# 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 'G Bowmaker' _publ_contact_author_email GA.BOWMAKER@AUCKLAND.AC.NZ _publ_section_title ; Structural and spectroscopic studies of some adducts of silver(I) halides with thiourea and N-ethyl substituted thioureas ; loop_ _publ_author_name 'G Bowmaker' 'Chaveng Pakawatchai' 'Saowanit Saithong' 'Brian W Skelton' 'Allan H. White' data_agbrdem _database_code_depnum_ccdc_archive 'CCDC 751797' _audit_creation_date 2009-10-06T12:17:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H36 Ag Br N6 S3' _chemical_formula_sum 'C15 H36 Ag Br N6 S3' _chemical_formula_weight 584.46 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P 3 1 c' _symmetry_space_group_name_Hall 'P 3 -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 12.5665(6) _cell_length_b 12.5665(6) _cell_length_c 9.5805(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1310.23(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2004 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 19.99 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 0.6 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_unetI/netI 0.0517 _diffrn_reflns_number 7843 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2028 _reflns_number_gt 1538 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0341P)^2^+0.0342P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2028 _refine_ls_number_parameters 109 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.004 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(14) _refine_diff_density_max 0.348 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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 0.66885(4) 0.0730(2) Uani 1 3 d S . . Br1 Br 0.3333 0.6667 0.94376(8) 0.0873(3) Uani 1 3 d S . . S1 S 0.17429(9) 0.44693(9) 0.59020(13) 0.0662(3) Uani 1 1 d . A . C1 C 0.0858(4) 0.4530(4) 0.4587(5) 0.0716(12) Uani 1 1 d . . . N1 N -0.0120(6) 0.3544(4) 0.4141(8) 0.128(3) Uani 1 1 d . A . H1 H -0.0462 0.3605 0.3391 0.154 Uiso 1 1 calc R . . C11 C -0.0668(10) 0.2355(8) 0.4822(15) 0.178(5) Uani 1 1 d . . . H11A H -0.0375 0.2454 0.5776 0.214 Uiso 1 1 calc R A . H11B H -0.1555 0.1992 0.4845 0.214 Uiso 1 1 calc R . . C12 C -0.0375(13) 0.1617(12) 0.4133(18) 0.204(6) Uani 1 1 d . A . H12A H -0.0609 0.1572 0.3172 0.306 Uiso 1 1 calc R . . H12B H -0.0799 0.0811 0.4539 0.306 Uiso 1 1 calc R . . H12C H 0.0496 0.1937 0.4192 0.306 Uiso 1 1 calc R . . N2A N 0.0949(14) 0.5509(9) 0.4087(13) 0.071(3) Uani 0.62(3) 1 d PD A 1 H2A H 0.157 0.6172 0.4394 0.086 Uiso 0.62(3) 1 calc PR A 1 C21A C 0.0178(14) 0.5725(11) 0.3066(18) 0.099(5) Uani 0.62(3) 1 d PD A 1 H21A H 0.0183 0.5322 0.2205 0.118 Uiso 0.62(3) 1 calc PR A 1 H21B H -0.0658 0.5288 0.3416 0.118 Uiso 0.62(3) 1 calc PR A 1 C22A C 0.038(3) 0.669(2) 0.277(4) 0.198(17) Uani 0.62(3) 1 d PD A 1 H22A H 0.0708 0.7226 0.3565 0.296 Uiso 0.62(3) 1 calc PR A 1 H22B H -0.0367 0.666 0.2476 0.296 Uiso 0.62(3) 1 calc PR A 1 H22C H 0.0967 0.7004 0.2023 0.296 Uiso 0.62(3) 1 calc PR A 1 N2B N 0.149(2) 0.5635(15) 0.3799(14) 0.062(4) Uani 0.38(3) 1 d PD A 2 H2B H 0.2222 0.6175 0.4042 0.074 Uiso 0.38(3) 1 calc PR A 2 C21B C 0.092(3) 0.5893(17) 0.2569(16) 0.078(6) Uani 0.38(3) 1 d PD A 2 H21C H 0.1278 0.5716 0.1765 0.093 Uiso 0.38(3) 1 calc PR A 2 H21D H 0.0067 0.5252 0.2589 0.093 Uiso 0.38(3) 1 calc PR A 2 C22B C 0.090(4) 0.678(3) 0.227(3) 0.116(10) Uani 0.38(3) 1 d PD A 2 H22D H 0.1296 0.7387 0.2982 0.174 Uiso 0.38(3) 1 calc PR A 2 H22E H 0.0066 0.659 0.2165 0.174 Uiso 0.38(3) 1 calc PR A 2 H22F H 0.133 0.7092 0.1398 0.174 Uiso 0.38(3) 1 calc PR A 2 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 0.0776(2) 0.0776(2) 0.0637(4) 0 0 0.03881(12) Br1 0.1028(4) 0.1028(4) 0.0565(5) 0 0 0.0514(2) S1 0.0614(6) 0.0649(6) 0.0666(6) 0.0069(5) -0.0016(5) 0.0274(5) C1 0.080(3) 0.058(3) 0.071(3) -0.007(2) -0.014(2) 0.029(2) N1 0.122(4) 0.069(3) 0.157(6) -0.001(3) -0.075(5) 0.021(3) C11 0.135(7) 0.098(6) 0.242(14) 0.000(7) -0.095(8) 0.013(5) C12 0.208(12) 0.146(9) 0.279(18) 0.021(10) -0.015(11) 0.104(9) N2A 0.059(6) 0.056(4) 0.084(6) 0.000(4) -0.024(4) 0.017(5) C21A 0.076(8) 0.091(7) 0.102(9) -0.001(6) -0.030(7) 0.021(6) C22A 0.27(4) 0.20(3) 0.22(3) -0.09(2) -0.12(3) 0.19(3) N2B 0.057(8) 0.058(6) 0.063(6) 0.007(5) 0.000(6) 0.022(7) C21B 0.092(15) 0.084(11) 0.072(9) 0.004(7) -0.006(8) 0.054(11) C22B 0.15(2) 0.122(19) 0.091(18) 0.022(15) -0.020(14) 0.083(15) #----------------------------------------------------------------------------# # 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 2.5823(10) 3_565 ? Ag1 S1 2.5823(11) . ? Ag1 S1 2.5823(11) 2_665 ? Ag1 Br1 2.6337(9) . ? S1 C1 1.707(5) . ? C1 N2A 1.272(10) . ? C1 N1 1.306(7) . ? C1 N2B 1.423(17) . ? N1 C11 1.451(11) . ? N1 H1 0.86 . ? C11 C12 1.331(17) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? N2A C21A 1.493(11) . ? N2A H2A 0.86 . ? C21A C22A 1.147(15) . ? C21A H21A 0.97 . ? C21A H21B 0.97 . ? C22A H22A 0.96 . ? C22A H22B 0.96 . ? C22A H22C 0.96 . ? N2B C21B 1.493(14) . ? N2B H2B 0.86 . ? C21B C22B 1.163(15) . ? C21B H21C 0.97 . ? C21B H21D 0.97 . ? C22B H22D 0.96 . ? C22B H22E 0.96 . ? C22B H22F 0.96 . ? 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 111.86(3) 3_565 . ? S1 Ag1 S1 111.86(3) 3_565 2_665 ? S1 Ag1 S1 111.86(3) . 2_665 ? S1 Ag1 Br1 106.97(3) 3_565 . ? S1 Ag1 Br1 106.97(3) . . ? S1 Ag1 Br1 106.97(3) 2_665 . ? C1 S1 Ag1 109.93(16) . . ? N2A C1 N1 112.3(6) . . ? N1 C1 N2B 123.5(8) . . ? N2A C1 S1 125.2(5) . . ? N1 C1 S1 121.7(4) . . ? N2B C1 S1 112.2(8) . . ? C1 N1 C11 124.5(6) . . ? C1 N1 H1 117.7 . . ? C11 N1 H1 117.7 . . ? C12 C11 N1 109.9(14) . . ? C12 C11 H11A 109.7 . . ? N1 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? N1 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? 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 . . ? C1 N2A C21A 132.1(9) . . ? C1 N2A H2A 113.9 . . ? C21A N2A H2A 113.9 . . ? C22A C21A N2A 122.3(19) . . ? C22A C21A H21A 106.7 . . ? N2A C21A H21A 106.7 . . ? C22A C21A H21B 106.8 . . ? N2A C21A H21B 106.8 . . ? H21A C21A H21B 106.6 . . ? C21A C22A H22A 109.5 . . ? C21A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C21A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C1 N2B C21B 122.6(13) . . ? C1 N2B H2B 118.7 . . ? C21B N2B H2B 118.7 . . ? C22B C21B N2B 130(2) . . ? C22B C21B H21C 104.7 . . ? N2B C21B H21C 104.7 . . ? C22B C21B H21D 104.7 . . ? N2B C21B H21D 104.7 . . ? H21C C21B H21D 105.7 . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Ag1 S1 C1 18.4(2) 3_565 . . . ? S1 Ag1 S1 C1 -107.9(2) 2_665 . . . ? Br1 Ag1 S1 C1 135.3(2) . . . . ? Ag1 S1 C1 N2A -1.4(11) . . . . ? Ag1 S1 C1 N1 -170.4(6) . . . . ? Ag1 S1 C1 N2B 27.3(9) . . . . ? N2A C1 N1 C11 -160.3(13) . . . . ? N2B C1 N1 C11 170.2(14) . . . . ? S1 C1 N1 C11 10.0(13) . . . . ? C1 N1 C11 C12 -102.9(11) . . . . ? N1 C1 N2A C21A -2.5(19) . . . . ? N2B C1 N2A C21A 117(3) . . . . ? S1 C1 N2A C21A -172.3(11) . . . . ? C1 N2A C21A C22A 177(3) . . . . ? N2A C1 N2B C21B -57.9(19) . . . . ? N1 C1 N2B C21B 16.4(19) . . . . ? S1 C1 N2B C21B 178.3(11) . . . . ? C1 N2B C21B C22B 135(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 N1 H1 S1 0.86 2.78 3.570(6) 153.9 6_554 N2B H2B S1 0.86 2.96 3.494(16) 122.1 3_565 N2A H2A S1 0.86 2.69 3.496(10) 155.8 3_565 data_agbreu _database_code_depnum_ccdc_archive 'CCDC 751798' _audit_creation_date 2007-01-04T12:44:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C9 H24 Ag Br N6 S3' _chemical_formula_moiety 'C9 H24 Ag Br N6 S3' _chemical_formula_weight 500.3 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/m_1 _symmetry_space_group_name_Hall -p_2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.2951(9) _cell_length_b 15.502(2) _cell_length_c 8.2810(10) _cell_angle_alpha 90 _cell_angle_beta 91.489(3) _cell_angle_gamma 90 _cell_volume 936.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7361 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 36.4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.545 _exptl_crystal_description tablet _exptl_crystal_size_max .17 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .40 _exptl_absorpt_correction_T_max .62 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .040 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_number 19407 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 37.63 _diffrn_reflns_theta_full 37 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5076 _reflns_number_gt 4095 _reflns_threshold_expression I>2sigma(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_molecular_graphics xtal _computing_publication_material WinGX _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^)+(0.0273P)^2^] 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 5076 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.909 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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 -0.165215(17) 0.25 0.131036(16) 0.01836(3) Uani 1 2 d S . . Br1 Br 0.09570(2) 0.25 -0.10313(2) 0.01646(4) Uani 1 2 d S . . S1 S -0.00190(6) 0.25 0.41092(5) 0.01997(8) Uani 1 2 d S . . C1 C 0.2332(2) 0.25 0.3995(2) 0.0169(3) Uani 1 2 d S . . N11 N 0.3350(2) 0.25 0.53489(18) 0.0217(3) Uani 1 2 d S . . H11 H 0.278 0.25 0.6272 0.026 Uiso 1 2 calc SR . . N12 N 0.3161(2) 0.25 0.25903(19) 0.0259(3) Uani 1 2 d S . . H12A H 0.4366 0.25 0.2565 0.031 Uiso 1 2 calc SR . . H12B H 0.2506 0.25 0.1683 0.031 Uiso 1 2 calc SR . . C11 C 0.5358(2) 0.25 0.5407(2) 0.0258(4) Uani 1 2 d S . . H11A H 0.5818 0.3017 0.4845 0.031 Uiso 0.5 1 calc PR . . H11B H 0.5818 0.1983 0.4845 0.031 Uiso 0.5 1 calc PR . . C12 C 0.6058(3) 0.25 0.7132(3) 0.0417(6) Uani 1 2 d S . . H12C H 0.5682 0.3034 0.7662 0.063 Uiso 0.5 1 calc PR . . H12D H 0.7399 0.2461 0.7156 0.063 Uiso 0.5 1 calc PR . . H12E H 0.5548 0.2004 0.7702 0.063 Uiso 0.5 1 calc PR . . S2 S -0.35174(4) 0.386805(19) 0.10482(4) 0.02177(6) Uani 1 1 d . . . C2 C -0.20916(17) 0.47118(8) 0.15747(16) 0.0196(2) Uani 1 1 d . . . N21 N -0.04988(15) 0.45960(7) 0.23535(14) 0.0215(2) Uani 1 1 d . . . H21 H -0.0189 0.4065 0.2622 0.026 Uiso 1 1 calc R . . N22 N -0.26074(18) 0.55078(7) 0.11692(17) 0.0303(3) Uani 1 1 d . . . H22A H -0.1895 0.5949 0.1418 0.036 Uiso 1 1 calc R . . H22B H -0.3661 0.5593 0.0652 0.036 Uiso 1 1 calc R . . C21 C 0.07844(18) 0.52917(9) 0.27984(18) 0.0248(3) Uani 1 1 d . . . H21A H 0.0188 0.5697 0.3545 0.03 Uiso 1 1 calc R . . H21B H 0.1116 0.5616 0.1818 0.03 Uiso 1 1 calc R . . C22 C 0.2506(2) 0.49237(9) 0.3607(2) 0.0309(3) Uani 1 1 d . . . H22C H 0.217 0.4583 0.4551 0.046 Uiso 1 1 calc R . . H22D H 0.3318 0.5397 0.395 0.046 Uiso 1 1 calc R . . H22E H 0.314 0.4554 0.2841 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01825(6) 0.01533(5) 0.02145(6) 0 -0.00046(4) 0 Br1 0.01875(7) 0.01555(7) 0.01510(7) 0 0.00103(5) 0 S1 0.01353(16) 0.0300(2) 0.01636(18) 0 -0.00022(13) 0 C1 0.0155(7) 0.0196(7) 0.0155(7) 0 -0.0010(5) 0 N11 0.0148(6) 0.0375(8) 0.0129(6) 0 0.0003(5) 0 N12 0.0146(6) 0.0476(10) 0.0156(7) 0 0.0005(5) 0 C11 0.0145(7) 0.0426(11) 0.0200(8) 0 -0.0019(6) 0 C12 0.0218(9) 0.0807(19) 0.0223(10) 0 -0.0071(8) 0 S2 0.01680(12) 0.01413(12) 0.03416(17) 0.00159(11) -0.00351(11) 0.00028(9) C2 0.0197(5) 0.0163(5) 0.0230(6) -0.0001(4) 0.0029(4) 0.0001(4) N21 0.0195(5) 0.0154(4) 0.0295(6) 0.0004(4) -0.0020(4) -0.0014(3) N22 0.0281(6) 0.0149(5) 0.0472(8) 0.0029(5) -0.0105(5) -0.0009(4) C21 0.0231(6) 0.0205(5) 0.0308(7) -0.0033(5) 0.0003(5) -0.0047(4) C22 0.0229(6) 0.0313(7) 0.0383(8) -0.0043(6) -0.0044(6) -0.0035(5) #----------------------------------------------------------------------------# # 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 2.5261(4) 4_565 ? Ag1 S2 2.5260(4) . ? Ag1 S1 2.5784(5) . ? Ag1 Br1 2.7523(3) . ? S1 C1 1.7202(17) . ? C1 N12 1.325(2) . ? C1 N11 1.329(2) . ? N11 C11 1.464(2) . ? N11 H11 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? C11 C12 1.505(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12C 0.98 . ? C12 H12D 0.98 . ? C12 H12E 0.98 . ? S2 C2 1.7202(13) . ? C2 N21 1.3264(16) . ? C2 N22 1.3306(16) . ? N21 C21 1.4688(16) . ? N21 H21 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? C21 C22 1.519(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22C 0.98 . ? C22 H22D 0.98 . ? C22 H22E 0.98 . ? 