Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'W. Clegg' 'Azizolla Beheshti' 'Sophie Dale' 'Farzanh Hussaini' 'Reza Hyvadi' _publ_contact_author_name 'W. Clegg' _publ_contact_author_address ; School of Natural Sciences (Chemistry) University of Newcastle Bedson Building NEWCASTLE UPON TYNE NE1 7RU UNITED KINGDOM ; _publ_contact_author_email W.CLEGG@NCL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, spectroscopic and crystallographic characterization of mixed-metal complexes of Ag/Cu and W/Mo and a complex of Ag with heterocyclic thione ligands ; data_ab45_compound_1 _database_code_depnum_ccdc_archive 'CCDC 636859' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Ag2 N4 S6 W' _chemical_formula_sum 'C6 H12 Ag2 N4 S6 W' _chemical_formula_weight 732.15 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' 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' W W -0.8490 6.8722 '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/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.3584(10) _cell_length_b 18.8244(11) _cell_length_c 13.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.281(10) _cell_angle_gamma 90.00 _cell_volume 1629.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 10.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.686 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14642 _diffrn_reflns_av_R_equivalents 0.1037 _diffrn_reflns_av_sigmaI/netI 0.0986 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3266 _reflns_number_gt 2218 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DIRAX _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0467P)^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 3266 _refine_ls_number_parameters 184 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.993 _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 W1 W 0.45886(9) 0.7500 0.40859(4) 0.00790(17) Uani 1 2 d S . . W2 W 0.74745(9) 0.7500 0.05691(4) 0.00717(17) Uani 1 2 d S . . Ag1 Ag -0.01156(19) 0.7500 0.57539(9) 0.0208(3) Uani 1 2 d S . . Ag2 Ag 0.49490(14) 0.63993(4) 0.15649(8) 0.0275(3) Uani 1 1 d . . . Ag3 Ag 1.0627(3) 0.7500 0.24655(12) 0.0547(5) Uani 1 2 d S . . S1 S -0.1686(4) 0.63562(15) 0.6361(2) 0.0199(7) Uani 1 1 d . . . S2 S 0.3246(5) 0.52085(14) 0.1431(2) 0.0182(7) Uani 1 1 d . . . S3 S 0.3901(6) 0.7500 0.5660(3) 0.0142(9) Uani 1 2 d S . . S4 S 0.7994(6) 0.7500 0.3948(3) 0.0192(9) Uani 1 2 d S . . S5 S 0.3312(5) 0.65164(16) 0.3401(2) 0.0257(8) Uani 1 1 d . . . S6 S 0.3905(5) 0.7500 0.0587(3) 0.0091(8) Uani 1 2 d S . . S7 S 0.8868(4) 0.65128(14) 0.1254(2) 0.0189(7) Uani 1 1 d . . . S8 S 0.8267(6) 0.7500 -0.0952(3) 0.0176(9) Uani 1 2 d S . . N1 N -0.0193(15) 0.5027(4) 0.6587(7) 0.0218(16) Uani 1 1 d U . . H1 H -0.1345 0.4892 0.6872 0.026 Uiso 1 1 calc R . . N2 N 0.1932(15) 0.5712(5) 0.5825(7) 0.0237(17) Uani 1 1 d U . . H2 H 0.2422 0.6097 0.5550 0.028 Uiso 1 1 calc R . . N3 N 0.5036(15) 0.3948(5) 0.1825(7) 0.0259(17) Uani 1 1 d U . . H3 H 0.3903 0.3797 0.2112 0.031 Uiso 1 1 calc R . . N4 N 0.7144(14) 0.4670(5) 0.1103(7) 0.0224(16) Uani 1 1 d U . . H4 H 0.7622 0.5075 0.0880 0.027 Uiso 1 1 calc R . . C1 C 0.0114(18) 0.5688(6) 0.6255(8) 0.0193(17) Uani 1 1 d U . . C2 C 0.1588(17) 0.4554(6) 0.6425(8) 0.0201(17) Uani 1 1 d U . . H2A H 0.1144 0.4131 0.6038 0.024 Uiso 1 1 calc R . . H2B H 0.2266 0.4398 0.7056 0.024 Uiso 1 1 calc R . . C3 C 0.3063(18) 0.5029(5) 0.5850(9) 0.0214(18) Uani 1 1 d U . . H3A H 0.4458 0.5074 0.6193 0.026 Uiso 1 1 calc R . . H3B H 0.3248 0.4843 0.5179 0.026 Uiso 1 1 calc R . . C4 C 0.5225(18) 0.4591(5) 0.1446(8) 0.0195(17) Uani 1 1 d U . . C5 C 0.6934(18) 0.3511(6) 0.1712(9) 0.0229(18) Uani 1 1 d U . . H5A H 0.6600 0.3071 0.1338 0.027 Uiso 1 1 calc R . . H5B H 0.7588 0.3382 0.2359 0.027 Uiso 1 1 calc R . . C6 C 0.8394(18) 0.4003(5) 0.1135(9) 0.0225(18) Uani 1 1 d U . . H6A H 0.9772 0.4070 0.1486 0.027 Uiso 1 1 calc R . . H6B H 0.8619 0.3817 0.0467 0.027 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 W1 0.0082(3) 0.0072(3) 0.0083(3) 0.000 0.0000(3) 0.000 W2 0.0063(3) 0.0067(3) 0.0085(3) 0.000 -0.0001(3) 0.000 Ag1 0.0215(7) 0.0094(6) 0.0309(8) 0.000 -0.0036(6) 0.000 Ag2 0.0179(5) 0.0149(5) 0.0497(7) 0.0167(5) 0.0009(5) -0.0012(4) Ag3 0.0450(11) 0.0883(14) 0.0303(9) 0.000 -0.0026(8) 0.000 S1 0.0168(16) 0.0135(15) 0.0297(18) 0.0079(13) 0.0055(13) 0.0026(13) S2 0.0182(16) 