# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bowmaker, G.' _publ_contact_author_email g.bowmaker@auckland.ac.nz _publ_section_title ; Novel complexes of silver(I) sulfate with 1-methylimidazole-2-thione: structures and vibrational spectroscopy ; loop_ _publ_author_name G.Bowmaker C.Pakawatchai B.Skelton A.H.White # Attachment '- agdesm.cif' data_agdesm _database_code_depnum_ccdc_archive 'CCDC 758121' #TrackingRef '- agdesm.cif' _audit_creation_date 2009-11-16T13:12:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C15 H36 Ag N6 S3), O4 S' _chemical_formula_sum 'C30 H72 Ag2 N12 O4 S7' _chemical_formula_weight 1105.16 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.4273(4) _cell_length_b 12.4273(4) _cell_length_c 28.2459(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3777.8(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4730 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.18 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.266 _exptl_crystal_size_mid 0.135 _exptl_crystal_size_min 0.107 _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1722 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # 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 'Bruker SMART CCD area-detector' _diffrn_measurement_method 'Frames each covering 0.3 \% in \w' _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_unetI/netI 0.0122 _diffrn_reflns_number 16824 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 1943 _reflns_number_gt 1597 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEPII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The sulphate anion has been modelled as being disordered about the crystallographic 3-bar axis with oxygen atom site occupancies at 1/6. Although the structure contains voids of 34 cubic Angstroms, the use of the program Squeeze did not improve the model. ; _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^)+(0.0903P)^2^+9.2227P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1943 _refine_ls_number_parameters 116 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.165 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.154 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.3333 0.6667 0.10684(2) 0.0812(3) Uani 1 3 d S . . S1 S 0.48552(11) 0.59549(10) 0.09776(5) 0.0845(4) Uani 1 1 d . . . N1 N 0.6993(4) 0.7293(5) 0.05532(17) 0.1005(13) Uani 1 1 d . . . H1 H 0.7716 0.7949 0.0539 0.121 Uiso 1 1 calc R . . N2 N 0.6582(4) 0.8241(4) 0.1163(2) 0.1048(15) Uani 1 1 d . . . H2 H 0.6062 0.8177 0.1377 0.126 Uiso 1 1 calc R . . C1 C 0.6254(4) 0.7250(4) 0.08799(17) 0.0737(10) Uani 1 1 d . . . C2 C 0.6709(7) 0.6325(9) 0.0205(2) 0.130(3) Uani 1 1 d . . . H2A H 0.7124 0.6711 -0.0089 0.155 Uiso 1 1 calc R . . H2B H 0.5822 0.5885 0.0145 0.155 Uiso 1 1 calc R . . C3 C 0.7085(9) 0.5415(10) 0.0349(4) 0.159(3) Uani 1 1 d . . . H3A H 0.7975 0.5819 0.0362 0.238 Uiso 1 1 calc R . . H3B H 0.6778 0.475 0.0123 0.238 Uiso 1 1 calc R . . H3C H 0.6746 0.5087 0.0655 0.238 Uiso 1 1 calc R . . C4 C 0.7729(8) 0.9389(7) 0.1133(4) 0.154(3) Uani 1 1 d D . . H4A H 0.8377 0.9277 0.1275 0.185 Uiso 1 1 calc R . . H4B H 0.7938 0.9589 0.0802 0.185 Uiso 1 1 calc R . . C5 C 0.7729(11) 1.0370(9) 0.1346(5) 0.237(8) Uani 1 1 d D . . H5A H 0.6934 1.0309 0.1303 0.355 Uiso 1 1 calc R . . H5B H 0.8364 1.1129 0.1208 0.355 Uiso 1 1 calc R . . H5C H 0.7889 1.0364 0.1678 0.355 Uiso 1 1 calc R . . S2 S 1 1 0 0.0547(5) Uani 1 6 d SD . . O21 O 0.935(3) 0.982(4) 0.0452(8) 0.107(16) Uani 0.167 1 d PD . . O22 O 1.0714(16) 1.1306(14) -0.0125(9) 0.053(5) Uani 0.167 1 d PD . . O23 O 0.9029(19) 0.932(2) -0.0379(10) 0.073(7) Uani 0.167 1 d PD . . O24 O 1.080(3) 0.944(3) 0.0018(12) 0.111(19) Uani 0.167 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0756(3) 0.0756(3) 0.0923(5) 0 0 0.03780(16) S1 0.0717(7) 0.0628(6) 0.1166(10) 0.0080(6) 0.0143(6) 0.0318(5) N1 0.076(2) 0.094(3) 0.106(3) 0.010(2) 0.010(2) 0.024(2) N2 0.079(3) 0.088(3) 0.134(4) -0.012(3) 0.002(3) 0.033(2) C1 0.063(2) 0.062(2) 0.087(3) 0.0061(19) -0.004(2) 0.0240(18) C2 0.113(5) 0.158(7) 0.105(4) -0.009(4) 0.025(4) 0.058(5) C3 0.140(7) 0.154(8) 0.185(9) -0.043(7) 0.007(6) 0.076(6) C4 0.103(5) 0.094(5) 0.221(10) -0.036(5) -0.009(5) 0.016(4) C5 0.198(11) 0.119(7) 0.281(15) -0.062(9) 0.112(11) -0.006(7) S2 0.0480(6) 0.0480(6) 0.0681(12) 0 0 0.0240(3) O21 0.064(12) 0.17(4) 0.072(13) 0.04(2) 0.026(9) 0.05(2) O22 0.048(10) 0.036(9) 0.059(16) -0.009(7) -0.005(8) 0.009(7) O23 0.064(17) 0.050(11) 0.076(17) -0.011(11) -0.001(13) 0.008(9) O24 0.13(3) 0.17(4) 0.073(18) 0.002(17) -0.015(16) 0.11(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.4694(12) 2_665 ? Ag1 S1 2.4694(12) 3_565 ? Ag1 S1 2.4694(12) . ? Ag1 Ag1 3.3798(13) 13_565 ? S1 C1 1.700(4) . ? N1 C1 1.284(6) . ? N1 C2 1.455(9) . ? N1 H1 0.86 . ? N2 C1 1.348(7) . ? N2 C4 1.428(9) . ? N2 H2 0.86 . ? C2 C3 1.479(13) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 C5 1.359(11) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? S2 O21 1.467(25) . ? S2 O22 1.451(16) . ? S2 O23 1.515(25) . ? S2 O24 1.472(32) . ? 