . ? C1 Ag1 C1 N1 -27(4) 10_556 . . . ? C1 Ag1 C1 N2 149(3) 10_556 . . . ? C1 N1 C2 C3 -0.4(8) . . . . ? C8 N1 C2 C3 177.1(7) . . . . ? C1 N1 C2 C7 -179.9(8) . . . . ? C8 N1 C2 C7 -2.4(12) . . . . ? C7 C2 C3 C4 0.2(13) . . . . ? N1 C2 C3 C4 -179.4(7) . . . . ? C7 C2 C3 N2 -179.9(7) . . . . ? N1 C2 C3 N2 0.5(8) . . . . ? C1 N2 C3 C2 -0.5(9) . . . . ? C15 N2 C3 C2 179.2(7) . . . . ? C1 N2 C3 C4 179.4(9) . . . . ? C15 N2 C3 C4 -0.9(14) . . . . ? C2 C3 C4 C5 0.2(13) . . . . ? N2 C3 C4 C5 -179.6(10) . . . . ? C3 C4 C5 C6 0.4(16) . . . . ? C4 C5 C6 C7 -1.4(18) . . . . ? C5 C6 C7 C2 1.7(14) . . . . ? C3 C2 C7 C6 -1.1(13) . . . . ? N1 C2 C7 C6 178.3(8) . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 169.1(18) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 -169.1(18) . . . . ? C1 N1 C8 C9 -97.5(12) . . . . ? C2 N1 C8 C9 85.4(13) . . . . ? C1 N1 C8 C9' -95.8(14) . . . . ? C2 N1 C8 C9' 87.0(14) . . . . ? C10 C9 C8 N1 -10(2) . . . . ? C14 C9 C8 N1 159.1(11) . . . . ? C10 C9 C8 C9' -20(10) . . . . ? C14 C9 C8 C9' 149(11) . . . . ? N1 C8 C9' C10' 25(2) . . . . ? C9 C8 C9' C10' -165(12) . . . . ? N1 C8 C9' C14' -153.0(15) . . . . ? C9 C8 C9' C14' 18(9) . . . . ? C14' C9' C10' C11' 0.0 . . . . ? C8 C9' C10' C11' -178(3) . . . . ? C9' C10' C11' C12' 0.0 . . . . ? C10' C11' C12' C13' 0.0 . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C12' C13' C14' C9' 0.0 . . . . ? C10' C9' C14' C13' 0.0 . . . . ? C8 C9' C14' C13' 178(3) . . . . ? C1 N2 C15 C16 103.8(9) . . . . ? C3 N2 C15 C16 -75.8(10) . . . . ? N2 C15 C16 C15 177.0(6) . . . 12_755 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.355 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.195