# 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 _publ_contact_author_name 'Ho, Mei-Lin' _publ_contact_author_email 'meilin ho@scu.edu.tw' _publ_section_title ; Synthesis, Structures and Photoluminescence Properties of Silver(I) Complexes with N,N'-di(pyrazin-2-yl)pyridine-2,6-diamine ; loop_ _publ_author_name M.-L.Ho C.-H.Shih G.-H.Lee C.-H.Lee # Attachment '- 1.cif' data_agclo4n5-2pz _database_code_depnum_ccdc_archive 'CCDC 780734' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Ag2 Cl2 N14 O8' _chemical_formula_weight 945.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.785(2) _cell_length_b 8.0179(16) _cell_length_c 19.629(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.61(3) _cell_angle_gamma 90.00 _cell_volume 1536.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3887 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7301 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9758 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3524 _reflns_number_gt 2435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3524 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.77683(3) 1.18065(3) 0.345124(13) 0.03164(10) Uani 1 1 d . . . N1 N 0.3090(3) 0.9633(3) 0.30830(13) 0.0308(7) Uani 1 1 d . . . N2 N 0.3235(3) 0.8430(3) 0.41387(13) 0.0276(6) Uani 1 1 d . . . H2 H 0.2339 0.8371 0.4068 0.033 Uiso 1 1 calc R . . N3 N 0.5097(3) 0.7836(3) 0.49009(13) 0.0237(6) Uani 1 1 d . . . N4 N 0.7024(3) 0.7344(3) 0.55649(13) 0.0237(6) Uani 1 1 d . . . H4 H 0.7346 0.8067 0.5278 0.028 Uiso 1 1 calc R . . N5 N 0.7658(3) 0.5561(4) 0.64807(13) 0.0337(7) Uani 1 1 d . . . N6 N 0.5796(3) 1.0695(3) 0.32198(13) 0.0264(6) Uani 1 1 d . . . N7 N 1.0262(3) 0.7028(3) 0.65324(13) 0.0256(6) Uani 1 1 d . . . C1 C 0.3669(4) 1.0514(5) 0.26000(17) 0.0350(9) Uani 1 1 d . . . H1 H 0.3133 1.0775 0.2194 0.042 Uiso 1 1 calc R . . C2 C 0.4994(3) 1.1059(5) 0.26617(17) 0.0325(8) Uani 1 1 d . . . H2A H 0.5349 1.1700 0.2306 0.039 Uiso 1 1 calc R . . C3 C 0.5255(3) 0.9816(4) 0.37107(16) 0.0256(7) Uani 1 1 d . . . H3 H 0.5805 0.9540 0.4111 0.031 Uiso 1 1 calc R . . C4 C 0.3893(3) 0.9290(4) 0.36482(15) 0.0258(7) Uani 1 1 d . . . C5 C 0.3770(3) 0.7637(4) 0.47314(16) 0.0246(7) Uani 1 1 d . . . C6 C 0.2903(3) 0.6659(4) 0.51039(16) 0.0279(7) Uani 1 1 d . . . H6 H 0.1948 0.6591 0.4984 0.033 Uiso 1 1 calc R . . C7 C 0.3492(3) 0.5799(4) 0.56532(16) 0.0268(7) Uani 1 1 d . . . H7 H 0.2939 0.5091 0.5909 0.032 Uiso 1 1 calc R . . C8 C 0.4866(3) 0.5944(4) 0.58388(15) 0.0254(7) Uani 1 1 d . . . H8 H 0.5273 0.5351 0.6219 0.031 Uiso 1 1 calc R . . C9 C 0.5638(3) 0.6992(4) 0.54487(15) 0.0227(7) Uani 1 1 d . . . C10 C 0.7976(3) 0.6757(4) 0.60501(15) 0.0244(7) Uani 1 1 d . . . C11 C 0.9297(3) 0.7472(4) 0.60667(16) 0.0250(7) Uani 1 1 d . . . H11 H 0.9495 0.8289 0.5736 0.030 Uiso 1 1 calc R . . C12 C 0.9942(3) 0.5841(5) 0.69862(16) 0.0338(8) Uani 1 1 d . . . H12 H 1.0598 0.5514 0.7338 0.041 Uiso 1 1 calc R . . C13 C 0.8687(4) 0.5118(5) 0.69402(18) 0.0412(10) Uani 1 1 d . . . H13 H 0.8517 0.4243 0.7250 0.049 Uiso 1 1 calc R . . Cl1 Cl -0.09379(8) 0.80350(10) 0.40560(4) 0.02633(19) Uani 1 1 d . . . O1 O 0.0260(2) 0.8647(3) 0.37519(12) 0.0375(6) Uani 1 1 d . . . O2 O -0.0589(2) 0.6619(3) 0.44802(12) 0.0382(6) Uani 1 1 d . . . O3 O -0.1486(2) 0.9352(3) 0.44697(11) 0.0330(6) Uani 1 1 d . . . O4 O -0.1954(2) 0.7580(3) 0.35332(12) 0.0402(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02241(15) 0.03754(17) 0.03428(16) 0.00289(13) -0.00377(10) -0.00517(12) N1 0.0213(15) 0.0414(17) 0.0287(15) 0.0040(14) -0.0068(12) 0.0021(14) N2 0.0148(14) 0.0347(16) 0.0332(15) 0.0025(13) -0.0008(11) -0.0010(13) N3 0.0173(14) 0.0273(15) 0.0262(14) 0.0002(12) -0.0013(11) -0.0014(12) N4 0.0212(15) 0.0267(14) 0.0226(14) 0.0052(12) -0.0031(11) -0.0066(12) N5 0.0251(16) 0.0442(18) 0.0316(15) 0.0122(14) -0.0010(12) -0.0045(14) N6 0.0251(15) 0.0284(15) 0.0252(14) -0.0015(13) -0.0017(11) -0.0015(13) N7 0.0235(15) 0.0293(16) 0.0237(14) -0.0020(12) -0.0016(11) -0.0008(12) C1 0.032(2) 0.044(2) 0.0279(18) 0.0029(17) -0.0095(15) 0.0022(18) C2 0.030(2) 0.039(2) 0.0283(18) 0.0055(16) -0.0048(15) -0.0036(17) C3 0.0222(17) 0.0288(18) 0.0252(17) -0.0018(15) -0.0039(13) 0.0011(15) C4 0.0241(18) 0.0243(17) 0.0286(17) -0.0034(15) -0.0019(14) 0.0032(15) C5 0.0225(18) 0.0256(17) 0.0255(17) -0.0026(14) -0.0014(14) 0.0030(15) C6 0.0194(17) 0.0307(18) 0.0341(18) -0.0041(16) 0.0066(14) -0.0043(16) C7 0.0277(19) 0.0258(17) 0.0274(17) -0.0019(15) 0.0054(14) -0.0030(15) C8 0.0236(18) 0.0280(17) 0.0246(17) -0.0001(15) 0.0006(13) -0.0009(15) C9 0.0185(16) 0.0245(17) 0.0245(16) -0.0032(14) -0.0023(13) -0.0022(14) C10 0.0245(17) 0.0279(17) 0.0206(15) -0.0021(15) 