# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1802 data_global _Publ_section_title ; Lead(II) complexes with phosphorylthiolato and thiophosphorylthiolato ligands. The X-ray crystal and molecular structures of [Pb{2-(Ph2PO)6-(Me3Si)C6H3S}2], [Pb{2-(Ph2P(O)CH2)C6H4S}2], [Pb{2-(Ph2P(S)CH2)C6H4S}2] and [Pb{2,6-(Ph2P(S)CH2)2C6H3S}2] ; data_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H16 O P Pb0.50 S' _chemical_formula_weight 426.94 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' 'Pb' 'Pb' -3.3944 10.1111 '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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 14.6460(10) _cell_length_b 15.5010(10) _cell_length_c 15.4290(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.583(2) _cell_angle_gamma 90.00 _cell_volume 3453.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour white _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 5.131 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'nraf-nonius DIP2000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6487 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.42 _reflns_number_total 3674 _reflns_number_gt 3359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP2000 software Xpress (MAC science, 1989)' _computing_cell_refinement 'DIP2000 software DENZO (Otwinowski & Minor, 1996)' _computing_data_reduction 'DIP2000 software DENZO (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0649P)^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 mixed _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 0.066(10) _refine_ls_number_reflns 3674 _refine_ls_number_parameters 384 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 0.506494(19) 0.102246(4) 0.90630(2) 0.04496(2) Uani 1 1 d . . . S1 S 0.54218(4) 0.21493(5) 1.03072(4) 0.0678(2) Uani 1 1 d . . . S2 S 0.47522(4) 0.21655(5) 0.78000(5) 0.0679(2) Uani 1 1 d . . . O1 O 0.67496(11) 0.10383(9) 0.88960(12) 0.0475(5) Uani 1 1 d . . . O2 O 0.33005(12) 0.10683(9) 0.91117(11) 0.0460(5) Uani 1 1 d . . . P1 P 0.76845(4) 0.14872(4) 0.93972(4) 0.04909(17) Uani 1 1 d . . . P2 P 0.24782(4) 0.15055(5) 0.87421(4) 0.05029(18) Uani 1 1 d . . . C11 C 0.61477(13) 0.15182(17) 1.09982(13) 0.0511(6) Uani 1 1 d . . . C12 C 0.71508(14) 0.15634(14) 1.09866(14) 0.0435(6) Uani 1 1 d . . . C13 C 0.76529(17) 0.10108(17) 1.15589(19) 0.0742(9) Uani 1 1 d . . . H13 H 0.8281 0.1017 1.1526 0.089 Uiso 1 1 calc R . . C14 C 0.7424(3) 0.0425(3) 1.21979(19) 0.1231(17) Uani 1 1 d . . . H14 H 0.7849 0.0094 1.2573 0.148 Uiso 1 1 calc R . . C15 C 0.6402(3) 0.0420(3) 1.21776(19) 0.1006(15) Uani 1 1 d . . . H15 H 0.6150 0.0043 1.2544 0.121 Uiso 1 1 calc R . . C16 C 0.5786(2) 0.0994(2) 1.15928(18) 0.0855(15) Uani 1 1 d . . . H16 H 0.5156 0.1009 1.1619 0.103 Uiso 1 1 calc R . . C17 C 0.7559(2) 0.20461(18) 1.0373(2) 0.0831(10) Uani 1 1 d . . . H17A H 0.8166 0.2238 1.0657 0.100 Uiso 1 1 calc R . . H17B H 0.7185 0.2556 1.0214 0.100 Uiso 1 1 calc R . . C21 C 0.85796(17) 0.0710(2) 0.96823(18) 0.0637(8) Uani 1 1 d . . . C22 C 0.8445(3) -0.0189(2) 0.9552(2) 0.1010(12) Uani 1 1 d . . . H22 H 0.7868 -0.0366 0.9260 0.121 Uiso 1 1 calc R . . C23 C 0.9061(3) -0.0798(2) 0.9807(4) 0.1401(16) Uani 1 1 d . . . H23 H 0.8944 -0.1387 0.9750 0.168 Uiso 1 1 calc R . . C24 C 1.00412(19) -0.0388(2) 1.0229(2) 0.0809(9) Uani 1 1 d . . . H24 H 1.0556 -0.0733 1.0413 0.097 Uiso 1 1 calc R . . C25 C 1.00830(19) 0.0382(3) 1.0297(3) 0.1184(14) Uani 1 1 d . . . H25 H 1.0678 0.0571 1.0521 0.142 Uiso 1 1 calc R . . C26 C 0.9509(3) 0.1012(2) 1.0135(4) 0.1031(17) Uani 1 1 d . . . C31 C 0.20857(13) 0.23581(11) 0.93542(13) 0.0692(9) Uani 1 1 d G . . C32 C 0.26363(19) 0.25628(17) 1.01484(16) 0.1103(16) Uani 1 1 d G . . H32 H 0.3167 0.2238 1.0333 0.132 Uiso 1 1 calc R . . C33 C 0.2432(3) 0.3219(2) 1.0667(2) 0.195(2) Uani 1 1 d G . . H33 H 0.2811 0.3345 1.1198 0.234 Uiso 1 1 calc R . . C34 C 0.1676(3) 0.3669(2) 1.0392(3) 0.1188(13) Uani 1 1 d G . . H34 H 0.1513 0.4124 1.0729 0.143 Uiso 1 1 calc R . . C35 C 0.1125(2) 0.3465(2) 0.9597(3) 0.208(3) Uani 1 1 d G . . H35 H 0.0595 0.3789 0.9413 0.250 Uiso 1 1 calc R . . C36 C 0.13300(16) 0.28089(16) 0.90785(19) 0.170(2) Uani 1 1 d G . . H36 H 0.0951 0.2682 0.8548 0.205 Uiso 1 1 calc R . . C41 C 0.38786(16) 0.14761(18) 0.70830(15) 0.0520(7) Uani 1 1 d . . . C42 C 0.29900(17) 0.14848(19) 0.70923(16) 0.0618(8) Uani 1 1 d . . . C43 C 0.23012(19) 0.10376(16) 0.64866(18) 0.0597(9) Uani 1 1 d . . . H43 H 0.1666 0.1071 0.6477 0.072 Uiso 1 1 calc R . . C44 C 0.2709(2) 0.0570(2) 0.5944(2) 0.0909(10) Uani 1 1 d . . . H44 H 0.2311 0.0229 0.5554 0.109 Uiso 1 1 calc R . . C45 C 0.3528(3) 0.0516(2) 0.58749(19) 0.0785(11) Uani 1 1 d . . . H45 H 0.3708 0.0171 0.5440 0.094 Uiso 1 1 calc R . . C46 C 0.4192(2) 0.09741(19) 0.6450(2) 0.0684(10) Uani 1 1 d . . . H46 H 0.4818 0.0943 0.6410 0.082 Uiso 1 1 calc R . . C47 C 0.26052(14) 0.21091(15) 0.77561(14) 0.0454(6) Uani 1 1 d . . . H47A H 0.2011 0.2341 0.7486 0.054 Uiso 1 1 calc R . . H47B H 0.3030 0.2586 0.7908 0.054 Uiso 1 1 calc R . . C51 C 0.15452(16) 0.07528(17) 0.84062(17) 0.0547(7) Uani 1 1 d . . . C52 C 0.1767(2) -0.00816(18) 0.85603(19) 0.0628(8) Uani 1 1 d . . . H52 H 0.2355 -0.0250 0.8832 0.075 Uiso 1 1 calc R . . C53 C 0.1045(3) -0.0700(3) 0.8282(3) 0.0982(14) Uani 1 1 d . . . H53 H 0.1218 -0.1270 0.8404 0.118 Uiso 1 1 calc R . . C54 C 0.0302(3) -0.0616(3) 0.7941(3) 0.1122(16) Uani 1 1 d . . . H54 H -0.0090 -0.1086 0.7806 0.135 Uiso 1 1 calc R . . C55 C -0.0015(2) 0.0282(2) 0.7719(2) 0.0894(11) Uani 1 1 d . . . H55 H -0.0598 