# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Konstantin V. Domasevitch' 'Alexander N Chernega' 'Anna S. Degtyarenko' 'Harald Krautscheid' 'Eduard B Rusanov' 'Pavlo V Solntsev' _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_email DK@MAIL.UNIV.KIEV.UA _publ_section_title ; Copper(I) and silver(I) coordination frameworks involving extended bipyridazine bridges ; # Attachment 'cif_data.cif' #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_(1) _database_code_depnum_ccdc_archive 'CCDC 685682' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) Dithionate bis(Acetonitrile) complex with 1,4-bi(pyridazin-4-yl)benzene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Cu2 N6 O6 S2' _chemical_formula_weight 603.57 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.3471(6) _cell_length_b 18.9283(11) _cell_length_c 12.4791(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.718(8) _cell_angle_gamma 90.00 _cell_volume 2161.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.12 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 2.212 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6105 _exptl_absorpt_correction_T_max 0.6738 _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 9065 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 28.12 _reflns_number_total 2606 _reflns_number_gt 2153 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms were located from difference maps and then refined a riding, with C---H (aromatic) distances constrained to 0.94 \%A, and C---H (methyl) distances constrained to 0.97 \%A, with U~iso~(H) = 1.2U~eq~ (parent aromatic carbon atoms) and U~iso~(H) = 1.5U~eq~ (parent methyl cartbon atom). The bipyridazine ligand lies across an inversion centre and the dithionate anion lies across twofold axis. ; _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^)+(0.0516P)^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 2606 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 Cu1 Cu 0.04797(3) 0.418835(13) 0.530166(18) 0.02712(10) Uani 1 1 d . . . S1 S -0.09029(5) 0.28933(2) 0.68150(3) 0.02068(12) Uani 1 1 d . . . O1 O -0.07845(17) 0.35520(8) 0.62431(13) 0.0371(4) Uani 1 1 d . . . O2 O -0.0662(2) 0.22689(8) 0.62124(12) 0.0409(4) Uani 1 1 d . . . O3 O -0.21931(17) 0.28690(9) 0.72844(12) 0.0367(4) Uani 1 1 d . . . N1 N 0.12176(18) 0.49728(8) 0.64054(12) 0.0242(3) Uani 1 1 d . . . N2 N 0.09979(18) 0.56503(8) 0.60553(12) 0.0215(3) Uani 1 1 d . . . N3 N 0.2228(2) 0.36085(11) 0.53621(15) 0.0364(4) Uani 1 1 d . . . C1 C 0.2154(2) 0.48390(9) 0.73432(14) 0.0240(4) Uani 1 1 d . . . H1 H 0.2282 0.4366 0.7573 0.029 Uiso 1 1 calc R . . C2 C 0.2961(2) 0.53596(9) 0.80074(13) 0.0191(4) Uani 1 1 d . . . C3 C 0.2746(2) 0.60456(10) 0.76258(15) 0.0245(4) Uani 1 1 d . . . H3 H 0.3257 0.6424 0.8016 0.029 Uiso 1 1 calc R . . C4 C 0.1751(2) 0.61607(9) 0.66473(15) 0.0247(4) Uani 1 1 d . . . H4 H 0.1605 0.6627 0.6391 0.030 Uiso 1 1 calc R . . C5 C 0.4009(2) 0.51707(9) 0.90281(13) 0.0178(3) Uani 1 1 d . . . C6 C 0.3816(2) 0.45565(9) 0.96081(14) 0.0218(4) Uani 1 1 d . . . H6 H 0.3021 0.4256 0.9348 0.026 Uiso 1 1 calc R . . C7 C 0.4800(2) 0.43906(10) 1.05684(14) 0.0215(4) Uani 1 1 d . . . H7 H 0.4662 0.3977 1.0952 0.026 Uiso 1 1 calc R . . C8 C 0.3219(3) 0.32623(13) 0.56406(16) 0.0340(5) Uani 1 1 d . . . C9 C 0.4493(3) 0.28146(16) 0.6008(2) 0.0459(6) Uani 1 1 d . . . H9A H 0.5267 0.3091 0.6451 0.069 Uiso 1 1 calc R . . H9B H 0.4826 0.2627 0.5378 0.069 Uiso 1 1 calc R . . H9C H 0.4232 0.2427 0.6441 0.069 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 Cu1 0.02665(16) 0.02754(14) 0.02111(13) 0.00407(9) -0.00942(9) -0.00021(9) S1 0.0217(3) 0.0200(2) 0.0200(2) 0.00024(16) 0.00349(16) -0.00038(16) O1 0.0306(9) 0.0341(8) 0.0446(9) 0.0210(7) 0.0030(7) 0.0041(6) O2 0.0563(11) 0.0343(8) 0.0292(7) -0.0124(6) 0.0018(7) 0.0064(7) O3 0.0228(8) 0.0546(10) 0.0330(8) -0.0036(7) 0.0065(6) -0.0092(7) N1 0.0273(9) 0.0217(7) 0.0184(7) 0.0048(6) -0.0074(6) -0.0038(6) N2 0.0221(9) 0.0213(7) 0.0170(7) 0.0041(5) -0.0058(6) 0.0013(6) N3 0.0313(11) 0.0447(11) 0.0325(9) 0.0087(8) 0.0051(8) 0.0052(8) C1 0.0292(11) 0.0195(8) 0.0180(8) 0.0050(6) -0.0077(7) -0.0040(7) C2 0.0204(9) 0.0211(8) 0.0133(7) 0.0024(6) -0.0025(6) -0.0016(7) C3 0.0281(11) 0.0217(8) 0.0193(8) 0.0001(7) -0.0057(7) -0.0026(7) C4 0.0284(11) 0.0190(9) 0.0220(9) 0.0045(7) -0.0060(7) 0.0011(7) C5 0.0195(9) 0.0191(8) 0.0124(7) 0.0009(6) -0.0028(6) -0.0008(6) C6 0.0212(10) 0.0228(8) 0.0177(8) 0.0023(6) -0.0049(7) -0.0068(7) C7 0.0245(10) 0.0207(8) 0.0163(8) 0.0062(6) -0.0027(7) -0.0042(7) C8 0.0302(12) 0.0466(13) 0.0250(10) 0.0052(9) 0.0047(8) 0.0033(10) C9 0.0354(14) 0.0658(16) 0.0354(12) 0.0087(11) 0.0047(10) 0.0186(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.958(2) . ? Cu1 N2 1.9794(15) 5_566 ? Cu1 N1 2.0474(15) . ? Cu1 O1 2.1888(15) . ? S1 O2 1.4426(15) . ? S1 O3 1.4444(16) . ? S1 O1 1.4521(15) . ? S1 S1 2.1446(9) 2_556 ? N1 C1 1.336(2) . ? N1 N2 1.357(2) . ? N2 C4 1.328(2) . ? N2 Cu1 1.9794(15) 5_566 ? N3 C8 1.130(3) . ? C1 C2 1.405(2) . ? C1 H1 0.9400 . ? C2 C3 1.384(3) . ? C2 C5 1.484(2) . ? C3 C4 1.393(2) . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C7 1.398(3) 5_667 ? C5 C6 1.400(2) . ? C6 C7 1.390(2) . ? C6 H6 0.9400 . ? C7 C5 1.398(3) 5_667 ? C7 H7 0.9400 . ? C8 C9 1.457(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? 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 Cu1 N2 123.47(8) . 5_566 ? N3 Cu1 N1 102.48(8) . . ? N2 Cu1 N1 123.02(6) 5_566 . ? N3 Cu1 O1 102.02(7) . . ? N2 Cu1 O1 100.67(6) 5_566 . ? N1 Cu1 O1 100.53(7) . . ? O2 S1 O3 114.63(10) . . ? O2 S1 O1 114.31(10) . . ? O3 S1 O1 112.32(10) . . ? O2 S1 S1 103.58(7) . 2_556 ? O3 S1 S1 105.28(7) . 2_556 ? O1 S1 S1 105.40(7) . 2_556 ? S1 O1 Cu1 147.11(10) . . ? C1 N1 N2 119.39(15) . . ? C1 N1 Cu1 121.55(13) . . ? N2 N1 Cu1 117.42(10) . . ? C4 N2 N1 118.67(14) . . ? C4 N2 Cu1 124.25(12) . 5_566 ? N1 N2 Cu1 117.06(11) . 5_566 ? C8 N3 Cu1 164.31(18) . . ? N1 C1 C2 124.18(16) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 115.61(15) . . ? C3 C2 C5 123.09(15) . . ? C1 C2 C5 121.26(15) . . ? C2 C3 C4 118.21(17) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? N2 C4 C3 123.91(17) . . ? N2 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C7 C5 C6 118.91(15) 5_667 . ? C7 C5 C2 120.28(15) 5_667 . ? C6 C5 C2 120.80(15) . . ? C7 C6 C5 120.08(16) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C5 121.01(16) . 5_667 ? C6 C7 H7 119.5 . . ? C5 C7 H7 119.5 5_667 . ? N3 C8 C9 179.5(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Cu1 -47.7(2) . . . . ? O3 S1 O1 Cu1 179.46(17) . . . . ? S1 S1 O1 Cu1 65.3(2) 2_556 . . . ? N3 Cu1 O1 S1 -5.2(2) . . . . ? N2 Cu1 O1 S1 122.65(19) 5_566 . . . ? N1 Cu1 O1 S1 -110.6(2) . . . . ? N3 Cu1 N1 C1 -38.97(17) . . . . ? N2 Cu1 N1 C1 176.20(15) 5_566 . . . ? O1 Cu1 N1 C1 65.99(17) . . . . ? N3 Cu1 N1 N2 126.32(15) . . . . ? N2 Cu1 N1 N2 -18.5(2) 5_566 . . . ? O1 Cu1 N1 N2 -128.72(14) . . . . ? C1 N1 N2 C4 1.5(3) . . . . ? Cu1 N1 N2 C4 -164.09(15) . . . . ? C1 N1 N2 Cu1 -176.98(15) . . . 5_566 ? Cu1 N1 N2 Cu1 17.40(19) . . . 5_566 ? N2 Cu1 N3 C8 -156.8(7) 5_566 . . . ? N1 Cu1 N3 C8 58.6(8) . . . . ? O1 Cu1 N3 C8 -45.2(8) . . . . ? N2 N1 C1 C2 -0.6(3) . . . . ? Cu1 N1 C1 C2 164.40(16) . . . . ? N1 C1 C2 C3 -0.7(3) . . . . ? N1 C1 C2 C5 -178.63(19) . . . . ? C1 C2 C3 C4 1.1(3) . . . . ? C5 C2 C3 C4 178.94(19) . . . . ? N1 N2 C4 C3 -1.2(3) . . . . ? Cu1 N2 C4 C3 177.24(16) 5_566 . . . ? C2 C3 C4 N2 -0.2(3) . . . . ? C3 C2 C5 C7 -24.3(3) . . . 5_667 ? C1 C2 C5 C7 153.43(19) . . . 5_667 ? C3 C2 C5 C6 155.07(19) . . . . ? C1 C2 C5 C6 -27.2(3) . . . . ? C7 C5 C6 C7 0.0(3) 5_667 . . . ? C2 C5 C6 C7 -179.39(18) . . . . ? C5 C6 C7 C5 0.0(3) . . . 5_667 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.631 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.086 #----------------------------------------------------# data_(2) _database_code_depnum_ccdc_archive 'CCDC 685683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) Tetrafluoroborate 4:5 complex with 1,4-bi(pyridazin-4-yl)benzene, solvate with 4 Chloroform ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H54 B4 Cl12 Cu4 F16 N20' _chemical_formula_weight 2250.17 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5703(9) _cell_length_b 13.7895(13) _cell_length_c 14.1629(12) _cell_angle_alpha 94.203(11) _cell_angle_beta 93.205(11) _cell_angle_gamma 107.835(10) _cell_volume 2322.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 27.08 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7230 _exptl_absorpt_correction_T_max 0.7952 _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 19140 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.08 _reflns_number_total 10016 _reflns_number_gt 6091 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All CH (aromatic) H atoms were located from difference maps and then refined a riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Both independent solvate chloroform molecules are disordered: one of them shows very typical 'rotational' disorder, while other one is disordered over two very closely separated positions. Contributions of the disorder components were refined (partial occupancy factors are 0.42/0.58 and 0.43/0.57). Atoms of these disordered chloroform molecules were left isotropic and the hydrogen atoms were not added. Standard geometry restraints (C---Cl bond lengths and Cl---C---Cl bond angles) were applied (generation in total 24 restraints) in order to improve the refinement stability. One of the BF~4~^-^ anions is possibly disordered, as was indicated by the relatively high values for the thermal motion. We were not successful to resolve the possible disorder. All atoms of the counter anions were refined anisotropically and without any constraints in the geometry. There are three independent bipyridazine molecules in the structure. Two of them are situated in general positions and the third one lies across an inversion centre. ; _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^)+(0.1005P)^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 10016 _refine_ls_number_parameters 576 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 Cu1 Cu 0.21412(4) 0.18221(3) 0.02312(3) 0.02527(14) Uani 1 1 d . . . Cu2 Cu 0.38379(4) 0.17190(3) 0.18579(3) 0.02526(14) Uani 1 1 d . . . B1 B 0.6504(5) -0.0360(5) 0.3003(4) 0.0470(14) Uani 1 1 d . . . F1 F 0.7374(3) 0.0515(3) 0.2823(2) 0.0597(8) Uani 1 1 d . . . F2 F 0.5511(2) -0.0272(3) 0.2616(2) 0.0637(9) Uani 1 1 d . . . F3 F 0.6488(3) -0.0401(3) 0.3964(2) 0.0663(9) Uani 1 1 d . . . F4 F 0.6706(4) -0.1200(3) 0.2556(3) 0.0805(11) Uani 1 1 d . . . B2 B 0.2149(9) 0.4833(8) -0.2661(8) 0.095(3) Uani 1 1 d . . . F5 F 0.1263(5) 0.4310(4) -0.3240(4) 0.137(2) Uani 1 1 d . . . F6 F 0.2498(6) 0.4312(4) -0.2015(5) 0.151(3) Uani 1 1 d . . . F7 F 0.3068(6) 0.5167(6) -0.3261(6) 0.166(3) Uani 1 1 d . . . F8 F 0.2186(5) 0.5778(4) -0.2304(4) 0.1253(19) Uani 1 1 d . . . N1 N 0.4922(3) 0.1796(2) 0.2967(2) 0.0283(7) Uani 1 1 d . . . N2 N 0.4511(3) 0.1370(3) 0.3748(3) 0.0407(9) Uani 1 1 d . . . N3 N 1.1040(3) 0.1790(2) 0.9140(2) 0.0277(7) Uani 1 1 d . . . N4 N 0.9940(3) 0.1544(3) 0.9286(3) 0.0454(10) Uani 1 1 d . . . N5 N 0.2934(3) 0.0721(2) 0.0011(2) 0.0247(7) Uani 1 1 d . . . N6 N 0.3592(3) 0.0610(2) 0.0763(2) 0.0236(6) Uani 1 1 d . . . N7 N 0.4068(3) -0.6872(2) 0.1367(2) 0.0291(7) Uani 1 1 d . . . N8 N 0.3325(3) -0.6805(2) 0.0668(2) 0.0260(7) Uani 1 1 d . . . N9 N 0.1453(3) 0.1392(3) 0.1480(2) 0.0295(7) Uani 1 1 d . . . N10 N 0.2189(3) 0.1338(3) 0.2191(2) 0.0286(7) Uani 1 1 d . . . C1 C 0.5226(4) 0.1419(4) 0.4492(3) 0.0426(11) Uani 1 1 d . . . H1 H 0.4933 0.1106 0.5029 0.051 Uiso 1 1 calc R . . C2 C 0.6391(3) 0.1905(3) 0.4531(3) 0.0321(9) Uani 1 1 d . . . C3 C 0.6766(4) 0.2349(4) 0.3738(3) 0.0402(10) Uani 1 1 d . . . H3 H 0.7532 0.2702 0.3713 0.048 Uiso 1 1 calc R . . C4 C 0.6008(4) 0.2275(3) 0.2966(3) 0.0367(10) Uani 1 1 d . . . H4 H 0.6277 0.2578 0.2417 0.044 Uiso 1 1 calc R . . C5 C 0.7152(4) 0.1898(3) 0.5367(3) 0.0374(10) Uani 1 1 d . . . C6 C 0.8291(5) 0.2421(7) 0.5374(5) 0.099(3) Uani 1 1 d . . . H6 H 0.8560 0.2791 0.4859 0.119 Uiso 1 1 calc R . . C7 C 0.9035(5) 0.2405(7) 0.6127(5) 0.095(3) Uani 1 1 d . . . H7 H 0.9799 0.2771 0.6117 0.114 Uiso 1 1 calc R . . C8 C 0.8676(3) 0.1861(3) 0.6894(3) 0.0349(10) Uani 1 1 d . . . C9 C 0.7556(4) 0.1385(5) 0.6904(3) 0.0562(15) Uani 1 1 d . . . H9 H 0.7285 0.1040 0.7432 0.067 Uiso 1 1 calc R . . C10 C 0.6799(4) 0.1399(5) 0.6148(3) 0.0533(14) Uani 1 1 d . . . H10 H 0.6031 0.1057 0.6176 0.064 Uiso 1 1 calc R . . C11 C 0.9227(4) 0.1573(5) 0.8566(3) 0.0497(13) Uani 1 1 d . . . H11 H 0.8463 0.1401 0.8676 0.060 Uiso 1 1 calc R . . C12 C 0.9520(3) 0.1839(3) 0.7662(3) 0.0319(9) Uani 1 1 d . . . C13 C 1.0639(4) 0.2063(4) 0.7531(3) 0.0409(11) Uani 1 1 d . . . H13 H 1.0910 0.2241 0.6942 0.049 Uiso 1 1 calc R . . C14 C 1.1365(4) 0.2021(4) 0.8296(3) 0.0372(10) Uani 1 1 d . . . H14 H 1.2130 0.2166 0.8203 0.045 Uiso 1 1 calc R . . C15 C 0.3861(3) -0.0251(3) 0.0796(3) 0.0249(8) Uani 1 1 d . . . H15 H 0.4332 -0.0302 0.1316 0.030 Uiso 1 1 calc R . . C16 C 0.3487(3) -0.1080(3) 0.0104(3) 0.0271(8) Uani 1 1 d . . . C17 C 0.2868(4) -0.0935(3) -0.0684(3) 0.0356(10) Uani 1 1 d . . . H17 H 0.2619 -0.1441 -0.1199 0.043 Uiso 1 1 calc R . . C18 C 0.2627(4) -0.0014(3) -0.0686(3) 0.0307(9) Uani 1 1 d . . . H18 H 0.2216 0.0088 -0.1224 0.037 Uiso 1 1 calc R . . C19 C 0.3694(3) -0.2069(3) 0.0235(3) 0.0285(8) Uani 1 1 d . . . C20 C 0.3061(5) -0.2952(3) -0.0278(4) 0.0513(14) Uani 1 1 d . . . H20 H 0.2524 -0.2927 -0.0757 0.062 Uiso 1 1 calc R . . C21 C 0.3195(5) -0.3898(3) -0.0105(4) 0.0533(14) Uani 1 1 d . . . H21 H 0.2755 -0.4495 -0.0474 0.064 Uiso 1 1 calc R . . C22 C 0.3967(4) -0.3959(3) 0.0601(3) 0.0332(9) Uani 1 1 d . . . C23 C 0.4658(4) -0.3053(3) 0.1074(4) 0.0457(12) Uani 1 1 d . . . H23 H 0.5232 -0.3071 0.1521 0.055 Uiso 1 1 calc R . . C24 C 0.4524(4) -0.2122(3) 0.0905(4) 0.0458(12) Uani 1 1 d . . . H24 H 0.4996 -0.1518 0.1245 0.055 Uiso 1 1 calc R . . C25 C 0.3326(3) -0.5890(3) 0.0424(3) 0.0294(8) Uani 1 1 d . . . H25 H 0.2810 -0.5869 -0.0074 0.035 Uiso 1 1 calc R . . C26 C 0.4044(3) -0.4958(3) 0.0860(3) 0.0312(9) Uani 1 1 d . . . C27 C 0.4811(4) -0.5048(3) 0.1558(4) 0.0473(13) Uani 1 1 d . . . H27 H 0.5341 -0.4461 0.1876 0.057 Uiso 1 1 calc R . . C28 C 0.4790(4) -0.6012(3) 0.1782(3) 0.0418(11) Uani 1 1 d . . . H28 H 0.5320 -0.6061 0.2257 0.050 Uiso 1 1 calc R . . C29 C 0.1833(3) 0.1036(3) 0.3016(3) 0.0300(8) Uani 1 1 d . . . H29 H 0.2369 0.1010 0.3496 0.036 Uiso 1 1 calc R . . C30 C 0.0707(3) 0.0753(3) 0.3215(3) 0.0311(9) Uani 1 1 d . . . C31 C -0.0030(4) 0.0828(4) 0.2485(3) 0.0439(11) Uani 1 1 d . . . H31 H -0.0801 0.0662 0.2563 0.053 Uiso 1 1 calc R . . C32 C 0.0376(4) 0.1147(4) 0.1643(3) 0.0413(11) Uani 1 1 d . . . H32 H -0.0137 0.1195 0.1154 0.050 Uiso 1 1 calc R . . C33 C 0.1082(5) 0.0187(7) 0.4797(4) 0.090(3) Uani 1 1 d . . . H33 H 0.1839 0.0320 0.4675 0.108 Uiso 1 1 calc R . . C34 C 0.0349(3) 0.0370(3) 0.4139(3) 0.0341(9) Uani 1 1 d . . . C35 C -0.0722(4) 0.0194(7) 0.4355(4) 0.084(3) Uani 1 1 d . . . H35 H -0.1238 0.0332 0.3921 0.101 Uiso 1 1 calc R . . C40 C 0.0252(17) 0.5041(10) 0.1087(14) 0.32(4) Uiso 0.429(14) 1 d PD . . Cl1 Cl 0.0331(8) 0.3853(6) 0.0672(8) 0.171(5) Uiso 0.429(14) 1 d PD . . Cl2 Cl 0.1437(10) 0.5778(8) 0.1799(9) 0.197(6) Uiso 0.429(14) 1 d PD . . Cl3 Cl -0.0112(12) 0.5699(9) 0.0185(11) 0.243(7) Uiso 0.429(14) 1 d PD . . C40A C 0.0468(15) 0.4834(15) 0.1763(16) 0.196(12) Uiso 0.571(14) 1 d PD . . Cl1A Cl 0.029(2) 0.3591(14) 0.130(2) 0.452(14) Uiso 0.571(14) 1 d PD . . Cl2A Cl 0.1799(12) 0.5384(11) 0.2347(12) 0.288(7) Uiso 0.571(14) 1 d PD . . Cl3A Cl 0.020(2) 0.5590(19) 0.091(2) 0.451(15) Uiso 0.571(14) 1 d PD . . C41 C 0.3700(10) 0.3649(10) 0.5272(7) 0.232(8) Uiso 1 1 d D . . Cl4 Cl 0.4916(11) 0.3563(12) 0.5952(9) 0.269(9) Uiso 0.419(12) 1 d PD . . Cl5 Cl 0.3871(9) 0.3672(7) 0.4091(6) 0.176(5) Uiso 0.419(12) 1 d PD . . Cl6 Cl 0.2632(9) 0.2500(8) 0.5437(8) 0.207(6) Uiso 0.419(12) 1 d PD . . Cl4A Cl 0.3669(10) 0.2802(8) 0.6037(7) 0.234(5) Uiso 0.581(12) 1 d PD . . Cl5A Cl 0.4820(12) 0.3911(12) 0.4542(10) 0.306(7) Uiso 0.581(12) 1 d PD . . Cl6A Cl 0.2430(13) 0.337(2) 0.4546(15) 0.490(16) Uiso 0.581(12) 1 d PD . . 