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 S2 114.185(17) 4_565 . ? S2 Ag1 S1 108.214(10) 4_565 . ? S2 Ag1 S1 108.214(10) . . ? S2 Ag1 Br1 108.681(10) 4_565 . ? S2 Ag1 Br1 108.681(10) . . ? S1 Ag1 Br1 108.752(14) . . ? C1 S1 Ag1 112.87(6) . . ? N12 C1 N11 118.88(15) . . ? N12 C1 S1 121.79(13) . . ? N11 C1 S1 119.33(13) . . ? C1 N11 C11 124.36(15) . . ? C1 N11 H11 117.8 . . ? C11 N11 H11 117.8 . . ? C1 N12 H12A 120 . . ? C1 N12 H12B 120 . . ? H12A N12 H12B 120 . . ? N11 C11 C12 110.22(16) . . ? N11 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N11 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? C11 C12 H12E 109.5 . . ? H12C C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? C2 S2 Ag1 107.20(4) . . ? N21 C2 N22 119.12(11) . . ? N21 C2 S2 122.46(9) . . ? N22 C2 S2 118.42(10) . . ? C2 N21 C21 124.55(11) . . ? C2 N21 H21 117.7 . . ? C21 N21 H21 117.7 . . ? C2 N22 H22A 120 . . ? C2 N22 H22B 120 . . ? H22A N22 H22B 120 . . ? N21 C21 C22 110.42(11) . . ? N21 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N21 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22D 109.5 . . ? H22C C22 H22D 109.5 . . ? C21 C22 H22E 109.5 . . ? H22C C22 H22E 109.5 . . ? H22D C22 H22E 109.5 . . ? _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. ; data_agettum _database_code_depnum_ccdc_archive 'CCDC 751799' _audit_creation_date 2009-09-10T19:31:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; tris(N-ethylthiourea)chlorosilver(I) ; _chemical_formula_moiety 'C9 H24 Ag Cl N6 S3' _chemical_formula_sum 'C9 H24 Ag Cl N6 S3' _chemical_formula_weight 455.84 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3489(1) _cell_length_b 15.3315(1) _cell_length_c 8.1959(1) _cell_angle_alpha 90 _cell_angle_beta 91.467(1) _cell_angle_gamma 90 _cell_volume 923.127(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 30.49 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ' SADABS; Sheldrick, 1996' _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.73 #----------------------------------------------------------------------------# # 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 diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_unetI/netI 0.0184 _diffrn_reflns_number 6843 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.938 _reflns_number_total 2732 _reflns_number_gt 2511 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. ; _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^)+(0.0297P)^2^+0.1355P] 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 2732 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.023 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.295 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 -0.160040(19) 0.25 0.126174(19) 0.03491(5) Uani 1 2 d S . . Cl1 Cl 0.10126(6) 0.25 -0.09675(5) 0.03188(9) Uani 1 2 d S . . S1 S -0.00028(6) 0.25 0.41167(6) 0.03523(10) Uani 1 2 d S . . C1 C 0.2322(2) 0.25 0.4004(2) 0.0292(3) Uani 1 2 d S . . N11 N 0.3328(2) 0.25 0.5379(2) 0.0379(4) Uani 1 2 d S . . H11 H 0.2773 0.25 0.629 0.045 Uiso 1 2 calc SR . . N12 N 0.3149(2) 0.25 0.2586(2) 0.0452(5) Uani 1 2 d S . . H12A H 0.4318 0.25 0.2564 0.054 Uiso 1 2 calc SR . . H12B H 0.2517 0.25 0.1689 0.054 Uiso 1 2 calc SR . . C11 C 0.5325(3) 0.25 0.5434(3) 0.0463(5) Uani 1 2 d S . . H11A H 0.5769 0.3012 0.4874 0.056 Uiso 0.5 1 calc PR . . H11B H 0.5769 0.1988 0.4874 0.056 Uiso 0.5 1 calc PR . . C12 C 0.6037(3) 0.25 0.7153(3) 0.0596(7) Uani 1 2 d S . . H12C H 0.5763 0.1952 0.7656 0.089 Uiso 0.5 1 calc PR . . H12D H 0.5475 0.2963 0.7746 0.089 Uiso 0.5 1 calc PR . . H12E H 0.7331 0.2585 0.7165 0.089 Uiso 0.5 1 calc PR . . S2 S -0.34638(4) 0.38863(2) 0.10466(5) 0.03792(9) Uani 1 1 d . . . C2 C -0.20663(18) 0.47503(8) 0.15676(17) 0.0309(2) Uani 1 1 d . . . N21 N -0.04761(16) 0.46353(8) 0.23347(16) 0.0365(2) Uani 1 1 d . . . H21 H -0.0159 0.411 0.2573 0.044 Uiso 1 1 calc R . . N22 N -0.2611(2) 0.55503(8) 0.1186(2) 0.0498(3) Uani 1 1 d . . . H22A H -0.1934 0.599 0.1436 0.06 Uiso 1 1 calc R . . H22B H -0.3642 0.5629 0.0687 0.06 Uiso 1 1 calc R . . C21 C 0.0783(2) 0.53384(10) 0.2808(2) 0.0415(3) Uani 1 1 d . . . H21A H 0.0201 0.5727 0.3569 0.05 Uiso 1 1 calc R . . H21B H 0.1093 0.5674 0.1851 0.05 Uiso 1 1 calc R . . C22 C 0.2504(2) 0.49615(13) 0.3597(3) 0.0551(4) Uani 1 1 d . . . H22C H 0.2189 0.4611 0.4519 0.083 Uiso 1 1 calc R . . H22D H 0.3289 0.5428 0.3953 0.083 Uiso 1 1 calc R . . H22E H 0.3119 0.4607 0.2818 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03449(8) 0.02573(8) 0.04427(9) 0 -0.00389(6) 0 Cl1 0.0375(2) 0.02654(19) 0.0317(2) 0 0.00223(16) 0 S1 0.02403(19) 0.0516(3) 0.0299(2) 0 -0.00122(16) 0 C1 0.0264(8) 0.0328(8) 0.0283(8) 0 -0.0032(6) 0 N11 0.0273(7) 0.0593(11) 0.0269(7) 0 -0.0032(6) 0 N12 0.0269(7) 0.0811(15) 0.0276(8) 0 0.0001(6) 0 C11 0.0285(9) 0.0735(16) 0.0365(10) 0 -0.0058(8) 0 C12 0.0399(12) 0.097(2) 0.0415(12) 0 -0.0128(10) 0 S2 0.02887(15) 0.02278(15) 0.0616(2) 0.00217(14) -0.00781(14) 0.00102(11) C2 0.0317(6) 0.0239(6) 0.0374(6) -0.0008(5) 0.0041(5) 0.0000(4) N21 0.0334(5) 0.0247(5) 0.0510(7) -0.0010(5) -0.0044(5) -0.0016(4) N22 0.0472(7) 0.0235(6) 0.0779(10) 0.0050(6) -0.0153(7) -0.0008(5) C21 0.0401(7) 0.0332(7) 0.0511(8) -0.0054(6) 0.0005(6) -0.0082(6) C22 0.0389(8) 0.0564(11) 0.0696(12) -0.0072(9) -0.0073(8) -0.0086(7) #----------------------------------------------------------------------------# # 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 2.5320(3) 4_565 ? Ag1 S2 2.5320(3) . ? Ag1 S1 2.5909(5) . ? Ag1 Cl1 2.6843(5) . ? S1 C1 1.7131(18) . ? C1 N12 1.325(2) . ? C1 N11 1.332(2) . ? N11 C11 1.467(3) . ? N11 H11 0.86 . ? N12 H12A 0.86 . ? N12 H12B 0.86 . ? C11 C12 1.490(3) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 H12C 0.96 . ? C12 H12D 0.96 . ? C12 H12E 0.96 . ? S2 C2 1.7232(14) . ? C2 N21 1.3245(18) . ? C2 N22 1.3253(18) . ? N21 C21 1.4664(18) . ? N21 H21 0.86 . ? N22 H22A 0.86 . ? N22 H22B 0.86 . ? C21 C22 1.520(2) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22C 0.96 . ? C22 H22D 0.96 . ? C22 H22E 0.96 . ? 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 S2 114.153(16) 4_565 . ? S2 Ag1 S1 107.136(11) 4_565 . ? S2 Ag1 S1 107.136(11) . . ? S2 Ag1 Cl1 110.344(11) 4_565 . ? S2 Ag1 Cl1 110.344(11) . . ? S1 Ag1 Cl1 107.408(15) . . ? C1 S1 Ag1 112.37(6) . . ? N12 C1 N11 118.98(17) . . ? N12 C1 S1 121.88(14) . . ? N11 C1 S1 119.14(14) . . ? C1 N11 C11 124.01(17) . . ? C1 N11 H11 118 . . ? C11 N11 H11 118 . . ? C1 N12 H12A 120 . . ? C1 N12 H12B 120 . . ? H12A N12 H12B 120 . . ? N11 C11 C12 110.84(19) . . ? N11 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? C11 C12 H12E 109.5 . . ? H12C C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? C2 S2 Ag1 108.07(5) . . ? N21 C2 N22 119.53(13) . . ? N21 C2 S2 121.89(10) . . ? N22 C2 S2 118.58(11) . . ? C2 N21 C21 124.81(12) . . ? C2 N21 H21 117.6 . . ? C21 N21 H21 117.6 . . ? C2 N22 H22A 120 . . ? C2 N22 H22B 120 . . ? H22A N22 H22B 120 . . ? N21 C21 C22 110.22(13) . . ? N21 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N21 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22D 109.5 . . ? H22C C22 H22D 109.5 . . ? C21 C22 H22E 109.5 . . ? H22C C22 H22E 109.5 . . ? H22D C22 H22E 109.5 . . ? 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 N11 H11 Cl1 0.86 2.62 3.4819(17) 178.7 1_556 N12 H12B Cl1 0.86 2.42 3.2733(18) 174.5 . N22 H22A Cl1 0.86 2.44 3.2184(13) 150 3_565 _chemical_name_common tris(N-ethylthiourea)chlorosilver(i) data_gb0910 _database_code_depnum_ccdc_archive 'CCDC 751800' _audit_creation_date 2009-07-02T10:07:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C4 H16 Ag2 Cl2 N8 S4' _chemical_formula_moiety 'C4 H16 Ag2 Cl2 N8 S4' _chemical_formula_weight 591.13 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.8920(2) _cell_length_b 8.2179(3) _cell_length_c 36.5632(15) _cell_angle_alpha 90 _cell_angle_beta 92.749(4) _cell_angle_gamma 90 _cell_volume 1768.35(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8140 _cell_measurement_theta_min 2.7887 _cell_measurement_theta_max 34.5303 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.055 _exptl_crystal_density_diffrn 2.22 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.99 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.86 #----------------------------------------------------------------------------# # 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 0.0497178684 _diffrn_orient_matrix_ub_12 0.0251377125 _diffrn_orient_matrix_ub_13 -0.0163403129 _diffrn_orient_matrix_ub_21 0.0187946663 _diffrn_orient_matrix_ub_22 0.0784928485 _diffrn_orient_matrix_ub_23 0.0075718288 _diffrn_orient_matrix_ub_31 0.1080601542 _diffrn_orient_matrix_ub_32 -0.0252176468 _diffrn_orient_matrix_ub_33 0.0071902718 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_number 25012 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 34.65 _diffrn_reflns_theta_full 34 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.966 _reflns_number_total 7314 _reflns_number_gt 5759 _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. ; _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^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7314 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.213 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.163 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 0.71035(3) 0.69239(3) 0.092644(6) 0.01409(5) Uani 1 1 d . . . Ag2 Ag 0.41533(4) 0.75519(3) 0.158084(6) 0.01510(5) Uani 1 1 d . . . Cl1 Cl 0.85067(10) 0.82901(8) 0.026206(17) 0.01294(11) Uani 1 1 d . . . Cl2 Cl 0.04504(10) 0.98670(8) 0.184710(17) 0.01282(11) Uani 1 1 d . . . S1 S 0.59605(11) 0.63598(10) 0.213473(19) 0.01773(14) Uani 1 1 d . . . C1 C 0.3866(4) 0.6139(3) 0.24439(7) 0.0137(5) Uani 1 1 d . . . N11 N 0.4425(4) 0.5586(3) 0.27760(7) 0.0214(5) Uani 1 1 d . . . H11A H 0.3374 0.5465 0.2937 0.026 Uiso 1 1 calc R . . H11B H 0.5848 0.5338 0.2836 0.026 Uiso 1 1 calc R . . N12 N 0.1698(4) 0.6496(3) 0.23663(7) 0.0202(5) Uani 1 1 d . . . H12A H 0.0687 0.6362 0.2533 0.024 Uiso 1 1 calc R . . H12B H 0.1271 0.6866 0.2148 0.024 Uiso 1 1 calc R . . S2 S 0.57092(10) 0.96458(8) 0.116359(17) 0.01003(11) Uani 1 1 d . . . C2 C 0.3430(4) 0.9972(3) 0.08480(7) 0.0102(4) Uani 1 1 d . . . N21 N 0.1352(4) 1.0156(3) 0.09642(6) 0.0155(4) Uani 1 1 d . . . H21A H 0.021 1.0347 0.0806 0.019 Uiso 1 1 calc R . . H21B H 0.1113 1.0087 0.1199 0.019 Uiso 1 1 calc R . . N22 N 0.3802(4) 1.0073(3) 0.04974(6) 0.0139(4) Uani 1 1 d . . . H22A H 0.2667 1.0264 0.0338 0.017 Uiso 1 1 calc R . . H22B H 0.5188 0.9949 0.0422 0.017 Uiso 1 1 calc R . . S3 S 1.08522(11) 0.60314(8) 0.126468(19) 0.01530(13) Uani 1 1 d . . . C3 C 1.0562(5) 0.4150(3) 0.14711(7) 0.0131(5) Uani 1 1 d . . . N31 N 0.8714(4) 0.3266(3) 0.14049(7) 0.0162(5) Uani 1 1 d . . . H31A H 0.8594 0.2301 0.1506 0.019 Uiso 1 1 calc R . . H31B H 0.7602 0.3644 0.126 0.019 Uiso 1 1 calc R . . N32 N 1.2220(4) 0.3559(3) 0.16911(7) 0.0212(5) Uani 1 1 d . . . H32A H 1.2079 0.2592 0.1791 0.025 Uiso 1 1 calc R . . H32B H 1.346 0.4135 0.1737 0.025 Uiso 1 1 calc R . . S4 S 0.52741(11) 0.43913(8) 0.066547(19) 0.01336(12) Uani 1 1 d . . . C4 C 0.7299(4) 0.3718(3) 0.03725(7) 0.0121(5) Uani 1 1 d . . . N41 N 0.6646(4) 0.2982(3) 0.00634(6) 0.0175(5) Uani 1 1 d . . . H41A H 0.7668 0.2616 -0.0084 0.021 Uiso 1 1 calc R . . H41B H 0.519 0.2859 0.0005 0.021 Uiso 1 1 calc R . . N42 N 0.9520(4) 0.3872(3) 0.04476(7) 0.0177(5) Uani 1 1 d . . . H42A H 1.0495 0.3492 0.0294 0.021 Uiso 1 1 calc R . . H42B H 1.0015 0.4355 0.0651 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01512(9) 0.01213(9) 0.01495(9) -0.00132(7) -0.00003(7) 0.00154(8) Ag2 0.01651(9) 0.01687(10) 0.01171(9) 0.00362(7) -0.00167(7) -0.00369(8) Cl1 0.0108(3) 0.0177(3) 0.0103(3) 0.0000(2) 0.0008(2) 0.0001(2) Cl2 0.0133(3) 0.0138(3) 0.0114(3) 0.0007(2) 0.0007(2) 0.0001(2) S1 0.0101(3) 0.0284(4) 0.0146(3) 0.0080(3) -0.0001(2) -0.0002(3) C1 0.0135(11) 0.0151(12) 0.0123(12) 0.0040(9) -0.0014(9) 0.0000(10) N11 0.0143(11) 0.0333(14) 0.0167(12) 0.0120(10) 0.0005(9) 0.0033(10) N12 0.0109(10) 0.0320(14) 0.0177(12) 0.0093(10) 0.0013(8) 0.0021(10) S2 0.0089(3) 0.0111(3) 0.0099(3) -0.0002(2) -0.0003(2) -0.0006(2) C2 0.0110(10) 0.0081(10) 0.0115(11) -0.0011(8) -0.0001(8) -0.0003(9) N21 0.0100(10) 0.0224(12) 0.0139(11) 0.0000(9) -0.0006(8) 0.0037(9) N22 0.0132(10) 0.0198(11) 0.0085(10) 0.0012(8) -0.0006(8) 0.0019(9) S3 0.0152(3) 0.0118(3) 0.0183(3) 0.0025(2) -0.0056(2) -0.0022(2) C3 0.0159(12) 0.0092(11) 0.0141(12) -0.0014(9) -0.0001(9) -0.0007(9) N31 0.0157(10) 0.0118(11) 0.0208(12) 0.0022(9) -0.0019(9) -0.0023(9) N32 0.0214(12) 0.0125(11) 0.0287(14) 0.0053(10) -0.0109(10) -0.0015(10) S4 0.0100(3) 0.0153(3) 0.0149(3) -0.0034(2) 0.0015(2) -0.0005(2) C4 0.0120(11) 0.0109(11) 0.0134(12) -0.0006(9) -0.0014(9) -0.0011(9) N41 0.0133(10) 0.0256(12) 0.0135(11) -0.0062(9) -0.0008(8) 0.0012(10) N42 0.0096(10) 0.0245(12) 0.0190(12) -0.0079(10) 0.0012(8) 0.0003(9) #----------------------------------------------------------------------------# # 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 S4 2.5111(7) . ? Ag1 S2 2.5492(7) . ? Ag1 S3 2.5853(7) . ? Ag1 Cl1 2.8351(7) . ? Ag1 Ag2 3.0679(3) . ? Ag2 Cl2 3.0873(7) . ? Ag2 S1 2.4471(7) . ? Ag2 S2 2.5026(7) . ? Ag2 S3 2.5426(7) 1_455 ? S1 C1 1.723(3) . ? C1 N11 1.323(3) . ? C1 N12 1.328(3) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.749(3) . ? C2 N22 1.314(3) . ? C2 N21 1.324(3) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.733(3) . ? S3 Ag2 2.5426(7) 1_655 ? C3 N31 1.322(3) . ? C3 N32 1.327(3) . ? N31 H31A 0.88 . ? N31 H31B 0.88 . ? N32 H32A 0.88 . ? N32 H32B 0.88 . ? S4 C4 1.732(3) . ? C4 N41 1.323(3) . ? C4 N42 1.331(3) . ? N41 H41A 0.88 . ? N41 H41B 0.88 . ? N42 H42A 0.88 . ? N42 H42B 0.88 . ? 