0.0004(13) -0.0001(15) C11 0.0230(18) 0.0249(16) 0.0265(18) 0.0004(15) -0.0035(14) -0.0024(15) C12 0.0249(19) 0.049(2) 0.0272(18) 0.0092(17) -0.0018(14) 0.0000(17) C13 0.029(2) 0.055(2) 0.040(2) 0.0257(19) -0.0023(16) -0.0049(19) Cl1 0.0191(4) 0.0297(4) 0.0297(4) 0.0022(4) -0.0025(3) -0.0028(3) O1 0.0233(13) 0.0448(15) 0.0449(14) 0.0060(12) 0.0069(11) -0.0062(11) O2 0.0354(15) 0.0350(14) 0.0437(14) 0.0103(12) -0.0025(11) 0.0024(12) O3 0.0337(14) 0.0310(13) 0.0345(13) -0.0013(11) 0.0038(10) 0.0010(11) O4 0.0311(15) 0.0463(14) 0.0412(15) -0.0047(12) -0.0146(11) -0.0039(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 Ag N7 2.140(3) 3_776 ? Ag N6 2.148(3) . ? N1 C1 1.337(4) . ? N1 C4 1.347(4) . ? N2 C4 1.377(4) . ? N2 C5 1.399(4) . ? N3 C5 1.330(4) . ? N3 C9 1.350(4) . ? N4 C10 1.373(4) . ? N4 C9 1.390(4) . ? N5 C10 1.327(4) . ? N5 C13 1.356(4) . ? N6 C3 1.331(4) . ? N6 C2 1.339(4) . ? N7 C11 1.321(4) . ? N7 C12 1.354(4) . ? N7 Ag 2.140(3) 3_776 ? C1 C2 1.367(5) . ? C3 C4 1.395(4) . ? C5 C6 1.395(4) . ? C6 C7 1.375(4) . ? C7 C8 1.376(4) . ? C8 C9 1.391(4) . ? C10 C11 1.412(4) . ? C12 C13 1.356(5) . ? Cl1 O4 1.431(2) . ? Cl1 O1 1.435(2) . ? Cl1 O2 1.436(2) . ? Cl1 O3 1.455(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ag N6 168.64(9) 3_776 . ? C1 N1 C4 116.1(3) . . ? C4 N2 C5 130.0(3) . . ? C5 N3 C9 117.8(3) . . ? C10 N4 C9 131.1(3) . . ? C10 N5 C13 114.8(3) . . ? C3 N6 C2 117.9(3) . . ? C3 N6 Ag 117.4(2) . . ? C2 N6 Ag 123.7(2) . . ? C11 N7 C12 117.4(3) . . ? C11 N7 Ag 119.8(2) . 3_776 ? C12 N7 Ag 122.9(2) . 3_776 ? N1 C1 C2 123.3(3) . . ? N6 C2 C1 120.5(3) . . ? N6 C3 C4 121.2(3) . . ? N1 C4 N2 113.8(3) . . ? N1 C4 C3 121.0(3) . . ? N2 C4 C3 125.2(3) . . ? N3 C5 C6 123.6(3) . . ? N3 C5 N2 117.5(3) . . ? C6 C5 N2 118.9(3) . . ? C7 C6 C5 117.0(3) . . ? C6 C7 C8 121.3(3) . . ? C7 C8 C9 117.4(3) . . ? N3 C9 N4 111.0(3) . . ? N3 C9 C8 122.8(3) . . ? N4 C9 C8 126.1(3) . . ? N5 C10 N4 120.9(3) . . ? N5 C10 C11 121.9(3) . . ? N4 C10 C11 117.2(3) . . ? N7 C11 C10 121.3(3) . . ? N7 C12 C13 120.2(3) . . ? C12 C13 N5 124.3(3) . . ? O4 Cl1 O1 109.75(15) . . ? O4 Cl1 O2 110.09(15) . . ? O1 Cl1 O2 109.90(15) . . ? O4 Cl1 O3 108.75(15) . . ? O1 Cl1 O3 108.88(14) . . ? O2 Cl1 O3 109.44(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.669 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.100 # Attachment '- 2.cif' data_ic14183 _database_code_depnum_ccdc_archive 'CCDC 780735' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Ag2 Cl2 N16 O10' _chemical_formula_weight 1091.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6693(10) _cell_length_b 10.2699(11) _cell_length_c 11.6983(13) _cell_angle_alpha 79.178(2) _cell_angle_beta 72.441(2) _cell_angle_gamma 64.003(2) _cell_volume 993.39(18) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3439 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6722 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12940 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4552 _reflns_number_gt 4054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0689P)^2^+2.3161P] 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 4552 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.53657(5) 0.86023(4) 0.59760(4) 0.02277(15) Uani 1 1 d . . . Cl1 Cl 0.31447(17) 0.81347(15) 0.44497(13) 0.0286(3) Uani 1 1 d . . . O1 O 0.3640(5) 0.9311(4) 0.4407(4) 0.0299(9) Uani 1 1 d . . . O2 O 0.3361(5) 0.6948(4) 0.5389(4) 0.0319(10) Uani 1 1 d . . . O3 O 0.1397(5) 0.8810(5) 0.4370(4) 0.0317(10) Uani 1 1 d . . . O4 O 0.3901(5) 0.7473(5) 0.3201(4) 0.0337(10) Uiso 1 1 d . . . N1 N 1.0334(5) 0.5457(5) 0.3280(4) 0.0215(9) Uani 1 1 d . . . N2 N 0.9227(5) 0.3838(5) 0.3279(4) 0.0196(9) Uani 1 1 d . . . H2 H 0.8359 0.3676 0.3525 0.023 Uiso 1 1 calc R . . N3 N 1.0119(5) 0.1784(5) 0.2323(4) 0.0179(9) Uani 1 1 d . . . N4 N 1.0884(5) -0.0347(5) 0.1414(4) 0.0209(9) Uani 1 1 d . . . H4 H 1.1693 -0.1067 0.1020 0.025 Uiso 1 1 calc R . . N5 N 0.9508(6) -0.1543(5) 0.1170(4) 0.0253(10) Uani 1 1 d . . . N6 N 0.7526(5) 0.7114(5) 0.4852(4) 0.0209(9) Uani 1 1 d . . . N7 N 0.6720(5) 0.0213(5) 0.2673(4) 0.0220(9) Uani 1 1 d . . . C1 C 1.0139(7) 0.6672(6) 0.3712(5) 0.0234(11) Uani 1 1 d . . . H1 H 1.0991 0.6973 0.3466 0.028 Uiso 1 1 calc R . . C2 C 0.8760(7) 0.7496(6) 0.4494(5) 0.0236(11) Uani 1 1 d . . . H2A H 0.8682 0.8338 0.4781 0.028 Uiso 1 1 calc R . . C3 C 0.7683(6) 0.5912(5) 0.4453(4) 0.0171(10) Uani 1 1 d . . . H3 H 0.6828 0.5617 0.4703 0.021 Uiso 1 1 calc R . . C4 C 0.9113(6) 0.5074(5) 0.3662(5) 0.0173(10) Uani 1 1 d . . . C5 C 1.0520(6) 0.2801(5) 0.2556(4) 0.0178(10) Uani 1 1 d . . . C6 C 1.2025(6) 0.2784(6) 0.2130(5) 0.0224(11) Uani 1 1 d . . . H6 