# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email chskcm@bath.ac.uk _publ_contact_author_name 'Kieran Molloy' loop_ _publ_author_name 'J M Clark' 'G Kociok-Kohn' 'N J Harnett' 'M S Hill' 'K C Molloy' ; H.Saponia ; 'D Stanton' 'A Sudlow' data_h09kcm33 _database_code_depnum_ccdc_archive 'CCDC 812549' #TrackingRef 'Compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 N4 O4 Pb2 S8' _chemical_formula_sum 'C32 H36 N4 O4 Pb2 S8' _chemical_formula_weight 1211.51 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1779(6) _cell_length_b 10.5781(6) _cell_length_c 11.4041(8) _cell_angle_alpha 112.535(4) _cell_angle_beta 111.534(4) _cell_angle_gamma 94.306(3) _cell_volume 1021.09(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52785 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 8.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3559 _exptl_absorpt_correction_T_max 0.4772 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '257 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15152 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 30.05 _reflns_number_total 5495 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0878P)^2^+6.0044P] 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 SHELXL _refine_ls_extinction_coef 0.0115(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5495 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Pb Pb 0.11519(3) 0.13238(3) 0.18824(3) 0.03692(16) Uani 1 1 d . A . S1 S 0.0647(3) 0.3407(3) 0.4079(3) 0.0573(7) Uani 1 1 d . . . S2 S 0.1151(3) 0.0677(3) 0.4118(3) 0.0556(6) Uani 1 1 d . . . S3 S -0.2220(2) 0.0362(3) 0.0583(3) 0.0420(5) Uani 1 1 d . . . S4 S -0.0942(2) 0.1947(2) -0.0595(3) 0.0403(5) Uani 1 1 d . . . O2 O -0.3319(7) 0.2160(8) -0.0362(8) 0.0433(14) Uani 1 1 d . . . N1 N 0.4019(8) 0.1713(8) 0.3261(8) 0.0392(15) Uani 1 1 d . . . N2 N 0.3017(8) 0.3677(8) 0.2423(9) 0.0441(17) Uani 1 1 d . . . C1 C 0.0991(11) 0.2346(13) 0.4878(12) 0.057(3) Uani 1 1 d . A . O1 O 0.1194(12) 0.2686(12) 0.6210(11) 0.048(3) Uani 0.75(3) 1 d P A 1 C2 C 0.1007(18) 0.4063(15) 0.7002(18) 0.054(4) Uani 0.75(3) 1 d P A 1 H2A H 0.1719 0.4826 0.7094 0.064 Uiso 0.75(3) 1 calc PR A 1 H2B H 0.0012 0.4140 0.6504 0.064 Uiso 0.75(3) 1 calc PR A 1 C3 C 0.124(2) 0.4203(19) 0.8389(19) 0.051(4) Uani 0.75(3) 1 d P A 1 H3A H 0.1113 0.5123 0.8934 0.077 Uiso 0.75(3) 1 calc PR A 1 H3B H 0.2225 0.4133 0.8877 0.077 Uiso 0.75(3) 1 calc PR A 1 H3C H 0.0523 0.3447 0.8289 0.077 Uiso 0.75(3) 1 calc PR A 1 O1A O 0.092(4) 0.348(4) 0.597(4) 0.064(13) Uani 0.25(3) 1 d P A 2 C2A C 0.114(8) 0.285(7) 0.689(8) 0.073(17) Uiso 0.25(3) 1 d P A 2 H2C H 0.2142 0.2721 0.7199 0.088 Uiso 0.25(3) 1 calc PR A 2 H2D H 0.0452 0.1900 0.6381 0.088 Uiso 0.25(3) 1 calc PR A 2 C3A C 0.091(9) 0.372(8) 0.820(8) 0.07(2) Uiso 0.25(3) 1 d P A 2 H3D H 0.1072 0.3236 0.8801 0.106 Uiso 0.25(3) 1 calc PR A 2 H3E H -0.0093 0.3833 0.7908 0.106 Uiso 0.25(3) 1 calc PR A 2 H3F H 0.1597 0.4656 0.8726 0.106 Uiso 0.25(3) 1 calc PR A 2 C4 C -0.2253(9) 0.1518(9) -0.0104(10) 0.0370(17) Uani 1 1 d . A . C5 C -0.4545(11) 0.1827(12) -0.0070(13) 0.051(2) Uani 1 1 d . A . H5A H -0.4202 0.2036 0.0933 0.061 Uiso 1 1 calc R . . H5B H -0.5064 0.0815 -0.0655 0.061 Uiso 1 1 calc R . . C6 C -0.5535(13) 0.2743(14) -0.0422(16) 0.062(3) Uani 1 1 d . . . H6A H -0.4985 0.3737 0.0115 0.093 Uiso 1 1 calc R A . H6B H -0.6347 0.2609 -0.0180 0.093 Uiso 1 1 calc R . . H6C H -0.5916 0.2479 -0.1430 0.093 Uiso 1 1 calc R . . C7 C 0.4459(11) 0.0639(10) 0.3519(11) 0.0432(19) Uani 1 1 d . A . H7 H 0.3756 -0.0087 0.3416 0.052 Uiso 1 1 calc R . . C8 C 0.5890(12) 0.0550(11) 0.3927(11) 0.048(2) Uani 1 1 d . . . H8 H 0.6166 -0.0223 0.4097 0.057 Uiso 1 1 calc R A . C9 C 0.6913(11) 0.1610(12) 0.4082(12) 0.050(2) Uani 1 1 d . A . H9 H 0.7904 0.1570 0.4352 0.060 Uiso 1 1 calc R . . C10 C 0.6480(10) 0.2730(11) 0.3840(12) 0.048(2) Uani 1 1 d . . . H10 H 0.7170 0.3478 0.3958 0.058 Uiso 1 1 calc R A . C11 C 0.5006(9) 0.2743(10) 0.3418(10) 0.0389(18) Uani 1 1 d . A . C12 C 0.4451(9) 0.3908(9) 0.3103(10) 0.0398(18) Uani 1 1 d . A . C13 C 0.5412(10) 0.5194(10) 0.3524(11) 0.046(2) Uani 1 1 d . . . H13 H 0.6431 0.5369 0.4058 0.055 Uiso 1 1 calc R A . C14 C 0.4835(13) 0.6189(11) 0.3142(12) 0.053(2) Uani 1 1 d . A . H14 H 0.5464 0.7049 0.3385 0.064 Uiso 1 1 calc R . . C15 C 0.3349(12) 0.5943(10) 0.2407(12) 0.049(2) Uani 1 1 d . . . H15 H 0.2932 0.6621 0.2142 0.059 Uiso 1 1 calc R A . C16 C 0.2490(11) 0.4662(10) 0.2070(12) 0.048(2) Uani 1 1 d . A . H16 H 0.1464 0.4475 0.1558 0.057 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 Pb 0.02865(18) 0.0414(2) 0.0398(2) 0.01747(14) 0.01408(13) 0.01003(12) S1 0.0473(13) 0.0479(13) 0.0609(16) 0.0109(11) 0.0204(12) 0.0157(10) S2 0.0532(14) 0.0725(17) 0.0570(15) 0.0378(14) 0.0297(13) 0.0200(12) S3 0.0324(10) 0.0536(12) 0.0515(12) 0.0312(10) 0.0208(9) 0.0147(8) S4 0.0331(9) 0.0455(11) 0.0505(12) 0.0256(9) 0.0215(9) 0.0119(8) O2 0.034(3) 0.058(4) 0.052(4) 0.031(3) 0.024(3) 0.020(3) N1 0.029(3) 0.045(4) 0.038(4) 0.018(3) 0.009(3) 0.006(3) N2 0.034(4) 0.041(4) 0.054(5) 0.020(3) 0.017(3) 0.007(3) C1 0.034(4) 0.069(7) 0.049(6) 0.007(5) 0.020(4) 0.007(4) O1 0.066(6) 0.046(6) 0.041(5) 0.020(4) 0.029(5) 0.022(4) C2 0.061(9) 0.049(8) 0.065(10) 0.027(7) 0.036(8) 0.022(6) C3 0.070(10) 0.035(7) 0.055(8) 0.018(6) 0.036(8) 0.015(7) O1A 0.08(2) 0.044(19) 0.06(2) -0.002(15) 0.040(18) 0.014(16) C4 0.033(4) 0.043(4) 0.040(4) 0.018(3) 0.021(3) 0.011(3) C5 0.041(5) 0.065(6) 0.068(7) 0.040(5) 0.031(5) 0.027(4) C6 0.050(6) 0.073(7) 0.088(9) 0.046(7) 0.041(6) 0.034(5) C7 0.039(4) 0.044(5) 0.048(5) 0.024(4) 0.017(4) 0.009(3) C8 0.046(5) 0.049(5) 0.045(5) 0.025(4) 0.012(4) 0.018(4) C9 0.034(4) 0.073(7) 0.050(5) 0.034(5) 0.018(4) 0.015(4) C10 0.029(4) 0.061(6) 0.060(6) 0.035(5) 0.019(4) 0.009(4) C11 0.030(4) 0.047(5) 0.036(4) 0.018(4) 0.011(3) 0.007(3) C12 0.032(4) 0.042(4) 0.040(4) 0.016(3) 0.013(3) 0.007(3) C13 0.034(4) 0.047(5) 0.051(5) 0.024(4) 0.013(4) 0.000(3) C14 0.058(6) 0.047(5) 0.047(5) 0.022(4) 0.016(5) 0.001(4) C15 0.054(6) 0.040(5) 0.050(5) 0.023(4) 0.016(5) 0.012(4) C16 0.037(4) 0.045(5) 0.057(6) 0.024(4) 0.015(4) 0.012(4) _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 Pb N1 2.667(7) . ? Pb N2 2.727(8) . ? Pb S1 2.877(3) . ? Pb S2 2.882(3) . ? Pb S3 3.098(2) . ? S1 C1 1.680(15) . ? S1 O1A 2.04(4) . ? S2 C1 1.693(12) . ? S3 C4 1.683(9) . ? S4 C4 1.718(8) . ? O2 C4 1.324(11) . ? O2 C5 1.456(12) . ? N1 C11 1.335(11) . ? N1 C7 1.346(12) . ? N2 C12 1.327(12) . ? N2 C16 1.335(13) . ? C1 O1 1.349(16) . ? C1 O1A 1.39(3) . ? O1 C2 1.461(18) . ? C2 C3 1.46(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O1A C2A 1.41(9) . ? C2A C3A 1.54(11) . ? C2A H2C 0.9900 . ? C2A H2D 0.9900 . ? C3A H3D 0.9800 . ? C3A H3E 0.9800 . ? C3A H3F 0.9800 . ? C5 C6 1.504(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.379(14) . ? C7 H7 0.9500 . ? C8 C9 1.382(15) . ? C8 H8 0.9500 . ? C9 C10 1.383(15) . ? C9 H9 0.9500 . ? C10 C11 1.400(12) . ? C10 H10 0.9500 . ? C11 C12 1.504(13) . ? C12 C13 1.412(12) . ? C13 C14 1.379(15) . ? C13 H13 0.9500 . ? C14 C15 1.378(16) . ? C14 H14 0.9500 . ? C15 C16 1.387(14) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? 