# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_9 _database_code_depnum_ccdc_archive 'CCDC 827117' #TrackingRef 'data_9_edited.cif' # data original saved as magbas0419 # start Validation Reply Form _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: RESPONSE:This manuscript is accepted for publication in Dalton Transactions. The authors listed have contributed to the paper in different areas of expertise: Aaron J. Rossini, Alan W. Macgregor, Robert W. Schurko: Measuring and interpretation of ^207^Pb Solid-State NMR Spectroscopy and writing the manuscript. Anita S. Smith, Glen G. Briand: Syntheses of the compounds and wrting the manuscript. Gabriele Schatte: X-ray data collection and refinement of the crystal structures discussed in the manuscript. ; # end Validation Reply Form # SUBMISSION DETAILS _audit_creation_method 'manual editing of SHELXL-2012 template' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H52 N2 Pb2 S4, C7 H8' _chemical_formula_sum 'C45 H60 N2 Pb2 S4' _chemical_formula_weight 1171.57 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' 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' # Crystal Data _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.91250(10) _cell_length_b 14.0434(2) _cell_length_c 14.9513(2) _cell_angle_alpha 99.7056(8) _cell_angle_beta 109.4720(8) _cell_angle_gamma 90.8606(8) _cell_volume 2317.58(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10729 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.679 _exptl_crystal_F_000 1144 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 7.467 _shelx_estimated_absorpt_T_min 0.317 _shelx_estimated_absorpt_T_max 0.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.31 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; The program Denzo-SMN/Scalepack uses a multiparameter algorithm for scaling diffraction intensities [Z. Otwinowski, D. Borek, W. Majewskia & W. Minorb (2003) Acta Cryst. A59, 228-234]. The parameters, refined by least squares methods, are unit cell, crystal orientatation and mosaicity, uniformaty of exposure, correction to the Lorentz factor due to misalignment of the spindle axis etc.. This method gives only a range of scale factors used in during the refinement. The values for the transmission factors estimated from size of the crystal and the absorption coefficient are mu are now in given as _shelx_estimated_absorpt_T_min and _shelx_estimated_absorpt_T_max in SHELXL-2012. These values are also stated for _exptl_absorpt_correction_T_min and _exptl_absorpt_correction_T_max. ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 20994 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.700 _diffrn_reflns_theta_max 27.902 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 11047 _reflns_number_gt 9667 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (SHELXTL-NT v6.14, Bruker AXS)' _computing_publication_material 'WinGX v1.80.05 2009 (L. J. Farrugia)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+2.7486P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11047 _refine_ls_number_parameters 510 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.23895(2) 0.58955(2) 0.41403(2) 0.02126(3) Uani 1 1 d . . . . . Pb2 Pb 0.30409(2) 0.75663(2) 0.19274(2) 0.02614(4) Uani 1 1 d . . . . . S1 S 0.09353(7) 0.61522(6) 0.51011(6) 0.02870(16) Uani 1 1 d . . . . . S2 S 0.16088(7) 0.74954(5) 0.29908(5) 0.02424(15) Uani 1 1 d . . . . . S3 S 0.18627(8) 0.62695(6) 0.04080(6) 0.02991(17) Uani 1 1 d . . . . . S4 S 0.43975(8) 0.63564(7) 0.28809(6) 0.03496(19) Uani 1 1 d . . . . . N1 N 0.0818(2) 0.48668(19) 0.28066(18) 0.0285(6) Uani 1 1 d . . . . . N2 N 0.2645(2) 0.4084(2) 0.4368(2) 0.0378(7) Uani 1 1 d . . . . . C1A C 0.0663(6) 0.3934(4) 0.3073(5) 0.0322(18) Uani 0.620(14) 1 d . . P A 1 H11A H 0.0100 0.3491 0.2510 0.039 Uiso 0.620(14) 1 calc R U P A 1 H12A H 0.0317 0.4024 0.3596 0.039 Uiso 0.620(14) 1 calc R U P A 1 C2A C 0.1842(8) 0.3492(5) 0.3407(6) 0.0384(19) Uani 0.620(14) 1 d . . P A 1 H21A H 0.2237 0.3478 0.2918 0.046 Uiso 0.620(14) 1 calc R U P A 1 H22A H 0.1707 0.2818 0.3483 0.046 Uiso 0.620(14) 1 calc R U P A 1 C1B C 0.1199(11) 0.3790(6) 0.2784(7) 0.030(3) Uani 0.380(14) 1 d . . P A 2 H11B H 0.0536 0.3342 0.2313 0.036 Uiso 0.380(14) 1 calc R U P A 2 H12B H 0.1898 0.3727 0.2567 0.036 Uiso 0.380(14) 1 calc R U P A 2 C2B C 0.1508(10) 0.3507(8) 0.3757(10) 0.031(3) Uani 0.380(14) 1 d . . P A 2 H21B H 0.0869 0.3660 0.4033 0.037 Uiso 0.380(14) 1 calc R U P A 2 H22B H 0.1614 0.2805 0.3708 0.037 Uiso 0.380(14) 1 calc R U P A 2 C3 C 0.1058(4) 0.4942(4) 0.1928(3) 0.0598(13) Uani 1 1 d . . . . . H3A H 0.1867 0.4757 0.1992 0.072 Uiso 1 1 calc R U . . . H3B H 0.0990 0.5612 0.1820 0.072 Uiso 1 1 calc R U . . . H3C H 0.0478 0.4510 0.1379 0.072 Uiso 1 1 calc R U . . . C4 C -0.0386(3) 0.5181(5) 0.2680(4) 0.088(2) Uani 1 1 d . . . . . H4A H -0.0955 0.4801 0.2086 0.106 Uiso 1 1 calc R U . . . H4B H -0.0395 0.5870 0.2636 0.106 Uiso 1 1 calc R U . . . H4C H -0.0612 0.5082 0.3232 0.106 Uiso 1 1 calc R U . . . C5 C 0.3838(4) 0.3841(3) 0.4377(3) 0.0504(10) Uani 1 1 d . . . . . H5A H 0.4435 0.4172 0.4982 0.061 Uiso 1 1 calc R U . . . H5B H 0.3988 0.4049 0.3831 0.061 Uiso 1 1 calc R U . . . H5C H 0.3889 0.3139 0.4324 0.061 Uiso 1 1 calc R U . . . C6 C 0.2512(4) 0.3935(3) 0.5277(3) 0.0520(11) Uani 1 1 d . . . . . H6A H 0.2626 0.3258 0.5345 0.062 Uiso 1 1 calc R U . . . H6B H 0.1711 0.4087 0.5274 0.062 Uiso 1 1 calc R U . . . H6C H 0.3111 0.4360 0.5820 0.062 Uiso 1 1 calc R U . . . C11 C 0.1540(3) 0.7342(2) 0.5740(2) 0.0261(6) Uani 1 1 d . . . . . C12 C 0.0935(3) 0.8151(2) 0.5443(2) 0.0294(7) Uani 1 1 d . . . . . C13 C 0.1416(3) 0.9070(3) 0.5956(3) 0.0397(8) Uani 1 1 d . . . . . H13 H 0.1016 0.9621 0.5763 0.048 Uiso 1 1 calc . U . . . C14 C 0.2467(4) 0.9199(3) 0.6742(3) 0.0431(9) Uani 1 1 d . . . . . H14 H 0.2789 0.9833 0.7078 0.052 Uiso 1 1 calc . U . . . C15 C 0.3044(3) 0.8400(3) 0.7035(2) 0.0387(8) Uani 1 1 d . . . . . H15 H 0.3761 0.8491 0.7576 0.046 Uiso 1 1 calc . U . . . C16 C 0.2596(3) 0.7466(2) 0.6551(2) 0.0302(7) Uani 1 1 d . . . . . C17 C -0.0200(3) 0.8046(3) 0.4594(3) 0.0365(8) Uani 1 1 d . . . . . H17A H -0.0452 0.8690 0.4483 0.044 Uiso 1 1 calc R U . . . H17B H -0.0824 0.7689 0.4724 0.044 Uiso 1 1 calc R U . . . H17C H -0.0066 0.7692 0.4020 0.044 Uiso 1 1 calc R U . . . C18 C 0.3255(3) 0.6616(3) 0.6889(3) 0.0409(8) Uani 1 1 d . . . . . H18A H 0.3621 0.6326 0.6419 0.049 Uiso 1 1 calc R U . . . H18B H 0.2696 0.6133 0.6949 0.049 Uiso 1 1 calc R U . . . H18C H 0.3879 0.6836 0.7517 0.049 Uiso 1 1 calc R U . . . C21 C 0.1951(3) 0.8744(2) 0.3563(2) 0.0227(6) Uani 1 1 d . . . . . C22 C 0.3006(3) 0.9054(2) 0.4349(2) 0.0249(6) Uani 1 1 d . . . . . C23 C 0.3240(3) 1.0035(2) 0.4741(2) 0.0325(7) Uani 1 1 d . . . . . H23 H 0.3956 1.0253 0.5266 0.039 Uiso 1 1 calc . U . . . C24 C 0.2450(3) 1.0697(2) 0.4379(3) 0.0380(8) Uani 1 1 d . . . . . H24 H 0.2629 1.1367 0.4651 0.046 Uiso 1 1 calc . U . . . C25 C 0.1399(3) 1.0388(2) 0.3622(3) 0.0358(8) Uani 1 1 d . . . . . H25 H 0.0852 1.0848 0.3386 0.043 Uiso 1 1 calc . U . . . C26 C 0.1133(3) 0.9415(2) 