Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University State Key Laboratory of Coordinatio Nanjing 210093 CHINA ; _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Silver(I) complexes with oxazoline-containing tripodal ligand: structure variation via counter anions and reaction conditions ; _audit_creation_date 'Mon May 8 15:54:09 2006' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name 'Wei-Yin Sun.' 'Yong-Qing Huang.' 'Taka-aki Okamura' 'Zhong-Liang Shen.' ; N.Ueyama ; 'Yan Wang.' 'Xiao-Feng Wang.' 'Jin-Quan Yu.' data_1 _database_code_depnum_ccdc_archive 'CCDC 644133' _chemical_name_systematic ; [Ag2(L)2](CF3SO3)2 ; _chemical_name_common (Ag2(L)2)(CF3SO3)2 _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Ag2 F6 N6 O12 S2 ' _chemical_formula_sum 'C32 H30 Ag2 F6 N6 O12 S2' _chemical_formula_weight 1084.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_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 12.650(4) _cell_length_b 8.565(3) _cell_length_c 17.176(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.554(10) _cell_angle_gamma 90.00 _cell_volume 1860.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 10845 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour light-brown _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 16858 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4223 _reflns_number_gt 3345 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+25.6233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4223 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2079 _refine_ls_wR_factor_gt 0.1976 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.33088(5) 0.52137(7) 0.50433(4) 0.0314(2) Uani 1 1 d . . . S1 S 0.53059(15) 0.6769(3) 0.62938(12) 0.0308(4) Uani 1 1 d . . . F1 F 0.3342(4) 0.6535(9) 0.6731(4) 0.0637(19) Uani 1 1 d . . . F2 F 0.4499(6) 0.5486(8) 0.7526(4) 0.072(2) Uani 1 1 d . . . F3 F 0.4291(5) 0.7922(8) 0.7475(4) 0.0586(16) Uani 1 1 d . . . O1 O 0.2007(4) 0.0861(7) 0.5958(4) 0.0360(13) Uani 1 1 d . . . O3 O 0.0964(5) 0.5575(8) 0.3190(4) 0.0409(15) Uani 1 1 d . . . O5 O -0.1731(4) 0.0592(7) 0.5828(3) 0.0307(12) Uani 1 1 d . . . O11 O 0.5118(5) 0.5329(8) 0.5861(4) 0.0411(15) Uani 1 1 d . . . O12 O 0.6298(5) 0.6802(9) 0.6724(4) 0.0489(17) Uani 1 1 d . . . O13 O 0.5028(5) 0.8173(8) 0.5873(4) 0.0440(16) Uani 1 1 d . . . N1 N 0.2915(5) 0.2892(8) 0.5503(4) 0.0314(15) Uani 1 1 d . . . N3 N -0.0819(6) 0.5442(9) 0.3067(4) 0.0355(16) Uani 1 1 d . . . N5 N -0.2751(5) 0.2479(8) 0.5329(4) 0.0270(13) Uani 1 1 d . . . C1 C 0.1045(5) 0.2568(9) 0.5087(4) 0.0230(14) Uani 1 1 d . . . C01 C 0.4316(7) 0.6667(10) 0.7043(5) 0.0358(19) Uani 1 1 d . . . C2 C 0.1036(6) 0.3521(8) 0.4445(4) 0.0243(15) Uani 1 1 d . . . H1 H 0.1681 0.3882 0.4239 0.029 Uiso 1 1 calc R . . C3 C 0.0071(6) 0.3956(9) 0.4096(4) 0.0233(14) Uani 1 1 d . . . C4 C -0.0885(6) 0.3408(9) 0.4394(4) 0.0235(14) Uani 1 1 d . . . H2 H -0.1542 0.3711 0.4160 0.028 Uiso 1 1 calc R . . C5 C -0.0859(5) 0.2408(8) 0.5042(4) 0.0221(14) Uani 1 1 d . . . C6 C 0.0105(6) 0.1975(9) 0.5377(4) 0.0248(15) Uani 1 1 d . . . H3 H 0.0127 0.1274 0.5806 0.030 Uiso 1 1 calc R . . C11 C 0.2054(6) 0.2145(9) 0.5513(4) 0.0254(15) Uani 1 1 d . . . C12 C 0.3682(7) 0.2055(12) 0.5992(6) 0.044(2) Uani 1 1 d . . . H4 H 0.3993 0.2750 0.6398 0.053 Uiso 1 1 calc R . . H5 H 0.4258 0.1628 0.5676 0.053 Uiso 1 1 calc R . . C13 C 0.3045(7) 0.0743(12) 0.6356(6) 0.043(2) Uani 1 1 d . . . H6 H 0.3374 -0.0286 0.6262 0.052 Uiso 1 1 calc R . . H7 H 0.2986 0.0900 0.6925 0.052 Uiso 1 1 calc R . . C31 C 0.0037(6) 0.5028(9) 0.3417(4) 0.0244(15) Uani 1 1 d . . . C32 C -0.0503(8) 0.6551(12) 0.2461(5) 0.043(2) Uani 1 1 d . . . H8 H -0.0790 0.7604 0.2564 0.052 Uiso 1 1 calc R . . H9 H -0.0760 0.6201 0.1940 0.052 Uiso 1 1 calc R . . C33 C 0.0696(8) 0.6566(13) 0.2509(6) 0.051(3) Uani 1 1 d . . . H10 H 0.0995 0.6128 0.2029 0.061 Uiso 1 1 calc R . . H11 H 0.0967 0.7641 0.2586 0.061 Uiso 1 1 calc R . . C51 C -0.1841(6) 0.1876(9) 0.5378(4) 0.0227(14) Uani 1 1 d . . . C52 C -0.3481(6) 0.1476(11) 0.5776(5) 0.038(2) Uani 1 1 d . . . H12 H -0.3978 0.0908 0.5423 0.045 Uiso 1 1 calc R . . H13 H -0.3890 0.2105 0.6146 0.045 Uiso 1 1 calc R . . C53 C -0.2742(6) 0.0360(13) 0.6202(6) 0.045(2) Uani 1 1 d . . . H14 H -0.2686 0.0617 0.6764 0.054 Uiso 1 1 calc R . . H15 H -0.2987 -0.0732 0.6142 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0273(3) 0.0280(3) 0.0389(4) 0.0037(3) 0.0014(2) -0.0002(2) S1 0.0259(9) 0.0371(11) 0.0295(10) 0.0025(8) 0.0012(8) -0.0049(8) F1 0.036(3) 0.103(6) 0.053(4) -0.015(4) 0.011(3) -0.013(3) F2 0.101(5) 0.050(4) 0.067(4) 0.033(3) 0.043(4) 0.025(4) F3 0.077(4) 0.051(4) 0.049(3) -0.013(3) 0.012(3) 0.006(3) O1 0.028(3) 0.038(3) 0.042(3) 0.010(3) -0.003(2) 0.000(2) O3 0.035(3) 0.046(4) 0.041(3) 0.017(3) 0.007(3) -0.004(3) O5 0.020(3) 0.034(3) 0.038(3) 0.010(2) 0.006(2) 0.000(2) O11 0.033(3) 0.054(4) 0.036(3) -0.015(3) 0.010(3) -0.010(3) O12 0.031(3) 0.059(4) 0.057(4) 0.005(3) -0.009(3) -0.007(3) O13 0.054(4) 0.042(4) 0.037(3) 0.014(3) 0.003(3) -0.004(3) N1 0.017(3) 0.034(4) 0.043(4) 0.006(3) -0.001(3) -0.002(3) N3 0.034(4) 0.039(4) 0.033(4) 0.012(3) -0.002(3) -0.004(3) N5 0.021(3) 0.029(3) 0.031(3) 0.003(3) 0.003(3) 0.000(2) C1 0.020(3) 0.024(4) 0.025(4) 0.000(3) 0.002(3) 0.004(3) C01 0.041(5) 0.034(5) 0.033(4) -0.001(3) 0.010(4) -0.005(4) C2 0.023(3) 0.021(4) 0.029(4) -0.001(3) 0.003(3) -0.001(3) C3 0.025(4) 0.023(4) 0.022(3) 0.000(3) 0.002(3) -0.001(3) C4 0.021(3) 0.027(4) 0.023(3) 0.003(3) 0.000(3) 0.001(3) C5 0.023(3) 0.020(3) 0.024(3) -0.003(3) 0.003(3) 0.002(3) C6 0.025(4) 0.022(4) 0.027(4) -0.002(3) 0.000(3) 0.000(3) C11 0.026(4) 0.024(4) 0.027(4) 0.002(3) 0.000(3) 0.004(3) C12 0.028(4) 0.046(6) 0.058(6) 0.011(5) -0.014(4) 0.001(4) C13 0.032(4) 0.043(5) 0.054(6) 0.020(4) -0.014(4) 0.000(4) C31 0.028(4) 0.022(4) 0.023(3) -0.002(3) -0.001(3) 0.001(3) C32 0.057(6) 0.041(5) 0.031(4) 0.017(4) -0.012(4) -0.002(4) C33 0.059(6) 0.055(6) 0.038(5) 0.023(5) 0.003(5) -0.002(5) C51 0.024(3) 0.023(4) 0.021(3) 0.000(3) 0.001(3) 0.000(3) C52 0.020(4) 0.048(5) 0.046(5) 0.012(4) 0.009(3) -0.002(3) C53 0.023(4) 0.057(6) 0.055(6) 0.025(5) 0.012(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N5 2.188(7) 3_566 ? Ag1 N1 2.202(7) . ? Ag1 O11 2.599(6) 3_666 ? S1 O12 1.439(7) . ? S1 O13 1.442(7) . ? S1 O11 1.456(7) . ? S1 C01 1.822(9) . ? F1 C01 1.335(11) . ? F2 C01 1.325(11) . ? F3 C01 1.307(10) . ? O1 C11 1.342(9) . ? O1 C13 1.467(10) . ? O3 C31 1.331(9) . ? O3 C33 1.478(11) . ? O5 C51 1.348(9) . ? O5 C53 1.460(9) . ? O11 Ag1 2.599(6) 3_666 ? N1 C11 1.263(10) . ? N1 C12 1.454(11) . ? N3 C31 1.275(10) . ? N3 C32 1.471(11) . ? N5 C51 1.263(9) . ? N5 C52 1.489(10) . ? N5 Ag1 2.188(7) 3_566 ? C1 C2 1.372(10) . ? C1 C6 1.397(10) . ? C1 C11 1.499(10) . ? C2 C3 1.396(10) . ? C2 H1 0.9500 . ? C3 C4 1.407(10) . ? C3 C31 1.484(10) . ? C4 C5 1.403(10) . ? C4 H2 0.9500 . ? C5 C6 1.385(10) . ? C5 C51 1.458(10) . ? C6 H3 0.9500 . ? C12 C13 1.527(13) . ? C12 H4 0.9900 . ? C12 H5 0.9900 . ? C13 H6 0.9900 . ? C13 H7 0.9900 . ? C32 C33 1.516(14) . ? C32 H8 0.9900 . ? C32 H9 0.9900 . ? C33 H10 0.9900 . ? C33 H11 0.9900 . ? C52 C53 1.512(12) . ? C52 H12 0.9900 . ? C52 H13 0.9900 . ? C53 H14 0.9900 . ? C53 H15 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N1 147.8(2) 3_566 . ? N5 Ag1 O11 103.5(2) 3_566 3_666 ? N1 Ag1 O11 103.7(2) . 3_666 ? O12 S1 O13 116.0(4) . . ? O12 S1 O11 114.0(4) . . ? O13 S1 O11 114.6(4) . . ? O12 S1 C01 104.2(4) . . ? O13 S1 C01 103.4(4) . . ? O11 S1 C01 102.4(4) . . ? C11 O1 C13 105.6(6) . . ? C31 O3 C33 104.4(7) . . ? C51 O5 C53 106.6(6) . . ? S1 O11 Ag1 109.9(3) . 3_666 ? C11 N1 C12 107.8(7) . . ? C11 N1 Ag1 131.7(5) . . ? C12 N1 Ag1 119.8(5) . . ? C31 N3 C32 105.7(7) . . ? C51 N5 C52 107.9(6) . . ? C51 N5 Ag1 132.5(5) . 3_566 ? C52 N5 Ag1 118.2(5) . 3_566 ? C2 C1 C6 121.0(7) . . ? C2 C1 C11 121.7(6) . . ? C6 C1 C11 117.4(7) . . ? F3 C01 F2 106.1(7) . . ? F3 C01 F1 105.2(8) . . ? F2 C01 F1 109.2(8) . . ? F3 C01 S1 112.9(6) . . ? F2 C01 S1 111.5(6) . . ? F1 C01 S1 111.4(6) . . ? C1 C2 C3 119.5(7) . . ? C1 C2 H1 120.3 . . ? C3 C2 H1 120.3 . . ? C2 C3 C4 120.3(7) . . ? C2 C3 C31 120.6(6) . . ? C4 C3 C31 119.1(6) . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H2 120.3 . . ? C3 C4 H2 120.3 . . ? C6 C5 C4 119.7(7) . . ? C6 C5 C51 120.1(7) . . ? C4 C5 C51 120.2(6) . . ? C5 C6 C1 120.1(7) . . ? C5 C6 H3 119.9 . . ? C1 C6 H3 119.9 . . ? N1 C11 O1 118.3(7) . . ? N1 C11 C1 126.5(7) . . ? O1 C11 C1 115.2(6) . . ? N1 C12 C13 104.3(7) . . ? N1 C12 H4 110.9 . . ? C13 C12 H4 110.9 . . ? N1 C12 H5 110.9 . . ? C13 C12 H5 110.9 . . ? H4 C12 H5 108.9 . . ? O1 C13 C12 103.5(7) . . ? O1 C13 H6 111.1 . . ? C12 C13 H6 111.1 . . ? O1 C13 H7 111.1 . . ? C12 C13 H7 111.1 . . ? H6 C13 H7 109.0 . . ? N3 C31 O3 120.5(7) . . ? N3 C31 C3 123.3(7) . . ? O3 C31 C3 116.2(6) . . ? N3 C32 C33 105.0(7) . . ? N3 C32 H8 110.8 . . ? C33 C32 H8 110.8 . . ? N3 C32 H9 110.8 . . ? C33 C32 H9 110.8 . . ? H8 C32 H9 108.8 . . ? O3 C33 C32 104.2(7) . . ? O3 C33 H10 110.9 . . ? C32 C33 H10 110.9 . . ? O3 C33 H11 110.9 . . ? C32 C33 H11 110.9 . . ? H10 C33 H11 108.9 . . ? N5 C51 O5 116.8(6) . . ? N5 C51 C5 129.1(7) . . ? O5 C51 C5 114.0(6) . . ? N5 C52 C53 103.3(6) . . ? N5 C52 H12 111.1 . . ? C53 C52 H12 111.1 . . ? N5 C52 H13 111.1 . . ? C53 C52 H13 111.1 . . ? H12 C52 H13 109.1 . . ? O5 C53 C52 103.8(7) . . ? O5 C53 H14 111.0 . . ? C52 C53 H14 111.0 . . ? O5 C53 H15 111.0 . . ? C52 C53 H15 111.0 . . ? H14 C53 H15 109.0 . . ? 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 O12 S1 O11 Ag1 -54.5(5) . . . 3_666 ? O13 S1 O11 Ag1 82.5(4) . . . 3_666 ? C01 S1 O11 Ag1 -166.4(4) . . . 3_666 ? N5 Ag1 N1 C11 20.2(11) 3_566 . . . ? O11 Ag1 N1 C11 -126.7(8) 3_666 . . . ? N5 Ag1 N1 C12 -149.3(7) 3_566 . . . ? O11 Ag1 N1 C12 63.8(7) 3_666 . . . ? O12 S1 C01 F3 65.6(8) . . . . ? O13 S1 C01 F3 -56.1(8) . . . . ? O11 S1 C01 F3 -175.5(7) . . . . ? O12 S1 C01 F2 -53.9(8) . . . . ? O13 S1 C01 F2 -175.5(7) . . . . ? O11 S1 C01 F2 65.1(8) . . . . ? O12 S1 C01 F1 -176.3(7) . . . . ? O13 S1 C01 F1 62.1(7) . . . . ? O11 S1 C01 F1 -57.3(7) . . . . ? C6 C1 C2 C3 2.6(11) . . . . ? C11 C1 C2 C3 -176.2(7) . . . . ? C1 C2 C3 C4 -0.7(11) . . . . ? C1 C2 C3 C31 177.9(7) . . . . ? C2 C3 C4 C5 -0.6(11) . . . . ? C31 C3 C4 C5 -179.2(7) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C3 C4 C5 C51 177.6(7) . . . . ? C4 C5 C6 C1 1.9(11) . . . . ? C51 C5 C6 C1 -175.8(7) . . . . ? C2 C1 C6 C5 -3.2(11) . . . . ? C11 C1 C6 C5 175.7(7) . . . . ? C12 N1 C11 O1 2.2(10) . . . . ? Ag1 N1 C11 O1 -168.2(6) . . . . ? C12 N1 C11 C1 -179.5(8) . . . . ? Ag1 N1 C11 C1 10.1(13) . . . . ? C13 O1 C11 N1 2.5(10) . . . . ? C13 O1 C11 C1 -176.0(7) . . . . ? C2 C1 C11 N1 21.9(12) . . . . ? C6 C1 C11 N1 -157.0(8) . . . . ? C2 C1 C11 O1 -159.8(7) . . . . ? C6 C1 C11 O1 21.3(10) . . . . ? C11 N1 C12 C13 -5.7(10) . . . . ? Ag1 N1 C12 C13 166.1(6) . . . . ? C11 O1 C13 C12 -5.7(10) . . . . ? N1 C12 C13 O1 6.8(10) . . . . ? C32 N3 C31 O3 -1.5(11) . . . . ? C32 N3 C31 C3 177.5(7) . . . . ? C33 O3 C31 N3 -2.0(11) . . . . ? C33 O3 C31 C3 178.9(7) . . . . ? C2 C3 C31 N3 178.7(8) . . . . ? C4 C3 C31 N3 -2.7(11) . . . . ? C2 C3 C31 O3 -2.3(10) . . . . ? C4 C3 C31 O3 176.3(7) . . . . ? C31 N3 C32 C33 4.2(10) . . . . ? C31 O3 C33 C32 4.4(10) . . . . ? N3 C32 C33 O3 -5.3(10) . . . . ? C52 N5 C51 O5 -3.2(9) . . . . ? Ag1 N5 C51 O5 162.1(5) 3_566 . . . ? C52 N5 C51 C5 179.8(8) . . . . ? Ag1 N5 C51 C5 -14.8(12) 3_566 . . . ? C53 O5 C51 N5 -5.4(10) . . . . ? C53 O5 C51 C5 172.0(7) . . . . ? C6 C5 C51 N5 155.7(8) . . . . ? C4 C5 C51 N5 -21.9(12) . . . . ? C6 C5 C51 O5 -21.4(10) . . . . ? C4 C5 C51 O5 161.0(7) . . . . ? C51 N5 C52 C53 10.0(10) . . . . ? Ag1 N5 C52 C53 -157.8(6) 3_566 . . . ? C51 O5 C53 C52 11.2(10) . . . . ? N5 C52 C53 O5 -12.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.988 _refine_diff_density_min -1.593 _refine_diff_density_rms 0.210 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 644134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Ag2 N6 O12 S2' _chemical_formula_sum 'C32 H36 Ag2 N6 O12 S2' _chemical_formula_weight 976.52 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' 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' _symmetry_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 12.3750(10) _cell_length_b 17.497(2) _cell_length_c 8.2580(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.634(2) _cell_angle_gamma 90.00 _cell_volume 1784.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1923 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 21.56 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8609 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9434 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3491 _reflns_number_gt 2883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+5.4321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3491 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.33818(4) 0.02880(4) 1.02079(7) 0.0509(2) Uani 1 1 d . . . S1 S 1.49971(18) 0.14396(11) 0.8446(3) 0.0553(5) Uani 1 1 d . . . O1 O 1.1728(4) 0.1243(3) 1.4295(6) 0.0473(12) Uani 1 1 d . . . O2 O 0.9462(4) -0.1884(3) 0.9621(6) 0.0481(12) Uani 1 1 d . . . O3 O 0.7975(4) 0.0673(3) 1.4409(6) 0.0452(12) Uani 1 1 d . . . O4 O 1.5211(7) 0.0803(5) 0.9428(14) 0.080(4) Uani 0.769(15) 1 d P . 1 O5 O 1.5020(8) 0.1315(7) 0.6760(10) 0.100(4) Uani 0.769(15) 1 d P . 1 O4' O 1.474(3) 0.1298(19) 1.016(4) 0.083(12) Uani 0.231(15) 1 d P . 2 O5' O 1.581(3) 0.0814(16) 0.821(4) 0.087(12) Uani 0.231(15) 1 d P . 