# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rosa Pedrido Castineiras' _publ_contact_author_email ROSA.PEDRIDO@USC.ES _publ_section_title ; Coordinative Trends of a Tridentate Thiosemicarbazone Ligand: Synthesis, Characterization, Luminescence Studies and Desulfurization Processes ; _publ_requested_category FM loop_ _publ_author_name 'Rosa Pedrido Castineiras' 'Manuel R. Bermejo' 'Ana M. Gonzalez-Noya' ; M.Martinez-Calvo ; 'Maria J Romero' 'Guillermo Zaragoza' # Attachment '1.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-02-25 at 17:10:44 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.reqdat # CIF files read : 2004be15 struct data_2004be15 _database_code_depnum_ccdc_archive 'CCDC 724495' _audit_creation_date 2009-02-25T17:10:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C9 H12 N4 S1' _chemical_formula_sum 'C9 H12 N4 S' _chemical_formula_weight 208.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 13.8982(6) _cell_length_b 13.8982(6) _cell_length_c 22.2966(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4306.8(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1949 _cell_measurement_theta_min 0.99 _cell_measurement_theta_max 66.6 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_coefficient_mu 2.407 _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.64 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_device '135mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 14 _diffrn_radiation_monochromator 'graded mirror' _diffrn_measurement_method CCD _diffrn_orient_matrix_ub_11 0.0602719 _diffrn_orient_matrix_ub_12 0.0373552 _diffrn_orient_matrix_ub_13 -0.0076075 _diffrn_orient_matrix_ub_21 0.0040867 _diffrn_orient_matrix_ub_22 -0.0281821 _diffrn_orient_matrix_ub_23 -0.0411877 _diffrn_orient_matrix_ub_31 -0.0390853 _diffrn_orient_matrix_ub_32 0.0546573 _diffrn_orient_matrix_ub_33 -0.0160377 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_number 11934 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 66.65 _diffrn_reflns_theta_full 66.65 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 1909 _reflns_number_gt 1611 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 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^)+(0.0592P)^2^+2.4318P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1909 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.128 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # 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' 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 S1 S 0.13936(4) 0.43637(5) 0.39314(2) 0.0695(2) Uani 1 1 d . . . N4 N 0.21550(12) 0.42735(12) 0.50269(7) 0.0574(4) Uani 1 1 d . . . H4 H 0.2647 0.4164 0.5251 0.069 Uiso 1 1 calc R . . N2 N 0.39215(11) 0.39545(11) 0.46465(7) 0.0521(4) Uani 1 1 d . . . N3 N 0.31933(11) 0.40902(12) 0.42433(7) 0.0555(4) Uani 1 1 d . . . H3 H 0.3314 0.4083 0.3865 0.067 Uiso 1 1 calc R . . N1 N 0.64371(12) 0.36066(12) 0.45392(7) 0.0580(4) Uani 1 1 d . . . C7 C 0.22792(14) 0.42369(13) 0.44378(8) 0.0515(5) Uani 1 1 d . . . C5 C 0.55895(14) 0.36983(13) 0.48222(8) 0.0503(4) Uani 1 1 d . . . C6 C 0.47671(14) 0.38801(14) 0.44331(8) 0.0545(5) Uani 1 1 d . . . H6 H 0.4862 0.3943 0.4022 0.065 Uiso 1 1 calc R . . C4 C 0.55022(15) 0.36044(14) 0.54402(9) 0.0579(5) Uani 1 1 d . . . H4A H 0.4909 0.3684 0.5627 0.07 Uiso 1 1 calc R . . C1 C 0.72084(16) 0.33985(16) 0.48736(10) 0.0666(6) Uani 1 1 d . . . H1 H 0.7799 0.3328 0.4682 0.08 Uiso 1 1 calc R . . C3 C 0.63087(17) 0.33910(16) 0.57687(10) 0.0680(6) Uani 1 1 d . . . H3A H 0.6267 0.332 0.6183 0.082 Uiso 1 1 calc R . . C8 C 0.12483(16) 0.44849(17) 0.53212(10) 0.0680(6) Uani 1 1 d . . . H8A H 0.0885 0.493 0.5074 0.082 Uiso 1 1 calc R . . H8B H 0.1379 0.4801 0.57 0.082 Uiso 1 1 calc R . . C2 C 0.71749(18) 0.32837(16) 0.54841(10) 0.0715(6) Uani 1 1 d . . . H2 H 0.7728 0.3136 0.57 0.086 Uiso 1 1 calc R . . C9 C 0.0647(2) 0.3611(2) 0.54358(14) 0.0983(9) Uani 1 1 d . . . H9A H 0.0059 0.3798 0.563 0.147 Uiso 1 1 calc R . . H9B H 0.0994 0.3174 0.5689 0.147 Uiso 1 1 calc R . . H9C H 0.05 0.3302 0.5062 0.147 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 S1 0.0647(4) 0.0957(5) 0.0481(3) 0.0019(3) -0.0090(2) 0.0020(3) N4 0.0595(9) 0.0707(11) 0.0421(9) -0.0015(7) -0.0009(7) 0.0049(8) N2 0.0594(10) 0.0530(9) 0.0437(9) -0.0007(6) -0.0035(7) -0.0008(7) N3 0.0608(10) 0.0693(10) 0.0364(8) 0.0000(7) -0.0012(7) 0.0022(8) N1 0.0591(10) 0.0651(10) 0.0497(10) 0.0006(8) -0.0011(7) -0.0025(8) C7 0.0603(11) 0.0494(10) 0.0448(10) -0.0014(8) 0.0011(8) -0.0015(8) C5 0.0606(11) 0.0472(9) 0.0431(10) 0.0009(7) -0.0014(8) -0.0049(8) C6 0.0605(12) 0.0606(11) 0.0424(10) 0.0007(8) 0.0005(8) -0.0021(9) C4 0.0679(12) 0.0595(11) 0.0464(11) 0.0000(8) 0.0005(9) -0.0027(9) C1 0.0592(12) 0.0728(14) 0.0678(14) -0.0003(11) -0.0040(10) -0.0013(10) C3 0.0868(16) 0.0705(13) 0.0467(12) 0.0043(10) -0.0110(11) -0.0022(11) C8 0.0686(13) 0.0829(15) 0.0524(12) -0.0029(10) 0.0048(10) 0.0118(11) C2 0.0762(15) 0.0732(14) 0.0651(14) 0.0032(11) -0.0210(12) 0.0014(11) C9 0.0838(18) 0.101(2) 0.110(2) 0.0209(17) 0.0299(16) 0.0009(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 S1 C7 1.680(2) . ? N4 C7 1.326(2) . ? N4 C8 1.451(3) . ? N4 H4 0.86 . ? N2 C6 1.272(2) . ? N2 N3 1.367(2) . ? N3 C7 1.358(2) . ? N3 H3 0.86 . ? N1 C1 1.337(3) . ? N1 C5 1.342(2) . ? C5 C4 1.389(3) . ? C5 C6 1.457(3) . ? C6 H6 0.93 . ? C4 C3 1.371(3) . ? C4 H4A 0.93 . ? C1 C2 1.371(3) . ? C1 H1 0.93 . ? C3 C2 1.369(3) . ? C3 H3A 0.93 . ? C8 C9 1.496(4) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C2 H2 0.93 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 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 C7 N4 C8 124.67(17) . . ? C7 N4 H4 117.7 . . ? C8 N4 H4 117.7 . . ? C6 N2 N3 116.71(16) . . ? C7 N3 N2 120.23(15) . . ? C7 N3 H3 119.9 . . ? N2 N3 H3 119.9 . . ? C1 N1 C5 117.50(18) . . ? N4 C7 N3 116.36(17) . . ? N4 C7 S1 124.52(15) . . ? N3 C7 S1 119.12(14) . . ? N1 C5 C4 122.27(18) . . ? N1 C5 C6 115.15(17) . . ? C4 C5 C6 122.57(18) . . ? N2 C6 C5 121.08(17) . . ? N2 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C3 C4 C5 118.6(2) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N1 C1 C2 123.5(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? N4 C8 C9 113.5(2) . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 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 C6 N2 N3 C7 -175.84(17) . . . . ? C8 N4 C7 N3 175.85(18) . . . . ? C8 N4 C7 S1 -3.8(3) . . . . ? N2 N3 C7 N4 2.4(3) . . . . ? N2 N3 C7 S1 -177.93(13) . . . . ? C1 N1 C5 C4 1.4(3) . . . . ? C1 N1 C5 C6 -177.23(17) . . . . ? N3 N2 C6 C5 -177.68(16) . . . . ? N1 C5 C6 N2 178.07(17) . . . . ? C4 C5 C6 N2 -0.5(3) . . . . ? N1 C5 C4 C3 -1.4(3) . . . . ? C6 C5 C4 C3 177.12(19) . . . . ? C5 N1 C1 C2 -0.5(3) . . . . ? C5 C4 C3 C2 0.5(3) . . . . ? C7 N4 C8 C9 88.8(3) . . . . ? C4 C3 C2 C1 0.3(3) . . . . ? N1 C1 C2 C3 -0.3(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 N4 H4 S1 0.86 2.74 3.4561(17) 141 3 N3 H3 N1 0.86 2.18 3.028(2) 168.6 12_656 # END of CIF # Attachment '7.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-02-25 at 17:47:05 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.reqdat # CIF files read : be03mj1n struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_be03mj1n _database_code_depnum_ccdc_archive 'CCDC 724496' _audit_creation_date 2009-02-25T17:47:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H22 Cu2 N8 O4 S3' _chemical_formula_sum 'C18 H22 Cu2 N8 O4 S3' _chemical_formula_weight 637.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -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' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+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' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, 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' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-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' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 20.8403(16) _cell_length_b 20.8403(16) _cell_length_c 29.327(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 11031(2) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.53 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.36 _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5832 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.395 _exptl_absorpt_correction_T_max 0.480 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_number 25575 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3005 _reflns_number_gt 2361 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Saint' _computing_structure_solution 'SIR97 (Altomare et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 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^)+(0.0299P)^2^+24.3797P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3005 _refine_ls_number_parameters 190 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.337 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 Cu1 Cu 0.701946(15) 0.081890(15) 0.230980(10) 0.03513(10) Uani 1 1 d . . . N1 N 0.75245(10) 0.18773(10) 0.25272(7) 0.0379(4) Uani 1 1 d . . . C2 C 0.82723(13) 0.22169(13) 0.24898(8) 0.0387(5) Uani 1 1 d . . . C3 C 0.87201(15) 0.29431(15) 0.26323(9) 0.0496(7) Uani 1 1 d . . . H3 H 0.9232 0.3172 0.2602 0.06 Uiso 1 1 calc R . . C4 C 0.84030(17) 0.33177(15) 0.28180(10) 0.0570(8) Uani 1 1 d . . . H4 H 0.8697 0.3801 0.2921 0.068 Uiso 1 1 calc R . . C5 C 0.76435(16) 0.29739(15) 0.28520(11) 0.0571(7) Uani 1 1 d . . . H5 H 0.7418 0.3225 0.2972 0.068 Uiso 1 1 calc R . . C6 C 0.72206(15) 0.22498(14) 0.27049(10) 0.0476(6) Uani 1 1 d . . . H6 H 0.6708 0.2016 0.2731 0.057 Uiso 1 1 calc R . . C21 C 0.85439(13) 0.17575(14) 0.22914(9) 0.0426(6) Uani 1 1 d . . . H21 H 0.9047 0.1935 0.2247 0.051 Uiso 1 1 calc R . . N22 N 0.80498(10) 0.10915(11) 0.21799(7) 0.0370(4) Uani 1 1 d . . . N23 N 0.82493(11) 0.06175(12) 0.19982(7) 0.0430(5) Uani 1 1 d . . . C24 C 0.76607(13) -0.00042(14) 0.18588(8) 0.0391(5) Uani 1 1 d . A . S25 S 0.67465(3) -0.01676(3) 0.18573(2) 0.03825(15) Uani 1 1 d . . . N25 N 0.77511(13) -0.05460(13) 0.16951(9) 0.0536(6) Uani 1 1 d . . . C26B C 0.849(3) -0.047(2) 0.1617(12) 0.072(3) Uani 0.398(11) 1 d PD A 2 H26A H 0.848 -0.0745 0.1347 0.086 Uiso 0.398(11) 1 calc PR A 2 H26B H 0.8862 0.0045 0.1576 0.086 Uiso 0.398(11) 1 calc PR A 2 C27B C 0.8654(8) -0.0776(10) 0.2022(6) 0.094(3) Uani 0.398(11) 1 d PD A 2 H27D H 0.8623 -0.0526 0.2289 0.142 Uiso 0.398(11) 1 calc PR A 2 H27E H 0.9145 -0.0705 0.1997 0.142 Uiso 0.398(11) 1 calc PR A 2 H27F H 0.8303 -0.1296 0.2046 0.142 Uiso 0.398(11) 1 calc PR A 2 C26A C 0.844(2) -0.0555(14) 0.1702(8) 0.072(3) Uani 0.602(11) 1 d PD A 1 H26C H 0.8805 -0.0134 0.1878 0.086 Uiso 0.602(11) 1 calc PR A 1 H26D H 0.863 -0.0496 0.1393 0.086 Uiso 0.602(11) 1 calc PR A 1 C27A C 0.8383(5) -0.1238(7) 0.1897(4) 0.094(3) Uani 0.602(11) 1 d PD A 1 H27A H 0.83 -0.1249 0.2219 0.142 Uiso 0.602(11) 1 calc PR A 1 H27B H 0.8833 -0.1245 0.1841 0.142 Uiso 0.602(11) 1 calc PR A 1 H27C H 0.7975 -0.1662 0.1757 0.142 Uiso 0.602(11) 1 calc PR A 1 S1 S 0.5306(3) -0.0047(6) 0.2445(3) 0.0356(12) Uani 0.5 1 d P B -1 O1 O 0.5361(9) -0.0668(9) 0.2656(3) 0.042(2) Uani 0.5 1 d P . . O2 O 0.6047(9) 0.0659(9) 0.2493(3) 0.0349(18) Uani 0.5 1 d P . . O3 O 0.4763(2) 0.0037(2) 0.26989(15) 0.0574(12) Uani 0.5 1 d P . . O4 O 0.5120(2) -0.0190(2) 0.19628(14) 0.0570(10) Uani 0.5 1 d P . . H25 H 0.7372 -0.0922 0.1577 0.068 Uiso 0.602(11) 1 d P A 1 H25B H 0.7363 -0.0963 0.1632 0.068 Uiso 0.398(11) 1 d P 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 Cu1 0.02422(14) 0.02802(15) 0.04813(18) -0.00211(12) -0.00091(11) 0.00928(11) N1 0.0292(9) 0.0296(9) 0.0449(11) -0.0006(8) 0.0005(8) 0.0072(8) C2 0.0308(11) 0.0349(12) 0.0388(12) 0.0015(10) -0.0010(9) 0.0077(10) C3 0.0350(13) 0.0403(14) 0.0496(15) -0.0033(12) 0.0010(11) 0.0009(11) C4 0.0544(17) 0.0326(13) 0.0601(17) -0.0090(12) 0.0059(14) 