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 118.935(13) 2_665 3_565 ? S1 Ag1 S1 118.935(14) 2_665 . ? S1 Ag1 S1 118.935(13) 3_565 . ? S1 Ag1 Ag1 95.96(4) 2_665 13_565 ? S1 Ag1 Ag1 95.96(4) 3_565 13_565 ? S1 Ag1 Ag1 95.96(4) . 13_565 ? C1 S1 Ag1 106.32(16) . . ? C1 N1 C2 125.4(5) . . ? C1 N1 H1 117.3 . . ? C2 N1 H1 117.3 . . ? C1 N2 C4 125.0(6) . . ? C1 N2 H2 117.5 . . ? C4 N2 H2 117.5 . . ? N1 C1 N2 120.3(4) . . ? N1 C1 S1 121.8(4) . . ? N2 C1 S1 117.9(4) . . ? N1 C2 C3 114.1(7) . . ? N1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 N2 115.0(8) . . ? C5 C4 H4A 108.5 . . ? N2 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? N2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O21 S2 O22 111(2) . . ? O21 S2 O23 107.8(15) . . ? O21 S2 O24 110(2) . . ? O22 S2 O23 108.8(13) . . ? O22 S2 O24 110.9(14) . . ? O23 S2 O24 107.416) . . ? 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 O24 0.86 2.03 2.69(3) 133 3_675 N1 H1 O22 0.86 2.06 2.77(2) 139.4 10_775 N1 H1 O23 0.86 2.19 3.00(3) 156 12_655 N1 H1 O21 0.86 2.21 3.05(3) 168 . N1 H1 O24 0.86 2.44 3.09(4) 132.7 11_565 N1 H1 O22 0.86 2.47 3.08(3) 129 2_765 #===END # Attachment '- agsoim.cif' #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_agsoim _database_code_depnum_ccdc_archive 'CCDC 758122' #TrackingRef '- agsoim.cif' _audit_creation_date 2009-12-14T21:57:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C32 H67 Ag6 N16 O21.50 S11' _chemical_formula_moiety 'C32 H48 Ag6 N16 O12 S11, 9.5(H2 O)' _chemical_formula_weight 2019.9 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -P_2yn 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 18.5850(10) _cell_length_b 18.3390(10) _cell_length_c 22.201(2) _cell_angle_alpha 90 _cell_angle_beta 113.3180(10) _cell_angle_gamma 90 _cell_volume 6948.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 29.1 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4004 _exptl_special_details ; ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .574 _exptl_absorpt_correction_T_max .914 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_number 74064 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 29.14 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.935 _reflns_number_total 17500 _reflns_number_gt 12697 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEPII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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. One sulphate anion modelled as being disordered over two sites with refined occupancy factors of 0.739(11) and its complement. Solvent water molecules oxygen atoms refined with occupancy factors set at 0.5 or 1.0 after trial refinement. Water molecule hydrogen atoms not located. Although structure contains voids of 38 Angstroms**3, the use of Squeeze did not improve the model. ; _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^)+(0.1406P)^2^+22.7863P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17500 _refine_ls_number_parameters 845 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.2388 _refine_ls_wR_factor_gt 0.221 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 3.696 _refine_diff_density_min -2.674 _refine_diff_density_rms 0.291 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.60452(3) 0.91575(3) 0.13124(3) 0.05034(16) Uani 1 1 d . A . Ag2 Ag 0.61161(5) 0.81051(4) 0.27062(4) 0.0665(2) Uani 1 1 d . A . Ag3 Ag 0.46962(4) 0.80277(3) 0.11569(3) 0.05435(17) Uani 1 1 d . . . Ag4 Ag 0.36418(4) 0.94322(3) 0.04209(3) 0.05269(17) Uani 1 1 d . . . Ag5 Ag 0.26562(4) 0.75916(4) -0.09020(4) 0.05881(18) Uani 1 1 d . . . Ag6 Ag 0.41150(4) 0.88103(3) -0.07858(3) 0.0611(2) Uani 1 1 d . . . S1 S 0.67473(10) 1.00985(9) 0.07671(9) 0.0411(4) Uani 1 1 d . . . C11 C 0.7747(4) 1.0172(3) 0.1146(4) 0.0425(15) Uani 1 1 d . A . N12 N 0.8201(3) 1.0331(3) 0.1781(3) 0.0455(13) Uani 1 1 d . . . C121 C 0.7893(5) 1.0529(5) 0.2274(4) 0.0553(19) Uani 1 1 d . A . H12A H 0.7533 1.0942 0.2115 0.083 Uiso 1 1 calc R . . H12B H 0.8328 1.0665 0.2684 0.083 Uiso 1 1 calc R . . H12C H 0.7614 1.0111 0.2354 0.083 Uiso 1 1 calc R . . C13 C 0.8972(4) 1.0268(4) 0.1896(5) 0.055(2) Uani 1 1 d . A . H13 H 0.94 1.0357 0.2301 0.066 Uiso 1 1 calc R . . C14 C 0.9022(5) 1.0058(5) 0.1343(6) 0.066(3) Uani 1 1 d . . . H14 H 0.949 0.9969 0.1279 0.079 Uiso 1 1 calc R A . N15 N 0.8268(4) 0.9995(4) 0.0878(4) 0.0526(15) Uani 1 1 d . A . H15 H 0.8142 0.986 0.0469 0.063 Uiso 1 1 calc R . . S2 S 0.70580(9) 0.85198(9) 0.22414(8) 0.0369(3) Uani 1 1 d . . . C21 C 0.7249(3) 0.7790(3) 0.1834(3) 0.0330(12) Uani 1 1 d . A . N22 N 0.7846(3) 0.7762(3) 0.1637(3) 0.0394(12) Uani 1 1 d . . . C221 C 0.8375(5) 0.8364(4) 0.1668(4) 0.0517(18) Uani 1 1 d . A . H22A H 0.8203 0.8599 0.1237 0.077 Uiso 1 1 calc R . . H22B H 0.8908 0.8175 0.1791 0.077 Uiso 