H 1.2262 0.3526 0.2293 0.027 Uiso 1 1 calc R . . C7 C 1.3190(6) 0.1621(6) 0.1446(5) 0.0250(12) Uani 1 1 d . . . H7 H 1.4242 0.1564 0.1137 0.030 Uiso 1 1 calc R . . C8 C 1.2816(6) 0.0576(6) 0.1225(5) 0.0228(11) Uani 1 1 d . . . H8 H 1.3603 -0.0221 0.0773 0.027 Uiso 1 1 calc R . . C9 C 1.1262(6) 0.0693(6) 0.1672(5) 0.0199(10) Uani 1 1 d . . . C10 C 0.9444(6) -0.0438(6) 0.1673(5) 0.0206(11) Uani 1 1 d . . . C11 C 0.8048(6) 0.0443(6) 0.2423(5) 0.0216(11) Uani 1 1 d . . . H11 H 0.8031 0.1220 0.2765 0.026 Uiso 1 1 calc R . . C12 C 0.6784(7) -0.0899(6) 0.2165(5) 0.0211(11) Uani 1 1 d . . . H12 H 0.5867 -0.1095 0.2330 0.025 Uiso 1 1 calc R . . C13 C 0.8177(7) -0.1746(6) 0.1411(5) 0.0225(11) Uani 1 1 d . . . H13 H 0.8190 -0.2506 0.1049 0.027 Uiso 1 1 calc R . . O5 O 1.3470(5) -0.2513(5) -0.0150(4) 0.0328(10) Uani 1 1 d . . . N8 N 1.3734(6) -0.4401(5) -0.1064(5) 0.0264(10) Uani 1 1 d . . . C14 C 1.3080(7) -0.3478(7) -0.0211(6) 0.0293(13) Uani 1 1 d . . . H14 H 1.2227 -0.3571 0.0414 0.035 Uiso 1 1 calc R . . C15 C 1.5034(8) -0.4340(7) -0.2068(6) 0.0362(15) Uani 1 1 d . . . H15A H 1.5248 -0.3509 -0.2009 0.054 Uiso 1 1 calc R . . H15B H 1.4743 -0.4231 -0.2824 0.054 Uiso 1 1 calc R . . H15C H 1.5987 -0.5238 -0.2046 0.054 Uiso 1 1 calc R . . C16 C 1.3190(8) -0.5512(7) -0.1044(6) 0.0339(14) Uani 1 1 d . . . H16A H 1.2367 -0.5486 -0.0303 0.051 Uiso 1 1 calc R . . H16B H 1.4084 -0.6466 -0.1078 0.051 Uiso 1 1 calc R . . H16C H 1.2749 -0.5336 -0.1739 0.051 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 Ag 0.0195(2) 0.0176(2) 0.0296(2) -0.01156(15) 0.00202(15) -0.00739(16) Cl1 0.0299(7) 0.0244(7) 0.0345(8) -0.0109(6) -0.0016(6) -0.0142(6) O1 0.034(2) 0.025(2) 0.040(2) -0.0066(18) -0.0090(19) -0.0195(18) O2 0.032(2) 0.023(2) 0.039(2) -0.0008(18) -0.0013(19) -0.0153(18) O3 0.0168(19) 0.028(2) 0.058(3) -0.001(2) -0.0180(19) -0.0110(17) N1 0.018(2) 0.017(2) 0.031(2) -0.0062(18) -0.0016(18) -0.0084(18) N2 0.015(2) 0.017(2) 0.028(2) -0.0117(18) 0.0014(17) -0.0086(17) N3 0.017(2) 0.017(2) 0.022(2) -0.0059(17) -0.0038(17) -0.0079(17) N4 0.021(2) 0.017(2) 0.027(2) -0.0134(18) 0.0026(18) -0.0097(18) N5 0.028(2) 0.020(2) 0.028(2) -0.0123(19) 0.001(2) -0.011(2) N6 0.023(2) 0.013(2) 0.028(2) -0.0039(17) -0.0076(19) -0.0071(17) N7 0.023(2) 0.017(2) 0.026(2) -0.0062(18) -0.0038(19) -0.0079(18) C1 0.025(3) 0.016(2) 0.034(3) -0.005(2) -0.009(2) -0.011(2) C2 0.025(3) 0.019(3) 0.031(3) -0.006(2) -0.007(2) -0.011(2) C3 0.019(2) 0.015(2) 0.019(2) -0.0061(19) -0.0016(19) -0.0078(19) C4 0.021(2) 0.014(2) 0.019(2) -0.0010(19) -0.007(2) -0.007(2) C5 0.023(3) 0.017(2) 0.016(2) -0.0047(19) -0.002(2) -0.010(2) C6 0.021(3) 0.023(3) 0.027(3) -0.010(2) -0.001(2) -0.012(2) C7 0.018(3) 0.030(3) 0.029(3) -0.010(2) -0.002(2) -0.011(2) C8 0.017(2) 0.022(3) 0.028(3) -0.012(2) -0.001(2) -0.004(2) C9 0.024(3) 0.018(2) 0.021(3) -0.006(2) -0.004(2) -0.012(2) C10 0.025(3) 0.022(3) 0.019(3) -0.004(2) -0.003(2) -0.014(2) C11 0.022(3) 0.017(2) 0.029(3) -0.009(2) -0.003(2) -0.009(2) C12 0.026(3) 0.018(2) 0.026(3) -0.004(2) -0.009(2) -0.014(2) C13 0.027(3) 0.017(2) 0.026(3) -0.010(2) -0.005(2) -0.009(2) O5 0.032(2) 0.027(2) 0.040(2) -0.0200(19) -0.0021(19) -0.0112(19) N8 0.027(2) 0.021(2) 0.033(3) -0.010(2) -0.002(2) -0.013(2) C14 0.021(3) 0.030(3) 0.032(3) -0.005(2) 0.000(2) -0.009(2) C15 0.044(4) 0.032(3) 0.035(3) -0.008(3) -0.002(3) -0.021(3) C16 0.040(4) 0.029(3) 0.043(4) -0.007(3) -0.008(3) -0.023(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 Ag N7 2.166(5) 2_666 ? Ag N6 2.175(5) . ? Ag Ag 3.2694(9) 2_676 ? Cl1 O2 1.465(4) . ? Cl1 O1 1.470(4) . ? Cl1 O3 1.545(4) . ? Cl1 O4 1.557(5) . ? N1 C4 1.332(7) . ? N1 C1 1.350(7) . ? N2 C4 1.373(6) . ? N2 C5 1.395(6) . ? N3 C9 1.336(7) . ? N3 C5 1.358(6) . ? N4 C10 1.374(7) . ? N4 C9 1.376(6) . ? N5 C13 1.331(7) . ? N5 C10 1.344(7) . ? N6 C3 1.331(6) . ? N6 C2 1.342(7) . ? N7 C11 1.343(7) . ? N7 C12 1.354(6) . ? N7 Ag 2.166(5) 2_666 ? C1 C2 1.377(8) . ? C3 C4 1.412(7) . ? C5 C6 1.382(7) . ? C6 C7 1.404(7) . ? C7 C8 1.360(7) . ? C8 C9 1.392(7) . ? C10 C11 1.387(7) . ? C12 C13 1.376(8) . ? O5 C14 1.225(7) . ? N8 C14 1.320(7) . ? N8 C16 1.445(7) . ? N8 C15 1.454(8) . ? 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 N7 Ag N6 170.32(17) 2_666 . ? N7 Ag Ag 91.81(12) 2_666 2_676 ? N6 Ag Ag 97.86(12) . 2_676 ? O2 Cl1 O1 122.5(3) . . ? O2 Cl1 O3 109.0(2) . . ? O1 Cl1 O3 108.8(2) . . ? O2 Cl1 O4 108.7(2) . . ? O1 Cl1 O4 107.8(3) . . ? O3 Cl1 O4 97.2(3) . . ? C4 N1 C1 116.2(5) . . ? C4 N2 C5 129.4(4) . . ? C9 N3 C5 117.6(4) . . ? C10 N4 C9 130.2(5) . . ? C13 N5 C10 117.3(5) . . ? C3 N6 C2 118.5(5) . . ? C3 N6 Ag 125.2(4) . . ? C2 N6 Ag 116.2(3) . . ? C11 N7 C12 117.9(5) . . ? C11 N7 Ag 120.9(3) . 