0.0038(12) C5 0.0538(17) 0.0356(14) 0.0703(19) -0.0083(13) 0.0111(14) 0.0137(12) C6 0.0380(13) 0.0352(13) 0.0615(16) -0.0028(12) 0.0042(12) 0.0122(11) C21 0.0245(11) 0.0418(13) 0.0495(14) -0.0002(11) -0.0002(10) 0.0076(10) N22 0.0290(9) 0.0382(10) 0.0394(10) 0.0007(8) 0.0003(8) 0.0136(8) N23 0.0321(10) 0.0457(12) 0.0508(12) -0.0039(10) 0.0004(9) 0.0193(9) C24 0.0382(12) 0.0421(13) 0.0375(12) 0.0016(10) 0.0027(10) 0.0206(11) S25 0.0320(3) 0.0384(3) 0.0421(3) -0.0066(2) -0.0053(2) 0.0159(2) N25 0.0416(12) 0.0489(13) 0.0731(16) -0.0128(12) 0.0006(11) 0.0247(11) C26B 0.054(4) 0.072(5) 0.101(8) -0.009(5) 0.012(7) 0.040(5) C27B 0.082(6) 0.123(8) 0.110(6) 0.020(6) 0.000(4) 0.076(6) C26A 0.054(4) 0.072(5) 0.101(8) -0.009(5) 0.012(7) 0.040(5) C27A 0.082(6) 0.123(8) 0.110(6) 0.020(6) 0.000(4) 0.076(6) S1 0.0218(9) 0.023(2) 0.061(4) -0.0001(19) 0.0034(12) 0.0105(13) O1 0.033(2) 0.029(2) 0.069(6) 0.006(5) 0.008(5) 0.018(2) O2 0.026(2) 0.022(2) 0.055(5) -0.001(4) 0.000(4) 0.0110(18) O3 0.042(2) 0.0330(18) 0.103(3) 0.008(3) 0.029(2) 0.0229(17) O4 0.049(2) 0.054(2) 0.059(2) -0.0079(19) -0.0169(19) 0.0185(19) #----------------------------------------------------------------------------# # 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 Cu1 O1 1.929(17) 4 ? Cu1 N22 1.9643(19) . ? Cu1 O2 1.958(17) . ? Cu1 N1 2.0144(19) . ? Cu1 S25 2.2676(7) . ? Cu1 S25 2.7494(8) 4 ? N1 C6 1.329(3) . ? N1 C2 1.356(3) . ? C2 C3 1.387(3) . ? C2 C21 1.455(4) . ? C3 C4 1.363(4) . ? C3 H3 0.93 . ? C4 C5 1.376(4) . ? C4 H4 0.93 . ? C5 C6 1.382(4) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C21 N22 1.290(3) . ? C21 H21 0.93 . ? N22 N23 1.358(3) . ? N23 C24 1.327(3) . ? C24 N25 1.324(3) . ? C24 S25 1.760(2) . ? S25 Cu1 2.7494(8) 4 ? N25 C26A 1.46(3) . ? N25 C26B 1.48(6) . ? N25 H25 0.860(2) . ? N25 H25B 0.860(2) . ? C26B C27B 1.467(18) . ? C26B H26A 0.97 . ? C26B H26B 0.97 . ? C27B H27D 0.96 . ? C27B H27E 0.96 . ? C27B H27F 0.96 . ? C26A C27A 1.477(16) . ? C26A H26C 0.97 . ? C26A H26D 0.97 . ? C27A H27A 0.96 . ? C27A H27B 0.96 . ? C27A H27C 0.96 . ? S1 O3 1.436(5) . ? S1 O4 1.458(10) . ? S1 O1 1.489(19) . ? S1 O2 1.515(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N22 169.5(4) 4 . ? O1 Cu1 O2 13.0(5) 4 . ? N22 Cu1 O2 172.5(4) . . ? O1 Cu1 N1 95.3(5) 4 . ? N22 Cu1 N1 81.23(8) . . ? O2 Cu1 N1 91.7(4) . . ? O1 Cu1 S25 96.9(5) 4 . ? N22 Cu1 S25 83.75(6) . . ? O2 Cu1 S25 103.7(4) . . ? N1 Cu1 S25 159.20(6) . . ? O1 Cu1 S25 93.3(3) 4 4 ? N22 Cu1 S25 96.95(6) . 4 ? O2 Cu1 S25 81.4(3) . 4 ? N1 Cu1 S25 97.38(6) . 4 ? S25 Cu1 S25 98.65(2) . 4 ? C6 N1 C2 119.1(2) . . ? C6 N1 Cu1 128.52(17) . . ? C2 N1 Cu1 112.38(16) . . ? N1 C2 C3 121.0(2) . . ? N1 C2 C21 114.4(2) . . ? C3 C2 C21 124.6(2) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N1 C6 C5 122.0(3) . . ? N1 C6 H6 119 . . ? C5 C6 H6 119 . . ? N22 C21 C2 116.4(2) . . ? N22 C21 H21 121.8 . . ? C2 C21 H21 121.8 . . ? C21 N22 N23 120.8(2) . . ? C21 N22 Cu1 115.53(17) . . ? N23 N22 Cu1 123.63(15) . . ? C24 N23 N22 111.19(19) . . ? N25 C24 N23 119.2(2) . . ? N25 C24 S25 115.84(19) . . ? N23 C24 S25 124.92(19) . . ? C24 S25 Cu1 93.81(8) . . ? C24 S25 Cu1 103.53(8) . 4 ? Cu1 S25 Cu1 77.41(2) . 4 ? C24 N25 C26A 124.9(11) . . ? C24 N25 C26B 123.3(17) . . ? C24 N25 H25 117.7(2) . . ? C26A N25 H25 117.5(11) . . ? C26B N25 H25 117.8(17) . . ? C24 N25 H25B 118.4(2) . . ? C26A N25 H25B 115.4(11) . . ? C26B N25 H25B 118.4(17) . . ? C27B C26B N25 107(3) . . ? C27B C26B H26A 110.4 . . ? N25 C26B H26A 110.4 . . ? C27B C26B H26B 110.4 . . ? N25 C26B H26B 110.4 . . ? H26A C26B H26B 108.6 . . ? C26B C27B H27D 109.5 . . ? C26B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? N25 C26A C27A 114(2) . . ? N25 C26A H26C 108.7 . . ? C27A C26A H26C 108.7 . . ? N25 C26A H26D 108.7 . . ? C27A C26A H26D 108.7 . . ? H26C C26A H26D 107.6 . . ? O3 S1 O4 112.5(4) . . ? O3 S1 O1 107.4(9) . . ? O4 S1 O1 110.6(7) . . ? O3 S1 O2 108.4(7) . . ? O4 S1 O2 109.0(8) . . ? O1 S1 O2 108.7(4) . . ? S1 O2 Cu1 127.3(9) . . ? 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 O1 Cu1 N1 C6 10.3(4) 4 . . . ? N22 Cu1 N1 C6 -179.7(2) . . . . ? O2 Cu1 N1 C6 -2.2(4) . . . . ? S25 Cu1 N1 C6 136.0(2) . . . . ? S25 Cu1 N1 C6 -83.8(2) 4 . . . ? O1 Cu1 N1 C2 -171.7(3) 4 . . . ? N22 Cu1 N1 C2 -1.69(17) . . . . ? O2 Cu1 N1 C2 175.8(3) . . . . ? S25 Cu1 N1 C2 -45.9(3) . . . . ? S25 Cu1 N1 C2 94.25(16) 4 . . . ? C6 N1 C2 C3 -0.2(4) . . . . ? Cu1 N1 C2 C3 -178.4(2) . . . . ? C6 N1 C2 C21 179.9(2) . . . . ? Cu1 N1 C2 C21 1.7(3) . . . . ? N1 C2 C3 C4 0.8(4) . . . . ? C21 C2 C3 C4 -179.3(3) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C2 N1 C6 C5 0.2(4) . . . . ? Cu1 N1 C6 C5 178.1(2) . . . . ? C4 C5 C6 N1 -0.7(5) . . . . ? N1 C2 C21 N22 -0.5(3) . . . . ? C3 C2 C21 N22 179.6(2) . . . . ? C2 C21 N22 N23 -179.1(2) . . . . ? C2 C21 N22 Cu1 -1.0(3) . . . . ? O1 Cu1 N22 C21 73(2) 4 . . . ? N1 Cu1 N22 C21 1.47(18) . . . . ? S25 Cu1 N22 C21 167.04(19) . . . . ? S25 Cu1 N22 C21 -94.97(18) 4 . . . ? O1 Cu1 N22 N23 -109(2) 4 . . . ? N1 Cu1 N22 N23 179.5(2) . . . . ? S25 Cu1 N22 N23 -14.92(18) . . . . ? S25 Cu1 N22 N23 83.08(18) 4 . . . ? C21 N22 N23 C24 -172.6(2) . . . . ? Cu1 N22 N23 C24 9.4(3) . . . . ? N22 N23 C24 N25 -176.3(2) . . . . ? N22 N23 C24 S25 5.6(3) . . . . ? N25 C24 S25 Cu1 167.9(2) . . . . ? N23 C24 S25 Cu1 -14.0(2) . . . . ? N25 C24 S25 Cu1 90.0(2) . . . 4 ? N23 C24 S25 Cu1 -91.9(2) . . . 4 ? O1 Cu1 S25 C24 -178.3(4) 4 . . . ? N22 Cu1 S25 C24 12.23(10) . . . . ? O2 Cu1 S25 C24 -167.1(3) . . . . ? N1 Cu1 S25 C24 56.16(19) . . . . ? S25 Cu1 S25 C24 -83.88(8) 4 . . . ? O1 Cu1 S25 Cu1 -75.3(3) 4 . . 4 ? N22 Cu1 S25 Cu1 115.26(6) . . . 4 ? O2 Cu1 S25 Cu1 -64.1(3) . . . 4 ? N1 Cu1 S25 Cu1 159.18(17) . . . 4 ? S25 Cu1 S25 Cu1 19.15(3) 4 . . 