0.0081(14) 0.0287(18) -0.0002(13) 0.0039(13) 0.0006(12) S3 0.018(2) 0.016(2) 0.009(2) 0.000 0.0011(17) 0.000 S4 0.012(2) 0.028(2) 0.018(2) 0.000 0.0000(18) 0.000 S5 0.0229(18) 0.0252(18) 0.0296(19) -0.0155(15) 0.0066(14) -0.0100(14) S6 0.0027(18) 0.0085(19) 0.016(2) 0.000 -0.0017(16) 0.000 S7 0.0134(15) 0.0179(16) 0.0254(17) 0.0114(13) 0.0026(13) 0.0092(12) S8 0.017(2) 0.022(2) 0.013(2) 0.000 0.0016(18) 0.000 N1 0.026(4) 0.012(3) 0.029(4) 0.003(3) 0.009(3) -0.003(3) N2 0.026(4) 0.014(3) 0.031(4) 0.006(3) 0.009(3) -0.003(3) N3 0.023(4) 0.014(3) 0.041(4) 0.007(3) 0.008(3) 0.005(3) N4 0.020(4) 0.015(3) 0.033(4) 0.003(3) 0.010(3) 0.008(3) C1 0.021(4) 0.011(3) 0.025(4) 0.004(3) 0.005(3) -0.004(3) C2 0.026(4) 0.011(3) 0.023(4) 0.003(3) 0.007(3) -0.001(3) C3 0.025(4) 0.013(4) 0.026(4) 0.001(3) 0.008(3) -0.002(3) C4 0.020(4) 0.009(3) 0.029(4) 0.001(3) 0.007(3) 0.004(3) C5 0.022(4) 0.015(4) 0.032(4) 0.003(3) 0.005(4) 0.006(3) C6 0.021(4) 0.015(4) 0.032(4) 0.001(4) 0.006(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 S3 2.206(4) . ? W1 S4 2.181(4) . ? W1 S5 2.213(3) . ? W1 S5 2.213(3) 4_575 ? W2 S6 2.271(4) . ? W2 S7 2.246(3) . ? W2 S7 2.246(3) 4_575 ? W2 S8 2.152(4) . ? Ag1 S1 2.526(3) . ? Ag1 S1 2.526(3) 4_575 ? Ag1 S3 2.562(4) . ? Ag1 S4 2.695(4) 1_455 ? Ag2 S2 2.493(3) . ? Ag2 S5 2.756(3) . ? Ag2 S6 2.538(2) . ? Ag2 S7 2.553(3) . ? Ag3 S4 2.674(5) . ? Ag3 S5 2.792(4) 4_675 ? Ag3 S5 2.792(4) 1_655 ? Ag3 S6 3.365(4) 1_655 ? Ag3 S7 2.699(3) . ? Ag3 S7 2.699(3) 4_575 ? S1 C1 1.710(11) . ? S2 C4 1.713(11) . ? S4 Ag1 2.695(4) 1_655 ? S5 Ag3 2.792(4) 1_455 ? S6 Ag2 2.538(2) 4_575 ? N1 C1 1.340(13) . ? N1 C2 1.465(13) . ? N2 C1 1.317(14) . ? N2 C3 1.473(13) . ? N3 C4 1.323(13) . ? N3 C5 1.473(13) . ? N4 C4 1.332(13) . ? N4 C6 1.486(13) . ? C2 C3 1.533(14) . ? C5 C6 1.547(15) . ? 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 S3 W1 S4 108.64(15) . . ? S3 W1 S5 109.05(10) . . ? S3 W1 S5 109.05(10) . 4_575 ? S4 W1 S5 108.20(10) . . ? S4 W1 S5 108.20(10) . 4_575 ? S5 W1 S5 113.59(18) . 4_575 ? S6 W2 S7 111.93(9) . . ? S6 W2 S7 111.93(9) . 4_575 ? S6 W2 S8 106.42(14) . . ? S7 W2 S7 111.70(16) . 4_575 ? S7 W2 S8 107.24(10) . . ? S7 W2 S8 107.24(10) 4_575 . ? S1 Ag1 S1 116.91(14) . 4_575 ? S1 Ag1 S3 115.09(8) . . ? S1 Ag1 S3 115.09(8) 4_575 . ? S1 Ag1 S4 97.55(9) . 1_455 ? S1 Ag1 S4 97.55(9) 4_575 1_455 ? S3 Ag1 S4 111.33(13) . 1_455 ? S2 Ag2 S5 87.68(9) . . ? S2 Ag2 S6 126.31(10) . . ? S2 Ag2 S7 119.14(10) . . ? S5 Ag2 S6 108.12(11) . . ? S5 Ag2 S7 123.38(10) . . ? S6 Ag2 S7 94.66(10) . . ? S4 Ag3 S5 92.58(10) . 4_675 ? S4 Ag3 S5 92.58(10) . 1_655 ? S4 Ag3 S6 179.53(12) . 1_655 ? S4 Ag3 S7 101.86(10) . . ? S4 Ag3 S7 101.86(10) . 4_575 ? S5 Ag3 S5 83.08(12) 4_675 1_655 ? S5 Ag3 S6 87.77(9) 4_675 1_655 ? S5 Ag3 S6 87.77(9) 1_655 1_655 ? S5 Ag3 S7 165.23(11) 4_675 . ? S5 Ag3 S7 93.08(8) 4_675 4_575 ? S5 Ag3 S7 93.08(8) 1_655 . ? S5 Ag3 S7 165.23(12) 1_655 4_575 ? S6 Ag3 S7 77.81(8) 1_655 . ? S6 Ag3 S7 77.81(8) 1_655 4_575 ? S7 Ag3 S7 87.04(12) . 4_575 ? Ag1 S1 C1 108.9(4) . . ? Ag2 S2 C4 107.0(4) . . ? W1 S3 Ag1 106.56(15) . . ? W1 S4 Ag1 109.24(16) . 1_655 ? W1 S4 Ag3 135.93(18) . . ? Ag1 S4 Ag3 114.83(15) 1_655 . ? W1 S5 Ag2 107.71(12) . . ? W1 S5 Ag3 81.08(10) . 1_455 ? Ag2 S5 Ag3 83.38(10) . 1_455 ? W2 S6 Ag2 76.40(9) . . ? W2 S6 Ag2 76.40(9) . 4_575 ? Ag2 S6 Ag2 109.48(14) . 4_575 ? W2 S7 Ag2 76.51(8) . . ? W2 S7 Ag3 80.28(9) . . ? Ag2 S7 Ag3 109.84(11) . . ? C1 N1 C2 112.9(9) . . ? C1 N2 C3 113.4(9) . . ? C4 N3 C5 112.5(9) . . ? C4 N4 C6 113.1(9) . . ? S1 C1 N1 123.1(9) . . ? S1 C1 N2 127.9(9) . . ? N1 C1 N2 108.9(10) . . ? N1 C2 C3 102.4(8) . . ? N2 C3 C2 102.3(9) . . ? S2 C4 N3 123.2(9) . . ? S2 C4 N4 127.1(8) . . ? N3 C4 N4 109.7(9) . . ? N3 C5 C6 103.3(8) . . ? N4 C6 C5 100.9(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 S2 0.88 2.66 3.417(10) 145 3_566 N1 H1 S5 0.88 2.95 3.519(9) 124 3_566 N2 H2 S3 0.88 2.80 3.602(9) 151 . N3 H3 S1 0.88 2.58 3.376(10) 152 3_566 N4 H4 S7 0.88 2.86 3.642(10) 149 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.446 _refine_diff_density_min -2.683 _refine_diff_density_rms 0.342 #===END data_ab52_compound_2 _database_code_depnum_ccdc_archive 'CCDC 636860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Ag2 N8 S8 W' _chemical_formula_sum 'C20 H40 Ag2 N8 S8 W' _chemical_formula_weight 1048.67 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' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 14.690(3) _cell_length_b 11.060(2) _cell_length_c 21.173(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.55(3) _cell_angle_gamma 90.00 _cell_volume 3423.