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 Cu1 0.0260(3) 0.0280(2) 0.0222(2) 0.00591(18) -0.00763(19) 0.00991(19) Cu2 0.0244(2) 0.0280(2) 0.0232(2) 0.00589(18) -0.00801(19) 0.00869(19) B1 0.039(3) 0.074(4) 0.036(3) 0.009(3) -0.001(2) 0.030(3) F1 0.0469(17) 0.086(2) 0.0479(16) 0.0144(16) 0.0046(14) 0.0216(17) F2 0.0461(16) 0.082(2) 0.0653(19) -0.0061(17) -0.0197(15) 0.0309(16) F3 0.062(2) 0.101(3) 0.0416(16) 0.0215(16) 0.0094(15) 0.0286(19) F4 0.105(3) 0.091(3) 0.071(2) 0.0087(19) 0.010(2) 0.068(2) B2 0.079(6) 0.087(6) 0.096(7) -0.003(5) -0.034(6) -0.001(5) F5 0.107(4) 0.110(3) 0.143(5) 0.018(3) -0.068(4) -0.026(3) F6 0.152(5) 0.094(3) 0.173(6) 0.021(4) -0.081(5) 0.001(3) F7 0.110(5) 0.185(6) 0.172(6) -0.042(5) -0.011(5) 0.014(4) F8 0.156(5) 0.082(3) 0.109(4) 0.010(3) -0.021(4) 0.000(3) N1 0.0275(17) 0.0326(16) 0.0243(15) 0.0074(13) -0.0094(14) 0.0097(14) N2 0.0271(18) 0.060(2) 0.0331(19) 0.0160(17) -0.0108(16) 0.0097(17) N3 0.0244(16) 0.0350(17) 0.0237(15) 0.0063(13) -0.0067(14) 0.0103(14) N4 0.0295(19) 0.078(3) 0.0294(18) 0.0186(19) -0.0071(16) 0.0155(19) N5 0.0267(16) 0.0244(14) 0.0245(15) 0.0074(12) -0.0045(13) 0.0101(13) N6 0.0253(16) 0.0228(14) 0.0238(15) 0.0051(12) -0.0052(13) 0.0099(13) N7 0.0290(17) 0.0255(15) 0.0328(17) 0.0065(13) -0.0104(14) 0.0097(13) N8 0.0274(16) 0.0217(14) 0.0290(16) 0.0053(12) -0.0080(14) 0.0087(13) N9 0.0251(16) 0.0427(18) 0.0219(15) 0.0096(14) -0.0029(13) 0.0119(15) N10 0.0244(16) 0.0385(17) 0.0227(15) 0.0076(13) -0.0049(13) 0.0096(14) C1 0.030(2) 0.066(3) 0.030(2) 0.023(2) -0.0051(18) 0.009(2) C2 0.029(2) 0.039(2) 0.0272(19) 0.0095(17) -0.0096(17) 0.0105(18) C3 0.026(2) 0.053(3) 0.039(2) 0.015(2) -0.0098(19) 0.0072(19) C4 0.031(2) 0.048(2) 0.031(2) 0.0147(19) -0.0049(18) 0.0109(19) C5 0.032(2) 0.044(2) 0.032(2) 0.0118(18) -0.0144(19) 0.0070(19) C6 0.038(3) 0.175(8) 0.067(4) 0.082(5) -0.019(3) -0.007(4) C7 0.031(3) 0.168(7) 0.067(4) 0.071(5) -0.018(3) -0.006(4) C8 0.031(2) 0.041(2) 0.030(2) 0.0111(18) -0.0122(18) 0.0092(18) C9 0.032(3) 0.101(4) 0.034(2) 0.037(3) -0.002(2) 0.013(3) C10 0.024(2) 0.091(4) 0.041(3) 0.031(3) -0.006(2) 0.007(2) C11 0.027(2) 0.089(4) 0.034(2) 0.020(2) -0.0063(19) 0.017(2) C12 0.032(2) 0.036(2) 0.0270(19) 0.0069(16) -0.0103(17) 0.0106(17) C13 0.035(2) 0.062(3) 0.025(2) 0.0149(19) -0.0063(18) 0.013(2) C14 0.025(2) 0.055(3) 0.031(2) 0.0149(19) -0.0053(18) 0.0103(19) C15 0.0250(18) 0.0255(17) 0.0241(17) 0.0072(14) -0.0036(15) 0.0077(15) C16 0.0275(19) 0.0267(18) 0.0304(19) 0.0091(15) 0.0025(16) 0.0118(16) C17 0.051(3) 0.030(2) 0.0272(19) -0.0004(16) -0.0089(19) 0.0174(19) C18 0.040(2) 0.0311(19) 0.0233(18) 0.0046(15) -0.0071(17) 0.0164(18) C19 0.032(2) 0.0235(17) 0.033(2) 0.0071(15) 0.0012(17) 0.0124(16) C20 0.072(3) 0.028(2) 0.053(3) 0.002(2) -0.030(3) 0.020(2) C21 0.075(4) 0.025(2) 0.055(3) -0.003(2) -0.033(3) 0.017(2) C22 0.037(2) 0.0238(18) 0.040(2) 0.0057(16) -0.0041(19) 0.0113(17) C23 0.043(3) 0.031(2) 0.062(3) 0.002(2) -0.024(2) 0.0145(19) C24 0.044(3) 0.026(2) 0.065(3) 0.001(2) -0.022(2) 0.0127(19) C25 0.030(2) 0.0276(18) 0.0305(19) 0.0064(16) -0.0085(17) 0.0102(16) C26 0.032(2) 0.0248(18) 0.036(2) 0.0053(16) -0.0064(18) 0.0092(16) C27 0.050(3) 0.025(2) 0.059(3) 0.0040(19) -0.027(2) 0.0039(19) C28 0.045(3) 0.027(2) 0.049(3) 0.0054(18) -0.024(2) 0.0080(18) C29 0.0251(19) 0.044(2) 0.0214(17) 0.0084(16) -0.0016(15) 0.0116(17) C30 0.028(2) 0.043(2) 0.0231(18) 0.0084(16) -0.0035(16) 0.0113(18) C31 0.023(2) 0.077(3) 0.032(2) 0.020(2) -0.0016(18) 0.013(2) C32 0.025(2) 0.073(3) 0.027(2) 0.017(2) -0.0043(17) 0.015(2) C33 0.027(3) 0.201(8) 0.049(3) 0.062(4) 0.007(2) 0.033(4) C34 0.027(2) 0.050(2) 0.0239(18) 0.0088(17) -0.0037(17) 0.0104(19) C35 0.030(3) 0.187(8) 0.043(3) 0.063(4) 0.005(2) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.005(3) 1_454 ? Cu1 N8 2.044(3) 1_565 ? Cu1 N9 2.059(3) . ? Cu1 N5 2.071(3) . ? Cu2 N1 1.996(3) . ? Cu2 N6 2.036(3) . ? Cu2 N7 2.054(3) 1_565 ? Cu2 N10 2.067(3) . ? B1 F3 1.367(6) . ? B1 F4 1.377(7) . ? B1 F2 1.379(5) . ? B1 F1 1.409(7) . ? B2 F5 1.323(9) . ? B2 F6 1.339(11) . ? B2 F8 1.349(11) . ? B2 F7 1.452(13) . ? N1 C4 1.322(5) . ? N1 N2 1.344(5) . ? N2 C1 1.330(5) . ? N3 C14 1.314(5) . ? N3 N4 1.351(5) . ? N3 Cu1 2.005(3) 1_656 ? N4 C11 1.330(5) . ? N5 C18 1.312(5) . ? N5 N6 1.359(4) . ? N6 C15 1.334(4) . ? N7 C28 1.324(5) . ? N7 N8 1.350(4) . ? N7 Cu2 2.054(3) 1_545 ? N8 C25 1.332(5) . ? N8 Cu1 2.044(3) 1_545 ? N9 C32 1.329(5) . ? N9 N10 1.350(4) . ? N10 C29 1.324(5) . ? C1 C2 1.407(6) . ? C1 H1 0.9400 . ? C2 C3 1.356(6) . ? C2 C5 1.483(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C10 1.369(7) . ? C5 C6 1.391(7) . ? C6 C7 1.384(7) . ? C6 H6 0.9400 . ? C7 C8 1.382(7) . ? C7 H7 0.9400 . ? C8 C9 1.360(7) . ? C8 C12 1.486(5) . ? C9 C10 1.397(6) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.397(6) . ? C11 H11 0.9400 . ? C12 C13 1.371(6) . ? C13 C14 1.392(5) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.393(5) . ? C15 H15 0.9400 . ? C16 C17 1.386(5) . ? C16 C19 1.487(5) . ? C17 C18 1.393(5) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.362(6) . ? C19 C24 1.392(5) . ? C20 C21 1.402(6) . ? C20 H20 0.9400 . ? C21 C22 1.379(6) . ? C21 H21 0.9400 . ? C22 C23 1.383(6) . ? C22 C26 1.481(5) . ? C23 C24 1.382(6) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 C26 1.399(5) . ? C25 H25 0.9400 . ? C26 C27 1.382(5) . ? C27 C28 1.382(6) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? C29 C30 1.400(6) . ? C29 H29 0.9400 . ? C30 C31 1.381(5) . ? C30 C34 1.487(6) . ? C31 C32 1.372(6) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.365(6) . ? C33 C35 1.390(8) 2_556 ? C33 H33 0.9400 . ? C34 C35 1.350(7) . ? C35 C33 1.390(8) 2_556 ? C35 H35 0.9400 . ? C40 Cl1 1.733(10) . ? C40 Cl3 1.738(10) . ? C40 Cl2 1.739(10) . ? C40A Cl3A 1.732(10) . ? C40A Cl1A 1.732(10) . ? C40A Cl2A 1.743(10) . ? C41 Cl4A 1.644(8) . ? C41 Cl5 1.700(9) . ? C41 Cl5A 1.757(9) . ? C41 Cl6A 1.771(9) . ? C41 Cl6 1.776(9) . ? C41 Cl4 1.801(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N8 117.37(12) 1_454 1_565 ? N3 Cu1 N9 115.45(13) 1_454 . ? N8 Cu1 N9 102.04(13) 1_565 . ? N3 Cu1 N5 112.24(12) 1_454 . ? N8 Cu1 N5 108.84(12) 1_565 . ? N9 Cu1 N5 98.94(13) . . ? N1 Cu2 N6 120.11(12) . . ? N1 Cu2 N7 111.49(13) . 1_565 ? N6 Cu2 N7 111.14(12) . 1_565 ? N1 Cu2 N10 113.55(13) . . ? N6 Cu2 N10 96.61(13) . . ? N7 Cu2 N10 101.56(13) 1_565 . ? F3 B1 F4 112.2(5) . . ? F3 B1 F2 110.8(5) . . ? F4 B1 F2 109.7(4) . . ? F3 B1 F1 108.7(4) . . ? F4 B1 F1 107.7(4) . . ? F2 B1 F1 107.7(4) . . ? F5 B2 F6 116.3(9) . . ? F5 B2 F8 117.1(9) . . ? F6 B2 F8 112.6(8) . . ? F5 B2 F7 105.9(9) . . ? F6 B2 F7 105.6(9) . . ? F8 B2 F7 96.2(8) . . ? C4 N1 N2 119.8(3) . . ? C4 N1 Cu2 122.3(3) . . ? N2 N1 Cu2 117.9(2) . . ? C1 N2 N1 118.3(4) . . ? C14 N3 N4 119.5(3) . . ? C14 N3 Cu1 121.7(3) . 1_656 ? N4 N3 Cu1 118.8(2) . 1_656 ? C11 N4 N3 118.0(4) . . ? C18 N5 N6 118.1(3) . . ? C18 N5 Cu1 123.7(2) . . ? N6 N5 Cu1 115.8(2) . . ? C15 N6 N5 119.7(3) . . ? C15 N6 Cu2 125.8(2) . . ? N5 N6 Cu2 113.6(2) . . ? C28 N7 N8 118.2(3) . . ? C28 N7 Cu2 123.9(2) . 1_545 ? N8 N7 Cu2 117.2(2) . 1_545 ? C25 N8 N7 119.8(3) . . ? C25 N8 Cu1 126.5(2) . 1_545 ? N7 N8 Cu1 113.1(2) . 1_545 ? C32 N9 N10 117.9(3) . . ? C32 N9 Cu1 126.9(2) . . ? N10 N9 Cu1 115.2(2) . . ? C29 N10 N9 120.4(3) . . ? C29 N10 Cu2 124.9(2) . . ? N9 N10 Cu2 114.7(2) . . ? N2 C1 C2 124.6(4) . . ? N2 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C3 C2 C1 115.2(3) . . ? C3 C2 C5 122.7(4) . . ? C1 C2 C5 122.1(4) . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C4 C3 122.9(4) . . ? N1 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C10 C5 C6 117.1(4) . . ? C10 C5 C2 123.6(4) . . ? C6 C5 C2 119.3(4) . . ? C7 C6 C5 121.1(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 121.3(5) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C7 117.5(4) . . ? C9 C8 C12 123.7(4) . . ? C7 C8 C12 118.8(4) . . ? C8 C9 C10 121.5(4) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C5 C10 C9 121.4(4) . . ? C5 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? N4 C11 C12 125.3(4) . . ? N4 C11 H11 117.4 . . ? C12 C11 H11 117.4 . . ? C13 C12 C11 115.2(3) . . ? C13 C12 C8 122.6(4) . . ? C11 C12 C8 122.3(4) . . ? C12 C13 C14 118.2(4) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? N3 C14 C13 123.8(4) . . ? N3 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? N6 C15 C16 124.0(3) . . ? N6 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C17 C16 C15 115.7(3) . . ? C17 C16 C19 122.7(3) . . ? C15 C16 C19 121.6(3) . . ? C16 C17 C18 117.7(3) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? N5 C18 C17 124.6(3) . . ? N5 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? C20 C19 C24 118.1(3) . . ? C20 C19 C16 121.1(3) . . ? C24 C19 C16 120.8(3) . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 117.7(4) . . ? C21 C22 C26 121.5(4) . . ? C23 C22 C26 120.8(3) . . ? C24 C23 C22 121.5(4) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 120.6(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? N8 C25 C26 124.4(3) . . ? N8 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C27 C26 C25 114.6(3) . . ? C27 C26 C22 123.0(3) . . ? C25 C26 C22 122.4(3) . . ? C26 C27 C28 119.1(4) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? N7 C28 C27 123.9(4) . . ? N7 C28 H28 118.1 . . ? C27 C28 H28 118.1 . . ? N10 C29 C30 123.8(3) . . ? N10 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C31 C30 C29 114.9(4) . . ? C31 C30 C34 123.6(4) . . ? C29 C30 C34 121.5(3) . . ? C32 C31 C30 119.2(4) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? N9 C32 C31 123.8(3) . . ? N9 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? C34 C33 C35 120.7(5) . 2_556 ? C34 C33 H33 119.7 . . ? C35 C33 H33 119.7 2_556 . ? C35 C34 C33 117.5(4) . . ? C35 C34 C30 120.7(4) . . ? C33 C34 C30 121.7(4) . . ? C34 C35 C33 121.8(4) . 2_556 ? C34 C35 H35 119.1 . . ? C33 C35 H35 119.1 2_556 . ? Cl1 C40 Cl3 112.7(9) . . ? Cl1 C40 Cl2 113.1(9) . . ? Cl3 C40 Cl2 112.5(9) . . ? Cl3A C40A Cl1A 112.7(9) . . ? Cl3A C40A Cl2A 111.2(8) . . ? Cl1A C40A Cl2A 110.7(8) . . ? Cl4A C41 Cl5A 116.6(7) . . ? Cl4A C41 Cl6A 113.0(7) . . ? Cl5A C41 Cl6A 108.6(7) . . ? Cl5 C41 Cl6 108.0(7) . . ? Cl5 C41 Cl4 112.6(7) . . ? Cl6 C41 Cl4 104.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cu2 N1 C4 84.5(3) . . . . ? N7 Cu2 N1 C4 -48.1(4) 1_565 . . . ? N10 Cu2 N1 C4 -162.1(3) . . . . ? N6 Cu2 N1 N2 -97.6(3) . . . . ? N7 Cu2 N1 N2 129.8(3) 1_565 . . . ? N10 Cu2 N1 N2 15.8(3) . . . . ? C4 N1 N2 C1 -2.0(6) . . . . ? Cu2 N1 N2 C1 -179.9(3) . . . . ? C14 N3 N4 C11 -1.8(6) . . . . ? Cu1 N3 N4 C11 176.9(4) 1_656 . . . ? N3 Cu1 N5 C18 -10.1(4) 1_454 . . . ? N8 Cu1 N5 C18 -141.8(3) 1_565 . . . ? N9 Cu1 N5 C18 112.2(3) . . . . ? N3 Cu1 N5 N6 -172.4(2) 1_454 . . . ? N8 Cu1 N5 N6 56.0(3) 1_565 . . . ? N9 Cu1 N5 N6 -50.1(3) . . . . ? C18 N5 N6 C15 -3.2(5) . . . . ? Cu1 N5 N6 C15 160.2(3) . . . . ? C18 N5 N6 Cu2 -172.8(3) . . . . ? Cu1 N5 N6 Cu2 -9.5(3) . . . . ? N1 Cu2 N6 C15 18.3(4) . . . . ? N7 Cu2 N6 C15 151.0(3) 1_565 . . . ? N10 Cu2 N6 C15 -103.8(3) . . . . ? N1 Cu2 N6 N5 -172.8(2) . . . . ? N7 Cu2 N6 N5 -40.1(3) 1_565 . . . ? N10 Cu2 N6 N5 65.1(3) . . . . ? C28 N7 N8 C25 -0.8(6) . . . . ? Cu2 N7 N8 C25 169.6(3) 1_545 . . . ? C28 N7 N8 Cu1 -172.2(4) . . . 1_545 ? Cu2 N7 N8 Cu1 -1.7(3) 1_545 . . 1_545 ? N3 Cu1 N9 C32 -3.4(4) 1_454 . . . ? N8 Cu1 N9 C32 125.0(4) 1_565 . . . ? N5 Cu1 N9 C32 -123.4(4) . . . . ? N3 Cu1 N9 N10 175.1(2) 1_454 . . . ? N8 Cu1 N9 N10 -56.5(3) 1_565 . . . ? N5 Cu1 N9 N10 55.1(3) . . . . ? C32 N9 N10 C29 0.9(5) . . . . ? Cu1 N9 N10 C29 -177.7(3) . . . . ? C32 N9 N10 Cu2 179.4(3) . . . . ? Cu1 N9 N10 Cu2 0.7(3) . . . . ? N1 Cu2 N10 C29 -8.7(4) . . . . ? N6 Cu2 N10 C29 118.3(3) . . . . ? N7 Cu2 N10 C29 -128.5(3) 1_565 . . . ? N1 Cu2 N10 N9 173.0(2) . . . . ? N6 Cu2 N10 N9 -60.1(3) . . . . ? N7 Cu2 N10 N9 53.1(3) 1_565 . . . ? N1 N2 C1 C2 1.3(7) . . . . ? N2 C1 C2 C3 0.4(7) . . . . ? N2 C1 C2 C5 -177.5(4) . . . . ? C1 C2 C3 C4 -1.4(6) . . . . ? C5 C2 C3 C4 176.5(4) . . . . ? N2 N1 C4 C3 1.0(6) . . . . ? Cu2 N1 C4 C3 178.9(3) . . . . ? C2 C3 C4 N1 0.7(7) . . . . ? C3 C2 C5 C10 -175.6(5) . . . . ? C1 C2 C5 C10 2.1(7) . . . . ? C3 C2 C5 C6 4.3(8) . . . . ? C1 C2 C5 C6 -178.0(6) . . . . ? C10 C5 C6 C7 2.1(12) . . . . ? C2 C5 C6 C7 -177.8(7) . . . . ? C5 C6 C7 C8 0.7(14) . . . . ? C6 C7 C8 C9 -3.3(12) . . . . ? C6 C7 C8 C12 177.6(7) . . . . ? C7 C8 C9 C10 3.2(9) . . . . ? C12 C8 C9 C10 -177.7(5) . . . . ? C6 C5 C10 C9 -2.2(9) . . . . ? C2 C5 C10 C9 177.7(5) . . . . ? C8 C9 C10 C5 -0.5(9) . . . . ? N3 N4 C11 C12 0.1(8) . . . . ? N4 C11 C12 C13 1.3(8) . . . . ? N4 C11 C12 C8 -179.6(5) . . . . ? C9 C8 C12 C13 161.2(5) . . . . ? C7 C8 C12 C13 -19.7(8) . . . . ? C9 C8 C12 C11 -17.9(7) . . . . ? C7 C8 C12 C11 161.2(6) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C8 C12 C13 C14 180.0(4) . . . . ? N4 N3 C14 C13 2.3(7) . . . . ? Cu1 N3 C14 C13 -176.4(3) 1_656 . . . ? C12 C13 C14 N3 -0.8(7) . . . . ? N5 N6 C15 C16 -1.5(6) . . . . ? Cu2 N6 C15 C16 166.8(3) . . . . ? N6 C15 C16 C17 4.8(6) . . . . ? N6 C15 C16 C19 -172.1(4) . . . . ? C15 C16 C17 C18 -3.6(6) . . . . ? C19 C16 C17 C18 173.4(4) . . . . ? N6 N5 C18 C17 4.4(6) . . . . ? Cu1 N5 C18 C17 -157.5(4) . . . . ? C16 C17 C18 N5 -0.9(7) . . . . ? C17 C16 C19 C20 -17.0(7) . . . . ? C15 C16 C19 C20 159.7(5) . . . . ? C17 C16 C19 C24 164.7(5) . . . . ? C15 C16 C19 C24 -18.6(6) . . . . ? C24 C19 C20 C21 3.3(8) . . . . ? C16 C19 C20 C21 -175.0(5) . . . . ? C19 C20 C21 C22 0.8(9) . . . . ? C20 C21 C22 C23 -5.1(8) . . . . ? C20 C21 C22 C26 173.8(5) . . . . ? C21 C22 C23 C24 5.3(8) . . . . ? C26 C22 C23 C24 -173.6(5) . . . . ? C22 C23 C24 C19 -1.2(9) . . . . ? C20 C19 C24 C23 -3.2(8) . . . . ? C16 C19 C24 C23 175.2(5) . . . . ? N7 N8 C25 C26 -1.4(7) . . . . ? Cu1 N8 C25 C26 168.7(3) 1_545 . . . ? N8 C25 C26 C27 2.6(7) . . . . ? N8 C25 C26 C22 -176.2(4) . . . . ? C21 C22 C26 C27 179.5(5) . . . . ? C23 C22 C26 C27 -1.6(8) . . . . ? C21 C22 C26 C25 -1.7(7) . . . . ? C23 C22 C26 C25 177.2(5) . . . . ? C25 C26 C27 C28 -1.7(7) . . . . ? C22 C26 C27 C28 177.1(5) . . . . ? N8 N7 C28 C27 1.6(8) . . . . ? Cu2 N7 C28 C27 -168.1(4) 1_545 . . . ? C26 C27 C28 N7 -0.3(9) . . . . ? N9 N10 C29 C30 0.2(6) . . . . ? Cu2 N10 C29 C30 -178.0(3) . . . . ? N10 C29 C30 C31 -1.2(6) . . . . ? N10 C29 C30 C34 177.0(4) . . . . ? C29 C30 C31 C32 1.0(7) . . . . ? C34 C30 C31 C32 -177.1(4) . . . . ? N10 N9 C32 C31 -1.1(7) . . . . ? Cu1 N9 C32 C31 177.4(4) . . . . ? C30 C31 C32 N9 0.1(8) . . . . ? C35 C33 C34 C35 1.7(13) 2_556 . . . ? C35 C33 C34 C30 -178.4(7) 2_556 . . . ? C31 C30 C34 C35 -8.4(8) . . . . ? C29 C30 C34 C35 173.6(6) . . . . ? C31 C30 C34 C33 171.7(6) . . . . ? C29 C30 C34 C33 -6.2(8) . . . . ? C33 C34 C35 C33 -1.8(13) . . . 2_556 ? C30 C34 C35 C33 178.4(7) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.895 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.093 #----------------------------------------------------# data_(3) _database_code_depnum_ccdc_archive 'CCDC 685684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) nitrate 1:1 complex with 1,4-bi(pyridazin-4-yl)benzene, Chloroform solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H11 Ag Cl3 N5 O3' _chemical_formula_weight 523.