Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Graham A Bowmaker' _publ_contact_author_email GA.BOWMAKER@AUCKLAND.AC.NZ _publ_section_title ; Solvent-assisted mechanochemical synthesis of metal complexes ; loop_ _publ_author_name 'Graham A Bowmaker' 'Chaveng Pakawatchai' 'Brian W Skelton' 'Allan H White' #===END # Attachment 'gb0737.cif' data_gb0777 _database_code_depnum_ccdc_archive 'CCDC 675960' _audit_creation_date 2007-12-28T18:52:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C9 H18 Ag Cl N6 S3' _chemical_formula_moiety 'C9 H18 Ag Cl N6 S3' _chemical_formula_weight 449.79 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R_3_c:h _symmetry_space_group_name_Hall r_3_-2"c 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' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 14.73800(10) _cell_length_b 14.73800(10) _cell_length_c 12.29650(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2313.07(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40774 _cell_measurement_theta_min 3.5863 _cell_measurement_theta_max 43.4143 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.81196 _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 -0.015512104 _diffrn_orient_matrix_ub_12 -0.0409384497 _diffrn_orient_matrix_ub_13 -0.0384939749 _diffrn_orient_matrix_ub_21 0.0391317434 _diffrn_orient_matrix_ub_22 -0.0102934319 _diffrn_orient_matrix_ub_23 0.0199144611 _diffrn_orient_matrix_ub_31 -0.0362594086 _diffrn_orient_matrix_ub_32 -0.0361277508 _diffrn_orient_matrix_ub_33 0.0380050088 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_unetI/netI 0.0076 _diffrn_reflns_number 49899 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 43.53 _diffrn_reflns_theta_full 43.53 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\p and \w scans' _reflns_number_total 3907 _reflns_number_gt 3807 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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^)+(0.0210P)^2^+0.9510P] 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 3907 _refine_ls_number_parameters 61 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0157 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.037 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(11) _refine_diff_density_max 0.296 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # 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 0.6667 0.3333 0.908610(8) 0.01399(2) Uani 1 3 d S . . Cl1 Cl 0.6667 0.3333 0.678507(18) 0.00981(4) Uani 1 3 d S . . S1 S 0.479485(12) 0.292968(13) 0.941459(17) 0.01359(2) Uani 1 1 d . . . C1 C 0.40339(5) 0.19151(5) 0.85694(5) 0.01085(8) Uani 1 1 d . . . N2 N 0.43384(4) 0.16824(4) 0.76340(5) 0.01249(7) Uani 1 1 d . . . H2 H 0.4993 0.197 0.7413 0.015 Uiso 1 1 calc R . . C3 C 0.34337(5) 0.08836(5) 0.70288(5) 0.01346(8) Uani 1 1 d . . . H3A