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 S4 Ag1 S2 135.81(2) . . ? S4 Ag1 S3 106.74(2) . . ? S2 Ag1 S3 111.60(2) . . ? S4 Ag1 Cl1 98.06(2) . . ? S2 Ag1 Cl1 93.21(2) . . ? S3 Ag1 Cl1 104.16(2) . . ? Cl2 Ag2 S1 105.77(2) . . ? Cl2 Ag2 S2 93.07(2) . . ? Cl2 Ag2 S3 84.81(2) . 1_455 ? S1 Ag2 S2 128.48(2) . . ? S1 Ag2 S3 118.20(2) . 1_455 ? S2 Ag2 S3 110.81(2) . 1_455 ? C1 S1 Ag2 106.76(9) . . ? N11 C1 N12 117.8(3) . . ? N11 C1 S1 118.9(2) . . ? N12 C1 S1 123.3(2) . . ? 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 Ag2 102.44(9) . . ? C2 S2 Ag1 99.20(9) . . ? Ag2 S2 Ag1 74.781(19) . . ? N22 C2 N21 120.4(2) . . ? N22 C2 S2 119.65(19) . . ? N21 C2 S2 119.9(2) . . ? 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 Ag2 109.26(9) . 1_655 ? C3 S3 Ag1 111.20(9) . . ? Ag2 S3 Ag1 134.06(3) 1_655 . ? N31 C3 N32 119.1(2) . . ? N31 C3 S3 120.5(2) . . ? N32 C3 S3 120.4(2) . . ? C3 N31 H31A 120 . . ? C3 N31 H31B 120 . . ? H31A N31 H31B 120 . . ? C3 N32 H32A 120 . . ? C3 N32 H32B 120 . . ? H32A N32 H32B 120 . . ? C4 S4 Ag1 101.77(9) . . ? N41 C4 N42 117.6(2) . . ? N41 C4 S4 119.6(2) . . ? N42 C4 S4 122.8(2) . . ? C4 N41 H41A 120 . . ? C4 N41 H41B 120 . . ? H41A N41 H41B 120 . . ? C4 N42 H42A 120 . . ? C4 N42 H42B 120 . . ? H42A N42 H42B 120 . . ? 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 N11 H11A Cl2 0.88 2.47 3.299(3) 156.5 2_545 N11 H11B Cl2 0.88 2.45 3.311(2) 165.8 2_645 N12 H12A Cl2 0.88 2.69 3.466(3) 147.8 2_545 N12 H12B Cl2 0.88 2.73 3.419(3) 135.6 . N21 H21A Cl1 0.88 2.76 3.368(2) 127.1 1_455 N21 H21B Cl2 0.88 2.43 3.305(2) 179.4 . N22 H22A Cl1 0.88 2.56 3.318(2) 144.6 3_675 N22 H22B Cl1 0.88 2.48 3.286(2) 153.2 . N31 H31A Cl2 0.88 2.57 3.363(2) 149.8 1_645 N31 H31B S4 0.88 2.59 3.427(2) 160.1 . N32 H32A Cl2 0.88 2.45 3.267(3) 155 1_645 N32 H32B S1 0.88 2.72 3.527(3) 152.4 1_655 N41 H41A Cl1 0.88 2.49 3.315(2) 156.5 3_765 N41 H41B Cl1 0.88 2.53 3.373(2) 161.6 3_665 N42 H42A Cl1 0.88 2.6 3.396(2) 151.6 3_765 N42 H42B S3 0.88 2.66 3.530(2) 170.8 . data_gb0912 _database_code_depnum_ccdc_archive 'CCDC 751801' _audit_creation_date 2009-07-01T20:04:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C4 H16 Ag2 Br2 N8 S4' _chemical_formula_moiety 'C4 H16 Ag2 Br2 N8 S4' _chemical_formula_weight 680.05 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.9595(4) _cell_length_b 8.2330(5) _cell_length_c 37.778(3) _cell_angle_alpha 90 _cell_angle_beta 92.261(7) _cell_angle_gamma 90 _cell_volume 1852.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6015 _cell_measurement_theta_min 2.9493 _cell_measurement_theta_max 30.9091 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.045 _exptl_crystal_density_diffrn 2.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.881 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.89 #----------------------------------------------------------------------------# # 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 0.0380947821 _diffrn_orient_matrix_ub_12 0.0164209169 _diffrn_orient_matrix_ub_13 -0.017174522 _diffrn_orient_matrix_ub_21 0.0286847484 _diffrn_orient_matrix_ub_22 0.0803286286 _diffrn_orient_matrix_ub_23 0.0053236348 _diffrn_orient_matrix_ub_31 0.1095233402 _diffrn_orient_matrix_ub_32 -0.0267709361 _diffrn_orient_matrix_ub_33 0.0053728406 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.0676 _diffrn_reflns_number 19813 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 31.05 _diffrn_reflns_theta_full 30.5 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 5690 _reflns_number_gt 4126 _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. ; _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^)+(0.0154P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5690 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.04 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.17 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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 0.70230(4) 0.69366(3) 0.093183(7) 0.01489(6) Uani 1 1 d . . . Ag2 Ag 0.39639(4) 0.75861(3) 0.156882(7) 0.01564(6) Uani 1 1 d . . . Br1 Br 0.85583(5) 0.82471(4) 0.026709(9) 0.01321(7) Uani 1 1 d . . . Br2 Br 0.02800(5) 0.97593(4) 0.185574(9) 0.01320(7) Uani 1 1 d . . . S1 S 0.59047(14) 0.62227(11) 0.20741(2) 0.01705(19) Uani 1 1 d . . . C1 C 0.3948(5) 0.5936(4) 0.23894(9) 0.0162(7) Uani 1 1 d . . . N11 N 0.4616(5) 0.5330(4) 0.27002(8) 0.0291(8) Uani 1 1 d . . . H11A H 0.3633 0.5157 0.2864 0.035 Uiso 1 1 calc R . . H11B H 0.6043 0.51 0.2743 0.035 Uiso 1 1 calc R . . N12 N 0.1792(5) 0.6259(3) 0.23387(8) 0.0198(7) Uani 1 1 d . . . H12A H 0.0857 0.607 0.2508 0.024 Uiso 1 1 calc R . . H12B H 0.1288 0.6663 0.2135 0.024 Uiso 1 1 calc R . . S2 S 0.56044(13) 0.96413(10) 0.11618(2) 0.01085(16) Uani 1 1 d . . . C2 C 0.3373(5) 1.0003(4) 0.08547(9) 0.0103(7) Uani 1 1 d . . . N21 N 0.1323(4) 1.0233(3) 0.09674(7) 0.0162(6) Uani 1 1 d . . . H21A H 0.0211 1.0451 0.0815 0.019 Uiso 1 1 calc R . . H21B H 0.1073 1.0167 0.1195 0.019 Uiso 1 1 calc R . . N22 N 0.3768(4) 1.0099(3) 0.05155(7) 0.0141(6) Uani 1 1 d . . . H22A H 0.2664 1.0317 0.0361 0.017 Uiso 1 1 calc R . . H22B H 0.5136 0.9945 0.0443 0.017 Uiso 1 1 calc R . . S3 S 1.07639(14) 0.60134(10) 0.12450(2) 0.01420(18) Uani 1 1 d . . . C3 C 1.0456(5) 0.4150(4) 0.14473(9) 0.0137(7) Uani 1 1 d . . . N31 N 0.8592(5) 0.3284(3) 0.13900(8) 0.0176(6) Uani 1 1 d . . . H31A H 0.846 0.2324 0.1489 0.021 Uiso 1 1 calc R . . H31B H 0.7491 0.3671 0.1253 0.021 Uiso 1 1 calc R . . N32 N 1.2084(5) 0.3552(3) 0.16535(8) 0.0239(7) Uani 1 1 d . . . H32A H 1.1932 0.259 0.1752 0.029 Uiso 1 1 calc R . . H32B H 1.3325 0.4113 0.1693 0.029 Uiso 1 1 calc R . . S4 S 0.51784(13) 0.44117(10) 0.06767(2) 0.01389(18) Uani 1 1 d . . . C4 C 0.7187(5) 0.3750(4) 0.03909(9) 0.0141(7) Uani 1 1 d . . . N41 N 0.6555(5) 0.3105(3) 0.00849(7) 0.0180(6) Uani 1 1 d . . . H41A H 0.7568 0.2738 -0.0058 0.022 Uiso 1 1 calc R . . H41B H 0.5118 0.3041 0.0023 0.022 Uiso 1 1 calc R . . N42 N 0.9380(4) 0.3819(3) 0.04719(8) 0.0176(6) Uani 1 1 d . . . H42A H 1.0349 0.344 0.0323 0.021 Uiso 1 1 calc R . . H42B H 0.9861 0.4244 0.0675 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01632(13) .01290(13) .01538(14) -0.00112(10) -0.00026(10) 0.00168(10) Ag2 0.01700(13) .01710(14) .01261(13) 0.00405(10) -0.00210(10) -0.00275(10) Br1 0.01116(16) .01815(18) .01030(17) -0.00014(13) 0.00025(13) -0.00059(13) Br2 0.01429(17) .01371(17) .01161(17) 0.00059(12) 0.00066(13) 0.00042(12) S1 0.0109(4) 0.0246(5) 0.0155(5) 0.0066(4) -0.0009(3) -0.0009(3) C1 0.0120(17) 0.0161(18) 0.020(2) 0.0039(14) -0.0041(15) 0.0000(13) N11 0.0159(16) 0.048(2) 0.0233(19) 0.0218(16) 0.0019(14) 0.0033(15) N12 0.0131(15) 0.0281(17) 0.0183(17) 0.0106(13) 0.0005(13) 0.0005(12) S2 0.0103(4) 0.0121(4) 0.0101(4) 0.0003(3) -0.0003(3) -0.0012(3) C2 0.0113(16) 0.0068(16) 0.0124(17) 0.0002(12) -0.0025(13) -0.0005(11) N21 0.0100(14) 0.0274(17) 0.0111(15) 0.0008(12) -0.0019(12) 0.0061(11) N22 0.0138(15) 0.0217(16) 0.0066(14) 0.0035(11) -0.0019(11) 0.0029(11) S3 0.0144(4) 0.0105(4) 0.0172(5) 0.0015(3) -0.0056(3) -0.0022(3) C3 0.0163(18) 0.0136(17) 0.0113(18) -0.0040(13) 0.0003(14) -0.0005(13) N31 0.0174(15) 0.0131(15) 0.0220(17) 0.0031(12) -0.0038(13) -0.0027(11) N32 0.0241(17) 0.0123(16) 0.034(2) 0.0045(13) -0.0116(15) -0.0045(12) S4 0.0100(4) 0.0168(4) 0.0149(5) -0.0034(3) 0.0012(3) -0.0010(3) C4 0.0146(17) 0.0114(17) 0.0160(19) -0.0005(13) -0.0028(14) -0.0006(13) N41 0.0099(14) 0.0270(17) 0.0169(17) -0.0087(13) -0.0014(12) 0.0019(12) N42 0.0088(14) 0.0270(17) 0.0168(17) -0.0069(12) 0.0001(12) 0.0008(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 S4 2.5249(9) . ? Ag1 S2 2.5467(8) . ? Ag1 S3 2.5960(9) . ? Ag1 Br1 2.9136(5) . ? Ag1 Ag2 3.1220(4) . ? Ag2 S1 2.4632(9) . ? Ag2 S2 2.5105(8) . ? Ag2 S3 2.5741(9) 1_455 ? Ag2 Br2 3.0633(4) . ? S1 C1 1.716(4) . ? C1 N12 1.319(4) . ? C1 N11 1.323(4) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.755(3) . ? C2 N22 1.314(4) . ? C2 N21 1.323(4) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.727(3) . ? S3 Ag2 2.5741(8) 1_655 ? C3 N32 1.316(4) . ? C3 N31 1.331(4) . ? N31 H31A 0.88 . ? N31 H31B 0.88 . ? N32 H32A 0.88 . ? N32 H32B 0.88 . ? S4 C4 1.731(3) . ? C4 N41 1.314(4) . ? C4 N42 1.332(4) . ? N41 H41A 0.88 . ? N41 H41B 0.88 . ? N42 H42A 0.88 . ? N42 H42B 0.88 . ? 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 S4 Ag1 S2 134.80(3) . . ? S4 Ag1 S3 106.62(3) . . ? S2 Ag1 S3 113.03(3) . . ? S4 Ag1 Br1 97.04(2) . . ? S2 Ag1 Br1 95.16(2) . . ? S3 Ag1 Br1 102.00(2) . . ? S4 Ag1 Ag2 100.17(2) . . ? S2 Ag1 Ag2 51.356(19) . . ? S3 Ag1 Ag2 102.47(2) . . ? Br1 Ag1 Ag2 144.463(12) . . ? S1 Ag2 S2 126.84(3) . . ? S1 Ag2 S3 117.10(3) . 1_455 ? S2 Ag2 S3 110.30(3) . 1_455 ? S1 Ag2 Br2 108.25(2) . . ? S2 Ag2 Br2 97.18(2) . . ? S3 Ag2 Br2 86.22(2) 1_455 . ? S1 Ag2 Ag1 104.40(2) . . ? S2 Ag2 Ag1 52.40(2) . . ? S3 Ag2 Ag1 89.52(2) 1_455 . ? Br2 Ag2 Ag1 145.209(12) . . ? C1 S1 Ag2 106.83(12) . . ? N12 C1 N11 117.5(3) . . ? N12 C1 S1 123.8(3) . . ? N11 C1 S1 118.7(3) . . ? 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 Ag2 102.48(11) . . ? C2 S2 Ag1 100.14(10) . . ? Ag2 S2 Ag1 76.24(2) . . ? N22 C2 N21 120.5(3) . . ? N22 C2 S2 119.6(2) . . ? N21 C2 S2 119.8(2) . . ? 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 Ag2 109.03(12) . 1_655 ? C3 S3 Ag1 110.95(12) . . ? Ag2 S3 Ag1 132.54(3) 1_655 . ? N32 C3 N31 119.1(3) . . ? N32 C3 S3 120.4(3) . . ? N31 C3 S3 120.4(3) . . ? C3 N31 H31A 120 . . ? C3 N31 H31B 120 . . ? H31A N31 H31B 120 . . ? C3 N32 H32A 120 . . ? C3 N32 H32B 120 . . ? H32A N32 H32B 120 . . ? C4 S4 Ag1 101.29(11) . . ? N41 C4 N42 117.7(3) . . ? N41 C4 S4 119.6(2) . . ? N42 C4 S4 122.7(3) . . ? C4 N41 H41A 120 . . ? C4 N41 H41B 120 . . ? H41A N41 H41B 120 . . ? C4 N42 H42A 120 . . ? C4 N42 H42B 120 . . ? H42A N42 H42B 120 . . ? 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 N11 H11A Br2 0.88 2.62 3.455(3) 158.8 2_545 N11 H11B Br2 0.88 2.63 3.447(3) 155.1 2_645 N12 H12A Br2 0.88 2.74 3.551(3) 153.3 2_545 N12 H12B Br2 0.88 2.81 3.510(3) 136.9 . N21 H21A Br1 0.88 2.9 3.470(3) 124.5 1_455 N21 H21B Br2 0.88 2.58 3.459(3) 176 . N22 H22A Br1 0.88 2.73 3.492(3) 146.3 3_675 N22 H22B Br1 0.88 2.58 3.401(3) 155.5 . N31 H31A Br2 0.88 2.73 3.520(3) 150.7 1_645 N31 H31B S4 0.88 2.6 3.439(3) 159.4 . N32 H32A Br2 0.88 2.57 3.399(3) 158.1 1_645 N32 H32B S1 0.88 2.7 3.501(3) 152.5 1_655 N41 H41A Br1 0.88 2.6 3.434(3) 158.9 3_765 N41 H41B Br1 0.88 2.63 3.460(3) 156.8 3_665 N42 H42A Br1 0.88 2.73 3.531(3) 152.7 3_765 N42 H42B S3 0.88 2.64 3.505(3) 168.3 . data_gb0938 _database_code_depnum_ccdc_archive 'CCDC 751802' _audit_creation_date 2009-08-20T11:56:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C9 H24 Ag I N6 S3' _chemical_formula_moiety 'C9 H24 Ag I N6 S3' _chemical_formula_weight 547.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2473(3) _cell_length_b 16.1800(9) _cell_length_c 16.4537(9) _cell_angle_alpha 90 _cell_angle_beta 95.984(5) _cell_angle_gamma 90 _cell_volume 1918.87(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14850 _cell_measurement_theta_min 2.8054 _cell_measurement_theta_max 37.2181 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.986 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.62 #----------------------------------------------------------------------------# # 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 0.0035232981 _diffrn_orient_matrix_ub_12 -0.0394675276 _diffrn_orient_matrix_ub_13 0.0188283225 _diffrn_orient_matrix_ub_21 -0.0302265458 _diffrn_orient_matrix_ub_22 -0.0186259425 _diffrn_orient_matrix_ub_23 -0.0381549637 _diffrn_orient_matrix_ub_31 0.0936765703 _diffrn_orient_matrix_ub_32 -0.0045125778 _diffrn_orient_matrix_ub_33 -0.0083934892 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_number 41655 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 37.36 _diffrn_reflns_theta_full 36.