# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Khrustalev, Victor' _publ_contact_author_email vkh@xrlab.ineos.ac.ru _publ_section_title ; A new stable monomeric lead(II) dithiolate Pb(SCH2CH2NMe2)2: an interplay between dynamic flip-flop process in solution and conformational isomerism in the solid-state ; loop_ _publ_author_name V.Khrustalev R.Aysin I.Borisova A.Peregudov L.Leites ; N.Zemlyansky ; # Attachment '- PbSR2_RT.CIF' data_Pb(SR)2_RT_1 _database_code_depnum_ccdc_archive 'CCDC 764409' #TrackingRef '- PbSR2_RT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 N2 Pb S2' _chemical_formula_sum 'C8 H20 N2 Pb S2' _chemical_formula_weight 415.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.4854(8) _cell_length_b 11.0707(8) _cell_length_c 11.5937(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1345.80(17) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 2283 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 24.16 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 12.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.361 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17566 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 30.55 _reflns_number_total 4077 _reflns_number_gt 2828 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0133P)^2^+0.1173P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(9) _refine_ls_number_reflns 4077 _refine_ls_number_parameters 118 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.905505(17) 0.49700(2) 0.737911(13) 0.05726(7) Uani 1 1 d . A . S1 S 0.88081(17) 0.34852(13) 0.56376(13) 0.0686(4) Uani 1 1 d D A . S2 S 0.91641(18) 0.69548(13) 0.61349(15) 0.0746(4) Uani 1 1 d D . . N1 N 0.6584(4) 0.5016(4) 0.6981(3) 0.0653(10) Uani 1 1 d D . . N2 N 1.1499(3) 0.5177(3) 0.6933(3) 0.0615(11) Uani 1 1 d D . . C1 C 0.7093(3) 0.3550(5) 0.5422(6) 0.0840(13) Uani 1 1 d D . . H1A H 0.6922 0.3395 0.4613 0.101 Uiso 1 1 calc R A . H1B H 0.6710 0.2896 0.5859 0.101 Uiso 1 1 calc R . . C2 C 0.6419(7) 0.4718(5) 0.5755(4) 0.0840(13) Uani 1 1 d D A . H2A H 0.6752 0.5374 0.5290 0.101 Uiso 1 1 calc R . . H2B H 0.5516 0.4641 0.5589 0.101 Uiso 1 1 calc R . . C3 C 0.6017(6) 0.4159(6) 0.7807(6) 0.084(2) Uani 1 1 d D A . H3A H 0.5155 0.3986 0.7585 0.126 Uiso 1 1 calc R . . H3B H 0.6025 0.4507 0.8566 0.126 Uiso 1 1 calc R . . H3C H 0.6504 0.3424 0.7810 0.126 Uiso 1 1 calc R . . C4 C 0.6023(6) 0.6215(5) 0.7197(6) 0.0783(18) Uani 1 1 d D A . H4A H 0.5133 0.6200 0.7003 0.117 Uiso 1 1 calc R . . H4B H 0.6450 0.6807 0.6731 0.117 Uiso 1 1 calc R . . H4C H 0.6120 0.6419 0.7997 0.117 Uiso 1 1 calc R . . C5 C 1.0732(4) 0.6649(8) 0.5525(5) 0.0710(17) Uani 0.70 1 d PD A 1 H5A H 1.0664 0.5967 0.5004 0.085 Uiso 0.70 1 calc PR A 1 H5B H 1.0998 0.7343 0.5076 0.085 Uiso 0.70 1 calc PR A 1 C6 C 1.1755(7) 0.6375(4) 0.6421(5) 0.0710(17) Uani 0.70 1 d PD A 1 H6A H 1.2589 0.6377 0.6059 0.085 Uiso 0.70 1 calc PR A 1 H6B H 1.1747 0.6989 0.7018 0.085 Uiso 0.70 1 calc PR A 1 C5' C 1.0874(4) 0.7222(12) 0.6095(18) 0.0710(17) Uani 0.30 1 d PD A 2 H5C H 1.1074 0.7749 0.5451 0.085 Uiso 0.30 1 calc PR A 2 H5D H 1.1134 0.7628 0.6799 0.085 Uiso 0.30 1 calc PR A 2 C6' C 1.1614(17) 0.6046(9) 0.5972(8) 0.0710(17) Uani 0.30 1 d PD A 2 H6C H 1.1334 0.5649 0.5271 0.085 Uiso 0.30 1 calc PR A 2 H6D H 1.2509 0.6243 0.5876 0.085 Uiso 0.30 1 calc PR A 2 C7 C 1.2069(8) 0.5114(6) 0.8101(4) 0.0683(16) Uani 0.70 1 d PD A 1 H7A H 1.2982 0.5120 0.8039 0.102 