H 0.3586 0.0362 0.6697 0.016 Uiso 1 1 calc R . . H3B H 0.3213 0.1202 0.6453 0.016 Uiso 1 1 calc R . . C4 C 0.26043(5) 0.03911(5) 0.79238(6) 0.01483(9) Uani 1 1 d . . . H4A H 0.1905 0.0229 0.7659 0.018 Uiso 1 1 calc R . . H4B H 0.2563 -0.0255 0.8215 0.018 Uiso 1 1 calc R . . N5 N 0.30134(4) 0.12318(5) 0.87383(5) 0.01440(8) Uani 1 1 d . . . H5 H 0.2639 0.1282 0.9268 0.017 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 0.01160(2) 0.01160(2) 0.01877(3) 0 0 0.005800(10) Cl1 0.00957(5) 0.00957(5) 0.01028(9) 0 0 0.00479(2) S1 0.01139(5) 0.01583(6) 0.01411(5) -0.00378(4) -0.00061(4) 0.00723(5) C1 0.00967(18) 0.01180(19) 0.01165(18) 0.00068(15) 0.00110(15) 0.00579(15) N2 0.00996(16) 0.01202(17) 0.01293(17) -0.00109(14) 0.00227(13) 0.00358(14) C3 0.0122(2) 0.0125(2) 0.0140(2) -0.00104(16) 0.00025(16) 0.00482(17) C4 0.01069(19) 0.0127(2) 0.0180(2) -0.00069(17) 0.00189(17) 0.00355(16) N5 0.01045(17) 0.0148(2) 0.01592(19) -0.00070(16) 0.00375(15) 0.00477(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S1 2.54682(16) 2_655 ? Ag1 S1 2.54682(16) 3_665 ? Ag1 S1 2.54682(16) . ? Ag1 Cl1 2.8295(2) . ? S1 C1 1.7020(7) . ? C1 N2 1.3401(8) . ? C1 N5 1.3434(8) . ? N2 C3 1.4656(8) . ? N2 H2 0.88 . ? C3 C4 1.5314(9) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 N5 1.4679(9) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? N5 H5 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 S1 117.534(3) 2_655 3_665 ? S1 Ag1 S1 117.534(3) 2_655 . ? S1 Ag1 S1 117.534(3) 3_665 . ? S1 Ag1 Cl1 99.126(5) 2_655 . ? S1 Ag1 Cl1 99.126(5) 3_665 . ? S1 Ag1 Cl1 99.126(5) . . ? C1 S1 Ag1 105.63(2) . . ? N2 C1 N5 109.48(6) . . ? N2 C1 S1 126.23(5) . . ? N5 C1 S1 124.27(5) . . ? C1 N2 C3 110.78(5) . . ? C1 N2 H2 124.6 . . ? C3 N2 H2 124.6 . . ? N2 C3 C4 101.87(5) . . ? N2 C3 H3A 111.4 . . ? C4 C3 H3A 111.4 . . ? N2 C3 H3B 111.4 . . ? C4 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? N5 C4 C3 101.34(5) . . ? N5 C4 H4A 111.5 . . ? C3 C4 H4A 111.5 . . ? N5 C4 H4B 111.5 . . ? C3 C4 H4B 111.5 . . ? H4A C4 H4B 109.3 . . ? C1 N5 C4 111.14(5) . . ? C1 N5 H5 124.4 . . ? C4 N5 H5 124.4 . . ? #===END # Attachment 'agetcl.cif' data_agetcl _database_code_depnum_ccdc_archive 'CCDC 681829' _audit_creation_date 2007-01-05T16:21:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C18 H36 Ag4 Cl4 N12 S6' _chemical_formula_moiety 'C18 H36 Ag4 Cl N12 S6, 3(Cl)' _chemical_formula_weight 1186.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C_2_2_21 _symmetry_space_group_name_Hall c_2c_2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 15.9435(2) _cell_length_b 16.2883(2) _cell_length_c 14.6276(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3798.68(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 2.