0.3201(2) 0.0273(6) Uani 1 1 d . . . . . C27 C 0.3869(3) 0.8358(2) 0.4801(2) 0.0297(7) Uani 1 1 d . . . . . H27A H 0.4590 0.8721 0.5277 0.036 Uiso 1 1 calc R U . . . H27B H 0.4085 0.7937 0.4300 0.036 Uiso 1 1 calc R U . . . H27C H 0.3497 0.7962 0.5121 0.036 Uiso 1 1 calc R U . . . C28 C -0.0015(3) 0.9108(3) 0.2363(2) 0.0374(8) Uani 1 1 d . . . . . H28A H -0.0519 0.9654 0.2289 0.045 Uiso 1 1 calc R U . . . H28B H -0.0438 0.8567 0.2485 0.045 Uiso 1 1 calc R U . . . H28C H 0.0169 0.8902 0.1770 0.045 Uiso 1 1 calc R U . . . C31 C 0.1137(3) 0.7190(2) -0.0212(2) 0.0264(6) Uani 1 1 d . . . . . C32 C 0.1695(3) 0.7668(3) -0.0730(2) 0.0329(7) Uani 1 1 d . . . . . C33 C 0.1108(3) 0.8375(3) -0.1214(3) 0.0446(9) Uani 1 1 d . . . . . H33 H 0.1472 0.8689 -0.1575 0.054 Uiso 1 1 calc . U . . . C34 C 0.0011(4) 0.8629(3) -0.1182(3) 0.0531(11) Uani 1 1 d . . . . . H34 H -0.0374 0.9120 -0.1512 0.064 Uiso 1 1 calc . U . . . C35 C -0.0531(3) 0.8167(3) -0.0669(3) 0.0437(9) Uani 1 1 d . . . . . H35 H -0.1284 0.8353 -0.0644 0.052 Uiso 1 1 calc . U . . . C36 C 0.0004(3) 0.7432(2) -0.0188(2) 0.0310(7) Uani 1 1 d . . . . . C37 C 0.2913(3) 0.7426(3) -0.0758(3) 0.0449(9) Uani 1 1 d . . . . . H37A H 0.3170 0.7851 -0.1123 0.054 Uiso 1 1 calc R U . . . H37B H 0.2877 0.6749 -0.1072 0.054 Uiso 1 1 calc R U . . . H37C H 0.3486 0.7521 -0.0098 0.054 Uiso 1 1 calc R U . . . C38 C -0.0643(3) 0.6924(3) 0.0328(2) 0.0375(8) Uani 1 1 d . . . . . H38A H -0.0738 0.6226 0.0072 0.045 Uiso 1 1 calc R U . . . H38B H -0.1432 0.7172 0.0227 0.045 Uiso 1 1 calc R U . . . H38C H -0.0182 0.7041 0.1020 0.045 Uiso 1 1 calc R U . . . C41 C 0.5418(3) 0.6262(2) 0.2232(2) 0.0275(7) Uani 1 1 d . . . . . C42 C 0.5367(3) 0.5397(2) 0.1586(2) 0.0319(7) Uani 1 1 d . . . . . C43 C 0.6187(4) 0.5298(3) 0.1101(3) 0.0458(9) Uani 1 1 d . . . . . H43 H 0.6159 0.4714 0.0665 0.055 Uiso 1 1 calc . U . . . C44 C 0.7034(4) 0.6036(4) 0.1246(3) 0.0568(12) Uani 1 1 d . . . . . H44 H 0.7588 0.5960 0.0912 0.068 Uiso 1 1 calc . U . . . C45 C 0.7082(3) 0.6881(4) 0.1872(3) 0.0550(11) Uani 1 1 d . . . . . H45 H 0.7673 0.7385 0.1964 0.066 Uiso 1 1 calc . U . . . C46 C 0.6281(3) 0.7022(3) 0.2379(3) 0.0380(8) Uani 1 1 d . . . . . C47 C 0.4436(4) 0.4591(3) 0.1403(3) 0.0446(9) Uani 1 1 d . . . . . H47A H 0.4563 0.4038 0.0961 0.054 Uiso 1 1 calc R U . . . H47B H 0.3642 0.4813 0.1113 0.054 Uiso 1 1 calc R U . . . H47C H 0.4492 0.4394 0.2014 0.054 Uiso 1 1 calc R U . . . C48 C 0.6359(4) 0.7962(3) 0.3048(3) 0.0595(12) Uani 1 1 d . . . . . H48A H 0.7157 0.8289 0.3233 0.071 Uiso 1 1 calc R U . . . H48B H 0.6213 0.7837 0.3626 0.071 Uiso 1 1 calc R U . . . H48C H 0.5759 0.8375 0.2722 0.071 Uiso 1 1 calc R U . . . C51 C 0.3560(4) 0.0900(4) 0.0454(4) 0.0672(13) Uani 1 1 d D . . . . C52 C 0.3799(3) 0.1827(3) 0.0951(3) 0.0533(11) Uani 1 1 d D . . . . H52 H 0.4011 0.2315 0.0654 0.064 Uiso 1 1 calc . U . . . C53 C 0.3748(4) 0.2085(4) 0.1852(4) 0.0758(16) Uani 1 1 d D . . . . H53 H 0.3887 0.2746 0.2160 0.091 Uiso 1 1 calc . U . . . C54 C 0.3497(4) 0.1391(4) 0.2319(4) 0.0700(14) Uani 1 1 d D . . . . H54 H 0.3485 0.1569 0.2958 0.084 Uiso 1 1 calc . U . . . C55 C 0.3270(6) 0.0474(4) 0.1877(4) 0.0798(16) Uani 1 1 d D . . . . H55 H 0.3085 -0.0005 0.2195 0.096 Uiso 1 1 calc . U . . . C56 C 0.3304(6) 0.0206(4) 0.0924(4) 0.0859(18) Uani 1 1 d D . . . . H56 H 0.3149 -0.0454 0.0611 0.103 Uiso 1 1 calc . U . . . C57 C 0.3596(6) 0.0652(6) -0.0538(4) 0.111(3) Uani 1 1 d D . . . . H57A H 0.2780 0.0580 -0.1003 0.134 Uiso 1 1 calc R U . . . H57B H 0.3973 0.0042 -0.0610 0.134 Uiso 1 1 calc R U . . . H57C H 0.4057 0.1170 -0.0658 0.134 Uiso 1 1 calc R U . . . 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 0.02160(6) 0.02040(6) 0.02146(6) 0.00418(4) 0.00683(4) 0.00037(4) Pb2 0.02959(6) 0.02639(7) 0.02333(6) 0.00641(5) 0.00930(5) 0.00219(5) S1 0.0316(4) 0.0254(4) 0.0329(4) 0.0026(3) 0.0173(3) 0.0002(3) S2 0.0291(4) 0.0195(4) 0.0233(3) 0.0030(3) 0.0085(3) 0.0003(3) S3 0.0408(4) 0.0262(4) 0.0235(4) 0.0050(3) 0.0117(3) 0.0048(3) S4 0.0349(4) 0.0490(5) 0.0272(4) 0.0140(4) 0.0148(3) 0.0164(4) N1 0.0308(14) 0.0283(14) 0.0214(12) 0.0068(11) 0.0015(11) -0.0057(11) N2 0.0328(15) 0.0225(14) 0.0467(17) 0.0080(12) -0.0021(13) 0.0012(11) C1A 0.032(3) 0.024(3) 0.039(3) 0.005(2) 0.012(3) -0.008(2) C2A 0.045(4) 0.022(3) 0.040(4) -0.001(3) 0.006(3) 0.003(3) C1B 0.042(6) 0.016(4) 0.027(5) 0.000(3) 0.008(4) -0.007(4) C2B 0.031(6) 0.021(5) 0.036(7) 0.009(4) 0.003(4) -0.003(4) C3 0.074(3) 0.074(3) 0.0261(19) -0.0094(19) 0.0208(19) -0.034(2) C4 0.024(2) 0.152(6) 0.056(3) -0.034(3) -0.0027(19) -0.007(3) C5 0.051(2) 0.048(2) 0.058(3) 0.016(2) 0.022(2) 0.0252(19) C6 0.043(2) 0.038(2) 0.091(3) 0.039(2) 0.030(2) 0.0134(17) C11 0.0315(16) 0.0251(16) 0.0280(15) 0.0030(12) 0.0192(13) 0.0024(12) C12 0.0348(17) 0.0280(17) 0.0341(17) 0.0088(13) 0.0217(14) 0.0052(13) C13 0.055(2) 0.0259(18) 0.049(2) 0.0099(15) 0.0304(18) 0.0047(15) C14 0.061(2) 0.032(2) 0.040(2) -0.0022(16) 0.0269(19) -0.0092(17) C15 0.046(2) 0.041(2) 0.0265(17) -0.0004(15) 0.0134(15) -0.0079(16) C16 0.0378(17) 0.0312(18) 0.0260(16) 0.0067(13) 0.0158(14) 0.0019(14) C17 0.0332(17) 0.0356(19) 0.047(2) 0.0148(16) 0.0181(16) 0.0107(14) C18 0.045(2) 0.043(2) 0.0309(18) 0.0063(15) 0.0078(16) 0.0071(16) C21 0.0285(15) 0.0167(14) 0.0258(15) 0.0007(11) 0.0143(12) -0.0006(11) C22 0.0284(15) 0.0231(16) 0.0262(15) 0.0031(12) 0.0139(12) -0.0012(12) C23 0.0366(17) 0.0289(18) 0.0303(17) -0.0013(13) 0.0126(14) -0.0059(14) C24 0.053(2) 0.0219(17) 0.0394(19) -0.0027(14) 0.0201(17) -0.0035(15) C25 0.048(2) 0.0263(17) 0.0411(19) 0.0092(14) 0.0234(16) 0.0100(15) C26 0.0341(16) 0.0232(16) 0.0286(16) 0.0056(12) 0.0154(13) 0.0035(12) C27 0.0291(16) 0.0290(17) 0.0267(16) 0.0020(13) 0.0055(13) -0.0014(13) C28 0.0373(18) 0.0327(19) 0.0375(19) 0.0112(15) 0.0041(15) 0.0069(15) C31 0.0324(16) 0.0255(16) 0.0193(14) 0.0037(12) 0.0068(12) -0.0009(12) C32 0.0344(17) 0.0345(19) 0.0287(16) 0.0070(14) 0.0091(14) -0.0028(14) C33 0.047(2) 0.047(2) 0.042(2) 0.0232(18) 0.0110(17) -0.0013(17) C34 0.046(2) 0.055(3) 0.059(3) 0.036(2) 0.007(2) 0.0094(19) C35 0.0330(18) 0.050(2) 0.049(2) 0.0178(18) 0.0104(16) 0.0060(16) C36 0.0303(16) 0.0358(19) 0.0237(15) 0.0061(13) 0.0050(13) -0.0034(13) C37 0.048(2) 0.051(2) 0.048(2) 0.0180(18) 0.0290(18) 0.0066(18) C38 0.0341(18) 0.048(2) 0.0303(17) 0.0059(15) 0.0115(14) -0.0020(15) C41 0.0249(15) 0.0337(18) 0.0243(15) 0.0109(13) 0.0061(12) 0.0084(13) C42 0.0330(17) 0.0350(18) 0.0291(16) 0.0110(14) 0.0096(14) 0.0131(14) C43 0.051(2) 0.054(2) 0.042(2) 0.0149(18) 0.0239(18) 0.0242(19) C44 0.040(2) 0.091(4) 0.051(3) 0.027(2) 0.0251(19) 0.016(2) C45 0.0280(18) 0.078(3) 0.059(3) 0.030(2) 0.0069(18) -0.0084(19) C46 0.0285(16) 0.041(2) 0.0384(19) 0.0120(16) 0.0020(14) 0.0010(14) C47 0.060(2) 0.0271(19) 0.047(2) 0.0091(16) 0.0181(19) 0.0051(17) C48 0.050(2) 0.044(2) 0.061(3) 0.001(2) -0.008(2) -0.0114(19) C51 0.062(3) 0.062(3) 0.067(3) 0.004(3) 0.013(2) 0.005(2) C52 0.037(2) 0.044(2) 0.076(3) 0.000(2) 0.021(2) -0.0033(17) C53 0.061(3) 0.057(3) 0.105(4) -0.009(3) 0.035(3) -0.012(2) C54 0.061(3) 0.072(4) 0.072(3) 0.005(3) 0.020(3) 0.004(3) C55 0.109(5) 0.056(3) 