Uiso 0.70 1 calc PR A 1 H7B H 1.1799 0.4382 0.8474 0.102 Uiso 0.70 1 calc PR A 1 H7C H 1.1794 0.5796 0.8546 0.102 Uiso 0.70 1 calc PR A 1 C8 C 1.2022(10) 0.4210(5) 0.6197(6) 0.0683(16) Uani 0.70 1 d PD A 1 H8A H 1.2930 0.4301 0.6139 0.102 Uiso 0.70 1 calc PR A 1 H8B H 1.1650 0.4262 0.5442 0.102 Uiso 0.70 1 calc PR A 1 H8C H 1.1826 0.3439 0.6531 0.102 Uiso 0.70 1 calc PR A 1 C7' C 1.2318(19) 0.5539(16) 0.7906(12) 0.0683(16) Uani 0.30 1 d PD A 2 H7D H 1.2950 0.6101 0.7641 0.102 Uiso 0.30 1 calc PR A 2 H7E H 1.2731 0.4839 0.8220 0.102 Uiso 0.30 1 calc PR A 2 H7F H 1.1806 0.5914 0.8492 0.102 Uiso 0.30 1 calc PR A 2 C8' C 1.185(2) 0.3951(6) 0.6532(12) 0.0683(16) Uani 0.30 1 d PD A 2 H8D H 1.2757 0.3875 0.6508 0.102 Uiso 0.30 1 calc PR A 2 H8E H 1.1502 0.3821 0.5774 0.102 Uiso 0.30 1 calc PR A 2 H8F H 1.1501 0.3362 0.7053 0.102 Uiso 0.30 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.05332(10) 0.07753(13) 0.04094(9) 0.00052(16) 0.00238(7) 0.00205(17) S1 0.0827(12) 0.0640(8) 0.0592(8) -0.0047(7) 0.0003(8) 0.0050(8) S2 0.0814(12) 0.0578(8) 0.0846(10) 0.0019(7) -0.0057(9) 0.0117(9) N1 0.054(2) 0.091(3) 0.0507(19) 0.011(4) -0.0001(17) 0.006(3) N2 0.056(2) 0.047(3) 0.082(3) 0.009(2) 0.014(2) 0.004(2) C1 0.098(4) 0.076(3) 0.079(3) -0.006(2) -0.027(3) 0.004(3) C2 0.098(4) 0.076(3) 0.079(3) -0.006(2) -0.027(3) 0.004(3) C3 0.065(4) 0.103(5) 0.085(5) 0.027(4) 0.010(4) 0.009(4) C4 0.072(4) 0.080(4) 0.083(4) 0.012(3) 0.001(4) 0.018(3) C5 0.078(4) 0.065(4) 0.070(4) 0.013(3) 0.005(3) -0.018(3) C6 0.078(4) 0.065(4) 0.070(4) 0.013(3) 0.005(3) -0.018(3) C5' 0.078(4) 0.065(4) 0.070(4) 0.013(3) 0.005(3) -0.018(3) C6' 0.078(4) 0.065(4) 0.070(4) 0.013(3) 0.005(3) -0.018(3) C7 0.056(4) 0.068(3) 0.082(3) 0.000(3) 0.011(3) -0.009(3) C8 0.056(4) 0.068(3) 0.082(3) 0.000(3) 0.011(3) -0.009(3) C7' 0.056(4) 0.068(3) 0.082(3) 0.000(3) 0.011(3) -0.009(3) C8' 0.056(4) 0.068(3) 0.082(3) 0.000(3) 0.011(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 S1 2.6164(14) . ? Pb1 N2 2.624(3) . ? Pb1 S2 2.6311(16) . ? Pb1 N1 2.632(4) . ? S1 C1 1.817(3) . ? S2 C5' 1.818(5) . ? S2 C5 1.821(5) . ? N1 C2 1.469(7) . ? N1 C4 1.473(7) . ? N1 C3 1.474(8) . ? N2 C7' 1.473(8) . ? N2 C8 1.474(7) . ? N2 C6 1.477(7) . ? N2 C6' 1.477(8) . ? N2 C8' 1.480(8) . ? N2 C7 1.481(7) . ? C1 C2 1.523(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.523(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5' C6' 1.522(8) . ? C5' H5C 0.9700 . ? C5' H5D 0.9700 . ? C6' H6C 0.9700 . ? C6' H6D 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7' H7D 0.9600 . ? C7' H7E 0.9600 . ? C7' H7F 0.9600 . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? 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 N2 89.97(9) . . ? S1 Pb1 S2 96.08(5) . . ? N2 Pb1 S2 77.09(8) . . ? S1 Pb1 N1 77.26(10) . . ? N2 Pb1 N1 157.66(11) . . ? S2 Pb1 N1 86.01(11) . . ? C1 S1 Pb1 100.33(19) . . ? C5' S2 Pb1 101.1(5) . . ? C5 S2 Pb1 95.5(2) . . ? C2 N1 C4 108.6(4) . . ? C2 N1 C3 115.9(5) . . ? C4 N1 C3 108.0(5) . . ? C2 N1 Pb1 106.4(3) . . ? C4 N1 Pb1 112.4(4) . . ? C3 N1 Pb1 105.7(3) . . ? C8 N2 C6 110.6(3) . . ? C7' N2 C6' 110.7(3) . . ? C7' N2 C8' 110.3(3) . . ? C6' N2 C8' 109.9(3) . . ? C8 N2 C7 110.2(3) . . ? C6 N2 C7 109.7(3) . . ? C7' N2 Pb1 116.2(9) . . ? C8 N2 Pb1 114.4(4) . . ? C6 N2 Pb1 109.6(3) . . ? C6' N2 Pb1 106.6(7) . . ? C8' N2 Pb1 102.8(9) . . ? C7 N2 Pb1 102.1(4) . . ? C2 C1 S1 117.2(4) . . ? C2 C1 H1A 108.0 . . ? S1 C1 H1A 108.0 . . ? C2 C1 H1B 108.0 . . ? S1 C1 H1B 108.0 . . ? H1A C1 H1B 107.2 . . ? N1 C2 C1 112.4(4) . . ? N1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? 