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 N1 Pb N2 60.5(2) . . ? N1 Pb S1 99.22(18) . . ? N2 Pb S1 80.49(19) . . ? N1 Pb S2 81.35(18) . . ? N2 Pb S2 121.3(2) . . ? S1 Pb S2 62.43(9) . . ? N1 Pb S3 166.11(18) . . ? N2 Pb S3 132.55(18) . . ? S1 Pb S3 80.70(7) . . ? S2 Pb S3 86.41(7) . . ? C1 S1 Pb 86.3(4) . . ? O1A S1 Pb 128.4(11) . . ? C1 S2 Pb 85.9(5) . . ? C4 S3 Pb 87.0(3) . . ? C4 O2 C5 118.6(7) . . ? C11 N1 C7 118.9(8) . . ? C11 N1 Pb 122.9(6) . . ? C7 N1 Pb 116.5(6) . . ? C12 N2 C16 118.6(8) . . ? C12 N2 Pb 121.3(6) . . ? C16 N2 Pb 120.0(6) . . ? O1 C1 S1 125.8(9) . . ? O1A C1 S1 83(2) . . ? O1 C1 S2 109.8(10) . . ? O1A C1 S2 153(2) . . ? S1 C1 S2 124.4(7) . . ? C1 O1 C2 117.3(11) . . ? C3 C2 O1 108.5(12) . . ? C3 C2 H2A 110.0 . . ? O1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? O1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 O1A C2A 97(4) . . ? C1 O1A S1 54.8(15) . . ? C2A O1A S1 151(4) . . ? O1A C2A C3A 113(5) . . ? O1A C2A H2C 109.0 . . ? C3A C2A H2C 109.0 . . ? O1A C2A H2D 109.0 . . ? C3A C2A H2D 109.0 . . ? H2C C2A H2D 107.8 . . ? C2A C3A H3D 109.5 . . ? C2A C3A H3E 109.5 . . ? H3D C3A H3E 109.5 . . ? C2A C3A H3F 109.5 . . ? H3D C3A H3F 109.5 . . ? H3E C3A H3F 109.5 . . ? O2 C4 S3 123.3(6) . . ? O2 C4 S4 113.0(7) . . ? S3 C4 S4 123.6(5) . . ? O2 C5 C6 106.1(9) . . ? O2 C5 H5A 110.5 . . ? C6 C5 H5A 110.5 . . ? O2 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 122.7(9) . . ? N1 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C9 118.6(9) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C10 119.4(9) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 118.8(9) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N1 C11 C10 121.6(9) . . ? N1 C11 C12 116.6(8) . . ? C10 C11 C12 121.8(8) . . ? N2 C12 C13 121.5(9) . . ? N2 C12 C11 117.0(8) . . ? C13 C12 C11 121.4(8) . . ? C14 C13 C12 118.4(9) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 120.3(9) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 117.1(9) . . ? C14 C15 H15 121.5 . . ? C16 C15 H15 121.5 . . ? N2 C16 C15 124.0(9) . . ? N2 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.617 _refine_diff_density_min -3.382 _refine_diff_density_rms 0.251 # Attachment 'Compound 2.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 812550' #TrackingRef 'Compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 N4 O4 Pb2 S8' _chemical_formula_sum 'C40 H52 N4 O4 Pb2 S8' _chemical_formula_weight 1323.72 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.15660(10) _cell_length_b 24.0033(3) _cell_length_c 10.32520(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.0970(10) _cell_angle_gamma 90.00 _cell_volume 2405.96(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 82006 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 7.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2599 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '513 1.1 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45959 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10193 _reflns_number_gt 8874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0653P)^2^+4.4395P] 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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.487(7) _refine_ls_number_reflns 10193 _refine_ls_number_parameters 524 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.83650(3) 0.221721(14) 0.12881(3) 0.02332(9) Uani 1 1 d . . . Pb2 Pb 1.08644(3) 0.278290(15) 0.45421(3) 0.02384(9) Uani 1 1 d . . . S1 S 0.8649(3) 0.17710(12) 0.4136(3) 0.0274(6) Uani 1 1 d . . . S2 S 1.1049(3) 0.15841(12) 0.3059(3) 0.0300(6) Uani 1 1 d . . . S3 S 0.7576(3) 0.11183(12) 0.0391(3) 0.0311(6) Uani 1 1 d . . . S4 S 0.9087(3) 0.17900(13) -0.1176(3) 0.0376(7) Uani 1 1 d . . . S5 S 0.8198(3) 0.33594(12) 0.2763(3) 0.0285(5) Uani 1 1 d . . . S6 S 1.0600(3) 0.32708(13) 0.1648(3) 0.0311(6) Uani 1 1 d . . . S7 S 1.1643(3) 0.38946(13) 0.5452(3) 0.0309(6) Uani 1 1 d . . . S8 S 1.0144(3) 0.31792(13) 0.6932(3) 0.0346(6) Uani 1 1 d . . . O1 O 1.0233(7) 0.0930(3) 0.4756(7) 0.0290(16) Uani 1 1 d . . . O2 O 0.7994(8) 0.0795(3) -0.1786(7) 0.0324(17) Uani 1 1 d . . . O3 O 0.8891(9) 0.4122(3) 0.1376(8) 0.0383(19) Uani 1 1 d . . . O4 O 1.0679(8) 0.4207(3) 0.7479(7) 0.0339(18) Uani 1 1 d . . . N1 N 0.5722(8) 0.2242(4) 0.1029(7) 0.0254(17) Uani 1 1 d . . . N2 N 0.6793(8) 0.2846(4) -0.0610(8) 0.0268(18) Uani 1 1 d . . . N3 N 1.2483(8) 0.2137(4) 0.6407(8) 0.030(2) Uani 1 1 d . . . N4 N 1.3537(8) 0.2748(5) 0.4771(8) 0.0288(18) Uani 1 1 d . . . C1 C 1.0014(10) 0.1399(4) 0.4008(9) 0.022(2) Uani 1 1 d . . . C2 C 1.1447(11) 0.0589(4) 0.4849(11) 0.029(2) Uani 1 1 d . . . H2A H 1.2290 0.0821 0.5131 0.035 Uiso 1 1 calc R . . H2B H 1.1383 0.0422 0.3956 0.035 Uiso 1 1 calc R . . C3 C 1.1504(11) 0.0141(5) 0.5875(11) 0.030(2) Uani 1 1 d . . . H3A H 1.0708 -0.0112 0.5527 0.036 Uiso 1 1 calc R . . H3B H 1.1423 0.0314 0.6719 0.036 Uiso 1 1 calc R . . C4 C 1.2826(11) -0.0198(4) 0.6200(10) 0.031(2) Uani 1 1 d . . . H4A H 1.3622 0.0058 0.6507 0.037 Uiso 1 1 calc R . . H4B H 1.2852 -0.0455 0.6956 0.037 Uiso 1 1 calc R . . C5 C 1.2975(15) -0.0533(5) 0.5010(13) 0.047(3) Uani 1 1 d . . . H5A H 1.3848 -0.0738 0.5281 0.070 Uiso 1 1 calc R . . H5B H 1.2965 -0.0281 0.4260 0.070 Uiso 1 1 calc R . . H5C H 1.2208 -0.0797 0.4719 0.070 Uiso 1 1 calc R . . C6 C 0.8236(10) 0.1217(5) -0.0931(10) 0.027(2) Uani 1 1 d . . . C7 C 0.8439(12) 0.0821(5) -0.3022(11) 0.034(2) Uani 1 1 d . . . H7A H 0.9457 0.0825 -0.2783 0.041 Uiso 1 1 calc R . . H7B H 0.8079 0.1162 -0.3544 0.041 Uiso 1 1 calc R . . C8 C 0.7872(13) 0.0310(6) -0.3850(13) 0.042(3) Uani 1 1 d . . . H8A H 0.8255 -0.0023 -0.3304 0.050 Uiso 1 1 calc R . . H8B H 0.8208 0.0307 -0.4657 0.050 Uiso 1 1 calc R . . C9 C 0.6311(15) 0.0258(6) -0.4323(15) 0.054(4) Uani 1 1 d . . . H9A H 0.5962 0.0257 -0.3523 0.065 Uiso 1 1 calc R . . H9B H 0.6056 -0.0102 -0.4799 0.065 Uiso 1 1 calc R . . C10 C 0.5618(15) 0.0734(7) -0.5277(14) 0.061(4) Uani 1 1 d . . . H10A H 0.4617 0.0683 -0.5550 0.091 Uiso 1 1 calc R . . H10B H 0.5941 0.0730 -0.6083 0.091 Uiso 1 1 calc R . . H10C H 0.5855 0.1091 -0.4807 0.091 Uiso 1 1 calc R . . C11 C 0.5226(10) 0.1917(5) 0.1818(11) 0.030(2) Uani 1 1 d . . . H11 H 0.5839 0.1669 0.2424 0.035 Uiso 1 1 calc R . . C12 C 0.3844(12) 0.1923(5) 0.1795(12) 0.036(3) Uani 1 1 d . . . H12 H 0.3523 0.1684 0.2369 0.043 Uiso 1 1 calc R . . C13 C 0.2958(11) 0.2284(6) 0.0922(11) 0.035(3) Uani 1 1 d . . . H13 H 0.2016 0.2304 0.0895 0.042 Uiso 1 1 calc R . . C14 C 0.3463(11) 0.2613(5) 0.0092(11) 0.032(2) Uani 1 1 d . . . H14 H 0.2861 0.2860 -0.0526 0.038 Uiso 1 1 calc R . . C15 C 0.4844(10) 0.2591(4) 0.0142(10) 0.026(2) Uani 