# 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 _publ_contact_author_name 'G Bowmaker' _publ_contact_author_email GA.BOWMAKER@AUCKLAND.AC.NZ _publ_section_title ; 1:1 Complexes of silver(I) thiocyanate with (substituted) thiourea ligands ; loop_ _publ_author_name 'G Bowmaker' 'Chaveng Pakawatchai' 'Saowanit Saithong' 'Brian W Skelton' 'Allan H White' # Attachment 'agscnd.cif' data_agscnd _database_code_depnum_ccdc_archive 'CCDC 692482' _audit_creation_date 2008-06-20T09:57:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C12 H24 Ag2 N6 S4' _chemical_formula_moiety 'C10 H24 Ag N4 S2, C2 Ag N2 S2' _chemical_formula_weight 596.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 18.3911(7) _cell_length_b 18.3911(7) _cell_length_c 6.2785(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2123.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4478 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.23 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_correction_T_max 0.57 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_number 13056 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 2585 _reflns_number_gt 2170 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART_NT V5.6' _computing_cell_refinement 'Bruker SAINT-NT V5.6' _computing_data_reduction 'Bruker SAINT V 5.6, SADABs V 2.0' _computing_structure_solution 'SHELXTL(Sheldrick 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL(Sheldrick 2000)' _computing_publication_material 'XSHELL(Sheldrick 2000)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0390P)^2^+1.4864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2585 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.349 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.135 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 0.25 0.25 1.25 0.04873(14) Uani 1 4 d S . . Ag2 Ag 0.25 0.25 0.75 0.04924(14) Uani 1 4 d S . . Ag3 Ag 0.75 0.25 0.43619(7) 0.05879(13) Uani 1 2 d S . . S1 S 0.35425(4) 0.29126(4) 0.99279(12) 0.04033(17) Uani 1 1 d . . . N1 N 0.46446(14) 0.22211(15) 0.8042(4) 0.0503(6) Uani 1 1 d . . . H1 H 0.4942 0.1861 0.7977 0.06 Uiso 1 1 calc R . . N2 N 0.42088(13) 0.16918(13) 1.1058(4) 0.0450(6) Uani 1 1 d . . . H2 H 0.3887 0.1691 1.205 0.054 Uiso 1 1 calc R . . C1 C 0.41827(14) 0.22225(15) 0.9645(4) 0.0373(6) Uani 1 1 d . . . C11 C 0.47044(19) 0.2771(2) 0.6350(6) 0.0592(8) Uani 1 1 d . . . H11A H 0.4236 0.3003 0.6145 0.071 Uiso 1 1 calc R . . H11B H 0.4839 0.2536 0.5025 0.071 Uiso 1 1 calc R . . C12 C 0.5253(3) 0.3328(2) 0.6890(7) 0.0824(12) Uani 1 1 d . . . H12A H 0.5096 0.3595 0.8121 0.124 Uiso 1 1 calc R . . H12B H 0.531 0.3656 0.5711 0.124 Uiso 1 1 calc R . . H12C H 0.5709 0.3096 0.7188 0.124 Uiso 1 1 calc R . . C21 C 0.47438(18) 0.11053(18) 