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3964(2) _cell_length_b 9.5399(2) _cell_length_c 12.4383(3) _cell_angle_alpha 80.0473(10) _cell_angle_beta 82.901(2) _cell_angle_gamma 64.9520(11) _cell_volume 887.61(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9394 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 26.42 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7383 _exptl_absorpt_correction_T_max 0.8552 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9394 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.42 _reflns_number_total 3592 _reflns_number_gt 2923 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms were located from difference maps and then refined a riding, with C---H distances (aromatic) constrained to 0.93 \%A, C---H distances (chloroform) constrained to 0.98 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atom). Both of two independent bipyridazine molecules in the structure lie across inversion centres. ; _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^)+(0.0293P)^2^+0.0933P] 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 3592 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.08269(3) 0.29858(3) 0.95226(2) 0.02422(10) Uani 1 1 d . . . N1 N 0.1343(3) 0.5117(3) 0.8564(2) 0.0210(6) Uani 1 1 d . . . N2 N 0.0737(3) 0.6561(3) 0.8864(2) 0.0191(6) Uani 1 1 d . . . N3 N 0.3385(3) 0.0831(3) 0.9063(2) 0.0202(6) Uani 1 1 d . . . N4 N 0.4703(4) 0.1031(3) 0.8416(2) 0.0233(6) Uani 1 1 d . . . N5 N -0.0569(3) 0.1889(3) 0.7806(2) 0.0256(7) Uani 1 1 d . . . O1 O -0.0423(3) 0.1219(3) 0.87777(19) 0.0282(6) Uani 1 1 d . . . O2 O -0.0877(3) 0.1306(3) 0.7077(2) 0.0368(6) Uani 1 1 d . . . O3 O -0.0404(3) 0.3153(3) 0.7585(2) 0.0385(7) Uani 1 1 d . . . C1 C 0.1099(4) 0.7654(4) 0.8207(3) 0.0212(7) Uani 1 1 d . . . H1 H 0.0646 0.8651 0.8409 0.025 Uiso 1 1 calc R . . C2 C 0.2116(4) 0.7392(4) 0.7233(3) 0.0207(7) Uani 1 1 d . . . H2 H 0.2339 0.8191 0.6795 0.025 Uiso 1 1 calc R . . C3 C 0.2783(4) 0.5922(4) 0.6932(3) 0.0179(7) Uani 1 1 d . . . C4 C 0.2319(4) 0.4829(4) 0.7643(3) 0.0218(8) Uani 1 1 d . . . H4 H 0.2726 0.3828 0.7453 0.026 Uiso 1 1 calc R . . C5 C 0.3923(4) 0.5459(4) 0.5932(3) 0.0189(7) Uani 1 1 d . . . C6 C 0.5322(4) 0.3990(4) 0.5968(3) 0.0222(8) Uani 1 1 d . . . H6 H 0.5539 0.3312 0.6620 0.027 Uiso 1 1 calc R . . C7 C 0.6387(4) 0.3538(4) 0.5041(3) 0.0215(8) Uani 1 1 d . . . H7 H 0.7316 0.2555 0.5070 0.026 Uiso 1 1 calc R . . C8 C 0.6049(4) -0.0207(4) 0.8110(3) 0.0246(8) Uani 1 1 d . . . H8 H 0.6944 -0.0050 0.7658 0.029 Uiso 1 1 calc R . . C9 C 0.6215(4) -0.1733(4) 0.8421(3) 0.0238(8) Uani 1 1 d . . . H9 H 0.7176 -0.2569 0.8168 0.029 Uiso 1 1 calc R . . C10 C 0.4914(4) -0.1968(4) 0.9114(3) 0.0204(7) Uani 1 1 d . . . C11 C 0.3494(4) -0.0602(4) 0.9391(3) 0.0200(7) Uani 1 1 d . . . H11 H 0.2568 -0.0713 0.9836 0.024 Uiso 1 1 calc R . . C12 C 0.4975(4) -0.3537(4) 0.9567(3) 0.0195(7) Uani 1 1 d . . . C13 C 0.5742(4) -0.4781(4) 0.8959(3) 0.0235(8) Uani 1 1 d . . . H13 H 0.6245 -0.4640 0.8263 0.028 Uiso 1 1 calc R . . C14 C 0.5758(4) -0.6221(4) 0.9384(3) 0.0231(8) Uani 1 1 d . . . H14 H 0.6263 -0.7040 0.8967 0.028 Uiso 1 1 calc R . . C15 C 0.8414(5) 0.7726(4) 0.4855(3) 0.0306(9) Uani 1 1 d . . . H15 H 0.9492 0.7260 0.4397 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.86568(12) 0.90581(11) 0.55624(8) 0.0357(2) Uani 1 1 d . . . Cl2 Cl 0.81266(17) 0.62264(12) 0.57839(9) 0.0543(3) Uani 1 1 d . . . Cl3 Cl 0.66427(14) 0.87013(14) 0.40019(10) 0.0528(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03196(16) 0.02015(15) 0.01942(16) -0.00655(11) 0.00916(11) -0.01098(12) N1 0.0261(15) 0.0174(15) 0.0189(16) -0.0076(12) 0.0058(12) -0.0085(12) N2 0.0232(14) 0.0164(15) 0.0162(15) -0.0039(12) 0.0022(12) -0.0068(12) N3 0.0241(14) 0.0194(15) 0.0166(15) -0.0022(12) 0.0008(12) -0.0089(12) N4 0.0282(15) 0.0225(16) 0.0202(16) -0.0032(12) 0.0004(13) -0.0115(13) N5 0.0219(15) 0.0237(17) 0.0278(19) -0.0031(14) 0.0022(13) -0.0074(13) O1 0.0316(13) 0.0259(14) 0.0220(14) -0.0019(11) 0.0011(11) -0.0081(11) O2 0.0504(16) 0.0388(16) 0.0306(16) -0.0058(13) -0.0073(13) -0.0256(14) O3 0.0525(17) 0.0216(14) 0.0462(18) -0.0040(12) 0.0053(14) -0.0221(13) C1 0.0219(17) 0.0147(17) 0.024(2) -0.0052(14) 0.0014(15) -0.0048(14) C2 0.0253(17) 0.0152(17) 0.0207(19) 0.0010(14) 0.0003(14) -0.0094(15) C3 0.0186(16) 0.0196(18) 0.0147(18) -0.0021(14) 0.0003(13) -0.0074(14) C4 0.0272(18) 0.0150(17) 0.0208(19) -0.0060(14) 0.0060(15) -0.0070(15) C5 0.0195(16) 0.0172(17) 0.0192(18) -0.0035(14) 0.0028(14) -0.0075(14) C6 0.0267(18) 0.0215(18) 0.0166(18) 0.0008(14) 0.0020(15) -0.0101(15) C7 0.0246(17) 0.0139(17) 0.0215(19) -0.0030(14) 0.0045(15) -0.0049(14) C8 0.0274(18) 0.025(2) 0.0210(19) -0.0038(15) 0.0037(15) -0.0117(16) C9 0.0230(17) 0.0241(19) 0.0212(19) -0.0079(15) 0.0002(15) -0.0053(15) C10 0.0219(17) 0.0221(18) 0.0186(19) -0.0051(14) -0.0020(14) -0.0093(15) C11 0.0187(16) 0.0197(18) 0.0203(19) -0.0036(14) -0.0008(14) -0.0063(14) C12 0.0158(16) 0.0168(17) 0.0233(19) -0.0011(14) -0.0043(14) -0.0040(14) C13 0.0248(18) 0.0225(19) 0.0220(19) -0.0039(15) 0.0022(15) -0.0091(15) C14 0.0220(17) 0.0187(18) 0.025(2) -0.0068(15) -0.0023(15) -0.0036(15) C15 0.039(2) 0.026(2) 0.027(2) -0.0040(16) 0.0007(17) -0.0137(17) Cl1 0.0402(5) 0.0358(6) 0.0372(6) -0.0095(4) -0.0019(4) -0.0199(5) Cl2 0.0837(8) 0.0400(6) 0.0458(7) -0.0052(5) 0.0163(6) -0.0372(6) Cl3 0.0476(6) 0.0638(8) 0.0508(7) -0.0113(6) -0.0163(5) -0.0218(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.259(2) 2_567 ? Ag1 N1 2.350(3) . ? Ag1 N3 2.352(3) . ? Ag1 O1 2.661(2) . ? Ag1 O3 2.691(3) . ? N1 C4 1.322(4) . ? N1 N2 1.354(3) . ? N2 C1 1.327(4) . ? N2 Ag1 2.259(2) 2_567 ? N3 C11 1.325(4) . ? N3 N4 1.347(3) . ? N4 C8 1.318(4) . ? N5 O2 1.247(4) . ? N5 O3 1.251(3) . ? N5 O1 1.260(3) . ? C1 C2 1.388(4) . ? C1 H1 0.9300 . ? C2 C3 1.372(4) . ? C2 H2 0.9300 . ? C3 C4 1.401(4) . ? C3 C5 1.482(4) . ? C4 H4 0.9300 . ? C5 C7 1.383(4) 2_666 ? C5 C6 1.394(4) . ? C6 C7 1.381(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.391(5) . ? C8 H8 0.9300 . ? C9 C10 1.376(4) . ? C9 H9 0.9300 . ? C10 C11 1.405(4) . ? C10 C12 1.487(4) . ? C11 H11 0.9300 . ? C12 C13 1.392(4) . ? C12 C14 1.397(4) 2_647 ? C13 C14 1.379(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 Cl3 1.755(4) . ? C15 Cl1 1.755(4) . ? C15 Cl2 1.759(4) . ? C15 H15 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 114.66(9) 2_567 . ? N2 Ag1 N3 130.49(9) 2_567 . ? N1 Ag1 N3 102.76(9) . . ? N2 Ag1 O1 101.79(8) 2_567 . ? N1 Ag1 O1 128.16(8) . . ? N3 Ag1 O1 76.65(8) . . ? N2 Ag1 O3 127.22(9) 2_567 . ? N1 Ag1 O3 80.61(8) . . ? N3 Ag1 O3 88.66(8) . . ? O1 Ag1 O3 47.67(7) . . ? C4 N1 N2 119.0(3) . . ? C4 N1 Ag1 114.5(2) . . ? N2 N1 Ag1 126.52(18) . . ? C1 N2 N1 118.9(3) . . ? C1 N2 Ag1 122.4(2) . 2_567 ? N1 N2 Ag1 118.76(18) . 2_567 ? C11 N3 N4 119.2(3) . . ? C11 N3 Ag1 119.7(2) . . ? N4 N3 Ag1 120.97(19) . . ? C8 N4 N3 118.9(3) . . ? O2 N5 O3 120.5(3) . . ? O2 N5 O1 120.6(3) . . ? O3 N5 O1 118.9(3) . . ? N5 O1 Ag1 96.73(19) . . ? N5 O3 Ag1 95.5(2) . . ? N2 C1 C2 123.6(3) . . ? N2 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 115.6(3) . . ? C2 C3 C5 124.4(3) . . ? C4 C3 C5 120.1(3) . . ? N1 C4 C3 124.7(3) . . ? N1 C4 H4 117.7 . . ? C3 C4 H4 117.7 . . ? C7 C5 C6 119.5(3) 2_666 . ? C7 C5 C3 120.9(3) 2_666 . ? C6 C5 C3 119.6(3) . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C5 120.2(3) . 2_666 ? C6 C7 H7 119.9 . . ? C5 C7 H7 119.9 2_666 . ? N4 C8 C9 124.1(3) . . ? N4 C8 H8 117.9 . . ? C9 C8 H8 117.9 . . ? C10 C9 C8 117.9(3) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 115.3(3) . . ? C9 C10 C12 123.7(3) . . ? C11 C10 C12 121.0(3) . . ? N3 C11 C10 124.5(3) . . ? N3 C11 H11 117.7 . . ? C10 C11 H11 117.7 . . ? C13 C12 C14 118.8(3) . 2_647 ? C13 C12 C10 121.1(3) . . ? C14 C12 C10 120.0(3) 2_647 . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C12 120.8(3) . 2_647 ? C13 C14 H14 119.6 . . ? C12 C14 H14 119.6 2_647 . ? Cl3 C15 Cl1 110.03(19) . . ? Cl3 C15 Cl2 111.4(2) . . ? Cl1 C15 Cl2 110.2(2) . . ? Cl3 C15 H15 108.4 . . ? Cl1 C15 H15 108.4 . . ? Cl2 C15 H15 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C4 177.4(2) 2_567 . . . ? N3 Ag1 N1 C4 30.6(2) . . . . ? O1 Ag1 N1 C4 -52.3(3) . . . . ? O3 Ag1 N1 C4 -55.9(2) . . . . ? N2 Ag1 N1 N2 -3.1(3) 2_567 . . . ? N3 Ag1 N1 N2 -149.8(2) . . . . ? O1 Ag1 N1 N2 127.2(2) . . . . ? O3 Ag1 N1 N2 123.7(3) . . . . ? C4 N1 N2 C1 2.0(4) . . . . ? Ag1 N1 N2 C1 -177.6(2) . . . . ? C4 N1 N2 Ag1 -177.3(2) . . . 2_567 ? Ag1 N1 N2 Ag1 3.2(3) . . . 2_567 ? N2 Ag1 N3 C11 46.6(3) 2_567 . . . ? N1 Ag1 N3 C11 -174.4(2) . . . . ? O1 Ag1 N3 C11 -47.7(2) . . . . ? O3 Ag1 N3 C11 -94.3(2) . . . . ? N2 Ag1 N3 N4 -137.4(2) 2_567 . . . ? N1 Ag1 N3 N4 1.7(2) . . . . ? O1 Ag1 N3 N4 128.4(2) . . . . ? O3 Ag1 N3 N4 81.8(2) . . . . ? C11 N3 N4 C8 1.4(5) . . . . ? Ag1 N3 N4 C8 -174.7(2) . . . . ? O2 N5 O1 Ag1 169.1(2) . . . . ? O3 N5 O1 Ag1 -11.1(3) . . . . ? N2 Ag1 O1 N5 136.30(17) 2_567 . . . ? N1 Ag1 O1 N5 1.4(2) . . . . ? N3 Ag1 O1 N5 -94.50(18) . . . . ? O3 Ag1 O1 N5 6.09(16) . . . . ? O2 N5 O3 Ag1 -169.3(2) . . . . ? O1 N5 O3 Ag1 11.0(3) . . . . ? N2 Ag1 O3 N5 -76.0(2) 2_567 . . . ? N1 Ag1 O3 N5 170.13(19) . . . . ? N3 Ag1 O3 N5 66.96(18) . . . . ? O1 Ag1 O3 N5 -6.12(16) . . . . ? N1 N2 C1 C2 -1.9(5) . . . . ? Ag1 N2 C1 C2 177.3(2) 2_567 . . . ? N2 C1 C2 C3 0.0(5) . . . . ? C1 C2 C3 C4 1.6(5) . . . . ? C1 C2 C3 C5 -178.5(3) . . . . ? N2 N1 C4 C3 -0.2(5) . . . . ? Ag1 N1 C4 C3 179.4(3) . . . . ? C2 C3 C4 N1 -1.6(5) . . . . ? C5 C3 C4 N1 178.5(3) . . . . ? C2 C3 C5 C7 -39.0(5) . . . 2_666 ? C4 C3 C5 C7 140.9(3) . . . 2_666 ? C2 C3 C5 C6 141.3(3) . . . . ? C4 C3 C5 C6 -38.8(4) . . . . ? C7 C5 C6 C7 -0.2(5) 2_666 . . . ? C3 C5 C6 C7 179.5(3) . . . . ? C5 C6 C7 C5 0.2(5) . . . 2_666 ? N3 N4 C8 C9 -0.6(5) . . . . ? N4 C8 C9 C10 -1.7(5) . . . . ? C8 C9 C10 C11 3.0(5) . . . . ? C8 C9 C10 C12 -176.1(3) . . . . ? N4 N3 C11 C10 0.2(5) . . . . ? Ag1 N3 C11 C10 176.3(2) . . . . ? C9 C10 C11 N3 -2.4(5) . . . . ? C12 C10 C11 N3 176.7(3) . . . . ? C9 C10 C12 C13 -34.1(5) . . . . ? C11 C10 C12 C13 146.8(3) . . . . ? C9 C10 C12 C14 146.4(3) . . . 2_647 ? C11 C10 C12 C14 -32.7(5) . . . 2_647 ? C14 C12 C13 C14 0.7(5) 2_647 . . . ? C10 C12 C13 C14 -178.8(3) . . . . ? C12 C13 C14 C12 -0.7(5) . . . 2_647 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.440 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.103 #----------------------------------------------------# data_(4) _database_code_depnum_ccdc_archive 'CCDC 685685' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Trifluoroacetate 4:3 complex with 1,4-bi(pyridazin-4-yl)benzene, Acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H33 Ag4 F12 N13 O8' _chemical_formula_weight 1627.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9059(10) _cell_length_b 11.1531(11) _cell_length_c 13.8012(13) _cell_angle_alpha 92.620(11) _cell_angle_beta 108.916(11) _cell_angle_gamma 117.522(10) _cell_volume 1369.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6747 _exptl_absorpt_correction_T_max 0.7212 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 223(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 12755 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 28.15 _reflns_number_total 6582 _reflns_number_gt 4636 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms (aromatic CH) were located from difference maps and then refined a riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atom). Both unique trifluoroacetate groups shows very typical rotational disorder. The refined partial contributions were 0.5/0.5 and 0.6/0.4. In each case, geometry of the CF~3~ group was restrained (either C---F distances or F---C---F bond angles), while all the disordered atoms were refined anisotropically. In total, 41 restraints were generated for four disorder components of two unique CF3 groups. The solvate acetonitrile molecule is disordered over two closely situated positions related by inversion center (0.5/0.5). The atoms were refined anisotropically and the hydrogen atoms of the methyl group were not added. There are two independent bipyridazine molecules in the structure (one of which is bidentate and second is tetradentate towards Ag ions). The bidentate organic molecule lies across an inversion centre). ; _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^)+(0.0498P)^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 6582 _refine_ls_number_parameters 469 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 1.23609(2) 0.50174(3) 0.226222(17) 0.04091(8) Uani 1 1 d . . . Ag2 Ag 0.89125(2) 0.38419(2) 0.208836(15) 0.03484(8) Uani 1 1 d . . . N1 N 1.0600(2) 0.3940(3) 0.05819(17) 0.0295(5) Uani 1 1 d . . . N2 N 0.9166(2) 0.3361(3) 0.05138(17) 0.0286(5) Uani 1 1 d . . . N3 N 0.0710(2) -0.4210(3) -0.65784(17) 0.0333(6) Uani 1 1 d . . . N4 N 0.2128(2) -0.3674(3) -0.65296(17) 0.0308(5) Uani 1 1 d . . . N5 N 0.6362(3) 0.2814(3) 0.15334(19) 0.0370(6) Uani 1 1 d . . . N6 N 0.5527(3) 0.1705(3) 0.07073(19) 0.0353(6) Uani 1 1 d . . . O1 O 1.1836(3) 0.3062(3) 0.3156(2) 0.0582(7) Uani 1 1 d . . . O2 O 0.9478(3) 0.2314(4) 0.3032(2) 0.0647(8) Uani 1 1 d . . . O3 O 1.4983(4) 0.5845(4) 0.2720(3) 0.0852(11) Uani 1 1 d . . . O4 O 1.4193(3) 0.6231(4) 0.1155(3) 0.0869(11) Uani 1 1 d . . . F1 F 1.2230(4) 0.1797(6) 0.4702(4) 0.0697(18) Uani 0.60 1 d PD . . F2 F 1.0305(8) 0.0123(4) 0.3499(4) 0.0667(17) Uani 0.60 1 d PD . . F3 F 1.0064(8) 0.1216(8) 0.4670(5) 0.101(3) Uani 0.60 1 d PD . . F1A F 1.2105(9) 0.1954(10) 0.4900(6) 0.158(8) Uani 0.40 1 d PD . . F2A F 1.0725(14) 0.0277(7) 0.3541(7) 0.123(7) Uani 0.40 1 d PD . . F3A F 0.9720(11) 0.0875(12) 0.4409(9) 0.112(5) Uani 0.40 1 d PD . . F4 F 1.6851(9) 0.6474(11) 0.1177(7) 0.145(7) Uani 0.50 1 d PD . . F5 F 1.7166(8) 0.8379(6) 0.1919(10) 0.126(6) Uani 0.50 1 d PD . . F6 F 1.7775(6) 0.7105(12) 0.2847(6) 0.120(5) Uani 0.50 1 d PD . . F6A F 1.7698(6) 0.6786(10) 0.2651(7) 0.090(3) Uani 0.50 1 d PD . . F4A F 1.6769(9) 0.6815(12) 0.1042(5) 0.121(5) Uani 0.50 1 d PD . . F5A F 1.7307(8) 0.8452(4) 0.2252(10) 0.104(4) Uani 0.50 1 d PD . . C1 C 1.0842(3) 0.3651(3) -0.0256(2) 0.0317(6) Uani 1 1 d . . . H1 H 1.1836 0.4081 -0.0211 0.038 Uiso 1 1 calc R . . C2 C 0.9697(3) 0.2742(3) -0.1200(2) 0.0304(6) Uani 1 1 d . . . H2 H 0.9916 0.2554 -0.1775 0.037 Uiso 1 1 calc R . . C3 C 0.8237(3) 0.2124(3) -0.12726(19) 0.0257(5) Uani 1 1 d . . . C4 C 0.8047(3) 0.2514(3) -0.0373(2) 0.0277(6) Uani 1 1 d . . . H4 H 0.7063 0.2149 -0.0405 0.033 Uiso 1 1 calc R . . C5 C 0.6930(3) 0.1072(3) -0.22081(19) 0.0253(5) Uani 1 1 d . . . C6 C 0.7111(3) 0.0292(3) -0.2910(2) 0.0318(6) Uani 1 1 d . . . H6 H 0.8079 0.0463 -0.2804 0.038 Uiso 1 1 calc R . . C7 C 0.5889(3) -0.0730(3) -0.3760(2) 0.0327(7) Uani 1 1 d . . . H7 H 0.6039 -0.1250 -0.4217 0.039 Uiso 1 1 calc R . . C8 C 0.4438(3) -0.1004(3) -0.39507(19) 0.0271(6) Uani 1 1 d . . . C9 C 0.4251(3) -0.0219(3) -0.3251(2) 0.0350(7) Uani 1 1 d . . . H9 H 0.3284 -0.0383 -0.3362 0.042 Uiso 1 1 calc R . . C10 C 0.5477(3) 0.0800(3) -0.2394(2) 0.0322(6) Uani 1 1 d . . . H10 H 0.5328 0.1316 -0.1932 0.039 Uiso 1 1 calc R . . C11 C 0.0515(3) -0.3715(4) -0.5786(2) 0.0391(8) Uani 1 1 d . . . H11 H -0.0472 -0.4083 -0.5824 0.047 Uiso 1 1 calc R . . C12 C 0.1672(3) -0.2686(3) -0.4902(2) 0.0373(7) Uani 1 1 d . . . H12 H 0.1472 -0.2388 -0.4353 0.045 Uiso 1 1 calc R . . C13 C 0.3123(3) -0.2113(3) -0.48530(19) 0.0279(6) Uani 1 1 d . . . C14 C 0.3268(3) -0.2670(3) -0.5714(2) 0.0301(6) Uani 1 1 d . . . H14 H 0.4236 -0.2308 -0.5713 0.036 Uiso 1 1 calc R . . C15 C 0.5670(3) 0.3241(4) 0.1959(3) 0.0466(9) Uani 1 1 d . . . H15 H 0.6266 0.4019 0.2532 0.056 Uiso 1 1 calc R . . C16 C 0.4132(3) 0.2628(4) 0.1623(3) 0.0432(8) Uani 1 1 d . . . H16 H 0.3699 0.2977 0.1959 0.052 Uiso 1 1 calc R . . C17 C 0.3247(3) 0.1491(3) 0.0781(2) 0.0280(6) Uani 1 1 d . . . C18 C 0.4043(3) 0.1077(3) 0.0359(2) 0.0328(6) Uani 1 1 d . . . H18 H 0.3481 0.0298 -0.0211 0.039 Uiso 1 1 calc R . . C19 C 0.0854(3) 0.0871(3) 0.0993(2) 0.0300(6) Uani 1 1 d . . . H19 H 0.1430 0.1462 0.1671 0.036 Uiso 1 1 calc R . . C20 C 0.1581(3) 0.0723(3) 0.0369(2) 0.0257(5) Uani 1 1 d . . . C21 C 0.0698(3) -0.0167(3) -0.0635(2) 0.0298(6) Uani 1 1 d . . . H21 H 0.1161 -0.0289 -0.1069 0.036 Uiso 1 1 calc R . . C22 C 1.0717(4) 0.2393(3) 0.3351(2) 0.0428(8) Uani 1 1 d D . . C23 C 1.0822(3) 0.1380(3) 0.4062(2) 0.0551(10) Uani 1 1 d D . . C24 C 1.5139(3) 0.6272(3) 0.1968(3) 0.0487(9) Uani 1 1 d D . . C25 C 1.6749(3) 0.7074(4) 0.1983(3) 0.0671(13) Uani 1 1 d D . . N7 N 1.7258(8) 0.5114(7) 0.4420(5) 0.0513(15) Uani 0.50 1 d PD . . C26 C 1.6288(9) 0.5013(9) 0.4594(6) 0.069(3) Uani 0.50 1 d PD . . C27 C 1.506(4) 0.504(7) 0.483(2) 0.105(7) Uani 0.50 1 d PD . . 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 0.02498(11) 0.05189(17) 0.03171(12) -0.00859(10) 0.00951(9) 0.01123(11) Ag2 0.02035(10) 0.04230(15) 0.02832(11) -0.00392(9) 0.00574(8) 0.00900(9) N1 0.0215(10) 0.0316(14) 0.0270(10) -0.0003(9) 0.0080(9) 0.0085(10) N2 0.0231(10) 0.0317(14) 0.0254(10) -0.0008(9) 0.0089(9) 0.0106(10) N3 0.0233(11) 0.0377(15) 0.0287(11) -0.0038(10) 0.0065(9) 0.0110(10) N4 0.0242(11) 0.0320(14) 0.0262(10) -0.0018(9) 0.0086(9) 0.0081(10) N5 0.0181(10) 0.0402(16) 0.0394(13) -0.0025(11) 0.0078(9) 0.0080(10) N6 0.0208(11) 0.0370(16) 0.0404(13) -0.0003(11) 0.0117(10) 0.0097(10) O1 0.0611(16) 0.0551(18) 0.0587(15) 0.0177(13) 0.0355(13) 0.0211(14) O2 0.0689(18) 0.086(2) 0.0739(18) 0.0451(16) 0.0422(15) 0.0540(18) O3 0.0562(18) 0.102(3) 0.077(2) 0.0250(19) 0.0413(17) 0.0141(18) O4 0.0426(16) 0.089(3) 0.099(2) 0.005(2) 0.0043(17) 0.0271(18) F1 0.072(4) 0.092(5) 0.082(4) 0.038(3) 0.034(3) 0.066(4) F2 0.082(4) 0.038(3) 0.100(4) 0.020(3) 0.053(3) 0.034(2) F3 0.173(8) 0.165(8) 0.118(5) 0.110(5) 0.126(5) 0.150(7) F1A 0.161(14) 0.153(14) 0.078(7) 0.070(8) 0.013(8) 0.036(11) F2A 0.149(12) 0.113(10) 0.242(16) 0.100(10) 0.162(12) 0.107(9) F3A 0.137(9) 0.145(11) 0.194(12) 0.145(10) 0.144(10) 0.117(8) F4 0.117(9) 0.265(16) 0.133(9) 0.060(10) 0.096(8) 0.124(11) F5 0.043(4) 0.136(11) 0.156(8) 0.119(8) 0.033(4) 0.008(5) F6 0.036(5) 0.152(10) 0.122(7) 0.076(7) 0.007(4) 0.022(5) F6A 0.036(4) 0.110(7) 0.141(8) 0.071(6) 0.038(5) 0.043(5) F4A 0.151(11) 0.210(13) 0.112(8) 0.094(9) 0.101(8) 0.137(11) F5A 0.065(5) 0.047(5) 0.191(11) 0.028(5) 0.053(6) 0.018(4) C1 0.0225(12) 0.0365(18) 0.0285(13) 0.0010(11) 0.0100(10) 0.0097(12) C2 0.0272(13) 0.0378(18) 0.0247(12) 0.0030(11) 0.0128(10) 0.0138(12) C3 0.0238(12) 0.0266(15) 0.0234(11) 0.0022(10) 0.0063(10) 0.0124(11) C4 0.0233(12) 0.0284(16) 0.0268(12) 0.0010(11) 0.0087(10) 0.0106(11) C5 0.0243(12) 0.0251(15) 0.0219(11) 0.0011(10) 0.0075(10) 0.0104(11) C6 0.0247(13) 0.0391(18) 0.0307(13) 0.0005(12) 0.0100(11) 0.0166(13) C7 0.0278(13) 0.0377(18) 0.0281(12) -0.0068(11) 0.0084(11) 0.0162(13) C8 0.0244(12) 0.0301(16) 0.0214(11) -0.0014(10) 0.0062(10) 0.0122(11) C9 0.0258(13) 0.0426(19) 0.0327(13) -0.0049(12) 0.0079(11) 0.0178(13) C10 0.0266(13) 0.0373(17) 0.0285(12) -0.0060(11) 0.0089(11) 0.0154(12) C11 0.0237(13) 0.047(2) 0.0363(14) -0.0074(13) 0.0099(11) 0.0131(13) C12 0.0258(13) 0.0438(19) 0.0342(14) -0.0077(13) 0.0106(11) 0.0136(13) C13 0.0245(12) 0.0296(16) 0.0236(11) -0.0010(10) 0.0058(10) 0.0121(11) C14 0.0228(12) 0.0314(17) 0.0275(12) -0.0003(11) 0.0095(10) 0.0079(11) C15 0.0230(13) 0.053(2) 0.0423(16) -0.0146(15) 0.0060(12) 0.0098(14) C16 0.0257(14) 0.043(2) 0.0511(17) -0.0090(15) 0.0148(13) 0.0116(13) C17 0.0186(11) 0.0286(16) 0.0327(13) 0.0054(11) 0.0102(10) 0.0088(11) C18 0.0213(12) 0.0349(17) 0.0357(14) -0.0008(12) 0.0121(11) 0.0092(12) C19 0.0227(12) 0.0327(17) 0.0290(12) -0.0012(11) 0.0090(10) 0.0112(12) C20 0.0184(11) 0.0257(15) 0.0318(12) 0.0060(10) 0.0107(10) 0.0098(11) C21 0.0244(13) 0.0357(17) 0.0305(13) 0.0035(11) 0.0135(11) 0.0147(12) C22 0.058(2) 0.045(2) 0.0368(15) 0.0092(14) 0.0277(15) 0.0291(17) C23 0.068(3) 0.066(3) 0.067(2) 0.031(2) 0.046(2) 0.047(2) C24 0.0300(16) 0.040(2) 0.072(2) -0.0008(17) 0.0242(17) 0.0124(14) C25 0.0391(19) 0.091(4) 0.082(3) 0.040(3) 0.033(2) 0.033(2) N7 0.059(4) 0.052(4) 0.043(3) 0.013(3) 0.022(3) 0.027(3) C26 0.079(6) 0.048(6) 0.042(4) 0.011(3) -0.007(4) 0.024(5) C27 0.074(8) 0.172(13) 0.059(17) 0.015(19) 0.007(10) 0.068(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 2.288(2) . ? Ag1 N4 2.317(2) 1_666 ? Ag1 O3 2.401(3) . ? Ag1 O1 2.481(3) . ? Ag1 Ag2 3.2786(5) . ? Ag2 N5 2.287(2) . ? Ag2 N3 2.304(2) 1_666 ? Ag2 N2 2.347(2) . ? Ag2 O2 2.374(3) . ? N1 C1 1.323(3) . ? N1 N2 1.356(3) . ? N2 C4 1.319(3) . ? N3 C11 1.322(3) . ? N3 N4 1.352(3) . ? N3 Ag2 2.304(2) 1_444 ? N4 C14 1.325(3) . ? N4 Ag1 2.317(2) 1_444 ? N5 C15 1.318(4) . ? N5 N6 1.348(3) . ? N6 C18 1.327(3) . ? O1 C22 1.228(4) . ? O2 C22 1.237(4) . ? O3 C24 1.190(5) . ? O4 C24 1.235(5) . ? F1 C23 1.334(4) . ? F2 C23 1.332(4) . ? F3 C23 1.321(4) . ? F1A C23 1.327(4) . ? F2A C23 1.339(4) . ? F3A C23 1.327(4) . ? F4 C25 1.333(4) . ? F5 C25 1.326(4) . ? F6 C25 1.330(4) . ? F6A C25 1.319(4) . ? F4A C25 1.327(4) . ? F5A C25 1.345(4) . ? C1 C2 1.393(4) . ? C1 H1 0.9400 . ? C2 C3 1.378(4) . ? C2 H2 0.9400 . ? C3 C4 1.405(3) . ? C3 C5 1.482(3) . ? C4 H4 0.9400 . ? C5 C6 1.393(3) . ? C5 C10 1.398(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9400 . ? C7 C8 1.394(4) . ? C7 H7 0.9400 . ? C8 C9 1.399(3) . ? C8 C13 1.483(3) . ? C9 C10 1.388(4) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.390(4) . ? C11 H11 0.9400 . ? C12 C13 1.382(4) . ? C12 H12 0.9400 . ? C13 C14 1.403(3) . ? C14 H14 0.9400 . ? C15 C16 1.379(4) . ? C15 H15 0.9400 . ? C16 C17 1.378(4) . ? C16 H16 0.9400 . ? C17 C18 1.406(4) . ? C17 C20 1.486(3) . ? C18 H18 0.9400 . ? C19 C21 1.386(4) 2 ? C19 C20 1.395(3) . ? C19 H19 0.9400 . ? C20 C21 1.399(4) . ? C21 C19 1.386(4) 2 ? C21 H21 0.9400 . ? C22 C23 1.550(3) . ? C24 C25 1.552(3) . ? N7 C26 1.116(4) . ? C26 C27 1.493(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 N4 122.97(8) . 