# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Tapan Paine' _publ_contact_author_email ICTKP@IACS.RES.IN _publ_section_title ; Self-Assembly of Silver(I) and Bis-Bidentate N,N-Donor Ligands: >From a Tetranuclear Complex to Coordination Polymers ; loop_ _publ_author_name 'Tapan Paine' 'Partha Halder' 'Ennio Zangrando' # Attachment 'Ag-comp1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 715094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Ag N4 1+, B F4 1-' _chemical_formula_sum 'C20 H18 Ag B F4 N4' _chemical_formula_weight 509.06 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.664(3) _cell_length_b 17.641(4) _cell_length_c 10.200(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.34(3) _cell_angle_gamma 90.00 _cell_volume 2042.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1323 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24611 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.73 _reflns_number_total 4203 _reflns_number_gt 2530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4203 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.26352(3) 0.40094(2) 0.48031(4) 0.0934(2) Uani 1 1 d . . . N1 N 0.4026(3) 0.4496(2) 0.3679(4) 0.0776(9) Uani 1 1 d . . . N2 N 0.4436(3) 0.3371(2) 0.5611(4) 0.0783(9) Uani 1 1 d . . . N3 N 0.0931(3) 0.1686(2) 0.8876(4) 0.0801(9) Uani 1 1 d . . . N4 N 0.1145(3) 0.0640(2) 1.0909(4) 0.0752(9) Uani 1 1 d . . . C1 C 0.3881(5) 0.5025(3) 0.2743(5) 0.0901(13) Uani 1 1 d . . . H1 H 0.3208 0.5325 0.2613 0.108 Uiso 1 1 calc R . . C2 C 0.4658(5) 0.5159(3) 0.1951(6) 0.1024(16) Uani 1 1 d . . . H2 H 0.4523 0.5551 0.1324 0.123 Uiso 1 1 calc R . . C3 C 0.5638(5) 0.4711(3) 0.2091(6) 0.1000(15) Uani 1 1 d . . . H3 H 0.6166 0.4774 0.1541 0.120 Uiso 1 1 calc R . . C4 C 0.5810(5) 0.4163(3) 0.3083(6) 0.0869(13) Uani 1 1 d . . . H4 H 0.6481 0.3860 0.3233 0.104 Uiso 1 1 calc R . . C5 C 0.5005(4) 0.4063(2) 0.3839(5) 0.0754(11) Uani 1 1 d . . . C6 C 0.5173(4) 0.3478(2) 0.4902(5) 0.0793(11) Uani 1 1 d . . . H6 H 0.5846 0.3178 0.5053 0.095 Uiso 1 1 calc R . . C7 C 0.4667(4) 0.2771(3) 0.6632(5) 0.0891(13) Uani 1 1 d . . . H7A H 0.4847 0.2992 0.7527 0.107 Uiso 1 1 calc R . . H7B H 0.5336 0.2468 0.6532 0.107 Uiso 1 1 calc R . . C8 C 0.3568(4) 0.2275(2) 0.6442(5) 0.0817(12) Uani 1 1 d . . . C9 C 0.2717(4) 0.2451(2) 0.7108(4) 0.0799(12) Uani 1 1 d . . . H9 H 0.2833 0.2859 0.7703 0.096 Uiso 1 1 calc R . . C10 C 0.1679(4) 0.2036(3) 0.6919(5) 0.0884(13) Uani 1 1 d . . . C11 C 0.1533(5) 0.1440(3) 0.5999(6) 0.1016(16) Uani 1 1 d . . . H11 H 0.0832 0.1166 0.5815 0.122 Uiso 1 1 calc R . . C12 C 0.2400(6) 0.1253(4) 0.5368(6) 0.112(2) Uani 1 1 d . . . H12 H 0.2307 0.0836 0.4796 0.134 Uiso 1 1 calc R . . C13 C 0.3412(5) 0.1679(3) 0.5572(5) 0.0959(14) Uani 1 1 d . . . H13 H 0.3992 0.1559 0.5114 0.115 Uiso 1 1 calc R . . C14 C 0.0773(4) 0.2206(3) 0.7710(6) 0.0938(14) Uani 1 1 d . . . H14A H 0.0854 0.2726 0.8023 0.113 Uiso 1 1 calc R . . H14B H -0.0011 0.2143 0.7139 0.113 Uiso 1 1 calc R . . C15 C 0.0096(4) 0.1609(2) 0.9469(5) 0.0814(12) Uani 1 1 d . . . H15 H -0.0597 0.1882 0.9168 0.098 Uiso 1 1 calc R . . C16 C 0.0199(4) 0.1098(2) 1.0617(5) 0.0730(11) Uani 1 1 d . . . C17 C -0.0663(5) 0.1077(3) 1.1342(6) 0.0895(14) Uani 1 1 d . . . H17 H -0.1320 0.1390 1.1110 0.107 Uiso 1 1 calc R . . C18 C -0.0537(5) 0.0587(4) 1.2412(6) 0.1012(16) Uani 1 1 d . . . H18 H -0.1096 0.0579 1.2931 0.121 Uiso 1 1 calc R . . C19 C 0.0398(5) 0.0117(3) 1.2709(6) 0.0960(15) Uani 1 1 d . . . H19 H 0.0485 -0.0224 1.3420 0.115 Uiso 1 1 calc R . . C20 C 0.1231(4) 0.0154(3) 1.1927(5) 0.0871(13) Uani 1 1 d . . . H20 H 0.1872 -0.0173 1.2124 0.105 Uiso 1 1 calc R . . B1 B 0.7527(6) 0.1681(5) 0.5127(8) 0.1010(19) Uani 1 1 d . . . F1 F 0.6358(4) 0.1658(2) 0.4866(5) 0.1581(16) Uani 1 1 d . . . F2 F 0.7870(6) 0.1409(7) 0.6383(13) 0.337(7) Uani 1 1 d . . . F3 F 0.7890(6) 0.2351(4) 0.5077(7) 0.236(3) Uani 1 1 d . . . F4 F 0.7946(10) 0.1198(8) 0.4517(14) 0.398(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0614(3) 0.1170(4) 0.1087(4) -0.0090(2) 0.0338(2) -0.00399(16) N1 0.0643(19) 0.085(2) 0.088(3) -0.0020(19) 0.0270(18) 0.0009(17) N2 0.065(2) 0.091(2) 0.081(2) -0.0015(18) 0.0208(18) -0.0090(16) N3 0.063(2) 0.088(2) 0.090(3) 0.0117(18) 0.0205(18) 0.0023(17) N4 0.0597(18) 0.082(2) 0.089(3) -0.0023(18) 0.0278(17) -0.0045(16) C1 0.081(3) 0.089(3) 0.101(4) 0.002(3) 0.022(3) 0.004(2) C2 0.092(4) 0.107(3) 0.107(4) 0.019(3) 0.022(3) -0.011(3) C3 0.086(3) 0.124(4) 0.096(4) 0.003(3) 0.033(3) -0.020(3) C4 0.066(3) 0.106(3) 0.094(4) 0.000(3) 0.030(2) -0.003(2) C5 0.063(2) 0.082(2) 0.083(3) -0.006(2) 0.022(2) -0.0060(19) C6 0.062(2) 0.085(3) 0.091(3) -0.001(2) 0.019(2) 0.0016(19) C7 0.072(3) 0.107(3) 0.088(3) 0.012(3) 0.016(2) -0.007(2) C8 0.082(3) 0.088(3) 0.075(3) 0.014(2) 0.018(2) -0.001(2) C9 0.076(3) 0.083(3) 0.079(3) 0.010(2) 0.014(2) -0.002(2) C10 0.083(3) 0.097(3) 0.084(3) 0.025(2) 0.016(2) -0.002(2) C11 0.103(4) 0.113(4) 0.088(3) 0.004(3) 0.019(3) -0.037(3) C12 0.142(6) 0.103(4) 0.093(4) -0.008(3) 0.035(4) -0.022(3) C13 0.104(4) 0.103(3) 0.084(3) 0.007(3) 0.028(3) -0.005(3) C14 0.077(3) 0.100(3) 0.105(4) 0.025(3) 0.021(3) 0.008(2) C15 0.064(2) 0.080(2) 0.102(3) 0.000(2) 0.021(2) 0.0045(19) C16 0.063(2) 0.076(2) 0.084(3) -0.0096(19) 0.027(2) -0.0075(18) C17 0.071(3) 0.101(3) 0.104(4) -0.011(3) 0.034(3) -0.007(2) C18 0.087(3) 0.127(4) 0.104(4) -0.012(3) 0.053(3) -0.022(3) C19 0.086(3) 0.106(3) 0.100(4) 0.005(3) 0.031(3) -0.018(3) C20 0.080(3) 0.091(3) 0.095(3) 0.009(2) 0.030(3) -0.007(2) B1 0.087(4) 0.111(5) 0.107(5) -0.008(4) 0.026(4) -0.008(3) F1 0.119(3) 0.160(3) 0.190(4) -0.023(3) 0.023(3) -0.010(3) F2 0.154(6) 0.398(12) 0.441(15) 0.244(12) 0.031(8) 0.030(7) F3 0.210(6) 0.209(6) 0.283(8) 0.026(5) 0.046(5) -0.105(5) F4 0.279(12) 0.507(19) 0.463(18) -0.243(15) 0.196(13) 0.058(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N3 2.342(4) 4_565 ? Ag N1 2.354(4) . ? Ag N2 2.358(4) . ? Ag N4 2.362(3) 4_565 ? N1 C1 1.318(6) . ? N1 C5 1.352(6) . ? N2 C6 1.258(6) . ? N2 C7 1.466(6) . ? N3 C15 1.267(6) . ? N3 C14 1.479(6) . ? N3 Ag 2.342(4) 4_566 ? N4 C20 1.333(6) . ? N4 C16 1.344(6) . ? N4 Ag 2.362(3) 4_566 ? C1 C2 1.366(8) . ? C2 C3 1.371(8) . ? C3 C4 1.380(7) . ? C4 C5 1.358(8) . ? C5 C6 1.477(7) . ? C7 C8 1.528(6) . ? C8 C13 1.361(7) . ? C8 C9 1.362(7) . ? C9 C10 1.390(6) . ? C10 C11 1.393(7) . ? C10 C14 1.501(8) . ? C11 C12 1.359(9) . ? C12 C13 1.375(8) . ? C15 C16 1.460(7) . ? C16 C17 1.379(7) . ? C17 C18 1.373(8) . ? C18 C19 1.347(8) . ? C19 C20 1.393(7) . ? B1 F4 1.221(10) . ? B1 F3 1.261(10) . ? B1 F1 1.328(8) . ? B1 F2 1.339(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag N1 127.63(14) 4_565 . ? N3 Ag N2 119.71(14) 4_565 . ? N1 Ag N2 71.70(13) . . ? N3 Ag N4 71.35(13) 4_565 4_565 ? N1 Ag N4 143.40(13) . 4_565 ? N2 Ag N4 130.72(13) . 