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 . . ? C6 C5 S2 114.1(5) . . ? C6 C5 H5A 108.7 . . ? S2 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? S2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N2 C6 C5 109.0(5) . . ? N2 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N2 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6' C5' S2 111.5(10) . . ? C6' C5' H5C 109.3 . . ? S2 C5' H5C 109.3 . . ? C6' C5' H5D 109.3 . . ? S2 C5' H5D 109.3 . . ? H5C C5' H5D 108.0 . . ? N2 C6' C5' 116.4(11) . . ? N2 C6' H6C 108.2 . . ? C5' C6' H6C 108.2 . . ? N2 C6' H6D 108.2 . . ? C5' C6' H6D 108.2 . . ? H6C C6' H6D 107.3 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? N2 C7' H7D 109.5 . . ? N2 C7' H7E 109.5 . . ? H7D C7' H7E 109.5 . . ? N2 C7' H7F 109.5 . . ? H7D C7' H7F 109.5 . . ? H7E C7' H7F 109.5 . . ? N2 C8' H8D 109.5 . . ? N2 C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? N2 C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 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 N2 Pb1 S1 C1 -162.1(2) . . . . ? S2 Pb1 S1 C1 -85.1(2) . . . . ? N1 Pb1 S1 C1 -0.6(2) . . . . ? S1 Pb1 S2 C5' -99.4(6) . . . . ? N2 Pb1 S2 C5' -10.9(6) . . . . ? N1 Pb1 S2 C5' -176.2(6) . . . . ? S1 Pb1 S2 C5 -70.1(3) . . . . ? N2 Pb1 S2 C5 18.5(3) . . . . ? N1 Pb1 S2 C5 -146.8(3) . . . . ? S1 Pb1 N1 C2 -26.6(3) . . . . ? N2 Pb1 N1 C2 30.0(6) . . . . ? S2 Pb1 N1 C2 70.6(3) . . . . ? S1 Pb1 N1 C4 -145.3(3) . . . . ? N2 Pb1 N1 C4 -88.7(4) . . . . ? S2 Pb1 N1 C4 -48.1(3) . . . . ? S1 Pb1 N1 C3 97.1(4) . . . . ? N2 Pb1 N1 C3 153.7(4) . . . . ? S2 Pb1 N1 C3 -165.7(4) . . . . ? S1 Pb1 N2 C7' -156.0(8) . . . . ? S2 Pb1 N2 C7' 107.7(8) . . . . ? N1 Pb1 N2 C7' 149.5(8) . . . . ? S1 Pb1 N2 C8 -18.1(3) . . . . ? S2 Pb1 N2 C8 -114.3(3) . . . . ? N1 Pb1 N2 C8 -72.5(4) . . . . ? S1 Pb1 N2 C6 106.7(3) . . . . ? S2 Pb1 N2 C6 10.5(3) . . . . ? N1 Pb1 N2 C6 52.3(4) . . . . ? S1 Pb1 N2 C6' 80.1(6) . . . . ? S2 Pb1 N2 C6' -16.1(6) . . . . ? N1 Pb1 N2 C6' 25.6(7) . . . . ? S1 Pb1 N2 C8' -35.4(6) . . . . ? S2 Pb1 N2 C8' -131.7(6) . . . . ? N1 Pb1 N2 C8' -89.9(7) . . . . ? S1 Pb1 N2 C7 -137.0(3) . . . . ? S2 Pb1 N2 C7 126.7(3) . . . . ? N1 Pb1 N2 C7 168.5(4) . . . . ? Pb1 S1 C1 C2 29.0(5) . . . . ? C4 N1 C2 C1 174.0(5) . . . . ? C3 N1 C2 C1 -64.3(7) . . . . ? Pb1 N1 C2 C1 52.8(6) . . . . ? S1 C1 C2 N1 -59.6(7) . . . . ? Pb1 S2 C5 C6 -52.8(5) . . . . ? C8 N2 C6 C5 83.4(7) . . . . ? C7 N2 C6 C5 -154.9(5) . . . . ? Pb1 N2 C6 C5 -43.6(5) . . . . ? S2 C5 C6 N2 70.7(7) . . . . ? Pb1 S2 C5' C6' 38.8(13) . . . . ? C7' N2 C6' C5' -78.7(15) . . . . ? C8' N2 C6' C5' 159.2(15) . . . . ? Pb1 N2 C6' C5' 48.5(13) . . . . ? S2 C5' C6' N2 -63.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.775 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.094 _publ_section_references ; Bruker (2001). SAINTPlus, v. 6.2. Data Reduction and Correction Program, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package, v. 1.27. Bruker Molecular Analysis Research Tool, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2003). SADABS, v. 2.03, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). Acta Cryst. A64, 112-122. ; # Attachment '- PbSR2_LT.CIF' data_Pb(SR)2_LT_1 _database_code_depnum_ccdc_archive 'CCDC 764410' #TrackingRef '- PbSR2_LT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 N2 Pb S2' _chemical_formula_sum 'C8 H20 N2 Pb S2' _chemical_formula_weight 415.