1 1 calc R . . H22C H 0.837 0.872 0.1995 0.077 Uiso 1 1 calc R . . C23 C 0.7856(5) 0.7076(4) 0.1362(4) 0.0474(16) Uani 1 1 d . A . H23 H 0.8212 0.6912 0.118 0.057 Uiso 1 1 calc R . . C24 C 0.7254(5) 0.6692(4) 0.1407(4) 0.0465(16) Uani 1 1 d . . . H24 H 0.7109 0.6206 0.1263 0.056 Uiso 1 1 calc R A . N25 N 0.6892(3) 0.7139(3) 0.1701(3) 0.0392(12) Uani 1 1 d . A . H25 H 0.6485 0.7016 0.1788 0.047 Uiso 1 1 calc R . . S3 S 0.62109(12) 0.71506(10) 0.35598(10) 0.0480(4) Uani 1 1 d . . . C31 C 0.5850(5) 0.7618(4) 0.4053(4) 0.0483(16) Uani 1 1 d . A . N32 N 0.5553(5) 0.7297(5) 0.4451(5) 0.070(2) Uani 1 1 d . . . C321 C 0.5438(11) 0.6530(7) 0.4502(9) 0.113(5) Uani 1 1 d . A . H32A H 0.4876 0.6426 0.4339 0.17 Uiso 1 1 calc R . . H32B H 0.5693 0.638 0.4962 0.17 Uiso 1 1 calc R . . H32C H 0.5668 0.6261 0.424 0.17 Uiso 1 1 calc R . . C33 C 0.5334(7) 0.7839(7) 0.4779(7) 0.086(3) Uani 1 1 d . A . H33 H 0.51 0.7773 0.5086 0.103 Uiso 1 1 calc R . . C34 C 0.5523(7) 0.8498(6) 0.4570(6) 0.074(3) Uani 1 1 d . . . H34 H 0.5443 0.8971 0.4705 0.089 Uiso 1 1 calc R A . N35 N 0.5836(4) 0.8335(4) 0.4143(4) 0.0525(15) Uani 1 1 d . A . H35 H 0.6013 0.866 0.3944 0.063 Uiso 1 1 calc R . . S4 S 0.49204(9) 1.00953(8) 0.11042(8) 0.0347(3) Uani 1 1 d . . . C41 C 0.4807(4) 1.0284(4) 0.1820(3) 0.0427(14) Uani 1 1 d . A . N42 N 0.5401(4) 1.0412(3) 0.2409(3) 0.0521(15) Uani 1 1 d . . . C421 C 0.6219(5) 1.0442(5) 0.2539(4) 0.057(2) Uani 1 1 d . A . H42A H 0.6377 0.9988 0.2394 0.086 Uiso 1 1 calc R . . H42B H 0.6521 1.0506 0.3011 0.086 Uiso 1 1 calc R . . H42C H 0.6319 1.0854 0.2302 0.086 Uiso 1 1 calc R . . C43 C 0.5083(8) 1.0528(7) 0.2869(6) 0.082(3) Uani 1 1 d . A . H43 H 0.5363 1.0609 0.3326 0.099 Uiso 1 1 calc R . . C44 C 0.4290(9) 1.0505(9) 0.2537(7) 0.101(5) Uani 1 1 d . . . H44 H 0.3909 1.0587 0.2715 0.121 Uiso 1 1 calc R A . N45 N 0.4144(5) 1.0337(5) 0.1888(4) 0.072(2) Uani 1 1 d . A . H45 H 0.3678 1.0277 0.1572 0.087 Uiso 1 1 calc R . . S5 S 0.46727(12) 0.85279(11) 0.22088(10) 0.0503(4) Uani 1 1 d . A . C51 C 0.4265(6) 0.7832(7) 0.2491(5) 0.072(3) Uani 1 1 d . . . N52 N 0.3871(7) 0.7863(8) 0.2854(7) 0.107(4) Uani 1 1 d . A . C521 C 0.3693(11) 0.8524(12) 0.3072(9) 0.134(7) Uani 1 1 d . . . H52A H 0.4164 0.883 0.3242 0.201 Uiso 1 1 calc R A . H52B H 0.3507 0.8434 0.3421 0.201 Uiso 1 1 calc R . . H52C H 0.3284 0.8775 0.2706 0.201 Uiso 1 1 calc R . . C53 C 0.3698(8) 0.7171(9) 0.2999(8) 0.101(4) Uani 1 1 d . . . H53 H 0.3418 0.7059 0.3265 0.122 Uiso 1 1 calc R A . C54 C 0.3970(8) 0.6708(9) 0.2721(8) 0.107(5) Uani 1 1 d . A . H54 H 0.3934 0.6192 0.2731 0.129 Uiso 1 1 calc R . . N55 N 0.4321(6) 0.7104(6) 0.2411(5) 0.096(4) Uani 1 1 d . A . H55 H 0.4563 0.6913 0.2179 0.115 Uiso 1 1 calc R . . S6 S 0.32181(13) 0.80979(11) 0.02908(10) 0.0511(4) Uani 1 1 d . A . C61 C 0.2669(5) 0.7947(5) 0.0747(5) 0.0561(19) Uani 1 1 d . . . N62 N 0.2476(5) 0.7285(5) 0.0913(5) 0.066(2) Uani 1 1 d . A . C621 C 0.2704(7) 0.6591(5) 0.0723(6) 0.070(2) Uani 1 1 d . . . H62A H 0.2464 0.6543 0.0244 0.104 Uiso 1 1 calc R A . H62B H 0.2526 0.6191 0.0923 0.104 Uiso 1 1 calc R . . H62C H 0.3275 0.6572 0.0873 0.104 Uiso 1 1 calc R . . C63 C 0.2069(7) 0.7381(8) 0.1315(7) 0.089(4) Uani 1 1 d . . . H63 H 0.188 0.701 0.1513 0.107 Uiso 1 1 calc R A . C64 C 0.1995(8) 0.8108(8) 0.1365(9) 0.102(5) Uani 1 1 d . A . H64 H 0.1732 0.8348 0.1599 0.123 Uiso 1 1 calc R . . N65 N 0.2372(5) 0.8438(5) 0.1016(5) 0.071(2) Uani 1 1 d . A . H65 H 0.2409 0.8913 0.0977 0.085 Uiso 1 1 calc R . . S7 S 0.34190(9) 0.78630(8) -0.16043(8) 0.0367(3) Uani 1 1 d . A . C71 C 0.4002(4) 0.7114(3) -0.1557(3) 0.0359(13) Uani 1 1 d . . . N72 N 0.4608(4) 0.7096(3) -0.1745(3) 0.0483(14) Uani 1 1 d . A . C721 C 0.4940(6) 0.7724(5) -0.1945(6) 0.068(3) Uani 1 1 d . . . H72A H 0.4589 0.7874 -0.2388 0.101 Uiso 1 1 calc R A . H72B H 0.5452 0.7593 -0.1943 0.101 Uiso 1 1 calc R . . H72C H 0.5003 0.8127 -0.1639 0.101 Uiso 1 1 calc R . . C73 C 0.4859(6) 0.6379(5) -0.1709(4) 0.061(2) Uani 1 1 d . . . H73 H 0.5282 0.6207 -0.1808 0.074 Uiso 1 1 calc R A . C74 C 0.4396(5) 0.5976(4) -0.1508(4) 0.060(2) Uani 1 1 d . A . H74 H 0.4422 0.5462 -0.1449 0.072 Uiso 1 1 calc R . . N75 N 0.3886(4) 0.6431(3) -0.1405(3) 0.0458(14) Uani 1 1 d . A . H75 H 0.3528 0.6298 -0.126 0.055 Uiso 1 1 calc R . . S8 S 0.51976(9) 0.84136(8) 0.02786(7) 0.0351(3) Uani 1 1 d . A . C81 C 0.5633(4) 0.7675(3) 0.0073(3) 0.0375(13) Uani 1 1 d . . . N82 N 0.6208(4) 0.7690(3) -0.0137(3) 0.0444(13) Uani 1 1 d . A . C821 C 0.6624(5) 0.8332(5) -0.0206(5) 0.0544(18) Uani 1 1 d . . . H82A H 0.6404 0.8493 -0.0664 0.082 Uiso 1 1 calc R A . H82B H 0.718 0.8214 -0.0074 0.082 Uiso 1 1 calc R . . H82C H 0.657 0.8723 0.0075 0.082 Uiso 1 1 calc R . . C83 C 0.6380(5) 0.6980(4) -0.0267(4) 0.0556(19) Uani 1 1 d . . . H83 H 0.677 0.6839 -0.042 0.067 Uiso 1 1 calc R A . C84 C 0.5897(5) 0.6541(4) -0.0135(4) 0.056(2) Uani 1 1 d . A . H84 H 0.5876 0.6025 -0.0175 0.067 Uiso 1 1 calc R . . N85 N 