0.0421 0.7412 0.107 Uiso 1 1 calc R . . C56 C 0.0732(3) 0.09486(19) 0.8057(4) 0.0923(16) Uani 1 1 d . . . H56 H 0.0577 0.1530 0.8000 0.111 Uiso 1 1 calc R . . C61 C 0.81385(12) 0.21818(15) 0.85644(12) 0.0728(10) Uani 1 1 d G . . C62 C 0.82010(19) 0.1823(2) 0.77276(16) 0.1326(18) Uani 1 1 d G . . H62 H 0.7993 0.1262 0.7604 0.159 Uiso 1 1 calc R . . C63 C 0.8562(3) 0.2281(3) 0.7089(2) 0.168(3) Uani 1 1 d G . . H63 H 0.8598 0.2037 0.6545 0.202 Uiso 1 1 calc R . . C64 C 0.8860(3) 0.3097(3) 0.7288(3) 0.193(3) Uani 1 1 d G . . H64 H 0.9106 0.3423 0.6875 0.231 Uiso 1 1 calc R . . C65 C 0.8797(3) 0.3457(2) 0.8124(3) 0.181(3) Uani 1 1 d G . . H65 H 0.9005 0.4017 0.8248 0.217 Uiso 1 1 calc R . . C66 C 0.8437(2) 0.29989(18) 0.87629(19) 0.1477(18) Uani 1 1 d G . . H66 H 0.8401 0.3243 0.9307 0.177 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 0.03312(3) 0.05364(3) 0.04605(3) -0.00036(9) 0.00054(3) 0.00004(9) S1 0.0496(3) 0.0720(4) 0.0714(4) -0.0212(3) -0.0207(3) 0.0264(3) S2 0.0428(3) 0.0858(4) 0.0749(4) 0.0279(3) 0.0088(3) -0.0176(3) O1 0.0215(7) 0.0660(10) 0.0516(8) -0.0195(6) -0.0041(7) 0.0012(6) O2 0.0280(7) 0.0638(10) 0.0398(7) 0.0044(6) -0.0130(7) 0.0121(6) P1 0.0305(2) 0.0496(3) 0.0635(3) 0.0027(3) -0.0032(3) 0.0045(2) P2 0.0380(3) 0.0600(4) 0.0549(3) 0.0122(3) 0.0137(2) 0.0001(3) C11 0.0237(8) 0.0868(14) 0.0405(9) -0.0348(9) -0.0010(7) 0.0170(9) C12 0.0363(9) 0.0407(9) 0.0458(10) -0.0154(8) -0.0162(8) -0.0001(9) C13 0.0366(10) 0.113(2) 0.0582(13) -0.0179(13) -0.0362(10) 0.0440(10) C14 0.148(3) 0.186(4) 0.0422(13) 0.022(2) 0.0369(16) 0.058(3) C15 0.093(2) 0.165(4) 0.0445(13) 0.0173(19) 0.0121(15) -0.008(3) C16 0.0471(15) 0.180(4) 0.0288(10) -0.0058(15) 0.0046(11) -0.0038(17) C17 0.0504(13) 0.0640(14) 0.131(2) -0.0507(14) 0.0031(15) -0.0109(12) C21 0.0373(11) 0.0848(16) 0.0606(14) -0.0126(14) -0.0162(11) -0.0174(12) C22 0.0837(19) 0.0707(17) 0.128(2) -0.0394(17) -0.0417(19) 0.0160(16) C23 0.093(2) 0.0939(18) 0.202(4) -0.076(2) -0.069(2) 0.0574(16) C24 0.0576(12) 0.0929(17) 0.0829(18) -0.0067(16) -0.0150(13) 0.0496(11) C25 0.0397(11) 0.193(3) 0.111(3) -0.021(3) -0.0185(14) 0.0659(15) C26 0.0405(16) 0.143(4) 0.115(3) -0.040(2) -0.0178(19) -0.0023(16) C31 0.0566(13) 0.0537(14) 0.1019(19) -0.0030(15) 0.0267(13) -0.0045(12) C32 0.129(3) 0.107(3) 0.096(2) -0.025(2) 0.022(2) 0.013(3) C33 0.218(5) 0.239(4) 0.135(2) -0.113(2) 0.044(3) 0.068(4) C34 0.160(3) 0.0730(18) 0.146(2) -0.0276(18) 0.0920(19) 0.024(2) C35 0.122(3) 0.149(3) 0.342(7) -0.131(3) 0.003(4) 0.071(2) C36 0.148(3) 0.128(3) 0.219(5) -0.066(3) -0.017(4) 0.078(2) C41 0.0451(11) 0.0644(14) 0.0392(10) 0.0122(10) -0.0143(10) -0.0073(11) C42 0.0562(12) 0.0793(15) 0.0479(11) 0.0214(11) 0.0032(11) -0.0324(12) C43 0.0300(11) 0.097(2) 0.0433(12) 0.0048(11) -0.0191(10) -0.0172(10) C44 0.0794(16) 0.0884(18) 0.089(2) -0.0157(16) -0.0324(15) -0.0472(14) C45 0.111(3) 0.0751(19) 0.0447(12) -0.0090(13) 0.0000(16) 0.0033(19) C46 0.0414(14) 0.096(2) 0.0664(17) 0.0169(14) 0.0058(13) -0.0043(12) C47 0.0327(9) 0.0548(12) 0.0451(10) 0.0109(10) -0.0041(9) -0.0038(9) C51 0.0460(10) 0.0641(12) 0.0582(12) 0.0047(11) 0.0206(9) -0.0334(9) C52 0.0534(12) 0.0582(14) 0.0741(16) 0.0033(13) 0.0028(12) -0.0202(12) C53 0.088(2) 0.077(2) 0.117(3) -0.013(2) -0.019(2) -0.009(2) C54 0.102(3) 0.072(2) 0.144(3) 0.019(2) -0.030(3) -0.015(2) C55 0.0465(12) 0.088(2) 0.116(2) 0.0230(19) -0.0412(14) -0.0186(14) C56 0.0404(15) 0.0699(19) 0.161(4) 0.0243(19) 0.002(2) -0.0130(12) C61 0.0468(13) 0.088(2) 0.0850(18) 0.0047(17) 0.0147(13) -0.0099(14) C62 0.218(4) 0.115(3) 0.0788(19) 0.023(2) 0.066(2) 0.039(3) C63 0.146(4) 0.279(8) 0.092(3) 0.015(4) 0.054(2) 0.025(5) C64 0.122(3) 0.348(8) 0.113(3) 0.018(4) 0.032(3) -0.111(4) C65 0.170(5) 0.241(6) 0.138(4) 0.050(4) 0.045(4) -0.047(5) C66 0.178(3) 0.121(3) 0.166(4) -0.033(3) 0.091(2) -0.088(2) _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 O1 2.5232(17) . ? Pb S1 2.5837(7) . ? Pb O2 2.5987(18) . ? Pb S2 2.6171(8) . ? S1 C11 1.687(2) . ? S2 C41 1.879(2) . ? O1 P1 1.6138(16) . ? O2 P2 1.4164(17) . ? P1 C17 1.773(3) . ? P1 C21 1.781(3) . ? P1 C61 1.881(2) . ? P2 C31 1.775(2) . ? P2 C51 1.806(2) . ? P2 C47 1.822(2) . ? C11 C16 1.394(4) . ? C11 C12 1.474(3) . ? C12 C13 1.356(3) . ? C12 C17 1.415(4) . ? C13 C14 1.421(5) . ? C14 C15 1.493(6) . ? C15 C16 1.466(5) . ? C21 C22 1.416(4) . ? C21 C26 1.498(5) . ? C22 C23 1.321(5) . ? C23 C24 1.605(5) . ? C24 C25 1.199(6) . ? C25 C26 1.285(5) . ? C31 C36 1.3181(11) . ? C31 C32 1.3870(11) . ? C32 C33 1.3580(11) . ? C33 C34 1.3178(11) . ? C34 C35 1.3874(11) . ? C35 C36 1.3578(11) . ? C41 C42 1.304(4) . ? C41 C46 1.385(4) . ? C42 C43 1.435(4) . ? C42 C47 1.580(4) . ? C43 C44 1.322(5) . ? C44 C45 1.226(5) . ? C45 C46 1.396(5) . ? C51 C56 1.260(4) . ? C51 C52 1.345(4) . ? C52 C53 1.439(5) . ? C53 C54 1.134(6) . ? C54 C55 1.489(5) . ? C55 C56 1.532(5) . ? C61 C66 1.3580(14) . ? C61 C62 1.4227(15) . ? C62 C63 1.3879(14) . ? C63 C64 1.3578(14) . ? C64 C65 1.4231(15) . ? C65 C66 1.3878(14) . ? 