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.3938(5) _cell_length_b 10.7759(5) _cell_length_c 11.4619(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1283.76(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5545 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 30.61 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 13.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.238 _exptl_absorpt_correction_T_max 0.347 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16634 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 30.61 _reflns_number_total 3889 _reflns_number_gt 3417 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.001P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(5) _refine_ls_number_reflns 3889 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0379 _refine_ls_wR_factor_gt 0.0365 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.409954(8) 0.496398(9) 0.748019(9) 0.01451(3) Uani 1 1 d . . . S1 S 0.38752(8) 0.34671(7) 0.56812(7) 0.01828(15) Uani 1 1 d . . . S2 S 0.41940(8) 0.69799(7) 0.61788(7) 0.01887(16) Uani 1 1 d . . . N1 N 0.1627(2) 0.5047(3) 0.7025(2) 0.0165(5) Uani 1 1 d . . . N2 N 0.6550(3) 0.5182(3) 0.7043(2) 0.0162(5) Uani 1 1 d . . . C1 C 0.2129(3) 0.3514(3) 0.5456(3) 0.0204(7) Uani 1 1 d . . . H1A H 0.1949 0.3345 0.4623 0.024 Uiso 1 1 calc R . . H1B H 0.1732 0.2838 0.5917 0.024 Uiso 1 1 calc R . . C2 C 0.1486(3) 0.4732(3) 0.5790(3) 0.0189(7) Uani 1 1 d . . . H2A H 0.1862 0.5408 0.5314 0.023 Uiso 1 1 calc R . . H2B H 0.0559 0.4680 0.5600 0.023 Uiso 1 1 calc R . . C3 C 0.0990(3) 0.4124(3) 0.7800(3) 0.0237(7) Uani 1 1 d . . . H3A H 0.0076 0.4064 0.7596 0.035 Uiso 1 1 calc R . . H3B H 0.1074 0.4390 0.8614 0.035 Uiso 1 1 calc R . . H3C H 0.1399 0.3312 0.7700 0.035 Uiso 1 1 calc R . . C4 C 0.1073(3) 0.6287(3) 0.7265(3) 0.0203(7) Uani 1 1 d . . . H4A H 0.0204 0.6333 0.6938 0.030 Uiso 1 1 calc R . . H4B H 0.1615 0.6926 0.6906 0.030 Uiso 1 1 calc R . . H4C H 0.1035 0.6423 0.8110 0.030 Uiso 1 1 calc R . . C5 C 0.5769(3) 0.6657(3) 0.5531(3) 0.0210(7) Uani 1 1 d . . . H5A H 0.5692 0.5939 0.4996 0.025 Uiso 1 1 calc R . . H5B H 0.6046 0.7383 0.5065 0.025 Uiso 1 1 calc R . . C6 C 0.6774(3) 0.6379(3) 0.6433(3) 0.0179(6) Uani 1 1 d . . . H6A H 0.7628 0.6355 0.6052 0.022 Uiso 1 1 calc R . . H6B H 0.6785 0.7057 0.7015 0.022 Uiso 1 1 calc R . . C7 C 0.7175(3) 0.5187(3) 0.8184(3) 0.0196(7) Uani 1 1 d . . . H7A H 0.8102 0.5312 0.8085 0.029 Uiso 1 1 calc R . . H7B H 0.7021 0.4392 0.8575 0.029 Uiso 1 1 calc R . . H7C H 0.6820 0.5861 0.8659 0.029 Uiso 1 1 calc R . . C8 C 0.7008(3) 0.4127(3) 0.6332(3) 0.0205(7) Uani 1 1 d . . . H8A H 0.7943 0.4184 0.6236 0.031 Uiso 1 1 calc R . . H8B H 0.6594 0.4151 0.5564 0.031 Uiso 1 1 calc R . . H8C H 0.6792 0.3346 0.6724 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01380(5) 0.01912(5) 0.01061(5) 0.00025(8) 0.00060(5) 0.00021(5) S1 0.0194(4) 0.0193(3) 0.0162(3) -0.0028(3) -0.0005(3) 0.0011(3) S2 0.0198(4) 0.0174(3) 0.0194(4) 0.0018(3) -0.0004(3) 0.0023(3) N1 0.0154(12) 0.0210(12) 0.0130(10) 0.0023(12) 0.0018(9) 0.0021(12) N2 0.0166(13) 0.0153(13) 0.0168(11) -0.0010(10) 0.0022(10) -0.0026(11) C1 0.0206(17) 0.0220(15) 0.0184(15) -0.0025(13) -0.0056(13) 0.0007(13) C2 0.0179(15) 0.0205(16) 0.0184(15) -0.0001(11) -0.0057(12) 0.0037(12) C3 