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 9610 _reflns_number_gt 7211 _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. ; _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^)+(0.0245P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9610 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.352 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.118 #----------------------------------------------------------------------------# # 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' I I -0.4742 1.8119 '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 0.641948(16) 0.709421(7) 0.705410(7) 0.01570(3) Uani 1 1 d . . . I1 I 0.387923(14) 0.705971(6) 0.825578(6) 0.01570(3) Uani 1 1 d . . . S1 S 0.45732(5) 0.71277(2) 0.56041(2) 0.01383(7) Uani 1 1 d . . . C1 C 0.2189(2) 0.71958(9) 0.55818(9) 0.0136(3) Uani 1 1 d . . . N11 N 0.11897(18) 0.72440(9) 0.48639(8) 0.0176(3) Uani 1 1 d . . . H11 H 0.179 0.7203 0.4427 0.021 Uiso 1 1 calc R . . C11 C -0.0827(2) 0.73591(11) 0.47266(10) 0.0202(3) Uani 1 1 d . . . H11A H -0.142 0.7045 0.5146 0.024 Uiso 1 1 calc R . . H11B H -0.1284 0.713 0.4185 0.024 Uiso 1 1 calc R . . C12 C -0.1407(2) 0.82655(12) 0.47608(12) 0.0255(4) Uani 1 1 d . . . H12A H -0.0986 0.8493 0.53 0.038 Uiso 1 1 calc R . . H12B H -0.2762 0.8306 0.4665 0.038 Uiso 1 1 calc R . . H12C H -0.0846 0.8578 0.434 0.038 Uiso 1 1 calc R . . N12 N 0.13636(19) 0.71949(9) 0.62619(8) 0.0207(3) Uani 1 1 d . . . H12D H 0.0147 0.7227 0.6237 0.025 Uiso 1 1 calc R . . H12E H 0.2031 0.7163 0.6739 0.025 Uiso 1 1 calc R . . S2 S 0.83392(5) 0.57697(2) 0.70663(3) 0.01913(8) Uani 1 1 d . . . C2 C 0.6867(2) 0.49890(9) 0.67125(10) 0.0155(3) Uani 1 1 d . . . N21 N 0.52109(17) 0.51414(8) 0.63167(8) 0.0160(2) Uani 1 1 d . . . H21 H 0.487 0.5661 0.6252 0.019 Uiso 1 1 calc R . . C21 C 0.3916(2) 0.45057(10) 0.59818(10) 0.0183(3) Uani 1 1 d . . . H21A H 0.3592 0.4137 0.6426 0.022 Uiso 1 1 calc R . . H21B H 0.4503 0.4167 0.5579 0.022 Uiso 1 1 calc R . . C22 C 0.2171(2) 0.49112(11) 0.55717(11) 0.0231(3) Uani 1 1 d . . . H22A H 0.1573 0.5231 0.5976 0.035 Uiso 1 1 calc R . . H22B H 0.1316 0.4484 0.5338 0.035 Uiso 1 1 calc R . . H22C H 0.2499 0.528 0.5136 0.035 Uiso 1 1 calc R . . N22 N 0.73778(19) 0.42048(9) 0.68359(9) 0.0234(3) Uani 1 1 d . . . H22D H 0.6625 0.3803 0.6656 0.028 Uiso 1 1 calc R . . H22E H 0.8469 0.4088 0.7097 0.028 Uiso 1 1 calc R . . S3 S 0.84612(5) 0.83894(2) 0.72452(2) 0.01508(7) Uani 1 1 d . . . C3 C 0.7108(2) 0.92048(10) 0.68652(9) 0.0150(3) Uani 1 1 d . . . N31 N 0.54662(17) 0.90926(8) 0.64419(8) 0.0179(3) Uani 1 1 d . . . H31 H 0.5078 0.8582 0.6352 0.021 Uiso 1 1 calc R . . C31 C 0.4268(2) 0.97633(10) 0.61177(11) 0.0194(3) Uani 1 1 d . . . H31A H 0.4919 1.0099 0.5733 0.023 Uiso 1 1 calc R . . H31B H 0.3965 1.0126 0.6569 0.023 Uiso 1 1 calc R . . C32 C 0.2495(2) 0.94089(12) 0.56781(13) 0.0309(4) Uani 1 1 d . . . H32A H 0.2804 0.9039 0.5241 0.046 Uiso 1 1 calc R . . H32B H 0.1711 0.986 0.5443 0.046 Uiso 1 1 calc R . . H32C H 0.1826 0.9099 0.6067 0.046 Uiso 1 1 calc R . . N32 N 0.7701(2) 0.99737(9) 0.70038(10) 0.0239(3) Uani 1 1 d . . . H32D H 0.7009 1.0393 0.6817 0.029 Uiso 1 1 calc R . . H32E H 0.8785 1.0064 0.7283 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01650(5) 0.01128(5) 0.01923(6) -0.00071(4) 0.00146(4) 0.00051(4) I1 0.02156(5) 0.01198(4) 0.01387(4) -0.00070(3) 0.00338(3) 0.00147(4) S1 0.01231(15) 0.01522(17) 0.01410(15) -0.00029(13) 0.00198(12) 0.00095(13) C1 0.0132(6) 0.0121(7) 0.0157(6) 0.0000(5) 0.0018(5) -0.0006(5) N11 0.0148(6) 0.0243(7) 0.0135(6) -0.0002(5) 0.0005(5) 0.0005(5) C11 0.0146(7) 0.0236(8) 0.0213(8) -0.0005(6) -0.0035(6) -0.0023(6) C12 0.0177(8) 0.0253(9) 0.0319(9) 0.0019(7) -0.0052(7) 0.0009(7) N12 0.0130(6) 0.0346(9) 0.0146(6) 0.0024(5) 0.0025(5) 0.0021(5) S2 0.01236(16) 0.01066(17) 0.0332(2) -0.00039(15) -0.00298(15) 0.00074(13) C2 0.0143(7) 0.0121(7) 0.0203(7) -0.0004(5) 0.0032(6) -0.0001(5) N21 0.0144(6) 0.0105(6) 0.0228(7) -0.0011(5) -0.0006(5) 0.0002(5) C21 0.0173(7) 0.0141(7) 0.0229(8) -0.0035(6) -0.0007(6) -0.0029(6) C22 0.0189(8) 0.0199(8) 0.0293(9) -0.0032(7) -0.0035(7) -0.0013(6) N22 0.0196(7) 0.0095(6) 0.0390(9) -0.0005(6) -0.0069(6) 0.0004(5) S3 0.01200(16) 0.01018(16) 0.02232(18) -0.00171(13) -0.00170(13) 0.00003(12) C3 0.0141(7) 0.0122(7) 0.0187(7) -0.0018(5) 0.0014(5) -0.0004(5) N31 0.0159(6) 0.0099(6) 0.0266(7) -0.0005(5) -0.0041(5) 0.0002(5) C31 0.0186(7) 0.0114(7) 0.0269(8) -0.0002(6) -0.0039(6) 0.0015(6) C32 0.0241(9) 0.0188(9) 0.0457(12) 0.0014(8) -0.0158(8) 0.0000(7) N32 0.0223(7) 0.0101(6) 0.0366(9) -0.0015(6) -0.0101(6) -0.0005(5) #----------------------------------------------------------------------------# # 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 2.5540(4) . ? Ag1 S3 2.5658(4) . ? Ag1 S1 2.6114(4) . ? Ag1 I1 2.8391(2) . ? S1 C1 1.7277(15) . ? C1 N11 1.322(2) . ? C1 N12 1.3227(19) . ? N11 C11 1.467(2) . ? N11 H11 0.88 . ? C11 C12 1.528(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? N12 H12D 0.88 . ? N12 H12E 0.88 . ? S2 C2 1.7157(16) . ? C2 N21 1.327(2) . ? C2 N22 1.331(2) . ? N21 C21 1.461(2) . ? N21 H21 0.88 . ? C21 C22 1.519(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? N22 H22D 0.88 . ? N22 H22E 0.88 . ? S3 C3 1.7219(16) . ? C3 N31 1.327(2) . ? C3 N32 1.328(2) . ? N31 C31 1.456(2) . ? N31 H31 0.88 . ? C31 C32 1.520(2) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? N32 H32D 0.88 . ? N32 H32E 0.88 . ? 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 S3 112.190(13) . . ? S2 Ag1 S1 104.562(14) . . ? S3 Ag1 S1 109.211(13) . . ? S2 Ag1 I1 111.731(11) . . ? S3 Ag1 I1 109.771(10) . . ? S1 Ag1 I1 109.204(10) . . ? C1 S1 Ag1 115.90(5) . . ? N11 C1 N12 120.12(14) . . ? N11 C1 S1 118.45(11) . . ? N12 C1 S1 121.43(12) . . ? C1 N11 C11 126.10(13) . . ? C1 N11 H11 116.9 . . ? C11 N11 H11 116.9 . . ? N11 C11 C12 112.93(14) . . ? N11 C11 H11A 109 . . ? C12 C11 H11A 109 . . ? N11 C11 H11B 109 . . ? C12 C11 H11B 109 . . ? H11A C11 H11B 107.8 . . ? 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 . . ? C1 N12 H12D 120 . . ? C1 N12 H12E 120 . . ? H12D N12 H12E 120 . . ? C2 S2 Ag1 107.22(5) . . ? N21 C2 N22 118.35(14) . . ? N21 C2 S2 121.88(12) . . ? N22 C2 S2 119.77(12) . . ? C2 N21 C21 124.51(13) . . ? C2 N21 H21 117.7 . . ? C21 N21 H21 117.7 . . ? N21 C21 C22 109.62(13) . . ? N21 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? N21 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? 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 . . ? C2 N22 H22D 120 . . ? C2 N22 H22E 120 . . ? H22D N22 H22E 120 . . ? C3 S3 Ag1 106.38(5) . . ? N31 C3 N32 118.32(14) . . ? N31 C3 S3 122.09(12) . . ? N32 C3 S3 119.59(12) . . ? C3 N31 C31 123.92(13) . . ? C3 N31 H31 118 . . ? C31 N31 H31 118 . . ? N31 C31 C32 109.60(13) . . ? N31 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? N31 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 N32 H32D 120 . . ? C3 N32 H32E 120 . . ? H32D N32 H32E 120 . . ? 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 N11 H11 I1 0.88 2.84 3.6256(13) 150.2 4_575 N12 H12E I1 0.88 2.71 3.5900(14) 176.3 . N22 H22D I1 0.88 2.85 3.5875(14) 142.4 2_646 N32 H32D I1 0.88 2.77 3.5753(14) 152.4 2_656 data_gb0939 _database_code_depnum_ccdc_archive 'CCDC 751803' _audit_creation_date 2009-08-17T13:42:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C3 H12 Ag2 Br2 N6 S3' _chemical_formula_moiety 'C3 H12 Ag2 Br2 N6 S3' _chemical_formula_weight 603.93 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1' _symmetry_space_group_name_Hall -P_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 4.1332(3) _cell_length_b 8.2724(4) _cell_length_c 20.9190(14) _cell_angle_alpha 90 _cell_angle_beta 95.291(6) _cell_angle_gamma 90 _cell_volume 712.20(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1993 _cell_measurement_theta_min 2.9114 _cell_measurement_theta_max 28.9686 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.84 #----------------------------------------------------------------------------# # 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 -0.0090292382 _diffrn_orient_matrix_ub_12 -0.0326235973 _diffrn_orient_matrix_ub_13 0.1481769492 _diffrn_orient_matrix_ub_21 0.0014448057 _diffrn_orient_matrix_ub_22 -0.0791719842 _diffrn_orient_matrix_ub_23 -0.0652761392 _diffrn_orient_matrix_ub_31 0.0327971769 _diffrn_orient_matrix_ub_32 -0.0056248242 _diffrn_orient_matrix_ub_33 0.0601608858 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_unetI/netI 0.0636 _diffrn_reflns_number 5042 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.909 _reflns_number_total 1745 _reflns_number_gt 1323 _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. ; _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^)+(0.0484P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1745 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.576 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.25 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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 0.51449(13) 0.56025(6) 0.67638(2) 0.01934(16) Uani 1 1 d . . . Br1 Br 0.45381(16) 0.75894(7) 0.57489(3) 0.01528(17) Uani 1 1 d . . . S1 S 0.3176(4) 0.27809(19) 0.66657(8) 0.0152(3) Uani 1 1 d . . . C1 C 0.0817(15) 0.2658(7) 0.5949(3) 0.0136(13) Uani 1 1 d . . . N11 N -0.0343(13) 0.3971(7) 0.5629(2) 0.0158(12) Uani 1 1 d . . . H11A H -0.1587 0.3862 0.5267 0.019 Uiso 1 1 calc R . . H11B H 0.0141 0.4942 0.5781 0.019 Uiso 1 1 calc R . . N12 N -0.0015(13) 0.1228(7) 0.5691(3) 0.0191(12) Uani 1 1 d . . . H12A H -0.1266 0.118 0.5328 0.023 Uiso 1 1 calc R . . H12B H 0.0687 0.0332 0.5884 0.023 Uiso 1 1 calc R . . S2 S 0 0.6639(3) 0.75 0.0128(5) Uani 1 2 d S . . C2 C 0 0.8732(10) 0.75 0.0079(16) Uani 1 2 d S . . N21 N 0.1746(14) 0.9547(6) 0.7954(3) 0.0192(12) Uani 1 1 d . . . H21A H 0.1731 1.061 0.795 0.023 Uiso 1 1 calc R . . H21B H 0.2923 0.9025 0.8259 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0267(3) 0.0143(3) 0.0163(3) -0.0007(2) -0.0019(2) -0.0049(2) Br1 0.0198(3) 0.0122(3) 0.0130(3) 0.0012(2) -0.0030(3) -0.0003(2) S1 0.0190(8) 0.0128(8) 0.0130(8) 0.0021(6) -0.0031(7) -0.0002(6) C1 0.015(3) 0.011(3) 0.015(3) -0.002(2) 0.004(3) 0.000(2) N11 0.021(3) 0.018(3) 0.008(2) 0.000(2) -0.002(2) -0.001(2) N12 0.025(3) 0.011(3) 0.021(3) 0.001(2) -0.003(3) 0.002(2) S2 0.0133(10) 0.0085(11) 0.0161(11) 0 -0.0024(9) 0 C2 0.012(4) 0.008(4) 0.004(4) 0 0.001(3) 0 N21 0.029(3) 0.011(3) 0.016(3) -0.003(2) -0.004(2) -0.001(2) #----------------------------------------------------------------------------# # 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 2.4743(17) . ? Ag1 S2 2.5620(9) 1_655 ? Ag1 Br1 2.6785(8) . ? Ag1 S2 2.8692(9) . ? Ag1 Ag1 3.0932(10) 2_656 ? S1 C1 1.714(7) . ? C1 N12 1.332(8) . ? C1 N11 1.342(8) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.732(9) . ? S2 Ag1 2.5620(9) 1_455 ? S2 Ag1 2.5620(9) 2_656 ? S2 Ag1 2.8692(9) 2_556 ? C2 N21 1.322(7) . ? C2 N21 1.322(7) 2_556 ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? 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 126.80(6) . 1_655 ? S1 Ag1 Br1 120.47(4) . . ? S2 Ag1 Br1 106.38(4) 1_655 . ? S1 Ag1 S2 94.13(6) . . ? S2 Ag1 S2 98.95(4) 1_655 . ? Br1 Ag1 S2 102.84(4) . . ? C1 S1 Ag1 106.6(2) . . ? N12 C1 N11 116.7(6) . . ? N12 C1 S1 120.8(5) . . ? N11 C1 S1 122.5(5) . . ? 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 109.55(5) . 1_455 ? C2 S2 Ag1 109.55(5) . 2_656 ? Ag1 S2 Ag1 140.89(9) 1_455 2_656 ? C2 S2 Ag1 107.39(4) . . ? Ag1 S2 Ag1 98.95(4) 1_455 . ? Ag1 S2 Ag1 69.17(3) 2_656 . ? C2 S2 Ag1 107.39(4) . 2_556 ? Ag1 S2 Ag1 69.17(3) 1_455 2_556 ? Ag1 S2 Ag1 98.95(4) 2_656 2_556 ? Ag1 S2 Ag1 145.22(8) . 2_556 ? N21 C2 N21 118.7(8) . 2_556 ? N21 C2 S2 120.6(4) . . ? N21 C2 S2 120.6(4) 2_556 . ? C2 N21 H21A 120 . . ? C2 N21 H21B 120 . . ? H21A N21 H21B 120 . . ? 