2 O6 O 1.3869(6) 0.1708(5) 0.8650(13) 0.119(3) Uani 1 1 d . . . N1 N 1.2794(4) 0.0786(3) 1.2437(7) 0.0397(13) Uani 1 1 d . . . N2 N 1.1270(5) -0.1745(3) 0.9759(7) 0.0446(14) Uani 1 1 d . . . N3 N 0.7083(4) 0.0134(3) 1.2282(7) 0.0401(13) Uani 1 1 d . . . C1 C 1.0970(5) 0.0249(3) 1.2622(7) 0.0295(13) Uani 1 1 d . . . C2 C 1.1090(5) -0.0406(3) 1.1690(7) 0.0305(13) Uani 1 1 d . . . H2A H 1.1774 -0.0550 1.1392 0.037 Uiso 1 1 calc R . . C3 C 1.0205(5) -0.0839(3) 1.1213(7) 0.0267(13) Uani 1 1 d . . . C4 C 0.9179(5) -0.0631(3) 1.1651(7) 0.0285(13) Uani 1 1 d . . . H4A H 0.8579 -0.0925 1.1318 0.034 Uiso 1 1 calc R . . C5 C 0.9054(5) 0.0016(3) 1.2586(7) 0.0267(12) Uani 1 1 d . . . C6 C 0.9952(5) 0.0446(3) 1.3102(7) 0.0285(13) Uani 1 1 d . . . H6A H 0.9873 0.0867 1.3772 0.034 Uiso 1 1 calc R . . C7 C 1.1890(5) 0.0759(3) 1.3074(8) 0.0321(14) Uani 1 1 d . . . C8 C 1.3434(6) 0.1401(5) 1.3276(10) 0.057(2) Uani 1 1 d . . . H8A H 1.3631 0.1790 1.2511 0.068 Uiso 1 1 calc R . . H8B H 1.4089 0.1196 1.3819 0.068 Uiso 1 1 calc R . . C9 C 1.2697(6) 0.1726(5) 1.4489(11) 0.060(2) Uani 1 1 d . . . H9A H 1.3027 0.1692 1.5583 0.072 Uiso 1 1 calc R . . H9B H 1.2523 0.2256 1.4246 0.072 Uiso 1 1 calc R . . C10 C 1.0337(5) -0.1520(3) 1.0175(7) 0.0308(13) Uani 1 1 d . . . C11 C 1.1051(7) -0.2407(5) 0.8720(11) 0.064(2) Uani 1 1 d . . . H11A H 1.1393 -0.2860 0.9193 0.076 Uiso 1 1 calc R . . H11B H 1.1319 -0.2324 0.7655 0.076 Uiso 1 1 calc R . . C12 C 0.9851(7) -0.2491(4) 0.8604(10) 0.056(2) Uani 1 1 d . . . H12A H 0.9563 -0.2432 0.7490 0.068 Uiso 1 1 calc R . . H12B H 0.9640 -0.2988 0.8998 0.068 Uiso 1 1 calc R . . C13 C 0.7974(5) 0.0257(3) 1.3050(7) 0.0319(14) Uani 1 1 d . . . C14 C 0.6232(6) 0.0496(5) 1.3209(10) 0.054(2) Uani 1 1 d . . . H14A H 0.5718 0.0118 1.3547 0.065 Uiso 1 1 calc R . . H14B H 0.5846 0.0885 1.2568 0.065 Uiso 1 1 calc R . . C15 C 0.6854(6) 0.0842(5) 1.4653(10) 0.058(2) Uani 1 1 d . . . H15A H 0.6737 0.1390 1.4693 0.070 Uiso 1 1 calc R . . H15B H 0.6637 0.0616 1.5654 0.070 Uiso 1 1 calc R . . C16 C 1.5904(9) 0.2171(6) 0.8965(14) 0.094(3) Uani 1 1 d . . . H16A H 1.5511 0.2633 0.9150 0.141 Uiso 1 1 calc R . . H16B H 1.6373 0.2250 0.8098 0.141 Uiso 1 1 calc R . . H16C H 1.6329 0.2034 0.9935 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0420(3) 0.0677(4) 0.0440(4) -0.0150(3) 0.0097(2) -0.0133(3) S1 0.0697(13) 0.0385(10) 0.0600(13) -0.0007(9) 0.0228(10) -0.0029(9) O1 0.036(3) 0.056(3) 0.050(3) -0.024(2) 0.007(2) -0.007(2) O2 0.053(3) 0.042(3) 0.050(3) -0.014(2) 0.008(2) -0.006(2) O3 0.037(3) 0.057(3) 0.042(3) -0.015(2) -0.001(2) 0.011(2) O4 0.061(5) 0.057(5) 0.118(10) 0.028(6) -0.023(6) -0.006(4) O5 0.094(7) 0.152(10) 0.053(6) 0.002(6) 0.005(5) -0.049(7) O4' 0.10(2) 0.08(2) 0.08(2) -0.024(17) 0.041(18) -0.037(19) O5' 0.13(3) 0.067(18) 0.07(2) 0.008(15) 0.05(2) 0.002(18) O6 0.083(5) 0.095(6) 0.182(9) -0.008(6) 0.030(6) 0.010(4) N1 0.030(3) 0.048(3) 0.041(3) -0.009(3) 0.000(2) -0.005(2) N2 0.036(3) 0.043(3) 0.055(4) -0.019(3) 0.001(3) 0.011(3) N3 0.030(3) 0.047(3) 0.044(3) -0.013(3) 0.003(2) 0.000(2) C1 0.034(3) 0.028(3) 0.025(3) 0.007(3) -0.003(2) 0.004(3) C2 0.035(3) 0.033(3) 0.024(3) 0.005(3) 0.006(2) 0.005(3) C3 0.033(3) 0.024(3) 0.023(3) 0.005(2) 0.000(2) 0.002(2) C4 0.030(3) 0.027(3) 0.028(3) -0.001(3) 0.001(2) -0.004(2) C5 0.030(3) 0.027(3) 0.023(3) 0.007(2) -0.001(2) -0.001(2) C6 0.038(3) 0.024(3) 0.024(3) -0.001(2) 0.001(2) 0.003(2) C7 0.031(3) 0.032(3) 0.032(3) -0.004(3) -0.004(3) 0.001(3) C8 0.035(4) 0.067(5) 0.068(5) -0.021(4) 0.005(4) -0.011(4) C9 0.040(4) 0.063(5) 0.078(6) -0.035(5) -0.001(4) -0.009(4) C10 0.044(4) 0.020(3) 0.028(3) 0.004(2) 0.001(3) -0.001(3) C11 0.073(6) 0.054(5) 0.064(6) -0.017(4) 0.000(4) 0.015(4) C12 0.082(6) 0.037(4) 0.051(5) -0.015(4) 0.009(4) -0.004(4) C13 0.040(3) 0.028(3) 0.028(3) 0.001(3) 0.007(3) 0.004(3) C14 0.037(4) 0.067(5) 0.058(5) -0.010(4) 0.011(3) 0.012(4) C15 0.053(5) 0.061(5) 0.061(5) -0.016(4) 0.007(4) 0.024(4) C16 0.107(9) 0.076(7) 0.101(9) 0.001(6) 0.015(7) -0.023(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 N1 2.201(5) . ? Ag1 N3 2.226(6) 3_757 ? Ag1 O4' 2.44(3) . ? Ag1 O5' 2.50(3) 3_857 ? Ag1 O4 2.556(9) . ? Ag1 O4 2.589(9) 3_857 ? S1 O4 1.393(8) . ? S1 O5 1.411(9) . ? S1 O4' 1.49(3) . ? S1 O6 1.493(8) . ? S1 O5' 1.51(3) . ? S1 C16 1.738(10) . ? O1 C7 1.341(7) . ? O1 C9 1.467(8) . ? O2 C10 1.313(8) . ? O2 C12 1.455(8) . ? O3 C13 1.337(7) . ? O3 C15 1.444(8) . ? O4 Ag1 2.589(9) 3_857 ? O4' O6 1.75(4) . ? O5' Ag1 2.50(3) 3_857 ? N1 C7 1.267(8) . ? N1 C8 1.482(9) . ? N2 C10 1.287(8) . ? N2 C11 1.457(9) . ? N3 C13 1.255(8) . ? N3 C14 1.482(8) . ? N3 Ag1 2.226(6) 3_757 ? C1 C6 1.387(8) . ? C1 C2 1.394(8) . ? C1 C7 1.476(8) . ? C2 C3 1.370(8) . ? C2 H2A 0.9300 . ? C3 C4 1.390(8) . ? C3 C10 1.483(8) . ? C4 C5 1.384(8) . ? C4 H4A 0.9300 . ? C5 C6 1.387(8) . ? C5 C13 1.475(8) . ? C6 H6A 0.9300 . ? C8 C9 1.508(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.489(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.505(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 145.48(19) . 3_757 ? N1 Ag1 O4' 89.5(7) . . ? N3 Ag1 O4' 111.3(7) 3_757 . ? N1 Ag1 O5' 90.6(7) . 3_857 ? N3 Ag1 O5' 107.4(7) 3_757 3_857 ? O4' Ag1 O5' 108.3(13) . 3_857 ? N1 Ag1 O4 114.6(3) . . ? N3 Ag1 O4 93.8(3) 3_757 . ? O4' Ag1 O4 28.3(7) . . ? O5' Ag1 O4 94.1(8) 3_857 . ? N1 Ag1 O4 116.7(3) . 3_857 ? N3 Ag1 O4 89.7(3) 3_757 3_857 ? O4' Ag1 O4 94.5(10) . 3_857 ? O5' Ag1 O4 29.2(7) 3_857 3_857 ? O4 Ag1 O4 71.9(3) . 3_857 ? O4 S1 O5 115.9(7) . . ? O4 S1 O4' 50.2(13) . . ? O5 S1 O4' 158.3(11) . . ? O4 S1 O6 109.3(6) . . ? O5 S1 O6 103.7(6) . . ? O4' S1 O6 71.6(15) . . ? O4 S1 O5' 52.5(11) . . ? O5 S1 O5' 72.8(13) . . ? O4' S1 O5' 100.8(19) . . ? O6 S1 O5' 151.5(13) . . ? O4 S1 C16 110.4(5) . . ? O5 S1 C16 107.7(5) . . ? O4' S1 C16 93.6(11) . . ? O6 S1 C16 109.6(5) . . ? O5' S1 C16 98.2(14) . . ? C7 O1 C9 106.6(5) . . ? C10 O2 C12 105.0(5) . . ? C13 O3 C15 106.2(5) . . ? S1 O4 Ag1 106.9(4) . . ? S1 O4 Ag1 139.3(7) . 3_857 ? Ag1 O4 Ag1 108.1(3) . 3_857 ? S1 O4' O6 54.2(12) . . ? S1 O4' Ag1 109.1(15) . . ? O6 O4' Ag1 85.3(12) . . ? S1 O5' Ag1 137.7(16) . 3_857 ? S1 O6 O4' 54.1(9) . . ? C7 N1 C8 107.0(5) . . ? C7 N1 Ag1 132.9(4) . . ? C8 N1 Ag1 118.9(4) . . ? C10 N2 C11 105.2(6) . . ? C13 N3 C14 107.2(6) . . ? C13 N3 Ag1 133.7(4) . 3_757 ? C14 N3 Ag1 117.9(4) . 3_757 ? C6 C1 C2 119.5(5) . . ? C6 C1 C7 118.5(5) . . ? C2 C1 C7 121.9(5) . . ? C3 C2 C1 120.1(6) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 C10 119.7(5) . . ? C4 C3 C10 119.8(5) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 119.9(5) . . ? C4 C5 C13 120.9(5) . . ? C6 C5 C13 119.2(5) . . ? C1 C6 C5 120.1(5) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? N1 C7 O1 117.9(5) . . ? N1 C7 C1 127.2(6) . . ? O1 C7 C1 115.0(5) . . ? N1 C8 C9 104.9(6) . . ? N1 C8 H8A 110.8 . . ? C9 C8 H8A 110.8 . . ? N1 C8 H8B 110.8 . . ? C9 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? O1 C9 C8 103.6(5) . . ? O1 C9 H9A 111.0 . . ? C8 C9 H9A 111.0 . . ? O1 C9 H9B 111.0 . . ? C8 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N2 C10 O2 119.5(5) . . ? N2 C10 C3 122.2(6) . . ? O2 C10 C3 118.2(5) . . ? N2 C11 C12 105.4(6) . . ? N2 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? N2 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? O2 C12 C11 104.8(6) . . ? O2 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? O2 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? N3 C13 O3 118.1(6) . . ? N3 C13 C5 126.9(6) . . ? O3 C13 C5 114.9(5) . . ? N3 C14 C15 103.7(6) . . ? N3 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? N3 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O3 C15 C14 104.7(5) . . ? O3 C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? O3 C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? S1 C16 H16A 109.5 . . ? S1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 O5 S1 O4 Ag1 -99.5(6) . . . . ? O4' S1 O4 Ag1 60.7(15) . . . . ? O6 S1 O4 Ag1 17.2(7) . . . . ? O5' S1 O4 Ag1 -137.6(18) . . . . ? C16 S1 O4 Ag1 137.8(5) . . . . ? O5 S1 O4 Ag1 48.9(10) . . . 3_857 ? O4' S1 O4 Ag1 -151(2) . . . 3_857 ? O6 S1 O4 Ag1 165.6(7) . . . 3_857 ? O5' S1 O4 Ag1 10.7(17) . . . 3_857 ? C16 S1 O4 Ag1 -73.9(10) . . . 3_857 ? N1 Ag1 O4 S1 -89.3(6) . . . . ? N3 Ag1 O4 S1 70.4(6) 3_757 . . . ? O4' Ag1 O4 S1 -59.8(18) . . . . ? O5' Ag1 O4 S1 178.2(9) 3_857 . . . ? O4 Ag1 O4 S1 158.9(9) 3_857 . . . ? N1 Ag1 O4 Ag1 111.8(4) . . . 3_857 ? N3 Ag1 O4 Ag1 -88.5(4) 3_757 . . 3_857 ? O4' Ag1 O4 Ag1 141(2) . . . 3_857 ? O5' Ag1 O4 Ag1 19.2(8) 3_857 . . 3_857 ? O4 Ag1 O4 Ag1 0.0 3_857 . . 3_857 ? O4 S1 O4' O6 -136.8(14) . . . . ? O5 S1 O4' O6 -81(4) . . . . ? O5' S1 O4' O6 -151.5(14) . . . . ? C16 S1 O4' O6 109.4(6) . . . . ? O4 S1 O4' Ag1 -67.8(13) . . . . ? O5 S1 O4' Ag1 -12(6) . . . . ? O6 S1 O4' Ag1 69.1(15) . . . . ? O5' S1 O4' Ag1 -82(2) . . . . ? C16 S1 O4' Ag1 178.5(15) . . . . ? N1 Ag1 O4' S1 -152(2) . . . . ? N3 Ag1 O4' S1 0(2) 3_757 . . . ? O5' Ag1 O4' S1 118(2) 3_857 . . . ? O4 Ag1 O4' S1 54.8(13) . . . . ? O4 Ag1 O4' S1 91(2) 3_857 . . . ? N1 Ag1 O4' O6 -102.3(10) . . . . ? N3 Ag1 O4' O6 49.4(13) 3_757 . . . ? O5' Ag1 O4' O6 167.2(11) 3_857 . . . ? O4 Ag1 O4' O6 104.3(19) . . . . ? O4 Ag1 O4' O6 140.9(11) 3_857 . . . ? O4 S1 O5' Ag1 -10.7(17) . . . 3_857 ? O5 S1 O5' Ag1 -155(3) . . . 3_857 ? O4' S1 O5' Ag1 4(3) . . . 3_857 ? O6 S1 O5' Ag1 -68(4) . . . 3_857 ? C16 S1 O5' Ag1 99(3) . . . 3_857 ? O4 S1 O6 O4' 33.8(12) . . . . ? O5 S1 O6 O4' 157.9(12) . . . . ? O5' S1 O6 O4' 79(3) . . . . ? C16 S1 O6 O4' -87.3(12) . . . . ? Ag1 O4' O6 S1 -117.7(12) . . . . ? N3 Ag1 N1 C7 26.3(8) 3_757 . . . ? O4' Ag1 N1 C7 155.2(11) . . . . ? O5' Ag1 N1 C7 -96.5(10) 3_857 . . . ? O4 Ag1 N1 C7 168.7(6) . . . . ? O4 Ag1 N1 C7 -110.0(6) 3_857 . . . ? N3 Ag1 N1 C8 -138.9(5) 3_757 . . . ? O4' Ag1 N1 C8 -10.0(11) . . . . ? O5' Ag1 N1 C8 98.3(10) 3_857 . . . ? O4 Ag1 N1 C8 3.5(6) . . . . ? O4 Ag1 N1 C8 84.7(6) 3_857 . . . ? C6 C1 C2 C3 2.0(8) . . . . ? C7 C1 C2 C3 -176.0(5) . . . . ? C1 C2 C3 C4 0.0(9) . . . . ? C1 C2 C3 C10 177.9(5) . . . . ? C2 C3 C4 C5 -0.4(9) . . . . ? C10 C3 C4 C5 -178.4(5) . . . . ? C3 C4 C5 C6 -1.1(8) . . . . ? C3 C4 C5 C13 179.2(5) . . . . ? C2 C1 C6 C5 -3.4(8) . . . . ? C7 C1 C6 C5 174.6(5) . . . . ? C4 C5 C6 C1 3.0(9) . . . . ? C13 C5 C6 C1 -177.2(5) . . . . ? C8 N1 C7 O1 -1.3(8) . . . . ? Ag1 N1 C7 O1 -167.8(5) . . . . ? C8 N1 C7 C1 178.5(6) . . . . ? Ag1 N1 C7 C1 12.0(10) . . . . ? C9 O1 C7 N1 3.2(8) . . . . ? C9 O1 C7 C1 -176.6(6) . . . . ? C6 C1 C7 N1 -161.1(6) . . . . ? C2 C1 C7 N1 16.9(10) . . . . ? C6 C1 C7 O1 18.7(8) . . . . ? C2 C1 C7 O1 -163.3(6) . . . . ? C7 N1 C8 C9 -1.2(8) . . . . ? Ag1 N1 C8 C9 167.6(5) . . . . ? C7 O1 C9 C8 -3.6(8) . . . . ? N1 C8 C9 O1 2.9(9) . . . . ? C11 N2 C10 O2 -1.0(8) . . . . ? C11 N2 C10 C3 -178.4(6) . . . . ? C12 O2 C10 N2 0.0(8) . . . . ? C12 O2 C10 C3 177.5(5) . . . . ? C2 C3 C10 N2 3.2(9) . . . . ? C4 C3 C10 N2 -178.8(6) . . . . ? C2 C3 C10 O2 -174.1(5) . . . . ? C4 C3 C10 O2 3.8(8) . . . . ? C10 N2 C11 C12 1.6(8) . . . . ? C10 O2 C12 C11 1.0(8) . . . . ? N2 C11 C12 O2 -1.5(9) . . . . ? C14 N3 C13 O3 -1.8(8) . . . . ? Ag1 N3 C13 O3 165.3(5) 3_757 . . . ? C14 N3 C13 C5 -179.1(6) . . . . ? Ag1 N3 C13 C5 -12.1(10) 3_757 . . . ? C15 O3 C13 N3 2.8(8) . . . . ? C15 O3 C13 C5 -179.6(6) . . . . ? C4 C5 C13 N3 -28.1(10) . . . . ? C6 C5 C13 N3 152.1(6) . . . . ? C4 C5 C13 O3 154.4(6) . . . . ? C6 C5 C13 O3 -25.3(8) . . . . ? C13 N3 C14 C15 0.0(8) . . . . ? Ag1 N3 C14 C15 -169.4(5) 3_757 . . . ? C13 O3 C15 C14 -2.4(8) . . . . ? N3 C14 C15 O3 1.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.086 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.118 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 644135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ag2(L)2](BF4)2 ; _chemical_name_common (Ag2(L)2)(BF4)2 _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Ag2 B2 F8 N6 O6' _chemical_formula_sum 'C30 H30 Ag2 B2 F8 N6 O6' _chemical_formula_weight 959.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1559(15) _cell_length_b 18.0657(18) _cell_length_c 14.3223(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.526(3) _cell_angle_gamma 90.00 _cell_volume 3452.