1 1 d . . . C16 C 0.5457(11) 0.2929(4) -0.0751(10) 0.025(2) Uani 1 1 d . . . C17 C 0.4676(11) 0.3306(5) -0.1708(11) 0.033(2) Uani 1 1 d . . . H17 H 0.3722 0.3356 -0.1819 0.039 Uiso 1 1 calc R . . C18 C 0.5328(12) 0.3604(5) -0.2487(11) 0.033(2) Uani 1 1 d . . . H18 H 0.4825 0.3866 -0.3133 0.040 Uiso 1 1 calc R . . C19 C 0.6718(12) 0.3519(4) -0.2325(11) 0.029(2) Uani 1 1 d . . . H19 H 0.7184 0.3721 -0.2849 0.035 Uiso 1 1 calc R . . C20 C 0.7398(12) 0.3134(5) -0.1380(10) 0.032(2) Uani 1 1 d . . . H20 H 0.8348 0.3069 -0.1270 0.038 Uiso 1 1 calc R . . C21 C 0.9237(10) 0.3615(5) 0.1896(11) 0.027(2) Uani 1 1 d . . . C22 C 0.9727(15) 0.4408(5) 0.0666(15) 0.047(3) Uani 1 1 d . . . H22A H 0.9786 0.4187 -0.0124 0.057 Uiso 1 1 calc R . . H22B H 1.0671 0.4467 0.1275 0.057 Uiso 1 1 calc R . . C23 C 0.9038(13) 0.4960(6) 0.0206(13) 0.048(3) Uani 1 1 d . . . H23A H 0.8877 0.5155 0.0991 0.057 Uiso 1 1 calc R . . H23B H 0.9657 0.5195 -0.0147 0.057 Uiso 1 1 calc R . . C24 C 0.7694(19) 0.4888(7) -0.0874(13) 0.065(4) Uani 1 1 d . . . H24A H 0.7118 0.4620 -0.0553 0.078 Uiso 1 1 calc R . . H24B H 0.7870 0.4727 -0.1690 0.078 Uiso 1 1 calc R . . C25 C 0.6894(17) 0.5436(7) -0.1264(14) 0.061(4) Uani 1 1 d . . . H25A H 0.6020 0.5363 -0.1960 0.091 Uiso 1 1 calc R . . H25B H 0.7442 0.5698 -0.1618 0.091 Uiso 1 1 calc R . . H25C H 0.6710 0.5597 -0.0462 0.091 Uiso 1 1 calc R . . C27 C 1.0842(10) 0.3786(5) 0.6661(10) 0.031(2) Uani 1 1 d . . . C28 C 1.1419(13) 0.4732(5) 0.7512(13) 0.042(3) Uani 1 1 d . . . H28A H 1.0925 0.5033 0.7831 0.050 Uiso 1 1 calc R . . H28B H 1.1434 0.4827 0.6583 0.050 Uiso 1 1 calc R . . C29 C 1.2879(12) 0.4699(5) 0.8432(11) 0.036(3) Uani 1 1 d . . . H29A H 1.3322 0.5068 0.8461 0.043 Uiso 1 1 calc R . . H29B H 1.3401 0.4429 0.8049 0.043 Uiso 1 1 calc R . . C30 C 1.2961(12) 0.4520(5) 0.9886(12) 0.040(3) Uani 1 1 d . . . H30A H 1.2513 0.4153 0.9858 0.048 Uiso 1 1 calc R . . H30B H 1.2448 0.4792 1.0273 0.048 Uiso 1 1 calc R . . C31 C 1.4458(15) 0.4483(8) 1.0815(14) 0.066(4) Uani 1 1 d . . . H31A H 1.4456 0.4369 1.1726 0.099 Uiso 1 1 calc R . . H31B H 1.4902 0.4848 1.0860 0.099 Uiso 1 1 calc R . . H31C H 1.4965 0.4208 1.0448 0.099 Uiso 1 1 calc R . . C32 C 1.1888(12) 0.1824(5) 0.7177(11) 0.035(3) Uani 1 1 d . . . H32 H 1.0946 0.1888 0.7106 0.042 Uiso 1 1 calc R . . C33 C 1.2590(13) 0.1418(5) 0.8057(11) 0.034(3) Uani 1 1 d . . . H33 H 1.2146 0.1208 0.8587 0.041 Uiso 1 1 calc R . . C34 C 1.3958(13) 0.1326(6) 0.8149(12) 0.040(3) Uani 1 1 d . . . H34 H 1.4471 0.1048 0.8741 0.048 Uiso 1 1 calc R . . C35 C 1.4572(12) 0.1646(5) 0.7359(11) 0.034(2) Uani 1 1 d . . . H35 H 1.5516 0.1592 0.7424 0.041 Uiso 1 1 calc R . . C36 C 1.3809(10) 0.2043(5) 0.6478(11) 0.029(2) Uani 1 1 d . . . C37 C 1.4395(11) 0.2394(4) 0.5603(11) 0.027(2) Uani 1 1 d . . . C38 C 1.5778(11) 0.2366(4) 0.5653(11) 0.029(2) Uani 1 1 d . . . H38 H 1.6377 0.2106 0.6231 0.035 Uiso 1 1 calc R . . C39 C 1.6272(10) 0.2727(6) 0.4837(11) 0.035(3) Uani 1 1 d . . . H39 H 1.7219 0.2724 0.4879 0.042 Uiso 1 1 calc R . . C40 C 1.5382(11) 0.3084(5) 0.3983(12) 0.033(3) Uani 1 1 d . . . H40 H 1.5689 0.3325 0.3402 0.040 Uiso 1 1 calc R . . C41 C 1.4022(12) 0.3086(5) 0.3984(11) 0.032(2) Uani 1 1 d . . . H41 H 1.3403 0.3338 0.3400 0.038 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 Pb1 0.02007(17) 0.03003(19) 0.02027(17) 0.00137(15) 0.00656(13) 0.00056(16) Pb2 0.01977(17) 0.03103(19) 0.02077(17) 0.00096(15) 0.00602(13) 0.00012(16) S1 0.0234(13) 0.0344(15) 0.0275(13) 0.0065(11) 0.0123(10) 0.0059(11) S2 0.0271(13) 0.0368(15) 0.0307(14) 0.0093(11) 0.0154(11) 0.0064(11) S3 0.0367(15) 0.0333(15) 0.0274(13) -0.0002(11) 0.0160(12) -0.0050(12) S4 0.0463(17) 0.0393(17) 0.0354(15) -0.0076(13) 0.0248(13) -0.0133(13) S5 0.0255(13) 0.0341(14) 0.0299(13) 0.0028(11) 0.0145(11) 0.0037(11) S6 0.0244(13) 0.0405(16) 0.0302(14) 0.0056(12) 0.0108(11) 0.0065(12) S7 0.0322(15) 0.0345(15) 0.0296(14) -0.0008(12) 0.0145(12) -0.0032(12) S8 0.0359(15) 0.0435(17) 0.0294(14) 0.0021(12) 0.0176(12) -0.0023(12) O1 0.024(4) 0.034(4) 0.031(4) 0.007(3) 0.011(3) 0.010(3) O2 0.038(4) 0.034(4) 0.030(4) -0.006(3) 0.017(3) -0.009(3) O3 0.041(5) 0.038(5) 0.044(5) 0.012(4) 0.024(4) 0.011(4) O4 0.031(4) 0.044(5) 0.028(4) -0.011(3) 0.010(3) -0.002(3) N1 0.026(4) 0.032(4) 0.021(4) -0.001(4) 0.009(3) -0.001(4) N2 0.023(4) 0.035(5) 0.023(4) 0.004(4) 0.007(3) -0.001(4) N3 0.023(4) 0.044(6) 0.023(4) 0.000(4) 0.008(3) 0.000(4) N4 0.022(4) 0.043(5) 0.021(4) 0.001(4) 0.006(3) 0.003(5) C1 0.020(5) 0.024(5) 0.019(5) -0.012(4) -0.001(4) -0.001(4) C2 0.030(6) 0.029(6) 0.032(6) -0.001(4) 0.014(5) 0.004(4) C3 0.034(6) 0.031(6) 0.026(5) 0.004(4) 0.010(4) 0.004(4) C4 0.025(5) 0.032(6) 0.030(5) 0.009(4) 0.001(4) 0.002(4) C5 0.054(8) 0.038(7) 0.048(7) 0.009(6) 0.015(6) 0.008(6) C6 0.020(5) 0.037(6) 0.025(5) 0.000(5) 0.009(4) -0.002(4) C7 0.037(6) 0.037(6) 0.032(6) -0.011(5) 0.018(5) -0.001(5) C8 0.041(7) 0.048(7) 0.039(7) -0.015(5) 0.015(5) -0.011(6) C9 0.055(8) 0.063(9) 0.053(8) -0.025(7) 0.030(7) -0.030(7) C10 0.043(8) 0.084(12) 0.049(8) -0.015(8) 0.004(6) -0.010(8) C11 0.019(5) 0.044(7) 0.025(5) 0.004(5) 0.005(4) 0.002(4) C12 0.032(6) 0.039(7) 0.038(6) -0.005(5) 0.013(5) -0.007(5) C13 0.021(5) 0.051(8) 0.035(5) -0.009(6) 0.011(4) -0.003(6) C14 0.025(5) 0.040(7) 0.030(6) -0.003(4) 0.009(4) 0.002(4) C15 0.026(5) 0.030(5) 0.019(5) -0.007(4) 0.001(4) 0.005(4) C16 0.027(5) 0.024(6) 0.022(5) -0.005(4) 0.004(4) -0.003(4) C17 0.019(5) 0.037(6) 0.038(6) 0.004(5) 0.002(4) 0.009(5) C18 0.035(6) 0.032(6) 0.026(5) 0.011(5) 0.001(5) 0.008(5) C19 0.036(6) 0.025(5) 0.027(5) 0.007(4) 0.009(5) -0.002(4) C20 0.030(6) 0.051(7) 0.013(5) 0.002(5) 0.006(4) 0.002(5) C21 0.020(5) 0.032(6) 0.028(5) 0.004(5) 0.005(4) -0.001(4) C22 0.054(8) 0.040(7) 0.061(8) 0.004(6) 0.039(7) -0.002(6) C23 0.052(8) 0.042(7) 0.053(8) 0.007(6) 0.022(6) -0.009(6) C24 0.100(13) 0.057(9) 0.031(7) -0.002(6) 0.008(7) -0.001(8) C25 0.079(10) 0.056(9) 0.043(8) 0.009(7) 0.012(7) 0.020(8) C27 0.018(5) 0.047(7) 0.025(5) 0.000(5) 0.003(4) 0.013(5) C28 0.040(7) 0.042(7) 0.045(7) -0.003(6) 0.015(5) 0.008(5) C29 0.036(6) 0.037(6) 0.036(6) -0.004(5) 0.012(5) 0.003(5) C30 0.037(7) 0.039(7) 0.042(7) -0.010(5) 0.009(5) -0.005(5) C31 0.044(8) 0.095(13) 0.043(8) -0.015(8) -0.013(6) 0.003(8) C32 0.035(6) 0.044(7) 0.029(6) 0.001(5) 0.015(5) 0.002(5) C33 0.044(7) 0.031(6) 0.027(6) 0.001(5) 0.008(5) -0.008(5) C34 0.039(7) 0.043(7) 0.034(6) 0.001(5) 0.005(5) 0.001(5) C35 0.032(6) 0.039(6) 0.028(5) -0.002(5) 0.002(4) 0.000(5) C36 0.015(5) 0.042(7) 0.026(5) 0.002(4) 0.002(4) 0.005(4) C37 0.029(5) 0.020(5) 0.030(5) -0.006(4) 0.007(4) 0.005(4) C38 0.023(5) 0.029(6) 0.036(6) -0.007(4) 0.007(4) 0.002(4) C39 0.020(5) 0.041(7) 0.048(6) -0.011(6) 0.016(5) 0.001(6) C40 0.030(6) 0.040(7) 0.034(6) 0.001(5) 0.018(5) -0.001(5) C41 0.033(6) 0.032(6) 0.033(6) 0.005(5) 0.012(5) -0.002(5) _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 Pb1 N2 2.613(9) . ? Pb1 