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 Pb S1 89.37(4) . . ? O1 Pb O2 175.34(6) . . ? S1 Pb O2 92.24(4) . . ? O1 Pb S2 88.30(4) . . ? S1 Pb S2 94.83(2) . . ? O2 Pb S2 87.21(4) . . ? C11 S1 Pb 96.07(8) . . ? C41 S2 Pb 94.07(8) . . ? P1 O1 Pb 136.17(10) . . ? P2 O2 Pb 141.67(10) . . ? O1 P1 C17 114.69(12) . . ? O1 P1 C21 110.94(11) . . ? C17 P1 C21 107.28(13) . . ? O1 P1 C61 106.73(9) . . ? C17 P1 C61 113.52(12) . . ? C21 P1 C61 103.11(12) . . ? O2 P2 C31 118.10(10) . . ? O2 P2 C51 111.01(11) . . ? C31 P2 C51 109.71(11) . . ? O2 P2 C47 112.56(11) . . ? C31 P2 C47 98.57(10) . . ? C51 P2 C47 105.65(11) . . ? C16 C11 C12 121.6(2) . . ? C16 C11 S1 119.02(19) . . ? C12 C11 S1 119.29(17) . . ? C13 C12 C17 121.7(2) . . ? C13 C12 C11 113.3(2) . . ? C17 C12 C11 124.5(2) . . ? C12 C13 C14 133.7(3) . . ? C13 C14 C15 109.9(3) . . ? C16 C15 C14 121.4(4) . . ? C11 C16 C15 119.8(3) . . ? C12 C17 P1 115.2(2) . . ? C22 C21 C26 117.9(3) . . ? C22 C21 P1 123.4(2) . . ? C26 C21 P1 118.5(2) . . ? C23 C22 C21 126.1(3) . . ? C22 C23 C24 111.0(3) . . ? C25 C24 C23 117.3(3) . . ? C24 C25 C26 135.8(3) . . ? C25 C26 C21 111.6(3) . . ? C36 C31 C32 119.8 . . ? C36 C31 P2 123.51(11) . . ? C32 C31 P2 116.63(11) . . ? C33 C32 C31 122.6 . . ? C34 C33 C32 117.6 . . ? C33 C34 C35 119.8 . . ? C36 C35 C34 122.6 . . ? C31 C36 C35 117.5 . . ? C42 C41 C46 117.5(2) . . ? C42 C41 S2 124.8(2) . . ? C46 C41 S2 117.4(2) . . ? C41 C42 C43 125.6(3) . . ? C41 C42 C47 118.6(2) . . ? C43 C42 C47 115.5(2) . . ? C44 C43 C42 109.5(3) . . ? C45 C44 C43 130.1(3) . . ? C44 C45 C46 119.9(3) . . ? C41 C46 C45 117.1(3) . . ? C42 C47 P2 108.90(17) . . ? C56 C51 C52 119.4(3) . . ? C56 C51 P2 125.7(2) . . ? C52 C51 P2 114.94(19) . . ? C51 C52 C53 116.3(3) . . ? C54 C53 C52 131.5(4) . . ? C53 C54 C55 116.9(4) . . ? C54 C55 C56 112.0(3) . . ? C51 C56 C55 123.6(3) . . ? C66 C61 C62 120.2 . . ? C66 C61 P1 121.12(12) . . ? C62 C61 P1 118.65(12) . . ? C63 C62 C61 122.3 . . ? C64 C63 C62 117.6 . . ? C63 C64 C65 120.2 . . ? C66 C65 C64 122.2 . . ? C61 C66 C65 117.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.669 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.104 #===END data_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 P2 Pb S4' _chemical_formula_weight 886.01 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' 'Pb' 'Pb' -3.3944 10.1111 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 15.5560(10) _cell_length_b 15.6120(10) _cell_length_c 15.0520(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.455(2) _cell_angle_gamma 90.00 _cell_volume 3594.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour yellow _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 5.041 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-nonius DIP2000 ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6712 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3804 _reflns_number_gt 3670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP2000 software Xpress (MAC science, 1989)' _computing_cell_refinement 'DIP2000 software DENZO (Otwinowski & Minor, 1996)' _computing_data_reduction 'DIP2000 software DENZO (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0589P)^2^+31.1723P] 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 mixed _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 0.047(10) _refine_ls_number_reflns 3804 _refine_ls_number_parameters 369 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.004 _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 0.78012(9) 0.14038(2) 0.26500(10) 0.03152(14) Uani 1 1 d . . . P1 P 0.5096(3) 0.1673(4) 0.2486(3) 0.0274(10) Uani 1 1 d . . . P2 P 1.0675(3) 0.1728(4) 0.2827(3) 0.0314(11) Uani 1 1 d . . . S1 S 0.7231(4) 0.2508(4) 0.1437(4) 0.0480(15) Uani 1 1 d . . . S2 S 0.8488(4) 0.2535(4) 0.3855(5) 0.0550(18) Uani 1 1 d . . . S3 S 0.9677(6) 0.0985(6) 0.2254(6) 0.0254(19) Uani 0.50 1 d P . . S4 S 0.6082(7) 0.0966(11) 0.3092(10) 0.048(3) Uani 0.50 1 d P . . S3' S 0.9555(10) 0.1575(12) 0.1979(10) 0.056(4) Uani 0.50 1 d P . . S4' S 0.6203(8) 0.1499(9) 0.3363(9) 0.039(3) Uani 0.50 1 d P . . C11 C 0.6582(13) 0.1787(13) 0.0869(12) 0.041(5) Uani 1 1 d . . . C12 C 0.5662(10) 0.1664(9) 0.0877(9) 0.024(3) Uani 1 1 d U . . C13 C 0.5170(10) 0.1025(11) 0.0308(9) 0.035(5) Uani 1 1 d U . . H13 H 0.4573 0.0982 0.0302 0.043 Uiso 1 1 calc R . . C14 C 0.556(2) 0.046(2) -0.025(2) 0.089(9) Uani 1 1 d U . . H14 H 0.5233 0.0029 -0.0587 0.107 Uiso 1 1 calc R . . C15 C 0.6441(10) 0.0570(11) -0.0249(9) 0.041(4) Uani 1 1 d U . . H15 H 0.6716 0.0209 -0.0603 0.049 Uiso 1 1 calc R . . C16 C 0.6944(15) 0.1221(14) 0.0272(14) 0.053(6) Uani 1 1 d U . . H16 H 0.7528 0.1284 0.0226 0.063 Uiso 1 1 calc R . . C17 C 0.5220(12) 0.2273(9) 0.1440(10) 0.021(3) Uani 1 1 d U . . H17A H 0.4653 0.2446 0.1108 0.025 Uiso 1 1 calc R . . H17B H 0.5575 0.2781 0.1594 0.025 Uiso 1 1 calc R . . C21 C 0.4097(7) 0.0926(6) 0.2154(7) 0.042(4) Uani 1 1 d G . . C22 C 0.3284(7) 0.1272(6) 0.1744(8) 0.049(4) Uani 1 1 d G . . H22 H 0.3219 0.1863 0.1693 0.059 Uiso 1 1 calc R . . C23 C 0.2572(7) 0.0740(7) 0.1412(8) 0.059(4) Uani 1 1 d G . . H23 H 0.2039 0.0974 0.1143 0.070 Uiso 1 1 calc R . . C24 C 0.2672(7) -0.0138(7) 0.1491(9) 0.064(5) Uani 1 1 d G . . H24 H 0.2206 -0.0499 0.1274 0.077 Uiso 1 1 calc R . . C25 C 0.3485(7) -0.0483(6) 0.1901(8) 0.072(7) Uani 1 1 d G . . H25 H 0.3550 -0.1074 0.1952 0.087 Uiso 1 1 calc R . . C26 C 0.4197(7) 0.0049(6) 0.2232(7) 0.042(3) Uani 1 1 d G . . H26 H 0.4730 -0.0185 0.2502 0.051 Uiso 1 1 calc R . . C31 C 0.4436(7) 0.2552(7) 0.2922(7) 0.049(5) Uani 1 1 d G . . C32 C 0.3867(8) 0.3070(8) 0.2337(7) 0.056(4) Uani 1 1 d G . . H32 H 0.3803 0.2997 0.1715 0.068 Uiso 1 1 calc R . . C33 C 0.3396(9) 0.3696(7) 0.2691(8) 0.072(6) Uani 1 1 d G . . H33 H 0.3013 0.4046 0.2305 0.086 Uiso 1 1 calc R . . C34 C 0.3494(10) 0.3804(8) 0.3629(8) 0.079(7) Uani 1 1 d G . . H34 H 0.3176 0.4225 0.3861 0.095 Uiso 1 1 calc R . . C35 C 0.4063(10) 0.3286(9) 0.4214(7) 0.086(8) Uani 1 1 d G . . H35 H 0.4127 0.3359 0.4835 0.103 Uiso 1 1 calc R . . C36 C 0.4534(8) 0.2660(8) 0.3860(7) 