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1103 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 16.08 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8564 _exptl_absorpt_correction_T_max 0.9188 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16775 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6056 _reflns_number_gt 3770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6056 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.27536(7) 0.60156(5) 0.67633(6) 0.0426(3) Uani 1 1 d . . . Ag2 Ag 0.18657(7) 0.47113(5) 0.87403(7) 0.0462(3) Uani 1 1 d . . . B1 B 0.3492(14) 0.6816(10) 0.4784(13) 0.060(4) Uani 1 1 d . . . B2 B 0.1396(17) 0.3316(11) 0.0575(16) 0.077(6) Uani 1 1 d . . . F1 F 0.2626(8) 0.6719(5) 0.4983(9) 0.133(4) Uani 1 1 d . . . F2 F 0.4279(9) 0.6664(5) 0.5622(7) 0.127(4) Uani 1 1 d . . . F3 F 0.3555(6) 0.7566(4) 0.4582(5) 0.068(2) Uani 1 1 d . . . F4 F 0.3532(7) 0.6379(4) 0.4049(6) 0.085(3) Uani 1 1 d . . . F5 F 0.0790(8) 0.3044(6) 0.0998(9) 0.145(5) Uani 1 1 d . . . F6 F 0.2054(6) 0.2832(5) 0.0457(7) 0.108(3) Uani 1 1 d . . . F7 F 0.1962(10) 0.3849(7) 0.1246(10) 0.161(5) Uani 1 1 d . . . F8 F 0.0913(8) 0.3695(7) -0.0244(8) 0.139(5) Uani 1 1 d . . . O1 O -0.1309(6) 0.4528(4) 0.6404(5) 0.050(2) Uani 1 1 d . . . O2 O 0.3096(6) 0.4072(4) 0.5067(6) 0.057(2) Uani 1 1 d . . . O3 O 0.0037(6) 0.2869(4) 0.3200(5) 0.046(2) Uani 1 1 d . . . O4 O 0.7404(5) 0.3489(4) 0.9077(5) 0.042(2) Uani 1 1 d . . . O5 O 0.5700(6) 0.6616(4) 0.9093(6) 0.052(2) Uani 1 1 d . . . O6 O 0.3803(6) 0.2917(4) 0.8390(6) 0.048(2) Uani 1 1 d . . . N1 N 0.0147(7) 0.4785(5) 0.7602(6) 0.040(2) Uani 1 1 d . . . N2 N 0.3189(7) 0.4962(5) 0.6192(6) 0.039(2) Uani 1 1 d . . . N3 N -0.1458(7) 0.3307(5) 0.3154(6) 0.036(2) Uani 1 1 d . . . N4 N 0.7965(7) 0.4345(4) 1.0284(6) 0.033(2) Uani 1 1 d . . . N5 N 0.4192(7) 0.6498(4) 0.7906(6) 0.036(2) Uani 1 1 d . . . N6 N 0.2661(6) 0.3767(4) 0.8378(6) 0.033(2) Uani 1 1 d . . . C1 C 0.0165(8) 0.4337(5) 0.5992(8) 0.031(3) Uani 1 1 d . . . C2 C 0.1152(8) 0.4500(5) 0.6142(7) 0.033(3) Uani 1 1 d . . . H2A H 0.1519 0.4772 0.6696 0.040 Uiso 1 1 calc R . . C3 C 0.1609(8) 0.4261(6) 0.5467(8) 0.034(3) Uani 1 1 d . . . C4 C 0.1049(8) 0.3850(5) 0.4655(8) 0.036(3) Uani 1 1 d . . . H4B H 0.1348 0.3671 0.4213 0.044 Uiso 1 1 calc R . . C5 C 0.0065(8) 0.3706(5) 0.4498(7) 0.028(2) Uani 1 1 d . . . C6 C -0.0398(8) 0.3938(5) 0.5147(7) 0.033(3) Uani 1 1 d . . . H6A H -0.1071 0.3834 0.5030 0.040 Uiso 1 1 calc R . . C7 C -0.0296(8) 0.4552(5) 0.6733(9) 0.035(3) Uani 1 1 d . . . C8 C -0.1614(9) 0.4765(7) 0.7232(8) 0.057(4) Uani 1 1 d . . . H8A H -0.1968 0.4371 0.7436 0.068 Uiso 1 1 calc R . . H8B H -0.2048 0.5195 0.7053 0.068 Uiso 1 1 calc R . . C9 C -0.0653(9) 0.4951(8) 0.8047(9) 0.067(4) Uani 1 1 d . . . H9A H -0.0639 0.5468 0.8232 0.080 Uiso 1 1 calc R . . H9B H -0.0570 0.4647 0.8628 0.080 Uiso 1 1 calc R . . C10 C 0.2655(8) 0.4466(6) 0.5616(8) 0.038(3) Uani 1 1 d . . . C11 C 0.4061(9) 0.4429(7) 0.5218(10) 0.060(4) Uani 1 1 d . . . H11A H 0.4046 0.4718 0.4643 0.072 Uiso 1 1 calc R . . H11B H 0.4594 0.4066 0.5351 0.072 Uiso 1 1 calc R . . C12 C 0.4200(8) 0.4913(7) 0.6092(10) 0.055(4) Uani 1 1 d . . . H12A H 0.4437 0.5399 0.5985 0.066 Uiso 1 1 calc R . . H12B H 0.4679 0.4697 0.6682 0.066 Uiso 1 1 calc R . . C13 C -0.0524(8) 0.3295(5) 0.3587(8) 0.030(3) Uani 1 1 d . . . C14 C -0.0666(9) 0.2472(6) 0.2389(8) 0.047(3) Uani 1 1 d . . . H14A H -0.0642 0.1946 0.2529 0.056 Uiso 1 1 calc R . . H14B H -0.0519 0.2549 0.1782 0.056 Uiso 1 1 calc R . . C15 C -0.1683(9) 0.2789(6) 0.2301(9) 0.049(3) Uani 1 1 d . . . H15A H -0.1974 0.3049 0.1678 0.059 Uiso 1 1 calc R . . H15B H -0.2139 0.2402 0.2349 0.059 Uiso 1 1 calc R . . C16 C 0.6193(8) 0.4361(6) 0.9223(8) 0.032(3) Uani 1 1 d . . . C17 C 0.6040(9) 0.5116(6) 0.9112(8) 0.040(3) Uani 1 1 d . . . H17A H 0.6586 0.5435 0.9260 0.048 Uiso 1 1 calc R . . C18 C 0.5062(8) 0.5401(6) 0.8775(7) 0.034(3) Uani 1 1 d . . . C19 C 0.4257(8) 0.4906(5) 0.8584(7) 0.030(2) Uani 1 1 d . . . H19A H 0.3607 0.5092 0.8380 0.035 Uiso 1 1 calc R . . C20 C 0.4402(8) 0.4152(5) 0.8692(7) 0.031(3) Uani 1 1 d . . . C21 C 0.5377(8) 0.3869(6) 0.9005(7) 0.037(3) Uani 1 1 d . . . H21A H 0.5486 0.3361 0.9068 0.044 Uiso 1 1 calc R . . C22 C 0.7232(8) 0.4062(6) 0.9560(8) 0.036(3) Uani 1 1 d . . . C23 C 0.8434(9) 0.3286(6) 0.9599(9) 0.051(3) Uani 1 1 d . . . H23A H 0.8803 0.3237 0.9140 0.062 Uiso 1 1 calc R . . H23B H 0.8466 0.2820 0.9944 0.062 Uiso 1 1 calc R . . C24 C 0.8858(8) 0.3894(6) 1.0315(9) 0.046(3) Uani 1 1 d . . . H24A H 0.9333 0.4186 1.0115 0.055 Uiso 1 1 calc R . . H24B H 0.9191 0.3700 1.0975 0.055 Uiso 1 1 calc R . . C25 C 0.4921(8) 0.6187(6) 0.8562(8) 0.034(3) Uani 1 1 d . . . C26 C 0.5446(9) 0.7378(6) 0.8736(10) 0.054(3) Uani 1 1 d . . . H26A H 0.5963 0.7589 0.8512 0.065 Uiso 1 1 calc R . . H26B H 0.5355 0.7691 0.9249 0.065 Uiso 1 1 calc R . . C27 C 0.4479(8) 0.7284(6) 0.7888(9) 0.043(3) Uani 1 1 d . . . H27A H 0.3964 0.7606 0.7973 0.052 Uiso 1 1 calc R . . H27B H 0.4572 0.7404 0.7264 0.052 Uiso 1 1 calc R . . C28 C 0.3552(8) 0.3631(6) 0.8484(7) 0.030(2) Uani 1 1 d . . . C29 C 0.2881(10) 0.2494(6) 0.8267(10) 0.062(4) Uani 1 1 d . . . H29A H 0.2941 0.2212 0.8861 0.074 Uiso 1 1 calc R . . H29B H 0.2744 0.2155 0.7712 0.074 Uiso 1 1 calc R . . C30 C 0.2063(9) 0.3066(6) 0.8077(9) 0.049(3) Uani 1 1 d . . . H30A H 0.1647 0.3077 0.7384 0.059 Uiso 1 1 calc R . . H30B H 0.1644 0.2977 0.8480 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0359(6) 0.0451(5) 0.0403(6) -0.0056(5) 0.0041(4) 0.0036(4) Ag2 0.0431(6) 0.0459(6) 0.0495(6) -0.0106(5) 0.0154(5) 0.0016(4) B1 0.072(13) 0.064(11) 0.042(11) -0.002(9) 0.016(9) 0.002(9) B2 0.094(16) 0.072(13) 0.076(15) -0.002(11) 0.044(13) 0.047(12) F1 0.131(10) 0.094(7) 0.233(13) -0.044(7) 0.138(10) -0.039(6) F2 0.165(11) 0.114(8) 0.067(6) 0.009(6) -0.008(7) 0.033(7) F3 0.074(6) 0.061(5) 0.064(5) 0.006(4) 0.018(4) -0.008(4) F4 0.121(8) 0.074(5) 0.068(6) -0.026(5) 0.042(5) -0.020(5) F5 0.093(8) 0.174(10) 0.205(12) 0.127(9) 0.097(9) 0.066(7) F6 0.058(6) 0.134(8) 0.127(8) -0.010(7) 0.025(6) 0.030(5) F7 0.162(13) 0.129(10) 0.195(13) -0.053(9) 0.063(11) 0.013(9) F8 0.101(9) 0.210(11) 0.123(9) 0.085(9) 0.060(7) 0.078(8) O1 0.028(5) 0.086(6) 0.034(5) -0.015(4) 0.007(4) -0.003(4) O2 0.047(6) 0.064(6) 0.073(6) -0.036(5) 0.035(5) -0.017(4) O3 0.035(5) 0.058(5) 0.043(5) -0.023(4) 0.009(4) 0.003(4) O4 0.028(5) 0.048(5) 0.045(5) -0.016(4) 0.004(4) 0.007(4) O5 0.030(5) 0.040(5) 0.067(6) -0.001(4) -0.010(4) -0.009(4) O6 0.041(5) 0.024(4) 0.076(6) -0.010(4) 0.016(5) -0.002(3) N1 0.034(6) 0.061(6) 0.023(5) -0.014(5) 0.006(5) -0.008(5) N2 0.028(5) 0.056(6) 0.035(6) 0.007(5) 0.014(5) 0.008(5) N3 0.027(6) 0.043(5) 0.035(6) -0.006(5) 0.005(5) -0.007(4) N4 0.032(6) 0.026(5) 0.034(5) 0.000(4) 0.000(5) 0.011(4) N5 0.040(6) 0.032(5) 0.032(5) 0.003(4) 0.006(5) 0.009(4) N6 0.027(5) 0.038(5) 0.029(5) -0.013(4) 0.004(4) -0.011(4) C1 0.022(6) 0.035(6) 0.033(7) 0.004(5) 0.005(5) -0.009(5) C2 0.033(7) 0.030(6) 0.024(6) 0.007(5) -0.008(5) -0.002(5) C3 0.021(6) 0.038(6) 0.039(7) 0.002(5) 0.005(5) -0.002(5) C4 0.030(7) 0.034(6) 0.046(7) 0.001(6) 0.012(6) 0.002(5) C5 0.030(7) 0.029(6) 0.020(6) 0.005(5) 0.001(5) -0.001(5) C6 0.033(7) 0.030(6) 0.030(6) 0.006(5) 0.001(5) -0.003(5) C7 0.030(7) 0.025(6) 0.050(8) 0.011(6) 0.015(6) -0.003(5) C8 0.041(8) 0.088(10) 0.044(8) -0.022(7) 0.018(7) -0.013(7) C9 0.048(9) 0.111(12) 0.047(9) 0.003(8) 0.025(8) 0.003(8) C10 0.035(7) 0.041(7) 0.034(7) -0.007(6) 0.007(6) -0.007(5) C11 0.038(8) 0.066(9) 0.065(10) -0.009(8) 0.003(7) -0.003(6) C12 0.025(7) 0.062(8) 0.082(10) -0.001(8) 0.022(7) -0.008(6) C13 0.042(7) 0.025(6) 0.030(7) 0.003(5) 0.023(6) -0.004(5) C14 0.054(9) 0.049(7) 0.038(7) -0.009(6) 0.016(6) -0.003(6) C15 0.040(8) 0.058(8) 0.046(8) -0.011(7) 0.009(6) -0.008(6) C16 0.019(6) 0.037(6) 0.030(6) -0.004(5) -0.006(5) 0.005(5) C17 0.035(7) 0.048(7) 0.034(7) -0.009(6) 0.007(6) -0.008(5) C18 0.037(7) 0.033(6) 0.027(6) 0.001(5) 0.006(5) -0.006(5) C19 0.027(6) 0.040(6) 0.018(6) -0.008(5) 0.003(5) 0.004(5) C20 0.032(7) 0.037(6) 0.016(6) -0.008(5) -0.002(5) 0.006(5) C21 0.041(7) 0.031(6) 0.030(6) 0.000(5) -0.001(6) -0.007(5) C22 0.033(7) 0.034(6) 0.041(7) -0.004(6) 0.013(6) -0.004(5) C23 0.054(9) 0.038(7) 0.065(9) -0.010(7) 0.023(7) 0.003(6) C24 0.022(6) 0.047(7) 0.062(8) -0.017(7) 0.005(6) 0.000(5) C25 0.035(7) 0.037(7) 0.038(7) -0.004(6) 0.021(6) -0.006(5) C26 0.051(9) 0.030(7) 0.084(10) -0.004(7) 0.027(8) -0.005(6) C27 0.029(7) 0.041(7) 0.052(8) 0.009(6) 0.003(6) -0.003(5) C28 0.030(7) 0.042(7) 0.016(6) 0.002(5) 0.004(5) -0.006(5) C29 0.064(10) 0.041(8) 0.079(10) -0.003(7) 0.021(8) -0.018(7) C30 0.040(8) 0.043(7) 0.063(9) -0.017(6) 0.017(7) -0.016(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 2.237(9) . ? Ag1 N3 2.241(9) 3_566 ? Ag1 N5 2.315(9) . ? Ag2 N4 2.167(8) 3_667 ? Ag2 N6 2.200(9) . ? Ag2 N1 2.438(9) . ? B1 F4 1.331(17) . ? B1 F1 1.359(18) . ? B1 F2 1.366(18) . ? B1 F3 1.395(17) . ? B2 F5 1.30(2) . ? B2 F6 1.329(16) . ? B2 F8 1.333(19) . ? B2 F7 1.41(2) . ? O1 C7 1.352(12) . ? O1 C8 1.455(12) . ? O2 C10 1.357(12) . ? O2 C11 1.460(13) . ? O3 C13 1.350(11) . ? O3 C14 1.443(12) . ? O4 C22 1.313(11) . ? O4 C23 1.446(13) . ? O5 C25 1.354(12) . ? O5 C26 1.471(12) . ? O6 C28 1.357(12) . ? O6 C29 1.472(13) . ? N1 C7 1.265(13) . ? N1 C9 1.504(14) . ? N2 C10 1.281(13) . ? N2 C12 1.488(13) . ? N3 C13 1.260(12) . ? N3 C15 1.486(13) . ? N3 Ag1 2.241(9) 3_566 ? N4 C22 1.301(13) . ? N4 C24 1.492(12) . ? N4 Ag2 2.167(8) 3_667 ? N5 C25 1.271(13) . ? N5 C27 1.479(12) . ? N6 C28 1.243(12) . ? N6 C30 1.505(12) . ? C1 C2 1.372(13) . ? C1 C6 1.406(13) . ? C1 C7 1.472(14) . ? C2 C3 1.399(14) . ? C2 H2A 0.9300 . ? C3 C4 1.384(14) . ? C3 C10 1.472(14) . ? C4 C5 1.360(13) . ? C4 H4B 0.9300 . ? C5 C6 1.369(14) . ? C5 C13 1.490(14) . ? C6 H6A 0.9300 . ? C8 C9 1.505(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.484(16) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.515(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.382(14) . ? C16 C21 1.407(14) . ? C16 C22 1.489(14) . ? C17 C18 1.403(14) . ? C17 H17A 0.9300 . ? C18 C19 1.401(13) . ? C18 C25 1.452(14) . ? C19 C20 1.380(13) . ? C19 H19A 0.9300 . ? C20 C21 1.398(14) . ? C20 C28 1.477(14) . ? C21 H21A 0.9300 . ? C23 C24 1.486(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C26 C27 1.505(15) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 C30 1.508(16) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 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 N2 Ag1 N3 144.5(3) . 3_566 ? N2 Ag1 N5 107.1(3) . . ? N3 Ag1 N5 107.4(3) 3_566 . ? N4 Ag2 N6 143.9(3) 3_667 . ? N4 Ag2 N1 105.0(3) 3_667 . ? N6 Ag2 N1 111.1(3) . . ? F4 B1 F1 111.7(14) . . ? F4 B1 F2 109.8(14) . . ? F1 B1 F2 108.5(14) . . ? F4 B1 F3 112.9(13) . . ? F1 B1 F3 107.1(13) . . ? F2 B1 F3 106.6(13) . . ? F5 B2 F6 114.2(17) . . ? F5 B2 F8 112.3(17) . . ? F6 B2 F8 113.7(15) . . ? F5 B2 F7 104.7(15) . . ? F6 B2 F7 105.9(18) . . ? F8 B2 F7 104.9(16) . . ? C7 O1 C8 106.0(8) . . ? C10 O2 C11 105.7(9) . . ? C13 O3 C14 105.8(9) . . ? C22 O4 C23 105.0(8) . . ? C25 O5 C26 106.3(8) . . ? C28 O6 C29 104.7(8) . . ? C7 N1 C9 106.7(10) . . ? C7 N1 Ag2 134.1(8) . . ? C9 N1 Ag2 116.9(7) . . ? C10 N2 C12 105.9(9) . . ? C10 N2 Ag1 131.0(8) . . ? C12 N2 Ag1 118.6(7) . . ? C13 N3 C15 107.1(9) . . ? C13 N3 Ag1 136.6(7) . 3_566 ? C15 N3 Ag1 115.7(7) . 3_566 ? C22 N4 C24 104.5(8) . . ? C22 N4 Ag2 135.3(7) . 3_667 ? C24 N4 Ag2 120.0(7) . 3_667 ? C25 N5 C27 106.1(9) . . ? C25 N5 Ag1 131.4(7) . . ? C27 N5 Ag1 122.1(6) . . ? C28 N6 C30 108.7(9) . . ? C28 N6 Ag2 134.6(7) . . ? C30 N6 Ag2 115.9(7) . . ? C2 C1 C6 120.0(10) . . ? C2 C1 C7 120.3(10) . . ? C6 C1 C7 119.7(9) . . ? C1 C2 C3 120.4(10) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 118.7(10) . . ? C4 C3 C10 121.5(10) . . ? C2 C3 C10 119.8(10) . . ? C5 C4 C3 120.6(10) . . ? C5 C4 H4B 119.7 . . ? C3 C4 H4B 119.7 . . ? C4 C5 C6 121.7(10) . . ? C4 C5 C13 118.8(9) . . ? C6 C5 C13 119.5(10) . . ? C5 C6 C1 118.6(10) . . ? C5 C6 H6A 120.7 . . ? C1 C6 H6A 120.7 . . ? N1 C7 O1 118.2(10) . . ? N1 C7 C1 127.2(10) . . ? O1 C7 C1 114.5(10) . . ? O1 C8 C9 105.1(9) . . ? O1 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? O1 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? N1 C9 C8 103.9(10) . . ? N1 C9 H9A 111.0 . . ? C8 C9 H9A 111.0 . . ? N1 C9 H9B 111.0 . . ? C8 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N2 C10 O2 117.0(10) . . ? N2 C10 C3 128.2(10) . . ? O2 C10 C3 114.8(9) . . ? O2 C11 C12 103.8(10) . . ? O2 C11 H11A 111.0 . . ? C12 C11 H11A 111.0 . . ? O2 C11 H11B 111.0 . . ? C12 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? C11 C12 N2 104.9(9) . . ? C11 C12 H12A 110.8 . . ? N2 C12 H12A 110.8 . . ? C11 C12 H12B 110.8 . . ? N2 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? N3 C13 O3 118.2(10) . . ? N3 C13 C5 127.6(9) . . ? O3 C13 C5 114.2(10) . . ? O3 C14 C15 105.1(9) . . ? O3 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? O3 C14 H14B 110.7 . . ? C15 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? N3 C15 C14 103.5(9) . . ? N3 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? N3 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.0 . . ? C17 C16 C21 120.9(10) . . ? C17 C16 C22 119.7(10) . . ? C21 C16 C22 119.4(9) . . ? C16 C17 C18 120.0(10) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 118.5(10) . . ? C19 C18 C25 122.5(10) . . ? C17 C18 C25 118.8(10) . . ? C20 C19 C18 121.8(10) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 119.4(10) . . ? C19 C20 C28 121.7(9) . . ? C21 C20 C28 118.9(9) . . ? C20 C21 C16 119.3(10) . . ? C20 C21 H21A 120.4 . . ? C16 C21 H21A 120.4 . . ? N4 C22 O4 119.4(10) . . ? N4 C22 C16 123.6(10) . . ? O4 C22 C16 116.9(9) . . ? O4 C23 C24 105.9(8) . . ? O4 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? O4 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? C23 C24 N4 103.9(9) . . ? C23 C24 H24A 111.0 . . ? N4 C24 H24A 111.0 . . ? C23 C24 H24B 111.0 . . ? N4 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? N5 C25 O5 118.0(9) . . ? N5 C25 C18 127.5(10) . . ? O5 C25 C18 114.3(10) . . ? O5 C26 C27 103.1(8) . . ? O5 C26 H26A 111.1 . . ? C27 C26 H26A 111.1 . . ? O5 C26 H26B 111.1 . . ? C27 C26 H26B 111.1 . . ? H26A C26 H26B 109.1 . . ? N5 C27 C26 105.9(9) . . ? N5 C27 H27A 110.6 . . ? C26 C27 H27A 110.6 . . ? N5 C27 H27B 110.6 . . ? C26 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? N6 C28 O6 117.7(9) . . ? N6 C28 C20 128.6(10) . . ? O6 C28 C20 113.7(9) . . ? O6 C29 C30 105.2(9) . . ? O6 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? O6 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? N6 C30 C29 101.6(9) . . ? N6 C30 H30A 111.5 . . ? C29 C30 H30A 111.5 . . ? N6 C30 H30B 111.5 . . ? C29 C30 H30B 111.5 . . ? H30A C30 H30B 109.3 . . ? 