0.0163(17) 0.0273(16) 0.0273(18) 0.0080(12) 0.0003(14) 0.0028(14) C4 0.0183(16) 0.0229(14) 0.0197(17) -0.0007(11) 0.0005(13) 0.0053(12) C5 0.0225(17) 0.0209(15) 0.0196(15) 0.0025(12) 0.0026(13) -0.0021(13) C6 0.0149(16) 0.0206(15) 0.0183(15) 0.0019(12) 0.0034(12) -0.0036(13) C7 0.0201(16) 0.0194(17) 0.0193(14) -0.0026(12) -0.0056(12) -0.0018(14) C8 0.0198(18) 0.0224(16) 0.0193(17) -0.0057(13) 0.0011(14) 0.0018(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 Pb1 N2 2.607(3) . ? Pb1 N1 2.623(2) . ? Pb1 S1 2.6283(8) . ? Pb1 S2 2.6370(8) . ? S1 C1 1.834(4) . ? S2 C5 1.831(3) . ? N1 C2 1.464(4) . ? N1 C4 1.481(4) . ? N1 C3 1.489(4) . ? N2 C7 1.460(4) . ? N2 C8 1.478(4) . ? N2 C6 1.485(4) . ? C1 C2 1.522(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 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 C6 1.499(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pb1 N1 156.33(8) . . ? N2 Pb1 S1 89.49(6) . . ? N1 Pb1 S1 77.18(6) . . ? N2 Pb1 S2 77.33(6) . . ? N1 Pb1 S2 84.03(6) . . ? S1 Pb1 S2 93.73(2) . . ? C1 S1 Pb1 100.44(11) . . ? C5 S2 Pb1 96.08(10) . . ? C2 N1 C4 110.4(2) . . ? C2 N1 C3 112.2(3) . . ? C4 N1 C3 108.6(2) . . ? C2 N1 Pb1 106.41(18) . . ? C4 N1 Pb1 112.0(2) . . ? C3 N1 Pb1 107.15(18) . . ? C7 N2 C8 110.7(3) . . ? C7 N2 C6 110.4(3) . . ? C8 N2 C6 111.0(3) . . ? C7 N2 Pb1 105.22(18) . . ? C8 N2 Pb1 110.59(19) . . ? C6 N2 Pb1 108.77(18) . . ? C2 C1 S1 115.0(2) . . ? C2 C1 H1A 108.5 . . ? S1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? S1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 113.5(3) . . ? N1 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? 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 . . ? C6 C5 S2 112.4(2) . . ? C6 C5 H5A 109.1 . . ? S2 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? S2 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C5 112.9(3) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 N2 Pb1 S1 C1 -162.76(13) . . . . ? N1 Pb1 S1 C1 -2.48(13) . . . . ? S2 Pb1 S1 C1 -85.49(11) . . . . ? N2 Pb1 S2 C5 20.06(12) . . . . ? N1 Pb1 S2 C5 -145.26(12) . . . . ? S1 Pb1 S2 C5 -68.58(11) . . . . ? N2 Pb1 N1 C2 32.2(3) . . . . ? S1 Pb1 N1 C2 -25.04(19) . . . . ? S2 Pb1 N1 C2 70.2(2) . . . . ? N2 Pb1 N1 C4 -88.6(3) . . . . ? S1 Pb1 N1 C4 -145.82(19) . . . . ? S2 Pb1 N1 C4 -50.60(18) . . . . ? N2 Pb1 N1 C3 152.4(2) . . . . ? S1 Pb1 N1 C3 95.18(19) . . . . ? S2 Pb1 N1 C3 -169.60(19) . . . . ? N1 Pb1 N2 C7 164.2(2) . . . . ? S1 Pb1 N2 C7 -140.7(2) . . . . ? S2 Pb1 N2 C7 125.4(2) . . . . ? N1 Pb1 N2 C8 -76.2(3) . . . . ? S1 Pb1 N2 C8 -21.1(2) . . . . ? S2 Pb1 N2 C8 -115.1(2) . . . . ? N1 Pb1 N2 C6 45.9(3) . . . . ? S1 Pb1 N2 C6 100.98(18) . . . . ? S2 Pb1 N2 C6 7.04(18) . . . . ? Pb1 S1 C1 C2 31.0(2) . . . . ? C4 N1 C2 C1 175.4(3) . . . . ? C3 N1 C2 C1 -63.3(3) . . . . ? Pb1 N1 C2 C1 53.6(3) . . . . ? S1 C1 C2 N1 -61.4(3) . . . . ? Pb1 S2 C5 C6 -51.8(2) . . . . ? C7 N2 C6 C5 -156.3(3) . . . . ? C8 N2 C6 C5 80.5(3) . . . . ? Pb1 N2 C6 C5 -41.3(3) . . . . ? S2 C5 C6 N2 68.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.412 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.104 _publ_section_references ; Bruker (2001). SAINTPlus, v. 6.2. Data Reduction and Correction Program, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package, v. 1.27. Bruker Molecular Analysis Research Tool, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2003). SADABS, v. 2.03, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). Acta Cryst. A64, 112-122. ; # Attachment '- PBSR2_HT.CIF' data_Pb(SR)2_HT _database_code_depnum_ccdc_archive 'CCDC 780360' #TrackingRef '- PBSR2_HT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 N2 Pb S2' _chemical_formula_sum 'C8 H20 N2 Pb S2' _chemical_formula_weight 415.