N1 2.619(7) . ? Pb1 S3 2.832(3) . ? Pb1 S4 3.026(3) . ? Pb1 S1 3.062(3) . ? Pb1 S5 3.165(3) . ? Pb1 S2 3.187(3) . ? Pb1 S6 3.345(3) . ? Pb1 Pb2 3.8159(5) . ? Pb2 N3 2.637(9) . ? Pb2 N4 2.656(8) . ? Pb2 S7 2.862(3) . ? Pb2 S8 2.931(3) . ? Pb2 S5 3.114(3) . ? Pb2 S6 3.147(3) . ? Pb2 S2 3.291(3) . ? S1 C1 1.687(10) . ? S2 C1 1.694(10) . ? S3 C6 1.706(10) . ? S4 C6 1.681(11) . ? S5 C21 1.688(10) . ? S6 C21 1.695(11) . ? S7 C27 1.698(11) . ? S8 C27 1.680(13) . ? O1 C1 1.345(12) . ? O1 C2 1.459(12) . ? O2 C6 1.319(13) . ? O2 C7 1.475(12) . ? O3 C21 1.334(13) . ? O3 C22 1.449(14) . ? O4 C27 1.358(13) . ? O4 C28 1.462(15) . ? N1 C11 1.328(14) . ? N1 C15 1.363(14) . ? N2 C20 1.332(14) . ? N2 C16 1.336(13) . ? N3 C36 1.346(13) . ? N3 C32 1.357(14) . ? N4 C37 1.333(14) . ? N4 C41 1.340(14) . ? C2 C3 1.499(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(17) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.508(16) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.521(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.54(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.397(15) . ? C11 H11 0.9500 . ? C12 C13 1.377(19) . ? C12 H12 0.9500 . ? C13 C14 1.372(16) . ? C13 H13 0.9500 . ? C14 C15 1.389(15) . ? C14 H14 0.9500 . ? C15 C16 1.495(14) . ? C16 C17 1.401(15) . ? C17 C18 1.382(16) . ? C17 H17 0.9500 . ? C18 C19 1.387(16) . ? C18 H18 0.9500 . ? C19 C20 1.375(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C22 C23 1.508(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.50(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.54(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C28 C29 1.510(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.539(17) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.543(17) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.380(16) . ? C32 H32 0.9500 . ? C33 C34 1.382(17) . ? C33 H33 0.9500 . ? C34 C35 1.395(17) . ? C34 H34 0.9500 . ? C35 C36 1.386(16) . ? C35 H35 0.9500 . ? C36 C37 1.482(15) . ? C37 C38 1.392(14) . ? C38 C39 1.401(17) . ? C38 H38 0.9500 . ? C39 C40 1.363(18) . ? C39 H39 0.9500 . ? C40 C41 1.381(15) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? 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 N2 Pb1 N1 61.9(3) . . ? N2 Pb1 S3 103.9(2) . . ? N1 Pb1 S3 78.7(2) . . ? N2 Pb1 S4 79.1(2) . . ? N1 Pb1 S4 114.60(18) . . ? S3 Pb1 S4 61.62(8) . . ? N2 Pb1 S1 141.87(18) . . ? N1 Pb1 S1 84.85(18) . . ? S3 Pb1 S1 85.76(8) . . ? S4 Pb1 S1 135.32(8) . . ? N2 Pb1 S5 75.7(2) . . ? N1 Pb1 S5 80.3(2) . . ? S3 Pb1 S5 156.09(7) . . ? S4 Pb1 S5 139.34(7) . . ? S1 Pb1 S5 81.03(7) . . ? N2 Pb1 S2 159.53(18) . . ? N1 Pb1 S2 138.4(2) . . ? S3 Pb1 S2 81.70(8) . . ? S4 Pb1 S2 86.73(8) . . ? S1 Pb1 S2 57.25(6) . . ? S5 Pb1 S2 107.14(7) . . ? N2 Pb1 S6 83.8(2) . . ? N1 Pb1 S6 129.5(2) . . ? S3 Pb1 S6 149.08(7) . . ? S4 Pb1 S6 91.45(7) . . ? S1 Pb1 S6 106.76(7) . . ? S5 Pb1 S6 54.70(6) . . ? S2 Pb1 S6 81.87(7) . . ? N2 Pb1 Pb2 123.8(2) . . ? N1 Pb1 Pb2 118.59(17) . . ? S3 Pb1 Pb2 132.10(6) . . ? S4 Pb1 Pb2 126.71(6) . . ? S1 Pb1 Pb2 55.15(5) . . ? S5 Pb1 Pb2 51.97(5) . . ? S2 Pb1 Pb2 55.18(5) . . ? S6 Pb1 Pb2 51.62(5) . . ? N3 Pb2 N4 61.0(3) . . ? N3 Pb2 S7 104.8(2) . . ? N4 Pb2 S7 79.9(2) . . ? N3 Pb2 S8 80.4(2) . . ? N4 Pb2 S8 115.93(19) . . ? S7 Pb2 S8 62.25(8) . . ? N3 Pb2 S5 159.95(18) . . ? N4 Pb2 S5 139.1(2) . . ? S7 Pb2 S5 83.55(8) . . ? S8 Pb2 S5 87.89(8) . . ? N3 Pb2 S6 140.64(18) . . ? N4 Pb2 S6 84.02(19) . . ? S7 Pb2 S6 84.42(8) . . ? S8 Pb2 S6 134.90(8) . . ? S5 Pb2 S6 57.17(7) . . ? N3 Pb2 S2 73.6(2) . . ? N4 Pb2 S2 79.4(2) . . ? S7 Pb2 S2 156.92(7) . . ? S8 Pb2 S2 137.56(7) . . ? S5 Pb2 S2 105.83(7) . . ? S6 Pb2 S2 83.35(7) . . ? N3 Pb2 Pb1 123.0(2) . . ? N4 Pb2 Pb1 117.70(18) . . ? S7 Pb2 Pb1 131.97(6) . . ? S8 Pb2 Pb1 126.19(6) . . ? S5 Pb2 Pb1 53.18(5) . . ? S6 Pb2 Pb1 56.45(5) . . ? S2 Pb2 Pb1 52.65(5) . . ? C1 S1 Pb1 87.6(4) . . ? C1 S2 Pb1 83.4(3) . . ? C1 S2 Pb2 80.3(3) . . ? Pb1 S2 Pb2 72.17(6) . . ? C6 S3 Pb1 89.5(4) . . ? C6 S4 Pb1 83.6(4) . . ? C21 S5 Pb2 84.5(4) . . ? C21 S5 Pb1 86.0(4) . . ? Pb2 S5 Pb1 74.85(6) . . ? C21 S6 Pb2 83.3(4) . . ? C21 S6 Pb1 80.1(4) . . ? Pb2 S6 Pb1 71.93(6) . . ? C27 S7 Pb2 87.3(4) . . ? C27 S8 Pb2 85.4(4) . . ? C1 O1 C2 120.0(8) . . ? C6 O2 C7 120.1(8) . . ? C21 O3 C22 120.8(9) . . ? C27 O4 C28 120.0(8) . . ? C11 N1 C15 118.8(8) . . ? C11 N1 Pb1 119.1(7) . . ? C15 N1 Pb1 122.1(7) . . ? C20 N2 C16 119.3(9) . . ? C20 N2 Pb1 117.3(7) . . ? C16 N2 Pb1 123.0(6) . . ? C36 N3 C32 119.1(10) . . ? C36 N3 Pb2 122.5(7) . . ? C32 N3 Pb2 117.6(7) . . ? C37 N4 C41 119.3(9) . . ? C37 N4 Pb2 122.3(7) . . ? C41 N4 Pb2 118.4(7) . . ? O1 C1 S1 113.5(7) . . ? O1 C1 S2 121.7(7) . . ? S1 C1 S2 124.8(6) . . ? O1 C2 C3 107.8(8) . . ? O1 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 C3 C4 112.8(9) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 113.4(9) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 S4 122.1(8) . . ? O2 C6 S3 112.8(8) . . ? S4 C6 S3 125.1(7) . . ? O2 C7 C8 107.0(9) . . ? O2 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O2 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C7 C8 C9 115.9(11) . . ? C7 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? C7 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 C10 112.5(12) . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 122.9(11) . . ? N1 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 118.6(11) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C12 118.6(10) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 120.9(11) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? N1 C15 C14 120.2(10) . . ? N1 C15 C16 116.1(9) . . ? C14 C15 C16 123.7(9) . . ? N2 C16 C17 121.3(10) . . ? N2 C16 C15 116.4(9) . . ? C17 C16 C15 122.3(10) . . ? C18 C17 C16 118.4(10) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C19 119.9(10) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 117.8(10) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? N2 C20 C19 123.3(10) . . ? N2 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? O3 C21 S5 114.4(8) . . ? O3 C21 S6 120.9(8) . . ? S5 C21 S6 124.6(7) . . ? O3 C22 C23 106.8(10) . . ? O3 C22 H22A 110.4 . . ? C23 C22 H22A 110.4 . . ? O3 C22 H22B 110.4 . . ? C23 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? C24 C23 C22 111.7(12) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 113.0(13) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 C27 S8 114.0(8) . . ? O4 C27 S7 121.1(9) . . ? S8 C27 S7 124.9(7) . . ? O4 C28 C29 111.9(10) . . ? O4 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? O4 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 113.0(10) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 C31 112.6(11) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 122.9(11) . . ? N3 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C32 C33 C34 118.2(11) . . ? C32 C33 H33 120.9 . . ? C34 C33 H33 120.9 . . ? C33 C34 C35 119.0(11) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C36 C35 C34 120.2(11) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? N3 C36 C35 120.5(10) . . ? N3 C36 C37 116.5(9) . . ? C35 C36 C37 122.9(10) . . ? N4 C37 C38 121.1(10) . . ? N4 C37 C36 116.8(9) . . ? C38 C37 C36 122.1(10) . . ? C37 C38 C39 118.8(10) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? C40 C39 C38 119.4(9) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 118.4(11) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? N4 C41 C40 123.0(11) . . ? N4 C41 H41 118.5 . . ? C40 C41 H41 118.