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 309 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 4.999 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.324 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_process_details 'Bruker SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23263 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3901 _reflns_number_gt 3385 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0100P)^2^+2.8096P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary . _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3901 _refine_ls_number_parameters 189 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0358 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.043 _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 W1 W 0.2500 0.741076(11) 0.5000 0.01457(4) Uani 1 2 d S . . Ag1 Ag 0.380433(13) 0.718916(16) 0.618748(9) 0.02132(5) Uani 1 1 d . . . S1 S 0.52399(4) 0.58876(5) 0.63438(3) 0.02565(15) Uani 1 1 d . . . N1 N 0.43718(15) 0.44049(18) 0.54932(10) 0.0234(5) Uani 1 1 d D . . H1 H 0.4309(18) 0.5080(14) 0.5279(11) 0.028 Uiso 1 1 d D . . C1 C 0.48389(16) 0.4505(2) 0.60684(11) 0.0183(5) Uani 1 1 d . . . C2 C 0.36360(19) 0.3546(2) 0.53066(13) 0.0314(7) Uani 1 1 d . . . H2A H 0.3349 0.3781 0.4882 0.038 Uiso 1 1 calc R . . H2B H 0.3164 0.3625 0.5608 0.038 Uiso 1 1 calc R . . C3 C 0.3910(2) 0.2233(2) 0.52819(14) 0.0356(7) Uani 1 1 d . . . H3A H 0.4414 0.2153 0.5007 0.043 Uiso 1 1 calc R . . H3B H 0.3384 0.1760 0.5086 0.043 Uiso 1 1 calc R . . C4 C 0.4214(2) 0.1702(2) 0.59290(14) 0.0350(7) Uani 1 1 d . . . H4A H 0.3727 0.1826 0.6215 0.042 Uiso 1 1 calc R . . H4B H 0.4309 0.0821 0.5887 0.042 Uiso 1 1 calc R . . C5 C 0.50915(18) 0.2282(2) 0.62175(13) 0.0234(6) Uani 1 1 d . . . H5A H 0.5338 0.1789 0.6585 0.028 Uiso 1 1 calc R . . H5B H 0.5544 0.2259 0.5900 0.028 Uiso 1 1 calc R . . N2 N 0.50050(14) 0.35354(17) 0.64292(9) 0.0186(4) Uani 1 1 d D . . H2 H 0.5337(15) 0.366(2) 0.6786(7) 0.022 Uiso 1 1 d D . . S2 S 0.37105(5) 0.82670(6) 0.72269(3) 0.02714(15) Uani 1 1 d . . . C6 C 0.28367(17) 0.9292(2) 0.71347(11) 0.0195(5) Uani 1 1 d . . . N3 N 0.21800(14) 0.92098(18) 0.66546(10) 0.0226(5) Uani 1 1 d D . . H3 H 0.2232(18) 0.8558(15) 0.6431(10) 0.027 Uiso 1 1 d D . . C7 C 0.17036(18) 1.0235(2) 0.63320(12) 0.0258(6) Uani 1 1 d . . . H7A H 0.1396 0.9946 0.5923 0.031 Uiso 1 1 calc R . . H7B H 0.2166 1.0841 0.6234 0.031 Uiso 1 1 calc R . . C8 C 0.09984(17) 1.0859(2) 0.66955(12) 0.0259(6) Uani 1 1 d . . . H8A H 0.0567 1.0247 0.6833 0.031 Uiso 1 1 calc R . . H8B H 0.0645 1.1435 0.6410 0.031 Uiso 1 1 calc R . . C9 C 0.14279(18) 1.1535(2) 0.72743(12) 0.0244(6) Uani 1 1 d . . . H9A H 0.1853 1.2155 0.7136 0.029 Uiso 1 1 calc R . . H9B H 0.0942 1.1958 0.7481 0.029 Uiso 1 1 calc R . . C10 C 0.19451(18) 1.0704(2) 0.77525(12) 0.0254(6) Uani 1 1 d . . . H10A H 0.2092 1.1158 0.8152 0.030 Uiso 1 1 calc R . . H10B H 0.1537 1.0027 0.7845 0.030 Uiso 1 1 calc R . . N4 N 0.27993(15) 1.01965(18) 0.75536(10) 0.0230(5) Uani 1 1 d D . . H4 H 0.3263(13) 1.026(2) 0.7847(10) 0.028 Uiso 1 1 d D . . S3 S 0.36936(5) 0.85993(6) 0.52217(3) 0.02406(14) Uani 1 1 d . . . S4 S 0.22232(4) 0.62375(5) 0.58068(3) 0.01954(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01623(7) 0.01427(7) 0.01268(7) 0.000 -0.00123(5) 0.000 Ag1 0.02105(11) 0.02138(10) 0.02056(11) -0.00230(7) -0.00301(8) 0.00387(7) S1 0.0205(3) 0.0169(3) 0.0373(4) -0.0030(3) -0.0086(3) 0.0031(2) N1 0.0256(12) 0.0230(11) 0.0201(12) 0.0016(8) -0.0052(10) 0.0042(9) C1 0.0137(12) 0.0192(12) 0.0218(13) -0.0022(9) 0.0001(10) 0.0033(9) C2 0.0248(15) 0.0381(16) 0.0285(15) -0.0066(12) -0.0112(13) 0.0018(12) C3 0.0275(16) 0.0370(17) 0.0395(18) -0.0157(12) -0.0115(14) 0.0001(12) C4 0.0311(16) 0.0241(15) 0.0479(19) -0.0061(12) -0.0057(14) -0.0053(12) C5 0.0247(14) 0.0159(12) 0.0280(14) -0.0007(9) -0.0054(12) 0.0032(10) N2 0.0178(11) 0.0193(10) 0.0176(11) -0.0016(8) -0.0038(9) -0.0012(8) S2 0.0242(4) 0.0348(4) 0.0207(3) -0.0090(3) -0.0069(3) 0.0115(3) C6 0.0174(13) 0.0221(12) 0.0191(13) -0.0008(9) 0.0023(10) -0.0005(10) N3 0.0174(11) 0.0247(11) 