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.541(11) _cell_length_b 11.148(12) _cell_length_c 11.645(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1368(2) _cell_formula_units_Z 4 _cell_measurement_temperature 333(2) _cell_measurement_reflns_used 2666 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 22.33 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 12.605 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.264 _exptl_absorpt_correction_T_max 0.383 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 333(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17933 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.71 _reflns_number_total 4204 _reflns_number_gt 2346 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.056P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.066(16) _chemical_absolute_configuration ad _refine_ls_number_reflns 4204 _refine_ls_number_parameters 124 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.90313(3) 0.49670(4) 0.73441(2) 0.08878(15) Uani 1 1 d . A . S1 S 0.8786(3) 0.3494(2) 0.5618(3) 0.1050(8) Uani 1 1 d D A . S2 S 0.9145(3) 0.6943(2) 0.6126(3) 0.1160(9) Uani 1 1 d D . . N1 N 0.6555(6) 0.4996(8) 0.6956(5) 0.101(2) Uani 1 1 d D . . N2 N 1.1474(5) 0.5169(6) 0.6890(5) 0.094(2) Uani 1 1 d D . . C1 C 0.7089(5) 0.3579(9) 0.5406(13) 0.136(4) Uani 1 1 d D . . H1A H 0.6922 0.3425 0.4600 0.163 Uiso 1 1 calc R A . H1B H 0.6705 0.2929 0.5837 0.163 Uiso 1 1 calc R . . C2 C 0.6397(10) 0.4731(9) 0.5729(6) 0.118(4) Uani 1 1 d D A . H2A H 0.6729 0.5392 0.5279 0.141 Uiso 1 1 calc R . . H2B H 0.5502 0.4648 0.5555 0.141 Uiso 1 1 calc R . . C3 C 0.5987(11) 0.4178(11) 0.7803(11) 0.121(4) Uani 1 1 d D A . H3A H 0.5104 0.4368 0.7897 0.181 Uiso 1 1 calc R . . H3B H 0.6414 0.4266 0.8526 0.181 Uiso 1 1 calc R . . H3C H 0.6070 0.3366 0.7541 0.181 Uiso 1 1 calc R . . C4 C 0.5992(11) 0.6179(9) 0.7179(11) 0.118(4) Uani 1 1 d D A . H4A H 0.5109 0.6165 0.6976 0.177 Uiso 1 1 calc R . . H4B H 0.6421 0.6774 0.6727 0.177 Uiso 1 1 calc R . . H4C H 0.6078 0.6371 0.7979 0.177 Uiso 1 1 calc R . . C5 C 1.0701(7) 0.6674(17) 0.5524(12) 0.110(4) Uani 0.60 1 d PD A 1 H5A H 1.0647 0.6014 0.4984 0.132 Uiso 0.60 1 calc PR A 1 H5B H 1.0968 0.7381 0.5103 0.132 Uiso 0.60 1 calc PR A 1 C6 C 1.1701(15) 0.6378(7) 0.6427(10) 0.110(4) Uani 0.60 1 d PD A 1 H6A H 1.2539 0.6415 0.6084 0.132 Uiso 0.60 1 calc PR A 1 H6B H 1.1665 0.6963 0.7043 0.132 Uiso 0.60 1 calc PR A 1 C5' C 1.0837(5) 0.7212(17) 0.615(3) 0.110(4) Uani 0.40 1 d PD A 2 H5C H 1.1053 0.7782 0.5551 0.132 Uiso 0.40 1 calc PR A 2 H5D H 1.1069 0.7563 0.6882 0.132 Uiso 0.40 1 calc PR A 2 C6' C 1.159(2) 0.6063(13) 0.5968(12) 0.110(4) Uani 0.40 1 d PD A 2 H6C H 1.1323 0.5698 0.5253 0.132 Uiso 0.40 1 calc PR A 2 H6D H 1.2483 0.6272 0.5887 0.132 Uiso 0.40 1 calc PR A 2 C7 C 1.1999(18) 0.5057(12) 0.8055(8) 0.101(3) Uani 0.60 1 d PD A 1 H7A H 1.2900 0.5179 0.8031 0.152 Uiso 0.60 1 calc PR A 1 H7B H 1.1820 0.4271 0.8349 0.152 Uiso 0.60 1 calc PR A 1 H7C H 1.1618 0.5649 0.8545 0.152 Uiso 0.60 1 calc PR A 1 C8 C 1.199(2) 0.4244(10) 0.6124(11) 0.101(3) Uani 0.60 1 d PD A 1 H8A H 1.2856 0.4441 