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 N11 H11A Br1 0.88 2.64 3.472(5) 158.4 3_566 N11 H11B Br1 0.88 2.85 3.605(5) 144.8 . N12 H12A Br1 0.88 2.72 3.534(5) 155.1 3_566 N12 H12B Br1 0.88 2.8 3.546(6) 143.4 1_545 N21 H21B Br1 0.88 2.53 3.403(5) 170 2_656 data_gb0942 _database_code_depnum_ccdc_archive 'CCDC 751804' _audit_creation_date 2009-08-19T20:43:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C15 H36 Ag Cl N6 S3' _chemical_formula_moiety 'C15 H36 Ag Cl N6 S3' _chemical_formula_weight 540 #----------------------------------------------------------------------------# # 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 13.2924(6) _cell_length_b 13.4749(6) _cell_length_c 16.3116(7) _cell_angle_alpha 74.412(4) _cell_angle_beta 74.071(4) _cell_angle_gamma 63.333(4) _cell_volume 2474.34(21) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9411 _cell_measurement_theta_min 3.702 _cell_measurement_theta_max 32.6717 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.91 #----------------------------------------------------------------------------# # 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 10.4738 _diffrn_orient_matrix_ub_11 0.0457088348 _diffrn_orient_matrix_ub_12 0.0159877104 _diffrn_orient_matrix_ub_13 -0.0233942699 _diffrn_orient_matrix_ub_21 -0.0279315395 _diffrn_orient_matrix_ub_22 0.0242446498 _diffrn_orient_matrix_ub_23 -0.0365892775 _diffrn_orient_matrix_ub_31 -0.0294764348 _diffrn_orient_matrix_ub_32 0.0524511016 _diffrn_orient_matrix_ub_33 0.0152642548 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_unetI/netI 0.1322 _diffrn_reflns_number 31962 _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 -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.7 _diffrn_reflns_theta_max 32.68 _diffrn_reflns_theta_full 30.75 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.894 _reflns_number_total 16275 _reflns_number_gt 8871 _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. ; _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^)+(0.0384P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 16275 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.107 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.124 _refine_diff_density_min -0.969 _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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.67102(2) 0.69532(2) 0.451755(19) 0.02132(7) Uani 1 1 d . . . Cl1 Cl 0.63023(7) 0.64742(7) 0.62457(6) 0.02061(19) Uani 1 1 d . . . S1 S 0.47346(7) 0.83778(7) 0.42064(6) 0.0207(2) Uani 1 1 d . . . C1 C 0.4069(3) 0.9262(3) 0.4966(3) 0.0209(8) Uani 1 1 d . . . N11 N 0.4314(3) 0.8943(2) 0.5751(2) 0.0219(7) Uani 1 1 d . . . H11 H 0.4866 0.8275 0.5863 0.026 Uiso 1 1 calc R . . C111 C 0.3748(3) 0.9605(3) 0.6453(2) 0.0224(8) Uani 1 1 d . . . H11A H 0.2912 0.9829 0.6546 0.027 Uiso 1 1 calc R . . H11B H 0.3889 1.0301 0.6287 0.027 Uiso 1 1 calc R . . C112 C 0.4180(4) 0.8945(3) 0.7280(3) 0.0358(11) Uani 1 1 d . . . H11C H 0.4052 0.825 0.7441 0.054 Uiso 1 1 calc R . . H11D H 0.3769 0.9399 0.7742 0.054 Uiso 1 1 calc R . . H11E H 0.5 0.8756 0.7197 0.054 Uiso 1 1 calc R . . N12 N 0.3259(3) 1.0299(2) 0.4770(2) 0.0249(7) Uani 1 1 d . . . H12 H 0.2947 1.0727 0.5172 0.03 Uiso 1 1 calc R . . C121 C 0.2856(4) 1.0773(3) 0.3947(3) 0.0308(10) Uani 1 1 d . . . H12A H 0.3491 1.0454 0.3478 0.037 Uiso 1 1 calc R . . H12B H 0.2628 1.1599 0.3834 0.037 Uiso 1 1 calc R . . C122 C 0.1859(4) 1.0540(4) 0.3932(4) 0.0498(13) Uani 1 1 d . . . H12C H 0.2082 0.9723 0.4037 0.075 Uiso 1 1 calc R . . H12D H 0.1625 1.0867 0.3366 0.075 Uiso 1 1 calc R . . H12E H 0.1219 1.0875 0.4384 0.075 Uiso 1 1 calc R . . S2 S 0.84236(7) 0.75103(7) 0.40919(6) 0.02019(19) Uani 1 1 d . . . C2 C 0.9304(3) 0.6677(3) 0.4841(2) 0.0186(8) Uani 1 1 d . . . N21 N 0.8896(2) 0.6198(2) 0.5596(2) 0.0206(7) Uani 1 1 d . . . H21 H 0.8182 0.6283 0.5677 0.025 Uiso 1 1 calc R . . C211 C 0.9519(3) 0.5539(3) 0.6310(2) 0.0214(8) Uani 1 1 d . . . H21A H 1.0317 0.5067 0.6073 0.026 Uiso 1 1 calc R . . H21B H 0.9158 0.5029 0.668 0.026 Uiso 1 1 calc R . . C212 C 0.9531(3) 0.6283(3) 0.6860(3) 0.0283(9) Uani 1 1 d . . . H21C H 0.9883 0.6793 0.6496 0.042 Uiso 1 1 calc R . . H21D H 0.9974 0.581 0.7319 0.042 Uiso 1 1 calc R . . H21E H 0.8745 0.6725 0.712 0.042 Uiso 1 1 calc R . . N22 N 1.0411(3) 0.6499(2) 0.4663(2) 0.0230(7) Uani 1 1 d . . . H22 H 1.082 0.6068 0.5067 0.028 Uiso 1 1 calc R . . C221 C 1.1011(3) 0.6953(3) 0.3861(2) 0.0248(9) Uani 1 1 d . . . H22A H 1.0559 0.7199 0.3397 0.03 Uiso 1 1 calc R . . H22B H 1.1762 0.635 0.3683 0.03 Uiso 1 1 calc R . . C222 C 1.1193(3) 0.7935(3) 0.3968(3) 0.0306(9) Uani 1 1 d . . . H22C H 1.045 0.8556 0.4101 0.046 Uiso 1 1 calc R . . H22D H 1.1632 0.8186 0.343 0.046 Uiso 1 1 calc R . . H22E H 1.1616 0.7702 0.4441 0.046 Uiso 1 1 calc R . . S3 S 0.74113(7) 0.50451(7) 0.40125(6) 0.0208(2) Uani 1 1 d . . . C3 C 0.6672(3) 0.4297(3) 0.4726(2) 0.0186(8) Uani 1 1 d . . . N31 N 0.6288(2) 0.4444(2) 0.5547(2) 0.0204(7) Uani 1 1 d . . . H31 H 0.6369 0.4981 0.5698 0.024 Uiso 1 1 calc R . . C311 C 0.5742(3) 0.3785(3) 0.6219(2) 0.0237(8) Uani 1 1 d . . . H31A H 0.6229 0.2972 0.6231 0.028 Uiso 1 1 calc R . . H31B H 0.4995 0.394 0.6089 0.028 Uiso 1 1 calc R . . C312 C 0.5566(3) 0.4091(3) 0.7092(2) 0.0261(9) Uani 1 1 d . . . H31C H 0.6308 0.392 0.7225 0.039 Uiso 1 1 calc R . . H31D H 0.519 0.3654 0.7539 0.039 Uiso 1 1 calc R . . H31E H 0.5084 0.4897 0.7077 0.039 Uiso 1 1 calc R . . N32 N 0.6496(3) 0.3521(2) 0.4482(2) 0.0220(7) Uani 1 1 d . . . H32 H 0.6122 0.3157 0.4876 0.026 Uiso 1 1 calc R . . C321 C 0.6871(3) 0.3231(3) 0.3617(3) 0.0282(9) Uani 1 1 d . . . H32A H 0.6952 0.3882 0.3191 0.034 Uiso 1 1 calc R . . H32B H 0.6279 0.3077 0.3479 0.034 Uiso 1 1 calc R . . C322 C 0.7998(4) 0.2212(4) 0.3532(3) 0.0431(12) Uani 1 1 d . . . H32C H 0.8587 0.2358 0.367 0.065 Uiso 1 1 calc R . . H32D H 0.8223 0.2063 0.2938 0.065 Uiso 1 1 calc R . . H32E H 0.7913 0.1556 0.3934 0.065 Uiso 1 1 calc R . . Ag2 Ag 0.67497(2) 0.15685(2) 1.029195(19) 0.02175(7) Uani 1 1 d . . . Cl2 Cl 0.72259(7) 0.19703(7) 0.85749(6) 0.02117(19) Uani 1 1 d . . . S4 S 0.46007(7) 0.20649(7) 1.06226(6) 0.0202(2) Uani 1 1 d . . . C4 C 0.4281(3) 0.1584(3) 0.9888(2) 0.0190(8) Uani 1 1 d . . . N41 N 0.4861(2) 0.1579(2) 0.9081(2) 0.0209(7) Uani 1 1 d . . . H41 H 0.5414 0.1815 0.8947 0.025 Uiso 1 1 calc R . . C411 C 0.4657(3) 0.1210(3) 0.8393(3) 0.0252(9) Uani 1 1 d . . . H41A H 0.4487 0.0535 0.8643 0.03 Uiso 1 1 calc R . . H41B H 0.5362 0.0994 0.7951 0.03 Uiso 1 1 calc R . . C412 C 0.3666(3) 0.2123(3) 0.7956(2) 0.0244(8) Uani 1 1 d . . . H41C H 0.2973 0.2367 0.8394 0.037 Uiso 1 1 calc R . . H41D H 0.3532 0.1819 0.7533 0.037 Uiso 1 1 calc R . . H41E H 0.386 0.2768 0.7661 0.037 Uiso 1 1 calc R . . N42 N 0.3422(3) 0.1244(2) 1.0120(2) 0.0231(7) Uani 1 1 d . . . H42 H 0.3266 0.1033 0.9721 0.028 Uiso 1 1 calc R . . C421 C 0.2729(3) 0.1195(3) 1.0974(3) 0.0271(9) Uani 1 1 d . . . H42A H 0.3181 0.1083 1.1408 0.033 Uiso 1 1 calc R . . H42B H 0.2528 0.0539 1.1097 0.033 Uiso 1 1 calc R . . C422 C 0.1635(3) 0.2259(3) 1.1065(3) 0.0322(10) Uani 1 1 d . . . H42C H 0.1828 0.29 1.1002 0.048 Uiso 1 1 calc R . . H42D H 0.1168 0.2163 1.1637 0.048 Uiso 1 1 calc R . . H42E H 0.1204 0.2398 1.0616 0.048 Uiso 1 1 calc R . . S5 S 0.79892(7) -0.04598(7) 1.08324(6) 0.01995(19) Uani 1 1 d . . . C5 C 0.9241(3) -0.0892(3) 1.0078(3) 0.0199(8) Uani 1 1 d . . . N51 N 0.9309(2) -0.0350(2) 0.9277(2) 0.0191(7) Uani 1 1 d . . . H51 H 0.8713 0.027 0.9146 0.023 Uiso 1 1 calc R . . C511 C 1.0304(3) -0.0702(3) 0.8587(2) 0.0201(8) Uani 1 1 d . . . H51A H 1.0514 -0.149 0.8538 0.024 Uiso 1 1 calc R . . H51B H 1.0965 -0.0667 0.8729 0.024 Uiso 1 1 calc R . . C512 C 1.0034(3) 0.0058(3) 0.7737(3) 0.0301(10) Uani 1 1 d . . . H51C H 0.9464 -0.0067 0.7552 0.045 Uiso 1 1 calc R . . H51D H 1.0733 -0.0111 0.7298 0.045 Uiso 1 1 calc R . . H51E H 0.9729 0.0847 0.7808 0.045 Uiso 1 1 calc R . . N52 N 1.0162(2) -0.1794(2) 1.0312(2) 0.0226(7) Uani 1 1 d . . . H52 H 1.0789 -0.1975 0.9918 0.027 Uiso 1 1 calc R . . C521 C 1.0217(3) -0.2500(3) 1.1162(3) 0.0268(9) Uani 1 1 d . . . H52A H 0.9691 -0.2033 1.1605 0.032 Uiso 1 1 calc R . . H52B H 1.1002 -0.28 1.1279 0.032 Uiso 1 1 calc R . . C522 C 0.9902(4) -0.3477(3) 1.1244(3) 0.0356(10) Uani 1 1 d . . . H52C H 0.9128 -0.3188 1.1122 0.053 Uiso 1 1 calc R . . H52D H 0.9927 -0.3907 1.1832 0.053 Uiso 1 1 calc R . . H52E H 1.0446 -0.3969 1.083 0.053 Uiso 1 1 calc R . . S6 S 0.71442(7) 0.29425(7) 1.08500(6) 0.01937(19) Uani 1 1 d . . . C6 C 0.6680(3) 0.4208(3) 1.0153(2) 0.0183(8) Uani 1 1 d . . . N61 N 0.6398(2) 0.4270(2) 0.9418(2) 0.0198(7) Uani 1 1 d . . . H61 H 0.6374 0.3666 0.9328 0.024 Uiso 1 1 calc R . . C611 C 0.6124(3) 0.5270(3) 0.8743(2) 0.0233(8) Uani 1 1 d . . . H61A H 0.5568 0.5936 0.9011 0.028 Uiso 1 1 calc R . . H61B H 0.5757 0.5174 0.8334 0.028 Uiso 1 1 calc R . . C612 C 0.7176(3) 0.5482(3) 0.8247(3) 0.0294(9) Uani 1 1 d . . . H61C H 0.7524 0.5609 0.8645 0.044 Uiso 1 1 calc R . . H61D H 0.6954 0.6148 0.7796 0.044 Uiso 1 1 calc R . . H61E H 0.7729 0.4826 0.798 0.044 Uiso 1 1 calc R . . N62 N 0.6591(3) 0.5149(2) 1.03560(19) 0.0198(7) Uani 1 1 d . . . H62 H 0.6342 0.578 0.9989 0.024 Uiso 1 1 calc R . . C621 C 0.6877(3) 0.5204(3) 1.1141(3) 0.0249(9) Uani 1 1 d . . . H62A H 0.6664 0.4667 1.1625 0.03 Uiso 1 1 calc R . . H62B H 0.6416 0.597 1.1285 0.03 Uiso 1 1 calc R . . C622 C 0.8132(4) 0.4933(4) 1.1061(3) 0.0400(11) Uani 1 1 d . . . H62C H 0.8594 0.4162 1.0947 0.06 Uiso 1 1 calc R . . H62D H 0.8266 0.5001 1.1602 0.06 Uiso 1 1 calc R . . H62E H 0.835 0.5461 1.0584 0.06 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01623(14) 0.01906(14) 0.02711(17) -0.00482(12) -0.00560(11) -0.00432(11) Cl1 0.0173(4) 0.0203(4) 0.0239(5) -0.0038(4) -0.0056(4) -0.0063(3) S1 0.0158(4) 0.0181(4) 0.0268(5) -0.0079(4) -0.0060(4) -0.0021(3) C1 0.0122(17) 0.0167(18) 0.033(2) -0.0054(16) -0.0042(15) -0.0044(13) N11 0.0207(16) 0.0166(15) 0.0237(18) -0.0051(13) -0.0042(13) -0.0025(12) C111 0.0209(19) 0.0179(18) 0.028(2) -0.0086(15) -0.0003(16) -0.0068(14) C112 0.043(3) 0.030(2) 0.028(2) -0.0072(18) -0.004(2) -0.0089(19) N12 0.0263(18) 0.0160(15) 0.0288(19) -0.0084(13) -0.0064(14) -0.0019(13) C121 0.031(2) 0.0179(19) 0.034(2) -0.0056(17) -0.0134(19) 0.0027(16) C122 0.043(3) 0.038(3) 0.067(4) -0.004(2) -0.034(3) -0.004(2) S2 0.0145(4) 0.0157(4) 0.0287(5) -0.0027(4) -0.0066(4) -0.0037(3) C2 0.0152(18) 0.0116(16) 0.027(2) -0.0059(14) -0.0047(15) -0.0016(13) N21 0.0110(14) 0.0209(16) 0.0273(18) -0.0015(13) -0.0055(12) -0.0044(12) C211 0.0149(18) 0.0204(18) 0.026(2) -0.0004(15) -0.0049(15) -0.0062(14) C212 0.024(2) 0.026(2) 0.031(2) -0.0074(17) -0.0053(17) -0.0054(16) N22 0.0150(16) 0.0245(16) 0.0275(18) -0.0007(13) -0.0055(13) -0.0072(12) C221 0.0130(18) 0.033(2) 0.026(2) 0.0002(17) -0.0045(15) -0.0089(15) C222 0.023(2) 0.029(2) 0.039(3) 0.0056(18) -0.0103(18) -0.0134(17) S3 0.0149(4) 0.0176(4) 0.0278(5) -0.0061(4) -0.0027(4) -0.0044(3) C3 0.0077(16) 0.0160(17) 0.029(2) -0.0061(15) -0.0067(14) 0.0008(13) N31 0.0184(16) 0.0171(15) 0.0272(18) -0.0061(13) -0.0043(13) -0.0071(12) C311 0.0170(19) 0.0183(18) 0.031(2) -0.0032(16) -0.0051(16) -0.0034(14) C312 0.021(2) 0.025(2) 0.029(2) -0.0011(16) -0.0019(16) -0.0096(16) N32 0.0189(16) 0.0195(16) 0.0283(19) -0.0053(13) -0.0022(13) -0.0088(12) C321 0.031(2) 0.032(2) 0.026(2) -0.0089(18) -0.0040(17) -0.0152(17) C322 0.040(3) 0.038(3) 0.048(3) -0.023(2) 0.005(2) -0.012(2) Ag2 0.01729(15) 0.01665(14) 0.03017(18) -0.00421(12) -0.00701(12) -0.00417(11) Cl2 0.0176(4) 0.0174(4) 0.0257(5) -0.0031(4) -0.0054(4) -0.0040(3) S4 0.0149(4) 0.0175(4) 0.0292(5) -0.0065(4) -0.0071(4) -0.0042(3) C4 0.0172(18) 0.0067(15) 0.032(2) -0.0023(14) -0.0126(15) 0.0000(13) N41 0.0177(16) 0.0220(16) 0.0268(18) -0.0056(13) -0.0050(13) -0.0099(12) C411 0.024(2) 0.0220(19) 0.032(2) -0.0113(17) -0.0044(17) -0.0079(15) C412 0.024(2) 0.027(2) 0.027(2) -0.0057(17) -0.0065(16) -0.0122(16) N42 0.0215(17) 0.0217(16) 0.0300(19) -0.0064(14) -0.0081(14) -0.0090(13) C421 0.025(2) 0.027(2) 0.034(2) -0.0026(17) -0.0069(17) -0.0143(16) C422 0.026(2) 0.043(2) 0.034(3) -0.013(2) -0.0018(18) -0.0170(18) S5 0.0155(4) 0.0151(4) 0.0277(5) -0.0049(4) -0.0047(4) -0.0037(3) C5 0.0155(18) 0.0159(17) 0.030(2) -0.0064(15) -0.0093(15) -0.0037(14) N51 0.0109(14) 0.0149(14) 0.0282(18) -0.0044(13) -0.0042(12) -0.0016(11) C511 0.0127(17) 0.0181(18) 0.029(2) -0.0064(15) -0.0036(15) -0.0046(13) C512 0.028(2) 0.024(2) 0.031(2) -0.0059(17) -0.0034(18) -0.0042(16) N52 0.0115(15) 0.0190(16) 0.0309(19) -0.0022(13) -0.0057(13) -0.0006(12) C521 0.0151(19) 0.028(2) 0.031(2) 0.0000(17) -0.0096(16) -0.0029(15) C522 0.030(2) 0.024(2) 0.049(3) 0.0054(19) -0.015(2) -0.0100(17) S6 0.0163(4) 0.0135(4) 0.0277(5) -0.0031(4) -0.0070(4) -0.0039(3) C6 0.0115(17) 0.0158(17) 0.023(2) -0.0054(14) -0.0002(14) -0.0024(13) N61 0.0187(16) 0.0111(14) 0.0315(19) -0.0053(13) -0.0084(13) -0.0043(11) C611 0.022(2) 0.0162(18) 0.028(2) -0.0053(15) -0.0111(16) 0.0005(14) C612 0.025(2) 0.032(2) 0.024(2) -0.0018(17) -0.0034(17) -0.0071(17) N62 0.0218(17) 0.0132(14) 0.0228(17) -0.0018(12) -0.0056(13) -0.0055(12) C621 0.034(2) 0.0144(18) 0.026(2) -0.0078(15) -0.0061(17) -0.0069(15) C622 0.041(3) 0.044(3) 0.048(3) -0.006(2) -0.022(2) -0.021(2) #----------------------------------------------------------------------------# # 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 2.5538(9) . ? Ag1 S2 2.5728(10) . ? Ag1 S3 2.5931(9) . ? Ag1 Cl1 2.6747(10) . ? S1 C1 1.727(4) . ? C1 N11 1.318(5) . ? C1 N12 1.347(4) . ? N11 