0.0245(12) -0.0103(8) -0.0045(10) 0.0059(9) C7 0.0234(14) 0.0316(14) 0.0205(14) -0.0029(10) -0.0072(12) 0.0036(11) C8 0.0195(14) 0.0224(13) 0.0347(16) -0.0039(11) -0.0031(12) 0.0046(10) C9 0.0241(14) 0.0187(12) 0.0308(15) -0.0036(10) 0.0040(12) 0.0025(10) C10 0.0315(16) 0.0248(13) 0.0210(13) -0.0037(10) 0.0075(12) 0.0059(11) N4 0.0211(12) 0.0259(11) 0.0206(12) -0.0076(8) -0.0046(10) 0.0032(9) S3 0.0286(4) 0.0227(3) 0.0201(3) 0.0014(2) -0.0013(3) -0.0105(3) S4 0.0188(3) 0.0205(3) 0.0190(3) 0.0048(2) 0.0000(3) -0.0026(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 S3 2.2053(7) . ? W1 S4 2.2139(7) . ? Ag1 S1 2.5483(8) . ? Ag1 S2 2.5185(7) . ? Ag1 S3 2.5643(7) . ? Ag1 S4 2.6058(8) . ? S1 C1 1.720(2) . ? N1 C1 1.343(3) . ? N1 C2 1.464(3) . ? C1 N2 1.326(3) . ? C2 C3 1.509(4) . ? C3 C4 1.518(4) . ? C4 C5 1.515(3) . ? C5 N2 1.466(3) . ? S2 C6 1.710(2) . ? C6 N3 1.335(3) . ? C6 N4 1.342(3) . ? N3 C7 1.466(3) . ? C7 C8 1.515(3) . ? C8 C9 1.520(3) . ? C9 C10 1.516(3) . ? C10 N4 1.473(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 W1 S3 106.82(4) . 2_556 ? S3 W1 S4 112.75(3) . . ? S3 W1 S4 108.18(3) 2_556 . ? S3 W1 S4 108.18(3) . 2_556 ? S3 W1 S4 112.75(3) 2_556 2_556 ? S4 W1 S4 108.24(4) . 2_556 ? S1 Ag1 S2 105.57(3) . . ? S1 Ag1 S3 115.79(3) . . ? S1 Ag1 S4 120.91(2) . . ? S2 Ag1 S3 113.85(3) . . ? S2 Ag1 S4 109.82(3) . . ? S3 Ag1 S4 90.75(3) . . ? Ag1 S1 C1 101.90(8) . . ? C1 N1 C2 126.7(2) . . ? S1 C1 N1 120.60(18) . . ? S1 C1 N2 119.08(18) . . ? N1 C1 N2 120.3(2) . . ? N1 C2 C3 116.2(2) . . ? C2 C3 C4 113.4(2) . . ? C3 C4 C5 111.4(2) . . ? C4 C5 N2 115.4(2) . . ? C1 N2 C5 127.3(2) . . ? Ag1 S2 C6 108.54(9) . . ? S2 C6 N3 121.40(18) . . ? S2 C6 N4 119.82(18) . . ? N3 C6 N4 118.8(2) . . ? C6 N3 C7 125.4(2) . . ? N3 C7 C8 115.7(2) . . ? C7 C8 C9 112.5(2) . . ? C8 C9 C10 112.4(2) . . ? C9 C10 N4 115.2(2) . . ? C6 N4 C10 124.3(2) . . ? W1 S3 Ag1 78.17(3) . . ? W1 S4 Ag1 77.13(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S2 0.870(10) 2.440(12) 3.272(2) 160(2) 4_546 N3 H3 S4 0.869(10) 2.887(11) 3.749(2) 172(2) . N4 H4 S1 0.879(10) 2.743(11) 3.610(2) 169(2) 4_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.515 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.096 #===END data_ab58_compound_4 _database_code_depnum_ccdc_archive 'CCDC 636861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Cu2 N8 S8 W' _chemical_formula_sum 'C20 H40 Cu2 N8 S8 W' _chemical_formula_weight 960.01 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 14.4050(19) _cell_length_b 11.0792(15) _cell_length_c 21.036(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.087(2) _cell_angle_gamma 90.00 _cell_volume 3315.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6406 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 28.28 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 5.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.216 _exptl_absorpt_correction_T_max 0.548 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14153 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3796 _reflns_number_gt 3663 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0171P)^2^+6.5486P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00092(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3796 _refine_ls_number_parameters 286 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0415 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.231 _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 W1 W 0.2500 0.721263(12) 0.5000 0.01549(5) Uani 1 2 d S . . Cu1 Cu 0.36826(2) 0.71123(3) 0.614733(15) 0.02572(8) Uani 1 1 d . . . S1 S 0.50108(5) 0.59155(6) 0.64939(4) 0.03505(17) Uani 1 1 d D B . C1 C 0.47967(17) 0.4525(2) 0.61436(11) 0.0233(5) Uani 1 1 d D . . N1 N 0.43675(19) 0.4423(2) 0.55327(11) 0.0348(6) Uani 1 1 d D A . H1 H 0.425(2) 0.5119(18) 0.5343(16) 0.042 Uiso 1 1 d D . . C2 C 0.3691(6) 0.3514(6) 0.5269(4) 0.056(2) Uani 0.50 1 d PDU A 1 H2A H 0.3068 0.3910 0.5182 0.067 Uiso 0.50 1 calc PR A 1 H2B H 0.3852 0.3265 0.4847 0.067 Uiso 0.50 1 calc PR A 1 C3 C 0.3589(4) 0.2477(5) 0.5613(3) 0.0370(12) Uani 0.50 1 d PDU A 1 H3A H 0.3214 0.1928 0.5301 0.044 Uiso 0.50 1 calc PR A 1 H3B H 0.3173 0.2709 0.5924 0.044 Uiso 0.50 1 calc PR A 1 C4 C 0.4324(2) 0.1696(3) 0.59843(17) 0.0415(7) Uani 1 1 d D . . H4A H 0.4475 0.1032 0.5702 0.050 Uiso 0.50 1 calc PR A 1 