4 ? N23 C24 N25 C26A 7.6(10) . . . . ? S25 C24 N25 C26A -174.2(10) . . . . ? N23 C24 N25 C26B -6.0(13) . . . . ? S25 C24 N25 C26B 172.3(12) . . . . ? C24 N25 C26B C27B 96(2) . . . . ? C26A N25 C26B C27B -6(12) . . . . ? C24 N25 C26A C27A 128.5(15) . . . . ? C26B N25 C26A C27A -146(16) . . . . ? O3 S1 O2 Cu1 169.3(6) . . . . ? O4 S1 O2 Cu1 -67.9(9) . . . . ? O1 S1 O2 Cu1 52.8(11) . . . . ? O1 Cu1 O2 S1 73(4) 4 . . . ? N1 Cu1 O2 S1 179.9(8) . . . . ? S25 Cu1 O2 S1 14.0(9) . . . . ? S25 Cu1 O2 S1 -82.9(8) 4 . . . ? 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 C4 H4 O3 0.93 2.45 3.125(5) 129.3 2_655 C4 H4 O4 0.93 2.58 3.480(5) 161.9 6_655 N25 H25 O3 0.860(2) 2.103(4) 2.886(5) 151.0(2) 30 N25 H25B O4 0.860(2) 2.137(4) 2.989(5) 170.9(2) 26 # END of CIF # END of CIF # Attachment '9.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-02-27 at 14:14:50 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.reqdat # CIF files read : be27mj2n struct data_be27mj2n _database_code_depnum_ccdc_archive 'CCDC 724497' _audit_creation_date 2009-02-27T14:14:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H66 Ag6 N24 S6, 2(C2 H3 N)' _chemical_formula_sum 'C58 H72 Ag6 N26 S6 ' _chemical_formula_weight 1973.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.997(3) _cell_length_b 16.404(3) _cell_length_c 16.081(3) _cell_angle_alpha 90 _cell_angle_beta 114.899(2) _cell_angle_gamma 90 _cell_volume 3827.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1001 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 26.13 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.900 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_number 33058 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 23.29 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 5528 _reflns_number_gt 3766 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Saint' _computing_structure_solution 'DIRDIF96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 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^)+(0.0233P)^2^+12.0699P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5528 _refine_ls_number_parameters 430 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.658 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.09240(4) 0.61767(4) 0.05537(4) 0.05714(18) Uani 1 1 d . . . Ag2 Ag 0.13250(4) 0.45257(3) 0.00176(4) 0.05764(18) Uani 1 1 d . . . Ag3 Ag 0.04052(4) 0.49357(4) 0.15946(4) 0.06278(19) Uani 1 1 d . . . S4 S 0.19571(14) 0.44978(12) 0.17205(13) 0.0566(5) Uani 1 1 d . . . S5 S 0.06577(13) 0.62675(11) -0.11056(12) 0.0512(5) Uani 1 1 d . . . S6 S -0.04505(14) 0.67393(12) 0.06744(15) 0.0618(5) Uani 1 1 d . . . C7 C -0.0272(6) 0.6672(6) 0.1801(6) 0.076(2) Uani 1 1 d U A . N8 N 0.0206(5) 0.6048(4) 0.2309(5) 0.0674(19) Uani 1 1 d . . . N9 N 0.0332(5) 0.6105(5) 0.3204(6) 0.080(2) Uani 1 1 d . . . C10 C 0.0771(7) 0.5520(7) 0.3713(6) 0.083(3) Uani 1 1 d . . . H10 H 0.0971 0.5097 0.3456 0.1 Uiso 1 1 calc R . . C11 C 0.0979(7) 0.5483(7) 0.4701(7) 0.094(3) Uani 1 1 d U . . N12 N 0.1414(7) 0.4813(6) 0.5119(6) 0.110(3) Uani 1 1 d U . . C13 C 0.1586(10) 0.4741(9) 0.6027(8) 0.141(5) Uani 1 1 d U . . H13 H 0.19 0.4284 0.635 0.169 Uiso 1 1 calc R . . C14 C 0.1314(10) 0.5314(11) 0.6466(9) 0.141(6) Uani 1 1 d U . . H14 H 0.1436 0.5236 0.7079 0.169 Uiso 1 1 calc R . . C15 C 0.0869(9) 0.5994(10) 0.6036(8) 0.134(5) Uani 1 1 d U . . H15 H 0.0687 0.6388 0.6342 0.161 Uiso 1 1 calc R . . C16 C 0.0693(7) 0.6084(8) 0.5122(7) 0.104(3) Uani 1 1 d U . . H16 H 0.0387 0.6543 0.4796 0.124 Uiso 1 1 calc R . . C20 C 0.1703(5) 0.5943(5) -0.1077(5) 0.0513(19) Uani 1 1 d . . . N21 N 0.2005(4) 0.5200(4) -0.0750(4) 0.0550(16) Uani 1 1 d . . . N22 N 0.2801(5) 0.4974(4) -0.0834(4) 0.0642(17) Uani 1 1 d . . . C23 C 0.3128(6) 0.4291(5) -0.0471(6) 0.068(2) Uani 1 1 d . . . H23 H 0.2848 0.4018 -0.015 0.081 Uiso 1 1 calc R . . C24 C 0.3921(6) 0.3920(6) -0.0537(6) 0.076(2) Uani 1 1 d U . . N25 N 0.4142(6) 0.3191(5) -0.0145(6) 0.101(3) Uani 1 1 d U . . C26 C 0.4860(8) 0.2815(8) -0.0183(8) 0.118(4) Uani 1 1 d U . . H26 H 0.5016 0.23 0.008 0.142 Uiso 1 1 calc R . . C27 C 0.5381(9) 0.3142(9) -0.0584(8) 0.130(5) Uani 1 1 d U . . H27 H 0.5882 0.2857 -0.0589 0.156 Uiso 1 1 calc R . . C28 C 0.5159(9) 0.3884(9) -0.0975(9) 0.147(6) Uani 1 1 d U . . H28 H 0.5508 0.4127 -0.1246 0.177 Uiso 1 1 calc R . . C29 C 0.4393(8) 0.4277(7) -0.0961(8) 0.120(4) Uani 1 1 d U . . H29 H 0.421 0.4782 -0.1243 0.144 Uiso 1 1 calc R . . N30 N 0.2160(5) 0.6417(4) -0.1408(5) 0.076(2) Uani 1 1 d D . . H30 H 0.2674 0.6226 -0.1376 0.091 Uiso 1 1 calc R . . C31 C 0.1899(6) 0.7229(5) -0.1826(6) 0.082(3) Uani 1 1 d D . . H31A H 0.1265 0.7338 -0.1933 0.098 Uiso 1 1 calc R . . H31B H 0.1928 0.7228 -0.2416 0.098 Uiso 1 1 calc R . . C32 C 0.2487(7) 0.7890(5) -0.1261(7) 0.101(3) Uani 1 1 d D . . H32A H 0.2457 0.7901 -0.0678 0.151 Uiso 1 1 calc R . . H32B H 0.2277 0.8402 -0.1567 0.151 Uiso 1 1 calc R . . H32C H 0.3113 0.7798 -0.1171 0.151 Uiso 1 1 calc R . . C33 C 0.2668(5) 0.5355(5) 0.2051(5) 0.0552(19) Uani 1 1 d . . . N34 N 0.2389(4) 0.6032(4) 0.1561(4) 0.0540(16) Uani 1 1 d . . . N35 N 0.3023(4) 0.6659(4) 0.1887(4) 0.0575(16) Uani 1 1 d . . . C36 C 0.2812(6) 0.7318(5) 0.1449(6) 0.059(2) Uani 1 1 d . . . H36 H 0.2267 0.7347 0.0918 0.071 Uiso 1 1 calc R . . C37 C 0.3398(6) 0.8040(5) 0.1751(6) 0.062(2) Uani 1 1 d U . . N38 N 0.3150(6) 0.8674(5) 0.1156(6) 0.089(2) Uani 1 1 d U . . C39 C 0.3682(8) 0.9346(6) 0.1427(8) 0.100(3) Uani 1 1 d U . . H39 H 0.3536 0.9792 0.1035 0.121 Uiso 1 1 calc R . . C40 C 0.4398(9) 0.9394(7) 0.2224(8) 0.113(4) Uani 1 1 d U . . H40 H 0.4739 0.9874 0.2388 0.135 Uiso 1 1 calc R . . C41 C 0.4637(9) 0.8773(9) 0.2792(8) 0.144(5) Uani 1 1 d U . . H41 H 0.5145 0.8815 0.3354 0.173 Uiso 1 1 calc R . . C42 C 0.4137(8) 0.8057(7) 0.2558(7) 0.110(4) Uani 1 1 d U . . H42 H 0.4306 0.7607 0.2945 0.133 Uiso 1 1 calc R . . N43 N 0.3480(5) 0.5305(4) 0.2767(4) 0.0716(19) Uani 1 1 d . . . H43 H 0.3868 0.5689 0.2833 0.086 Uiso 1 1 calc R . . C44 C 0.3774(6) 0.4663(6) 0.3450(6) 0.087(3) Uani 1 1 d . . . H44A H 0.4429 0.4569 0.3652 0.105 Uiso 1 1 calc R . . H44B H 0.3453 0.4163 0.3177 0.105 Uiso 1 1 calc R . . C45 C 0.3590(10) 0.4873(8) 