# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Rong Cao' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry FuJian Institute of Research on the Structure of Matter Fuzhou, FuJian, 350002 P.R.China ; _publ_contact_author_email rcao@ms.fjirsm.ac.cn _publ_section_title ; Hydroxyl-Directed Dinitration of Carboxylate Ligands Mediated by Lead and Nickel Nitrates and Preparation of Pb/Ni Heterometallic Complexes under Hydrothermal Conditions ; _publ_section_references ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; loop_ _publ_author_name 'Xiaoju Li' 'Rong Cao' 'Zhengang Guo' 'Jian Lu' data_1 _database_code_depnum_ccdc_archive 'CCDC 288164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 N4 Ni O26 Pb6' _chemical_formula_weight 1976.13 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.083(2) _cell_length_b 9.299(3) _cell_length_c 10.922(3) _cell_angle_alpha 67.735(6) _cell_angle_beta 82.665(9) _cell_angle_gamma 85.860(8) _cell_volume 753.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2727 _cell_measurement_theta_min 2.0263 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.2300 _exptl_crystal_size_mid 0.1100 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 34.132 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.0521 _exptl_absorpt_correction_T_max 0.3378 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_source_power 4.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 80.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_measurement_details ; scan: Number of images: 360 Slice: -62.0000 - 118.0000 Image width: 0.5000 Exp time: 6.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 50.3107 2theta: 27.9030 scan: Number of images: 280 Slice: -62.0000 - 78.0000 Image width: 0.5000 Exp time: 6.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 50.3107 2theta: 27.9030 scan: Number of images: 160 Slice: -62.0000 - 18.0000 Image width: 0.5000 Exp time: 6.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 180.0000 XTD: 50.3107 2theta: 27.9030 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5877 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3409 _reflns_number_gt 2604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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. ; _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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3409 _refine_ls_number_parameters 241 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.990 _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 0.85145(6) 0.33950(6) 0.83064(5) 0.01920(14) Uani 1 1 d . . . Pb2 Pb 1.26349(6) 0.55733(6) 0.70391(5) 0.01788(14) Uani 1 1 d . . . Pb3 Pb 0.87962(7) 0.78563(6) 0.62210(5) 0.02352(15) Uani 1 1 d . . . Ni1 Ni 1.0000 0.5000 0.5000 0.0119(5) Uani 1 2 d S . . O1 O 1.0918(10) 0.3727(10) 0.6786(8) 0.0150(19) Uani 1 1 d U . . O2 O 0.7942(10) 0.5377(10) 0.6292(8) 0.019(2) Uani 1 1 d . . . O3 O 0.9891(11) 0.5801(10) 0.7990(9) 0.021(2) Uani 1 1 d U . . O4 O 1.0861(10) 0.6856(10) 0.5185(8) 0.0149(19) Uani 1 1 d U . . O5 O 0.7665(11) 0.1580(11) 0.7306(9) 0.022(2) Uani 1 1 d . . . O6 O 0.8058(14) -0.0909(16) 1.0486(12) 0.057(4) Uani 1 1 d . . . O7 O 0.9535(12) -0.1360(13) 0.8907(10) 0.038(3) Uani 1 1 d . . . O8 O 0.7356(12) -0.4063(11) 1.0480(9) 0.029(2) Uani 1 1 d U . . O9 O 0.4659(12) -0.4231(12) 1.1156(9) 0.038(3) Uani 1 1 d . . . O10 O 0.1810(11) -0.1494(11) 0.6698(9) 0.025(2) Uani 1 1 d . . . O11 O 0.1761(11) 0.1064(10) 0.6292(9) 0.023(2) Uani 1 1 d . . . O12 O 0.4871(13) 0.1893(12) 0.4800(10) 0.037(3) Uani 1 1 d . . . O13 O 0.4878(14) 0.3304(12) 0.6002(10) 0.036(3) Uani 1 1 d . . . N1 N 0.8164(14) -0.1084(13) 0.9447(11) 0.021(3) Uani 1 1 d U . . N2 N 0.4914(13) 0.2032(13) 0.5887(11) 0.019(3) Uani 1 1 d . . . C1 C 0.5889(16) -0.3570(16) 1.0356(14) 0.023(3) Uani 1 1 d . . . C2 C 0.2387(15) -0.0314(15) 0.6759(12) 0.012(3) Uani 1 1 d U . . C3 C 0.5601(15) -0.2074(14) 0.9220(11) 0.013(3) Uani 1 1 d . . . C4 C 0.4218(14) -0.1888(14) 0.8552(12) 0.013(3) Uani 1 1 d . . . H3A H 0.3462 -0.2687 0.8834 0.016 Uiso 1 1 calc R . . C5 C 0.3914(14) -0.0516(14) 0.7448(12) 0.013(3) Uani 1 1 d . . . C6 C 0.5111(16) 0.0632(14) 0.7094(12) 0.014(3) Uani 1 1 d . . . C7 C 0.6580(15) 0.0529(15) 0.7701(12) 0.015(3) Uani 1 1 d . . . C8 C 0.6709(16) -0.0936(16) 0.8806(12) 0.018(3) Uani 1 1 d . . . 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 0.0198(3) 0.0208(3) 0.0134(3) -0.0028(2) -0.00052(19) -0.0009(2) Pb2 0.0156(3) 0.0201(3) 0.0157(3) -0.0031(2) -0.00556(19) 0.0008(2) Pb3 0.0302(3) 0.0198(3) 0.0203(3) -0.0087(2) -0.0054(2) 0.0126(2) Ni1 0.0144(12) 0.0129(12) 0.0082(12) -0.0037(9) -0.0025(8) 0.0008(9) O1 0.014(2) 0.015(3) 0.013(2) -0.0028(18) -0.0021(17) 0.0009(18) O2 0.014(5) 0.022(6) 0.020(5) -0.005(4) -0.005(4) 0.005(4) O3 0.019(3) 0.021(3) 0.021(3) -0.0064(18) -0.0032(18) 0.0004(18) O4 0.016(2) 0.016(3) 0.013(2) -0.0069(18) -0.0020(17) 0.0007(18) O5 0.022(5) 0.021(5) 0.021(5) -0.005(4) -0.005(4) -0.002(4) O6 0.040(8) 0.094(11) 0.053(9) -0.043(8) -0.024(6) 0.016(7) O7 0.020(6) 0.051(8) 0.043(7) -0.018(6) -0.001(5) -0.002(5) O8 0.027(3) 0.029(3) 0.027(3) -0.0073(19) -0.0033(18) 0.0001(19) O9 0.020(6) 0.043(7) 0.023(6) 