# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 # Attachment '- 1-6-crystaldata.CIF' data_publication_text #TrackingRef '- 1-6-crystaldata.CIF' _publ_contact_author_name 'Christoph Janiak' _publ_contact_author_address ;Institut f\"ur Anorganische Chemie und Strukturchemie Universit\"at D\"usseldorf Universit\"atsstr. 1 40225 D\"usseldorf Germany ; _publ_contact_author_email janiak@uni-duesseldorf.de _publ_contact_author_phone +49-211-8112286 loop_ _publ_author_name _publ_author_address A.B.Caballero ;Departamento de Qu\'imica Inorg\'anica Universidad de Granada Severo Ochoa, s/n E-18071 Granada Spain ; J.K.Vieth ;Institut f\"ur Anorganische und Analytische Chemie Universit\"at Freiburg Albertstr. 21 79104 Freiburg Germany ; A.Rodriguez-Dieguez ;Departamento de Qu\'imica Inorg\'anica Universidad de Granada Severo Ochoa, s/n E-18071 Granada Spain ; I.Vidal ;Departamento de Qu\'imica Org\'anica Universidad de Granada Severo Ochoa, s/n E-18071 Granada Spain ; ; J.A.Dobado ; ;Departamento de Qu\'imica Org\'anica Universidad de Granada Severo Ochoa, s/n E-18071 Granada Spain ; J.M.Salas ;Departamento de Qu\'imica Inorg\'anica Universidad de Granada Severo Ochoa, s/n E-18071 Granada Spain ; C.Janiak ;Institut f\"ur Anorganische Chemie und Strukturchemie Universit\"at D\"usseldorf Universit\"atsstr. 1 40225 D\"usseldorf Germany ; _publ_requested_journal XXXXX _publ_section_title ; Dinuclear silver(I) complexes for the design of metal-ligand networks based on triazolopyrimidines ; #============================================================================== data_AC15 _database_code_depnum_ccdc_archive 'CCDC 819202' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [tetrakisacetonitrile-bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)] bis(tetrafluoroborate) ; _chemical_name_common ; (tetrakisacetonitrile-bis(mu-1,2,4-triazolo(1,5- a)pyrimidine)disilver(i)) bis(tetrafluoroborate) ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag2 N12, 2(B F4)' _chemical_formula_sum 'C18 H20 Ag2 B2 F8 N12' _chemical_formula_weight 793.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2201(2) _cell_length_b 10.6272(2) _cell_length_c 11.5588(8) _cell_angle_alpha 110.016(8) _cell_angle_beta 99.817(7) _cell_angle_gamma 91.442(6) _cell_volume 704.51(6) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 61337 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 45.8 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7567 _exptl_absorpt_correction_T_max 0.8725 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Rigaku R-axis Spider Image plate detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33624 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 33.14 _reflns_number_total 5349 _reflns_number_gt 4679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)' _computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn, Germany. Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1). Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~, C---H = 0.97 \%A for CH~3~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~), with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~). ; _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^)+(0.0095P)^2^+0.5767P] 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 5349 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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 0.830421(19) 0.387818(12) 0.405267(12) 0.01624(3) Uani 1 1 d . . . N1 N 0.7546(2) 0.91121(13) 0.51574(13) 0.0186(3) Uani 1 1 d . . . C2 C 0.9360(2) 0.86510(15) 0.55821(15) 0.0180(3) Uani 1 1 d . . . H21 H 1.0624 0.9231 0.6071 0.022 Uiso 1 1 calc R . . N3 N 0.9291(2) 0.72889(12) 0.52703(12) 0.0143(2) Uani 1 1 d . . . C3A C 0.7274(2) 0.68630(14) 0.45974(13) 0.0128(2) Uani 1 1 d . . . N4 N 0.6326(2) 0.55981(12) 0.40569(12) 0.0139(2) Uani 1 1 d . . . C5 C 0.4266(2) 0.54631(15) 0.34491(14) 0.0159(3) Uani 1 1 d . . . H51 H 0.3542 0.4583 0.3056 0.019 Uiso 1 1 calc R . . C6 C 0.3103(2) 0.65561(15) 0.33570(14) 0.0163(3) Uani 1 1 d . . . H61 H 0.1626 0.6408 0.2922 0.020 Uiso 1 1 calc R . . C7 C 0.4116(2) 0.78317(15) 0.38988(14) 0.0162(3) Uani 1 1 d . . . H71 H 0.3395 0.8592 0.3841 0.019 Uiso 1 1 calc R . . N8 N 0.6207(2) 0.79507(12) 0.45228(12) 0.0140(2) Uani 1 1 d . . . N11 N 0.9394(3) 0.35868(19) 0.19869(16) 0.0375(4) Uani 1 1 d . . . C11 C 0.8559(3) 0.36883(19) 0.10715(17) 0.0262(3) Uani 1 1 d . . . C12 C 0.7492(3) 0.3822(2) -0.00966(18) 0.0331(4) Uani 1 1 d . . . H121 H 0.5915 0.3577 -0.0236 0.050 Uiso 1 1 calc R . . H122 H 0.8100 0.3224 -0.0793 0.050 Uiso 1 1 calc R . . H123 H 0.7742 0.4754 -0.0048 0.050 Uiso 1 1 calc R . . N21 N 0.5149(2) 0.22252(15) 0.30291(15) 0.0279(3) Uani 1 1 d . . . C21 C 0.4065(3) 0.14194(18) 0.22132(17) 0.0253(3) Uani 1 1 d . . . C22 C 0.2670(4) 0.0393(2) 0.1154(2) 0.0446(6) Uani 1 1 d . . . H221 H 0.3514 -0.0366 0.0806 0.067 Uiso 1 1 calc R . . H222 H 0.2130 0.0773 0.0508 0.067 Uiso 1 1 calc R . . H223 H 0.1425 0.0083 0.1435 0.067 Uiso 1 1 calc R . . F1 F 0.23263(18) 0.32109(10) 0.79326(10) 0.0282(2) Uani 1 1 d . . . F2 F -0.01278(18) 0.14924(11) 0.77067(12) 0.0349(3) Uani 1 1 d . . . F3 F 0.3482(2) 0.11608(12) 0.78015(13) 0.0380(3) Uani 1 1 d . . . F4 F 0.2283(2) 0.24631(14) 0.95427(11) 0.0395(3) Uani 1 1 d . . . B B 0.2006(3) 0.20728(19) 0.82458(18) 0.0201(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01438(5) 0.01284(5) 0.02100(6) 0.00688(4) -0.00031(4) 0.00375(4) N1 0.0165(6) 0.0118(6) 0.0261(7) 0.0064(5) 0.0003(5) 0.0019(5) C2 0.0165(6) 0.0135(7) 0.0232(7) 0.0066(6) 0.0015(5) 0.0022(5) N3 0.0138(5) 0.0121(5) 0.0172(6) 0.0059(5) 0.0015(4) 0.0030(4) C3A 0.0140(6) 0.0124(6) 0.0140(6) 0.0062(5) 0.0038(5) 0.0052(5) N4 0.0137(5) 0.0121(5) 0.0161(6) 0.0054(5) 0.0023(4) 0.0020(4) C5 0.0153(6) 0.0141(6) 0.0179(7) 0.0061(5) 0.0015(5) 0.0018(5) C6 0.0137(6) 0.0174(7) 0.0184(7) 0.0078(6) 0.0013(5) 0.0032(5) C7 0.0142(6) 0.0168(7) 0.0192(7) 0.0085(6) 0.0026(5) 0.0056(5) N8 0.0142(5) 0.0106(5) 0.0171(6) 0.0054(5) 0.0020(4) 0.0033(4) N11 0.0425(10) 0.0476(11) 0.0246(8) 0.0128(8) 