# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Qichun Zhang' _publ_contact_author_email qczhang@ntu.edu.sg _publ_section_title ; In situ Formation of New Organic Ligands to Construct Two Novel Pb(II)-based Frameworks with Ligand-to-metal Charge Transfer ; _publ_author_name 'Qichun Zhang' # Attachment '- compound-1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 836172' #TrackingRef '- compound-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H7 Cl2 N O5 Pb' _chemical_formula_weight 487.25 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.1370(16) _cell_length_b 14.468(3) _cell_length_c 10.377(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1221.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 14.258 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.05 _exptl_absorpt_correction_T_max 0.08 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8992 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 34.72 _reflns_number_total 2553 _reflns_number_gt 1911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPERP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. There are some hydrogen atoms coming from DMF molecule,which have low scattering power. Some _refine_ls_number_restraints were used when sovled and refine the structure, which ensures that a sensible geometry is retained.At the same time,ISOR, BOND$H and AFIX were used in SHELXL.ins file. ; _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^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2553 _refine_ls_number_parameters 100 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.988 _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 0.20337(2) 0.7500 0.687081(15) 0.03101(7) Uani 1 2 d SU . . Cl1 Cl -0.32236(16) 0.51429(10) 0.66912(11) 0.0586(3) Uani 1 1 d U . . N1 N 0.1126(8) 0.7500 1.1084(5) 0.0592(14) Uani 1 2 d SU . . C3 C 0.1225(5) 0.5721(2) 0.5010(3) 0.0359(7) Uani 1 1 d U . . C5 C -0.0337(5) 0.5782(2) 0.5826(3) 0.0356(7) Uani 1 1 d U . . C4 C -0.1452(5) 0.5062(3) 0.5778(3) 0.0385(7) Uani 1 1 d U . . C2 C 0.0533(12) 0.7088(6) 1.0072(8) 0.052(2) Uani 0.50 1 d PU . . H2A H 0.0379 0.6431 1.0099 0.062 Uiso 0.50 1 d PR . . C1A C 0.138(2) 0.6577(10) 1.1170(15) 0.098(4) Uani 0.50 1 d PU . . H1AA H 0.1257 0.6300 1.0335 0.148 Uiso 0.50 1 d PR . . H1AB H 0.2456 0.6450 1.1498 0.148 Uiso 0.50 1 d PR . . H1AC H 0.0569 0.6324 1.1745 0.148 Uiso 0.50 1 d PR . . O3 O 0.0183(6) 0.7500 0.9068(3) 0.0504(10) Uani 1 2 d SU . . O1 O -0.0481(4) 0.64913(17) 0.6499(3) 0.0429(6) Uani 1 1 d U . . O2 O 0.2192(4) 0.6374(2) 0.5076(3) 0.0515(8) Uani 1 1 d U . . C1B C 0.153(2) 0.6898(12) 1.2253(14) 0.103(4) Uani 0.50 1 d PU . . H1BA H 0.1608 0.7292 1.2995 0.155 Uiso 0.50 1 d PR . . H1BB H 0.0671 0.6455 1.2380 0.155 Uiso 0.50 1 d PR . . H1BC H 0.2558 0.6581 1.2133 0.155 Uiso 0.50 1 d PR . . 