0.4250(8) 0.155(6) Uani 1 1 d . . . H45A H 0.3872 0.5387 0.4496 0.233 Uiso 1 1 calc R . . H45B H 0.3841 0.4458 0.471 0.233 Uiso 1 1 calc R . . H45C H 0.2937 0.4911 0.4063 0.233 Uiso 1 1 calc R . . N50 N 0.5307(9) 0.6343(7) 0.3581(8) 0.155(4) Uiso 1 1 d . . . C51 C 0.5969(11) 0.6701(10) 0.3584(10) 0.157(5) Uiso 1 1 d D . . C52 C 0.6752(15) 0.7273(13) 0.3619(16) 0.306(12) Uiso 1 1 d D . . H52A H 0.6533 0.7825 0.3519 0.459 Uiso 1 1 calc R . . H52B H 0.6945 0.7118 0.3151 0.459 Uiso 1 1 calc R . . H52C H 0.7264 0.7231 0.4209 0.459 Uiso 1 1 calc R . . N17 N -0.0560(5) 0.7274(5) 0.2174(5) 0.0946(19) Uani 1 1 d DU . . H17A H -0.0404 0.7246 0.2757 0.114 Uiso 0.630(13) 1 d P A 1 H17B H -0.0438 0.7231 0.2759 0.114 Uiso 0.370(13) 1 d P A 2 C18 C -0.1072(9) 0.8017(10) 0.1620(12) 0.098(2) Uani 0.630(13) 1 d PDU A 1 H18A H -0.0906 0.81 0.1112 0.117 Uiso 0.630(13) 1 calc PR A 1 H18B H -0.0891 0.8498 0.2006 0.117 Uiso 0.630(13) 1 calc PR A 1 C19 C -0.2111(9) 0.7898(11) 0.1254(13) 0.116(3) Uani 0.630(13) 1 d PDU A 1 H19A H -0.2244 0.7332 0.129 0.173 Uiso 0.630(13) 1 calc PR A 1 H19B H -0.2401 0.8075 0.0627 0.173 Uiso 0.630(13) 1 calc PR A 1 H19C H -0.2343 0.8214 0.1615 0.173 Uiso 0.630(13) 1 calc PR A 1 C19B C -0.2002(16) 0.7618(19) 0.216(2) 0.116(3) Uani 0.370(13) 1 d PDU A 2 H19D H -0.2492 0.801 0.1919 0.173 Uiso 0.370(13) 1 calc PR A 2 H19E H -0.1738 0.7633 0.2818 0.173 Uiso 0.370(13) 1 calc PR A 2 H19F H -0.2242 0.7083 0.1952 0.173 Uiso 0.370(13) 1 calc PR A 2 C18B C -0.1289(16) 0.7815(17) 0.184(2) 0.098(2) Uani 0.370(13) 1 d PDU A 2 H18C H -0.156 0.7803 0.1175 0.117 Uiso 0.370(13) 1 calc PR A 2 H18D H -0.1063 0.8362 0.2034 0.117 Uiso 0.370(13) 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 0.0588(4) 0.0585(4) 0.0568(4) 0.0066(3) 0.0269(3) 0.0066(3) Ag2 0.0686(4) 0.0514(4) 0.0539(4) 0.0007(3) 0.0268(3) -0.0036(3) Ag3 0.0667(4) 0.0600(4) 0.0630(4) 0.0013(3) 0.0286(3) -0.0057(3) S4 0.0624(13) 0.0530(12) 0.0519(12) 0.0045(9) 0.0218(10) 0.0009(10) S5 0.0547(12) 0.0509(11) 0.0515(11) 0.0046(9) 0.0259(10) 0.0023(9) S6 0.0622(13) 0.0509(12) 0.0777(14) -0.0125(10) 0.0347(12) -0.0036(10) C7 0.056(4) 0.092(5) 0.086(5) -0.041(4) 0.035(4) -0.008(4) N8 0.072(5) 0.080(5) 0.059(4) -0.022(4) 0.036(4) -0.019(4) N9 0.081(6) 0.097(6) 0.070(5) -0.022(5) 0.039(5) -0.027(5) C10 0.098(8) 0.106(8) 0.062(6) -0.029(6) 0.048(6) -0.045(7) C11 0.089(8) 0.116(8) 0.079(7) -0.021(5) 0.037(6) -0.039(6) N12 0.116(8) 0.125(7) 0.080(6) -0.003(5) 0.033(6) -0.043(6) C13 0.145(12) 0.180(12) 0.079(7) -0.010(7) 0.028(8) -0.056(9) C14 0.119(12) 0.232(17) 0.070(8) -0.013(7) 0.038(8) -0.066(10) C15 0.110(11) 0.220(15) 0.077(7) -0.050(8) 0.044(8) -0.052(9) C16 0.079(7) 0.162(9) 0.075(6) -0.036(6) 0.038(6) -0.041(6) C20 0.060(5) 0.055(5) 0.045(4) -0.002(4) 0.028(4) -0.010(4) N21 0.062(4) 0.050(4) 0.063(4) 0.004(3) 0.036(3) 0.005(3) N22 0.065(4) 0.068(5) 0.068(4) 0.003(4) 0.037(4) 0.006(4) C23 0.079(6) 0.060(5) 0.074(6) 0.006(5) 0.041(5) 0.014(5) C24 0.080(6) 0.087(6) 0.069(6) 0.004(5) 0.040(5) 0.021(5) N25 0.100(6) 0.097(6) 0.125(7) 0.024(5) 0.067(6) 0.040(5) C26 0.103(9) 0.130(9) 0.132(10) 0.023(7) 0.060(8) 0.052(7) C27 0.121(10) 0.182(12) 0.112(9) 0.030(8) 0.073(8) 0.080(9) C28 0.133(10) 0.207(14) 0.155(11) 0.070(10) 0.114(10) 0.079(10) C29 0.123(9) 0.136(9) 0.142(10) 0.056(8) 0.097(8) 0.057(7) N30 0.064(5) 0.078(5) 0.101(6) 0.037(4) 0.049(4) 0.015(4) C31 0.072(6) 0.087(7) 0.095(7) 0.040(6) 0.044(6) 0.009(5) C32 0.131(9) 0.068(6) 0.105(8) -0.004(6) 0.050(7) 0.008(7) C33 0.056(5) 0.062(5) 0.050(5) 0.000(4) 0.025(4) -0.001(4) N34 0.053(4) 0.057(4) 0.050(4) 0.006(3) 0.020(3) -0.003(3) N35 0.054(4) 0.065(4) 0.058(4) 0.002(4) 0.027(3) -0.002(4) C36 0.064(5) 0.056(5) 0.067(5) -0.002(4) 0.038(5) -0.002(4) C37 0.072(6) 0.057(5) 0.072(5) -0.009(4) 0.046(4) -0.007(4) N38 0.098(6) 0.072(5) 0.109(6) 0.008(4) 0.055(5) -0.008(4) C39 0.144(10) 0.071(6) 0.111(8) 0.010(6) 0.078(7) -0.019(6) C40 0.158(11) 0.103(8) 0.106(8) -0.042(6) 0.084(7) -0.060(8) C41 0.138(11) 0.170(12) 0.090(8) 0.003(7) 0.016(7) -0.081(9) C42 0.110(8) 0.123(8) 0.080(7) 0.010(6) 0.021(5) -0.045(7) N43 0.058(4) 0.076(5) 0.062(4) 0.010(4) 0.008(4) -0.001(4) C44 0.082(7) 0.098(7) 0.062(6) 0.022(5) 0.011(5) 0.015(6) C45 0.234(16) 0.148(12) 0.098(9) 0.040(8) 0.083(10) 0.038(11) N17 0.069(3) 0.113(4) 0.096(4) -0.047(3) 0.029(3) 0.011(3) C18 0.068(3) 0.116(4) 0.102(4) -0.048(3) 0.028(3) 0.017(3) C19 0.075(5) 0.130(6) 0.122(6) -0.039(5) 0.022(5) 0.018(5) C19B 0.075(5) 0.130(6) 0.122(6) -0.039(5) 0.022(5) 0.018(5) C18B 0.068(3) 0.116(4) 0.102(4) -0.048(3) 0.028(3) 0.017(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N34 2.231(6) . ? Ag1 S6 2.467(2) . ? Ag1 S5 2.5233(19) . ? Ag1 Ag3 2.9673(9) . ? Ag1 Ag2 2.9927(9) . ? Ag2 N21 2.251(6) . ? Ag2 S6 2.488(2) 3_565 ? Ag2 S4 2.488(2) . ? Ag2 Ag3 3.0201(9) 3_565 ? Ag3 N8 2.250(7) . ? Ag3 S5 2.506(2) 3_565 ? Ag3 S4 2.510(2) . ? Ag3 Ag2 3.0201(9) 3_565 ? S4 C33 1.745(8) . ? S5 C20 1.736(7) . ? S5 Ag3 2.506(2) 3_565 ? S6 C7 1.714(10) . ? S6 Ag2 2.488(2) 3_565 ? C7 N8 1.331(11) . ? C7 N17 1.336(10) . ? N8 N9 1.369(9) . ? N9 C10 1.265(11) . ? C10 C11 1.482(13) . ? C10 H10 0.93 . ? C11 N12 1.323(13) . ? C11 C16 1.377(14) . ? N12 C13 1.372(14) . ? C13 C14 1.353(18) . ? C13 H13 0.93 . ? C14 C15 1.347(18) . ? C14 H14 0.93 . ? C15 C16 1.384(14) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C20 N30 1.324(8) . ? C20 N21 1.334(9) . ? N21 N22 1.385(8) . ? N22 C23 1.270(9) . ? C23 C24 1.450(11) . ? C23 H23 0.93 . ? C24 N25 1.329(11) . ? C24 C29 1.347(12) . ? N25 C26 1.328(11) . ? C26 C27 1.360(15) . ? C26 H26 0.93 . ? C27 C28 1.347(16) . ? C27 H27 0.93 . ? C28 C29 1.393(13) . ? C28 H28 0.93 . ? C29 H29 0.93 . ? N30 C31 1.472(9) . ? N30 H30 0.86 . ? C31 C32 1.472(11) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? C33 N43 1.327(9) . ? C33 N34 1.326(9) . ? N34 N35 1.382(8) . ? N35 C36 1.256(9) . ? C36 C37 1.461(10) . ? C36 H36 0.93 . ? C37 C42 1.338(12) . ? C37 N38 1.354(10) . ? N38 