1_666 ? N1 Ag1 O3 122.88(10) . . ? N4 Ag1 O3 108.36(11) 1_666 . ? N1 Ag1 O1 102.42(9) . . ? N4 Ag1 O1 93.55(9) 1_666 . ? O3 Ag1 O1 97.33(12) . . ? N1 Ag1 Ag2 66.65(6) . . ? N4 Ag1 Ag2 65.48(6) 1_666 . ? O3 Ag1 Ag2 169.47(8) . . ? O1 Ag1 Ag2 75.13(7) . . ? N5 Ag2 N3 127.43(8) . 1_666 ? N5 Ag2 N2 101.36(8) . . ? N3 Ag2 N2 122.90(8) 1_666 . ? N5 Ag2 O2 103.71(11) . . ? N3 Ag2 O2 93.71(11) 1_666 . ? N2 Ag2 O2 102.41(9) . . ? N5 Ag2 Ag1 165.59(6) . . ? N3 Ag2 Ag1 65.20(6) 1_666 . ? N2 Ag2 Ag1 64.24(5) . . ? O2 Ag2 Ag1 80.47(7) . . ? C1 N1 N2 118.8(2) . . ? C1 N1 Ag1 126.55(17) . . ? N2 N1 Ag1 113.72(15) . . ? C4 N2 N1 119.8(2) . . ? C4 N2 Ag2 124.92(17) . . ? N1 N2 Ag2 115.06(15) . . ? C11 N3 N4 117.9(2) . . ? C11 N3 Ag2 125.87(19) . 1_444 ? N4 N3 Ag2 115.43(15) . 1_444 ? C14 N4 N3 120.1(2) . . ? C14 N4 Ag1 124.69(18) . 1_444 ? N3 N4 Ag1 113.74(16) . 1_444 ? C15 N5 N6 118.6(2) . . ? C15 N5 Ag2 124.50(19) . . ? N6 N5 Ag2 116.88(17) . . ? C18 N6 N5 118.9(2) . . ? C22 O1 Ag1 127.1(2) . . ? C22 O2 Ag2 124.6(2) . . ? C24 O3 Ag1 100.6(2) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 115.6(2) . . ? C2 C3 C5 123.6(2) . . ? C4 C3 C5 120.7(2) . . ? N2 C4 C3 124.0(2) . . ? N2 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C6 C5 C10 118.0(2) . . ? C6 C5 C3 120.7(2) . . ? C10 C5 C3 121.2(2) . . ? C7 C6 C5 121.0(2) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 121.2(2) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 118.0(2) . . ? C7 C8 C13 121.3(2) . . ? C9 C8 C13 120.7(2) . . ? C10 C9 C8 120.8(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C5 121.0(2) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? N3 C11 C12 124.4(3) . . ? N3 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C13 C12 C11 118.2(2) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 C14 115.1(2) . . ? C12 C13 C8 122.6(2) . . ? C14 C13 C8 122.2(2) . . ? N4 C14 C13 124.3(2) . . ? N4 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? N5 C15 C16 124.6(3) . . ? N5 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? C17 C16 C15 118.2(3) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 114.8(2) . . ? C16 C17 C20 122.9(2) . . ? C18 C17 C20 122.2(2) . . ? N6 C18 C17 124.9(3) . . ? N6 C18 H18 117.6 . . ? C17 C18 H18 117.6 . . ? C21 C19 C20 121.4(2) 2 . ? C21 C19 H19 119.3 2 . ? C20 C19 H19 119.3 . . ? C19 C20 C21 118.2(2) . . ? C19 C20 C17 119.9(2) . . ? C21 C20 C17 121.9(2) . . ? C19 C21 C20 120.4(2) 2 . ? C19 C21 H21 119.8 2 . ? C20 C21 H21 119.8 . . ? O1 C22 O2 131.8(3) . . ? O1 C22 C23 114.7(3) . . ? O2 C22 C23 113.3(3) . . ? F1A C23 F3A 107.2(4) . . ? F3 C23 F2 107.2(4) . . ? F3 C23 F1 106.4(4) . . ? F2 C23 F1 105.2(3) . . ? F1A C23 F2A 105.9(4) . . ? F3A C23 F2A 106.1(4) . . ? F3 C23 C22 113.0(3) . . ? F1A C23 C22 113.2(4) . . ? F3A C23 C22 112.5(4) . . ? F2 C23 C22 111.8(3) . . ? F1 C23 C22 112.7(3) . . ? F2A C23 C22 111.5(4) . . ? O3 C24 O4 129.5(3) . . ? O3 C24 C25 118.3(3) . . ? O4 C24 C25 112.1(3) . . ? F6A C25 F4A 107.3(4) . . ? F5 C25 F6 107.4(4) . . ? F5 C25 F4 107.1(4) . . ? F6 C25 F4 105.9(4) . . ? F6A C25 F5A 107.4(4) . . ? F4A C25 F5A 106.2(4) . . ? F6A C25 C24 113.4(4) . . ? F5 C25 C24 112.2(4) . . ? F4A C25 C24 112.0(4) . . ? F6 C25 C24 112.6(4) . . ? F4 C25 C24 111.2(4) . . ? F5A C25 C24 110.2(3) . . ? N7 C26 C27 174(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 Ag2 N5 3.3(3) . . . . ? N4 Ag1 Ag2 N5 151.4(3) 1_666 . . . ? O3 Ag1 Ag2 N5 -152.7(6) . . . . ? O1 Ag1 Ag2 N5 -107.6(3) . . . . ? N1 Ag1 Ag2 N3 -149.84(11) . . . 1_666 ? N4 Ag1 Ag2 N3 -1.79(11) 1_666 . . 1_666 ? O3 Ag1 Ag2 N3 54.1(6) . . . 1_666 ? O1 Ag1 Ag2 N3 99.25(10) . . . 1_666 ? N1 Ag1 Ag2 N2 2.70(10) . . . . ? N4 Ag1 Ag2 N2 150.75(10) 1_666 . . . ? O3 Ag1 Ag2 N2 -153.3(6) . . . . ? O1 Ag1 Ag2 N2 -108.21(10) . . . . ? N1 Ag1 Ag2 O2 111.54(11) . . . . ? N4 Ag1 Ag2 O2 -100.41(11) 1_666 . . . ? O3 Ag1 Ag2 O2 -44.5(6) . . . . ? O1 Ag1 Ag2 O2 0.63(10) . . . . ? N4 Ag1 N1 C1 151.9(2) 1_666 . . . ? O3 Ag1 N1 C1 1.8(3) . . . . ? O1 Ag1 N1 C1 -105.5(3) . . . . ? Ag2 Ag1 N1 C1 -173.1(3) . . . . ? N4 Ag1 N1 N2 -39.6(2) 1_666 . . . ? O3 Ag1 N1 N2 170.3(2) . . . . ? O1 Ag1 N1 N2 63.0(2) . . . . ? Ag2 Ag1 N1 N2 -4.60(17) . . . . ? C1 N1 N2 C4 0.9(4) . . . . ? Ag1 N1 N2 C4 -168.6(2) . . . . ? C1 N1 N2 Ag2 176.0(2) . . . . ? Ag1 N1 N2 Ag2 6.5(2) . . . . ? N5 Ag2 N2 C4 -9.6(3) . . . . ? N3 Ag2 N2 C4 -159.9(2) 1_666 . . . ? O2 Ag2 N2 C4 97.4(2) . . . . ? Ag1 Ag2 N2 C4 170.2(3) . . . . ? N5 Ag2 N2 N1 175.5(2) . . . . ? N3 Ag2 N2 N1 25.3(2) 1_666 . . . ? O2 Ag2 N2 N1 -77.5(2) . . . . ? Ag1 Ag2 N2 N1 -4.62(17) . . . . ? C11 N3 N4 C14 -1.0(4) . . . . ? Ag2 N3 N4 C14 -171.1(2) 1_444 . . . ? C11 N3 N4 Ag1 165.8(2) . . . 1_444 ? Ag2 N3 N4 Ag1 -4.3(3) 1_444 . . 1_444 ? N3 Ag2 N5 C15 -1.8(4) 1_666 . . . ? N2 Ag2 N5 C15 -150.1(3) . . . . ? O2 Ag2 N5 C15 103.9(3) . . . . ? Ag1 Ag2 N5 C15 -150.7(3) . . . . ? N3 Ag2 N5 N6 177.6(2) 1_666 . . . ? N2 Ag2 N5 N6 29.3(2) . . . . ? O2 Ag2 N5 N6 -76.7(2) . . . . ? Ag1 Ag2 N5 N6 28.7(5) . . . . ? C15 N5 N6 C18 -0.6(5) . . . . ? Ag2 N5 N6 C18 -180.0(2) . . . . ? N1 Ag1 O1 C22 -67.8(3) . . . . ? N4 Ag1 O1 C22 57.1(3) 1_666 . . . ? O3 Ag1 O1 C22 166.1(3) . . . . ? Ag2 Ag1 O1 C22 -6.4(3) . . . . ? N5 Ag2 O2 C22 170.3(3) . . . . ? N3 Ag2 O2 C22 -59.7(3) 1_666 . . . ? N2 Ag2 O2 C22 65.1(3) . . . . ? Ag1 Ag2 O2 C22 4.4(3) . . . . ? N1 Ag1 O3 C24 37.9(3) . . . . ? N4 Ag1 O3 C24 -115.9(3) 1_666 . . . ? O1 Ag1 O3 C24 147.9(3) . . . . ? Ag2 Ag1 O3 C24 -168.4(4) . . . . ? N2 N1 C1 C2 -2.2(5) . . . . ? Ag1 N1 C1 C2 165.8(2) . . . . ? N1 C1 C2 C3 0.8(5) . . . . ? C1 C2 C3 C4 1.7(4) . . . . ? C1 C2 C3 C5 -176.0(3) . . . . ? N1 N2 C4 C3 1.8(5) . . . . ? Ag2 N2 C4 C3 -172.8(2) . . . . ? C2 C3 C4 N2 -3.0(4) . . . . ? C5 C3 C4 N2 174.7(3) . . . . ? C2 C3 C5 C6 22.6(5) . . . . ? C4 C3 C5 C6 -154.9(3) . . . . ? C2 C3 C5 C10 -159.6(3) . . . . ? C4 C3 C5 C10 22.9(4) . . . . ? C10 C5 C6 C7 -0.6(5) . . . . ? C3 C5 C6 C7 177.3(3) . . . . ? C5 C6 C7 C8 0.7(5) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C6 C7 C8 C13 -179.1(3) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C13 C8 C9 C10 178.7(3) . . . . ? C8 C9 C10 C5 0.1(5) . . . . ? C6 C5 C10 C9 0.1(5) . . . . ? C3 C5 C10 C9 -177.7(3) . . . . ? N4 N3 C11 C12 -0.5(5) . . . . ? Ag2 N3 C11 C12 168.5(3) 1_444 . . . ? N3 C11 C12 C13 1.6(6) . . . . ? C11 C12 C13 C14 -1.2(5) . . . . ? C11 C12 C13 C8 179.6(3) . . . . ? C7 C8 C13 C12 160.8(3) . . . . ? C9 C8 C13 C12 -17.8(5) . . . . ? C7 C8 C13 C14 -18.4(5) . . . . ? C9 C8 C13 C14 163.0(3) . . . . ? N3 N4 C14 C13 1.3(5) . . . . ? Ag1 N4 C14 C13 -163.9(2) 1_444 . . . ? C12 C13 C14 N4 -0.2(5) . . . . ? C8 C13 C14 N4 179.0(3) . . . . ? N6 N5 C15 C16 0.3(6) . . . . ? Ag2 N5 C15 C16 179.7(3) . . . . ? N5 C15 C16 C17 -0.2(6) . . . . ? C15 C16 C17 C18 0.4(5) . . . . ? C15 C16 C17 C20 178.3(3) . . . . ? N5 N6 C18 C17 0.8(5) . . . . ? C16 C17 C18 N6 -0.7(5) . . . . ? C20 C17 C18 N6 -178.6(3) . . . . ? C21 C19 C20 C21 -0.3(5) 2 . . . ? C21 C19 C20 C17 -179.8(3) 2 . . . ? C16 C17 C20 C19 -18.2(5) . . . . ? C18 C17 C20 C19 159.5(3) . . . . ? C16 C17 C20 C21 162.3(3) . . . . ? C18 C17 C20 C21 -20.0(5) . . . . ? C19 C20 C21 C19 0.3(5) . . . 2 ? C17 C20 C21 C19 179.8(3) . . . 2 ? Ag1 O1 C22 O2 13.7(5) . . . . ? Ag1 O1 C22 C23 -171.35(18) . . . . ? Ag2 O2 C22 O1 -12.3(5) . . . . ? Ag2 O2 C22 C23 172.71(19) . . . . ? O1 C22 C23 F3 148.2(5) . . . . ? O2 C22 C23 F3 -35.9(6) . . . . ? O1 C22 C23 F2 -90.8(5) . . . . ? O2 C22 C23 F2 85.2(4) . . . . ? O1 C22 C23 F1 27.5(4) . . . . ? O2 C22 C23 F1 -156.6(4) . . . . ? Ag1 O3 C24 O4 -3.3(5) . . . . ? Ag1 O3 C24 C25 173.1(2) . . . . ? O3 C24 C25 F5 -117.4(7) . . . . ? O4 C24 C25 F5 59.6(6) . . . . ? O3 C24 C25 F6 4.0(7) . . . . ? O4 C24 C25 F6 -179.0(6) . . . . ? O3 C24 C25 F4 122.6(7) . . . . ? O4 C24 C25 F4 -60.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.761 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.086 #----------------------------------------------------# data_(5) _database_code_depnum_ccdc_archive 'CCDC 685686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Pentafluoropropionate 1:1 complex with 1,4-bi(pyridazin-4-yl)benzene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H10 Ag F5 N4 O2' _chemical_formula_weight 505.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5566(7) _cell_length_b 10.5875(13) _cell_length_c 15.419(2) _cell_angle_alpha 72.987(10) _cell_angle_beta 84.721(11) _cell_angle_gamma 82.058(11) _cell_volume 857.81(19) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6535 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.20 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7881 _exptl_absorpt_correction_T_max 0.8346 _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 6535 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 28.20 _reflns_number_total 4169 _reflns_number_gt 2719 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms were located from difference maps and then refined a riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atom). Relatively high thermal values for atoms of pentafluoropropionate group indicated possible disorder. It was not possible to resolve it. The atoms were refined anisotropically for the sake of overall convergence and no geometry restraints were applied. Both unique bipyridazine molecules, either bidentate and tetradentate, lie across inversion centres. ; _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^)+(0.0425P)^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 4169 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.17582(5) 0.04146(2) 0.386125(18) 0.03185(9) Uani 1 1 d . . . O1 O 0.0893(5) -0.0831(3) 0.28858(19) 0.0476(7) Uani 1 1 d . . . O2 O 0.4575(5) -0.1947(4) 0.3118(2) 0.0644(9) Uani 1 1 d . . . F1 F 0.0238(6) -0.2372(4) 0.1849(2) 0.1001(13) Uani 1 1 d . . . F2 F 0.3893(7) -0.3298(2) 0.19990(18) 0.0844(10) Uani 1 1 d . . . F3 F 0.5468(8) -0.0925(5) 0.1038(2) 0.1205(17) Uani 1 1 d . . . F4 F 0.1887(10) -0.0085(4) 0.0816(2) 0.142(2) Uani 1 1 d . . . F5 F 0.3311(6) -0.1702(3) 0.03313(17) 0.0817(10) Uani 1 1 d . . . N1 N 0.3211(5) -0.1271(2) 0.51248(17) 0.0254(5) Uani 1 1 d . . . N2 N 0.1547(5) -0.1783(2) 0.57859(17) 0.0258(5) Uani 1 1 d . . . N3 N 0.4131(5) 0.1713(2) 0.26941(17) 0.0288(6) Uani 1 1 d . . . N4 N 0.3307(5) 0.2994(3) 0.22958(18) 0.0307(6) Uani 1 1 d . . . C1 C 0.5214(6) -0.2032(3) 0.4983(2) 0.0248(6) Uani 1 1 d . . . H1 H 0.6378 -0.1643 0.4540 0.030 Uiso 1 1 calc R . . C2 C 0.5717(5) -0.3385(3) 0.54517(19) 0.0227(6) Uani 1 1 d . . . C3 C 0.3984(6) -0.3893(3) 0.6124(2) 0.0256(6) Uani 1 1 d . . . H3 H 0.4187 -0.4788 0.6474 0.031 Uiso 1 1 calc R . . C4 C 0.1939(6) -0.3044(3) 0.6268(2) 0.0258(6) Uani 1 1 d . . . H4 H 0.0776 -0.3384 0.6730 0.031 Uiso 1 1 calc R . . C5 C 0.8863(6) -0.5359(3) 0.5854(2) 0.0295(7) Uani 1 1 d . . . H5 H 0.8084 -0.5608 0.6436 0.035 Uiso 1 1 calc R . . C6 C 0.7925(5) -0.4202(3) 0.5219(2) 0.0231(6) Uani 1 1 d . . . C7 C 0.9094(6) -0.3852(3) 0.4348(2) 0.0292(7) Uani 1 1 d . . . H7 H 0.8489 -0.3083 0.3905 0.035 Uiso 1 1 calc R . . C8 C 0.6289(6) 0.1204(3) 0.2418(2) 0.0297(7) Uani 1 1 d . . . H8 H 0.6807 0.0299 0.2682 0.036 Uiso 1 1 calc R . . C9 C 0.7814(6) 0.1948(3) 0.1756(2) 0.0296(7) Uani 1 1 d . . . H9 H 0.9346 0.1559 0.1591 0.035 Uiso 1 1 calc R . . C10 C 0.7042(6) 0.3257(3) 0.1349(2) 0.0255(6) Uani 1 1 d . . . C11 C 0.4691(6) 0.3717(3) 0.1647(2) 0.0286(6) Uani 1 1 d . . . H11 H 0.4066 0.4600 0.1364 0.034 Uiso 1 1 calc R . . C12 C 1.0220(6) 0.3661(3) 0.0069(2) 0.0312(7) Uani 1 1 d . . . H12 H 1.0380 0.2750 0.0109 0.037 Uiso 1 1 calc R . . C13 C 0.8543(6) 0.4155(3) 0.0654(2) 0.0262(6) Uani 1 1 d . . . C14 C 0.8345(6) 0.5513(3) 0.0571(2) 0.0327(7) Uani 1 1 d . . . H14 H 0.7221 0.5873 0.0955 0.039 Uiso 1 1 calc R . . C15 C 0.2676(7) -0.1593(3) 0.2742(2) 0.0325(7) Uani 1 1 d . . . C16 C 0.2501(7) -0.2118(3) 0.1909(3) 0.0403(8) Uani 1 1 d . . . C17 C 0.3300(9) -0.1208(4) 0.1016(3) 0.0477(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 0.03177(15) 0.02695(12) 0.02994(13) -0.00311(8) 0.00858(10) 0.00234(8) O1 0.0454(16) 0.0456(14) 0.0568(16) -0.0276(13) -0.0059(14) 0.0088(12) O2 0.0419(18) 0.101(3) 0.0480(17) -0.0235(17) -0.0132(16) 0.0107(16) F1 0.077(2) 0.180(4) 0.087(2) -0.086(2) 0.0256(18) -0.077(2) F2 0.153(3) 0.0345(12) 0.0517(15) -0.0113(11) 0.0275(18) 0.0120(15) F3 0.119(3) 0.196(4) 0.0498(16) -0.004(2) 0.0098(19) -0.107(3) F4 0.239(6) 0.085(2) 0.0521(18) 0.0092(17) 0.017(3) 0.074(3) F5 0.121(3) 0.097(2) 0.0384(13) -0.0330(15) 0.0108(16) -0.0325(19) N1 0.0238(14) 0.0240(12) 0.0245(12) -0.0044(10) 0.0023(11) 0.0022(10) N2 0.0228(14) 0.0289(12) 0.0244(12) -0.0084(10) 0.0043(12) -0.0005(10) N3 0.0269(15) 0.0312(13) 0.0257(13) -0.0040(11) 0.0054(12) -0.0074(11) N4 0.0261(15) 0.0315(13) 0.0302(14) -0.0036(11) 0.0043(12) -0.0043(11) C1 0.0225(16) 0.0256(14) 0.0235(14) -0.0046(11) 0.0046(13) -0.0023(11) C2 0.0208(15) 0.0252(14) 0.0218(14) -0.0081(11) -0.0018(13) 0.0013(11) C3 0.0238(16) 0.0229(14) 0.0264(15) -0.0030(11) 0.0027(14) -0.0021(11) C4 0.0212(16) 0.0290(15) 0.0247(15) -0.0053(12) 0.0041(13) -0.0034(11) C5 0.0298(18) 0.0307(15) 0.0218(14) -0.0016(12) 0.0058(14) -0.0001(13) C6 0.0198(15) 0.0216(13) 0.0272(15) -0.0068(11) 0.0005(13) -0.0012(11) C7 0.0306(18) 0.0214(14) 0.0282(16) 0.0005(12) -0.0007(15) 0.0045(12) C8 0.0306(18) 0.0245(14) 0.0308(16) -0.0030(12) 0.0012(15) -0.0044(12) C9 0.0221(16) 0.0320(16) 0.0321(16) -0.0084(13) 0.0083(15) -0.0024(12) C10 0.0257(17) 0.0297(15) 0.0218(14) -0.0088(12) 0.0048(13) -0.0059(12) C11 0.0262(17) 0.0266(14) 0.0281(15) -0.0020(12) 0.0023(14) -0.0018(12) C12 0.0359(19) 0.0241(14) 0.0330(17) -0.0094(13) 0.0113(16) -0.0078(13) C13 0.0254(17) 0.0281(15) 0.0236(14) -0.0051(12) 0.0058(14) -0.0077(12) C14 0.0332(19) 0.0315(16) 0.0317(17) -0.0111(13) 0.0156(16) -0.0043(13) C15 0.037(2) 0.0301(16) 0.0286(16) -0.0064(13) 0.0018(16) -0.0059(14) C16 0.048(2) 0.0356(18) 0.0407(19) -0.0161(16) 0.0048(18) -0.0079(16) C17 0.069(3) 0.0387(19) 0.0339(19) -0.0072(16) -0.006(2) -0.0061(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 N2 2.304(3) 2_556 ? Ag1 N3 2.341(3) . ? Ag1 N1 2.343(2) . ? Ag1 O1 2.388(2) . ? O1 C15 1.235(4) . ? O2 C15 1.211(4) . ? F1 C16 1.339(5) . ? F2 C16 1.353(5) . ? F3 C17 1.287(5) . ? F4 C17 1.303(5) . ? F5 C17 1.307(4) . ? N1 C1 1.321(4) . ? N1 N2 1.353(4) . ? N2 C4 1.324(4) . ? N2 Ag1 2.304(3) 2_556 ? N3 C8 1.331(4) . ? N3 N4 1.349(4) . ? N4 C11 1.323(4) . ? C1 C2 1.404(4) . ? C1 H1 0.9400 . ? C2 C3 1.387(4) . ? C2 C6 1.480(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C7 1.382(4) 2_746 ? C5 C6 1.395(4) . ? C5 H5 0.9400 . ? C6 C7 1.406(4) . ? C7 C5 1.382(4) 2_746 ? C7 H7 0.9400 . ? C8 C9 1.391(5) . ? C8 H8 0.9400 . ? C9 C10 1.370(4) . ? C9 H9 0.9400 . ? C10 C11 1.414(4) . ? C10 C13 1.486(4) . ? C11 H11 0.9400 . ? C12 C14 1.384(4) 2_765 ? C12 C13 1.395(4) . ? C12 H12 0.9400 . ? C13 C14 1.395(4) . ? C14 C12 1.384(4) 2_765 ? C14 H14 0.9400 . ? C15 C16 1.557(4) . ? C16 C17 1.500(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 N2 Ag1 N3 108.01(9) 2_556 . ? N2 Ag1 N1 113.36(9) 2_556 . ? N3 Ag1 N1 126.20(9) . . ? N2 Ag1 O1 113.85(9) 2_556 . ? N3 Ag1 O1 90.87(9) . . ? N1 Ag1 O1 101.95(9) . . ? C15 O1 Ag1 112.0(2) . . ? C1 N1 N2 119.4(2) . . ? C1 N1 Ag1 116.59(19) . . ? N2 N1 Ag1 117.08(18) . . ? C4 N2 N1 119.3(2) . . ? C4 N2 Ag1 120.8(2) . 