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.676 _exptl_crystal_description prism _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _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 ? _exptl_absorpt_correction_T_max ? #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .019 _diffrn_reflns_av_unetI/netI 0.0169 _diffrn_reflns_number 12883 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.2 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 4621 _reflns_number_gt 4361 _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 _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^)+(0.0491P)^2^+13.6866P] 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 4621 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack .01(4) _refine_diff_density_max 1.912 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # 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 0.92538(3) 0.59705(2) 0.59627(3) 0.04901(11) Uani 1 1 d . . . Ag2 Ag 0.89453(3) 0.63246(3) 0.38350(3) 0.05257(12) Uani 1 1 d . . . Cl1 Cl 1.03492(11) 0.5 0.5 0.0451(4) Uani 1 2 d S . . Cl2 Cl 0.95344(13) 1 0.5 0.0554(5) Uani 1 2 d S . . Cl3 Cl 0.74273(7) 0.76339(7) 0.79942(11) 0.0486(3) Uani 1 1 d . . . S1 S 0.91916(7) 0.73597(7) 0.51237(8) 0.0381(2) Uani 1 1 d . . . C11 C 1.0240(3) 0.7577(3) 0.4951(3) 0.0326(8) Uani 1 1 d . . . N12 N 1.0539(3) 0.8337(3) 0.4867(4) 0.0468(10) Uani 1 1 d . . . H12 H 1.0232 0.8771 0.4861 0.056 Uiso 1 1 calc R . . C13 C 1.1458(4) 0.8345(4) 0.4784(5) 0.0544(14) Uani 1 1 d . . . H13A H 1.172 0.8547 0.5339 0.065 Uiso 1 1 calc R . . H13B H 1.1638 0.8678 0.4271 0.065 Uiso 1 1 calc R . . C14 C 1.1658(3) 0.7435(3) 0.4628(4) 0.0483(12) Uani 1 1 d . . . H14A H 1.1801 0.7329 0.3994 0.058 Uiso 1 1 calc R . . H14B H 1.2115 0.7253 0.5016 0.058 Uiso 1 1 calc R . . N15 N 1.0863(2) 0.7030(2) 0.4881(3) 0.0438(9) Uani 1 1 d . . . H15 H 1.0807 0.6512 0.4972 0.053 Uiso 1 1 calc R . . S2 S 0.80486(7) 0.49550(6) 0.61941(7) 0.03258(19) Uani 1 1 d . . . C21 C 0.7824(2) 0.5026(2) 0.7353(3) 0.0280(7) Uani 1 1 d . . . N22 N 0.7726(4) 0.4397(3) 0.7903(3) 0.0592(14) Uani 1 1 d . . . H22 H 0.7772 0.3894 0.7732 0.071 Uiso 1 1 calc R . . C23 C 0.7530(4) 0.4647(3) 0.8836(3) 0.0480(11) Uani 1 1 d . . . H23A H 0.7935 0.4427 0.9267 0.058 Uiso 1 1 calc R . . H23B H 0.6972 0.4472 0.9012 0.058 Uiso 1 1 calc R . . C24 C 0.7587(4) 0.5580(3) 0.8780(3) 0.0452(11) Uani 1 1 d . . . H24A H 0.7077 0.5838 0.9 0.054 Uiso 1 1 calc R . . H24B H 0.8061 0.5786 0.9128 0.054 Uiso 1 1 calc R . . N25 N 0.7702(4) 0.5717(2) 0.7801(3) 0.0493(11) Uani 1 1 d . . . H25 H 0.7691 0.6193 0.7547 0.059 Uiso 1 1 calc R . . S3 S 1 0.63193(14) 0.75 0.0659(6) Uani 1 2 d S . . C31 C 1 0.7377(5) 0.75 0.0412(14) Uani 1 2 d S . . N32 N 0.9365(3) 0.7842(3) 0.7749(4) 0.0589(13) Uani 1 1 d . . . H32 H 0.8908 0.7659 0.7984 0.071 Uiso 1 1 calc R . . C33 C 0.9534(4) 0.8704(4) 0.7576(6) 0.0662(17) Uani 1 1 d . . . H33A