0.5933 0.152 Uiso 0.60 1 calc PR A 1 H8B H 1.1497 0.4208 0.5434 0.152 Uiso 0.60 1 calc PR A 1 H8C H 1.1970 0.3480 0.6503 0.152 Uiso 0.60 1 calc PR A 1 C7' C 1.217(3) 0.554(2) 0.7923(15) 0.101(3) Uani 0.40 1 d PD A 2 H7D H 1.2423 0.6364 0.7846 0.152 Uiso 0.40 1 calc PR A 2 H7E H 1.2904 0.5045 0.8016 0.152 Uiso 0.40 1 calc PR A 2 H7F H 1.1627 0.5458 0.8582 0.152 Uiso 0.40 1 calc PR A 2 C8' C 1.189(3) 0.3980(10) 0.6495(17) 0.101(3) Uani 0.40 1 d PD A 2 H8D H 1.2740 0.4036 0.6197 0.152 Uiso 0.40 1 calc PR A 2 H8E H 1.1334 0.3699 0.5903 0.152 Uiso 0.40 1 calc PR A 2 H8F H 1.1880 0.3428 0.7128 0.152 Uiso 0.40 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0877(2) 0.1077(3) 0.07084(18) 0.0001(3) 0.00342(12) 0.0020(3) S1 0.122(2) 0.0929(15) 0.1002(17) -0.0081(13) -0.0004(15) 0.0028(15) S2 0.125(2) 0.0896(17) 0.134(2) 0.0022(15) -0.0081(19) 0.0163(17) N1 0.083(4) 0.133(6) 0.088(4) 0.023(7) -0.002(3) 0.014(6) N2 0.088(4) 0.079(5) 0.115(5) 0.010(5) 0.012(4) 0.001(4) C1 0.152(10) 0.103(8) 0.152(10) 0.000(7) -0.054(9) -0.017(8) C2 0.112(7) 0.132(10) 0.108(7) -0.004(6) -0.027(5) 0.021(7) C3 0.099(8) 0.147(10) 0.116(9) 0.034(7) 0.014(7) -0.007(7) C4 0.096(7) 0.138(9) 0.119(9) 0.012(7) 0.010(7) 0.028(6) C5 0.118(8) 0.099(8) 0.112(10) 0.012(6) 0.012(7) -0.023(6) C6 0.118(8) 0.099(8) 0.112(10) 0.012(6) 0.012(7) -0.023(6) C5' 0.118(8) 0.099(8) 0.112(10) 0.012(6) 0.012(7) -0.023(6) C6' 0.118(8) 0.099(8) 0.112(10) 0.012(6) 0.012(7) -0.023(6) C7 0.100(6) 0.089(7) 0.115(7) -0.009(7) 0.009(6) -0.016(7) C8 0.100(6) 0.089(7) 0.115(7) -0.009(7) 0.009(6) -0.016(7) C7' 0.100(6) 0.089(7) 0.115(7) -0.009(7) 0.009(6) -0.016(7) C8' 0.100(6) 0.089(7) 0.115(7) -0.009(7) 0.009(6) -0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 S1 2.608(3) . ? Pb1 S2 2.623(4) . ? Pb1 N2 2.638(6) . ? Pb1 N1 2.649(7) . ? S1 C1 1.809(8) . ? S2 C5' 1.809(9) . ? S2 C5 1.809(11) . ? N1 C2 1.468(12) . ? N1 C4 1.470(13) . ? N1 C3 1.471(12) . ? N2 C7' 1.468(14) . ? N2 C6' 1.469(13) . ? N2 C8 1.470(11) . ? N2 C7 1.471(12) . ? N2 C6 1.471(11) . ? N2 C8' 1.472(13) . ? C1 C2 1.524(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.524(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5' C6' 1.524(12) . ? C5' H5C 0.9700 . ? C5' H5D 0.9700 . ? C6' H6C 0.9700 . ? C6' H6D 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7' H7D 0.9600 . ? C7' H7E 0.9600 . ? C7' H7F 0.9600 . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? 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 96.71(13) . . ? S1 Pb1 N2 89.76(17) . . ? S2 Pb1 N2 77.00(15) . . ? S1 Pb1 N1 77.22(18) . . ? S2 Pb1 N1 86.71(19) . . ? N2 Pb1 N1 157.9(2) . . ? C1 S1 Pb1 99.8(4) . . ? C5' S2 Pb1 100.1(8) . . ? C5 S2 Pb1 96.4(5) . . ? C2 N1 C4 107.8(8) . . ? C2 N1 C3 118.8(10) . . ? C4 N1 C3 105.9(9) . . ? C2 N1 Pb1 106.0(5) . . ? C4 N1 Pb1 112.2(6) . . ? C3 N1 Pb1 106.2(6) . . ? C7' N2 C6' 111.3(3) . . ? C7' N2 C8 120.7(19) . . ? C6' N2 C8 90.0(9) . . ? C6' N2 C7 134.3(10) . . ? C8 N2 C7 111.1(3) . . ? C7' N2 C6 87.7(9) . . ? C8 N2 C6 111.1(3) . . ? C7 N2 C6 110.8(3) . . ? C7' N2 C8' 111.2(3) . . ? C6' N2 C8' 110.9(3) . . ? C7 N2 C8' 95.6(13) . . ? C6 N2 C8' 131.5(11) . . ? C7' N2 Pb1 110.2(13) . . ? C6' N2 Pb1 106.8(10) . . ? C8 N2 Pb1 115.2(10) . . ? C7 N2 Pb1 100.1(8) . . ? C6 N2 Pb1 108.1(7) . . ? C8' N2 Pb1 106.2(13) . . ? C2 C1 S1 118.9(7) . . ? C2 C1 H1A 107.6 . . ? S1 C1 H1A 107.6 . . ? C2 C1 H1B 107.6 . . ? S1 C1 H1B 107.6 . . ? H1A C1 H1B 107.0 . . ? N1 C2 C1 110.9(9) . . ? N1 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? 