2_556 ? N1 N2 Ag1 119.76(18) . 2_556 ? C8 N3 N4 119.4(2) . . ? C8 N3 Ag1 120.9(2) . . ? N4 N3 Ag1 119.7(2) . . ? C11 N4 N3 118.8(3) . . ? N1 C1 C2 124.3(3) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 115.4(3) . . ? C3 C2 C6 123.1(3) . . ? C1 C2 C6 121.5(3) . . ? C2 C3 C4 118.3(3) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? N2 C4 C3 123.3(3) . . ? N2 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C7 C5 C6 121.8(3) 2_746 . ? C7 C5 H5 119.1 2_746 . ? C6 C5 H5 119.1 . . ? C5 C6 C7 118.4(3) . . ? C5 C6 C2 120.6(3) . . ? C7 C6 C2 121.0(3) . . ? C5 C7 C6 119.8(3) 2_746 . ? C5 C7 H7 120.1 2_746 . ? C6 C7 H7 120.1 . . ? N3 C8 C9 123.1(3) . . ? N3 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 115.1(3) . . ? C9 C10 C13 123.5(3) . . ? C11 C10 C13 121.4(3) . . ? N4 C11 C10 124.7(3) . . ? N4 C11 H11 117.7 . . ? C10 C11 H11 117.7 . . ? C14 C12 C13 121.2(3) 2_765 . ? C14 C12 H12 119.4 2_765 . ? C13 C12 H12 119.4 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 C10 120.8(3) . . ? C14 C13 C10 121.4(3) . . ? C12 C14 C13 121.0(3) 2_765 . ? C12 C14 H14 119.5 2_765 . ? C13 C14 H14 119.5 . . ? O2 C15 O1 130.4(3) . . ? O2 C15 C16 115.0(3) . . ? O1 C15 C16 114.4(3) . . ? F1 C16 F2 104.7(3) . . ? F1 C16 C17 108.5(3) . . ? F2 C16 C17 106.4(3) . . ? F1 C16 C15 111.3(3) . . ? F2 C16 C15 111.0(3) . . ? C17 C16 C15 114.4(3) . . ? F3 C17 F4 106.9(4) . . ? F3 C17 F5 106.8(4) . . ? F4 C17 F5 106.6(4) . . ? F3 C17 C16 111.0(3) . . ? F4 C17 C16 111.3(4) . . ? F5 C17 C16 113.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 O1 C15 -177.2(2) 2_556 . . . ? N3 Ag1 O1 C15 72.7(3) . . . . ? N1 Ag1 O1 C15 -54.7(3) . . . . ? N2 Ag1 N1 C1 -175.18(18) 2_556 . . . ? N3 Ag1 N1 C1 -38.0(2) . . . . ? O1 Ag1 N1 C1 62.0(2) . . . . ? N2 Ag1 N1 N2 34.1(2) 2_556 . . . ? N3 Ag1 N1 N2 171.28(16) . . . . ? O1 Ag1 N1 N2 -88.69(19) . . . . ? C1 N1 N2 C4 -1.2(4) . . . . ? Ag1 N1 N2 C4 148.7(2) . . . . ? C1 N1 N2 Ag1 173.77(19) . . . 2_556 ? Ag1 N1 N2 Ag1 -36.4(2) . . . 2_556 ? N2 Ag1 N3 C8 173.1(2) 2_556 . . . ? N1 Ag1 N3 C8 34.1(3) . . . . ? O1 Ag1 N3 C8 -71.4(2) . . . . ? N2 Ag1 N3 N4 -6.8(2) 2_556 . . . ? N1 Ag1 N3 N4 -145.76(19) . . . . ? O1 Ag1 N3 N4 108.7(2) . . . . ? C8 N3 N4 C11 -0.9(4) . . . . ? Ag1 N3 N4 C11 179.0(2) . . . . ? N2 N1 C1 C2 2.9(4) . . . . ? Ag1 N1 C1 C2 -147.1(2) . . . . ? N1 C1 C2 C3 -2.6(4) . . . . ? N1 C1 C2 C6 176.0(3) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C6 C2 C3 C4 -178.0(2) . . . . ? N1 N2 C4 C3 -0.8(4) . . . . ? Ag1 N2 C4 C3 -175.7(2) 2_556 . . . ? C2 C3 C4 N2 1.0(4) . . . . ? C7 C5 C6 C7 0.7(5) 2_746 . . . ? C7 C5 C6 C2 179.3(3) 2_746 . . . ? C3 C2 C6 C5 -24.2(4) . . . . ? C1 C2 C6 C5 157.2(3) . . . . ? C3 C2 C6 C7 154.3(3) . . . . ? C1 C2 C6 C7 -24.2(4) . . . . ? C5 C6 C7 C5 -0.7(5) . . . 2_746 ? C2 C6 C7 C5 -179.3(3) . . . 2_746 ? N4 N3 C8 C9 2.8(4) . . . . ? Ag1 N3 C8 C9 -177.1(2) . . . . ? N3 C8 C9 C10 -1.8(5) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C8 C9 C10 C13 178.2(3) . . . . ? N3 N4 C11 C10 -2.0(4) . . . . ? C9 C10 C11 N4 2.8(4) . . . . ? C13 C10 C11 N4 -176.3(3) . . . . ? C14 C12 C13 C14 0.4(5) 2_765 . . . ? C14 C12 C13 C10 -178.9(3) 2_765 . . . ? C9 C10 C13 C12 30.7(4) . . . . ? C11 C10 C13 C12 -150.2(3) . . . . ? C9 C10 C13 C14 -148.6(3) . . . . ? C11 C10 C13 C14 30.5(4) . . . . ? C12 C13 C14 C12 -0.4(5) . . . 2_765 ? C10 C13 C14 C12 178.9(3) . . . 2_765 ? Ag1 O1 C15 O2 13.2(5) . . . . ? Ag1 O1 C15 C16 -163.0(2) . . . . ? O2 C15 C16 F1 144.7(4) . . . . ? O1 C15 C16 F1 -38.5(4) . . . . ? O2 C15 C16 F2 28.5(5) . . . . ? O1 C15 C16 F2 -154.7(3) . . . . ? O2 C15 C16 C17 -92.0(4) . . . . ? O1 C15 C16 C17 84.8(4) . . . . ? F1 C16 C17 F3 179.7(4) . . . . ? F2 C16 C17 F3 -68.1(4) . . . . ? C15 C16 C17 F3 54.8(5) . . . . ? F1 C16 C17 F4 60.7(5) . . . . ? F2 C16 C17 F4 172.9(4) . . . . ? C15 C16 C17 F4 -64.2(5) . . . . ? F1 C16 C17 F5 -59.8(5) . . . . ? F2 C16 C17 F5 52.4(5) . . . . ? C15 C16 C17 F5 175.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.624 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.092 #----------------------------------------------------# data_(6) _database_code_depnum_ccdc_archive 'CCDC 685687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Methanesulfonate 4:3 complex with 1,4-bi(pyridazin-4-yl)benzene, solvate with 2 Chloroform ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Ag4 Cl6 N12 O12 S4' _chemical_formula_weight 1753.37 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 19.3101(19) _cell_length_b 17.3714(15) _cell_length_c 18.1903(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.346(5) _cell_angle_gamma 90.00 _cell_volume 6020.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 10705 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6484 _exptl_absorpt_correction_T_max 0.7202 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 20 _diffrn_reflns_number 25245 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10705 _reflns_number_gt 7019 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms (aromatic CH) were located from difference maps, while methyl CH~3~ atoms were added geometrically and then refined a riding, with C---H distances (aromatic CH) constrained to 0.94 \%A, C---H distances (methyl) constrained to 0.97 \%A, and with U~iso~(H) = 1.2U~eq~ (parent aromatic carbon atom) and U~iso~(H) = 1.5U~eq~ (parent methyl carbon atoms). One of the unique methanesulfonate anions is equally disordered over two overlapping position. The disorder was resolved with a set of restraints in geometry: S---C 1.77(1) \%A, S---O 1.45(1) \%A and with idealized tetrahedral geometry around sulfur atom. In total, this produces 14 restraints during the structure refinement. Also, EADP constraint was applied separately to atoms of each of the disorder components. The hydrogen atoms were not added to this disordered methanesulfonate. Both solvate chloroform molecules were badly disordered and was impossible to find a resonable and refinable disordering scheme. Therefore, the remaining electron density in the structure was modelled using a SQUEEZE routine. ; _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^)+(0.0850P)^2^+40.2604P] 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 0.0011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10705 _refine_ls_number_parameters 713 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2555 _refine_ls_wR_factor_gt 0.2418 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.25729(4) 0.13552(5) 0.25530(4) 0.0495(3) Uani 1 1 d . . . Ag2 Ag 0.38938(4) 0.02106(7) 0.34088(5) 0.0630(3) Uani 1 1 d . . . Ag3 Ag 0.23864(5) -0.07180(6) 0.24021(5) 0.0585(3) Uani 1 1 d . . . Ag4 Ag 0.10674(4) 0.05295(7) 0.15644(5) 0.0637(3) Uani 1 1 d . . . S1 S 0.3638(2) 0.2431(2) 0.4052(3) 0.0899(13) Uani 1 1 d . . . S2 S 0.4034(2) -0.1597(2) 0.2584(2) 0.0867(13) Uani 1 1 d . . . S3 S 0.0663(2) -0.1335(3) 0.2119(3) 0.1028(17) Uani 1 1 d . . . N1 N 0.3449(4) 0.1168(4) 0.1935(4) 0.0382(17) Uani 1 1 d . . . N2 N 0.3944(4) 0.0690(5) 0.2236(4) 0.0393(18) Uani 1 1 d . . . N3 N 0.8043(5) -0.0224(6) -0.0959(5) 0.058(2) Uani 1 1 d . . . N4 N 0.7558(4) 0.0291(5) -0.1243(4) 0.044(2) Uani 1 1 d . . . N5 N 0.2955(4) -0.0021(5) 0.3956(4) 0.0408(18) Uani 1 1 d . . . N6 N 0.2390(4) -0.0412(4) 0.3607(4) 0.0403(19) Uani 1 1 d . . . N7 N -0.1661(4) -0.1255(5) 0.6857(4) 0.0425(19) Uani 1 1 d . . . N8 N -0.1101(4) -0.0878(5) 0.7205(4) 0.0388(18) Uani 1 1 d . . . N9 N 0.4955(5) 0.0714(8) 0.4022(6) 0.075(3) Uani 1 1 d . . . N10 N 0.5055(7) 0.0948(8) 0.4712(7) 0.093(4) Uani 1 1 d . . . N11 N 0.9984(5) 0.3930(7) 0.6060(6) 0.073(3) Uani 1 1 d . . . N12 N 0.9692(10) 0.4027(11) 0.5354(9) 0.138(7) Uani 1 1 d . . . C1 C 0.3525(5) 0.1505(6) 0.1329(5) 0.047(2) Uani 1 1 d . . . H1 H 0.3176 0.1858 0.1128 0.056 Uiso 1 1 calc R . . C2 C 0.4086(5) 0.1392(6) 0.0939(6) 0.049(3) Uani 1 1 d . . . H2 H 0.4105 0.1650 0.0489 0.058 Uiso 1 1 calc R . . C3 C 0.4600(5) 0.0899(6) 0.1234(5) 0.039(2) Uani 1 1 d . . . C4 C 0.4502(4) 0.0547(6) 0.1895(5) 0.039(2) Uani 1 1 d . . . H4 H 0.4841 0.0193 0.2115 0.047 Uiso 1 1 calc R . . C5 C 0.7995(6) -0.0554(12) -0.0307(6) 0.100(6) Uani 1 1 d . . . H5 H 0.8333 -0.0920 -0.0109 0.120 Uiso 1 1 calc R . . C6 C 0.7455(6) -0.0369(10) 0.0087(6) 0.080(5) Uani 1 1 d . . . H6 H 0.7440 -0.0597 0.0553 0.096 Uiso 1 1 calc R . . C7 C 0.6948(5) 0.0145(7) -0.0206(5) 0.045(2) Uani 1 1 d . . . C8 C 0.7032(5) 0.0449(6) -0.0888(5) 0.040(2) Uani 1 1 d . . . H8 H 0.6688 0.0794 -0.1116 0.048 Uiso 1 1 calc R . . C9 C 0.5203(5) 0.0723(6) 0.0877(5) 0.039(2) Uani 1 1 d . . . C10 C 0.5529(5) 0.0017(6) 0.0983(5) 0.041(2) Uani 1 1 d . . . H10 H 0.5363 -0.0349 0.1294 0.049 Uiso 1 1 calc R . . C11 C 0.6103(5) -0.0162(6) 0.0636(6) 0.045(2) Uani 1 1 d . . . H11 H 0.6327 -0.0641 0.0727 0.054 Uiso 1 1 calc R . . C12 C 0.6342(5) 0.0347(6) 0.0167(5) 0.036(2) Uani 1 1 d . . . C13 C 0.5993(6) 0.1054(6) 0.0039(7) 0.060(3) Uani 1 1 d . . . H13 H 0.6144 0.1412 -0.0289 0.072 Uiso 1 1 calc R . . C14 C 0.5446(6) 0.1225(6) 0.0381(7) 0.059(3) Uani 1 1 d . . . H14 H 0.5219 0.1702 0.0281 0.070 Uiso 1 1 calc R . . C15 C 0.2966(5) 0.0179(7) 0.4663(5) 0.049(3) Uani 1 1 d . . . H15 H 0.3370 0.0423 0.4916 0.059 Uiso 1 1 calc R . . C16 C 0.2419(5) 0.0048(7) 0.5042(5) 0.053(3) Uani 1 1 d . . . H16 H 0.2439 0.0224 0.5534 0.064 Uiso 1 1 calc R . . C17 C 0.1841(5) -0.0346(5) 0.4690(5) 0.039(2) Uani 1 1 d . . . C18 C 0.1853(5) -0.0553(6) 0.3953(6) 0.045(2) Uani 1 1 d . . . H18 H 0.1459 -0.0805 0.3688 0.054 Uiso 1 1 calc R . . C19 C -0.1651(5) -0.1536(6) 0.6204(6) 0.049(3) Uani 1 1 d . . . H19 H -0.2040 -0.1824 0.5978 0.059 Uiso 1 1 calc R . . C20 C -0.1088(6) -0.1435(7) 0.5809(6) 0.055(3) Uani 1 1 d . . . H20 H -0.1106 -0.1638 0.5327 0.066 Uiso 1 1 calc R . . C21 C -0.0522(5) -0.1040(6) 0.6141(5) 0.045(2) Uani 1 1 d . . . C22 C -0.0550(5) -0.0772(6) 0.6867(5) 0.044(2) Uani 1 1 d . . . H22 H -0.0160 -0.0506 0.7123 0.053 Uiso 1 1 calc R . . C23 C 0.1226(4) -0.0514(5) 0.5070(5) 0.035(2) Uani 1 1 d . . . C24 C 0.1061(5) -0.0043(6) 0.5616(5) 0.046(2) Uani 1 1 d . . . H24 H 0.1337 0.0395 0.5755 0.055 Uiso 1 1 calc R . . C25 C 0.0493(5) -0.0202(6) 0.5968(5) 0.042(2) Uani 1 1 d . . . H25 H 0.0373 0.0137 0.6329 0.051 Uiso 1 1 calc R . . C26 C 0.0095(5) -0.0874(6) 0.5782(5) 0.044(2) Uani 1 1 d . . . C27 C 0.0240(5) -0.1344(6) 0.5207(6) 0.050(3) Uani 1 1 d . . . H27 H -0.0041 -0.1777 0.5060 0.060 Uiso 1 1 calc R . . C28 C 0.0811(5) -0.1164(6) 0.4852(6) 0.045(2) Uani 1 1 d . . . H28 H 0.0916 -0.1479 0.4465 0.054 Uiso 1 1 calc R . . C29 C 0.5457(6) 0.0743(13) 0.3635(7) 0.116(8) Uani 1 1 d . . . H29 H 0.5435 0.0457 0.3193 0.139 Uiso 1 1 calc R . . C30 C 0.6006(8) 0.1188(17) 0.3879(10) 0.154(11) Uani 1 1 d . . . H30 H 0.6331 0.1262 0.3553 0.185 Uiso 1 1 calc R . . C31 C 0.6147(6) 0.1554(8) 0.4566(6) 0.062(3) Uani 1 1 d . . . C32 C 0.5660(7) 0.1379(8) 0.4997(7) 0.066(3) Uani 1 1 d . . . H32 H 0.5725 0.1547 0.5494 0.079 Uiso 1 1 calc R . . C33 C 0.9696(7) 0.3451(11) 0.6510(7) 0.087(5) Uani 1 1 d . . . H33 H 0.9927 0.3356 0.6997 0.104 Uiso 1 1 calc R . . C34 C 0.9104(7) 0.3124(12) 0.6269(8) 0.102(6) Uani 1 1 d . . . H34 H 0.8901 0.2819 0.6604 0.123 Uiso 1 1 calc R . . C35 C 0.8741(6) 0.3197(7) 0.5533(7) 0.059(3) Uani 1 1 d . . . C36 C 0.9073(8) 0.3649(9) 0.5081(8) 0.086(5) Uani 1 1 d . . . H36 H 0.8877 0.3704 0.4576 0.103 Uiso 1 1 calc R . . C37 C 0.6806(6) 0.1988(7) 0.4815(6) 0.057(3) Uani 1 1 d . . . C38 C 0.7060(6) 0.2078(7) 0.5560(7) 0.064(3) Uani 1 1 d . . . H38 H 0.6809 0.1867 0.5914 0.077 Uiso 1 1 calc R . . C39 C 0.7678(6) 0.2474(7) 0.5802(6) 0.061(3) Uani 1 1 d . . . H39 H 0.7843 0.2525 0.6316 0.073 Uiso 1 1 calc R . . C40 C 0.8058(6) 0.2798(7) 0.5288(7) 0.059(3) Uani 1 1 d . . . C41 C 0.7793(7) 0.2702(8) 0.4550(7) 0.071(3) Uani 1 1 d . . . H41 H 0.8036 0.2923 0.4195 0.085 Uiso 1 1 calc R . . C42 C 0.7189(6) 0.2299(9) 0.4300(7) 0.073(4) Uani 1 1 d . . . H42 H 0.7035 0.2233 0.3786 0.087 Uiso 1 1 calc R . . C43 C 0.4127(13) 0.2709(12) 0.3377(13) 0.145(9) Uani 1 1 d . . . H43A H 0.4458 0.2305 0.3308 0.218 Uiso 1 1 calc R . . H43B H 0.4382 0.3178 0.3534 0.218 Uiso 1 1 calc R . . H43C H 0.3816 0.2800 0.2910 0.218 Uiso 1 1 calc R . . C44 C 0.4414(14) -0.2489(11) 0.2887(14) 0.171(12) Uani 1 1 d . . . H44A H 0.4228 -0.2659 0.3324 0.257 Uiso 1 1 calc R . . H44B H 0.4919 -0.2431 0.3010 0.257 Uiso 1 1 calc R . . H44C H 0.4303 -0.2866 0.2493 0.257 Uiso 1 1 calc R . . C45 C 0.0177(13) -0.2155(12) 0.1755(12) 0.150(10) Uani 1 1 d . . . H45A H 0.0342 -0.2325 0.1305 0.226 Uiso 1 1 calc R . . H45B H -0.0317 -0.2023 0.1638 0.226 Uiso 1 1 calc R . . H45C H 0.0240 -0.2566 0.2121 0.226 Uiso 1 1 calc R . . O1 O 0.3329(6) 0.1696(6) 0.3828(6) 0.098(3) Uani 1 1 d . . . O2 O 0.4158(7) 0.2357(9) 0.4735(8) 0.141(5) Uani 1 1 d . . . O3 O 0.3168(7) 0.3012(7) 0.4161(9) 0.132(5) Uani 1 1 d . . . O4 O 0.4128(11) -0.1142(9) 0.3224(7) 0.165(7) Uani 1 1 d . . . O5 O 0.3260(7) -0.1702(8) 0.2340(10) 0.142(5) Uani 1 1 d . . . O6 O 0.4309(7) -0.1363(7) 0.1949(7) 0.117(4) Uani 1 1 d . . . O7 O 0.1351(9) -0.1569(9) 0.2221(13) 0.175(8) Uani 1 1 d . . . O8 O 0.0620(13) -0.0770(10) 0.1533(10) 0.194(9) Uani 1 1 d . . . O9 O 0.0428(9) -0.1099(11) 0.2760(8) 0.180(8) Uani 1 1 d . . . S4 S 0.1485(8) 0.2588(9) 0.1060(10) 0.155(9) Uani 0.50 1 d PD . . C46 C 0.102(2) 0.295(2) 0.1748(16) 0.093(4) Uani 0.50 1 d PD . . O10 O 0.1863(10) 0.1914(10) 0.1347(11) 0.093(4) Uani 0.50 1 d PD . . O11 O 0.0924(9) 0.2409(11) 0.0447(11) 0.093(4) Uani 0.50 1 d PD . . O12 O 0.1918(10) 0.3212(9) 0.0876(13) 0.093(4) Uani 0.50 1 d PD . . S4A S 0.1655(5) 0.2744(6) 0.1267(6) 0.071(3) Uani 0.50 1 d PD . . C46A C 0.116(3) 0.291(3) 0.1988(19) 0.131(6) Uani 0.50 1 d PD . . O10A O 0.2268(9) 0.2381(12) 0.1677(12) 0.131(6) Uani 0.50 1 d PD . . O11A O 0.1234(12) 0.2237(11) 0.0748(14) 0.131(6) Uani 0.50 1 d PD . . O12A O 0.1810(11) 0.3466(9) 0.0933(15) 0.131(6) Uani 0.50 1 d PD . . 