0.090(4) 0.030(3) 0.046(4) 0.016(3) C56 0.121(5) 0.041(3) 0.092(4) 0.010(3) 0.032(4) 0.008(3) C57 0.106(5) 0.155(7) 0.054(3) -0.015(4) 0.020(3) 0.016(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. ; # MOLECULAR GEOMETRY 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 N1 2.455(2) . ? Pb1 S1 2.5880(8) . ? Pb1 N2 2.632(3) . ? Pb1 S2 3.0276(8) . ? Pb2 S3 2.6172(8) . ? Pb2 S4 2.6257(8) . ? Pb2 S2 2.7027(8) . ? S1 C11 1.785(3) . ? S2 C21 1.793(3) . ? S3 C31 1.783(3) . ? S4 C41 1.785(3) . ? N1 C3 1.455(4) . ? N1 C1A 1.458(6) . ? N1 C4 1.467(5) . ? N1 C1B 1.583(10) . ? N2 C5 1.463(5) . ? N2 C6 1.468(5) . ? N2 C2B 1.490(11) . ? N2 C2A 1.525(7) . ? C1A C2A 1.507(12) . ? C1A H11A 0.9900 . ? C1A H12A 0.9900 . ? C2A H21A 0.9900 . ? C2A H22A 0.9900 . ? C1B C2B 1.500(18) . ? C1B H11B 0.9900 . ? C1B H12B 0.9900 . ? C2B H21B 0.9900 . ? C2B H22B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C16 1.410(4) . ? C11 C12 1.411(4) . ? C12 C13 1.390(5) . ? C12 C17 1.499(5) . ? C13 C14 1.387(6) . ? C13 H13 0.9500 . ? C14 C15 1.383(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(5) . ? C15 H15 0.9500 . ? C16 C18 1.504(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C22 1.406(4) . ? C21 C26 1.407(4) . ? C22 C23 1.388(4) . ? C22 C27 1.503(4) . ? C23 C24 1.378(5) . ? C23 H23 0.9500 . ? C24 C25 1.383(5) . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C28 1.511(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C36 1.407(4) . ? C31 C32 1.414(5) . ? C32 C33 1.386(5) . ? C32 C37 1.509(5) . ? C33 C34 1.374(6) . ? C33 H33 0.9500 . ? C34 C35 1.382(6) . ? C34 H34 0.9500 . ? C35 C36 1.398(5) . ? C35 H35 0.9500 . ? C36 C38 1.505(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 C42 1.404(5) . ? C41 C46 1.408(5) . ? C42 C43 1.394(5) . ? C42 C47 1.498(5) . ? C43 C44 1.373(6) . ? C43 H43 0.9500 . ? C44 C45 1.369(7) . ? C44 H44 0.9500 . ? C45 C46 1.400(6) . ? C45 H45 0.9500 . ? C46 C48 1.497(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C51 C52 1.359(6) . ? C51 C56 1.380(7) . ? C51 C57 1.480(7) . ? C52 C53 1.357(7) . ? C52 H52 0.9500 . ? C53 C54 1.373(7) . ? C53 H53 0.9500 . ? C54 C55 1.323(7) . ? C54 H54 0.9500 . ? C55 C56 1.425(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 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 Pb1 S1 89.57(7) . . ? N1 Pb1 N2 71.94(9) . . ? S1 Pb1 N2 93.16(7) . . ? N1 Pb1 S2 85.28(6) . . ? S1 Pb1 S2 97.12(2) . . ? N2 Pb1 S2 154.91(7) . . ? S3 Pb2 S4 96.07(3) . . ? S3 Pb2 S2 99.62(2) . . ? S4 Pb2 S2 89.42(2) . . ? C11 S1 Pb1 96.35(10) . . ? C21 S2 Pb2 94.16(10) . . ? C21 S2 Pb1 120.84(10) . . ? Pb2 S2 Pb1 107.27(2) . . ? C31 S3 Pb2 91.12(10) . . ? C41 S4 Pb2 96.63(10) . . ? C3 N1 C1A 122.0(4) . . ? C3 N1 C4 106.9(4) . . ? C1A N1 C4 98.3(5) . . ? C3 N1 C1B 92.8(5) . . ? C4 N1 C1B 126.5(6) . . ? C3 N1 Pb1 106.7(2) . . ? C1A N1 Pb1 109.3(3) . . ? C4 N1 Pb1 113.5(2) . . ? C1B N1 Pb1 106.9(4) . . ? C5 N2 C6 108.9(3) . . ? C5 N2 C2B 125.4(7) . . ? C6 N2 C2B 93.8(7) . . ? C5 N2 C2A 102.3(5) . . ? C6 N2 C2A 120.5(5) . . ? C5 N2 Pb1 108.5(2) . . ? C6 N2 Pb1 111.5(2) . . ? C2B N2 Pb1 107.7(4) . . ? C2A N2 Pb1 104.2(3) . . ? N1 C1A C2A 110.7(7) . . ? N1 C1A H11A 109.5 . . ? C2A C1A H11A 109.5 . . ? N1 C1A H12A 109.5 . . ? C2A C1A H12A 109.5 . . ? H11A C1A H12A 108.1 . . ? C1A C2A N2 110.0(6) . . ? C1A C2A H21A 109.7 . . ? N2 C2A H21A 109.7 . . ? C1A C2A H22A 109.7 . . ? N2 C2A H22A 109.7 . . ? H21A C2A H22A 108.2 . . ? C2B C1B N1 111.8(10) . . ? C2B C1B H11B 109.3 . . ? N1 C1B H11B 109.3 . . ? C2B C1B H12B 109.3 . . ? N1 C1B H12B 109.3 . . ? H11B C1B H12B 107.9 . . ? N2 C2B C1B 105.7(10) . . ? N2 C2B H21B 110.6 . . ? C1B C2B H21B 110.6 . . ? N2 C2B H22B 110.6 . . ? C1B C2B H22B 110.6 . . ? H21B C2B H22B 108.7 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C16 C11 C12 120.5(3) . . ? C16 C11 S1 120.1(2) . . ? C12 C11 S1 119.5(2) . . ? C13 C12 C11 118.5(3) . . ? C13 C12 C17 119.5(3) . . ? C11 C12 C17 122.0(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 121.2(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 118.8(3) . . ? C15 C16 C18 119.6(3) . . ? C11 C16 C18 121.6(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C21 C26 120.4(3) . . ? C22 C21 S2 121.5(2) . . ? C26 C21 S2 118.1(2) . . ? C23 C22 C21 118.8(3) . . ? C23 C22 C27 118.8(3) . . ? C21 C22 C27 122.3(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 118.8(3) . . ? C25 C26 C28 119.3(3) . . ? C21 C26 C28 121.9(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C36 C31 C32 120.2(3) . . ? C36 C31 S3 119.7(2) . . ? C32 C31 S3 120.1(2) . . ? C33 C32 C31 119.1(3) . . ? C33 C32 C37 119.8(3) . . ? C31 C32 C37 121.1(3) . . ? C34 C33 C32 121.2(4) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 119.8(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 121.5(3) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 118.2(3) . . ? C35 C36 C38 119.5(3) . . ? C31 C36 C38 122.3(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42 C41 C46 120.3(3) . . ? C42 C41 S4 118.5(3) . . ? C46 C41 S4 121.2(3) . . ? C43 C42 C41 119.2(3) . . ? C43 C42 C47 119.8(3) . . ? C41 C42 C47 121.0(3) . . ? C44 C43 C42 120.7(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 121.6(4) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C45 C46 C41 118.0(4) . . ? C45 C46 C48 119.8(4) . . ? C41 C46 C48 122.2(4) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C51 C56 116.8(5) . . ? C52 C51 C57 121.2(5) . . ? C56 C51 C57 121.9(5) . . ? C53 C52 C51 122.9(5) . . ? C53 C52 H52 118.6 . . ? C51 C52 H52 118.6 . . ? C52 C53 C54 120.1(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.8(5) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.1(5) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.2(5) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C1A C2A 72.9(7) . . . . ? C4 N1 C1A C2A -171.1(6) . . . . ? C1B N1 C1A C2A 39.3(8) . . . . ? Pb1 N1 C1A C2A -52.5(8) . . . . ? N1 C1A C2A N2 68.5(10) . . . . ? C5 N2 C2A C1A -156.9(7) . . . . ? C6 N2 C2A C1A 82.2(8) . . . . ? C2B N2 C2A C1A 57.0(12) . . . . ? Pb1 N2 C2A C1A -43.9(9) . . . . ? C3 N1 C1B C2B 159.7(10) . . . . ? C1A N1 C1B C2B -48.3(10) . . . . ? C4 N1 C1B C2B -86.7(10) . . . . ? Pb1 N1 C1B C2B 51.3(11) . . . . ? C5 N2 C2B C1B -81.2(10) . . . . ? C6 N2 C2B C1B 162.2(10) . . . . ? C2A N2 C2B C1B -39.3(11) . . . . ? Pb1 N2 C2B C1B 48.2(12) . . . . ? N1 C1B C2B N2 -69.5(14) . . . . ? Pb1 S1 C11 C16 -79.0(2) . . . . ? Pb1 S1 C11 C12 102.7(2) . . . . ? C16 C11 C12 C13 1.2(5) . . . . ? S1 C11 C12 C13 179.5(2) . . . . ? C16 C11 C12 C17 -179.0(3) . . . . ? S1 C11 C12 C17 -0.8(4) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C17 C12 C13 C14 -179.6(3) . . . . ? C12 C13 C14 C15 -1.0(6) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C11 0.9(5) . . . . ? C14 C15 C16 C18 179.6(3) . . . . ? C12 C11 C16 C15 -1.7(5) . . . . ? S1 C11 C16 C15 -180.0(2) . . . . ? C12 C11 C16 C18 179.6(3) . . . . ? S1 C11 C16 C18 1.4(4) . . . . ? Pb2 S2 C21 C22 -80.3(2) . . . . ? Pb1 S2 C21 C22 32.7(3) . . . . ? Pb2 S2 C21 C26 99.4(2) . . . . ? Pb1 S2 C21 C26 -147.6(2) . . . . ? C26 C21 C22 C23 -1.9(4) . . . . ? S2 C21 C22 C23 