Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # 1. SUBMISSION DETAILS _publ_contact_author ; Konstantin V. Domasevitch Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@univ.kiev.ua #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Silver(I) ions bridged by pyridazine: Doubling the ligand functionality for the design of unusual 3D coordination frameworks ; loop_ _publ_author_name _publ_author_address K.V.Domasevitch ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; I.A.Gural'skiy ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; P.V.Solntsev ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; E.B.Rusanov ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; ; H.Krautscheid ; ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; J.A.K.Howard ; Department of Chemistry University of Durham Durham DH1 3LE UK ; A.N.Chernega ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; KVD and HK acknowledge support from Deutsche Forschungsgemeinschaft. ; _publ_contact_author_name 'Konstantin V. Domasevitch' #============================================================================== data_(1) _database_code_depnum_ccdc_archive 'CCDC 643960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Perchlorate 4:5 Complex with Pyridazino[4,5-d]pyridazine ; _chemical_name_common ;Silver(i) Perchlorate 4:5 Complex with Pyridazino(4,5- d)pyridazine ; _chemical_melting_point ? _chemical_formula_moiety '(C30 H20 Ag4 N20), 4(Cl O4)' _chemical_formula_sum 'C30 H20 Ag4 Cl4 N20 O16' _chemical_formula_weight 1489.94 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 Tetragonal _symmetry_space_group_name_H-M 'P4(2)/mnm ' _space_group_name_Hall '-P 4n 2n ' _symmetry_Int_Tables_number 136 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y-1/2, -x-1/2, -z-1/2' '-y-1/2, x-1/2, -z-1/2' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'y, x, z' _cell_length_a 17.0076(10) _cell_length_b 17.0076(10) _cell_length_c 7.8591(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2273.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5.36 _cell_measurement_theta_max 26.01 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 2.025 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7931 _exptl_absorpt_correction_T_max 0.8231 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 10426 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 5.36 _diffrn_reflns_theta_max 26.01 _reflns_number_total 1238 _reflns_number_gt 866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. One of the unique perchlorate anions was badly disordered over overlapping positions related to the overall tetragonal symmetry. It was not possible to resolve this disorder. Thus the remaining disordered electron density was successfully modeled using Squeeze (A. L. Spek, PLATON/PLUTON, Jan. 1999, Acta Crystallogr. Sect. A. 1990, 46, C-34) ; _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^)+(0.0422P)^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_number_reflns 1238 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Ag1 Ag 0.687353(13) 0.312647(13) 0.25893(3) 0.02562(14) Uani 1 2 d S . . N1 N 0.59964(16) 0.40036(16) 0.4135(4) 0.0310(9) Uani 1 2 d S . . N2 N 0.6751(2) 0.18619(17) 0.4124(3) 0.0378(7) Uani 1 1 d . . . N3 N 0.75562(18) -0.08353(17) 0.4126(3) 0.0333(7) Uani 1 1 d . . . C1 C 0.5522(2) 0.4478(2) 0.3326(5) 0.0413(13) Uani 1 2 d S . . H1A H 0.5530 0.4470 0.2130 0.050 Uiso 1 2 calc SR . . C2 C 0.5000 0.5000 0.4134(7) 0.0263(14) Uani 1 4 d S . . C3 C 0.6903(3) 0.1213(2) 0.3309(4) 0.0418(10) Uani 1 1 d . . . H3A H 0.6879 0.1219 0.2114 0.050 Uiso 1 1 calc R . . C4 C 0.7102(2) 0.05045(19) 0.4119(3) 0.0324(8) Uani 1 1 d . . . C5 C 0.7334(2) -0.0202(2) 0.3314(4) 0.0390(9) Uani 1 1 d . . . H5A H 0.7329 -0.0217 0.2118 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.34694(13) 0.34694(13) 0.5456(4) 0.0669(12) Uani 0.50 2 d SP . . O1 O 0.2879(3) 0.2879(3) 0.5000 0.0646(18) Uani 1 4 d S . . O2 O 0.4216(4) 0.3196(4) 0.5000 0.0940(17) Uani 1 2 d S . . O4 O 0.3564(6) 0.3564(6) 0.7186(19) 0.139(6) Uani 0.50 2 d SP . . Cl2 Cl 0.4128(2) 0.4128(2) 0.0000 0.0612(12) Uani 0.50 4 d SP . . O5 O 0.3968(14) 0.4852(14) 0.0000 0.172(7) Uiso 0.50 2 d SP . . O6 O 0.3808(13) 0.3808(13) -0.150(4) 0.234(11) Uiso 0.50 2 d SP . . 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 0.02375(16) 0.02375(16) 0.02938(18) 0.00149(10) -0.00149(10) -0.00228(13) N1 0.0344(15) 0.0344(15) 0.0242(16) -0.0006(11) 0.0006(11) 0.0102(18) N2 0.060(2) 0.0282(17) 0.0247(12) -0.0001(11) -0.0004(13) 0.0092(15) N3 0.053(2) 0.0287(16) 0.0178(11) 0.0007(11) 0.0002(11) 0.0093(13) C1 0.050(2) 0.050(2) 0.023(2) -0.0008(13) 0.0008(13) 0.027(3) C2 0.027(2) 0.027(2) 0.025(3) 0.000 0.000 0.006(3) C3 0.075(3) 0.0292(19) 0.0208(13) 0.0010(12) -0.0027(17) 0.010(2) C4 0.051(2) 0.0246(19) 0.0213(14) 0.0006(12) -0.0003(13) 0.0065(16) C5 0.070(3) 0.030(2) 0.0175(13) 0.0001(13) -0.0002(14) 0.0130(17) Cl1 0.0582(12) 0.0582(12) 0.084(4) -0.0115(10) -0.0115(10) -0.0210(16) O1 0.065(3) 0.065(3) 0.063(3) 0.000 0.000 -0.032(4) O2 0.068(4) 0.097(5) 0.117(4) 0.000 0.000 -0.012(3) O4 0.143(9) 0.143(9) 0.132(10) -0.066(6) -0.066(6) -0.048(11) Cl2 0.067(2) 0.067(2) 0.050(2) 0.000 0.000 -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.424(3) 12_656 ? Ag1 N3 2.424(3) 5_655 ? Ag1 N1 2.434(4) . ? Ag1 N2 2.475(3) 15_665 ? Ag1 N2 2.475(3) . ? N1 C1 1.305(6) . ? N1 N1 1.360(6) 10_556 ? N2 C3 1.302(4) . ? N2 N2 1.377(4) 10_556 ? N3 C5 1.308(4) . ? N3 N3 1.374(5) 10_556 ? C1 C2 1.408(5) . ? C2 C2 1.361(11) 9_666 ? C2 C1 1.408(5) 2_665 ? C3 C4 1.404(5) . ? C4 C4 1.385(5) 10_556 ? C4 C5 1.414(5) . ? Cl1 O4 1.378(14) . ? Cl1 O2 1.399(6) 7_556 ? Cl1 O2 1.399(6) . ? Cl1 O1 1.465(7) . ? Cl1 O4 2.089(15) 10_556 ? Cl2 O5 1.26(2) . ? Cl2 O5 1.26(2) 7 ? Cl2 O6 1.41(3) . ? Cl2 O6 1.41(3) 10 ? 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 Ag1 N3 105.89(13) 12_656 5_655 ? N3 Ag1 N1 94.37(9) 12_656 . ? N3 Ag1 N1 94.37(9) 5_655 . ? N3 Ag1 N2 159.69(11) 12_656 15_665 ? N3 Ag1 N2 82.07(10) 5_655 15_665 ? N1 Ag1 N2 103.77(9) . 15_665 ? N3 Ag1 N2 82.07(10) 12_656 . ? N3 Ag1 N2 159.69(11) 5_655 . ? N1 Ag1 N2 103.77(9) . . ? N2 Ag1 N2 84.76(15) 15_665 . ? C1 N1 N1 119.1(2) . 10_556 ? C1 N1 Ag1 120.9(3) . . ? N1 N1 Ag1 119.93(8) 10_556 . ? C3 N2 N2 119.46(17) . 10_556 ? C3 N2 Ag1 118.7(2) . . ? N2 N2 Ag1 119.17(6) 10_556 . ? C5 N3 N3 119.21(17) . 10_556 ? C5 N3 Ag1 116.37(19) . 11_666 ? N3 N3 Ag1 123.78(6) 10_556 11_666 ? N1 C1 C2 124.0(4) . . ? C2 C2 C1 116.8(3) 9_666 2_665 ? C2 C2 C1 116.8(3) 9_666 . ? C1 C2 C1 126.4(5) 2_665 . ? N2 C3 C4 123.5(3) . . ? C4 C4 C3 116.97(17) 10_556 . ? C4 C4 C5 116.59(16) 10_556 . ? C3 C4 C5 126.4(3) . . ? N3 C5 C4 124.2(3) . . ? O4 Cl1 O2 100.7(3) . 7_556 ? O4 Cl1 O2 100.7(3) . . ? O2 Cl1 O2 122.5(5) 7_556 . ? O4 Cl1 O1 113.7(7) . . ? O2 Cl1 O1 109.4(3) 7_556 . ? O2 Cl1 O1 109.4(3) . . ? O5 Cl2 O5 115(2) . 7 ? O5 Cl2 O6 107.1(7) . . ? O5 Cl2 O6 107.1(7) 7 . ? O5 Cl2 O6 107.1(7) . 10 ? O5 Cl2 O6 107.1(7) 7 10 ? O6 Cl2 O6 114(2) . 10 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.572 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.078 #============================================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 643961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Hexaflurosilicate Tetrafluoroborate Complex with Pyridazino[4,5-d]pyridazine Hydrate ; _chemical_name_common ; Silver(i) Hexaflurosilicate Tetrafluoroborate Complex with Pyridazino(4,5-d)pyridazine Hydrate ; _chemical_melting_point ? _chemical_formula_moiety '2(C15 H10 Ag2 N10), F6 Si, 2(B F4), 4(H2 O)' _chemical_formula_sum 'C30 H28 Ag4 B2 F14 N20 O4 Si' _chemical_formula_weight 1479.91 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Orthorhombic _symmetry_space_group_name_H-M 'P n n m ' _space_group_name_Hall '-P 2 2n ' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.0801(11) _cell_length_b 17.0782(11) _cell_length_c 7.5920(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2214.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5722 _cell_measurement_theta_min 5.34 _cell_measurement_theta_max 26.72 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 1.894 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7515 _exptl_absorpt_correction_T_max 0.8633 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 5722 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 5.34 _diffrn_reflns_theta_max 26.72 _reflns_number_total 2495 _reflns_number_gt 1870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0810P)^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_number_reflns 2495 _refine_ls_number_parameters 184 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.060 _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 0.81416(3) 0.18978(3) 0.24346(4) 0.02393(18) Uani 1 1 d . . . Si1 Si 0.5000 0.0000 0.0000 0.0557(11) Uani 1 4 d S . . B1 B 0.6559(8) 0.3557(6) 0.5000 0.048(3) Uani 1 2 d SD . . F1 F 0.7153(4) 0.3012(4) 0.5000 0.0571(17) Uani 1 2 d SD . . F2 F 0.5803(5) 0.3259(6) 0.5000 0.086(3) Uani 1 2 d S . . F3 F 0.6584(7) 0.3980(6) 0.6469(7) 0.325(14) Uani 1 1 d D . . F4 F 0.5000 0.0000 0.2143(16) 0.261(14) Uani 1 2 d S . . F5 F 0.5848(7) 0.0365(7) 0.0000 0.127(4) Uani 1 2 d S . . F6 F 0.4504(7) 0.0817(6) 0.0000 0.116(4) Uani 1 2 d S . . O1 O 1.0864(7) 0.0773(7) 0.5000 0.090(3) Uani 1 2 d S . . O2 O 0.4619(7) -0.1072(8) 0.5000 0.092(4) Uani 1 2 d S . . N1 N 0.9031(3) 0.1005(3) 0.0904(6) 0.0274(9) Uani 1 1 d . . . N2 N 0.6932(3) 0.1931(3) 0.0913(7) 0.0293(12) Uani 1 1 d . . . N3 N 0.4214(3) 0.2627(3) 0.0929(7) 0.0270(11) Uani 1 1 d . . . N4 N 0.8408(4) 0.3208(3) 0.0909(8) 0.0403(14) Uani 1 1 d . . . N5 N 0.7499(4) 0.5858(3) 0.0874(7) 0.0348(14) Uani 1 1 d . . . C1 C 0.9487(5) 0.0530(4) 0.1757(8) 0.0355(13) Uani 1 1 d . . . H1A H 0.9478 0.0537 0.2995 0.043 Uiso 1 1 calc R . . C2 C 1.0000 0.0000 0.0883(10) 0.0321(17) Uani 1 2 d S . . C3 C 0.6269(4) 0.2049(4) 0.1747(10) 0.0309(14) Uani 1 1 d . . . H3A H 0.6276 0.2014 0.2983 0.037 Uiso 1 1 calc R . . C4 C 0.5554(4) 0.2220(3) 0.0943(8) 0.0230(12) Uani 1 1 d . . . C5 C 0.4852(3) 0.2431(4) 0.1731(9) 0.0281(14) Uani 1 1 d . . . H5A H 0.4839 0.2432 0.2969 0.034 Uiso 1 1 calc R . . C6 C 0.8241(5) 0.3864(4) 0.1778(11) 0.0393(17) Uani 1 1 d . . . H6A H 0.8263 0.3864 0.3015 0.047 Uiso 1 1 calc R . . C7 C 0.8027(4) 0.4568(4) 0.0875(10) 0.0330(15) Uani 1 1 d . . . C8 C 0.7755(5) 0.5238(4) 0.1820(12) 0.0372(17) Uani 1 1 d . . . H8A H 0.7754 0.5247 0.3058 0.045 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 0.0172(4) 0.0205(4) 0.0340(3) 0.00117(18) -0.00384(17) -0.00061(13) Si1 0.064(3) 0.046(3) 0.057(3) 0.000 0.000 0.000(2) B1 0.051(8) 0.038(7) 0.055(7) 0.000 0.000 0.034(5) F1 0.046(4) 0.063(4) 0.062(4) 0.000 0.000 0.015(3) F2 0.074(6) 0.107(7) 0.076(6) 0.000 0.000 0.009(5) F3 0.255(15) 0.38(2) 0.341(16) -0.313(17) -0.203(14) 0.250(16) F4 0.24(2) 0.49(4) 0.051(8) 0.000 0.000 0.12(3) F5 0.137(10) 0.124(10) 0.120(8) 0.000 0.000 -0.039(8) F6 0.133(10) 0.062(6) 0.154(9) 0.000 0.000 -0.013(6) O1 0.086(8) 0.080(8) 0.103(7) 0.000 0.000 -0.005(5) O2 0.065(7) 0.125(11) 0.087(8) 0.000 0.000 -0.004(6) N1 0.022(3) 0.031(3) 0.029(2) -0.002(3) 0.002(2) 0.0133(17) N2 0.023(3) 0.045(4) 0.021(3) 0.007(3) -0.0023(19) 0.011(2) N3 0.017(2) 0.044(3) 0.021(3) -0.001(2) -0.002(2) 0.002(2) N4 0.047(4) 0.028(3) 0.046(4) 0.000(2) -0.001(3) 0.014(2) N5 0.051(4) 0.023(3) 0.031(3) -0.009(3) -0.001(3) 0.015(2) C1 0.053(4) 0.027(4) 0.027(2) 0.002(3) 0.001(4) 0.022(2) C2 0.040(6) 0.035(5) 0.021(4) 0.000 0.000 0.015(3) C3 0.014(3) 0.050(4) 0.028(4) 0.010(3) 0.003(2) 0.002(3) C4 0.022(3) 0.024(3) 0.023(3) -0.005(3) 0.003(2) 0.000(2) C5 0.023(3) 0.049(4) 0.012(3) 0.006(3) 0.007(2) 0.012(3) C6 0.074(5) 0.019(3) 0.025(4) 0.000(3) -0.010(4) 0.003(3) C7 0.043(4) 0.028(3) 0.029(4) 0.004(3) 0.005(3) 0.018(3) C8 0.058(5) 0.021(3) 0.032(4) -0.002(3) -0.010(4) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.358(5) 4 ? Ag1 N2 2.368(5) . ? Ag1 N1 2.447(4) . ? Ag1 N5 2.449(5) 3_645 ? Ag1 N4 2.561(6) . ? Si1 F5 1.577(11) . ? Si1 F5 1.577(11) 5_655 ? Si1 F4 1.627(12) . ? Si1 F4 1.627(12) 5_655 ? Si1 F6 1.633(11) 5_655 ? Si1 F6 1.633(11) . ? B1 F3 1.329(6) . ? B1 F3 1.329(6) 6_556 ? B1 F1 1.377(11) . ? B1 F2 1.388(17) . ? N1 C1 1.296(7) . ? N1 N1 1.372(8) 6 ? N2 C3 1.314(8) . ? N2 N2 1.386(11) 6 ? N3 C5 1.291(8) . ? N3 N3 1.411(11) 6 ? N3 Ag1 2.358(5) 4_455 ? N4 C6 1.331(9) . ? N4 N4 1.380(13) 6 ? N5 N5 1.327(11) 6 ? N5 C8 1.352(9) . ? N5 Ag1 2.449(5) 3_655 ? C1 C2 1.425(6) . ? C2 C2 1.340(15) 5_755 ? C2 C1 1.425(6) 2_755 ? C3 C4 1.395(9) . ? C4 C5 1.388(8) . ? C4 C4 1.432(13) 6 ? C6 C7 1.432(9) . ? C7 C7 1.328(15) 6 ? C7 C8 1.428(10) . ? 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 Ag1 N2 157.9(2) 4 . ? N3 Ag1 N1 88.98(17) 4 . ? N2 Ag1 N1 108.98(18) . . ? N3 Ag1 N5 108.68(16) 4 3_645 ? N2 Ag1 N5 83.34(19) . 3_645 ? N1 Ag1 N5 94.26(18) . 3_645 ? N3 Ag1 N4 78.4(2) 4 . ? N2 Ag1 N4 85.0(2) . . ? N1 Ag1 N4 102.67(18) . . ? N5 Ag1 N4 161.87(19) 3_645 . ? F5 Si1 F5 180.0(8) . 5_655 ? F5 Si1 F4 90.0 . . ? F5 Si1 F4 90.0 5_655 . ? F5 Si1 F4 90.0 . 5_655 ? F5 Si1 F4 90.0 5_655 5_655 ? F4 Si1 F4 180.0 . 5_655 ? F5 Si1 F6 82.0(7) . 5_655 ? F5 Si1 F6 98.0(7) 5_655 5_655 ? F4 Si1 F6 90.0 . 5_655 ? F4 Si1 F6 90.0 5_655 5_655 ? F5 Si1 F6 98.0(7) . . ? F5 Si1 F6 82.0(7) 5_655 . ? F4 Si1 F6 90.0 . . ? F4 Si1 F6 90.0 5_655 . ? F6 Si1 F6 180.0(9) 5_655 . ? F3 B1 F3 114.1(10) . 6_556 ? F3 B1 F1 110.1(7) . . ? F3 B1 F1 110.1(7) 6_556 . ? F3 B1 F2 103.2(8) . . ? F3 B1 F2 103.2(8) 6_556 . ? F1 B1 F2 116.0(10) . . ? C1 N1 N1 120.0(3) . 6 ? C1 N1 Ag1 121.7(4) . . ? N1 N1 Ag1 118.36(10) 6 . ? C3 N2 N2 118.8(4) . 6 ? C3 N2 Ag1 121.4(5) . . ? N2 N2 Ag1 119.21(13) 6 . ? C5 N3 N3 118.1(4) . 6 ? C5 N3 Ag1 119.7(4) . 4_455 ? N3 N3 Ag1 121.79(13) 6 4_455 ? C6 N4 N4 119.7(4) . 6 ? C6 N4 Ag1 118.2(5) . . ? N4 N4 Ag1 116.90(14) 6 . ? N5 N5 C8 122.1(4) 6 . ? N5 N5 Ag1 121.62(13) 6 3_655 ? C8 N5 Ag1 115.7(5) . 3_655 ? N1 C1 C2 122.2(5) . . ? C2 C2 C1 117.8(4) 5_755 2_755 ? C2 C2 C1 117.8(4) 5_755 . ? C1 C2 C1 124.5(7) 2_755 . ? N2 C3 C4 125.1(7) . . ? C5 C4 C3 128.4(6) . . ? C5 C4 C4 115.5(4) . 6 ? C3 C4 C4 115.9(4) . 