0.052(4) Uani 1 1 d G . . H36 H 0.4916 0.2310 0.4246 0.062 Uiso 1 1 calc R . . C41 C 0.9160(9) 0.1676(9) 0.4508(8) 0.031(4) Uani 1 1 d G . . C42 C 1.0032(8) 0.1613(9) 0.4493(9) 0.042(5) Uani 1 1 d GU . . C43 C 1.0525(8) 0.1024(9) 0.5009(9) 0.052(6) Uani 1 1 d GU . . H43 H 1.1119 0.0980 0.5000 0.062 Uiso 1 1 calc R . . C44 C 1.0145(8) 0.0498(9) 0.5540(8) 0.032(4) Uani 1 1 d GU . . H44 H 1.0481 0.0091 0.5897 0.038 Uiso 1 1 calc R . . C45 C 0.9273(9) 0.0561(10) 0.5554(10) 0.089(10) Uani 1 1 d GU . . H45 H 0.9017 0.0197 0.5921 0.107 Uiso 1 1 calc R . . C46 C 0.8780(8) 0.1150(10) 0.5039(10) 0.042(5) Uani 1 1 d GU . . H46 H 0.8186 0.1194 0.5047 0.051 Uiso 1 1 calc R . . C47 C 1.0478(15) 0.2122(13) 0.3856(15) 0.046(5) Uani 1 1 d . . . H47A H 1.1040 0.2294 0.4199 0.055 Uiso 1 1 calc R . . H47B H 1.0139 0.2642 0.3719 0.055 Uiso 1 1 calc R . . C51 C 1.1255(8) 0.0828(6) 0.3154(8) 0.049(5) Uani 1 1 d G . . C52 C 1.2122(9) 0.0910(8) 0.3619(9) 0.062(5) Uani 1 1 d G . . H52 H 1.2372 0.1451 0.3712 0.075 Uiso 1 1 calc R . . C53 C 1.2607(9) 0.0194(10) 0.3939(11) 0.101(9) Uani 1 1 d G . . H53 H 1.3179 0.0250 0.4245 0.121 Uiso 1 1 calc R . . C54 C 1.2226(11) -0.0604(9) 0.3794(11) 0.105(10) Uani 1 1 d G . . H54 H 1.2543 -0.1090 0.4005 0.126 Uiso 1 1 calc R . . C55 C 1.1359(11) -0.0686(6) 0.3330(10) 0.096(9) Uani 1 1 d G . . H55 H 1.1110 -0.1227 0.3236 0.115 Uiso 1 1 calc R . . C56 C 1.0874(10) 0.0030(6) 0.3010(7) 0.052(4) Uani 1 1 d G . . H56 H 1.0301 -0.0026 0.2703 0.062 Uiso 1 1 calc R . . C61 C 1.1028(8) 0.2417(6) 0.2031(7) 0.056(5) Uani 1 1 d G . . C62 C 1.1350(8) 0.2100(7) 0.1299(7) 0.052(4) Uani 1 1 d G . . H62 H 1.1442 0.1514 0.1256 0.063 Uiso 1 1 calc R . . C63 C 1.1536(8) 0.2633(7) 0.0633(7) 0.061(4) Uani 1 1 d G . . H63 H 1.1752 0.2412 0.0144 0.073 Uiso 1 1 calc R . . C64 C 1.1400(9) 0.3484(7) 0.0700(8) 0.054(4) Uani 1 1 d G . . H64 H 1.1522 0.3854 0.0255 0.065 Uiso 1 1 calc R . . C65 C 1.1079(10) 0.3801(6) 0.1432(8) 0.078(6) Uani 1 1 d G . . H65 H 1.0987 0.4387 0.1475 0.093 Uiso 1 1 calc R . . C66 C 1.0893(9) 0.3268(6) 0.2098(8) 0.059(5) Uani 1 1 d G . . H66 H 1.0677 0.3488 0.2587 0.071 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 0.0319(2) 0.0316(2) 0.0289(2) 0.0010(4) -0.00040(13) 0.0029(4) P1 0.024(2) 0.041(2) 0.017(2) -0.0002(19) 0.0049(16) 0.0106(18) P2 0.026(2) 0.040(3) 0.026(3) -0.003(2) -0.0014(17) -0.0133(19) S1 0.057(3) 0.040(3) 0.038(3) 0.023(2) -0.014(2) -0.023(3) S2 0.053(3) 0.035(3) 0.064(4) -0.003(3) -0.024(3) 0.011(3) S3 0.034(5) 0.025(4) 0.019(4) -0.012(3) 0.010(3) -0.012(3) S4 0.012(4) 0.074(8) 0.053(8) 0.031(7) -0.006(4) -0.002(5) S3' 0.046(6) 0.092(10) 0.033(6) -0.013(7) 0.010(5) -0.034(7) S4' 0.020(4) 0.070(8) 0.026(5) 0.030(6) 0.001(3) 0.006(5) C11 0.056(11) 0.043(10) 0.024(9) 0.011(7) 0.008(8) -0.021(8) C12 0.040(7) 0.023(6) 0.007(5) 0.003(5) -0.002(5) -0.010(6) C13 0.049(8) 0.048(8) 0.013(6) -0.016(5) 0.014(6) -0.015(6) C14 0.094(12) 0.089(12) 0.082(12) -0.012(9) 0.012(9) -0.010(9) C15 0.051(7) 0.056(8) 0.022(6) -0.019(5) 0.024(5) -0.018(6) C16 0.055(9) 0.063(9) 0.040(9) 0.015(7) 0.009(7) -0.014(7) C17 0.034(6) 0.012(5) 0.015(5) 0.012(4) -0.001(5) -0.002(5) C21 0.069(12) 0.034(8) 0.028(7) -0.010(6) 0.021(8) -0.007(8) C22 0.050(9) 0.050(10) 0.043(8) -0.007(7) -0.005(7) -0.009(8) C23 0.060(10) 0.039(8) 0.078(12) -0.011(8) 0.016(9) 0.009(8) C24 0.068(12) 0.059(10) 0.054(10) -0.022(8) -0.021(9) -0.019(9) C25 0.082(15) 0.026(8) 0.102(17) 0.008(9) -0.005(12) -0.028(9) C26 0.043(8) 0.043(8) 0.034(7) 0.004(6) -0.011(7) -0.005(7) C31 0.065(11) 0.031(7) 0.065(11) -0.024(7) 0.049(10) -0.004(7) C32 0.062(10) 0.074(11) 0.033(7) 0.014(7) 0.009(7) 0.017(9) C33 0.108(17) 0.049(9) 0.062(11) 0.014(8) 0.026(12) 0.031(10) C34 0.122(19) 0.053(10) 0.073(13) -0.001(9) 0.049(14) 0.027(12) C35 0.086(16) 0.13(2) 0.046(12) -0.020(13) 0.028(11) 0.003(16) C36 0.064(10) 0.063(10) 0.029(7) -0.008(7) 0.012(7) 0.014(8) C41 0.052(10) 0.022(7) 0.011(7) -0.002(5) -0.014(6) 0.016(7) C42 0.054(9) 0.041(8) 0.031(8) -0.006(7) 0.004(7) 0.007(7) C43 0.057(9) 0.052(9) 0.043(9) -0.019(7) 0.001(7) 0.021(7) C44 0.041(6) 0.045(7) 0.012(5) 0.022(5) 0.012(5) 0.026(5) C45 0.093(13) 0.094(13) 0.080(12) 0.002(9) 0.017(9) 0.009(9) C46 0.049(8) 0.055(8) 0.024(7) 0.003(6) 0.012(6) 0.018(7) C47 0.047(10) 0.025(8) 0.056(11) -0.010(7) -0.016(9) 0.002(7) C51 0.105(15) 0.027(7) 0.022(7) 0.000(5) 0.029(8) 0.001(9) C52 0.082(15) 0.042(10) 0.070(12) 0.003(9) 0.031(11) 0.024(10) C53 0.089(17) 0.13(2) 0.090(16) 0.054(16) 0.024(14) 0.063(17) C54 0.080(18) 0.068(16) 0.16(3) 0.014(18) 0.017(18) 0.027(14) C55 0.20(3) 0.021(7) 0.074(13) 0.006(8) 0.045(17) 0.010(12) C56 0.095(13) 0.028(6) 0.033(7) -0.006(5) 0.012(9) -0.002(9) C61 0.040(9) 0.054(10) 0.074(13) 0.008(9) 0.008(9) 0.033(8) C62 0.077(11) 0.049(9) 0.037(8) 0.004(7) 0.027(8) -0.001(8) C63 0.069(11) 0.078(12) 0.038(8) -0.001(8) 0.016(8) 0.010(9) C64 0.066(11) 0.046(9) 0.058(11) 0.009(8) 0.029(9) 0.008(8) C65 0.102(17) 0.050(10) 0.087(15) 0.024(10) 0.033(13) 0.009(11) C66 0.088(13) 0.048(8) 0.054(9) 0.013(7) 0.049(9) 0.027(9) _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 S1 2.550(5) . ? Pb S2 2.617(6) . ? Pb S4' 2.885(12) . ? Pb S4 2.950(12) . ? Pb S3' 3.088(14) . ? P1 C17 1.872(15) . ? P1 C31 1.901(11) . ? P1 C21 1.935(12) . ? P1 S4 1.973(13) . ? P1 S4' 1.989(14) . ? P2 C51 1.694(12) . ? P2 C47 1.74(2) . ? P2 C61 1.771(12) . ? P2 S3' 1.978(17) . ? P2 S3 2.003(10) . ? S1 C11 1.64(2) . ? S2 C41 1.866(14) . ? S3 S3' 1.01(2) . ? S4 S4' 0.930(19) . ? C11 C16 1.44(3) . ? C11 C12 1.44(2) . ? C12 C13 