1.1062(6) 0.0565(8) Uani 1 1 d . . . H21A H 0.5229 0.1309 1.1167 0.068 Uiso 1 1 calc R . . H21B H 0.4712 0.0836 0.9737 0.068 Uiso 1 1 calc R . . C22 C 0.4611(2) 0.0604(2) 1.2897(6) 0.0694(11) Uani 1 1 d . . . H22A H 0.465 0.087 1.4208 0.104 Uiso 1 1 calc R . . H22B H 0.4965 0.022 1.288 0.104 Uiso 1 1 calc R . . H22C H 0.4132 0.0399 1.2782 0.104 Uiso 1 1 calc R . . S S 0.73884(4) 0.13633(4) 0.68593(14) 0.0503(2) Uani 1 1 d . . . C C 0.64831(18) 0.13281(16) 0.6873(5) 0.0487(7) Uani 1 1 d . . . N N 0.58635(17) 0.12957(17) 0.6894(6) 0.0671(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04819(18) 0.04819(18) 0.0498(3) 0 0 0 Ag2 0.05048(19) 0.05048(19) 0.0468(3) 0 0 0 Ag3 0.0579(2) 0.0673(3) 0.0512(2) 0 0 -0.00325(18) S1 0.0393(4) 0.0353(3) 0.0464(4) -0.0036(3) -0.0001(3) 0.0010(3) N1 0.0442(14) 0.0504(15) 0.0563(15) 0.0094(12) 0.0117(12) 0.0055(11) N2 0.0414(13) 0.0424(13) 0.0511(14) 0.0065(11) 0.0104(11) 0.0062(10) C1 0.0305(13) 0.0385(14) 0.0430(14) -0.0022(11) 0.0003(11) -0.0026(11) C11 0.0565(19) 0.069(2) 0.0522(19) 0.0098(17) 0.0078(16) 0.0033(17) C12 0.103(3) 0.072(3) 0.072(3) 0.014(2) 0.003(2) -0.021(2) C21 0.0517(18) 0.0483(17) 0.069(2) 0.0096(16) 0.0142(16) 0.0137(14) C22 0.078(3) 0.058(2) 0.073(2) 0.0179(19) 0.011(2) 0.0217(19) S 0.0483(4) 0.0461(4) 0.0566(5) -0.0030(4) 0.0035(3) 0.0062(3) C 0.058(2) 0.0381(15) 0.0498(17) -0.0024(13) 0.0119(15) 0.0021(13) N 0.0526(18) 0.0649(19) 0.084(2) -0.0075(17) 0.0194(16) -0.0018(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.6191(7) 2 ? Ag1 S1 2.6191(7) 8_658 ? Ag1 S1 2.6191(7) . ? Ag1 S1 2.6191(7) 7_568 ? Ag1 Ag2 3.1392(3) 1_556 ? Ag1 Ag2 3.1392(3) . ? Ag2 S1 2.5643(7) . ? Ag2 S1 2.5643(7) 7_567 ? Ag2 S1 2.5643(7) 8_657 ? Ag2 S1 2.5643(7) 2 ? Ag2 Ag1 3.1393(3) 1_554 ? Ag3 S 2.6212(9) 2_655 ? Ag3 S 2.6212(9) . ? Ag3 S 2.6232(9) 4_564 ? Ag3 S 2.6232(9) 3_644 ? Ag3 Ag3 3.1392(7) 3_645 ? Ag3 Ag3 3.1393(7) 3_644 ? S1 C1 1.740(3) . ? N1 C1 1.317(4) . ? N1 C11 1.471(4) . ? N1 H1 0.86 . ? N2 C1 1.320(4) . ? N2 C21 1.460(4) . ? N2 H2 0.86 . ? C11 C12 1.478(5) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C21 C22 1.496(5) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? S C 1.666(3) . ? S Ag3 2.6232(9) 3_645 ? C N 1.141(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 S1 Ag1 S1 112.344(17) 2 8_658 ? S1 Ag1 S1 103.87(3) 2 . ? S1 Ag1 S1 112.344(17) 8_658 . ? S1 Ag1 S1 112.344(17) 2 7_568 ? S1 Ag1 S1 103.87(3) 8_658 7_568 ? S1 Ag1 S1 112.344(17) . 7_568 ? S1 Ag1 Ag2 128.066(16) 2 1_556 ? S1 Ag1 Ag2 51.934(16) 8_658 1_556 ? S1 Ag1 Ag2 128.066(16) . 1_556 ? S1 Ag1 Ag2 51.934(16) 7_568 1_556 ? S1 Ag1 Ag2 51.934(16) 2 . ? S1 Ag1 Ag2 128.066(16) 8_658 . ? S1 Ag1 Ag2 51.934(16) . . ? S1 Ag1 Ag2 128.066(16) 7_568 . ? Ag2 Ag1 Ag2 180 1_556 . ? S1 Ag2 S1 110.695(17) . 