6 ? N3 C5 C4 126.3(6) . . ? N4 C6 C7 121.6(7) . . ? C7 C7 C8 120.2(4) 6 . ? C7 C7 C6 118.6(4) 6 . ? C8 C7 C6 121.0(7) . . ? N5 C8 C7 117.8(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.384 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.145 #============================================================================== data_(3) _database_code_depnum_ccdc_archive 'CCDC 643962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Trifluorometanesulfonate Complex with Pyridazino[4,5-d]pyridazine, Solvate with 0.33 Water ; _chemical_name_common ; Silver(i) Trifluorometanesulfonate Complex with Pyridazino(4,5-d)pyridazine, Solvate with 0.33 Water ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 Ag3 N12 O, 3(C F3 O3 S) ' _chemical_formula_sum 'C21 H14 Ag3 F9 N12 O10 S3' _chemical_formula_weight 1185.23 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 Trigonal _symmetry_space_group_name_H-M 'R 3 c ' _space_group_name_Hall 'R 3 -2"c ' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' '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+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' '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+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 15.6887(9) _cell_length_b 15.6887(9) _cell_length_c 24.4805(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5218.2(6) _cell_formula_units_Z 6 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.30 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 1.972 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7698 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 10789 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.30 _diffrn_reflns_theta_max 27.87 _reflns_number_total 2695 _reflns_number_gt 1790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. The structure of the metal-organic framework is actually centrosymmetric. Solution of the structure in the centrosymetric space group R-3c led to visibility of the main coordination motif, but with unresoluble disorder in the region of inherently acentric triflate anions. In contrary, for the acentric space group R3c such the disorder disappears and this was suggestive for the refinement of the structure in R3c (even when the PLATON check routine indicates a pseudo inversion center). The structure was refined as a racemic twin leading to a resonable Flack x parameter at 0.42. ; _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^)+(0.0486P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(6) _refine_ls_number_reflns 2695 _refine_ls_number_parameters 176 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.3333 0.6667 0.484452(18) 0.02700(19) Uani 1 3 d S . . Ag2 Ag 0.3333 0.6667 0.33674(5) 0.02614(12) Uani 1 3 d S . . Ag3 Ag 0.6667 1.3333 0.35406(2) 0.0365(2) Uani 1 3 d S . . S1 S 0.36488(11) 1.11396(11) 0.29874(8) 0.0447(3) Uani 1 1 d . . . O1 O 0.3333 0.6667 0.5820(7) 0.124(4) Uani 1 3 d S . . O2 O 0.4608(3) 1.1952(4) 0.2870(2) 0.0651(13) Uani 1 1 d . . . O3 O 0.2911(4) 1.0927(5) 0.2577(2) 0.0785(18) Uani 1 1 d . . . O4 O 0.3613(4) 1.0296(4) 0.3226(2) 0.0750(16) Uani 1 1 d . . . F1 F 0.3271(4) 1.2457(4) 0.3351(4) 0.122(2) Uani 1 1 d . . . F2 F 0.3865(4) 1.1842(5) 0.3975(2) 0.124(3) Uani 1 1 d . . . F3 F 0.2345(4) 1.0951(4) 0.3714(2) 0.106(2) Uani 1 1 d . . . N1 N 0.4097(3) 0.8253(4) 0.4478(3) 0.0254(11) Uani 1 1 d . . . N2 N 0.4120(3) 0.8243(4) 0.3912(3) 0.0270(12) Uani 1 1 d . . . N3 N 0.6002(3) 1.1769(4) 0.4478(2) 0.0288(13) Uani 1 1 d . . . N4 N 0.6023(4) 1.1768(4) 0.3909(2) 0.0260(12) Uani 1 1 d . . . C1 C 0.4541(4) 0.9073(5) 0.4742(3) 0.0262(14) Uani 1 1 d . . . H1A H 0.4517 0.9055 0.5134 0.031 Uiso 1 1 d R . . C2 C 0.5065(4) 1.0005(4) 0.4483(2) 0.0245(14) Uani 1 1 d . . . C3 C 0.5550(4) 1.0935(4) 0.4753(3) 0.0284(15) Uani 1 1 d . . . H3A H 0.5546 1.0957 0.5145 0.034 Uiso 1 1 d R . . C4 C 0.4592(4) 0.9082(5) 0.3654(3) 0.0293(15) Uani 1 1 d . . . H4A H 0.4601 0.9073 0.3262 0.035 Uiso 1 1 d R . . C5 C 0.5092(3) 1.0007(4) 0.3917(2) 0.0212(15) Uani 1 1 d . . . C6 C 0.5603(4) 1.0929(4) 0.3638(3) 0.0256(13) Uani 1 1 d . . . H6A H 0.5654 1.0938 0.3247 0.031 Uiso 1 1 d R . . C7 C 0.3259(5) 1.1582(6) 0.3553(3) 0.065(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0274(3) 0.0274(3) 0.0263(4) 0.000 0.000 0.01369(13) Ag2 0.02189(14) 0.02189(14) 0.0346(2) 0.000 0.000 0.01094(7) Ag3 0.0394(3) 0.0394(3) 0.0307(5) 0.000 0.000 0.01969(17) S1 0.0395(8) 0.0511(9) 0.0340(6) 0.0033(7) -0.0054(6) 0.0156(7) O1 0.178(7) 0.178(7) 0.018(5) 0.000 0.000 0.089(3) O2 0.040(3) 0.065(3) 0.058(3) 0.018(3) 0.011(2) 0.002(2) O3 0.065(3) 0.108(5) 0.041(3) 0.008(3) -0.018(2) 0.027(3) O4 0.062(3) 0.054(3) 0.105(5) 0.015(3) -0.016(3) 0.026(2) F1 0.086(4) 0.086(4) 0.204(6) -0.040(5) -0.016(4) 0.051(3) F2 0.068(3) 0.176(7) 0.050(3) -0.047(3) -0.013(3) 0.003(3) F3 0.056(3) 0.129(4) 0.088(4) -0.042(3) 0.022(3) 0.013(3) N1 0.028(2) 0.027(3) 0.023(3) 0.005(2) 0.0021(19) 0.015(2) N2 0.037(3) 0.014(2) 0.025(3) 0.000(2) -0.001(2) 0.008(2) N3 0.033(2) 0.033(3) 0.019(3) -0.001(2) 0.003(2) 0.016(2) N4 0.028(2) 0.022(3) 0.023(3) -0.003(2) 0.0003(19) 0.0089(19) C1 0.033(3) 0.027(3) 0.017(3) 0.010(2) 0.007(2) 0.014(2) C2 0.033(3) 0.019(3) 0.019(3) -0.003(3) 0.000(2) 0.010(2) C3 0.038(3) 0.014(3) 0.022(3) -0.007(2) -0.002(2) 0.005(2) C4 0.035(3) 0.032(4) 0.019(3) 0.004(3) 0.000(2) 0.015(3) C5 0.022(3) 0.022(4) 0.025(4) 0.005(3) -0.001(2) 0.015(2) C6 0.030(3) 0.019(3) 0.028(3) -0.007(3) -0.003(2) 0.013(2) C7 0.026(3) 0.079(6) 0.064(4) -0.022(4) -0.004(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.335(6) 2_665 ? Ag1 N1 2.335(6) . ? Ag1 N1 2.335(6) 3_565 ? Ag1 O1 2.387(17) . ? Ag2 N2 2.522(6) . ? Ag2 N2 2.522(6) 2_665 ? Ag2 N2 2.522(6) 3_565 ? Ag2 N3 2.531(6) 12_664 ? Ag2 N3 2.531(6) 10_444 ? Ag2 N3 2.531(6) 11_464 ? Ag3 N4 2.320(6) . ? Ag3 N4 2.320(6) 2_775 ? Ag3 N4 2.320(6) 3_575 ? Ag3 O1 2.581(17) 13_554 ? S1 O4 1.423(5) . ? S1 O2 1.434(4) . ? S1 O3 1.440(5) . ? S1 C7 1.787(7) . ? O1 Ag3 2.581(17) 7_445 ? F1 C7 1.450(10) . ? F2 C7 1.323(9) . ? F3 C7 1.332(8) . ? N1 C1 1.288(9) . ? N1 N2 1.388(10) . ? N2 C4 1.307(8) . ? N3 C3 1.318(8) . ? N3 N4 1.394(9) . ? N3 Ag2 2.531(6) 16_554 ? N4 C6 1.319(8) . ? C1 C2 1.420(8) . ? C2 C5 1.387(4) . ? C2 C3 1.427(8) . ? C4 C5 1.413(8) . ? C5 C6 1.429(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 N1 Ag1 N1 106.19(18) 2_665 . ? N1 Ag1 N1 106.19(18) 2_665 3_565 ? N1 Ag1 N1 106.19(18) . 3_565 ? N1 Ag1 O1 112.58(16) 2_665 . ? N1 Ag1 O1 112.58(16) . . ? N1 Ag1 O1 112.58(16) 3_565 . ? N2 Ag2 N2 94.66(19) . 2_665 ? N2 Ag2 N2 94.66(19) . 3_565 ? N2 Ag2 N2 94.66(19) 2_665 3_565 ? N2 Ag2 N3 88.96(12) . 12_664 ? N2 Ag2 N3 175.71(14) 2_665 12_664 ? N2 Ag2 N3 82.73(12) 3_565 12_664 ? N2 Ag2 N3 175.71(14) . 10_444 ? N2 Ag2 N3 82.72(12) 2_665 10_444 ? N2 Ag2 N3 88.96(12) 3_565 10_444 ? N3 Ag2 N3 93.80(18) 12_664 10_444 ? N2 Ag2 N3 82.72(12) . 11_464 ? N2 Ag2 N3 88.96(12) 2_665 11_464 ? N2 Ag2 N3 175.71(14) 3_565 11_464 ? N3 Ag2 N3 93.79(18) 12_664 11_464 ? N3 Ag2 N3 93.79(18) 10_444 11_464 ? N4 Ag3 N4 105.88(17) . 2_775 ? N4 Ag3 N4 105.88(17) . 3_575 ? N4 Ag3 N4 105.88(17) 2_775 3_575 ? N4 Ag3 O1 112.86(15) . 13_554 ? N4 Ag3 O1 112.86(15) 2_775 13_554 ? N4 Ag3 O1 112.86(15) 3_575 13_554 ? O4 S1 O2 116.5(3) . . ? O4 S1 O3 114.7(4) . . ? O2 S1 O3 115.5(3) . . ? O4 S1 C7 100.4(4) . . ? O2 S1 C7 102.7(3) . . ? O3 S1 C7 103.9(4) . . ? Ag1 O1 Ag3 180.0 . 7_445 ? C1 N1 N2 120.7(5) . . ? C1 N1 Ag1 127.1(4) . . ? N2 N1 Ag1 111.9(4) . . ? C4 N2 N1 118.4(6) . . ? C4 N2 Ag2 119.1(5) . . ? N1 N2 Ag2 122.5(4) . . ? C3 N3 N4 120.7(6) . . ? C3 N3 Ag2 116.3(4) . 16_554 ? N4 N3 Ag2 122.7(4) . 16_554 ? C6 N4 N3 120.2(6) . . ? C6 N4 Ag3 126.7(5) . . ? N3 N4 Ag3 112.7(4) . . ? N1 C1 C2 123.3(5) . . ? C5 C2 C1 116.8(4) . . ? C5 C2 C3 117.4(4) . . ? C1 C2 C3 125.8(5) . . ? N3 C3 C2 121.7(6) . . ? N2 C4 C5 123.9(6) . . ? C2 C5 C4 116.9(4) . . ? C2 C5 C6 118.7(4) . . ? C4 C5 C6 124.3(5) . . ? N4 C6 C5 121.2(6) . . ? F2 C7 F3 109.7(7) . . ? F2 C7 F1 107.9(7) . . ? F3 C7 F1 107.7(7) . . ? F2 C7 S1 113.1(6) . . ? F3 C7 S1 113.1(5) . . ? F1 C7 S1 105.0(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.239 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.097 #============================================================================== data_(4) _database_code_depnum_ccdc_archive 'CCDC 643963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Hexafluorosilicate 2:3 Complex with Pyridazino[4,5-d]pyridazine, Decahydrate ; _chemical_name_common ; Silver(i) Hexafluorosilicate 2:3 Complex with Pyridazino(4,5- d)pyridazine, Decahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag4 N12 O4, 2(F6 Si), 6(H2 O)' _chemical_formula_sum 'C18 H32 Ag4 F12 N12 O10 Si2' _chemical_formula_weight 1292.22 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _space_group_name_Hall '-P 2ybc ' _symmetry_Int_Tables_number 14 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 8.85070(10) _cell_length_b 17.2093(3) _cell_length_c 12.0859(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.7850(10) _cell_angle_gamma 90.00 _cell_volume 1808.34(5) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 14014 _cell_measurement_theta_min 5.27 _cell_measurement_theta_max 30.51 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 2.330 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5145 _exptl_absorpt_correction_T_max 0.5968 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 14014 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.27 _diffrn_reflns_theta_max 30.51 _reflns_number_total 5420 _reflns_number_gt 4543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0463P)^2^+5.7522P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0075(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5420 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Ag1 Ag 1.13478(3) 0.09522(2) 0.16329(3) 0.04282(12) Uani 1 1 d . . . Ag2 Ag 1.05257(3) 0.10507(2) -0.13012(2) 0.04062(12) Uani 1 1 d . . . Si1 Si 0.65640(19) 0.32634(8) -0.04392(11) 0.0494(3) Uani 1 1 d . . . F1 F 0.8087(8) 0.2749(5) 0.0036(6) 0.178(4) Uani 1 1 d . . . F2 F 0.5668(8) 0.2685(3) 0.0320(5) 0.130(2) Uani 1 1 d . . . F3 F 0.6197(9) 0.2672(3) -0.1547(5) 0.138(2) Uani 1 1 d . . . F4 F 0.6938(7) 0.3851(3) 0.0645(4) 0.1079(17) Uani 1 1 d . . . F5 F 0.7398(7) 0.3853(3) -0.1211(4) 0.1078(17) Uani 1 1 d . . . F6 F 0.4916(5) 0.3726(3) -0.0919(5) 0.1029(15) Uani 1 1 d . . . O1 O 1.2311(9) 0.2067(3) 0.2918(6) 0.119(2) Uani 1 1 d . . . O2 O 0.8901(7) 0.2114(3) -0.2460(4) 0.0820(14) Uani 1 1 d . . . O3 O 1.0990(6) 0.2450(3) -0.0242(5) 0.0888(15) Uani 1 1 d . . . O4 O 0.4860(7) 0.0290(3) -0.3300(4) 0.0827(15) Uani 1 1 d . . . O5 O 1.3345(8) 0.2987(4) 0.1425(6) 0.113(2) Uani 1 1 d . . . C1 C 0.7626(4) 0.1033(2) 0.1299(3) 0.0305(7) Uani 1 1 d . . . H1A H 0.7848 0.1089 0.2078 0.037 Uiso 1 1 calc R . . C2 C 0.6078(4) 0.1032(2) 0.0740(3) 0.0244(6) Uani 1 1 d . . . C3 C 0.4798(4) 0.1064(2) 0.1290(3) 0.0281(7) Uani 1 1 d . . . H3A H 0.4970 0.1120 0.2069 0.034 Uiso 1 1 calc R . . C4 C 0.7061(4) 0.0902(2) -0.0960(3) 0.0310(7) Uani 1 1 d . . . H4A H 0.6887 0.0868 -0.1741 0.037 Uiso 1 1 calc R . . C5 C 0.5783(4) 0.0967(2) -0.0419(3) 0.0251(6) Uani 1 1 d . . . C6 C 0.4222(4) 0.0950(2) -0.0970(3) 0.0301(7) Uani 1 1 d . . . H6A H 0.4000 0.0919 -0.1752 0.036 Uiso 1 1 calc R . . C7 C 1.1277(5) 0.0496(3) 0.4192(3) 0.0391(9) Uani 1 1 d . . . H7A H 1.2084 0.0851 0.4323 0.047 Uiso 1 1 calc R . . C8 C 1.0585(4) 0.0265(2) 0.5108(3) 0.0312(7) Uani 1 1 d . . . C9 C 1.0975(5) 0.0566(3) 0.6213(3) 0.0370(8) Uani 1 1 d . . . H9A H 1.1731 0.0946 0.6367 0.044 Uiso 1 1 calc R . . N1 N 0.8766(4) 0.0958(2) 0.0745(3) 0.0325(7) Uani 1 1 d . . . N2 N 0.8472(4) 0.0889(2) -0.0407(3) 0.0321(6) Uani 1 1 d . . . N3 N 0.3379(3) 0.10189(18) 0.0735(2) 0.0272(6) Uani 1 1 d . . . N4 N 0.3083(3) 0.09747(19) -0.0424(3) 0.0299(6) Uani 1 1 d . . . N5 N 1.0824(4) 0.0229(2) 0.3172(3) 0.0358(7) Uani 1 1 d . . . N6 N 1.0303(4) 0.0325(2) 0.7026(3) 0.0348(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02533(15) 0.0748(3) 0.03053(16) 0.00196(14) 0.01082(11) -0.00717(13) Ag2 0.02318(15) 0.0694(2) 0.03030(16) -0.00957(13) 0.00751(10) -0.00187(13) Si1 0.0662(9) 0.0445(7) 0.0415(6) 0.0073(5) 0.0200(6) 0.0189(6) F1 0.148(5) 0.262(9) 0.137(5) 0.070(5) 0.057(4) 0.150(6) F2 0.205(7) 0.063(3) 0.156(5) 0.035(3) 0.118(5) 0.016(3) F3 0.226(7) 0.098(4) 0.103(4) -0.047(3) 0.062(4) -0.013(4) F4 0.138(5) 0.119(4) 0.067(3) -0.034(3) 0.022(3) -0.015(3) F5 0.136(4) 0.121(4) 0.080(3) 0.007(3) 0.056(3) -0.042(3) F6 0.069(3) 0.108(3) 0.127(4) 0.022(3) 0.005(3) 0.019(2) O1 0.159(6) 0.082(4) 0.137(5) -0.037(4) 0.085(5) -0.034(4) O2 0.109(4) 0.087(3) 0.048(2) 0.006(2) 0.008(2) 0.021(3) O3 0.068(3) 0.091(4) 0.108(4) -0.010(3) 0.017(3) 0.006(3) O4 0.129(4) 0.066(3) 0.061(2) -0.014(2) 0.039(3) -0.019(3) O5 0.121(5) 0.075(4) 0.152(6) 0.005(4) 0.049(5) 0.004(3) C1 0.0248(16) 0.043(2) 0.0238(14) 0.0019(13) 0.0053(12) -0.0009(14) C2 0.0196(14) 0.0282(16) 0.0262(14) -0.0009(12) 0.0069(11) -0.0004(11) C3 0.0249(15) 0.0368(19) 0.0241(14) -0.0021(13) 0.0082(12) -0.0004(13) C4 0.0213(15) 0.046(2) 0.0268(15) -0.0034(14) 0.0079(12) -0.0039(14) C5 0.0202(14) 0.0304(17) 0.0261(15) -0.0010(12) 0.0077(11) 0.0000(12) C6 0.0193(14) 0.046(2) 0.0259(15) -0.0028(14) 0.0052(12) -0.0006(13) C7 0.041(2) 0.054(3) 0.0247(16) -0.0010(16) 0.0114(15) -0.0153(18) C8 0.0353(18) 0.039(2) 0.0202(14) -0.0003(13) 0.0077(13) -0.0033(15) C9 0.041(2) 0.046(2) 0.0240(15) -0.0041(15) 0.0077(14) -0.0122(17) N1 0.0218(13) 0.0475(19) 0.0283(14) 0.0001(13) 0.0055(11) -0.0013(12) N2 0.0221(14) 0.0453(18) 0.0303(14) -0.0026(13) 0.0083(11) -0.0002(12) N3 0.0198(12) 0.0375(16) 0.0260(13) -0.0005(11) 0.0087(10) -0.0009(11) N4 0.0196(13) 0.0439(18) 0.0271(13) -0.0032(12) 0.0065(10) -0.0006(11) N5 0.0379(17) 0.0472(19) 0.0241(13) 0.0007(13) 0.0104(12) -0.0064(14) N6 0.0383(17) 0.0451(19) 0.0220(13) -0.0029(12) 0.0079(12) -0.0056(14) _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 N3 2.270(3) 1_655 ? Ag1 N1 2.336(3) . ? Ag1 N5 2.355(3) . ? Ag1 O1 2.515(6) . ? Ag2 N2 2.299(3) . ? Ag2 N4 2.316(3) 1_655 ? Ag2 N6 2.354(3) 1_554 ? Ag2 O2 2.574(5) . ? Si1 F1 1.625(5) . ? Si1 F4 1.639(4) . ? Si1 F5 1.644(4) . ? Si1 F2 1.654(5) . ? Si1 F3 1.665(5) . ? Si1 F6 1.668(5) . ? C1 N1 1.317(5) . ? C1 C2 1.410(5) . ? C2 C5 1.381(5) . ? C2 C3 1.417(5) . ? C3 N3 1.310(4) . ? C4 N2 1.302(5) . ? C4 C5 1.413(5) . ? C5 C6 1.418(5) . ? C6 N4 1.304(4) . ? C7 N5 1.306(5) . ? C7 C8 1.418(5) . ? C8 C8 1.370(8) 3_756 ? C8 C9 1.414(5) . ? C9 N6 1.307(5) . ? N1 N2 1.373(4) . ? N3 N4 1.379(4) . ? N5 N6 1.368(5) 3_756 ? 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 Ag1 N1 125.07(11) 1_655 . ? N3 Ag1 N5 134.02(12) 1_655 . ? N1 Ag1 N5 92.56(12) . . ? N3 Ag1 O1 92.83(16) 1_655 . ? N1 Ag1 O1 118.0(2) . . ? N5 Ag1 O1 90.51(17) . . ? N2 Ag2 N4 124.68(11) . 1_655 ? N2 Ag2 N6 113.16(12) . 1_554 ? N4 Ag2 N6 106.29(11) 1_655 1_554 ? N2 Ag2 O2 86.07(15) . . ? N4 Ag2 O2 133.45(16) 1_655 . ? N6 Ag2 O2 87.79(14) 1_554 . ? F1 Si1 F4 91.3(4) . . ? F1 Si1 F5 96.1(4) . . ? F4 Si1 F5 91.6(3) . . ? F1 Si1 F2 85.9(4) . . ? F4 Si1 F2 88.5(3) . . ? F5 Si1 F2 178.0(3) . . ? F1 Si1 F3 88.6(4) . . ? F4 Si1 F3 179.4(3) . . ? F5 Si1 F3 87.8(3) . . ? F2 Si1 F3 92.1(3) . . ? F1 Si1 F6 175.3(4) . . ? F4 Si1 F6 90.9(3) . . ? F5 Si1 F6 88.0(3) . . ? F2 Si1 F6 90.1(3) . . ? F3 Si1 F6 89.2(3) . . ? N1 C1 C2 121.6(3) . . ? C5 C2 C1 117.9(3) . . ? C5 C2 C3 117.6(3) . . ? C1 C2 C3 124.5(3) . . ? N3 C3 C2 122.1(3) . . ? N2 C4 C5 122.5(3) . . ? C2 C5 C4 117.4(3) . . ? C2 C5 C6 117.4(3) . . ? C4 C5 C6 125.1(3) . . ? N4 C6 C5 122.6(3) . . ? N5 C7 C8 122.5(4) . . ? C8 C8 C9 117.7(4) 3_756 . ? C8 C8 C7 117.4(4) 3_756 . ? C9 C8 C7 124.8(4) . . ? N6 C9 C8 122.0(4) . . ? C1 N1 N2 120.4(3) . . ? C1 N1 Ag1 122.9(2) . . ? N2 N1 Ag1 116.7(2) . . ? C4 N2 N1 120.1(3) . . ? C4 N2 Ag2 121.6(2) . . ? N1 N2 Ag2 116.7(2) . . ? C3 N3 N4 120.3(3) . . ? C3 N3 Ag1 121.8(2) . 1_455 ? N4 N3 Ag1 117.8(2) . 1_455 ? C6 N4 N3 119.9(3) . . ? C6 N4 Ag2 123.5(2) . 1_455 ? N3 N4 Ag2 116.4(2) . 