2_666 ? C12 N7 Ag 120.6(4) . 2_666 ? N1 C1 C2 122.9(5) . . ? N6 C2 C1 120.2(5) . . ? N6 C3 C4 120.4(5) . . ? N1 C4 N2 119.8(5) . . ? N1 C4 C3 121.7(5) . . ? N2 C4 C3 118.5(4) . . ? N3 C5 C6 123.5(5) . . ? N3 C5 N2 111.1(4) . . ? C6 C5 N2 125.3(4) . . ? C5 C6 C7 117.0(5) . . ? C8 C7 C6 120.2(5) . . ? C7 C8 C9 119.0(5) . . ? N3 C9 N4 118.7(5) . . ? N3 C9 C8 122.7(5) . . ? N4 C9 C8 118.5(5) . . ? N5 C10 N4 113.3(5) . . ? N5 C10 C11 121.0(5) . . ? N4 C10 C11 125.6(5) . . ? N7 C11 C10 121.0(5) . . ? N7 C12 C13 120.0(5) . . ? N5 C13 C12 122.7(5) . . ? C14 N8 C16 121.6(5) . . ? C14 N8 C15 121.3(5) . . ? C16 N8 C15 117.1(5) . . ? O5 C14 N8 126.1(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.876 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.155 # Attachment '- 3.cif' data_agpzpypzotf _database_code_depnum_ccdc_archive 'CCDC 780736' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag2 F6 N14 O6 S2' _chemical_formula_weight 1044.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7471(2) _cell_length_b 22.0918(4) _cell_length_c 9.0346(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.2432(9) _cell_angle_gamma 90.00 _cell_volume 1787.53(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4345 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7356 _exptl_absorpt_correction_T_max 0.8279 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12283 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4095 _reflns_number_gt 3525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0468P)^2^+1.0021P] 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 4095 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.66612(2) 0.024217(9) 0.14839(3) 0.02950(9) Uani 1 1 d . . . N1 N 0.5504(3) 0.23569(10) 0.2149(3) 0.0275(5) Uani 1 1 d . . . N2 N 0.7193(2) 0.27187(10) 0.1212(2) 0.0235(4) Uani 1 1 d . . . H2 H 0.6877 0.3070 0.1412 0.028 Uiso 1 1 calc R . . N3 N 0.8887(2) 0.22399(10) 0.0341(2) 0.0226(4) Uani 1 1 d . . . N4 N 1.0453(2) 0.16983(10) -0.0429(3) 0.0261(5) Uani 1 1 d . . . H4 H 1.0020 0.1399 -0.0135 0.031 Uiso 1 1 calc R . . N5 N 1.2274(2) 0.19271(10) -0.1450(3) 0.0271(5) Uani 1 1 d . . . N6 N 0.6119(3) 0.11630(10) 0.1685(3) 0.0265(5) Uani 1 1 d . . . N7 N 1.2695(2) 0.06866(9) -0.1683(3) 0.0246(4) Uani 1 1 d . . . C1 C 0.4845(3) 0.18909(12) 0.2556(4) 0.0312(6) Uani 1 1 d . . . H1 H 0.4136 0.1976 0.3008 0.037 Uiso 1 1 calc R . . C2 C 0.5141(3) 0.12998(12) 0.2353(3) 0.0306(6) Uani 1 1 d . . . H2A H 0.4659 0.0985 0.2683 0.037 Uiso 1 1 calc R . . C3 C 0.6791(3) 0.16171(12) 0.1260(3) 0.0245(5) Uani 1 1 d . . . H3 H 0.7469 0.1530 0.0767 0.029 Uiso 1 1 calc R . . C4 C 0.6511(3) 0.22233(12) 0.1531(3) 0.0224(5) Uani 1 1 d . . . C5 C 0.8313(3) 0.27517(12) 0.0619(3) 0.0230(5) Uani 1 1 d . . . C6 C 0.8767(3) 0.33241(12) 0.0321(3) 0.0263(5) Uani 1 1 d . . . H6 H 0.8339 0.3684 0.0529 0.032 Uiso 1 1 calc R . . C7 C 0.9861(3) 0.33440(12) -0.0288(3) 0.0276(6) Uani 1 1 d . . . H7 H 1.0187 0.3725 -0.0515 0.033 Uiso 1 1 calc R . . C8 C 1.0494(3) 0.28189(12) -0.0575(3) 0.0269(5) Uani 1 1 d . . . H8 H 1.1250 0.2830 -0.0991 0.032 Uiso 1 1 calc R . . C9 C 0.9969(3) 0.22756(11) -0.0226(3) 0.0228(5) Uani 1 1 d . . . C10 C 1.1497(3) 0.15219(11) -0.1012(3) 0.0224(5) Uani 1 1 d . . . C11 C 1.1722(3) 0.08950(12) -0.1104(3) 0.0243(5) Uani 1 1 d . . . H11 H 1.1172 0.0617 -0.0748 0.029 Uiso 1 1 calc R . . C12 C 1.3432(3) 0.10966(12) -0.2200(3) 0.0272(6) Uani 1 1 d . . . H12 H 1.4102 0.0964 -0.2663 0.033 Uiso 1 1 calc R . . C13 C 1.3219(3) 0.16997(13) -0.2061(3) 0.0294(6) Uani 1 1 d . . . H13 H 1.3771 0.1976 -0.2417 0.035 Uiso 1 1 calc R . . S1 S 0.72002(7) 0.45428(3) 0.29354(8) 0.02577(15) Uani 1 1 d . . . O1 O 0.6635(2) 0.40261(9) 0.1904(3) 0.0374(5) Uani 1 1 d . . . O3 O 0.6084(2) 0.48904(8) 0.3238(2) 0.0298(4) Uani 1 1 d . . . O2 O 0.8547(2) 0.44380(9) 0.4354(2) 0.0350(5) Uani 1 1 d . . . C14 C 0.7784(3) 0.50626(14) 0.1711(4) 0.0338(6) Uani 1 1 d . . . F1 F 0.8890(2) 0.48311(9) 0.1381(3) 0.0508(5) Uani 1 1 d . . . F2 F 0.6669(2) 0.51835(10) 0.0335(2) 0.0564(6) Uani 1 1 d . . . F3 F 0.8267(2) 0.55840(8) 0.2473(2) 0.0505(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 Ag 0.03438(14) 0.01857(13) 0.04380(15) -0.00066(8) 0.02426(10) 0.00169(8) N1 0.0279(11) 0.0223(12) 0.0380(12) -0.0027(9) 0.0191(10) 0.0013(9) N2 0.0275(11) 0.0184(11) 0.0296(11) -0.0018(8) 0.0167(9) 0.0030(8) N3 0.0246(11) 0.0205(11) 0.0261(10) -0.0010(8) 0.0139(9) 0.0007(8) N4 0.0304(12) 0.0204(11) 0.0367(12) 0.0006(9) 0.0232(10) -0.0003(9) N5 0.0261(11) 0.0219(11) 0.0396(12) 0.0003(9) 0.0196(10) -0.0013(9) N6 0.0295(12) 0.0192(11) 0.0347(12) -0.0029(9) 0.0170(10) -0.0014(9) N7 0.0289(11) 