0.0121(7) 0.0037(8) C11 0.0237(8) 0.0274(9) 0.0237(8) 0.0025(7) 0.0084(6) -0.0004(7) C12 0.0294(9) 0.0343(10) 0.0264(9) 0.0032(8) -0.0036(7) 0.0063(8) N21 0.0244(7) 0.0230(7) 0.0332(8) 0.0082(6) 0.0014(6) -0.0037(6) C21 0.0245(8) 0.0218(8) 0.0311(9) 0.0140(7) 0.0002(7) -0.0022(6) C22 0.0531(13) 0.0349(11) 0.0355(11) 0.0140(9) -0.0187(10) -0.0203(10) F1 0.0365(6) 0.0218(5) 0.0303(5) 0.0126(4) 0.0102(5) 0.0032(4) F2 0.0224(5) 0.0281(6) 0.0468(7) 0.0089(5) -0.0032(5) -0.0025(4) F3 0.0336(6) 0.0331(6) 0.0527(8) 0.0184(6) 0.0138(5) 0.0186(5) F4 0.0432(7) 0.0564(8) 0.0229(5) 0.0200(6) 0.0045(5) 0.0017(6) B 0.0198(8) 0.0202(8) 0.0215(8) 0.0092(7) 0.0025(6) 0.0034(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 Ag N3 2.1786(12) 2_766 ? Ag N4 2.2281(12) . ? Ag N21 2.4393(15) . ? Ag N11 2.5127(16) . ? Ag Ag 3.0868(4) 2_766 ? N1 C2 1.3260(19) . ? N1 N8 1.3692(18) . ? C2 N3 1.3644(19) . ? C2 H21 0.9500 . ? N3 C3A 1.3351(18) . ? N3 Ag 2.1786(12) 2_766 ? C3A N4 1.3433(19) . ? C3A N8 1.3679(17) . ? N4 C5 1.3305(18) . ? C5 C6 1.409(2) . ? C5 H51 0.9500 . ? C6 C7 1.367(2) . ? C6 H61 0.9500 . ? C7 N8 1.3556(18) . ? C7 H71 0.9500 . ? N11 C11 1.138(2) . ? C11 C12 1.454(3) . ? C12 H121 0.9800 . ? C12 H122 0.9800 . ? C12 H123 0.9800 . ? N21 C21 1.131(2) . ? C21 C22 1.455(3) . ? C22 H221 0.9800 . ? C22 H222 0.9800 . ? C22 H223 0.9800 . ? F1 B 1.395(2) . ? F2 B 1.394(2) . ? F3 B 1.382(2) . ? F4 B 1.390(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 N3 Ag N4 159.12(5) 2_766 . ? N3 Ag N21 102.45(5) 2_766 . ? N4 Ag N21 92.84(5) . . ? N3 Ag N11 98.93(6) 2_766 . ? N4 Ag N11 94.71(6) . . ? N21 Ag N11 91.59(6) . . ? N3 Ag Ag 78.52(3) 2_766 2_766 ? N4 Ag Ag 83.04(3) . 2_766 ? N21 Ag Ag 164.87(4) . 2_766 ? N11 Ag Ag 103.23(4) . 2_766 ? C2 N1 N8 101.92(12) . . ? N1 C2 N3 115.55(14) . . ? N1 C2 H21 122.2 . . ? N3 C2 H21 122.2 . . ? C3A N3 C2 103.30(12) . . ? C3A N3 Ag 127.97(10) . 2_766 ? C2 N3 Ag 128.12(10) . 2_766 ? N3 C3A N4 128.59(13) . . ? N3 C3A N8 108.96(12) . . ? N4 C3A N8 122.45(13) . . ? C5 N4 C3A 115.90(12) . . ? C5 N4 Ag 124.02(10) . . ? C3A N4 Ag 119.78(9) . . ? N4 C5 C6 123.48(14) . . ? N4 C5 H51 118.3 . . ? C6 C5 H51 118.3 . . ? C7 C6 C5 119.48(13) . . ? C7 C6 H61 120.3 . . ? C5 C6 H61 120.3 . . ? N8 C7 C6 116.20(13) . . ? N8 C7 H71 121.9 . . ? C6 C7 H71 121.9 . . ? C7 N8 C3A 122.48(13) . . ? C7 N8 N1 127.26(12) . . ? C3A N8 N1 110.27(12) . . ? C11 N11 Ag 135.01(16) . . ? N11 C11 C12 179.8(2) . . ? C11 C12 H121 109.5 . . ? C11 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? C11 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? C21 N21 Ag 155.29(15) . . ? N21 C21 C22 179.3(2) . . ? C21 C22 H221 109.5 . . ? C21 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? C21 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? F3 B F4 110.37(14) . . ? F3 B F2 109.80(15) . . ? F4 B F2 109.25(15) . . ? F3 B F1 110.02(14) . . ? F4 B F1 108.76(15) . . ? F2 B F1 108.60(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.392 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.116 #===END data_AC84 _database_code_depnum_ccdc_archive 'CCDC 819203' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [tetrakisacetonitrile-bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)] bis(perchlorate) ; _chemical_name_common ; (tetrakisacetonitrile-bis(mu-1,2,4-triazolo(1,5- a)pyrimidine)disilver(i)) bis(perchlorate) ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag2 N12, 2(Cl O4)' _chemical_formula_sum 'C18 H20 Ag2 Cl2 N12 O8' _chemical_formula_weight 819.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.32530(10) _cell_length_b 10.7545(2) _cell_length_c 11.5478(8) _cell_angle_alpha 110.093(8) _cell_angle_beta 100.489(7) _cell_angle_gamma 90.426(6) _cell_volume 723.32(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 58005 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 41.1 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7296 _exptl_absorpt_correction_T_max 0.8692 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Rigaku R-axis Spider Image plate detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73832 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 41.13 _reflns_number_total 9586 _reflns_number_gt 7488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)' _computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn, Germany. Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1). Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~, C---H = 0.97 \%A for CH~3~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~), with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~). ; _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^)+(0.0299P)^2^+1.5795P] 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 9586 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.83137(2) 0.390209(15) 0.405003(16) 0.01971(4) Uani 1 1 d . . . N11 N 0.9528(5) 0.3690(3) 0.2034(2) 0.0412(6) Uani 1 1 d . . . C11 C 0.8647(4) 0.3754(3) 0.1107(3) 0.0324(5) Uani 1 1 d . . . C12 C 0.7517(6) 0.3857(4) -0.0072(3) 0.0467(8) Uani 1 1 d . . . H12A H 0.8003 0.4694 -0.0136 0.070 Uiso 1 1 calc R . . H12B H 0.5961 0.3836 -0.0092 0.070 Uiso 1 1 calc R . . H12C H 0.7828 0.3110 -0.0779 0.070 Uiso 1 1 calc R . . N21 N 0.5230(4) 0.2291(2) 0.2980(2) 0.0323(4) Uani 1 1 d . . . C21 C 0.4086(4) 0.1499(2) 0.2202(2) 0.0280(4) Uani 1 1 d . . . C22 C 0.2606(6) 0.0500(3) 0.1206(3) 0.0433(7) Uani 1 1 d . . . H22A H 0.1658 0.0927 0.0709 0.052 Uiso 1 1 calc R . . H22B H 0.1734 0.0035 0.1574 0.052 Uiso 1 1 calc R . . H22C H 0.3423 -0.0138 0.0662 0.052 Uiso 1 1 calc R . . N1 N 0.7522(3) 0.90890(18) 0.5216(2) 0.0232(3) Uani 1 1 d . . . C2 C 0.9330(3) 0.8617(2) 0.5612(2) 0.0222(4) Uani 1 1 d . . . H21 H 1.0583 0.9178 0.6091 0.027 Uiso 1 1 calc R . . N3 N 0.9273(3) 0.72709(17) 0.52883(16) 0.0176(3) Uani 1 1 d . . . C3A C 0.7278(3) 0.68667(18) 0.46390(18) 0.0153(3) Uani 1 1 d . . . N4 N 0.6344(3) 0.56270(16) 0.40913(16) 0.0157(3) Uani 1 1 d . . . C5 C 0.4303(3) 0.55088(19) 0.34967(19) 0.0182(3) Uani 1 1 d . . . H51 H 0.3598 0.4643 0.3098 0.022 Uiso 1 