1_455 ? C7 N5 N6 119.7(3) . 3_756 ? C7 N5 Ag1 119.2(3) . . ? N6 N5 Ag1 118.4(2) 3_756 . ? C9 N6 N5 120.6(3) . 3_756 ? C9 N6 Ag2 120.0(3) . 1_556 ? N5 N6 Ag2 117.5(2) 3_756 1_556 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.376 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.128 #============================================================================== data_(5) _database_code_depnum_ccdc_archive 'CCDC 643964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Trifluoroacetate Complex with Pyridazino[4,5-d]pyridazine ; _chemical_name_common ;Silver(i) Trifluoroacetate Complex with Pyridazino(4,5- d)pyridazine ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H4 Ag F3 N4 O2' _chemical_formula_sum 'C8 H4 Ag F3 N4 O2' _chemical_formula_weight 353.02 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _space_group_name_Hall '-P 2ac 2n ' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.3514(2) _cell_length_b 12.5897(3) _cell_length_c 11.3054(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1046.34(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4178 _cell_measurement_theta_min 4.55 _cell_measurement_theta_max 30.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.970 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4911 _exptl_absorpt_correction_T_max 0.6732 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4178 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 30.50 _reflns_number_total 1638 _reflns_number_gt 1338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0290P)^2^+1.8500P] 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_number_reflns 1638 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.05432(4) 0.2500 0.82500(2) 0.03221(10) Uani 1 2 d S . . O1 O -0.1103(5) 0.3347(4) 1.0105(4) 0.1230(19) Uani 1 1 d . . . N1 N 0.3076(4) 0.3759(2) 0.8829(2) 0.0361(5) Uani 1 1 d . . . N2 N 0.5277(4) 0.6188(2) 1.1744(2) 0.0377(5) Uani 1 1 d . . . F1 F -0.4555(5) 0.2500 1.1093(4) 0.0896(14) Uani 1 2 d S . . F2 F -0.2712(6) 0.3332(3) 1.2200(3) 0.1276(15) Uani 1 1 d . . . C1 C 0.2823(4) 0.4307(2) 0.9797(2) 0.0351(6) Uani 1 1 d . . . H1A H 0.1677 0.4246 1.0198 0.042 Uiso 1 1 d R . . C2 C 0.4178(4) 0.4969(2) 1.0291(2) 0.0293(5) Uani 1 1 d . . . C3 C 0.3982(4) 0.5584(2) 1.1334(3) 0.0371(6) Uani 1 1 d . . . H3A H 0.2861 0.5540 1.1767 0.045 Uiso 1 1 d R . . C4 C -0.1517(7) 0.2500 1.0497(4) 0.0503(12) Uani 1 2 d S . . C5 C -0.2860(8) 0.2500 1.1536(4) 0.0515(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03684(19) 0.03435(15) 0.02545(14) 0.000 -0.00236(11) 0.000 O1 0.051(2) 0.157(4) 0.161(4) 0.103(3) 0.019(2) 0.001(2) N1 0.0351(14) 0.0399(12) 0.0333(11) -0.0069(9) -0.0039(9) -0.0056(10) N2 0.0371(15) 0.0449(13) 0.0312(11) -0.0100(10) 0.0014(10) -0.0054(10) F1 0.032(2) 0.146(4) 0.091(3) 0.000 0.0137(17) 0.000 F2 0.123(3) 0.155(3) 0.105(2) -0.087(2) 0.005(2) 0.018(3) C1 0.0286(15) 0.0411(14) 0.0356(12) -0.0060(11) 0.0010(10) -0.0036(11) C2 0.0286(14) 0.0316(11) 0.0278(10) -0.0051(9) -0.0016(9) 0.0000(9) C3 0.0338(16) 0.0454(15) 0.0322(12) -0.0122(12) 0.0063(11) -0.0044(12) C4 0.020(2) 0.086(4) 0.045(2) 0.000 -0.0027(17) 0.000 C5 0.044(3) 0.069(3) 0.042(2) 0.000 0.007(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.448(2) 8_655 ? Ag1 N2 2.448(2) 2_564 ? Ag1 N1 2.531(2) . ? Ag1 N1 2.531(2) 7_565 ? Ag1 O1 2.646(5) . ? O1 C4 1.194(4) . ? N1 C1 1.307(3) . ? N1 N2 1.374(4) 5_667 ? N2 C3 1.303(4) . ? F1 C5 1.343(7) . ? F2 C5 1.294(4) . ? C1 C2 1.414(4) . ? C2 C2 1.378(5) 5_667 ? C2 C3 1.418(4) . ? C4 O1 1.194(4) 7_565 ? C4 C5 1.535(7) . ? 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 N2 Ag1 N2 84.89(13) 8_655 2_564 ? N2 Ag1 N1 141.59(9) 8_655 . ? N2 Ag1 N1 86.47(8) 2_564 . ? N2 Ag1 N1 86.47(8) 8_655 7_565 ? N2 Ag1 N1 141.59(9) 2_564 7_565 ? N1 Ag1 N1 77.53(12) . 7_565 ? N2 Ag1 O1 135.29(12) 8_655 . ? N2 Ag1 O1 99.59(10) 2_564 . ? N1 Ag1 O1 83.07(12) . . ? N1 Ag1 O1 112.59(10) 7_565 . ? C4 O1 Ag1 92.9(4) . . ? C1 N1 N2 119.6(2) . 5_667 ? C1 N1 Ag1 116.25(19) . . ? N2 N1 Ag1 123.83(17) 5_667 . ? C3 N2 N1 120.3(2) . 5_667 ? C3 N2 Ag1 117.5(2) . 2_565 ? N1 N2 Ag1 120.78(18) 5_667 2_565 ? N1 C1 C2 122.8(3) . . ? C2 C2 C1 117.5(3) 5_667 . ? C2 C2 C3 117.1(3) 5_667 . ? C1 C2 C3 125.4(3) . . ? N2 C3 C2 122.7(3) . . ? O1 C4 O1 126.5(7) . 7_565 ? O1 C4 C5 116.6(3) . . ? O1 C4 C5 116.6(3) 7_565 . ? F2 C5 F2 108.2(6) . 7_565 ? F2 C5 F1 107.2(4) . . ? F2 C5 F1 107.2(4) 7_565 . ? F2 C5 C4 112.9(3) . . ? F2 C5 C4 112.9(3) 7_565 . ? F1 C5 C4 108.2(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.856 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.090 #============================================================================== data_(6) _database_code_depnum_ccdc_archive 'CCDC 643965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Pentafluoropropionate 2:1 Complex with Pyridazino[4,5-d]pyridazine ; _chemical_name_common ;Silver(i) Pentafluoropropionate 2:1 Complex with Pyridazino(4,5-d)pyridazine ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H4 Ag2 F10 N4 O4' _chemical_formula_sum 'C12 H4 Ag2 F10 N4 O4' _chemical_formula_weight 673.93 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' 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _space_group_name_Hall '-R 3 ' _symmetry_Int_Tables_number 148 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 25.2810(10) _cell_length_b 25.2810(10) _cell_length_c 7.4007(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4096.3(3) _cell_formula_units_Z 9 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9710 _cell_measurement_theta_min 5.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 2.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5813 _exptl_absorpt_correction_T_max 0.6636 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9710 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 5.41 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2208 _reflns_number_gt 1835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0415P)^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_number_reflns 2208 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.003 _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 0.366175(8) 0.980631(9) 0.01447(3) 0.03517(9) Uani 1 1 d . . . O1 O 0.38482(10) 0.92168(9) 0.2306(3) 0.0468(5) Uani 1 1 d . . . O2 O 0.30488(9) 0.89464(9) 0.4167(2) 0.0416(4) Uani 1 1 d . . . N1 N 0.42786(9) 0.98637(10) -0.2514(3) 0.0325(4) Uani 1 1 d . . . N2 N 0.57986(9) 0.97910(9) -0.6177(3) 0.0306(4) Uani 1 1 d . . . C1 C 0.46752(11) 0.96871(12) -0.2761(3) 0.0331(5) Uani 1 1 d . . . H1A H 0.4724 0.9459 -0.1858 0.040 Uiso 1 1 d R . . C2 C 0.50378(10) 0.98252(11) -0.4344(3) 0.0267(5) Uani 1 1 d . . . C3 C 0.54715(11) 0.96391(11) -0.4697(3) 0.0304(5) Uani 1 1 d . . . H3A H 0.5526 0.9400 -0.3845 0.036 Uiso 1 1 d R . . C4 C 0.34828(13) 0.89112(12) 0.3504(4) 0.0389(6) Uani 1 1 d . . . C5 C 0.35867(15) 0.84066(15) 0.4410(4) 0.0512(7) Uani 1 1 d . . . C6 C 0.31744(17) 0.77873(17) 0.3670(6) 0.0660(9) Uani 1 1 d . . . F1 F 0.34789(11) 0.83822(10) 0.6256(3) 0.0739(6) Uani 1 1 d . . . F2 F 0.41705(9) 0.85300(9) 0.4218(3) 0.0644(5) Uani 1 1 d . . . F3 F 0.33053(14) 0.73827(11) 0.4438(5) 0.1164(11) Uani 1 1 d . . . F4 F 0.32494(9) 0.77958(10) 0.1911(3) 0.0728(6) Uani 1 1 d . . . F5 F 0.25906(9) 0.76189(9) 0.4010(4) 0.0847(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03013(12) 0.03405(13) 0.02963(12) 0.00156(7) 0.00265(7) 0.00729(8) O1 0.0491(12) 0.0515(12) 0.0429(11) 0.0132(9) 0.0075(9) 0.0274(10) O2 0.0543(12) 0.0443(11) 0.0387(10) 0.0082(8) 0.0098(8) 0.0341(10) N1 0.0360(11) 0.0403(11) 0.0264(10) 0.0063(8) 0.0060(8) 0.0229(10) N2 0.0319(11) 0.0359(11) 0.0279(10) 0.0025(8) 0.0023(8) 0.0199(9) C1 0.0371(13) 0.0416(14) 0.0264(11) 0.0078(10) 0.0049(9) 0.0241(11) C2 0.0281(11) 0.0317(12) 0.0224(10) 0.0007(8) -0.0009(8) 0.0165(10) C3 0.0350(12) 0.0362(13) 0.0241(11) 0.0039(9) 0.0000(9) 0.0209(11) C4 0.0513(16) 0.0350(14) 0.0351(13) 0.0017(11) 0.0021(11) 0.0251(13) C5 0.0588(19) 0.0518(18) 0.0512(17) 0.0007(14) -0.0042(14) 0.0337(16) C6 0.064(2) 0.057(2) 0.080(3) 0.0019(18) 0.0092(19) 0.0323(18) F1 0.1211(19) 0.0859(14) 0.0415(10) 0.0013(10) -0.0080(11) 0.0718(14) F2 0.0502(11) 0.0574(11) 0.0958(15) -0.0187(10) -0.0207(10) 0.0345(10) F3 0.132(2) 0.0509(14) 0.189(3) 0.0190(17) 0.005(2) 0.0626(16) F4 0.0635(13) 0.0784(15) 0.0681(13) -0.0278(11) 0.0010(10) 0.0291(11) F5 0.0505(12) 0.0515(12) 0.136(2) -0.0088(12) 0.0308(13) 0.0136(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O2 2.2547(18) 8_664 ? Ag1 N2 2.2591(19) 15_554 ? Ag1 O1 2.3886(19) . ? Ag1 N1 2.4693(19) . ? Ag1 Ag1 3.1768(2) 8_664 ? Ag1 Ag1 3.1770(2) 6_465 ? O1 C4 1.234(3) . ? O2 C4 1.245(3) . ? N1 C1 1.298(3) . ? N1 N2 1.382(3) 10_674 ? N2 C3 1.309(3) . ? C1 C2 1.419(3) . ? C2 C2 1.389(4) 10_674 ? C2 C3 1.417(3) . ? C4 C5 1.575(4) . ? C5 F2 1.355(4) . ? C5 F1 1.388(4) . ? C5 C6 1.485(5) . ? C6 F4 1.314(4) . ? C6 F5 1.340(4) . ? C6 F3 1.348(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 O2 Ag1 N2 148.98(7) 8_664 15_554 ? O2 Ag1 O1 102.38(7) 8_664 . ? N2 Ag1 O1 99.02(7) 15_554 . ? O2 Ag1 N1 88.17(7) 8_664 . ? N2 Ag1 N1 107.81(7) 15_554 . ? O1 Ag1 N1 104.74(7) . . ? O2 Ag1 Ag1 79.73(5) 8_664 8_664 ? N2 Ag1 Ag1 82.86(5) 15_554 8_664 ? O1 Ag1 Ag1 170.51(5) . 8_664 ? N1 Ag1 Ag1 65.94(5) . 8_664 ? O2 Ag1 Ag1 94.67(5) 8_664 6_465 ? N2 Ag1 Ag1 69.34(5) 15_554 6_465 ? O1 Ag1 Ag1 75.36(5) . 6_465 ? N1 Ag1 Ag1 177.07(5) . 6_465 ? Ag1 Ag1 Ag1 113.858(8) 8_664 6_465 ? C4 O1 Ag1 123.53(18) . . ? C4 O2 Ag1 124.86(16) . 6_465 ? C1 N1 N2 119.71(19) . 10_674 ? C1 N1 Ag1 131.74(16) . . ? N2 N1 Ag1 108.14(13) 10_674 . ? C3 N2 N1 120.3(2) . 10_674 ? C3 N2 Ag1 123.23(16) . 14_454 ? N1 N2 Ag1 116.44(13) 10_674 14_454 ? N1 C1 C2 123.1(2) . . ? C2 C2 C3 117.3(3) 10_674 . ? C2 C2 C1 117.1(3) 10_674 . ? C3 C2 C1 125.6(2) . . ? N2 C3 C2 122.5(2) . . ? O1 C4 O2 130.5(3) . . ? O1 C4 C5 115.9(3) . . ? O2 C4 C5 113.6(2) . . ? F2 C5 F1 106.3(2) . . ? F2 C5 C6 108.3(3) . . ? F1 C5 C6 107.3(3) . . ? F2 C5 C4 111.9(3) . . ? F1 C5 C4 110.3(2) . . ? C6 C5 C4 112.6(3) . . ? F4 C6 F5 108.6(3) . . ? F4 C6 F3 110.0(3) . . ? F5 C6 F3 109.2(3) . . ? F4 C6 C5 109.2(3) . . ? F5 C6 C5 110.3(3) . . ? F3 C6 C5 109.6(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.654 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.088 #============================================================================== data_(7) _database_code_depnum_ccdc_archive 'CCDC 643966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Tetrafluoroborate 4:3 Complex with 4,4'-Bipyridazine Hydrate ; _chemical_name_common ;Silver(i) Tetrafluoroborate 4:3 Complex with 4,4'- Bipyridazine Hydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C24 H18 Ag4 N12), 4(B F4), (H2 O)' _chemical_formula_sum 'C24 H20 Ag4 B4 F16 N12 O' _chemical_formula_weight 1271.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6823(8) _cell_length_b 12.1323(7) _cell_length_c 14.6844(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.017(8) _cell_angle_gamma 90.00 _cell_volume 1888.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5.11 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6279 _exptl_absorpt_correction_T_max 0.6757 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 17163 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4457 _reflns_number_gt 3545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. One of two unique BF~4~^-^ anions shows very typical disorder of fluorine atoms, which was resolved considering equal contributions of two components of the disorder (Fluorine atoms F5-8 and F5A-8A). A set of the restraints was applied to improve the refinement stability. In this way, B---F bond lengths were constrained to 1.37 and corresponding intramolecular F...F contacts to 2.24. Also, SIMU restraints were applied for parameters for termal motion of the disordered fluorine atoms and this afforded well-refinable model. ; _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^)+(0.0682P)^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_number_reflns 4457 _refine_ls_number_parameters 316 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.41740(3) 0.57643(2) 0.15513(2) 0.03021(11) Uani 1 1 d . . . Ag2 Ag 0.61457(3) 0.39720(3) 0.08458(2) 0.03347(11) Uani 1 1 d . . . N1 N 0.4862(3) 0.4439(3) 0.2615(2) 0.0269(7) Uani 1 1 d . . . N2 N 0.5838(3) 0.3862(3) 0.2365(2) 0.0272(7) Uani 1 1 d . . . N3 N 0.8232(4) 0.0684(3) 0.5593(2) 0.0303(7) Uani 1 1 d . . . N4 N 0.8080(3) 0.0547(3) 0.4673(2) 0.0254(7) Uani 1 1 d . . . N5 N 0.5461(3) 0.2490(3) -0.0079(2) 0.0283(7) Uani 1 1 d . . . N6 N 0.5385(3) 0.2593(3) -0.0997(2) 0.0293(7) Uani 1 1 d . . . C1 C 0.4540(4) 0.4310(3) 0.3443(3) 0.0305(9) Uani 1 1 d . . . H1A H 0.3849 0.4715 0.3604 0.037 Uiso 1 1 calc R . . C2 C 0.5166(4) 0.3605(3) 0.4097(3) 0.0294(8) Uani 1 1 d . . . H2A H 0.4910 0.3535 0.4684 0.035 Uiso 1 1 calc R . . C3 C 0.6176(4) 0.3012(3) 0.3853(3) 0.0244(8) Uani 1 1 d . . . C4 C 0.6475(4) 0.3180(3) 0.2958(3) 0.0273(8) Uani 1 1 d . . . H4A H 0.7160 0.2791 0.2771 0.033 Uiso 1 1 calc R . . C5 C 0.7733(5) 0.1555(4) 0.5953(3) 0.0352(10) Uani 1 1 d . . . H5A H 0.7845 0.1639 0.6594 0.042 Uiso 1 1 calc R . . C6 C 0.7046(4) 0.2353(4) 0.5419(3) 0.0331(9) Uani 1 1 d . . . H6A H 0.6700 0.2962 0.5695 0.040 Uiso 1 1 calc R . . C7 C 0.6887(4) 0.2230(3) 0.4480(3) 0.0249(8) Uani 1 1 d . . . C8 C 0.7435(4) 0.1278(3) 0.4138(3) 0.0255(8) Uani 1 1 d . . . H8A H 0.7336 0.1159 0.3500 0.031 Uiso 1 1 calc R . . C9 C 0.5321(4) 0.1506(3) 0.0284(3) 0.0292(8) Uani 1 1 d . . . H9A H 0.5400 0.1451 0.0927 0.035 Uiso 1 1 calc R . . C10 C 0.5064(4) 0.0538(3) -0.0229(3) 0.0274(8) Uani 1 1 d . . . C11 C 0.4938(7) 0.0670(4) -0.1170(4) 0.0528(15) Uani 1 1 d . . . H11A H 0.4737 0.0070 -0.1565 0.063 Uiso 1 1 calc R . . C12 C 0.5118(6) 0.1714(4) -0.1513(3) 0.0472(13) Uani 1 1 d . . . H12A H 0.5045 0.1802 -0.2154 0.057 Uiso 1 1 calc R . . B1 B 0.8549(6) 0.1755(6) 0.1340(4) 0.0493(15) Uani 1 1 d . . . F1 F 0.8145(4) 0.2841(4) 0.1269(3) 0.0885(14) Uani 1 1 d . . . F2 F 0.8201(4) 0.1178(5) 0.0534(3) 0.0905(15) Uani 1 1 d . . . F3 F 0.8025(4) 0.1274(4) 0.2048(3) 0.0816(13) Uani 1 1 d . . . F4 F 0.9859(3) 0.1729(3) 0.1516(3) 0.0608(9) Uani 1 1 d . . . B2 B 0.1313(5) 0.6080(5) 0.2180(5) 0.0609(19) Uani 1 1 d D . . F5 F 0.0167(6) 0.6284(8) 0.2462(6) 0.077(2) Uani 0.50 1 d PDU . . F6 F 0.1688(10) 0.5028(6) 0.2282(8) 0.110(3) Uani 0.50 1 d PDU . . F7 F 0.2177(9) 0.6883(8) 0.2245(7) 0.112(3) Uani 0.50 1 d PDU . . F8 F 0.0859(11) 0.6029(10) 0.1185(5) 0.128(3) Uani 0.50 1 d PDU . . F5A F 0.0701(8) 0.6725(7) 0.2781(6) 0.075(3) Uani 0.50 1 d PDU . . F6A F 0.2137(9) 0.5456(8) 0.2717(8) 0.119(4) Uani 0.50 1 d PDU . . F7A F 0.1926(9) 0.6747(9) 0.1627(7) 0.113(3) Uani 0.50 1 d PDU . . F8A F 0.0427(9) 0.5542(9) 0.1605(7) 0.121(3) Uani 0.50 1 d PDU . . O1 O 0.0374(14) 0.5648(13) -0.0246(13) 0.123(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04144(19) 0.01821(15) 0.03073(19) 0.00526(11) 0.00342(13) -0.00005(11) Ag2 0.0496(2) 0.02651(17) 0.02537(19) 0.00134(11) 0.00896(14) -0.00839(13) N1 0.0320(17) 0.0220(15) 0.0263(18) 0.0022(13) 0.0028(14) 