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 0.03945(12) 0.02710(9) 0.02647(11) 0.000 -0.00033(6) 0.000 Cl1 0.0575(7) 0.0571(7) 0.0614(7) -0.0204(5) 0.0214(5) -0.0049(5) N1 0.063(4) 0.077(4) 0.038(3) 0.000 -0.007(2) 0.000 C3 0.043(2) 0.0334(15) 0.0312(16) -0.0074(13) 0.0006(15) -0.0015(15) C5 0.0436(19) 0.0312(14) 0.0321(16) -0.0072(12) -0.0059(14) 0.0045(15) C4 0.0407(18) 0.0374(17) 0.0374(18) -0.0105(14) 0.0066(15) -0.0007(16) C2 0.065(5) 0.050(4) 0.040(4) -0.003(3) -0.006(4) -0.003(4) C1A 0.126(8) 0.084(7) 0.086(7) 0.009(6) -0.016(7) 0.009(7) O3 0.053(2) 0.069(3) 0.0298(18) 0.000 -0.0041(16) 0.000 O1 0.0466(16) 0.0339(12) 0.0481(13) -0.0172(11) 0.0010(12) 0.0029(12) O2 0.062(2) 0.0436(15) 0.0485(17) -0.0181(13) 0.0147(13) -0.0177(14) C1B 0.112(8) 0.123(9) 0.075(6) 0.028(7) -0.031(7) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O2 2.478(3) . ? Pb1 O2 2.478(3) 7_575 ? Pb1 O1 2.543(3) . ? Pb1 O1 2.543(3) 7_575 ? Pb1 O3 2.732(4) . ? Pb1 O3 2.741(4) 6_657 ? Cl1 C4 1.729(4) . ? N1 C2 1.300(9) . ? N1 C2 1.300(9) 7_575 ? N1 C1A 1.354(14) 7_575 ? N1 C1A 1.354(14) . ? N1 C1B 1.530(15) 7_575 ? N1 C1B 1.530(15) . ? C3 O2 1.232(4) . ? C3 C4 1.409(5) 5_566 ? C3 C5 1.530(5) . ? C5 O1 1.247(4) . ? C5 C4 1.382(5) . ? C4 C3 1.409(5) 5_566 ? C2 C2 1.191(17) 7_575 ? C2 O3 1.233(9) . ? C2 C1A 1.523(17) . ? C2 H2A 0.9600 . ? C2 H1AA 1.3133 . ? C1A C1B 1.22(2) . ? C1A H2A 1.3922 . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9599 . ? C1A H1AC 0.9600 . ? C1A H1BB 1.3918 . ? C1A H1BC 1.3865 . ? O3 C2 1.233(9) 7_575 ? O3 Pb1 2.741(4) 6_557 ? C1B C1B 1.74(4) 7_575 ? C1B H1AB 1.2645 . ? C1B H1AC 1.2585 . ? C1B H1BA 0.9600 . ? C1B H1BB 0.9599 . ? C1B H1BC 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 O2 Pb1 O2 82.24(16) . 7_575 ? O2 Pb1 O1 63.28(9) . . ? O2 Pb1 O1 107.77(11) 7_575 . ? O2 Pb1 O1 107.77(11) . 7_575 ? O2 Pb1 O1 63.28(9) 7_575 7_575 ? O1 Pb1 O1 70.04(12) . 7_575 ? O2 Pb1 O3 130.98(8) . . ? O2 Pb1 O3 130.98(8) 7_575 . ? O1 Pb1 O3 71.52(9) . . ? O1 Pb1 O3 71.52(9) 7_575 . ? O2 Pb1 O3 71.60(9) . 6_657 ? O2 Pb1 O3 71.60(9) 7_575 6_657 ? O1 Pb1 O3 134.29(7) . 6_657 ? O1 Pb1 O3 134.29(7) 7_575 6_657 ? O3 Pb1 O3 144.26(12) . 6_657 ? C2 N1 C2 54.5(8) . 7_575 ? C2 N1 C1A 124.1(8) . 7_575 ? C2 N1 C1A 70.0(8) 7_575 7_575 ? C2 N1 C1A 70.0(8) . . ? C2 N1 C1A 124.1(8) 7_575 . ? C1A N1 C1A 161.1(17) 7_575 . ? C2 N1 C1B 169.0(9) . 7_575 ? C2 N1 C1B 117.4(8) 7_575 7_575 ? C1A N1 C1B 49.7(10) 7_575 7_575 ? C1A N1 C1B 118.4(10) . 