4_565 ? C1 N1 C5 116.8(4) . . ? C1 N1 Ag 128.6(3) . . ? C5 N1 Ag 113.1(3) . . ? C6 N2 C7 118.6(4) . . ? C6 N2 Ag 113.5(3) . . ? C7 N2 Ag 126.6(3) . . ? C15 N3 C14 119.0(4) . . ? C15 N3 Ag 115.1(3) . 4_566 ? C14 N3 Ag 125.9(3) . 4_566 ? C20 N4 C16 118.0(4) . . ? C20 N4 Ag 127.6(3) . 4_566 ? C16 N4 Ag 113.2(3) . 4_566 ? N1 C1 C2 124.0(5) . . ? C1 C2 C3 119.3(5) . . ? C2 C3 C4 117.2(5) . . ? C5 C4 C3 120.3(5) . . ? N1 C5 C4 122.3(5) . . ? N1 C5 C6 116.7(4) . . ? C4 C5 C6 121.1(4) . . ? N2 C6 C5 122.3(4) . . ? N2 C7 C8 108.2(4) . . ? C13 C8 C9 120.0(5) . . ? C13 C8 C7 120.5(5) . . ? C9 C8 C7 119.5(4) . . ? C8 C9 C10 121.4(5) . . ? C9 C10 C11 117.3(5) . . ? C9 C10 C14 121.3(5) . . ? C11 C10 C14 121.4(5) . . ? C12 C11 C10 120.9(5) . . ? C11 C12 C13 120.2(6) . . ? C8 C13 C12 120.1(6) . . ? N3 C14 C10 109.7(4) . . ? N3 C15 C16 121.3(4) . . ? N4 C16 C17 121.9(5) . . ? N4 C16 C15 117.4(4) . . ? C17 C16 C15 120.7(4) . . ? C18 C17 C16 119.1(5) . . ? C19 C18 C17 119.9(5) . . ? C18 C19 C20 118.5(5) . . ? N4 C20 C19 122.7(5) . . ? F4 B1 F3 117.1(11) . . ? F4 B1 F1 112.9(8) . . ? F3 B1 F1 111.1(7) . . ? F4 B1 F2 99.9(11) . . ? F3 B1 F2 110.2(8) . . ? F1 B1 F2 104.3(7) . . ? 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 Ag N1 C1 65.4(4) 4_565 . . . ? N2 Ag N1 C1 179.3(4) . . . . ? N4 Ag N1 C1 -45.7(5) 4_565 . . . ? N3 Ag N1 C5 -100.1(3) 4_565 . . . ? N2 Ag N1 C5 13.7(3) . . . . ? N4 Ag N1 C5 148.7(3) 4_565 . . . ? N3 Ag N2 C6 110.4(3) 4_565 . . . ? N1 Ag N2 C6 -13.1(3) . . . . ? N4 Ag N2 C6 -159.3(3) 4_565 . . . ? N3 Ag N2 C7 -56.3(4) 4_565 . . . ? N1 Ag N2 C7 -179.8(4) . . . . ? N4 Ag N2 C7 34.0(4) 4_565 . . . ? C5 N1 C1 C2 -0.6(7) . . . . ? Ag N1 C1 C2 -165.7(4) . . . . ? N1 C1 C2 C3 2.0(9) . . . . ? C1 C2 C3 C4 -2.9(8) . . . . ? C2 C3 C4 C5 2.5(8) . . . . ? C1 N1 C5 C4 0.2(7) . . . . ? Ag N1 C5 C4 167.5(4) . . . . ? C1 N1 C5 C6 179.2(4) . . . . ? Ag N1 C5 C6 -13.4(5) . . . . ? C3 C4 C5 N1 -1.2(8) . . . . ? C3 C4 C5 C6 179.8(5) . . . . ? C7 N2 C6 C5 179.3(4) . . . . ? Ag N2 C6 C5 11.4(6) . . . . ? N1 C5 C6 N2 1.4(7) . . . . ? C4 C5 C6 N2 -179.5(5) . . . . ? C6 N2 C7 C8 -129.3(5) . . . . ? Ag N2 C7 C8 36.8(5) . . . . ? N2 C7 C8 C13 87.3(5) . . . . ? N2 C7 C8 C9 -90.0(5) . . . . ? C13 C8 C9 C10 -0.2(7) . . . . ? C7 C8 C9 C10 177.1(4) . . . . ? C8 C9 C10 C11 -1.2(6) . . . . ? C8 C9 C10 C14 176.6(4) . . . . ? C9 C10 C11 C12 3.2(8) . . . . ? C14 C10 C11 C12 -174.7(5) . . . . ? C10 C11 C12 C13 -3.7(9) . . . . ? C9 C8 C13 C12 -0.3(7) . . . . ? C7 C8 C13 C12 -177.5(5) . . . . ? C11 C12 C13 C8 2.2(9) . . . . ? C15 N3 C14 C10 -162.7(4) . . . . ? Ag N3 C14 C10 18.8(6) 4_566 . . . ? C9 C10 C14 N3 -96.9(5) . . . . ? C11 C10 C14 N3 80.8(6) . . . . ? C14 N3 C15 C16 179.4(4) . . . . ? Ag N3 C15 C16 -2.0(6) 4_566 . . . ? C20 N4 C16 C17 0.3(6) . . . . ? Ag N4 C16 C17 -167.8(4) 4_566 . . . ? C20 N4 C16 C15 -177.9(4) . . . . ? Ag N4 C16 C15 14.0(5) 4_566 . . . ? N3 C15 C16 N4 -8.6(6) . . . . ? N3 C15 C16 C17 173.2(5) . . . . ? N4 C16 C17 C18 1.6(7) . . . . ? C15 C16 C17 C18 179.7(5) . . . . ? C16 C17 C18 C19 -2.4(8) . . . . ? C17 C18 C19 C20 1.3(8) . . . . ? C16 N4 C20 C19 -1.5(7) . . . . ? Ag N4 C20 C19 164.7(4) 4_566 . . . ? C18 C19 C20 N4 0.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.086 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.111 # Attachment 'Ag-comp2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 715095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 Ag N4 1+, Cl O4 1-' _chemical_formula_sum 'C22 H26 Ag Cl N4 O4' _chemical_formula_weight 553.79 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.709(3) _cell_length_b 13.440(4) _cell_length_c 18.810(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2201.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Bruker (2000) SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD' _diffrn_measurement_method 'w/ and f/ scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24272 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5020 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.1-0 (Bruker AXS)' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(2) _refine_ls_number_reflns 5020 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.44346(3) 0.228006(17) 0.147691(13) 0.02624(7) Uani 1 1 d . . . N1 N 0.3631(3) 0.0563(2) 0.11119(14) 0.0286(6) Uani 1 1 d . . . N2 N 0.2022(3) 0.23987(18) 0.09306(12) 0.0220(5) Uani 1 1 d . . . N3 N 0.3728(3) 0.66705(17) 0.26335(13) 0.0216(5) Uani 1 1 d . . . N4 N 0.3729(3) 0.84892(17) 0.33589(12) 0.0226(6) Uani 1 1 d . . . C1 C 0.4435(5) -0.0255(2) 0.09724(16) 0.0328(7) Uani 1 1 d . . . H1 H 0.5469 -0.0262 0.1096 0.039 Uiso 1 1 calc R . . C2 C 0.3831(4) -0.1096(3) 0.06543(18) 0.0360(9) Uani 1 1 d . . . H2 H 0.4444 -0.1646 0.0557 0.043 Uiso 1 1 calc R . . C3 C 0.2288(5) -0.1094(2) 0.04850(19) 0.0357(9) Uani 1 1 d . . . H3 H 0.1838 -0.1644 0.0270 0.043 Uiso 1 1 calc R . . C4 C 0.1434(4) -0.0268(2) 0.06387(17) 0.0307(8) Uani 1 1 d . . . H4 H 0.0388 -0.0260 0.0540 0.037 Uiso 1 1 calc R . . C5 C 0.2127(4) 0.0556(2) 0.09412(16) 0.0234(7) Uani 1 1 d . . . C6 C 0.1224(4) 0.1470(2) 0.11225(18) 0.0262(7) Uani 1 1 d . . . H6A H 0.0246 0.1446 0.0876 0.031 Uiso 1 1 calc R . . H6B H 0.1016 0.1473 0.1629 0.031 Uiso 1 1 calc R . . C7 C 0.1080(4) 0.3248(2) 0.11911(17) 0.0259(7) Uani 1 1 d . . . H7A H 0.0855 0.3150 0.1691 0.031 Uiso 1 1 calc R . . H7B H 0.0113 0.3258 0.0936 0.031 Uiso 1 1 calc R . . C8 C 0.1875(4) 0.4237(2) 0.10964(17) 0.0229(7) Uani 1 1 d . . . C9 C 0.2773(3) 0.4619(2) 0.16442(15) 0.0217(7) Uani 1 1 d . . . H9 H 0.2851 0.4268 0.2069 0.026 Uiso 1 1 calc R . . C10 C 0.3555(3) 0.5516(2) 0.15695(17) 0.0243(7) Uani 1 1 d . . . C11 C 0.3434(4) 0.6025(2) 0.09306(17) 0.0281(8) Uani 1 1 d . . . H11 H 0.3977 0.6614 0.0867 0.034 Uiso 1 1 calc R . . C12 C 0.2518(5) 0.5668(2) 0.03873(18) 0.0345(9) Uani 1 1 d . . . H12 H 0.2424 0.6024 -0.0034 0.041 Uiso 1 1 calc R . . C13 C 0.1737(4) 0.4775(2) 0.04748(17) 0.0313(8) Uani 1 1 d . . . H13 H 0.1114 0.4538 0.0111 0.038 Uiso 1 1 calc R . . C14 C 0.4502(4) 0.5932(2) 0.21727(15) 0.0247(6) Uani 1 1 d . . . H14A H 0.4839 0.5382 0.2468 0.030 Uiso 1 1 calc R . . H14B H 0.5413 0.6239 0.1973 0.030 Uiso 1 1 calc R . . C15 C 0.3358(3) 0.7585(2) 0.22490(15) 0.0250(7) Uani 1 1 d . . . H15A H 0.2510 0.7460 0.1927 0.030 Uiso 1 1 calc R . . H15B H 0.4238 0.7786 0.1967 0.030 Uiso 1 1 calc R . . C16 C 0.2928(3) 0.8419(2) 0.27498(15) 0.0214(6) Uani 1 1 d . . . C17 C 0.1789(4) 0.9097(2) 0.25769(17) 0.0252(7) Uani 1 1 d . . . H17 H 0.1242 0.9029 0.2155 0.030 Uiso 1 1 calc R . . C18 C 0.1473(4) 0.9871(2) 0.30309(18) 0.0272(7) Uani 1 1 d . . . H18 H 0.0722 1.0337 0.2918 0.033 Uiso 1 1 calc R . . C19 C 0.2285(4) 0.9945(2) 0.36555(18) 0.0288(8) Uani 1 1 d . . . H19 H 0.2081 1.0453 0.3977 0.035 Uiso 1 1 calc R . . C20 C 0.3405(4) 0.9250(2) 0.37939(16) 0.0245(7) Uani 1 1 d . . . H20 H 0.3968 0.9312 0.4212 0.029 Uiso 1 1 calc R . . C21 C 0.2234(4) 0.2447(3) 0.01563(15) 0.0293(8) Uani 1 1 d . . . H21A H 0.2757 0.1860 -0.0004 