0.0167(11) 0.0333(11) -0.0002(8) 0.0178(9) 0.0010(9) C1 0.0305(14) 0.0255(14) 0.0472(16) -0.0042(12) 0.0254(13) -0.0005(11) C2 0.0314(14) 0.0251(14) 0.0436(16) -0.0032(11) 0.0235(13) -0.0028(11) C3 0.0250(13) 0.0214(13) 0.0305(13) -0.0029(10) 0.0147(10) 0.0009(10) C4 0.0238(12) 0.0216(13) 0.0234(12) -0.0016(9) 0.0109(10) 0.0004(10) C5 0.0236(12) 0.0241(13) 0.0230(12) -0.0018(9) 0.0112(10) 0.0009(10) C6 0.0299(14) 0.0201(13) 0.0316(13) -0.0019(10) 0.0149(11) 0.0012(10) C7 0.0336(14) 0.0203(13) 0.0316(13) -0.0015(10) 0.0157(11) -0.0055(11) C8 0.0285(13) 0.0260(14) 0.0316(13) -0.0017(10) 0.0175(11) -0.0018(11) C9 0.0266(13) 0.0206(13) 0.0234(12) -0.0011(9) 0.0121(10) 0.0005(10) C10 0.0213(12) 0.0203(13) 0.0278(12) 0.0000(9) 0.0119(10) -0.0001(10) C11 0.0226(12) 0.0218(13) 0.0333(13) 0.0017(10) 0.0161(10) 0.0007(10) C12 0.0272(13) 0.0234(14) 0.0381(14) 0.0027(11) 0.0206(12) 0.0033(11) C13 0.0284(14) 0.0249(14) 0.0423(15) 0.0029(12) 0.0219(12) -0.0020(11) S1 0.0273(3) 0.0202(3) 0.0364(3) 0.0002(2) 0.0197(3) 0.0015(3) O1 0.0432(12) 0.0252(11) 0.0531(12) -0.0101(9) 0.0287(10) -0.0028(9) O3 0.0300(10) 0.0237(10) 0.0420(11) -0.0017(8) 0.0209(9) 0.0037(8) O2 0.0304(10) 0.0347(12) 0.0426(11) 0.0079(9) 0.0173(9) 0.0054(9) C14 0.0337(15) 0.0318(16) 0.0408(16) 0.0021(12) 0.0200(13) 0.0008(12) F1 0.0548(12) 0.0482(12) 0.0728(14) 0.0057(9) 0.0503(11) 0.0037(9) F2 0.0517(12) 0.0709(15) 0.0451(11) 0.0234(9) 0.0174(10) -0.0008(10) F3 0.0672(13) 0.0309(10) 0.0660(12) -0.0019(9) 0.0397(11) -0.0147(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N6 2.128(2) . ? Ag N7 2.133(2) 3_755 ? N1 C1 1.339(4) . ? N1 C4 1.340(3) . ? N2 C4 1.369(3) . ? N2 C5 1.395(3) . ? N3 C5 1.329(3) . ? N3 C9 1.344(3) . ? N4 C10 1.375(3) . ? N4 C9 1.397(3) . ? N5 C10 1.329(3) . ? N5 C13 1.345(3) . ? N6 C3 1.335(3) . ? N6 C2 1.348(3) . ? N7 C11 1.332(3) . ? N7 C12 1.349(3) . ? N7 Ag 2.133(2) 3_755 ? C1 C2 1.365(4) . ? C3 C4 1.408(4) . ? C5 C6 1.400(4) . ? C6 C7 1.381(4) . ? C7 C8 1.386(4) . ? C8 C9 1.389(4) . ? C10 C11 1.410(4) . ? C12 C13 1.362(4) . ? S1 O1 1.439(2) . ? S1 O3 1.4433(19) . ? S1 O2 1.446(2) . ? S1 C14 1.834(3) . ? C14 F2 1.316(4) . ? C14 F1 1.329(3) . ? C14 F3 1.329(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag N7 170.97(8) . 3_755 ? C1 N1 C4 117.0(2) . . ? C4 N2 C5 129.9(2) . . ? C5 N3 C9 118.3(2) . . ? C10 N4 C9 130.4(2) . . ? C10 N5 C13 115.7(2) . . ? C3 N6 C2 118.3(2) . . ? C3 N6 Ag 121.80(17) . . ? C2 N6 Ag 119.74(18) . . ? C11 N7 C12 117.6(2) . . ? C11 N7 Ag 122.05(17) . 3_755 ? C12 N7 Ag 119.71(17) . 3_755 ? N1 C1 C2 123.3(2) . . ? N6 C2 C1 119.9(2) . . ? N6 C3 C4 120.9(2) . . ? N1 C4 N2 114.1(2) . . ? N1 C4 C3 120.5(2) . . ? N2 C4 C3 125.5(2) . . ? N3 C5 N2 118.7(2) . . ? N3 C5 C6 122.9(2) . . ? N2 C5 C6 118.4(2) . . ? C7 C6 C5 117.2(2) . . ? C6 C7 C8 121.3(2) . . ? C7 C8 C9 116.7(2) . . ? N3 C9 C8 123.5(2) . . ? N3 C9 N4 110.7(2) . . ? C8 C9 N4 125.8(2) . . ? N5 C10 N4 121.2(2) . . ? N5 C10 C11 121.6(2) . . ? N4 C10 C11 117.2(2) . . ? N7 C11 C10 120.9(2) . . ? N7 C12 C13 120.2(2) . . ? N5 C13 C12 123.9(2) . . ? O1 S1 O3 114.86(12) . . ? O1 S1 O2 115.37(13) . . ? O3 S1 O2 113.96(12) . . ? O1 S1 C14 103.68(13) . . ? O3 S1 C14 102.57(13) . . ? O2 S1 C14 104.22(13) . . ? F2 C14 F1 107.9(3) . . ? F2 C14 F3 107.8(3) . . ? F1 C14 F3 107.2(2) . . ? F2 C14 S1 111.1(2) . . ? F1 C14 S1 111.5(2) . . ? F3 C14 S1 111.2(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.634 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.115 # Attachment '- 4.cif' data_agpf6n5-2pz _database_code_depnum_ccdc_archive 'CCDC 780737' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 Ag2 F12 N12 O5 P2' _chemical_formula_weight 1136.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1853(3) _cell_length_b 12.2037(2) _cell_length_c 26.1827(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.1668(9) _cell_angle_gamma 90.00 _cell_volume 4394.72(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10755 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'SORTAV, (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25820 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10020 _reflns_number_gt 5975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10020 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 -0.64206(2) -0.16676(3) -0.009110(14) 0.02709(11) Uani 1 1 d . . . Ag2 Ag -0.16148(2) -0.15971(3) -0.054057(14) 0.02931(12) Uani 1 1 d . . . O1 O -0.6124(2) -0.1456(3) 0.08989(13) 0.0419(9) Uani 1 1 d . . . O2 O -0.6486(4) -0.3586(4) -0.0313(2) 0.0925(16) Uiso 1 1 d . . . O3 O -0.1835(3) -0.1572(3) -0.14977(14) 0.0449(9) Uani 1 1 d . . . O4 O -0.1698(3) -0.3610(3) -0.05779(18) 