0.0062(13) N2 0.0359(18) 0.0247(16) 0.0218(17) 0.0033(13) 0.0064(14) 0.0046(13) N3 0.0396(19) 0.0279(17) 0.0227(18) 0.0003(13) 0.0014(15) 0.0076(14) N4 0.0306(17) 0.0242(16) 0.0212(17) 0.0003(12) 0.0027(13) 0.0018(12) N5 0.0381(18) 0.0204(15) 0.0273(19) 0.0013(13) 0.0068(15) -0.0029(13) N6 0.0403(19) 0.0193(15) 0.0289(19) 0.0035(13) 0.0071(15) 0.0004(13) C1 0.032(2) 0.031(2) 0.029(2) 0.0015(16) 0.0072(17) 0.0105(16) C2 0.033(2) 0.032(2) 0.025(2) 0.0048(16) 0.0095(17) 0.0081(16) C3 0.0285(19) 0.0235(17) 0.0213(19) 0.0016(14) 0.0027(15) 0.0031(14) C4 0.033(2) 0.0259(19) 0.024(2) 0.0014(15) 0.0072(16) 0.0058(15) C5 0.046(3) 0.038(2) 0.022(2) -0.0013(17) 0.0050(18) 0.0134(19) C6 0.043(2) 0.032(2) 0.025(2) -0.0019(16) 0.0068(18) 0.0159(18) C7 0.0274(18) 0.0235(17) 0.024(2) 0.0025(15) 0.0045(15) 0.0034(14) C8 0.033(2) 0.0245(18) 0.0193(19) -0.0003(14) 0.0039(15) 0.0046(15) C9 0.042(2) 0.0231(18) 0.023(2) 0.0013(15) 0.0050(17) -0.0042(16) C10 0.037(2) 0.0193(18) 0.027(2) 0.0024(15) 0.0076(17) -0.0005(15) C11 0.107(5) 0.023(2) 0.028(3) -0.0050(18) 0.010(3) -0.009(2) C12 0.091(4) 0.027(2) 0.024(2) 0.0001(17) 0.006(2) -0.003(2) B1 0.047(3) 0.064(4) 0.039(3) 0.000(3) 0.015(3) 0.020(3) F1 0.085(3) 0.090(3) 0.094(3) 0.027(3) 0.027(2) 0.053(2) F2 0.073(3) 0.138(4) 0.064(3) -0.036(3) 0.020(2) -0.002(3) F3 0.097(3) 0.084(3) 0.076(3) 0.011(2) 0.060(3) 0.024(2) F4 0.0510(19) 0.0550(19) 0.078(3) 0.0090(17) 0.0161(17) 0.0148(15) B2 0.037(3) 0.064(4) 0.082(6) -0.005(4) 0.007(3) 0.014(3) F5 0.064(5) 0.082(5) 0.092(5) 0.041(4) 0.043(4) 0.034(4) F6 0.103(6) 0.100(6) 0.132(7) 0.006(5) 0.039(5) 0.051(5) F7 0.109(6) 0.125(6) 0.115(8) 0.016(7) 0.068(6) 0.001(5) F8 0.139(6) 0.132(6) 0.120(6) 0.024(5) 0.047(5) 0.017(5) F5A 0.085(6) 0.064(5) 0.086(6) 0.013(4) 0.051(5) 0.031(4) F6A 0.080(6) 0.116(7) 0.157(8) 0.052(6) -0.006(6) 0.049(5) F7A 0.110(5) 0.125(6) 0.117(7) 0.043(6) 0.073(6) 0.021(4) F8A 0.120(5) 0.123(5) 0.123(5) 0.015(4) 0.030(5) 0.011(4) O1 0.098(10) 0.114(11) 0.156(15) 0.001(10) 0.011(10) 0.033(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6 2.225(3) 3_665 ? Ag1 N1 2.299(3) . ? Ag1 N3 2.395(3) 4_565 ? Ag1 Ag2 3.2820(5) . ? Ag2 N4 2.252(3) 2_655 ? Ag2 N2 2.298(3) . ? Ag2 N5 2.317(3) . ? Ag2 F1 2.550(4) . ? N1 C1 1.313(6) . ? N1 N2 1.344(5) . ? N2 C4 1.327(5) . ? N3 C5 1.322(6) . ? N3 N4 1.350(5) . ? N4 C8 1.322(5) . ? N5 C9 1.324(5) . ? N5 N6 1.346(5) . ? N6 C12 1.319(6) . ? C1 C2 1.394(6) . ? C2 C3 1.379(5) . ? C3 C4 1.404(6) . ? C3 C7 1.468(5) . ? C5 C6 1.397(6) . ? C6 C7 1.377(6) . ? C7 C8 1.414(5) . ? C9 C10 1.404(6) . ? C10 C11 1.381(7) . ? C10 C10 1.482(7) 3_655 ? C11 C12 1.385(7) . ? B1 F3 1.370(7) . ? B1 F1 1.386(8) . ? B1 F2 1.387(8) . ? B1 F4 1.392(8) . ? B2 F7 1.337(8) . ? B2 F6 1.341(8) . ? B2 F6A 1.343(8) . ? B2 F8A 1.356(8) . ? B2 F5 1.362(7) . ? B2 F7A 1.368(8) . ? B2 F5A 1.400(7) . ? B2 F8 1.483(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 N6 Ag1 N1 144.16(13) 3_665 . ? N6 Ag1 N3 122.34(13) 3_665 4_565 ? N1 Ag1 N3 87.85(13) . 4_565 ? N6 Ag1 Ag2 107.76(9) 3_665 . ? N1 Ag1 Ag2 65.60(8) . . ? N3 Ag1 Ag2 64.40(9) 4_565 . ? N4 Ag2 N2 118.70(12) 2_655 . ? N4 Ag2 N5 124.24(12) 2_655 . ? N2 Ag2 N5 116.83(12) . . ? N4 Ag2 F1 102.00(15) 2_655 . ? N2 Ag2 F1 86.98(14) . . ? N5 Ag2 F1 85.42(16) . . ? N4 Ag2 Ag1 79.69(9) 2_655 . ? N2 Ag2 Ag1 63.81(8) . . ? N5 Ag2 Ag1 122.03(9) . . ? F1 Ag2 Ag1 146.12(12) . . ? C1 N1 N2 119.4(3) . . ? C1 N1 Ag1 127.9(3) . . ? N2 N1 Ag1 111.9(2) . . ? C4 N2 N1 119.9(3) . . ? C4 N2 Ag2 123.4(3) . . ? N1 N2 Ag2 116.3(3) . . ? C5 N3 N4 119.5(4) . . ? C5 N3 Ag1 120.8(3) . 4_666 ? N4 N3 Ag1 119.2(2) . 4_666 ? C8 N4 N3 120.2(3) . . ? C8 N4 Ag2 123.6(3) . 2_645 ? N3 N4 Ag2 116.0(2) . 2_645 ? C9 N5 N6 119.4(3) . . ? C9 N5 Ag2 120.4(3) . . ? N6 N5 Ag2 119.4(2) . . ? C12 N6 N5 118.9(3) . . ? C12 N6 Ag1 123.7(3) . 3_665 ? N5 N6 Ag1 117.4(2) . 3_665 ? N1 C1 C2 123.5(4) . . ? C3 C2 C1 117.8(4) . . ? C2 C3 C4 116.2(4) . . ? C2 C3 C7 122.4(4) . . ? C4 C3 C7 121.4(3) . . ? N2 C4 C3 123.2(4) . . ? N3 C5 C6 122.7(4) . . ? C7 C6 C5 118.6(4) . . ? C6 C7 C8 116.1(4) . . ? C6 C7 C3 123.3(3) . . ? C8 C7 C3 120.7(4) . . ? N4 C8 C7 123.0(4) . . ? N5 C9 C10 124.2(4) . . ? C11 C10 C9 115.4(4) . . ? C11 C10 C10 123.6(5) . 3_655 ? C9 C10 C10 121.1(5) . 3_655 ? C10 C11 C12 118.0(4) . . ? N6 C12 C11 124.0(5) . . ? F3 B1 F1 108.0(4) . . ? F3 B1 F2 109.9(6) . . ? F1 B1 F2 111.5(6) . . ? F3 B1 F4 110.2(5) . . ? F1 B1 F4 109.4(6) . . ? F2 B1 F4 107.8(4) . . ? B1 F1 Ag2 140.7(4) . . ? F7 B2 F6 119.4(7) . . ? F6A B2 F8A 116.8(7) . . ? F7 B2 F5 119.0(7) . . ? F6 B2 F5 114.0(7) . . ? F6A B2 F7A 110.8(7) . . ? F8A B2 F7A 105.3(6) . . ? F6A B2 F5A 105.6(7) . . ? F8A B2 F5A 108.5(6) . . ? F7A B2 F5A 109.7(7) . . ? F7 B2 F8 103.9(6) . . ? F6 B2 F8 97.3(6) . . ? F5 B2 F8 96.3(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.202 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.129 #============================================================================== data_(8) _database_code_depnum_ccdc_archive 'CCDC 643967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Hexafluorosilicate 2:3 Complex with 4,4'-Bipyridazine, Trihydrate ; _chemical_name_common ;Silver(i) Hexafluorosilicate 2:3 Complex with 4,4'- Bipyridazine, Trihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Ag4 N12 O2, 2(F6 Si), H2 O' _chemical_formula_sum 'C24 H24 Ag4 F12 N12 O3 Si2' _chemical_formula_weight 1244.21 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 7.7384(2) _cell_length_b 38.1690(8) _cell_length_c 50.8067(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15006.6(6) _cell_formula_units_Z 16 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 18785 _cell_measurement_theta_min 3.84 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9600 _exptl_absorpt_coefficient_mu 2.229 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5831 _exptl_absorpt_correction_T_max 0.7025 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 18785 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 67 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4586 _reflns_number_gt 3893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0725P)^2^+181.1421P] 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_number_reflns 4586 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.004 _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 0.53320(6) 0.266956(10) 1.030621(7) 0.04417(14) Uani 1 1 d . . . Ag2 Ag 0.53118(6) 0.215348(10) 0.973613(7) 0.04605(15) Uani 1 1 d . . . Si1 Si 0.3750 0.27263(4) 0.8750 0.0287(3) Uani 1 2 d S . . Si2 Si 0.1250 0.1250 0.94105(4) 0.0367(4) Uani 1 2 d S . . F1 F 0.5849(8) 0.26923(18) 0.88631(13) 0.1124(19) Uani 1 1 d . . . F2 F 0.3273(10) 0.2400(2) 0.89775(16) 0.141(3) Uani 1 1 d . . . F3 F 0.3333(11) 0.30495(19) 0.89698(12) 0.134(2) Uani 1 1 d . . . F4 F 0.1880(7) 0.15315(13) 0.96476(9) 0.0889(14) Uani 1 1 d . . . F5 F 0.1842(5) 0.15407(11) 0.91866(8) 0.0671(10) Uani 1 1 d . . . F6 F -0.0734(5) 0.14198(13) 0.94159(12) 0.0933(16) Uani 1 1 d . . . O1 O 0.2536(5) 0.22034(11) 0.94741(11) 0.0604(12) Uani 1 1 d . . . H1 H 0.2768 0.2294 0.9313 0.091 Uiso 1 1 d . . . H2 H 0.2389 0.1991 0.9432 0.091 Uiso 1 1 d . . . O2 O 0.6250 0.1250 0.96404(12) 0.0650(16) Uani 1 2 d S . . H3 H 0.5235 0.1200 0.9539 0.097 Uiso 1 1 d . . . N1 N 0.5652(5) 0.29650(10) 0.99217(8) 0.0366(8) Uani 1 1 d . . . N2 N 0.5737(6) 0.27645(11) 0.97044(8) 0.0418(9) Uani 1 1 d . . . N3 N 0.7161(6) 0.43933(10) 0.98881(8) 0.0391(9) Uani 1 1 d . . . N4 N 0.7010(6) 0.45815(10) 0.96705(8) 0.0433(10) Uani 1 1 d . . . N5 N 0.6642(5) 0.20147(10) 0.93535(7) 0.0359(8) Uani 1 1 d . . . N6 N 0.8212(5) 0.21601(10) 0.93217(7) 0.0357(8) Uani 1 1 d . . . C1 C 0.5917(10) 0.29230(14) 0.94700(10) 0.0541(15) Uani 1 1 d . . . H1A H 0.5914 0.2785 0.9319 0.065 Uiso 1 1 calc R . . C2 C 0.6107(9) 0.32834(13) 0.94423(10) 0.0492(13) Uani 1 1 d . . . H2A H 0.6258 0.3384 0.9277 0.059 Uiso 1 1 calc R . . C3 C 0.6066(6) 0.34860(11) 0.96663(9) 0.0347(9) Uani 1 1 d . . . C4 C 0.5803(7) 0.33100(12) 0.99043(9) 0.0378(10) Uani 1 1 d . . . H4A H 0.5730 0.3442 1.0058 0.045 Uiso 1 1 calc R . . C5 C 0.6466(12) 0.44254(15) 0.94526(12) 0.068(2) Uani 1 1 d . . . H5A H 0.6314 0.4562 0.9303 0.081 Uiso 1 1 calc R . . C6 C 0.6110(11) 0.40680(14) 0.94361(11) 0.0629(18) Uani 1 1 d . . . H6A H 0.5743 0.3967 0.9279 0.075 Uiso 1 1 calc R . . C7 C 0.6319(6) 0.38708(11) 0.96590(9) 0.0340(9) Uani 1 1 d . . . C8 C 0.6822(8) 0.40521(12) 0.98821(10) 0.0428(11) Uani 1 1 d . . . H8A H 0.6930 0.3927 1.0038 0.051 Uiso 1 1 calc R . . C9 C 0.5921(7) 0.18441(14) 0.91546(9) 0.0399(10) Uani 1 1 d . . . H9A H 0.4847 0.1741 0.9181 0.048 Uiso 1 1 calc R . . C10 C 0.6687(7) 0.18124(14) 0.89094(9) 0.0407(10) Uani 1 1 d . . . H10A H 0.6136 0.1696 0.8772 0.049 Uiso 1 1 calc R . . C11 C 0.8276(6) 0.19586(12) 0.88767(8) 0.0338(9) Uani 1 1 d . . . C12 C 0.9007(6) 0.21293(13) 0.90923(9) 0.0360(9) Uani 1 1 d . . . H12A H 1.0103 0.2226 0.9074 0.043 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 0.0625(3) 0.0406(2) 0.0294(2) -0.00392(14) 0.00290(16) -0.01108(17) Ag2 0.0654(3) 0.0434(2) 0.0294(2) 0.00032(14) 0.01209(16) -0.00663(18) Si1 0.0341(8) 0.0398(8) 0.0120(6) 0.000 0.0011(6) 0.000 Si2 0.0331(9) 0.0392(9) 0.0379(9) 0.000 0.000 -0.0013(7) F1 0.081(3) 0.139(5) 0.117(5) -0.015(4) -0.012(3) -0.011(3) F2 0.130(5) 0.133(5) 0.159(6) 0.090(5) -0.026(5) -0.016(4) F3 0.184(7) 0.134(5) 0.084(4) -0.040(4) 0.015(4) 0.024(5) F4 0.115(4) 0.088(3) 0.064(3) -0.033(2) 0.002(2) -0.029(3) F5 0.072(2) 0.071(2) 0.058(2) 0.0178(18) 0.0022(18) -0.0227(19) F6 0.0404(19) 0.083(3) 0.157(5) 0.018(3) 0.023(3) 0.0152(19) O1 0.043(2) 0.052(2) 0.086(3) -0.020(2) 0.000(2) -0.0030(17) O2 0.055(4) 0.093(5) 0.048(3) 0.000 0.000 -0.010(3) N1 0.047(2) 0.0298(17) 0.0333(19) -0.0050(15) 0.0051(16) -0.0066(16) N2 0.062(3) 0.0348(19) 0.0287(19) -0.0042(15) 0.0040(18) -0.0049(18) N3 0.055(2) 0.0312(18) 0.0314(19) 0.0015(15) -0.0077(17) -0.0069(17) N4 0.065(3) 0.0312(18) 0.034(2) 0.0045(15) -0.0106(19) -0.0088(18) N5 0.040(2) 0.0396(19) 0.0285(18) -0.0005(15) 0.0058(15) -0.0010(16) N6 0.041(2) 0.0394(19) 0.0268(18) -0.0028(15) 0.0009(15) -0.0008(16) C1 0.097(5) 0.035(2) 0.030(2) -0.0047(19) -0.004(3) -0.004(3) C2 0.083(4) 0.036(2) 0.028(2) 0.0019(18) -0.001(2) -0.006(3) C3 0.038(2) 0.0285(19) 0.037(2) -0.0028(17) -0.0035(18) -0.0040(17) C4 0.048(3) 0.033(2) 0.033(2) -0.0039(17) 0.0014(19) -0.0051(19) C5 0.125(6) 0.040(3) 0.038(3) 0.011(2) -0.025(3) -0.013(3) C6 0.116(6) 0.039(3) 0.034(3) 0.001(2) -0.026(3) -0.015(3) C7 0.043(2) 0.0291(19) 0.030(2) 0.0010(16) -0.0062(18) -0.0035(18) C8 0.068(3) 0.031(2) 0.030(2) 0.0018(17) -0.007(2) -0.006(2) C9 0.039(2) 0.049(3) 0.032(2) -0.0046(19) 0.0054(19) -0.006(2) C10 0.041(2) 0.055(3) 0.027(2) -0.0085(19) -0.0012(18) -0.002(2) C11 0.036(2) 0.044(2) 0.0216(19) -0.0015(16) 0.0031(17) 0.0049(18) C12 0.032(2) 0.050(2) 0.027(2) 0.0026(18) 0.0037(17) -0.0043(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 Ag1 N1 2.269(4) . ? Ag1 N6 2.295(4) 29_657 ? Ag1 N4 2.336(4) 30_557 ? Ag1 O1 2.531(4) 29_557 ? Ag2 N3 2.210(4) 30_557 ? Ag2 N5 2.263(4) . ? Ag2 N2 2.361(4) . ? Ag2 O1 2.534(5) . ? Si1 F3 1.695(6) . ? Si1 F3 1.695(6) 3_556 ? Si1 F1 1.728(6) . ? Si1 F1 1.728(6) 3_556 ? Si1 F2 1.740(6) . ? Si1 F2 1.740(6) 3_556 ? Si2 F5 1.654(4) 14_445 ? Si2 F5 1.654(4) . ? Si2 F6 1.667(4) 14_445 ? Si2 F6 1.667(4) . ? Si2 F4 1.686(4) . ? Si2 F4 1.686(4) 14_445 ? O1 Ag1 2.531(4) 29_557 ? N1 C4 1.325(6) . ? N1 N2 1.345(5) . ? N2 C1 1.343(7) . ? N3 N4 1.324(6) . ? N3 C8 1.329(6) . ? N3 Ag2 2.210(4) 18_667 ? N4 C5 1.326(7) . ? N4 Ag1 2.336(4) 18_667 ? N5 C9 1.325(6) . ? N5 N6 1.345(6) . ? N6 C12 1.323(6) . ? N6 Ag1 2.295(4) 29_657 ? C1 C2 1.390(7) . ? C2 C3 1.376(7) . ? C3 C4 1.398(7) . ? C3 C7 1.482(6) . ? C5 C6 1.394(8) . ? C6 C7 1.370(7) . ? C7 C8 1.384(6) . ? C9 C10 1.385(6) . ? C10 C11 1.360(7) . ? C11 C12 1.394(6) . ? C11 C11 1.482(8) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 120.99(14) . 29_657 ? N1 Ag1 N4 123.43(14) . 30_557 ? N6 Ag1 N4 111.35(15) 29_657 30_557 ? N1 Ag1 O1 112.33(16) . 29_557 ? N6 Ag1 O1 90.74(15) 29_657 29_557 ? N4 Ag1 O1 85.59(15) 30_557 29_557 ? N3 Ag2 N5 137.79(15) 30_557 . ? N3 Ag2 N2 122.31(14) 30_557 . ? N5 Ag2 N2 96.27(14) . . ? N3 Ag2 O1 107.12(17) 30_557 . ? N5 Ag2 O1 87.24(15) . . ? N2 Ag2 O1 90.47(15) . . ? F3 Si1 F3 86.6(5) . 3_556 ? F3 Si1 F1 90.8(4) . . ? F3 Si1 F1 95.4(4) 3_556 . ? F3 Si1 F1 95.4(4) . 3_556 ? F3 Si1 F1 90.8(4) 3_556 3_556 ? F1 Si1 F1 171.4(5) . 3_556 ? F3 Si1 F2 92.5(4) . . ? F3 Si1 F2 178.6(4) 3_556 . ? F1 Si1 F2 85.7(3) . . ? F1 Si1 F2 88.1(3) 3_556 . ? F3 Si1 F2 178.6(4) . 3_556 ? F3 Si1 F2 92.5(4) 3_556 3_556 ? F1 Si1 F2 88.1(3) . 3_556 ? F1 Si1 F2 85.7(3) 3_556 3_556 ? F2 Si1 F2 88.4(7) . 3_556 ? F5 Si2 F5 93.1(3) 14_445 . ? F5 Si2 F6 90.3(2) 14_445 14_445 ? F5 Si2 F6 91.0(3) . 14_445 ? F5 Si2 F6 91.0(3) 14_445 . ? F5 Si2 F6 90.3(2) . . ? F6 Si2 F6 178.1(4) 14_445 . ? F5 Si2 F4 177.4(3) 14_445 . ? F5 Si2 F4 89.1(2) . . ? F6 Si2 F4 88.3(3) 14_445 . ? F6 Si2 F4 90.4(3) . . ? F5 Si2 F4 89.1(2) 14_445 14_445 ? F5 Si2 F4 177.4(3) . 14_445 ? F6 Si2 F4 90.4(3) 14_445 14_445 ? F6 Si2 F4 88.3(3) . 14_445 ? F4 Si2 F4 88.8(4) . 14_445 ? Ag1 O1 Ag2 121.7(2) 29_557 . ? C4 N1 N2 120.4(4) . . ? C4 N1 Ag1 124.1(3) . . ? N2 N1 Ag1 115.4(3) . . ? C1 N2 N1 118.5(4) . . ? C1 N2 Ag2 121.3(3) . . ? N1 N2 Ag2 119.9(3) . . ? N4 N3 C8 119.7(4) . . ? N4 N3 Ag2 119.9(3) . 18_667 ? C8 N3 Ag2 120.3(3) . 18_667 ? N3 N4 C5 118.8(4) . . ? N3 N4 Ag1 117.1(3) . 18_667 ? C5 N4 Ag1 124.1(3) . 18_667 ? C9 N5 N6 119.4(4) . . ? C9 N5 Ag2 125.4(3) . . ? N6 N5 Ag2 114.7(3) . . ? C12 N6 N5 119.3(4) . . ? C12 N6 Ag1 121.5(3) . 29_657 ? N5 N6 Ag1 117.5(3) . 29_657 ? N2 C1 C2 123.1(5) . . ? C3 C2 C1 118.0(5) . . ? C2 C3 C4 116.7(4) . . ? C2 C3 C7 122.2(4) . . ? C4 C3 C7 121.1(4) . . ? N1 C4 C3 123.3(4) . . ? N4 C5 C6 123.5(5) . . ? C7 C6 C5 117.7(5) . . ? C6 C7 C8 115.8(4) . . ? C6 C7 C3 123.3(4) . . ? C8 C7 C3 120.8(4) . . ? N3 C8 C7 124.4(4) . . ? N5 C9 C10 123.3(5) . . ? C11 C10 C9 117.4(4) . . ? C10 C11 C12 117.6(4) . . ? C10 C11 C11 123.6(5) . 3_656 ? C12 C11 C11 118.8(5) . 3_656 ? N6 C12 C11 123.0(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.203 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.132 #============================================================================== data_(9) _database_code_depnum_ccdc_archive 'CCDC 643968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Trifluoromethylsulfonate Complex with 4,4'-Bipyridazine, Solvate with 2/3 Water ; _chemical_name_common ; Silver(i) Trifluoromethylsulfonate Complex with 4,4'- Bipyridazine, Solvate with 2/3 Water ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Ag3 N12 O, 3(C F3 O3 S), H2 O' _chemical_formula_sum 'C27 H22 Ag3 F9 N12 O11 S3' _chemical_formula_weight 1281.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21 ' _space_group_name_Hall 'P 2yb ' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7652(6) _cell_length_b 22.1004(15) _cell_length_c 10.4417(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.8740(10) _cell_angle_gamma 90.00 _cell_volume 2021.