0.044 Uiso 1 1 calc R . . H21B H 0.2834 0.3023 0.0038 0.044 Uiso 1 1 calc R . . H21C H 0.1250 0.2491 -0.0072 0.044 Uiso 1 1 calc R . . C22 C 0.2355(4) 0.6265(2) 0.29704(18) 0.0309(8) Uani 1 1 d . . . H22A H 0.1998 0.6718 0.3329 0.046 Uiso 1 1 calc R . . H22B H 0.2596 0.5636 0.3185 0.046 Uiso 1 1 calc R . . H22C H 0.1569 0.6174 0.2619 0.046 Uiso 1 1 calc R . . Cl1 Cl 0.18818(8) 0.28124(5) 0.34596(4) 0.02916(16) Uani 1 1 d . . . O1 O 0.1724(3) 0.38704(15) 0.34569(15) 0.0482(6) Uani 1 1 d . . . O2 O 0.0481(3) 0.2383(2) 0.3655(2) 0.0928(12) Uani 1 1 d . . . O3 O 0.2309(4) 0.2469(2) 0.27722(13) 0.0673(10) Uani 1 1 d . . . O4 O 0.3038(3) 0.2518(2) 0.39490(13) 0.0520(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02103(11) 0.02754(11) 0.03015(12) -0.00080(11) -0.00552(11) -0.00281(10) N1 0.0266(15) 0.0303(15) 0.0288(15) -0.0014(12) -0.0017(12) -0.0048(12) N2 0.0218(13) 0.0218(13) 0.0224(12) -0.0030(10) 0.0032(10) -0.0017(11) N3 0.0195(13) 0.0195(13) 0.0257(14) 0.0002(11) -0.0002(11) -0.0002(10) N4 0.0235(13) 0.0205(12) 0.0239(15) 0.0017(11) -0.0020(10) -0.0026(10) C1 0.0349(19) 0.0341(18) 0.0295(17) 0.0051(14) 0.0042(17) 0.0036(19) C2 0.051(2) 0.0246(18) 0.032(2) 0.0081(15) 0.0096(17) 0.0047(16) C3 0.054(3) 0.0212(17) 0.032(2) 0.0015(15) 0.0021(18) -0.0097(17) C4 0.037(2) 0.0284(18) 0.0268(18) 0.0004(14) 0.0012(16) -0.0084(15) C5 0.0224(17) 0.0265(17) 0.0214(16) 0.0004(13) 0.0033(13) -0.0055(14) C6 0.0190(17) 0.0274(18) 0.0321(18) -0.0052(14) 0.0036(14) -0.0064(14) C7 0.0224(17) 0.0268(17) 0.0284(17) -0.0070(14) -0.0001(13) 0.0024(13) C8 0.0174(16) 0.0219(16) 0.0293(17) -0.0054(13) -0.0001(14) 0.0032(14) C9 0.0242(16) 0.0233(15) 0.0175(17) -0.0001(12) 0.0021(12) 0.0055(13) C10 0.0201(15) 0.0241(15) 0.0286(18) -0.0029(14) 0.0038(14) 0.0044(12) C11 0.038(2) 0.0199(16) 0.0259(18) -0.0016(13) 0.0068(15) 0.0053(15) C12 0.053(2) 0.0279(18) 0.0226(18) 0.0041(14) 0.0004(16) 0.0051(17) C13 0.038(2) 0.0322(18) 0.0241(18) -0.0035(14) -0.0069(16) 0.0048(16) C14 0.0249(16) 0.0214(14) 0.0277(16) 0.0000(12) 0.0015(15) 0.0025(15) C15 0.0236(16) 0.0266(18) 0.0247(15) -0.0003(13) -0.0033(12) 0.0002(14) C16 0.0187(16) 0.0212(15) 0.0243(16) 0.0020(13) 0.0029(13) -0.0035(13) C17 0.0235(17) 0.0269(16) 0.0252(16) 0.0034(14) -0.0006(14) -0.0005(14) C18 0.0223(18) 0.0213(16) 0.0381(19) 0.0076(14) 0.0033(15) 0.0036(13) C19 0.0309(18) 0.0207(15) 0.035(2) -0.0029(14) 0.0078(15) -0.0032(13) C20 0.0285(18) 0.0217(16) 0.0234(16) -0.0009(13) 0.0028(14) -0.0071(14) C21 0.0308(18) 0.0321(19) 0.0251(16) -0.0048(15) 0.0010(13) 0.0036(15) C22 0.034(2) 0.0280(18) 0.0307(18) -0.0027(14) 0.0086(15) -0.0044(15) Cl1 0.0283(4) 0.0247(4) 0.0345(4) 0.0005(4) -0.0017(3) 0.0011(3) O1 0.0619(17) 0.0231(11) 0.0594(17) -0.0016(13) 0.0023(16) 0.0067(12) O2 0.0399(16) 0.0556(18) 0.183(4) 0.021(2) 0.023(2) -0.0092(16) O3 0.110(3) 0.057(2) 0.0347(15) -0.0064(14) -0.0080(15) 0.033(2) O4 0.0621(18) 0.0533(18) 0.0408(14) -0.0005(12) -0.0197(13) 0.0164(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 Ag N4 2.301(2) 4_645 ? Ag N2 2.344(2) . ? Ag N3 2.456(2) 4_645 ? Ag N1 2.507(3) . ? N1 C1 1.330(4) . ? N1 C5 1.348(4) . ? N2 C21 1.470(4) . ? N2 C6 1.474(4) . ? N2 C7 1.488(4) . ? N3 C22 1.459(4) . ? N3 C15 1.462(4) . ? N3 C14 1.481(4) . ? N3 Ag 2.456(2) 4_655 ? N4 C20 1.340(4) . ? N4 C16 1.345(4) . ? N4 Ag 2.301(2) 4_655 ? C1 C2 1.383(5) . ? C2 C3 1.381(5) . ? C3 C4 1.367(5) . ? C4 C5 1.384(4) . ? C5 C6 1.497(4) . ? C7 C8 1.510(4) . ? C8 C13 1.380(4) . ? C8 C9 1.392(4) . ? C9 C10 1.392(4) . ? C10 C11 1.387(4) . ? C10 C14 1.510(4) . ? C11 C12 1.383(5) . ? C12 C13 1.389(5) . ? C15 C16 1.511(4) . ? C16 C17 1.386(4) . ? C17 C18 1.374(4) . ? C18 C19 1.375(4) . ? C19 C20 1.375(4) . ? Cl1 O2 1.399(3) . ? Cl1 O4 1.421(2) . ? Cl1 O3 1.422(3) . ? Cl1 O1 1.429(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag N2 129.32(8) 4_645 . ? N4 Ag N3 72.02(8) 4_645 4_645 ? N2 Ag N3 154.87(8) . 4_645 ? N4 Ag N1 151.75(9) 4_645 . ? N2 Ag N1 72.08(9) . . ? N3 Ag N1 93.53(8) 4_645 . ? C1 N1 C5 117.3(3) . . ? C1 N1 Ag 131.9(2) . . ? C5 N1 Ag 110.0(2) . . ? C21 N2 C6 109.8(2) . . ? C21 N2 C7 111.2(2) . . ? C6 N2 C7 108.0(2) . . ? C21 N2 Ag 108.98(18) . . ? C6 N2 Ag 104.93(18) . . ? C7 N2 Ag 113.70(17) . . ? C22 N3 C15 110.4(2) . . ? C22 N3 C14 112.1(2) . . ? C15 N3 C14 112.0(2) . . ? C22 N3 Ag 111.27(19) . 4_655 ? C15 N3 Ag 101.54(17) . 4_655 ? C14 N3 Ag 109.01(18) . 4_655 ? C20 N4 C16 117.7(3) . . ? C20 N4 Ag 127.1(2) . 4_655 ? C16 N4 Ag 115.17(19) . 4_655 ? N1 C1 C2 124.1(4) . . ? C3 C2 C1 117.9(3) . . ? C4 C3 C2 118.8(3) . . ? C3 C4 C5 120.0(3) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 116.8(3) . . ? C4 C5 C6 121.4(3) . . ? N2 C6 C5 113.0(2) . . ? N2 C7 C8 112.6(2) . . ? C13 C8 C9 118.9(3) . . ? C13 C8 C7 121.4(3) . . ? C9 C8 C7 119.7(3) . . ? C8 C9 C10 121.3(3) . . ? C11 C10 C9 118.5(3) . . ? C11 C10 C14 120.7(3) . . ? C9 C10 C14 120.8(3) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C13 119.6(3) . . ? C8 C13 C12 120.7(3) . . ? N3 C14 C10 116.1(3) . . ? N3 C15 C16 111.7(2) . . ? N4 C16 C17 121.7(3) . . ? N4 C16 C15 117.1(3) . . ? C17 C16 C15 121.3(3) . . ? C18 C17 C16 119.7(3) . . ? C17 C18 C19 118.8(3) . . ? C18 C19 C20 118.6(3) . . ? N4 C20 C19 123.5(3) . . ? O2 Cl1 O4 109.4(2) . . ? O2 Cl1 O3 109.5(2) . . ? O4 Cl1 O3 108.24(17) . . ? O2 Cl1 O1 109.12(17) . . ? O4 Cl1 O1 110.37(17) . . ? O3 Cl1 O1 110.20(18) . . ? 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 Ag N1 C1 12.4(4) 4_645 . . . ? N2 Ag N1 C1 156.1(3) . . . . ? N3 Ag N1 C1 -45.0(3) 4_645 . . . ? N4 Ag N1 C5 -157.21(19) 4_645 . . . ? N2 Ag N1 C5 -13.6(2) . . . . ? N3 Ag N1 C5 145.4(2) 4_645 . . . ? N4 Ag N2 C21 74.8(2) 4_645 . . . ? N3 Ag N2 C21 -141.4(2) 4_645 . . . ? N1 Ag N2 C21 -83.9(2) . . . . ? N4 Ag N2 C6 -167.58(16) 4_645 . . . ? N3 Ag N2 C6 -23.8(3) 4_645 . . . ? N1 Ag N2 C6 33.69(17) . . . . ? N4 Ag N2 C7 -49.8(2) 4_645 . . . ? N3 Ag N2 C7 94.0(3) 4_645 . . . ? N1 Ag N2 C7 151.5(2) . . . . ? C5 N1 C1 C2 1.2(5) . . . . ? Ag N1 C1 C2 -167.9(2) . . . . ? N1 C1 C2 C3 -1.4(5) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 1.7(5) . . . . ? C1 N1 C5 C4 0.6(4) . . . . ? Ag N1 C5 C4 171.9(2) . . . . ? C1 N1 C5 C6 178.1(3) . . . . ? Ag N1 C5 C6 -10.6(3) . . . . ? C3 C4 C5 N1 -2.0(5) . . . . ? C3 C4 C5 C6 -179.4(3) . . . . ? C21 N2 C6 C5 63.4(3) . . . . ? C7 N2 C6 C5 -175.2(3) . . . . ? Ag N2 C6 C5 -53.6(3) . . . . ? N1 C5 C6 N2 45.0(4) . . . . ? C4 C5 C6 N2 -137.5(3) . . . . ? C21 N2 C7 C8 -65.9(3) . . . . ? C6 N2 C7 C8 173.6(3) . . . . ? Ag N2 C7 C8 57.6(3) . . . . ? N2 C7 C8 C13 87.9(4) . . . . ? N2 C7 C8 C9 -91.9(3) . . . . ? C13 C8 C9 C10 -1.5(5) . . . . ? C7 C8 C9 C10 178.3(3) . . . . ? C8 C9 C10 C11 -0.5(4) . . . . ? C8 C9 C10 C14 178.9(3) . . . . ? C9 C10 C11 C12 2.1(5) . . . . ? C14 C10 C11 C12 -177.3(3) . . . . ? C10 C11 C12 C13 -1.7(5) . . . . ? C9 C8 C13 C12 2.0(5) . . . . ? C7 C8 C13 C12 -177.8(3) . . . . ? C11 C12 C13 C8 -0.5(5) . . . . ? C22 N3 C14 C10 59.3(3) . . . . ? C15 N3 C14 C10 -65.5(3) . . . . ? Ag N3 C14 C10 -177.05(19) 4_655 . . . ? C11 C10 C14 N3 83.9(4) . . . . ? C9 C10 C14 N3 -95.5(3) . . . . ? C22 N3 C15 C16 68.0(3) . . . . ? C14 N3 C15 C16 -166.2(2) . . . . ? Ag N3 C15 C16 -50.1(3) 4_655 . . . ? C20 N4 C16 C17 -0.8(4) . . . . ? Ag N4 C16 C17 -179.7(2) 4_655 . . . ? C20 N4 C16 C15 177.2(3) . . . . ? Ag N4 C16 C15 -1.7(3) 4_655 . . . ? N3 C15 C16 N4 38.9(4) . . . . ? N3 C15 C16 C17 -143.1(3) . . . . ? N4 C16 C17 C18 0.7(4) . . . . ? C15 C16 C17 C18 -177.2(3) . . . . ? C16 C17 C18 C19 -0.9(4) . . . . ? C17 C18 C19 C20 1.3(4) . . . . ? C16 N4 C20 C19 1.2(4) . . . . ? Ag N4 C20 C19 179.9(2) 4_655 . . . ? C18 C19 C20 N4 -1.