177.8(2) . . . . ? C26 C21 C22 C27 176.1(3) . . . . ? S2 C21 C22 C27 -4.2(4) . . . . ? C21 C22 C23 C24 0.9(5) . . . . ? C27 C22 C23 C24 -177.1(3) . . . . ? C22 C23 C24 C25 0.7(5) . . . . ? C23 C24 C25 C26 -1.3(5) . . . . ? C24 C25 C26 C21 0.3(5) . . . . ? C24 C25 C26 C28 -178.9(3) . . . . ? C22 C21 C26 C25 1.3(5) . . . . ? S2 C21 C26 C25 -178.4(2) . . . . ? C22 C21 C26 C28 -179.5(3) . . . . ? S2 C21 C26 C28 0.8(4) . . . . ? Pb2 S3 C31 C36 -94.7(2) . . . . ? Pb2 S3 C31 C32 85.7(2) . . . . ? C36 C31 C32 C33 -0.2(5) . . . . ? S3 C31 C32 C33 179.4(3) . . . . ? C36 C31 C32 C37 179.5(3) . . . . ? S3 C31 C32 C37 -1.0(4) . . . . ? C31 C32 C33 C34 1.3(6) . . . . ? C37 C32 C33 C34 -178.3(4) . . . . ? C32 C33 C34 C35 -0.8(7) . . . . ? C33 C34 C35 C36 -0.9(7) . . . . ? C34 C35 C36 C31 1.9(6) . . . . ? C34 C35 C36 C38 -177.6(4) . . . . ? C32 C31 C36 C35 -1.4(5) . . . . ? S3 C31 C36 C35 179.1(3) . . . . ? C32 C31 C36 C38 178.1(3) . . . . ? S3 C31 C36 C38 -1.5(4) . . . . ? Pb2 S4 C41 C42 -107.7(2) . . . . ? Pb2 S4 C41 C46 74.1(3) . . . . ? C46 C41 C42 C43 0.6(5) . . . . ? S4 C41 C42 C43 -177.6(3) . . . . ? C46 C41 C42 C47 -178.5(3) . . . . ? S4 C41 C42 C47 3.3(4) . . . . ? C41 C42 C43 C44 -0.3(5) . . . . ? C47 C42 C43 C44 178.8(4) . . . . ? C42 C43 C44 C45 0.0(6) . . . . ? C43 C44 C45 C46 0.0(6) . . . . ? C44 C45 C46 C41 0.4(6) . . . . ? C44 C45 C46 C48 -179.4(4) . . . . ? C42 C41 C46 C45 -0.7(5) . . . . ? S4 C41 C46 C45 177.5(3) . . . . ? C42 C41 C46 C48 179.1(3) . . . . ? S4 C41 C46 C48 -2.7(5) . . . . ? C56 C51 C52 C53 -2.6(7) . . . . ? C57 C51 C52 C53 178.4(5) . . . . ? C51 C52 C53 C54 2.9(7) . . . . ? C52 C53 C54 C55 -1.9(8) . . . . ? C53 C54 C55 C56 0.9(9) . . . . ? C52 C51 C56 C55 1.4(9) . . . . ? C57 C51 C56 C55 -179.6(6) . . . . ? C54 C55 C56 C51 -0.7(10) . . . . ? _refine_diff_density_max 0.825 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.101 data_10 _database_code_depnum_ccdc_archive 'CCDC 827118' #TrackingRef 'data_10_sq_s_edited.cif' # data original saved as magbas0417_sq_s # start Validation Reply Form _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: This manuscript is accepted for publication in Dalton Transactions. The authors listed have contributed to the paper in different areas of expertise: Aaron J. Rossini, Alan W. Macgregor, Robert W. Schurko: Measuring and interpretation of ^207^Pb Solid-State NMR Spectroscopy and writing the manuscript. Anita S. Smith, Glen G. Briand: Syntheses of the compounds and wrting the manuscript. Gabriele Schatte: X-ray data collection and refinement of the crystal structures discussed in the manuscript. ; # end Validation Reply Form # SUBMISSION DETAILS _audit_creation_method 'manual editing of SHELXL-2012 template' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 P2 Pb3 S6' _chemical_formula_sum 'C54 H70 P2 Pb3 S6' _chemical_formula_weight 1594.97 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' P P 0.1023 0.0942 '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' # Crystal Data _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2754(2) _cell_length_b 20.1016(2) _cell_length_c 18.9169(2) _cell_angle_alpha 90 _cell_angle_beta 114.6800(6) _cell_angle_gamma 90 _cell_volume 7005.65(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13542 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 33.14 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.512 _exptl_crystal_F_000 3064 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _exptl_absorpt_coefficient_mu 7.444 _shelx_estimated_absorpt_T_min 0.279 _shelx_estimated_absorpt_T_max 0.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.279 _exptl_absorpt_correction_T_max 0.348 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; The program Denzo-SMN/Scalepack uses a multiparameter algorithm for scaling diffraction intensities [Z. Otwinowski, D. Borek, W. Majewskia & W. Minorb (2003) Acta Cryst. A59, 228-234]. The parameters, refined by least squares methods, are unit cell, crystal orientatation and mosaicity, uniformaty of exposure, correction to the Lorentz factor due to misalignment of the spindle axis etc.. This method gives only a range of scale factors used in during the refinement. The values for the transmission factors estimated from size of the crystal and the absorption coefficient are mu are now in given as _shelx_estimated_absorpt_T_min and _shelx_estimated_absorpt_T_max in SHELXL-2012. These values are also stated for _exptl_absorpt_correction_T_min and _exptl_absorpt_correction_T_max. ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 19559 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.119 _diffrn_reflns_theta_max 30.034 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 10209 _reflns_number_gt 8098 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (SHELXTL-NT v6.14, Bruker AXS)' _computing_publication_material 'WinGX v1.80.05 2009 (L. J. Farrugia)' _refine_special_details ; The carbon atoms C(41), C(42) and C(43) were disordered over two site. The disorder was modelled using the atom-split model. The site occupancy factors were allowed to refine and converged to 0.065 and 0.035, respectively. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.312 0.250 0.062 788 74 ' ' 2 0.812 0.750 0.062 788 74 ' ' _platon_squeeze_details ;Approximately 23% of the unit cell volume (1576 ^3^) comprises a region of disordered solvent which could not be modeled as discrete atomic sites. The program PLATON/SQUEEZE was used to calculate the contribution from the solvent region to the diffraction. A total electron count of 148 electrons was found in the total solvent-accessible void volume within the unit cell. The eletcron count of 74 e^-^ corresponds to 1.5 molecules of toluene in each void. Toluene was used as a solvent for growing the crystals. The data were corrected for disordered electron density through use of the SQUEEZE procedure as implemented in PLATON leading to a set of solvent-free diffraction intensities. The modified data improved the R-factors (before SQUEEZE: R~1~ = 0.0361, wR~2~ = 0.1009; largest difference peak and hole, 1.470 and -1.372 e-/ ^3^; after SQUEEZE: R~1~ = 0.0316, wR~2~ = 0.0743; largest difference peak and hole, 0.996 and -1.392 e^-^/ ^3^). Derived values (formula weight, density, absorption coefficient) do not contain the contribution of the disordered solvent. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+14.0431P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary heavy _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 10209 _refine_ls_number_parameters 331 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.0000 0.16887(2) 0.2500 0.02813(5) Uani 1 2 d S T P A . Pb2 Pb 0.14909(2) 0.22142(2) 0.49981(2) 0.03416(5) Uani 1 1 d . . . . . S1 S 0.14022(5) 0.13562(5) 0.38372(5) 0.03274(19) Uani 1 1 d . . . . . S2 S 0.13512(7) 0.11346(6) 0.57213(6) 0.0524(3) Uani 1 1 d . . . . . S3 S 0.00631(5) 0.23828(6) 0.41413(6) 0.0437(2) Uani 1 1 d . . . . . P1 P 0.04666(6) 0.05571(6) 0.19347(6) 0.0420(2) Uani 1 1 d D . . . . C11 C 0.22681(19) 0.1434(2) 0.3801(2) 0.0329(8) Uani 1 1 d . . . . . C12 C 0.2847(2) 0.1043(2) 0.4324(2) 0.0402(9) Uani 1 1 d . . . . . C13 C 0.3527(2) 0.1110(3) 0.4305(3) 0.0503(11) Uani 1 1 d . . . . . H13 H 0.3925 0.0859 0.4657 0.060 Uiso 1 1 calc . U . . . C14 C 0.3632(2) 0.1529(3) 0.3790(3) 0.0545(12) Uani 1 1 d . . . . . H14 H 0.4099 0.1567 0.3791 0.065 Uiso 1 1 calc . U . . . C15 C 0.3059(2) 0.1896(3) 0.3268(2) 0.0477(11) Uani 1 1 d . . . . . H15 H 0.3135 0.2176 0.2905 0.057 Uiso 1 1 calc . U . . . C16 C 0.2369(2) 0.1863(2) 0.3266(2) 0.0352(8) Uani 1 1 d . . . . . C17 C 0.2750(3) 0.0563(3) 0.4866(3) 0.0577(12) Uani 1 1 d . . . . . H17A H 0.3220 0.0366 0.5198 0.087 Uiso 1 1 calc R U . . . H17B H 0.2414 0.0212 0.4569 0.087 Uiso 1 1 calc R U . . . H17C H 0.2553 0.0795 0.5191 0.087 Uiso 1 1 calc R U . . . C18 C 0.1766(2) 0.2268(2) 0.2683(3) 0.0482(10) Uani 1 1 d . . . . . H18A H 0.1397 0.1970 0.2320 0.072 Uiso 1 1 calc R U . . . H18B H 0.1960 0.2554 0.2396 0.072 Uiso 1 1 calc R U . . . H18C H 0.1546 0.2544 0.2954 0.072 Uiso 1 1 calc R U . . . C21 C 0.1514(3) 0.1372(2) 0.6682(2) 0.0498(11) Uani 1 1 d . . . . . C22 C 0.0967(3) 0.1679(3) 0.6846(3) 0.0608(14) Uani 1 1 d . . . . . C23 C 0.1097(4) 0.1824(4) 0.7610(4) 0.087(2) Uani 1 1 d . . . . . H23 H 0.0735 0.2042 0.7721 0.105 Uiso 1 1 calc . U . . . C24 C 0.1746(5) 0.1652(5) 0.8207(4) 0.111(3) Uani 1 1 d . . . . . H24 H 0.1821 0.1732 0.8731 0.133 Uiso 1 1 calc . U . . . C25 C 0.2274(4) 0.1372(4) 0.8058(3) 0.096(3) Uani 1 1 d . . . . . H25 H 0.2726 0.1276 0.8480 0.115 Uiso 1 1 calc . U . . . C26 C 0.2181(3) 0.1213(3) 0.7294(3) 0.0663(15) Uani 1 1 d . . . . . C27 C 0.0249(3) 0.1852(3) 0.6216(4) 0.0787(17) Uani 1 1 d . . . . . H27A H 0.0320 0.2096 0.5805 0.118 Uiso 1 1 calc R U . . . H27B H -0.0022 0.2130 0.6428 0.118 Uiso 1 1 calc R U . . . H27C H -0.0024 0.1443 0.5999 0.118 Uiso 1 1 calc R U . . . C28 C 0.2777(3) 0.0887(4) 0.7154(4) 0.090(2) Uani 1 1 d . . . . . H28A H 0.2659 0.0417 0.7026 0.136 Uiso 1 1 calc R U . . . H28B H 0.3232 0.0922 0.7624 0.136 Uiso 1 1 calc R U . . . H28C H 0.2833 0.1109 0.6721 0.136 Uiso 1 1 calc R U . . . C31 C -0.0091(2) 0.3265(2) 0.4075(2) 0.0464(11) Uani 1 1 d . . . . . C32 C 0.0241(2) 0.3687(2) 0.3734(3) 0.0524(12) Uani 1 1 d . . . . . C33 C 0.0089(3) 0.4372(3) 0.3681(3) 0.0725(16) Uani 1 1 d . . . . . H33 H 0.0305 0.4659 0.3439 0.087 Uiso 1 1 calc . U . . . C34 C -0.0365(4) 0.4623(4) 0.3973(4) 0.095(2) Uani 1 1 d . . . . . H34 H -0.0462 0.5087 0.3939 0.114 Uiso 1 1 calc . U . . . C35 C -0.0686(4) 0.4217(4) 0.4317(3) 0.090(2) Uani 1 1 d . . . . . H35 H -0.0996 0.4403 0.4528 0.108 Uiso 1 1 calc . U . . . C36 C -0.0565(3) 0.3532(3) 0.4364(3) 0.0714(17) Uani 1 1 d . . . . . C37 C 0.0767(3) 0.3438(2) 0.3425(3) 0.0534(11) Uani 1 1 d . . . . . H37A H 0.1241 0.3364 0.3858 0.080 Uiso 1 1 calc R U . . . H37B H 0.0815 0.3768 0.3068 0.080 Uiso 1 1 calc R U . . . H37C H 0.0588 0.3019 0.3146 0.080 Uiso 1 1 calc R U . . . C38 C -0.0956(3) 0.3082(5) 0.4708(3) 0.108(3) Uani 1 1 d . . . . . H38A H -0.1257 0.2763 0.4313 0.162 Uiso 1 1 calc R U . . . H38B H -0.1264 0.3351 0.4881 0.162 Uiso 1 1 calc R U . . . H38C H -0.0598 0.2840 0.5153 0.162 Uiso 1 1 calc R U . . . C41A C -0.0011(8) 0.0327(8) 0.0940(6) 0.053(3) Uani 0.65 1 d . . P A 1 H41A H 0.0010 0.0693 0.0607 0.080 Uiso 0.65 1 calc R U P A 1 H41B H -0.0518 0.0232 0.0830 0.080 Uiso 0.65 1 calc R U P A 1 H41C H 0.0213 -0.0071 0.0834 0.080 Uiso 0.65 1 calc R U P A 1 C42A C 0.1391(6) 0.0501(9) 0.2100(9) 0.079(5) Uani 0.65 1 d . . P A 1 H42A H 0.1696 0.0497 0.2661 0.119 Uiso 0.65 1 calc R U P A 1 H42B H 0.1520 0.0885 0.1864 0.119 Uiso 0.65 1 calc R U P A 1 H42C H 0.1470 0.0090 0.1867 0.119 Uiso 0.65 1 calc R U P A 1 C43A C 0.0375(6) -0.0150(4) 0.2482(6) 0.065(2) Uani 0.65 1 d . . P A 1 H43A H 0.0432 -0.0566 0.2233 0.078 Uiso 0.65 1 calc R U P A 1 H43B H 0.0764 -0.0135 0.3016 0.078 Uiso 0.65 1 calc R U P A 1 C41B C 0.1433(7) 0.0327(16) 0.2344(16) 0.073(9) Uani 0.35 1 d D . P A 2 H41D H 0.1492 -0.0087 0.2104 0.110 Uiso 0.35 1 calc R U P A 2 H41E H 0.1610 0.0264 0.2907 0.110 Uiso 0.35 1 calc R U P A 2 H41F H 0.1711 0.0683 0.2240 0.110 Uiso 0.35 1 calc R U P A 2 C42B C 0.0183(15) 0.0538(15) 0.0872(6) 0.071(8) Uani 0.35 1 d D . P A 2 H42D H 0.0382 0.0140 0.0732 0.106 Uiso 0.35 1 calc R U P A 2 H42E H 0.0365 0.0936 0.0712 0.106 Uiso 0.35 1 calc R U P A 2 H42F H -0.0348 0.0529 0.0607 0.106 Uiso 0.35 1 calc R U P A 2 C43B C -0.0044(9) -0.0163(6) 0.2050(12) 0.069(5) Uani 0.35 1 d D . P A 2 H43C H -0.0562 -0.0127 0.1686 0.083 Uiso 0.35 1 calc R U P A 2 H43D H 0.0152 -0.0581 0.1937 0.083 Uiso 0.35 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.03233(9) 0.02507(9) 0.02784(9) 0.000 0.01340(7) 0.000 Pb2 0.03191(7) 0.03989(9) 0.02801(7) -0.00431(5) 0.00987(5) -0.00306(6) S1 0.0281(4) 0.0409(5) 0.0267(4) -0.0041(4) 0.0090(3) -0.0006(4) S2 0.0748(8) 0.0452(6) 0.0333(5) -0.0008(5) 0.0186(5) -0.0096(6) S3 0.0321(5) 0.0610(7) 0.0354(5) -0.0035(5) 0.0116(4) 0.0020(5) P1 0.0502(6) 0.0377(6) 0.0342(5) -0.0069(4) 0.0137(5) 0.0104(5) C11 0.0289(17) 0.036(2) 0.0318(17) -0.0108(15) 0.0110(14) -0.0031(15) C12 0.0362(19) 0.041(2) 0.0380(19) -0.0109(17) 0.0103(16) 0.0047(17) C13 0.0316(19) 0.058(3) 0.051(2) -0.018(2) 0.0075(18) 0.011(2) C14 0.033(2) 0.073(3) 0.061(3) -0.024(3) 0.023(2) -0.004(2) C15 0.042(2) 0.060(3) 0.049(2) -0.015(2) 0.027(2) -0.013(2) C16 0.0319(18) 0.037(2) 0.0361(18) -0.0124(16) 0.0139(15) -0.0059(16) C17 0.052(3) 0.054(3) 0.055(3) 0.013(2) 0.010(2) 0.015(2) C18 0.047(2) 0.054(3) 0.048(2) 0.006(2) 0.024(2) -0.002(2) C21 0.064(3) 0.055(3) 0.0319(19) -0.0039(19) 0.022(2) -0.029(2) C22 0.079(3) 0.066(3) 0.047(2) -0.001(2) 0.035(3) -0.030(3) C23 0.116(5) 0.107(5) 0.070(4) -0.022(4) 0.070(4) -0.043(4) C24 0.126(6) 0.172(8) 0.049(3) -0.031(4) 0.050(4) -0.069(6) C25 0.081(4) 0.155(7) 0.033(2) -0.001(3) 0.006(3) -0.059(5) C26 0.060(3) 0.089(4) 0.043(2) 0.001(3) 0.015(2) -0.038(3) C27 0.087(4) 0.081(4) 0.080(4) 0.014(3) 0.048(4) 0.002(3) C28 0.059(3) 0.120(6) 0.075(4) 0.017(4) 0.010(3) -0.029(4) C31 0.036(2) 0.062(3) 0.0292(18) -0.0117(19) 0.0018(16) 0.014(2) C32 0.048(2) 0.048(3) 0.044(2) -0.009(2) 0.001(2) 0.009(2) C33 0.072(3) 0.055(3) 0.063(3) -0.017(3) 0.001(3) 0.011(3) C34 0.092(5) 0.080(5) 0.076(4) -0.029(4) -0.003(4) 0.041(4) C35 0.071(4) 0.124(6) 0.056(3) -0.028(4) 0.008(3) 0.055(4) C36 0.049(3) 0.114(5) 0.042(2) -0.010(3) 0.010(2) 0.035(3) C37 0.052(3) 0.049(3) 0.056(3) -0.003(2) 0.020(2) -0.006(2) C38 0.063(4) 0.204(9) 0.064(3) 0.017(5) 0.035(3) 0.065(5) C41A 0.060(7) 0.058(8) 0.034(4) -0.016(4) 0.012(4) -0.001(5) C42A 0.049(6) 0.086(12) 0.074(10) -0.049(8) -0.003(5) 0.028(5) C43A 0.108(8) 0.033(4) 0.059(5) 0.003(4) 0.041(5) 0.022(5) C41B 0.054(10) 0.040(11) 0.066(15) -0.016(9) -0.034(8) 0.028(8) C42B 0.066(17) 0.08(2) 0.041(9) -0.019(10) -0.005(8) 0.033(13) C43B 0.063(10) 0.023(7) 0.114(15) -0.017(9) 0.029(11) 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. ; # MOLECULAR GEOMETRY 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 P1 2.8386(10) 2 ? Pb1 P1 2.8386(10) . ? Pb1 S1 2.9870(9) . ? Pb1 S1 2.9871(9) 2 ? Pb2 S2 2.6428(12) . ? Pb2 S3 2.6840(10) . ? Pb2 S1 2.7387(9) . ? S1 C11 