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 0.0447(4) 0.0587(5) 0.0536(5) 0.0023(4) 0.0338(4) 0.0031(4) Ag2 0.0433(5) 0.1080(8) 0.0433(5) 0.0100(4) 0.0239(4) -0.0015(5) Ag3 0.0706(6) 0.0677(6) 0.0470(5) 0.0020(4) 0.0387(4) 0.0010(4) Ag4 0.0421(5) 0.1095(8) 0.0447(5) -0.0015(5) 0.0233(4) 0.0142(5) S1 0.088(2) 0.078(2) 0.117(3) -0.046(2) 0.058(2) -0.035(2) S2 0.120(3) 0.071(2) 0.084(2) 0.0329(19) 0.060(2) 0.052(2) S3 0.097(3) 0.114(3) 0.113(3) -0.068(3) 0.063(3) -0.072(3) N1 0.038(4) 0.039(4) 0.043(4) -0.001(3) 0.021(3) 0.008(3) N2 0.037(4) 0.055(5) 0.030(4) 0.000(3) 0.018(3) 0.005(4) N3 0.040(5) 0.098(7) 0.040(5) 0.004(5) 0.019(4) 0.002(5) N4 0.037(4) 0.059(5) 0.040(4) -0.006(4) 0.020(4) -0.013(4) N5 0.041(4) 0.049(5) 0.037(4) -0.002(4) 0.019(3) 0.002(4) N6 0.056(5) 0.031(4) 0.040(4) 0.004(3) 0.029(4) 0.001(4) N7 0.036(4) 0.057(5) 0.037(4) 0.007(4) 0.014(3) 0.006(4) N8 0.030(4) 0.064(5) 0.025(4) 0.006(4) 0.014(3) 0.000(4) N9 0.038(5) 0.139(10) 0.048(6) -0.021(6) 0.003(4) -0.011(6) N10 0.100(9) 0.094(9) 0.084(9) 0.005(7) 0.009(7) -0.008(8) N11 0.051(5) 0.092(8) 0.066(7) -0.010(6) -0.021(5) 0.002(5) N12 0.138(13) 0.160(15) 0.097(11) 0.034(10) -0.045(10) -0.044(12) C1 0.048(5) 0.057(6) 0.042(5) 0.010(5) 0.024(5) 0.019(5) C2 0.058(6) 0.047(6) 0.049(6) 0.018(5) 0.031(5) 0.014(5) C3 0.042(5) 0.046(5) 0.036(5) -0.002(4) 0.025(4) -0.003(4) C4 0.025(4) 0.063(6) 0.031(5) 0.007(4) 0.004(4) 0.003(4) C5 0.042(6) 0.225(19) 0.036(6) 0.036(9) 0.017(5) 0.047(9) C6 0.045(6) 0.161(14) 0.040(6) 0.026(7) 0.023(5) 0.037(8) C7 0.033(5) 0.075(7) 0.033(5) -0.007(5) 0.018(4) -0.002(5) C8 0.041(5) 0.045(5) 0.039(5) -0.005(4) 0.026(4) -0.005(4) C9 0.037(5) 0.053(6) 0.030(5) -0.002(4) 0.014(4) 0.008(4) C10 0.045(5) 0.052(6) 0.029(5) 0.014(4) 0.018(4) 0.005(5) C11 0.045(5) 0.048(6) 0.047(6) 0.004(5) 0.020(5) 0.016(5) C12 0.033(4) 0.053(6) 0.027(4) 0.000(4) 0.019(4) -0.009(4) C13 0.076(7) 0.048(6) 0.072(7) -0.012(5) 0.059(6) -0.008(6) C14 0.070(7) 0.043(6) 0.077(8) 0.010(5) 0.056(6) 0.007(5) C15 0.038(5) 0.079(8) 0.033(5) 0.002(5) 0.012(4) 0.001(5) C16 0.040(5) 0.089(8) 0.032(5) -0.009(5) 0.015(4) 0.000(5) C17 0.043(5) 0.046(5) 0.032(5) 0.007(4) 0.020(4) 0.008(4) C18 0.039(5) 0.049(6) 0.054(6) 0.003(5) 0.029(5) -0.002(4) C19 0.041(5) 0.063(7) 0.051(6) 0.008(5) 0.028(5) 0.006(5) C20 0.068(7) 0.065(7) 0.041(6) 0.008(5) 0.033(5) 0.021(6) C21 0.036(5) 0.063(7) 0.043(5) 0.010(5) 0.023(4) 0.007(5) C22 0.030(4) 0.077(7) 0.027(5) 0.003(5) 0.009(4) 0.010(5) C23 0.033(4) 0.037(5) 0.040(5) 0.006(4) 0.019(4) 0.002(4) C24 0.043(5) 0.055(6) 0.045(6) -0.005(5) 0.022(5) 0.007(5) C25 0.045(5) 0.054(6) 0.031(5) -0.005(4) 0.019(4) -0.002(5) C26 0.047(5) 0.054(6) 0.037(5) 0.007(4) 0.023(4) 0.014(5) C27 0.052(6) 0.052(6) 0.054(6) -0.004(5) 0.035(5) 0.001(5) C28 0.049(5) 0.043(6) 0.052(6) -0.005(4) 0.033(5) 0.001(5) C29 0.041(6) 0.26(2) 0.044(7) -0.051(10) 0.002(6) -0.053(10) C30 0.056(8) 0.32(3) 0.087(11) -0.098(16) 0.023(8) -0.048(14) C31 0.042(6) 0.096(9) 0.042(6) -0.011(6) -0.008(5) 0.006(6) C32 0.074(8) 0.081(9) 0.043(6) -0.015(6) 0.008(6) -0.025(7) C33 0.056(7) 0.165(15) 0.041(6) -0.017(8) 0.014(6) -0.043(9) C34 0.054(7) 0.194(18) 0.058(8) -0.011(10) 0.004(6) -0.039(10) C35 0.049(6) 0.057(7) 0.062(7) -0.014(6) -0.014(5) 0.012(5) C36 0.080(9) 0.092(10) 0.070(9) 0.004(8) -0.029(7) -0.038(8) C37 0.047(6) 0.070(8) 0.052(6) -0.022(6) 0.000(5) 0.008(5) C38 0.065(7) 0.062(7) 0.058(7) -0.003(6) -0.009(6) -0.004(6) C39 0.061(7) 0.072(8) 0.044(6) -0.006(6) -0.008(5) 0.004(6) C40 0.056(6) 0.056(7) 0.063(7) -0.012(6) 0.001(6) 0.008(6) C41 0.064(7) 0.089(9) 0.059(8) -0.005(7) 0.009(6) -0.019(7) C42 0.053(7) 0.118(11) 0.045(7) -0.006(7) 0.002(5) -0.010(7) C43 0.19(2) 0.102(14) 0.17(2) -0.018(13) 0.123(18) -0.058(14) C44 0.23(2) 0.109(14) 0.21(2) 0.109(15) 0.15(2) 0.136(16) C45 0.18(2) 0.137(17) 0.143(17) -0.090(14) 0.067(15) -0.119(16) O1 0.110(8) 0.099(7) 0.095(7) -0.050(6) 0.047(6) -0.055(6) O2 0.113(9) 0.161(12) 0.138(11) -0.097(10) -0.011(8) -0.001(9) O3 0.123(10) 0.092(8) 0.194(14) -0.008(9) 0.063(10) 0.007(8) O4 0.27(2) 0.146(12) 0.072(8) -0.004(8) 0.020(10) 0.085(13) O5 0.092(8) 0.120(10) 0.222(16) -0.021(10) 0.055(9) 0.026(7) O6 0.141(10) 0.120(9) 0.106(8) 0.041(7) 0.074(8) 0.063(8) O7 0.123(12) 0.110(11) 0.30(2) -0.073(13) 0.069(13) -0.055(9) O8 0.29(2) 0.138(13) 0.143(13) -0.028(11) 0.012(14) -0.127(16) O9 0.184(14) 0.240(18) 0.138(11) -0.116(12) 0.096(11) -0.140(14) S4 0.146(15) 0.106(12) 0.23(2) 0.081(15) 0.081(14) 0.024(11) C46 0.099(8) 0.080(8) 0.103(9) 0.036(7) 0.027(7) 0.026(7) O10 0.099(8) 0.080(8) 0.103(9) 0.036(7) 0.027(7) 0.026(7) O11 0.099(8) 0.080(8) 0.103(9) 0.036(7) 0.027(7) 0.026(7) O12 0.099(8) 0.080(8) 0.103(9) 0.036(7) 0.027(7) 0.026(7) S4A 0.072(4) 0.067(5) 0.091(5) 0.045(4) 0.064(4) 0.048(4) C46A 0.116(11) 0.124(12) 0.171(14) 0.076(11) 0.077(11) 0.065(10) O10A 0.116(11) 0.124(12) 0.171(14) 0.076(11) 0.077(11) 0.065(10) O11A 0.116(11) 0.124(12) 0.171(14) 0.076(11) 0.077(11) 0.065(10) O12A 0.116(11) 0.124(12) 0.171(14) 0.076(11) 0.077(11) 0.065(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 2.202(7) . ? Ag1 N7 2.213(7) 3_556 ? Ag1 O10A 2.399(15) . ? Ag1 O10 2.581(15) . ? Ag2 N5 2.242(7) . ? Ag2 N2 2.306(7) . ? Ag2 N9 2.338(9) . ? Ag2 O4 2.425(15) . ? Ag3 N4 2.254(8) 3_655 ? Ag3 N6 2.255(8) . ? Ag3 O5 2.416(12) . ? Ag3 O7 2.466(13) . ? Ag4 N3 2.250(8) 3_655 ? Ag4 N8 2.310(7) 3_556 ? Ag4 N11 2.341(10) 4_465 ? Ag4 O8 2.415(14) . ? S1 O3 1.394(13) . ? S1 O1 1.439(9) . ? S1 O2 1.471(14) . ? S1 C43 1.736(17) . ? S2 O4 1.395(14) . ? S2 O6 1.407(10) . ? S2 O5 1.500(14) . ? S2 C44 1.764(13) . ? S3 O7 1.371(17) . ? S3 O9 1.381(12) . ? S3 O8 1.442(18) . ? S3 C45 1.774(14) . ? N1 C1 1.278(12) . ? N1 N2 1.317(10) . ? N2 C4 1.352(11) . ? N3 C5 1.334(15) . ? N3 N4 1.337(12) . ? N3 Ag4 2.250(8) 3_655 ? N4 C8 1.317(11) . ? N4 Ag3 2.254(8) 3_655 ? N5 C15 1.329(12) . ? N5 N6 1.352(11) . ? N6 C18 1.319(11) . ? N7 C19 1.287(13) . ? N7 N8 1.333(11) . ? N7 Ag1 2.213(7) 3_556 ? N8 C22 1.325(11) . ? N8 Ag4 2.310(7) 3_556 ? N9 C29 1.287(15) . ? N9 N10 1.303(15) . ? N10 C32 1.413(17) . ? N11 N12 1.325(16) . ? N11 C33 1.348(17) . ? N11 Ag4 2.341(10) 4_666 ? N12 C36 1.384(19) . ? C1 C2 1.402(13) . ? C1 H1 0.9400 . ? C2 C3 1.353(14) . ? C2 H2 0.9400 . ? C3 C4 1.388(12) . ? C3 C9 1.455(12) . ? C4 H4 0.9400 . ? C5 C6 1.396(15) . ? C5 H5 0.9400 . ? C6 C7 1.368(16) . ? C6 H6 0.9400 . ? C7 C8 1.382(13) . ? C7 C12 1.487(12) . ? C8 H8 0.9400 . ? C9 C10 1.378(13) . ? C9 C14 1.390(13) . ? C10 C11 1.397(13) . ? C10 H10 0.9400 . ? C11 C12 1.360(13) . ? C11 H11 0.9400 . ? C12 C13 1.401(15) . ? C13 C14 1.345(13) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.370(13) . ? C15 H15 0.9400 . ? C16 C17 1.376(14) . ? C16 H16 0.9400 . ? C17 C18 1.391(13) . ? C17 C23 1.497(11) . ? C18 H18 0.9400 . ? C19 C20 1.407(13) . ? C19 H19 0.9400 . ? C20 C21 1.346(16) . ? C20 H20 0.9400 . ? C21 C22 1.410(13) . ? C21 C26 1.477(12) . ? C22 H22 0.9400 . ? C23 C24 1.364(13) . ? C23 C28 1.404(13) . ? C24 C25 1.386(13) . ? C24 H24 0.9400 . ? C25 C26 1.407(14) . ? C25 H25 0.9400 . ? C26 C27 1.391(13) . ? C27 C28 1.401(13) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? C29 C30 1.33(2) . ? C29 H29 0.9400 . ? C30 C31 1.390(19) . ? C30 H30 0.9400 . ? C31 C32 1.353(17) . ? C31 C37 1.486(16) . ? C32 H32 0.9400 . ? C33 C34 1.288(17) . ? C33 H33 0.9400 . ? C34 C35 1.413(17) . ? C34 H34 0.9400 . ? C35 C36 1.369(19) . ? C35 C40 1.492(16) . ? C36 H36 0.9400 . ? C37 C38 1.374(15) . ? C37 C42 1.393(17) . ? C38 C39 1.386(16) . ? C38 H38 0.9400 . ? C39 C40 1.398(17) . ? C39 H39 0.9400 . ? C40 C41 1.368(16) . ? C41 C42 1.373(17) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? S4 O10 1.433(9) . ? S4 O12 1.442(9) . ? S4 O11 1.456(10) . ? S4 C46 1.770(10) . ? S4A O10A 1.439(9) . ? S4A O11A 1.441(9) . ? S4A O12A 1.446(9) . ? S4A C46A 1.766(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 N1 Ag1 N7 166.8(3) . 3_556 ? N1 Ag1 O10A 84.1(5) . . ? N7 Ag1 O10A 104.6(5) 3_556 . ? N1 Ag1 O10 88.1(5) . . ? N7 Ag1 O10 95.0(5) 3_556 . ? O10A Ag1 O10 28.0(6) . . ? N5 Ag2 N2 129.4(3) . . ? N5 Ag2 N9 124.4(3) . . ? N2 Ag2 N9 98.1(3) . . ? N5 Ag2 O4 94.0(5) . . ? N2 Ag2 O4 100.7(4) . . ? N9 Ag2 O4 105.1(6) . . ? N4 Ag3 N6 147.0(3) 3_655 . ? N4 Ag3 O5 92.8(5) 3_655 . ? N6 Ag3 O5 108.7(5) . . ? N4 Ag3 O7 103.4(6) 3_655 . ? N6 Ag3 O7 98.4(5) . . ? O5 Ag3 O7 97.3(5) . . ? N3 Ag4 N8 129.3(3) 3_655 3_556 ? N3 Ag4 N11 127.4(4) 3_655 4_465 ? N8 Ag4 N11 99.1(4) 3_556 4_465 ? N3 Ag4 O8 93.8(7) 3_655 . ? N8 Ag4 O8 102.8(5) 3_556 . ? N11 Ag4 O8 94.1(7) 4_465 . ? O3 S1 O1 115.7(8) . . ? O3 S1 O2 108.3(9) . . ? O1 S1 O2 110.9(9) . . ? O3 S1 C43 109.9(11) . . ? O1 S1 C43 107.2(8) . . ? O2 S1 C43 104.2(12) . . ? O4 S2 O6 120.5(11) . . ? O4 S2 O5 107.7(11) . . ? O6 S2 O5 106.4(9) . . ? O4 S2 C44 104.3(11) . . ? O6 S2 C44 108.4(8) . . ? O5 S2 C44 109.2(12) . . ? O7 S3 O9 114.7(13) . . ? O7 S3 O8 103.8(13) . . ? O9 S3 O8 115.8(13) . . ? O7 S3 C45 104.8(11) . . ? O9 S3 C45 109.1(9) . . ? O8 S3 C45 107.9(11) . . ? C1 N1 N2 118.1(7) . . ? C1 N1 Ag1 125.3(6) . . ? N2 N1 Ag1 116.6(5) . . ? N1 N2 C4 120.2(7) . . ? N1 N2 Ag2 118.4(5) . . ? C4 N2 Ag2 121.0(6) . . ? C5 N3 N4 119.1(9) . . ? C5 N3 Ag4 120.2(8) . 3_655 ? N4 N3 Ag4 120.7(6) . 3_655 ? C8 N4 N3 119.8(8) . . ? C8 N4 Ag3 123.2(7) . 3_655 ? N3 N4 Ag3 116.4(6) . 3_655 ? C15 N5 N6 118.0(8) . . ? C15 N5 Ag2 119.7(7) . . ? N6 N5 Ag2 122.1(5) . . ? C18 N6 N5 120.4(8) . . ? C18 N6 Ag3 122.8(7) . . ? N5 N6 Ag3 116.7(5) . . ? C19 N7 N8 119.4(8) . . ? C19 N7 Ag1 123.4(7) . 3_556 ? N8 N7 Ag1 117.2(5) . 3_556 ? C22 N8 N7 119.9(8) . . ? C22 N8 Ag4 121.0(6) . 3_556 ? N7 N8 Ag4 118.8(5) . 3_556 ? C29 N9 N10 120.5(11) . . ? C29 N9 Ag2 115.7(8) . . ? N10 N9 Ag2 123.9(8) . . ? N9 N10 C32 120.2(12) . . ? N12 N11 C33 121.0(12) . . ? N12 N11 Ag4 122.7(11) . 4_666 ? C33 N11 Ag4 116.0(8) . 4_666 ? N11 N12 C36 119.6(15) . . ? N1 C1 C2 125.3(9) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C3 C2 C1 117.8(9) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 115.3(8) . . ? C2 C3 C9 123.0(8) . . ? C4 C3 C9 121.6(9) . . ? N2 C4 C3 123.2(9) . . ? N2 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? N3 C5 C6 121.6(12) . . ? N3 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 119.8(11) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 114.7(9) . . ? C6 C7 C12 122.8(9) . . ? C8 C7 C12 122.4(9) . . ? N4 C8 C7 125.0(10) . . ? N4 C8 H8 117.5 . . ? C7 C8 H8 117.5 . . ? C10 C9 C14 117.1(8) . . ? C10 C9 C3 120.4(8) . . ? C14 C9 C3 122.4(9) . . ? C9 C10 C11 120.9(9) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 120.9(9) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 118.1(8) . . ? C11 C12 C7 120.3(9) . . ? C13 C12 C7 121.5(8) . . ? C14 C13 C12 120.6(10) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 122.3(10) . . ? C13 C14 H14 118.8 . . ? C9 C14 H14 118.8 . . ? N5 C15 C16 123.5(10) . . ? N5 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 118.7(9) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C16 C17 C18 116.0(8) . . ? C16 C17 C23 121.7(8) . . ? C18 C17 C23 122.2(9) . . ? N6 C18 C17 123.2(10) . . ? N6 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? N7 C19 C20 123.5(11) . . ? N7 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C21 C20 C19 118.2(10) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C20 C21 C22 115.9(8) . . ? C20 C21 C26 123.8(9) . . ? C22 C21 C26 120.3(9) . . ? N8 C22 C21 123.0(9) . . ? N8 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C28 119.8(8) . . ? C24 C23 C17 121.1(9) . . ? C28 C23 C17 119.1(8) . . ? C23 C24 C25 120.8(10) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C26 119.8(9) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.9(8) . . ? C27 C26 C21 119.5(10) . . ? C25 C26 C21 120.3(9) . . ? C26 C27 C28 119.0(10) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C27 C28 C23 120.4(9) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? N9 C29 C30 118.1(13) . . ? N9 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? C29 C30 C31 126.6(15) . . ? C29 C30 H30 116.7 . . ? C31 C30 H30 116.7 . . ? C32 C31 C30 111.4(12) . . ? C32 C31 C37 125.4(10) . . ? C30 C31 C37 122.7(12) . . ? C31 C32 N10 121.2(11) . . ? C31 C32 H32 119.4 . . ? N10 C32 H32 119.4 . . ? C34 C33 N11 119.7(13) . . ? C34 C33 H33 120.2 . . ? N11 C33 H33 120.2 . . ? C33 C34 C35 124.0(15) . . ? C33 C34 H34 118.0 . . ? C35 C34 H34 118.0 . . ? C36 C35 C34 114.3(11) . . ? C36 C35 C40 124.4(11) . . ? C34 C35 C40 121.3(12) . . ? C35 C36 N12 121.2(13) . . ? C35 C36 H36 119.4 . . ? N12 C36 H36 119.4 . . ? C38 C37 C42 118.5(11) . . ? C38 C37 C31 120.6(11) . . ? C42 C37 C31 120.9(10) . . ? C37 C38 C39 121.4(12) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C40 120.4(11) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 117.0(11) . . ? C41 C40 C35 121.4(12) . . ? C39 C40 C35 121.5(11) . . ? C40 C41 C42 123.4(12) . . ? C40 C41 H41 118.3 . . ? C42 C41 H41 118.3 . . ? C41 C42 C37 119.3(11) . . ? C41 C42 H42 120.3 . . ? C37 C42 H42 120.3 . . ? S1 C43 H43A 109.5 . . ? S1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S2 C44 H44A 109.5 . . ? S2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? S3 C45 H45A 109.5 . . ? S3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S2 O4 Ag2 131.5(8) . . ? S2 O5 Ag3 124.7(8) . . ? S3 O7 Ag3 126.0(9) . . ? S3 O8 Ag4 129.9(9) . . ? O10 S4 O12 114.7(10) . . ? O10 S4 O11 112.1(10) . . ? O12 S4 O11 111.7(9) . . ? O10 S4 C46 108.7(17) . . ? O12 S4 C46 106(2) . . ? O11 S4 C46 102.6(18) . . ? S4 O10 Ag1 141.8(13) . . ? O10A S4A O11A 113.6(9) . . ? O10A S4A O12A 112.9(8) . . ? O11A S4A O12A 112.9(9) . . ? O10A S4A C46A 100.7(17) . . ? O11A S4A C46A 106(3) . . ? O12A S4A C46A 110(2) . . ? S4A O10A Ag1 139.7(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Ag1 N1 C1 124.0(13) 3_556 . . . ? O10A Ag1 N1 C1 -8.0(10) . . . . ? O10 Ag1 N1 C1 19.7(9) . . . . ? N7 Ag1 N1 N2 -58.8(15) 3_556 . . . ? O10A Ag1 N1 N2 169.2(9) . . . . ? O10 Ag1 N1 N2 -163.1(8) . . . . ? C1 N1 N2 C4 -2.2(13) . . . . ? Ag1 N1 N2 C4 -179.6(7) . . . . ? C1 N1 N2 Ag2 171.5(7) . . . . ? Ag1 N1 N2 Ag2 -5.9(8) . . . . ? N5 Ag2 N2 N1 30.0(8) . . . . ? N9 Ag2 N2 N1 -118.6(7) . . . . ? O4 Ag2 N2 N1 134.3(8) . . . . ? N5 Ag2 N2 C4 -156.4(7) . . . . ? N9 Ag2 N2 C4 55.0(8) . . . . ? O4 Ag2 N2 C4 -52.1(9) . . . . ? C5 N3 N4 C8 -1.9(17) . . . . ? Ag4 N3 N4 C8 178.4(7) 3_655 . . . ? C5 N3 N4 Ag3 -173.4(11) . . . 3_655 ? Ag4 N3 N4 Ag3 6.9(10) 3_655 . . 3_655 ? N2 Ag2 N5 C15 -136.8(7) . . . . ? N9 Ag2 N5 C15 4.6(10) . . . . ? O4 Ag2 N5 C15 115.9(8) . . . . ? N2 Ag2 N5 N6 48.1(8) . . . . ? N9 Ag2 N5 N6 -170.5(7) . . . . ? O4 Ag2 N5 N6 -59.2(7) . . . . ? C15 N5 N6 C18 3.3(13) . . . . ? Ag2 N5 N6 C18 178.4(7) . . . . ? C15 N5 N6 Ag3 178.9(7) . . . . ? Ag2 N5 N6 Ag3 -6.0(9) . . . . ? N4 Ag3 N6 C18 117.8(8) 3_655 . . . ? O5 Ag3 N6 C18 -114.1(8) . . . . ? O7 Ag3 N6 C18 -13.4(9) . . . . ? N4 Ag3 N6 N5 -57.7(9) 3_655 . . . ? O5 Ag3 N6 N5 70.4(7) . . . . ? O7 Ag3 N6 N5 171.1(7) . . . . ? C19 N7 N8 C22 2.5(13) . . . . ? Ag1 N7 N8 C22 -177.3(7) 3_556 . . . ? C19 N7 N8 Ag4 -171.4(7) . . . 3_556 ? Ag1 N7 N8 Ag4 8.8(8) 3_556 . . 3_556 ? N5 Ag2 N9 C29 173.9(13) . . . . ? N2 Ag2 N9 C29 -35.3(14) . . . . ? O4 Ag2 N9 C29 68.1(15) . . . . ? N5 Ag2 N9 N10 -5.3(14) . . . . ? N2 Ag2 N9 N10 145.6(12) . . . . ? O4 Ag2 N9 N10 -111.0(12) . . . . ? C29 N9 N10 C32 13(2) . . . . ? Ag2 N9 N10 C32 -167.7(10) . . . . ? C33 N11 N12 C36 2(3) . . . . ? Ag4 N11 N12 C36 175.7(13) 4_666 . . . ? N2 N1 C1 C2 2.2(16) . . . . ? Ag1 N1 C1 C2 179.3(8) . . . . ? N1 C1 C2 C3 -1.6(17) . . . . ? C1 C2 C3 C4 1.0(15) . . . . ? C1 C2 C3 C9 178.9(10) . . . . ? N1 N2 C4 C3 1.9(14) . . . . ? Ag2 N2 C4 C3 -171.7(7) . . . . ? C2 C3 C4 N2 -1.2(15) . . . . ? C9 C3 C4 N2 -179.1(9) . . . . ? N4 N3 C5 C6 -1(2) . . . . ? Ag4 N3 C5 C6 179.1(13) 3_655 . . . ? N3 C5 C6 C7 2(3) . . . . ? C5 C6 C7 C8 -1(2) . . . . ? C5 C6 C7 C12 177.5(13) . . . . ? N3 N4 C8 C7 3.2(15) . . . . ? Ag3 N4 C8 C7 174.0(8) 3_655 . . . ? C6 C7 C8 N4 -1.7(16) . . . . ? C12 C7 C8 N4 179.9(9) . . . . ? C2 C3 C9 C10 -150.9(10) . . . . ? C4 C3 C9 C10 26.8(14) . . . . ? C2 C3 C9 C14 24.7(16) . . . . ? C4 C3 C9 C14 -157.6(10) . . . . ? C14 C9 C10 C11 3.4(15) . . . . ? C3 C9 C10 C11 179.2(9) . . . . ? C9 C10 C11 C12 -1.9(16) . . . . ? C10 C11 C12 C13 -0.3(15) . . . . ? C10 C11 C12 C7 -179.3(9) . . . . ? C6 C7 C12 C11 -26.5(16) . . . . ? C8 C7 C12 C11 151.8(10) . . . . ? C6 C7 C12 C13 154.6(12) . . . . ? C8 C7 C12 C13 -27.1(15) . . . . ? C11 C12 C13 C14 1.0(17) . . . . ? C7 C12 C13 C14 179.9(11) . . . . ? C12 C13 C14 C9 0.6(19) . . . . ? C10 C9 C14 C13 -2.8(17) . . . . ? C3 C9 C14 C13 -178.5(11) . . . . ? N6 N5 C15 C16 -3.8(16) . . . . ? Ag2 N5 C15 C16 -179.0(9) . . . . ? N5 C15 C16 C17 3.5(18) . . . . ? C15 C16 C17 C18 -2.6(15) . . . . ? C15 C16 C17 C23 179.7(10) . . . . ? N5 N6 C18 C17 -2.8(14) . . . . ? Ag3 N6 C18 C17 -178.1(7) . . . . ? C16 C17 C18 N6 2.4(15) . . . . ? C23 C17 C18 N6 -179.9(9) . . . . ? N8 N7 C19 C20 -3.5(15) . . . . ? Ag1 N7 C19 C20 176.2(8) 3_556 . . . ? N7 C19 C20 C21 1.8(16) . . . . ? C19 C20 C21 C22 0.8(15) . . . . ? C19 C20 C21 C26 -178.2(9) . . . . ? N7 N8 C22 C21 0.2(15) . . . . ? Ag4 N8 C22 C21 173.9(7) 3_556 . . . ? C20 C21 C22 N8 -1.7(15) . . . . ? C26 C21 C22 N8 177.3(9) . . . . ? C16 C17 C23 C24 28.2(14) . . . . ? C18 C17 C23 C24 -149.4(10) . . . . ? C16 C17 C23 C28 -152.4(10) . . . . ? C18 C17 C23 C28 30.0(14) . . . . ? C28 C23 C24 C25 0.9(15) . . . . ? C17 C23 C24 C25 -179.8(9) . . . . ? C23 C24 C25 C26 2.5(15) . . . . ? C24 C25 C26 C27 -4.9(15) . . . . ? C24 C25 C26 C21 -178.6(9) . . . . ? C20 C21 C26 C27 -23.8(15) . . . . ? C22 C21 C26 C27 157.2(10) . . . . ? C20 C21 C26 C25 149.8(11) . . . . ? C22 C21 C26 C25 -29.1(14) . . . . ? C25 C26 C27 C28 3.8(15) . . . . ? C21 C26 C27 C28 177.6(9) . . . . ? C26 C27 C28 C23 -0.5(16) . . . . ? C24 C23 C28 C27 -1.9(15) . . . . ? C17 C23 C28 C27 178.7(9) . . . . ? N10 N9 C29 C30 -17(3) . . . . ? Ag2 N9 C29 C30 163.6(18) . . . . ? N9 C29 C30 C31 9(4) . . . . ? C29 C30 C31 C32 3(3) . . . . ? C29 C30 C31 C37 175(2) . . . . ? C30 C31 C32 N10 -7(2) . . . . ? C37 C31 C32 N10 -178.6(12) . . . . ? N9 N10 C32 C31 0(2) . . . . ? N12 N11 C33 C34 -5(3) . . . . ? Ag4 N11 C33 C34 -179.2(14) 4_666 . . . ? N11 C33 C34 C35 4(3) . . . . ? C33 C34 C35 C36 0(2) . . . . ? C33 C34 C35 C40 179.6(16) . . . . ? C34 C35 C36 N12 -3(2) . . . . ? C40 C35 C36 N12 177.3(15) . . . . ? N11 N12 C36 C35 2(3) . . . . ? C32 C31 C37 C38 16.9(19) . . . . ? C30 C31 C37 C38 -154.1(18) . . . . ? C32 C31 C37 C42 -164.4(14) . . . . ? C30 C31 C37 C42 25(2) . . . . ? C42 C37 C38 C39 0.6(19) . . . . ? C31 C37 C38 C39 179.3(11) . . . . ? C37 C38 C39 C40 0.4(18) . . . . ? C38 C39 C40 C41 -0.1(18) . . . . ? C38 C39 C40 C35 -177.3(11) . . . . ? C36 C35 C40 C41 16.1(19) . . . . ? C34 C35 C40 C41 -163.3(14) . . . . ? C36 C35 C40 C39 -166.9(13) . . . . ? C34 C35 C40 C39 13.6(18) . . . . ? C39 C40 C41 C42 -1(2) . . . . ? C35 C40 C41 C42 175.9(13) . . . . ? C40 C41 C42 C37 2(2) . . . . ? C38 C37 C42 C41 -2(2) . . . . ? C31 C37 C42 C41 179.5(12) . . . . ? O6 S2 O4 Ag2 52.0(19) . . . . ? O5 S2 O4 Ag2 -70.2(18) . . . . ? C44 S2 O4 Ag2 173.8(15) . . . . ? N5 Ag2 O4 S2 107.0(17) . . . . ? N2 Ag2 O4 S2 -24.3(18) . . . . ? N9 Ag2 O4 S2 -125.8(16) . . . . ? O4 S2 O5 Ag3 38.1(13) . . . . ? O6 S2 O5 Ag3 -92.4(11) . . . . ? C44 S2 O5 Ag3 150.7(11) . . . . ? N4 Ag3 O5 S2 90.9(11) 3_655 . . . ? N6 Ag3 O5 S2 -63.7(12) . . . . ? O7 Ag3 O5 S2 -165.2(12) . . . . ? O9 S3 O7 Ag3 -77.0(18) . . . . ? O8 S3 O7 Ag3 50.3(16) . . . . ? C45 S3 O7 Ag3 163.4(13) . . . . ? N4 Ag3 O7 S3 -77.7(16) 3_655 . . . ? N6 Ag3 O7 S3 77.4(16) . . . . ? O5 Ag3 O7 S3 -172.4(15) . . . . ? O7 S3 O8 Ag4 -73.2(19) . . . . ? O9 S3 O8 Ag4 53(2) . . . . ? C45 S3 O8 Ag4 176.0(16) . . . . ? N3 Ag4 O8 S3 105.3(19) 3_655 . . . ? N8 Ag4 O8 S3 -26(2) 3_556 . . . ? N11 Ag4 O8 S3 -126.7(19) 4_465 . . . ? O12 S4 O10 Ag1 80(2) . . . . ? O11 S4 O10 Ag1 -151.1(16) . . . . ? C46 S4 O10 Ag1 -38(3) . . . . ? N1 Ag1 O10 S4 -124.4(18) . . . . ? N7 Ag1 O10 S4 68.4(18) 3_556 . . . ? O11A S4A O10A Ag1 -62(3) . . . . ? O12A S4A O10A Ag1 167(2) . . . . ? C46A S4A O10A Ag1 50(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.982 _refine_diff_density_min -1.874 _refine_diff_density_rms 0.144 #----------------------------------------------------# data_(7) _database_code_depnum_ccdc_archive 'CCDC 685688' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Benzoate 2:1 complex with 1,4-bi(pyridazin-4-yl)benzene, Hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag2 N4 O6' _chemical_formula_weight 728.