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.464 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.067 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 715096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 Ag4 N16 4+, 4(Cl O4 1-)' _chemical_formula_sum 'C88 H88 Ag4 Cl4 N16 O16' _chemical_formula_weight 2199.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.221(3) _cell_length_b 25.437(4) _cell_length_c 19.302(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.71(3) _cell_angle_gamma 90.00 _cell_volume 9927(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7087 _exptl_absorpt_correction_T_max 0.8802 _exptl_absorpt_process_details ; Bruker (2000) SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD' _diffrn_measurement_method 'w/ and f/ scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56470 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.52 _reflns_number_total 9199 _reflns_number_gt 3234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.1-0 (Bruker AXS)' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The routine SQUEEZE (Platon, Speck) was applied to the data set in order to take into account the disordered solvent molecules. Perchlorate Cl2, heavily disordered over two positions with occupancy 0.5, was refined with geometrical restraints: it was considered similar to Cl1 group by using instruction "SAME" of Shelx refinement program. ; _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^)+(0.0619P)^2^+34.0290P] 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 9199 _refine_ls_number_parameters 574 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.071 _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 0.63678(3) 0.88130(2) 0.51050(4) 0.0596(3) Uani 1 1 d . . . Ag2 Ag 0.71112(4) 0.82964(3) 0.18600(4) 0.0913(4) Uani 1 1 d . . . N1 N 0.5850(4) 0.8106(3) 0.5547(4) 0.0588(19) Uani 1 1 d . . . N2 N 0.6826(4) 0.8037(3) 0.4538(4) 0.064(2) Uani 1 1 d . . . N3 N 0.8159(5) 0.8382(3) 0.1484(7) 0.092(3) Uani 1 1 d . . . N4 N 0.7086(5) 0.8167(3) 0.0635(5) 0.071(2) Uani 1 1 d . . . C1 C 0.5392(5) 0.8129(4) 0.6044(5) 0.065(3) Uani 1 1 d . . . C2 C 0.5081(5) 0.7663(5) 0.6272(6) 0.097(4) Uani 1 1 d . . . H2 H 0.4768 0.7675 0.6621 0.116 Uiso 1 1 calc R . . C3 C 0.5245(6) 0.7196(5) 0.5973(8) 0.121(5) Uani 1 1 d . . . H3 H 0.5037 0.6887 0.6110 0.145 Uiso 1 1 calc R . . C4 C 0.5716(6) 0.7182(4) 0.5469(8) 0.116(4) Uani 1 1 d . . . H4 H 0.5833 0.6866 0.5262 0.139 Uiso 1 1 calc R . . C5 C 0.6013(4) 0.7647(4) 0.5274(6) 0.073(3) Uani 1 1 d . . . C6 C 0.6525(5) 0.7633(4) 0.4747(6) 0.084(3) Uani 1 1 d . . . H6 H 0.6635 0.7310 0.4554 0.100 Uiso 1 1 calc R . . C7 C 0.7323(4) 0.8023(4) 0.4030(5) 0.067(3) Uani 1 1 d . . . C8 C 0.7575(5) 0.8498(4) 0.3826(5) 0.068(3) Uani 1 1 d . . . H8 H 0.7422 0.8806 0.4028 0.082 Uiso 1 1 calc R . . C9 C 0.8052(5) 0.8524(4) 0.3325(5) 0.077(3) Uani 1 1 d . . . H9 H 0.8221 0.8850 0.3199 0.092 Uiso 1 1 calc R . . C10 C 0.8284(4) 0.8078(5) 0.3006(5) 0.077(3) Uani 1 1 d . . . C11 C 0.8035(6) 0.7602(5) 0.3221(6) 0.097(4) Uani 1 1 d . . . H11 H 0.8194 0.7295 0.3020 0.116 Uiso 1 1 calc R . . C12 C 0.7560(5) 0.7565(4) 0.3720(6) 0.083(3) Uani 1 1 d . . . H12 H 0.7398 0.7238 0.3852 0.100 Uiso 1 1 calc R . . C13 C 0.8831(5) 0.8096(5) 0.2475(7) 0.102(4) Uani 1 1 d . . . H13A H 0.8865 0.7754 0.2257 0.122 Uiso 1 1 calc R . . H13B H 0.9248 0.8166 0.2713 0.122 Uiso 1 1 calc R . . C14 C 0.8728(6) 0.8511(5) 0.1912(8) 0.109(5) Uani 1 1 d . . . H14A H 0.8663 0.8852 0.2125 0.131 Uiso 1 1 calc R . . H14B H 0.9118 0.8530 0.1626 0.131 Uiso 1 1 calc R . . C15 C 0.8227(7) 0.8379(4) 0.0829(9) 0.092(4) Uani 1 1 d . . . H15 H 0.8639 0.8453 0.0644 0.110 Uiso 1 1 calc R . . C16 C 0.7665(7) 0.8259(4) 0.0355(7) 0.082(3) Uani 1 1 d . . . C17 C 0.7785(7) 0.8247(4) -0.0344(8) 0.102(4) Uani 1 1 d . . . H17 H 0.8205 0.8309 -0.0515 0.122 Uiso 1 1 calc R . . C18 C 0.7266(9) 0.8139(5) -0.0777(7) 0.120(5) Uani 1 1 d . . . H18 H 0.7321 0.8139 -0.1254 0.143 Uiso 1 1 calc R . . C19 C 0.6657(6) 0.8030(4) -0.0496(6) 0.090(3) Uani 1 1 d . . . H19 H 0.6299 0.7947 -0.0783 0.108 Uiso 1 1 calc R . . C20 C 0.6580(7) 0.8046(4) 0.0215(7) 0.080(3) Uani 1 1 d . . . C41 C 0.5214(4) 0.8645(4) 0.6330(5) 0.075(3) Uani 1 1 d . . . H41A H 0.5474 0.8913 0.6115 0.112 Uiso 1 1 calc R . . H41B H 0.5297 0.8647 0.6821 0.112 Uiso 1 1 calc R . . H41C H 0.4753 0.8712 0.6242 0.112 Uiso 1 1 calc R . . C42 C 0.5939(5) 0.7914(4) 0.0543(5) 0.090(3) Uani 1 1 d . . . H42A H 0.5982 0.7947 0.1037 0.135 Uiso 1 1 calc R . . H42B H 0.5818 0.7560 0.0427 0.135 Uiso 1 1 calc R . . H42C H 0.5603 0.8151 0.0376 0.135 Uiso 1 1 calc R . . N5 N 0.7151(4) 0.9464(3) 0.5167(4) 0.0570(19) Uani 1 1 d . . . N6 N 0.5930(4) 0.9554(3) 0.4526(4) 0.0568(19) Uani 1 1 d . . . N7 N 0.3441(4) 0.8955(3) 0.2551(4) 0.071(2) Uani 1 1 d . . . N8 N 0.3672(4) 0.7901(3) 0.2467(4) 0.069(2) Uani 1 1 d . . . C21 C 0.7753(6) 0.9414(4) 0.5440(5) 0.068(3) Uani 1 1 d . . . C22 C 0.8231(5) 0.9809(5) 0.5368(6) 0.096(3) Uani 1 1 d . . . H22 H 0.8653 0.9775 0.5558 0.115 Uiso 1 1 calc R . . C23 C 0.8041(7) 1.0254(5) 0.4997(8) 0.118(5) Uani 1 1 d . . . H23 H 0.8345 1.0524 0.4940 0.142 Uiso 1 1 calc R . . C24 C 0.7429(6) 1.0304(4) 0.4717(7) 0.100(4) Uani 1 1 d . . . H24 H 0.7310 1.0603 0.4469 0.120 Uiso 1 1 calc R . . C25 C 0.6989(6) 0.9902(4) 0.4810(5) 0.066(3) Uani 1 1 d . . . C26 C 0.6335(6) 0.9933(4) 0.4511(5) 0.066(3) Uani 1 1 d . . . H26 H 0.6204 1.0244 0.4298 0.079 Uiso 1 1 calc R . . C27 C 0.5289(5) 0.9608(3) 0.4222(5) 0.060(2) Uani 1 1 d . . . C28 C 0.5118(5) 0.9958(3) 0.3679(5) 0.063(3) Uani 1 1 d . . . H28 H 0.5442 1.0175 0.3497 0.076 Uiso 1 1 calc R . . C29 C 0.4491(6) 0.9984(4) 0.3417(5) 0.066(3) Uani 1 1 d . . . H29 H 0.4394 1.0221 0.3063 0.079 Uiso 1 1 calc R . . C30 C 0.4002(5) 0.9667(4) 0.3667(5) 0.061(2) Uani 1 1 d . . . C31 C 0.4158(5) 0.9314(3) 0.4184(5) 0.059(2) Uani 1 1 d . . . H31 H 0.3829 0.9095 0.4353 0.070 Uiso 1 1 calc R . . C32 C 0.4791(5) 0.9279(3) 0.4457(4) 0.061(2) Uani 1 1 d . . . H32 H 0.4885 0.9034 0.4801 0.073 Uiso 1 1 calc R . . C33 C 0.3324(5) 0.9705(4) 0.3355(5) 0.078(3) Uani 1 1 d . . . H33A H 0.3175 1.0067 0.3378 0.094 