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 N4 Ag2 N1 C7 155.0(10) 3_667 . . . ? N6 Ag2 N1 C7 -23.0(11) . . . . ? N4 Ag2 N1 C9 -44.9(9) 3_667 . . . ? N6 Ag2 N1 C9 137.0(8) . . . . ? N3 Ag1 N2 C10 7.6(12) 3_566 . . . ? N5 Ag1 N2 C10 173.6(9) . . . . ? N3 Ag1 N2 C12 160.1(7) 3_566 . . . ? N5 Ag1 N2 C12 -33.9(8) . . . . ? N2 Ag1 N5 C25 -39.3(10) . . . . ? N3 Ag1 N5 C25 132.2(9) 3_566 . . . ? N2 Ag1 N5 C27 132.2(8) . . . . ? N3 Ag1 N5 C27 -56.3(8) 3_566 . . . ? N4 Ag2 N6 C28 -25.2(13) 3_667 . . . ? N1 Ag2 N6 C28 151.6(10) . . . . ? N4 Ag2 N6 C30 143.2(7) 3_667 . . . ? N1 Ag2 N6 C30 -39.9(8) . . . . ? C6 C1 C2 C3 -1.2(15) . . . . ? C7 C1 C2 C3 176.4(9) . . . . ? C1 C2 C3 C4 -0.7(15) . . . . ? C1 C2 C3 C10 177.5(9) . . . . ? C2 C3 C4 C5 2.4(15) . . . . ? C10 C3 C4 C5 -175.8(10) . . . . ? C3 C4 C5 C6 -2.2(15) . . . . ? C3 C4 C5 C13 176.9(9) . . . . ? C4 C5 C6 C1 0.3(15) . . . . ? C13 C5 C6 C1 -178.8(9) . . . . ? C2 C1 C6 C5 1.4(14) . . . . ? C7 C1 C6 C5 -176.2(9) . . . . ? C9 N1 C7 O1 2.2(13) . . . . ? Ag2 N1 C7 O1 163.7(7) . . . . ? C9 N1 C7 C1 178.2(10) . . . . ? Ag2 N1 C7 C1 -20.3(17) . . . . ? C8 O1 C7 N1 -2.8(13) . . . . ? C8 O1 C7 C1 -179.4(9) . . . . ? C2 C1 C7 N1 -11.6(16) . . . . ? C6 C1 C7 N1 166.0(10) . . . . ? C2 C1 C7 O1 164.6(9) . . . . ? C6 C1 C7 O1 -17.9(13) . . . . ? C7 O1 C8 C9 2.1(13) . . . . ? C7 N1 C9 C8 -0.5(13) . . . . ? Ag2 N1 C9 C8 -165.7(8) . . . . ? O1 C8 C9 N1 -1.0(14) . . . . ? C12 N2 C10 O2 -2.6(13) . . . . ? Ag1 N2 C10 O2 152.4(8) . . . . ? C12 N2 C10 C3 177.2(11) . . . . ? Ag1 N2 C10 C3 -27.8(17) . . . . ? C11 O2 C10 N2 -8.0(14) . . . . ? C11 O2 C10 C3 172.2(10) . . . . ? C4 C3 C10 N2 163.7(11) . . . . ? C2 C3 C10 N2 -14.5(17) . . . . ? C4 C3 C10 O2 -16.5(15) . . . . ? C2 C3 C10 O2 165.3(9) . . . . ? C10 O2 C11 C12 14.6(12) . . . . ? O2 C11 C12 N2 -15.9(12) . . . . ? C10 N2 C12 C11 11.9(12) . . . . ? Ag1 N2 C12 C11 -146.9(8) . . . . ? C15 N3 C13 O3 2.0(12) . . . . ? Ag1 N3 C13 O3 -168.5(7) 3_566 . . . ? C15 N3 C13 C5 -178.4(9) . . . . ? Ag1 N3 C13 C5 11.1(17) 3_566 . . . ? C14 O3 C13 N3 -5.3(12) . . . . ? C14 O3 C13 C5 175.1(8) . . . . ? C4 C5 C13 N3 -155.9(10) . . . . ? C6 C5 C13 N3 23.3(15) . . . . ? C4 C5 C13 O3 23.8(13) . . . . ? C6 C5 C13 O3 -157.1(9) . . . . ? C13 O3 C14 C15 5.9(11) . . . . ? C13 N3 C15 C14 2.0(11) . . . . ? Ag1 N3 C15 C14 174.8(7) 3_566 . . . ? O3 C14 C15 N3 -4.8(11) . . . . ? C21 C16 C17 C18 -0.1(16) . . . . ? C22 C16 C17 C18 178.7(10) . . . . ? C16 C17 C18 C19 1.8(16) . . . . ? C16 C17 C18 C25 -173.4(10) . . . . ? C17 C18 C19 C20 -1.9(15) . . . . ? C25 C18 C19 C20 173.1(10) . . . . ? C18 C19 C20 C21 0.3(15) . . . . ? C18 C19 C20 C28 -179.5(9) . . . . ? C19 C20 C21 C16 1.3(15) . . . . ? C28 C20 C21 C16 -178.8(9) . . . . ? C17 C16 C21 C20 -1.5(16) . . . . ? C22 C16 C21 C20 179.8(9) . . . . ? C24 N4 C22 O4 1.6(13) . . . . ? Ag2 N4 C22 O4 176.4(7) 3_667 . . . ? C24 N4 C22 C16 -177.1(10) . . . . ? Ag2 N4 C22 C16 -2.3(17) 3_667 . . . ? C23 O4 C22 N4 5.3(13) . . . . ? C23 O4 C22 C16 -175.9(9) . . . . ? C17 C16 C22 N4 44.2(16) . . . . ? C21 C16 C22 N4 -136.9(11) . . . . ? C17 C16 C22 O4 -134.5(10) . . . . ? C21 C16 C22 O4 44.4(14) . . . . ? C22 O4 C23 C24 -9.7(12) . . . . ? O4 C23 C24 N4 10.5(12) . . . . ? C22 N4 C24 C23 -7.5(12) . . . . ? Ag2 N4 C24 C23 176.7(7) 3_667 . . . ? C27 N5 C25 O5 3.7(13) . . . . ? Ag1 N5 C25 O5 176.2(7) . . . . ? C27 N5 C25 C18 -171.5(10) . . . . ? Ag1 N5 C25 C18 1.0(17) . . . . ? C26 O5 C25 N5 0.9(13) . . . . ? C26 O5 C25 C18 176.7(9) . . . . ? C19 C18 C25 N5 -27.4(17) . . . . ? C17 C18 C25 N5 147.6(11) . . . . ? C19 C18 C25 O5 157.3(10) . . . . ? C17 C18 C25 O5 -27.7(14) . . . . ? C25 O5 C26 C27 -4.8(12) . . . . ? C25 N5 C27 C26 -6.5(12) . . . . ? Ag1 N5 C27 C26 -179.9(7) . . . . ? O5 C26 C27 N5 6.8(12) . . . . ? C30 N6 C28 O6 -4.8(13) . . . . ? Ag2 N6 C28 O6 164.2(7) . . . . ? C30 N6 C28 C20 174.5(10) . . . . ? Ag2 N6 C28 C20 -16.5(17) . . . . ? C29 O6 C28 N6 -5.0(13) . . . . ? C29 O6 C28 C20 175.6(9) . . . . ? C19 C20 C28 N6 -14.6(17) . . . . ? C21 C20 C28 N6 165.5(10) . . . . ? C19 C20 C28 O6 164.7(9) . . . . ? C21 C20 C28 O6 -15.1(13) . . . . ? C28 O6 C29 C30 12.2(12) . . . . ? C28 N6 C30 C29 12.0(12) . . . . ? Ag2 N6 C30 C29 -159.4(7) . . . . ? O6 C29 C30 N6 -14.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.773 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.129 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 644136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ag3(L)2(NO3)2]NO3-5(H2O) ; _chemical_name_common (Ag3(L)2(NO3)2)NO3-5(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C30 H40 Ag3 N9 O20' _chemical_formula_sum 'C30 H40 Ag3 N9 O20' _chemical_formula_weight 1170.32 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.323(3) _cell_length_b 13.128(3) _cell_length_c 14.870(4) _cell_angle_alpha 73.928(6) _cell_angle_beta 72.712(5) _cell_angle_gamma 86.275(7) _cell_volume 2027.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1037 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 17.37 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6171 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Brucker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10090 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.2166 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7011 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7011 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1680 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.00483(10) 0.27515(7) 0.29530(7) 0.0538(3) Uani 1 1 d . . . Ag2 Ag 0.27754(9) 0.60068(7) -0.25018(7) 0.0473(3) Uani 1 1 d . . . Ag3 Ag 0.29673(9) 0.41107(7) 0.30912(7) 0.0506(3) Uani 1 1 d . . . O1 O 0.2531(7) 0.3719(6) 0.0018(5) 0.045(2) Uani 1 1 d . . . O2 O -0.1842(7) 0.7315(6) 0.1833(5) 0.052(2) Uani 1 1 d . . . O3 O 0.1889(7) 0.8521(6) -0.1029(5) 0.053(2) Uani 1 1 d . . . O4 O -0.2331(7) 0.3463(6) 0.5568(5) 0.044(2) Uani 1 1 d . . . O5 O -0.1729(7) 0.8392(6) 0.4198(5) 0.052(2) Uani 1 1 d . . . O6 O 0.1872(7) 0.7326(5) 0.1901(5) 0.050(2) Uani 1 1 d . . . O7 O -0.0361(10) 0.0789(8) 0.2841(9) 0.106(4) Uani 1 1 d . . . O8 O 0.0997(12) -0.0467(8) 0.2913(9) 0.127(6) Uani 1 1 d . . . O9 O 0.0885(13) 0.0731(10) 0.3647(9) 0.124(5) Uani 1 1 d . . . O10 O 0.3943(9) 0.7099(8) -0.4128(6) 0.085(4) Uani 1 1 d . . . O11 O 0.5173(9) 0.5813(8) -0.4083(8) 0.096(4) Uani 1 1 d . . . O12 O 0.5528(8) 0.7201(7) -0.5321(6) 0.065(3) Uani 1 1 d . . . O14 O 0.3964(10) 0.2995(9) 0.1997(8) 0.100(4) Uani 1 1 d . . . O15 O 0.5640(8) 0.2988(8) 0.0890(7) 0.079(3) Uani 1 1 d . . . O16 O 0.5278(9) 0.4209(8) 0.1657(9) 0.094(4) Uani 1 1 d . . . O17 O 0.4801(8) 0.9450(7) -0.5649(7) 0.093(3) Uani 1 1 d . . . O18 O -0.3731(10) 0.0130(7) 0.7133(8) 0.117(4) Uani 1 1 d . . . O19 O 0.4897(11) 0.0858(10) 0.1052(10) 0.165(6) Uani 1 1 d . . . O20 O 0.3415(18) 0.0360(10) -0.0176(13) 0.261(10) Uani 1 1 d . . . O21 O 0.0785(15) -0.0103(16) 0.0668(17) 0.346(15) Uani 1 1 d . . . N1 N 0.1319(8) 0.3022(7) 0.1519(6) 0.041(3) Uani 1 1 d . . . N2 N -0.2483(8) 0.5654(7) 0.2364(6) 0.037(3) Uani 1 1 d . . . N3 N 0.2409(8) 0.7451(7) -0.2023(7) 0.043(3) Uani 1 1 d . . . N4 N -0.1126(8) 0.2898(7) 0.4337(6) 0.040(3) Uani 1 1 d . . . N5 N -0.2455(9) 0.7276(7) 0.5685(7) 0.044(3) Uani 1 1 d . . . N6 N 0.2672(8) 0.5708(6) 0.2325(6) 0.042(3) Uani 1 1 d . . . N7 N 0.0492(13) 0.0315(11) 0.3130(10) 0.071(4) Uani 1 1 d . . . N8 N 0.4876(11) 0.6693(9) -0.4496(9) 0.060(4) Uani 1 1 d . . . N9 N 0.4960(10) 0.3386(11) 0.1496(9) 0.062(4) Uani 1 1 d . . . C1 C 0.1618(11) 0.3834(10) 0.0798(8) 0.042(3) Uani 1 1 d . . . C2 C 0.2941(10) 0.2631(9) 0.0243(8) 0.047(4) Uani 1 1 d . . . H2B H 0.3790 0.2598 0.0267 0.057 Uiso 1 1 calc R . . H2C H 0.2872 0.2279 -0.0233 0.057 Uiso 1 1 calc R . . C3 C 0.2050(11) 0.2147(9) 0.1244(9) 0.050(4) Uani 1 1 d . . . H3A H 0.1524 0.1610 0.1214 0.061 Uiso 1 1 calc R . . H3B H 0.2498 0.1825 0.1713 0.061 Uiso 1 1 calc R . . C4 C -0.1677(11) 0.6307(9) 0.1850(8) 0.029(3) Uani 1 1 d . . . C5 C -0.3032(11) 0.7359(9) 0.2515(8) 0.054(4) Uani 1 1 d . . . H5B H -0.3582 0.7813 0.2195 0.065 Uiso 1 1 calc R . . H5C H -0.2960 0.7620 0.3046 0.065 Uiso 1 1 calc R . . C6 C -0.3503(10) 0.6207(9) 0.2889(9) 0.053(4) Uani 1 1 d . . . H6A H -0.3650 0.5944 0.3591 0.064 Uiso 1 1 calc R . . H6B H -0.4258 0.6133 0.2731 0.064 Uiso 1 1 calc R . . C7 C 0.1881(10) 0.7564(8) -0.1172(8) 0.033(3) Uani 1 1 d . . . C8 C 0.2559(11) 0.9203(9) -0.1984(8) 0.053(4) Uani 1 1 d . . . H8A H 0.3256 0.9559 -0.1940 0.064 Uiso 1 1 calc R . . H8B H 0.2019 0.9732 -0.2243 0.064 Uiso 1 1 calc R . . C9 C 0.2990(12) 0.8453(8) -0.2614(8) 0.057(4) Uani 1 1 d . . . H9A H 0.2739 0.8692 -0.3206 0.069 Uiso 1 1 calc R . . H9B H 0.3884 0.8399 -0.2792 0.069 Uiso 1 1 calc R . . C10 C 0.1125(10) 0.4907(8) 0.0655(8) 0.025(3) Uani 1 1 d . . . C11 C 0.0027(10) 0.5117(8) 0.1292(7) 0.031(3) Uani 1 1 d . . . H11A H -0.0391 0.4572 0.1820 0.038 Uiso 1 1 calc R . . C12 C -0.0462(10) 0.6127(8) 0.1158(7) 0.027(3) Uani 1 1 d . . . C13 C 0.0176(10) 0.6932(9) 0.0353(7) 0.035(3) Uani 1 1 d . . . H13A H -0.0123 0.7618 0.0260 0.042 Uiso 1 1 calc R . . C14 C 0.1201(11) 0.6727(8) -0.0278(8) 0.039(3) Uani 1 1 d . . . C15 C 0.1739(10) 0.5721(8) -0.0144(7) 0.033(3) Uani 1 1 d . . . H15A H 0.2484 0.5602 -0.0576 0.040 Uiso 1 1 calc R . . C16 C -0.1473(10) 0.3659(8) 0.4701(7) 0.027(3) Uani 1 1 d . . . C17 C -0.1803(11) 0.1935(8) 0.5035(8) 0.055(4) Uani 1 1 d . . . H17A H -0.1238 0.1418 0.5273 0.066 Uiso 1 1 calc R . . H17B H -0.2273 0.1614 0.4732 0.066 Uiso 1 1 calc R . . C18 C -0.2652(11) 0.2334(8) 0.5855(8) 0.050(4) Uani 1 1 d . . . H18A H -0.3513 0.2229 0.5908 0.060 Uiso 1 1 calc R . . H18B H -0.2503 0.1977 0.6475 0.060 Uiso 1 1 calc R . . C19 C -0.1845(10) 0.7409(9) 0.4788(8) 0.037(3) Uani 1 1 d . . . C20 C -0.2942(11) 0.8338(8) 0.5778(8) 0.048(4) Uani 1 1 d . . . H20A H -0.2722 0.8528 0.6294 0.057 Uiso 1 1 calc R . . H20B H -0.3834 0.8351 0.5913 0.057 Uiso 1 1 calc R . . C21 C -0.2311(12) 0.9083(9) 0.4780(9) 0.064(4) Uani 1 1 d . . . H21A H -0.2912 0.9519 0.4507 0.076 Uiso 1 1 calc R . . H21B H -0.1706 0.9540 0.4828 0.076 Uiso 1 1 calc R . . C22 C 0.1791(10) 0.6279(9) 0.2478(7) 0.030(3) Uani 1 1 d . . . C23 C 0.3122(10) 0.7413(8) 0.1248(8) 0.047(4) Uani 1 1 d . . . H23A H 0.3616 0.7909 0.1369 0.056 Uiso 1 1 calc R . . H23B H 0.3118 0.7650 0.0570 0.056 Uiso 1 1 calc R . . C24 C 0.3625(10) 0.6308(9) 0.1475(8) 0.050(4) Uani 1 1 d . . . H24A H 0.3757 0.6008 0.0927 0.060 Uiso 1 1 calc R . . H24B H 0.4401 0.6313 0.1625 0.060 Uiso 1 1 calc R . . C25 C -0.0999(10) 0.4773(8) 0.4305(8) 0.028(3) Uani 1 1 d . . . C26 C -0.1640(10) 0.5553(8) 0.4667(7) 0.030(3) Uani 1 1 d . . . H26A H -0.2393 0.5386 0.5150 0.035 Uiso 1 1 calc R . . C27 C -0.1207(9) 0.6582(8) 0.4339(7) 0.024(3) Uani 1 1 d . . . C28 C -0.0123(9) 0.6836(8) 0.3581(7) 0.028(3) Uani 1 1 d . . . H28A H 0.0148 0.7539 0.3319 0.034 Uiso 1 1 calc R . . C29 C 0.0566(9) 0.6055(8) 0.3206(8) 0.026(3) Uani 1 1 d . . . C30 C 0.0122(9) 0.5027(8) 0.3572(7) 0.027(3) Uani 1 1 d . . . H30A H 0.0575 0.4495 0.3328 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0718(8) 0.0405(6) 0.0340(6) -0.0097(5) 0.0065(5) 0.0010(5) Ag2 0.0526(7) 0.0437(6) 0.0393(6) -0.0148(5) 0.0008(5) -0.0074(5) Ag3 0.0538(7) 0.0460(6) 0.0345(6) -0.0010(5) 0.0019(5) 0.0107(5) O1 0.050(6) 0.042(5) 0.035(5) -0.010(4) 0.000(4) 0.002(4) O2 0.074(7) 0.037(5) 0.034(5) -0.013(4) 0.003(5) 0.002(5) O3 0.077(7) 0.037(5) 0.034(5) -0.010(4) 0.001(5) 0.001(5) O4 0.042(5) 0.044(5) 0.035(5) -0.016(4) 0.012(4) -0.017(4) O5 0.067(6) 0.029(5) 0.036(5) 0.007(4) 0.005(4) -0.005(4) O6 0.058(6) 0.028(5) 0.038(5) 0.000(4) 0.019(4) -0.007(4) O7 0.084(10) 0.079(8) 0.148(12) -0.002(8) -0.046(8) -0.019(7) O8 0.143(12) 0.050(7) 0.148(12) -0.016(7) -0.003(9) 0.032(7) O9 0.173(14) 0.111(11) 0.118(12) -0.036(9) -0.083(10) 0.012(9) O10 0.070(7) 0.142(9) 0.021(5) -0.011(6) 0.004(5) 0.033(7) O11 0.053(7) 0.072(7) 0.160(12) -0.025(8) -0.029(7) -0.009(6) O12 0.052(6) 0.098(7) 0.033(6) -0.027(5) 0.019(5) -0.020(5) O14 0.060(8) 0.128(9) 0.106(9) -0.054(8) 0.007(7) -0.006(7) O15 0.051(7) 0.127(9) 0.057(7) -0.043(6) 0.003(5) 0.009(6) O16 0.061(8) 0.069(7) 0.152(11) -0.042(7) -0.021(7) 0.012(6) O17 0.087(8) 0.076(7) 0.132(10) -0.033(6) -0.051(7) 0.006(6) O18 0.138(11) 0.083(8) 0.123(10) -0.017(7) -0.043(8) 0.018(7) O19 0.098(10) 0.167(12) 0.216(16) -0.054(11) -0.024(10) 0.006(9) O20 0.46(3) 0.134(13) 0.32(2) -0.137(14) -0.25(2) 0.100(16) O21 0.245(19) 0.49(3) 0.61(4) -0.52(3) -0.28(2) 0.26(2) N1 0.046(7) 0.044(6) 0.021(6) -0.002(5) 0.006(5) -0.007(5) N2 0.027(6) 0.053(6) 0.032(6) -0.029(5) 0.009(5) -0.012(5) N3 0.041(7) 0.046(6) 0.034(6) -0.012(5) 0.002(5) -0.011(5) N4 0.039(7) 0.033(6) 0.039(6) -0.012(5) 0.005(5) -0.005(5) N5 0.054(7) 0.036(6) 0.042(7) -0.019(5) -0.005(6) 0.001(5) N6 0.033(6) 0.029(6) 0.027(6) 0.012(4) 0.024(5) 0.009(5) N7 0.062(11) 0.065(11) 0.057(10) 0.025(8) -0.009(8) -0.012(8) N8 0.053(9) 0.045(8) 0.077(10) -0.024(7) -0.009(8) 0.008(7) N9 0.013(7) 0.094(10) 0.074(10) -0.033(8) 0.006(6) -0.003(7) C1 0.036(8) 0.067(9) 0.021(7) -0.025(7) 0.008(6) -0.008(7) C2 0.045(9) 0.054(8) 0.034(8) -0.021(6) 0.007(6) 0.013(7) C3 0.057(9) 0.037(8) 0.055(9) -0.018(7) -0.008(7) -0.003(7) C4 0.039(8) 0.036(7) 0.023(7) -0.022(6) -0.018(6) 0.025(6) C5 0.055(9) 0.064(9) 0.039(8) -0.028(7) 0.003(7) 0.024(7) C6 0.043(9) 0.051(8) 0.051(9) -0.011(7) 0.007(7) -0.005(7) C7 0.031(7) 0.028(7) 0.026(7) -0.007(6) 0.011(6) 0.001(6) C8 0.072(10) 0.054(9) 0.027(8) 0.002(7) -0.013(7) -0.011(7) C9 0.090(11) 0.031(7) 0.037(8) 0.003(6) -0.007(8) -0.016(7) C10 0.032(7) 0.023(6) 0.025(7) -0.008(5) -0.014(6) 0.000(5) C11 0.036(8) 0.039(7) 0.012(6) 0.005(5) -0.004(5) -0.018(6) C12 0.036(8) 0.036(7) 0.015(6) -0.010(5) -0.014(6) -0.001(6) C13 