0.0633(12) Uani 1 1 d . . . N1 N -0.4873(2) -0.1572(3) -0.01564(14) 0.0223(8) Uani 1 1 d . . . N2 N -0.4295(2) -0.0910(3) 0.06841(14) 0.0236(8) Uani 1 1 d . . . H2 H -0.4786 -0.1254 0.0763 0.028 Uiso 1 1 calc R . . N3 N -0.3047(2) 0.0358(3) 0.09501(13) 0.0212(8) Uani 1 1 d . . . N4 N -0.1773(2) 0.1603(3) 0.11876(14) 0.0260(9) Uani 1 1 d . . . H4 H -0.1448 0.2057 0.1429 0.031 Uiso 1 1 calc R . . N5 N -0.1983(2) 0.1306(3) 0.02725(14) 0.0213(8) Uani 1 1 d . . . N6 N -0.3055(3) -0.1419(3) -0.03636(15) 0.0256(9) Uani 1 1 d . . . N7 N 0.0028(2) 0.1344(3) 0.04265(15) 0.0263(9) Uani 1 1 d . . . N8 N -0.6840(3) -0.1832(3) 0.15543(15) 0.0343(10) Uani 1 1 d . . . N9 N -0.6414(4) -0.5306(4) -0.05354(19) 0.0563(13) Uani 1 1 d . . . N10 N -0.2410(3) -0.2056(4) -0.23505(17) 0.0422(11) Uani 1 1 d . . . N11 N -0.1468(3) -0.5222(4) -0.0135(2) 0.0592(15) Uani 1 1 d . . . C1 C -0.4715(3) -0.1889(4) -0.06179(18) 0.0290(11) Uani 1 1 d . . . H1 H -0.5242 -0.2186 -0.0877 0.035 Uiso 1 1 calc R . . C2 C -0.3828(3) -0.1801(4) -0.07308(18) 0.0298(11) Uani 1 1 d . . . H2A H -0.3753 -0.2009 -0.1068 0.036 Uiso 1 1 calc R . . C3 C -0.3184(3) -0.1118(3) 0.01030(18) 0.0225(10) Uani 1 1 d . . . H3 H -0.2646 -0.0857 0.0367 0.027 Uiso 1 1 calc R . . C4 C -0.4112(3) -0.1182(3) 0.02107(17) 0.0220(10) Uani 1 1 d . . . C5 C -0.3803(3) -0.0155(3) 0.10604(17) 0.0214(10) Uani 1 1 d . . . C6 C -0.4143(3) 0.0054(4) 0.15028(17) 0.0282(11) Uani 1 1 d . . . H6 H -0.4660 -0.0357 0.1579 0.034 Uiso 1 1 calc R . . C7 C -0.3693(3) 0.0892(4) 0.18298(18) 0.0332(12) Uani 1 1 d . . . H7 H -0.3922 0.1082 0.2130 0.040 Uiso 1 1 calc R . . C8 C -0.2917(3) 0.1456(4) 0.17260(18) 0.0305(11) Uani 1 1 d . . . H8 H -0.2615 0.2041 0.1945 0.037 Uiso 1 1 calc R . . C9 C -0.2593(3) 0.1133(4) 0.12870(17) 0.0244(10) Uani 1 1 d . . . C10 C -0.1407(3) 0.1444(3) 0.07567(17) 0.0229(10) Uani 1 1 d . . . C11 C -0.0385(3) 0.1468(3) 0.08281(17) 0.0245(10) Uani 1 1 d . . . H11 H 0.0018 0.1576 0.1172 0.029 Uiso 1 1 calc R . . C12 C -0.0564(3) 0.1171(4) -0.00550(18) 0.0266(10) Uani 1 1 d . . . H12 H -0.0293 0.1065 -0.0349 0.032 Uiso 1 1 calc R . . C13 C -0.1545(3) 0.1148(4) -0.01224(18) 0.0236(10) Uani 1 1 d . . . H13 H -0.1940 0.1014 -0.0466 0.028 Uiso 1 1 calc R . . C14 C -0.6323(3) -0.2083(4) 0.12207(19) 0.0347(12) Uani 1 1 d . . . H14 H -0.6083 -0.2811 0.1229 0.042 Uiso 1 1 calc R . . C15 C -0.7219(4) -0.0730(4) 0.1587(2) 0.0440(14) Uani 1 1 d . . . H15A H -0.6993 -0.0456 0.1948 0.066 Uiso 1 1 calc R . . H15B H -0.7931 -0.0749 0.1489 0.066 Uiso 1 1 calc R . . H15C H -0.6986 -0.0245 0.1346 0.066 Uiso 1 1 calc R . . C16 C -0.7046(5) -0.2631(5) 0.1933(2) 0.0606(17) Uani 1 1 d . . . H16A H -0.6765 -0.3342 0.1878 0.091 Uiso 1 1 calc R . . H16B H -0.7751 -0.2707 0.1881 0.091 Uiso 1 1 calc R . . H16C H -0.6758 -0.2376 0.2293 0.091 Uiso 1 1 calc R . . C17 C -0.6569(4) -0.4289(5) -0.0686(3) 0.0649(18) Uani 1 1 d . . . H17A H -0.6732 -0.4082 -0.1047 0.078 Uiso 0.67 1 calc PR A 1 H17B H -0.6732 -0.4082 -0.1047 0.078 Uiso 0.33 1 calc PR A 2 C18 C -0.6171(5) -0.5704(6) -0.0016(3) 0.081(2) Uani 1 1 d . . . H18A H -0.6160 -0.5095 0.0230 0.122 Uiso 1 1 calc R . . H18B H -0.5528 -0.6049 0.0057 0.122 Uiso 1 1 calc R . . H18C H -0.6655 -0.6246 0.0028 0.122 Uiso 1 1 calc R . . C19 C -0.6450(6) -0.6156(7) -0.0943(3) 0.105(3) Uiso 1 1 d . . . H19A H -0.6719 -0.5839 -0.1292 0.126 Uiso 1 1 calc R . . H19B H -0.6864 -0.6763 -0.0885 0.126 Uiso 1 1 calc R . . H19C H -0.5792 -0.6428 -0.0923 0.126 Uiso 1 1 calc R . . C20 C -0.2343(4) -0.2146(4) -0.1841(2) 0.0411(13) Uani 1 1 d . . . H20 H -0.2720 -0.2701 -0.1731 0.049 Uiso 1 1 calc R . . C21 C -0.1874(5) -0.1199(5) -0.2547(2) 0.0640(18) Uani 1 1 d . . . H21A H -0.2334 -0.0679 -0.2760 0.096 Uiso 1 1 calc R . . H21B H -0.1477 -0.1530 -0.2765 0.096 Uiso 1 1 calc R . . H21C H -0.1451 -0.0813 -0.2250 0.096 Uiso 1 1 calc R . . C22 C -0.3060(4) -0.2746(6) -0.2743(2) 0.0659(18) Uani 1 1 d . . . H22A H -0.3394 -0.3270 -0.2565 0.099 Uiso 1 1 calc R . . H22B H -0.2679 -0.3145 -0.2949 0.099 Uiso 1 1 calc R . . H22C H -0.3542 -0.2284 -0.2979 0.099 Uiso 1 1 calc R . . C23 C -0.1374(4) -0.4142(5) -0.0171(3) 0.0546(16) Uani 1 1 d . . . H23 H -0.1037 -0.3757 0.0135 0.066 Uiso 1 1 calc R . . C24 C -0.1057(5) -0.5770(6) 0.0350(3) 0.082(2) Uani 1 1 d . . . H24A H -0.0829 -0.5226 0.0628 0.123 Uiso 1 1 calc R . . H24B H -0.0509 -0.6223 0.0311 0.123 Uiso 1 1 calc R . . H24C H -0.1552 -0.6236 0.0444 0.123 Uiso 1 1 calc R . . C25 C -0.2001(6) -0.5836(6) -0.0582(3) 0.088(2) Uani 1 1 d . . . H25A H -0.2297 -0.5331 -0.0867 0.132 Uiso 1 1 calc R . . H25B H -0.2512 -0.6263 -0.0481 0.132 Uiso 1 1 calc R . . H25C H -0.1558 -0.6333 -0.0703 0.132 Uiso 1 1 