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 . . ? C6 C5 S2 113.3(10) . . ? C6 C5 H5A 108.9 . . ? S2 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? S2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 C5 109.7(10) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6' C5' S2 112.0(14) . . ? C6' C5' H5C 109.2 . . ? S2 C5' H5C 109.2 . . ? C6' C5' H5D 109.2 . . ? S2 C5' H5D 109.2 . . ? H5C C5' H5D 107.9 . . ? N2 C6' C5' 115.1(16) . . ? N2 C6' H6C 108.5 . . ? C5' C6' H6C 108.5 . . ? N2 C6' H6D 108.5 . . ? C5' C6' H6D 108.5 . . ? H6C C6' H6D 107.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? N2 C7' H7D 109.5 . . ? N2 C7' H7E 109.5 . . ? H7D C7' H7E 109.5 . . ? N2 C7' H7F 109.5 . . ? H7D C7' H7F 109.5 . . ? H7E C7' H7F 109.5 . . ? N2 C8' H8D 109.5 . . ? N2 C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? N2 C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 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 S2 Pb1 S1 C1 -84.5(5) . . . . ? N2 Pb1 S1 C1 -161.4(5) . . . . ? N1 Pb1 S1 C1 0.5(5) . . . . ? S1 Pb1 S2 C5' -101.4(9) . . . . ? N2 Pb1 S2 C5' -13.2(9) . . . . ? N1 Pb1 S2 C5' -178.1(9) . . . . ? S1 Pb1 S2 C5 -70.7(6) . . . . ? N2 Pb1 S2 C5 17.5(6) . . . . ? N1 Pb1 S2 C5 -147.4(6) . . . . ? S1 Pb1 N1 C2 -28.2(6) . . . . ? S2 Pb1 N1 C2 69.5(7) . . . . ? N2 Pb1 N1 C2 27.1(10) . . . . ? S1 Pb1 N1 C4 -145.6(7) . . . . ? S2 Pb1 N1 C4 -48.0(6) . . . . ? N2 Pb1 N1 C4 -90.3(8) . . . . ? S1 Pb1 N1 C3 99.1(8) . . . . ? S2 Pb1 N1 C3 -163.3(7) . . . . ? N2 Pb1 N1 C3 154.4(8) . . . . ? S1 Pb1 N2 C7' -156.5(9) . . . . ? S2 Pb1 N2 C7' 106.6(9) . . . . ? N1 Pb1 N2 C7' 150.2(11) . . . . ? S1 Pb1 N2 C6' 82.4(8) . . . . ? S2 Pb1 N2 C6' -14.5(8) . . . . ? N1 Pb1 N2 C6' 29.1(10) . . . . ? S1 Pb1 N2 C8 -15.7(6) . . . . ? S2 Pb1 N2 C8 -112.7(6) . . . . ? N1 Pb1 N2 C8 -69.0(8) . . . . ? S1 Pb1 N2 C7 -134.9(6) . . . . ? S2 Pb1 N2 C7 128.1(6) . . . . ? N1 Pb1 N2 C7 171.8(8) . . . . ? S1 Pb1 N2 C6 109.2(5) . . . . ? S2 Pb1 N2 C6 12.2(5) . . . . ? N1 Pb1 N2 C6 55.9(8) . . . . ? S1 Pb1 N2 C8' -36.0(8) . . . . ? S2 Pb1 N2 C8' -132.9(8) . . . . ? N1 Pb1 N2 C8' -89.3(10) . . . . ? Pb1 S1 C1 C2 28.7(11) . . . . ? C4 N1 C2 C1 173.7(9) . . . . ? C3 N1 C2 C1 -66.0(12) . . . . ? Pb1 N1 C2 C1 53.3(10) . . . . ? S1 C1 C2 N1 -60.2(14) . . . . ? C5' S2 C5 C6 47.5(17) . . . . ? Pb1 S2 C5 C6 -51.6(11) . . . . ? C7' N2 C6 C5 -156.4(17) . . . . ? C6' N2 C6 C5 45(2) . . . . ? C8 N2 C6 C5 81.5(12) . . . . ? C7 N2 C6 C5 -154.6(11) . . . . ? C8' N2 C6 C5 87(2) . . . . ? Pb1 N2 C6 C5 -45.8(10) . . . . ? S2 C5 C6 N2 71.7(14) . . . . ? C5 S2 C5' C6' -43.0(12) . . . . ? Pb1 S2 C5' C6' 42.4(19) . . . . ? C7' N2 C6' C5' -73(2) . . . . ? C8 N2 C6' C5' 163.6(19) . . . . ? C7 N2 C6' C5' -76(2) . . . . ? C6 N2 C6' C5' -49.8(19) . . . . ? C8' N2 C6' C5' 162(2) . . . . ? Pb1 N2 C6' C5' 47.2(18) . . . . ? S2 C5' C6' N2 -66(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.71 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.909 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.140 _publ_section_references ; Bruker (2001). SAINTPlus, v. 6.2. Data Reduction and Correction Program, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package, v. 1.27. Bruker Molecular Analysis Research Tool, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). Acta Cryst. A64, 112-122. ;