0.018(5) 0.001(4) 0.005(5) O10 0.022(5) 0.029(6) 0.031(6) -0.015(5) -0.011(4) -0.002(4) O11 0.027(6) 0.018(5) 0.023(6) -0.008(4) -0.007(4) 0.007(4) O12 0.035(7) 0.038(7) 0.030(7) -0.005(5) 0.002(5) 0.003(5) O13 0.052(8) 0.012(6) 0.037(7) 0.000(5) -0.015(5) 0.003(5) N1 0.021(3) 0.021(3) 0.020(3) -0.008(2) -0.0028(19) 0.0009(19) N2 0.016(6) 0.018(7) 0.018(7) -0.004(5) -0.002(4) 0.002(5) C1 0.020(8) 0.020(8) 0.024(8) -0.004(6) 0.001(6) 0.001(6) C2 0.013(3) 0.013(3) 0.011(3) -0.004(2) -0.0019(19) -0.0003(19) C3 0.018(7) 0.012(7) 0.008(7) -0.004(5) -0.004(5) 0.006(5) C4 0.013(7) 0.010(7) 0.014(7) -0.004(5) 0.003(5) 0.002(5) C5 0.010(6) 0.015(7) 0.015(7) -0.008(5) 0.004(5) 0.003(5) C6 0.029(8) 0.003(6) 0.009(7) -0.002(5) -0.002(5) 0.001(5) C7 0.009(6) 0.019(8) 0.017(7) -0.006(6) -0.003(5) 0.001(5) C8 0.018(7) 0.025(8) 0.010(7) -0.003(6) -0.005(5) 0.000(6) _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 O1 2.345(8) . ? Pb1 O2 2.349(9) . ? Pb1 O3 2.457(9) . ? Pb1 O5 2.504(9) . ? Pb1 O9 2.684(10) 2_657 ? Pb2 O3 2.357(9) . ? Pb2 O1 2.398(8) . ? Pb2 O4 2.498(9) . ? Pb2 O8 2.537(9) 2_757 ? Pb2 O10 2.656(10) 1_665 ? Pb2 Pb3 3.6403(11) . ? Pb3 O4 2.241(8) . ? Pb3 O3 2.358(9) . ? Pb3 O2 2.424(9) . ? Pb3 O11 2.628(9) 2_666 ? Pb3 O10 2.710(9) 1_665 ? Ni1 O4 1.995(8) 2_766 ? Ni1 O4 1.995(8) . ? Ni1 O1 2.062(8) . ? Ni1 O1 2.062(8) 2_766 ? Ni1 O2 2.138(8) 2_766 ? Ni1 O2 2.138(8) . ? O5 C7 1.272(14) . ? O6 N1 1.198(14) . ? O7 N1 1.245(14) . ? O8 C1 1.245(16) . ? O8 Pb2 2.537(9) 2_757 ? O9 C1 1.260(14) . ? O9 Pb1 2.684(9) 2_657 ? O10 C2 1.250(14) . ? O10 Pb2 2.656(10) 1_445 ? O10 Pb3 2.710(9) 1_445 ? O11 C2 1.279(15) . ? O11 Pb3 2.628(9) 2_666 ? O12 N2 1.247(14) . ? O13 N2 1.234(14) . ? N1 C8 1.417(16) . ? N2 C6 1.477(15) . ? C1 C3 1.499(17) . ? C2 C5 1.491(17) . ? C3 C8 1.340(16) . ? C3 C4 1.376(17) . ? C4 C5 1.417(16) . ? C4 H3A 0.9300 . ? C5 C6 1.402(16) . ? C6 C7 1.413(17) . ? C7 C8 1.445(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O2 71.9(3) . . ? O1 Pb1 O3 69.8(3) . . ? O2 Pb1 O3 69.2(3) . . ? O1 Pb1 O5 85.0(3) . . ? O2 Pb1 O5 85.3(3) . . ? O3 Pb1 O5 148.4(3) . . ? O1 Pb1 O9 149.0(3) . 2_657 ? O2 Pb1 O9 77.1(3) . 2_657 ? O3 Pb1 O9 99.4(3) . 2_657 ? O5 Pb1 O9 92.6(3) . 2_657 ? O3 Pb2 O1 70.6(3) . . ? O3 Pb2 O4 72.1(3) . . ? O1 Pb2 O4 68.9(3) . . ? O3 Pb2 O8 74.2(3) . 2_757 ? O1 Pb2 O8 92.9(3) . 2_757 ? O4 Pb2 O8 145.5(3) . 2_757 ? O3 Pb2 O10 68.6(3) . 1_665 ? O1 Pb2 O10 126.6(3) . 1_665 ? O4 Pb2 O10 66.9(3) . 