H4B H 0.4066 0.1329 0.6348 0.050 Uiso 0.50 1 calc PR A 1 H4C H 0.3853 0.1819 0.6273 0.050 Uiso 0.50 1 calc PR A 2 H4D H 0.4451 0.0820 0.5962 0.050 Uiso 0.50 1 calc PR A 2 C5 C 0.52160(19) 0.2354(2) 0.62437(14) 0.0284(6) Uani 1 1 d D A . H5A H 0.5573 0.1869 0.6595 0.034 Uiso 1 1 calc R . . H5B H 0.5606 0.2422 0.5897 0.034 Uiso 1 1 calc R . . N2 N 0.50696(16) 0.3555(2) 0.64876(10) 0.0256(5) Uani 1 1 d D A . H2 H 0.5366(19) 0.369(3) 0.6875(8) 0.031 Uiso 1 1 d D . . C2X C 0.4094(5) 0.3363(7) 0.5170(3) 0.0352(14) Uani 0.50 1 d PU A 2 H2C H 0.3499 0.3606 0.4897 0.042 Uiso 0.50 1 calc PR A 2 H2D H 0.4561 0.3313 0.4872 0.042 Uiso 0.50 1 calc PR A 2 C3X C 0.3940(5) 0.2183(7) 0.5305(4) 0.0453(15) Uani 0.50 1 d PU A 2 H3C H 0.4210 0.1683 0.4989 0.054 Uiso 0.50 1 calc PR A 2 H3D H 0.3252 0.2047 0.5227 0.054 Uiso 0.50 1 calc PR A 2 S2 S 0.34743(12) 0.78427(14) 0.71577(6) 0.0246(3) Uani 0.50 1 d PD B 1 N3 N 0.2675(4) 0.9697(4) 0.6479(2) 0.0261(10) Uani 0.50 1 d PD B 1 H3 H 0.300(4) 0.940(5) 0.620(2) 0.031 Uiso 0.50 1 d PD C 1 C6 C 0.2745(5) 0.9061(6) 0.7021(3) 0.020(2) Uani 0.50 1 d PD B 1 C7 C 0.1875(7) 1.0407(8) 0.6169(5) 0.029(3) Uani 0.50 1 d PD B 1 H7A H 0.1313 0.9880 0.6110 0.035 Uiso 0.50 1 calc PR B 1 H7B H 0.1996 1.0640 0.5735 0.035 Uiso 0.50 1 calc PR B 1 C8 C 0.1648(5) 1.1520(5) 0.6510(3) 0.0401(15) Uani 0.50 1 d PD B 1 H8A H 0.2220 1.2028 0.6590 0.048 Uiso 0.50 1 calc PR B 1 H8B H 0.1165 1.1978 0.6220 0.048 Uiso 0.50 1 calc PR B 1 C9 C 0.1303(13) 1.1336(15) 0.7133(5) 0.048(4) Uani 0.50 1 d PD B 1 H9A H 0.0686 1.0924 0.7049 0.058 Uiso 0.50 1 calc PR B 1 H9B H 0.1205 1.2135 0.7323 0.058 Uiso 0.50 1 calc PR B 1 C10 C 0.1952(11) 1.0614(11) 0.7610(8) 0.033(5) Uani 0.50 1 d PD B 1 H10A H 0.2536 1.1092 0.7718 0.040 Uiso 0.50 1 calc PR B 1 H10B H 0.1662 1.0573 0.8006 0.040 Uiso 0.50 1 calc PR B 1 N4 N 0.2235(4) 0.9391(4) 0.7476(2) 0.0298(10) Uani 0.50 1 d PD B 1 H4 H 0.222(5) 0.881(4) 0.776(2) 0.036 Uiso 0.50 1 d PD D 1 S2X S 0.37903(10) 0.83796(16) 0.70490(6) 0.0242(3) Uani 0.50 1 d PD B 2 N3X N 0.2177(3) 0.9330(4) 0.6497(2) 0.0229(9) Uani 0.50 1 d PD B 2 H3X H 0.218(4) 0.870(3) 0.625(2) 0.027 Uiso 0.50 1 d PD E 2 C6X C 0.2890(4) 0.9396(6) 0.6987(3) 0.0166(17) Uani 0.50 1 d PD B 2 C7X C 0.1612(7) 1.0346(9) 0.6214(4) 0.027(3) Uani 0.50 1 d PD B 2 H7C H 0.1249 1.0078 0.5799 0.033 Uiso 0.50 1 calc PR B 2 H7D H 0.2046 1.0990 0.6117 0.033 Uiso 0.50 1 calc PR B 2 C8X C 0.0939(4) 1.0885(5) 0.6609(3) 0.0307(12) Uani 0.50 1 d PD B 2 H8C H 0.0556 1.1505 0.6350 0.037 Uiso 0.50 1 calc PR B 2 H8D H 0.0508 1.0246 0.6716 0.037 Uiso 0.50 1 calc PR B 2 C9X C 0.1419(11) 1.1447(15) 0.7220(4) 0.034(3) Uani 0.50 1 d PD B 2 H9C H 0.1787 1.2143 0.7101 0.041 Uiso 0.50 1 calc PR B 2 H9D H 0.0924 1.1775 0.7449 0.041 Uiso 0.50 1 calc PR B 2 C10X C 0.2059(10) 1.0694(11) 0.7687(8) 0.020(3) Uani 0.50 1 d PD B 2 H10C H 0.2271 1.1181 0.8078 0.024 Uiso 0.50 1 calc PR B 2 H10D H 0.1699 0.9999 0.7817 0.024 Uiso 0.50 1 calc PR B 2 N4X N 0.2883(3) 1.0238(4) 0.74445(19) 0.0220(8) Uani 0.50 1 d PD B 2 H4X H 0.340(2) 1.028(6) 0.772(2) 0.026 Uiso 0.50 1 d PD F 2 S3 S 0.37567(4) 0.83579(6) 0.52796(3) 0.02601(13) Uani 1 1 d . B . S4 S 0.23016(4) 0.60585(6) 0.58226(3) 0.02398(13) Uani 1 1 d . B . 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 W1 0.01438(7) 0.01989(8) 0.01177(7) 0.000 0.00079(4) 0.000 Cu1 0.02107(16) 0.03636(18) 0.01763(15) -0.00728(12) -0.00339(12) 0.00851(12) S1 0.0239(3) 0.0264(3) 0.0483(4) -0.0035(3) -0.0145(3) 0.0045(3) C1 0.0174(11) 0.0304(13) 0.0221(12) 0.0001(10) 0.0029(9) 0.0033(10) N1 0.0433(14) 0.0359(13) 0.0217(11) 0.0031(10) -0.0054(10) 0.0111(11) C2 0.055(4) 0.047(3) 0.051(4) -0.014(3) -0.039(4) 0.020(4) C3 0.020(3) 0.054(3) 0.034(3) -0.016(2) -0.004(2) -0.001(2) C4 0.0358(16) 0.0372(16) 0.0477(18) -0.0011(14) -0.0046(14) -0.0084(13) C5 0.0248(13) 0.0279(13) 0.0304(14) -0.0016(11) -0.0017(11) 0.0046(10) N2 0.0317(12) 0.0265(11) 0.0164(10) 0.0003(8) -0.0027(8) 0.0020(9) C2X 0.028(3) 0.051(3) 0.023(3) -0.008(2) -0.007(2) 0.023(3) C3X 0.037(3) 0.053(3) 0.040(3) -0.012(3) -0.013(3) 0.001(3) S2 0.0320(8) 0.0264(7) 0.0137(6) -0.0017(5) -0.0021(5) 0.0038(6) N3 0.044(3) 0.018(2) 0.018(2) 0.0009(17) 0.011(2) 0.001(2) C6 0.029(4) 0.014(3) 0.018(3) -0.002(2) 0.006(2) -0.010(3) C7 0.040(7) 0.024(4) 0.022(3) 0.003(3) 0.007(4) -0.001(4) C8 0.064(4) 0.024(3) 0.035(3) 0.006(2) 