0.035(8) 0.055(8) 0.013(6) -0.018(6) 0.002(6) 0.001(6) C14 0.051(9) 0.032(7) 0.036(8) -0.012(6) -0.007(7) -0.020(6) C15 0.029(7) 0.046(8) 0.019(7) -0.011(6) 0.001(5) 0.008(6) C16 0.025(7) 0.033(7) 0.020(7) -0.008(5) -0.005(5) 0.003(6) C17 0.091(11) 0.022(7) 0.041(8) -0.009(6) 0.002(8) -0.016(7) C18 0.073(10) 0.030(7) 0.034(8) 0.000(6) -0.002(7) -0.016(7) C19 0.030(8) 0.038(7) 0.033(8) -0.009(6) 0.009(6) -0.008(6) C20 0.065(10) 0.035(7) 0.037(8) -0.017(6) -0.004(7) 0.020(7) C21 0.088(11) 0.039(8) 0.060(10) -0.032(7) -0.001(8) 0.017(8) C22 0.036(8) 0.043(7) 0.010(6) -0.012(5) 0.007(5) -0.025(6) C23 0.036(8) 0.051(8) 0.038(8) 0.002(6) 0.002(6) -0.015(7) C24 0.041(8) 0.050(8) 0.044(9) -0.005(7) 0.001(7) 0.005(7) C25 0.026(7) 0.029(7) 0.031(7) -0.011(6) -0.007(6) -0.002(6) C26 0.029(8) 0.036(7) 0.021(7) -0.003(5) -0.008(5) 0.001(6) C27 0.016(6) 0.029(6) 0.023(7) -0.005(5) -0.002(5) 0.006(5) C28 0.030(7) 0.032(7) 0.025(7) -0.005(5) -0.011(6) -0.008(6) C29 0.026(7) 0.029(6) 0.037(7) -0.013(6) -0.025(6) 0.008(5) C30 0.039(8) 0.026(6) 0.020(6) -0.013(5) -0.012(6) 0.011(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 N1 2.137(9) . ? Ag1 N4 2.145(9) . ? Ag2 N2 2.170(9) 2_565 ? Ag2 N3 2.179(9) . ? Ag2 O10 2.465(8) . ? Ag3 N6 2.150(8) . ? Ag3 N5 2.153(9) 2_566 ? Ag3 O14 2.466(10) . ? O1 C1 1.342(11) . ? O1 C2 1.451(11) . ? O2 C4 1.318(11) . ? O2 C5 1.435(11) . ? O3 C7 1.332(12) . ? O3 C8 1.462(11) . ? O4 C16 1.333(11) . ? O4 C18 1.462(11) . ? O5 C19 1.334(11) . ? O5 C21 1.422(12) . ? O6 C22 1.397(11) . ? O6 C23 1.450(11) . ? O7 N7 1.235(14) . ? O8 N7 1.218(16) . ? O9 N7 1.246(16) . ? O10 N8 1.202(12) . ? O11 N8 1.226(12) . ? O12 N8 1.253(12) . ? O14 N9 1.206(12) . ? O15 N9 1.214(12) . ? O16 N9 1.266(13) . ? N1 C1 1.265(12) . ? N1 C3 1.451(13) . ? N2 C4 1.216(12) . ? N2 C6 1.463(12) . ? N2 Ag2 2.170(9) 2_565 ? N3 C7 1.273(12) . ? N3 C9 1.437(12) . ? N4 C16 1.251(12) . ? N4 C17 1.480(11) . ? N5 C19 1.274(12) . ? N5 C20 1.493(12) . ? N5 Ag3 2.153(9) 2_566 ? N6 C22 1.213(12) . ? N6 C24 1.459(11) . ? C1 C10 1.464(15) . ? C2 C3 1.519(13) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C12 1.503(13) . ? C5 C6 1.531(14) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C14 1.504(13) . ? C8 C9 1.503(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.386(13) . ? C10 C15 1.392(12) . ? C11 C12 1.388(13) . ? C11 H11A 0.9300 . ? C12 C13 1.398(13) . ? C13 C14 1.324(13) . ? C13 H13A 0.9300 . ? C14 C15 1.406(13) . ? C15 H15A 0.9300 . ? C16 C25 1.486(13) . ? C17 C18 1.509(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C27 1.470(13) . ? C20 C21 1.525(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C29 1.472(13) . ? C23 C24 1.509(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.358(13) . ? C25 C30 1.393(12) . ? C26 C27 1.372(12) . ? C26 H26A 0.9300 . ? C27 C28 1.382(12) . ? C28 C29 1.388(13) . ? C28 H28A 0.9300 . ? C29 C30 1.375(12) . ? C30 H30A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N4 165.4(3) . . ? N2 Ag2 N3 154.0(3) 2_565 . ? N2 Ag2 O10 116.9(3) 2_565 . ? N3 Ag2 O10 88.2(3) . . ? N6 Ag3 N5 152.1(3) . 2_566 ? N6 Ag3 O14 113.5(3) . . ? N5 Ag3 O14 90.6(3) 2_566 . ? C1 O1 C2 107.8(8) . . ? C4 O2 C5 105.7(8) . . ? C7 O3 C8 104.7(9) . . ? C16 O4 C18 106.7(8) . . ? C19 O5 C21 107.5(8) . . ? C22 O6 C23 103.2(8) . . ? N8 O10 Ag2 113.3(9) . . ? N9 O14 Ag3 108.4(9) . . ? C1 N1 C3 107.7(9) . . ? C1 N1 Ag1 133.2(8) . . ? C3 N1 Ag1 119.0(7) . . ? C4 N2 C6 107.8(9) . . ? C4 N2 Ag2 134.1(8) . 2_565 ? C6 N2 Ag2 117.6(7) . 2_565 ? C7 N3 C9 106.7(10) . . ? C7 N3 Ag2 129.4(8) . . ? C9 N3 Ag2 122.6(7) . . ? C16 N4 C17 107.7(9) . . ? C16 N4 Ag1 134.5(8) . . ? C17 N4 Ag1 117.6(7) . . ? C19 N5 C20 106.0(9) . . ? C19 N5 Ag3 133.0(8) . 2_566 ? C20 N5 Ag3 120.7(7) . 2_566 ? C22 N6 C24 107.7(9) . . ? C22 N6 Ag3 130.8(7) . . ? C24 N6 Ag3 121.5(7) . . ? O8 N7 O7 125.7(18) . . ? O8 N7 O9 119.3(17) . . ? O7 N7 O9 114.9(17) . . ? O10 N8 O11 121.4(13) . . ? O10 N8 O12 117.3(12) . . ? O11 N8 O12 121.3(12) . . ? O14 N9 O15 121.6(15) . . ? O14 N9 O16 116.7(13) . . ? O15 N9 O16 121.7(12) . . ? N1 C1 O1 116.5(11) . . ? N1 C1 C10 130.8(10) . . ? O1 C1 C10 112.8(10) . . ? O1 C2 C3 102.3(8) . . ? O1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? O1 C2 H2C 111.3 . . ? C3 C2 H2C 111.3 . . ? H2B C2 H2C 109.2 . . ? N1 C3 C2 105.4(9) . . ? N1 C3 H3A 110.7 . . ? C2 C3 H3A 110.7 . . ? N1 C3 H3B 110.7 . . ? C2 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? N2 C4 O2 120.0(10) . . ? N2 C4 C12 127.7(10) . . ? O2 C4 C12 112.3(10) . . ? O2 C5 C6 103.8(8) . . ? O2 C5 H5B 111.0 . . ? C6 C5 H5B 111.0 . . ? O2 C5 H5C 111.0 . . ? C6 C5 H5C 111.0 . . ? H5B C5 H5C 109.0 . . ? N2 C6 C5 102.6(8) . . ? N2 C6 H6A 111.2 . . ? C5 C6 H6A 111.2 . . ? N2 C6 H6B 111.2 . . ? C5 C6 H6B 111.2 . . ? H6A C6 H6B 109.2 . . ? N3 C7 O3 118.7(9) . . ? N3 C7 C14 127.2(10) . . ? O3 C7 C14 114.0(9) . . ? O3 C8 C9 104.1(9) . . ? O3 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? O3 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 109.0 . . ? N3 C9 C8 105.1(9) . . ? N3 C9 H9A 110.7 . . ? C8 C9 H9A 110.7 . . ? N3 C9 H9B 110.7 . . ? C8 C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? C11 C10 C15 119.3(9) . . ? C11 C10 C1 120.6(9) . . ? C15 C10 C1 120.1(10) . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C11 C12 C13 118.3(10) . . ? C11 C12 C4 119.2(9) . . ? C13 C12 C4 122.4(10) . . ? C14 C13 C12 120.7(11) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 122.2(10) . . ? C13 C14 C7 122.0(10) . . ? C15 C14 C7 115.8(10) . . ? C10 C15 C14 118.1(9) . . ? C10 C15 H15A 120.9 . . ? C14 C15 H15A 120.9 . . ? N4 C16 O4 117.8(10) . . ? N4 C16 C25 127.8(10) . . ? O4 C16 C25 114.4(9) . . ? N4 C17 C18 104.1(8) . . ? N4 C17 H17A 110.9 . . ? C18 C17 H17A 110.9 . . ? N4 C17 H17B 110.9 . . ? C18 C17 H17B 110.9 . . ? H17A C17 H17B 109.0 . . ? O4 C18 C17 103.6(8) . . ? O4 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? O4 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? N5 C19 O5 117.9(10) . . ? N5 C19 C27 126.1(10) . . ? O5 C19 C27 115.9(9) . . ? N5 C20 C21 103.5(8) . . ? N5 C20 H20A 111.1 . . ? C21 C20 H20A 111.1 . . ? N5 C20 H20B 111.1 . . ? C21 C20 H20B 111.1 . . ? H20A C20 H20B 109.0 . . ? O5 C21 C20 104.2(8) . . ? O5 C21 H21A 110.9 . . ? C20 C21 H21A 110.9 . . ? O5 C21 H21B 110.9 . . ? C20 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? N6 C22 O6 119.2(9) . . ? N6 C22 C29 130.3(10) . . ? O6 C22 C29 110.5(10) . . ? O6 C23 C24 104.9(8) . . ? O6 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? O6 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.8 . . ? N6 C24 C23 104.5(9) . . ? N6 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? N6 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C26 C25 C30 119.0(10) . . ? C26 C25 C16 120.4(10) . . ? C30 C25 C16 120.5(9) . . ? C25 C26 C27 121.8(10) . . ? C25 C26 H26A 119.1 . . ? C27 C26 H26A 119.1 . . ? C26 C27 C28 118.7(10) . . ? C26 C27 C19 121.8(9) . . ? C28 C27 C19 119.4(10) . . ? C27 C28 C29 120.8(10) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 118.7(10) . . ? C30 C29 C22 119.0(10) . . ? C28 C29 C22 122.2(10) . . ? C29 C30 C25 120.7(10) . . ? C29 C30 H30A 119.6 . . ? C25 C30 H30A 119.6 . . ? 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 N2 Ag2 O10 N8 -47.3(11) 2_565 . . . ? N3 Ag2 O10 N8 139.5(11) . . . . ? N6 Ag3 O14 N9 60.3(10) . . . . ? N5 Ag3 O14 N9 -134.2(10) 2_566 . . . ? N4 Ag1 N1 C1 -28(2) . . . . ? N4 Ag1 N1 C3 150.7(13) . . . . ? N2 Ag2 N3 C7 19.9(16) 2_565 . . . ? O10 Ag2 N3 C7 -174.2(11) . . . . ? N2 Ag2 N3 C9 -174.4(9) 2_565 . . . ? O10 Ag2 N3 C9 -8.5(9) . . . . ? N1 Ag1 N4 C16 9(2) . . . . ? N1 Ag1 N4 C17 -177.9(13) . . . . ? N5 Ag3 N6 C22 -9.9(18) 2_566 . . . ? O14 Ag3 N6 C22 137.7(12) . . . . ? N5 Ag3 N6 C24 168.7(8) 2_566 . . . ? O14 Ag3 N6 C24 -43.6(10) . . . . ? Ag2 O10 N8 O11 1.0(18) . . . . ? Ag2 O10 N8 O12 -179.5(9) . . . . ? Ag3 O14 N9 O15 -179.9(10) . . . . ? Ag3 O14 N9 O16 2.6(16) . . . . ? C3 N1 C1 O1 -3.4(16) . . . . ? Ag1 N1 C1 O1 175.6(8) . . . . ? C3 N1 C1 C10 176.1(13) . . . . ? Ag1 N1 C1 C10 -5(2) . . . . ? C2 O1 C1 N1 -0.3(15) . . . . ? C2 O1 C1 C10 -179.9(10) . . . . ? C1 O1 C2 C3 3.6(13) . . . . ? C1 N1 C3 C2 5.5(15) . . . . ? Ag1 N1 C3 C2 -173.8(7) . . . . ? O1 C2 C3 N1 -5.4(13) . . . . ? C6 N2 C4 O2 -1.3(15) . . . . ? Ag2 N2 C4 O2 170.0(8) 2_565 . . . ? C6 N2 C4 C12 -178.6(10) . . . . ? Ag2 N2 C4 C12 -7.2(19) 2_565 . . . ? C5 O2 C4 N2 1.8(15) . . . . ? C5 O2 C4 C12 179.4(9) . . . . ? C4 O2 C5 C6 -1.3(12) . . . . ? C4 N2 C6 C5 0.3(14) . . . . ? Ag2 N2 C6 C5 -172.7(7) 2_565 . . . ? O2 C5 C6 N2 0.7(13) . . . . ? C9 N3 C7 O3 4.7(15) . . . . ? Ag2 N3 C7 O3 172.1(7) . . . . ? C9 N3 C7 C14 -176.8(11) . . . . ? Ag2 N3 C7 C14 -9.3(19) . . . . ? C8 O3 C7 N3 0.3(14) . . . . ? C8 O3 C7 C14 -178.5(10) . . . . ? C7 O3 C8 C9 -4.8(13) . . . . ? C7 N3 C9 C8 -7.3(14) . . . . ? Ag2 N3 C9 C8 -175.8(8) . . . . ? O3 C8 C9 N3 7.3(13) . . . . ? N1 C1 C10 C11 -13(2) . . . . ? O1 C1 C10 C11 167.0(10) . . . . ? N1 C1 C10 C15 169.5(13) . . . . ? O1 C1 C10 C15 -10.9(16) . . . . ? C15 C10 C11 C12 -1.1(17) . . . . ? C1 C10 C11 C12 -179.0(11) . . . . ? C10 C11 C12 C13 0.7(17) . . . . ? C10 C11 C12 C4 178.0(10) . . . . ? N2 C4 C12 C11 -22.1(18) . . . . ? O2 C4 C12 C11 160.5(10) . . . . ? N2 C4 C12 C13 155.0(12) . . . . ? O2 C4 C12 C13 -22.3(15) . . . . ? C11 C12 C13 C14 1.8(17) . . . . ? C4 C12 C13 C14 -175.4(11) . . . . ? C12 C13 C14 C15 -4.1(19) . . . . ? C12 C13 C14 C7 177.6(10) . . . . ? N3 C7 C14 C13 -141.3(13) . . . . ? O3 C7 C14 C13 37.3(17) . . . . ? N3 C7 C14 C15 40.2(18) . . . . ? O3 C7 C14 C15 -141.1(11) . . . . ? C11 C10 C15 C14 -1.0(17) . . . . ? C1 C10 C15 C14 176.9(11) . . . . ? C13 C14 C15 C10 3.6(19) . . . . ? C7 C14 C15 C10 -177.9(10) . . . . ? C17 N4 C16 O4 -1.0(15) . . . . ? Ag1 N4 C16 O4 172.9(7) . . . . ? C17 N4 C16 C25 175.7(11) . . . . ? Ag1 N4 C16 C25 -10(2) . . . . ? C18 O4 C16 N4 -0.9(14) . . . . ? C18 O4 C16 C25 -178.1(9) . . . . ? C16 N4 C17 C18 2.4(14) . . . . ? Ag1 N4 C17 C18 -172.7(8) . . . . ? C16 O4 C18 C17 2.3(12) . . . . ? N4 C17 C18 O4 -2.8(13) . . . . ? C20 N5 C19 O5 3.5(16) . . . . ? Ag3 N5 C19 O5 177.5(8) 2_566 . . . ? C20 N5 C19 C27 -179.0(11) . . . . ? Ag3 N5 C19 C27 -5(2) 2_566 . . . ? C21 O5 C19 N5 2.8(16) . . . . ? C21 O5 C19 C27 -175.0(10) . . . . ? C19 N5 C20 C21 -7.8(14) . . . . ? Ag3 N5 C20 C21 177.4(8) 2_566 . . . ? C19 O5 C21 C20 -7.5(14) . . . . ? N5 C20 C21 O5 9.1(14) . . . . ? C24 N6 C22 O6 -3.4(16) . . . . ? Ag3 N6 C22 O6 175.4(7) . . . . ? C24 N6 C22 C29 176.2(11) . . . . ? Ag3 N6 C22 C29 -5(2) . . . . ? C23 O6 C22 N6 -1.2(15) . . . . ? C23 O6 C22 C29 179.1(9) . . . . ? C22 O6 C23 C24 5.0(12) . . . . ? C22 N6 C24 C23 6.3(14) . . . . ? Ag3 N6 C24 C23 -172.7(8) . . . . ? O6 C23 C24 N6 -6.8(13) . . . . ? N4 C16 C25 C26 165.7(12) . . . . ? O4 C16 C25 C26 -17.5(15) . . . . ? N4 C16 C25 C30 -15.7(18) . . . . ? O4 C16 C25 C30 161.1(9) . . . . ? C30 C25 C26 C27 -0.7(17) . . . . ? C16 C25 C26 C27 177.8(10) . . . . ? C25 C26 C27 C28 3.7(16) . . . . ? C25 C26 C27 C19 -174.6(11) . . . . ? N5 C19 C27 C26 31.9(19) . . . . ? O5 C19 C27 C26 -150.5(10) . . . . ? N5 C19 C27 C28 -146.3(12) . . . . ? O5 C19 C27 C28 31.2(16) . . . . ? C26 C27 C28 C29 -4.7(16) . . . . ? C19 C27 C28 C29 173.6(10) . . . . ? C27 C28 C29 C30 2.9(16) . . . . ? C27 C28 C29 C22 -172.9(10) . . . . ? N6 C22 C29 C30 -24.7(19) . . . . ? O6 C22 C29 C30 154.9(9) . . . . ? N6 C22 C29 C28 151.2(13) . . . . ? O6 C22 C29 C28 -29.2(14) . . . . ? C28 C29 C30 C25 0.1(16) . . . . ? C22 C29 C30 C25 176.1(10) . . . . ? C26 C25 C30 C29 -1.2(16) . . . . ? C16 C25 C30 C29 -179.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.760 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.126 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 644137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Ag2(L)(NO3)2]-MeOH ; _chemical_name_common (Ag2(L)(NO3)2)-MeOH _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 Ag2 N5 O10' _chemical_formula_sum 'C16 H18 Ag2 N5 O10' _chemical_formula_weight 656.09 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3073(10) _cell_length_b 11.3195(19) _cell_length_c 12.486(2) _cell_angle_alpha 116.370(4) _cell_angle_beta 96.813(3) _cell_angle_gamma 98.940(4) _cell_volume 1015.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 485 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 18.59 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 1.