1 calc R . . C6 C 0.3129(3) 0.6595(2) 0.3426(2) 0.0192(3) Uani 1 1 d . . . H61 H 0.1667 0.6459 0.2999 0.023 Uiso 1 1 calc R . . C7 C 0.4125(3) 0.7855(2) 0.3983(2) 0.0195(3) Uani 1 1 d . . . H71 H 0.3401 0.8615 0.3944 0.023 Uiso 1 1 calc R . . N8 N 0.6197(3) 0.79520(16) 0.45902(17) 0.0174(3) Uani 1 1 d . . . Cl Cl 0.20575(8) 0.20693(5) 0.82528(5) 0.02404(9) Uani 1 1 d . . . O1 O -0.0112(3) 0.1475(2) 0.7700(3) 0.0439(5) Uani 1 1 d . . . O2 O 0.2367(5) 0.2517(3) 0.9599(2) 0.0511(6) Uani 1 1 d . . . O3 O 0.2341(4) 0.32122(19) 0.78922(19) 0.0332(4) Uani 1 1 d . . . O4 O 0.3596(4) 0.1136(2) 0.7795(3) 0.0486(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 0.01607(6) 0.01597(6) 0.02628(7) 0.00851(5) -0.00013(4) 0.00485(4) N11 0.0482(14) 0.0502(15) 0.0295(11) 0.0152(11) 0.0157(10) 0.0046(12) C11 0.0269(10) 0.0339(12) 0.0314(11) 0.0041(10) 0.0082(9) 0.0005(9) C12 0.0403(15) 0.0455(17) 0.0377(15) 0.0022(13) -0.0091(12) 0.0089(13) N21 0.0270(9) 0.0250(9) 0.0392(11) 0.0084(8) -0.0014(8) -0.0044(7) C21 0.0263(10) 0.0247(10) 0.0333(11) 0.0137(9) 0.0000(8) -0.0020(8) C22 0.0482(16) 0.0355(14) 0.0397(14) 0.0170(12) -0.0141(12) -0.0167(12) N1 0.0183(7) 0.0145(7) 0.0333(9) 0.0067(6) -0.0005(6) 0.0028(5) C2 0.0190(8) 0.0155(8) 0.0297(10) 0.0067(7) 0.0008(7) 0.0019(6) N3 0.0151(6) 0.0155(6) 0.0213(7) 0.0066(5) 0.0011(5) 0.0025(5) C3A 0.0144(6) 0.0144(7) 0.0188(7) 0.0075(6) 0.0043(5) 0.0057(5) N4 0.0153(6) 0.0138(6) 0.0191(6) 0.0073(5) 0.0026(5) 0.0032(5) C5 0.0163(7) 0.0150(7) 0.0239(8) 0.0087(6) 0.0018(6) 0.0029(6) C6 0.0138(7) 0.0195(8) 0.0242(8) 0.0090(7) 0.0010(6) 0.0035(6) C7 0.0162(7) 0.0162(7) 0.0265(9) 0.0089(7) 0.0021(6) 0.0050(6) N8 0.0152(6) 0.0140(6) 0.0229(7) 0.0074(5) 0.0020(5) 0.0043(5) Cl 0.0227(2) 0.0247(2) 0.0263(2) 0.01161(18) 0.00361(17) 0.00152(17) O1 0.0281(9) 0.0311(10) 0.0638(15) 0.0114(10) -0.0021(9) -0.0041(7) O2 0.0642(16) 0.0659(16) 0.0286(10) 0.0253(11) 0.0053(10) 0.0010(13) O3 0.0446(11) 0.0244(8) 0.0367(10) 0.0151(7) 0.0140(8) 0.0026(7) O4 0.0438(12) 0.0410(12) 0.0660(16) 0.0235(12) 0.0128(11) 0.0243(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 Ag N3 2.1845(16) 2_766 ? Ag N4 2.2339(15) . ? Ag N21 2.436(2) . ? Ag N11 2.520(2) . ? Ag Ag 3.0987(5) 2_766 ? N11 C11 1.138(4) . ? C11 C12 1.459(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N21 C21 1.134(3) . ? C21 C22 1.448(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N1 C2 1.324(3) . ? N1 N8 1.370(2) . ? C2 N3 1.363(3) . ? C2 H21 0.9500 . ? N3 C3A 1.329(2) . ? N3 Ag 2.1845(16) 2_766 ? C3A N4 1.341(2) . ? C3A N8 1.369(2) . ? N4 C5 1.330(2) . ? C5 C6 1.407(3) . ? C5 H51 0.9500 . ? C6 C7 1.374(3) . ? C6 H61 0.9500 . ? C7 N8 1.354(2) . ? C7 H71 0.9500 . ? Cl O2 1.435(2) . ? Cl O4 1.439(2) . ? Cl O1 1.445(2) . ? Cl O3 1.4464(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag N4 158.63(6) 2_766 . ? N3 Ag N21 103.05(7) 2_766 . ? N4 Ag N21 92.94(7) . . ? N3 Ag N11 97.48(8) 2_766 . ? N4 Ag N11 95.62(8) . . ? N21 Ag N11 93.32(9) . . ? N3 Ag Ag 78.31(4) 2_766 2_766 ? N4 Ag Ag 82.84(4) . 2_766 ? N21 Ag Ag 166.32(6) . 2_766 ? N11 Ag Ag 100.02(7) . 2_766 ? C11 N11 Ag 132.3(2) . . ? N11 C11 C12 179.1(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 N21 Ag 160.2(2) . . ? N21 C21 C22 179.2(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 N1 N8 101.91(16) . . ? N1 C2 N3 115.52(18) . . ? N1 C2 H21 122.2 . . ? N3 C2 H21 122.2 . . ? C3A N3 C2 103.47(16) . . ? C3A N3 Ag 127.93(13) . 2_766 ? C2 N3 Ag 127.85(13) . 2_766 ? N3 C3A N4 128.93(16) . . ? N3 C3A N8 108.98(16) . . ? N4 C3A N8 122.09(16) . . ? C5 N4 C3A 116.21(16) . . ? C5 N4 Ag 123.76(13) . . ? C3A N4 Ag 119.73(12) . . ? N4 C5 C6 123.64(18) . . ? N4 C5 H51 118.2 . . ? C6 C5 H51 118.2 . . ? C7 C6 C5 119.13(17) . . ? C7 C6 H61 120.4 . . ? C5 C6 H61 120.4 . . ? N8 C7 C6 116.19(17) . . ? N8 C7 H71 121.9 . . ? C6 C7 H71 121.9 . . ? C7 N8 C3A 122.73(17) . . ? C7 N8 N1 127.15(16) . . ? C3A N8 N1 110.11(15) . . ? O2 Cl O4 111.26(16) . . ? O2 Cl O1 109.84(16) . . ? O4 Cl O1 110.18(15) . . ? O2 Cl O3 108.16(14) . . ? O4 Cl O3 108.96(14) . . ? O1 Cl O3 108.37(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 41.13 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.585 _refine_diff_density_min -1.580 _refine_diff_density_rms 0.189 #===END data_an93 _database_code_depnum_ccdc_archive 'CCDC 819204' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [bis(\m-7-amine-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)] bis(perchlorate) ; _chemical_name_common ;(bis(mu-7-amine-1,2,4-triazolo(1,5-a)pyrimidine)disilver(i)) bis(perchlorate) ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Ag2 N10, 2(Cl O4) ' _chemical_formula_sum 'C10 H10 Ag2 Cl2 N10 O8' _chemical_formula_weight 684.92 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7889(15) _cell_length_b 8.389(2) _cell_length_c 10.138(3) _cell_angle_alpha 109.414(3) _cell_angle_beta 91.774(3) _cell_angle_gamma 102.566(3) _cell_volume 450.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2206 _cell_measurement_theta_min 2.653 _cell_measurement_theta_max 26.855 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 2.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4966 _exptl_absorpt_correction_T_max 0.6864 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Rigaku R-axis Spider Image plate detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4319 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1575 _reflns_number_gt 1450 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)' _computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn, Germany. Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1). Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~, C---H = 0.97 \%A for CH~3~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~), with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~). ; _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^)+(0.0637P)^2^+0.7405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1575 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.49054(7) 0.56828(5) 0.38359(4) 0.0292(2) Uani 1 1 d . . . Cl Cl 0.5676(2) 0.80527(17) 0.17999(13) 0.0262(3) Uani 1 1 d . . . C2 C 0.0975(9) 0.7806(7) 0.4737(6) 0.0269(12) Uani 1 1 d . . . H2 H 0.1030 0.8062 0.3912 0.032 Uiso 1 1 calc R . . C3A C 0.1864(9) 0.6727(7) 0.6262(6) 0.0266(12) Uani 1 1 d . . . C5 C 0.1753(10) 0.6090(7) 0.8237(6) 0.0268(12) Uani 1 1 d . . . H5 H 0.2264 0.5548 0.8816 0.032 Uiso 1 1 calc R . . C6 C 0.0128(10) 0.7035(7) 0.8675(6) 0.0275(12) Uani 1 1 d . . . H6 H -0.0453 0.7087 0.9529 0.033 Uiso 1 1 calc R . . C7 C -0.0712(11) 0.7926(8) 0.7919(6) 0.0355(14) Uani 1 1 d . . . N1 N -0.0449(8) 0.8384(6) 0.5670(5) 0.0286(10) Uani 1 1 d . . . N3 N 0.2347(8) 0.6831(6) 0.5018(5) 0.0264(10) Uani 1 1 d . . . N4 N 0.2672(8) 0.5894(6) 0.6998(5) 0.0274(10) Uani 1 1 d . . . N8 N 0.0198(9) 0.7701(7) 0.6686(5) 0.0369(13) Uani 1 1 d . . . N71 N -0.2300(9) 0.8892(7) 0.8175(7) 0.0361(13) Uani 1 1 d . . . O1 O 0.4043(8) 0.6405(6) 0.1479(5) 0.0432(11) Uani 1 1 d . . . O2 O 0.5154(7) 0.9276(6) 0.3068(4) 0.0378(10) Uani 1 1 d . . . O3 O 0.5481(8) 0.8699(6) 0.0675(4) 0.0357(10) Uani 1 1 d . . . O4 O 0.8043(7) 0.7868(6) 0.2000(4) 0.0378(10) Uani 1 1 d . . . H72 H -0.281(16) 0.923(13) 0.753(9) 0.08(3) Uiso 1 1 d . . . H71 H -0.310(16) 0.884(12) 0.884(10) 0.08(3) Uiso 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 0.0304(3) 0.0329(3) 0.0229(3) 0.00412(19) 0.01018(18) 0.0127(2) Cl 0.0296(7) 0.0273(7) 0.0206(7) 0.0058(5) 0.0062(5) 0.0080(5) C2 0.026(3) 0.034(3) 0.020(3) 0.007(2) 0.006(2) 0.009(2) C3A 0.021(3) 0.026(3) 0.026(3) -0.002(2) 0.005(2) 0.008(2) C5 0.032(3) 0.026(3) 0.016(3) 0.002(2) 0.008(2) 0.004(2) C6 0.030(3) 0.029(3) 0.022(3) 0.007(2) 0.010(2) 0.004(2) C7 0.034(3) 0.037(3) 0.029(3) 0.005(3) 0.010(2) 0.004(3) N1 0.033(3) 0.032(3) 0.023(2) 0.011(2) 0.0064(19) 0.009(2) N3 0.023(2) 0.030(3) 0.022(2) 0.0030(19) 0.0035(18) 0.007(2) N4 0.028(2) 0.029(3) 0.020(2) 0.0009(19) 0.0077(19) 0.009(2) N8 0.028(3) 0.035(3) 0.035(3) -0.004(2) 0.010(2) 0.005(2) N71 0.031(3) 0.031(3) 0.048(4) 0.009(3) 0.022(3) 0.014(2) O1 0.050(3) 0.034(2) 0.034(2) 0.0079(19) -0.001(2) -0.004(2) O2 0.035(2) 0.045(3) 0.024(2) -0.0007(18) 0.0115(17) 0.0105(19) O3 0.042(2) 0.043(2) 0.030(2) 0.0175(19) 0.0109(18) 0.019(2) O4 0.036(2) 0.040(2) 0.033(2) 0.0035(19) 0.0043(18) 0.0166(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N3 2.126(4) . ? Ag N4 2.137(4) 2_666 ? Ag Ag 2.9549(10) 2_666 ? Cl O1 1.423(5) . ? Cl O3 1.427(4) . ? Cl O4 1.428(4) . ? Cl O2 1.442(4) . ? C2 N1 1.314(7) . ? C2 N3 1.344(7) . ? C3A N4 1.316(7) . ? C3A N3 1.327(7) . ? C3A N8 1.385(7) . ? C5 C6 1.351(8) . ? C5 N4 1.353(7) . ? C6 C7 1.378(9) . ? C7 N71 1.330(8) . ? C7 N8 1.342(8) . ? N1 N8 1.411(7) . ? N4 Ag 2.137(4) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag N4 164.43(18) . 2_666 ? N3 Ag Ag 81.07(13) . 2_666 ? N4 Ag Ag 83.90(13) 2_666 2_666 ? O1 Cl O3 110.0(3) . . ? O1 Cl O4 109.3(3) . . ? O3 Cl O4 109.5(3) . . ? O1 Cl O2 109.8(3) . . ? O3 Cl O2 108.8(3) . . ? O4 Cl O2 109.4(2) . . ? N1 C2 N3 117.6(5) . . ? N4 C3A N3 130.8(5) . . ? N4 C3A N8 124.0(5) . . ? N3 C3A N8 105.2(5) . . ? C6 C5 N4 123.3(5) . . ? C5 C6 C7 123.3(5) . . ? N71 C7 N8 115.9(6) . . ? N71 C7 C6 131.5(6) . . ? N8 C7 C6 112.6(5) . . ? C2 N1 N8 98.6(4) . . ? C3A N3 C2 106.2(4) . . ? C3A N3 Ag 123.8(4) . . ? C2 N3 Ag 130.0(4) . . ? C3A N4 C5 113.9(5) . . ? C3A N4 Ag 120.1(3) . 2_666 ? C5 N4 Ag 126.0(4) . 2_666 ? C7 N8 C3A 122.9(6) . . ? C7 N8 N1 124.7(5) . . ? C3A N8 N1 112.4(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.403 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.178 #===END data_an86 _database_code_depnum_ccdc_archive 'CCDC 819205' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [acetonitrile-bis(\m-5,7-dimethyl-1,2,4- triazolo[1,5-a]pyrimidine)disilver(I)] tetrafluoroborate perchlorate ; _chemical_name_common ; (acetonitrile-bis(mu-5,7-dimethyl-1,2,4-triazolo(1,5- a)pyrimidine)disilver(i)) tetrafluoroborate perchlorate ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H19 Ag2 N9, F6 P, Cl O4' _chemical_formula_sum 'C16 H19 Ag2 Cl F6 N9 O4 P' _chemical_formula_weight 797.56 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.228(5) _cell_length_b 11.471(5) _cell_length_c 12.191(5) _cell_angle_alpha 110.932(5) _cell_angle_beta 112.874(5) _cell_angle_gamma 97.284(5) _cell_volume 1285.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4452 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.57 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_T_max 0.7176 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13078 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.30 _reflns_number_total 4676 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn, Germany. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~, C---H = 0.97 \%A for CH~3~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~), with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~). ; _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^)+(0.0646P)^2^+1.1555P] 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 4676 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.41587(4) 0.07347(4) 0.40362(4) 0.05776(15) Uani 1 1 d . . . Ag2 Ag 0.66352(4) 0.27337(4) 0.64737(4) 0.06584(16) Uani 1 1 d . . . N1 N 0.6114(4) 0.0810(4) 0.1593(4) 0.0626(11) Uani 1 1 d . . . C2 C 0.5103(5) 0.0496(5) 0.1816(5) 0.0613(13) Uani 1 1 d . . . H2 H 0.4234 -0.0009 0.1129 0.074 Uiso 1 1 calc R . . N3 N 0.5401(4) 0.0954(4) 0.3118(4) 0.0545(10) Uani 1 1 d . . . C3A C 0.6727(5) 0.1642(4) 0.3769(5) 0.0492(10) Uani 1 1 d . . . N4 N 0.7534(4) 0.2312(4) 0.5077(4) 0.0533(9) Uani 1 1 d . . . C5 C 0.8833(5) 0.2891(5) 0.5451(5) 0.0613(13) Uani 1 1 d . . . C51 C 0.9796(6) 0.3648(7) 0.6907(6) 0.090(2) Uani 1 1 d . . . H51A H 0.9558 0.4418 0.7274 0.135 Uiso 1 1 calc R . . H51B H 1.0706 0.3903 0.7034 0.135 Uiso 1 1 calc R . . H51C H 0.9741 0.3110 0.7344 0.135 Uiso 1 1 calc R . . C6 C 0.9292(6) 0.2816(6) 0.4521(6) 0.0693(14) Uani 1 1 d . . . H6 H 1.0201 0.3236 0.4826 0.083 Uiso 1 1 calc R . . C7 C 0.8466(5) 0.2157(5) 0.3197(6) 0.0644(13) Uani 1 1 d . . . C71 C 0.8812(6) 