7_567 ? S1 Ag2 S1 110.695(17) . 8_657 ? S1 Ag2 S1 107.05(3) 7_567 8_657 ? S1 Ag2 S1 107.05(3) . 2 ? S1 Ag2 S1 110.695(17) 7_567 2 ? S1 Ag2 S1 110.695(17) 8_657 2 ? S1 Ag2 Ag1 53.525(17) . . ? S1 Ag2 Ag1 126.475(17) 7_567 . ? S1 Ag2 Ag1 126.475(17) 8_657 . ? S1 Ag2 Ag1 53.526(17) 2 . ? S1 Ag2 Ag1 126.475(17) . 1_554 ? S1 Ag2 Ag1 53.525(17) 7_567 1_554 ? S1 Ag2 Ag1 53.525(17) 8_657 1_554 ? S1 Ag2 Ag1 126.474(17) 2 1_554 ? Ag1 Ag2 Ag1 180 . 1_554 ? S Ag3 S 106.52(4) 2_655 . ? S Ag3 S 110.996(11) 2_655 4_564 ? S Ag3 S 110.996(11) . 4_564 ? S Ag3 S 110.996(11) 2_655 3_644 ? S Ag3 S 110.996(11) . 3_644 ? S Ag3 S 106.40(4) 4_564 3_644 ? S Ag3 Ag3 53.26(2) 2_655 3_645 ? S Ag3 Ag3 53.26(2) . 3_645 ? S Ag3 Ag3 126.80(2) 4_564 3_645 ? S Ag3 Ag3 126.80(2) 3_644 3_645 ? S Ag3 Ag3 126.74(2) 2_655 3_644 ? S Ag3 Ag3 126.74(2) . 3_644 ? S Ag3 Ag3 53.20(2) 4_564 3_644 ? S Ag3 Ag3 53.20(2) 3_644 3_644 ? Ag3 Ag3 Ag3 180 3_645 3_644 ? C1 S1 Ag2 103.26(9) . . ? C1 S1 Ag1 110.29(9) . . ? Ag2 S1 Ag1 74.541(19) . . ? C1 N1 C11 126.8(3) . . ? C1 N1 H1 116.6 . . ? C11 N1 H1 116.6 . . ? C1 N2 C21 124.9(3) . . ? C1 N2 H2 117.5 . . ? C21 N2 H2 117.5 . . ? N1 C1 N2 119.3(3) . . ? N1 C1 S1 121.0(2) . . ? N2 C1 S1 119.7(2) . . ? N1 C11 C12 111.2(3) . . ? N1 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N1 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C21 C22 110.3(3) . . ? N2 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N2 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C S Ag3 96.45(11) . . ? C S Ag3 96.08(11) . 3_645 ? Ag3 S Ag3 73.54(2) . 3_645 ? N C S 179.2(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 S1 0.86 2.64 3.496(3) 170.7 7_568 N1 H1 N 0.86 2.1 2.905(4) 155.4 . #===END # Attachment 'gb0831.cif' data_gb0831 _database_code_depnum_ccdc_archive 'CCDC 693245' _audit_creation_date 2008-06-17T13:30:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C2 H4 Ag N3 S2' _chemical_formula_moiety 'C2 H4 Ag N3 S2' _chemical_formula_weight 242.07 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.39260(10) _cell_length_b 16.5167(4) _cell_length_c 8.60550(10) _cell_angle_alpha 90 _cell_angle_beta 96.802(2) _cell_angle_gamma 90 _cell_volume 619.95(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10595 _cell_measurement_theta_min 2.6756 _cell_measurement_theta_max 45.2195 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.76629 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_number 30449 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 45.4 _diffrn_reflns_theta_full 45.4 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 5206 _reflns_number_gt 3833 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5206 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.06 _refine_ls_goodness_of_fit_ref 0.93 _refine_ls_restrained_S_all 0.93 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.281 _refine_diff_density_min -1.356 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.82409(3) 0.423072(7) 0.525344(12) 0.01722(3) Uani 1 1 d . . . S1 S 0.37079(8) 0.34563(2) 0.58652(3) 0.01161(5) Uani 1 1 d . . . C1 C 0.4003(3) 0.33425(8) 0.78818(14) 0.01126(18) Uani 1 1 d . . . N11 N 0.2286(3) 0.27927(8) 0.84681(13) 0.01463(19) Uani 1 1 d . . . H11A H 0.2397 0.2727 0.9488 0.018 Uiso 1 1 calc R . . H11B H 0.1029 0.2491 0.7839 0.018 Uiso 1 1 calc R . . N12 N 0.5887(3) 0.37928(8) 0.88394(13) 0.0153(2) Uani 1 1 d . . . H12A H 0.5986 0.3724 0.9858 0.018 Uiso 1 1 calc R . . H12B H 0.704 0.4161 0.8457 0.018 Uiso 1 1 calc R . . S S 0.92448(8) 0.47168(2) 0.24909(4) 0.01266(5) Uani 1 1 d . . . C C 1.1458(3) 0.39387(8) 0.21228(14) 0.01235(19) Uani 1 1 d . . . N N 1.2952(3) 0.33942(8) 0.18196(14) 0.0166(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01718(5) 0.02226(5) 0.01281(4) 0.00108(3) 0.00431(3) -0.00448(4) S1 0.01171(12) 0.01520(13) 0.00808(10) 0.00028(9) 0.00187(9) 0.00001(10) C1 0.0117(5) 0.0128(5) 0.0094(4) 0.0003(3) 0.0019(3) 0.0015(4) N11 0.0179(5) 0.0160(5) 0.0104(4) 0.0007(3) 0.0035(3) -0.0035(4) N12 0.0166(5) 0.0194(5) 0.0099(4) -0.0003(3) 0.0014(3) -0.0042(4) S 0.01368(13) 0.01335(13) 0.01097(11) 0.00041(9) 0.00152(9) 0.00032(10) C 0.0147(5) 0.0135(5) 0.0089(4) -0.0002(4) 0.0013(4) -0.0019(4) N 0.0200(5) 0.0174(5) 0.0126(4) -0.0007(4) 0.0030(4) 0.0017(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.4751(4) . ? Ag1 S 2.5960(3) . ? Ag1 S1 2.7167(4) 1_655 ? Ag1 S 2.7389(4) 3_766 ? Ag1 Ag1 3.0325(2) 3_766 ? S1 C1 1.7351(12) . ? S1 Ag1 2.7167(4) 1_455 ? C1 N11 1.3183(18) . ? C1 N12 1.3250(18) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S C 1.6643(14) . ? S Ag1 2.7389(4) 3_766 ? C N 1.1612(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S 125.647(11) . . ? S1 Ag1 S1 115.494(13) . 1_655 ? S Ag1 S1 94.642(11) . 1_655 ? S1 Ag1 S 116.376(11) . 3_766 ? S Ag1 S 110.779(9) . 3_766 ? S1 Ag1 S 83.598(11) 1_655 3_766 ? S1 Ag1 Ag1 154.179(11) . 3_766 ? S Ag1 Ag1 57.613(8) . 3_766 ? S1 Ag1 Ag1 88.198(9) 1_655 3_766 ? S Ag1 Ag1 53.166(8) 3_766 3_766 ? C1 S1 Ag1 107.58(5) . . ? C1 S1 Ag1 101.79(4) . 1_455 ? Ag1 S1 Ag1 115.494(13) . 1_455 ? N11 C1 N12 119.48(11) . . ? N11 C1 S1 118.62(10) . . ? N12 C1 S1 121.89(10) . . ? C1 N11 H11A 120 . . ? C1 N11 H11B 120 . . ? H11A N11 H11B 120 . . ? C1 N12 H12A 120 . . ? C1 N12 H12B 120 . . ? H12A N12 H12B 120 . . ? C S Ag1 95.84(4) . . ? C S Ag1 115.43(5) . 3_766 ? Ag1 S Ag1 69.221(9) . 