C39 1.348(12) . ? C39 C40 1.313(14) . ? C39 H39 0.93 . ? C40 C41 1.314(15) . ? C40 H40 0.93 . ? C41 C42 1.380(14) . ? C41 H41 0.93 . ? C42 H42 0.93 . ? N43 C44 1.449(10) . ? N43 H43 0.86 . ? C44 C45 1.476(13) . ? C44 H44A 0.97 . ? C44 H44B 0.97 . ? C45 H45A 0.96 . ? C45 H45B 0.96 . ? C45 H45C 0.96 . ? N50 C51 1.209(16) . ? C51 C52 1.547(16) . ? C52 H52A 0.96 . ? C52 H52B 0.96 . ? C52 H52C 0.96 . ? N17 C18B 1.381(17) . ? N17 C18 1.528(15) . ? N17 H17A 0.863(8) . ? N17 H17B 0.879(8) . ? C18 C19 1.524(16) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C19B C18B 1.471(19) . ? C19B H19D 0.96 . ? C19B H19E 0.96 . ? C19B H19F 0.96 . ? C18B H18C 0.97 . ? C18B H18D 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 N34 Ag1 S6 132.98(16) . . ? N34 Ag1 S5 115.58(15) . . ? S6 Ag1 S5 107.57(7) . . ? N34 Ag1 Ag3 88.61(15) . . ? S6 Ag1 Ag3 75.05(5) . . ? S5 Ag1 Ag3 132.40(5) . . ? N34 Ag1 Ag2 79.97(16) . . ? S6 Ag1 Ag2 131.89(5) . . ? S5 Ag1 Ag2 73.14(5) . . ? Ag3 Ag1 Ag2 71.72(2) . . ? N21 Ag2 S6 118.39(16) . 3_565 ? N21 Ag2 S4 123.12(16) . . ? S6 Ag2 S4 111.62(7) 3_565 . ? N21 Ag2 Ag1 85.69(15) . . ? S6 Ag2 Ag1 137.33(5) 3_565 . ? S4 Ag2 Ag1 74.73(5) . . ? N21 Ag2 Ag3 82.26(16) . 3_565 ? S6 Ag2 Ag3 73.77(5) 3_565 3_565 ? S4 Ag2 Ag3 138.68(5) . 3_565 ? Ag1 Ag2 Ag3 75.66(2) . 3_565 ? N8 Ag3 S5 125.17(17) . 3_565 ? N8 Ag3 S4 122.62(18) . . ? S5 Ag3 S4 108.50(7) 3_565 . ? N8 Ag3 Ag1 82.23(17) . . ? S5 Ag3 Ag1 132.64(5) 3_565 . ? S4 Ag3 Ag1 74.91(5) . . ? N8 Ag3 Ag2 85.72(19) . 3_565 ? S5 Ag3 Ag2 72.87(5) 3_565 3_565 ? S4 Ag3 Ag2 132.14(5) . 3_565 ? Ag1 Ag3 Ag2 71.82(2) . 3_565 ? C33 S4 Ag2 103.4(3) . . ? C33 S4 Ag3 106.8(3) . . ? Ag2 S4 Ag3 88.63(7) . . ? C20 S5 Ag3 106.6(3) . 3_565 ? C20 S5 Ag1 102.8(2) . . ? Ag3 S5 Ag1 94.33(6) 3_565 . ? C7 S6 Ag1 107.5(3) . . ? C7 S6 Ag2 103.3(3) . 3_565 ? Ag1 S6 Ag2 90.27(7) . 3_565 ? N8 C7 N17 120.7(9) . . ? N8 C7 S6 119.7(6) . . ? N17 C7 S6 119.5(8) . . ? C7 N8 N9 112.7(7) . . ? C7 N8 Ag3 118.5(5) . . ? N9 N8 Ag3 127.0(6) . . ? C10 N9 N8 115.1(8) . . ? N9 C10 C11 122.5(11) . . ? N9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? N12 C11 C16 123.9(11) . . ? N12 C11 C10 114.3(11) . . ? C16 C11 C10 121.8(12) . . ? C11 N12 C13 116.1(12) . . ? C14 C13 N12 122.0(15) . . ? C14 C13 H13 119 . . ? N12 C13 H13 119 . . ? C15 C14 C13 121.6(15) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 117.4(15) . . ? C14 C15 H15 121.3 . . ? C16 C15 H15 121.3 . . ? C11 C16 C15 119.0(13) . . ? C11 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? N30 C20 N21 121.6(7) . . ? N30 C20 S5 119.9(6) . . ? N21 C20 S5 118.5(5) . . ? C20 N21 N22 113.7(6) . . ? C20 N21 Ag2 119.0(5) . . ? N22 N21 Ag2 126.7(5) . . ? C23 N22 N21 114.2(7) . . ? N22 C23 C24 122.7(8) . . ? N22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? N25 C24 C29 122.5(9) . . ? N25 C24 C23 114.2(8) . . ? C29 C24 C23 123.3(9) . . ? C26 N25 C24 117.3(9) . . ? N25 C26 C27 123.6(11) . . ? N25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C28 C27 C26 119.0(11) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 118.1(11) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C24 C29 C28 119.5(11) . . ? C24 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C20 N30 C31 128.0(7) . . ? C20 N30 H30 116 . . ? C31 N30 H30 116 . . ? N30 C31 C32 113.6(8) . . ? N30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? N30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? 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 . . ? N43 C33 N34 122.0(7) . . ? N43 C33 S4 119.2(6) . . ? N34 C33 S4 118.7(6) . . ? C33 N34 N35 112.8(6) . . ? C33 N34 Ag1 120.5(5) . . ? N35 N34 Ag1 125.1(5) . . ? C36 N35 N34 116.5(7) . . ? N35 C36 C37 121.9(8) . . ? N35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C42 C37 N38 123.0(9) . . ? C42 C37 C36 121.4(9) . . ? N38 C37 C36 115.6(8) . . ? C39 N38 C37 116.2(9) . . ? C40 C39 N38 122.5(11) . . ? C40 C39 H39 118.7 . . ? N38 C39 H39 118.7 . . ? C41 C40 C39 120.7(12) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.3(12) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C37 C42 C41 117.1(11) . . ? C37 C42 H42 121.4 . . ? C41 C42 H42 121.4 . . ? C33 N43 C44 126.2(7) . . ? C33 N43 H43 116.9 . . ? C44 N43 H43 116.9 . . ? N43 C44 C45 111.7(8) . . ? N43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? N43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N50 C51 C52 171.6(18) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C7 N17 C18B 134.0(15) . . ? C7 N17 C18 122.0(10) . . ? C7 N17 H17A 116.8(9) . . ? C18B N17 H17A 105.6(14) . . ? C18 N17 H17A 121.0(10) . . ? C7 N17 H17B 117.3(9) . . ? C18B N17 H17B 103.9(14) . . ? C18 N17 H17B 120.7(10) . . ? N17 C18 C19 110.7(12) . . ? N17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N17 C18B C19B 112(2) . . ? N17 C18B H18C 109.2 . . ? C19B C18B H18C 109.2 . . ? N17 C18B H18D 109.2 . . ? C19B C18B H18D 109.2 . . ? H18C C18B H18D 107.9 . . ? 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 N34 Ag1 Ag2 N21 -80.3(2) . . . . ? S6 Ag1 Ag2 N21 139.25(18) . . . . ? S5 Ag1 Ag2 N21 40.50(17) . . . . ? Ag3 Ag1 Ag2 N21 -172.14(16) . . . . ? N34 Ag1 Ag2 S6 151.28(17) . . . 3_565 ? S6 Ag1 Ag2 S6 10.80(15) . . . 3_565 ? S5 Ag1 Ag2 S6 -87.94(9) . . . 3_565 ? Ag3 Ag1 Ag2 S6 59.42(8) . . . 3_565 ? N34 Ag1 Ag2 S4 45.78(16) . . . . ? S6 Ag1 Ag2 S4 -94.70(9) . . . . ? S5 Ag1 Ag2 S4 166.56(7) . . . . ? Ag3 Ag1 Ag2 S4 -46.08(5) . . . . ? N34 Ag1 Ag2 Ag3 -163.38(15) . . . 3_565 ? S6 Ag1 Ag2 Ag3 56.15(8) . . . 3_565 ? S5 Ag1 Ag2 Ag3 -42.60(5) . . . 3_565 ? Ag3 Ag1 Ag2 Ag3 104.76(2) . . . 3_565 ? N34 Ag1 Ag3 N8 92.5(2) . . . . ? S6 Ag1 Ag3 N8 -42.90(19) . . . . ? S5 Ag1 Ag3 N8 -143.23(19) . . . . ? Ag2 Ag1 Ag3 N8 172.42(18) . . . . ? N34 Ag1 Ag3 S5 -135.82(17) . . . 3_565 ? S6 Ag1 Ag3 S5 88.76(8) . . . 3_565 ? S5 Ag1 Ag3 S5 -11.57(13) . . . 3_565 ? Ag2 Ag1 Ag3 S5 -55.92(7) . . . 