7_575 ? C2 N1 C1B 117.4(8) . . ? C2 N1 C1B 169.0(9) 7_575 . ? C1A N1 C1B 118.4(10) 7_575 . ? C1A N1 C1B 49.7(10) . . ? C1B N1 C1B 69.4(13) 7_575 . ? O2 C3 C4 124.5(3) . 5_566 ? O2 C3 C5 117.1(3) . . ? C4 C3 C5 118.5(3) 5_566 . ? O1 C5 C4 125.3(3) . . ? O1 C5 C3 115.9(3) . . ? C4 C5 C3 118.8(3) . . ? C5 C4 C3 122.7(3) . 5_566 ? C5 C4 Cl1 118.5(3) . . ? C3 C4 Cl1 118.8(3) 5_566 . ? C2 C2 O3 61.1(4) 7_575 . ? C2 C2 N1 62.7(4) 7_575 . ? O3 C2 N1 123.2(7) . . ? C2 C2 C1A 119.1(7) 7_575 . ? O3 C2 C1A 166.2(11) . . ? N1 C2 C1A 56.7(7) . . ? C2 C2 H2A 172.3 7_575 . ? O3 C2 H2A 118.2 . . ? N1 C2 H2A 118.6 . . ? C1A C2 H2A 63.6 . . ? C2 C2 H1AA 150.4 7_575 . ? O3 C2 H1AA 134.3 . . ? N1 C2 H1AA 93.7 . . ? C1A C2 H1AA 38.7 . . ? H2A C2 H1AA 36.0 . . ? C1B C1A N1 72.6(12) . . ? C1B C1A C2 123.3(14) . . ? N1 C1A C2 53.3(6) . . ? C1B C1A H2A 148.4 . . ? N1 C1A H2A 90.5 . . ? C2 C1A H2A 38.1 . . ? C1B C1A H1AA 177.7 . . ? N1 C1A H1AA 109.7 . . ? C2 C1A H1AA 58.8 . . ? H2A C1A H1AA 32.5 . . ? C1B C1A H1AB 69.6 . . ? N1 C1A H1AB 110.4 . . ? C2 C1A H1AB 140.4 . . ? H2A C1A H1AB 142.0 . . ? H1AA C1A H1AB 109.5 . . ? C1B C1A H1AC 69.2 . . ? N1 C1A H1AC 108.3 . . ? C2 C1A H1AC 110.0 . . ? H2A C1A H1AC 92.3 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C1B C1A H1BB 42.5 . . ? N1 C1A H1BB 97.0 . . ? C2 C1A H1BB 123.4 . . ? H2A C1A H1BB 117.4 . . ? H1AA C1A H1BB 136.1 . . ? H1AB C1A H1BB 91.9 . . ? H1AC C1A H1BB 26.9 . . ? C1B C1A H1BC 42.6 . . ? N1 C1A H1BC 98.5 . . ? C2 C1A H1BC 148.1 . . ? H2A C1A H1BC 168.6 . . ? H1AA C1A H1BC 136.3 . . ? H1AB C1A H1BC 27.2 . . ? H1AC C1A H1BC 91.6 . . ? H1BB C1A H1BC 68.7 . . ? C2 O3 C2 57.7(8) 7_575 . ? C2 O3 Pb1 125.3(5) 7_575 . ? C2 O3 Pb1 125.3(5) . . ? C2 O3 Pb1 121.1(5) 7_575 6_557 ? C2 O3 Pb1 121.1(5) . 6_557 ? Pb1 O3 Pb1 102.63(11) . 6_557 ? C5 O1 Pb1 118.8(2) . . ? C3 O2 Pb1 120.9(2) . . ? C1A C1B N1 57.7(9) . . ? C1A C1B C1B 112.4(10) . 7_575 ? N1 C1B C1B 55.3(7) . 7_575 ? C1A C1B H1AB 45.4 . . ? N1 C1B H1AB 85.9 . . ? C1B C1B H1AB 120.8 7_575 . ? C1A C1B H1AC 45.5 . . ? N1 C1B H1AC 84.8 . . ? C1B C1B H1AC 131.3 7_575 . ? H1AB C1B H1AC 76.8 . . ? C1A C1B H1BA 165.8 . . ? N1 C1B H1BA 108.2 . . ? C1B C1B H1BA 53.6 7_575 . ? H1AB C1B H1BA 139.8 . . ? H1AC C1B H1BA 140.1 . . ? C1A C1B H1BB 78.2 . . ? N1 C1B H1BB 109.3 . . ? C1B C1B H1BB 132.0 7_575 . ? H1AB C1B H1BB 100.2 . . ? H1AC C1B H1BB 32.9 . . ? H1BA C1B H1BB 109.5 . . ? C1A C1B H1BC 77.8 . . ? N1 C1B H1BC 110.9 . . ? C1B C1B H1BC 118.5 7_575 . ? H1AB C1B H1BC 32.7 . . ? H1AC C1B H1BC 99.9 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 34.72 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.394 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.165 # Attachment '- compound-2.