Uiso 1 1 calc R . . H33B H 0.3023 0.9493 0.3624 0.094 Uiso 1 1 calc R . . C34 C 0.3296(5) 0.9521(4) 0.2597(5) 0.078(3) Uani 1 1 d . . . H34A H 0.2860 0.9590 0.2403 0.093 Uiso 1 1 calc R . . H34B H 0.3616 0.9717 0.2329 0.093 Uiso 1 1 calc R . . C35 C 0.3898(5) 0.8802(4) 0.2172(5) 0.066(3) Uani 1 1 d . . . H35 H 0.4148 0.9047 0.1932 0.079 Uiso 1 1 calc R . . C36 C 0.4046(5) 0.8239(4) 0.2100(5) 0.069(3) Uani 1 1 d . . . C37 C 0.4530(5) 0.8074(4) 0.1655(5) 0.081(3) Uani 1 1 d . . . H37 H 0.4781 0.8315 0.1410 0.097 Uiso 1 1 calc R . . C38 C 0.4633(5) 0.7537(5) 0.1580(5) 0.096(4) Uani 1 1 d . . . H38 H 0.4952 0.7413 0.1278 0.115 Uiso 1 1 calc R . . C39 C 0.4265(5) 0.7198(4) 0.1953(5) 0.095(3) Uani 1 1 d . . . H39 H 0.4328 0.6837 0.1911 0.114 Uiso 1 1 calc R . . C40 C 0.3790(5) 0.7396(5) 0.2399(5) 0.087(3) Uani 1 1 d . . . C43 C 0.7908(5) 0.8922(4) 0.5818(5) 0.086(3) Uani 1 1 d . . . H43A H 0.7525 0.8698 0.5816 0.129 Uiso 1 1 calc R . . H43B H 0.8032 0.9003 0.6288 0.129 Uiso 1 1 calc R . . H43C H 0.8266 0.8744 0.5596 0.129 Uiso 1 1 calc R . . C44 C 0.3370(6) 0.7025(4) 0.2814(6) 0.117(4) Uani 1 1 d . . . H44A H 0.3069 0.7223 0.3093 0.176 Uiso 1 1 calc R . . H44B H 0.3649 0.6814 0.3109 0.176 Uiso 1 1 calc R . . H44C H 0.3123 0.6800 0.2506 0.176 Uiso 1 1 calc R . . Cl1 Cl 0.15936(14) 0.61332(10) 0.27150(14) 0.0739(7) Uani 1 1 d D . . O1 O 0.2208(6) 0.6068(4) 0.3020(7) 0.221(7) Uani 1 1 d D . . O2 O 0.1347(3) 0.6647(2) 0.2850(3) 0.0770(18) Uani 1 1 d D . . O3 O 0.1158(5) 0.5770(3) 0.2916(5) 0.193(6) Uani 1 1 d D . . O4 O 0.1709(5) 0.6046(3) 0.2002(5) 0.161(4) Uani 1 1 d D . . Cl2 Cl 0.47332(13) 0.61765(10) 0.4281(2) 0.1070(11) Uani 1 1 d D . . O5 O 0.4470(9) 0.5737(7) 0.4534(12) 0.150(7) Uiso 0.50 1 d PD . . O6 O 0.4557(7) 0.6653(5) 0.4633(8) 0.110(5) Uiso 0.50 1 d PD . . O7 O 0.4587(12) 0.6289(10) 0.3572(9) 0.205(10) Uiso 0.50 1 d PD . . O8 O 0.5390(6) 0.6145(5) 0.4111(8) 0.076(4) Uiso 0.50 1 d PD . . O14 O 0.4426(9) 0.6644(8) 0.4056(11) 0.140(6) Uiso 0.50 1 d P . . O11 O 0.4335(11) 0.5778(10) 0.4008(13) 0.176(8) Uiso 0.50 1 d P . . O12 O 0.4550(10) 0.6094(8) 0.5036(11) 0.150(7) Uiso 0.50 1 d P . . O13 O 0.5434(9) 0.6151(7) 0.4492(11) 0.126(7) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0597(5) 0.0387(4) 0.0809(5) 0.0087(3) 0.0238(4) 0.0009(3) Ag2 0.0836(6) 0.0999(7) 0.0917(6) -0.0236(5) 0.0580(5) -0.0180(5) N1 0.050(5) 0.041(5) 0.085(6) 0.014(4) 0.011(5) 0.007(4) N2 0.051(5) 0.037(5) 0.104(6) 0.004(4) 0.014(5) 0.000(4) N3 0.099(8) 0.066(6) 0.112(8) -0.022(6) 0.063(7) -0.015(5) N4 0.083(7) 0.048(5) 0.084(7) -0.003(4) 0.054(7) 0.007(5) C1 0.043(6) 0.068(8) 0.084(7) 0.022(6) 0.009(6) 0.002(6) C2 0.059(7) 0.087(9) 0.145(10) 0.047(8) 0.031(7) 0.002(7) C3 0.085(9) 0.062(9) 0.217(15) 0.035(9) 0.041(10) -0.005(7) C4 0.070(8) 0.058(8) 0.222(14) 0.011(8) 0.053(9) -0.007(6) C5 0.040(6) 0.029(6) 0.150(10) 0.024(6) 0.020(6) 0.005(5) C6 0.058(7) 0.047(7) 0.146(10) 0.000(6) 0.028(7) 0.006(6) C7 0.048(6) 0.053(7) 0.099(8) -0.007(6) 0.024(6) 0.000(6) C8 0.064(7) 0.054(7) 0.086(7) -0.013(5) 0.035(6) -0.002(5) C9 0.071(7) 0.057(7) 0.103(8) -0.024(6) 0.030(7) 0.004(5) C10 0.052(6) 0.071(8) 0.109(8) -0.023(7) 0.025(6) -0.005(6) C11 0.081(8) 0.076(9) 0.133(10) -0.040(7) 0.033(8) 0.013(7) C12 0.068(7) 0.053(7) 0.130(9) -0.018(6) 0.028(7) 0.011(6) C13 0.065(8) 0.102(9) 0.139(11) -0.040(9) 0.051(7) 0.004(7) C14 0.090(9) 0.088(9) 0.152(12) -0.053(9) 0.085(9) -0.034(8) C15 0.087(10) 0.050(6) 0.141(13) 0.009(7) 0.067(10) 0.009(6) C16 0.104(11) 0.055(7) 0.089(10) 0.015(6) 0.071(10) 0.015(6) C17 0.102(11) 0.091(8) 0.114(12) 0.047(8) 0.064(10) 0.058(8) C18 0.138(13) 0.135(11) 0.087(10) 0.050(9) 0.064(11) 0.082(10) C19 0.114(10) 0.079(7) 0.078(9) 0.011(6) 0.035(8) 0.048(7) C20 0.099(10) 0.070(7) 0.073(9) -0.005(6) 0.043(8) 0.016(6) C41 0.069(7) 0.081(8) 0.074(7) 0.010(6) 0.022(5) 0.001(6) C42 0.100(8) 0.078(7) 0.092(8) -0.026(6) 0.052(7) -0.016(6) N5 0.056(6) 0.046(5) 0.069(5) -0.006(4) 0.029(4) -0.006(4) N6 0.062(6) 0.038(5) 0.070(5) 0.008(4) 0.033(4) 0.004(5) N7 0.064(5) 0.081(6) 0.068(5) 0.025(4) 0.019(5) 0.011(5) N8 0.069(5) 0.068(6) 0.072(5) 0.022(5) 0.042(4) 0.022(5) C21 0.065(8) 0.055(7) 0.084(7) -0.009(5) 0.028(6) -0.009(7) C22 0.069(8) 0.070(8) 0.148(11) -0.005(8) 0.027(7) -0.006(7) C23 0.088(11) 0.058(9) 0.210(14) 0.015(9) 0.059(10) -0.016(7) C24 0.064(8) 0.055(8) 0.182(12) 0.018(7) 0.036(8) 0.001(7) C25 0.067(8) 0.041(7) 0.092(7) 0.007(6) 0.037(6) -0.003(6) C26 0.074(8) 0.034(6) 0.091(8) 0.001(5) 0.035(6) 0.009(6) C27 0.076(8) 0.037(6) 0.066(7) -0.003(5) 0.037(6) 0.011(6) C28 0.082(8) 0.039(5) 0.069(7) 0.019(5) 0.040(6) 0.010(5) C29 0.064(7) 0.058(6) 0.076(7) 0.022(5) 0.016(6) 0.016(6) C30 0.063(7) 0.058(6) 0.062(6) 0.008(5) 0.024(6) 0.023(6) C31 0.052(7) 0.058(6) 0.067(7) 0.003(5) 0.024(5) 0.008(5) C32 0.075(8) 0.045(6) 0.064(6) 0.013(5) 0.031(6) 0.007(6) C33 0.076(8) 0.073(7) 0.088(8) 0.007(6) 0.036(6) 0.025(6) C34 0.084(7) 0.070(7) 0.080(8) 0.023(6) 0.027(6) 0.028(6) C35 0.053(6) 0.083(8) 0.063(6) 0.026(5) 0.034(5) 0.019(5) C36 0.058(7) 0.079(8) 0.070(7) 0.021(6) 0.029(6) 0.009(6) C37 0.072(7) 0.084(9) 0.088(8) 0.024(6) 0.044(6) 0.019(6) C38 0.096(9) 0.102(10) 0.090(8) 0.023(7) 0.061(7) 0.020(7) C39 0.102(9) 0.090(8) 0.094(8) 0.024(7) 0.051(7) 0.024(7) C40 0.078(8) 0.096(10) 0.088(8) 0.026(7) 0.049(6) 0.022(7) C43 0.063(7) 0.082(8) 0.112(8) 0.012(7) 0.010(6) -0.008(6) C44 0.140(10) 0.080(8) 0.134(10) 0.038(7) 0.084(9) 0.029(7) Cl1 0.0838(19) 0.0583(18) 0.0794(19) 0.0028(14) -0.0089(15) -0.0137(16) O1 0.188(11) 0.153(9) 0.321(16) -0.122(10) -0.119(11) 0.082(8) O2 0.093(5) 0.045(4) 0.094(5) 0.019(3) 0.031(4) 0.008(3) O3 0.300(12) 0.085(6) 0.201(9) -0.044(6) 0.215(9) -0.100(7) O4 0.226(11) 0.133(7) 0.127(8) 0.019(6) 0.113(7) 0.041(7) Cl2 0.0677(19) 0.0506(17) 0.203(4) 0.022(2) 0.006(2) -0.0066(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.255(7) . ? Ag1 N5 2.293(7) . ? Ag1 N6 2.357(7) . ? Ag1 N2 2.445(7) . ? Ag2 N3 2.258(9) . ? Ag2 N8 2.293(7) 2_655 ? Ag2 N7 2.318(7) 2_655 ? Ag2 N4 2.387(9) . ? N1 C5 1.324(10) . ? N1 C1 1.345(10) . ? N2 C6 1.262(11) . ? N2 C7 1.414(11) . ? N3 C15 1.273(14) . ? N3 C14 1.445(14) . ? N4 C16 1.317(12) . ? N4 C20 1.333(12) . ? C1 C2 1.415(13) . ? C1 C41 1.470(12) . ? C2 C3 1.363(15) . ? C3 C4 1.371(15) . ? C4 C5 1.379(13) . ? C5 C6 1.462(13) . ? C7 C8 1.370(12) . ? C7 C12 1.398(12) . ? C8 C9 1.376(11) . ? C9 C10 1.376(12) . ? C10 C11 1.377(13) . ? C10 C13 1.519(13) . ? C11 C12 1.373(13) . ? C13 C14 1.527(15) . ? C15 C16 1.482(15) . ? C16 C17 1.373(15) . ? C17 C18 1.361(17) . ? C18 C19 1.380(16) . ? C19 C20 1.383(13) . ? C20 C42 1.488(13) . ? N5 C21 1.327(11) . ? N5 C25 1.347(11) . ? N6 C26 1.265(10) . ? N6 C27 1.424(11) . ? N7 C35 1.248(10) . ? N7 C34 1.473(11) . ? N7 Ag2 2.318(7) 2_655 ? N8 C40 1.313(12) . ? N8 C36 1.349(11) . ? N8 Ag2 2.293(7) 2_655 ? C21 C22 1.401(13) . ? C21 C43 1.481(12) . ? C22 C23 1.391(15) . ? C23 C24 1.350(15) . ? C24 C25 1.370(13) . ? C25 C26 1.439(12) . ? C27 C32 1.389(11) . ? C27 C28 1.413(12) . ? C28 C29 1.360(11) . ? C29 C30 1.368(12) . ? C30 C31 1.376(11) . ? C30 C33 1.495(12) . ? C31 C32 1.382(11) . ? C33 C34 1.536(12) . ? C35 C36 1.469(12) . ? C36 C37 1.377(12) . ? C37 C38 1.388(13) . ? C38 C39 1.353(13) . ? C39 C40 1.393(13) . ? C40 C44 1.509(13) . ? Cl1 O3 1.337(7) . ? Cl1 O1 1.379(9) . ? Cl1 O4 1.416(8) . ? Cl1 O2 1.425(6) . ? Cl2 O5 1.333(15) . ? Cl2 O8 1.374(12) . ? Cl2 O7 1.426(16) . ? Cl2 O6 1.437(12) . ? Cl2 O11 1.39(2) . ? Cl2 O14 1.409(19) . ? Cl2 O13 1.471(19) . ? Cl2 O12 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N5 151.6(3) . . ? N1 Ag1 N6 130.1(3) . . ? N5 Ag1 N6 72.7(3) . . ? N1 Ag1 N2 72.8(3) . . ? N5 Ag1 N2 110.0(3) . . ? N6 Ag1 N2 125.1(2) . . ? N3 Ag2 N8 151.8(3) . 