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8566 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details 'sadabs(Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5099 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.1314 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3514 _reflns_number_gt 1836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3514 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1505 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.92934(12) 0.05060(12) 0.33803(8) 0.0584(4) Uani 1 1 d . . . Ag2 Ag 1.08048(15) 0.32588(13) 0.84914(10) 0.0748(5) Uani 1 1 d . . . N1 N 0.8045(11) -0.1317(10) -0.3734(7) 0.040(2) Uani 1 1 d . . . N2 N 1.1083(11) 0.3346(10) 0.0280(8) 0.043(3) Uani 1 1 d . . . N3 N 0.6908(11) -0.0617(10) 0.2079(8) 0.043(3) Uani 1 1 d . . . N4 N 0.8512(15) 0.1621(11) 0.6094(10) 0.051(3) Uani 1 1 d . . . N5 N 1.2864(16) 0.5110(13) 0.7896(10) 0.059(3) Uani 1 1 d . . . O1 O 0.5527(9) -0.2083(8) -0.3505(6) 0.049(2) Uani 1 1 d . . . O2 O 1.0988(9) 0.3140(8) 0.1967(6) 0.042(2) Uani 1 1 d . . . O3 O 0.4925(9) -0.1815(8) 0.0380(6) 0.0388(19) Uani 1 1 d . . . O4 O 0.7607(13) 0.0981(11) 0.5087(8) 0.082(3) Uani 1 1 d . . . O5 O 0.7960(12) 0.2253(10) 0.7008(8) 0.073(3) Uani 1 1 d . . . O6 O 1.0026(12) 0.1657(11) 0.6253(9) 0.079(3) Uani 1 1 d . . . O7 O 1.3501(13) 0.4388(13) 0.8186(12) 0.107(4) Uani 1 1 d . . . O8 O 1.1455(15) 0.5137(13) 0.8018(13) 0.115(5) Uani 1 1 d . . . O9 O 1.3647(13) 0.5765(11) 0.7485(10) 0.090(4) Uani 1 1 d . . . O10 O 0.891(2) 0.3445(14) 0.4457(14) 0.126(6) Uani 1 1 d . . . C1 C 0.7476(13) -0.0511(11) -0.1666(9) 0.033(3) Uani 1 1 d . . . C2 C 0.8687(13) 0.0687(11) -0.1101(9) 0.034(3) Uani 1 1 d . . . H2B H 0.9215 0.1007 -0.1569 0.041 Uiso 1 1 calc R . . C3 C 0.9116(13) 0.1410(11) 0.0162(9) 0.032(3) Uani 1 1 d . . . C4 C 0.8313(13) 0.0913(11) 0.0846(9) 0.030(3) Uani 1 1 d . . . H4A H 0.8582 0.1405 0.1695 0.036 Uiso 1 1 calc R . . C5 C 0.7132(13) -0.0290(11) 0.0290(9) 0.034(3) Uani 1 1 d . . . C6 C 0.6684(12) -0.0996(11) -0.0989(9) 0.030(3) Uani 1 1 d . . . H6A H 0.5851 -0.1792 -0.1378 0.037 Uiso 1 1 calc R . . C7 C 0.7046(14) -0.1334(12) -0.3028(9) 0.037(3) Uani 1 1 d . . . C8 C 0.5457(16) -0.2783(15) -0.4829(10) 0.064(4) Uani 1 1 d . . . H8A H 0.5318 -0.3751 -0.5126 0.077 Uiso 1 1 calc R . . H8B H 0.4534 -0.2632 -0.5268 0.077 Uiso 1 1 calc R . . C9 C 0.7040(15) -0.2203(15) -0.4997(10) 0.062(4) Uani 1 1 d . . . H9A H 0.6876 -0.1679 -0.5423 0.075 Uiso 1 1 calc R . . H9B H 0.7583 -0.2910 -0.5461 0.075 Uiso 1 1 calc R . . C10 C 0.6342(13) -0.0876(11) 0.0974(9) 0.029(3) Uani 1 1 d . . . C11 C 0.4503(14) -0.2381(11) 0.1177(9) 0.040(3) Uani 1 1 d . . . H11A H 0.4691 -0.3288 0.0877 0.048 Uiso 1 1 calc R . . H11B H 0.3346 -0.2417 0.1242 0.048 Uiso 1 1 calc R . . C12 C 0.5667(13) -0.1411(12) 0.2404(10) 0.042(3) Uani 1 1 d . . . H12A H 0.5078 -0.0833 0.2972 0.051 Uiso 1 1 calc R . . H12B H 0.6188 -0.1900 0.2762 0.051 Uiso 1 1 calc R . . C13 C 1.0428(15) 0.2689(13) 0.0784(11) 0.046(3) Uani 1 1 d . . . C14 C 1.2234(16) 0.4415(13) 0.2434(11) 0.059(4) Uani 1 1 d . . . H14A H 1.3291 0.4374 0.2822 0.070 Uiso 1 1 calc R . . H14B H 1.1859 0.5173 0.3014 0.070 Uiso 1 1 calc R . . C15 C 1.2371(16) 0.4526(14) 0.1256(11) 0.066(4) Uani 1 1 d . . . H15A H 1.2147 0.5373 0.1332 0.079 Uiso 1 1 calc R . . H15B H 1.3474 0.4475 0.1084 0.079 Uiso 1 1 calc R . . C16 C 0.876(4) 0.460(5) 0.457(3) 0.220(17) 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 0.0428(6) 0.0848(9) 0.0396(6) 0.0288(6) 0.0052(4) -0.0026(6) Ag2 0.0833(9) 0.0845(10) 0.0647(8) 0.0506(7) 0.0119(6) -0.0040(7) N1 0.047(6) 0.047(7) 0.021(5) 0.017(5) 0.001(4) 0.003(5) N2 0.039(6) 0.046(7) 0.038(6) 0.020(5) 0.009(5) -0.006(5) N3 0.039(6) 0.067(8) 0.042(6) 0.038(6) 0.015(5) 0.022(5) N4 0.065(8) 0.051(8) 0.057(8) 0.039(7) 0.025(7) 0.018(7) N5 0.055(8) 0.063(9) 0.057(7) 0.032(7) 0.009(6) 0.003(7) O1 0.035(5) 0.062(6) 0.032(4) 0.017(4) -0.005(4) -0.011(4) O2 0.046(5) 0.034(5) 0.034(4) 0.010(4) 0.002(4) 0.002(4) O3 0.041(4) 0.047(5) 0.037(4) 0.030(4) 0.009(4) 0.000(4) O4 0.093(8) 0.091(9) 0.044(6) 0.024(6) 0.004(5) 0.009(7) O5 0.077(7) 0.082(8) 0.047(6) 0.016(6) 0.034(5) 0.016(6) O6 0.060(7) 0.094(9) 0.100(8) 0.054(7) 0.041(6) 0.024(6) O7 0.068(8) 0.112(11) 0.177(13) 0.099(10) 0.016(8) 0.025(7) O8 0.079(8) 0.132(12) 0.200(14) 0.118(11) 0.073(9) 0.043(8) O9 0.093(8) 0.098(9) 0.098(8) 0.074(8) 0.018(6) -0.013(7) O10 0.181(16) 0.100(11) 0.157(13) 0.085(10) 0.100(12) 0.068(11) C1 0.038(6) 0.038(7) 0.037(6) 0.028(6) 0.011(5) 0.014(6) C2 0.043(7) 0.026(7) 0.038(6) 0.018(6) 0.012(5) 0.009(6) C3 0.042(7) 0.022(6) 0.034(6) 0.014(5) 0.010(5) 0.007(6) C4 0.040(6) 0.027(7) 0.022(5) 0.011(5) 0.004(5) 0.007(6) C5 0.040(7) 0.031(7) 0.031(6) 0.015(6) 0.007(5) 0.012(6) C6 0.023(6) 0.032(7) 0.035(6) 0.019(6) 0.002(5) -0.005(5) C7 0.040(7) 0.040(8) 0.025(6) 0.012(6) 0.008(5) 0.006(6) C8 0.060(9) 0.086(12) 0.028(7) 0.017(7) 0.000(6) 0.010(8) C9 0.060(8) 0.084(11) 0.020(6) 0.018(7) -0.002(6) -0.016(8) C10 0.038(6) 0.029(7) 0.026(6) 0.015(5) 0.013(5) 0.014(6) C11 0.052(7) 0.025(7) 0.043(7) 0.019(6) 0.012(6) 0.001(6) C12 0.046(7) 0.047(8) 0.040(7) 0.025(6) 0.017(6) 0.007(6) C13 0.050(7) 0.047(9) 0.043(7) 0.019(7) 0.018(6) 0.020(7) C14 0.058(8) 0.047(9) 0.044(8) 0.007(7) -0.004(6) -0.006(7) C15 0.061(9) 0.062(10) 0.069(9) 0.042(8) -0.006(7) -0.023(8) C16 0.22(3) 0.36(5) 0.18(3) 0.21(4) 0.02(2) 0.10(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.169(9) 2_755 ? Ag1 N3 2.191(9) . ? Ag1 O4 2.592(10) . ? Ag2 N2 2.174(9) 1_556 ? Ag2 O8 2.449(12) . ? Ag2 O6 2.494(10) . ? Ag2 O7 2.558(12) . ? Ag2 O5 2.562(9) . ? N1 C7 1.285(13) . ? N1 C9 1.488(12) . ? N1 Ag1 2.169(9) 2_755 ? N2 C13 1.272(14) . ? N2 C15 1.489(14) . ? N2 Ag2 2.174(9) 1_554 ? N3 C10 1.286(12) . ? N3 C12 1.473(13) . ? N4 O4 1.212(12) . ? N4 O5 1.235(12) . ? N4 O6 1.241(12) . ? N5 O7 1.196(14) . ? N5 O8 1.201(14) . ? N5 O9 1.227(14) . ? O1 C7 1.306(12) . ? O1 C8 1.472(12) . ? O2 C13 1.324(13) . ? O2 C14 1.462(13) . ? O3 C10 1.330(12) . ? O3 C11 1.451(12) . ? O10 C16 1.27(4) . ? C1 C6 1.372(13) . ? C1 C2 1.381(14) . ? C1 C7 1.494(14) . ? C2 C3 1.383(14) . ? C2 H2B 0.9300 . ? C3 C4 1.392(14) . ? C3 C13 1.482(16) . ? C4 C5 1.372(14) . ? C4 H4A 0.9300 . ? C5 C6 1.399(13) . ? C5 C10 1.450(14) . ? C6 H6A 0.9300 . ? C8 C9 1.457(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.520(14) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.547(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 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 N1 Ag1 N3 149.7(3) 2_755 . ? N1 Ag1 O4 123.6(3) 2_755 . ? N3 Ag1 O4 86.5(3) . . ? N2 Ag2 O8 128.0(4) 1_556 . ? N2 Ag2 O6 142.9(4) 1_556 . ? O8 Ag2 O6 89.0(4) . . ? N2 Ag2 O7 112.4(4) 1_556 . ? O8 Ag2 O7 48.1(4) . . ? O6 Ag2 O7 89.6(4) . . ? N2 Ag2 O5 120.5(3) 1_556 . ? O8 Ag2 O5 93.0(4) . . ? O6 Ag2 O5 49.4(3) . . ? O7 Ag2 O5 126.9(4) . . ? C7 N1 C9 105.1(9) . . ? C7 N1 Ag1 132.5(7) . 2_755 ? C9 N1 Ag1 121.9(7) . 2_755 ? C13 N2 C15 106.7(9) . . ? C13 N2 Ag2 138.7(8) . 1_554 ? C15 N2 Ag2 114.5(7) . 1_554 ? C10 N3 C12 107.4(9) . . ? C10 N3 Ag1 134.0(8) . . ? C12 N3 Ag1 118.1(6) . . ? O4 N4 O5 121.2(12) . . ? O4 N4 O6 121.6(12) . . ? O5 N4 O6 117.2(12) . . ? O7 N5 O8 116.9(14) . . ? O7 N5 O9 119.7(14) . . ? O8 N5 O9 123.4(15) . . ? C7 O1 C8 104.5(9) . . ? C13 O2 C14 108.1(9) . . ? C10 O3 C11 106.5(8) . . ? N4 O4 Ag1 111.3(8) . . ? N4 O5 Ag2 95.0(8) . . ? N4 O6 Ag2 98.2(8) . . ? N5 O7 Ag2 94.4(9) . . ? N5 O8 Ag2 99.8(10) . . ? C6 C1 C2 120.7(10) . . ? C6 C1 C7 118.5(10) . . ? C2 C1 C7 120.7(10) . . ? C1 C2 C3 120.0(10) . . ? C1 C2 H2B 120.0 . . ? C3 C2 H2B 120.0 . . ? C2 C3 C4 119.1(10) . . ? C2 C3 C13 120.7(10) . . ? C4 C3 C13 120.2(10) . . ? C5 C4 C3 121.1(10) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 119.1(10) . . ? C4 C5 C10 122.6(10) . . ? C6 C5 C10 118.3(10) . . ? C1 C6 C5 119.9(10) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? N1 C7 O1 119.5(9) . . ? N1 C7 C1 124.4(10) . . ? O1 C7 C1 116.0(9) . . ? C9 C8 O1 105.8(9) . . ? C9 C8 H8A 110.6 . . ? O1 C8 H8A 110.6 . . ? C9 C8 H8B 110.6 . . ? O1 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? C8 C9 N1 104.5(9) . . ? C8 C9 H9A 110.8 . . ? N1 C9 H9A 110.8 . . ? C8 C9 H9B 110.8 . . ? N1 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? N3 C10 O3 117.0(9) . . ? N3 C10 C5 126.5(10) . . ? O3 C10 C5 116.5(9) . . ? O3 C11 C12 104.1(8) . . ? O3 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? O3 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? N3 C12 C11 102.8(8) . . ? N3 C12 H12A 111.2 . . ? C11 C12 H12A 111.2 . . ? N3 C12 H12B 111.2 . . ? C11 C12 H12B 111.2 . . ? H12A C12 H12B 109.1 . . ? N2 C13 O2 118.3(11) . . ? N2 C13 C3 126.2(11) . . ? O2 C13 C3 115.4(11) . . ? O2 C14 C15 102.2(9) . . ? O2 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? O2 C14 H14B 111.3 . . ? C15 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? N2 C15 C14 104.4(9) . . ? N2 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? N2 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? 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 N3 C10 -23.1(15) 2_755 . . . ? O4 Ag1 N3 C10 151.6(11) . . . . ? N1 Ag1 N3 C12 148.4(8) 2_755 . . . ? O4 Ag1 N3 C12 -36.9(8) . . . . ? O5 N4 O4 Ag1 160.6(9) . . . . ? O6 N4 O4 Ag1 -20.2(15) . . . . ? N1 Ag1 O4 N4 -5.2(10) 2_755 . . . ? N3 Ag1 O4 N4 178.0(9) . . . . ? O4 N4 O5 Ag2 -177.0(10) . . . . ? O6 N4 O5 Ag2 3.8(12) . . . . ? N2 Ag2 O5 N4 -137.8(7) 1_556 . . . ? O8 Ag2 O5 N4 83.9(8) . . . . ? O6 Ag2 O5 N4 -2.2(7) . . . . ? O7 Ag2 O5 N4 46.8(9) . . . . ? O4 N4 O6 Ag2 176.9(10) . . . . ? O5 N4 O6 Ag2 -3.9(12) . . . . ? N2 Ag2 O6 N4 90.8(9) 1_556 . . . ? O8 Ag2 O6 N4 -92.6(8) . . . . ? O7 Ag2 O6 N4 -140.7(8) . . . . ? O5 Ag2 O6 N4 2.2(7) . . . . ? O8 N5 O7 Ag2 9.0(15) . . . . ? O9 N5 O7 Ag2 -170.3(11) . . . . ? N2 Ag2 O7 N5 -127.0(9) 1_556 . . . ? O8 Ag2 O7 N5 -5.3(9) . . . . ? O6 Ag2 O7 N5 83.7(9) . . . . ? O5 Ag2 O7 N5 48.8(11) . . . . ? O7 N5 O8 Ag2 -9.5(15) . . . . ? O9 N5 O8 Ag2 169.8(11) . . . . ? N2 Ag2 O8 N5 92.4(10) 1_556 . . . ? O6 Ag2 O8 N5 -85.0(10) . . . . ? O7 Ag2 O8 N5 5.3(9) . . . . ? O5 Ag2 O8 N5 -134.3(10) . . . . ? C6 C1 C2 C3 0.1(16) . . . . ? C7 C1 C2 C3 -177.5(10) . . . . ? C1 C2 C3 C4 0.1(16) . . . . ? C1 C2 C3 C13 179.3(10) . . . . ? C2 C3 C4 C5 1.2(16) . . . . ? C13 C3 C4 C5 -178.0(10) . . . . ? C3 C4 C5 C6 -2.7(16) . . . . ? C3 C4 C5 C10 176.3(10) . . . . ? C2 C1 C6 C5 -1.6(16) . . . . ? C7 C1 C6 C5 176.1(10) . . . . ? C4 C5 C6 C1 2.8(16) . . . . ? C10 C5 C6 C1 -176.2(10) . . . . ? C9 N1 C7 O1 2.3(15) . . . . ? Ag1 N1 C7 O1 -169.3(8) 2_755 . . . ? C9 N1 C7 C1 -175.8(11) . . . . ? Ag1 N1 C7 C1 12.7(19) 2_755 . . . ? C8 O1 C7 N1 2.4(15) . . . . ? C8 O1 C7 C1 -179.3(10) . . . . ? C6 C1 C7 N1 -152.0(12) . . . . ? C2 C1 C7 N1 25.6(17) . . . . ? C6 C1 C7 O1 29.8(15) . . . . ? C2 C1 C7 O1 -152.5(11) . . . . ? C7 O1 C8 C9 -6.1(14) . . . . ? O1 C8 C9 N1 7.2(15) . . . . ? C7 N1 C9 C8 -5.9(15) . . . . ? Ag1 N1 C9 C8 166.7(9) 2_755 . . . ? C12 N3 C10 O3 -4.7(13) . . . . ? Ag1 N3 C10 O3 167.5(7) . . . . ? C12 N3 C10 C5 178.3(11) . . . . ? Ag1 N3 C10 C5 -9.6(18) . . . . ? C11 O3 C10 N3 -5.3(13) . . . . ? C11 O3 C10 C5 172.1(9) . . . . ? C4 C5 C10 N3 -21.0(18) . . . . ? C6 C5 C10 N3 158.0(11) . . . . ? C4 C5 C10 O3 161.9(10) . . . . ? C6 C5 C10 O3 -19.1(15) . . . . ? C10 O3 C11 C12 12.4(11) . . . . ? C10 N3 C12 C11 11.9(12) . . . . ? Ag1 N3 C12 C11 -161.7(7) . . . . ? O3 C11 C12 N3 -14.4(11) . . . . ? C15 N2 C13 O2 -0.6(15) . . . . ? Ag2 N2 C13 O2 -178.5(8) 1_554 . . . ? C15 N2 C13 C3 -178.1(11) . . . . ? Ag2 N2 C13 C3 4(2) 1_554 . . . ? C14 O2 C13 N2 3.7(15) . . . . ? C14 O2 C13 C3 -178.6(10) . . . . ? C2 C3 C13 N2 11.4(18) . . . . ? C4 C3 C13 N2 -169.4(12) . . . . ? C2 C3 C13 O2 -166.1(10) . . . . ? C4 C3 C13 O2 13.1(16) . . . . ? C13 O2 C14 C15 -4.7(13) . . . . ? C13 N2 C15 C14 -2.5(14) . . . . ? Ag2 N2 C15 C14 176.0(8) 1_554 . . . ? O2 C14 C15 N2 4.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.660 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.133 #====END data_6 _database_code_depnum_ccdc_archive 'CCDC 644138' _audit_creation_date 'Sat Apr 30 09:11:18 2005' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Ag2(L)2](ClO4)2 ; _chemical_name_common (Ag2(L)2)(ClO4)2 _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Ag2 Cl2 N6 O14 ' _chemical_formula_sum 'C30 H30 Ag2 Cl2 N6 O14' _chemical_formula_weight 985.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_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 14.177(3) _cell_length_b 17.872(4) _cell_length_c 14.392(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.670(9) _cell_angle_gamma 90.00 _cell_volume 3433.