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.2863(3) _cell_length_b 14.3867(6) _cell_length_c 12.2774(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.945(3) _cell_angle_gamma 90.00 _cell_volume 1286.81(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8074 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 26.54 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.574 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5249 _exptl_absorpt_correction_T_max 0.8584 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 8074 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.54 _reflns_number_total 2634 _reflns_number_gt 2079 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms were located from difference maps and then refined a riding, with C---H distances constrained to 0.93 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atom). For solvate water molecule, the oxygen atom was disoredred over two closely separated positions with partial occupancies 0.7 and 0.3, and with common positions of hydrogen atoms for two components. These hydrogen atoms were located from the map and then their positions were fixed, with U~iso~(H) = 1.5U~eq~ of the parent oxygen atom (which was a predominant 0.7 component of the disorder). The bipyridazine ligand lies across an inversion centre. ; _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^)+(0.0291P)^2^+0.0077P] 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 2634 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.21935(4) 0.047736(19) 0.529325(18) 0.04612(12) Uani 1 1 d . . . O1 O 0.4686(3) 0.13728(16) 0.6522(2) 0.0543(6) Uani 1 1 d . . . O2 O 0.5021(3) 0.11499(16) 0.47559(19) 0.0585(7) Uani 1 1 d . . . N1 N 0.0361(3) 0.02061(16) 0.67188(18) 0.0286(5) Uani 1 1 d . . . N2 N -0.1337(3) -0.01318(16) 0.65023(17) 0.0284(5) Uani 1 1 d . . . C1 C -0.2563(4) -0.01654(19) 0.7283(2) 0.0263(6) Uani 1 1 d . . . H1 H -0.3726 -0.0394 0.7109 0.032 Uiso 1 1 calc R . . C2 C -0.2216(4) 0.01236(18) 0.8361(2) 0.0236(6) Uani 1 1 d . . . C3 C -0.0487(4) 0.04644(19) 0.8565(2) 0.0304(7) Uani 1 1 d . . . H3 H -0.0150 0.0670 0.9258 0.036 Uiso 1 1 calc R . . C4 C 0.0751(4) 0.04984(19) 0.7720(2) 0.0318(7) Uani 1 1 d . . . H4 H 0.1915 0.0739 0.7864 0.038 Uiso 1 1 calc R . . C5 C -0.3655(4) 0.00621(19) 0.9196(2) 0.0245(6) Uani 1 1 d . . . C6 C -0.5032(4) -0.06046(19) 0.9128(2) 0.0316(7) Uani 1 1 d . . . H6 H -0.5060 -0.1016 0.8544 0.038 Uiso 1 1 calc R . . C7 C -0.3637(4) 0.0666(2) 1.0085(2) 0.0319(7) Uani 1 1 d . . . H7 H -0.2722 0.1114 1.0149 0.038 Uiso 1 1 calc R . . C8 C 0.5563(4) 0.1457(2) 0.5669(3) 0.0370(7) Uani 1 1 d . . . C9 C 0.7408(4) 0.19201(19) 0.5704(2) 0.0287(7) Uani 1 1 d . . . C10 C 0.8505(5) 0.1926(2) 0.4796(2) 0.0367(7) Uani 1 1 d . . . H10 H 0.8077 0.1658 0.4151 0.044 Uiso 1 1 calc R . . C11 C 1.0240(5) 0.2327(2) 0.4834(3) 0.0412(8) Uani 1 1 d . . . H11 H 1.0975 0.2323 0.4222 0.049 Uiso 1 1 calc R . . C12 C 1.0860(5) 0.2734(2) 0.5791(3) 0.0433(8) Uani 1 1 d . . . H12 H 1.2024 0.2999 0.5826 0.052 Uiso 1 1 calc R . . C13 C 0.9773(5) 0.2747(2) 0.6686(3) 0.0428(8) Uani 1 1 d . . . H13 H 1.0194 0.3030 0.7324 0.051 Uiso 1 1 calc R . . C14 C 0.8053(4) 0.2344(2) 0.6652(2) 0.0343(7) Uani 1 1 d . . . H14 H 0.7324 0.2356 0.7267 0.041 Uiso 1 1 calc R . . O3 O 0.3689(8) 0.2241(4) 0.3013(4) 0.0648(15) Uani 0.70 1 d P . . H1W H 0.4456 0.2155 0.3636 0.097 Uiso 1 1 d . . . H2W H 0.4348 0.2627 0.2594 0.097 Uiso 1 1 d . . . O3A O 0.3741(18) 0.2762(9) 0.3349(11) 0.070(4) Uani 0.30 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 0.03875(17) 0.0715(2) 0.02850(14) -0.00850(11) 0.01234(10) -0.02338(13) O1 0.0327(14) 0.0602(16) 0.0704(16) -0.0074(13) 0.0190(13) -0.0102(12) O2 0.0499(16) 0.0649(17) 0.0603(15) -0.0025(12) -0.0121(13) -0.0234(14) N1 0.0237(13) 0.0358(14) 0.0265(12) -0.0004(10) 0.0070(10) -0.0031(11) N2 0.0258(13) 0.0344(14) 0.0253(12) -0.0020(10) 0.0063(10) -0.0068(11) C1 0.0222(15) 0.0310(16) 0.0259(14) -0.0005(11) 0.0053(12) -0.0019(13) C2 0.0260(16) 0.0246(14) 0.0205(13) 0.0009(11) 0.0091(11) 0.0018(12) C3 0.0324(17) 0.0366(17) 0.0223(13) -0.0032(12) 0.0039(12) -0.0041(14) C4 0.0252(16) 0.0404(18) 0.0299(15) -0.0027(13) 0.0051(12) -0.0071(14) C5 0.0240(15) 0.0255(15) 0.0242(13) 0.0006(11) 0.0067(11) -0.0016(12) C6 0.0357(18) 0.0332(17) 0.0262(14) -0.0088(12) 0.0130(13) -0.0051(14) C7 0.0301(17) 0.0337(17) 0.0322(15) -0.0060(12) 0.0089(13) -0.0108(14) C8 0.0292(18) 0.0276(16) 0.054(2) 0.0013(15) -0.0046(16) 0.0009(14) C9 0.0260(17) 0.0263(16) 0.0339(15) -0.0001(12) 0.0005(13) 0.0012(13) C10 0.0407(19) 0.0346(18) 0.0349(16) 0.0027(13) 0.0001(14) 0.0002(15) C11 0.035(2) 0.043(2) 0.0461(19) 0.0081(15) 0.0142(16) 0.0033(16) C12 0.0274(18) 0.039(2) 0.063(2) 0.0093(16) 0.0015(17) -0.0084(15) C13 0.042(2) 0.043(2) 0.0428(18) -0.0012(15) -0.0096(16) -0.0066(16) C14 0.0332(18) 0.0366(18) 0.0332(15) -0.0002(13) 0.0021(13) -0.0011(15) O3 0.049(3) 0.085(4) 0.060(3) 0.025(3) -0.003(2) -0.022(3) O3A 0.040(7) 0.082(9) 0.088(9) 0.027(7) 0.023(6) 0.020(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 N1 2.253(2) . ? Ag1 N2 2.335(2) 3_556 ? Ag1 O2 2.379(2) . ? Ag1 O1 2.673(2) . ? O1 C8 1.242(4) . ? O2 C8 1.262(4) . ? N1 C4 1.326(4) . ? N1 N2 1.352(3) . ? N2 C1 1.322(3) . ? C1 C2 1.407(4) . ? C1 H1 0.9300 . ? C2 C3 1.371(4) . ? C2 C5 1.481(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 C7 1.395(4) . ? C6 C7 1.382(4) 3_457 ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.501(4) . ? C9 C10 1.383(4) . ? C9 C14 1.389(4) . ? C10 C11 1.389(5) . ? C10 H10 0.9300 . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.366(4) . ? C12 H12 0.9300 . ? C13 C14 1.381(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O3 H1W 0.9476 . ? O3 H2W 0.9007 . ? O3A H1W 1.0728 . ? O3A H2W 1.0513 . ? 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 N2 122.96(8) . 3_556 ? N1 Ag1 O2 144.38(8) . . ? N2 Ag1 O2 92.52(8) 3_556 . ? N1 Ag1 O1 92.92(8) . . ? N2 Ag1 O1 143.53(8) 3_556 . ? O2 Ag1 O1 51.47(7) . . ? C8 O1 Ag1 85.70(19) . . ? C8 O2 Ag1 98.9(2) . . ? C4 N1 N2 118.5(2) . . ? C4 N1 Ag1 123.0(2) . . ? N2 N1 Ag1 117.51(16) . . ? C1 N2 N1 119.9(2) . . ? C1 N2 Ag1 120.24(18) . 3_556 ? N1 N2 Ag1 119.46(16) . 3_556 ? N2 C1 C2 123.9(3) . . ? N2 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 115.3(3) . . ? C3 C2 C5 123.7(2) . . ? C1 C2 C5 121.0(3) . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? N1 C4 C3 123.4(3) . . ? N1 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? C6 C5 C7 118.3(3) . . ? C6 C5 C2 121.2(2) . . ? C7 C5 C2 120.4(3) . . ? C7 C6 C5 121.1(3) 3_457 . ? C7 C6 H6 119.5 3_457 . ? C5 C6 H6 119.5 . . ? C6 C7 C5 120.6(3) 3_457 . ? C6 C7 H7 119.7 3_457 . ? C5 C7 H7 119.7 . . ? O1 C8 O2 123.9(3) . . ? O1 C8 C9 119.5(3) . . ? O2 C8 C9 116.6(3) . . ? C10 C9 C14 118.7(3) . . ? C10 C9 C8 120.6(3) . . ? C14 C9 C8 120.7(3) . . ? C9 C10 C11 120.9(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.3(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C9 120.3(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? H1W O3 H2W 103.3 . . ? H1W O3A H2W 86.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 O1 C8 178.99(19) . . . . ? N2 Ag1 O1 C8 -10.8(3) 3_556 . . . ? O2 Ag1 O1 C8 -0.16(18) . . . . ? N1 Ag1 O2 C8 -1.3(3) . . . . ? N2 Ag1 O2 C8 173.8(2) 3_556 . . . ? O1 Ag1 O2 C8 0.15(18) . . . . ? N2 Ag1 N1 C4 -171.9(2) 3_556 . . . ? O2 Ag1 N1 C4 2.3(3) . . . . ? O1 Ag1 N1 C4 1.1(2) . . . . ? N2 Ag1 N1 N2 -3.1(3) 3_556 . . . ? O2 Ag1 N1 N2 171.07(17) . . . . ? O1 Ag1 N1 N2 169.9(2) . . . . ? C4 N1 N2 C1 -0.1(4) . . . . ? Ag1 N1 N2 C1 -169.36(19) . . . . ? C4 N1 N2 Ag1 172.34(19) . . . 3_556 ? Ag1 N1 N2 Ag1 3.0(3) . . . 3_556 ? N1 N2 C1 C2 -0.8(4) . . . . ? Ag1 N2 C1 C2 -173.1(2) 3_556 . . . ? N2 C1 C2 C3 0.8(4) . . . . ? N2 C1 C2 C5 -179.7(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C5 C2 C3 C4 -179.4(3) . . . . ? N2 N1 C4 C3 0.9(4) . . . . ? Ag1 N1 C4 C3 169.6(2) . . . . ? C2 C3 C4 N1 -0.9(4) . . . . ? C3 C2 C5 C6 -152.4(3) . . . . ? C1 C2 C5 C6 28.1(4) . . . . ? C3 C2 C5 C7 26.4(4) . . . . ? C1 C2 C5 C7 -153.1(3) . . . . ? C7 C5 C6 C7 0.5(5) . . . 3_457 ? C2 C5 C6 C7 179.3(3) . . . 3_457 ? C6 C5 C7 C6 -0.5(5) . . . 3_457 ? C2 C5 C7 C6 -179.3(3) . . . 3_457 ? Ag1 O1 C8 O2 0.3(3) . . . . ? Ag1 O1 C8 C9 -177.7(3) . . . . ? Ag1 O2 C8 O1 -0.3(4) . . . . ? Ag1 O2 C8 C9 177.7(2) . . . . ? O1 C8 C9 C10 172.4(3) . . . . ? O2 C8 C9 C10 -5.7(4) . . . . ? O1 C8 C9 C14 -7.0(4) . . . . ? O2 C8 C9 C14 174.9(3) . . . . ? C14 C9 C10 C11 1.5(4) . . . . ? C8 C9 C10 C11 -177.9(3) . . . . ? C9 C10 C11 C12 -0.7(5) . . . . ? C10 C11 C12 C13 -0.6(5) . . . . ? C11 C12 C13 C14 1.0(5) . . . . ? C12 C13 C14 C9 -0.1(5) . . . . ? C10 C9 C14 C13 -1.1(4) . . . . ? C8 C9 C14 C13 178.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.319 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.082 #----------------------------------------------------# data_(8) _database_code_depnum_ccdc_archive 'CCDC 685689' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Isophthalate 1:1 complex with 1,4-bi(pyridazin-4-yl)benzene, Hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H62 Ag6 N12 O22' _chemical_formula_weight 2022.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4238(6) _cell_length_b 14.2038(12) _cell_length_c 14.2032(10) _cell_angle_alpha 104.457(8) _cell_angle_beta 98.140(8) _cell_angle_gamma 108.924(9) _cell_volume 1689.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.86 _cell_measurement_theta_max 27.09 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.794 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6327 _exptl_absorpt_correction_T_max 0.6904 _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 11283 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.09 _reflns_number_total 7302 _reflns_number_gt 4313 _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)' #------------------------------- Refinement data-----------------------# _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 was solved by direct methods. All H atoms for the pyridazine ligand, coordinated isophthalate anion and three coordinated water molecules were located from difference maps and then refined as riding (for water molecules the hydrogen atoms were fixed), with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atom) and U~iso~(H) = 1.5U~eq~ (parent oxygen atoms). The non-coordinated isophthalate anion was disordered by the symmetry, and in such a manner that carbon-2 atom of the carbocycle occupies a center of inversion and it is common for both the disorder components. The carboxyl groups from both components were overlapped with very short interatomic separations and therefore some minor restraints were applied in order to improve the refinement stability. In particular, planarity of both C-CO~2~ fragments was imposed with FLAT restraints and with distance C---C fixed at 1.480(5) \%A. For carboxylic atoms of two disorder components the corresponding C---C distance was about 0.16 \%A and therefore EADP restraint was applied to thermal parameters of these two atoms. However, it was possible to refine all disordered atoms anisotropically, and the hydrogen atoms were added geometrically, with partial contribution factors 0.5. Two unique solvate water molecules are hydrogen bonded to the disordered isophthalate anion and therefore they are also disordered over two equal positions (0.5/0.5), depending on the orientation of the isophthalate. Both contributions were refined isotropically, and hydrogen atoms were not added to these water molecules. One of two unique bipyridazine molecules lies across an inversion centre. ; _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^)+(0.0815P)^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 7302 _refine_ls_number_parameters 541 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.65919(4) 0.14847(3) 0.42149(3) 0.04546(15) Uani 1 1 d . . . Ag2 Ag 0.20079(5) -0.43376(3) -0.44344(3) 0.04857(15) Uani 1 1 d . . . Ag3 Ag 0.42076(5) 0.14904(4) 0.57667(3) 0.06078(18) Uani 1 1 d . . . N1 N 0.6726(5) 0.2628(3) 0.6477(3) 0.0347(9) Uani 1 1 d . . . N2 N 0.7677(5) 0.2650(3) 0.5850(3) 0.0341(9) Uani 1 1 d . . . N3 N 0.3220(5) 0.0209(3) 0.4287(2) 0.0315(9) Uani 1 1 d . . . N4 N 0.4128(4) 0.0241(3) 0.3634(3) 0.0322(9) Uani 1 1 d . . . N5 N 0.0237(5) -0.4064(3) -0.3510(3) 0.0380(10) Uani 1 1 d . . . N6 N -0.1315(5) -0.4651(3) -0.3948(3) 0.0342(9) Uani 1 1 d . . . C1 C 0.7299(6) 0.3189(4) 0.7439(3) 0.0356(11) Uani 1 1 d . . . H1 H 0.6603 0.3170 0.7854 0.043 Uiso 1 1 calc R . . C2 C 0.8882(6) 0.3814(3) 0.7888(3) 0.0312(10) Uani 1 1 d . . . C3 C 0.9846(6) 0.3811(4) 0.7241(3) 0.0360(11) Uani 1 1 d . . . H3 H 1.0917 0.4196 0.7476 0.043 Uiso 1 1 calc R . . C4 C 0.9198(6) 0.3226(4) 0.6233(3) 0.0365(11) Uani 1 1 d . . . H4 H 0.9859 0.3234 0.5796 0.044 Uiso 1 1 calc R . . C5 C 0.8471(7) 0.4705(5) 0.9520(4) 0.0512(15) Uani 1 1 d . . . H5 H 0.7424 0.4506 0.9205 0.061 Uiso 1 1 calc R . . C6 C 0.9449(6) 0.4418(3) 0.8972(3) 0.0307(10) Uani 1 1 d . . . C7 C 1.0986(7) 0.4721(5) 0.9476(4) 0.0504(15) Uani 1 1 d . . . H7 H 1.1671 0.4528 0.9121 0.060 Uiso 1 1 calc R . . C8 C 0.3532(5) -0.0334(3) 0.2686(3) 0.0299(10) Uani 1 1 d . . . H8 H 0.4188 -0.0290 0.2244 0.036 Uiso 1 1 calc R . . C9 C 0.1944(6) -0.1023(3) 0.2287(3) 0.0311(10) Uani 1 1 d . . . C10 C 0.1042(6) -0.1042(4) 0.2952(3) 0.0349(11) Uani 1 1 d . . . H10 H -0.0015 -0.1471 0.2746 0.042 Uiso 1 1 calc R . . C11 C 0.1720(6) -0.0407(4) 0.3955(3) 0.0370(12) Uani 1 1 d . . . H11 H 0.1090 -0.0417 0.4413 0.044 Uiso 1 1 calc R . . C12 C 0.1355(5) -0.1636(3) 0.1202(3) 0.0302(10) Uani 1 1 d . . . C13 C 0.2360(6) -0.1890(5) 0.0642(4) 0.0475(14) Uani 1 1 d . . . H13 H 0.3416 -0.1667 0.0948 0.057 Uiso 1 1 calc R . . C14 C 0.1798(6) -0.2470(5) -0.0361(4) 0.0471(14) Uani 1 1 d . . . H14 H 0.2481 -0.2649 -0.0726 0.056 Uiso 1 1 calc R . . C15 C 0.0237(6) -0.2800(3) -0.0851(3) 0.0297(10) Uani 1 1 d . . . C16 C -0.0754(6) -0.2561(4) -0.0290(4) 0.0437(13) Uani 1 1 d . . . H16 H -0.1808 -0.2782 -0.0599 0.052 Uiso 1 1 calc R . . C17 C -0.0213(6) -0.1996(4) 0.0725(4) 0.0442(14) Uani 1 1 d . . . H17 H -0.0911 -0.1854 0.1096 0.053 Uiso 1 1 calc R . . C18 C 0.0655(5) -0.3484(4) -0.2565(3) 0.0347(11) Uani 1 1 d . . . H18 H 0.1713 -0.3078 -0.2288 0.042 Uiso 1 1 calc R . . C19 C -0.0354(5) -0.3425(3) -0.1936(3) 0.0293(10) Uani 1 1 d . . . C20 C -0.1920(6) -0.4013(4) -0.2400(3) 0.0359(11) Uani 1 1 d . . . H20 H -0.2679 -0.4019 -0.2036 0.043 Uiso 1 1 calc R . . C21 C -0.2332(6) -0.4592(4) -0.3417(3) 0.0410(12) Uani 1 1 d . . . H21 H -0.3388 -0.4957 -0.3735 0.049 Uiso 1 1 calc R . . C22 C 0.8980(6) 0.1254(4) 0.3246(4) 0.0392(12) Uani 1 1 d . . . C23 C 1.4747(6) 0.2858(4) 0.3743(4) 0.0450(13) Uani 1 1 d . . . C24 C 1.0343(5) 0.1353(3) 0.2819(3) 0.0317(10) Uani 1 1 d . . . C25 C 1.1844(6) 0.2022(4) 0.3417(3) 0.0351(11) Uani 1 1 d . . . H25 H 1.1953 0.2411 0.4082 0.042 Uiso 1 1 calc R . . C26 C 1.3149(6) 0.2122(4) 0.3054(3) 0.0347(11) Uani 1 1 d . . . C27 C 1.2984(6) 0.1564(4) 0.2064(4) 0.0393(11) Uani 1 1 d . . . H27 H 1.3862 0.1627 0.1805 0.047 Uiso 1 1 calc R . . C28 C 1.1496(7) 0.0902(4) 0.1445(3) 0.0401(12) Uani 1 1 d . . . H28 H 1.1395 0.0523 0.0778 0.048 Uiso 1 1 calc R . . C29 C 1.0199(6) 0.0807(4) 0.1812(3) 0.0379(12) Uani 1 1 d . . . H29 H 0.9216 0.0378 0.1390 0.045 Uiso 1 1 calc R . . O1 O 0.9232(5) 0.1645(3) 0.4186(3) 0.0575(12) Uani 1 1 d . . . O2 O 0.7627(4) 0.0793(3) 0.2672(3) 0.0529(10) Uani 1 1 d . . . O3 O 1.4830(5) 0.3370(4) 0.4601(3) 0.0737(15) Uani 1 1 d . . . O4 O 1.5893(4) 0.2890(3) 0.3372(3) 0.0522(10) Uani 1 1 d . . . O5 O 0.1683(5) 0.1668(3) 0.5756(3) 0.0476(9) Uani 1 1 d . . . H1W H 0.0980 0.1703 0.5324 0.071 Uiso 1 1 d . . . H2W H 0.2051 0.2257 0.6230 0.071 Uiso 1 1 d . . . O6 O 0.4013(5) 0.1274(3) 0.7391(3) 0.0504(10) Uani 1 1 d . . . H3W H 0.3868 0.1765 0.7806 0.076 Uiso 1 1 d . . . H4W H 0.3451 0.0685 0.7443 0.076 Uiso 1 1 d . . . O7 O 0.3067(8) -0.5761(4) -0.4139(3) 0.0843(18) Uani 1 1 d . . . H5W H 0.3608 -0.6016 -0.4494 0.126 Uiso 1 1 d . . . H6W H 0.3441 -0.5691 -0.3531 0.126 Uiso 1 1 d . . . C30 C 0.5000 0.5000 1.0000 0.0368(16) Uani 1 2 d S . . H30 H 0.5009 0.4436 1.0260 0.044 Uiso 0.50 1 d P . . C31 C 0.5550(11) 0.6039(8) 1.0609(6) 0.034(2) Uani 0.50 1 d PD . . C32 C 0.5586(12) 0.6845(8) 1.0240(8) 0.039(2) Uani 0.50 1 d P . . H32 H 0.5998 0.7555 1.0698 0.047 Uiso 0.50 1 d P . . C33 C 0.5012(12) 0.6641(9) 0.9228(7) 0.044(3) Uani 0.50 1 d P . . H33 H 0.5030 0.7237 0.8979 0.053 Uiso 0.50 1 d P . . C34 C 0.4418(12) 0.5626(8) 0.8544(7) 0.035(2) Uani 0.50 1 d P . . H34 H 0.4031 0.5484 0.7836 0.042 Uiso 0.50 1 d P . . C35 C 0.4383(11) 0.4793(8) 0.8909(7) 0.037(2) Uani 0.50 1 d PD . . C36 C 0.6201(11) 0.6271(13) 1.1692(7) 0.0406(15) Uani 0.50 1 d PD . . C37 C 0.3704(10) 0.3710(10) 0.8199(9) 0.0406(15) Uani 0.50 1 d PD . . O8 O 0.5730(13) 0.5499(6) 1.2061(5) 0.065(3) Uani 0.50 1 d PD . . O9 O 0.7158(10) 0.7167(6) 1.2225(6) 0.051(2) Uani 0.50 1 d PD . . O10 O 0.3891(14) 0.2976(6) 0.8554(6) 0.066(3) Uani 0.50 1 d PD . . O11 O 0.3007(13) 0.3493(8) 0.7333(6) 0.071(3) Uani 0.50 1 d PD . . O12 O 0.4174(12) 0.1985(8) 0.9962(6) 0.067(3) Uani 0.50 1 d P . . O13 O 0.6008(12) 0.3589(7) 1.1758(6) 0.062(2) Uani 0.50 1 d P . . O14 O 0.3792(14) 0.0575(9) 0.9536(8) 0.076(3) Uani 0.50 1 d P . . O15 O 0.5733(16) 0.0028(10) 1.0777(9) 0.093(4) 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 0.02716(19) 0.0513(3) 0.03602(19) -0.00604(16) 0.00552(14) 0.00275(17) Ag2 0.0384(2) 0.0542(3) 0.02929(18) -0.00373(16) 0.00425(15) 0.00154(18) Ag3 0.0334(2) 0.0837(4) 0.0325(2) -0.0142(2) 0.00327(15) 0.0068(2) N1 0.030(2) 0.035(2) 0.0294(17) 0.0040(16) 0.0035(15) 0.0060(17) N2 0.033(2) 0.035(2) 0.0288(17) 0.0027(16) 0.0064(15) 0.0120(18) N3 0.032(2) 0.033(2) 0.0250(16) 0.0032(14) 0.0068(14) 0.0106(17) N4 0.0286(19) 0.0287(19) 0.0302(17) 0.0037(15) 0.0047(15) 0.0044(16) N5 0.029(2) 0.040(2) 0.0303(17) 0.0060(16) 0.0043(15) -0.0003(18) N6 0.0251(19) 0.037(2) 0.0298(17) 0.0047(16) 0.0007(14) 0.0042(17) C1 0.036(3) 0.031(2) 0.032(2) 0.0044(18) 0.0049(18) 0.009(2) C2 0.039(3) 0.022(2) 0.0255(18) 0.0026(16) 0.0030(17) 0.0073(19) C3 0.036(3) 0.031(2) 0.033(2) 0.0036(19) 0.0031(19) 0.010(2) C4 0.035(3) 0.033(2) 0.033(2) 0.0022(19) 0.0074(19) 0.008(2) C5 0.039(3) 0.061(3) 0.035(2) -0.006(2) -0.001(2) 0.015(3) C6 0.036(2) 0.021(2) 0.0280(19) 0.0034(16) 0.0062(17) 0.0066(18) C7 0.041(3) 0.065(4) 0.034(2) -0.003(2) 0.007(2) 0.019(3) C8 0.028(2) 0.028(2) 0.0300(19) 0.0057(17) 0.0074(17) 0.0075(18) C9 0.035(2) 0.022(2) 0.0294(19) 0.0037(17) 0.0038(17) 0.0058(19) C10 0.034(2) 0.028(2) 0.033(2) 0.0033(18) 0.0067(18) 0.005(2) C11 0.036(3) 0.031(2) 0.032(2) 0.0034(18) 0.0097(19) 0.003(2) C12 0.031(2) 0.025(2) 0.0268(19) 0.0033(16) 0.0055(17) 0.0051(18) C13 0.034(3) 0.056(3) 0.037(2) 0.000(2) 0.005(2) 0.009(2) C14 0.034(3) 0.060(3) 0.035(2) -0.002(2) 0.007(2) 0.015(3) C15 0.036(2) 0.020(2) 0.0268(19) 0.0039(16) 0.0047(17) 0.0065(18) C16 0.029(2) 0.050(3) 0.035(2) -0.001(2) 0.0033(19) 0.006(2) C17 0.031(2) 0.053(3) 0.036(2) -0.003(2) 0.0087(19) 0.012(2) C18 0.026(2) 0.032(2) 0.032(2) 0.0010(18) 0.0036(17) 0.0001(19) C19 0.033(2) 0.022(2) 0.0272(18) 0.0060(16) 0.0036(16) 0.0066(18) C20 0.033(2) 0.038(3) 0.029(2) 0.0050(19) 0.0062(18) 0.009(2) C21 0.030(2) 0.044(3) 0.035(2) 0.004(2) -0.0004(19) 0.006(2) C22 0.034(3) 0.032(2) 0.052(3) 0.017(2) 0.013(2) 0.009(2) C23 0.024(2) 0.045(3) 0.059(3) 0.019(3) 0.002(2) 0.004(2) C24 0.029(2) 0.025(2) 0.037(2) 0.0123(18) 0.0066(18) 0.0030(19) C25 0.030(2) 0.031(2) 0.036(2) 0.0111(19) 0.0037(18) 0.004(2) C26 0.030(2) 0.028(2) 0.042(2) 0.0150(19) 0.0042(19) 0.0047(19) C27 0.035(3) 0.040(3) 0.050(3) 0.022(2) 0.018(2) 0.014(2) C28 0.046(3) 0.036(3) 0.034(2) 0.0087(19) 0.009(2) 0.012(2) C29 0.036(3) 0.029(2) 0.037(2) 0.0055(19) 0.0018(19) 0.004(2) O1 0.043(2) 0.065(3) 0.051(2) 0.0031(19) 0.0215(17) 0.009(2) O2 0.0271(18) 0.062(2) 0.065(2) 0.024(2) 0.0102(17) 0.0088(18) O3 0.038(2) 0.090(3) 0.056(2) -0.008(2) -0.0047(19) 0.006(2) O4 0.0265(18) 0.048(2) 0.068(2) 0.0135(19) 0.0048(17) 0.0032(17) O5 0.043(2) 0.049(2) 0.0453(18) 0.0085(16) 0.0103(16) 0.0154(18) O6 0.054(2) 0.044(2) 0.0484(19) 0.0104(16) 0.0159(17) 0.0138(18) O7 0.123(5) 0.081(3) 0.058(3) 0.013(2) 0.006(3) 0.065(4) C30 0.038(4) 0.038(4) 0.040(3) 0.013(3) 0.014(3) 0.018(3) C31 0.024(4) 0.040(5) 0.038(4) 0.008(4) 0.014(4) 0.013(4) C32 0.034(5) 0.029(5) 0.051(5) 0.010(4) 0.014(4) 0.009(4) C33 0.030(5) 0.056(7) 0.046(5) 0.021(5) 0.018(4) 0.010(5) C34 0.031(5) 0.044(5) 0.037(4) 0.016(4) 0.013(4) 0.016(4) C35 0.031(5) 0.039(5) 0.037(4) 0.004(4) 0.011(4) 0.013(4) C36 0.043(3) 0.046(3) 0.029(3) 0.006(3) 0.009(2) 0.017(3) C37 0.043(3) 0.046(3) 0.029(3) 0.006(3) 0.009(2) 0.017(3) O8 0.109(8) 0.045(5) 0.031(3) 0.011(3) 0.005(4) 0.021(5) O9 0.052(5) 0.040(4) 0.045(4) -0.001(4) 0.004(3) 0.010(4) O10 0.118(9) 0.038(4) 0.038(4) 0.007(3) 0.009(4) 0.032(5) O11 0.090(7) 0.061(6) 0.042(4) -0.002(4) -0.018(4) 0.031(5) O12 0.072(6) 0.084(7) 0.056(5) 0.025(5) 0.017(4) 0.040(6) O13 0.080(7) 0.069(6) 0.047(4) 0.027(4) 0.023(4) 0.032(5) O14 0.068(7) 0.070(7) 0.075(6) 0.019(5) -0.005(5) 0.021(6) O15 0.090(9) 0.070(7) 0.086(7) 0.017(6) -0.018(6) 0.010(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 N4 2.294(4) . ? Ag1 N2 2.342(3) . ? Ag1 O1 2.431(4) . ? Ag1 O2 2.622(4) . ? Ag1 Ag3 3.3633(6) . ? Ag2 N6 2.256(3) 2_544 ? Ag2 O4 2.321(3) 2_755 ? Ag2 N5 2.333(4) . ? Ag2 O7 2.621(5) . ? Ag3 N3 2.243(3) . ? Ag3 N1 2.298(4) . ? Ag3 O6 2.427(4) . ? Ag3 O5 2.471(4) . ? N1 C1 1.328(5) . ? N1 N2 1.349(6) . ? N2 C4 1.347(6) . ? N3 C11 1.338(6) . ? N3 N4 1.348(6) . ? N4 C8 1.318(5) . ? N5 C18 1.313(5) . ? N5 N6 1.384(5) . ? N6 C21 1.311(7) . ? N6 Ag2 2.256(3) 2_544 ? C1 C2 1.418(7) . ? C1 H1 0.9400 . ? C2 C3 1.381(7) . ? C2 C6 1.484(5) . ? C3 C4 1.394(6) . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C7 1.380(6) 2_767 ? C5 C6 1.382(7) . ? C5 H5 0.9400 . ? C6 C7 1.395(7) . ? C7 C5 1.380(6) 2_767 ? C7 H7 0.9400 . ? C8 C9 1.432(6) . ? C8 H8 0.9400 . ? C9 C10 1.356(7) . ? C9 C12 1.488(5) . ? C10 C11 1.407(6) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.397(7) . ? C12 C17 1.400(7) . ? C13 C14 1.380(6) . ? C13 H13 0.9400 . ? C14 C15 1.402(7) . ? C14 H14 0.9400 . ? C15 C16 1.379(7) . ? C15 C19 1.493(5) . ? C16 C17 1.389(6) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C19 1.401(7) . ? C18 H18 0.9400 . ? C19 C20 1.400(7) . ? C20 C21 1.397(6) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 O1 1.266(6) . ? C22 O2 1.271(6) . ? C22 C24 1.478(7) . ? C23 O3 1.230(7) . ? C23 O4 1.260(7) . ? C23 C26 1.539(6) . ? C24 C29 1.411(6) . ? C24 C25 1.418(6) . ? C25 C26 1.378(7) . ? C25 H25 0.9400 . ? C26 C27 1.389(7) . ? C27 C28 1.416(7) . ? C27 H27 0.9400 . ? C28 C29 1.375(8) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? O4 Ag2 2.321(3) 2_755 ? O5 H1W 0.8599 . ? O5 H2W 0.8585 . ? O6 H3W 0.8560 . ? O6 H4W 0.8596 . ? O7 H5W 0.8651 . ? O7 H6W 0.8535 . ? C30 C31 1.391(9) . ? C30 C35 1.494(10) . ? C30 H30 0.9647 . ? C31 C32 1.366(16) . ? C31 C36 1.482(5) . ? C32 C33 1.382(15) . ? C32 H32 0.9684 . ? C33 C34 1.399(15) . ? C33 H33 0.9914 . ? C34 C35 1.398(16) . ? C34 H34 0.9661 . ? C35 C37 1.483(5) . ? C36 O9 1.260(16) . ? C36 O8 1.309(19) . ? C37 O10 1.314(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N2 125.69(14) . . ? N4 Ag1 O1 139.53(14) . . ? N2 Ag1 O1 85.07(13) . . ? N4 Ag1 O2 96.47(12) . . ? N2 Ag1 O2 136.34(13) . . ? O1 Ag1 O2 52.20(12) . . ? N4 Ag1 Ag3 62.70(9) . . ? N2 Ag1 Ag3 63.30(10) . . ? O1 Ag1 Ag3 141.89(10) . . ? O2 Ag1 Ag3 158.54(8) . . ? N6 Ag2 O4 137.37(15) 2_544 2_755 ? N6 Ag2 N5 123.54(14) 2_544 . ? O4 Ag2 N5 95.17(14) 2_755 . ? N6 Ag2 O7 83.39(15) 2_544 . ? O4 Ag2 O7 96.65(18) 2_755 . ? N5 Ag2 O7 115.01(19) . . ? N3 Ag3 N1 128.87(14) . . ? N3 Ag3 O6 125.76(14) . . ? N1 Ag3 O6 88.73(14) . . ? N3 Ag3 O5 91.29(13) . . ? N1 Ag3 O5 133.57(14) . . ? O6 Ag3 O5 82.98(14) . . ? N3 Ag3 Ag1 64.48(10) . . ? N1 Ag3 Ag1 65.24(9) . . ? O6 Ag3 Ag1 139.73(11) . . ? O5 Ag3 Ag1 137.26(9) . . ? C1 N1 N2 119.6(4) . . ? C1 N1 Ag3 125.3(3) . . ? N2 N1 Ag3 115.0(2) . . ? C4 N2 N1 118.3(4) . . ? C4 N2 Ag1 124.7(3) . . ? N1 N2 Ag1 116.4(3) . . ? C11 N3 N4 119.0(3) . . ? C11 N3 Ag3 123.2(3) . . ? N4 N3 Ag3 115.9(3) . . ? C8 N4 N3 119.8(4) . . ? C8 N4 Ag1 123.1(3) . . ? N3 N4 Ag1 116.6(2) . . ? C18 N5 N6 118.9(4) . . ? C18 N5 Ag2 122.9(3) . . ? N6 N5 Ag2 117.6(3) . . ? C21 N6 N5 119.2(4) . . ? C21 N6 Ag2 122.3(3) . 2_544 ? N5 N6 Ag2 118.5(3) . 2_544 ? N1 C1 C2 124.8(5) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C3 C2 C1 114.9(4) . . ? C3 C2 C6 123.0(4) . . ? C1 C2 C6 122.1(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? N2 C4 C3 123.8(4) . . ? N2 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? C7 C5 C6 120.7(5) 2_767 . ? C7 C5 H5 119.7 2_767 . ? C6 C5 H5 119.7 . . ? C5 C6 C7 117.5(4) . . ? C5 C6 C2 121.1(4) . . ? C7 C6 C2 121.4(4) . . ? C5 C7 C6 121.8(5) 2_767 . ? C5 C7 H7 119.1 2_767 . ? C6 C7 H7 119.1 . . ? N4 C8 C9 123.9(4) . . ? N4 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C10 C9 C8 115.7(4) . . ? C10 C9 C12 123.7(4) . . ? C8 C9 C12 120.6(4) . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? N3 C11 C10 123.0(4) . . ? N3 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C13 C12 C17 118.4(4) . . ? C13 C12 C9 120.3(4) . . ? C17 C12 C9 121.3(4) . . ? C14 C13 C12 119.8(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 122.0(5) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 117.9(4) . . ? C16 C15 C19 120.7(4) . . ? C14 C15 C19 121.4(4) . . ? C15 C16 C17 120.9(5) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 121.0(5) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? N5 C18 C19 125.1(4) . . ? N5 C18 H18 117.5 . . ? C19 C18 H18 117.5 . . ? C20 C19 C18 114.8(4) . . ? C20 C19 C15 123.8(4) . . ? C18 C19 C15 121.3(4) . . ? C21 C20 C19 118.7(5) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N6 C21 C20 123.1(4) . . ? N6 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? O1 C22 O2 123.0(5) . . ? O1 C22 C24 117.2(4) . . ? O2 C22 C24 119.8(4) . . ? O3 C23 O4 124.5(5) . . ? O3 C23 C26 119.1(5) . . ? O4 C23 C26 116.3(5) . . ? C29 C24 C25 118.0(5) . . ? C29 C24 C22 121.7(4) . . ? C25 C24 C22 120.3(4) . . ? C26 C25 C24 122.2(4) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C25 C26 C27 118.9(4) . . ? C25 C26 C23 119.7(4) . . ? C27 C26 C23 121.4(5) . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C24 120.1(4) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? C22 O1 Ag1 96.4(3) . . ? C22 O2 Ag1 87.5(3) . . ? C23 O4 Ag2 107.0(3) . 2_755 ? Ag3 O5 H1W 135.7 . . ? Ag3 O5 H2W 94.9 . . ? H1W O5 H2W 106.9 . . ? Ag3 O6 H3W 115.7 . . ? Ag3 O6 H4W 121.3 . . ? H3W O6 H4W 108.2 . . ? Ag2 O7 H5W 125.2 . . ? Ag2 O7 H6W 116.5 . . ? H5W O7 H6W 106.8 . . ? C31 C30 C35 116.5(6) . . ? C31 C30 H30 122.4 . . ? C35 C30 H30 121.1 . . ? C32 C31 C30 122.6(8) . . ? C32 C31 C36 119.5(10) . . ? C30 C31 C36 117.8(9) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 120.8 . . ? C32 C33 C34 122.3(12) . . ? C32 C33 H33 118.7 . . ? C34 C33 H33 118.9 . . ? C35 C34 C33 118.2(9) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 122.4 . . ? C34 C35 C37 118.9(10) . . ? C34 C35 C30 120.1(7) . . ? C37 C35 C30 121.1(10) . . ? O9 C36 O8 121.9(10) . . ? O9 C36 C31 121.5(14) . . ? O8 C36 C31 116.6(11) . . ? O11 C37 O10 120.9(10) . . ? O11 C37 C35 123.1(14) . . ? O10 C37 C35 116.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ag1 Ag3 N3 2.54(18) . . . . ? N2 Ag1 Ag3 N3 -171.42(17) . . . . ? O1 Ag1 Ag3 N3 -134.3(2) . . . . ? O2 Ag1 Ag3 N3 -12.4(3) . . . . ? N4 Ag1 Ag3 N1 172.93(18) . . . . ? N2 Ag1 Ag3 N1 -1.02(18) . . . . ? O1 Ag1 Ag3 N1 36.1(2) . . . . ? O2 Ag1 Ag3 N1 158.0(3) . . . . ? N4 Ag1 Ag3 O6 118.53(19) . . . . ? N2 Ag1 Ag3 O6 -55.42(18) . . . . ? O1 Ag1 Ag3 O6 -18.3(2) . . . . ? O2 Ag1 Ag3 O6 103.6(3) . . . . ? N4 Ag1 Ag3 O5 -58.80(18) . . . . ? N2 Ag1 Ag3 O5 127.25(18) . . . . ? O1 Ag1 Ag3 O5 164.4(2) . . . . ? O2 Ag1 Ag3 O5 -73.7(3) . . . . ? N3 Ag3 N1 C1 -162.6(4) . . . . ? O6 Ag3 N1 C1 -25.4(4) . . . . ? O5 Ag3 N1 C1 53.6(5) . . . . ? Ag1 Ag3 N1 C1 -173.7(5) . . . . ? N3 Ag3 N1 N2 12.9(5) . . . . ? O6 Ag3 N1 N2 150.0(4) . . . . ? O5 Ag3 N1 N2 -130.9(3) . . . . ? Ag1 Ag3 N1 N2 1.8(3) . . . . ? C1 N1 N2 C4 1.6(7) . . . . ? Ag3 N1 N2 C4 -174.1(4) . . . . ? C1 N1 N2 Ag1 173.2(4) . . . . ? Ag3 N1 N2 Ag1 -2.6(5) . . . . ? N4 Ag1 N2 C4 166.1(4) . . . . ? O1 Ag1 N2 C4 14.7(4) . . . . ? O2 Ag1 N2 C4 3.6(5) . . . . ? Ag3 Ag1 N2 C4 172.7(5) . . . . ? N4 Ag1 N2 N1 -4.8(4) . . . . ? O1 Ag1 N2 N1 -156.3(4) . . . . ? O2 Ag1 N2 N1 -167.3(3) . . . . ? Ag3 Ag1 N2 N1 1.8(3) . . . . ? N1 Ag3 N3 C11 179.9(4) . . . . ? O6 Ag3 N3 C11 56.8(5) . . . . ? O5 Ag3 N3 C11 -25.5(4) . . . . ? Ag1 Ag3 N3 C11 -168.9(5) . . . . ? N1 Ag3 N3 N4 -15.5(4) . . . . ? O6 Ag3 N3 N4 -138.5(3) . . . . ? O5 Ag3 N3 N4 139.2(4) . . . . ? Ag1 Ag3 N3 N4 -4.3(3) . . . . ? C11 N3 N4 C8 -0.3(7) . . . . ? Ag3 N3 N4 C8 -165.6(3) . . . . ? C11 N3 N4 Ag1 171.6(4) . . . . ? Ag3 N3 N4 Ag1 6.3(5) . . . . ? N2 Ag1 N4 C8 174.0(4) . . . . ? O1 Ag1 N4 C8 -53.2(5) . . . . ? O2 Ag1 N4 C8 -18.0(4) . . . . ? Ag3 Ag1 N4 C8 167.4(4) . . . . ? N2 Ag1 N4 N3 2.4(4) . . . . ? O1 Ag1 N4 N3 135.1(3) . . . . ? O2 Ag1 N4 N3 170.3(4) . . . . ? Ag3 Ag1 N4 N3 -4.3(3) . . . . ? N6 Ag2 N5 C18 179.0(4) 2_544 . . . ? O4 Ag2 N5 C18 -19.8(4) 2_755 . . . ? O7 Ag2 N5 C18 80.0(4) . . . . ? N6 Ag2 N5 N6 7.7(5) 2_544 . . . ? O4 Ag2 N5 N6 168.9(4) 2_755 . . . ? O7 Ag2 N5 N6 -91.3(4) . . . . ? C18 N5 N6 C21 1.9(8) . . . . ? Ag2 N5 N6 C21 173.5(4) . . . . ? C18 N5 N6 Ag2 -179.0(4) . . . 2_544 ? Ag2 N5 N6 Ag2 -7.3(5) . . . 2_544 ? N2 N1 C1 C2 -1.4(8) . . . . ? Ag3 N1 C1 C2 173.8(4) . . . . ? N1 C1 C2 C3 0.1(8) . . . . ? N1 C1 C2 C6 -179.6(5) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C6 C2 C3 C4 -179.4(5) . . . . ? N1 N2 C4 C3 -0.6(8) . . . . ? Ag1 N2 C4 C3 -171.4(4) . . . . ? C2 C3 C4 N2 -0.7(8) . . . . ? C7 C5 C6 C7 0.7(10) 2_767 . . . ? C7 C5 C6 C2 -179.1(6) 2_767 . . . ? C3 C2 C6 C5 157.3(6) . . . . ? C1 C2 C6 C5 -23.0(8) . . . . ? C3 C2 C6 C7 -22.5(8) . . . . ? C1 C2 C6 C7 157.2(6) . . . . ? C5 C6 C7 C5 -0.8(10) . . . 2_767 ? C2 C6 C7 C5 179.1(6) . . . 2_767 ? N3 N4 C8 C9 -0.8(7) . . . . ? Ag1 N4 C8 C9 -172.2(4) . . . . ? N4 C8 C9 C10 1.2(8) . . . . ? N4 C8 C9 C12 179.1(5) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C12 C9 C10 C11 -178.3(5) . . . . ? N4 N3 C11 C10 1.0(8) . . . . ? Ag3 N3 C11 C10 165.2(4) . . . . ? C9 C10 C11 N3 -0.6(8) . . . . ? C10 C9 C12 C13 -156.6(6) . . . . ? C8 C9 C12 C13 25.6(7) . . . . ? C10 C9 C12 C17 21.5(8) . . . . ? C8 C9 C12 C17 -156.2(5) . . . . ? C17 C12 C13 C14 1.0(9) . . . . ? C9 C12 C13 C14 179.2(5) . . . . ? C12 C13 C14 C15 1.3(9) . . . . ? C13 C14 C15 C16 -2.3(9) . . . . ? C13 C14 C15 C19 179.9(5) . . . . ? C14 C15 C16 C17 0.9(9) . . . . ? C19 C15 C16 C17 178.8(5) . . . . ? C15 C16 C17 C12 1.3(9) . . . . ? C13 C12 C17 C16 -2.3(9) . . . . ? C9 C12 C17 C16 179.5(5) . . . . ? N6 N5 C18 C19 1.6(8) . . . . ? Ag2 N5 C18 C19 -169.6(4) . . . . ? N5 C18 C19 C20 -2.5(8) . . . . ? N5 C18 C19 C15 175.8(5) . . . . ? C16 C15 C19 C20 -15.9(8) . . . . ? C14 C15 C19 C20 161.9(5) . . . . ? C16 C15 C19 C18 166.0(5) . . . . ? C14 C15 C19 C18 -16.2(8) . . . . ? C18 C19 C20 C21 0.1(8) . . . . ? C15 C19 C20 C21 -178.1(5) . . . . ? N5 N6 C21 C20 -4.3(9) . . . . ? Ag2 N6 C21 C20 176.6(4) 2_544 . . . ? C19 C20 C21 N6 3.3(9) . . . . ? O1 C22 C24 C29 169.8(5) . . . . ? O2 C22 C24 C29 -10.3(8) . . . . ? O1 C22 C24 C25 -11.3(8) . . . . ? O2 C22 C24 C25 168.6(5) . . . . ? C29 C24 C25 C26 -2.3(8) . . . . ? C22 C24 C25 C26 178.7(5) . . . . ? C24 C25 C26 C27 1.3(8) . . . . ? C24 C25 C26 C23 -179.6(5) . . . . ? O3 C23 C26 C25 -2.1(9) . . . . ? O4 C23 C26 C25 178.1(5) . . . . ? O3 C23 C26 C27 176.9(6) . . . . ? O4 C23 C26 C27 -2.9(8) . . . . ? C25 C26 C27 C28 -0.3(8) . . . . ? C23 C26 C27 C28 -179.3(5) . . . . ? C26 C27 C28 C29 0.4(9) . . . . ? C27 C28 C29 C24 -1.5(9) . . . . ? C25 C24 C29 C28 2.4(8) . . . . ? C22 C24 C29 C28 -178.7(5) . . . . ? O2 C22 O1 Ag1 -10.7(6) . . . . ? C24 C22 O1 Ag1 169.1(4) . . . . ? N4 Ag1 O1 C22 51.9(5) . . . . ? N2 Ag1 O1 C22 -164.9(4) . . . . ? O2 Ag1 O1 C22 5.5(3) . . . . ? Ag3 Ag1 O1 C22 162.4(3) . . . . ? O1 C22 O2 Ag1 9.9(6) . . . . ? C24 C22 O2 Ag1 -170.0(5) . . . . ? N4 Ag1 O2 C22 -157.2(3) . . . . ? N2 Ag1 O2 C22 8.5(4) . . . . ? O1 Ag1 O2 C22 -5.5(3) . . . . ? Ag3 Ag1 O2 C22 -143.9(3) . . . . ? O3 C23 O4 Ag2 -13.5(8) . . . 2_755 ? C26 C23 O4 Ag2 166.3(4) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.516 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.135 #------------- END of CIF -----------------#