0.5431(4) 0.6968(3) 0.0069(3) 0.0432(13) Uani 1 1 d . A . H85 H 0.5057 0.6805 0.0182 0.052 Uiso 1 1 calc R . . S01 S 0.24041(13) 0.56074(10) -0.09335(13) 0.0592(5) Uani 1 1 d . . . O11 O 0.2844(4) 0.6289(3) -0.0744(3) 0.0589(14) Uani 1 1 d . A . O12 O 0.2351(5) 0.5282(5) -0.0337(5) 0.106(3) Uani 1 1 d . A . O13 O 0.1595(4) 0.5758(4) -0.1405(3) 0.0643(16) Uani 1 1 d . A . O14 O 0.2803(4) 0.5115(4) -0.1214(5) 0.102(3) Uani 1 1 d . A . S02 S 0.20810(13) 1.03955(13) 0.08407(14) 0.0648(6) Uani 1 1 d U A . O21 O 0.2747(4) 0.9909(4) 0.0922(5) 0.086(2) Uani 1 1 d U . . O22 O 0.2301(5) 1.0922(6) 0.1361(5) 0.107(3) Uani 1 1 d U . . O23 O 0.1424(5) 0.9950(5) 0.0793(6) 0.101(3) Uani 1 1 d U . . O24 O 0.1929(6) 1.0782(5) 0.0223(5) 0.099(2) Uani 1 1 d U . . S03 S 0.50821(14) 0.61962(17) 0.13103(18) 0.0353(9) Uani 0.739(11) 1 d P A 1 O31 O 0.5399(6) 0.6893(5) 0.1681(5) 0.0476(19) Uani 0.739(11) 1 d P A 1 O32 O 0.5729(4) 0.5788(4) 0.1254(4) 0.049(2) Uani 0.739(11) 1 d P A 1 O33 O 0.4666(5) 0.5775(5) 0.1625(4) 0.060(2) Uani 0.739(11) 1 d P A 1 O34 O 0.4519(4) 0.6421(4) 0.0648(4) 0.0428(18) Uani 0.739(11) 1 d P A 1 S03' S 0.5007(5) 0.6359(4) 0.1588(7) 0.049(3) Uani 0.261(11) 1 d P A 2 O31' O 0.4544(18) 0.6769(12) 0.0968(15) 0.068(8) Uani 0.261(11) 1 d P A 2 O32' O 0.535(2) 0.5684(18) 0.1407(16) 0.076(8) Uiso 0.261(11) 1 d P A 2 O33' O 0.4534(15) 0.6231(11) 0.1941(13) 0.059(6) Uani 0.261(11) 1 d P A 2 O34' O 0.5690(18) 0.6740(15) 0.1968(15) 0.056(7) Uani 0.261(11) 1 d P A 2 O1 O 0.4285(6) 0.5218(5) -0.0142(4) 0.101(3) Uani 1 1 d . . . O2 O 0.3483(6) 0.4778(5) 0.0940(6) 0.120(4) Uani 1 1 d . . . O3 O 0.0169(14) 1.2638(9) -0.1418(9) 0.205(9) Uani 1 1 d . . . O4 O 0.2611(10) 1.0440(12) 0.2699(10) 0.199(9) Uani 1 1 d . . . O5 O 0.3807(15) 1.0359(12) 0.3942(10) 0.248(12) Uani 1 1 d . . . O6 O 0.6045(5) 1.0939(8) 0.4743(4) 0.124(4) Uani 1 1 d . . . O7 O 0.0801(15) 0.9683(15) 0.1730(17) 0.163(12) Uani 0.5 1 d P . . O8 O 0.5145(9) 1.1114(7) 0.4256(7) 0.067(3) Uani 0.5 1 d P . . O09 O 0.6343(12) 1.0529(12) 0.5216(11) 0.120(8) Uani 0.5 1 d P . . O010 O 0.5043(12) 0.4680(13) 0.4588(11) 0.118(7) Uani 0.5 1 d P . . O011 O 0.113(2) 1.197(2) -0.0217(19) 0.189(13) Uiso 0.5 1 d P . . O012 O 0.348(3) 0.446(3) 0.218(3) 0.25(2) Uiso 0.5 1 d P . . O013 O 0.382(2) 1.301(2) 0.262(2) 0.192(14) Uiso 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0443(3) 0.0410(3) 0.0467(3) -0.0031(2) -0.0022(2) 0.0087(2) Ag2 0.0757(5) 0.0621(4) 0.0848(5) 0.0073(3) 0.0562(4) 0.0041(3) Ag3 0.0728(4) 0.0457(3) 0.0457(3) 0.0054(2) 0.0246(3) -0.0003(3) Ag4 0.0440(3) 0.0465(3) 0.0549(3) -0.0008(2) 0.0060(3) -0.0019(2) Ag5 0.0497(3) 0.0621(4) 0.0713(4) 0.0012(3) 0.0310(3) -0.0067(3) Ag6 0.0745(4) 0.0456(3) 0.0391(3) -0.0089(2) -0.0034(3) 0.0214(3) S1 0.0367(8) 0.0333(7) 0.0464(9) -0.0003(6) 0.0092(7) 0.0020(6) C11 0.037(3) 0.028(3) 0.056(4) 0.004(3) 0.011(3) 0.001(2) N12 0.036(3) 0.034(3) 0.052(3) 0.004(2) 0.002(3) -0.003(2) C121 0.043(4) 0.057(4) 0.048(4) -0.005(3) -0.001(3) -0.001(3) C13 0.033(3) 0.044(4) 0.075(6) 0.003(4) 0.009(4) -0.006(3) C14 0.036(4) 0.053(5) 0.098(7) 0.007(5) 0.015(4) -0.004(3) N15 0.054(4) 0.043(3) 0.067(4) 0.001(3) 0.031(3) -0.005(3) S2 0.0327(7) 0.0388(7) 0.0346(7) 0.0024(6) 0.0082(6) 0.0018(6) C21 0.026(3) 0.033(3) 0.033(3) 0.001(2) 0.003(2) 0.002(2) N22 0.037(3) 0.037(3) 0.043(3) 0.011(2) 0.015(2) 0.006(2) C221 0.048(4) 0.047(4) 0.063(5) 0.010(3) 0.025(4) -0.007(3) C23 0.056(4) 0.044(4) 0.042(4) 0.004(3) 0.020(3) 0.011(3) C24 0.051(4) 0.036(3) 0.045(4) 0.002(3) 0.010(3) 0.002(3) N25 0.042(3) 0.035(3) 0.036(3) -0.002(2) 0.011(2) -0.003(2) S3 0.0483(10) 0.0439(9) 0.0503(10) -0.0024(7) 0.0179(8) 0.0027(7) C31 0.045(4) 0.051(4) 0.052(4) 0.005(3) 0.023(3) 0.007(3) N32 0.082(6) 0.064(5) 0.081(6) 0.007(4) 0.052(5) 0.003(4) C321 0.165(15) 0.072(7) 0.153(14) 0.032(8) 0.115(13) 0.007(8) C33 0.091(8) 0.099(8) 0.100(9) -0.015(7) 0.071(8) -0.008(6) C34 0.086(7) 0.073(6) 0.080(7) -0.007(5) 0.051(6) 0.006(5) N35 0.051(4) 0.052(4) 0.062(4) 0.001(3) 0.030(3) 0.002(3) S4 0.0340(7) 0.0296(6) 0.0353(7) 0.0013(5) 0.0083(6) 0.0026(5) C41 0.052(4) 0.036(3) 0.039(3) -0.001(3) 0.017(3) 0.003(3) N42 0.069(4) 0.040(3) 0.041(3) -0.001(3) 0.016(3) -0.003(3) C421 0.059(5) 0.048(4) 0.045(4) -0.004(3) -0.001(3) -0.003(3) C43 0.099(9) 0.098(8) 0.061(6) -0.021(6) 0.043(6) -0.005(7) C44 0.114(11) 0.129(11) 0.092(9) -0.038(8) 0.076(9) -0.015(9) N45 0.065(5) 0.088(6) 0.073(5) -0.018(4) 0.037(4) 0.000(4) S5 0.0541(11) 0.0512(10) 0.0470(9) 0.0014(8) 0.0215(8) 0.0005(8) C51 0.047(5) 0.093(7) 0.067(6) 0.021(5) 0.012(4) -0.016(5) N52 0.087(7) 0.140(11) 0.126(10) 0.034(8) 0.077(8) 0.017(7) C521 0.132(14) 0.180(19) 0.128(14) -0.002(13) 0.093(12) 0.010(13) C53 0.088(9) 0.126(12) 0.119(11) 0.020(9) 0.072(9) -0.016(8) C54 0.083(9) 0.108(11) 0.126(12) 0.030(9) 0.035(9) -0.027(8) N55 0.073(6) 0.100(7) 0.085(7) 0.024(6) -0.002(5) -0.040(5) S6 0.0593(11) 0.0474(9) 0.0516(10) -0.0101(8) 0.0271(9) -0.0137(8) C61 