0.2051(7) 0.2118(7) 0.0857(18) Uani 1 1 d . . . H71A H 0.9706 0.2637 0.2491 0.129 Uiso 1 1 calc R . . H71B H 0.8165 0.2281 0.1507 0.129 Uiso 1 1 calc R . . H71C H 0.8791 0.1167 0.1657 0.129 Uiso 1 1 calc R . . N8 N 0.7153(4) 0.1553(4) 0.2847(4) 0.0551(10) Uani 1 1 d . . . N11 N 0.1913(5) 0.0881(5) 0.6259(5) 0.0694(12) Uani 1 1 d . . . C12 C 0.2076(6) 0.0557(5) 0.5201(6) 0.0656(13) Uani 1 1 d . . . H12 H 0.1353 0.0040 0.4354 0.079 Uiso 1 1 calc R . . N13 N 0.3355(4) 0.1011(4) 0.5394(4) 0.0536(9) Uani 1 1 d . . . C13A C 0.4065(5) 0.1735(4) 0.6720(5) 0.0509(11) Uani 1 1 d . . . N14 N 0.5384(4) 0.2437(4) 0.7446(4) 0.0533(9) Uani 1 1 d . . . C15 C 0.5825(5) 0.3069(5) 0.8757(5) 0.0601(12) Uani 1 1 d . . . C151 C 0.7276(6) 0.3901(6) 0.9611(6) 0.0815(17) Uani 1 1 d . . . H51D H 0.7839 0.3446 0.9320 0.122 Uiso 1 1 calc R . . H51E H 0.7539 0.4079 1.0518 0.122 Uiso 1 1 calc R . . H51F H 0.7384 0.4712 0.9543 0.122 Uiso 1 1 calc R . . C16 C 0.4970(7) 0.2985(6) 0.9328(6) 0.0732(15) Uani 1 1 d . . . H16 H 0.5326 0.3430 1.0245 0.088 Uiso 1 1 calc R . . C17 C 0.3635(6) 0.2272(5) 0.8575(5) 0.0659(13) Uani 1 1 d . . . C171 C 0.2638(7) 0.2123(7) 0.9072(6) 0.092(2) Uani 1 1 d . . . H71D H 0.2262 0.1211 0.8815 0.138 Uiso 1 1 calc R . . H71E H 0.1922 0.2459 0.8699 0.138 Uiso 1 1 calc R . . H71F H 0.3085 0.2601 1.0024 0.138 Uiso 1 1 calc R . . N18 N 0.3225(4) 0.1655(4) 0.7248(4) 0.0577(10) Uani 1 1 d . . . N9 N 0.7491(6) 0.5051(5) 0.7411(6) 0.0919(16) Uani 1 1 d . . . C8 C 0.7452(6) 0.6023(6) 0.7434(6) 0.0736(15) Uani 1 1 d . . . C9 C 0.7406(7) 0.7300(6) 0.7494(7) 0.0887(18) Uani 1 1 d . . . H9A H 0.6498 0.7343 0.7266 0.133 Uiso 1 1 calc R . . H9B H 0.7674 0.7433 0.6879 0.133 Uiso 1 1 calc R . . H9C H 0.8017 0.7969 0.8379 0.133 Uiso 1 1 calc R . . Cl Cl 0.89216(12) 0.11221(13) 0.86396(12) 0.0635(3) Uani 1 1 d . . . O1 O 0.9825(6) 0.2214(6) 0.9780(5) 0.144(2) Uani 1 1 d . . . O2 O 0.8313(8) 0.1505(7) 0.7637(6) 0.162(3) Uani 1 1 d . . . O3 O 0.9488(6) 0.0162(5) 0.8133(7) 0.130(2) Uani 1 1 d . . . O4 O 0.7848(7) 0.0531(6) 0.8783(7) 0.162(3) Uani 1 1 d . . . P P 0.34735(14) 0.49710(14) 0.65543(15) 0.0618(4) Uani 1 1 d . . . F1 F 0.2784(7) 0.5728(7) 0.7312(6) 0.171(2) Uani 1 1 d . . . F2 F 0.2746(7) 0.3763(7) 0.6471(10) 0.225(4) Uani 1 1 d . . . F3 F 0.4664(7) 0.5093(7) 0.7801(5) 0.179(3) Uani 1 1 d . . . F4 F 0.4249(7) 0.6196(6) 0.6725(11) 0.246(5) Uani 1 1 d . . . F5 F 0.2269(6) 0.4813(7) 0.5287(6) 0.163(2) Uani 1 1 d . . . F6 F 0.4141(6) 0.4124(6) 0.5772(5) 0.1445(18) 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 0.0487(2) 0.0663(3) 0.0485(2) 0.02208(19) 0.01953(18) 0.00905(18) Ag2 0.0576(3) 0.0697(3) 0.0522(2) 0.0200(2) 0.02076(19) 0.00222(19) N1 0.055(2) 0.075(3) 0.050(2) 0.023(2) 0.023(2) 0.016(2) C2 0.055(3) 0.068(3) 0.047(3) 0.020(2) 0.017(2) 0.014(2) N3 0.045(2) 0.061(2) 0.048(2) 0.0231(19) 0.0163(18) 0.0086(18) C3A 0.044(2) 0.049(2) 0.051(3) 0.025(2) 0.018(2) 0.012(2) N4 0.044(2) 0.059(2) 0.050(2) 0.0255(19) 0.0157(18) 0.0093(18) C5 0.042(3) 0.065(3) 0.063(3) 0.028(3) 0.015(2) 0.008(2) C51 0.055(3) 0.107(5) 0.069(4) 0.026(4) 0.010(3) 0.004(3) C6 0.047(3) 0.077(4) 0.079(4) 0.036(3) 0.026(3) 0.015(3) C7 0.050(3) 0.071(3) 0.077(4) 0.035(3) 0.031(3) 0.020(3) C71 0.075(4) 0.103(5) 0.098(5) 0.047(4) 0.056(4) 0.026(4) N8 0.049(2) 0.060(2) 0.055(2) 0.026(2) 0.023(2) 0.0159(19) N11 0.061(3) 0.071(3) 0.064(3) 0.020(2) 0.030(2) 0.009(2) C12 0.059(3) 0.066(3) 0.060(3) 0.021(3) 0.026(3) 0.010(3) N13 0.055(2) 0.055(2) 0.048(2) 0.0211(19) 0.0239(19) 0.0129(19) C13A 0.058(3) 0.044(2) 0.048(3) 0.019(2) 0.023(2) 0.016(2) N14 0.057(2) 0.049(2) 0.044(2) 0.0171(18) 0.0199(19) 0.0108(18) C15 0.063(3) 0.058(3) 0.050(3) 0.023(2) 0.020(2) 0.017(2) C151 0.074(4) 0.086(4) 0.051(3) 0.017(3) 0.016(3) 0.008(3) C16 0.090(4) 0.075(4) 0.054(3) 0.024(3) 0.037(3) 0.025(3) C17 0.073(4) 0.063(3) 0.058(3) 0.022(3) 0.035(3) 0.016(3) C171 0.107(5) 0.105(5) 0.072(4) 0.031(4) 0.061(4) 0.021(4) N18 0.061(3) 0.055(2) 0.053(2) 0.020(2) 0.029(2) 0.0117(19) N9 0.093(4) 0.063(3) 0.102(4) 0.034(3) 0.037(3) 0.010(3) C8 0.053(3) 0.070(4) 0.069(4) 0.018(3) 0.020(3) 0.000(3) C9 0.090(5) 0.077(4) 0.106(5) 0.048(4) 0.044(4) 0.027(3) Cl 0.0497(7) 0.0702(8) 0.0546(7) 0.0237(6) 0.0164(6) 0.0078(6) O1 0.086(4) 0.143(5) 0.086(4) -0.013(3) 0.004(3) -0.017(3) O2 0.248(8) 0.160(5) 0.088(4) 0.069(4) 0.056(5) 0.123(6) O3 0.122(4) 0.119(4) 0.200(6) 0.081(4) 0.105(4) 0.069(4) O4 0.133(5) 0.150(5) 0.181(6) 0.024(5) 0.117(5) -0.014(4) P 0.0527(7) 0.0625(8) 0.0659(8) 0.0315(7) 0.0223(7) 0.0139(6) F1 0.187(6) 0.203(6) 0.156(5) 0.076(4) 0.097(5) 0.124(5) F2 0.160(6) 0.191(6) 0.451(13) 0.220(8) 0.176(8) 0.107(5) F3 0.170(6) 0.228(7) 0.102(4) 0.051(4) 0.037(4) 0.111(5) F4 0.132(5) 0.137(5) 0.503(15) 0.175(7) 0.148(7) 0.051(4) F5 0.112(4) 0.231(6) 0.140(5) 0.106(5) 0.030(3) 0.059(4) F6 0.150(5) 0.171(5) 0.121(4) 0.055(3) 0.073(3) 0.074(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 N13 2.124(4) . ? Ag1 N3 2.141(4) . ? Ag1 Ag2 2.9852(10) . ? Ag2 N14 2.227(4) . ? Ag2 N4 2.241(4) . ? Ag2 N9 2.371(6) . ? N1 C2 1.303(7) . ? N1 N8 1.362(6) . ? C2 N3 1.362(6) . ? C2 H2 0.9300 . ? N3 C3A 1.344(6) . ? C3A N4 1.334(6) . ? C3A N8 1.360(6) . ? N4 C5 1.340(6) . ? C5 C6 1.398(8) . ? C5 C51 1.497(8) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C6 C7 1.350(7) . ? C6 H6 0.9300 . ? C7 N8 1.369(6) . ? C7 C71 1.481(8) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? N11 C12 1.302(7) . ? N11 N18 1.391(6) . ? C12 N13 1.361(7) . ? C12 H12 0.9300 . ? N13 C13A 1.346(6) . ? C13A N14 1.339(6) . ? C13A N18 1.343(6) . ? N14 C15 1.338(6) . ? C15 C16 1.400(8) . ? C15 C151 1.491(8) . ? C151 H51D 0.9600 . ? C151 H51E 0.9600 . ? C151 H51F 0.9600 . ? C16 C17 1.357(8) . ? C16 H16 0.9300 . ? C17 N18 1.360(6) . ? C17 C171 1.484(8) . ? C171 H71D 0.9600 . ? C171 H71E 0.9600 . ? C171 H71F 0.9600 . ? N9 C8 1.112(7) . ? C8 C9 1.448(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? Cl O1 1.367(5) . ? Cl O2 1.402(5) . ? Cl O4 1.408(5) . ? Cl O3 1.413(5) . ? P F4 1.454(6) . ? P F2 1.465(6) . ? P F3 1.530(5) . ? P F1 1.536(5) . ? P F5 1.537(5) . ? P F6 1.579(5) . ? 