C111 1.466(4) . ? N11 H11 0.88 . ? C111 C112 1.505(6) . ? C111 H11A 0.99 . ? C111 H11B 0.99 . ? C112 H11C 0.98 . ? C112 H11D 0.98 . ? C112 H11E 0.98 . ? N12 C121 1.457(5) . ? N12 H12 0.88 . ? C121 C122 1.501(6) . ? C121 H12A 0.99 . ? C121 H12B 0.99 . ? C122 H12C 0.98 . ? C122 H12D 0.98 . ? C122 H12E 0.98 . ? S2 C2 1.730(4) . ? C2 N21 1.322(4) . ? C2 N22 1.339(4) . ? N21 C211 1.464(5) . ? N21 H21 0.88 . ? C211 C212 1.522(5) . ? C211 H21A 0.99 . ? C211 H21B 0.99 . ? C212 H21C 0.98 . ? C212 H21D 0.98 . ? C212 H21E 0.98 . ? N22 C221 1.468(5) . ? N22 H22 0.88 . ? C221 C222 1.508(5) . ? C221 H22A 0.99 . ? C221 H22B 0.99 . ? C222 H22C 0.98 . ? C222 H22D 0.98 . ? C222 H22E 0.98 . ? S3 C3 1.722(4) . ? C3 N31 1.330(4) . ? C3 N32 1.344(4) . ? N31 C311 1.460(5) . ? N31 H31 0.88 . ? C311 C312 1.516(5) . ? C311 H31A 0.99 . ? C311 H31B 0.99 . ? C312 H31C 0.98 . ? C312 H31D 0.98 . ? C312 H31E 0.98 . ? N32 C321 1.458(5) . ? N32 H32 0.88 . ? C321 C322 1.513(5) . ? C321 H32A 0.99 . ? C321 H32B 0.99 . ? C322 H32C 0.98 . ? C322 H32D 0.98 . ? C322 H32E 0.98 . ? Ag2 S5 2.5341(9) . ? Ag2 S4 2.5557(9) . ? Ag2 S6 2.5633(9) . ? Ag2 Cl2 2.6567(10) . ? S4 C4 1.726(4) . ? C4 N41 1.330(5) . ? C4 N42 1.341(5) . ? N41 C411 1.471(5) . ? N41 H41 0.88 . ? C411 C412 1.531(5) . ? C411 H41A 0.99 . ? C411 H41B 0.99 . ? C412 H41C 0.98 . ? C412 H41D 0.98 . ? C412 H41E 0.98 . ? N42 C421 1.447(5) . ? N42 H42 0.88 . ? C421 C422 1.522(5) . ? C421 H42A 0.99 . ? C421 H42B 0.99 . ? C422 H42C 0.98 . ? C422 H42D 0.98 . ? C422 H42E 0.98 . ? S5 C5 1.736(4) . ? C5 N51 1.316(5) . ? C5 N52 1.339(4) . ? N51 C511 1.466(4) . ? N51 H51 0.88 . ? C511 C512 1.510(5) . ? C511 H51A 0.99 . ? C511 H51B 0.99 . ? C512 H51C 0.98 . ? C512 H51D 0.98 . ? C512 H51E 0.98 . ? N52 C521 1.455(5) . ? N52 H52 0.88 . ? C521 C522 1.515(5) . ? C521 H52A 0.99 . ? C521 H52B 0.99 . ? C522 H52C 0.98 . ? C522 H52D 0.98 . ? C522 H52E 0.98 . ? S6 C6 1.726(4) . ? C6 N61 1.322(5) . ? C6 N62 1.342(4) . ? N61 C611 1.464(5) . ? N61 H61 0.88 . ? C611 C612 1.518(5) . ? C611 H61A 0.99 . ? C611 H61B 0.99 . ? C612 H61C 0.98 . ? C612 H61D 0.98 . ? C612 H61E 0.98 . ? N62 C621 1.460(5) . ? N62 H62 0.88 . ? C621 C622 1.515(6) . ? C621 H62A 0.99 . ? C621 H62B 0.99 . ? C622 H62C 0.98 . ? C622 H62D 0.98 . ? C622 H62E 0.98 . ? 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 121.03(3) . . ? S1 Ag1 S3 114.46(3) . . ? S2 Ag1 S3 106.80(3) . . ? S1 Ag1 Cl1 101.54(3) . . ? S2 Ag1 Cl1 106.59(3) . . ? S3 Ag1 Cl1 104.81(3) . . ? C1 S1 Ag1 110.17(13) . . ? N11 C1 N12 118.2(3) . . ? N11 C1 S1 121.8(3) . . ? N12 C1 S1 120.0(3) . . ? C1 N11 C111 125.7(3) . . ? C1 N11 H11 117.2 . . ? C111 N11 H11 117.2 . . ? N11 C111 C112 111.3(3) . . ? N11 C111 H11A 109.4 . . ? C112 C111 H11A 109.4 . . ? N11 C111 H11B 109.4 . . ? C112 C111 H11B 109.4 . . ? H11A C111 H11B 108 . . ? C111 C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? C111 C112 H11E 109.5 . . ? H11C C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C1 N12 C121 125.6(3) . . ? C1 N12 H12 117.2 . . ? C121 N12 H12 117.2 . . ? N12 C121 C122 112.5(4) . . ? N12 C121 H12A 109.1 . . ? C122 C121 H12A 109.1 . . ? N12 C121 H12B 109.1 . . ? C122 C121 H12B 109.1 . . ? H12A C121 H12B 107.8 . . ? C121 C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C122 H12E 109.5 . . ? H12C C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C2 S2 Ag1 105.90(13) . . ? N21 C2 N22 119.0(3) . . ? N21 C2 S2 120.4(3) . . ? N22 C2 S2 120.6(3) . . ? C2 N21 C211 126.3(3) . . ? C2 N21 H21 116.9 . . ? C211 N21 H21 116.9 . . ? N21 C211 C212 112.2(3) . . ? N21 C211 H21A 109.2 . . ? C212 C211 H21A 109.2 . . ? N21 C211 H21B 109.2 . . ? C212 C211 H21B 109.2 . . ? H21A C211 H21B 107.9 . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C2 N22 C221 126.5(3) . . ? C2 N22 H22 116.8 . . ? C221 N22 H22 116.8 . . ? N22 C221 C222 112.0(3) . . ? N22 C221 H22A 109.2 . . ? C222 C221 H22A 109.2 . . ? N22 C221 H22B 109.2 . . ? C222 C221 H22B 109.2 . . ? H22A C221 H22B 107.9 . . ? C221 C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C222 H22E 109.5 . . ? H22C C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C3 S3 Ag1 107.81(12) . . ? N31 C3 N32 117.6(3) . . ? N31 C3 S3 121.1(3) . . ? N32 C3 S3 121.3(3) . . ? C3 N31 C311 125.2(3) . . ? C3 N31 H31 117.4 . . ? C311 N31 H31 117.4 . . ? N31 C311 C312 109.8(3) . . ? N31 C311 H31A 109.7 . . ? C312 C311 H31A 109.7 . . ? N31 C311 H31B 109.7 . . ? C312 C311 H31B 109.7 . . ? H31A C311 H31B 108.2 . . ? C311 C312 H31C 109.5 . . ? C311 C312 H31D 109.5 . . ? H31C C312 H31D 109.5 . . ? C311 C312 H31E 109.5 . . ? H31C C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C3 N32 C321 125.4(3) . . ? C3 N32 H32 117.3 . . ? C321 N32 H32 117.3 . . ? N32 C321 C322 112.5(4) . . ? N32 C321 H32A 109.1 . . ? C322 C321 H32A 109.1 . . ? N32 C321 H32B 109.1 . . ? C322 C321 H32B 109.1 . . ? H32A C321 H32B 107.8 . . ? C321 C322 H32C 109.5 . . ? C321 C322 H32D 109.5 . . ? H32C C322 H32D 109.5 . . ? C321 C322 H32E 109.5 . . ? H32C C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? S5 Ag2 S4 115.08(3) . . ? S5 Ag2 S6 111.30(3) . . ? S4 Ag2 S6 109.52(3) . . ? S5 Ag2 Cl2 109.16(3) . . ? S4 Ag2 Cl2 103.60(3) . . ? S6 Ag2 Cl2 107.68(3) . . ? C4 S4 Ag2 108.56(12) . . ? N41 C4 N42 119.4(3) . . ? N41 C4 S4 120.5(3) . . ? N42 C4 S4 120.1(3) . . ? C4 N41 C411 125.6(3) . . ? C4 N41 H41 117.2 . . ? C411 N41 H41 117.2 . . ? N41 C411 C412 112.8(3) . . ? N41 C411 H41A 109 . . ? C412 C411 H41A 109 . . ? N41 C411 H41B 109 . . ? C412 C411 H41B 109 . . ? H41A C411 H41B 107.8 . . ? C411 C412 H41C 109.5 . . ? C411 C412 H41D 109.5 . . ? H41C C412 H41D 109.5 . . ? C411 C412 H41E 109.5 . . ? H41C C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C4 N42 C421 125.4(3) . . ? C4 N42 H42 117.3 . . ? C421 N42 H42 117.3 . . ? N42 C421 C422 112.5(3) . . ? N42 C421 H42A 109.1 . . ? C422 C421 H42A 109.1 . . ? N42 C421 H42B 109.1 . . ? C422 C421 H42B 109.1 . . ? H42A C421 H42B 107.8 . . ? C421 C422 H42C 109.5 . . ? C421 C422 H42D 109.5 . . ? H42C C422 H42D 109.5 . . ? C421 C422 H42E 109.5 . . ? H42C C422 H42E 109.5 . . ? H42D C422 H42E 109.5 . . ? C5 S5 Ag2 108.41(13) . . ? N51 C5 N52 118.9(3) . . ? N51 C5 S5 121.4(3) . . ? N52 C5 S5 119.7(3) . . ? C5 N51 C511 124.9(3) . . ? C5 N51 H51 117.6 . . ? C511 N51 H51 117.6 . . ? N51 C511 C512 110.0(3) . . ? N51 C511 H51A 109.7 . . ? C512 C511 H51A 109.7 . . ? N51 C511 H51B 109.7 . . ? C512 C511 H51B 109.7 . . ? H51A C511 H51B 108.2 . . ? C511 C512 H51C 109.5 . . ? C511 C512 H51D 109.5 . . ? H51C C512 H51D 109.5 . . ? C511 C512 H51E 109.5 . . ? H51C C512 H51E 109.5 . . ? H51D C512 H51E 109.5 . . ? C5 N52 C521 125.6(3) . . ? C5 N52 H52 117.2 . . ? C521 N52 H52 117.2 . . ? N52 C521 C522 113.0(3) . . ? N52 C521 H52A 109 . . ? C522 C521 H52A 109 . . ? N52 C521 H52B 109 . . ? C522 C521 H52B 109 . . ? H52A C521 H52B 107.8 . . ? C521 C522 H52C 109.5 . . ? C521 C522 H52D 109.5 . . ? H52C C522 H52D 109.5 . . ? C521 C522 H52E 109.5 . . ? H52C C522 H52E 109.5 . . ? H52D C522 H52E 109.5 . . ? C6 S6 Ag2 106.00(13) . . ? N61 C6 N62 119.0(3) . . ? N61 C6 S6 120.9(3) . . ? N62 C6 S6 120.1(3) . . ? C6 N61 C611 124.8(3) . . ? C6 N61 H61 117.6 . . ? C611 N61 H61 117.6 . . ? N61 C611 C612 112.3(3) . . ? N61 C611 H61A 109.1 . . ? C612 C611 H61A 109.1 . . ? N61 C611 H61B 109.1 . . ? C612 C611 H61B 109.1 . . ? H61A C611 H61B 107.9 . . ? C611 C612 H61C 109.5 . . ? C611 C612 H61D 109.5 . . ? H61C C612 H61D 109.5 . . ? C611 C612 H61E 109.5 . . ? H61C C612 H61E 109.5 . . ? H61D C612 H61E 109.5 . . ? C6 N62 C621 124.9(3) . . ? C6 N62 H62 117.6 . . ? C621 N62 H62 117.6 . . ? N62 C621 C622 113.4(3) . . ? N62 C621 H62A 108.9 . . ? C622 C621 H62A 108.9 . . ? N62 C621 H62B 108.9 . . ? C622 C621 H62B 108.9 . . ? H62A C621 H62B 107.7 . . ? C621 C622 H62C 109.5 . . ? C621 C622 H62D 109.5 . . ? H62C C622 H62D 109.5 . . ? C621 C622 H62E 109.5 . . ? H62C C622 H62E 109.5 . . ? H62D C622 H62E 109.5 . . ? 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 N11 H11 Cl1 0.88 2.37 3.247(3) 176.9 . N21 H21 Cl1 0.88 2.33 3.195(3) 165.9 . N31 H31 Cl1 0.88 2.37 3.243(3) 171 . N41 H41 Cl2 0.88 2.41 3.267(3) 165.6 . N51 H51 Cl2 0.88 2.41 3.286(3) 171.8 . N61 H61 Cl2 0.88 2.54 3.332(3) 150.7 . data_gb0945 _database_code_depnum_ccdc_archive 'CCDC 751805' _audit_creation_date 2009-10-13T11:34:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C H4 Ag Cl N2 S' _chemical_formula_moiety 'C H4 Ag Cl N2 S' _chemical_formula_weight 219.44 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4640(2) _cell_length_b 7.0191(2) _cell_length_c 16.7986(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 998.00(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6201 _cell_measurement_theta_min 3.7745 _cell_measurement_theta_max 37.5779 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.76975 _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 10.4738 _diffrn_orient_matrix_ub_11 0.0143727768 _diffrn_orient_matrix_ub_12 -0.024479453 _diffrn_orient_matrix_ub_13 0.0399280893 _diffrn_orient_matrix_ub_21 0.065564273 _diffrn_orient_matrix_ub_22 -0.0580841143 _diffrn_orient_matrix_ub_23 -0.0131956967 _diffrn_orient_matrix_ub_31 0.0755207597 _diffrn_orient_matrix_ub_32 0.0551622491 _diffrn_orient_matrix_ub_33 0.0038253143 _diffrn_measurement_device_type 'Oxford Diffraction Gemini,Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_number 17363 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 37.67 _diffrn_reflns_theta_full 37.25 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 2600 _reflns_number_gt 1909 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _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. ; _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^)+(0.0117P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2600 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0307 _refine_ls_wR_factor_gt 0.0294 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.917 _refine_diff_density_min -0.972 _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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.172478(12) 0.652826(16) 0.291784(6) 0.01586(3) Uani 1 1 d . . . Cl1 Cl 0.19255(4) 0.45900(4) 0.420142(19) 0.01053(6) Uani 1 1 d . . . S1 S 0.10597(4) 0.30603(4) 0.214985(19) 0.00949(6) Uani 1 1 d . . . C1 C 0.16962(15) 0.33814(18) 0.11748(7) 0.0089(2) Uani 1 1 d . . . N1 N 0.32211(13) 0.35653(17) 0.10129(7) 0.0136(2) Uani 1 1 d . . . H1A H 0.3533 0.3744 0.0519 0.016 Uiso 1 1 calc R . . H1B H 0.3921 0.3508 0.1399 0.016 Uiso 1 1 calc R . . N2 N 0.06698(13) 0.34704(16) 0.05891(7) 0.0125(2) Uani 1 1 d . . . H2A H 0.0998 0.365 0.0098 0.015 Uiso 1 1 calc R . . H2B H -0.0346 0.3351 0.0688 0.015 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01384(4) 0.02158(5) 0.01217(4) 0.00528(4) 0.00309(4) 0.00096(4) Cl1 0.01038(13) 0.01134(13) 0.00986(13) 0.00105(10) -0.00095(11) 0.00007(11) S1 0.00861(13) 0.01238(14) 0.00749(13) -0.00003(11) 0.00032(12) -0.00051(10) C1 0.0088(5) 0.0078(5) 0.0100(5) -0.0002(4) 0.0006(5) 0.0004(5) N1 0.0084(4) 0.0197(6) 0.0126(5) 0.0022(4) 0.0006(4) -0.0001(5) N2 0.0100(5) 0.0186(6) 0.0090(5) 0.0021(4) -0.0001(4) -0.0015(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 2.5174(3) 7_665 ? Ag1 Cl1 2.5552(3) . ? Ag1 S1 2.5930(3) 4 ? Ag1 S1 2.8119(3) . ? S1 C1 1.7390(13) . ? S1 Ag1 2.5174(3) 7_655 ? S1 Ag1 2.5930(3) 4_545 ? C1 N2 1.3140(16) . ? C1 N1 1.3253(16) . ? N1 H1A 0.88 . ? N1 H1B 0.88 . ? N2 H2A 0.88 . ? N2 H2B 0.88 . ? 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 Cl1 127.615(11) 7_665 . ? S1 Ag1 S1 118.518(11) 7_665 4 ? Cl1 Ag1 S1 108.557(10) . 4 ? S1 Ag1 S1 106.487(12) 7_665 . ? Cl1 Ag1 S1 86.534(11) . . ? S1 Ag1 S1 99.028(7) 4 . ? C1 S1 Ag1 107.90(4) . 7_655 ? C1 S1 Ag1 107.10(4) . 4_545 ? Ag1 S1 Ag1 121.492(13) 7_655 4_545 ? C1 S1 Ag1 104.95(4) . . ? Ag1 S1 Ag1 89.170(10) 7_655 . ? Ag1 S1 Ag1 124.132(12) 4_545 . ? N2 C1 N1 119.05(12) . . ? N2 C1 S1 120.43(10) . . ? N1 C1 S1 120.51(10) . . ? C1 N1 H1A 120 . . ? C1 N1 H1B 120 . . ? H1A N1 H1B 120 . . ? C1 N2 H2A 120 . . ? C1 N2 H2B 120 . . ? H2A N2 H2B 120 . . ? 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 H1A Cl1 0.88 2.53 3.3094(12) 147.5 2_564 N2 H2A Cl1 0.88 2.62 3.3809(12) 144.8 2_564 N2 H2B Cl1 0.88 2.47 3.2840(12) 153.2 6_556 data_gb0945b _database_code_depnum_ccdc_archive 'CCDC 751806' _audit_creation_date 2009-09-15T09:18:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C4 H18 Ag3 Cl2 N9 O4 S4' _chemical_formula_moiety 'C4 H16 Ag3 Cl2 N8 S4, N O3, H2 O' _chemical_formula_weight 779.02 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.306(3) _cell_length_b 11.1677(9) _cell_length_c 7.7507(6) _cell_angle_alpha 90 _cell_angle_beta 98.057(9) _cell_angle_gamma 90 _cell_volume 2083.