H 0.9381 0.9041 0.8097 0.079 Uiso 1 1 calc R . . H33B H 0.9236 0.8897 0.7039 0.079 Uiso 1 1 calc R . . S4 S 1 0.66614(12) 0.25 0.0512(5) Uani 1 2 d S . . C41 C 1 0.7716(4) 0.25 0.0394(13) Uani 1 2 d S . . N42 N 0.9342(3) 0.8186(3) 0.2692(4) 0.0550(12) Uani 1 1 d . . . H42 H 0.8858 0.7997 0.2843 0.066 Uiso 1 1 calc R . . C43 C 0.9535(3) 0.9063(3) 0.2617(4) 0.0517(12) Uani 1 1 d . . . H43A H 0.943 0.9345 0.319 0.062 Uiso 1 1 calc R . . H43B H 0.9207 0.9319 0.2137 0.062 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 0.0578(2) 0.04592(19) 0.04328(19) 0.00098(16) 0.00487(16) -0.01540(17) Ag2 0.0593(2) 0.0532(2) 0.0452(2) -0.00214(17) -0.00725(17) -0.02488(19) Cl1 0.0374(7) 0.0332(7) 0.0646(11) -0.0104(7) 0 0 Cl2 0.0501(10) 0.0350(8) 0.0812(14) -0.0080(8) 0 0 Cl3 0.0352(5) 0.0306(5) 0.0800(9) 0.0053(5) 0.0043(5) 0.0013(4) S1 0.0353(5) 0.0360(5) 0.0429(5) -0.0010(4) -0.0020(4) -0.0005(4) C11 0.037(2) 0.0309(19) 0.0302(19) -0.0020(15) -0.0066(16) -0.0035(16) N12 0.045(2) 0.0264(17) 0.069(3) 0.0031(18) -0.003(2) -0.0018(15) C13 0.047(3) 0.043(3) 0.073(4) 0.008(3) -0.006(3) -0.013(2) C14 0.037(2) 0.048(3) 0.060(3) 0.002(2) 0.000(2) -0.005(2) N15 0.036(2) 0.0290(17) 0.066(3) -0.0008(17) -0.0031(19) 0.0000(15) S2 0.0406(5) 0.0295(4) 0.0276(4) 0.0000(4) 0.0010(4) -0.0008(4) C21 0.0291(17) 0.0241(16) 0.0307(18) -0.0004(14) -0.0012(14) 0.0021(15) N22 0.114(5) 0.0289(19) 0.035(2) -0.0028(17) 0.018(2) 0.003(2) C23 0.065(3) 0.045(2) 0.034(2) 0.004(2) 0.006(2) 0.004(2) C24 0.061(3) 0.045(2) 0.030(2) -0.0140(19) 0.002(2) 0.006(2) N25 0.081(3) 0.0267(17) 0.040(2) -0.0064(15) 0.012(2) 0.0013(19) S3 0.0951(17) 0.0468(10) 0.0557(11) 0 -0.0373(12) 0 C31 0.041(3) 0.053(4) 0.030(3) 0 -0.011(2) 0 N32 0.035(2) 0.056(3) 0.086(4) -0.001(3) 0.007(2) -0.004(2) C33 0.054(3) 0.051(3) 0.094(5) 0.003(3) 0.000(3) 0.017(3) S4 0.0602(11) 0.0403(8) 0.0531(10) 0 0.0245(9) 0 C41 0.049(4) 0.041(3) 0.028(3) 0 0.002(2) 0 N42 0.041(2) 0.043(2) 0.081(4) 0.004(2) 0.019(2) 0.0017(19) C43 0.050(3) 0.040(2) 0.066(3) -0.004(3) 0.008(2) 0.007(2) #----------------------------------------------------------------------------# # 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 2.5579(11) . ? Ag1 S1 2.5760(12) . ? Ag1 S3 2.6067(6) . ? Ag1 Cl1 2.7444(12) . ? Ag2 S2 2.5278(11) 3_566 ? Ag2 S1 2.5593(12) . ? Ag2 S4 2.6347(6) . ? Cl1 Ag1 2.7444(12) 3_566 ? S1 C11 1.727(4) . ? C11 N12 1.333(6) . ? C11 N15 1.337(6) . ? N12 C13 1.470(7) . ? N12 H12 0.86 . ? C13 C14 1.534(8) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 N15 1.476(6) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? N15 H15 0.86 . ? S2 C21 1.736(4) . ? S2 Ag2 2.5278(11) 3_566 ? C21 N22 1.312(6) . ? C21 N25 1.317(6) . ? N22 C23 1.458(6) . ? N22 H22 0.86 . ? C23 C24 1.525(7) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 N25 