1.442(17) . ? C12 C17 1.52(2) . ? C13 C14 1.42(3) . ? C14 C15 1.39(3) . ? C15 C16 1.43(2) . ? C21 C26 1.380(7) . ? C21 C22 1.409(7) . ? C22 C23 1.402(7) . ? C23 C24 1.381(7) . ? C24 C25 1.409(7) . ? C25 C26 1.402(7) . ? C31 C32 1.389(7) . ? C31 C36 1.403(7) . ? C32 C33 1.384(7) . ? C33 C34 1.403(7) . ? C34 C35 1.389(7) . ? C35 C36 1.384(7) . ? C41 C46 1.354(8) . ? C41 C42 1.365(8) . ? C42 C43 1.349(8) . ? C42 C47 1.51(3) . ? C43 C44 1.354(8) . ? C44 C45 1.364(8) . ? C45 C46 1.349(8) . ? C51 C56 1.380(8) . ? C51 C52 1.407(8) . ? C52 C53 1.385(8) . ? C53 C54 1.380(8) . ? C54 C55 1.407(8) . ? C55 C56 1.385(8) . ? C61 C66 1.351(7) . ? C61 C62 1.382(7) . ? C62 C63 1.373(7) . ? C63 C64 1.351(7) . ? C64 C65 1.382(7) . ? C65 C66 1.373(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pb S2 94.90(9) . . ? S1 Pb S4' 91.2(3) . . ? S2 Pb S4' 88.8(4) . . ? S1 Pb S4 96.1(3) . . ? S2 Pb S4 105.8(4) . . ? S4' Pb S4 18.3(4) . . ? S1 Pb S3' 85.5(4) . . ? S2 Pb S3' 84.0(3) . . ? S4' Pb S3' 171.7(3) . . ? S4 Pb S3' 169.9(5) . . ? C17 P1 C31 94.2(6) . . ? C17 P1 C21 106.6(7) . . ? C31 P1 C21 93.7(5) . . ? C17 P1 S4 118.6(7) . . ? C31 P1 S4 131.9(7) . . ? C21 P1 S4 107.7(6) . . ? C17 P1 S4' 114.7(7) . . ? C31 P1 S4' 109.1(6) . . ? C21 P1 S4' 130.3(6) . . ? S4 P1 S4' 27.2(5) . . ? C51 P2 C47 101.8(9) . . ? C51 P2 C61 119.1(6) . . ? C47 P2 C61 120.9(8) . . ? C51 P2 S3' 116.6(7) . . ? C47 P2 S3' 109.8(9) . . ? C61 P2 S3' 89.0(7) . . ? C51 P2 S3 88.6(6) . . ? C47 P2 S3 109.8(8) . . ? C61 P2 S3 111.8(6) . . ? S3' P2 S3 29.5(6) . . ? C11 S1 Pb 90.6(7) . . ? C41 S2 Pb 90.0(5) . . ? S3' S3 P2 73.9(10) . . ? S4' S4 P1 77.4(12) . . ? S4' S4 Pb 76.9(10) . . ? P1 S4 Pb 115.3(6) . . ? S3 S3' P2 76.6(11) . . ? S3 S3' Pb 84.2(9) . . ? P2 S3' Pb 121.7(6) . . ? S4 S4' P1 75.5(11) . . ? S4 S4' Pb 84.8(11) . . ? P1 S4' Pb 117.4(5) . . ? C16 C11 C12 115.0(15) . . ? C16 C11 S1 118.0(15) . . ? C12 C11 S1 127.0(15) . . ? C13 C12 C11 120.4(13) . . ? C13 C12 C17 121.3(13) . . ? C11 C12 C17 118.1(14) . . ? C14 C13 C12 123.1(16) . . ? C15 C14 C13 116(2) . . ? C14 C15 C16 122.3(18) . . ? C15 C16 C11 122.7(17) . . ? C12 C17 P1 106.4(10) . . ? C26 C21 C22 119.7 . . ? C26 C21 P1 120.2(6) . . ? C22 C21 P1 119.8(6) . . ? C23 C22 C21 121.2 . . ? C24 C23 C22 119.2 . . ? C23 C24 C25 119.7 . . ? C26 C25 C24 121.2 . . ? C21 C26 C25 119.2 . . ? C32 C31 C36 120.6 . . ? C32 C31 P1 121.6(6) . . ? C36 C31 P1 117.9(6) . . ? C33 C32 C31 119.2 . . ? C32 C33 C34 120.2 . . ? C35 C34 C33 120.6 . . ? C36 C35 C34 119.2 . . ? C35 C36 C31 120.2 . . ? C46 C41 C42 120.5 . . ? C46 C41 S2 118.9(8) . . ? C42 C41 S2 120.4(8) . . ? C43 C42 C41 120.1 . . ? C43 C42 C47 116.5(12) . . ? C41 C42 C47 123.1(12) . . ? C42 C43 C44 119.3 . . ? C43 C44 C45 120.5 . . ? C46 C45 C44 120.1 . . ? C45 C46 C41 119.4 . . ? C42 C47 P2 123.7(14) . . ? C56 C51 C52 120.4 . . ? C56 C51 P2 120.8(7) . . ? C52 C51 P2 118.8(7) . . ? C53 C52 C51 120.8 . . ? C54 C53 C52 118.8 . . ? C53 C54 C55 120.4 . . ? C56 C55 C54 120.8 . . ? C51 C56 C55 118.8 . . ? C66 C61 C62 119.7 . . ? C66 C61 P2 118.3(6) . . ? C62 C61 P2 121.6(6) . . ? C63 C62 C61 121.3 . . ? C64 C63 C62 119.0 . . ? C63 C64 C65 119.7 . . ? C66 C65 C64 121.3 . . ? C61 C66 C65 119.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.216 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.150 #===END data_compound6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H54 P4 Pb S6' _chemical_formula_weight 1346.52 _chemical_melting_point ? _chemical_compound_source ? 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' 'Pb' 'Pb' -3.3944 10.1111 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 16.212(3) _cell_length_b 14.4198(10) _cell_length_c 25.146(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.014(14) _cell_angle_gamma 90.00 _cell_volume 5874.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 17 _exptl_crystal_description brick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method ? _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 3.234 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.0 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius CAD4 ' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5678 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.52 _reflns_number_total 5678 _reflns_number_observed 3702 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD-4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'SHELXL-96 (Sheldrick, 1993)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.3420P] 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 ? _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 0.037(9) _refine_ls_number_reflns 5678 _refine_ls_number_parameters 676 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_obs 0.0362 _refine_ls_wR_factor_all 0.1003 _refine_ls_wR_factor_obs 0.0849 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.125 _refine_ls_shift/esd_max 0.108 _refine_ls_shift/esd_mean 0.016 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pb Pb 0.01512(10) 0.06656(2) 0.00021(8) 0.05746(14) Uani 1 d . . S01 S -0.1634(4) 0.0985(5) 0.0112(3) 0.077(2) Uani 1 d . . S02 S 0.0401(4) 0.2276(4) -0.0950(2) 0.0577(16) Uani 1 d . . S03 S -0.0043(6) 0.2277(6) 0.0969(3) 0.090(3) Uani 1 d . . S04 S 0.1976(4) 0.1008(4) -0.0105(3) 0.0586(17) Uani 1 d . . P1 P -0.2322(4) -0.0072(5) -0.0061(2) 0.0595(18) Uani 1 d . . P2 P 0.0667(3) 0.1719(5) -0.1646(2) 0.0539(17) Uani 1 d . . P3 P -0.0330(5) 0.1743(4) 0.1632(3) 0.063(2) Uani 1 d . . P4 P 0.2671(3) -0.0082(4) 0.0068(2) 0.0520(17) Uani 1 d . . S1 S -0.0040(4) -0.0695(4) -0.0724(2) 0.0478(13) Uani 1 d . . S2 S 0.0334(5) -0.0707(5) 0.0703(3) 0.076(2) Uani 1 d . . C11 C -0.0770(16) -0.0208(15) -0.1110(9) 0.061(6) Uani 1 d . . C12 C -0.1597(14) -0.0332(12) -0.1038(8) 0.045(5) Uani 1 d . . C13 C -0.2151(14) 0.0099(17) -0.1446(10) 0.063(7) Uani 1 d . . H13 H -0.2713 0.0005 -0.1407 0.076 Uiso 1 calc R . C14 C -0.1971(13) 0.0544(13) -0.1813(8) 0.046(5) Uani 1 d . . H14 H -0.2388 0.0813 -0.2024 0.056 Uiso 1 calc R . C15 C -0.1223(14) 0.0672(15) -0.1932(9) 0.050(5) Uani 1 d . . H15 H -0.1096 0.0977 -0.2244 0.060 Uiso 1 calc R . C16 C -0.0561(18) 0.0330(17) -0.1566(11) 0.076(8) Uani 1 d . . C17 C -0.1909(8) -0.0800(12) -0.0588(8) 0.045(5) Uani 1 d . . H17A H -0.1469 -0.1178 -0.0432 0.054 Uiso 1 calc R . H17B H -0.2343 -0.1217 -0.0714 0.054 Uiso 1 calc R . C18 C 0.0380(10) 0.0547(14) -0.1701(8) 0.061(7) Uani 1 d . . H18A H 0.0472 0.0341 -0.2062 0.073 Uiso 1 calc R . H18B H 0.0738 0.0184 -0.1464 0.073 Uiso 1 calc R . C21 C -0.2452(14) -0.0751(13) 0.0552(10) 0.051(6) Uani 1 d . . C22 C -0.2312(13) -0.0424(12) 0.1001(6) 0.059(5) Uani 1 d . . H22 H -0.2097 0.0170 0.1042 0.071 Uiso 1 calc R . C23 C -0.248(2) -0.097(2) 0.1442(10) 0.095(9) Uani 1 d . . H23 H -0.2522 -0.0650 0.1763 0.113 Uiso 1 calc R . C24 C -0.2600(12) -0.1858(16) 0.1460(10) 0.074(7) Uani 1 d . . H24 H -0.2540 -0.2209 0.1769 0.089 Uiso 1 calc R . C25 C -0.2831(17) -0.2242(16) 0.0945(12) 0.070(7) Uani 1 d . . H25 H -0.3060 -0.2833 0.0922 0.084 Uiso 1 calc R . C26 C -0.2713(17) -0.1735(17) 0.0489(11) 0.095(10) Uani 1 d . . H26 H -0.2793 -0.1999 0.0154 0.114 Uiso 1 calc R . C31 C -0.3340(9) 0.0316(14) -0.0302(8) 0.053(6) Uani 1 d . . C32 C -0.3789(17) -0.033(2) -0.0488(11) 0.118(11) Uani 1 d . . H32 H -0.3585 -0.0932 -0.0513 0.142 Uiso 1 calc R . C33 C -0.4674(17) -0.0100(18) -0.0672(9) 0.081(9) Uani 1 d . . H33 H -0.5053 -0.0570 -0.0747 0.098 Uiso 1 calc R . C34 C -0.4875(16) 0.0731(19) -0.0718(7) 0.092(9) Uani 1 d . . H34 H -0.5388 0.0883 -0.0872 0.110 Uiso 1 calc R . C35 C -0.441(3) 0.134(3) -0.0567(15) 0.147(18) Uani 1 d . . H35 H -0.4616 0.1944 -0.0572 0.176 Uiso 1 calc R . C36 C -0.3495(13) 0.1192(19) -0.0363(10) 0.088(9) Uani 1 d . . H36 H -0.3117 0.1666 -0.0296 0.106 Uiso 1 calc R . C41 C 0.0267(17) 0.2362(16) -0.2218(12) 0.074(7) Uani 1 d . . C42 C 0.0210(17) 0.2036(18) -0.2723(13) 0.077(7) Uani 1 d . . H42 H 0.0479 0.1494 -0.2818 0.093 Uiso 1 calc R . C43 C -0.024(2) 0.251(3) -0.3078(13) 0.133(14) Uani 1 d . . H43 H -0.0335 0.2216 -0.3404 0.159 Uiso 1 calc R . C44 C -0.0572(14) 0.3326(16) -0.3041(8) 0.092(8) Uani 1 d . . H44 H -0.0863 0.3613 -0.3321 0.110 Uiso 1 calc R . C45 C -0.0449(19) 0.373(3) -0.2535(14) 0.133(13) Uani 1 d . . H45 H -0.0595 0.4349 -0.2479 0.159 Uiso 1 calc R . C46 C -0.0113(16) 0.3215(19) -0.2128(11) 0.088(9) Uani 1 d . . H46 H -0.0138 0.3436 -0.1782 0.106 Uiso 1 calc R . C51 C 0.1774(12) 0.1719(9) -0.1741(8) 0.053(6) Uani 1 d . . C52 C 0.215(2) 0.135(2) -0.2184(11) 0.113(11) Uani 1 d . . H52 H 0.1799 0.1118 -0.2452 0.136 Uiso 1 calc R . C53 C 0.2930(9) 0.1293(13) -0.2265(7) 0.060(6) Uani 1 d . . H53 H 0.3140 0.0979 -0.2553 0.072 Uiso 1 calc R . C54 C 0.339(2) 0.1704(18) -0.1917(15) 0.108(11) Uani 1 d . . H54 H 0.3948 0.1739 -0.1989 0.130 Uiso 1 calc R . C55 C 0.3166(11) 0.2087(16) -0.1465(7) 0.055(5) Uani 1 d . . H55 H 0.3543 0.2270 -0.1198 0.066 Uiso 1 calc R . C56 C 0.2305(17) 0.2192(19) -0.1425(12) 0.109(10) Uani 1 d . . H56 H 0.2103 0.2598 -0.1174 0.131 Uiso 1 calc R . C01 C 0.1128(9) -0.0141(14) 0.1165(9) 0.049(6) Uani 1 d . . C02 C 0.2009(15) -0.0272(17) 0.1086(10) 0.070(7) Uani 1 d . . C03 C 0.2626(13) -0.0002(17) 0.1392(9) 0.056(5) Uani 1 d . . H03 H 0.3174 -0.0120 0.1317 0.067 Uiso 1 calc R . C04 C 0.2354(18) 0.056(2) 0.1914(11) 0.095(9) Uani 1 d . . H04 H 0.2725 0.0775 0.2175 0.114 Uiso 1 calc R . C05 C 0.1422(16) 0.0687(19) 0.1932(11) 0.072(8) Uani 1 d . . H05 H 0.1229 0.1061 0.2202 0.086 Uiso 1 calc R . C06 C 0.0888(11) 0.0338(12) 0.1615(7) 0.036(4) Uani 1 d . . C07 C 0.0057(14) 0.0509(12) 0.1724(9) 0.067(8) Uani 1 d . . H07A H -0.0030 0.0327 0.2089 0.080 Uiso 1 calc R . H07B H -0.0283 0.0107 0.1498 0.080 Uiso 1 calc R . C08 C 0.2233(15) -0.0912(16) 0.0552(8) 0.085(8) Uani 1 d . . H08A H 0.1739 -0.1204 0.0401 0.102 Uiso 1 calc R . H08B H 0.2632 -0.1390 0.0648 0.102 Uiso 1 calc R . C61 C 0.0188(14) 0.2366(15) 0.2202(8) 0.053(6) Uani 1 d . . C62 C 0.0295(15) 0.1934(18) 0.2703(8) 0.068(6) Uani 1 d . . H62 H 0.0164 0.1311 0.2743 0.082 Uiso 1 calc R . C63 C 0.0610(14) 0.2466(14) 0.3153(9) 0.067(6) Uani 1 d . . H63 H 0.0650 0.2235 0.3498 0.080 Uiso 1 calc R . C64 C 0.0857(16) 0.341(2) 0.3009(13) 0.157(19) Uani 1 d . . H64 H 0.1057 0.3798 0.3277 0.189 Uiso 1 calc R . C65 C 0.0813(17) 0.3709(16) 0.2536(11) 0.091(9) Uani 1 d . . H65 H 0.1075 0.4268 0.2468 0.109 Uiso 1 calc R . C66 C 0.0413(16) 0.3278(15) 0.2120(11) 0.082(9) Uani 1 d . . H66 H 0.0297 0.3580 0.1799 0.098 Uiso 1 calc R . C71 C -0.1424(9) 0.1707(15) 0.1778(9) 0.072(7) Uani 1 d . . C72 C -0.1960(14) 0.2102(13) 0.1390(8) 0.056(5) Uani 1 d . . H72 H -0.1759 0.2295 0.1067 0.067 Uiso 1 calc R . C73 C -0.280(2) 0.220(3) 0.1493(15) 0.130(13) Uani 1 d . . H73 H -0.3127 0.2604 0.1285 0.157 Uiso 1 calc R . C74 C -0.3134(14) 0.1731(19) 0.1884(12) 0.073(7) Uani 1 d . . H74 H -0.3704 0.1676 0.1899 0.087 Uiso 1 calc R . C75 C -0.264(2) 0.1333(17) 0.2259(13) 0.139(15) Uani 1 d . . H75 H -0.2882 0.1081 0.2557 0.166 Uiso 1 calc R . C76 C -0.1703(9) 0.1273(11) 0.2222(8) 0.051(5) Uani 1 d . . H76 H -0.1361 0.0975 0.2473 0.061 Uiso 