2_655 ? N3 Ag2 N7 123.2(3) . 2_655 ? N8 Ag2 N7 72.4(3) 2_655 2_655 ? N3 Ag2 N4 72.8(4) . . ? N8 Ag2 N4 119.6(3) 2_655 . ? N7 Ag2 N4 125.5(3) 2_655 . ? C5 N1 C1 120.0(8) . . ? C5 N1 Ag1 115.8(6) . . ? C1 N1 Ag1 124.2(6) . . ? C6 N2 C7 123.4(8) . . ? C6 N2 Ag1 109.1(6) . . ? C7 N2 Ag1 127.4(6) . . ? C15 N3 C14 118.3(11) . . ? C15 N3 Ag2 115.6(9) . . ? C14 N3 Ag2 125.6(8) . . ? C16 N4 C20 118.0(10) . . ? C16 N4 Ag2 112.0(9) . . ? C20 N4 Ag2 129.9(7) . . ? N1 C1 C2 119.8(9) . . ? N1 C1 C41 118.9(8) . . ? C2 C1 C41 121.3(10) . . ? C3 C2 C1 119.2(10) . . ? C2 C3 C4 119.8(10) . . ? C3 C4 C5 118.7(11) . . ? N1 C5 C4 122.4(10) . . ? N1 C5 C6 118.6(8) . . ? C4 C5 C6 119.0(10) . . ? N2 C6 C5 123.5(9) . . ? C8 C7 C12 118.8(9) . . ? C8 C7 N2 116.6(8) . . ? C12 C7 N2 124.6(9) . . ? C7 C8 C9 120.7(8) . . ? C10 C9 C8 121.3(9) . . ? C9 C10 C11 117.6(9) . . ? C9 C10 C13 122.1(10) . . ? C11 C10 C13 120.1(10) . . ? C12 C11 C10 122.2(9) . . ? C11 C12 C7 119.3(9) . . ? C10 C13 C14 114.0(9) . . ? N3 C14 C13 110.6(10) . . ? N3 C15 C16 121.5(11) . . ? N4 C16 C17 124.6(14) . . ? N4 C16 C15 117.5(11) . . ? C17 C16 C15 117.9(13) . . ? C18 C17 C16 117.6(13) . . ? C17 C18 C19 118.9(12) . . ? C18 C19 C20 119.7(13) . . ? N4 C20 C19 121.0(11) . . ? N4 C20 C42 117.4(10) . . ? C19 C20 C42 121.6(13) . . ? C21 N5 C25 119.9(8) . . ? C21 N5 Ag1 125.6(6) . . ? C25 N5 Ag1 114.0(7) . . ? C26 N6 C27 120.1(8) . . ? C26 N6 Ag1 112.4(7) . . ? C27 N6 Ag1 127.5(6) . . ? C35 N7 C34 119.3(8) . . ? C35 N7 Ag2 115.2(6) . 2_655 ? C34 N7 Ag2 125.4(6) . 2_655 ? C40 N8 C36 117.8(8) . . ? C40 N8 Ag2 127.8(6) . 2_655 ? C36 N8 Ag2 114.4(6) . 2_655 ? N5 C21 C22 121.5(10) . . ? N5 C21 C43 117.6(9) . . ? C22 C21 C43 120.9(11) . . ? C23 C22 C21 116.7(11) . . ? C24 C23 C22 121.9(11) . . ? C23 C24 C25 118.1(11) . . ? N5 C25 C24 122.0(10) . . ? N5 C25 C26 117.8(9) . . ? C24 C25 C26 120.1(11) . . ? N6 C26 C25 122.7(9) . . ? C32 C27 C28 116.7(9) . . ? C32 C27 N6 117.8(9) . . ? C28 C27 N6 125.5(9) . . ? C29 C28 C27 121.7(9) . . ? C28 C29 C30 120.9(9) . . ? C29 C30 C31 118.7(9) . . ? C29 C30 C33 119.0(9) . . ? C31 C30 C33 122.3(9) . . ? C30 C31 C32 121.4(8) . . ? C31 C32 C27 120.6(8) . . ? C30 C33 C34 112.7(7) . . ? N7 C34 C33 110.5(7) . . ? N7 C35 C36 120.8(9) . . ? N8 C36 C37 122.7(9) . . ? N8 C36 C35 117.0(8) . . ? C37 C36 C35 120.2(9) . . ? C36 C37 C38 118.3(9) . . ? C39 C38 C37 119.2(9) . . ? C38 C39 C40 119.0(10) . . ? N8 C40 C39 122.9(9) . . ? N8 C40 C44 117.1(9) . . ? C39 C40 C44 119.9(11) . . ? O3 Cl1 O1 112.8(8) . . ? O3 Cl1 O4 106.9(6) . . ? O1 Cl1 O4 103.7(7) . . ? O3 Cl1 O2 110.3(5) . . ? O1 Cl1 O2 110.4(5) . . ? O4 Cl1 O2 112.6(4) . . ? O5 Cl2 O8 115.5(10) . . ? O5 Cl2 O7 116.2(13) . . ? O8 Cl2 O7 88.3(12) . . ? O5 Cl2 O6 115.6(11) . . ? O8 Cl2 O6 114.1(8) . . ? O7 Cl2 O6 103.6(11) . . ? O11 Cl2 O14 104.3(13) . . ? O11 Cl2 O13 128.6(12) . . ? O14 Cl2 O13 122.8(11) . . ? O11 Cl2 O12 96.7(12) . . ? O14 Cl2 O12 107.5(11) . . ? O13 Cl2 O12 88.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ag1 N1 C5 -103.5(8) . . . . ? N6 Ag1 N1 C5 118.7(6) . . . . ? N2 Ag1 N1 C5 -3.1(6) . . . . ? N5 Ag1 N1 C1 77.8(9) . . . . ? N6 Ag1 N1 C1 -60.0(8) . . . . ? N2 Ag1 N1 C1 178.2(7) . . . . ? N1 Ag1 N2 C6 3.2(6) . . . . ? N5 Ag1 N2 C6 153.4(7) . . . . ? N6 Ag1 N2 C6 -124.1(7) . . . . ? N1 Ag1 N2 C7 -179.8(7) . . . . ? N5 Ag1 N2 C7 -29.6(8) . . . . ? N6 Ag1 N2 C7 52.9(8) . . . . ? N8 Ag2 N3 C15 128.2(9) 2_655 . . . ? N7 Ag2 N3 C15 -114.6(7) 2_655 . . . ? N4 Ag2 N3 C15 7.0(7) . . . . ? N8 Ag2 N3 C14 -60.9(12) 2_655 . . . ? N7 Ag2 N3 C14 56.4(10) 2_655 . . . ? N4 Ag2 N3 C14 177.9(9) . . . . ? N3 Ag2 N4 C16 -6.2(6) . . . . ? N8 Ag2 N4 C16 -158.5(6) 2_655 . . . ? N7 Ag2 N4 C16 112.7(6) 2_655 . . . ? N3 Ag2 N4 C20 177.6(9) . . . . ? N8 Ag2 N4 C20 25.2(9) 2_655 . . . ? N7 Ag2 N4 C20 -63.6(9) 2_655 . . . ? C5 N1 C1 C2 -0.5(13) . . . . ? Ag1 N1 C1 C2 178.1(7) . . . . ? C5 N1 C1 C41 -179.2(8) . . . . ? Ag1 N1 C1 C41 -0.6(11) . . . . ? N1 C1 C2 C3 -1.1(15) . . . . ? C41 C1 C2 C3 177.6(10) . . . . ? C1 C2 C3 C4 1.4(19) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C1 N1 C5 C4 1.8(15) . . . . ? Ag1 N1 C5 C4 -176.9(9) . . . . ? C1 N1 C5 C6 -178.5(8) . . . . ? Ag1 N1 C5 C6 2.8(11) . . . . ? C3 C4 C5 N1 -1.4(18) . . . . ? C3 C4 C5 C6 178.8(11) . . . . ? C7 N2 C6 C5 179.7(9) . . . . ? Ag1 N2 C6 C5 -3.1(12) . . . . ? N1 C5 C6 N2 0.5(15) . . . . ? C4 C5 C6 N2 -179.7(10) . . . . ? C6 N2 C7 C8 176.1(9) . . . . ? Ag1 N2 C7 C8 -0.5(12) . . . . ? C6 N2 C7 C12 -2.8(15) . . . . ? Ag1 N2 C7 C12 -179.4(7) . . . . ? C12 C7 C8 C9 0.1(14) . . . . ? N2 C7 C8 C9 -178.8(8) . . . . ? C7 C8 C9 C10 0.9(15) . . . . ? C8 C9 C10 C11 -1.8(15) . . . . ? C8 C9 C10 C13 -177.3(10) . . . . ? C9 C10 C11 C12 1.7(16) . . . . ? C13 C10 C11 C12 177.2(10) . . . . ? C10 C11 C12 C7 -0.7(16) . . . . ? C8 C7 C12 C11 -0.3(15) . . . . ? N2 C7 C12 C11 178.6(9) . . . . ? C9 C10 C13 C14 -48.5(15) . . . . ? C11 C10 C13 C14 136.1(12) . . . . ? C15 N3 C14 C13 -129.1(9) . . . . ? Ag2 N3 C14 C13 60.2(11) . . . . ? C10 C13 C14 N3 -66.1(12) . . . . ? C14 N3 C15 C16 -179.0(9) . . . . ? Ag2 N3 C15 C16 -7.3(12) . . . . ? C20 N4 C16 C17 0.9(14) . . . . ? Ag2 N4 C16 C17 -175.9(8) . . . . ? C20 N4 C16 C15 -178.3(8) . . . . ? Ag2 N4 C16 C15 4.9(10) . . . . ? N3 C15 C16 N4 1.3(14) . . . . ? N3 C15 C16 C17 -177.9(9) . . . . ? N4 C16 C17 C18 1.1(16) . . . . ? C15 C16 C17 C18 -179.8(10) . . . . ? C16 C17 C18 C19 -2.3(17) . . . . ? C17 C18 C19 C20 1.7(17) . . . . ? C16 N4 C20 C19 -1.5(14) . . . . ? Ag2 N4 C20 C19 174.6(6) . . . . ? C16 N4 C20 C42 176.8(8) . . . . ? Ag2 N4 C20 C42 -7.1(13) . . . . ? C18 C19 C20 N4 0.3(15) . . . . ? C18 C19 C20 C42 -177.9(10) . . . . ? N1 Ag1 N5 C21 36.7(9) . . . . ? N6 Ag1 N5 C21 -175.9(7) . . . . ? N2 Ag1 N5 C21 -54.0(7) . . . . ? N1 Ag1 N5 C25 -152.3(6) . . . . ? N6 Ag1 N5 C25 -4.9(5) . . . . ? N2 Ag1 N5 C25 117.0(6) . . . . ? N1 Ag1 N6 C26 162.6(5) . . . . ? N5 Ag1 N6 C26 2.2(5) . . . . ? N2 Ag1 N6 C26 -100.4(6) . . . . ? N1 Ag1 N6 C27 -16.5(7) . . . . ? N5 Ag1 N6 C27 -177.0(6) . . . . ? N2 Ag1 N6 C27 80.4(6) . . . . ? C25 N5 C21 