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 N13 Ag1 N3 163.84(15) . . ? N13 Ag1 Ag2 82.31(12) . . ? N3 Ag1 Ag2 82.05(11) . . ? N14 Ag2 N4 160.78(14) . . ? N14 Ag2 N9 103.04(18) . . ? N4 Ag2 N9 95.83(18) . . ? N14 Ag2 Ag1 82.18(11) . . ? N4 Ag2 Ag1 82.24(11) . . ? N9 Ag2 Ag1 133.17(15) . . ? C2 N1 N8 102.2(4) . . ? N1 C2 N3 115.8(5) . . ? N1 C2 H2 122.1 . . ? N3 C2 H2 122.1 . . ? C3A N3 C2 103.3(4) . . ? C3A N3 Ag1 125.3(3) . . ? C2 N3 Ag1 131.4(3) . . ? N4 C3A N3 128.5(4) . . ? N4 C3A N8 123.7(4) . . ? N3 C3A N8 107.9(4) . . ? C3A N4 C5 115.6(4) . . ? C3A N4 Ag2 120.1(3) . . ? C5 N4 Ag2 123.2(3) . . ? N4 C5 C6 121.7(5) . . ? N4 C5 C51 118.3(5) . . ? C6 C5 C51 120.0(5) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C7 C6 C5 122.5(5) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 N8 114.4(5) . . ? C6 C7 C71 127.7(5) . . ? N8 C7 C71 117.9(5) . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C3A N8 N1 110.9(4) . . ? C3A N8 C7 122.1(4) . . ? N1 N8 C7 127.0(4) . . ? C12 N11 N18 101.0(4) . . ? N11 C12 N13 116.7(5) . . ? N11 C12 H12 121.6 . . ? N13 C12 H12 121.6 . . ? C13A N13 C12 102.8(4) . . ? C13A N13 Ag1 125.6(3) . . ? C12 N13 Ag1 131.5(4) . . ? N14 C13A N18 123.4(4) . . ? N14 C13A N13 128.0(5) . . ? N18 C13A N13 108.6(4) . . ? C15 N14 C13A 115.3(4) . . ? C15 N14 Ag2 123.2(3) . . ? C13A N14 Ag2 120.9(3) . . ? N14 C15 C16 122.2(5) . . ? N14 C15 C151 117.7(5) . . ? C16 C15 C151 120.2(5) . . ? C15 C151 H51D 109.5 . . ? C15 C151 H51E 109.5 . . ? H51D C151 H51E 109.5 . . ? C15 C151 H51F 109.5 . . ? H51D C151 H51F 109.5 . . ? H51E C151 H51F 109.5 . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 N18 114.3(5) . . ? C16 C17 C171 126.2(5) . . ? N18 C17 C171 119.6(5) . . ? C17 C171 H71D 109.5 . . ? C17 C171 H71E 109.5 . . ? H71D C171 H71E 109.5 . . ? C17 C171 H71F 109.5 . . ? H71D C171 H71F 109.5 . . ? H71E C171 H71F 109.5 . . ? C13A N18 C17 123.2(5) . . ? C13A N18 N11 110.8(4) . . ? C17 N18 N11 126.0(4) . . ? C8 N9 Ag2 153.5(5) . . ? N9 C8 C9 178.7(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 Cl O2 108.6(4) . . ? O1 Cl O4 111.6(4) . . ? O2 Cl O4 105.5(5) . . ? O1 Cl O3 115.4(4) . . ? O2 Cl O3 105.8(4) . . ? O4 Cl O3 109.2(4) . . ? F4 P F2 176.4(6) . . ? F4 P F3 89.3(5) . . ? F2 P F3 87.4(5) . . ? F4 P F1 89.9(4) . . ? F2 P F1 89.0(4) . . ? F3 P F1 94.5(3) . . ? F4 P F5 91.9(5) . . ? F2 P F5 91.5(4) . . ? F3 P F5 178.6(4) . . ? F1 P F5 86.3(3) . . ? F4 P F6 93.1(4) . . ? F2 P F6 88.0(4) . . ? F3 P F6 85.3(3) . . ? F1 P F6 176.9(4) . . ? F5 P F6 93.8(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.695 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.086 #===END data_AC43 _database_code_depnum_ccdc_archive 'CCDC 819206' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [bis(\m-trifluoromethylsulfonate)-bis(\m-5,7-dimethyl-1,2,4- triazolo[1,5-a]pyrimidine)disilver(I)] ; _chemical_name_common ; (bis(mu-trifluoromethylsulfonate)-bis(mu-5,7-dimethyl-1,2,4- triazolo(1,5-a)pyrimidine)disilver(i)) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H8 Ag F3 N4 O3 S' _chemical_formula_sum 'C8 H8 Ag F3 N4 O3 S' _chemical_formula_weight 405.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3689(2) _cell_length_b 8.6550(2) _cell_length_c 9.0743(6) _cell_angle_alpha 93.984(7) _cell_angle_beta 94.541(7) _cell_angle_gamma 112.430(8) _cell_volume 602.09(4) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 69702 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 52.2 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.900 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7025 _exptl_absorpt_correction_T_max 0.8327 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_source_power 2.0 _diffrn_source_voltage 50.0 _diffrn_source_current 40.0 _diffrn_measurement_specimen_support Loop _diffrn_detector RX _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 'Rigaku R-axis Spider Image plate detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55683 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0178 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 33.14 _reflns_number_total 4585 _reflns_number_gt 4237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)' _computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn, Germany. Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1). Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~, C---H = 0.97 \%A for CH~3~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~), with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~). ; _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^)+(0.0163P)^2^+0.6612P] 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 4585 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 0.305239(15) 0.399819(16) 0.465250(13) 0.01730(4) Uani 1 1 d . . . N1 N 0.66482(19) 0.83090(19) 0.12436(17) 0.0200(3) Uani 1 1 d . . . C2 C 0.7299(2) 0.8133(2) 0.2566(2) 0.0201(3) Uani 1 1 d . . . H21 H 0.8405 0.8898 0.3028 0.024 Uiso 1 1 calc R . . N3 N 0.62892(17) 0.67896(18) 0.32278(15) 0.0167(2) Uani 1 1 d . . . C3A C 0.4873(2) 0.6061(2) 0.22440(17) 0.0143(3) Uani 1 1 d . . . N4 N 0.34237(17) 0.46952(17) 0.23496(15) 0.0148(2) Uani 1 1 d . . . C5 C 0.2195(2) 0.4213(2) 0.11843(18) 0.0162(3) Uani 1 1 d . . . C51 C 0.0594(2) 0.2681(2) 0.1246(2) 0.0214(3) Uani 1 1 d . . . H51A H 0.0165 0.2733 0.2215 0.032 Uiso 1 1 calc R . . H51B H 0.0867 0.1679 0.1109 0.032 Uiso 1 1 calc R . . H51C H -0.0302 0.2623 0.0455 0.032 Uiso 1 1 calc R . . C6 C 0.2392(2) 0.5104(2) -0.00849(18) 0.0182(3) Uani 1 1 d . . . H61 H 0.1502 0.4708 -0.0900 0.022 Uiso 1 1 calc R . . C7 C 0.3840(2) 0.6527(2) -0.01610(17) 0.0172(3) Uani 1 1 d . . . C71 C 0.4153(3) 0.7626(2) -0.1386(2) 0.0232(3) Uani 1 1 d . . . H71A H 0.4045 0.8680 -0.1052 0.035 Uiso 1 1 calc R . . H71B H 0.3293 0.7053 -0.2248 0.035 Uiso 1 1 calc R . . H71C H 0.5326 0.7871 -0.1664 0.035 Uiso 1 1 calc R . . N8 N 0.50810(18) 0.69569(18) 0.10368(15) 0.0160(2) Uani 1 1 d . . . S S 0.12324(5) 0.72124(5) 0.42754(4) 0.01527(7) Uani 1 1 d . . . O11 O 