1 calc R . C81 C 0.2802(17) -0.0884(17) -0.0485(9) 0.068(7) Uani 1 d . . C82 C 0.255(2) -0.047(2) -0.1046(15) 0.168(17) Uani 1 d . . H82 H 0.2364 0.0137 -0.1071 0.201 Uiso 1 calc R . C83 C 0.259(2) -0.100(2) -0.1500(12) 0.107(11) Uani 1 d . . H83 H 0.2395 -0.0802 -0.1833 0.128 Uiso 1 calc R . C84 C 0.299(2) -0.190(2) -0.1404(11) 0.133(13) Uani 1 d . . H84 H 0.3170 -0.2238 -0.1691 0.160 Uiso 1 calc R . C85 C 0.308(2) -0.221(2) -0.0947(14) 0.106(12) Uani 1 d . . H85 H 0.3169 -0.2846 -0.0913 0.127 Uiso 1 calc R . C86 C 0.3068(15) -0.1696(12) -0.0487(8) 0.072(8) Uani 1 d . . H86 H 0.3262 -0.1960 -0.0169 0.086 Uiso 1 calc R . C91 C 0.3646(17) 0.0263(18) 0.0311(8) 0.089(9) Uani 1 d . . C92 C 0.4326(10) -0.0361(14) 0.0492(8) 0.063(6) Uani 1 d . . H92 H 0.4233 -0.0992 0.0443 0.076 Uiso 1 calc R . C93 C 0.5038(14) -0.013(3) 0.0710(11) 0.113(12) Uani 1 d . . H93 H 0.5420 -0.0567 0.0840 0.135 Uiso 1 calc R . C94 C 0.5178(16) 0.089(3) 0.0731(11) 0.16(2) Uani 1 d . . H94 H 0.5676 0.1101 0.0881 0.187 Uiso 1 calc R . C95 C 0.4619(12) 0.1538(19) 0.0544(9) 0.078(6) Uani 1 d . . H95 H 0.4727 0.2171 0.0557 0.093 Uiso 1 calc R . C96 C 0.3943(15) 0.1212(17) 0.0351(7) 0.076(8) Uani 1 d . . H96 H 0.3578 0.1656 0.0213 0.091 Uiso 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 0.0506(2) 0.0661(2) 0.0557(2) 0.0010(8) 0.00205(14) -0.0002(8) S01 0.066(5) 0.084(4) 0.081(4) 0.018(3) 0.015(4) 0.004(4) S02 0.064(4) 0.056(3) 0.053(4) -0.007(3) 0.009(3) -0.002(3) S03 0.093(6) 0.102(6) 0.074(5) 0.004(4) 0.006(5) -0.018(5) S04 0.050(4) 0.037(2) 0.089(4) 0.024(3) 0.013(3) 0.015(3) P1 0.073(4) 0.054(4) 0.052(4) 0.005(3) 0.015(3) 0.003(3) P2 0.036(3) 0.077(4) 0.049(3) -0.002(3) 0.006(3) 0.005(3) P3 0.074(5) 0.048(3) 0.068(4) 0.002(3) -0.003(4) 0.008(3) P4 0.028(3) 0.058(4) 0.071(4) 0.012(3) 0.005(3) 0.005(3) S1 0.041(2) 0.056(3) 0.047(2) 0.004(2) 0.006(2) 0.006(2) S2 0.077(5) 0.069(4) 0.079(4) 0.010(3) -0.010(4) -0.011(4) C11 0.097(16) 0.044(10) 0.043(10) -0.007(8) 0.021(10) -0.016(10) C12 0.052(12) 0.031(7) 0.052(11) -0.024(8) -0.002(9) 0.007(7) C13 0.033(9) 0.070(12) 0.086(18) -0.020(12) 0.004(9) -0.008(8) C14 0.042(10) 0.063(10) 0.033(8) -0.008(7) -0.016(7) 0.015(8) C15 0.036(9) 0.069(9) 0.044(9) -0.001(8) -0.014(7) 0.005(8) C16 0.079(17) 0.077(15) 0.071(15) -0.038(12) 0.013(13) 0.009(14) C17 0.024(6) 0.037(7) 0.073(11) -0.004(7) -0.009(7) -0.010(6) C18 0.016(6) 0.099(16) 0.068(13) 0.017(10) 0.011(7) -0.008(8) C21 0.044(10) 0.034(7) 0.076(15) -0.010(8) 0.015(9) 0.015(7) C22 0.100(11) 0.050(9) 0.028(7) 0.005(6) 0.017(7) 0.001(8) C23 0.13(2) 0.088(16) 0.061(14) -0.017(11) -0.003(13) 0.000(13) C24 0.069(10) 0.062(14) 0.092(17) 0.008(11) 0.011(10) 0.000(9) C25 0.075(12) 0.053(11) 0.083(16) 0.013(10) 0.031(11) -0.026(10) C26 0.084(18) 0.099(18) 0.10(2) -0.061(14) 0.019(16) -0.003(14) C31 0.017(6) 0.074(12) 0.069(11) 0.013(8) -0.002(6) -0.020(7) C32 0.079(18) 0.18(3) 0.094(18) 0.038(17) 0.032(12) 0.074(18) C33 0.10(2) 0.089(16) 0.059(13) -0.029(11) 0.020(12) -0.049(14) C34 0.111(18) 0.114(18) 0.053(10) -0.033(11) 0.037(10) -0.052(15) C35 0.19(4) 0.12(2) 0.14(3) 0.029(19) 0.07(3) 0.09(3) C36 0.043(10) 0.091(19) 0.13(2) 0.016(15) 0.032(11) 0.029(10) C41 0.057(14) 0.064(14) 0.100(19) -0.014(13) 0.004(11) 0.002(9) C42 0.060(12) 0.062(11) 0.11(2) -0.003(12) 0.018(10) -0.010(8) C43 0.09(2) 0.23(4) 0.074(18) 0.03(2) 0.023(16) 0.03(2) C44 0.069(13) 0.149(18) 0.058(10) -0.040(11) 0.009(9) 0.047(12) C45 0.10(2) 0.18(3) 0.11(3) 0.01(2) -0.037(18) 0.07(2) C46 0.060(14) 0.13(2) 0.072(15) -0.021(14) -0.018(13) 0.018(14) C51 0.088(14) 0.015(6) 0.058(12) 0.012(6) 0.001(10) 0.015(7) C52 0.14(3) 0.14(2) 0.061(15) -0.013(14) -0.018(15) -0.023(18) C53 0.022(7) 0.089(13) 0.068(10) -0.035(9) -0.004(7) 0.013(7) C54 0.09(2) 0.079(17) 0.16(3) -0.017(16) 0.018(19) -0.024(14) C55 0.034(9) 0.079(12) 0.052(9) -0.011(8) 0.000(7) -0.010(8) C56 0.062(16) 0.108(19) 0.16(2) -0.049(16) -0.011(16) -0.011(14) C01 0.015(7) 0.053(11) 0.077(15) 0.011(10) -0.007(8) -0.003(7) C02 0.051(13) 0.098(15) 0.063(14) -0.003(11) 0.025(11) 0.012(11) C03 0.035(8) 0.091(14) 0.042(9) -0.003(9) 0.000(6) 0.011(7) C04 0.072(15) 0.16(2) 0.055(12) 0.007(12) 0.013(10) 0.026(14) C05 0.062(15) 0.095(13) 0.061(12) 0.014(11) 0.024(11) 0.015(12) C06 0.025(8) 0.050(9) 0.033(8) -0.012(7) 0.000(7) 0.001(7) C07 0.099(17) 0.041(10) 0.061(13) 0.026(9) -0.001(10) -0.010(9) C08 0.123(18) 0.075(12) 0.061(11) -0.001(9) 0.056(11) -0.023(11) C61 0.031(8) 0.082(15) 0.047(11) -0.026(11) 0.011(7) 0.005(8) C62 0.066(11) 0.101(15) 0.038(9) -0.008(9) 0.002(7) 0.008(10) C63 0.071(14) 0.077(11) 0.052(10) -0.031(9) -0.017(10) 0.017(10) C64 0.056(14) 0.23(4) 0.18(3) -0.18(3) -0.009(16) 0.000(16) C65 0.12(2) 0.076(14) 0.083(18) -0.031(13) 0.051(16) -0.041(13) C66 0.086(18) 0.060(12) 0.102(18) -0.028(12) 0.026(15) -0.022(11) C71 0.021(8) 0.132(17) 0.065(13) 0.008(11) 0.005(8) 0.018(9) C72 0.064(13) 0.049(9) 0.057(10) -0.017(8) 0.012(9) -0.003(9) C73 0.10(2) 0.10(2) 0.19(3) 0.02(2) 0.01(2) 0.011(17) C74 0.027(8) 0.086(16) 0.104(17) -0.024(13) -0.012(10) 0.005(9) C75 0.17(3) 0.075(17) 0.17(3) -0.048(17) 0.11(2) 0.002(17) C76 0.026(7) 0.046(8) 0.081(13) 0.004(8) 0.016(7) 0.000(5) C81 0.063(13) 0.099(16) 0.042(9) -0.003(10) 0.004(9) 0.013(12) C82 0.22(4) 0.10(2) 0.18(3) 0.007(18) -0.06(3) 0.08(2) C83 0.16(3) 0.093(15) 0.066(12) -0.036(10) -0.027(14) 0.024(15) C84 0.25(3) 0.10(2) 0.060(13) -0.007(13) 0.085(17) -0.009(19) C85 0.14(3) 0.079(17) 0.10(2) 0.010(15) 0.04(2) -0.004(17) C86 0.098(18) 0.044(10) 0.073(14) -0.030(9) 0.001(12) 