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2761 _cell_measurement_theta_min 3.6659 _cell_measurement_theta_max 66.9733 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 28.824 _exptl_absorpt_correction_type analytical _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) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.67559 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0735603791 _diffrn_orient_matrix_ub_12 -0.1179762383 _diffrn_orient_matrix_ub_13 -0.0198643563 _diffrn_orient_matrix_ub_21 -0.0523431492 _diffrn_orient_matrix_ub_22 0.0387459259 _diffrn_orient_matrix_ub_23 -0.0608382596 _diffrn_orient_matrix_ub_31 0.1793479983 _diffrn_orient_matrix_ub_32 0.059860771 _diffrn_orient_matrix_ub_33 0.0003054977 _diffrn_measurement_device_type 'Oxford Diffraction Gemini ultra, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.1378 _diffrn_reflns_av_unetI/netI 0.0886 _diffrn_reflns_number 18916 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 68.46 _diffrn_reflns_theta_full 67.25 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 3716 _reflns_number_gt 2331 _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. ; _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^)+(0.1149P)^2^+7.3170P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3716 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.897 _refine_diff_density_min -1.835 _refine_diff_density_rms 0.268 #----------------------------------------------------------------------------# # 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 0.0181 0.0091 '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 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.282 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 0.29545(6) 0.40521(11) 0.60997(14) 0.0369(4) Uani 1 1 d . . . Ag2 Ag 0.37331(7) 0.67413(11) 0.62113(17) 0.0544(5) Uani 1 1 d . . . Ag3 Ag 0.20312(6) 0.71593(11) 0.38690(15) 0.0373(4) Uani 1 1 d . . . Cl1 Cl 0.27965(18) 0.2129(3) 0.8010(4) 0.0347(9) Uani 1 1 d . . . Cl2 Cl 0.44671(17) 0.7995(3) 0.8313(4) 0.0320(8) Uani 1 1 d . . . S1 S 0.39466(18) 0.4584(3) 0.6666(5) 0.0323(9) Uani 1 1 d . . . C1 C 0.4129(7) 0.4416(14) 0.8921(17) 0.029(3) Uani 1 1 d . . . N11 N 0.4004(7) 0.3431(12) 0.9715(16) 0.041(4) Uani 1 1 d . . . H11A H 0.4091 0.3365 1.0852 0.049 Uiso 1 1 calc R . . H11B H 0.3835 0.2839 0.9108 0.049 Uiso 1 1 calc R . . N12 N 0.4381(6) 0.5285(11) 0.9851(17) 0.035(3) Uani 1 1 d . . . H12A H 0.4465 0.5205 1.0987 0.043 Uiso 1 1 calc R . . H12B H 0.4467 0.595 0.934 0.043 Uiso 1 1 calc R . . S2 S 0.30234(17) 0.7972(3) 0.4409(4) 0.0297(8) Uani 1 1 d . . . C2 C 0.2975(6) 0.9282(12) 0.5605(18) 0.023(3) Uani 1 1 d . . . N21 N 0.3314(6) 0.9534(11) 0.7017(16) 0.032(3) Uani 1 1 d . . . H21A H 0.328 1.0214 0.7565 0.038 Uiso 1 1 calc R . . H21B H 0.3577 0.9024 0.742 0.038 Uiso 1 1 calc R . . N22 N 0.2587(6) 1.0078(12) 0.5049(15) 0.035(3) Uani 1 1 d . . . H22A H 0.2564 1.075 0.5627 0.042 Uiso 1 1 calc R . . H22B H 0.2351 0.9935 0.4101 0.042 Uiso 1 1 calc R . . S3 S 0.15351(18) 0.8472(3) 0.5948(5) 0.0333(9) Uani 1 1 d . . . C3 C 0.0870(8) 0.7819(15) 0.5533(19) 0.036(4) Uani 1 1 d . . . N31 N 0.0478(7) 0.8486(13) 0.478(2) 0.048(4) Uani 1 1 d . . . H31A H 0.0145 0.8186 0.4468 0.058 Uiso 1 1 calc R . . H31B H 0.0543 0.9245 0.4581 0.058 Uiso 1 1 calc R . . N32 N 0.0793(6) 0.6679(13) 0.5862(19) 0.043(4) Uani 1 1 d . . . H32A H 0.0464 0.6351 0.5564 0.052 Uiso 1 1 calc R . . H32B H 0.107 0.6245 0.6379 0.052 Uiso 1 1 calc R . . S4 S 0.20466(19) 0.5117(3) 0.5739(5) 0.0348(9) Uani 1 1 d . . . C4 C 0.1596(8) 0.4000(14) 0.488(2) 0.039(4) Uani 1 1 d . . . N41 N 0.1207(7) 0.4228(14) 0.352(2) 0.053(4) Uani 1 1 d . . . H41A H 0.0962 0.3675 0.3149 0.064 Uiso 1 1 calc R . . H41B H 0.1197 0.4931 0.3008 0.064 Uiso 1 1 calc R . . N42 N 0.1588(7) 0.2929(13) 0.5593(19) 0.048(4) Uani 1 1 d . . . H42A H 0.1334 0.2404 0.5173 0.058 Uiso 1 1 calc R . . H42B H 0.1837 0.2739 0.6489 0.058 Uiso 1 1 calc R . . N1 N 0.0475(7) 0.1344(14) 0.2639(19) 0.046(4) Uani 1 1 d . . . O11 O 0.0809(5) 0.0985(11) 0.3922(17) 0.049(3) Uani 1 1 d . . . O12 O 0.0193(7) 0.0637(11) 0.170(2) 0.065(4) Uani 1 1 d . . . O13 O 0.0437(6) 0.2439(12) 0.236(2) 0.061(4) Uani 1 1 d . . . O1 O 0.4614(5) 0.3793(11) 1.3099(14) 0.041(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 0.0494(8) 0.0361(7) 0.0238(6) 0.0022(5) 0.0004(5) -0.0010(5) Ag2 0.0876(12) 0.0292(7) 0.0380(7) -0.0068(5) -0.0210(7) 0.0139(7) Ag3 0.0469(8) 0.0344(7) 0.0297(6) -0.0059(5) 0.0022(5) -0.0019(6) Cl1 0.059(3) 0.0245(18) 0.0193(16) -0.0002(13) 0.0019(16) -0.0002(17) Cl2 0.047(2) 0.0279(18) 0.0205(16) -0.0026(13) 0.0017(15) -0.0009(16) S1 0.050(3) 0.0260(19) 0.0215(17) -0.0052(14) 0.0064(16) -0.0009(17) C1 0.046(10) 0.034(8) 0.011(6) -0.004(6) 0.013(6) 0.008(7) N11 0.075(11) 0.026(7) 0.019(6) 0.007(5) 0.001(7) 0.000(7) N12 0.050(9) 0.023(6) 0.032(7) 0.005(5) 0.001(6) 0.004(6) S2 0.046(2) 0.0241(18) 0.0192(16) -0.0015(14) 0.0042(16) -0.0006(16) C2 0.029(8) 0.020(7) 0.023(7) 0.001(5) 0.009(6) -0.002(6) N21 0.042(8) 0.028(7) 0.024(6) -0.003(5) -0.002(6) 0.003(6) N22 0.054(9) 0.031(7) 0.017(6) -0.008(5) -0.001(6) 0.004(6) S3 0.043(2) 0.029(2) 0.0279(19) -0.0012(15) 0.0039(17) -0.0005(16) C3 0.052(11) 0.037(9) 0.019(7) 0.002(6) 0.004(7) -0.002(8) N31 0.051(10) 0.037(8) 0.054(10) 0.002(7) -0.001(8) 0.005(7) N32 0.034(8) 0.049(9) 0.043(8) -0.005(7) -0.008(6) 0.004(7) S4 0.053(3) 0.0222(18) 0.0269(18) 0.0010(14) -0.0015(17) -0.0003(17) C4 0.073(13) 0.027(8) 0.021(8) -0.003(6) 0.019(8) -0.006(8) N41 0.051(10) 0.035(8) 0.067(11) 0.018(7) -0.013(8) -0.011(7) N42 0.071(12) 0.030(8) 0.042(8) 0.013(6) 0.004(8) -0.006(7) N1 0.062(11) 0.039(9) 0.038(8) -0.004(7) 0.008(8) 0.000(8) O11 0.045(8) 0.048(7) 0.049(7) 0.015(6) -0.016(6) -0.006(6) O12 0.089(12) 0.029(7) 0.068(9) -0.009(6) -0.022(8) 0.009(7) O13 0.063(10) 0.042(8) 0.069(10) 0.006(7) -0.021(8) -0.004(7) O1 0.048(8) 0.051(7) 0.025(6) 0.009(5) 0.005(5) 0.003(6) #----------------------------------------------------------------------------# # 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 2.463(5) . ? Ag1 S4 2.488(5) . ? Ag1 Cl1 2.667(4) . ? Ag1 Cl1 2.713(4) 4_565 ? Ag2 S2 2.478(4) . ? Ag2 S1 2.479(4) . ? Ag2 Cl2 2.643(4) . ? Ag3 S3 2.513(4) 4_575 ? Ag3 S2 2.556(4) . ? Ag3 S3 2.597(4) . ? Ag3 S4 2.700(4) . ? Cl1 Ag1 2.713(4) 4_566 ? S1 C1 1.752(14) . ? C1 N12 1.31(2) . ? C1 N11 1.32(2) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.745(14) . ? C2 N21 1.306(19) . ? C2 N22 1.32(2) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.762(18) . ? S3 Ag3 2.513(4) 4_576 ? C3 N31 1.28(2) . ? C3 N32 1.32(2) . ? N31 H31A 0.88 . ? N31 H31B 0.88 . ? N32 H32A 0.88 . ? N32 H32B 0.88 . ? S4 C4 1.730(18) . ? C4 N42 1.32(2) . ? C4 N41 1.34(2) . ? N41 H41A 0.88 . ? N41 H41B 0.88 . ? N42 H42A 0.88 . ? N42 H42B 0.88 . ? N1 O12 1.22(2) . ? N1 O13 1.24(2) . ? N1 O11 1.26(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S4 137.37(13) . . ? S1 Ag1 Cl1 108.00(13) . . ? S4 Ag1 Cl1 104.64(14) . . ? S1 Ag1 Cl1 106.77(13) . 4_565 ? S4 Ag1 Cl1 96.87(13) . 4_565 ? Cl1 Ag1 Cl1 94.88(6) . 4_565 ? S2 Ag2 S1 137.26(14) . . ? S2 Ag2 Cl2 114.22(13) . . ? S1 Ag2 Cl2 108.50(13) . . ? S3 Ag3 S2 124.74(13) 4_575 . ? S3 Ag3 S3 120.77(17) 4_575 . ? S2 Ag3 S3 101.98(13) . . ? S3 Ag3 S4 102.44(12) 4_575 . ? S2 Ag3 S4 105.69(13) . . ? S3 Ag3 S4 96.70(13) . . ? Ag1 Cl1 Ag1 150.20(16) . 4_566 ? C1 S1 Ag1 104.8(6) . . ? C1 S1 Ag2 105.3(5) . . ? Ag1 S1 Ag2 91.66(15) . . ? N12 C1 N11 118.9(13) . . ? N12 C1 S1 120.2(12) . . ? N11 C1 S1 120.9(12) . . ? 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 Ag2 105.0(5) . . ? C2 S2 Ag3 104.6(5) . . ? Ag2 S2 Ag3 117.49(15) . . ? N21 C2 N22 117.8(13) . . ? N21 C2 S2 123.0(11) . . ? N22 C2 S2 119.2(11) . . ? 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 Ag3 111.1(5) . 4_576 ? C3 S3 Ag3 98.5(6) . . ? Ag3 S3 Ag3 101.22(15) 4_576 . ? N31 C3 N32 122.3(17) . . ? N31 C3 S3 116.5(14) . . ? N32 C3 S3 121.1(14) . . ? C3 N31 H31A 120 . . ? C3 N31 H31B 120 . . ? H31A N31 H31B 120 . . ? C3 N32 H32A 120 . . ? C3 N32 H32B 120 . . ? H32A N32 H32B 120 . . ? C4 S4 Ag1 101.7(6) . . ? C4 S4 Ag3 116.2(6) . . ? Ag1 S4 Ag3 114.16(17) . . ? N42 C4 N41 116.9(16) . . ? N42 C4 S4 122.5(15) . . ? N41 C4 S4 120.4(12) . . ? C4 N41 H41A 120 . . ? C4 N41 H41B 120 . . ? H41A N41 H41B 120 . . ? C4 N42 H42A 120 . . ? C4 N42 H42B 120 . . ? H42A N42 H42B 120 . . ? O12 N1 O13 121.0(16) . . ? O12 N1 O11 120.8(15) . . ? O13 N1 O11 118.2(15) . . ? 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 N11 H11B Cl1 0.88 2.67 3.376(16) 138.2 . N11 H11A O1 0.88 2.06 2.855(18) 149.2 . N12 H12A O1 0.88 2.27 3.007(17) 141.7 . N12 H12B Cl2 0.88 2.42 3.270(13) 162.8 . N12 H12A Cl2 0.88 2.7 3.283(14) 124.8 4_576 N21 H21B Cl2 0.88 2.46 3.320(14) 165.4 . N21 H21A Cl1 0.88 2.49 3.293(14) 152.5 1_565 N22 H22A Cl1 0.88 2.41 3.232(13) 155.6 1_565 N31 H31A O13 0.88 2.04 2.84(2) 150.7 2 N31 H31B O11 0.88 2.13 3.00(2) 171.1 1_565 N32 H32A O12 0.88 2.34 3.12(2) 146.8 2 N32 H32A O12 0.88 2.51 3.08(2) 123.3 4_566 N42 H42B Cl1 0.88 2.55 3.375(17) 155.5 . N41 H41A O13 0.88 1.92 2.80(2) 178.5 . N42 H42A O11 0.88 2.18 3.05(2) 170.9 . #===END data_gb0918 _database_code_depnum_ccdc_archive 'CCDC 759157' #TrackingRef 'gb0918.cif' _audit_creation_date 2009-11-08T16:24:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C6 H28 Ag2 Cl2 N12 O2 S6' _chemical_formula_moiety 'C6 H24 Ag2 N12 S6, 2(H2 O), 2(Cl)' _chemical_formula_weight 779.46 #----------------------------------------------------------------------------# # 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 6.1240(6) _cell_length_b 9.9644(9) _cell_length_c 11.0625(5) _cell_angle_alpha 99.931(5) _cell_angle_beta 92.390(5) _cell_angle_gamma 102.725(8) _cell_volume 646.37(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5674 _cell_measurement_theta_min 3.5816 _cell_measurement_theta_max 37.6168 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 8 9 0.1596 0 -1 1 0.1012 0 11 -11 0.0103 -1 5 -15 0.0096 -8 5 -3 0.0249 -1 1 0 0.0417 8 0 -2 0.0185 8 -2 -5 0.0317 -3 -4 -12 0.133 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.236 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.871 #----------------------------------------------------------------------------# # 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 10.4738 _diffrn_orient_matrix_ub_11 -0.0983974663 _diffrn_orient_matrix_ub_12 -0.0545205745 _diffrn_orient_matrix_ub_13 -0.0078642388 _diffrn_orient_matrix_ub_21 -0.0645169732 _diffrn_orient_matrix_ub_22 0.0498280382 _diffrn_orient_matrix_ub_23 0.0183347951 _diffrn_orient_matrix_ub_31 -0.0169452328 _diffrn_orient_matrix_ub_32 0.0070141445 _diffrn_orient_matrix_ub_33 -0.0621743661 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby,' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_unetI/netI 0.0528 _diffrn_reflns_number 11442 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 37.73 _diffrn_reflns_theta_full 36.