0.01579(16) 0.77724(17) 0.51710(15) 0.0228(2) Uani 1 1 d . . . O12 O 0.25063(18) 0.67575(17) 0.50953(15) 0.0240(3) Uani 1 1 d . . . O13 O 0.0326(2) 0.6094(2) 0.29673(17) 0.0325(3) Uani 1 1 d . . . C11 C 0.2554(3) 0.9130(3) 0.3525(3) 0.0293(4) Uani 1 1 d . . . F11 F 0.1558(2) 0.9677(2) 0.2662(2) 0.0626(6) Uani 1 1 d . . . F12 F 0.3449(2) 1.03526(17) 0.4571(2) 0.0551(5) Uani 1 1 d . . . F13 F 0.36797(19) 0.88628(18) 0.26820(18) 0.0407(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01622(5) 0.02163(6) 0.01347(6) 0.00579(4) 0.00062(4) 0.00626(4) N1 0.0175(6) 0.0232(7) 0.0203(7) 0.0078(5) 0.0040(5) 0.0077(5) C2 0.0164(7) 0.0225(7) 0.0217(8) 0.0076(6) 0.0022(6) 0.0069(6) N3 0.0148(5) 0.0213(6) 0.0146(6) 0.0049(5) 0.0008(4) 0.0073(5) C3A 0.0162(6) 0.0185(6) 0.0119(6) 0.0044(5) 0.0029(5) 0.0101(5) N4 0.0151(5) 0.0183(6) 0.0128(6) 0.0031(4) 0.0018(4) 0.0083(5) C5 0.0174(6) 0.0193(7) 0.0142(6) 0.0012(5) 0.0010(5) 0.0101(5) C51 0.0180(7) 0.0228(8) 0.0209(8) 0.0027(6) -0.0006(6) 0.0056(6) C6 0.0202(7) 0.0242(7) 0.0130(7) 0.0016(6) -0.0009(5) 0.0123(6) C7 0.0218(7) 0.0229(7) 0.0124(6) 0.0036(5) 0.0026(5) 0.0146(6) C71 0.0300(8) 0.0300(9) 0.0153(7) 0.0096(6) 0.0039(6) 0.0167(7) N8 0.0164(6) 0.0205(6) 0.0141(6) 0.0061(5) 0.0036(4) 0.0096(5) S 0.01423(15) 0.01622(16) 0.01467(16) 0.00183(13) 0.00040(12) 0.00538(13) O11 0.0183(5) 0.0271(6) 0.0242(6) 0.0048(5) 0.0082(5) 0.0087(5) O12 0.0281(6) 0.0269(6) 0.0212(6) 0.0039(5) -0.0023(5) 0.0162(5) O13 0.0283(7) 0.0377(8) 0.0260(7) -0.0110(6) -0.0099(5) 0.0116(6) C11 0.0295(9) 0.0258(9) 0.0436(12) 0.0151(8) 0.0212(8) 0.0176(7) F11 0.0589(10) 0.0767(12) 0.0900(14) 0.0674(11) 0.0425(10) 0.0517(10) F12 0.0459(8) 0.0187(6) 0.0901(13) -0.0093(7) 0.0327(9) -0.0015(6) F13 0.0443(7) 0.0382(7) 0.0571(9) 0.0235(6) 0.0374(7) 0.0264(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 Ag N3 2.1839(14) 2_666 ? Ag N4 2.2277(13) . ? Ag O11 2.5598(13) 2_566 ? Ag O12 2.6081(13) . ? Ag Ag 3.0398(4) 2_666 ? N1 C2 1.321(2) . ? N1 N8 1.373(2) . ? C2 N3 1.362(2) . ? C2 H21 0.9500 . ? N3 C3A 1.335(2) . ? N3 Ag 2.1839(14) 2_666 ? C3A N4 1.348(2) . ? C3A N8 1.370(2) . ? N4 C5 1.337(2) . ? C5 C6 1.416(2) . ? C5 C51 1.491(2) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C6 C7 1.369(2) . ? C6 H61 0.9500 . ? C7 N8 1.367(2) . ? C7 C71 1.487(2) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? S O13 1.4349(14) . ? S O12 1.4424(13) . ? S O11 1.4483(13) . ? S C11 1.821(2) . ? O11 Ag 2.5598(13) 2_566 ? C11 F12 1.314(3) . ? C11 F13 1.335(2) . ? C11 F11 1.335(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 N3 Ag N4 155.91(5) 2_666 . ? N3 Ag O11 88.87(5) 2_666 2_566 ? N4 Ag O11 110.23(5) . 2_566 ? N3 Ag O12 110.30(5) 2_666 . ? N4 Ag O12 84.81(5) . . ? O11 Ag O12 90.68(4) 2_566 . ? N3 Ag Ag 76.19(4) 2_666 2_666 ? N4 Ag Ag 85.47(4) . 2_666 ? O11 Ag Ag 164.28(3) 2_566 2_666 ? O12 Ag Ag 89.98(3) . 2_666 ? C2 N1 N8 101.64(13) . . ? N1 C2 N3 115.96(15) . . ? N1 C2 H21 122.0 . . ? N3 C2 H21 122.0 . . ? C3A N3 C2 103.38(13) . . ? C3A N3 Ag 129.49(11) . 2_666 ? C2 N3 Ag 127.07(11) . 2_666 ? N3 C3A N4 128.69(14) . . ? N3 C3A N8 108.64(14) . . ? N4 C3A N8 122.67(14) . . ? C5 N4 C3A 116.50(14) . . ? C5 N4 Ag 126.31(11) . . ? C3A N4 Ag 114.59(10) . . ? N4 C5 C6 121.83(15) . . ? N4 C5 C51 117.95(15) . . ? C6 C5 C51 120.22(15) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C7 C6 C5 121.33(15) . . ? C7 C6 H61 119.3 . . ? C5 C6 H61 119.3 . . ? N8 C7 C6 115.03(14) . . ? N8 C7 C71 118.51(15) . . ? C6 C7 C71 126.45(15) . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C7 N8 C3A 122.58(14) . . ? C7 N8 N1 127.04(14) . . ? C3A N8 N1 110.37(13) . . ? O13 S O12 114.80(9) . . ? O13 S O11 115.20(9) . . ? O12 S O11 115.39(8) . . ? O13 S C11 103.13(11) . . ? O12 S C11 103.25(9) . . ? O11 S C11 102.47(8) . . ? S O11 Ag 123.38(8) . 2_566 ? S O12 Ag 127.46(8) . . ? F12 C11 F13 107.70(18) . . ? F12 C11 F11 107.59(19) . . ? F13 C11 F11 106.94(18) . . ? F12 C11 S 112.48(16) . . ? F13 C11 S 111.12(13) . . ? F11 C11 S 110.76(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.861 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.104 #===END data_acad _database_code_depnum_ccdc_archive 'CCDC 819207' #TrackingRef '- 1-6-crystaldata.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-[bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)] bis(hexafluorophosphate) hexahydrate ; _chemical_name_common ; catena-(bis(mu-1,2,4-triazolo(1,5-a)pyrimidine)disilver(i)) bis(hexafluorophosphate) hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C5 H4 Ag N4 O0.12, F6 P' _chemical_formula_sum 'C5 H4 Ag F6 N4 O0.12 P' _chemical_formula_weight 374.91 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 26.0272(3) _cell_length_b 26.0272(3) _cell_length_c 11.0746(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6497.01(16) _cell_formula_units_Z 18 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9913 _cell_measurement_theta_min 2.578 _cell_measurement_theta_max 29.7 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3222 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8921 _exptl_absorpt_correction_T_max 0.9262 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; with 3 H2O crystal water per formula unit 54 H2O per cell included for calculation: _chemical_formula_moiety 'C5 H10 Ag N4 O3 (P F6)' _chemical_formula_sum 'C5 H10 Ag F6 N4 O3 P' _chemical_formula_weight 427.01 _exptl_crystal_density_diffrn 1.964 _exptl_crystal_F_000 3744 _exptl_absorpt_correction_T_min 0.8904 _exptl_absorpt_correction_T_max 0.9250 ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3592 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3592 _reflns_number_gt 3041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)' _computing_publication_material ? _publ_section_references ; Bruker (2006). APEX2 (Version 2.1-0) and SAINT. Bruker Analytical X-ray Systems, Madison, Wisconsin, USA. Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn, Germany. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_exptl_refinement ; Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~ were positioned geometrically (C---H = 0.94 \%A for aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~) and refined using a riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH, AFIX 23 for CH~2~), with U~iso~(H) = 1.2U~eq~(CH). The largest residual Fourier peak (1.06 e \%A^-3^) is found within 0.8 \%A of the Ag atom. The deepest hole (-0.95) is 0.73 \%A from the Ag atom. ; _platon_calc_solv_details ; Note: Expected volumes for solvent molecules are: A hydrogen bonded H2O-molecule 40 Ang^3^ rea #GridPoint VolPerc. Vol(A^3^) X(av) Y(av) Z(av) #----------------------------------------------------- 1 120136[ 55980] 11 747[ 347.9] 0.000 0.000-0.010 2 120136[ 55980] 11 747[ 347.9] 0.333 0.667-0.066 3 120136[ 55980] 11 747[ 347.9] 0.667 0.333 0.042 Each of the three solvent accessible voids of 747 Ang^3^ fits 18 water molecules The voids fit a total of 54 water molecules per cell ; _platon_squeeze_details ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material Nr of gridpoints at least 1.20 Ang. from nearest vdWaals Surface= 167508 N: Total Potential Solvent Accessible Void Vol ..2244.3 Ang^3^ N: Water Count / Cell = 54 - To be included in D(calc), F000 and Mol.Wght. ; 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 _platon_squeeze_void_content 1 0.000 0.000 -0.010 739 318 . 2 0.333 0.667 -0.068 750 318 . 3 0.667 0.333 0.043 750 318 . _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^)+(0.0296P)^2^+12.7529P] 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 3592 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.446243(7) 0.461321(8) 0.574994(14) 0.03309(7) Uani 1 1 d . . . N1 N 0.60307(10) 0.67690(8) 0.69684(16) 0.0371(5) Uani 1 1 d . . . C2 C 0.60347(10) 0.65385(9) 0.59070(18) 0.0301(5) Uani 1 1 d . . . H21 H 0.6304 0.6766 0.5283 0.036 Uiso 1 1 calc R . . N3 N 0.56322(8) 0.59611(8) 0.57714(14) 0.0249(4) Uani 1 1 d . . . C3A C 0.53529(9) 0.58104(9) 0.68323(17) 0.0245(4) Uani 1 1 d . . . N4 N 0.49125(8) 0.52821(8) 0.71900(15) 0.0309(4) Uani 1 1 d . . . C5 C 0.47320(12) 0.52529(11) 0.8324(2) 0.0420(6) Uani 1 1 d . . . H51 H 0.4423 0.4883 0.8615 0.050 Uiso 1 1 calc R . . C6 C 0.49726(12) 0.57383(12) 0.9112(2) 0.0447(7) Uani 1 1 d . . . H61 H 0.4830 0.5693 0.9917 0.054 Uiso 1 1 calc R . . C7 C 0.54103(12) 0.62735(11) 0.87199(19) 0.0398(6) Uani 1 1 d . . . H71 H 0.5579 0.6614 0.9225 0.048 Uiso 1 1 calc R . . N8 N 0.55935(9) 0.62945(8) 0.75668(15) 0.0299(4) Uani 1 1 d . . . O1W O 0.4319(9) 0.5238(9) 0.4635(17) 0.063(7) Uiso 0.121(8) 1 d P . . P P 0.43450(3) 0.32088(3) 0.77647(5) 0.03536(15) Uani 1 1 d . . . F1 F 0.48859(8) 0.34220(9) 0.86690(15) 0.0564(5) Uani 1 1 d . . . F2 F 0.37986(9) 0.30013(9) 0.68593(14) 0.0638(5) Uani 1 1 d . . . F3 F 0.47478(10) 0.32509(14) 0.66672(17) 0.1008(9) Uani 1 1 d . . . F4 F 0.44935(10) 0.38716(9) 0.7599(2) 0.0772(6) Uani 1 1 d . . . F5 F 0.41750(12) 0.25411(9) 0.7951(2) 0.0888(8) Uani 1 1 d . . . F6 F 0.39244(8) 0.31493(9) 0.88577(13) 0.0584(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 0.02770(10) 0.02904(10) 0.02124(9) -0.01103(6) 0.00918(6) -0.00178(7) N1 0.0519(13) 0.0223(9) 0.0201(8) -0.0038(7) 0.0071(8) 0.0057(9) C2 0.0378(12) 0.0225(11) 0.0182(9) -0.0021(8) 0.0049(8) 0.0062(9) N3 0.0283(9) 0.0229(9) 0.0155(7) -0.0037(6) 0.0018(6) 0.0068(7) C3A 0.0266(10) 0.0248(10) 0.0162(8) -0.0066(7) -0.0014(7) 0.0085(9) N4 0.0306(10) 0.0269(9) 0.0191(8) -0.0062(7) 0.0055(7) 0.0024(8) C5 0.0412(14) 0.0351(13) 0.0228(10) -0.0060(9) 0.0110(10) -0.0013(11) C6 0.0522(16) 0.0406(14) 0.0188(10) -0.0078(9) 0.0099(10) 0.0063(12) C7 0.0513(15) 0.0337(13) 0.0188(10) -0.0102(9) 0.0054(10) 0.0094(11) N8 0.0372(11) 0.0225(9) 0.0175(8) -0.0054(7) 0.0028(7) 0.0055(8) P 0.0467(4) 0.0442(4) 0.0190(2) -0.0084(2) -0.0036(2) 0.0256(3) F1 0.0545(10) 0.0835(13) 0.0446(9) -0.0229(8) -0.0172(8) 0.0445(10) F2 0.0687(12) 0.0888(14) 0.0328(8) -0.0174(8) -0.0207(8) 0.0386(11) F3 0.0801(15) 0.181(3) 0.0414(10) -0.0269(13) 0.0131(10) 0.0653(17) F4 0.0922(16) 0.0481(11) 0.0817(14) 0.0083(10) -0.0189(12) 0.0278(11) F5 0.146(2) 0.0516(12) 0.0806(14) -0.0269(10) -0.0393(14) 0.0581(14) F6 0.0548(10) 0.0875(13) 0.0283(7) -0.0122(8) 0.0013(7) 0.0323(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 Ag N3 2.1831(16) 10_666 ? Ag N4 2.2151(17) . ? Ag O1W 2.218(19) . ? Ag N1 2.4137(19) 14_456 ? Ag Ag 3.0016(3) 10_666 ? N1 C2 1.322(3) . ? N1 N8 1.362(3) . ? N1 Ag 2.4136(19) 15_556 ? C2 N3 1.343(3) . ? N3 C3A 1.333(2) . ? N3 Ag 2.1831(16) 10_666 ? C3A N4 1.336(3) . ? C3A N8 1.361(3) . ? N4 C5 1.330(3) . ? C5 C6 1.399(3) . ? C6 C7 1.356(4) . ? C7 N8 1.355(3) . ? P F3 1.5727(19) . ? P F5 1.578(2) . ? P F4 1.579(2) . ? P F1 1.5847(17) . ? P F6 1.5870(16) . ? P F2 1.5974(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag N4 158.13(7) 10_666 . ? N3 Ag O1W 94.0(5) 10_666 . ? N4 Ag O1W 92.4(5) . . ? N3 Ag N1 96.03(7) 10_666 14_456 ? N4 Ag N1 104.58(7) . 14_456 ? O1W Ag N1 92.4(5) . 14_456 ? N3 Ag Ag 77.31(5) 10_666 10_666 ? N4 Ag Ag 85.52(5) . 10_666 ? O1W Ag Ag 69.1(5) . 10_666 ? N1 Ag Ag 159.48(5) 14_456 10_666 ? C2 N1 N8 102.34(17) . . ? C2 N1 Ag 129.41(15) . 15_556 ? N8 N1 Ag 127.17(13) . 15_556 ? N1 C2 N3 115.37(19) . . ? C3A N3 C2 103.66(16) . . ? C3A N3 Ag 128.35(14) . 10_666 ? C2 N3 Ag 127.61(14) . 10_666 ? N3 C3A N4 128.68(18) . . ? N3 C3A N8 108.87(18) . . ? N4 C3A N8 122.44(18) . . ? C5 N4 C3A 115.81(19) . . ? C5 N4 Ag 127.03(16) . . ? C3A N4 Ag 116.09(13) . . ? N4 C5 C6 123.5(2) . . ? C7 C6 C5 119.6(2) . . ? N8 C7 C6 116.2(2) . . ? C7 N8 C3A 122.43(19) . . ? C7 N8 N1 127.82(18) . . ? C3A N8 N1 109.75(16) . . ? F3 P F5 89.31(15) . . ? F3 P F4 92.50(15) . . ? F5 P F4 177.97(14) . . ? F3 P F1 91.12(11) . . ? F5 P F1 90.79(11) . . ? F4 P F1 90.07(11) . . ? F3 P F6 178.41(13) . . ? F5 P F6 89.59(13) . . ? F4 P F6 88.57(12) . . ? F1 P F6 90.05(9) . . ? F3 P F2 89.33(11) . . ? F5 P F2 89.88(12) . . ? F4 P F2 89.24(11) . . ? F1 P F2 179.19(11) . . ? F6 P F2 89.52(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.065 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.070 #===END