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 10521 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 29.02 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 1.707 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7486 _exptl_absorpt_correction_T_max 0.7960 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 17561 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 29.02 _reflns_number_total 10521 _reflns_number_gt 8301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0316P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(12) _refine_ls_number_reflns 10521 _refine_ls_number_parameters 586 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Ag1 Ag 0.34332(2) 0.803470(7) 0.51196(2) 0.02943(5) Uani 1 1 d . . . Ag2 Ag 0.25102(2) 0.707808(10) 0.756727(17) 0.02673(5) Uani 1 1 d . . . Ag3 Ag 0.17730(2) 0.795840(6) 1.01653(2) 0.02930(5) Uani 1 1 d . . . S1 S 0.48847(9) 0.53751(3) 0.96002(7) 0.03275(16) Uani 1 1 d . . . S2 S 0.98949(9) 0.54006(3) 0.53371(6) 0.03162(16) Uani 1 1 d . . . S3 S -0.18853(9) 0.79606(4) 0.34953(7) 0.03798(16) Uani 1 1 d . . . F1 F 0.6590(4) 0.62484(16) 0.8791(4) 0.1173(13) Uani 1 1 d . . . F2 F 0.6928(3) 0.60390(13) 1.0775(3) 0.0960(11) Uani 1 1 d . . . F3 F 0.4931(3) 0.65268(10) 1.0123(3) 0.0862(9) Uani 1 1 d . . . F4 F 0.8128(3) 0.61871(12) 0.4156(3) 0.0787(8) Uani 1 1 d . . . F5 F 1.0259(3) 0.65394(11) 0.4852(3) 0.0884(9) Uani 1 1 d . . . F6 F 0.8475(4) 0.63545(15) 0.6151(3) 0.1060(11) Uani 1 1 d . . . F7 F -0.4210(3) 0.79138(15) 0.1866(3) 0.0911(9) Uani 1 1 d . . . F8 F -0.2037(3) 0.78220(14) 0.1004(2) 0.0781(8) Uani 1 1 d . . . F9 F -0.2987(3) 0.70872(12) 0.2085(2) 0.0825(8) Uani 1 1 d . . . O1 O 0.2322(2) 0.80915(10) 1.26325(17) 0.0390(5) Uani 1 1 d . . . H1 H 0.1387 0.7973 1.2962 0.058 Uiso 1 1 d . . . H2 H 0.2455 0.8495 1.2541 0.058 Uiso 1 1 d . . . O2 O 0.6095(3) 0.49491(11) 0.9391(3) 0.0561(7) Uani 1 1 d . . . O3 O 0.4134(3) 0.52897(13) 1.0790(2) 0.0543(7) Uani 1 1 d . . . O4 O 0.3886(3) 0.54795(12) 0.8520(2) 0.0504(6) Uani 1 1 d . . . O5 O 1.0953(3) 0.54618(11) 0.6407(2) 0.0449(6) Uani 1 1 d . . . O6 O 0.8574(3) 0.50413(12) 0.5561(3) 0.0626(8) Uani 1 1 d . . . O7 O 1.0582(3) 0.52741(11) 0.4133(2) 0.0528(7) Uani 1 1 d . . . O8 O -0.1786(3) 0.86036(10) 0.3296(3) 0.0565(7) Uani 1 1 d . . . O9 O -0.0425(3) 0.76661(11) 0.3483(3) 0.0549(7) Uani 1 1 d . . . O10 O -0.2895(3) 0.77788(11) 0.4471(2) 0.0573(7) Uani 1 1 d . . . O11 O 0.2664(3) 0.92981(13) 1.2588(2) 0.0560(7) Uani 1 1 d . . . H3 H 0.2932 0.9560 1.2044 0.084 Uiso 1 1 d . . . H4 H 0.2118 0.9534 1.3110 0.084 Uiso 1 1 d . . . N1 N 0.3731(3) 0.70413(9) 0.4793(2) 0.0247(4) Uani 1 1 d . . . N2 N 0.3732(3) 0.66854(9) 0.5847(2) 0.0257(5) Uani 1 1 d . . . N3 N 0.5545(3) 0.39579(9) 0.4629(2) 0.0283(5) Uani 1 1 d . . . N4 N 0.6042(3) 0.43221(10) 0.3694(2) 0.0319(6) Uani 1 1 d . . . N5 N 0.1141(3) 0.82542(10) 0.6224(2) 0.0281(5) Uani 1 1 d . . . N6 N 0.0631(3) 0.77886(10) 0.6922(2) 0.0286(5) Uani 1 1 d . . . N7 N -0.5494(3) 0.77395(10) 0.8260(2) 0.0293(5) Uani 1 1 d . . . N8 N -0.6008(3) 0.81906(10) 0.9018(2) 0.0292(5) Uani 1 1 d . . . N9 N 0.1249(3) 0.66478(9) 0.9221(2) 0.0262(5) Uani 1 1 d . . . N10 N 0.1226(3) 0.69635(9) 1.0331(2) 0.0260(5) Uani 1 1 d . . . N11 N -0.0643(3) 0.38783(10) 1.0062(2) 0.0275(5) Uani 1 1 d . . . N12 N -0.1106(3) 0.42100(10) 1.1059(2) 0.0300(5) Uani 1 1 d . . . C1 C 0.4029(3) 0.61020(11) 0.5751(3) 0.0265(6) Uani 1 1 d . . . H1A H 0.4044 0.5868 0.6503 0.032 Uiso 1 1 calc R . . C2 C 0.4325(3) 0.58104(11) 0.4587(3) 0.0234(5) Uani 1 1 d . . . C3 C 0.4271(3) 0.61687(11) 0.3513(3) 0.0307(6) Uani 1 1 d . . . H3A H 0.4416 0.6002 0.2697 0.037 Uiso 1 1 calc R . . C4 C 0.3995(3) 0.67893(11) 0.3664(3) 0.0291(6) Uani 1 1 d . . . H4A H 0.3995 0.7039 0.2934 0.035 Uiso 1 1 calc R . . C5 C 0.5617(4) 0.48944(12) 0.3682(3) 0.0308(6) Uani 1 1 d . . . H5A H 0.5965 0.5143 0.3022 0.037 Uiso 1 1 calc R . . C6 C 0.4679(3) 0.51562(10) 0.4593(3) 0.0240(5) Uani 1 1 d . . . C7 C 0.4151(3) 0.47784(12) 0.5520(3) 0.0331(6) Uani 1 1 d . . . H7A H 0.3489 0.4918 0.6145 0.040 Uiso 1 1 calc R . . C8 C 0.4638(4) 0.41756(12) 0.5498(3) 0.0344(7) Uani 1 1 d . . . H8A H 0.4299 0.3912 0.6136 0.041 Uiso 1 1 calc R . . C9 C 0.0285(3) 0.87444(11) 0.6085(3) 0.0302(6) Uani 1 1 d . . . H9A H 0.0668 0.9070 0.5613 0.036 Uiso 1 1 calc R . . C10 C -0.1152(3) 0.88040(12) 0.6597(3) 0.0307(6) Uani 1 1 d . . . H10A H -0.1722 0.9162 0.6486 0.037 Uiso 1 1 calc R . . C11 C -0.1714(3) 0.83226(12) 0.7272(3) 0.0256(5) Uani 1 1 d . . . C12 C -0.0737(3) 0.78222(12) 0.7418(3) 0.0301(6) Uani 1 1 d . . . H12A H -0.1075 0.7491 0.7897 0.036 Uiso 1 1 calc R . . C13 C -0.4167(3) 0.77984(12) 0.7710(3) 0.0298(6) Uani 1 1 d . . . H13A H -0.3833 0.7481 0.7190 0.036 Uiso 1 1 calc R . . C14 C -0.3224(3) 0.83111(11) 0.7861(3) 0.0253(5) Uani 1 1 d . . . C15 C -0.3786(3) 0.87780(12) 0.8569(3) 0.0317(6) Uani 1 1 d . . . H15A H -0.3242 0.9142 0.8671 0.038 Uiso 1 1 calc R . . C16 C -0.5194(3) 0.86948(12) 0.9134(3) 0.0340(7) Uani 1 1 d . . . H16A H -0.5584 0.9013 0.9622 0.041 Uiso 1 1 calc R . . C17 C 0.0902(3) 0.60634(11) 0.9215(2) 0.0247(6) Uani 1 1 d . . . H17A H 0.0895 0.5856 0.8429 0.030 Uiso 1 1 calc R . . C18 C 0.0547(3) 0.57376(10) 1.0320(2) 0.0221(5) Uani 1 1 d . . . C19 C 0.0554(3) 0.60556(11) 1.1448(3) 0.0283(6) Uani 1 1 d . . . H19A H 0.0353 0.5864 1.2228 0.034 Uiso 1 1 calc R . . C20 C 0.0871(3) 0.66761(11) 1.1399(3) 0.0293(6) Uani 1 1 d . . . H20A H 0.0831 0.6901 1.2162 0.035 Uiso 1 1 calc R . . C21 C 0.0207(4) 0.41280(11) 0.9187(3) 0.0317(6) Uani 1 1 d . . . H21A H 0.0519 0.3886 0.8503 0.038 Uiso 1 1 calc R . . C22 C 0.0669(3) 0.47331(12) 0.9223(3) 0.0313(6) Uani 1 1 d . . . H22A H 0.1293 0.4895 0.8593 0.038 Uiso 1 1 calc R . . C23 C 0.0174(3) 0.50830(10) 1.0219(2) 0.0223(5) Uani 1 1 d . . . C24 C -0.0700(3) 0.47845(12) 1.1124(3) 0.0297(6) Uani 1 1 d . . . H24A H -0.1021 0.5010 1.1830 0.036 Uiso 1 1 calc R . . C25 C 0.5890(5) 0.60815(17) 0.9809(4) 0.0577(10) Uani 1 1 d . . . C26 C 0.9144(5) 0.61627(16) 0.5128(4) 0.0503(9) Uani 1 1 d . . . C27 C -0.2833(5) 0.7685(2) 0.2031(4) 0.0561(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03841(12) 0.01604(10) 0.03416(11) 0.00046(8) 0.00604(9) -0.00215(8) Ag2 0.03020(11) 0.02496(10) 0.02543(11) -0.00020(7) 0.00683(8) -0.00037(7) Ag3 0.03970(12) 0.01613(10) 0.03254(11) -0.00036(8) 0.00835(9) 0.00147(8) S1 0.0400(4) 0.0321(3) 0.0261(4) 0.0021(3) 0.0014(3) 0.0006(3) S2 0.0402(4) 0.0301(3) 0.0245(4) -0.0008(2) 0.0012(3) -0.0019(3) S3 0.0422(4) 0.0325(4) 0.0400(4) -0.0020(3) 0.0134(3) -0.0024(3) F1 0.119(3) 0.090(2) 0.146(3) 0.020(2) 0.049(2) -0.050(2) F2 0.0624(17) 0.0753(18) 0.147(3) -0.0389(18) -0.0527(18) 0.0082(13) F3 0.092(2) 0.0353(12) 0.128(2) -0.0171(13) -0.0356(18) 0.0151(12) F4 0.0664(17) 0.0739(17) 0.0936(19) 0.0191(14) -0.0290(15) 0.0151(12) F5 0.0911(19) 0.0404(13) 0.132(2) 0.0249(14) -0.0264(18) -0.0164(12) F6 0.140(3) 0.087(2) 0.092(2) -0.0177(16) 0.024(2) 0.062(2) F7 0.0478(14) 0.134(3) 0.0909(18) 0.0193(19) -0.0126(13) 0.0031(16) F8 0.0772(17) 0.118(2) 0.0399(12) -0.0106(12) 0.0126(12) -0.0243(15) F9 0.0983(19) 0.0652(16) 0.0837(17) -0.0256(14) -0.0002(15) -0.0288(15) O1 0.0459(14) 0.0340(12) 0.0370(12) 0.0016(8) 0.0011(10) -0.0004(9) O2 0.0688(18) 0.0424(13) 0.0575(16) -0.0023(11) 0.0107(14) 0.0177(12) O3 0.0631(18) 0.0669(17) 0.0335(13) 0.0059(11) 0.0092(12) 0.0012(13) O4 0.0523(16) 0.0678(17) 0.0305(12) 0.0060(11) -0.0105(11) -0.0096(12) O5 0.0514(15) 0.0525(14) 0.0302(12) -0.0063(10) -0.0069(11) 0.0072(11) O6 0.0597(18) 0.0601(16) 0.0681(19) 0.0120(13) 0.0033(15) -0.0252(13) O7 0.077(2) 0.0546(15) 0.0274(12) -0.0032(10) 0.0085(12) 0.0081(13) O8 0.0719(18) 0.0295(11) 0.0701(17) 0.0013(10) 0.0327(15) -0.0010(11) O9 0.0409(15) 0.0524(14) 0.0713(18) -0.0076(12) 0.0023(13) 0.0036(11) O10 0.0706(18) 0.0510(15) 0.0518(15) -0.0021(11) 0.0275(14) -0.0141(12) O11 0.078(2) 0.0392(14) 0.0509(16) -0.0036(9) 0.0127(15) -0.0078(11) N1 0.0291(12) 0.0185(9) 0.0267(11) 0.0023(8) 0.0057(9) 0.0008(8) N2 0.0356(13) 0.0175(9) 0.0242(12) -0.0011(8) 0.0045(10) 0.0034(8) N3 0.0320(14) 0.0207(10) 0.0324(13) -0.0006(9) 0.0026(11) 0.0001(9) N4 0.0437(16) 0.0271(12) 0.0254(13) -0.0019(9) 0.0071(11) 0.0083(10) N5 0.0293(13) 0.0236(10) 0.0317(13) 0.0033(8) 0.0039(10) -0.0018(9) N6 0.0262(13) 0.0248(11) 0.0350(13) 0.0044(9) 0.0042(10) 0.0010(8) N7 0.0249(13) 0.0268(11) 0.0363(13) -0.0068(9) 0.0023(11) -0.0016(8) N8 0.0284(13) 0.0242(11) 0.0352(13) -0.0057(8) 0.0043(10) 0.0018(8) N9 0.0356(14) 0.0171(9) 0.0262(12) 0.0006(8) 0.0059(10) -0.0008(8) N10 0.0336(13) 0.0197(10) 0.0250(11) -0.0008(8) 0.0045(10) -0.0009(8) N11 0.0346(14) 0.0209(10) 0.0270(12) 0.0008(8) 0.0036(10) -0.0019(9) N12 0.0413(15) 0.0222(11) 0.0270(13) -0.0002(9) 0.0058(11) -0.0058(9) C1 0.0362(16) 0.0190(11) 0.0242(14) 0.0018(9) 0.0018(12) 0.0011(10) C2 0.0253(14) 0.0172(11) 0.0280(14) -0.0016(9) 0.0031(11) 0.0011(9) C3 0.0420(17) 0.0252(13) 0.0250(14) -0.0006(10) 0.0038(13) 0.0060(11) C4 0.0400(17) 0.0219(12) 0.0259(14) 0.0048(9) 0.0086(12) 0.0050(10) C5 0.0438(18) 0.0233(13) 0.0255(15) -0.0007(10) 0.0065(13) 0.0047(11) C6 0.0265(15) 0.0192(11) 0.0261(14) -0.0015(9) -0.0006(11) 0.0022(9) C7 0.0336(16) 0.0225(12) 0.0442(17) 0.0033(11) 0.0159(13) 0.0050(11) C8 0.0405(18) 0.0207(12) 0.0430(17) 0.0039(11) 0.0149(14) 0.0029(11) C9 0.0360(17) 0.0226(12) 0.0323(15) 0.0036(10) 0.0062(13) -0.0047(10) C10 0.0315(16) 0.0231(12) 0.0374(16) 0.0036(10) -0.0001(13) 0.0034(10) C11 0.0226(15) 0.0271(12) 0.0269(14) -0.0005(10) -0.0012(11) 0.0006(10) C12 0.0322(16) 0.0244(12) 0.0337(15) 0.0057(10) 0.0019(13) -0.0009(10) C13 0.0264(15) 0.0296(13) 0.0335(15) -0.0061(10) 0.0045(13) -0.0012(10) C14 0.0225(14) 0.0245(12) 0.0287(14) 0.0030(10) -0.0020(12) 0.0008(10) C15 0.0281(16) 0.0242(13) 0.0428(17) -0.0039(11) 0.0010(13) -0.0026(10) C16 0.0354(17) 0.0269(13) 0.0401(17) -0.0073(11) 0.0080(14) 0.0000(11) C17 0.0334(16) 0.0208(12) 0.0200(13) -0.0017(9) 0.0032(11) -0.0029(10) C18 0.0263(14) 0.0156(10) 0.0247(13) 0.0011(9) 0.0029(11) -0.0025(9) C19 0.0383(17) 0.0212(12) 0.0256(14) 0.0019(9) 0.0047(12) -0.0036(10) C20 0.0423(17) 0.0213(12) 0.0248(14) -0.0029(9) 0.0075(12) -0.0023(10) C21 0.0420(18) 0.0196(12) 0.0341(16) -0.0057(10) 0.0109(13) -0.0048(11) C22 0.0375(17) 0.0241(13) 0.0333(16) -0.0012(10) 0.0145(13) -0.0075(11) C23 0.0284(15) 0.0146(10) 0.0241(13) 0.0014(8) 0.0027(11) -0.0023(9) C24 0.0382(17) 0.0239(13) 0.0271(15) 0.0014(10) 0.0056(13) -0.0056(11) C25 0.049(2) 0.0411(19) 0.082(3) -0.0025(18) -0.009(2) -0.0051(15) C26 0.055(2) 0.0408(18) 0.055(2) -0.0017(15) -0.0041(19) 0.0083(15) C27 0.049(2) 0.070(3) 0.050(2) -0.0059(19) 0.0069(19) -0.0140(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 Ag1 N1 2.238(2) . ? Ag1 N3 2.240(2) 2_656 ? Ag1 N5 2.399(2) . ? Ag1 O1 2.7467(18) 1_554 ? Ag2 N9 2.288(2) . ? Ag2 N2 2.292(2) . ? Ag2 N6 2.358(2) . ? Ag2 N7 2.374(2) 1_655 ? Ag3 N10 2.258(2) . ? Ag3 N11 2.270(2) 2_557 ? Ag3 N8 2.373(2) 1_655 ? Ag3 O1 2.6217(18) . ? S1 O4 1.424(2) . ? S1 O3 1.437(3) . ? S1 O2 1.441(3) . ? S1 C25 1.802(4) . ? S2 O6 1.430(3) . ? S2 O5 1.435(2) . ? S2 O7 1.439(3) . ? S2 C26 1.819(4) . ? S3 O10 1.429(3) . ? S3 O9 1.437(3) . ? S3 O8 1.439(2) . ? S3 C27 1.821(4) . ? F1 C25 1.298(5) . ? F2 C25 1.339(5) . ? F3 C25 1.342(5) . ? F4 C26 1.330(4) . ? F5 C26 1.323(5) . ? F6 C26 1.306(5) . ? F7 C27 1.315(5) . ? F8 C27 1.333(4) . ? F9 C27 1.329(5) . ? N1 C4 1.331(3) . ? N1 N2 1.353(3) . ? N2 C1 1.320(3) . ? N3 C8 1.316(4) . ? N3 N4 1.349(3) . ? N3 Ag1 2.240(2) 2_646 ? N4 C5 1.318(3) . ? N5 C9 1.323(3) . ? N5 N6 1.346(3) . ? N6 C12 1.323(4) . ? N7 C13 1.321(4) . ? N7 N8 1.359(3) . ? N7 Ag2 2.374(2) 1_455 ? N8 C16 1.327(4) . ? N8 Ag3 2.373(2) 1_455 ? N9 C17 1.327(3) . ? N9 N10 1.354(3) . ? N10 C20 1.329(3) . ? N11 C21 1.318(4) . ? N11 N12 1.347(3) . ? N11 Ag3 2.270(2) 2_547 ? N12 C24 1.320(3) . ? C1 C2 1.408(4) . ? C2 C3 1.372(4) . ? C2 C6 1.479(3) . ? C3 C4 1.403(3) . ? C5 C6 1.402(4) . ? C6 C7 1.370(4) . ? C7 C8 1.399(4) . ? C9 C10 1.391(4) . ? C10 C11 1.376(4) . ? C11 C12 1.404(4) . ? C11 C14 1.479(4) . ? C13 C14 1.408(4) . ? C14 C15 1.370(4) . ? C15 C16 1.397(4) . ? C17 C18 1.404(3) . ? C18 C19 1.371(4) . ? C18 C23 1.486(3) . ? C19 C20 1.400(3) . ? C21 C22 1.397(3) . ? C22 C23 1.377(4) . ? C23 C24 1.402(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 149.64(9) . 2_656 ? N1 Ag1 N5 112.05(8) . . ? N3 Ag1 N5 95.60(8) 2_656 . ? N1 Ag1 O1 86.57(7) . 1_554 ? N3 Ag1 O1 101.37(8) 2_656 1_554 ? N5 Ag1 O1 99.70(7) . 1_554 ? N9 Ag2 N2 133.15(8) . . ? N9 Ag2 N6 98.17(8) . . ? N2 Ag2 N6 111.62(8) . . ? N9 Ag2 N7 113.28(8) . 1_655 ? N2 Ag2 N7 96.51(8) . 1_655 ? N6 Ag2 N7 100.24(9) . 1_655 ? N10 Ag3 N11 141.89(9) . 2_557 ? N10 Ag3 N8 115.40(8) . 1_655 ? N11 Ag3 N8 96.63(8) 2_557 1_655 ? N10 Ag3 O1 93.81(8) . . ? N11 Ag3 O1 93.87(7) 2_557 . ? N8 Ag3 O1 110.16(7) 1_655 . ? O4 S1 O3 114.78(17) . . ? O4 S1 O2 114.98(17) . . ? O3 S1 O2 113.94(16) . . ? O4 S1 C25 103.94(18) . . ? O3 S1 C25 104.19(19) . . ? O2 S1 C25 102.99(18) . . ? O6 S2 O5 115.58(16) . . ? O6 S2 O7 113.54(17) . . ? O5 S2 O7 114.83(16) . . ? O6 S2 C26 103.99(18) . . ? O5 S2 C26 103.19(16) . . ? O7 S2 C26 103.62(17) . . ? O10 S3 O9 116.85(17) . . ? O10 S3 O8 114.99(15) . . ? O9 S3 O8 112.84(16) . . ? O10 S3 C27 103.23(17) . . ? O9 S3 C27 102.90(18) . . ? O8 S3 C27 103.70(18) . . ? C4 N1 N2 118.8(2) . . ? C4 N1 Ag1 124.75(17) . . ? N2 N1 Ag1 116.31(15) . . ? C1 N2 N1 120.1(2) . . ? C1 N2 Ag2 121.86(19) . . ? N1 N2 Ag2 115.44(15) . . ? C8 N3 N4 119.8(2) . . ? C8 N3 Ag1 120.02(18) . 2_646 ? N4 N3 Ag1 119.39(17) . 2_646 ? C5 N4 N3 118.8(2) . . ? C9 N5 N6 119.2(2) . . ? C9 N5 Ag1 126.41(19) . . ? N6 N5 Ag1 113.83(16) . . ? C12 N6 N5 119.4(2) . . ? C12 N6 Ag2 123.99(17) . . ? N5 N6 Ag2 114.99(17) . . ? C13 N7 N8 119.7(2) . . ? C13 N7 Ag2 125.38(18) . 1_455 ? N8 N7 Ag2 111.96(16) . 1_455 ? C16 N8 N7 118.7(2) . . ? C16 N8 Ag3 125.70(19) . 1_455 ? N7 N8 Ag3 115.35(16) . 1_455 ? C17 N9 N10 119.7(2) . . ? C17 N9 Ag2 121.17(18) . . ? N10 N9 Ag2 116.95(15) . . ? C20 N10 N9 118.9(2) . . ? C20 N10 Ag3 125.85(17) . . ? N9 N10 Ag3 115.27(15) . . ? C21 N11 N12 119.9(2) . . ? C21 N11 Ag3 123.85(18) . 2_547 ? N12 N11 Ag3 115.28(16) . 