3_766 ? N C S 177.86(12) . . ? #===END # Attachment 'gab822.cif' data_gab822 _database_code_depnum_ccdc_archive 'CCDC 693246' _audit_creation_date 2008-05-23T10:48:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C7 H12 Ag N5 S3' _chemical_formula_moiety 'C7 H12 Ag N5 S3' _chemical_formula_weight 370.27 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7492(2) _cell_length_b 8.8638(3) _cell_length_c 11.7894(4) _cell_angle_alpha 91.307(3) _cell_angle_beta 97.162(3) _cell_angle_gamma 102.787(3) _cell_volume 580.52(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10208 _cell_measurement_theta_min 2.8464 _cell_measurement_theta_max 34.3672 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.83012 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.1115980494 _diffrn_orient_matrix_ub_12 0.0371707873 _diffrn_orient_matrix_ub_13 0.0320607308 _diffrn_orient_matrix_ub_21 0.0256321613 _diffrn_orient_matrix_ub_22 -0.0732500822 _diffrn_orient_matrix_ub_23 0.011281245 _diffrn_orient_matrix_ub_31 0.0565960594 _diffrn_orient_matrix_ub_32 0.002136948 _diffrn_orient_matrix_ub_33 -0.0502209554 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_number 21145 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 34.54 _diffrn_reflns_theta_full 33.3 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 4728 _reflns_number_gt 3729 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4728 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.299 _refine_diff_density_min -0.78 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.44618(3) 0.558320(18) 0.646041(13) 0.01751(5) Uani 1 1 d . . . S1 S 0.21505(8) 0.36937(6) 0.76684(4) 0.01327(9) Uani 1 1 d . . . C11 C 0.4170(3) 0.3322(2) 0.87568(15) 0.0109(3) Uani 1 1 d . . . N12 N 0.6444(3) 0.41042(19) 0.90273(13) 0.0143(3) Uani 1 1 d . . . H12 H 0.7091 0.4953 0.8704 0.017 Uiso 1 1 calc R . . C13 C 0.7735(3) 0.3373(2) 0.99305(16) 0.0159(4) Uani 1 1 d . . . H13A H 0.8633 0.4143 1.0541 0.019 Uiso 1 1 calc R . . H13B H 0.8866 0.283 0.9618 0.019 Uiso 1 1 calc R . . C14 C 0.5682(3) 0.2230(2) 1.03721(16) 0.0153(4) Uani 1 1 d . . . H14A H 0.6046 0.1193 1.0448 0.018 Uiso 1 1 calc R . . H14B H 0.5353 0.2604 1.112 0.018 Uiso 1 1 calc R . . N15 N 0.3658(3) 0.2196(2) 0.94752(13) 0.0146(3) Uani 1 1 d . . . H15 H 0.2274 0.1514 0.9419 0.017 Uiso 1 1 calc R . . S2 S 0.24414(8) 0.62828(6) 0.46177(4) 0.01339(9) Uani 1 1 d . . . C21 C 0.4306(3) 0.7862(2) 0.41667(15) 0.0119(3) Uani 1 1 d . . . N22 N 0.6501(3) 0.85536(19) 0.46872(13) 0.0131(3) Uani 1 1 d . . . H22 H 0.7135 0.8305 0.5356 0.016 Uiso 1 1 calc R . . C23 C 0.7719(3) 0.9777(2) 0.40075(16) 0.0134(3) Uani 1 1 d . . . H23A H 0.9062 0.9471 0.3681 0.016 Uiso 1 1 calc R . . H23B H 0.8346 1.076 0.4473 0.016 Uiso 1 1 calc R . . C24 C 0.5695(3) 0.9927(2) 0.30618(15) 0.0130(3) Uani 1 1 d . . . H24A H 0.5205 1.092 0.3157 0.016 Uiso 1 1 calc R . . H24B H 0.619 0.9846 