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 21365 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 33294 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7848 _reflns_number_gt 6497 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR 92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+5.8777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7848 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.313493(18) 0.531234(14) 0.125758(19) 0.02971(7) Uani 1 1 d . . . Ag2 Ag 0.223610(17) 0.396398(14) 0.323570(18) 0.02865(7) Uani 1 1 d . . . Cl1 Cl 0.14908(6) 0.31752(5) 0.51730(6) 0.03077(18) Uani 1 1 d . . . Cl2 Cl 0.35796(6) 0.66705(5) -0.05043(6) 0.03481(19) Uani 1 1 d . . . O1 O 0.11923(16) 0.70905(12) 0.16792(18) 0.0325(5) Uani 1 1 d . . . O3 O -0.24025(15) 0.64973(13) 0.09492(16) 0.0311(5) Uani 1 1 d . . . O5 O -0.06784(16) 0.33431(12) 0.08935(17) 0.0316(5) Uani 1 1 d . . . O11 O 0.14365(18) 0.24100(14) 0.54352(17) 0.0382(6) Uani 1 1 d . . . O12 O 0.0608(2) 0.33363(19) 0.4333(2) 0.0673(9) Uani 1 1 d . . . O13 O 0.2362(2) 0.33016(19) 0.4921(3) 0.0741(10) Uani 1 1 d . . . O14 O 0.1481(2) 0.36577(15) 0.59613(19) 0.0468(7) Uani 1 1 d . . . O21 O 0.4123(2) 0.62854(18) 0.0397(2) 0.0570(8) Uani 1 1 d . . . O22 O 0.2991(3) 0.61376(19) -0.1201(3) 0.0728(10) Uani 1 1 d . . . O23 O 0.4274(2) 0.70201(18) -0.0886(3) 0.0683(10) Uani 1 1 d . . . O24 O 0.29281(19) 0.72154(16) -0.0324(2) 0.0528(7) Uani 1 1 d . . . O101 O 0.62934(15) 0.54684(14) 0.35887(16) 0.0332(6) Uani 1 1 d . . . O103 O 0.49521(16) 0.71219(14) 0.68067(17) 0.0356(6) Uani 1 1 d . . . O105 O 0.19067(16) 0.59124(13) 0.49548(18) 0.0331(5) Uani 1 1 d . . . N1 N 0.23533(18) 0.62442(14) 0.16718(18) 0.0221(5) Uani 1 1 d . . . N3 N -0.29499(18) 0.56458(15) -0.02585(19) 0.0244(6) Uani 1 1 d . . . N5 N 0.08148(18) 0.34687(14) 0.20871(18) 0.0241(5) Uani 1 1 d . . . N101 N 0.48375(19) 0.51919(16) 0.24073(18) 0.0277(6) Uani 1 1 d . . . N103 N 0.64511(18) 0.66984(15) 0.68414(18) 0.0250(6) Uani 1 1 d . . . N105 N 0.17957(18) 0.50476(15) 0.37903(19) 0.0252(6) Uani 1 1 d . . . C1 C 0.0598(2) 0.58440(16) 0.1316(2) 0.0199(6) Uani 1 1 d . . . C2 C -0.0385(2) 0.61209(17) 0.1019(2) 0.0222(6) Uani 1 1 d . . . H1 H -0.0501 0.6645 0.0978 0.027 Uiso 1 1 calc R . . C3 C -0.1183(2) 0.56281(17) 0.0787(2) 0.0214(6) Uani 1 1 d . . . C4 C -0.1023(2) 0.48607(17) 0.0877(2) 0.0228(6) Uani 1 1 d . . . H2 H -0.1576 0.4526 0.0712 0.027 Uiso 1 1 calc R . . C5 C -0.0044(2) 0.45832(17) 0.1213(2) 0.0204(6) Uani 1 1 d . . . C6 C 0.0761(2) 0.50752(17) 0.1411(2) 0.0210(6) Uani 1 1 d . . . H3 H 0.1425 0.4885 0.1612 0.025 Uiso 1 1 calc R . . C11 C 0.1437(2) 0.63765(17) 0.1553(2) 0.0216(6) Uani 1 1 d . . . C12 C 0.2907(2) 0.69573(18) 0.1974(2) 0.0293(7) Uani 1 1 d . . . H4 H 0.3345 0.7058 0.1578 0.035 Uiso 1 1 calc R . . H5 H 0.3321 0.6948 0.2682 0.035 Uiso 1 1 calc R . . C13 C 0.2080(2) 0.75397(19) 0.1773(3) 0.0379(8) Uani 1 1 d . . . H6 H 0.2217 0.7899 0.2327 0.045 Uiso 1 1 calc R . . H7 H 0.2002 0.7818 0.1157 0.045 Uiso 1 1 calc R . . C31 C -0.2218(2) 0.59103(17) 0.0449(2) 0.0216(6) Uani 1 1 d . . . C32 C -0.3849(2) 0.60806(18) -0.0301(2) 0.0271(7) Uani 1 1 d . . . H8 H -0.4331 0.5767 -0.0112 0.032 Uiso 1 1 calc R . . H9 H -0.4185 0.6283 -0.0972 0.032 Uiso 1 1 calc R . . C33 C -0.3446(2) 0.6708(2) 0.0438(3) 0.0357(8) Uani 1 1 d . . . H10 H -0.3488 0.7195 0.0099 0.043 Uiso 1 1 calc R . . H11 H -0.3821 0.6742 0.0905 0.043 Uiso 1 1 calc R . . C51 C 0.0094(2) 0.37776(17) 0.1421(2) 0.0218(6) Uani 1 1 d . . . C52 C 0.0530(2) 0.26750(18) 0.2126(2) 0.0297(7) Uani 1 1 d . . . H12 H 0.0418 0.2564 0.2755 0.036 Uiso 1 1 calc R . . H13 H 0.1057 0.2337 0.2060 0.036 Uiso 1 1 calc R . . C53 C -0.0436(2) 0.25848(19) 0.1255(3) 0.0330(8) Uani 1 1 d . . . H14 H -0.0333 0.2259 0.0742 0.040 Uiso 1 1 calc R . . H15 H -0.0974 0.2370 0.1469 0.040 Uiso 1 1 calc R . . C101 C 0.4821(2) 0.56639(17) 0.4001(2) 0.0193(6) Uani 1 1 d . . . C102 C 0.5383(2) 0.60511(16) 0.4846(2) 0.0213(6) Uani 1 1 d . . . H16 H 0.6070 0.6156 0.4961 0.026 Uiso 1 1 calc R . . C103 C 0.4935(2) 0.62834(16) 0.5523(2) 0.0200(6) Uani 1 1 d . . . C104 C 0.3929(2) 0.61329(16) 0.5357(2) 0.0217(6) Uani 1 1 d . . . H17 H 0.3620 0.6310 0.5807 0.026 Uiso 1 1 calc R . . C105 C 0.3377(2) 0.57243(16) 0.4533(2) 0.0204(6) Uani 1 1 d . . . C106 C 0.3824(2) 0.54933(16) 0.3853(2) 0.0208(6) Uani 1 1 d . . . H18 H 0.3444 0.5218 0.3286 0.025 Uiso 1 1 calc R . . C111 C 0.5283(2) 0.54278(17) 0.3273(2) 0.0217(6) Uani 1 1 d . . . C112 C 0.5631(2) 0.5011(2) 0.1978(3) 0.0400(9) Uani 1 1 d . . . H19 H 0.5536 0.5305 0.1370 0.048 Uiso 1 1 calc R . . H20 H 0.5623 0.4472 0.1819 0.048 Uiso 1 1 calc R . . C113 C 0.6603(2) 0.5222(2) 0.2773(2) 0.0367(8) Uani 1 1 d . . . H21 H 0.7058 0.4787 0.2966 0.044 Uiso 1 1 calc R . . H22 H 0.6945 0.5630 0.2547 0.044 Uiso 1 1 calc R . . C131 C 0.5507(2) 0.66970(17) 0.6415(2) 0.0221(6) Uani 1 1 d . . . C132 C 0.6667(2) 0.7216(2) 0.7692(2) 0.0322(8) Uani 1 1 d . . . H23 H 0.7132 0.7617 0.7650 0.039 Uiso 1 1 calc R . . H24 H 0.6965 0.6945 0.8323 0.039 Uiso 1 1 calc R . . C133 C 0.5643(2) 0.7540(2) 0.7611(2) 0.0316(7) Uani 1 1 d . . . H25 H 0.5498 0.7464 0.8231 0.038 Uiso 1 1 calc R . . H26 H 0.5611 0.8082 0.7459 0.038 Uiso 1 1 calc R . . C151 C 0.2331(2) 0.55308(17) 0.4387(2) 0.0220(6) Uani 1 1 d . . . C152 C 0.0772(2) 0.5112(2) 0.3852(3) 0.0306(7) Uani 1 1 d . . . H27 H 0.0478 0.4613 0.3873 0.037 Uiso 1 1 calc R . . H28 H 0.0323 0.5397 0.3285 0.037 Uiso 1 1 calc R . . C153 C 0.0952(2) 0.5530(2) 0.4809(3) 0.0361(8) Uani 1 1 d . . . H29 H 0.0409 0.5894 0.4752 0.043 Uiso 1 1 calc R . . H30 H 0.1005 0.5181 0.5358 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02580(13) 0.03017(14) 0.03453(14) -0.00697(11) 0.01194(10) 0.00050(10) Ag2 0.02217(12) 0.03201(14) 0.02930(13) -0.00330(10) 0.00542(10) 0.00241(10) Cl1 0.0332(4) 0.0327(4) 0.0288(4) 0.0005(3) 0.0134(3) -0.0035(3) Cl2 0.0262(4) 0.0392(5) 0.0426(5) 0.0062(4) 0.0162(4) 0.0060(4) O1 0.0212(11) 0.0208(12) 0.0535(15) -0.0083(10) 0.0100(11) -0.0021(9) O3 0.0189(10) 0.0358(13) 0.0359(13) -0.0120(10) 0.0057(10) 0.0019(10) O5 0.0237(11) 0.0233(12) 0.0386(13) -0.0014(10) -0.0016(10) -0.0038(9) O11 0.0442(14) 0.0320(14) 0.0366(14) 0.0025(11) 0.0112(12) -0.0039(11) O12 0.075(2) 0.071(2) 0.0374(16) 0.0066(15) -0.0052(15) 0.0193(18) O13 0.064(2) 0.068(2) 0.117(3) -0.014(2) 0.066(2) -0.0200(17) O14 0.0611(18) 0.0406(15) 0.0419(15) -0.0130(12) 0.0216(14) -0.0090(13) O21 0.0436(16) 0.075(2) 0.0575(18) 0.0295(16) 0.0232(14) 0.0166(15) O22 0.072(2) 0.067(2) 0.079(2) -0.0265(19) 0.0253(19) -0.0052(18) O23 0.0453(16) 0.075(2) 0.101(3) 0.052(2) 0.0464(18) 0.0221(16) O24 0.0327(14) 0.0564(18) 0.070(2) -0.0056(15) 0.0183(14) 0.0148(13) O101 0.0163(10) 0.0568(16) 0.0274(12) -0.0109(11) 0.0089(9) -0.0035(10) O103 0.0210(11) 0.0468(15) 0.0361(13) -0.0206(11) 0.0058(10) 0.0035(10) O105 0.0220(11) 0.0370(14) 0.0459(14) -0.0154(11) 0.0187(11) -0.0065(10) N1 0.0173(12) 0.0226(13) 0.0252(13) -0.0040(10) 0.0057(10) -0.0039(10) N3 0.0180(12) 0.0258(14) 0.0271(14) -0.0022(11) 0.0046(11) 0.0027(11) N5 0.0220(12) 0.0224(14) 0.0249(13) -0.0011(11) 0.0039(11) -0.0007(11) N101 0.0223(13) 0.0401(17) 0.0204(13) -0.0038(12) 0.0069(11) 0.0030(12) N103 0.0191(12) 0.0324(15) 0.0225(13) -0.0054(11) 0.0054(10) -0.0012(11) N105 0.0163(12) 0.0321(15) 0.0275(14) -0.0037(11) 0.0079(11) -0.0018(11) C1 0.0190(14) 0.0222(15) 0.0166(14) -0.0006(11) 0.0034(11) -0.0014(12) C2 0.0199(14) 0.0228(16) 0.0210(14) -0.0017(12) 0.0029(12) 0.0015(12) C3 0.0163(13) 0.0255(16) 0.0210(14) -0.0023(12) 0.0042(12) -0.0006(12) C4 0.0170(14) 0.0264(16) 0.0216(15) -0.0012(12) 0.0022(12) -0.0034(12) C5 0.0193(14) 0.0229(15) 0.0173(14) 0.0003(12) 0.0038(11) -0.0007(12) C6 0.0163(13) 0.0277(16) 0.0172(14) 0.0021(12) 0.0031(11) 0.0009(12) C11 0.0227(15) 0.0215(15) 0.0190(14) -0.0008(12) 0.0047(12) 0.0000(12) C12 0.0240(16) 0.0269(17) 0.0358(18) -0.0054(14) 0.0084(14) -0.0089(13) C13 0.0297(18) 0.0250(18) 0.055(2) -0.0054(16) 0.0097(17) -0.0104(15) C31 0.0188(14) 0.0225(16) 0.0240(15) -0.0013(12) 0.0078(12) -0.0008(12) C32 0.0159(14) 0.0294(17) 0.0335(17) -0.0021(14) 0.0051(13) 0.0012(13) C33 0.0212(16) 0.035(2) 0.050(2) -0.0072(16) 0.0109(15) 0.0061(14) C51 0.0180(14) 0.0234(16) 0.0247(15) -0.0022(12) 0.0081(12) -0.0033(12) C52 0.0327(17) 0.0214(16) 0.0356(18) 0.0033(14) 0.0124(15) -0.0018(14) C53 0.0275(17) 0.0240(17) 0.048(2) -0.0016(15) 0.0128(16) -0.0043(14) C101 0.0167(13) 0.0226(15) 0.0181(14) 0.0043(11) 0.0050(11) 0.0018(12) C102 0.0161(13) 0.0235(16) 0.0228(15) 0.0039(12) 0.0046(12) -0.0002(12) C103 0.0182(14) 0.0198(15) 0.0202(14) -0.0003(11) 0.0042(12) 0.0010(12) C104 0.0195(14) 0.0206(15) 0.0261(15) -0.0007(12) 0.0093(12) 0.0024(12) C105 0.0156(13) 0.0196(15) 0.0252(15) 0.0042(12) 0.0060(12) 0.0017(11) C106 0.0172(14) 0.0226(16) 0.0200(14) 0.0010(12) 0.0028(11) -0.0012(12) C111 0.0168(13) 0.0253(16) 0.0231(15) 0.0032(12) 0.0068(12) -0.0005(12) C112 0.0229(17) 0.067(3) 0.0299(19) -0.0112(18) 0.0087(15) 0.0035(17) C113 0.0232(16) 0.059(2) 0.0313(18) -0.0115(17) 0.0130(14) -0.0027(16) C131 0.0192(14) 0.0271(16) 0.0212(15) -0.0006(12) 0.0082(12) -0.0003(12) C132 0.0276(16) 0.042(2) 0.0249(17) -0.0074(15) 0.0061(14) -0.0026(15) C133 0.0305(17) 0.0343(19) 0.0291(17) -0.0086(14) 0.0088(14) -0.0017(15) C151 0.0177(14) 0.0243(16) 0.0247(15) 0.0006(12) 0.0081(12) 0.0029(12) C152 0.0172(15) 0.0357(19) 0.0400(19) -0.0034(15) 0.0111(14) -0.0024(14) C153 0.0226(16) 0.041(2) 0.050(2) -0.0073(17) 0.0196(16) -0.0064(15) _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 2.191(2) . ? Ag1 N3 2.194(3) 3_565 ? Ag1 N101 2.434(3) . ? Ag2 N103 2.240(2) 3_666 ? Ag2 N105 2.261(3) . ? Ag2 N5 2.310(3) . ? Cl1 O13 1.417(3) . ? Cl1 O11 1.428(3) . ? Cl1 O14 1.429(3) . ? Cl1 O12 1.447(3) . ? Cl2 O23 1.423(3) . ? Cl2 O24 1.425(3) . ? Cl2 O22 1.430(3) . ? Cl2 O21 1.441(3) . ? O1 C11 1.351(4) . ? O1 C13 1.460(4) . ? O3 C31 1.347(4) . ? O3 C33 1.462(4) . ? O5 C51 1.349(4) . ? O5 C53 1.451(4) . ? O101 C111 1.351(3) . ? O101 C113 1.452(4) . ? O103 C131 1.346(3) . ? O103 C133 1.447(4) . ? O105 C151 1.352(3) . ? O105 C153 1.467(4) . ? N1 C11 1.274(4) . ? N1 C12 1.483(4) . ? N3 C31 1.275(4) . ? N3 C32 1.476(4) . ? N3 Ag1 2.194(3) 3_565 ? N5 C51 1.268(4) . ? N5 C52 1.481(4) . ? N101 C111 1.264(4) . ? N101 C112 1.490(4) . ? N103 C131 1.271(4) . ? N103 C132 1.483(4) . ? N103 Ag2 2.240(2) 3_666 ? N105 C151 1.273(4) . ? N105 C152 1.488(4) . ? C1 C6 1.392(4) . ? C1 C2 1.402(4) . ? C1 C11 1.471(4) . ? C2 C3 1.384(4) . ? C2 H1 0.9500 . ? C3 C4 1.389(4) . ? C3 C31 1.471(4) . ? C4 C5 1.399(4) . ? C4 H2 0.9500 . ? C5 C6 1.391(4) . ? C5 C51 1.470(4) . ? C6 H3 0.9500 . ? C12 C13 1.521(5) . ? C12 H4 0.9900 . ? C12 H5 0.9900 . ? C13 H6 0.9900 . ? C13 H7 0.9900 . ? C32 C33 1.519(5) . ? C32 H8 0.9900 . ? C32 H9 0.9900 . ? C33 H10 0.9900 . ? C33 H11 0.9900 . ? C52 C53 1.522(5) . ? C52 H12 0.9900 . ? C52 H13 0.9900 . ? C53 H14 0.9900 . ? C53 H15 0.9900 . ? C101 C106 1.391(4) . ? C101 C102 1.393(4) . ? C101 C111 1.472(4) . ? C102 C103 1.392(4) . ? C102 H16 0.9500 . ? C103 C104 1.391(4) . ? C103 C131 1.467(4) . ? C104 C105 1.388(4) . ? C104 H17 0.9500 . ? C105 C106 1.394(4) . ? C105 C151 1.468(4) . ? C106 H18 0.9500 . ? C112 C113 1.512(5) . ? C112 H19 0.9900 . ? C112 H20 0.9900 . ? C113 H21 0.9900 . ? C113 H22 0.9900 . ? C132 C133 1.529(4) . ? C132 H23 0.9900 . ? C132 H24 0.9900 . ? C133 H25 0.9900 . ? C133 H26 0.9900 . ? C152 C153 1.511(5) . ? C152 H27 0.9900 . ? C152 H28 0.9900 . ? C153 H29 0.9900 . ? C153 H30 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 144.25(9) . 3_565 ? N1 Ag1 N101 111.04(9) . . ? N3 Ag1 N101 104.42(9) 3_565 . ? N103 Ag2 N105 143.41(9) 3_666 . ? N103 Ag2 N5 107.53(9) 3_666 . ? N105 Ag2 N5 107.63(9) . . ? O13 Cl1 O11 110.45(18) . . ? O13 Cl1 O14 110.44(19) . . ? O11 Cl1 O14 110.64(15) . . ? O13 Cl1 O12 109.7(2) . . ? O11 Cl1 O12 107.65(18) . . ? O14 Cl1 O12 107.87(18) . . ? O23 Cl2 O24 110.18(18) . . ? O23 Cl2 O22 109.7(2) . . ? O24 Cl2 O22 108.79(19) . . ? O23 Cl2 O21 109.12(17) . . ? O24 Cl2 O21 110.22(18) . . ? O22 Cl2 O21 108.8(2) . . ? C11 O1 C13 106.2(2) . . ? C31 O3 C33 106.1(2) . . ? C51 O5 C53 106.6(2) . . ? C111 O101 C113 106.6(2) . . ? C131 O103 C133 107.0(2) . . ? C151 O105 C153 104.8(2) . . ? C11 N1 C12 107.2(2) . . ? C11 N1 Ag1 133.7(2) . . ? C12 N1 Ag1 117.82(18) . . ? C31 N3 C32 107.3(2) . . ? C31 N3 Ag1 134.3(2) . 3_565 ? C32 N3 Ag1 118.21(19) . 3_565 ? C51 N5 C52 106.5(3) . . ? C51 N5 Ag2 131.4(2) . . ? C52 N5 Ag2 121.57(19) . . ? C111 N101 C112 106.5(3) . . ? C111 N101 Ag1 133.8(2) . . ? C112 N101 Ag1 116.88(19) . . ? C131 N103 C132 106.9(2) . . ? C131 N103 Ag2 137.1(2) . 3_666 ? C132 N103 Ag2 115.30(19) . 3_666 ? C151 N105 C152 106.2(2) . . ? C151 N105 Ag2 130.3(2) . . ? C152 N105 Ag2 118.6(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 C11 121.4(3) . . ? C2 C1 C11 119.0(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H1 120.1 . . ? C1 C2 H1 120.1 . . ? C2 C3 C4 120.8(3) . . ? C2 C3 C31 120.4(3) . . ? C4 C3 C31 118.9(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H2 120.2 . . ? C5 C4 H2 120.2 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 C51 122.3(3) . . ? C4 C5 C51 117.8(3) . . ? C5 C6 C1 120.4(3) . . ? C5 C6 H3 119.8 . . ? C1 C6 H3 119.8 . . ? N1 C11 O1 117.0(3) . . ? N1 C11 C1 128.3(3) . . ? O1 C11 C1 114.7(2) . . ? N1 C12 C13 103.5(2) . . ? N1 C12 H4 111.1 . . ? C13 C12 H4 111.1 . . ? N1 C12 H5 111.1 . . ? C13 C12 H5 111.1 . . ? H4 C12 H5 109.0 . . ? O1 C13 C12 103.1(3) . . ? O1 C13 H6 111.1 . . ? C12 C13 H6 111.1 . . ? O1 C13 H7 111.1 . . ? C12 C13 H7 111.1 . . ? H6 C13 H7 109.1 . . ? N3 C31 O3 117.6(3) . . ? N3 C31 C3 126.2(3) . . ? O3 C31 C3 116.2(3) . . ? N3 C32 C33 104.1(2) . . ? N3 C32 H8 110.9 . . ? C33 C32 H8 110.9 . . ? N3 C32 H9 110.9 . . ? C33 C32 H9 110.9 . . ? H8 C32 H9 109.0 . . ? O3 C33 C32 103.9(2) . . ? O3 C33 H10 111.0 . . ? C32 C33 H10 111.0 . . ? O3 C33 H11 111.0 . . ? C32 C33 H11 111.0 . . ? H10 C33 H11 109.0 . . ? N5 C51 O5 118.0(3) . . ? N5 C51 C5 126.7(3) . . ? O5 C51 C5 115.0(3) . . ? N5 C52 C53 104.6(3) . . ? N5 C52 H12 110.8 . . ? C53 C52 H12 110.8 . . ? N5 C52 H13 110.8 . . ? C53 C52 H13 110.8 . . ? H12 C52 H13 108.9 . . ? O5 C53 C52 103.6(2) . . ? O5 C53 H14 111.0 . . ? C52 C53 H14 111.0 . . ? O5 C53 H15 111.0 . . ? C52 C53 H15 111.0 . . ? H14 C53 H15 109.0 . . ? C106 C101 C102 119.7(3) . . ? C106 C101 C111 120.1(3) . . ? C102 C101 C111 120.2(3) . . ? C103 C102 C101 119.8(3) . . ? C103 C102 H16 120.1 . . ? C101 C102 H16 120.1 . . ? C104 C103 C102 120.3(3) . . ? C104 C103 C131 118.7(3) . . ? C102 C103 C131 121.0(3) . . ? C105 C104 C103 119.9(3) . . ? C105 C104 H17 120.0 . . ? C103 C104 H17 120.0 . . ? C104 C105 C106 119.8(3) . . ? C104 C105 C151 119.9(3) . . ? C106 C105 C151 120.3(3) . . ? C101 C106 C105 120.4(3) . . ? C101 C106 H18 119.8 . . ? C105 C106 H18 119.8 . . ? N101 C111 O101 118.1(3) . . ? N101 C111 C101 127.0(3) . . ? O101 C111 C101 114.9(2) . . ? N101 C112 C113 104.8(3) . . ? N101 C112 H19 110.8 . . ? C113 C112 H19 110.8 . . ? N101 C112 H20 110.8 . . ? C113 C112 H20 110.8 . . ? H19 C112 H20 108.9 . . ? O101 C113 C112 104.0(2) . . ? O101 C113 H21 111.0 . . ? C112 C113 H21 111.0 . . ? O101 C113 H22 111.0 . . ? C112 C113 H22 111.0 . . ? H21 C113 H22 109.0 . . ? N103 C131 O103 117.7(3) . . ? N103 C131 C103 127.3(3) . . ? O103 C131 C103 115.0(2) . . ? N103 C132 C133 104.3(2) . . ? N103 C132 H23 110.9 . . ? C133 C132 H23 110.9 . . ? N103 C132 H24 110.9 . . ? C133 C132 H24 110.9 . . ? H23 C132 H24 108.9 . . ? O103 C133 C132 103.6(2) . . ? O103 C133 H25 111.0 . . ? C132 C133 H25 111.0 . . ? O103 C133 H26 111.0 . . ? C132 C133 H26 111.0 . . ? H25 C133 H26 109.0 . . ? N105 C151 O105 117.7(3) . . ? N105 C151 C105 127.0(3) . . ? O105 C151 C105 115.4(3) . . ? N105 C152 C153 102.9(2) . . ? N105 C152 H27 111.2 . . ? C153 C152 H27 111.2 . . ? N105 C152 H28 111.2 . . ? C153 C152 H28 111.2 . . ? H27 C152 H28 109.1 . . ? O105 C153 C152 103.0(2) . . ? O105 C153 H29 111.2 . . ? C152 C153 H29 111.2 . . ? O105 C153 H30 111.2 . . ? C152 C153 H30 111.2 . . ? H29 C153 H30 109.1 . . ? 