0.050(4) 0.059(5) 0.059(5) -0.007(4) 0.022(4) -0.002(4) N62 0.057(4) 0.067(5) 0.087(6) 0.000(4) 0.041(4) -0.009(3) C621 0.078(6) 0.055(5) 0.087(7) -0.004(5) 0.045(6) -0.011(4) C63 0.080(8) 0.105(9) 0.106(9) -0.005(7) 0.063(7) -0.007(7) C64 0.094(9) 0.101(9) 0.153(14) -0.019(9) 0.092(10) -0.002(7) N65 0.062(5) 0.071(5) 0.090(6) -0.011(4) 0.042(5) 0.006(4) S7 0.0352(7) 0.0338(7) 0.0373(7) 0.0018(6) 0.0105(6) 0.0027(6) C71 0.030(3) 0.033(3) 0.033(3) -0.001(2) 0.000(2) -0.001(2) N72 0.049(3) 0.041(3) 0.055(4) -0.005(3) 0.020(3) 0.006(3) C721 0.069(6) 0.062(5) 0.093(7) 0.016(5) 0.054(6) 0.005(4) C73 0.067(5) 0.056(5) 0.051(4) -0.006(4) 0.012(4) 0.023(4) C74 0.055(5) 0.038(4) 0.060(5) 0.002(3) -0.007(4) 0.006(3) N75 0.041(3) 0.030(3) 0.051(3) 0.008(2) 0.000(3) -0.001(2) S8 0.0377(8) 0.0294(6) 0.0336(7) -0.0011(5) 0.0092(6) 0.0007(5) C81 0.039(3) 0.031(3) 0.036(3) 0.001(2) 0.007(3) 0.002(2) N82 0.047(3) 0.039(3) 0.044(3) -0.004(2) 0.015(3) 0.006(2) C821 0.055(4) 0.051(4) 0.064(5) -0.003(4) 0.030(4) 0.003(3) C83 0.065(5) 0.041(4) 0.056(5) -0.008(3) 0.018(4) 0.011(3) C84 0.060(5) 0.037(3) 0.053(4) -0.009(3) 0.004(4) 0.016(3) N85 0.046(3) 0.027(2) 0.045(3) -0.003(2) 0.005(3) -0.002(2) S01 0.0501(11) 0.0335(8) 0.0769(14) -0.0052(8) 0.0070(10) -0.0023(7) O11 0.071(4) 0.036(3) 0.068(4) -0.004(2) 0.027(3) -0.005(2) O12 0.084(5) 0.076(5) 0.139(8) 0.045(5) 0.022(5) -0.021(4) O13 0.054(3) 0.067(4) 0.066(4) -0.019(3) 0.016(3) 0.002(3) O14 0.060(4) 0.078(5) 0.161(9) -0.065(5) 0.037(5) -0.003(4) S02 0.0493(11) 0.0582(12) 0.0919(17) -0.0121(11) 0.0332(11) 0.0043(9) O21 0.056(4) 0.082(5) 0.131(6) -0.030(4) 0.050(4) -0.002(3) O22 0.079(5) 0.116(7) 0.118(7) -0.044(5) 0.032(5) 0.016(5) O23 0.059(4) 0.102(6) 0.151(8) 0.005(5) 0.050(5) -0.001(4) O24 0.111(7) 0.079(5) 0.107(6) -0.004(4) 0.045(5) 0.011(5) S03 0.0345(11) 0.0268(12) 0.0395(15) 0.0036(11) 0.0091(10) -0.0037(8) O31 0.048(5) 0.044(4) 0.051(5) -0.015(4) 0.018(4) -0.004(4) O32 0.042(4) 0.033(3) 0.055(4) 0.001(3) 0.002(3) 0.004(3) O33 0.056(5) 0.070(5) 0.052(4) 0.016(4) 0.020(4) -0.017(4) O34 0.032(3) 0.043(4) 0.047(4) 0.007(3) 0.009(3) 0.005(3) S03' 0.054(4) 0.028(3) 0.060(6) -0.004(3) 0.018(4) 0.006(3) O31' 0.11(2) 0.023(9) 0.076(17) 0.009(11) 0.037(15) 0.018(10) O33' 0.081(16) 0.032(10) 0.081(16) -0.002(10) 0.048(14) -0.003(9) O34' 0.052(16) 0.053(14) 0.057(16) 0.009(12) 0.016(13) 0.002(11) O1 0.134(8) 0.068(5) 0.082(5) -0.003(4) 0.023(5) -0.007(5) O2 0.092(6) 0.078(6) 0.176(11) 0.004(6) 0.038(7) 0.006(5) O3 0.34(3) 0.150(13) 0.211(17) 0.008(12) 0.200(19) 0.005(15) O4 0.156(13) 0.25(2) 0.228(18) 0.115(16) 0.119(14) 0.074(13) O5 0.39(3) 0.243(19) 0.221(18) -0.108(16) 0.24(2) -0.17(2) O6 0.071(5) 0.243(13) 0.060(4) -0.014(6) 0.027(4) 0.066(7) O7 0.130(18) 0.16(2) 0.27(3) -0.06(2) 0.16(2) -0.046(16) O8 0.090(9) 0.071(8) 0.063(7) -0.004(6) 0.055(7) 0.008(7) O09 0.095(13) 0.128(16) 0.130(16) 0.086(14) 0.039(12) 0.050(12) O010 0.089(13) 0.140(18) 0.131(17) 0.043(14) 0.048(12) -0.009(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.4680(16) . ? Ag1 S8 2.5976(16) . ? Ag1 S4 2.6032(16) . ? Ag1 S1 2.7198(19) . ? Ag1 Ag3 3.1642(9) . ? Ag2 S2 2.4775(18) . ? Ag2 S3 2.534(2) . ? Ag2 S5 2.583(2) . ? Ag3 O31' 2.34(2) . ? Ag3 O31 2.487(11) . ? Ag3 S5 2.526(2) . ? Ag3 S8 2.5709(17) . ? Ag3 S6 2.660(2) . ? Ag3 Ag4 3.2572(9) . ? Ag4 O21 2.496(7) . ? Ag4 S6 2.552(2) . ? Ag4 S4 2.5639(16) . ? Ag4 S1 2.5903(19) 3_675 ? Ag4 Ag6 3.3341(10) . ? Ag5 O11 2.420(5) . ? Ag5 S3 2.515(2) 4_575 ? Ag5 S7 2.5373(18) . ? Ag5 S6 2.603(2) . ? Ag6 S7 2.4764(17) . ? Ag6 S8 2.5294(16) . ? Ag6 S1 2.5744(17) 3_675 ? Ag6 S4 2.9570(18) 3_675 ? S1 C11 1.715(7) . ? S1 Ag6 2.5744(17) 3_675 ? S1 Ag4 2.5903(19) 3_675 ? C11 N12 1.357(10) . ? C11 N15 1.360(10) . ? N12 C13 1.359(10) . ? N12 C121 1.468(11) . ? C121 H12A 0.98 . ? C121 H12B 0.98 . ? C121 H12C 0.98 . ? C13 C14 1.323(14) . ? C13 H13 0.95 . ? C14 N15 1.377(11) . ? C14 H14 0.95 . ? N15 H15 0.88 . ? S2 C21 1.728(6) . ? C21 N25 1.340(8) . ? C21 N22 1.347(8) . ? N22 C23 1.402(9) . ? N22 C221 1.462(9) . ? C221 H22A 0.98 . ? C221 H22B 0.98 . ? C221 H22C 0.98 . ? C23 C24 1.359(11) . ? C23 H23 0.95 . ? C24 N25 1.377(10) . ? C24 H24 0.95 . ? N25 H25 0.88 . ? S3 C31 1.721(8) . ? S3 Ag5 2.515(2) 4_676 ? C31 N35 1.331(10) . ? C31 N32 1.348(11) . ? N32 C33 1.386(14) . ? N32 C321 1.433(15) . ? C321 H32A 0.98 . ? C321 H32B 0.98 . ? C321 H32C 0.98 . ? C33 C34 1.388(17) . ? C33 H33 0.95 . ? C34 N35 1.329(11) . ? C34 H34 0.95 . ? N35 H35 0.88 . ? S4 C41 1.718(7) . ? S4 Ag6 2.9570(18) 3_675 ? C41 N45 1.302(11) . ? C41 N42 1.357(10) . ? N42 C43 1.384(12) . ? N42 C421 1.433(12) . ? C421 H42A 0.98 . ? C421 H42B 0.98 . ? C421 H42C 0.98 . ? C43 C44 1.363(19) . ? C43 H43 0.95 . ? C44 N45 1.392(14) . ? C44 H44 0.95 . ? N45 H45 0.88 . ? S5 C51 1.724(10) . ? C51 N52 1.288(14) . ? C51 N55 1.356(17) . ? N52 C53 1.377(19) . ? N52 C521 1.39(2) . ? C521 H52A 0.98 . ? C521 H52B 0.98 . ? C521 