1.461(6) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? N25 H25 0.86 . ? S3 C31 1.723(8) . ? S3 Ag1 2.6067(6) 4_756 ? C31 N32 1.316(7) 4_756 ? C31 N32 1.316(7) . ? N32 C33 1.451(8) . ? N32 H32 0.86 . ? C33 C33 1.503(13) 4_756 ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? S4 C41 1.717(7) . ? S4 Ag2 2.6347(6) 4_755 ? C41 N42 1.329(6) 4_755 ? C41 N42 1.329(6) . ? N42 C43 1.465(7) . ? N42 H42 0.86 . ? C43 C43 1.523(11) 4_755 ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ag1 S1 127.03(4) . . ? S2 Ag1 S3 111.69(4) . . ? S1 Ag1 S3 103.72(6) . . ? S2 Ag1 Cl1 99.99(4) . . ? S1 Ag1 Cl1 106.62(3) . . ? S3 Ag1 Cl1 106.13(4) . . ? S2 Ag2 S1 129.97(4) 3_566 . ? S2 Ag2 S4 121.34(4) 3_566 . ? S1 Ag2 S4 108.11(4) . . ? Ag1 Cl1 Ag1 100.96(6) 3_566 . ? C11 S1 Ag2 100.12(15) . . ? C11 S1 Ag1 102.27(15) . . ? Ag2 S1 Ag1 77.18(3) . . ? N12 C11 N15 110.2(4) . . ? N12 C11 S1 123.4(4) . . ? N15 C11 S1 126.4(3) . . ? C11 N12 C13 111.8(4) . . ? C11 N12 H12 124.1 . . ? C13 N12 H12 124.1 . . ? N12 C13 C14 102.2(4) . . ? N12 C13 H13A 111.3 . . ? C14 C13 H13A 111.3 . . ? N12 C13 H13B 111.3 . . ? C14 C13 H13B 111.3 . . ? H13A C13 H13B 109.2 . . ? N15 C14 C13 102.4(4) . . ? N15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? N15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C11 N15 C14 111.1(4) . . ? C11 N15 H15 124.4 . . ? C14 N15 H15 124.4 . . ? C21 S2 Ag2 100.85(14) . 3_566 ? C21 S2 Ag1 103.95(14) . . ? Ag2 S2 Ag1 96.09(4) 3_566 . ? N22 C21 N25 110.1(4) . . ? N22 C21 S2 124.8(3) . . ? N25 C21 S2 125.0(3) . . ? C21 N22 C23 112.4(4) . . ? C21 N22 H22 123.8 . . ? C23 N22 H22 123.8 . . ? N22 C23 C24 102.4(4) . . ? N22 C23 H23A 111.3 . . ? C24 C23 H23A 111.3 . . ? N22 C23 H23B 111.3 . . ? C24 C23 H23B 111.3 . . ? H23A C23 H23B 109.2 . . ? N25 C24 C23 102.2(4) . . ? N25 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? N25 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C21 N25 C24 112.1(4) . . ? C21 N25 H25 123.9 . . ? C24 N25 H25 123.9 . . ? C31 S3 Ag1 102.59(5) . . ? C31 S3 Ag1 102.59(5) . 4_756 ? Ag1 S3 Ag1 154.83(10) . 4_756 ? N32 C31 N32 109.6(7) 4_756 . ? N32 C31 S3 125.2(3) 4_756 . ? N32 C31 S3 125.2(3) . . ? C31 N32 C33 111.5(5) . . ? C31 N32 H32 124.3 . . ? C33 N32 H32 124.3 . . ? N32 C33 C33 102.1(3) . 4_756 ? N32 C33 H33A 111.4 . . ? C33 C33 H33A 111.4 4_756 . ? N32 C33 H33B 111.4 . . ? C33 C33 H33B 111.4 4_756 . ? H33A C33 H33B 109.2 . . ? C41 S4 Ag2 102.02(4) . 4_755 ? C41 S4 Ag2 102.02(4) . . ? Ag2 S4 Ag2 155.96(8) 4_755 . ? N42 C41 N42 109.6(6) 4_755 . ? N42 C41 S4 125.2(3) 4_755 . ? N42 C41 S4 125.2(3) . . ? C41 N42 C43 112.4(5) . . ? C41 N42 H42 123.8 . . ? C43 N42 H42 123.8 . . ? N42 C43 C43 102.8(3) . 4_755 ? N42 C43 H43A 111.2 . . ? C43 C43 H43A 111.2 4_755 . ? N42 C43 H43B 111.2 . . ? C43 C43 H43B 111.2 4_755 . ? H43A C43 H43B 109.1 . . ?