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 6535 _reflns_number_gt 5049 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _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. ; _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^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6535 _refine_ls_number_parameters 144 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.584 _refine_diff_density_min -1.01 _refine_diff_density_rms 0.166 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 0.62502(2) 0.531909(14) 0.384905(11) 0.01377(3) Uani 1 1 d . . . Cl1 Cl 0.76390(6) 0.04424(4) -0.10286(3) 0.01137(7) Uani 1 1 d . . . S1 S 0.62608(7) 0.72141(4) 0.56886(4) 0.01083(7) Uani 1 1 d . . . C1 C 0.4180(3) 0.81013(17) 0.54656(14) 0.0109(3) Uani 1 1 d . . . N11 N 0.2889(2) 0.78111(16) 0.44280(13) 0.0140(3) Uani 1 1 d . . . H11A H 0.1856 0.8283 0.4334 0.017 Uiso 1 1 calc R . . H11B H 0.3059 0.7145 0.3829 0.017 Uiso 1 1 calc R . . N12 N 0.3923(2) 0.91069(16) 0.63698(13) 0.0137(3) Uani 1 1 d . . . H12A H 0.2891 0.9579 0.6275 0.016 Uiso 1 1 calc R . . H12B H 0.4786 0.9301 0.7063 0.016 Uiso 1 1 calc R . . C2 C 0.6905(3) 0.69779(18) 0.14528(14) 0.0121(3) Uani 1 1 d . . . S2 S 0.45668(7) 0.58952(5) 0.18602(4) 0.01261(7) Uani 1 1 d . . . N21 N 0.8901(2) 0.66708(17) 0.14530(15) 0.0177(3) Uani 1 1 d . . . H21A H 1.0051 0.7238 0.1216 0.021 Uiso 1 1 calc R . . H21B H 0.9078 0.59 0.169 0.021 Uiso 1 1 calc R . . N22 N 0.6726(2) 0.81568(16) 0.10864(13) 0.0150(3) Uani 1 1 d . . . H22A H 0.7911 0.87 0.0856 0.018 Uiso 1 1 calc R . . H22B H 0.5424 0.8393 0.1075 0.018 Uiso 1 1 calc R . . S3 S 0.97175(7) 0.44250(4) 0.33504(3) 0.01078(7) Uani 1 1 d . . . C3 C 0.8908(3) 0.31501(18) 0.20585(14) 0.0121(3) Uani 1 1 d . . . N31 N 1.0209(3) 0.22730(17) 0.17179(13) 0.0172(3) Uani 1 1 d . . . H31A H 0.9799 0.1614 0.1057 0.021 Uiso 1 1 calc R . . H31B H 1.1482 0.235 0.2152 0.021 Uiso 1 1 calc R . . N32 N 0.7005(3) 0.29907(18) 0.13719(13) 0.0188(3) Uani 1 1 d . . . H32A H 0.6645 0.2321 0.0717 0.023 Uiso 1 1 calc R . . H32B H 0.6103 0.3555 0.1572 0.023 Uiso 1 1 calc R . . O1 O 0.0154(2) 0.97366(14) 0.36902(11) 0.0134(2) Uani 1 1 d D . . H1AO H 0.053(4) 0.959(2) 0.2985(14) 0.023(6) Uiso 1 1 d D . . H1BO H 0.094(4) 1.050(2) 0.4034(19) 0.035(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01630(6) 0.01477(6) 0.01245(5) 0.00247(4) 0.00335(4) 0.00795(5) Cl1 0.01211(16) 0.01091(16) 0.01161(15) 0.00137(12) 0.00139(12) 0.00427(13) S1 0.01048(17) 0.00962(17) 0.01249(16) 0.00057(13) -0.00057(13) 0.00397(14) C1 0.0102(6) 0.0095(7) 0.0134(6) 0.0029(5) 0.0023(5) 0.0022(5) N11 0.0148(6) 0.0132(7) 0.0148(6) 0.0014(5) -0.0022(5) 0.0067(5) N12 0.0123(6) 0.0138(7) 0.0151(6) -0.0014(5) -0.0006(5) 0.0066(5) C2 0.0121(7) 0.0148(7) 0.0100(6) 0.0027(5) 0.0006(5) 0.0040(6) S2 0.00979(17) 0.01499(19) 0.01375(16) 0.00463(14) 0.00103(13) 0.00284(15) N21 0.0120(6) 0.0161(7) 0.0282(8) 0.0107(6) 0.0054(6) 0.0046(6) N22 0.0130(6) 0.0156(7) 0.0192(6) 0.0082(5) 0.0028(5) 0.0053(5) S3 0.01076(16) 0.01013(17) 0.01101(15) -0.00070(13) -0.00029(13) 0.00380(14) C3 0.0171(7) 0.0107(7) 0.0093(6) 0.0018(5) 0.0023(5) 0.0049(6) N31 0.0225(7) 0.0176(7) 0.0140(6) -0.0007(5) 0.0003(5) 0.0128(6) N32 0.0204(7) 0.0209(8) 0.0138(6) -0.0056(5) -0.0052(5) 0.0099(6) O1 0.0136(6) 0.0140(6) 0.0127(5) 0.0015(4) 0.0017(4) 0.0041(5) #----------------------------------------------------------------------------# # 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 S3 2.5235(5) . ? Ag1 S1 2.5249(5) . ? Ag1 S2 2.5963(4) . ? Ag1 S1 2.7926(5) 2_666 ? Ag1 Ag1 3.1126(3) 2_666 ? S1 C1 1.7352(16) . ? S1 Ag1 2.7926(5) 2_666 ? C1 N11 1.317(2) . ? C1 N12 1.329(2) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? C2 N21 1.324(2) . ? C2 N22 1.332(2) . ? C2 S2 1.7199(18) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.7144(16) . ? C3 N31 1.326(2) . ? C3 N32 1.328(2) . ? N31 H31A 0.88 . ? N31 H31B 0.88 . ? N32 H32A 0.88 . ? N32 H32B 0.88 . ? O1 H1AO 0.822(15) . ? O1 H1BO 0.826(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ag1 S1 121.834(15) . . ? S3 Ag1 S2 108.418(14) . . ? S1 Ag1 S2 111.184(15) . . ? S3 Ag1 S1 95.389(15) . 2_666 ? S1 Ag1 S1 108.545(13) . 2_666 ? S2 Ag1 S1 110.132(15) . 2_666 ? Ag1 S1 Ag1 71.455(13) . 2_666 ? N11 C1 N12 119.99(15) . . ? N11 C1 S1 121.71(13) . . ? N12 C1 S1 118.30(12) . . ? C1 N11 H11A 120 . . ? C1 N11 H11B 120 . . ? H11A N11 H11B 120 . . ? C1 N12 H12A 120 . . ? C1 N12 H12B 120 . . ? H12A N12 H12B 120 . . ? N21 C2 N22 117.64(16) . . ? N21 C2 S2 122.56(13) . . ? N22 C2 S2 119.78(13) . . ? C2 S2 Ag1 99.86(5) . . ? 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 105.27(6) . . ? N31 C3 N32 117.67(15) . . ? N31 C3 S3 119.61(13) . . ? N32 C3 S3 122.72(13) . . ? C3 N31 H31A 120 . . ? C3 N31 H31B 120 . . ? H31A N31 H31B 120 . . ? C3 N32 H32A 120 . . ? C3 N32 H32B 120 . . ? H32A N32 H32B 120 . . ? H1AO O1 H1BO 106.9(19) . . ? 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 N11 H11A O1 0.88 2.16 2.9993(19) 160.2 . N11 H11B S2 0.88 2.62 3.4651(15) 160.2 . N12 H12A O1 0.88 2.12 2.9741(19) 163.1 2_576 N12 H12B Cl1 0.88 2.61 3.4686(14) 166.7 1_566 N21 H21A Cl1 0.88 2.48 3.2936(17) 154.5 2_765 N21 H21B S3 0.88 2.61 3.4189(16) 153.3 . N22 H22A Cl1 0.88 2.66 3.4333(16) 147.4 2_765 N22 H22B Cl1 0.88 2.42 3.2801(15) 167 2_665 N31 H31A Cl1 0.88 2.56 3.3852(16) 155.7 . N31 H31B S1 0.88 2.63 3.4143(15) 149.3 2_766 N32 H32A Cl1 0.88 2.64 3.4417(16) 152.5 . N32 H32B S2 0.88 2.68 3.5113(17) 159 . O1 H1AO Cl1 0.822(15) 2.476(16) 3.2842(13) 168(2) 2_665 O1 H1BO S1 0.826(16) 2.490(18) 3.2773(14) 160(2) 2_676 data_gb0952 _database_code_depnum_ccdc_archive 'CCDC 759158' #TrackingRef 'gb0952.cif' _audit_creation_date 2009-11-17T15:06:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C8 H36 Ag2 Br2 N16 O2 S8' _chemical_formula_moiety 'C6 H24 Ag2 N12 S6, 2(C H4 N2 S), 2(H2 O), 2(Br)' _chemical_formula_weight 1020.57 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.26580(10) _cell_length_b 11.0737(2) _cell_length_c 24.9169(4) _cell_angle_alpha 90 _cell_angle_beta 94.684(2) _cell_angle_gamma 90 _cell_volume 1723.10(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15542 _cell_measurement_theta_min 3.5209 _cell_measurement_theta_max 37.1653 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0632 0 0 -1 0.0504 0 10 27 0.0599 1 -12 -22 0.0154 0 -8 30 0.0493 0 9 -29 0.0369 8 -4 13 0.1186 -9 -4 -1 0.2303 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.978 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.375 _exptl_absorpt_correction_T_max 0.759 #----------------------------------------------------------------------------# # 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 10.4738 _diffrn_orient_matrix_ub_11 -0.0539442332 _diffrn_orient_matrix_ub_12 -0.0443087462 _diffrn_orient_matrix_ub_13 -0.0165968558 _diffrn_orient_matrix_ub_21 -0.007102939 _diffrn_orient_matrix_ub_22 0.0411579568 _diffrn_orient_matrix_ub_23 -0.0218855762 _diffrn_orient_matrix_ub_31 0.0995936046 _diffrn_orient_matrix_ub_32 -0.0210847778 _diffrn_orient_matrix_ub_33 -0.0078745281 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby,' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_number 35235 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 37.28 _diffrn_reflns_theta_full 36.75 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 8699 _reflns_number_gt 6196 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _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. ; _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^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8699 _refine_ls_number_parameters 180 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0521 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.552 _refine_diff_density_min -0.62 _refine_diff_density_rms 0.118 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.006 '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 0.616854(19) 0.383158(11) 0.492910(5) 0.01555(3) Uani 1 1 d . . . Br1 Br 0.98046(2) 0.029784(13) 0.316839(6) 0.01272(3) Uani 1 1 d . . . S1 S 0.52437(6) 0.52412(3) 0.413846(15) 0.01279(7) Uani 1 1 d . . . C1 C 0.2829(2) 0.47986(14) 0.38056(6) 0.0131(3) Uani 1 1 d . . . N11 N 0.1918(2) 0.37640(12) 0.39136(5) 0.0165(3) Uani 1 1 d . . . H11A H 0.0721 0.3544 0.373 0.02 Uiso 1 1 calc R . . H11B H 0.2506 0.3293 0.4169 0.02 Uiso 1 1 calc R . . N12 N 0.1924(2) 0.55025(12) 0.34184(5) 0.0158(3) Uani 1 1 d . . . H12A H 0.0727 0.5276 0.3237 0.019 Uiso 1 1 calc R . . H12B H 0.2522 0.6195 0.3344 0.019 Uiso 1 1 calc R . . S2 S 0.43231(6) 0.17320(3) 0.477234(16) 0.01376(7) Uani 1 1 d . . . C2 C 0.5970(2) 0.11769(14) 0.43122(6) 0.0155(3) Uani 1 1 d . . . N21 N 0.8076(2) 0.12391(14) 0.43819(6) 0.0228(3) Uani 1 1 d . . . H21A H 0.8863 0.0926 0.414 0.027 Uiso 1 1 calc R . . H21B H 0.8694 0.1594 0.467 0.027 Uiso 1 1 calc R . . N22 N 0.5100(2) 0.06313(14) 0.38694(6) 0.0235(3) Uani 1 1 d . . . H22A H 0.5927 0.0327 0.3635 0.028 Uiso 1 1 calc R . . H22B H 0.3699 0.0576 0.3812 0.028 Uiso 1 1 calc R . . S3 S 1.00479(6) 0.35075(4) 0.524973(15) 0.01320(7) Uani 1 1 d . . . C3 C 1.0052(2) 0.24362(14) 0.57451(6) 0.0133(3) Uani 1 1 d . . . N31 N 1.1808(2) 0.22675(13) 0.60695(6) 0.0207(3) Uani 1 1 d . . . H31A H 1.1829 0.1714 0.6323 0.025 Uiso 1 1 calc R . . H31B H 1.2954 0.2708 0.6031 0.025 Uiso 1 1 calc R . . N32 N 0.8345(2) 0.17452(13) 0.58180(6) 0.0189(3) Uani 1 1 d . . . H32A H 0.8412 0.1199 0.6075 0.023 Uiso 1 1 calc R . . H32B H 0.7156 0.1837 0.5608 0.023 Uiso 1 1 calc R . . S4 S 0.57801(6) 0.30761(3) 0.208847(15) 0.01332(7) Uani 1 1 d . . . C4 C 0.3940(2) 0.22209(14) 0.23914(6) 0.0126(3) Uani 1 1 d . . . N41 N 0.4408(2) 0.11028(12) 0.25535(6) 0.0186(3) Uani 1 1 d . . . H41A H 0.345 0.0668 0.2706 0.022 Uiso 1 1 calc R . . H41B H 0.5678 0.0797 0.2509 0.022 Uiso 1 1 calc R . . N42 N 0.1996(2) 0.26350(13) 0.24697(6) 0.0215(3) Uani 1 1 d . . . H42A H 0.1081 0.2172 0.2624 0.026 Uiso 1 1 calc R . . H42B H 0.1626 0.3372 0.2368 0.026 Uiso 1 1 calc R . . O1 O -0.18724(19) 0.39915(12) 0.32290(5) 0.0234(3) Uani 1 1 d D . . H1AO H -0.286(3) 0.4283(18) 0.3414(7) 0.032(6) Uiso 1 1 d D . . H1BO H -0.257(4) 0.376(3) 0.2951(8) 0.074(10) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01515(5) 0.01386(5) 0.01684(6) -0.00088(5) -0.00355(4) 0.00256(4) Br1 0.01197(6) 0.01238(7) 0.01405(7) 0.00106(6) 0.00256(5) -0.00054(5) S1 0.01091(15) 0.01526(17) 0.01192(16) 0.00020(14) -0.00070(13) -0.00129(13) C1 0.0140(7) 0.0147(7) 0.0105(6) -0.0012(5) 0.0007(5) 0.0013(5) N11 0.0138(6) 0.0175(6) 0.0171(6) 0.0031(5) -0.0056(5) -0.0038(5) N12 0.0135(6) 0.0186(7) 0.0145(6) 0.0031(5) -0.0031(5) -0.0031(5) S2 0.01294(16) 0.01351(17) 0.01513(17) -0.00161(14) 0.00301(14) 0.00011(13) C2 0.0171(7) 0.0142(7) 0.0150(7) -0.0012(6) 0.0000(6) 0.0012(6) N21 0.0157(6) 0.0335(8) 0.0194(7) -0.0138(6) 0.0016(5) 0.0019(6) N22 0.0166(7) 0.0331(8) 0.0207(7) -0.0136(6) 0.0010(6) 0.0017(6) S3 0.01108(16) 0.01484(17) 0.01351(17) 0.00341(14) 0.00002(13) 0.00012(13) C3 0.0142(7) 0.0134(7) 0.0120(7) 0.0005(5) -0.0003(5) 0.0013(5) N31 0.0227(7) 0.0184(7) 0.0195(7) 0.0088(6) -0.0071(6) -0.0033(6) N32 0.0171(6) 0.0204(7) 0.0185(7) 0.0087(6) -0.0014(5) -0.0033(5) S4 0.01423(16) 0.01218(16) 0.01377(17) 0.00017(14) 0.00236(14) -0.00280(13) C4 0.0129(6) 0.0138(7) 0.0109(6) -0.0003(5) -0.0008(5) -0.0021(5) N41 0.0165(6) 0.0143(6) 0.0256(7) 0.0068(6) 0.0048(6) 0.0003(5) N42 0.0179(7) 0.0178(7) 0.0298(8) 0.0103(6) 0.0081(6) 0.0035(5) O1 0.0159(6) 0.0354(8) 0.0182(6) -0.0077(6) -0.0029(5) 0.0014(5) #----------------------------------------------------------------------------# # 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 S3 2.5216(4) . ? Ag1 S1 2.5430(4) . ? Ag1 S2 2.6119(4) . ? Ag1 S1 2.7516(4) 3_666 ? Ag1 Ag1 3.0083(2) 3_666 ? S1 C1 1.7356(15) . ? S1 Ag1 2.7516(4) 3_666 ? C1 N11 1.3177(19) . ? C1 N12 1.3306(19) . ? N11 H11A 0.88 . ? N11 H11B 0.88 . ? N12 H12A 0.88 . ? N12 H12B 0.88 . ? S2 C2 1.7179(16) . ? C2 N21 1.318(2) . ? C2 N22 1.335(2) . ? N21 H21A 0.88 . ? N21 H21B 0.88 . ? N22 H22A 0.88 . ? N22 H22B 0.88 . ? S3 C3 1.7118(16) . ? C3 N31 1.324(2) . ? C3 N32 1.339(2) . ? N31 H31A 0.88 . ? N31 H31B 0.88 . ? N32 H32A 0.88 . ? N32 H32B 0.88 . ? S4 C4 1.7141(15) . ? C4 N41 1.328(2) . ? C4 N42 1.3305(19) . ? N41 H41A 0.88 . ? N41 H41B 0.88 . ? N42 H42A 0.88 . ? N42 H42B 0.88 . ? O1 H1AO 0.866(14) . ? O1 H1BO 0.830(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ag1 S1 119.051(13) . . ? S3 Ag1 S2 108.920(13) . . ? S1 Ag1 S2 111.128(13) . . ? S3 Ag1 S1 98.843(12) . 3_666 ? S1 Ag1 S1 110.880(10) . 3_666 ? S2 Ag1 S1 106.829(12) . 3_666 ? C1 S1 Ag1 109.36(5) . . ? C1 S1 Ag1 100.43(5) . 3_666 ? Ag1 S1 Ag1 69.120(10) . 3_666 ? N11 C1 N12 119.43(14) . . ? N11 C1 S1 121.55(12) . . ? N12 C1 S1 118.97(12) . . ? 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 97.79(5) . . ? N21 C2 N22 118.01(14) . . ? N21 C2 S2 122.86(12) . . ? N22 C2 S2 119.10(12) . . ? 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 105.76(5) . . ? N31 C3 N32 118.00(14) . . ? N31 C3 S3 119.34(12) . . ? N32 C3 S3 122.66(12) . . ? C3 N31 H31A 120 . . ? C3 N31 H31B 120 . . ? H31A N31 H31B 120 . . ? C3 N32 H32A 120 . . ? C3 N32 H32B 120 . . ? H32A N32 H32B 120 . . ? N41 C4 N42 117.33(14) . . ? N41 C4 S4 120.61(12) . . ? N42 C4 S4 122.06(12) . . ? C4 N41 H41A 120 . . ? C4 N41 H41B 120 . . ? H41A N41 H41B 120 . . ? C4 N42 H42A 120 . . ? C4 N42 H42B 120 . . ? H42A N42 H42B 120 . . ? H1AO O1 H1BO 102.2(19) . . ? 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 N11 H11A O1 0.88 2.03 2.8198(18) 149.1 . N11 H11B S2 0.88 2.5 3.3744(14) 170.6 . N12 H12A O1 0.88 2.16 2.9150(18) 143.4 . N12 H12B S4 0.88 2.61 3.4762(13) 167.8 2_655 N21 H21A Br1 0.88 2.63 3.4552(14) 156 . N21 H21B S3 0.88 2.66 3.4751(15) 153.7 . N22 H22A Br1 0.88 2.78 3.5663(14) 149.9 . N22 H22B Br1 0.88 2.83 3.6400(14) 154.6 1_455 N31 H31A Br1 0.88 2.8 3.6070(14) 153.5 3_756 N31 H31B S1 0.88 2.59 3.3836(15) 151.2 3_766 N32 H32A Br1 0.88 2.68 3.5162(14) 158.2 3_756 N32 H32B S2 0.88 2.63 3.4736(14) 161.8 . N41 H41A Br1 0.88 2.67 3.4908(14) 155.2 1_455 N42 H42A Br1 0.88 2.64 3.4649(14) 156.6 1_455 N42 H42B Br1 0.88 2.63 3.4934(14) 165.4 2_655 O1 H1AO S1 0.866(14) 2.477(15) 3.3142(13) 162.7(18) 1_455 O1 H1BO S4 0.830(16) 2.428(16) 3.2534(13) 173(2) 1_455 #===END