0.015(3) 0.011(3) C9 0.055(8) 0.055(9) 0.038(6) 0.020(5) 0.019(5) 0.041(7) C10 0.048(8) 0.034(7) 0.019(6) -0.011(4) 0.013(6) -0.002(5) N4 0.048(3) 0.022(2) 0.021(2) 0.0030(17) 0.012(2) 0.004(2) S2X 0.0193(6) 0.0357(8) 0.0161(6) -0.0070(6) -0.0022(5) 0.0042(6) N3X 0.017(2) 0.024(2) 0.027(2) -0.0085(18) -0.0010(18) -0.0020(19) C6X 0.014(3) 0.017(4) 0.019(3) -0.001(2) 0.003(2) -0.005(3) C7X 0.026(5) 0.030(4) 0.022(4) 0.002(3) -0.008(3) -0.006(3) C8X 0.027(3) 0.022(2) 0.037(3) -0.008(2) -0.011(2) 0.007(2) C9X 0.036(5) 0.034(5) 0.030(5) 0.000(4) 0.002(4) -0.003(4) C10X 0.027(4) 0.014(4) 0.017(4) -0.003(3) -0.004(3) 0.001(3) N4X 0.021(2) 0.027(2) 0.0163(19) -0.0042(16) -0.0016(15) -0.0002(17) S3 0.0228(3) 0.0273(3) 0.0283(3) -0.0069(3) 0.0053(2) -0.0071(2) S4 0.0231(3) 0.0320(3) 0.0165(3) 0.0070(2) 0.0022(2) 0.0013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate PRIVILEGED DOCUMENT FOR REVIEW PURPOSES ONLY (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 W1 S3 2.2129(7) . ? W1 S4 2.2061(7) . ? Cu1 S1 2.3473(7) . ? Cu1 S2 2.3375(14) . ? Cu1 S2X 2.3454(13) . ? Cu1 S3 2.3042(8) . ? Cu1 S4 2.3147(8) . ? S1 C1 1.714(3) . ? C1 N1 1.340(3) . ? C1 N2 1.320(3) . ? N1 C2 1.449(6) . ? N1 C2X 1.422(8) . ? C2 C3 1.377(7) . ? C3 C4 1.490(5) . ? C4 C5 1.503(4) . ? C4 C3X 1.546(8) . ? C5 N2 1.454(3) . ? C2X C3X 1.364(11) . ? S2 C6 1.707(6) . ? N3 C6 1.331(6) . ? N3 C7 1.460(7) . ? C6 N4 1.345(6) . ? C7 C8 1.489(7) . ? C8 C9 1.487(8) . ? C9 C10 1.491(7) . ? C10 N4 1.456(8) . ? S2X C6X 1.707(6) . ? N3X C6X 1.337(6) . ? N3X C7X 1.460(7) . ? C6X N4X 1.342(6) . ? C7X C8X 1.498(7) . ? C8X C9X 1.494(8) . ? C9X C10X 1.493(7) . ? C10X N4X 1.454(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 W1 S3 110.03(4) . 2_556 ? S3 W1 S4 109.01(3) . . ? S3 W1 S4 109.81(2) . 2_556 ? S3 W1 S4 109.81(2) 2_556 . ? S3 W1 S4 109.01(3) 2_556 2_556 ? S4 W1 S4 109.16(4) . 2_556 ? S1 Cu1 S2 97.39(4) . . ? S1 Cu1 S2X 98.08(4) . . ? S1 Cu1 S3 116.54(3) . . ? S1 Cu1 S4 115.29(3) . . ? S2 Cu1 S3 122.79(5) . . ? S2 Cu1 S4 102.43(5) . . ? S2X Cu1 S3 106.06(5) . . ? S2X Cu1 S4 118.99(5) . . ? S3 Cu1 S4 102.33(2) . . ? Cu1 S1 C1 106.95(8) . . ? S1 C1 N1 120.8(2) . . ? S1 C1 N2 118.56(18) . . ? N1 C1 N2 120.6(2) . . ? C1 N1 C2 127.3(4) . . ? C1 N1 C2X 129.2(4) . . ? N1 C2 C3 120.0(5) . . ? C2 C3 C4 129.3(5) . . ? C3 C4 C5 113.8(3) . . ? C5 C4 C3X 109.1(4) . . ? C4 C5 N2 114.1(2) . . ? C1 N2 C5 126.8(2) . . ? N1 C2X C3X 136.1(6) . . ? C4 C3X C2X 118.7(5) . . ? Cu1 S2 C6 106.6(2) . . ? C6 N3 C7 127.9(7) . . ? S2 C6 N3 121.6(5) . . ? S2 C6 N4 119.0(4) . . ? N3 C6 N4 119.4(5) . . ? N3 C7 C8 116.7(7) . . ? C7 C8 C9 116.1(9) . . ? C8 C9 C10 113.9(12) . . ? C9 C10 N4 122.3(14) . . ? C6 N4 C10 126.2(8) . . ? Cu1 S2X C6X 112.4(2) . . ? C6X N3X C7X 125.6(7) . . ? S2X C6X N3X 120.3(4) . . ? S2X C6X N4X 119.7(4) . . ? N3X C6X N4X 119.9(5) . . ? N3X C7X C8X 116.6(6) . . ? C7X C8X C9X 113.1(9) . . ? C8X C9X C10X 119.1(15) . . ? C9X C10X N4X 114.6(13) . . ? C6X N4X C10X 126.3(8) . . ? W1 S3 Cu1 74.26(2) . . ? W1 S4 Cu1 74.18(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S2X 0.872(11) 2.419(15) 3.258(2) 162(3) 4_546 N2 H2 S2 0.872(11) 2.60(2) 3.355(3) 146(3) 4_546 N3 H3 S3 0.880(12) 2.625(16) 3.497(5) 172(6) . N4 H4 S2 0.878(12) 2.11(4) 2.830(5) 139(6) 7_566 N4 H4 S4 0.878(12) 2.96(5) 3.570(4) 128(5) 7_566 N4X H4X S1 0.877(12) 2.692(18) 3.552(4) 167(5) 4_556 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.807 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.075 #===END data_ab53_compound_5 _database_code_depnum_ccdc_archive 'CCDC 636862' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H10 Ag I N2 S' _chemical_formula_sum 'C5 H10 Ag I N2 S' _chemical_formula_weight 364.98 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6065(7) _cell_length_b 13.3546(11) _cell_length_c 13.7726(11) _cell_angle_alpha 111.035(1) _cell_angle_beta 107.816(1) _cell_angle_gamma 90.096(1) _cell_volume 1395.5(2) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10916 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.82 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 5.