2_547 ? C24 N12 N11 118.5(2) . . ? N2 C1 C2 123.7(2) . . ? C3 C2 C1 116.0(2) . . ? C3 C2 C6 124.7(2) . . ? C1 C2 C6 119.2(2) . . ? C2 C3 C4 118.3(2) . . ? N1 C4 C3 123.0(2) . . ? N4 C5 C6 124.2(3) . . ? C7 C6 C5 116.5(2) . . ? C7 C6 C2 121.6(2) . . ? C5 C6 C2 121.9(2) . . ? C6 C7 C8 117.3(3) . . ? N3 C8 C7 123.4(3) . . ? N5 C9 C10 123.5(2) . . ? C11 C10 C9 117.9(2) . . ? C10 C11 C12 116.0(3) . . ? C10 C11 C14 124.5(2) . . ? C12 C11 C14 119.5(2) . . ? N6 C12 C11 124.0(2) . . ? N7 C13 C14 123.5(3) . . ? C15 C14 C13 116.5(3) . . ? C15 C14 C11 123.6(2) . . ? C13 C14 C11 119.8(2) . . ? C14 C15 C16 117.8(2) . . ? N8 C16 C15 123.5(3) . . ? N9 C17 C18 123.5(2) . . ? C19 C18 C17 116.6(2) . . ? C19 C18 C23 123.7(2) . . ? C17 C18 C23 119.6(2) . . ? C18 C19 C20 117.8(2) . . ? N10 C20 C19 123.4(2) . . ? N11 C21 C22 123.5(3) . . ? C23 C22 C21 117.4(3) . . ? C22 C23 C24 115.9(2) . . ? C22 C23 C18 121.8(2) . . ? C24 C23 C18 122.3(2) . . ? N12 C24 C23 124.8(3) . . ? F1 C25 F2 108.0(4) . . ? F1 C25 F3 108.0(4) . . ? F2 C25 F3 106.4(3) . . ? F1 C25 S1 112.9(3) . . ? F2 C25 S1 110.3(3) . . ? F3 C25 S1 110.9(3) . . ? F6 C26 F5 109.2(4) . . ? F6 C26 F4 107.7(3) . . ? F5 C26 F4 106.8(3) . . ? F6 C26 S2 111.9(3) . . ? F5 C26 S2 110.0(3) . . ? F4 C26 S2 111.1(3) . . ? F7 C27 F9 107.1(3) . . ? F7 C27 F8 108.1(4) . . ? F9 C27 F8 108.5(3) . . ? F7 C27 S3 111.9(3) . . ? F9 C27 S3 109.9(3) . . ? F8 C27 S3 111.3(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.402 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.068 #============================================================================== data_(10) _database_code_depnum_ccdc_archive 'CCDC 643969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Trifluoroacetate 2:1 Complex with 4,4'-Bipyridazine, Solvate with 2/7 Chloroform ; _chemical_name_common ; Silver(i) Trifluoroacetate 2:1 Complex with 4,4'- Bipyridazine, Solvate with 2/7 Chloroform ; _chemical_melting_point ? _chemical_formula_moiety 'C84 H42 Ag14 F42 N28 O28, 2(C H Cl3)' _chemical_formula_sum 'C86 H44 Ag14 Cl6 F42 N28 O28' _chemical_formula_weight 4438.37 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' 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 ' _space_group_name_Hall '-P 1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9023(2) _cell_length_b 14.4405(3) _cell_length_c 18.2666(2) _cell_angle_alpha 107.0790(10) _cell_angle_beta 111.5920(10) _cell_angle_gamma 94.2320(10) _cell_volume 3190.47(10) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 14474 _cell_measurement_theta_min 4.19 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2118 _exptl_absorpt_coefficient_mu 2.362 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5780 _exptl_absorpt_correction_T_max 0.7039 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 43985 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14474 _reflns_number_gt 11517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. Two trifluoriacetate groups (of seven unique) were disordered in a very typical manner when two components of -CF3 group are related by rotation. The disorder was resolved with unequal contributions of the components (0.6 and 0.4) and some restraints were applied to improve the refinement stability: for these groups, the C---F bond lengths were constrained at 1.33(1) and intramolecular F...F contacts at 2.14(1). ; _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^)+(0.0317P)^2^+3.4341P] 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_number_reflns 14474 _refine_ls_number_parameters 973 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.22634(2) 0.44372(2) 1.10576(2) 0.04861(8) Uani 1 1 d . . . Ag2 Ag 0.34498(2) 0.319555(19) 1.003306(18) 0.04340(8) Uani 1 1 d . . . Ag3 Ag 0.30923(2) 0.09424(2) 0.869145(18) 0.04329(8) Uani 1 1 d . . . Ag4 Ag 0.21300(2) -0.039125(19) 0.672256(18) 0.04003(7) Uani 1 1 d . . . Ag5 Ag 0.27046(2) -0.11909(2) 0.522490(18) 0.04124(7) Uani 1 1 d . . . Ag6 Ag 0.31769(2) -0.318617(19) 0.421231(17) 0.03925(7) Uani 1 1 d . . . Ag7 Ag 0.19522(3) -0.51689(2) 0.27896(2) 0.05784(10) Uani 1 1 d . . . O1 O 0.1225(3) 0.2981(2) 1.0686(2) 0.0768(10) Uani 1 1 d . . . O2 O 0.1312(4) 0.3135(2) 1.1959(2) 0.0888(13) Uani 1 1 d . . . O3 O 0.1585(3) 0.4572(2) 0.9662(2) 0.0622(8) Uani 1 1 d . . . O4 O 0.2572(3) 0.3842(2) 0.90435(19) 0.0560(8) Uani 1 1 d . . . O5 O 0.4840(3) 0.2980(3) 0.9547(3) 0.0876(12) Uani 1 1 d . . . O6 O 0.4804(2) 0.1411(2) 0.8873(2) 0.0623(8) Uani 1 1 d . . . O7 O 0.3265(3) -0.0777(2) 0.8379(2) 0.0803(11) Uani 1 1 d . . . O8 O 0.2421(2) -0.17659(19) 0.70498(18) 0.0503(7) Uani 1 1 d . . . O9 O 0.0603(3) -0.1029(3) 0.5385(2) 0.0808(11) Uani 1 1 d . . . O10 O 0.1015(2) -0.2101(2) 0.44658(19) 0.0585(8) Uani 1 1 d . . . O11 O 0.3083(3) -0.0944(3) 0.4135(2) 0.0801(11) Uani 1 1 d . . . O12 O 0.3456(3) -0.2284(2) 0.3415(2) 0.0588(8) Uani 1 1 d . . . O13 O 0.4529(2) -0.39967(18) 0.40326(19) 0.0520(7) Uani 1 1 d . . . O14 O 0.3642(2) -0.5539(2) 0.3213(2) 0.0595(8) Uani 1 1 d . . . N1 N 0.3998(2) 0.5160(2) 1.16375(19) 0.0368(7) Uani 1 1 d . . . N2 N 0.4496(2) 0.4681(2) 1.1172(2) 0.0423(7) Uani 1 1 d . . . N3 N 0.3460(3) 0.1976(2) 1.05895(18) 0.0402(7) Uani 1 1 d . . . N4 N 0.3429(3) 0.1070(2) 1.00735(19) 0.0478(8) Uani 1 1 d . . . N5 N 0.1440(2) 0.1110(2) 0.79939(19) 0.0385(7) Uani 1 1 d . . . N6 N 0.0994(2) 0.0467(2) 0.71982(19) 0.0386(7) Uani 1 1 d . . . N7 N -0.1427(2) 0.3988(2) 0.7814(2) 0.0403(7) Uani 1 1 d . . . N8 N -0.1436(3) 0.4243(2) 0.8584(2) 0.0444(8) Uani 1 1 d . . . N9 N 0.6904(2) 0.91472(19) 1.34108(18) 0.0363(7) Uani 1 1 d . . . N10 N 0.6817(2) 0.9428(2) 1.41504(19) 0.0380(7) Uani 1 1 d . . . N11 N 0.5816(2) 0.1608(2) 1.39289(18) 0.0346(6) Uani 1 1 d . . . N12 N 0.5415(2) 0.2222(2) 1.44033(18) 0.0376(7) Uani 1 1 d . . . N13 N 0.1986(2) -0.3907(2) 0.45668(19) 0.0360(7) Uani 1 1 d . . . N14 N 0.1201(3) -0.4647(2) 0.3956(2) 0.0470(8) Uani 1 1 d . . . C1 C 0.4471(3) 0.6033(2) 1.2221(2) 0.0344(8) Uani 1 1 d . . . H1A H 0.4111 0.6350 1.2529 0.041 Uiso 1 1 calc R . . C2 C 0.5487(3) 0.6509(2) 1.2403(2) 0.0338(7) Uani 1 1 d . . . C3 C 0.5981(3) 0.6032(3) 1.1922(3) 0.0449(9) Uani 1 1 d . . . H3A H 0.6652 0.6313 1.2002 0.054 Uiso 1 1 calc R . . C4 C 0.5443(3) 0.5112(3) 1.1310(3) 0.0505(11) Uani 1 1 d . . . H4A H 0.5774 0.4784 1.0981 0.061 Uiso 1 1 calc R . . C5 C 0.3756(3) 0.2129(2) 1.1394(2) 0.0376(8) Uani 1 1 d . . . H5A H 0.3761 0.2749 1.1740 0.045 Uiso 1 1 calc R . . C6 C 0.4064(3) 0.1414(2) 1.1762(2) 0.0353(8) Uani 1 1 d . . . C7 C 0.4045(4) 0.0504(3) 1.1237(2) 0.0498(10) Uani 1 1 d . . . H7A H 0.4252 -0.0002 1.1439 0.060 Uiso 1 1 calc R . . C8 C 0.3703(4) 0.0375(3) 1.0389(2) 0.0564(12) Uani 1 1 d . . . H8A H 0.3667 -0.0244 1.0023 0.068 Uiso 1 1 calc R . . C9 C 0.0916(3) 0.1761(2) 0.8259(2) 0.0393(8) Uani 1 1 d . . . H9A H 0.1227 0.2184 0.8815 0.047 Uiso 1 1 calc R . . C10 C -0.0081(3) 0.1848(2) 0.7748(2) 0.0348(8) Uani 1 1 d . . . C11 C -0.0533(3) 0.1182(3) 0.6946(2) 0.0422(9) Uani 1 1 d . . . H11A H -0.1203 0.1187 0.6575 0.051 Uiso 1 1 calc R . . C12 C 0.0038(3) 0.0500(3) 0.6703(2) 0.0443(9) Uani 1 1 d . . . H12A H -0.0270 0.0040 0.6161 0.053 Uiso 1 1 calc R . . C13 C -0.1023(3) 0.3215(2) 0.7565(2) 0.0375(8) Uani 1 1 d . . . H13A H -0.1038 0.3030 0.7028 0.045 Uiso 1 1 calc R . . C14 C -0.0577(3) 0.2662(2) 0.8064(2) 0.0359(8) Uani 1 1 d . . . C15 C -0.0562(3) 0.2943(3) 0.8850(3) 0.0456(9) Uani 1 1 d . . . H15A H -0.0259 0.2613 0.9219 0.055 Uiso 1 1 calc R . . C16 C -0.1021(4) 0.3743(3) 0.9076(3) 0.0503(10) Uani 1 1 d . . . H16A H -0.1034 0.3934 0.9604 0.060 Uiso 1 1 calc R . . C17 C 0.6505(3) 0.8220(2) 1.2888(2) 0.0349(8) Uani 1 1 d . . . H17A H 0.6587 0.8036 1.2385 0.042 Uiso 1 1 calc R . . C18 C 0.5971(3) 0.7508(2) 1.3056(2) 0.0322(7) Uani 1 1 d . . . C19 C 0.5889(3) 0.7794(2) 1.3811(2) 0.0382(8) Uani 1 1 d . . . H19A H 0.5546 0.7355 1.3963 0.046 Uiso 1 1 calc R . . C20 C 0.6342(3) 0.8775(2) 1.4343(2) 0.0411(9) Uani 1 1 d . . . H20A H 0.6304 0.8976 1.4862 0.049 Uiso 1 1 calc R . . C21 C 0.5348(3) 0.1336(2) 1.3106(2) 0.0326(7) Uani 1 1 d . . . H21A H 0.5623 0.0896 1.2790 0.039 Uiso 1 1 calc R . . C22 C 0.4463(3) 0.1670(2) 1.2679(2) 0.0315(7) Uani 1 1 d . . . C23 C 0.4049(3) 0.2275(3) 1.3165(2) 0.0388(8) Uani 1 1 d . . . H23A H 0.3449 0.2512 1.2925 0.047 Uiso 1 1 calc R . . C24 C 0.4559(3) 0.2522(3) 1.4033(2) 0.0406(8) Uani 1 1 d . . . H24A H 0.4276 0.2921 1.4368 0.049 Uiso 1 1 calc R . . C25 C 0.1992(3) -0.3606(3) 0.5324(2) 0.0444(9) Uani 1 1 d . . . H25A H 0.2538 -0.3096 0.5745 0.053 Uiso 1 1 calc R . . C26 C 0.1232(3) -0.4009(3) 0.5528(2) 0.0458(9) Uani 1 1 d . . . H26A H 0.1269 -0.3768 0.6072 0.055 Uiso 1 1 calc R . . C27 C 0.0427(3) -0.4762(2) 0.4922(2) 0.0363(8) Uani 1 1 d . . . C28 C 0.0468(3) -0.5048(3) 0.4132(3) 0.0505(10) Uani 1 1 d . . . H28A H -0.0064 -0.5560 0.3698 0.061 Uiso 1 1 calc R . . C29 C 0.1057(4) 0.2711(3) 1.1213(3) 0.0699(15) Uani 1 1 d D . . C30 C 0.0441(6) 0.1626(3) 1.0847(4) 0.130(4) Uani 1 1 d D . . C31 C 0.1943(3) 0.4377(2) 0.9132(2) 0.0384(8) Uani 1 1 d . . . C32 C 0.1537(3) 0.4837(3) 0.8440(3) 0.0502(10) Uani 1 1 d . . . C33 C 0.5215(3) 0.2297(3) 0.9270(3) 0.0449(9) Uani 1 1 d . . . C34 C 0.6355(4) 0.2576(3) 0.9405(3) 0.0566(11) Uani 1 1 d . . . C35 C 0.2884(3) -0.1571(2) 0.7818(3) 0.0415(9) Uani 1 1 d . . . C36 C 0.3002(4) -0.2478(3) 0.8087(3) 0.0650(13) Uani 1 1 d D . . C37 C 0.0410(3) -0.1751(3) 0.4772(2) 0.0418(9) Uani 1 1 d . . . C38 C -0.0755(3) -0.2288(3) 0.4284(3) 0.0531(10) Uani 1 1 d . . . C39 C 0.3362(3) -0.1420(3) 0.3606(2) 0.0387(8) Uani 1 1 d . . . C40 C 0.3559(4) -0.0832(3) 0.3084(3) 0.0585(12) Uani 1 1 d . . . C41 C 0.4438(3) -0.4882(3) 0.3654(2) 0.0409(8) Uani 1 1 d . . . C42 C 0.5498(3) -0.5189(3) 0.3761(3) 0.0530(11) Uani 1 1 d . . . C43 C 0.8692(4) -0.2321(4) 0.6635(4) 0.0734(14) Uani 1 1 d . . . H43A H 0.8724 -0.2477 0.7129 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.78354(13) -0.32858(14) 0.57498(14) 0.1119(6) Uani 1 1 d . . . Cl2 Cl 0.99716(12) -0.21580(12) 0.66698(12) 0.0907(5) Uani 1 1 d . . . Cl3 Cl 0.82153(16) -0.12350(13) 0.66696(17) 0.1248(8) Uani 1 1 d . . . F1 F -0.0099(12) 0.1466(8) 1.1268(8) 0.173(7) Uani 0.60 1 d PD . . F2 F 0.1145(9) 0.1030(7) 1.0916(15) 0.199(6) Uani 0.60 1 d PD . . F3 F -0.0218(14) 0.1344(12) 1.0058(6) 0.184(9) Uani 0.60 1 d PD . . F1A F 0.059(3) 0.1135(12) 1.0181(15) 0.232(16) Uani 0.40 1 d PD . . F2A F 0.068(3) 0.1167(13) 1.1378(9) 0.30(3) Uani 0.40 1 d PD . . F3A F -0.0561(9) 0.1703(14) 1.061(3) 0.303(19) Uani 0.40 1 d PD . . F4 F 0.0915(3) 0.5450(3) 0.8559(2) 0.0960(11) Uani 1 1 d . . . F5 F 0.0981(3) 0.4129(2) 0.76946(18) 0.0864(9) Uani 1 1 d . . . F6 F 0.2313(2) 0.5308(2) 0.8351(2) 0.0755(8) Uani 1 1 d . . . F7 F 0.6852(4) 0.3398(3) 0.9980(4) 0.181(3) Uani 1 1 d . . . F8 F 0.6916(2) 0.1935(3) 0.9571(3) 0.1182(15) Uani 1 1 d . . . F9 F 0.6414(3) 0.2676(4) 0.8736(3) 0.1288(16) Uani 1 1 d . . . F10 F 0.3825(8) -0.2343(8) 0.8742(6) 0.102(3) Uani 0.60 1 d P . . F11 F 0.2225(8) -0.2730(12) 0.8260(13) 0.135(4) Uani 0.60 1 d P . . F12 F 0.3041(18) -0.3257(8) 0.7541(6) 0.139(6) Uani 0.60 1 d P . . F10A F 0.2102(9) -0.3135(10) 0.7685(11) 0.104(6) Uani 0.40 1 d PD . . F11A F 0.331(2) -0.2282(14) 0.8894(5) 0.186(14) Uani 0.40 1 d PD . . F12A F 0.3711(18) -0.2886(14) 0.785(2) 0.186(14) Uani 0.40 1 d PD . . F13 F -0.1383(2) -0.1857(3) 0.4606(2) 0.1035(12) Uani 1 1 d . . . F14 F -0.0885(3) -0.3203(2) 0.4271(3) 0.1064(13) Uani 1 1 d . . . F15 F -0.1144(2) -0.2329(3) 0.34932(18) 0.0855(9) Uani 1 1 d . . . F16 F 0.3789(5) 0.0125(3) 0.3492(4) 0.161(2) Uani 1 1 d . . . F17 F 0.4322(3) -0.1005(3) 0.2857(2) 0.0910(11) Uani 1 1 d . . . F18 F 0.2698(3) -0.0955(4) 0.2422(3) 0.1347(18) Uani 1 1 d . . . F19 F 0.6227(2) -0.4487(2) 0.3829(2) 0.0743(8) Uani 1 1 d . . . F20 F 0.5422(3) -0.5974(2) 0.3141(3) 0.1101(14) Uani 1 1 d . . . F21 F 0.5891(3) -0.5417(3) 0.4447(3) 0.1065(13) 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 0.04532(18) 0.04044(14) 0.0589(2) 0.00831(13) 0.02703(15) 0.00839(12) Ag2 0.05672(19) 0.03287(13) 0.03863(15) 0.01116(11) 0.01747(13) 0.01357(12) Ag3 0.04202(17) 0.04959(15) 0.03316(15) 0.01276(12) 0.01038(12) 0.01313(12) Ag4 0.04883(17) 0.03623(13) 0.04015(15) 0.01329(11) 0.02313(13) 0.01144(12) Ag5 0.04166(16) 0.04113(14) 0.03611(15) 0.00800(11) 0.01423(12) 0.01195(12) Ag6 0.04059(16) 0.03911(13) 0.03672(15) 0.00862(11) 0.01906(12) 0.00177(11) Ag7 0.0632(2) 0.04053(15) 0.05279(19) 0.00937(13) 0.00983(16) 0.01497(14) O1 0.088(3) 0.0598(19) 0.063(2) 0.0195(17) 0.0178(19) -0.0185(17) O2 0.134(4) 0.0482(17) 0.056(2) 0.0102(16) 0.022(2) -0.0186(19) O3 0.071(2) 0.079(2) 0.0531(19) 0.0248(16) 0.0395(17) 0.0260(17) O4 0.073(2) 0.0612(17) 0.0594(19) 0.0350(15) 0.0389(16) 0.0382(16) O5 0.106(3) 0.074(2) 0.133(4) 0.050(2) 0.086(3) 0.054(2) O6 0.0456(18) 0.0602(18) 0.070(2) 0.0126(16) 0.0207(15) 0.0066(14) O7 0.110(3) 0.0401(15) 0.060(2) 0.0026(14) 0.0124(19) 0.0190(17) O8 0.070(2) 0.0412(13) 0.0445(16) 0.0181(12) 0.0254(14) 0.0122(13) O9 0.063(2) 0.089(2) 0.051(2) -0.0168(18) 0.0140(16) 0.0108(18) O10 0.0417(17) 0.0636(18) 0.0554(18) 0.0056(14) 0.0151(14) 0.0127(14) O11 0.115(3) 0.092(3) 0.066(2) 0.035(2) 0.063(2) 0.045(2) O12 0.083(2) 0.0415(14) 0.0609(19) 0.0201(13) 0.0383(17) 0.0092(14) O13 0.0633(19) 0.0377(13) 0.0631(19) 0.0110(13) 0.0391(15) 0.0138(12) O14 0.0440(17) 0.0446(15) 0.081(2) 0.0201(15) 0.0171(15) 0.0114(13) N1 0.0389(17) 0.0310(13) 0.0402(17) 0.0061(12) 0.0210(13) 0.0050(12) N2 0.0395(18) 0.0356(14) 0.0430(18) -0.0011(13) 0.0193(14) 0.0040(13) N3 0.056(2) 0.0338(14) 0.0281(15) 0.0103(12) 0.0139(14) 0.0140(13) N4 0.075(2) 0.0352(15) 0.0280(16) 0.0086(12) 0.0160(15) 0.0159(15) N5 0.0341(16) 0.0372(14) 0.0374(16) 0.0066(12) 0.0117(13) 0.0100(12) N6 0.0392(18) 0.0370(14) 0.0363(16) 0.0071(12) 0.0156(13) 0.0108(13) N7 0.0380(17) 0.0418(15) 0.0446(18) 0.0152(14) 0.0191(14) 0.0158(13) N8 0.0469(19) 0.0445(16) 0.049(2) 0.0152(15) 0.0264(15) 0.0180(14) N9 0.0427(17) 0.0305(13) 0.0351(16) 0.0096(12) 0.0174(13) 0.0030(12) N10 0.0471(18) 0.0295(13) 0.0354(16) 0.0072(12) 0.0186(14) 0.0042(12) N11 0.0310(16) 0.0359(14) 0.0339(15) 0.0102(12) 0.0114(12) 0.0073(12) N12 0.0404(17) 0.0379(14) 0.0309(15) 0.0092(12) 0.0127(13) 0.0094(13) N13 0.0365(17) 0.0330(14) 0.0416(17) 0.0131(12) 0.0195(13) 0.0051(12) N14 0.052(2) 0.0446(17) 0.0412(18) 0.0060(14) 0.0250(15) -0.0051(15) C1 0.043(2) 0.0303(15) 0.0339(18) 0.0091(13) 0.0216(15) 0.0088(14) C2 0.039(2) 0.0302(15) 0.0318(18) 0.0095(13) 0.0145(15) 0.0067(14) C3 0.041(2) 0.0396(18) 0.049(2) 0.0025(16) 0.0244(18) 0.0008(16) C4 0.044(2) 0.044(2) 0.056(3) -0.0032(18) 0.030(2) 0.0055(17) C5 0.048(2) 0.0315(16) 0.0333(18) 0.0105(14) 0.0162(16) 0.0136(15) C6 0.039(2) 0.0353(16) 0.0320(18) 0.0148(14) 0.0117(15) 0.0094(14) C7 0.074(3) 0.0352(18) 0.037(2) 0.0149(16) 0.0159(19) 0.0200(18) C8 0.092(3) 0.0330(18) 0.034(2) 0.0067(15) 0.017(2) 0.019(2) C9 0.039(2) 0.0354(17) 0.0359(19) 0.0050(14) 0.0125(15) 0.0089(15) C10 0.0342(19) 0.0320(15) 0.0400(19) 0.0114(14) 0.0170(15) 0.0109(14) C11 0.033(2) 0.048(2) 0.037(2) 0.0099(16) 0.0091(15) 0.0127(16) C12 0.042(2) 0.0412(18) 0.039(2) 0.0031(15) 0.0134(17) 0.0104(16) C13 0.036(2) 0.0391(17) 0.0375(19) 0.0103(15) 0.0166(15) 0.0108(15) C14 0.0310(19) 0.0349(16) 0.040(2) 0.0097(14) 0.0147(15) 0.0080(14) C15 0.051(2) 0.048(2) 0.046(2) 0.0205(17) 0.0238(19) 0.0220(18) C16 0.062(3) 0.052(2) 0.047(2) 0.0160(19) 0.032(2) 0.022(2) C17 0.039(2) 0.0355(16) 0.0299(17) 0.0097(14) 0.0158(15) 0.0046(14) C18 0.0327(18) 0.0285(15) 0.0323(17) 0.0093(13) 0.0115(14) 0.0036(13) C19 0.048(2) 0.0326(16) 0.0367(19) 0.0111(14) 0.0217(16) 0.0038(15) C20 0.058(2) 0.0354(17) 0.0310(18) 0.0080(14) 0.0231(17) 0.0065(16) C21 0.0349(19) 0.0331(15) 0.0312(17) 0.0112(13) 0.0146(14) 0.0087(14) C22 0.0356(19) 0.0292(15) 0.0279(16) 0.0103(13) 0.0109(14) 0.0047(13) C23 0.039(2) 0.0408(18) 0.0373(19) 0.0164(15) 0.0131(16) 0.0141(15) C24 0.043(2) 0.0437(18) 0.0349(19) 0.0080(15) 0.0188(16) 0.0140(16) C25 0.040(2) 0.047(2) 0.037(2) 0.0050(16) 0.0169(16) -0.0063(16) C26 0.044(2) 0.050(2) 0.035(2) 0.0057(16) 0.0170(17) -0.0060(17) C27 0.038(2) 