1_665 ? O8 Pb2 O10 107.3(3) 2_757 1_665 ? O3 Pb2 Pb3 39.5(2) . . ? O1 Pb2 Pb3 78.7(2) . . ? O4 Pb2 Pb3 37.29(19) . . ? O8 Pb2 Pb3 112.5(2) 2_757 . ? O10 Pb2 Pb3 47.91(19) 1_665 . ? O4 Pb3 O3 76.9(3) . . ? O4 Pb3 O2 71.2(3) . . ? O3 Pb3 O2 69.7(3) . . ? O4 Pb3 O11 74.4(3) . 2_666 ? O3 Pb3 O11 146.9(3) . 2_666 ? O2 Pb3 O11 85.7(3) . 2_666 ? O4 Pb3 O10 69.4(3) . 1_665 ? O3 Pb3 O10 67.6(3) . 1_665 ? O2 Pb3 O10 126.7(3) . 1_665 ? O11 Pb3 O10 115.6(3) 2_666 1_665 ? O4 Pb3 Pb2 42.5(2) . . ? O3 Pb3 Pb2 39.4(2) . . ? O2 Pb3 Pb2 80.1(2) . . ? O11 Pb3 Pb2 116.6(2) 2_666 . ? O10 Pb3 Pb2 46.7(2) 1_665 . ? O4 Ni1 O4 180.000(1) 2_766 . ? O4 Ni1 O1 93.9(3) 2_766 . ? O4 Ni1 O1 86.1(3) . . ? O4 Ni1 O1 86.1(3) 2_766 2_766 ? O4 Ni1 O1 93.9(3) . 2_766 ? O1 Ni1 O1 180.0(3) . 2_766 ? O4 Ni1 O2 82.2(3) 2_766 2_766 ? O4 Ni1 O2 97.8(3) . 2_766 ? O1 Ni1 O2 97.9(3) . 2_766 ? O1 Ni1 O2 82.1(3) 2_766 2_766 ? O4 Ni1 O2 97.8(3) 2_766 . ? O4 Ni1 O2 82.2(3) . . ? O1 Ni1 O2 82.1(3) . . ? O1 Ni1 O2 97.9(3) 2_766 . ? O2 Ni1 O2 180.000(1) 2_766 . ? Ni1 O1 Pb1 102.1(3) . . ? Ni1 O1 Pb2 102.0(3) . . ? Pb1 O1 Pb2 108.3(3) . . ? Ni1 O2 Pb1 99.7(3) . . ? Ni1 O2 Pb3 97.3(3) . . ? Pb1 O2 Pb3 110.0(4) . . ? Pb3 O3 Pb2 101.1(3) . . ? Pb3 O3 Pb1 108.6(4) . . ? Pb2 O3 Pb1 106.0(4) . . ? Ni1 O4 Pb3 108.0(3) . . ? Ni1 O4 Pb2 100.6(3) . . ? Pb3 O4 Pb2 100.2(3) . . ? C7 O5 Pb1 132.4(8) . . ? C1 O8 Pb2 104.0(8) . 2_757 ? C1 O9 Pb1 135.2(9) . 2_657 ? C2 O10 Pb2 141.0(9) . 1_445 ? C2 O10 Pb3 133.5(9) . 1_445 ? Pb2 O10 Pb3 85.4(3) 1_445 1_445 ? C2 O11 Pb3 116.8(8) . 2_666 ? O6 N1 O7 121.2(13) . . ? O6 N1 C8 119.4(11) . . ? O7 N1 C8 119.4(12) . . ? O13 N2 O12 123.0(12) . . ? O13 N2 C6 117.3(11) . . ? O12 N2 C6 119.6(11) . . ? O8 C1 O9 123.5(13) . . ? O8 C1 C3 117.4(11) . . ? O9 C1 C3 119.0(12) . . ? O10 C2 O11 125.3(12) . . ? O10 C2 C5 118.0(12) . . ? O11 C2 C5 116.6(11) . . ? C8 C3 C4 119.3(12) . . ? C8 C3 C1 120.9(12) . . ? C4 C3 C1 119.7(11) . . ? C3 C4 C5 122.0(11) . . ? C3 C4 H3A 119.0 . . ? C5 C4 H3A 119.0 . . ? C4 C5 C6 115.3(12) . . ? C4 C5 C2 121.3(11) . . ? C6 C5 C2 123.4(11) . . ? C5 C6 C7 126.6(11) . . ? C5 C6 N2 117.1(11) . . ? C7 C6 N2 116.0(10) . . ? O5 C7 C6 124.1(12) . . ? O5 C7 C8 124.5(12) . . ? C6 C7 C8 111.3(11) . . ? C3 C8 C7 125.5(12) . . ? C3 C8 N1 121.4(12) . . ? C7 C8 N1 113.1(11) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.294 _refine_diff_density_min -2.926 _refine_diff_density_rms 0.418 data_2 _database_code_depnum_ccdc_archive 'CCDC 288165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H4.50 N2 O8.25 Pb' _chemical_formula_weight 455.82 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' 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 Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.125(3) _cell_length_b 23.399(5) _cell_length_c 7.0102(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1988.