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 836173' #TrackingRef '- compound-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 N2 O5 Pb S' _chemical_formula_weight 551.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.550(3) _cell_length_b 8.9600(18) _cell_length_c 13.820(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.16(3) _cell_angle_gamma 90.00 _cell_volume 1656.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 10.341 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.45 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11739 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3783 _reflns_number_gt 2970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPERP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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.There are some hydrogen atoms coming from DMF molecule,which have low scattering power. Some _refine_ls_number_restraints were used when sovled and refine the structure, which ensures that a sensible geometry is retained.At the same time, ISOR, BOND$H and AFIX were used in SHELXL.ins file when solved the structure. ; _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^)+(0.0729P)^2^+9.5687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 3783 _refine_ls_number_parameters 228 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.019 _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 0.64652(2) 0.05023(3) 0.49958(2) 0.03657(13) Uani 1 1 d U . . N2 N 0.9629(6) 0.1662(14) 0.4004(6) 0.066(3) Uani 1 1 d U . . N1 N 0.9272(8) -0.3731(15) 0.3627(9) 0.090(4) Uani 1 1 d U . . S1 S 0.40468(16) -0.2167(3) 0.19374(16) 0.0438(5) Uani 1 1 d U . . O3 O 0.5384(5) -0.1009(8) 0.3695(5) 0.0481(15) Uani 1 1 d U . . O2 O 0.7283(5) -0.1569(8) 0.4326(5) 0.0529(16) Uani 1 1 d U . . O1 O 0.8170(6) 0.1385(13) 0.4569(7) 0.088(3) Uani 1 1 d U . . C16 C 0.5837(6) -0.1811(9) 0.3174(5) 0.0342(16) Uani 1 1 d U . . C13 C 0.5338(6) -0.2467(10) 0.2297(6) 0.0401(18) Uani 1 1 d U . . C12 C 0.6934(6) -0.2136(10) 0.3541(6) 0.0396(18) Uani 1 1 d U . . C11 C 0.7440(6) -0.3042(10) 0.2957(6) 0.0419(19) Uani 1 1 d U . . C10 C 0.4037(8) -0.4068(12) 0.3540(8) 0.055(2) Uani 1 1 d U . . H10A H 0.4712 -0.4239 0.3532 0.065 Uiso 1 1 calc R . . C9 C 0.2513(8) -0.2857(15) 0.2887(9) 0.066(3) Uani 1 1 d U . . H9A H 0.2159 -0.2202 0.2438 0.080 Uiso 1 1 calc R . . C8 C 0.3518(6) -0.3104(11) 0.2869(6) 0.044(2) Uani 1 1 d U . . C7 C 0.3566(10) -0.4787(13) 0.4230(10) 0.068(3) Uani 1 1 d U . . H7A H 0.3927 -0.5418 0.4691 0.081 