0.0321(15) 0.041(2) 0.0111(14) 0.0201(16) 0.0041(14) C28 0.054(3) 0.046(2) 0.042(2) -0.0001(17) 0.0258(19) -0.0151(18) C29 0.082(4) 0.042(2) 0.062(3) 0.014(2) 0.011(3) -0.013(2) C30 0.190(10) 0.075(4) 0.075(5) 0.011(4) 0.024(6) -0.053(6) C31 0.039(2) 0.0347(16) 0.039(2) 0.0118(15) 0.0157(16) 0.0021(15) C32 0.045(2) 0.052(2) 0.060(3) 0.027(2) 0.021(2) 0.0156(19) C33 0.048(2) 0.049(2) 0.047(2) 0.0221(18) 0.0236(18) 0.0198(18) C34 0.059(3) 0.047(2) 0.059(3) 0.013(2) 0.024(2) 0.006(2) C35 0.046(2) 0.0321(17) 0.049(2) 0.0133(16) 0.0226(18) 0.0098(15) C36 0.086(4) 0.051(2) 0.059(3) 0.027(2) 0.025(3) 0.016(3) C37 0.038(2) 0.047(2) 0.037(2) 0.0164(16) 0.0102(16) 0.0117(16) C38 0.041(2) 0.061(2) 0.050(3) 0.016(2) 0.0126(19) 0.0103(19) C39 0.0326(19) 0.0456(19) 0.038(2) 0.0147(16) 0.0148(15) 0.0049(15) C40 0.064(3) 0.056(2) 0.080(3) 0.035(2) 0.046(3) 0.022(2) C41 0.047(2) 0.0384(18) 0.046(2) 0.0217(16) 0.0226(18) 0.0129(17) C42 0.047(2) 0.041(2) 0.072(3) 0.018(2) 0.026(2) 0.0118(18) C43 0.076(4) 0.074(3) 0.091(4) 0.038(3) 0.048(3) 0.018(3) Cl1 0.0702(10) 0.1027(12) 0.1367(16) 0.0148(11) 0.0357(10) 0.0128(9) Cl2 0.0635(9) 0.0932(10) 0.1257(14) 0.0448(9) 0.0441(9) 0.0174(7) Cl3 0.1076(14) 0.0832(10) 0.226(3) 0.0650(13) 0.1014(16) 0.0376(10) F1 0.210(13) 0.127(10) 0.128(9) 0.038(7) 0.042(8) -0.111(9) F2 0.286(15) 0.054(5) 0.26(2) 0.052(10) 0.122(17) 0.021(7) F3 0.240(16) 0.129(10) 0.073(6) 0.015(5) -0.010(7) -0.127(11) F1A 0.46(5) 0.056(7) 0.093(13) -0.023(8) 0.078(19) -0.064(18) F2A 0.66(7) 0.058(8) 0.114(14) 0.017(8) 0.13(3) -0.07(2) F3A 0.20(2) 0.29(3) 0.26(3) 0.01(3) 0.04(3) -0.18(2) F4 0.089(2) 0.113(3) 0.130(3) 0.074(2) 0.058(2) 0.070(2) F5 0.084(2) 0.104(2) 0.0494(17) 0.0287(16) 0.0071(15) -0.0022(18) F6 0.0620(17) 0.0853(19) 0.109(2) 0.0706(18) 0.0380(16) 0.0150(14) F7 0.127(4) 0.105(3) 0.210(6) -0.063(3) 0.068(4) -0.053(3) F8 0.0477(18) 0.132(3) 0.204(5) 0.108(3) 0.040(2) 0.0378(19) F9 0.085(3) 0.227(5) 0.139(4) 0.123(4) 0.067(3) 0.045(3) F10 0.102(5) 0.118(7) 0.090(7) 0.068(7) 0.015(5) 0.043(4) F11 0.116(8) 0.162(10) 0.196(12) 0.144(10) 0.075(8) 0.032(6) F12 0.287(18) 0.060(4) 0.095(5) 0.037(4) 0.087(8) 0.087(8) F10A 0.131(11) 0.065(6) 0.100(9) 0.061(6) 0.014(8) -0.020(7) F11A 0.40(4) 0.144(12) 0.052(7) 0.067(8) 0.094(17) 0.09(3) F12A 0.189(17) 0.114(13) 0.40(4) 0.156(19) 0.21(2) 0.127(13) F13 0.0511(18) 0.140(3) 0.105(3) 0.019(2) 0.0331(18) 0.0281(19) F14 0.067(2) 0.073(2) 0.156(4) 0.053(2) 0.015(2) -0.0092(16) F15 0.0554(18) 0.117(2) 0.0536(17) 0.0268(16) -0.0037(13) -0.0069(16) F16 0.258(6) 0.058(2) 0.236(6) 0.052(3) 0.179(5) 0.017(3) F17 0.090(2) 0.134(3) 0.122(3) 0.088(2) 0.081(2) 0.054(2) F18 0.084(3) 0.245(5) 0.139(4) 0.155(4) 0.042(2) 0.048(3) F19 0.0539(16) 0.0662(16) 0.115(2) 0.0407(16) 0.0396(16) 0.0128(13) F20 0.079(2) 0.0725(19) 0.156(4) -0.017(2) 0.066(2) 0.0188(16) F21 0.075(2) 0.139(3) 0.144(3) 0.108(3) 0.036(2) 0.049(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.227(3) . ? Ag1 N1 2.264(3) . ? Ag1 N8 2.351(3) 2_567 ? Ag1 O3 2.444(3) . ? Ag1 Ag2 3.1899(4) . ? Ag1 Ag7 3.2415(5) 1_566 ? Ag2 O4 2.273(3) . ? Ag2 N3 2.276(3) . ? Ag2 N2 2.395(3) . ? Ag2 O5 2.410(4) . ? Ag2 Ag3 3.3197(4) . ? Ag3 N5 2.251(3) . ? Ag3 O6 2.297(3) . ? Ag3 N4 2.339(3) . ? Ag3 O7 2.430(3) . ? Ag3 Ag4 3.2317(4) . ? Ag4 O8 2.258(3) . ? Ag4 N9 2.287(3) 2_667 ? Ag4 N6 2.335(3) . ? Ag4 O9 2.429(3) . ? Ag4 Ag5 3.0570(4) . ? Ag5 O10 2.291(3) . ? Ag5 N11 2.318(3) 2_657 ? Ag5 O11 2.351(3) . ? Ag5 N10 2.390(3) 2_667 ? Ag5 Ag6 3.1932(4) . ? Ag6 N13 2.275(3) . ? Ag6 O12 2.330(3) . ? Ag6 O13 2.359(3) . ? Ag6 N12 2.460(3) 2_657 ? Ag6 Ag7 3.0828(4) . ? Ag7 N7 2.313(3) 2_556 ? Ag7 O14 2.343(3) . ? Ag7 O2 2.366(3) 1_544 ? Ag7 Ag1 3.2415(5) 1_544 ? O1 C29 1.226(6) . ? O2 C29 1.218(6) . ? O2 Ag7 2.366(3) 1_566 ? O3 C31 1.216(5) . ? O4 C31 1.232(4) . ? O5 C33 1.215(5) . ? O6 C33 1.238(5) . ? O7 C35 1.210(4) . ? O8 C35 1.240(5) . ? O9 C37 1.209(5) . ? O10 C37 1.233(5) . ? O11 C39 1.218(5) . ? O12 C39 1.224(4) . ? O13 C41 1.234(4) . ? O14 C41 1.230(5) . ? N1 C1 1.316(4) . ? N1 N2 1.357(4) . ? N2 C4 1.314(5) . ? N3 C5 1.315(5) . ? N3 N4 1.356(4) . ? N4 C8 1.312(5) . ? N5 C9 1.320(4) . ? N5 N6 1.348(4) . ? N6 C12 1.318(5) . ? N7 C13 1.323(4) . ? N7 N8 1.352(4) . ? N7 Ag7 2.313(3) 2_556 ? N8 C16 1.312(5) . ? N8 Ag1 2.351(3) 2_567 ? N9 C17 1.328(4) . ? N9 N10 1.346(4) . ? N9 Ag4 2.287(3) 2_667 ? N10 C20 1.312(5) . ? N10 Ag5 2.390(3) 2_667 ? N11 C21 1.316(4) . ? N11 N12 1.350(4) . ? N11 Ag5 2.318(3) 2_657 ? N12 C24 1.311(5) . ? N12 Ag6 2.460(3) 2_657 ? N13 C25 1.319(5) . ? N13 N14 1.345(4) . ? N14 C28 1.321(5) . ? C1 C2 1.399(5) . ? C2 C3 1.369(5) . ? C2 C18 1.486(4) . ? C3 C4 1.394(5) . ? C5 C6 1.400(5) . ? C6 C7 1.372(5) . ? C6 C22 1.474(5) . ? C7 C8 1.391(6) . ? C9 C10 1.397(5) . ? C10 C11 1.369(5) . ? C10 C14 1.484(5) . ? C11 C12 1.382(5) . ? C13 C14 1.391(5) . ? C14 C15 1.366(5) . ? C15 C16 1.391(5) . ? C17 C18 1.394(5) . ? C18 C19 1.369(5) . ? C19 C20 1.399(5) . ? C21 C22 1.400(5) . ? C22 C23 1.370(5) . ? C23 C24 1.396(5) . ? C25 C26 1.386(5) . ? C26 C27 1.364(5) . ? C27 C28 1.404(5) . ? C27 C27 1.485(7) 2_546 ? C29 C30 1.5498(10) . ? C30 F2A 1.290(9) . ? C30 F3 1.307(8) . ? C30 F1 1.309(8) . ? C30 F1A 1.312(9) . ? C30 F3A 1.322(9) . ? C30 F2 1.347(8) . ? C31 C32 1.542(6) . ? C32 F4 1.311(5) . ? C32 F6 1.320(5) . ? C32 F5 1.338(5) . ? C33 C34 1.515(6) . ? C34 F7 1.265(5) . ? C34 F8 1.286(5) . ? C34 F9 1.303(6) . ? C35 C36 1.529(6) . ? C36 F10 1.265(9) . ? C36 F12 1.285(9) . ? C36 F11 1.288(10) . ? C36 F11A 1.307(8) . ? C36 F10A 1.320(7) . ? C36 F12A 1.324(8) . ? C37 C38 1.537(6) . ? C38 F14 1.313(5) . ? C38 F13 1.318(5) . ? C38 F15 1.323(5) . ? C39 C40 1.529(6) . ? C40 F17 1.288(5) . ? C40 F18 1.306(6) . ? C40 F16 1.312(6) . ? C41 C42 1.529(6) . ? C42 F20 1.313(5) . ? C42 F21 1.320(6) . ? C42 F19 1.324(5) . ? C43 Cl1 1.728(6) . ? C43 Cl3 1.740(5) . ? C43 Cl2 1.753(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 O1 Ag1 N1 140.34(13) . . ? O1 Ag1 N8 111.55(14) . 2_567 ? N1 Ag1 N8 103.79(11) . 2_567 ? O1 Ag1 O3 95.99(13) . . ? N1 Ag1 O3 104.49(11) . . ? N8 Ag1 O3 85.25(11) 2_567 . ? O1 Ag1 Ag2 84.91(11) . . ? N1 Ag1 Ag2 70.04(7) . . ? N8 Ag1 Ag2 153.64(9) 2_567 . ? O3 Ag1 Ag2 72.24(7) . . ? O1 Ag1 Ag7 82.72(10) . 1_566 ? N1 Ag1 Ag7 97.45(8) . 1_566 ? N8 Ag1 Ag7 64.15(9) 2_567 1_566 ? O3 Ag1 Ag7 145.92(7) . 1_566 ? Ag2 Ag1 Ag7 140.865(14) . 1_566 ? O4 Ag2 N3 148.43(12) . . ? O4 Ag2 N2 100.24(12) . . ? N3 Ag2 N2 106.81(11) . . ? O4 Ag2 O5 92.52(13) . . ? N3 Ag2 O5 102.21(12) . . ? N2 Ag2 O5 92.28(13) . . ? O4 Ag2 Ag1 83.96(7) . . ? N3 Ag2 Ag1 93.60(8) . . ? N2 Ag2 Ag1 63.63(8) . . ? O5 Ag2 Ag1 154.38(10) . . ? O4 Ag2 Ag3 95.69(8) . . ? N3 Ag2 Ag3 66.00(7) . . ? N2 Ag2 Ag3 154.03(8) . . ? O5 Ag2 Ag3 66.51(10) . . ? Ag1 Ag2 Ag3 139.044(13) . . ? N5 Ag3 O6 141.14(12) . . ? N5 Ag3 N4 112.09(12) . . ? O6 Ag3 N4 98.21(13) . . ? N5 Ag3 O7 112.66(12) . . ? O6 Ag3 O7 90.49(13) . . ? N4 Ag3 O7 89.59(11) . . ? N5 Ag3 Ag4 67.75(7) . . ? O6 Ag3 Ag4 98.21(8) . . ? N4 Ag3 Ag4 149.18(8) . . ? O7 Ag3 Ag4 64.38(8) . . ? N5 Ag3 Ag2 86.84(7) . . ? O6 Ag3 Ag2 85.55(8) . . ? N4 Ag3 Ag2 63.43(7) . . ? O7 Ag3 Ag2 151.74(8) . . ? Ag4 Ag3 Ag2 143.880(12) . . ? O8 Ag4 N9 136.43(11) . 2_667 ? O8 Ag4 N6 116.37(11) . . ? N9 Ag4 N6 100.35(11) 2_667 . ? O8 Ag4 O9 102.71(12) . . ? N9 Ag4 O9 103.51(13) 2_667 . ? N6 Ag4 O9 84.35(11) . . ? O8 Ag4 Ag5 90.25(7) . . ? N9 Ag4 Ag5 69.42(7) 2_667 . ? N6 Ag4 Ag5 144.79(8) . . ? O9 Ag4 Ag5 66.69(9) . . ? O8 Ag4 Ag3 90.51(7) . . ? N9 Ag4 Ag3 85.38(7) 2_667 . ? N6 Ag4 Ag3 63.53(7) . . ? O9 Ag4 Ag3 147.81(8) . . ? Ag5 Ag4 Ag3 143.458(13) . . ? O10 Ag5 N11 129.13(11) . 2_657 ? O10 Ag5 O11 99.70(14) . . ? N11 Ag5 O11 106.49(13) 2_657 . ? O10 Ag5 N10 125.56(11) . 2_667 ? N11 Ag5 N10 99.93(10) 2_657 2_667 ? O11 Ag5 N10 84.84(12) . 2_667 ? O10 Ag5 Ag4 88.59(8) . . ? N11 Ag5 Ag4 89.82(7) 2_657 . ? O11 Ag5 Ag4 149.70(9) . . ? N10 Ag5 Ag4 66.99(8) 2_667 . ? O10 Ag5 Ag6 80.37(7) . . ? N11 Ag5 Ag6 68.59(7) 2_657 . ? O11 Ag5 Ag6 71.01(9) . . ? N10 Ag5 Ag6 147.91(8) 2_667 . ? Ag4 Ag5 Ag6 139.294(13) . . ? N13 Ag6 O12 146.65(11) . . ? N13 Ag6 O13 119.36(10) . . ? O12 Ag6 O13 87.75(11) . . ? N13 Ag6 N12 101.85(11) . 2_657 ? O12 Ag6 N12 100.27(11) . 2_657 ? O13 Ag6 N12 83.22(10) . 2_657 ? N13 Ag6 Ag7 71.65(7) . . ? O12 Ag6 Ag7 99.07(7) . . ? O13 Ag6 Ag7 76.67(7) . . ? N12 Ag6 Ag7 151.39(7) 2_657 . ? N13 Ag6 Ag5 82.97(7) . . ? O12 Ag6 Ag5 84.66(7) . . ? O13 Ag6 Ag5 144.28(7) . . ? N12 Ag6 Ag5 64.03(7) 2_657 . ? Ag7 Ag6 Ag5 139.007(13) . . ? N7 Ag7 O14 126.22(11) 2_556 . ? N7 Ag7 O2 119.30(12) 2_556 1_544 ? O14 Ag7 O2 86.74(14) . 1_544 ? N7 Ag7 Ag6 75.96(8) 2_556 . ? O14 Ag7 Ag6 81.42(7) . . ? O2 Ag7 Ag6 164.54(10) 1_544 . ? N7 Ag7 Ag1 67.74(8) 2_556 1_544 ? O14 Ag7 Ag1 80.67(9) . 1_544 ? O2 Ag7 Ag1 70.80(10) 1_544 1_544 ? Ag6 Ag7 Ag1 116.578(14) . 1_544 ? C29 O1 Ag1 120.7(3) . . ? C29 O2 Ag7 130.7(3) . 1_566 ? C31 O3 Ag1 129.5(3) . . ? C31 O4 Ag2 122.0(3) . . ? C33 O5 Ag2 137.0(3) . . ? C33 O6 Ag3 115.9(3) . . ? C35 O7 Ag3 140.4(3) . . ? C35 O8 Ag4 111.9(2) . . ? C37 O9 Ag4 130.7(3) . . ? C37 O10 Ag5 111.1(2) . . ? C39 O11 Ag5 136.4(3) . . ? C39 O12 Ag6 117.7(3) . . ? C41 O13 Ag6 127.1(3) . . ? C41 O14 Ag7 121.3(2) . . ? C1 N1 N2 119.8(3) . . ? C1 N1 Ag1 128.0(2) . . ? N2 N1 Ag1 110.6(2) . . ? C4 N2 N1 118.8(3) . . ? C4 N2 Ag2 125.3(2) . . ? N1 N2 Ag2 115.4(2) . . ? C5 N3 N4 118.8(3) . . ? C5 N3 Ag2 124.6(2) . . ? N4 N3 Ag2 114.2(2) . . ? C8 N4 N3 119.4(3) . . ? C8 N4 Ag3 124.5(3) . . ? N3 N4 Ag3 115.6(2) . . ? C9 N5 N6 119.6(3) . . ? C9 N5 Ag3 128.3(2) . . ? N6 N5 Ag3 112.1(2) . . ? C12 N6 N5 119.0(3) . . ? C12 N6 Ag4 123.9(2) . . ? N5 N6 Ag4 115.7(2) . . ? C13 N7 N8 118.6(3) . . ? C13 N7 Ag7 130.2(3) . 2_556 ? N8 N7 Ag7 110.7(2) . 2_556 ? C16 N8 N7 119.8(3) . . ? C16 N8 Ag1 123.9(3) . 2_567 ? N7 N8 Ag1 116.3(2) . 2_567 ? C17 N9 N10 119.6(3) . . ? C17 N9 Ag4 128.3(2) . 2_667 ? N10 N9 Ag4 111.97(19) . 2_667 ? C20 N10 N9 119.2(3) . . ? C20 N10 Ag5 130.2(2) . 2_667 ? N9 N10 Ag5 109.4(2) . 2_667 ? C21 N11 N12 119.4(3) . . ? C21 N11 Ag5 130.3(2) . 2_657 ? N12 N11 Ag5 110.3(2) . 2_657 ? C24 N12 N11 119.2(3) . . ? C24 N12 Ag6 124.5(2) . 2_657 ? N11 N12 Ag6 110.2(2) . 2_657 ? C25 N13 N14 118.5(3) . . ? C25 N13 Ag6 123.7(2) . . ? N14 N13 Ag6 117.7(2) . . ? C28 N14 N13 119.2(3) . . ? N1 C1 C2 123.4(3) . . ? C3 C2 C1 116.6(3) . . ? C3 C2 C18 122.3(3) . . ? C1 C2 C18 121.0(3) . . ? C2 C3 C4 117.7(4) . . ? N2 C4 C3 123.7(3) . . ? N3 C5 C6 124.0(3) . . ? C7 C6 C5 116.8(3) . . ? C7 C6 C22 122.6(3) . . ? C5 C6 C22 120.4(3) . . ? C6 C7 C8 116.9(3) . . ? N4 C8 C7 124.1(3) . . ? N5 C9 C10 123.4(3) . . ? C11 C10 C9 116.5(3) . . ? C11 C10 C14 123.0(3) . . ? C9 C10 C14 120.4(3) . . ? C10 C11 C12 117.9(3) . . ? N6 C12 C11 123.6(3) . . ? N7 C13 C14 123.6(4) . . ? C15 C14 C13 117.4(3) . . ? C15 C14 C10 123.1(3) . . ? C13 C14 C10 119.4(3) . . ? C14 C15 C16 117.0(4) . . ? N8 C16 C15 123.6(4) . . ? N9 C17 C18 123.3(3) . . ? C19 C18 C17 117.0(3) . . ? C19 C18 C2 123.9(3) . . ? C17 C18 C2 119.1(3) . . ? C18 C19 C20 117.2(3) . . ? N10 C20 C19 123.7(3) . . ? N11 C21 C22 123.8(3) . . ? C23 C22 C21 116.3(3) . . ? C23 C22 C6 123.6(3) . . ? C21 C22 C6 120.0(3) . . ? C22 C23 C24 117.6(3) . . ? N12 C24 C23 123.6(3) . . ? N13 C25 C26 123.7(3) . . ? C27 C26 C25 119.2(4) . . ? C26 C27 C28 114.3(3) . . ? C26 C27 C27 123.3(4) . 2_546 ? C28 C27 C27 122.5(4) . 2_546 ? N14 C28 C27 125.1(3) . . ? O2 C29 O1 131.4(4) . . ? O2 C29 C30 116.0(5) . . ? O1 C29 C30 112.5(5) . . ? F2A C30 F3 132.0(13) . . ? F2A C30 F1 53.4(16) . . ? F3 C30 F1 107.3(7) . . ? F2A C30 F1A 109.8(9) . . ? F3 C30 F1A 51.7(11) . . ? F1 C30 F1A 138.0(10) . . ? F2A C30 F3A 110.4(9) . . ? F3 C30 F3A 57.3(14) . . ? F1 C30 F3A 59.1(16) . . ? F1A C30 F3A 108.5(8) . . ? F2A C30 F2 55.1(13) . . ? F3 C30 F2 108.0(7) . . ? F1 C30 F2 106.8(7) . . ? F1A C30 F2 60.5(11) . . ? F3A C30 F2 147.6(11) . . ? F2A C30 C29 113.8(12) . . ? F3 C30 C29 114.3(7) . . ? F1 C30 C29 111.9(6) . . ? F1A C30 C29 110.0(9) . . ? F3A C30 C29 104.1(10) . . ? F2 C30 C29 108.3(7) . . ? O3 C31 O4 130.0(4) . . ? O3 C31 C32 116.4(4) . . ? O4 C31 C32 113.5(3) . . ? F4 C32 F6 108.0(4) . . ? F4 C32 F5 106.6(4) . . ? F6 C32 F5 105.4(4) . . ? F4 C32 C31 113.6(4) . . ? F6 C32 C31 112.5(3) . . ? F5 C32 C31 110.3(3) . . ? O5 C33 O6 130.2(4) . . ? O5 C33 C34 115.2(4) . . ? O6 C33 C34 114.6(3) . . ? F7 C34 F8 106.5(5) . . ? F7 C34 F9 104.3(5) . . ? F8 C34 F9 105.4(5) . . ? F7 C34 C33 114.3(4) . . ? F8 C34 C33 114.5(4) . . ? F9 C34 C33 111.0(4) . . ? O7 C35 O8 129.9(4) . . ? O7 C35 C36 115.7(4) . . ? O8 C35 C36 114.4(3) . . ? F10 C36 F12 104.5(9) . . ? F10 C36 F11 105.3(8) . . ? F12 C36 F11 106.0(9) . . ? F10 C36 F11A 39.0(11) . . ? F12 C36 F11A 128.0(12) . . ? F11 C36 F11A 69.0(9) . . ? F10 C36 F10A 134.0(8) . . ? F12 C36 F10A 66.9(8) . . ? F11 C36 F10A 44.2(7) . . ? F11A C36 F10A 109.0(8) . . ? F10 C36 F12A 72.2(12) . . ? F12 C36 F12A 41.0(8) . . ? F11 C36 F12A 138.9(9) . . ? F11A C36 F12A 108.9(8) . . ? F10A C36 F12A 107.4(7) . . ? F10 C36 C35 113.9(6) . . ? F12 C36 C35 115.3(6) . . ? F11 C36 C35 111.0(6) . . ? F11A C36 C35 114.3(9) . . ? F10A C36 C35 110.0(6) . . ? F12A C36 C35 107.0(8) . . ? O9 C37 O10 128.9(4) . . ? O9 C37 C38 116.1(4) . . ? O10 C37 C38 114.9(4) . . ? F14 C38 F13 106.4(4) . . ? F14 C38 F15 106.9(4) . . ? F13 C38 F15 105.5(4) . . ? F14 C38 C37 111.7(4) . . ? F13 C38 C37 113.0(4) . . ? F15 C38 C37 112.9(4) . . ? O11 C39 O12 130.0(4) . . ? O11 C39 C40 112.7(4) . . ? O12 C39 C40 117.2(4) . . ? F17 C40 F18 109.2(5) . . ? F17 C40 F16 105.0(4) . . ? F18 C40 F16 103.6(5) . . ? F17 C40 C39 115.8(4) . . ? F18 C40 C39 110.7(4) . . ? F16 C40 C39 111.7(4) . . ? O14 C41 O13 130.3(4) . . ? O14 C41 C42 116.4(3) . . ? O13 C41 C42 113.3(3) . . ? F20 C42 F21 105.9(4) . . ? F20 C42 F19 106.6(4) . . ? F21 C42 F19 106.5(4) . . ? F20 C42 C41 113.0(4) . . ? F21 C42 C41 110.7(4) . . ? F19 C42 C41 113.6(3) . . ? Cl1 C43 Cl3 109.9(3) . . ? Cl1 C43 Cl2 111.7(3) . . ? Cl3 C43 Cl2 110.3(3) . . ? F2A F1 F3A 121.0(11) . . ? F2A F1 C30 62.5(9) . . ? F3A F1 C30 61.0(9) . . ? F2A F2 F1A 112.3(12) . . ? F2A F2 C30 60.1(8) . . ? F1A F2 C30 58.4(7) . . ? F1A F3 F3A 125.7(11) . . ? F1A F3 C30 64.4(7) . . ? F3A F3 C30 62.0(9) . . ? F3 F1A C30 64.0(8) . . ? F3 F1A F2 119.7(11) . . ? C30 F1A F2 61.0(7) . . ? F1 F2A F2 126.4(12) . . ? F1 F2A C30 64.1(10) . . ? F2 F2A C30 64.8(8) . . ? F3 F3A F1 110.8(12) . . ? F3 F3A C30 60.7(8) . . ? F1 F3A C30 60.0(10) . . ? F11A F10 C36 73.1(11) . . ? F11A F10 F12A 125.1(13) . . ? C36 F10 F12A 55.7(7) . . ? F10A F11 C36 69.6(8) . . ? F10A F11 F11A 120.1(14) . . ? C36 F11 F11A 56.1(7) . . ? F12A F12 C36 71.8(9) . . ? F12A F12 F10A 128.7(12) . . ? C36 F12 F10A 57.7(6) . . ? F11 F10A C36 66.2(8) . . ? F11 F10A F12 115.1(11) . . ? C36 F10A F12 55.4(5) . . ? F10 F11A C36 67.8(9) . . ? F10 F11A F11 118.7(13) . . ? C36 F11A F11 54.9(5) . . ? F12 F12A C36 67.2(8) . . ? F12 F12A F10 108.9(14) . . ? C36 F12A F10 52.1(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.931 _refine_diff_density_min -2.247 _refine_diff_density_rms 0.091 #============================================================================== data_(11) _database_code_depnum_ccdc_archive 