H52C 0.98 . ? C53 C54 1.27(2) . ? C53 H53 0.95 . ? C54 N55 1.334(16) . ? C54 H54 0.95 . ? N55 H55 0.88 . ? S6 C61 1.721(9) . ? C61 N65 1.317(11) . ? C61 N62 1.357(12) . ? N62 C63 1.390(13) . ? N62 C621 1.456(13) . ? C621 H62A 0.98 . ? C621 H62B 0.98 . ? C621 H62C 0.98 . ? C63 C64 1.350(19) . ? C63 H63 0.95 . ? C64 N65 1.374(15) . ? C64 H64 0.95 . ? N65 H65 0.88 . ? S7 C71 1.727(7) . ? C71 N75 1.335(8) . ? C71 N72 1.349(9) . ? N72 C73 1.386(10) . ? N72 C721 1.456(11) . ? C721 H72A 0.98 . ? C721 H72B 0.98 . ? C721 H72C 0.98 . ? C73 C74 1.338(14) . ? C73 H73 0.95 . ? C74 N75 1.350(11) . ? C74 H74 0.95 . ? N75 H75 0.88 . ? S8 C81 1.730(7) . ? C81 N82 1.323(9) . ? C81 N85 1.349(8) . ? N82 C83 1.399(9) . ? N82 C821 1.449(10) . ? C821 H82A 0.98 . ? C821 H82B 0.98 . ? C821 H82C 0.98 . ? C83 C84 1.322(13) . ? C83 H83 0.95 . ? C84 N85 1.369(10) . ? C84 H84 0.95 . ? N85 H85 0.88 . ? S01 O14 1.455(7) . ? S01 O11 1.462(6) . ? S01 O13 1.479(7) . ? S01 O12 1.492(10) . ? S02 O22 1.436(9) . ? S02 O23 1.438(9) . ? S02 O24 1.468(10) . ? S02 O21 1.478(7) . ? S03 O33 1.453(8) . ? S03 O32 1.463(8) . ? S03 O34 1.486(7) . ? S03 O31 1.507(8) . ? S03' O34' 1.40(3) . ? S03' O33' 1.41(3) . ? S03' O31' 1.50(3) . ? S03' O32' 1.52(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 S2 Ag1 S8 118.99(5) . . ? S2 Ag1 S4 138.99(6) . . ? S8 Ag1 S4 91.53(5) . . ? S2 Ag1 S1 109.33(6) . . ? S8 Ag1 S1 99.79(6) . . ? S4 Ag1 S1 89.70(5) . . ? S2 Ag1 Ag3 95.18(4) . . ? S8 Ag1 Ag3 51.87(4) . . ? S4 Ag1 Ag3 82.38(4) . . ? S1 Ag1 Ag3 149.99(4) . . ? S2 Ag2 S3 132.23(7) . . ? S2 Ag2 S5 121.02(6) . . ? S3 Ag2 S5 106.26(7) . . ? O31' Ag3 O31 42.5(7) . . ? O31' Ag3 S5 118.5(7) . . ? O31 Ag3 S5 94.0(2) . . ? O31' Ag3 S8 101.0(7) . . ? O31 Ag3 S8 107.7(2) . . ? S5 Ag3 S8 138.20(6) . . ? O31' Ag3 S6 84.3(7) . . ? O31 Ag3 S6 125.4(2) . . ? S5 Ag3 S6 105.06(7) . . ? S8 Ag3 S6 91.10(6) . . ? O31' Ag3 Ag1 134.4(7) . . ? O31 Ag3 Ag1 104.5(2) . . ? S5 Ag3 Ag1 87.95(5) . . ? S8 Ag3 Ag1 52.63(4) . . ? S6 Ag3 Ag1 126.44(5) . . ? O31' Ag3 Ag4 133.1(7) . . ? O31 Ag3 Ag4 175.2(2) . . ? S5 Ag3 Ag4 87.10(5) . . ? S8 Ag3 Ag4 74.25(4) . . ? S6 Ag3 Ag4 49.84(4) . . ? Ag1 Ag3 Ag4 80.23(2) . . ? O21 Ag4 S6 98.99(19) . . ? O21 Ag4 S4 101.24(19) . . ? S6 Ag4 S4 133.95(7) . . ? O21 Ag4 S1 111.8(2) . 3_675 ? S6 Ag4 S1 104.72(6) . 3_675 ? S4 Ag4 S1 105.35(6) . 3_675 ? O21 Ag4 Ag3 115.3(2) . . ? S6 Ag4 Ag3 52.83(5) . . ? S4 Ag4 Ag3 81.12(4) . . ? S1 Ag4 Ag3 130.06(5) 3_675 . ? O21 Ag4 Ag6 155.8(2) . . ? S6 Ag4 Ag6 75.45(5) . . ? S4 Ag4 Ag6 99.21(4) . . ? S1 Ag4 Ag6 49.58(4) 3_675 . ? Ag3 Ag4 Ag6 80.50(2) . . ? O11 Ag5 S3 108.68(16) . 4_575 ? O11 Ag5 S7 101.48(16) . . ? S3 Ag5 S7 115.00(6) 4_575 . ? O11 Ag5 S6 103.17(16) . . ? S3 Ag5 S6 109.83(7) 4_575 . ? S7 Ag5 S6 117.29(6) . . ? S7 Ag6 S8 118.36(5) . . ? S7 Ag6 S1 114.17(6) . 3_675 ? S8 Ag6 S1 118.59(6) . 3_675 ? S7 Ag6 S4 119.39(6) . 3_675 ? S8 Ag6 S4 94.89(5) . 3_675 ? S1 Ag6 S4 85.21(5) 3_675 3_675 ? S7 Ag6 Ag4 127.03(5) . . ? S8 Ag6 Ag4 73.32(4) . . ? S1 Ag6 Ag4 50.00(4) 3_675 . ? S4 Ag6 Ag4 109.73(4) 3_675 . ? C11 S1 Ag6 119.5(2) . 3_675 ? C11 S1 Ag4 106.5(3) . 3_675 ? Ag6 S1 Ag4 80.41(5) 3_675 3_675 ? C11 S1 Ag1 116.7(2) . . ? Ag6 S1 Ag1 94.28(6) 3_675 . ? Ag4 S1 Ag1 132.40(7) 3_675 . ? N12 C11 N15 104.4(6) . . ? N12 C11 S1 129.3(6) . . ? N15 C11 S1 126.0(6) . . ? C11 N12 C13 110.7(7) . . ? C11 N12 C121 124.3(6) . . ? C13 N12 C121 125.0(7) . . ? N12 C121 H12A 109.5 . . ? N12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? N12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 N12 107.8(8) . . ? C14 C13 H13 126.1 . . ? N12 C13 H13 126.1 . . ? C13 C14 N15 107.3(8) . . ? C13 C14 H14 126.4 . . ? N15 C14 H14 126.4 . . ? C11 N15 C14 109.9(8) . . ? C11 N15 H15 125 . . ? C14 N15 H15 125 . . ? C21 S2 Ag1 100.2(2) . . ? C21 S2 Ag2 107.8(2) . . ? Ag1 S2 Ag2 93.59(6) . . ? N25 C21 N22 107.1(6) . . ? N25 C21 S2 128.3(5) . . ? N22 C21 S2 124.5(5) . . ? C21 N22 C23 109.4(6) . . ? C21 N22 C221 125.6(6) . . ? C23 N22 C221 125.0(6) . . ? N22 C221 H22A 109.5 . . ? N22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? N22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C24 C23 N22 106.2(6) . . ? C24 C23 H23 126.9 . . ? N22 C23 H23 126.9 . . ? C23 C24 N25 107.4(6) . . ? C23 C24 H24 126.3 . . ? N25 C24 H24 126.3 . . ? C21 N25 C24 110.1(6) . . ? C21 N25 H25 125 . . ? C24 N25 H25 125 . . ? C31 S3 Ag5 102.5(3) . 4_676 ? C31 S3 Ag2 101.7(3) . . ? Ag5 S3 Ag2 88.31(7) 4_676 . ? N35 C31 N32 107.2(7) . . ? N35 C31 S3 128.5(6) . . ? N32 C31 S3 124.3(6) . . ? C31 N32 C33 108.3(8) . . ? C31 N32 C321 126.3(9) . . ? C33 N32 C321 125.3(9) . . ? N32 C321 H32A 109.5 . . ? N32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? N32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? N32 C33 C34 106.3(9) . . ? N32 C33 H33 126.8 . . ? C34 C33 H33 126.8 . . ? N35 C34 C33 106.5(9) . . ? N35 C34 H34 126.7 . . ? C33 C34 H34 126.7 . . ? C34 N35 C31 111.6(8) . . ? C34 N35 H35 124.2 . . ? C31 N35 H35 124.2 . . ? C41 S4 Ag4 102.6(3) . . ? C41 S4 Ag1 110.6(2) . . ? Ag4 S4 Ag1 106.42(6) . . ? C41 S4 Ag6 113.1(3) . 