C22 0.2(13) . . . . ? Ag1 N5 C21 C22 170.7(7) . . . . ? C25 N5 C21 C43 -179.1(8) . . . . ? Ag1 N5 C21 C43 -8.6(11) . . . . ? N5 C21 C22 C23 0.0(15) . . . . ? C43 C21 C22 C23 179.3(10) . . . . ? C21 C22 C23 C24 -0.2(18) . . . . ? C22 C23 C24 C25 0.2(18) . . . . ? C21 N5 C25 C24 -0.2(13) . . . . ? Ag1 N5 C25 C24 -171.8(8) . . . . ? C21 N5 C25 C26 178.6(7) . . . . ? Ag1 N5 C25 C26 7.1(9) . . . . ? C23 C24 C25 N5 0.0(16) . . . . ? C23 C24 C25 C26 -178.8(10) . . . . ? C27 N6 C26 C25 180.0(7) . . . . ? Ag1 N6 C26 C25 0.8(10) . . . . ? N5 C25 C26 N6 -5.5(13) . . . . ? C24 C25 C26 N6 173.4(9) . . . . ? C26 N6 C27 C32 -156.9(8) . . . . ? Ag1 N6 C27 C32 22.2(10) . . . . ? C26 N6 C27 C28 25.5(12) . . . . ? Ag1 N6 C27 C28 -155.4(6) . . . . ? C32 C27 C28 C29 2.3(12) . . . . ? N6 C27 C28 C29 179.9(8) . . . . ? C27 C28 C29 C30 -0.6(13) . . . . ? C28 C29 C30 C31 -0.9(13) . . . . ? C28 C29 C30 C33 -179.1(8) . . . . ? C29 C30 C31 C32 0.7(12) . . . . ? C33 C30 C31 C32 178.8(8) . . . . ? C30 C31 C32 C27 1.1(12) . . . . ? C28 C27 C32 C31 -2.5(11) . . . . ? N6 C27 C32 C31 179.8(7) . . . . ? C29 C30 C33 C34 66.2(11) . . . . ? C31 C30 C33 C34 -111.9(9) . . . . ? C35 N7 C34 C33 -124.6(9) . . . . ? Ag2 N7 C34 C33 55.0(10) 2_655 . . . ? C30 C33 C34 N7 65.7(10) . . . . ? C34 N7 C35 C36 -178.4(8) . . . . ? Ag2 N7 C35 C36 1.9(11) 2_655 . . . ? C40 N8 C36 C37 1.2(15) . . . . ? Ag2 N8 C36 C37 -178.4(8) 2_655 . . . ? C40 N8 C36 C35 178.8(9) . . . . ? Ag2 N8 C36 C35 -0.8(10) 2_655 . . . ? N7 C35 C36 N8 -0.8(14) . . . . ? N7 C35 C36 C37 176.9(9) . . . . ? N8 C36 C37 C38 0.3(15) . . . . ? C35 C36 C37 C38 -177.2(9) . . . . ? C36 C37 C38 C39 -1.0(16) . . . . ? C37 C38 C39 C40 0.2(17) . . . . ? C36 N8 C40 C39 -2.0(16) . . . . ? Ag2 N8 C40 C39 177.5(8) 2_655 . . . ? C36 N8 C40 C44 179.7(9) . . . . ? Ag2 N8 C40 C44 -0.7(14) 2_655 . . . ? C38 C39 C40 N8 1.3(17) . . . . ? C38 C39 C40 C44 179.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.715 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.067 # Attachment 'ag-comp5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 715097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 Ag N4 1+, (Cl O4 1-), H2 O' _chemical_formula_sum 'C22 H28 Ag Cl N4 O5' _chemical_formula_weight 571.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.428(2) _cell_length_b 10.093(3) _cell_length_c 13.372(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.29(3) _cell_angle_gamma 90.00 _cell_volume 1227.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5994 _exptl_absorpt_correction_T_max 0.8056 _exptl_absorpt_process_details ; Bruker (2000) SADABS ; _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 Apex II CCD' _diffrn_measurement_method 'w/ and f/ scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16979 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 29.57 _reflns_number_total 6280 _reflns_number_gt 4585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.1-0 (Bruker AXS)' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. O-H water distances restrained at 0.85 ; _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^)+(0.0596P)^2^+0.1214P] 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 0.47(3) _refine_ls_number_reflns 6280 _refine_ls_number_parameters 301 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 1.01868(8) 0.74776(3) 0.51344(6) 0.05943(10) Uani 1 1 d . . . N1 N 1.1706(4) 0.7104(4) 0.6671(3) 0.0545(8) Uani 1 1 d . . . N2 N 0.9461(4) 0.9012(3) 0.6525(3) 0.0564(8) Uani 1 1 d . . . N3 N 0.0926(3) 0.8693(3) 0.3718(2) 0.0508(7) Uani 1 1 d . . . N4 N -0.1469(4) 0.6961(4) 0.3665(3) 0.0541(7) Uani 1 1 d . . . C1 C 1.3007(5) 0.6504(4) 0.6764(4) 0.0639(11) Uani 1 1 d . . . H1 H 1.3234 0.6196 0.6169 0.077 Uiso 1 1 calc R . . C2 C 1.4017(6) 0.6327(5) 0.7708(4) 0.0764(14) Uani 1 1 d . . . H2 H 1.4909 0.5909 0.7749 0.092 Uiso 1 1 calc R . . C3 C 1.3696(6) 0.6765(5) 0.8560(4) 0.0803(14) Uani 1 1 d . . . H3 H 1.4359 0.6655 0.9206 0.096 Uiso 1 1 calc R . . C4 C 1.2380(8) 0.7377(4) 0.8472(5) 0.0659(14) Uani 1 1 d . . . H4 H 1.2158 0.7703 0.9064 0.079 Uiso 1 1 calc R . . C5 C 1.1364(9) 0.7522(3) 0.7517(5) 0.0521(14) Uani 1 1 d . . . C6 C 0.9907(5) 0.8146(7) 0.7429(4) 0.0722(12) Uani 1 1 d . . . H6A H 0.9174 0.7458 0.7380 0.087 Uiso 1 1 calc R . . H6B H 0.9950 0.8658 0.8051 0.087 Uiso 1 1 calc R . . C7 C 0.7887(5) 0.9194(4) 0.6136(3) 0.0562(9) Uani 1 1 d . . . C8 C 0.6996(5) 0.8126(5) 0.5976(4) 0.0737(12) Uani 1 1 d . . . H8 H 0.7402 0.7287 0.6130 0.088 Uiso 1 1 calc R . . C9 C 0.5498(5) 0.8256(4) 0.5588(4) 0.0763(12) Uani 1 1 d . . . H9 H 0.4905 0.7507 0.5521 0.092 Uiso 1 1 calc R . . C10 C 0.4859(4) 0.9473(4) 0.5297(3) 0.0560(9) Uani 1 1 d . . . C11 C 0.5761(5) 1.0551(4) 0.5423(3) 0.0613(9) Uani 1 1 d . . . H11 H 0.5352 1.1379 0.5221 0.074 Uiso 1 1 calc R . . C12 C 0.7290(5) 1.0451(4) 0.5847(3) 0.0540(9) Uani 1 1 d . . . H12 H 0.7887 1.1198 0.5934 0.065 Uiso 1 1 calc R . . C13 C 0.3190(5) 0.9667(5) 0.4903(4) 0.0749(13) Uani 1 1 d . . . H13A H 0.2735 0.9426 0.5449 0.090 Uiso 1 1 calc R . . H13B H 0.2983 1.0595 0.4742 0.090 Uiso 1 1 calc R . . C14 C 0.2522(5) 0.8848(5) 0.3954(4) 0.0659(12) Uani 1 1 d . . . H14A H 0.2764 0.9256 0.3363 0.079 Uiso 1 1 calc R . . H14B H 0.2970 0.7976 0.4047 0.079 Uiso 1 1 calc R . . C15 C 0.0417(6) 0.7739(5) 0.2886(4) 0.0588(12) Uani 1 1 d . . . H15A H 0.1082 0.6987 0.3006 0.071 Uiso 1 1 calc R . . H15B H 0.0456 0.8145 0.2236 0.071 Uiso 1 1 calc R . . C16 C -0.1143(7) 0.7241(5) 0.2784(5) 0.0518(13) Uani 1 1 d . . . C17 C -0.2098(6) 0.7020(6) 0.1824(4) 0.0665(12) Uani 1 1 d . . . H17 H -0.1829 0.7217 0.1220 0.080 Uiso 1 1 calc R . . C18 C -0.3482(6) 0.6494(5) 0.1785(5) 0.0786(14) Uani 1 1 d . . . H18 H -0.4161 0.6340 0.1152 0.094 Uiso 1 1 calc R . . C19 C -0.3816(6) 0.6209(5) 0.2692(4) 0.0772(14) Uani 1 1 d . . . H19 H -0.4728 0.5853 0.2686 0.093 Uiso 1 1 calc R . . C20 C -0.2797(5) 0.6453(5) 0.3612(4) 0.0730(12) Uani 1 1 d . . . H20 H -0.3039 0.6257 0.4226 0.088 Uiso 1 1 calc R . . C21 C 1.0298(5) 1.0233(5) 0.6662(5) 0.0793(14) Uani 1 1 d . . . H21A H 1.0023 1.0774 0.7170 0.119 Uiso 1 1 calc R . . H21B H 1.0098 1.0700 0.6014 0.119 Uiso 1 1 calc R . . H21C H 1.1328 1.0032 0.6891 0.119 Uiso 1 1 calc R . . C22 C 0.0159(6) 0.9972(4) 0.3468(5) 0.0760(13) Uani 1 1 d . . . H22A H 0.0431 1.0546 0.4061 0.114 Uiso 1 1 calc R . . H22B H -0.0884 0.9828 0.3287 0.114 Uiso 1 1 calc R . . H22C H 0.0430 1.0375 0.2895 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.81694(12) 0.56039(11) 0.90867(9) 0.0652(3) Uani 1 1 d . . . O1 O 0.7041(6) 0.4991(5) 0.9461(4) 0.1246(16) Uani 1 1 d . . . O2 O 0.7923(5) 0.5317(5) 0.8024(3) 0.1095(13) Uani 1 1 d . . . O3 O 0.8014(9) 0.6948(5) 0.9214(5) 0.154(2) Uani 1 1 d . . . O4 O 0.9535(7) 0.5162(13) 0.9628(6) 0.234(5) Uani 1 1 d . . . O1W O 0.7490(7) 0.4163(8) 0.5940(4) 0.150(3) Uani 1 1 d . . . H1W H 0.6494 0.4093 0.5650 0.225 Uiso 1 1 d R . . H2W H 0.7535 0.3768 