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5329 _cell_measurement_theta_min 2.4188 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3100 _exptl_crystal_size_mid 0.1700 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 17.011 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.0558 _exptl_absorpt_correction_T_max 0.4192 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_measurement_details ; scan: Number of images: 360 Slice: -62.0000 - 118.0000 Image width: 0.5000 Exp time: 5.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 50.3139 2theta: 27.9057 scan: Number of images: 280 Slice: -62.0000 - 78.0000 Image width: 0.5000 Exp time: 5.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 50.3139 2theta: 27.9057 scan: Number of images: 160 Slice: -62.0000 - 18.0000 Image width: 0.5000 Exp time: 5.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 180.0000 XTD: 50.3139 2theta: 27.9057 ; _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14138 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2277 _reflns_number_gt 1950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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. ; _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^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2277 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.834847(14) 0.425853(7) 0.03684(3) 0.02461(9) Uani 1 1 d . . . O1 O 0.7267(3) 0.49640(13) -0.1881(6) 0.0327(9) Uani 1 1 d . . . O2 O 0.3489(3) 0.59503(19) -0.1644(7) 0.0468(11) Uani 1 1 d . . . O3 O 0.3742(3) 0.61901(15) 0.1345(5) 0.0387(9) Uani 1 1 d . . . O4 O 0.4694(3) 0.72040(18) -0.0164(7) 0.0586(14) Uani 1 1 d . . . O5 O 0.6215(3) 0.74025(15) 0.1339(7) 0.0576(14) Uani 1 1 d . . . O6 O 0.9345(3) 0.63086(17) -0.0512(6) 0.0449(12) Uani 1 1 d . . . O7 O 0.9226(3) 0.54025(15) -0.0925(6) 0.0418(10) Uani 1 1 d . . . N1 N 0.5627(4) 0.70804(18) 0.0397(7) 0.0345(11) Uani 1 1 d . . . N2 N 0.8787(3) 0.58745(18) -0.0749(6) 0.0267(10) Uani 1 1 d . . . C1 C 0.4093(4) 0.60873(19) -0.0283(7) 0.0221(10) Uani 1 1 d . . . C2 C 0.5317(3) 0.60780(19) -0.0606(6) 0.0197(10) Uani 1 1 d . . . C3 C 0.6041(4) 0.6521(2) -0.0134(7) 0.0240(10) Uani 1 1 d . . . C4 C 0.7175(4) 0.6447(2) -0.0178(7) 0.0241(11) Uani 1 1 d . . . H4A H 0.7644 0.6743 0.0169 0.029 Uiso 1 1 calc R . . C5 C 0.7600(4) 0.5923(2) -0.0749(8) 0.0230(10) Uani 1 1 d . . . C6 C 0.6915(4) 0.54529(18) -0.1305(7) 0.0213(10) Uani 1 1 d . . . C7 C 0.5767(4) 