calc R . . P1 P 0.49228(11) 0.44323(13) 0.18876(6) 0.0477(4) Uani 1 1 d . . . F1 F 0.4771(3) 0.4470(5) 0.12787(17) 0.135(2) Uani 1 1 d . . . F2 F 0.5073(3) 0.4303(4) 0.24944(14) 0.0952(15) Uani 1 1 d . . . F3 F 0.6058(2) 0.4260(3) 0.19526(14) 0.0762(11) Uani 1 1 d . . . F4 F 0.4740(3) 0.3162(3) 0.18366(19) 0.0955(14) Uani 1 1 d . . . F5 F 0.3788(2) 0.4611(3) 0.18339(16) 0.0781(11) Uani 1 1 d . . . F6 F 0.5089(3) 0.5672(3) 0.1914(3) 0.153(3) Uani 1 1 d . . . P2 P -0.05517(13) -0.22039(15) 0.12457(7) 0.0593(5) Uani 1 1 d . . . F7 F -0.1363(3) -0.1728(3) 0.14925(18) 0.1026(16) Uani 1 1 d . . . F8 F 0.0274(3) -0.2703(4) 0.09991(18) 0.1013(15) Uani 1 1 d . . . F9 F -0.1078(3) -0.1833(5) 0.06883(17) 0.147(3) Uani 1 1 d . . . F10 F -0.1001(5) -0.3366(4) 0.1214(2) 0.145(2) Uani 1 1 d . . . F11 F 0.0042(4) -0.2542(5) 0.18128(18) 0.139(2) Uani 1 1 d . . . F12 F 0.0009(4) -0.1097(4) 0.1323(2) 0.1277(19) Uani 1 1 d . . . O5 O -0.0489(3) 0.3067(4) 0.1763(2) 0.0868(16) Uani 1 1 d . . . N12 N 0.0478(4) 0.4460(4) 0.2127(2) 0.0603(15) Uani 1 1 d . . . C26 C -0.0195(5) 0.3723(6) 0.2121(3) 0.0678(19) Uani 1 1 d . . . H26 H -0.0475 0.3694 0.2415 0.081 Uiso 1 1 calc R . . C27 C 0.0764(6) 0.5195(6) 0.2574(3) 0.104(3) Uani 1 1 d . . . H27A H 0.0399 0.5014 0.2836 0.156 Uiso 1 1 calc R . . H27B H 0.0625 0.5953 0.2456 0.156 Uiso 1 1 calc R . . H27C H 0.1462 0.5114 0.2733 0.156 Uiso 1 1 calc R . . C28 C 0.0943(5) 0.4588(6) 0.1710(4) 0.089(3) Uani 1 1 d . . . H28A H 0.0777 0.3967 0.1467 0.134 Uiso 1 1 calc R . . H28B H 0.1649 0.4613 0.1854 0.134 Uiso 1 1 calc R . . H28C H 0.0725 0.5271 0.1521 0.134 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 0.01604(18) 0.0353(2) 0.0307(2) 0.00138(16) 0.00735(14) 0.00036(15) Ag2 0.01777(18) 0.0365(2) 0.0365(2) -0.00247(17) 0.01211(15) -0.00033(15) O1 0.031(2) 0.068(3) 0.031(2) 0.0040(18) 0.0151(16) -0.0113(17) O3 0.046(2) 0.050(2) 0.037(2) -0.0028(18) 0.0063(18) 0.0021(18) O4 0.080(3) 0.039(2) 0.074(3) -0.008(2) 0.024(3) -0.003(2) N1 0.0163(18) 0.029(2) 0.023(2) 0.0010(17) 0.0067(15) 0.0017(16) N2 0.0202(19) 0.024(2) 0.028(2) -0.0029(17) 0.0103(16) -0.0076(16) N3 0.0139(18) 0.025(2) 0.026(2) -0.0030(16) 0.0077(15) 0.0009(15) N4 0.0195(19) 0.033(2) 0.026(2) -0.0118(17) 0.0078(16) -0.0120(17) N5 0.0160(18) 0.025(2) 0.024(2) 0.0004(16) 0.0060(15) -0.0019(15) N6 0.0190(19) 0.029(2) 0.032(2) -0.0031(18) 0.0113(17) 0.0023(16) N7 0.0164(19) 0.029(2) 0.035(2) -0.0012(18) 0.0085(17) -0.0021(16) N8 0.037(2) 0.042(3) 0.029(2) 0.0075(19) 0.0180(19) 0.0027(19) N9 0.062(3) 0.062(4) 0.045(3) 0.012(3) 0.013(3) -0.006(3) N10 0.040(3) 0.056(3) 0.034(3) -0.003(2) 0.014(2) 0.002(2) N11 0.050(3) 0.029(3) 0.106(5) 0.000(3) 0.032(3) -0.003(2) C1 0.021(2) 0.039(3) 0.026(3) -0.007(2) 0.004(2) 0.000(2) C2 0.023(2) 0.041(3) 0.026(3) -0.006(2) 0.007(2) 0.000(2) C3 0.019(2) 0.019(2) 0.031(3) -0.003(2) 0.0091(19) -0.0006(19) C4 0.022(2) 0.018(2) 0.027(3) 0.0000(19) 0.009(2) 0.0026(19) C5 0.016(2) 0.020(2) 0.027(2) 0.0030(19) 0.0044(18) 0.0015(18) C6 0.026(2) 0.039(3) 0.024(2) 0.002(2) 0.014(2) -0.004(2) C7 0.031(3) 0.048(3) 0.024(3) -0.008(2) 0.014(2) -0.006(2) C8 0.025(2) 0.043(3) 0.025(3) -0.010(2) 0.010(2) -0.005(2) C9 0.021(2) 0.026(3) 0.027(3) -0.001(2) 0.008(2) -0.001(2) C10 0.022(2) 0.020(2) 0.028(2) -0.0024(19) 0.0075(19) -0.0033(18) C11 0.020(2) 0.032(3) 0.022(2) 0.002(2) 0.0058(19) -0.003(2) C12 0.026(3) 0.030(3) 0.027(3) -0.001(2) 0.012(2) 0.004(2) C13 0.023(2) 0.026(3) 0.023(2) -0.003(2) 0.0082(19) -0.0021(19) C14 0.024(3) 0.048(3) 0.032(3) 0.002(2) 0.006(2) 0.001(2) C15 0.051(3) 0.046(3) 0.038(3) -0.002(3) 0.017(3) 0.009(3) C16 0.079(4) 0.066(4) 0.045(4) 0.024(3) 0.033(3) 0.001(3) C17 0.061(4) 0.052(4) 0.091(5) -0.012(4) 0.035(4) -0.006(3) C18 0.065(5) 0.098(6) 0.082(6) 0.020(5) 0.020(4) 0.012(4) C20 0.039(3) 0.045(3) 0.040(3) -0.004(3) 0.010(3) 0.005(3) C21 0.086(5) 0.067(4) 0.048(4) 0.003(3) 0.033(4) -0.011(4) C22 0.060(4) 0.092(5) 0.044(4) -0.020(4) 0.012(3) -0.014(4) C23 0.051(4) 0.035(4) 0.080(5) -0.003(3) 0.020(3) 0.002(3) C24 0.057(4) 0.053(4) 0.137(8) 0.026(5) 0.025(5) 0.007(3) C25 0.112(6) 0.046(4) 0.119(7) -0.014(4) 0.052(5) -0.014(4) P1 0.0419(9) 0.0575(11) 0.0440(9) -0.0032(7) 0.0108(7) 0.0001(7) F1 0.089(3) 0.257(7) 0.056(3) 0.021(4) 0.010(2) -0.018(4) F2 0.063(2) 0.179(5) 0.046(2) -0.014(3) 0.0194(19) -0.006(3) F3 0.041(2) 0.123(3) 0.067(3) 0.015(2) 0.0191(18) 0.013(2) F4 0.086(3) 0.067(3) 0.132(4) -0.029(3) 0.025(3) 0.001(2) F5 0.040(2) 0.078(3) 0.113(3) 0.005(2) 0.013(2) 0.0038(18) F6 0.084(3) 0.043(3) 0.331(8) 0.012(4) 0.051(4) -0.014(2) P2 0.0662(11) 0.0679(12) 0.0516(11) 0.0156(9) 0.0296(9) 0.0065(9) F7 0.115(4) 0.114(4) 0.111(4) 0.015(3) 