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.081 _exptl_absorpt_correction_T_max 0.173 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10747 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5412 _reflns_number_gt 5065 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. Some NH hydrogen atoms selected from difference Fourier map, some placed in positions between N and I. N-H bond lengths restrained to be 0.88 \%A using DFIX 0.88(1) \%A. ; _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^)+(0.0327P)^2^+9.6054P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5412 _refine_ls_number_parameters 290 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.200 _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 0.42440(11) 0.47355(7) 0.57318(6) 0.0533(2) Uani 1 1 d . . . Ag2 Ag 0.44915(7) 0.11203(5) 0.43730(5) 0.02994(16) Uani 1 1 d . . . Ag3 Ag 0.66759(8) 0.69779(5) 0.77504(5) 0.03602(17) Uani 1 1 d . . . I1 I 0.33809(6) 0.62814(4) 0.73285(4) 0.03346(15) Uani 1 1 d . . . I2 I 0.73577(6) 0.00485(4) 0.48596(4) 0.02662(14) Uani 1 1 d . . . I3 I 0.87175(6) 0.70222(4) 0.97716(4) 0.03135(15) Uani 1 1 d . . . S1 S 0.2173(3) 0.40776(17) 0.38226(17) 0.0373(5) Uani 1 1 d . . . C1 C 0.1102(9) 0.5137(6) 0.3612(6) 0.0274(15) Uani 1 1 d . . . N1 N 0.0652(8) 0.5159(5) 0.2608(5) 0.0281(13) Uani 1 1 d D . . H1 H 0.109(10) 0.488(7) 0.208(5) 0.034 Uiso 1 1 d D . . C2 C -0.0617(10) 0.5705(7) 0.2098(7) 0.0339(17) Uani 1 1 d . . . H2A H -0.1702 0.5333 0.1966 0.041 Uiso 1 1 calc R . . H2B H -0.0534 0.5614 0.1371 0.041 Uiso 1 1 calc R . . C3 C -0.0578(10) 0.6906(7) 0.2739(7) 0.0338(17) Uani 1 1 d . . . H3A H 0.0533 0.7280 0.2935 0.041 Uiso 1 1 calc R . . H3B H -0.1371 0.7211 0.2263 0.041 Uiso 1 1 calc R . . C4 C -0.0999(11) 0.7123(7) 0.3780(7) 0.0364(18) Uani 1 1 d . . . H4A H -0.1992 0.6632 0.3609 0.044 Uiso 1 1 calc R . . H4B H -0.1258 0.7875 0.4051 0.044 Uiso 1 1 calc R . . C5 C 0.0392(11) 0.6963(7) 0.4678(7) 0.0349(18) Uani 1 1 d . . . H5A H 0.1396 0.7421 0.4804 0.042 Uiso 1 1 calc R . . H5B H 0.0116 0.7229 0.5367 0.042 Uiso 1 1 calc R . . N2 N 0.0779(8) 0.5850(5) 0.4470(5) 0.0295(14) Uani 1 1 d D . . H2 H 0.096(11) 0.556(6) 0.497(5) 0.035 Uiso 1 1 d D . . S2 S 0.5477(2) 0.30710(15) 0.57752(16) 0.0297(4) Uani 1 1 d . . . C6 C 0.5937(9) 0.3049(6) 0.7083(6) 0.0250(15) Uani 1 1 d . . . N3 N 0.5896(9) 0.3918(5) 0.7911(5) 0.0320(14) Uani 1 1 d D . . H3 H 0.548(11) 0.447(5) 0.776(7) 0.038 Uiso 1 1 d D . . C7 C 0.6629(12) 0.4095(7) 0.9073(7) 0.0385(19) Uani 1 1 d . . . H7A H 0.6723 0.4875 0.9518 0.046 Uiso 1 1 calc R . . H7B H 0.7754 0.3883 0.9202 0.046 Uiso 1 1 calc R . . C8 C 0.5655(14) 0.3468(7) 0.9453(8) 0.049(2) Uani 1 1 d . . . H8A H 0.4633 0.3795 0.9490 0.058 Uiso 1 1 calc R . . H8B H 0.6304 0.3524 1.0204 0.058 Uiso 1 1 calc R . . C9 C 0.5207(12) 0.2278(7) 0.8696(8) 0.044(2) Uani 1 1 d . . . H9A H 0.5069 0.1853 0.9130 0.053 Uiso 1 1 calc R . . H9B H 0.4136 0.2188 0.8118 0.053 Uiso 1 1 calc R . . C10 C 0.6471(11) 0.1823(6) 0.8149(7) 0.0384(19) Uani 1 1 d . . . H10A H 0.7583 0.2065 0.8706 0.046 Uiso 1 1 calc R . . H10B H 0.6289 0.1024 0.7871 0.046 Uiso 1 1 calc R . . N4 N 0.6405(9) 0.2157(5) 0.7231(5) 0.0342(15) Uani 1 1 d D . . H4 H 0.658(11) 0.169(6) 0.665(5) 0.041 Uiso 1 1 d D . . S3 S 0.3208(2) 0.11590(15) 0.24783(15) 0.0256(4) Uani 1 1 d . . . C11 C 0.1096(9) 0.0852(6) 0.2119(6) 0.0238(14) Uani 1 1 d . . . N5 N 0.0144(8) 0.0904(6) 0.1177(5) 0.0304(14) Uani 1 1 d D . . H5 H 0.072(9) 0.113(7) 0.085(7) 0.036 Uiso 1 1 d D . . C12 C -0.1489(10) 0.1294(8) 0.0999(8) 0.043(2) Uani 1 1 d . . . H12A H -0.1820 0.1393 0.0288 0.051 Uiso 1 1 calc R . . H12B H -0.1381 0.2012 0.1587 0.051 Uiso 1 1 calc R . . C13 C -0.2865(10) 0.0562(8) 0.0988(7) 0.042(2) Uani 1 1 d . . . H13A H -0.3920 0.0853 0.0778 0.050 Uiso 1 1 calc R . . H13B H -0.2956 -0.0167 0.0420 0.050 Uiso 1 1 calc R . . C14 C -0.2595(10) 0.0462(7) 0.2072(7) 0.0389(19) Uani 1 1 d . . . H14A H -0.3589 0.0056 0.2034 0.047 Uiso 1 1 calc R . . H14B H -0.2447 0.1194 0.2646 0.047 Uiso 1 1 calc R . . C15 C -0.1129(10) -0.0098(7) 0.2406(7) 0.0345(18) Uani 1 1 d . . . H15A H -0.1184 -0.0297 0.3022 0.041 Uiso 1 1 calc R . . H15B H -0.1181 -0.0774 0.1779 0.041 Uiso 1 1 calc R . . N6 N 0.0472(7) 0.0569(6) 0.2751(6) 0.0308(14) Uani 1 1 d D . . H6 H 0.113(9) 0.061(7) 0.340(3) 0.037 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0763(5) 0.0580(5) 0.0505(4) 0.0346(4) 0.0375(4) 0.0437(4) Ag2 0.0287(3) 0.0314(3) 0.0289(3) 0.0118(2) 0.0079(2) 0.0030(2) Ag3 0.0336(3) 0.0383(3) 0.0399(4) 0.0198(3) 0.0111(3) 0.0022(3) I1 0.0293(3) 0.0361(3) 0.0330(3) 