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.096 _refine_diff_density_min -1.632 _refine_diff_density_rms 0.175 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 812551' #TrackingRef 'Compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H26 N2 O2 Pb S4' _chemical_formula_sum 'C12 H26 N2 O2 Pb S4' _chemical_formula_weight 565.78 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.4830(3) _cell_length_b 12.0326(4) _cell_length_c 8.1257(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.893(2) _cell_angle_gamma 90.00 _cell_volume 1024.40(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8464 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 8.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2767 _exptl_absorpt_correction_T_max 0.6717 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '144 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12071 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4569 _reflns_number_gt 3873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0481P)^2^+3.8090P] 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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.586(11) _refine_ls_number_reflns 4569 _refine_ls_number_parameters 197 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Pb Pb -0.71908(4) -0.69230(3) -0.91685(4) 0.02587(11) Uani 1 1 d . . . S1 S -0.8160(3) -0.8815(3) -1.0460(5) 0.0458(9) Uani 1 1 d . . . S2 S -0.9824(3) -0.6815(3) -1.0979(4) 0.0389(7) Uani 1 1 d . . . S3 S -0.4885(3) -0.7623(3) -1.0754(4) 0.0387(7) Uani 1 1 d . . . S4 S -0.6163(3) -0.5580(3) -1.2136(3) 0.0303(6) Uani 1 1 d . . . O1 O -1.0411(8) -0.8900(8) -1.1718(11) 0.036(2) Uani 1 1 d . . . O2 O -0.3794(7) -0.6249(7) -1.2612(9) 0.0292(17) Uani 1 1 d . . . N1 N -0.8778(11) -0.7209(10) -0.6587(13) 0.041(3) Uani 1 1 d . . . N2 N -0.6053(10) -0.8137(8) -0.6757(12) 0.031(2) Uani 1 1 d . . . C1 C -0.9562(12) -0.8146(11) -1.1074(15) 0.035(3) Uani 1 1 d . . . C2 C -1.1648(12) -0.8522(13) -1.2310(17) 0.043(3) Uani 1 1 d . . . H2A H -1.1554 -0.7910 -1.3111 0.051 Uiso 1 1 calc R . . H2B H -1.2150 -0.8246 -1.1383 0.051 Uiso 1 1 calc R . . C3 C -1.2294(15) -0.9479(15) -1.310(2) 0.060(4) Uani 1 1 d . . . H3A H -1.2381 -1.0078 -1.2299 0.091 Uiso 1 1 calc R . . H3B H -1.1789 -0.9743 -1.4020 0.091 Uiso 1 1 calc R . . H3C H -1.3142 -0.9253 -1.3523 0.091 Uiso 1 1 calc R . . C4 C -0.4907(14) -0.6422(14) -1.1899(15) 0.027(3) Uani 1 1 d . . . C5 C -0.3632(11) -0.5238(10) -1.3565(14) 0.032(3) Uani 1 1 d . . . H5A H -0.3645 -0.4579 -1.2835 0.038 Uiso 1 1 calc R . . H5B H -0.4330 -0.5165 -1.4408 0.038 Uiso 1 1 calc R . . C6 C -0.2343(16) -0.5325(11) -1.439(2) 0.036(4) Uani 1 1 d . . . H6A H -0.2316 -0.6013 -1.5032 0.054 Uiso 1 1 calc R . . H6B H -0.1656 -0.5333 -1.3540 0.054 Uiso 1 1 calc R . . H6C H -0.2233 -0.4686 -1.5116 0.054 Uiso 1 1 calc R . . C7 C -0.925(2) -0.6120(19) -0.631(3) 0.080(9) Uani 1 1 d . . . H7A H -0.9468 -0.6041 -0.5152 0.121 Uiso 1 1 calc R . . H7B H -1.0019 -0.5995 -0.7011 0.121 Uiso 1 1 calc R . . H7C H -0.8600 -0.5572 -0.6579 0.121 Uiso 1 1 calc R . . C8 C -0.982(3) -0.7969(19) -0.668(3) 0.110(11) Uani 1 1 d . . . H8A H -1.0358 -0.7801 -0.7659 0.165 Uiso 1 1 calc R . . H8B H -1.0323 -0.7900 -0.5694 0.165 Uiso 1 1 calc R . . H8C H -0.9490 -0.8729 -0.6763 0.165 Uiso 1 1 calc R . . C9 C -0.7785(19) -0.730(2) -0.518(2) 0.077(6) Uani 1 1 d . . . H9A H -0.7282 -0.6601 -0.5130 0.092 Uiso 1 1 calc R . . H9B H -0.8230 -0.7370 -0.4132 0.092 Uiso 1 1 calc R . . C10 C -0.6927(16) -0.8218(15) -0.5338(17) 0.055(4) Uani 1 1 d . . . H10A H -0.7436 -0.8908 -0.5460 0.065 Uiso 1 1 calc R . . H10B H -0.6402 -0.8283 -0.4307 0.065 Uiso 1 1 calc R . . C11 C -0.5701(16) -0.9293(11) -0.7211(16) 0.048(3) Uani 1 1 d . . . H11A H -0.5351 -0.9681 -0.6236 0.071 Uiso 1 1 calc R . . H11B H -0.5059 -0.9274 -0.8061 0.071 Uiso 1 1 calc R . . H11C H -0.6462 -0.9687 -0.7635 0.071 Uiso 1 1 calc R . . C12 C -0.4916(15) -0.7521(13) -0.6240(19) 0.048(4) Uani 1 1 d . . . H12A H -0.4549 -0.7847 -0.5225 0.073 Uiso 1 1 calc R . . H12B H -0.5143 -0.6743 -0.6040 0.073 Uiso 1 1 calc R . . H12C H -0.4288 -0.7556 -0.7106 0.073 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 Pb 0.02783(17) 0.02456(17) 0.02530(16) -0.0002(4) 0.00210(11) -0.0003(4) S1 0.0362(17) 0.0322(18) 0.068(2) -0.0169(17) -0.0146(16) 0.0100(14) S2 0.0286(15) 0.0307(17) 0.057(2) -0.0034(14) -0.0056(14) 0.0080(13) S3 0.0409(18) 0.0282(16) 0.0479(18) 0.0124(14) 0.0136(15) 0.0070(14) S4 0.0287(14) 0.0346(16) 0.0275(13) 0.0054(11) 0.0032(11) 0.0085(12) O1 0.023(4) 0.042(5) 0.043(5) -0.004(4) -0.007(4) 0.006(4) O2 0.028(4) 0.032(4) 0.028(4) 0.003(3) 0.004(3) 0.001(3) N1 0.044(7) 0.051(7) 0.031(5) 0.004(5) 0.014(5) 0.007(6) N2 0.037(5) 0.021(5) 0.036(5) -0.003(4) 0.003(4) -0.004(4) C1 0.033(6) 0.040(7) 0.031(6) -0.001(5) -0.009(5) 0.003(5) C2 0.031(6) 0.057(9) 0.039(7) 0.003(6) -0.014(5) 0.002(6) C3 0.049(9) 0.058(11) 0.073(10) -0.003(8) -0.016(8) -0.008(8) C4 0.027(6) 0.040(9) 0.015(5) -0.003(5) -0.003(5) -0.002(6) C5 0.034(6) 0.033(6) 0.028(6) 0.010(5) -0.003(5) -0.001(5) C6 0.026(8) 0.053(7) 0.030(9) 0.011(6) 0.000(6) -0.010(6) C7 0.069(14) 0.058(14) 0.118(18) -0.028(12) 0.059(13) 0.001(11) C8 0.14(2) 0.088(16) 0.111(17) -0.036(13) 0.097(17) -0.081(15) C9 0.068(13) 0.098(16) 0.066(11) 0.013(10) 0.026(10) 0.020(11) C10 0.060(10) 0.074(12) 0.030(6) 0.013(7) 0.001(6) -0.008(8) C11 0.076(10) 0.029(7) 0.036(7) 0.004(6) -0.019(7) 0.009(7) C12 0.050(8) 0.035(8) 0.059(9) 0.014(7) -0.013(7) -0.005(7) _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 Pb N2 2.691(10) . ? Pb S1 2.692(4) . ? Pb N1 2.741(10) . ? Pb S3 2.901(4) . ? Pb S2 3.088(3) . ? Pb S4 3.123(3) . ? S1 C1 1.735(13) . ? S2 C1 1.628(13) . ? S3 C4 1.718(16) . ? S4 C4 1.668(15) . ? O1 C1 1.363(15) . ? O1 C2 1.442(15) . ? O2 C4 1.336(17) . ? O2 C5 1.455(14) . ? N1 C7 1.42(2) . ? N1 C8 1.42(2) . ? N1 C9 1.52(2) . ? N2 C12 1.455(17) . ? N2 C11 1.489(16) . ? N2 C10 1.499(17) . ? C2 C3 1.47(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 C6 1.53(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.44(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 N2 Pb S1 88.7(2) . . ? N2 Pb N1 68.9(3) . . ? S1 Pb N1 87.8(3) . . ? N2 Pb S3 79.1(2) . . ? S1 Pb S3 83.72(11) . . ? N1 Pb S3 147.0(3) . . ? N2 Pb S2 137.5(2) . . ? S1 Pb S2 