'CCDC 643970' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Pentafluoropropionate 2:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common ;Silver(i) Pentafluoropropionate 2:1 Complex with 4,4'- Bipyridazine ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Ag2 F10 N4 O4' _chemical_formula_sum 'C14 H6 Ag2 F10 N4 O4' _chemical_formula_weight 699.97 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _space_group_name_Hall '-R 3 ' _symmetry_Int_Tables_number 148 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 26.9862(12) _cell_length_b 26.9862(12) _cell_length_c 7.6176(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4804.3(4) _cell_formula_units_Z 9 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 22279 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 28.70 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3006 _exptl_absorpt_coefficient_mu 1.950 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5512 _exptl_absorpt_correction_T_max 0.6157 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 22279 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 28.70 _reflns_number_total 2753 _reflns_number_gt 2285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. Relatively high U values for the atoms of pentafluoroethyl group indicated possible disorder. However, we was not successful to resolve it. To improve the refinement stability, geometry of the -C~2~F~5~ group were constrained. Thus, C---F (CF~2~) bonds lenghts were fixed at 1.35(1) and C---F (CF~3~) bond lengths at 1.32(1). Also, geometry restraints were applied for C---C bond length of C~2~F~5~ group and for intramolecular F...F contacts. ; _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^+16.7071P] 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_number_reflns 2753 _refine_ls_number_parameters 154 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.025664(13) 0.317573(14) 0.93617(4) 0.05201(15) Uani 1 1 d . . . N1 N -0.06894(13) 0.25508(15) 0.8929(4) 0.0466(7) Uani 1 1 d . . . N2 N -0.10031(14) 0.25606(16) 1.0284(4) 0.0522(8) Uani 1 1 d . . . C1 C -0.09435(16) 0.22098(16) 0.7571(5) 0.0443(8) Uani 1 1 d . . . H1A H -0.0711 0.2209 0.6619 0.053 Uiso 1 1 d R . . C2 C -0.15356(15) 0.18480(15) 0.7445(4) 0.0410(7) Uani 1 1 d . . . C3 C -0.18474(18) 0.18580(19) 0.8837(5) 0.0566(10) Uani 1 1 d . . . H3A H -0.2256 0.1615 0.8857 0.068 Uiso 1 1 d R . . C4 C -0.15613(18) 0.2230(2) 1.0232(5) 0.0588(11) Uani 1 1 d . . . H4A H -0.1782 0.2240 1.1205 0.071 Uiso 1 1 d R . . C5 C 0.0156(2) 0.23211(19) 1.2417(6) 0.0575(10) Uani 1 1 d D . . C6 C 0.0266(3) 0.1831(2) 1.2981(9) 0.111(3) Uani 1 1 d D . . O1 O 0.04883(15) 0.26232(17) 1.1276(5) 0.0709(9) Uani 1 1 d . . . O2 O -0.01980(14) 0.23744(14) 1.3298(5) 0.0657(8) Uani 1 1 d . . . C7 C -0.0064(4) 0.1318(4) 1.1898(15) 0.299(17) Uani 1 1 d D . . F1 F 0.0131(4) 0.1686(3) 1.4669(8) 0.177(3) Uani 1 1 d D . . F2 F 0.0833(2) 0.1942(2) 1.2722(10) 0.172(3) Uani 1 1 d D . . F3 F -0.0605(3) 0.1172(3) 1.2197(16) 0.278(8) Uani 1 1 d D . . F4 F 0.0093(4) 0.1451(4) 1.0232(10) 0.226(5) Uani 1 1 d D . . F5 F 0.0060(5) 0.0913(3) 1.2425(17) 0.357(8) Uani 1 1 d 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 0.04508(19) 0.0595(2) 0.04163(19) 0.00426(12) 0.00583(11) 0.01874(14) N1 0.0422(16) 0.0527(18) 0.0358(14) -0.0050(12) -0.0009(12) 0.0170(14) N2 0.0480(17) 0.058(2) 0.0393(15) -0.0094(14) 0.0015(13) 0.0181(15) C1 0.0421(18) 0.0462(18) 0.0352(15) -0.0040(13) 0.0006(13) 0.0151(15) C2 0.0421(17) 0.0376(16) 0.0340(15) -0.0005(13) 0.0011(13) 0.0130(14) C3 0.0425(19) 0.059(2) 0.046(2) -0.0106(18) 0.0061(16) 0.0090(18) C4 0.045(2) 0.069(3) 0.0441(19) -0.0130(18) 0.0067(16) 0.0152(19) C5 0.060(2) 0.052(2) 0.060(2) 0.0060(19) -0.004(2) 0.027(2) C6 0.151(8) 0.094(5) 0.120(6) 0.023(4) 0.025(5) 0.085(6) O1 0.065(2) 0.083(2) 0.065(2) 0.0203(17) 0.0061(16) 0.0370(18) O2 0.0629(19) 0.0533(17) 0.083(2) 0.0151(16) 0.0141(17) 0.0307(15) C7 0.40(3) 0.108(10) 0.39(3) -0.053(16) -0.24(3) 0.128(17) F1 0.276(9) 0.154(5) 0.147(5) 0.076(4) 0.044(5) 0.142(6) F2 0.130(4) 0.118(4) 0.285(9) -0.004(5) -0.056(5) 0.075(4) F3 0.103(4) 0.142(6) 0.57(2) -0.065(9) 0.066(8) 0.049(4) F4 0.286(12) 0.200(9) 0.192(8) -0.091(7) -0.035(8) 0.122(8) F5 0.517(19) 0.134(6) 0.50(2) -0.004(9) 0.047(17) 0.225(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.273(3) . ? Ag1 O2 2.291(3) 8_554 ? Ag1 N2 2.372(3) 8_554 ? Ag1 O1 2.382(3) . ? Ag1 Ag1 3.0516(3) 8_554 ? N1 C1 1.325(5) . ? N1 N2 1.344(4) . ? N2 C4 1.313(5) . ? C1 C2 1.398(5) . ? C2 C3 1.362(5) . ? C2 C2 1.474(7) 13_456 ? C3 C4 1.400(6) . ? C5 O1 1.223(6) . ? C5 O2 1.232(6) . ? C5 C6 1.555(6) . ? C6 F1 1.340(7) . ? C6 F2 1.417(7) . ? C6 C7 1.468(9) . ? C7 F3 1.328(9) . ? C7 F4 1.330(9) . ? C7 F5 1.353(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 N1 Ag1 O2 147.85(12) . 8_554 ? N1 Ag1 N2 108.33(12) . 8_554 ? O2 Ag1 N2 92.43(14) 8_554 8_554 ? N1 Ag1 O1 99.99(12) . . ? O2 Ag1 O1 102.74(13) 8_554 . ? N2 Ag1 O1 94.20(12) 8_554 . ? N1 Ag1 Ag1 84.52(8) . 8_554 ? O2 Ag1 Ag1 81.60(9) 8_554 8_554 ? N2 Ag1 Ag1 66.49(8) 8_554 8_554 ? O1 Ag1 Ag1 160.52(9) . 8_554 ? N1 Ag1 Ag1 70.04(8) . 6_455 ? O2 Ag1 Ag1 93.53(10) 8_554 6_455 ? N2 Ag1 Ag1 169.84(9) 8_554 6_455 ? O1 Ag1 Ag1 76.45(9) . 6_455 ? Ag1 Ag1 Ag1 122.581(15) 8_554 6_455 ? C1 N1 N2 120.1(3) . . ? C1 N1 Ag1 128.9(3) . . ? N2 N1 Ag1 111.0(2) . . ? C4 N2 N1 118.9(3) . . ? C4 N2 Ag1 128.8(3) . 6_455 ? N1 N2 Ag1 111.3(2) . 6_455 ? N1 C1 C2 123.5(3) . . ? C3 C2 C1 115.8(3) . . ? C3 C2 C2 122.9(4) . 13_456 ? C1 C2 C2 121.3(4) . 13_456 ? C2 C3 C4 118.7(4) . . ? N2 C4 C3 123.0(4) . . ? O1 C5 O2 131.5(4) . . ? O1 C5 C6 112.0(5) . . ? O2 C5 C6 116.0(4) . . ? F1 C6 F2 107.6(6) . . ? F1 C6 C7 108.5(7) . . ? F2 C6 C7 101.8(6) . . ? F1 C6 C5 111.9(5) . . ? F2 C6 C5 115.3(5) . . ? C7 C6 C5 111.3(5) . . ? C5 O1 Ag1 121.2(3) . . ? C5 O2 Ag1 121.3(3) . 6_455 ? F3 C7 F4 113.5(9) . . ? F3 C7 F5 112.9(8) . . ? F4 C7 F5 109.0(8) . . ? F3 C7 C6 104.0(7) . . ? F4 C7 C6 108.7(7) . . ? F5 C7 C6 108.4(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.856 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.100 #============================================================================== data_(12) _database_code_depnum_ccdc_archive 'CCDC 643971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Heptafluorobutyrate 2:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common ;Silver(i) Heptafluorobutyrate 2:1 Complex with 4,4'- Bipyridazine ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H6 Ag2 F14 N4 O4' _chemical_formula_sum 'C16 H6 Ag2 F14 N4 O4' _chemical_formula_weight 799.99 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _space_group_name_Hall '-R 3 ' _symmetry_Int_Tables_number 148 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 28.4273(11) _cell_length_b 28.4273(11) _cell_length_c 7.5353(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5273.5(4) _cell_formula_units_Z 9 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 22669 _cell_measurement_theta_min 5.48 _cell_measurement_theta_max 28.68 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3438 _exptl_absorpt_coefficient_mu 1.815 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7138 _exptl_absorpt_correction_T_max 0.8116 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 22669 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.48 _diffrn_reflns_theta_max 28.68 _reflns_number_total 3002 _reflns_number_gt 2541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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. The heptafluoropropyl group of the anion was disordered. The disorder was resolved considering unequal contributions of the components (0.6 and 0.4) and refined with a set of restraints: for both the components, all C---F and C---F bond lengths as well as intramolecular F...F contacts within the -C~3~F~7~ groups were constrained at the typical values and SIMU restraints were applied separately to two disorder components. This afforded a well- refinable model and therefore the disordered atoms were refined anisotropically for the sake of overall convergence. ; _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^)+(0.1015P)^2^+12.7678P] 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_number_reflns 3002 _refine_ls_number_parameters 262 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.151 _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 Ag1 Ag 0.311885(14) 0.019376(12) 0.59013(4) 0.05492(18) Uani 1 1 d . . . C1 C 0.34933(18) 0.11290(17) 1.0882(5) 0.0467(8) Uani 1 1 d . . . H1A H 0.3695 0.1129 1.1854 0.056 Uiso 1 1 calc R . . C3 C 0.3019(2) 0.1489(2) 0.9406(6) 0.0586(11) Uani 1 1 d . . . H3A H 0.2888 0.1729 0.9293 0.070 Uiso 1 1 calc R . . C2 C 0.32893(17) 0.14896(15) 1.0889(5) 0.0436(8) Uani 1 1 d . . . N2 N 0.34134(15) 0.07901(14) 0.9563(4) 0.0475(7) Uani 1 1 d . . . C5 C 0.23882(19) 0.0090(2) 0.2472(8) 0.0609(11) Uani 1 1 d D . . N1 N 0.31273(16) 0.07811(15) 0.8134(5) 0.0512(8) Uani 1 1 d . . . C4 C 0.2941(2) 0.1124(2) 0.8061(6) 0.0596(11) Uani 1 1 d . . . H4A H 0.2748 0.1120 0.7059 0.072 Uiso 1 1 calc R . . O1 O 0.26691(18) 0.04196(17) 0.3634(6) 0.0764(11) Uani 1 1 d . . . O2 O 0.24405(15) -0.02590(16) 0.1693(6) 0.0723(10) Uani 1 1 d . . . C6 C 0.1906(2) 0.0161(3) 0.1813(9) 0.094(2) Uani 1 1 d D . . C7 C 0.1450(5) -0.0087(8) 0.3211(19) 0.304(7) Uani 0.60 1 d PDU . . C8 C 0.0892(6) -0.0178(8) 0.265(3) 0.312(7) Uani 0.60 1 d PDU . . F1 F 0.2035(8) 0.0680(4) 0.150(3) 0.185(12) Uani 0.60 1 d PD . . F2 F 0.1675(9) -0.0137(9) 0.032(2) 0.28(2) Uani 0.60 1 d PD . . F3 F 0.1527(6) 0.0021(7) 0.494(2) 0.306(7) Uani 0.60 1 d PDU . . F4 F 0.1343(7) -0.0602(8) 0.290(4) 0.303(7) Uani 0.60 1 d PDU . . F5 F 0.0941(6) 0.0216(7) 0.156(3) 0.307(7) Uani 0.60 1 d PDU . . F6 F 0.0584(7) -0.0202(8) 0.404(3) 0.314(7) Uani 0.60 1 d PDU . . F7 F 0.0615(7) -0.0663(7) 0.181(4) 0.322(7) Uani 0.60 1 d PDU . . C7A C 0.1345(5) -0.0201(5) 0.252(2) 0.216(5) Uani 0.40 1 d PDU . . C8A C 0.1402(8) -0.0171(7) 0.442(2) 0.224(5) Uani 0.40 1 d PDU . . F1A F 0.2049(10) 0.0689(5) 0.215(3) 0.104(6) Uani 0.40 1 d PD . . F2A F 0.1896(12) 0.0108(11) 0.0007(13) 0.141(8) Uani 0.40 1 d PD . . F3A F 0.1179(6) -0.0708(4) 0.210(3) 0.216(5) Uani 0.40 1 d PDU . . F4A F 0.1008(5) -0.0022(7) 0.217(4) 0.214(5) Uani 0.40 1 d PDU . . F5A F 0.1635(8) -0.0462(8) 0.495(4) 0.227(5) Uani 0.40 1 d PDU . . F6A F 0.0916(6) -0.0381(8) 0.528(4) 0.228(5) Uani 0.40 1 d PDU . . F7A F 0.1711(7) 0.0346(6) 0.497(4) 0.225(5) Uani 0.40 1 d PDU . . 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 0.0621(3) 0.0440(2) 0.0467(3) -0.00572(11) -0.00544(12) 0.01757(15) C1 0.061(2) 0.0503(19) 0.0377(17) -0.0028(14) -0.0054(15) 0.0343(18) C3 0.084(3) 0.065(3) 0.049(2) -0.0124(19) -0.018(2) 0.054(3) C2 0.055(2) 0.0417(17) 0.0383(17) -0.0010(14) -0.0021(15) 0.0274(16) N2 0.0598(19) 0.0506(17) 0.0402(15) -0.0034(13) -0.0028(13) 0.0336(15) C5 0.052(2) 0.065(3) 0.066(3) 0.005(2) -0.008(2) 0.029(2) N1 0.067(2) 0.0531(18) 0.0410(16) -0.0083(13) -0.0081(15) 0.0359(17) C4 0.082(3) 0.065(3) 0.048(2) -0.0106(19) -0.015(2) 0.049(2) O1 0.078(2) 0.071(2) 0.073(2) 0.0020(18) -0.0168(19) 0.031(2) O2 0.0584(19) 0.072(2) 0.089(3) -0.004(2) -0.0116(18) 0.0347(18) C6 0.080(4) 0.118(6) 0.101(5) -0.005(4) -0.018(4) 0.062(4) C7 0.102(5) 0.189(8) 0.63(2) -0.011(10) 0.020(8) 0.077(5) C8 0.109(5) 0.197(8) 0.63(2) -0.011(10) 0.017(8) 0.074(5) F1 0.091(7) 0.164(14) 0.29(2) 0.154(16) 0.005(10) 0.052(8) F2 0.23(3) 0.61(5) 0.146(14) -0.15(2) -0.112(16) 0.32(3) F3 0.104(5) 0.190(8) 0.63(2) -0.010(10) 0.022(9) 0.074(6) F4 0.102(5) 0.185(8) 0.63(2) -0.012(10) 0.021(8) 0.075(6) F5 0.107(5) 0.195(8) 0.63(2) -0.009(10) 0.015(8) 0.081(6) F6 0.110(5) 0.201(8) 0.63(2) -0.012(10) 0.016(8) 0.075(6) F7 0.117(5) 0.202(8) 0.63(2) -0.013(10) 0.016(8) 0.065(6) C7A 0.158(8) 0.179(8) 0.350(12) 0.115(9) 0.130(8) 0.114(7) C8A 0.162(8) 0.186(8) 0.350(12) 0.113(9) 0.136(8) 0.107(7) F1A 0.113(11) 0.078(8) 0.148(13) 0.017(8) -0.012(9) 0.069(9) F2A 0.148(18) 0.27(2) 0.068(8) 0.015(11) -0.021(8) 0.152(16) F3A 0.159(8) 0.178(8) 0.351(13) 0.115(9) 0.127(9) 0.113(7) F4A 0.158(8) 0.179(8) 0.349(13) 0.117(9) 0.128(9) 0.116(7) F5A 0.163(8) 0.187(8) 0.351(13) 0.115(9) 0.137(9) 0.103(7) F6A 0.165(8) 0.190(8) 0.350(13) 0.113(9) 0.139(8) 0.104(7) F7A 0.162(8) 0.189(8) 0.348(13) 0.111(9) 0.138(9) 0.105(7) _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 N2 2.266(3) 8_544 ? Ag1 O2 2.325(4) 6 ? Ag1 N1 2.362(3) . ? Ag1 O1 2.405(4) . ? Ag1 Ag1 3.0564(4) 6 ? C1 N2 1.322(5) . ? C1 C2 1.408(5) . ? C3 C2 1.357(6) . ? C3 C4 1.386(6) . ? C2 C2 1.482(7) 13_557 ? N2 N1 1.342(5) . ? C5 O2 1.226(7) . ? C5 O1 1.238(7) . ? C5 C6 1.563(6) . ? N1 C4 1.324(6) . ? C6 F1 1.352(9) . ? C6 F2 1.360(9) . ? C6 F1A 1.368(9) . ? C6 F2A 1.368(9) . ? C6 C7A 1.498(10) . ? C6 C7 1.541(10) . ? C7 F3 1.332(10) . ? C7 F4 1.360(10) . ? C7 C8 1.534(7) . ? C7 F4A 1.57(3) . ? C7 F7A 1.70(3) . ? C7 F3A 1.746(19) . ? C8 C7A 1.33(2) . ? C8 F5 1.339(10) . ? C8 F6 1.344(10) . ? C8 F7 1.355(10) . ? C7A F3A 1.310(10) . ? C7A F4A 1.319(10) . ? C7A C8A 1.439(7) . ? C8A F7A 1.344(10) . ? C8A F5A 1.354(10) . ? C8A F6A 1.363(10) . ? 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 N2 Ag1 O2 148.45(14) 8_544 6 ? N2 Ag1 N1 118.05(13) 8_544 . ? O2 Ag1 N1 87.61(15) 6 . ? N2 Ag1 O1 101.61(13) 8_544 . ? O2 Ag1 O1 91.89(15) 6 . ? N1 Ag1 O1 97.82(14) . . ? N2 Ag1 Ag1 90.87(9) 8_544 6 ? O2 Ag1 Ag1 82.73(11) 6 6 ? N1 Ag1 Ag1 66.42(9) . 6 ? O1 Ag1 Ag1 163.44(11) . 6 ? N2 Ag1 Ag1 70.12(8) 8_544 8_544 ? O2 Ag1 Ag1 86.75(11) 6 8_544 ? N1 Ag1 Ag1 170.04(9) . 8_544 ? O1 Ag1 Ag1 74.18(11) . 8_544 ? Ag1 Ag1 Ag1 120.864(16) 6 8_544 ? N2 C1 C2 123.4(4) . . ? C2 C3 C4 118.7(4) . . ? C3 C2 C1 115.9(3) . . ? C3 C2 C2 123.7(4) . 13_557 ? C1 C2 C2 120.4(4) . 13_557 ? C1 N2 N1 119.9(3) . . ? C1 N2 Ag1 128.7(3) . 6 ? N1 N2 Ag1 111.3(2) . 6 ? O2 C5 O1 131.1(5) . . ? O2 C5 C6 114.9(5) . . ? O1 C5 C6 113.8(5) . . ? C4 N1 N2 118.8(3) . . ? C4 N1 Ag1 128.7(3) . . ? N2 N1 Ag1 112.1(2) . . ? N1 C4 C3 123.3(4) . . ? C5 O1 Ag1 121.9(4) . . ? C5 O2 Ag1 118.2(3) . 8_544 ? F1 C6 F2 108.6(9) . . ? F1A C6 F2A 106.6(9) . . ? F1 C6 C7A 115.4(11) . . ? F1A C6 C7A 108.6(12) . . ? F2A C6 C7A 108.9(15) . . ? F1 C6 C7 109.1(13) . . ? F2 C6 C7 104.2(13) . . ? F1 C6 C5 114.8(9) . . ? F2 C6 C5 111.3(11) . . ? C7 C6 C5 108.4(8) . . ? F3 C7 F4 109.7(12) . . ? F3 C7 C8 110.4(16) . . ? F4 C7 C8 96.7(14) . . ? F3 C7 C6 124.0(14) . . ? F4 C7 C6 93.5(15) . . ? C8 C7 C6 116.7(13) . . ? F5 C8 F6 108.4(10) . . ? F5 C8 F7 109.4(11) . . ? F6 C8 F7 106.1(10) . . ? F5 C8 C7 111.2(16) . . ? F6 C8 C7 112.6(14) . . ? F7 C8 C7 108.9(15) . . ? F3A C7A F4A 116.4(11) . . ? F3A C7A C8A 105.9(9) . . ? F4A C7A C8A 104.8(19) . . ? F7A C8A F5A 109.0(11) . . ? F7A C8A F6A 107.4(10) . . ? F5A C8A F6A 107.0(10) . . ? F7A C8A C7A 111.2(18) . . ? F5A C8A C7A 109.2(19) . . ? F6A C8A C7A 112.9(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.890 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.119 #==============================================================================