3_565 ? N34 Ag1 Ag3 S4 -34.37(16) . . . . ? S6 Ag1 Ag3 S4 -169.79(7) . . . . ? S5 Ag1 Ag3 S4 89.88(8) . . . . ? Ag2 Ag1 Ag3 S4 45.53(5) . . . . ? N34 Ag1 Ag3 Ag2 -179.45(16) . . . 3_565 ? S6 Ag1 Ag3 Ag2 45.13(5) . . . 3_565 ? S5 Ag1 Ag3 Ag2 -55.21(7) . . . 3_565 ? Ag2 Ag1 Ag3 Ag2 -99.56(2) . . . 3_565 ? N21 Ag2 S4 C33 21.3(3) . . . . ? S6 Ag2 S4 C33 171.6(3) 3_565 . . . ? Ag1 Ag2 S4 C33 -53.0(3) . . . . ? Ag3 Ag2 S4 C33 -98.6(3) 3_565 . . . ? N21 Ag2 S4 Ag3 128.27(19) . . . . ? S6 Ag2 S4 Ag3 -81.37(7) 3_565 . . . ? Ag1 Ag2 S4 Ag3 54.00(4) . . . . ? Ag3 Ag2 S4 Ag3 8.37(11) 3_565 . . . ? N8 Ag3 S4 C33 -21.2(4) . . . . ? S5 Ag3 S4 C33 179.5(3) 3_565 . . . ? Ag1 Ag3 S4 C33 49.0(3) . . . . ? Ag2 Ag3 S4 C33 96.1(3) 3_565 . . . ? N8 Ag3 S4 Ag2 -124.8(2) . . . . ? S5 Ag3 S4 Ag2 75.90(7) 3_565 . . . ? Ag1 Ag3 S4 Ag2 -54.61(4) . . . . ? Ag2 Ag3 S4 Ag2 -7.45(9) 3_565 . . . ? N34 Ag1 S5 C20 14.0(3) . . . . ? S6 Ag1 S5 C20 174.8(3) . . . . ? Ag3 Ag1 S5 C20 -99.6(3) . . . . ? Ag2 Ag1 S5 C20 -55.7(3) . . . . ? N34 Ag1 S5 Ag3 122.13(18) . . . 3_565 ? S6 Ag1 S5 Ag3 -77.06(7) . . . 3_565 ? Ag3 Ag1 S5 Ag3 8.51(9) . . . 3_565 ? Ag2 Ag1 S5 Ag3 52.42(5) . . . 3_565 ? N34 Ag1 S6 C7 -24.3(4) . . . . ? S5 Ag1 S6 C7 179.6(3) . . . . ? Ag3 Ag1 S6 C7 49.3(3) . . . . ? Ag2 Ag1 S6 C7 96.8(3) . . . . ? N34 Ag1 S6 Ag2 -128.4(2) . . . 3_565 ? S5 Ag1 S6 Ag2 75.55(8) . . . 3_565 ? Ag3 Ag1 S6 Ag2 -54.81(5) . . . 3_565 ? Ag2 Ag1 S6 Ag2 -7.30(10) . . . 3_565 ? Ag1 S6 C7 N8 -33.7(8) . . . . ? Ag2 S6 C7 N8 60.9(7) 3_565 . . . ? Ag1 S6 C7 N17 141.8(6) . . . . ? Ag2 S6 C7 N17 -123.6(7) 3_565 . . . ? N17 C7 N8 N9 1.2(11) . . . . ? S6 C7 N8 N9 176.6(5) . . . . ? N17 C7 N8 Ag3 167.0(6) . . . . ? S6 C7 N8 Ag3 -17.5(9) . . . . ? S5 Ag3 N8 C7 -89.9(6) 3_565 . . . ? S4 Ag3 N8 C7 114.3(6) . . . . ? Ag1 Ag3 N8 C7 47.8(6) . . . . ? Ag2 Ag3 N8 C7 -24.4(6) 3_565 . . . ? S5 Ag3 N8 N9 73.7(7) 3_565 . . . ? S4 Ag3 N8 N9 -82.1(6) . . . . ? Ag1 Ag3 N8 N9 -148.5(6) . . . . ? Ag2 Ag3 N8 N9 139.3(6) 3_565 . . . ? C7 N8 N9 C10 179.0(8) . . . . ? Ag3 N8 N9 C10 14.6(11) . . . . ? N8 N9 C10 C11 179.4(7) . . . . ? N9 C10 C11 N12 177.7(9) . . . . ? N9 C10 C11 C16 0.9(15) . . . . ? C16 C11 N12 C13 -0.7(16) . . . . ? C10 C11 N12 C13 -177.4(9) . . . . ? C11 N12 C13 C14 1.1(18) . . . . ? N12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C16 0(2) . . . . ? N12 C11 C16 C15 0.3(16) . . . . ? C10 C11 C16 C15 176.8(9) . . . . ? C14 C15 C16 C11 -0.1(18) . . . . ? Ag3 S5 C20 N30 137.3(6) 3_565 . . . ? Ag1 S5 C20 N30 -124.1(6) . . . . ? Ag3 S5 C20 N21 -40.0(6) 3_565 . . . ? Ag1 S5 C20 N21 58.6(6) . . . . ? N30 C20 N21 N22 -2.8(10) . . . . ? S5 C20 N21 N22 174.5(5) . . . . ? N30 C20 N21 Ag2 169.6(6) . . . . ? S5 C20 N21 Ag2 -13.2(8) . . . . ? S6 Ag2 N21 C20 113.9(5) 3_565 . . . ? S4 Ag2 N21 C20 -97.6(5) . . . . ? Ag1 Ag2 N21 C20 -28.9(5) . . . . ? Ag3 Ag2 N21 C20 47.1(5) 3_565 . . . ? S6 Ag2 N21 N22 -74.8(6) 3_565 . . . ? S4 Ag2 N21 N22 73.7(6) . . . . ? Ag1 Ag2 N21 N22 142.3(6) . . . . ? Ag3 Ag2 N21 N22 -141.6(6) 3_565 . . . ? C20 N21 N22 C23 175.6(7) . . . . ? Ag2 N21 N22 C23 3.9(9) . . . . ? N21 N22 C23 C24 175.8(7) . . . . ? N22 C23 C24 N25 -177.4(9) . . . . ? N22 C23 C24 C29 2.1(15) . . . . ? C29 C24 N25 C26 0.2(16) . . . . ? C23 C24 N25 C26 179.8(9) . . . . ? C24 N25 C26 C27 1.0(18) . . . . ? N25 C26 C27 C28 -1(2) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? N25 C24 C29 C28 -1.8(18) . . . . ? C23 C24 C29 C28 178.7(11) . . . . ? C27 C28 C29 C24 2(2) . . . . ? N21 C20 N30 C31 177.1(8) . . . . ? S5 C20 N30 C31 -0.1(12) . . . . ? C20 N30 C31 C32 110.8(10) . . . . ? Ag2 S4 C33 N43 -138.9(6) . . . . ? Ag3 S4 C33 N43 128.5(6) . . . . ? Ag2 S4 C33 N34 39.3(6) . . . . ? Ag3 S4 C33 N34 -53.4(6) . . . . ? N43 C33 N34 N35 -0.8(10) . . . . ? S4 C33 N34 N35 -178.9(5) . . . . ? N43 C33 N34 Ag1 -167.4(5) . . . . ? S4 C33 N34 Ag1 14.5(8) . . . . ? S6 Ag1 N34 C33 90.7(6) . . . . ? S5 Ag1 N34 C33 -114.6(5) . . . . ? Ag3 Ag1 N34 C33 22.8(5) . . . . ? Ag2 Ag1 N34 C33 -48.9(5) . . . . ? S6 Ag1 N34 N35 -74.1(5) . . . . ? S5 Ag1 N34 N35 80.6(5) . . . . ? Ag3 Ag1 N34 N35 -142.0(5) . . . . ? Ag2 Ag1 N34 N35 146.3(5) . . . . ? C33 N34 N35 C36 179.1(7) . . . . ? Ag1 N34 N35 C36 -15.1(9) . . . . ? N34 N35 C36 C37 176.6(6) . . . . ? N35 C36 C37 C42 -7.1(12) . . . . ? N35 C36 C37 N38 171.9(7) . . . . ? C42 C37 N38 C39 -1.2(14) . . . . ? C36 C37 N38 C39 179.7(8) . . . . ? C37 N38 C39 C40 -0.6(15) . . . . ? N38 C39 C40 C41 1(2) . . . . ? C39 C40 C41 C42 0(2) . . . . ? N38 C37 C42 C41 2.4(16) . . . . ? C36 C37 C42 C41 -178.6(10) . . . . ? C40 C41 C42 C37 -2(2) . . . . ? N34 C33 N43 C44 166.9(8) . . . . ? S4 C33 N43 C44 -15.0(11) . . . . ? C33 N43 C44 C45 -93.2(11) . . . . ? N8 C7 N17 C18B -152.9(19) . . . . ? S6 C7 N17 C18B 32(2) . . . . ? N8 C7 N17 C18 177.2(9) . . . . ? S6 C7 N17 C18 1.8(13) . . . . ? C7 N17 C18 C19 95.2(14) . . . . ? C18B N17 C18 C19 -31(3) . . . . ? C7 N17 C18B C19B 108(2) . . . . ? C18 N17 C18B C19B -179(6) . . . . ? 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 N43 H43 N50 0.86 2.36 3.152(14) 153.5 . # END of CIF # Attachment '12.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-02-26 at 13:13:02 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.reqdat # CIF files read : be44mj3n struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_be44mj3n _database_code_depnum_ccdc_archive 'CCDC 724498' _audit_creation_date 2009-02-26T13:13:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H22 N8 Pb1 S2' _chemical_formula_sum 'C18 H22 N8 Pb S2' _chemical_formula_weight 621.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.194(2) _cell_length_b 13.2451(17) _cell_length_c 12.1918(19) _cell_angle_alpha 90 _cell_angle_beta 109.195(7) _cell_angle_gamma 90 _cell_volume 2164.