61.97(9) . . ? N1 Pb S2 79.3(3) . . ? S3 Pb S2 123.06(10) . . ? N2 Pb S4 133.4(2) . . ? S1 Pb S4 105.78(11) . . ? N1 Pb S4 152.7(3) . . ? S3 Pb S4 59.59(8) . . ? S2 Pb S4 86.33(9) . . ? C1 S1 Pb 91.4(4) . . ? C1 S2 Pb 80.3(4) . . ? C4 S3 Pb 90.0(5) . . ? C4 S4 Pb 83.6(5) . . ? C1 O1 C2 119.1(10) . . ? C4 O2 C5 118.7(10) . . ? C7 N1 C8 109.2(17) . . ? C7 N1 C9 100.4(16) . . ? C8 N1 C9 120.0(17) . . ? C7 N1 Pb 103.3(11) . . ? C8 N1 Pb 121.4(10) . . ? C9 N1 Pb 99.5(9) . . ? C12 N2 C11 109.9(11) . . ? C12 N2 C10 109.1(11) . . ? C11 N2 C10 107.0(11) . . ? C12 N2 Pb 105.8(7) . . ? C11 N2 Pb 115.7(7) . . ? C10 N2 Pb 109.1(8) . . ? O1 C1 S2 124.4(9) . . ? O1 C1 S1 109.7(9) . . ? S2 C1 S1 125.9(8) . . ? O1 C2 C3 107.1(12) . . ? O1 C2 H2A 110.3 . . ? C3 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C3 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 S4 123.6(12) . . ? O2 C4 S3 111.7(10) . . ? S4 C4 S3 124.7(9) . . ? O2 C5 C6 107.2(9) . . ? O2 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? O2 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 113.7(16) . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? N1 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 N2 114.7(13) . . ? C9 C10 H10A 108.6 . . ? N2 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? N2 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.269 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.175 # Attachment 'Compound 5.cif' data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 812552' #TrackingRef 'Compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H33 N3 O2 Pb S4' _chemical_formula_sum 'C15 H33 N3 O2 Pb S4' _chemical_formula_weight 622.87 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 13.1961(4) _cell_length_b 12.4450(4) _cell_length_c 15.2419(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.177(2) _cell_angle_gamma 90.00 _cell_volume 2364.21(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23061 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 7.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2118 _exptl_absorpt_correction_T_max 0.5208 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '293 2.0 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34275 _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5399 _reflns_number_gt 3855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.3994P] 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_extinction_coef ? _refine_ls_number_reflns 5399 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Pb Pb 0.251594(17) 0.324854(18) 0.681024(15) 0.03038(8) Uani 1 1 d . . . S1 S 0.32650(12) 0.14029(13) 0.59087(12) 0.0376(4) Uani 1 1 d . . . S2 S 0.13105(16) 0.10839(16) 0.64601(16) 0.0610(6) Uani 1 1 d . . . S3 S 0.12557(13) 0.41601(16) 0.50854(13) 0.0463(4) Uani 1 1 d . . . S4 S 0.36514(12) 0.43613(14) 0.57013(12) 0.0412(4) Uani 1 1 d . . . O1 O 0.2175(3) -0.0328(3) 0.5637(3) 0.0383(10) Uani 1 1 d . . . O2 O 0.2266(3) 0.4775(4) 0.4023(3) 0.0482(12) Uani 1 1 d . . . N1 N 0.0974(4) 0.3714(4) 0.7639(4) 0.0349(11) Uani 1 1 d . . . N2 N 0.2837(4) 0.5185(4) 0.7743(4) 0.0354(11) Uani 1 1 d . . . N3 N 0.4467(4) 0.3370(4) 0.8252(4) 0.0415(13) Uani 1 1 d . . . C1 C 0.2231(5) 0.0658(5) 0.6003(4) 0.0309(13) Uani 1 1 d . . . C2 C 0.1359(5) -0.1066(5) 0.5713(5) 0.0438(16) Uani 1 1 d . . . H2A H 0.0636 -0.0752 0.5422 0.053 Uiso 1 1 calc R . . H2B H 0.1459 -0.1215 0.6375 0.053 Uiso 1 1 calc R . . C3 C 0.1468(6) -0.2089(5) 0.5221(5) 0.0484(17) Uani 1 1 d . . . H3A H 0.1398 -0.1926 0.4574 0.073 Uiso 1 1 calc R . . H3B H 0.0904 -0.2594 0.5235 0.073 Uiso 1 1 calc R . . H3C H 0.2173 -0.2410 0.5533 0.073 Uiso 1 1 calc R . . C4 C 0.2425(5) 0.4457(5) 0.4906(5) 0.0375(14) Uani 1 1 d . . . C5 C 0.3167(6) 0.5197(6) 0.3776(5) 0.0508(18) Uani 1 1 d . . . H5A H 0.3068 0.5030 0.3118 0.061 Uiso 1 1 calc R . . H5B H 0.3842 0.4857 0.4167 0.061 Uiso 1 1 calc R . . C6 C 0.3232(6) 0.6394(6) 0.3920(6) 0.057(2) Uani 1 1 d . . . H6A H 0.2574 0.6730 0.3513 0.085 Uiso 1 1 calc R . . H6B H 0.3850 0.6677 0.3772 0.085 Uiso 1 1 calc R . . H6C H 0.3315 0.6556 0.4569 0.085 Uiso 1 1 calc R . . C7 C 0.1218(5) 0.3003(5) 0.8431(5) 0.0445(17) Uani 1 1 d . . . H7A H 0.0719 0.3140 0.8773 0.067 Uiso 1 1 calc R . . H7B H 0.1954 0.3132 0.8839 0.067 Uiso 1 1 calc R . . H7C H 0.1146 0.2255 0.8217 0.067 Uiso 1 1 calc R . . C8 C -0.0109(5) 0.3495(6) 0.7002(5) 0.0529(19) Uani 1 1 d . . . H8A H -0.0169 0.2733 0.6829 0.079 Uiso 1 1 calc R . . H8B H -0.0245 0.3936 0.6442 0.079 Uiso 1 1 calc R . . H8C H -0.0636 0.3669 0.7307 0.079 Uiso 1 1 calc R . . C9 C 0.1054(5) 0.4849(6) 0.7919(5) 0.0456(16) Uani 1 1 d . . . H9A H 0.0653 0.4959 0.8359 0.055 Uiso 1 1 calc R . . H9B H 0.0713 0.5299 0.7365 0.055 Uiso 1 1 calc R . . C10 C 0.2189(6) 0.5212(6) 0.8368(5) 0.0458(17) Uani 1 1 d . . . H10A H 0.2184 0.5955 0.8598 0.055 Uiso 1 1 calc R . . H10B H 0.2534 0.4747 0.8911 0.055 Uiso 1 1 calc R . . C11 C 0.2520(5) 0.6069(5) 0.7062(5) 0.0466(17) Uani 1 1 d . . . H11A H 0.1766 0.5980 0.6678 0.070 Uiso 1 1 calc R . . H11B H 0.2972 0.6057 0.6665 0.070 Uiso 1 1 calc R . . H11C H 0.2610 0.6758 0.7391 0.070 Uiso 1 1 calc R . . C12 C 0.4000(5) 0.5294(5) 0.8273(5) 0.0411(15) Uani 1 1 d . . . H12A H 0.4104 0.5917 0.8697 0.049 Uiso 1 1 calc R . . H12B H 0.4391 0.5444 0.7833 0.049 Uiso 1 1 calc R . . C13 C 0.4478(6) 0.4308(5) 0.8836(5) 0.0448(16) Uani 1 1 d . . . H13A H 0.5228 0.4465 0.9222 0.054 Uiso 1 1 calc R . . H13B H 0.4070 0.4138 0.9259 0.054 Uiso 1 1 calc R . . C14 C 0.5351(6) 0.3414(6) 0.7851(6) 0.056(2) Uani 1 1 d . . . H14A H 0.5337 0.4109 0.7544 0.084 Uiso 1 1 calc R . . H14B H 0.5260 0.2835 0.7396 0.084 Uiso 1 1 calc R . . H14C H 0.6041 0.3328 0.8348 0.084 Uiso 1 1 calc R . . C15 C 0.4526(7) 0.2365(7) 0.8756(6) 0.071(2) Uani 1 1 d . . . H15A H 0.5197 0.2342 0.9281 0.106 Uiso 1 1 calc R . . H15B H 0.4503 0.1759 0.8339 0.106 Uiso 1 1 calc R . . H15C H 0.3916 0.2318 0.8988 0.106 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 Pb 0.02996(12) 0.03183(13) 0.03320(13) -0.00445(11) 0.01560(9) -0.00329(10) S1 0.0352(8) 0.0374(8) 0.0467(10) -0.0094(7) 0.0223(7) -0.0055(7) S2 0.0571(11) 0.0492(11) 0.0977(16) -0.0274(11) 0.0540(12) -0.0172(9) S3 0.0326(8) 0.0612(11) 0.0491(10) -0.0016(9) 0.0190(8) -0.0041(8) S4 0.0333(8) 0.0519(10) 0.0423(10) 0.0024(8) 0.0177(7) -0.0041(7) O1 0.041(2) 0.031(2) 0.048(3) -0.005(2) 0.021(2) -0.0052(19) O2 0.044(3) 0.060(3) 0.044(3) 0.011(2) 0.019(2) -0.003(2) N1 0.029(2) 0.039(3) 0.036(3) -0.001(2) 0.010(2) 0.002(2) N2 0.040(3) 0.031(3) 0.038(3) -0.004(2) 0.017(2) -0.001(2) N3 0.040(3) 0.042(3) 0.043(3) 0.003(3) 0.015(2) 0.001(2) C1 0.034(3) 0.032(3) 0.024(3) -0.002(2) 0.006(2) 0.002(2) C2 0.046(4) 0.035(4) 0.056(4) -0.001(3) 0.025(3) -0.008(3) C3 0.059(4) 0.038(4) 0.048(4) -0.003(3) 0.017(3) -0.013(3) C4 0.040(3) 0.037(4) 0.041(4) -0.001(3) 0.020(3) 0.000(3) C5 0.055(4) 0.056(5) 0.053(4) 0.010(4) 0.034(4) -0.003(4) C6 0.046(4) 