0.55667(19) -0.1201(7) 0.0238(10) Uani 1 1 d . . . H7A H 0.5285 0.5277 -0.1559 0.029 Uiso 1 1 calc R . . OW1 O 0.8200(9) 0.3172(5) 0.0614(16) 0.053(3) Uani 0.50 1 d P . . OW1' O 0.8281(9) 0.3152(4) -0.0605(15) 0.047(3) Uani 0.50 1 d P . . OW2 O 0.2500 0.7500 0.2382(18) 0.055(3) Uani 0.50 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.01860(12) 0.02905(13) 0.02618(15) -0.00027(7) 0.00076(8) 0.00075(6) O1 0.0307(18) 0.0238(17) 0.044(2) -0.0099(16) -0.0069(17) 0.0067(14) O2 0.0196(16) 0.078(3) 0.042(3) -0.026(2) -0.0018(18) -0.0036(18) O3 0.0290(17) 0.055(2) 0.033(3) 0.0079(18) 0.0062(18) 0.0050(17) O4 0.034(2) 0.034(2) 0.107(4) -0.004(2) 0.001(2) 0.0154(19) O5 0.050(2) 0.034(2) 0.088(4) -0.028(2) 0.011(3) -0.0122(19) O6 0.0192(18) 0.037(2) 0.078(4) -0.0074(19) 0.0024(19) -0.0086(16) O7 0.0250(17) 0.031(2) 0.070(3) -0.0037(19) 0.003(2) 0.0065(15) N1 0.025(2) 0.026(2) 0.053(3) -0.0013(19) 0.013(2) -0.0012(18) N2 0.0181(19) 0.032(2) 0.030(3) 0.0025(19) -0.0014(19) 0.0027(17) C1 0.019(2) 0.019(2) 0.029(3) 0.0008(19) 0.001(2) -0.0022(18) C2 0.015(2) 0.026(2) 0.018(3) 0.0012(18) 0.0008(18) -0.0006(17) C3 0.020(2) 0.021(2) 0.030(3) 0.0005(19) 0.005(2) 0.0029(18) C4 0.023(2) 0.024(2) 0.025(3) 0.0018(19) -0.001(2) -0.0039(19) C5 0.017(2) 0.023(2) 0.029(3) 0.000(2) 0.002(2) 0.0018(18) C6 0.021(2) 0.024(2) 0.019(3) -0.0010(19) -0.001(2) 0.0028(18) C7 0.019(2) 0.024(2) 0.029(3) -0.003(2) 0.002(2) -0.0023(18) OW1 0.052(6) 0.037(5) 0.071(8) -0.016(6) -0.024(7) 0.001(4) OW1' 0.057(6) 0.024(4) 0.058(7) 0.000(5) 0.009(6) 0.014(4) OW2 0.071(9) 0.046(7) 0.047(8) 0.000 0.000 -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb O2 2.450(4) 5_665 ? Pb OW1 2.554(11) . ? Pb O3 2.577(4) 3_565 ? Pb O1 2.633(3) . ? Pb O1 2.646(3) 7_756 ? Pb O2 2.662(5) 3_564 ? Pb OW1' 2.680(10) . ? O1 C6 1.286(5) . ? O1 Pb 2.646(3) 7_755 ? O2 C1 1.244(6) . ? O2 Pb 2.450(4) 5_665 ? O2 Pb 2.662(5) 3_464 ? O3 C1 1.241(6) . ? O3 Pb 2.577(4) 3_465 ? O4 N1 1.231(6) . ? O5 N1 1.230(6) . ? O6 N2 1.232(5) . ? O7 N2 1.232(5) . ? N1 C3 1.450(6) . ? N2 C5 1.444(6) . ? C1 C2 1.501(6) . ? C2 C7 1.380(6) . ? C2 C3 1.398(6) . ? C3 C4 1.386(7) . ? C4 C5 1.389(7) . ? C4 H4A 0.9300 . ? C5 C6 1.431(6) . ? C6 C7 1.419(6) . ? C7 H7A 0.9300 . ? OW1 OW1' 0.862(13) . ? 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 Pb OW1 73.3(3) 5_665 . ? O2 Pb O3 76.16(14) 5_665 3_565 ? OW1 Pb O3 63.1(3) . 3_565 ? O2 Pb O1 83.73(14) 5_665 . ? OW1 Pb O1 129.0(2) . . ? O3 Pb O1 152.05(11) 3_565 . ? O2 Pb O1 66.54(12) 5_665 7_756 ? OW1 Pb O1 123.5(3) . 7_756 ? O3 Pb O1 69.80(11) 3_565 7_756 ? O1 Pb O1 84.54(8) . 