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 N3 Ag1 N1 C11 20.7(4) 3_565 . . . ? N101 Ag1 N1 C11 -151.5(3) . . . . ? N3 Ag1 N1 C12 -144.1(2) 3_565 . . . ? N101 Ag1 N1 C12 43.7(2) . . . . ? N103 Ag2 N5 C51 -130.5(3) 3_666 . . . ? N105 Ag2 N5 C51 39.2(3) . . . . ? N103 Ag2 N5 C52 58.8(2) 3_666 . . . ? N105 Ag2 N5 C52 -131.4(2) . . . . ? N1 Ag1 N101 C111 18.2(3) . . . . ? N3 Ag1 N101 C111 -157.0(3) 3_565 . . . ? N1 Ag1 N101 C112 -139.9(2) . . . . ? N3 Ag1 N101 C112 44.8(3) 3_565 . . . ? N103 Ag2 N105 C151 -12.7(4) 3_666 . . . ? N5 Ag2 N105 C151 -176.1(3) . . . . ? N103 Ag2 N105 C152 -164.1(2) 3_666 . . . ? N5 Ag2 N105 C152 32.5(2) . . . . ? C6 C1 C2 C3 -2.5(4) . . . . ? C11 C1 C2 C3 179.5(3) . . . . ? C1 C2 C3 C4 2.3(4) . . . . ? C1 C2 C3 C31 -178.4(3) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C31 C3 C4 C5 -179.0(3) . . . . ? C3 C4 C5 C6 -2.8(4) . . . . ? C3 C4 C5 C51 172.2(3) . . . . ? C4 C5 C6 C1 2.6(4) . . . . ? C51 C5 C6 C1 -172.2(3) . . . . ? C2 C1 C6 C5 0.1(4) . . . . ? C11 C1 C6 C5 177.9(3) . . . . ? C12 N1 C11 O1 2.6(4) . . . . ? Ag1 N1 C11 O1 -163.4(2) . . . . ? C12 N1 C11 C1 -175.7(3) . . . . ? Ag1 N1 C11 C1 18.3(5) . . . . ? C13 O1 C11 N1 8.9(4) . . . . ? C13 O1 C11 C1 -172.6(3) . . . . ? C6 C1 C11 N1 15.0(5) . . . . ? C2 C1 C11 N1 -167.1(3) . . . . ? C6 C1 C11 O1 -163.4(3) . . . . ? C2 C1 C11 O1 14.5(4) . . . . ? C11 N1 C12 C13 -12.3(3) . . . . ? Ag1 N1 C12 C13 156.3(2) . . . . ? C11 O1 C13 C12 -15.6(3) . . . . ? N1 C12 C13 O1 16.6(3) . . . . ? C32 N3 C31 O3 -1.7(4) . . . . ? Ag1 N3 C31 O3 -175.9(2) 3_565 . . . ? C32 N3 C31 C3 177.4(3) . . . . ? Ag1 N3 C31 C3 3.2(5) 3_565 . . . ? C33 O3 C31 N3 -5.0(4) . . . . ? C33 O3 C31 C3 175.9(3) . . . . ? C2 C3 C31 N3 137.1(3) . . . . ? C4 C3 C31 N3 -43.5(4) . . . . ? C2 C3 C31 O3 -43.8(4) . . . . ? C4 C3 C31 O3 135.5(3) . . . . ? C31 N3 C32 C33 7.3(3) . . . . ? Ag1 N3 C32 C33 -177.5(2) 3_565 . . . ? C31 O3 C33 C32 9.0(3) . . . . ? N3 C32 C33 O3 -9.7(3) . . . . ? C52 N5 C51 O5 -4.0(4) . . . . ? Ag2 N5 C51 O5 -175.69(19) . . . . ? C52 N5 C51 C5 169.8(3) . . . . ? Ag2 N5 C51 C5 -1.8(5) . . . . ? C53 O5 C51 N5 -1.1(4) . . . . ? C53 O5 C51 C5 -175.7(3) . . . . ? C6 C5 C51 N5 28.5(5) . . . . ? C4 C5 C51 N5 -146.4(3) . . . . ? C6 C5 C51 O5 -157.4(3) . . . . ? C4 C5 C51 O5 27.6(4) . . . . ? C51 N5 C52 C53 7.1(3) . . . . ? Ag2 N5 C52 C53 179.76(19) . . . . ? C51 O5 C53 C52 5.5(3) . . . . ? N5 C52 C53 O5 -7.5(3) . . . . ? C106 C101 C102 C103 -1.9(4) . . . . ? C111 C101 C102 C103 178.9(3) . . . . ? C101 C102 C103 C104 -0.2(4) . . . . ? C101 C102 C103 C131 -179.5(3) . . . . ? C102 C103 C104 C105 2.5(4) . . . . ? C131 C103 C104 C105 -178.2(3) . . . . ? C103 C104 C105 C106 -2.7(4) . . . . ? C103 C104 C105 C151 176.7(3) . . . . ? C102 C101 C106 C105 1.7(4) . . . . ? C111 C101 C106 C105 -179.1(3) . . . . ? C104 C105 C106 C101 0.6(4) . . . . ? C151 C105 C106 C101 -178.8(3) . . . . ? C112 N101 C111 O101 0.6(4) . . . . ? Ag1 N101 C111 O101 -159.1(2) . . . . ? C112 N101 C111 C101 -178.8(3) . . . . ? Ag1 N101 C111 C101 21.5(5) . . . . ? C113 O101 C111 N101 1.0(4) . . . . ? C113 O101 C111 C101 -179.5(3) . . . . ? C106 C101 C111 N101 13.8(5) . . . . ? C102 C101 C111 N101 -166.9(3) . . . . ? C106 C101 C111 O101 -165.6(3) . . . . ? C102 C101 C111 O101 13.6(4) . . . . ? C111 N101 C112 C113 -1.9(4) . . . . ? Ag1 N101 C112 C113 161.8(2) . . . . ? C111 O101 C113 C112 -2.2(4) . . . . ? N101 C112 C113 O101 2.5(4) . . . . ? C132 N103 C131 O103 -1.0(4) . . . . ? Ag2 N103 C131 O103 168.5(2) 3_666 . . . ? C132 N103 C131 C103 178.5(3) . . . . ? Ag2 N103 C131 C103 -11.9(5) 3_666 . . . ? C133 O103 C131 N103 5.2(4) . . . . ? C133 O103 C131 C103 -174.4(3) . . . . ? C104 C103 C131 N103 157.5(3) . . . . ? C102 C103 C131 N103 -23.2(5) . . . . ? C104 C103 C131 O103 -23.0(4) . . . . ? C102 C103 C131 O103 156.4(3) . . . . ? C131 N103 C132 C133 -3.3(4) . . . . ? Ag2 N103 C132 C133 -175.5(2) 3_666 . . . ? C131 O103 C133 C132 -6.6(3) . . . . ? N103 C132 C133 O103 6.0(3) . . . . ? C152 N105 C151 O105 5.3(4) . . . . ? Ag2 N105 C151 O105 -148.7(2) . . . . ? C152 N105 C151 C105 -174.8(3) . . . . ? Ag2 N105 C151 C105 31.2(5) . . . . ? C153 O105 C151 N105 10.0(4) . . . . ? C153 O105 C151 C105 -169.9(3) . . . . ? C104 C105 C151 N105 -165.3(3) . . . . ? C106 C105 C151 N105 14.1(5) . . . . ? C104 C105 C151 O105 14.6(4) . . . . ? C106 C105 C151 O105 -166.0(3) . . . . ? C151 N105 C152 C153 -17.6(3) . . . . ? Ag2 N105 C152 C153 140.0(2) . . . . ? C151 O105 C153 C152 -20.0(3) . . . . ? N105 C152 C153 O105 22.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.037 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.095 #====END data_7 _database_code_depnum_ccdc_archive 'CCDC 644139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H39 Ag3 Cl3 N9 O18' _chemical_formula_sum 'C36 H39 Ag3 Cl3 N9 O18' _chemical_formula_weight 1315.72 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 trigonal _symmetry_space_group_name_H-M R3C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 24.013(2) _cell_length_b 24.013(2) _cell_length_c 14.319(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7150.5(12) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3342 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 20.95 _exptl_crystal_description NEEDLE _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3924 _exptl_absorpt_coefficient_mu 1.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5389 _exptl_absorpt_correction_T_max 0.9170 _exptl_absorpt_process_details 'SADABS(Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13663 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3425 _reflns_number_gt 3003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+29.5321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(8) _refine_ls_number_reflns 3425 _refine_ls_number_parameters 183 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1855 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.81556(4) 0.96362(4) -0.09415(8) 0.0595(3) Uani 1 1 d . . . Cl1 Cl 0.71031(12) 0.83339(12) -0.2540(2) 0.0595(6) Uani 1 1 d . . . O1 O 0.8627(4) 0.8420(4) 0.0776(7) 0.066(2) Uani 1 1 d . . . O2 O 0.9604(4) 1.1253(4) -0.2569(8) 0.077(3) Uani 1 1 d . . . O3 O 0.6629(8) 0.8259(8) -0.3139(11) 0.135(5) Uiso 1 1 d . . . O4 O 0.7055(9) 0.8677(9) -0.1774(16) 0.165(6) Uiso 1 1 d . . . O5 O 0.7053(6) 0.7761(7) -0.2170(9) 0.114(4) Uiso 1 1 d . . . O6 O 0.7703(10) 0.8847(10) -0.2709(16) 0.184(8) Uiso 1 1 d . . . N1 N 0.8231(4) 0.8926(4) -0.0082(6) 0.0496(18) Uani 1 1 d . . . N2 N 0.8755(4) 1.0483(4) -0.1823(7) 0.0529(19) Uani 1 1 d . . . N3 N 0.7420(9) 0.9877(8) -0.0296(11) 0.106(4) Uani 1 1 d . . . C1 C 0.9489(4) 1.0124(5) 0.0356(6) 0.046(2) Uani 1 1 d . . . H1A H 0.9149 1.0203 0.0415 0.056 Uiso 1 1 calc R . . C2 C 0.9369(4) 0.9483(5) 0.0311(6) 0.045(2) Uani 1 1 d . . . C3 C 0.8710(5) 0.8934(4) 0.0315(7) 0.046(2) Uani 1 1 d . . . C4 C 0.7674(6) 0.8269(5) 0.0103(9) 0.066(3) Uani 1 1 d . . . H4A H 0.7326 0.8295 0.0403 0.079 Uiso 1 1 calc R . . H4B H 0.7516 0.8028 -0.0474 0.079 Uiso 1 1 calc R . . C5 C 0.7934(6) 0.7966(7) 0.0723(16) 0.099(5) Uani 1 1 d . . . H5A H 0.7851 0.7557 0.0470 0.118 Uiso 1 1 calc R . . H5B H 0.7740 0.7894 0.1338 0.118 Uiso 1 1 calc R . . C6 C 0.9334(4) 0.9657(4) -0.2218(6) 0.0366(16) Uani 1 1 d . . . H6A H 0.8888 0.9426 -0.2258 0.044 Uiso 1 1 calc R . . C7 C 0.9656(4) 1.0316(4) -0.2188(5) 0.0345(16) Uani 1 1 d . . . C8 C 0.9305(4) 1.0680(5) -0.2173(7) 0.045(2) Uani 1 1 d . . . C9 C 0.8609(6) 1.1008(5) -0.1961(11) 0.071(3) Uani 1 1 d . . . H9A H 0.8540 1.1158 -0.1367 0.086 Uiso 1 1 calc R . . H9B H 0.8228 1.0864 -0.2345 0.086 Uiso 1 1 calc R . . C10 C 0.9187(6) 1.1525(7) -0.2441(12) 0.080 Uani 1 1 d . . . H10A H 0.9072 1.1631 -0.3038 0.096 Uiso 1 1 calc R . . H10B H 0.9395 1.1910 -0.2059 0.096 Uiso 1 1 calc R . . C11 C 0.7165(7) 1.0017(7) 0.0293(11) 0.077(3) Uani 1 1 d . . . C12 C 0.6855(6) 1.0160(7) 0.1001(10) 0.072(3) Uani 1 1 d . . . H12A H 0.6424 1.0029 0.0810 0.108 Uiso 1 1 calc R . . H12B H 0.7085 1.0614 0.1119 0.108 Uiso 1 1 calc R . . H12C H 0.6845 0.9934 0.1560 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0568(5) 0.0589(5) 0.0694(5) 0.0068(4) 0.0037(4) 0.0338(4) Cl1 0.0435(12) 0.0532(13) 0.0758(16) 0.0015(12) -0.0045(11) 0.0199(11) O1 0.056(4) 0.051(4) 0.084(6) 0.019(4) -0.001(4) 0.020(3) O2 0.049(4) 0.040(4) 0.135(9) 0.024(5) 0.003(4) 0.018(3) N1 0.037(4) 0.051(4) 0.055(5) 0.004(4) 0.008(3) 0.018(3) N2 0.053(5) 0.043(4) 0.065(5) -0.003(4) -0.006(4) 0.026(4) N3 0.128(12) 0.114(10) 0.109(11) -0.005(8) 0.007(9) 0.087(10) C1 0.045(5) 0.063(6) 0.037(4) -0.011(4) -0.003(4) 0.030(4) C2 0.048(5) 0.056(5) 0.033(4) 0.008(4) 0.003(4) 0.027(4) C3 0.047(5) 0.043(5) 0.046(5) 0.002(4) 0.012(4) 0.022(4) C4 0.059(6) 0.052(6) 0.073(8) 0.005(5) 0.008(5) 0.018(5) C5 0.050(7) 0.063(8) 0.161(16) 0.041(9) 0.017(8) 0.012(6) C6 0.032(4) 0.037(4) 0.040(4) -0.001(3) -0.003(3) 0.016(3) C7 0.035(4) 0.039(4) 0.030(4) 0.005(3) 0.000(3) 0.019(3) C8 0.043(5) 0.050(5) 0.048(5) -0.005(4) -0.016(4) 0.028(4) C9 0.058(6) 0.057(6) 0.116(11) 0.001(6) 0.001(6) 0.042(5) C10 0.055 0.064 0.131 0.027 -0.006 0.038 C11 0.071(8) 0.077(8) 0.087(9) 0.004(7) -0.006(7) 0.040(7) C12 0.069(7) 0.089(9) 0.067(8) -0.006(6) 0.007(6) 0.046(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 2.183(8) . ? Ag1 N2 2.207(9) . ? Ag1 N3 2.308(15) . ? Cl1 O3 1.365(16) . ? Cl1 O6 1.37(2) . ? Cl1 O4 1.41(2) . ? Cl1 O5 1.421(15) . ? O1 C3 1.324(13) . ? O1 C5 1.465(15) . ? O2 C8 1.319(13) . ? O2 C10 1.454(14) . ? N1 C3 1.274(13) . ? N1 C4 1.496(13) . ? N2 C8 1.263(13) . ? N2 C9 1.481(12) . ? N3 C11 1.19(2) . ? C1 C2 1.382(14) 3_675 ? C1 C2 1.420(14) . ? C1 H1A 0.9300 . ? C2 C1 1.382(14) 2_765 ? C2 C3 1.467(14) . ? C4 C5 1.47(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.372(12) . ? C6 C7 1.388(12) 2_765 ? C6 H6A 0.9300 . ? C7 C6 1.388(12) 3_675 ? C7 C8 1.487(11) . ? C9 C10 1.489(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.40(2) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 140.4(3) . . ? N1 Ag1 N3 110.1(4) . . ? N2 Ag1 N3 103.1(4) . . ? O3 Cl1 O6 116.1(11) . . ? O3 Cl1 O4 104.9(11) . . ? O6 Cl1 O4 88.2(12) . . ? O3 Cl1 O5 116.5(9) . . ? O6 Cl1 O5 118.6(11) . . ? O4 Cl1 O5 106.6(10) . . ? C3 O1 C5 104.7(9) . . ? C8 O2 C10 106.1(9) . . ? C3 N1 C4 105.1(8) . . ? C3 N1 Ag1 131.8(6) . . ? C4 N1 Ag1 123.0(7) . . ? C8 N2 C9 106.0(9) . . ? C8 N2 Ag1 130.6(7) . . ? C9 N2 Ag1 122.5(8) . . ? C11 N3 Ag1 157.6(14) . . ? C2 C1 C2 119.7(9) 3_675 . ? C2 C1 H1A 120.1 3_675 . ? C2 C1 H1A 120.1 . . ? C1 C2 C1 119.9(9) 2_765 . ? C1 C2 C3 118.7(9) 2_765 . ? C1 C2 C3 121.1(8) . . ? N1 C3 O1 119.6(8) . . ? N1 C3 C2 124.8(9) . . ? O1 C3 C2 115.6(9) . . ? C5 C4 N1 104.6(10) . . ? C5 C4 H4A 110.8 . . ? N1 C4 H4A 110.8 . . ? C5 C4 H4B 110.8 . . ? N1 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C4 C5 O1 105.6(10) . . ? C4 C5 H5A 110.6 . . ? O1 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? O1 C5 H5B 110.6 . . ? H5A C5 H5B 108.8 . . ? C7 C6 C7 119.1(8) . 2_765 ? C7 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 2_765 . ? C6 C7 C6 120.7(8) . 3_675 ? C6 C7 C8 121.4(8) . . ? C6 C7 C8 117.8(7) 3_675 . ? N2 C8 O2 118.8(8) . . ? N2 C8 C7 125.3(9) . . ? O2 C8 C7 115.8(8) . . ? N2 C9 C10 104.7(9) . . ? N2 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? N2 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? O2 C10 C9 104.3(9) . . ? O2 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? O2 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? N3 C11 C12 178.0(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 C3 21.8(12) . . . . ? N3 Ag1 N1 C3 -123.4(10) . . . . ? N2 Ag1 N1 C4 -154.1(7) . . . . ? N3 Ag1 N1 C4 60.7(9) . . . . ? N1 Ag1 N2 C8 15.9(12) . . . . ? N3 Ag1 N2 C8 162.5(10) . . . . ? N1 Ag1 N2 C9 -151.9(8) . . . . ? N3 Ag1 N2 C9 -5.3(10) . . . . ? N1 Ag1 N3 C11 48(4) . . . . ? N2 Ag1 N3 C11 -110(4) . . . . ? C2 C1 C2 C1 9.1(18) 3_675 . . 2_765 ? C2 C1 C2 C3 -177.3(6) 3_675 . . . ? C4 N1 C3 O1 -1.0(13) . . . . ? Ag1 N1 C3 O1 -177.4(7) . . . . ? C4 N1 C3 C2 179.2(9) . . . . ? Ag1 N1 C3 C2 2.8(15) . . . . ? C5 O1 C3 N1 -3.3(16) . . . . ? C5 O1 C3 C2 176.6(11) . . . . ? C1 C2 C3 N1 -150.0(10) 2_765 . . . ? C1 C2 C3 N1 36.3(14) . . . . ? C1 C2 C3 O1 30.2(13) 2_765 . . . ? C1 C2 C3 O1 -143.5(9) . . . . ? C3 N1 C4 C5 4.8(14) . . . . ? Ag1 N1 C4 C5 -178.4(11) . . . . ? N1 C4 C5 O1 -6.5(17) . . . . ? C3 O1 C5 C4 6.0(17) . . . . ? C7 C6 C7 C6 6.2(16) 2_765 . . 3_675 ? C7 C6 C7 C8 -177.1(6) 2_765 . . . ? C9 N2 C8 O2 -1.1(14) . . . . ? Ag1 N2 C8 O2 -170.5(8) . . . . ? C9 N2 C8 C7 179.3(9) . . . . ? Ag1 N2 C8 C7 9.9(15) . . . . ? C10 O2 C8 N2 2.5(15) . . . . ? C10 O2 C8 C7 -177.9(10) . . . . ? C6 C7 C8 N2 30.1(14) . . . . ? C6 C7 C8 N2 -153.1(9) 3_675 . . . ? C6 C7 C8 O2 -149.5(9) . . . . ? C6 C7 C8 O2 27.3(12) 3_675 . . . ? C8 N2 C9 C10 -0.7(14) . . . . ? Ag1 N2 C9 C10 169.7(9) . . . . ? C8 O2 C10 C9 -2.5(15) . . . . ? N2 C9 C10 O2 1.9(15) . . . . ? Ag1 N3 C11 C12 -71(48) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.064 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.137 #====END