0.2292 0.016 Uiso 1 1 calc R . . N25 N 0.3757(3) 0.86056(19) 0.32420(13) 0.0141(3) Uani 1 1 d . . . H25 H 0.2382 0.8336 0.2787 0.017 Uiso 1 1 calc R . . S S 0.88528(9) 0.70570(6) 0.72642(4) 0.01488(9) Uani 1 1 d . . . C C 0.8950(3) 0.8650(2) 0.80627(15) 0.0136(3) Uani 1 1 d . . . N N 0.9090(3) 0.9781(2) 0.86106(14) 0.0177(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02113(8) 0.01622(8) 0.01331(7) 0.00511(5) 0.00057(5) 0.00076(5) S1 0.0120(2) 0.0160(2) 0.01123(19) 0.00382(17) 0.00025(15) 0.00219(17) C11 0.0127(8) 0.0103(8) 0.0092(7) -0.0010(6) 0.0013(6) 0.0021(6) N12 0.0117(7) 0.0158(8) 0.0127(7) 0.0068(6) -0.0017(6) -0.0016(6) C13 0.0111(8) 0.0216(10) 0.0139(8) 0.0056(7) 0.0001(6) 0.0014(7) C14 0.0139(8) 0.0178(9) 0.0126(8) 0.0044(7) -0.0009(7) 0.0013(7) N15 0.0121(7) 0.0168(8) 0.0131(7) 0.0045(6) 0.0003(6) -0.0002(6) S2 0.0124(2) 0.0141(2) 0.01247(19) 0.00330(17) 0.00120(16) 0.00028(16) C21 0.0130(8) 0.0140(9) 0.0094(7) 0.0006(6) 0.0023(6) 0.0038(7) N22 0.0127(7) 0.0160(8) 0.0086(6) 0.0042(6) -0.0004(5) -0.0005(6) C23 0.0130(8) 0.0143(9) 0.0123(8) 0.0035(7) 0.0029(6) 0.0011(7) C24 0.0137(8) 0.0135(9) 0.0110(8) 0.0038(7) 0.0011(6) 0.0015(7) N25 0.0123(7) 0.0166(8) 0.0115(7) 0.0043(6) 0.0003(6) -0.0002(6) S 0.0150(2) 0.0148(2) 0.0145(2) 0.00206(17) 0.00195(16) 0.00251(17) C 0.0104(8) 0.0177(9) 0.0116(8) 0.0058(7) 0.0008(6) 0.0008(7) N 0.0159(8) 0.0192(9) 0.0152(8) 0.0019(7) -0.0001(6) -0.0007(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.4889(5) . ? Ag1 S2 2.4908(5) . ? Ag1 S 2.6201(5) . ? S1 C11 1.7086(19) . ? C11 N15 1.331(2) . ? C11 N12 1.333(2) . ? N12 C13 1.467(2) . ? N12 H12 0.88 . ? C13 C14 1.529(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 N15 1.466(2) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? N15 H15 0.88 . ? S2 C21 1.704(2) . ? C21 N25 1.327(2) . ? C21 N22 1.339(2) . ? N22 C23 1.467(2) . ? N22 H22 0.88 . ? C23 C24 1.538(3) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 N25 1.467(2) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? N25 H25 0.88 . ? S C 1.666(2) . ? C N 1.162(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 S1 Ag1 S2 119.938(16) . . ? S1 Ag1 S 119.090(16) . . ? S2 Ag1 S 120.571(16) . . ? C11 S1 Ag1 106.89(7) . . ? N15 C11 N12 109.94(16) . . ? N15 C11 S1 123.91(14) . . ? N12 C11 S1 126.14(14) . . ? C11 N12 C13 111.58(16) . . ? C11 N12 H12 124.2 . . ? C13 N12 H12 124.2 . . ? N12 C13 C14 102.18(15) . . ? N12 C13 H13A 111.3 . . ? C14 C13 H13A 111.3 . . ? N12 C13 H13B 111.3 . . ? C14 C13 H13B 111.3 . . ? H13A C13 H13B 109.2 . . ? N15 C14 C13 102.39(15) . . ? N15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? N15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C11 N15 C14 111.69(16) . . ? C11 N15 H15 124.2 . . ? C14 N15 H15 