7_756 ? O2 Pb O2 112.31(12) 5_665 3_564 ? OW1 Pb O2 83.6(3) . 3_564 ? O3 Pb O2 142.24(13) 3_565 3_564 ? O1 Pb O2 63.86(12) . 3_564 ? O1 Pb O2 147.94(13) 7_756 3_564 ? O2 Pb OW1' 82.7(3) 5_665 . ? OW1 Pb OW1' 18.8(3) . . ? O3 Pb OW1' 80.8(2) 3_565 . ? O1 Pb OW1' 116.0(2) . . ? O1 Pb OW1' 141.3(2) 7_756 . ? O2 Pb OW1' 64.8(2) 3_564 . ? C6 O1 Pb 122.3(3) . . ? C6 O1 Pb 133.7(3) . 7_755 ? Pb O1 Pb 100.71(10) . 7_755 ? C1 O2 Pb 107.9(3) . 5_665 ? C1 O2 Pb 146.8(3) . 3_464 ? Pb O2 Pb 105.27(13) 5_665 3_464 ? C1 O3 Pb 143.8(3) . 3_465 ? O5 N1 O4 124.0(5) . . ? O5 N1 C3 119.3(4) . . ? O4 N1 C3 116.6(5) . . ? O6 N2 O7 121.0(4) . . ? O6 N2 C5 118.9(4) . . ? O7 N2 C5 120.1(4) . . ? O3 C1 O2 123.6(4) . . ? O3 C1 C2 118.7(4) . . ? O2 C1 C2 117.5(4) . . ? C7 C2 C3 117.8(4) . . ? C7 C2 C1 116.7(4) . . ? C3 C2 C1 125.0(4) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 N1 117.6(4) . . ? C2 C3 N1 120.9(4) . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C4 C5 C6 122.8(4) . . ? C4 C5 N2 116.0(4) . . ? C6 C5 N2 121.2(4) . . ? O1 C6 C7 120.5(4) . . ? O1 C6 C5 125.2(4) . . ? C7 C6 C5 114.2(4) . . ? C2 C7 C6 124.5(4) . . ? C2 C7 H7A 117.7 . . ? C6 C7 H7A 117.7 . . ? OW1' OW1 Pb 88.9(12) . . ? OW1 OW1' Pb 72.4(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.364 _refine_diff_density_min -1.394 _refine_diff_density_rms 0.190 # Attachment 'compound3.CIF' # Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_3 _database_code_depnum_ccdc_archive 'CCDC 288166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 N0 O6.50 Pb1.50' _chemical_formula_weight 516.93 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-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 10.000(9) _cell_length_b 13.053(12) _cell_length_c 15.555(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.858(11) _cell_angle_gamma 90.00 _cell_volume 2000(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2909 _cell_measurement_theta_min 3.0677 _cell_measurement_theta_max 25.0264 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 25.260 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.3674 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5887 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1758 _reflns_number_gt 1361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1758 _refine_ls_number_parameters 154 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.2083 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 0.509(5) 1.38051(12) 0.246(4) 0.015(3) Uani 0.50 1 d P . . Pb2 Pb 0.29142(9) 0.73776(7) 0.15136(5) 0.0161(4) Uani 1 1 d . . . O1 O 0.5516(17) 1.2604(12) 