Uiso 1 1 calc R . . C6 C 0.2566(11) -0.4560(16) 0.4225(11) 0.080(4) Uani 1 1 d U . . H6A H 0.2243 -0.5072 0.4670 0.096 Uiso 1 1 calc R . . C5 C 0.2028(9) -0.3576(19) 0.3565(9) 0.079(4) Uani 1 1 d U . . H5A H 0.1354 -0.3402 0.3578 0.095 Uiso 1 1 calc R . . C4 C 0.8899(9) 0.212(2) 0.4421(9) 0.100(6) Uani 1 1 d U . . H4A H 0.8927 0.3104 0.4634 0.121 Uiso 1 1 calc R . . C3 C 1.0443(12) 0.2707(19) 0.3897(12) 0.099(5) Uani 1 1 d U . . H3A H 1.0299 0.3666 0.4152 0.149 Uiso 1 1 calc R . . H3B H 1.0502 0.2801 0.3217 0.149 Uiso 1 1 calc R . . H3C H 1.1060 0.2336 0.4255 0.149 Uiso 1 1 calc R . . C2 C 0.9782(18) 0.021(2) 0.3679(13) 0.130(8) Uani 1 1 d U . . H2A H 0.9453 -0.0490 0.4045 0.195 Uiso 1 1 calc R . . H2B H 1.0485 -0.0001 0.3773 0.195 Uiso 1 1 calc R . . H2C H 0.9512 0.0129 0.2995 0.195 Uiso 1 1 calc R . . C1 C 0.8458(7) -0.3446(12) 0.3319(6) 0.047(2) Uani 1 1 d U . . C15 C 0.6987(6) -0.3575(9) 0.2032(6) 0.0362(17) Uani 1 1 d U . . O4 O 0.7442(5) -0.4343(7) 0.1502(5) 0.0419(14) Uani 1 1 d U . . C14 C 0.5886(6) -0.3202(9) 0.1670(5) 0.0335(16) Uani 1 1 d U . . O5 O 0.5568(4) -0.3563(7) 0.0815(4) 0.0365(12) Uani 1 1 d 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 0.03868(19) 0.04141(19) 0.02944(18) -0.00061(13) 0.00486(12) -0.00160(13) N2 0.043(4) 0.111(8) 0.042(5) 0.007(5) 0.004(4) 0.007(5) N1 0.053(6) 0.109(9) 0.103(9) -0.029(8) 0.002(6) 0.022(6) S1 0.0350(10) 0.0570(13) 0.0384(11) -0.0055(10) 0.0023(8) 0.0052(9) O3 0.044(3) 0.061(4) 0.036(3) -0.019(3) -0.002(3) 0.005(3) O2 0.048(3) 0.065(4) 0.044(4) -0.022(3) 0.004(3) 0.005(3) O1 0.059(5) 0.115(8) 0.093(7) -0.001(6) 0.019(5) -0.032(5) C16 0.039(4) 0.036(4) 0.027(4) -0.002(3) 0.003(3) -0.001(3) C13 0.036(4) 0.036(4) 0.050(5) -0.006(4) 0.012(4) 0.000(3) C12 0.038(4) 0.046(5) 0.034(4) 0.001(4) 0.003(3) -0.001(4) C11 0.041(4) 0.049(5) 0.038(4) -0.009(4) 0.011(4) 0.003(4) C10 0.057(6) 0.054(5) 0.056(6) -0.004(5) 0.017(5) -0.007(5) C9 0.046(5) 0.093(9) 0.062(7) -0.017(6) 0.015(5) -0.004(6) C8 0.039(4) 0.057(5) 0.035(4) -0.018(4) 0.004(3) -0.002(4) C7 0.077(8) 0.057(7) 0.075(8) -0.008(6) 0.032(6) -0.008(6) C6 0.077(9) 0.096(10) 0.076(9) -0.009(7) 0.040(7) -0.025(7) C5 0.047(6) 0.136(12) 0.056(7) -0.031(8) 0.016(5) -0.017(7) C4 0.059(7) 0.194(18) 0.045(6) 0.011(9) -0.002(6) 0.000(10) C3 0.095(11) 0.099(11) 0.106(12) -0.006(9) 0.024(9) -0.019(9) C2 0.20(2) 0.100(13) 0.073(11) 0.006(10) -0.032(12) 0.009(14) C1 0.045(5) 0.069(6) 0.025(4) -0.013(4) -0.002(3) 0.010(5) C15 0.032(4) 0.039(4) 0.037(4) -0.002(3) 0.005(3) -0.002(3) O4 0.038(3) 0.052(4) 0.036(3) -0.012(3) 0.008(2) 0.005(3) C14 0.034(4) 0.044(4) 0.021(3) 0.003(3) -0.001(3) -0.005(3) O5 