1.792(4) . ? S2 C21 1.771(4) . ? S3 C31 1.797(5) . ? P1 C42A 1.771(11) . ? P1 C41A 1.781(10) . ? P1 C43A 1.812(8) . ? P1 C41B 1.839(10) . ? P1 C43B 1.844(9) . ? P1 C42B 1.847(10) . ? C11 C16 1.408(5) . ? C11 C12 1.416(5) . ? C12 C13 1.400(6) . ? C12 C17 1.480(6) . ? C13 C14 1.369(7) . ? C13 H13 0.9500 . ? C14 C15 1.382(7) . ? C14 H14 0.9500 . ? C15 C16 1.398(5) . ? C15 H15 0.9500 . ? C16 C18 1.500(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C26 1.402(7) . ? C21 C22 1.411(7) . ? C22 C23 1.388(7) . ? C22 C27 1.488(8) . ? C23 C24 1.373(10) . ? C23 H23 0.9500 . ? C24 C25 1.341(11) . ? C24 H24 0.9500 . ? C25 C26 1.414(7) . ? C25 H25 0.9500 . ? C26 C28 1.492(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C36 1.396(6) . ? C31 C32 1.397(7) . ? C32 C33 1.404(7) . ? C32 C37 1.500(7) . ? C33 C34 1.354(9) . ? C33 H33 0.9500 . ? C34 C35 1.367(11) . ? C34 H34 0.9500 . ? C35 C36 1.395(10) . ? C35 H35 0.9500 . ? C36 C38 1.517(10) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A C43A 1.55(2) 2 ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B C43B 1.64(4) 2 ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? 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 P1 Pb1 P1 73.48(5) 2 . ? P1 Pb1 S1 81.42(3) 2 . ? P1 Pb1 S1 77.91(3) . . ? P1 Pb1 S1 77.91(3) 2 2 ? P1 Pb1 S1 81.42(3) . 2 ? S1 Pb1 S1 154.14(4) . 2 ? S2 Pb2 S3 95.43(4) . . ? S2 Pb2 S1 84.99(3) . . ? S3 Pb2 S1 84.38(3) . . ? C11 S1 Pb2 103.79(12) . . ? C11 S1 Pb1 123.32(12) . . ? Pb2 S1 Pb1 105.00(3) . . ? C21 S2 Pb2 107.17(15) . . ? C31 S3 Pb2 106.20(14) . . ? C42A P1 C41A 103.8(7) . . ? C42A P1 C43A 101.7(7) . . ? C41A P1 C43A 105.1(5) . . ? C41B P1 C43B 107.7(11) . . ? C41B P1 C42B 104.3(13) . . ? C43B P1 C42B 100.2(11) . . ? C42A P1 Pb1 118.6(6) . . ? C41A P1 Pb1 119.1(6) . . ? C43A P1 Pb1 106.5(3) . . ? C41B P1 Pb1 120.4(11) . . ? C43B P1 Pb1 107.0(5) . . ? C42B P1 Pb1 115.2(10) . . ? C16 C11 C12 120.9(3) . . ? C16 C11 S1 121.3(3) . . ? C12 C11 S1 117.7(3) . . ? C13 C12 C11 117.8(4) . . ? C13 C12 C17 119.9(4) . . ? C11 C12 C17 122.3(4) . . ? C14 C13 C12 121.6(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 121.2(4) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 118.2(4) . . ? C15 C16 C18 119.0(4) . . ? C11 C16 C18 122.8(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C26 C21 C22 119.6(4) . . ? C26 C21 S2 119.2(4) . . ? C22 C21 S2 121.1(4) . . ? C23 C22 C21 119.8(6) . . ? C23 C22 C27 118.8(6) . . ? C21 C22 C27 121.4(4) . . ? C24 C23 C22 120.2(6) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 122.2(6) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C21 C26 C25 117.6(6) . . ? C21 C26 C28 121.9(5) . . ? C25 C26 C28 120.5(6) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C36 C31 C32 119.4(5) . . ? C36 C31 S3 118.6(4) . . ? C32 C31 S3 121.9(3) . . ? C31 C32 C33 119.6(5) . . ? C31 C32 C37 122.3(4) . . ? C33 C32 C37 118.1(5) . . ? C34 C33 C32 120.2(7) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.7(6) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 121.0(6) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.0(6) . . ? C35 C36 C38 120.5(6) . . ? C31 C36 C38 120.5(6) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P1 C41A H41A 109.5 . . ? P1 C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? P1 C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? P1 C42A H42A 109.5 . . ? P1 C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? P1 C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C43A C43A P1 111.2(6) 2 . ? C43A C43A H43A 109.4 2 . ? P1 C43A H43A 109.4 . . ? C43A C43A H43B 109.4 2 . ? P1 C43A H43B 109.4 . . ? H43A C43A H43B 108.0 . . ? P1 C41B H41D 109.5 . . ? P1 C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? P1 C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? P1 C42B H42D 109.5 . . ? P1 C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? P1 C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C43B C43B P1 107.5(10) 2 . ? C43B C43B H43C 110.2 2 . ? P1 C43B H43C 110.2 . . ? C43B C43B H43D 110.2 2 . ? P1 C43B H43D 110.2 . . ? H43C C43B H43D 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pb2 S1 C11 C16 -96.0(3) . . . . ? Pb1 S1 C11 C16 22.7(4) . . . . ? Pb2 S1 C11 C12 84.7(3) . . . . ? Pb1 S1 C11 C12 -156.6(2) . . . . ? C16 C11 C12 C13 1.7(5) . . . . ? S1 C11 C12 C13 -179.1(3) . . . . ? C16 C11 C12 C17 -176.9(4) . . . . ? S1 C11 C12 C17 2.4(5) . . . . ? C11 C12 C13 C14 -1.2(6) . . . . ? C17 C12 C13 C14 177.4(4) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C16 1.6(7) . . . . ? C14 C15 C16 C11 -1.1(6) . . . . ? C14 C15 C16 C18 -179.5(4) . . . . ? C12 C11 C16 C15 -0.5(5) . . . . ? S1 C11 C16 C15 -179.8(3) . . . . ? C12 C11 C16 C18 177.8(4) . . . . ? S1 C11 C16 C18 -1.4(5) . . . . ? Pb2 S2 C21 C26 -103.6(4) . . . . ? Pb2 S2 C21 C22 80.6(4) . . . . ? C26 C21 C22 C23 0.3(7) . . . . ? S2 C21 C22 C23 176.1(4) . . . . ? C26 C21 C22 C27 -179.5(5) . . . . ? S2 C21 C22 C27 -3.7(7) . . . . ? C21 C22 C23 C24 -1.8(9) . . . . ? C27 C22 C23 C24 178.0(6) . . . . ? C22 C23 C24 C25 3.1(11) . . . . ? C23 C24 C25 C26 -2.9(12) . . . . ? C22 C21 C26 C25 0.0(7) . . . . ? S2 C21 C26 C25 -175.9(4) . . . . ? C22 C21 C26 C28 179.9(5) . . . . ? S2 C21 C26 C28 4.0(7) . . . . ? C24 C25 C26 C21 1.3(10) . . . . ? C24 C25 C26 C28 -178.6(7) . . . . ? Pb2 S3 C31 C36 -120.2(3) . . . . ? Pb2 S3 C31 C32 60.8(3) . . . . ? C36 C31 C32 C33 -0.4(6) . . . . ? S3 C31 C32 C33 178.5(3) . . . . ? C36 C31 C32 C37 178.9(4) . . . . ? S3 C31 C32 C37 -2.2(6) . . . . ? C31 C32 C33 C34 1.4(7) . . . . ? C37 C32 C33 C34 -178.0(5) . . . . ? C32 C33 C34 C35 -0.5(9) . . . . ? C33 C34 C35 C36 -1.2(10) . . . . ? C34 C35 C36 C31 2.1(8) . . . . ? C34 C35 C36 C38 -176.7(6) . . . . ? C32 C31 C36 C35 -1.2(7) . . . . ? S3 C31 C36 C35 179.8(4) . . . . ? C32 C31 C36 C38 177.6(4) . . . . ? S3 C31 C36 C38 -1.4(6) . . . . ? C42A P1 C43A C43A 172.1(9) . . . 2 ? C41A P1 C43A C43A -80.0(10) . . . 2 ? C41B P1 C43A C43A 167.5(13) . . . 2 ? C43B P1 C43A C43A -48.2(14) . . . 2 ? C42B P1 C43A C43A -89.0(13) . . . 2 ? Pb1 P1 C43A C43A 47.3(9) . . . 2 ? C42A P1 C43B C43B 90.7(12) . . . 2 ? C41A P1 C43B C43B -168.9(14) . . . 2 ? C43A P1 C43B C43B 42.1(13) . . . 2 ? C41B P1 C43B C43B 79.7(15) . . . 2 ? C42B P1 C43B C43B -171.6(15) . . . 2 ? Pb1 P1 C43B C43B -51.2(13) . . . 2 ? _refine_diff_density_max 0.998 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.116 data_11 _database_code_depnum_ccdc_archive 'CCDC 827119' #TrackingRef 'data_11_edited.cif' # data original saved as magbas0413 # start Validation Reply Form _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE:This manuscript is accepted for publication in Dalton Transactions. The authors listed have contributed to the paper in different areas of expertise: Aaron J. Rossini, Alan W. Macgregor, Robert W. Schurko: Measuring and interpretation of ^207^Pb Solid-State NMR Spectroscopy and writing the manuscript. Anita S. Smith, Glen G. Briand: Syntheses of the compounds and wrting the manuscript. Gabriele Schatte: X-ray data collection and refinement of the crystal structures discussed in the manuscript. PROBLEM: Alert level G - PLAT003_ALERT_2_G Number of Uiso or Uij Restrained Atom Sites .... 