0.053(5) 0.070(6) 0.008(4) 0.018(4) -0.001(4) C7 0.045(4) 0.048(4) 0.045(4) 0.002(3) 0.020(3) -0.001(3) C8 0.034(3) 0.074(5) 0.049(4) -0.003(4) 0.011(3) 0.001(3) C9 0.042(4) 0.047(4) 0.054(4) -0.003(3) 0.025(3) 0.003(3) C10 0.062(4) 0.041(4) 0.044(4) -0.012(3) 0.030(3) -0.002(3) C11 0.057(4) 0.030(4) 0.058(5) 0.003(3) 0.026(4) 0.001(3) C12 0.048(4) 0.040(4) 0.042(4) -0.008(3) 0.024(3) -0.013(3) C13 0.053(4) 0.047(4) 0.035(4) 0.000(3) 0.015(3) -0.005(3) C14 0.045(4) 0.060(5) 0.063(5) 0.003(4) 0.019(4) 0.011(3) C15 0.080(6) 0.058(5) 0.072(6) 0.030(5) 0.024(5) 0.014(5) _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 Pb N2 2.759(5) . ? Pb N3 2.786(5) . ? Pb N1 2.786(5) . ? Pb S3 2.8446(19) . ? Pb S4 2.9468(16) . ? Pb S1 3.0055(16) . ? Pb S2 3.0846(18) . ? S1 C1 1.694(6) . ? S2 C1 1.673(6) . ? S3 C4 1.695(6) . ? S4 C4 1.677(7) . ? O1 C1 1.339(7) . ? O1 C2 1.450(7) . ? O2 C4 1.350(8) . ? O2 C5 1.459(7) . ? N1 C7 1.444(8) . ? N1 C8 1.465(8) . ? N1 C9 1.470(8) . ? N2 C10 1.475(8) . ? N2 C11 1.476(8) . ? N2 C12 1.487(8) . ? N3 C15 1.458(9) . ? N3 C13 1.465(8) . ? N3 C14 1.486(9) . ? C2 C3 1.509(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 C6 1.504(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.497(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.511(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 N2 Pb N3 66.45(15) . . ? N2 Pb N1 66.18(15) . . ? N3 Pb N1 104.74(15) . . ? N2 Pb S3 94.14(11) . . ? N3 Pb S3 144.62(12) . . ? N1 Pb S3 92.52(11) . . ? N2 Pb S4 82.20(11) . . ? N3 Pb S4 85.09(12) . . ? N1 Pb S4 138.36(11) . . ? S3 Pb S4 62.32(5) . . ? N2 Pb S1 152.28(11) . . ? N3 Pb S1 92.56(12) . . ? N1 Pb S1 139.91(11) . . ? S3 Pb S1 93.58(5) . . ? S4 Pb S1 77.96(5) . . ? N2 Pb S2 146.62(11) . . ? N3 Pb S2 118.33(12) . . ? N1 Pb S2 81.25(11) . . ? S3 Pb S2 94.40(6) . . ? S4 Pb S2 129.92(5) . . ? S1 Pb S2 58.79(4) . . ? C1 S1 Pb 89.1(2) . . ? C1 S2 Pb 86.9(2) . . ? C4 S3 Pb 87.1(2) . . ? C4 S4 Pb 84.1(2) . . ? C1 O1 C2 119.2(5) . . ? C4 O2 C5 119.3(5) . . ? C7 N1 C8 110.0(5) . . ? C7 N1 C9 111.8(5) . . ? C8 N1 C9 109.5(5) . . ? C7 N1 Pb 104.8(4) . . ? C8 N1 Pb 111.0(4) . . ? C9 N1 Pb 109.7(4) . . ? C10 N2 C11 110.3(5) . . ? C10 N2 C12 111.2(5) . . ? C11 N2 C12 108.5(5) . . ? C10 N2 Pb 109.2(4) . . ? C11 N2 Pb 109.2(4) . . ? C12 N2 Pb 108.4(3) . . ? C15 N3 C13 112.0(6) . . ? C15 N3 C14 109.6(6) . . ? C13 N3 C14 111.6(5) . . ? C15 N3 Pb 104.2(4) . . ? C13 N3 Pb 110.2(4) . . ? C14 N3 Pb 109.0(4) . . ? O1 C1 S2 121.0(4) . . ? O1 C1 S1 113.7(4) . . ? S2 C1 S1 125.2(4) . . ? O1 C2 C3 107.4(5) . . ? O1 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 S4 122.6(4) . . ? O2 C4 S3 111.9(5) . . ? S4 C4 S3 125.5(4) . . ? O2 C5 C6 109.3(6) . . ? O2 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O2 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 112.8(5) . . ? N1 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C9 113.8(5) . . ? N2 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? N2 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 113.5(5) . . ? N2 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N2 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N3 C13 C12 112.5(5) . . ? N3 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? N3 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.022 _refine_diff_density_min -1.957 _refine_diff_density_rms 0.160 # Attachment 'Compound 6.cif' data_h10kcm25 _database_code_depnum_ccdc_archive 'CCDC 812553' #TrackingRef 'Compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H41 N3 O2 Pb S4' _chemical_formula_sum 'C19 H41 N3 O2 Pb S4' _chemical_formula_weight 678.98 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.8180(4) _cell_length_b 8.1220(4) _cell_length_c 16.2173(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.683(3) _cell_angle_gamma 90.00 _cell_volume 1415.23(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15320 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 6.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3030 _exptl_absorpt_correction_T_max 0.6337 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '274 2.0 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20361 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_sigmaI/netI 0.1229 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.34 _reflns_number_total 6222 _reflns_number_gt 4419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(9) _refine_ls_number_reflns 6222 _refine_ls_number_parameters 269 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Pb Pb 0.60245(3) 0.75376(5) 0.25235(2) 0.02725(13) Uani 1 1 d . . . S1 S 0.4518(3) 0.6116(4) 0.11581(19) 0.0346(7) Uani 1 1 d . . . S2 S 0.3496(3) 0.6034(4) 0.2803(2) 0.0410(8) Uani 1 1 d . . . S3 S 0.7594(3) 0.4738(4) 0.2207(2) 0.0339(7) Uani 1 1 d . . . S4 S 0.8498(4) 0.6576(5) 0.3757(3) 0.0612(11) Uani 1 1 d . . . O1 O 0.2424(7) 0.4902(10) 0.1372(5) 0.033(2) Uani 1 1 d . . . O2 O 0.9434(8) 0.3837(10) 0.3219(5) 0.040(2) Uani 1 1 d . . . N1 N 0.7228(10) 0.8986(11) 0.1410(7) 0.041(3) Uani 1 1 d . . . N2 N 0.4881(9) 1.0423(12) 0.1975(6) 0.034(2) Uani 1 1 d . . . N3 N 0.5902(9) 1.0053(12) 0.3821(6) 0.032(2) Uani 1 1 d . . . C1 C 0.3379(12) 0.5644(14) 0.1783(9) 0.029(3) Uani 1 1 d . . . C2 C 0.8562(12) 0.5007(15) 0.3083(8) 0.040(3) Uani 1 1 d . . . C3 C 0.1400(12) 0.4386(17) 0.1817(8) 0.044(3) Uani 1 1 d . . . H3A H 0.1038 0.5349 0.2076 0.053 Uiso 1 1 calc R . . H3B H 0.1696 0.3591 0.2259 0.053 Uiso 1 1 calc R . . C4 C 0.0432(11) 0.3589(14) 0.1191(8) 0.034(3) Uani 1 1 d . . . H4A H 0.0823 0.2672 0.0914 0.040 Uiso 1 1 calc R . . H4B H -0.0237 0.3120 0.1487 0.040 Uiso 1 1 calc R . . C5 C -0.0131(11) 0.4786(14) 0.0543(7) 0.036(3) Uani 1 1 d . . . H5A H -0.0422 0.5768 0.0827 0.043 Uiso 1 1 calc R . . H5B H 0.0526 0.5152 0.0207 0.043 Uiso 1 1 calc R . . C6 C -0.1193(11) 0.4113(15) -0.0027(9) 0.042(3) Uani 1 1 d . . . H6A H -0.0898 0.3207 -0.0352 0.063 Uiso 1 1 calc R . . H6B H -0.1542 0.4984 -0.0403 0.063 Uiso 1 1 calc R . . H6C H -0.1837 0.3706 0.0300 0.063 Uiso 1 1 calc R . . C7 C 1.0343(17) 0.388(2) 0.3982(10) 0.051(5) Uani 1 1 d . . . H7A H 0.9907 0.3806 0.4485 0.061 Uiso 1 1 calc R . . H7B H 1.0828 0.4919 0.4007 0.061 Uiso 1 1 calc R . . C8 C 1.1192(10) 0.241(3) 0.3924(8) 0.048(3) Uani 1 1 d . . . H8A H 1.1598 0.2505 0.3409 0.058 Uiso 1 1 calc R . . H8B H 1.1855 0.2437 0.4399 0.058 Uiso 1 1 calc R . . C9 C 1.0563(16) 0.082(2) 0.3920(12) 0.050(5) Uani 1 1 d . . . H9A H 0.9967 0.0732 0.3410 0.060 Uiso 1 1 calc R . . H9B H 1.0081 0.0764 0.4402 0.060 Uiso 1 1 calc R . . C10 C 1.1444(14) -0.0646(19) 0.3956(12) 0.070(5) Uani 1 1 d . . . H10A H 1.1857 -0.0677 0.3449 0.105 Uiso 1 1 calc R . . H10B H 1.0972 -0.1666 0.4001 0.105 Uiso 1 1 calc R . . H10C H 1.2071 -0.0539 0.4440 0.105 Uiso 1 1 calc R . . C11 C 0.7084(11) 0.8084(13) 0.0620(6) 0.032(3) Uani 1 1 d . . . H11A H 0.6202 0.8050 0.0399 0.048 Uiso 1 1 calc R . . H11B H 0.7397 0.6959 