0.037(10) C91 0.14(2) 0.091(16) 0.038(10) 0.023(10) 0.037(12) -0.024(15) C92 0.019(7) 0.102(12) 0.070(11) 0.042(9) 0.006(6) 0.030(7) C93 0.042(12) 0.22(3) 0.074(17) 0.010(18) -0.001(11) -0.039(16) C94 0.067(16) 0.31(5) 0.093(18) -0.09(2) -0.005(12) -0.10(3) C95 0.041(9) 0.121(16) 0.070(11) -0.040(10) -0.019(8) -0.011(9) C96 0.11(2) 0.078(16) 0.037(9) -0.023(9) -0.006(10) 0.000(13) _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 S2 2.659(7) . ? Pb S1 2.690(6) . ? Pb S01 2.953(8) . ? Pb S04 3.020(6) . ? S01 P1 1.929(10) . ? S02 P2 1.987(9) . ? S03 P3 1.909(11) . ? S04 P4 1.975(7) . ? P1 C31 1.827(18) . ? P1 C21 1.84(2) . ? P1 C17 1.84(2) . ? P2 C18 1.76(2) . ? P2 C41 1.81(3) . ? P2 C51 1.82(2) . ? P3 C71 1.824(18) . ? P3 C61 1.87(2) . ? P3 C07 1.899(19) . ? P4 C91 1.75(3) . ? P4 C81 1.83(3) . ? P4 C08 1.86(2) . ? S1 C11 1.66(2) . ? S2 C01 1.889(19) . ? C11 C12 1.37(3) . ? C11 C16 1.43(3) . ? C12 C17 1.42(3) . ? C12 C13 1.48(3) . ? C13 C14 1.17(3) . ? C14 C15 1.27(3) . ? C15 C16 1.47(3) . ? C16 C18 1.61(3) . ? C21 C22 1.24(3) . ? C21 C26 1.49(3) . ? C22 C23 1.39(3) . ? C23 C24 1.30(3) . ? C24 C25 1.45(4) . ? C25 C26 1.38(4) . ? C31 C36 1.30(3) . ? C31 C32 1.26(4) . ? C32 C33 1.53(4) . ? C33 C34 1.25(4) . ? C34 C35 1.21(4) . ? C35 C36 1.57(4) . ? C41 C42 1.35(4) . ? C41 C46 1.40(3) . ? C42 C43 1.33(4) . ? C43 C44 1.30(4) . ? C44 C45 1.41(4) . ? C45 C46 1.36(4) . ? C51 C56 1.34(3) . ? C51 C52 1.40(4) . ? C52 C53 1.29(4) . ? C53 C54 1.27(3) . ? C54 C55 1.33(4) . ? C55 C56 1.41(3) . ? C01 C06 1.39(3) . ? C01 C02 1.46(3) . ? C02 C03 1.30(3) . ? C02 C08 1.68(3) . ? C03 C04 1.62(3) . ? C04 C05 1.53(4) . ? C05 C06 1.26(3) . ? C06 C07 1.41(3) . ? C61 C66 1.38(3) . ? C61 C62 1.41(3) . ? C62 C63 1.45(3) . ? C63 C64 1.46(5) . ? C64 C65 1.27(4) . ? C65 C66 1.36(4) . ? C71 C76 1.37(3) . ? C71 C72 1.40(3) . ? C72 C73 1.40(4) . ? C73 C74 1.33(4) . ? C74 C75 1.34(4) . ? C75 C76 1.53(4) . ? C81 C86 1.25(3) . ? C81 C82 1.57(4) . ? C82 C83 1.37(5) . ? C83 C84 1.46(4) . ? C84 C85 1.24(4) . ? C85 C86 1.38(4) . ? C91 C92 1.48(3) . ? C91 C96 1.45(3) . ? C92 C93 1.30(3) . ? C93 C94 1.50(5) . ? C94 C95 1.37(5) . ? C95 C96 1.27(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pb S1 85.09(10) . . ? S2 Pb S01 98.1(2) . . ? S1 Pb S01 95.0(2) . . ? S2 Pb S04 95.4(2) . . ? S1 Pb S04 98.55(19) . . ? S01 Pb S04 161.60(8) . . ? P1 S01 Pb 114.6(4) . . ? P4 S04 Pb 113.8(3) . . ? C31 P1 C21 108.1(10) . . ? C31 P1 C17 106.4(9) . . ? C21 P1 C17 110.9(9) . . ? C31 P1 S01 109.9(7) . . ? C21 P1 S01 108.3(8) . . ? C17 P1 S01 113.1(6) . . ? C18 P2 C41 110.1(11) . . ? C18 P2 C51 104.4(7) . . ? C41 P2 C51 102.9(10) . . ? C18 P2 S02 113.2(7) . . ? C41 P2 S02 114.2(9) . . ? C51 P2 S02 111.2(7) . . ? C71 P3 C61 105.8(10) . . ? C71 P3 C07 105.6(10) . . ? C61 P3 C07 102.7(10) . . ? C71 P3 S03 117.1(8) . . ? C61 P3 S03 111.1(9) . . ? C07 P3 S03 113.3(8) . . ? C91 P4 C81 108.6(12) . . ? C91 P4 C08 108.4(10) . . ? C81 P4 C08 98.5(11) . . ? C91 P4 S04 110.6(9) . . ? C81 P4 S04 114.6(9) . . ? C08 P4 S04 115.3(8) . . ? C11 S1 Pb 98.8(7) . . ? C01 S2 Pb 98.3(6) . . ? C12 C11 C16 116(2) . . ? C12 C11 S1 123.2(19) . . ? C16 C11 S1 121(2) . . ? C11 C12 C17 123(2) . . ? C11 C12 C13 115(2) . . ? C17 C12 C13 122(2) . . ? C14 C13 C12 128(2) . . ? C13 C14 C15 122(2) . . ? C14 C15 C16 119(2) . . ? C11 C16 C15 120(2) . . ? C11 C16 C18 122(2) . . ? C15 C16 C18 119(2) . . ? C12 C17 P1 116.8(12) . . ? C16 C18 P2 114.9(15) . . ? C22 C21 C26 120(2) . . ? C22 C21 P1 122.5(16) . . ? C26 C21 P1 117.2(18) . . ? C21 C22 C23 119(2) . . ? C24 C23 C22 128(2) . . ? C23 C24 C25 112(2) . . ? C26 C25 C24 120(2) . . ? C25 C26 C21 118(2) . . ? C36 C31 C32 125(2) . . ? C36 C31 P1 120.5(15) . . ? C32 C31 P1 113.5(17) . . ? C31 C32 C33 118(2) . . ? C34 C33 C32 119(2) . . ? C35 C34 C33 121(3) . . ? C34 C35 C36 125(3) . . ? C31 C36 C35 110(2) . . ? C42 C41 C46 116(3) . . ? C42 C41 P2 125(2) . . ? C46 C41 P2 118(2) . . ? C41 C42 C43 118(3) . . ? C44 C43 C42 130(3) . . ? C43 C44 C45 113(3) . . ? C46 C45 C44 119(3) . . ? C45 C46 C41 122(3) . . ? C56 C51 C52 112(2) . . ? C56 C51 P2 122.7(19) . . ? C52 C51 P2 124.5(18) . . ? C53 C52 C51 127(2) . . ? C54 C53 C52 115(2) . . ? C53 C54 C55 128(3) . . ? C54 C55 C56 114(2) . . ? C51 C56 C55 121(3) . . ? C06 C01 C02 118.5(18) . . ? C06 C01 S2 120.7(12) . . ? C02 C01 S2 120.5(18) . . ? C03 C02 C01 128(2) . . ? C03 C02 C08 117(2) . . ? C01 C02 C08 115(2) . . ? C02 C03 C04 114(2) . . ? C05 C04 C03 113(2) . . ? C06 C05 C04 126(3) . . ? C05 C06 C01 120.4(19) . . ? C05 C06 C07 117(2) . . ? C01 C06 C07 122.8(17) . . ? C06 C07 P3 117.1(14) . . ? C02 C08 P4 105.5(15) . . ? C66 C61 C62 122(2) . . ? C66 C61 P3 117.2(18) . . ? C62 C61 P3 120.8(17) . . ? C61 C62 C63 120(2) . . ? C62 C63 C64 113(2) . . ? C65 C64 C63 123(2) . . ? C64 C65 C66 125(3) . . ? C65 C66 C61 116(3) . . ? C76 C71 C72 122.4(17) . . ? C76 C71 P3 121.9(14) . . ? C72 C71 P3 115.6(16) . . ? C73 C72 C71 120(2) . . ? C74 C73 C72 120(3) . . ? C73 C74 C75 120(3) . . ? C74 C75 C76 123(3) . . ? C71 C76 C75 112(2) . . ? C86 C81 C82 115(2) . . ? C86 C81 P4 130(2) . . ? C82 C81 P4 114(2) . . ? C83 C82 C81 121(3) . . ? C82 C83 C84 113(3) . . ? C85 C84 C83 121(3) . . ? C84 C85 C86 125(3) . . ? C81 C86 C85 122(2) . . ? C92 C91 C96 108(2) . . ? C92 C91 P4 126.0(18) . . ? C96 C91 P4 125.9(19) . . ? C93 C92 C91 128(2) . . ? C92 C93 C94 113(3) . . ? C95 C94 C93 124.2(16) . . ? C96 C95 C94 115(2) . . ? C95 C96 C91 131(2) . . ? _refine_diff_density_max 1.358 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.108 #===END