124.2 . . ? C21 S2 Ag1 107.57(7) . . ? N25 C21 N22 109.85(17) . . ? N25 C21 S2 124.25(15) . . ? N22 C21 S2 125.90(14) . . ? C21 N22 C23 111.73(15) . . ? C21 N22 H22 124.1 . . ? C23 N22 H22 124.1 . . ? N22 C23 C24 102.59(14) . . ? N22 C23 H23A 111.2 . . ? C24 C23 H23A 111.2 . . ? N22 C23 H23B 111.2 . . ? C24 C23 H23B 111.2 . . ? H23A C23 H23B 109.2 . . ? N25 C24 C23 102.32(14) . . ? N25 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? N25 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C21 N25 C24 112.54(16) . . ? C21 N25 H25 123.7 . . ? C24 N25 H25 123.7 . . ? C S Ag1 113.08(7) . . ? N C S 177.81(18) . . ? #===END # Attachment 'gb0833.cif' data_gb0833 _database_code_depnum_ccdc_archive 'CCDC 693247' _audit_creation_date 2008-06-08T21:08:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C6 H16 Ag2 N10 S6' _chemical_formula_moiety 'C6 H16 Ag2 N10 S6' _chemical_formula_weight 636.45 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 11.0271(4) _cell_length_b 13.7937(6) _cell_length_c 13.6913(8) _cell_angle_alpha 90 _cell_angle_beta 111.889(5) _cell_angle_gamma 90 _cell_volume 1932.38(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12007 _cell_measurement_theta_min 2.9383 _cell_measurement_theta_max 40.6635 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.89415 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0548109173 _diffrn_orient_matrix_ub_12 0.0185142725 _diffrn_orient_matrix_ub_13 0.0419640586 _diffrn_orient_matrix_ub_21 -0.0334728037 _diffrn_orient_matrix_ub_22 0.0443272275 _diffrn_orient_matrix_ub_23 -0.0025443199 _diffrn_orient_matrix_ub_31 -0.0258476205 _diffrn_orient_matrix_ub_32 -0.0181277243 _diffrn_orient_matrix_ub_33 0.0365920917 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_number 26113 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 40.89 _diffrn_reflns_theta_full 40 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 6232 _reflns_number_gt 4889 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6232 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.056 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.354 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.174 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.013343(9) 0.543590(7) 0.104922(8) 0.01525(3) Uani 1 1 d . . . S1 S 0.11285(3) 0.38058(2) 0.11840(2) 0.01127(5) Uani 1 1 d . . . C1 C 0.00348(11) 0.29244(9) 0.12244(9) 0.01085(18) Uani 1 1 d . . . N11 N 0.03901(11) 0.20038(8) 0.12951(10) 0.0165(2) Uani 1 1 d . . . H11A H -0.0158 0.1548 0.1317 0.02 Uiso 1 1 calc R . . H11B H 0.1175 0.1847 0.132 0.02 Uiso 1 1 calc R . . N12 N -0.11451(10) 0.31449(8) 0.11876(9) 0.01475(19) Uani 1 1 d . . . H12A H -0.1683 0.2682 0.121 0.018 Uiso 1 1 calc R . . H12B H -0.1394 0.3755 0.1141 