0.090(3) 0.021(3) F8 0.097(3) 0.110(3) 0.117(4) 0.043(3) 0.066(3) 0.049(3) F9 0.074(3) 0.305(8) 0.066(3) 0.068(4) 0.026(2) 0.093(4) F10 0.187(6) 0.110(4) 0.182(6) -0.046(4) 0.129(5) -0.065(4) F11 0.189(6) 0.155(5) 0.068(3) 0.029(3) 0.024(3) 0.043(4) F12 0.152(5) 0.098(4) 0.157(5) -0.008(3) 0.083(4) -0.038(3) O5 0.074(3) 0.094(4) 0.091(4) -0.052(3) 0.016(3) -0.037(3) N12 0.054(3) 0.040(3) 0.071(4) 0.003(3) -0.016(3) -0.010(3) C26 0.069(5) 0.070(5) 0.062(5) -0.024(4) 0.012(4) -0.019(4) C27 0.123(7) 0.070(5) 0.088(6) -0.016(4) -0.035(5) -0.020(5) C28 0.070(5) 0.063(5) 0.142(8) 0.025(5) 0.041(5) 0.015(4) _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 N5 2.241(3) 3_455 ? Ag1 N1 2.247(3) . ? Ag1 O2 2.408(6) . ? Ag1 O1 2.535(3) . ? Ag2 N6 2.213(3) . ? Ag2 N7 2.218(3) 3 ? Ag2 O3 2.449(4) . ? Ag2 O4 2.460(4) . ? O1 C14 1.222(6) . ? O2 C17 1.284(7) . ? O3 C20 1.225(6) . ? O4 C23 1.236(7) . ? N1 C1 1.338(5) . ? N1 C4 1.345(5) . ? N2 C4 1.368(5) . ? N2 C5 1.404(5) . ? N3 C5 1.334(5) . ? N3 C9 1.344(5) . ? N4 C10 1.366(5) . ? N4 C9 1.378(5) . ? N5 C10 1.340(5) . ? N5 C13 1.344(5) . ? N5 Ag1 2.241(3) 3_455 ? N6 C3 1.331(5) . ? N6 C2 1.352(6) . ? N7 C11 1.332(5) . ? N7 C12 1.350(6) . ? N7 Ag2 2.218(3) 3 ? N8 C14 1.307(6) . ? N8 C15 1.458(6) . ? N8 C16 1.470(6) . ? N9 C17 1.305(8) . ? N9 C18 1.406(8) . ? N9 C19 1.481(9) . ? N10 C20 1.319(6) . ? N10 C21 1.459(7) . ? N10 C22 1.468(7) . ? N11 C23 1.330(7) . ? N11 C24 1.428(8) . ? N11 C25 1.439(8) . ? C1 C2 1.366(6) . ? C3 C4 1.415(6) . ? C5 C6 1.383(6) . ? C6 C7 1.385(6) . ? C7 C8 1.380(6) . ? C8 C9 1.395(6) . ? C10 C11 1.416(6) . ? C12 C13 1.359(6) . ? P1 F6 1.530(4) . ? P1 F1 1.556(4) . ? P1 F2 1.559(4) . ? P1 F4 1.572(4) . ? P1 F3 1.592(3) . ? P1 F5 1.597(3) . ? P2 F9 1.536(4) . ? P2 F10 1.549(5) . ? P2 F12 1.556(5) . ? P2 F7 1.563(4) . ? P2 F11 1.572(5) . ? P2 F8 1.590(4) . ? O5 C26 1.225(7) . ? N12 C26 1.309(8) . ? N12 C28 1.415(8) . ? N12 C27 1.452(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N1 158.32(13) 3_455 . ? N5 Ag1 O2 99.39(15) 3_455 . ? N1 Ag1 O2 90.74(15) . . ? N5 Ag1 O1 95.92(12) 3_455 . ? N1 Ag1 O1 98.71(12) . . ? O2 Ag1 O1 109.43(16) . . ? N6 Ag2 N7 156.36(14) . 3 ? N6 Ag2 O3 108.66(13) . . ? N7 Ag2 O3 90.41(13) 3 . ? N6 Ag2 O4 93.95(14) . . ? N7 Ag2 O4 100.46(14) 3 . ? O3 Ag2 O4 88.79(14) . . ? C14 O1 Ag1 129.2(3) . . ? C17 O2 Ag1 145.5(5) . . ? C20 O3 Ag2 130.4(4) . . ? C23 O4 Ag2 119.1(4) . . ? C1 N1 C4 117.7(4) . . ? C1 N1 Ag1 115.8(3) . . ? C4 N1 Ag1 126.3(3) . . ? C4 N2 C5 128.5(4) . . ? C5 N3 C9 118.0(4) . . ? C10 N4 C9 127.3(4) . . ? C10 N5 C13 117.1(4) . . ? C10 N5 Ag1 121.7(3) . 3_455 ? C13 N5 Ag1 119.9(3) . 3_455 ? C3 N6 C2 118.6(4) . . ? C3 N6 Ag2 124.1(3) . . ? C2 N6 Ag2 116.5(3) . . ? C11 N7 C12 117.5(4) . . ? C11 N7 Ag2 120.4(3) . 3 ? C12 N7 Ag2 121.8(3) . 3 ? C14 N8 C15 122.0(4) . . ? C14 N8 C16 122.1(4) . . ? C15 N8 C16 115.8(4) . . ? C17 N9 C18 127.2(6) . . ? C17 N9 C19 118.4(6) . . ? C18 N9 C19 114.4(6) . . ? C20 N10 C21 120.2(5) . . ? C20 N10 C22 122.6(5) . . ? C21 N10 C22 117.1(5) . . ? C23 N11 C24 120.0(6) . . ? C23 N11 C25 120.1(6) . . ? C24 N11 C25 119.9(5) . . ? N1 C1 C2 122.6(4) . . ? N6 C2 C1 120.2(4) . . ? N6 C3 C4 120.8(4) . . ? N1 C4 N2 115.8(4) . . ? N1 C4 C3 120.0(4) . . ? N2 C4 C3 124.1(4) . . ? N3 C5 C6 123.9(4) . . ? N3 C5 N2 116.4(4) . . ? C6 C5 N2 119.6(4) . . ? C5 C6 C7 116.9(4) . . ? C8 C7 C6 121.0(4) . . ? C7 C8 C9 117.4(4) . . ? N3 C9 N4 117.4(4) . . ? N3 C9 C8 122.6(4) . . ? N4 C9 C8 120.1(4) . . ? N5 C10 N4 122.2(4) . . ? N5 C10 C11 119.7(4) . . ? N4 C10 C11 118.2(4) . . ? N7 C11 C10 121.8(4) . . ? N7 C12 C13 120.5(4) . . ? N5 C13 C12 123.3(4) . . ? O1 C14 N8 125.2(5) . . ? O2 C17 N9 115.4(7) . . ? O3 C20 N10 125.3(5) . . ? O4 C23 N11 123.9(6) . . ? F6 P1 F1 89.9(4) . . ? F6 P1 F2 94.2(3) . . ? F1 P1 F2 175.9(3) . . ? F6 P1 F4 177.8(3) . . ? F1 P1 F4 87.9(3) . . ? F2 P1 F4 88.0(3) . . ? F6 P1 F3 89.2(2) . . ? F1 P1 F3 89.8(2) . . ? F2 P1 F3 89.7(2) . . ? F4 P1 F3 91.2(2) . . ? F6 P1 F5 90.5(2) . . ? F1 P1 F5 91.3(2) . . ? F2 P1 F5 89.2(2) . . ? F4 P1 F5 89.2(2) . . ? F3 P1 F5 178.9(2) . . ? F9 P2 F10 96.9(4) . . ? F9 P2 F12 88.9(3) . . ? F10 P2 F12 173.2(4) . . ? F9 P2 F7 92.7(3) . . ? F10 P2 F7 91.6(3) . . ? F12 P2 F7 91.6(3) . . ? F9 P2 F11 176.5(3) . . ? F10 P2 F11 85.9(3) . . ? F12 P2 F11 88.1(3) . . ? F7 P2 F11 89.2(3) . . ? F9 P2 F8 87.8(2) . . ? F10 P2 F8 87.8(3) . . ? F12 P2 F8 88.9(3) . . ? F7 P2 F8 179.2(3) . . ? F11 P2 F8 90.3(3) . . ? C26 N12 C28 122.8(6) . . ? C26 N12 C27 119.6(7) . . ? C28 N12 C27 117.6(6) . . ? O5 C26 N12 124.7(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.263 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.163