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1980 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.43 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.172 _exptl_absorpt_correction_T_max 0.355 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1159 _diffrn_reflns_av_unetI/netI 0.0813 _diffrn_reflns_number 10551 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 2200 _reflns_number_gt 1668 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 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^)+(0.1119P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2200 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.372 _refine_diff_density_min -4.994 _refine_diff_density_rms 0.364 #----------------------------------------------------------------------------# # 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' Pb Pb -3.3944 10.1111 '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 Pb1 Pb 0.5 0.49670(2) 0.25 0.0197(2) Uani 1 2 d S . . N1 N 0.6937(5) 0.5467(5) 0.2428(6) 0.0267(18) Uani 1 1 d . . . C2 C 0.7189(8) 0.5056(5) 0.1564(10) 0.022(2) Uani 1 1 d . . . C3 C 0.8036(7) 0.5345(7) 0.1316(8) 0.030(2) Uani 1 1 d . . . H3 H 0.8188 0.5032 0.0694 0.036 Uiso 1 1 calc R . . C4 C 0.8640(7) 0.6060(6) 0.1945(8) 0.036(2) Uani 1 1 d . . . H4 H 0.9212 0.6265 0.1761 0.043 Uiso 1 1 calc R . . C5 C 0.8426(7) 0.6498(6) 0.2866(8) 0.033(2) Uani 1 1 d . . . H5 H 0.8846 0.7001 0.3334 0.039 Uiso 1 1 calc R . . C6 C 0.7572(7) 0.6171(6) 0.3078(8) 0.031(2) Uani 1 1 d . . . H6 H 0.7424 0.6458 0.3716 0.038 Uiso 1 1 calc R . . C21 C 0.6482(7) 0.4321(6) 0.0815(7) 0.025(2) Uani 1 1 d . . . N22 N 0.5645(5) 0.4116(4) 0.0928(6) 0.0194(15) Uani 1 1 d . . . N23 N 0.5100(5) 0.3417(8) 0.0103(5) 0.0198(19) Uani 1 1 d . . . C24 C 0.4218(6) 0.3179(5) 0.0192(7) 0.0208(19) Uani 1 1 d . . . S25 S 0.36705(17) 0.36268(15) 0.11710(19) 0.0275(6) Uani 1 1 d . . . N25 N 0.3680(5) 0.2511(5) -0.0592(6) 0.0270(18) Uani 1 1 d . . . H25 H 0.308 0.2359 -0.0579 0.032 Uiso 1 1 calc R . . C26 C 0.4024(7) 0.2018(6) -0.1466(7) 0.028(2) Uani 1 1 d . . . H26A H 0.44 0.2513 -0.177 0.033 Uiso 1 1 calc R . . H26B H 0.3438 0.1798 -0.2123 0.033 Uiso 1 1 calc R . . C27 C 0.4678(8) 0.1122(7) -0.0996(9) 0.046(3) Uani 1 1 d . . . H27A H 0.5289 0.1343 -0.0394 0.069 Uiso 1 1 calc R . . H27B H 0.4849 0.0793 -0.1626 0.069 Uiso 1 1 calc R . . H27C H 0.4322 0.0642 -0.0662 0.069 Uiso 1 1 calc R . . H21 H 0.660(8) 0.401(8) 0.022(9) 0.055 Uiso 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 Pb1 0.0254(3) 0.0114(3) 0.0201(3) 0 0.0044(2) 0 N1 0.037(4) 0.017(4) 0.027(4) 0.003(3) 0.011(4) -0.001(3) C2 0.022(5) 0.019(5) 0.024(5) 0.011(3) 0.005(4) 0.001(3) C3 0.030(5) 0.025(4) 0.032(5) 0.005(4) 0.007(4) 0.002(4) C4 0.030(5) 0.028(5) 0.041(6) 0.012(4) 0.000(4) -0.008(4) C5 0.044(6) 0.023(4) 0.029(5) 0.006(4) 0.009(4) -0.011(4) C6 0.045(6) 0.019(4) 0.026(5) 0.009(3) 0.006(4) 0.000(4) C21 0.033(5) 0.016(4) 0.023(5) 0.000(3) 0.006(4) 0.008(4) N22 0.026(4) 0.015(3) 0.020(4) 0.004(3) 0.011(3) -0.005(3) N23 0.024(4) 0.021(5) 0.015(4) -0.004(3) 0.009(3) 0.005(3) C24 0.029(5) 0.013(4) 0.022(4) -0.001(3) 0.011(4) -0.005(3) S25 0.0375(13) 0.0221(10) 0.0242(11) -0.0059(8) 0.0121(10) -0.0082(9) N25 0.032(4) 0.021(3) 0.023(4) -0.007(3) 0.001(3) 0.001(3) C26 0.041(5) 0.026(4) 0.017(4) 0.001(4) 0.012(4) -0.006(4) C27 0.060(7) 0.034(5) 0.040(6) -0.017(5) 0.012(5) 0.015(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 Pb1 N22 2.634(7) . ? Pb1 N22 2.634(7) 2_655 ? Pb1 S25 2.707(2) . ? Pb1 S25 2.707(2) 2_655 ? N1 C2 1.335(14) . ? N1 C6 1.356(10) . ? C2 C3 1.386(16) . ? C2 C21 1.479(13) . ? C3 C4 1.336(12) . ? C3 H3 0.95 . ? C4 C5 1.383(14) . ? C4 H4 0.95 . ? C5 C6 1.389(13) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C21 N22 1.269(11) . ? C21 H21 0.90(11) . ? N22 N23 1.399(10) . ? N23 C24 1.329(10) . ? C24 N25 1.341(9) . ? C24 S25 1.729(9) . ? N25 C26 1.465(11) . ? N25 H25 0.88 . ? C26 C27 1.500(12) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 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 N22 Pb1 N22 129.3(3) . 2_655 ? N22 Pb1 S25 67.95(15) . . ? N22 Pb1 S25 79.30(14) 2_655 . ? N22 Pb1 S25 79.30(14) . 2_655 ? N22 Pb1 S25 67.95(15) 2_655 2_655 ? S25 Pb1 S25 98.04(9) . 2_655 ? C2 N1 C6 116.2(9) . . ? N1 C2 C3 122.4(9) . . ? N1 C2 C21 116.9(10) . . ? C3 C2 C21 120.5(10) . . ? C4 C3 C2 120.6(11) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.5(10) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 117.3(8) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? N1 C6 C5 124.0(10) . . ? N1 C6 H6 118 . . ? C5 C6 H6 118 . . ? N22 C21 C2 122.8(9) . . ? N22 C21 H21 114(7) . . ? C2 C21 H21 123(7) . . ? C21 N22 N23 112.3(7) . . ? C21 N22 Pb1 123.4(6) . . ? N23 N22 Pb1 124.3(5) . . ? C24 N23 N22 114.4(6) . . ? N23 C24 N25 115.4(8) . . ? N23 C24 S25 128.6(6) . . ? N25 C24 S25 116.0(7) . . ? C24 S25 Pb1 104.8(3) . . ? C24 N25 C26 124.4(8) . . ? C24 N25 H25 117.8 . . ? C26 N25 H25 117.8 . . ? N25 C26 C27 112.8(7) . . ? N25 C26 H26A 109 . . ? C27 C26 H26A 109 . . ? N25 C26 H26B 109 . . ? C27 C26 H26B 109 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 C6 N1 C2 C3 -1.7(12) . . . . ? C6 N1 C2 C21 -177.4(7) . . . . ? N1 C2 C3 C4 -0.1(14) . . . . ? C21 C2 C3 C4 175.5(8) . . . . ? C2 C3 C4 C5 1.4(13) . . . . ? C3 C4 C5 C6 -0.8(12) . . . . ? C2 N1 C6 C5 2.3(12) . . . . ? C4 C5 C6 N1 -1.1(12) . . . . ? N1 C2 C21 N22 3.8(12) . . . . ? C3 C2 C21 N22 -172.0(8) . . . . ? C2 C21 N22 N23 178.6(7) . . . . ? C2 C21 N22 Pb1 0.5(11) . . . . ? N22 Pb1 N22 C21 -126.4(6) 2_655 . . . ? S25 Pb1 N22 C21 179.8(6) . . . . ? S25 Pb1 N22 C21 -76.9(6) 2_655 . . . ? N22 Pb1 N22 N23 55.6(5) 2_655 . . . ? S25 Pb1 N22 N23 1.9(5) . . . . ? S25 Pb1 N22 N23 105.2(6) 2_655 . . . ? C21 N22 N23 C24 179.9(7) . . . . ? Pb1 N22 N23 C24 -2.0(10) . . . . ? N22 N23 C24 N25 179.8(6) . . . . ? N22 N23 C24 S25 0.6(12) . . . . ? N23 C24 S25 Pb1 0.9(8) . . . . ? N25 C24 S25 Pb1 -178.4(5) . . . . ? N22 Pb1 S25 C24 -1.1(3) . . . . ? N22 Pb1 S25 C24 -141.7(3) 2_655 . . . ? S25 Pb1 S25 C24 -76.1(3) 2_655 . . . ? N23 C24 N25 C26 2.9(11) . . . . ? S25 C24 N25 C26 -177.8(6) . . . . ? C24 N25 C26 C27 82.1(10) . . . . ? 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 N25 H25 S25 0.88 2.69 3.515(8) 157.1 7