0.0711 0.048 Uiso 1 1 calc R . . H11C H 0.7558 0.8643 0.0222 0.048 Uiso 1 1 calc R . . C12 C 0.8603(12) 0.8972(17) 0.1747(8) 0.047(4) Uani 1 1 d . . . H12A H 0.9083 0.9541 0.1357 0.070 Uiso 1 1 calc R . . H12B H 0.8892 0.7831 0.1816 0.070 Uiso 1 1 calc R . . H12C H 0.8717 0.9534 0.2286 0.070 Uiso 1 1 calc R . . C13 C 0.6786(15) 1.0682(15) 0.1265(9) 0.050(4) Uani 1 1 d . . . H13A H 0.7170 1.1390 0.1721 0.060 Uiso 1 1 calc R . . H13B H 0.7064 1.1087 0.0741 0.060 Uiso 1 1 calc R . . C14 C 0.5432(15) 1.0837(17) 0.1213(8) 0.056(4) Uani 1 1 d . . . H14A H 0.5054 1.0116 0.0760 0.067 Uiso 1 1 calc R . . H14B H 0.5203 1.1986 0.1058 0.067 Uiso 1 1 calc R . . C15 C 0.3540(14) 1.0184(19) 0.1775(10) 0.049(4) Uani 1 1 d . . . H15A H 0.3166 1.1185 0.1518 0.074 Uiso 1 1 calc R . . H15B H 0.3168 0.9946 0.2285 0.074 Uiso 1 1 calc R . . H15C H 0.3387 0.9259 0.1389 0.074 Uiso 1 1 calc R . . C16 C 0.5112(14) 1.1733(16) 0.2608(8) 0.045(3) Uani 1 1 d . . . H16A H 0.4534 1.2656 0.2454 0.055 Uiso 1 1 calc R . . H16B H 0.5970 1.2152 0.2598 0.055 Uiso 1 1 calc R . . C17 C 0.4962(12) 1.1209(16) 0.3478(8) 0.041(3) Uani 1 1 d . . . H17A H 0.4994 1.2197 0.3837 0.050 Uiso 1 1 calc R . . H17B H 0.4131 1.0700 0.3482 0.050 Uiso 1 1 calc R . . C18 C 0.7091(13) 1.0827(19) 0.4078(10) 0.058(4) Uani 1 1 d . . . H18A H 0.7296 1.1585 0.3644 0.087 Uiso 1 1 calc R . . H18B H 0.7738 0.9980 0.4170 0.087 Uiso 1 1 calc R . . H18C H 0.7044 1.1439 0.4594 0.087 Uiso 1 1 calc R . . C19 C 0.5478(13) 0.9141(18) 0.4521(8) 0.053(4) Uani 1 1 d . . . H19A H 0.5334 0.9914 0.4964 0.079 Uiso 1 1 calc R . . H19B H 0.6115 0.8341 0.4732 0.079 Uiso 1 1 calc R . . H19C H 0.4701 0.8563 0.4332 0.079 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 Pb 0.0327(2) 0.01985(18) 0.0299(2) -0.0006(4) 0.00653(14) 0.0002(3) S1 0.0364(17) 0.0358(17) 0.0332(17) -0.0025(13) 0.0114(14) -0.0068(14) S2 0.047(2) 0.0435(19) 0.0343(19) -0.0081(15) 0.0130(16) -0.0052(15) S3 0.0343(17) 0.0256(16) 0.0411(18) -0.0028(13) 0.0017(15) 0.0013(13) S4 0.076(3) 0.047(2) 0.055(2) -0.0188(19) -0.017(2) 0.022(2) O1 0.023(4) 0.037(5) 0.042(5) -0.005(4) 0.014(4) -0.009(4) O2 0.051(5) 0.034(5) 0.035(5) -0.003(4) 0.010(4) 0.006(4) N1 0.061(7) 0.018(5) 0.047(7) 0.007(5) 0.023(6) 0.002(5) N2 0.029(6) 0.027(6) 0.043(6) -0.004(5) -0.009(5) 0.005(4) N3 0.033(6) 0.028(5) 0.035(6) 0.000(4) 0.008(5) 0.003(5) C1 0.027(7) 0.008(6) 0.053(9) 0.002(6) 0.004(6) 0.005(5) C2 0.047(8) 0.023(7) 0.051(9) -0.004(6) 0.013(7) 0.000(6) C3 0.038(8) 0.045(8) 0.053(9) -0.003(7) 0.024(7) -0.004(6) C4 0.031(7) 0.028(7) 0.042(8) 0.003(6) 0.003(6) -0.008(5) C5 0.033(7) 0.027(6) 0.049(8) 0.003(6) 0.017(6) 0.003(5) C6 0.034(7) 0.025(7) 0.065(10) 0.000(6) 0.000(7) -0.001(5) C7 0.060(11) 0.061(11) 0.027(9) -0.007(8) -0.011(8) 0.004(9) C8 0.034(6) 0.048(8) 0.061(8) 0.016(11) -0.001(5) -0.009(10) C9 0.035(9) 0.060(11) 0.053(11) 0.002(8) -0.006(8) -0.001(8) C10 0.047(9) 0.048(10) 0.117(15) -0.011(10) 0.018(10) 0.002(8) C11 0.044(7) 0.026(7) 0.028(6) -0.005(4) 0.010(6) -0.002(5) C12 0.045(9) 0.055(9) 0.041(8) -0.003(7) 0.011(7) -0.014(7) C13 0.089(12) 0.024(7) 0.039(8) 0.001(6) 0.015(8) -0.007(7) C14 0.100(13) 0.037(8) 0.029(8) 0.006(6) 0.008(8) 0.024(8) C15 0.057(10) 0.042(10) 0.048(9) 0.002(8) 0.000(8) 0.019(8) C16 0.060(9) 0.027(6) 0.049(9) -0.004(6) 0.004(7) 0.011(6) C17 0.046(8) 0.038(8) 0.043(8) -0.012(6) 0.016(7) -0.001(6) C18 0.040(8) 0.060(10) 0.073(11) -0.021(8) 0.005(8) -0.008(7) C19 0.062(10) 0.056(9) 0.042(8) 0.011(7) 0.019(7) 0.017(7) _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 Pb N1 2.624(9) . ? Pb N2 2.749(9) . ? Pb S1 2.838(3) . ? Pb S3 2.919(3) . ? Pb N3 2.947(9) . ? Pb S2 3.077(3) . ? Pb S4 3.245(4) . ? S1 C1 1.727(13) . ? S2 C1 1.675(15) . ? S3 C2 1.677(14) . ? S4 C2 1.686(13) . ? O1 C1 1.309(15) . ? O1 C3 1.452(13) . ? O2 C2 1.339(15) . ? O2 C7 1.489(19) . ? N1 C13 1.468(16) . ? N1 C11 1.469(14) . ? N1 C12 1.523(17) . ? N2 C15 1.463(17) . ? N2 C14 1.472(16) . ? N2 C16 1.480(16) . ? N3 C17 1.448(16) . ? N3 C18 1.449(16) . ? N3 C19 1.472(15) . ? C3 C4 1.515(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.508(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.492(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.52(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.46(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.52(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.46(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.500(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 N1 Pb N2 68.6(3) . . ? N1 Pb S1 86.1(3) . . ? N2 Pb S1 84.2(2) . . ? N1 Pb S3 83.3(2) . . ? N2 Pb S3 148.9(2) . . ? S1 Pb S3 80.74(9) . . ? N1 Pb N3 104.3(3) . . ? N2 Pb N3 65.4(3) . . ? S1 Pb N3 140.3(2) . . ? S3 Pb N3 137.8(2) . . ? N1 Pb S2 143.1(3) . . ? N2 Pb S2 90.7(2) . . ? S1 Pb S2 60.91(8) . . ? S3 Pb S2 105.20(9) . . ? N3 Pb S2 93.16(19) . . ? N1 Pb S4 95.3(3) . . ? N2 Pb S4 135.4(2) . . ? S1 Pb S4 137.80(9) . . ? S3 Pb S4 57.71(9) . . ? N3 Pb S4 80.2(2) . . ? S2 Pb S4 119.82(11) . . ? C1 S1 Pb 91.0(5) . . ? C1 S2 Pb 84.0(5) . . ? C2 S3 Pb 93.9(4) . . ? C2 S4 Pb 82.8(5) . . ? C1 O1 C3 118.9(10) . . ? C2 O2 C7 120.3(11) . . ? C13 N1 C11 109.1(10) . . ? C13 N1 C12 110.6(11) . . ? C11 N1 C12 108.0(9) . . ? C13 N1 Pb 110.6(7) . . ? C11 N1 Pb 111.5(7) . . ? C12 N1 Pb 106.9(7) . . ? C15 N2 C14 109.4(11) . . ? C15 N2 C16 109.4(10) . . ? C14 N2 C16 111.5(10) . . ? C15 N2 Pb 110.8(8) . . ? C14 N2 Pb 104.8(7) . . ? C16 N2 Pb 110.8(7) . . ? C17 N3 C18 112.9(11) . . ? C17 N3 C19 110.8(9) . . ? C18 N3 C19 110.0(11) . . ? C17 N3 Pb 105.3(7) . . ? C18 N3 Pb 113.2(7) . . ? C19 N3 Pb 104.2(7) . . ? O1 C1 S2 123.6(10) . . ? O1 C1 S1 112.3(10) . . ? S2 C1 S1 124.1(8) . . ? O2 C2 S3 113.9(9) . . ? O2 C2 S4 120.7(10) . . ? S3 C2 S4 125.4(8) . . ? O1 C3 C4 107.4(10) . . ? O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C5 C4 C3 112.5(10) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 114.5(10) . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 C8 105.9(12) . . ? O2 C7 H7A 110.6 . . ? C8 C7 H7A 110.6 . . ? O2 C7 H7B 110.6 . . ? C8 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C9 C8 C7 114.4(11) . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 113.7(14) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N1 113.3(11) . . ? C14 C13 H13A 108.9 . . ? N1 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? N1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 N2 115.6(11) . . ? C13 C14 H14A 108.4 . . ? N2 C14 H14A 108.4 . . ? C13 C14 H14B 108.4 . . ? N2 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 114.9(11) . . ? N2 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? N2 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N3 C17 C16 113.4(10) . . ? N3 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? N3 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.799 _refine_diff_density_min -2.404 _refine_diff_density_rms 0.220