3_675 ? Ag4 S4 Ag6 133.48(6) . 3_675 ? Ag1 S4 Ag6 88.32(5) . 3_675 ? N45 C41 N42 108.7(7) . . ? N45 C41 S4 126.2(6) . . ? N42 C41 S4 125.1(6) . . ? C41 N42 C43 108.5(8) . . ? C41 N42 C421 126.5(7) . . ? C43 N42 C421 125.0(8) . . ? N42 C421 H42A 109.5 . . ? N42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? N42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C44 C43 N42 106.3(10) . . ? C44 C43 H43 126.8 . . ? N42 C43 H43 126.8 . . ? C43 C44 N45 107.0(9) . . ? C43 C44 H44 126.5 . . ? N45 C44 H44 126.5 . . ? C41 N45 C44 109.4(10) . . ? C41 N45 H45 125.3 . . ? C44 N45 H45 125.3 . . ? C51 S5 Ag3 103.8(4) . . ? C51 S5 Ag2 98.8(4) . . ? Ag3 S5 Ag2 83.74(7) . . ? N52 C51 N55 102.6(11) . . ? N52 C51 S5 129.5(12) . . ? N55 C51 S5 127.9(10) . . ? C51 N52 C53 110.4(13) . . ? C51 N52 C521 121.9(13) . . ? C53 N52 C521 127.7(12) . . ? N52 C521 H52A 109.5 . . ? N52 C521 H52B 109.5 . . ? H52A C521 H52B 109.5 . . ? N52 C521 H52C 109.5 . . ? H52A C521 H52C 109.5 . . ? H52B C521 H52C 109.5 . . ? C54 C53 N52 109.2(11) . . ? C54 C53 H53 125.4 . . ? N52 C53 H53 125.4 . . ? C53 C54 N55 104.9(14) . . ? C53 C54 H54 127.6 . . ? N55 C54 H54 127.6 . . ? C54 N55 C51 112.9(14) . . ? C54 N55 H55 123.5 . . ? C51 N55 H55 123.5 . . ? C61 S6 Ag4 108.4(3) . . ? C61 S6 Ag5 116.7(3) . . ? Ag4 S6 Ag5 116.02(8) . . ? C61 S6 Ag3 104.4(3) . . ? Ag4 S6 Ag3 77.32(6) . . ? Ag5 S6 Ag3 126.98(8) . . ? N65 C61 N62 106.6(8) . . ? N65 C61 S6 127.5(8) . . ? N62 C61 S6 125.9(7) . . ? C61 N62 C63 109.3(9) . . ? C61 N62 C621 124.3(8) . . ? C63 N62 C621 126.3(9) . . ? N62 C621 H62A 109.5 . . ? N62 C621 H62B 109.5 . . ? H62A C621 H62B 109.5 . . ? N62 C621 H62C 109.5 . . ? H62A C621 H62C 109.5 . . ? H62B C621 H62C 109.5 . . ? C64 C63 N62 106.1(11) . . ? C64 C63 H63 126.9 . . ? N62 C63 H63 126.9 . . ? C63 C64 N65 107.3(10) . . ? C63 C64 H64 126.4 . . ? N65 C64 H64 126.4 . . ? C61 N65 C64 110.7(10) . . ? C61 N65 H65 124.7 . . ? C64 N65 H65 124.7 . . ? C71 S7 Ag6 112.4(2) . . ? C71 S7 Ag5 107.2(2) . . ? Ag6 S7 Ag5 86.75(6) . . ? N75 C71 N72 107.0(6) . . ? N75 C71 S7 127.0(5) . . ? N72 C71 S7 125.5(5) . . ? C71 N72 C73 107.9(7) . . ? C71 N72 C721 125.6(6) . . ? C73 N72 C721 126.5(8) . . ? N72 C721 H72A 109.5 . . ? N72 C721 H72B 109.5 . . ? H72A C721 H72B 109.5 . . ? N72 C721 H72C 109.5 . . ? H72A C721 H72C 109.5 . . ? H72B C721 H72C 109.5 . . ? C74 C73 N72 107.4(8) . . ? C74 C73 H73 126.3 . . ? N72 C73 H73 126.3 . . ? C73 C74 N75 107.5(7) . . ? C73 C74 H74 126.2 . . ? N75 C74 H74 126.2 . . ? C71 N75 C74 110.1(7) . . ? C71 N75 H75 125 . . ? C74 N75 H75 125 . . ? C81 S8 Ag6 105.1(2) . . ? C81 S8 Ag3 109.4(2) . . ? Ag6 S8 Ag3 113.24(7) . . ? C81 S8 Ag1 117.5(2) . . ? Ag6 S8 Ag1 130.87(6) . . ? Ag3 S8 Ag1 75.50(5) . . ? N82 C81 N85 106.3(6) . . ? N82 C81 S8 127.1(5) . . ? N85 C81 S8 126.6(6) . . ? C81 N82 C83 109.5(7) . . ? C81 N82 C821 126.4(6) . . ? C83 N82 C821 124.0(7) . . ? N82 C821 H82A 109.5 . . ? N82 C821 H82B 109.5 . . ? H82A C821 H82B 109.5 . . ? N82 C821 H82C 109.5 . . ? H82A C821 H82C 109.5 . . ? H82B C821 H82C 109.5 . . ? C84 C83 N82 106.9(7) . . ? C84 C83 H83 126.6 . . ? N82 C83 H83 126.6 . . ? C83 C84 N85 107.4(7) . . ? C83 C84 H84 126.3 . . ? N85 C84 H84 126.3 . . ? C81 N85 C84 109.9(7) . . ? C81 N85 H85 125 . . ? C84 N85 H85 125 . . ? O14 S01 O11 109.4(4) . . ? O14 S01 O13 111.1(5) . . ? O11 S01 O13 109.9(4) . . ? O14 S01 O12 110.8(6) . . ? O11 S01 O12 108.2(5) . . ? O13 S01 O12 107.3(5) . . ? S01 O11 Ag5 140.4(4) . . ? O22 S02 O23 113.9(6) . . ? O22 S02 O24 108.3(6) . . ? O23 S02 O24 111.2(6) . . ? O22 S02 O21 110.5(5) . . ? O23 S02 O21 108.2(5) . . ? O24 S02 O21 104.4(5) . . ? S02 O21 Ag4 146.1(6) . . ? O33 S03 O32 112.4(5) . . ? O33 S03 O34 108.8(4) . . ? O32 S03 O34 109.8(5) . . ? O33 S03 O31 110.8(6) . . ? O32 S03 O31 108.9(5) . . ? O34 S03 O31 106.0(5) . . ? S03 O31 Ag3 115.8(6) . . ? O34' S03' O33' 111.2(18) . . ? O34' S03' O31' 110.9(16) . . ? O33' S03' O31' 109.5(17) . . ? O34' S03' O32' 101.1(18) . . ? O33' S03' O32' 115.4(16) . . ? O31' S03' O32' 108.3(17) . . ? S03' O31' Ag3 110.1(16) . . ? 