0.0102(2) 0.0110(2) 0.0012(2) I2 0.0256(2) 0.0309(3) 0.0313(3) 0.0155(2) 0.0156(2) 0.00917(19) I3 0.0358(3) 0.0335(3) 0.0278(3) 0.0141(2) 0.0117(2) 0.0040(2) S1 0.0559(13) 0.0322(10) 0.0351(11) 0.0178(9) 0.0240(10) 0.0206(9) C1 0.027(4) 0.029(4) 0.027(4) 0.010(3) 0.011(3) 0.006(3) N1 0.033(3) 0.028(3) 0.028(3) 0.011(3) 0.015(3) 0.009(3) C2 0.035(4) 0.037(4) 0.035(4) 0.018(4) 0.012(3) 0.008(3) C3 0.032(4) 0.032(4) 0.049(5) 0.024(4) 0.019(4) 0.013(3) C4 0.038(4) 0.037(4) 0.040(5) 0.020(4) 0.016(4) 0.017(4) C5 0.042(5) 0.034(4) 0.034(4) 0.013(3) 0.018(4) 0.008(4) N2 0.040(4) 0.027(3) 0.030(3) 0.015(3) 0.019(3) 0.010(3) S2 0.0352(10) 0.0251(9) 0.0284(9) 0.0097(8) 0.0106(8) 0.0055(8) C6 0.022(3) 0.024(3) 0.027(4) 0.006(3) 0.009(3) 0.001(3) N3 0.046(4) 0.025(3) 0.030(3) 0.009(3) 0.020(3) 0.010(3) C7 0.052(5) 0.030(4) 0.030(4) 0.007(3) 0.014(4) 0.000(4) C8 0.074(7) 0.038(5) 0.038(5) 0.010(4) 0.030(5) 0.002(5) C9 0.053(6) 0.038(5) 0.048(5) 0.019(4) 0.021(4) -0.001(4) C10 0.051(5) 0.025(4) 0.035(4) 0.011(3) 0.008(4) 0.002(4) N4 0.045(4) 0.025(3) 0.025(3) 0.004(3) 0.008(3) 0.007(3) S3 0.0239(8) 0.0284(9) 0.0299(9) 0.0145(8) 0.0119(7) 0.0054(7) C11 0.027(4) 0.021(3) 0.021(3) 0.003(3) 0.011(3) 0.002(3) N5 0.024(3) 0.043(4) 0.027(3) 0.017(3) 0.008(3) 0.001(3) C12 0.024(4) 0.064(6) 0.047(5) 0.029(5) 0.011(4) 0.007(4) C13 0.021(4) 0.049(5) 0.044(5) 0.008(4) 0.006(3) -0.001(4) C14 0.025(4) 0.041(5) 0.047(5) 0.011(4) 0.015(4) -0.007(3) C15 0.032(4) 0.037(4) 0.038(4) 0.013(4) 0.018(4) -0.002(3) N6 0.018(3) 0.046(4) 0.035(4) 0.020(3) 0.012(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 Ag1 2.9800(15) 2_666 ? Ag1 I1 2.7194(9) . ? Ag1 S1 2.516(2) . ? Ag1 S2 2.477(2) . ? Ag2 I2 2.8761(8) . ? Ag2 I2 2.8796(7) 2_656 ? Ag2 S2 2.572(2) . ? Ag2 S3 2.5231(19) . ? Ag3 I1 2.7999(8) . ? Ag3 I3 2.7799(8) . ? Ag3 S1 2.605(2) 2_666 ? Ag3 S3 2.6230(19) 2_666 ? S1 C1 1.752(8) . ? C1 N1 1.329(10) . ? C1 N2 1.332(10) . ? N1 C2 1.455(10) . ? C2 C3 1.523(11) . ? C3 C4 1.513(11) . ? C4 C5 1.514(11) . ? C5 N2 1.469(10) . ? S2 C6 1.734(8) . ? C6 N3 1.313(10) . ? C6 N4 1.321(10) . ? N3 C7 1.458(11) . ? C7 C8 1.503(12) . ? C8 C9 1.524(13) . ? C9 C10 1.515(13) . ? C10 N4 1.470(11) . ? S3 C11 1.737(7) . ? C11 N5 1.332(10) . ? C11 N6 1.307(9) . ? N5 C12 1.480(10) . ? C12 C13 1.527(12) . ? C13 C14 1.494(13) . ? C14 C15 1.503(12) . ? C15 N6 1.486(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag1 Ag1 I1 122.40(4) 2_666 . ? Ag1 Ag1 S1 71.79(6) 2_666 . ? Ag1 Ag1 S2 100.14(6) 2_666 . ? I1 Ag1 S1 116.23(6) . . ? I1 Ag1 S2 129.04(5) . . ? S1 Ag1 S2 101.97(7) . . ? I2 Ag2 I2 93.69(2) . 2_656 ? I2 Ag2 S2 102.63(5) . . ? I2 Ag2 S2 110.60(5) 2_656 . ? I2 Ag2 S3 120.74(5) . . ? I2 Ag2 S3 118.60(5) 2_656 . ? S2 Ag2 S3 108.91(6) . . ? I1 Ag3 I3 112.54(3) . . ? I1 Ag3 S1 113.98(6) . 2_666 ? I1 Ag3 S3 107.80(5) . 2_666 ? I3 Ag3 S1 110.99(5) . 2_666 ? I3 Ag3 S3 113.91(5) . 2_666 ? S1 Ag3 S3 96.66(6) 2_666 2_666 ? Ag1 I1 Ag3 75.88(3) . . ? Ag2 I2 Ag2 86.31(2) . 2_656 ? Ag1 S1 Ag3 114.99(9) . 2_666 ? Ag1 S1 C1 110.0(3) . . ? Ag3 S1 C1 113.9(3) 2_666 . ? S1 C1 N1 117.7(5) . . ? S1 C1 N2 117.3(6) . . ? N1 C1 N2 125.0(7) . . ? C1 N1 C2 129.9(6) . . ? N1 C2 C3 116.6(7) . . ? C2 C3 C4 112.6(7) . . ? C3 C4 C5 112.3(7) . . ? C4 C5 N2 116.2(7) . . ? C1 N2 C5 130.3(6) . . ? Ag1 S2 Ag2 128.15(8) . . ? Ag1 S2 C6 109.6(3) . . ? Ag2 S2 C6 107.9(2) . . ? S2 C6 N3 120.2(6) . . ? S2 C6 N4 118.4(6) . . ? N3 C6 N4 121.3(7) . . ? C6 N3 C7 125.4(7) . . ? N3 C7 C8 113.1(8) . . ? C7 C8 C9 112.8(7) . . ? C8 C9 C10 113.8(8) . . ? C9 C10 N4 113.1(7) . . ? C6 N4 C10 129.1(7) . . ? Ag2 S3 Ag3 118.46(7) . 2_666 ? Ag2 S3 C11 107.0(2) . . ? Ag3 S3 C11 100.1(2) 2_666 . ? S3 C11 N5 117.8(5) . . ? S3 C11 N6 120.8(6) . . ? N5 C11 N6 121.4(7) . . ? C11 N5 C12 125.2(7) . . ? N5 C12 C13 115.7(8) . . ? C12 C13 C14 113.1(7) . . ? C13 C14 C15 113.4(7) . . ? C14 C15 N6 113.6(7) . . ? C11 N6 C15 126.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 I3 0.880(5) 2.94(5) 3.709(6) 148(7) 2_666 N2 H2 I1 0.880(5) 3.07(7) 3.718(7) 132(7) . N3 H3 I1 0.880(5) 3.14(2) 4.008(7) 168(8) . N4 H4 I2 0.880(5) 2.908(13) 3.784(7) 174(8) . N5 H5 I3 0.880(5) 2.97(6) 3.703(7) 141(7) 2_666 N6 H6 I2 0.880(5) 2.80(3) 3.632(7) 159(8) 2_656 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.704 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.184 #===END