30 RESPONSE: Hydrogen atoms were included at geometrically idealized positions and were not refined. The isotropic thermal parameters of these hydrogen atoms were fixed at 1.2 or 1.5 times that of the preceding carbon atom. ; # end Validation Reply Form # SUBMISSION DETAILS _audit_creation_method 'manual editing of SHELXL-2012 template' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H60 P2 Pb2 S4' _chemical_formula_sum 'C58 H60 P2 Pb2 S4' _chemical_formula_weight 1361.62 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' P P 0.1023 0.0942 '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' # Crystal Data _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0551(2) _cell_length_b 11.3774(2) _cell_length_c 12.8875(3) _cell_angle_alpha 87.0455(9) _cell_angle_beta 71.5348(10) _cell_angle_gamma 81.6016(7) _cell_volume 1383.42(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30250 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 33.14 _exptl_crystal_description rod _exptl_crystal_colour yellow-orange _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.634 _exptl_crystal_F_000 666 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 6.321 _shelx_estimated_absorpt_T_min 0.632 _shelx_estimated_absorpt_T_max 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; The program Denzo-SMN/Scalepack uses a multiparameter algorithm for scaling diffraction intensities [Z. Otwinowski, D. Borek, W. Majewskia & W. Minorb (2003) Acta Cryst. A59, 228-234]. The parameters, refined by least squares methods, are unit cell, crystal orientatation and mosaicity, uniformaty of exposure, correction to the Lorentz factor due to misalignment of the spindle axis etc.. This method gives only a range of scale factors used in during the refinement. The values for the transmission factors estimated from size of the crystal and the absorption coefficient are mu are now in given as _shelx_estimated_absorpt_T_min and _shelx_estimated_absorpt_T_max in SHELXL-2012. These values are also stated for _exptl_absorpt_correction_T_min and _exptl_absorpt_correction_T_max. ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 28280 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.666 _diffrn_reflns_theta_max 28.278 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6863 _reflns_number_gt 6041 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (SHELXTL-NT v6.14, Bruker AXS)' _computing_publication_material 'WinGX v1.80.05 2009 (L. J. Farrugia)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+3.7127P] 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 6863 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.55694(2) 0.81671(2) 0.08521(2) 0.02161(6) Uani 1 1 d . . . . . P1 P 0.56350(12) 0.66837(9) -0.08514(9) 0.0164(2) Uani 1 1 d . . . . . S1 S 0.30522(13) 0.75862(10) 0.18182(10) 0.0273(3) Uani 1 1 d . . . . . S2 S 0.69838(13) 0.63555(10) 0.15520(10) 0.0254(3) Uani 1 1 d . . . . . C1 C 0.4663(5) 0.5423(4) -0.0356(4) 0.0197(9) Uani 1 1 d . . . . . H1A H 0.3676 0.5722 0.0075 0.024 Uiso 1 1 calc R U . . . H1B H 0.4634 0.4982 -0.0989 0.024 Uiso 1 1 calc R U . . . C11 C 0.2207(5) 0.9063(4) 0.2202(4) 0.0221(9) Uani 1 1 d . . . . . C12 C 0.1795(5) 0.9837(4) 0.1445(4) 0.0242(10) Uani 1 1 d . . . . . C13 C 0.1126(5) 1.0988(4) 0.1774(5) 0.0317(11) Uani 1 1 d . . . . . H13 H 0.0856 1.1522 0.1261 0.038 Uiso 1 1 calc . U . . . C14 C 0.0857(5) 1.1351(4) 0.2825(5) 0.0347(12) Uani 1 1 d . . . . . H14 H 0.0419 1.2137 0.3035 0.042 Uiso 1 1 calc . U . . . C15 C 0.1223(6) 1.0574(5) 0.3581(5) 0.0354(12) Uani 1 1 d . . . . . H15 H 0.1002 1.0828 0.4314 0.042 Uiso 1 1 calc . U . . . C16 C 0.1906(5) 0.9430(5) 0.3293(4) 0.0297(11) Uani 1 1 d . . . . . C17 C 0.2024(6) 0.9452(4) 0.0293(4) 0.0330(12) Uani 1 1 d . . . . . H17A H 0.3040 0.9343 -0.0108 0.040 Uiso 1 1 calc R U . . . H17B H 0.1534 1.0062 -0.0072 0.040 Uiso 1 1 calc R U . . . H17C H 0.1649 0.8701 0.0311 0.040 Uiso 1 1 calc R U . . . C18 C 0.2306(7) 0.8617(5) 0.4131(5) 0.0435(14) Uani 1 1 d . . . . . H18A H 0.1977 0.9017 0.4841 0.052 Uiso 1 1 calc R U . . . H18B H 0.3338 0.8410 0.3909 0.052 Uiso 1 1 calc R U . . . H18C H 0.1866 0.7892 0.4192 0.052 Uiso 1 1 calc R U . . . C21 C 0.6965(5) 0.6967(4) 0.2801(4) 0.0207(9) Uani 1 1 d . . . . . C22 C 0.7992(5) 0.7681(4) 0.2809(4) 0.0226(9) Uani 1 1 d . . . . . C23 C 0.8004(6) 0.8088(4) 0.3805(4) 0.0331(12) Uani 1 1 d . . . . . H23 H 0.8698 0.8566 0.3818 0.040 Uiso 1 1 calc . U . . . C24 C 0.7033(7) 0.7813(5) 0.4766(5) 0.0398(14) Uani 1 1 d . . . . . H24 H 0.7059 0.8097 0.5439 0.048 Uiso 1 1 calc . U . . . C25 C 0.6006(6) 0.7116(5) 0.4758(4) 0.0350(12) Uani 1 1 d . . . . . H25 H 0.5322 0.6943 0.5427 0.042 Uiso 1 1 calc . U . . . C26 C 0.5971(5) 0.6670(4) 0.3784(4) 0.0252(10) Uani 1 1 d . . . . . C27 C 0.9097(6) 0.8009(5) 0.1770(4) 0.0359(12) Uani 1 1 d . . . . . H27A H 0.9439 0.8739 0.1888 0.043 Uiso 1 1 calc R U . . . H27B H 0.8676 0.8137 0.1177 0.043 Uiso 1 1 calc R U . . . H27C H 0.9890 0.7363 0.1573 0.043 Uiso 1 1 calc R U . . . C28 C 0.4887(6) 0.5888(5) 0.3800(5) 0.0359(12) Uani 1 1 d . . . . . H28A H 0.5362 0.5091 0.3550 0.043 Uiso 1 1 calc R U . . . H28B H 0.4349 0.6222 0.3314 0.043 Uiso 1 1 calc R U . . . H28C H 0.4241 0.5839 0.4547 0.043 Uiso 1 1 calc R U . . . C31 C 0.7323(5) 0.6045(4) -0.1786(4) 0.0194(9) Uani 1 1 d . . . . . C32 C 0.8505(5) 0.5805(4) -0.1422(4) 0.0284(11) Uani 1 1 d . . . . . H32 H 0.8429 0.5995 -0.0695 0.034 Uiso 1 1 calc . U . . . C33 C 0.9788(6) 0.5288(5) -0.2122(5) 0.0395(13) Uani 1 1 d . . . . . H33 H 1.0592 0.5130 -0.1874 0.047 Uiso 1 1 calc . U . . . C34 C 0.9905(6) 0.5000(5) -0.3181(4) 0.0409(14) Uani 1 1 d . . . . . H34 H 1.0784 0.4639 -0.3656 0.049 Uiso 1 1 calc . U . . . C35 C 0.8747(6) 0.5240(5) -0.3543(4) 0.0409(14) Uani 1 1 d . . . . . H35 H 0.8828 0.5048 -0.4271 0.049 Uiso 1 1 calc . U . . . C36 C 0.7463(5) 0.5760(4) -0.2850(4) 0.0296(11) Uani 1 1 d . . . . . H36 H 0.6667 0.5923 -0.3108 0.036 Uiso 1 1 calc . U . . . C41 C 0.4699(5) 0.7523(4) -0.1711(3) 0.0193(9) Uani 1 1 d . . . . . C42 C 0.3517(5) 0.7173(4) -0.1881(4) 0.0290(11) Uani 1 1 d . . . . . H42 H 0.3196 0.6448 -0.1576 0.035 Uiso 1 1 calc . U . . . C43 C 0.2809(6) 0.7887(5) -0.2499(5) 0.0386(13) Uani 1 1 d . . . . . H43 H 0.2004 0.7646 -0.2618 0.046 Uiso 1 1 calc . U . . . C44 C 0.3260(7) 0.8944(5) -0.2942(5) 0.0434(15) Uani 1 1 d . . . . . H44 H 0.2756 0.9435 -0.3350 0.052 Uiso 1 1 calc . U . . . C45 C 0.4451(6) 0.9288(4) -0.2790(4) 0.0335(12) Uani 1 1 d . . . . . H45 H 0.4777 1.0005 -0.3111 0.040 Uiso 1 1 calc . U . . . C46 C 0.5168(5) 0.8590(4) -0.2172(4) 0.0251(10) Uani 1 1 d . . . . . H46 H 0.5977 0.8833 -0.2061 0.030 Uiso 1 1 calc . U . . . 