0.018 Uiso 1 1 calc R . . S2 S 0.14552(3) 0.69170(2) 0.16403(2) 0.01245(5) Uani 1 1 d . . . C2 C 0.04062(12) 0.78765(9) 0.14612(9) 0.01112(18) Uani 1 1 d . . . N21 N 0.08908(11) 0.87608(8) 0.17347(9) 0.01528(19) Uani 1 1 d . . . H21A H 0.036 0.9259 0.1641 0.018 Uiso 1 1 calc R . . H21B H 0.1742 0.8849 0.2009 0.018 Uiso 1 1 calc R . . N22 N -0.08818(10) 0.77673(8) 0.10493(8) 0.01390(18) Uani 1 1 d . . . H22A H -0.1395 0.8275 0.0963 0.017 Uiso 1 1 calc R . . H22B H -0.1223 0.7188 0.0863 0.017 Uiso 1 1 calc R . . S3 S -0.22173(3) 0.54718(2) 0.10776(3) 0.01301(5) Uani 1 1 d . . . C3 C -0.30606(12) 0.50422(9) -0.01168(11) 0.0142(2) Uani 1 1 d . . . N3 N -0.36752(12) 0.47532(9) -0.09544(10) 0.0202(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01235(4) 0.01017(4) 0.02246(5) -0.00192(3) 0.00562(3) -0.00115(3) S1 0.00956(11) 0.00978(11) 0.01462(13) 0.00092(9) 0.00470(10) -0.00030(9) C1 0.0108(5) 0.0105(4) 0.0110(5) 0.0002(3) 0.0038(4) -0.0002(3) N11 0.0142(5) 0.0093(4) 0.0280(6) -0.0003(4) 0.0101(4) -0.0003(3) N12 0.0120(4) 0.0111(4) 0.0227(5) 0.0027(4) 0.0083(4) 0.0002(3) S2 0.00951(12) 0.01032(11) 0.01699(13) -0.00103(9) 0.00432(10) -0.00063(9) C2 0.0125(5) 0.0106(4) 0.0112(5) 0.0008(4) 0.0054(4) -0.0006(4) N21 0.0143(5) 0.0102(4) 0.0203(5) -0.0009(4) 0.0052(4) -0.0014(3) N22 0.0110(4) 0.0109(4) 0.0183(5) -0.0007(3) 0.0036(4) 0.0008(3) S3 0.01100(12) 0.01209(12) 0.01660(13) -0.00008(10) 0.00591(10) 0.00010(9) C3 0.0112(5) 0.0110(5) 0.0202(6) 0.0018(4) 0.0056(4) -0.0001(4) N3 0.0163(5) 0.0164(5) 0.0243(6) -0.0005(4) 0.0033(4) -0.0017(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S2 2.4646(3) . ? Ag1 S1 2.4785(3) . ? Ag1 S3 2.6074(3) . ? Ag1 S1 3.0343(3) 5_565 ? Ag1 Ag1 3.0260(2) 5_565 ? S1 C1 1.7278(12) . ? C1 N12 1.3188(16) . ? C1 N11 1.3218(16) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.7141(12) . ? C2 N22 1.3269(16) . ? C2 N21 1.3283(16) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.6602(14) . ? C3 N3 1.1636(18) . ? 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 S2 Ag1 S1 122.439(11) . . ? S2 Ag1 S3 116.674(10) . . ? S1 Ag1 S3 115.538(10) . . ? S2 Ag1 Ag1 118.521(9) . 5_565 ? S1 Ag1 Ag1 66.034(8) . 5_565 ? S3 Ag1 Ag1 106.045(10) . 5_565 ? C1 S1 Ag1 110.23(4) . . ? N12 C1 N11 119.06(11) . . ? N12 C1 S1 121.80(9) . . ? N11 C1 S1 119.14(9) . . ? C1 N11 H11A 120 . . ? C1 N11 H11B 120 . . ? H11A N11 H11B 120 . . ? C1 N12 H12A 120 . . ? C1 N12 H12B 120 . . ? H12A N12 H12B 120 . . ? C2 S2 Ag1 107.94(4) . . ? N22 C2 N21 118.58(11) . . ? N22 C2 S2 122.11(9) . . ? N21 C2 S2 119.31(9) . . ? C2 N21 H21A 120 . . ? C2 N21 H21B 120 . . ? H21A N21 H21B 120 . . ? C2 N22 H22A 120 . . ? C2 N22 H22B 120 . . ? H22A N22 H22B 120 . . ? C3 S3 Ag1 99.99(4) . . ? N3 C3 S3 178.49(13) . . ? #===END