0.039(3) 0.046(3) 0.023(3) -0.003(2) 0.000(2) 0.004(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 O2 2.420(6) . ? Pb1 O5 2.494(6) 4_556 ? Pb1 O4 2.507(6) 4_556 ? Pb1 O3 2.524(6) . ? Pb1 O1 2.597(8) . ? N2 C4 1.289(16) . ? N2 C2 1.40(2) . ? N2 C3 1.472(17) . ? N1 C1 1.147(13) . ? S1 C13 1.761(9) . ? S1 C8 1.781(10) . ? O3 C16 1.247(10) . ? O2 C12 1.223(10) . ? O1 C4 1.230(17) . ? C16 C13 1.419(11) . ? C16 C12 1.520(11) . ? C13 C14 1.392(11) . ? C12 C11 1.398(12) . ? C11 C15 1.411(12) . ? C11 C1 1.436(12) . ? C10 C8 1.376(14) . ? C10 C7 1.387(16) . ? C10 H10A 0.9300 . ? C9 C8 1.383(13) . ? C9 C5 1.386(17) . ? C9 H9A 0.9300 . ? C7 C6 1.369(19) . ? C7 H7A 0.9300 . ? C6 C5 1.39(2) . ? C6 H6A 0.9300 . ? C5 H5A 0.9300 . ? C4 H4A 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C15 O4 1.238(10) . ? C15 C14 1.532(11) . ? O4 Pb1 2.507(6) 4 ? C14 O5 1.236(9) . ? O5 Pb1 2.494(6) 4 ? 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 O2 Pb1 O5 85.7(2) . 4_556 ? O2 Pb1 O4 77.7(2) . 4_556 ? O5 Pb1 O4 64.24(18) 4_556 4_556 ? O2 Pb1 O3 64.2(2) . . ? O5 Pb1 O3 71.3(2) 4_556 . ? O4 Pb1 O3 122.6(2) 4_556 . ? O2 Pb1 O1 70.6(3) . . ? O5 Pb1 O1 146.2(3) 4_556 . ? O4 Pb1 O1 86.8(3) 4_556 . ? O3 Pb1 O1 116.0(3) . . ? C4 N2 C2 126.9(17) . . ? C4 N2 C3 119.0(14) . . ? C2 N2 C3 114.0(14) . . ? C13 S1 C8 102.7(4) . . ? C16 O3 Pb1 115.9(5) . . ? C12 O2 Pb1 121.5(6) . . ? C4 O1 Pb1 165.3(12) . . ? O3 C16 C13 121.4(7) . . ? O3 C16 C12 117.6(7) . . ? C13 C16 C12 120.9(7) . . ? C14 C13 C16 119.8(7) . . ? C14 C13 S1 120.1(6) . . ? C16 C13 S1 119.7(6) . . ? O2 C12 C11 126.7(8) . . ? O2 C12 C16 115.8(8) . . ? C11 C12 C16 117.5(7) . . ? C12 C11 C15 122.5(8) . . ? C12 C11 C1 118.5(8) . . ? C15 C11 C1 119.0(7) . . ? C8 C10 C7 120.9(11) . . ? C8 C10 H10A 119.6 . . ? C7 C10 H10A 119.6 . . ? C8 C9 C5 120.8(12) . . ? C8 C9 H9A 119.6 . . ? C5 C9 H9A 119.6 . . ? C10 C8 C9 119.2(10) . . ? C10 C8 S1 124.2(7) . . ? C9 C8 S1 116.6(8) . . ? C6 C7 C10 119.4(13) . . ? C6 C7 H7A 120.3 . . ? C10 C7 H7A 120.3 . . ? C7 C6 C5 120.9(12) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C9 C5 C6 118.9(11) . . ? C9 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? O1 C4 N2 126.8(19) . . ? O1 C4 H4A 116.6 . . ? N2 C4 H4A 116.6 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C1 C11 177.9(11) . . ? O4 C15 C11 122.6(7) . . ? O4 C15 C14 118.6(7) . . ? C11 C15 C14 118.8(7) . . ? C15 O4 Pb1 118.3(5) . 4 ? O5 C14 C13 125.4(7) . . ? O5 C14 C15 115.4(7) . . ? C13 C14 C15 119.2(7) . . ? C14 O5 Pb1 119.7(5) . 4 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.567 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.274