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 N15 H15 O24 0.88 1.9 2.727(12) 156.3 3_675 N25 H25 O34' 0.88 1.75 2.63(3) 178 . N25 H25 O31 0.88 1.95 2.794(11) 160 . N35 H35 O13 0.88 1.89 2.755(9) 167.6 4_676 N45 H45 O21 0.88 1.88 2.747(12) 166.1 . N45 H45 S02 0.88 2.77 3.614(9) 161.2 . N55 H55 O33' 0.88 1.35 2.03(3) 130.4 . N55 H55 O31 0.88 2.24 3.060(16) 155.9 . N55 H55 O34' 0.88 2.34 3.14(3) 151.1 . N55 H55 O33 0.88 2.47 3.206(17) 141.9 . N65 H65 O21 0.88 1.95 2.814(13) 166.4 . N65 H65 O23 0.88 2.56 3.217(13) 132.2 . N75 H75 O11 0.88 2.02 2.867(10) 161 . N75 H75 O14 0.88 2.58 3.277(11) 137 . N85 H85 O34 0.88 1.84 2.694(10) 163 . N85 H85 O31' 0.88 2.3 3.07(3) 147 . #===END # Attachment '- gb0956.cif' data_gb0956 _database_code_depnum_ccdc_archive 'CCDC 758123' #TrackingRef '- gb0956.cif' _audit_creation_date 2009-12-10T12:28:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C16 H26 Ag2 N8 O5 S5' _chemical_formula_moiety '2(C8 H12 Ag N4 S2), O4 S, H2 O' _chemical_formula_weight 786.49 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'p -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 13.3395(4) _cell_length_b 13.3395(4) _cell_length_c 7.1811(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1277.82(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4212 _cell_measurement_theta_min 2.8318 _cell_measurement_theta_max 32.2707 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.96117 _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 0.0515083752 _diffrn_orient_matrix_ub_12 -0.0072816013 _diffrn_orient_matrix_ub_13 0.0198111249 _diffrn_orient_matrix_ub_21 0.0091740341 _diffrn_orient_matrix_ub_22 0.0515881299 _diffrn_orient_matrix_ub_23 -0.0161138026 _diffrn_orient_matrix_ub_31 -0.0091504029 _diffrn_orient_matrix_ub_32 0.0102191925 _diffrn_orient_matrix_ub_33 0.0953483452 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_unetI/netI 0.0654 _diffrn_reflns_number 13726 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 32.33 _diffrn_reflns_theta_full 30.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.963 _reflns_number_total 2175 _reflns_number_gt 1656 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The water molecule was modelled as being disordered about the 4bar axis with the associated hydrogen atoms not being located. ; _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^)+(0.0157P)^2^+4.7195P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2175 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.075 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.22 _refine_ls_restrained_S_all 1.22 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(8) _refine_diff_density_max 2.2 _refine_diff_density_min -3.045 _refine_diff_density_rms 0.178 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' N N 0.0061 0.0033 '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 0.5 0.02955(6) 0.01491(12) Uani 1 2 d S . . S1 S 0.01228(9) 0.35938(9) 0.28065(18) 0.0101(2) Uani 1 1 d . . . C1 C 0.1289(5) 0.3138(4) 0.3270(8) 0.0118(12) Uani 1 1 d . . . N2 N 0.2176(4) 0.3617(4) 0.3293(7) 0.0121(10) Uani 1 1 d . . . C21 C 0.2358(4) 0.4668(4) 0.2898(9) 0.0152(11) Uani 1 1 d . . . H2A H 0.2031 0.485 0.1724 0.023 Uiso 1 1 calc R . . H2B H 0.3082 0.4784 0.2794 0.023 Uiso 1 1 calc R . . H2C H 0.2085 0.5079 0.3909 0.023 Uiso 1 1 calc R . . C3 C 0.2918(5) 0.2964(5) 0.3863(9) 0.0177(13) Uani 1 1 d . . . H3 H 0.361 0.3116 0.4006 0.021 Uiso 1 1 calc R . . C4 C 0.2480(5) 0.2076(5) 0.4177(9) 0.0174(13) Uani 1 1 d . . . H4 H 0.2804 0.1481 0.4588 0.021 Uiso 1 1 calc R . . N5 N 0.1471(4) 0.2184(4) 0.3791(7) 0.0147(10) Uani 1 1 d . . . H5 H 0.1019 0.1706 0.3874 0.018 Uiso 1 1 calc R . . S2 S 0 0 0.5 0.0191(5) Uani 1 4 d S . . O2 O -0.0103(7) 0.0886(4) 0.3851(10) 0.071(2) Uani 1 1 d . . . O1 O -0.0177(16) 0.0504(12) -0.001(3) 0.033(5) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0158(3) 0.0178(3) 0.01119(19) 0 0 0.0072(3) S1 0.0085(6) 0.0129(5) 0.0119(5) 0.0005(5) -0.0001(5) -0.0011(5) C1 0.017(3) 0.011(3) 0.007(3) 0.001(2) 0.003(2) 0.002(2) N2 0.014(2) 0.012(2) 0.010(3) 0.0014(18) 0.0026(18) 0.001(2) C21 0.017(3) 0.012(2) 0.017(3) 0.000(2) 0.001(3) -0.0036(19) C3 0.011(3) 0.028(4) 0.013(3) 0.001(3) 0.002(2) 0.006(3) C4 0.022(3) 0.015(3) 0.015(3) 0.001(2) -0.001(2) 0.010(3) N5 0.018(3) 0.012(2) 0.014(3) 0.0000(19) 0.002(2) 0.000(2) S2 0.0203(8) 0.0203(8) 0.0168(13) 0 0 0 O2 0.073(5) 0.044(3) 0.096(5) 0.047(3) -0.033(6) -0.035(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.5961(13) 5_454 ? Ag1 S1 2.5961(13) 6_554 ? Ag1 S1 2.6071(13) 2_565 ? Ag1 S1 2.6071(13) . ? S1 C1 1.703(6) . ? S1 Ag1 2.5961(13) 5_455 ? C1 N2 1.345(7) . ? C1 N5 1.348(7) . ? N2 C3 1.381(8) . ? N2 C21 1.450(7) . ? C3 C4 1.340(9) . ? C4 N5 1.382(8) . ? S2 O2 1.448(5) 7_556 ? S2 O2 1.448(5) . ? S2 O2 1.448(5) 2 ? S2 O2 1.448(5) 8_556 ? 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 92.98(6) 5_454 6_554 ? S1 Ag1 S1 112.67(5) 5_454 2_565 ? S1 Ag1 S1 124.54(5) 6_554 2_565 ? S1 Ag1 S1 124.54(5) 5_454 . ? S1 Ag1 S1 112.67(5) 6_554 . ? S1 Ag1 S1 92.48(6) 2_565 . ? C1 S1 Ag1 100.4(2) . 5_455 ? C1 S1 Ag1 116.7(2) . . ? Ag1 S1 Ag1 87.27(4) 5_455 . ? N2 C1 N5 106.6(5) . . ? N2 C1 S1 129.5(4) . . ? N5 C1 S1 123.8(5) . . ? C1 N2 C3 109.5(5) . . ? C1 N2 C21 127.2(5) . . ? C3 N2 C21 123.2(5) . . ? C4 C3 N2 107.2(6) . . ? C3 C4 N5 107.4(5) . . ? C1 N5 C4 109.3(5) . . ? O2 S2 O2 108.9(3) 7_556 . ? O2 S2 O2 108.9(3) 7_556 2 ? O2 S2 O2 110.5(6) . 2 ? O2 S2 O2 110.5(6) 7_556 8_556 ? O2 S2 O2 108.9(3) . 8_556 ? O2 S2 O2 108.9(3) 2 8_556 ? 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 N5 H5 O2 0.88 1.85 2.722(9) 168.8 . #===END