0.6520 0.225 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.05584(14) 0.08443(18) 0.03409(11) 0.00044(13) 0.00492(9) -0.00112(14) N1 0.053(2) 0.0655(18) 0.0387(18) -0.0010(16) 0.0019(15) 0.0024(17) N2 0.0453(19) 0.069(2) 0.0547(19) -0.0023(16) 0.0131(15) 0.0010(15) N3 0.0404(16) 0.0677(19) 0.0424(16) 0.0025(13) 0.0078(13) 0.0027(13) N4 0.048(2) 0.070(2) 0.0431(18) -0.0022(18) 0.0106(15) -0.0082(18) C1 0.063(3) 0.068(2) 0.058(2) 0.000(2) 0.010(2) 0.010(2) C2 0.063(3) 0.076(3) 0.077(3) -0.001(2) -0.004(3) 0.013(2) C3 0.078(3) 0.085(3) 0.057(3) 0.000(2) -0.020(2) 0.008(3) C4 0.076(3) 0.074(3) 0.039(2) -0.0035(17) -0.001(2) 0.008(2) C5 0.061(3) 0.060(3) 0.033(2) 0.0024(14) 0.008(2) -0.0005(17) C6 0.061(3) 0.113(4) 0.046(2) 0.007(3) 0.021(2) 0.008(3) C7 0.0456(19) 0.068(2) 0.058(2) -0.0129(18) 0.0178(17) 0.0001(17) C8 0.058(2) 0.057(2) 0.108(4) 0.003(2) 0.026(2) 0.002(2) C9 0.058(3) 0.061(3) 0.110(4) 0.004(2) 0.023(2) -0.0080(19) C10 0.055(2) 0.0560(19) 0.058(2) -0.0015(16) 0.0163(17) -0.0020(16) C11 0.061(2) 0.066(2) 0.056(2) 0.0005(17) 0.0150(17) 0.0001(18) C12 0.056(2) 0.050(2) 0.055(2) 0.0008(16) 0.0149(17) -0.0051(16) C13 0.051(2) 0.102(3) 0.076(3) -0.037(3) 0.026(2) -0.009(2) C14 0.048(2) 0.084(3) 0.063(3) 0.009(2) 0.008(2) -0.0142(19) C15 0.064(3) 0.072(3) 0.042(2) 0.0009(16) 0.017(2) 0.0019(19) C16 0.047(3) 0.055(2) 0.048(3) -0.002(2) 0.003(2) -0.001(2) C17 0.089(4) 0.057(2) 0.042(2) -0.008(2) -0.002(2) 0.000(3) C18 0.072(3) 0.078(3) 0.068(3) -0.006(2) -0.014(2) -0.012(2) C19 0.053(3) 0.092(3) 0.079(3) -0.014(3) 0.005(2) -0.015(2) C20 0.063(3) 0.090(3) 0.064(3) -0.004(3) 0.014(2) -0.017(2) C21 0.055(3) 0.082(3) 0.097(4) -0.017(3) 0.012(3) -0.008(2) C22 0.067(3) 0.064(3) 0.085(3) 0.013(2) -0.001(2) 0.004(2) Cl1 0.0615(5) 0.0770(6) 0.0549(5) -0.0004(5) 0.0116(4) -0.0037(5) O1 0.121(4) 0.165(4) 0.094(3) 0.028(3) 0.038(3) -0.045(3) O2 0.123(3) 0.142(4) 0.070(2) -0.027(2) 0.039(2) -0.012(3) O3 0.256(7) 0.088(3) 0.134(4) -0.020(3) 0.079(4) -0.016(4) O4 0.099(4) 0.439(14) 0.138(6) -0.008(7) -0.013(4) 0.093(6) O1W 0.129(5) 0.217(7) 0.087(3) -0.014(4) -0.001(3) 0.030(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 Ag N1 2.206(4) . ? Ag N4 2.226(4) 1_655 ? Ag N3 2.505(3) 1_655 ? Ag N2 2.645(3) . ? N1 C5 1.324(8) . ? N1 C1 1.344(6) . ? N2 C21 1.448(6) . ? N2 C7 1.449(5) . ? N2 C6 1.461(6) . ? N3 C15 1.455(6) . ? N3 C14 1.462(5) . ? N3 C22 1.474(5) . ? N3 Ag 2.505(3) 1_455 ? N4 C16 1.324(8) . ? N4 C20 1.338(6) . ? N4 Ag 2.226(4) 1_455 ? C1 C2 1.378(7) . ? C2 C3 1.328(8) . ? C3 C4 1.363(9) . ? C4 C5 1.388(10) . ? C5 C6 1.487(9) . ? C7 C8 1.348(6) . ? C7 C12 1.400(6) . ? C8 C9 1.377(6) . ? C9 C10 1.378(6) . ? C10 C11 1.364(6) . ? C10 C13 1.535(6) . ? C11 C12 1.407(6) . ? C13 C14 1.506(6) . ? C15 C16 1.526(9) . ? C16 C17 1.377(8) . ? C17 C18 1.397(8) . ? C18 C19 1.362(8) . ? C19 C20 1.369(7) . ? Cl1 O4 1.374(6) . ? Cl1 O3 1.380(6) . ? Cl1 O2 1.409(4) . ? Cl1 O1 1.431(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N4 156.15(12) . 1_655 ? N1 Ag N3 123.13(14) . 1_655 ? N4 Ag N3 73.57(13) 1_655 1_655 ? N1 Ag N2 70.74(13) . . ? N4 Ag N2 120.44(13) 1_655 . ? N3 Ag N2 114.82(10) 1_655 . ? C5 N1 C1 119.1(5) . . ? C5 N1 Ag 119.8(4) . . ? C1 N1 Ag 121.1(3) . . ? C21 N2 C7 114.2(3) . . ? C21 N2 C6 112.1(4) . . ? C7 N2 C6 114.6(3) . . ? C21 N2 Ag 110.7(3) . . ? C7 N2 Ag 104.6(2) . . ? C6 N2 Ag 99.2(3) . . ? C15 N3 C14 110.4(4) . . ? C15 N3 C22 111.3(4) . . ? C14 N3 C22 111.8(4) . . ? C15 N3 Ag 98.8(3) . 1_455 ? C14 N3 Ag 111.4(2) . 1_455 ? C22 N3 Ag 112.5(3) . 1_455 ? C16 N4 C20 117.9(4) . . ? C16 N4 Ag 117.6(4) . 1_455 ? C20 N4 Ag 124.4(3) . 1_455 ? N1 C1 C2 122.5(5) . . ? C3 C2 C1 118.9(5) . . ? C2 C3 C4 119.0(5) . . ? C3 C4 C5 121.2(6) . . ? N1 C5 C4 119.2(7) . . ? N1 C5 C6 119.7(6) . . ? C4 C5 C6 121.1(6) . . ? N2 C6 C5 112.1(4) . . ? C8 C7 C12 119.5(4) . . ? C8 C7 N2 119.5(4) . . ? C12 C7 N2 120.8(4) . . ? C7 C8 C9 121.2(4) . . ? C8 C9 C10 121.3(4) . . ? C11 C10 C9 117.7(4) . . ? C11 C10 C13 119.3(4) . . ? C9 C10 C13 122.9(4) . . ? C10 C11 C12 122.1(4) . . ? C7 C12 C11 118.1(4) . . ? C14 C13 C10 112.5(4) . . ? N3 C14 C13 114.7(4) . . ? N3 C15 C16 113.7(4) . . ? N4 C16 C17 123.1(6) . . ? N4 C16 C15 115.8(6) . . ? C17 C16 C15 120.9(6) . . ? C16 C17 C18 118.1(5) . . ? C19 C18 C17 118.7(5) . . ? C18 C19 C20 119.3(5) . . ? N4 C20 C19 122.8(5) . . ? O4 Cl1 O3 111.7(6) . . ? O4 Cl1 O2 110.3(4) . . ? O3 Cl1 O2 109.4(3) . . ? O4 Cl1 O1 110.8(5) . . ? O3 Cl1 O1 105.6(4) . . ? O2 Cl1 O1 108.9(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 Ag N1 C5 -107.0(4) 1_655 . . . ? N3 Ag N1 C5 123.1(4) 1_655 . . . ? N2 Ag N1 C5 15.5(4) . . . . ? N4 Ag N1 C1 75.8(6) 1_655 . . . ? N3 Ag N1 C1 -54.1(4) 1_655 . . . ? N2 Ag N1 C1 -161.8(4) . . . . ? N1 Ag N2 C21 86.5(3) . . . . ? N4 Ag N2 C21 -116.8(3) 1_655 . . . ? N3 Ag N2 C21 -32.0(3) 1_655 . . . ? N1 Ag N2 C7 -150.0(3) . . . . ? N4 Ag N2 C7 6.7(3) 1_655 . . . ? N3 Ag N2 C7 91.6(3) 1_655 . . . ? N1 Ag N2 C6 -31.4(3) . . . . ? N4 Ag N2 C6 125.3(3) 1_655 . . . ? N3 Ag N2 C6 -149.9(3) 1_655 . . . ? C5 N1 C1 C2 -1.2(7) . . . . ? Ag N1 C1 C2 176.0(4) . . . . ? N1 C1 C2 C3 0.0(8) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C1 N1 C5 C4 2.4(7) . . . . ? Ag N1 C5 C4 -174.8(4) . . . . ? C1 N1 C5 C6 -177.9(5) . . . . ? Ag N1 C5 C6 4.8(6) . . . . ? C3 C4 C5 N1 -2.6(8) . . . . ? C3 C4 C5 C6 177.7(5) . . . . ? C21 N2 C6 C5 -72.9(6) . . . . ? C7 N2 C6 C5 154.8(4) . . . . ? Ag N2 C6 C5 44.0(5) . . . . ? N1 C5 C6 N2 -39.5(7) . . . . ? C4 C5 C6 N2 140.1(5) . . . . ? C21 N2 C7 C8 179.8(4) . . . . ? C6 N2 C7 C8 -48.9(6) . . . . ? Ag N2 C7 C8 58.6(4) . . . . ? C21 N2 C7 C12 5.0(5) . . . . ? C6 N2 C7 C12 136.3(5) . . . . ? Ag N2 C7 C12 -116.2(3) . . . . ? C12 C7 C8 C9 -3.8(7) . . . . ? N2 C7 C8 C9 -178.7(4) . . . . ? C7 C8 C9 C10 3.5(8) . . . . ? C8 C9 C10 C11 -1.1(7) . . . . ? C8 C9 C10 C13 -177.4(4) . . . . ? C9 C10 C11 C12 -1.0(6) . . . . ? C13 C10 C11 C12 175.5(4) . . . . ? C8 C7 C12 C11 1.7(6) . . . . ? N2 C7 C12 C11 176.5(4) . . . . ? C10 C11 C12 C7 0.7(6) . . . . ? C11 C10 C13 C14 125.0(5) . . . . ? C9 C10 C13 C14 -58.7(6) . . . . ? C15 N3 C14 C13 -171.7(4) . . . . ? C22 N3 C14 C13 63.7(5) . . . . ? Ag N3 C14 C13 -63.0(5) 1_455 . . . ? C10 C13 C14 N3 163.4(4) . . . . ? C14 N3 C15 C16 164.6(4) . . . . ? C22 N3 C15 C16 -70.7(5) . . . . ? Ag N3 C15 C16 47.7(4) 1_455 . . . ? C20 N4 C16 C17 -0.6(8) . . . . ? Ag N4 C16 C17 -177.2(4) 1_455 . . . ? C20 N4 C16 C15 -176.4(4) . . . . ? Ag N4 C16 C15 7.0(6) 1_455 . . . ? N3 C15 C16 N4 -42.5(6) . . . . ? N3 C15 C16 C17 141.6(5) . . . . ? N4 C16 C17 C18 0.9(8) . . . . ? C15 C16 C17 C18 176.4(5) . . . . ? C16 C17 C18 C19 -0.7(8) . . . . ? C17 C18 C19 C20 0.4(8) . . . . ? C16 N4 C20 C19 0.3(7) . . . . ? Ag N4 C20 C19 176.6(4) 1_455 . . . ? C18 C19 C20 N4 -0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.471 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.063