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 0.02325(10) 0.01795(8) 0.02669(10) -0.00221(6) -0.01146(7) -0.00359(6) P1 0.0168(6) 0.0153(5) 0.0185(6) 0.0007(4) -0.0076(5) -0.0023(4) S1 0.0232(6) 0.0225(5) 0.0332(7) -0.0001(5) -0.0052(5) -0.0024(5) S2 0.0291(6) 0.0253(5) 0.0282(6) -0.0058(5) -0.0194(5) 0.0017(5) C1 0.021(2) 0.018(2) 0.021(2) -0.0006(17) -0.0067(19) -0.0055(17) C11 0.015(2) 0.022(2) 0.029(2) -0.0019(18) -0.0051(19) -0.0061(17) C12 0.013(2) 0.028(2) 0.030(3) 0.0006(19) -0.004(2) -0.0051(18) C13 0.024(3) 0.029(2) 0.042(3) 0.001(2) -0.011(2) -0.002(2) C14 0.023(3) 0.027(2) 0.052(3) -0.014(2) -0.011(3) 0.004(2) C15 0.026(3) 0.040(3) 0.041(3) -0.019(2) -0.011(2) -0.002(2) C16 0.019(2) 0.041(3) 0.031(3) -0.004(2) -0.009(2) -0.005(2) C17 0.038(3) 0.032(3) 0.029(3) 0.004(2) -0.010(2) -0.006(2) C18 0.040(3) 0.056(4) 0.034(3) -0.006(3) -0.013(3) 0.001(3) C21 0.023(2) 0.021(2) 0.023(2) 0.0032(17) -0.016(2) -0.0009(18) C22 0.022(2) 0.025(2) 0.027(2) 0.0030(18) -0.015(2) -0.0064(18) C23 0.044(3) 0.031(3) 0.036(3) 0.003(2) -0.025(3) -0.015(2) C24 0.059(4) 0.037(3) 0.031(3) -0.006(2) -0.023(3) -0.008(3) C25 0.040(3) 0.042(3) 0.023(3) 0.007(2) -0.010(2) -0.006(2) C26 0.030(3) 0.025(2) 0.025(2) 0.0077(18) -0.016(2) -0.0056(19) C27 0.036(3) 0.040(3) 0.037(3) 0.007(2) -0.015(3) -0.017(2) C28 0.035(3) 0.038(3) 0.043(3) 0.017(2) -0.020(3) -0.017(2) C31 0.021(2) 0.0163(19) 0.019(2) 0.0024(16) -0.0051(19) 0.0004(17) C32 0.024(3) 0.033(2) 0.026(3) 0.002(2) -0.010(2) 0.005(2) C33 0.022(3) 0.048(3) 0.041(3) 0.009(3) -0.006(2) 0.005(2) C34 0.032(3) 0.046(3) 0.028(3) -0.002(2) 0.005(2) 0.016(3) C35 0.035(3) 0.055(3) 0.027(3) -0.007(2) -0.006(2) 0.004(3) C36 0.026(3) 0.035(3) 0.027(3) -0.002(2) -0.007(2) -0.002(2) C41 0.023(2) 0.0180(19) 0.016(2) -0.0024(16) -0.0060(18) 0.0034(17) C42 0.025(3) 0.030(2) 0.035(3) 0.002(2) -0.016(2) -0.001(2) C43 0.036(3) 0.042(3) 0.046(3) -0.003(3) -0.028(3) 0.003(2) C44 0.058(4) 0.039(3) 0.039(3) -0.004(2) -0.033(3) 0.020(3) C45 0.050(4) 0.024(2) 0.026(3) 0.006(2) -0.014(3) -0.002(2) C46 0.030(3) 0.022(2) 0.023(2) 0.0016(18) -0.009(2) -0.0010(19) _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. ; # MOLECULAR GEOMETRY 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 S1 2.6079(13) . ? Pb1 S2 2.6171(11) . ? Pb1 P1 2.8161(11) . ? P1 C31 1.815(5) . ? P1 C41 1.821(4) . ? P1 C1 1.828(4) . ? S1 C11 1.787(4) . ? S2 C21 1.779(4) . ? C1 C1 1.530(8) 2_665 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 C12 1.399(6) . ? C11 C16 1.413(7) . ? C12 C13 1.402(7) . ? C12 C17 1.507(7) . ? C13 C14 1.368(8) . ? C13 H13 0.9500 . ? C14 C15 1.382(8) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C18 1.500(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C26 1.404(7) . ? C21 C22 1.407(6) . ? C22 C23 1.391(7) . ? C22 C27 1.514(7) . ? C23 C24 1.366(8) . ? C23 H23 0.9500 . ? C24 C25 1.393(8) . ? C24 H24 0.9500 . ? C25 C26 1.391(7) . ? C25 H25 0.9500 . ? C26 C28 1.499(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C36 1.385(6) . ? C31 C32 1.397(6) . ? C32 C33 1.386(7) . ? C32 H32 0.9500 . ? C33 C34 1.385(8) . ? C33 H33 0.9500 . ? C34 C35 1.373(8) . ? C34 H34 0.9500 . ? C35 C36 1.385(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.389(6) . ? C41 C46 1.402(6) . ? C42 C43 1.388(7) . ? C42 H42 0.9500 . ? C43 C44 1.379(8) . ? C43 H43 0.9500 . ? C44 C45 1.385(8) . ? C44 H44 0.9500 . ? C45 C46 1.384(7) . ? C45 H45 0.9500 . ? C46 H46 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 S1 Pb1 S2 96.86(4) . . ? S1 Pb1 P1 85.43(4) . . ? S2 Pb1 P1 86.84(3) . . ? C31 P1 C41 105.3(2) . . ? C31 P1 C1 105.0(2) . . ? C41 P1 C1 104.4(2) . . ? C31 P1 Pb1 119.77(15) . . ? C41 P1 Pb1 108.43(14) . . ? C1 P1 Pb1 112.64(15) . . ? C11 S1 Pb1 95.85(15) . . ? C21 S2 Pb1 98.91(14) . . ? C1 C1 P1 112.1(4) 2_665 . ? C1 C1 H1A 109.2 2_665 . ? P1 C1 H1A 109.2 . . ? C1 C1 H1B 109.2 2_665 . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C12 C11 C16 120.1(4) . . ? C12 C11 S1 120.6(4) . . ? C16 C11 S1 119.3(4) . . ? C11 C12 C13 119.2(4) . . ? C11 C12 C17 121.5(4) . . ? C13 C12 C17 119.3(4) . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 121.5(5) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 118.4(5) . . ? C15 C16 C18 120.0(5) . . ? C11 C16 C18 121.6(5) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C26 C21 C22 120.4(4) . . ? C26 C21 S2 119.3(3) . . ? C22 C21 S2 120.2(4) . . ? C23 C22 C21 118.9(4) . . ? C23 C22 C27 118.9(4) . . ? C21 C22 C27 122.2(4) . . ? C24 C23 C22 121.1(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.9(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 118.6(4) . . ? C25 C26 C28 119.9(5) . . ? C21 C26 C28 121.5(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C36 C31 C32 118.8(4) . . ? C36 C31 P1 121.4(4) . . ? C32 C31 P1 119.7(3) . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.8(5) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C42 C41 C46 119.6(4) . . ? C42 C41 P1 122.6(3) . . ? C46 C41 P1 117.7(3) . . ? C43 C42 C41 119.6(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.7(5) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.2(5) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C41 119.9(5) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 P1 C1 C1 67.1(5) . . . 2_665 ? C41 P1 C1 C1 177.7(4) . . . 2_665 ? Pb1 P1 C1 C1 -64.8(5) . . . 2_665 ? Pb1 S1 C11 C12 80.6(4) . . . . ? Pb1 S1 C11 C16 -102.0(4) . . . . ? C16 C11 C12 C13 2.2(7) . . . . ? S1 C11 C12 C13 179.6(4) . . . . ? C16 C11 C12 C17 -176.5(4) . . . . ? S1 C11 C12 C17 1.0(6) . . . . ? C11 C12 C13 C14 -1.0(7) . . . . ? C17 C12 C13 C14 177.7(5) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C13 C14 C15 C16 2.1(8) . . . . ? C14 C15 C16 C11 -0.9(8) . . . . ? C14 C15 C16 C18 179.1(5) . . . . ? C12 C11 C16 C15 -1.2(7) . . . . ? S1 C11 C16 C15 -178.7(4) . . . . ? C12 C11 C16 C18 178.8(5) . . . . ? S1 C11 C16 C18 1.3(7) . . . . ? Pb1 S2 C21 C26 99.2(3) . . . . ? Pb1 S2 C21 C22 -84.7(3) . . . . ? C26 C21 C22 C23 -0.1(7) . . . . ? S2 C21 C22 C23 -176.2(4) . . . . ? C26 C21 C22 C27 179.1(4) . . . . ? S2 C21 C22 C27 3.1(6) . . . . ? C21 C22 C23 C24 -0.4(7) . . . . ? C27 C22 C23 C24 -179.7(5) . . . . ? C22 C23 C24 C25 -0.2(8) . . . . ? C23 C24 C25 C26 1.4(8) . . . . ? C24 C25 C26 C21 -2.0(7) . . . . ? C24 C25 C26 C28 177.9(5) . . . . ? C22 C21 C26 C25 1.3(7) . . . . ? S2 C21 C26 C25 177.4(4) . . . . ? C22 C21 C26 C28 -178.5(4) . . . . ? S2 C21 C26 C28 -2.5(6) . . . . ? C41 P1 C31 C36 -29.7(4) . . . . ? C1 P1 C31 C36 80.2(4) . . . . ? Pb1 P1 C31 C36 -152.0(3) . . . . ? C41 P1 C31 C32 152.0(4) . . . . ? C1 P1 C31 C32 -98.1(4) . . . . ? Pb1 P1 C31 C32 29.7(4) . . . . ? C36 C31 C32 C33 -0.1(7) . . . . ? P1 C31 C32 C33 178.3(4) . . . . ? C31 C32 C33 C34 -0.4(8) . . . . ? C32 C33 C34 C35 0.7(9) . . . . ? C33 C34 C35 C36 -0.4(9) . . . . ? C34 C35 C36 C31 -0.1(9) . . . . ? C32 C31 C36 C35 0.3(7) . . . . ? P1 C31 C36 C35 -178.0(4) . . . . ? C31 P1 C41 C42 110.3(4) . . . . ? C1 P1 C41 C42 -0.1(4) . . . . ? Pb1 P1 C41 C42 -120.4(4) . . . . ? C31 P1 C41 C46 -72.7(4) . . . . ? C1 P1 C41 C46 177.0(3) . . . . ? Pb1 P1 C41 C46 56.6(4) . . . . ? C46 C41 C42 C43 -0.4(7) . . . . ? P1 C41 C42 C43 176.5(4) . . . . ? C41 C42 C43 C44 -0.3(8) . . . . ? C42 C43 C44 C45 1.4(9) . . . . ? C43 C44 C45 C46 -1.7(9) . . . . ? C44 C45 C46 C41 0.9(8) . . . . ? C42 C41 C46 C45 0.2(7) . . . . ? P1 C41 C46 C45 -177.0(4) . . . . ? _refine_diff_density_max 2.037 _refine_diff_density_min -1.779 _refine_diff_density_rms 0.246