0.1480(11) 0.020(4) Uani 1 1 d U . . O2 O 0.346(2) 0.9159(14) 0.1449(11) 0.034(5) Uani 1 1 d . . . O3 O 0.240(2) 0.8836(15) 0.0090(12) 0.039(5) Uani 1 1 d . . . O4 O 0.2453(16) 1.1828(13) -0.2099(10) 0.021(4) Uani 1 1 d U . . O5 O 0.4239(18) 1.2823(17) -0.1774(12) 0.039(5) Uani 1 1 d . . . C1 C 0.319(3) 0.943(2) 0.0676(15) 0.028(6) Uani 1 1 d . . . C2 C 0.349(3) 1.216(2) -0.1546(18) 0.027(6) Uani 1 1 d . . . C3 C 0.480(2) 1.204(2) 0.0906(14) 0.015(5) Uani 1 1 d . . . C4 C 0.432(2) 1.1078(18) 0.1099(16) 0.021(5) Uani 1 1 d . . . H4B H 0.4537 1.0822 0.1678 0.026 Uiso 1 1 calc R . . C5 C 0.349(2) 1.0466(18) 0.0441(14) 0.016(5) Uani 1 1 d U . . C6 C 0.321(2) 1.0832(18) -0.0425(14) 0.017(5) Uani 1 1 d U . . H6A H 0.2706 1.0426 -0.0874 0.020 Uiso 1 1 calc R . . C7 C 0.368(2) 1.1793(16) -0.0610(14) 0.014(5) Uani 1 1 d U . . C8 C 0.442(2) 1.2411(18) -0.0014(16) 0.019(5) Uani 1 1 d . . . H8A H 0.4684 1.3072 -0.0176 0.023 Uiso 1 1 calc R . . OW1 O 0.716(3) 1.5436(18) 0.2560(16) 0.065(7) Uani 1 1 d . . . OW2 O 0.503(3) 1.494(3) -0.088(2) 0.023(7) Uani 0.50 1 d P . . 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 0.017(9) 0.0116(7) 0.017(8) 0.0005(16) 0.006(5) 0.0006(14) Pb2 0.0234(6) 0.0137(6) 0.0110(6) -0.0022(3) 0.0017(4) -0.0034(3) O1 0.024(7) 0.025(7) 0.011(7) -0.004(6) -0.001(6) 0.000(6) O2 0.065(13) 0.018(10) 0.019(9) 0.006(8) 0.005(9) -0.018(9) O3 0.075(16) 0.020(11) 0.021(10) 0.000(7) 0.003(10) -0.019(9) O4 0.026(7) 0.026(7) 0.009(6) 0.000(6) -0.001(5) -0.007(6) O5 0.020(10) 0.068(15) 0.027(11) 0.029(10) 0.000(8) -0.010(9) C1 0.039(14) 0.027(15) 0.014(13) -0.003(11) -0.002(11) -0.018(12) C2 0.026(13) 0.020(14) 0.036(16) 0.016(12) 0.010(12) 0.004(11) C3 0.004(10) 0.028(14) 0.012(11) 0.008(10) -0.002(8) -0.003(9) C4 0.028(13) 0.019(14) 0.018(12) 0.008(10) 0.007(10) 0.007(10) C5 0.021(8) 0.014(8) 0.011(8) 0.000(7) -0.003(7) -0.005(7) C6 0.017(8) 0.016(8) 0.017(8) 0.005(7) 0.000(7) -0.008(7) C7 0.017(8) 0.009(8) 0.013(8) 0.004(7) -0.007(7) 0.005(6) C8 0.007(10) 0.029(15) 0.019(14) 0.007(10) -0.002(10) -0.004(9) OW1 0.11(2) 0.028(13) 0.066(16) 0.003(11) 0.033(15) 0.022(13) OW2 0.027(18) 0.015(18) 0.029(19) 0.008(14) 0.005(15) 0.011(14) _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 Pb1 0.24(7) 2_655 ? Pb1 O1 2.28(4) . ? Pb1 O1 2.43(4) 2_655 ? Pb1 O4 2.49(5) 8_576 ? Pb1 O4 2.64(5) 7_575 ? Pb2 O2 2.394(18) . ? Pb2 O1 2.408(17) 3_445 ? Pb2 O4 2.507(15) 6_576 ? O1 C3 1.27(3) . ? O1 Pb2 2.408(17) 3 ? O1 Pb1 2.43(4) 2_655 ? O2 C1 1.24(3) . ? O3 C1 1.35(3) . ? O4 C2 1.30(3) . ? O4 Pb1 2.49(5) 8_475 ? O4 Pb2 2.507(15) 6_575 ? O4 Pb1 2.64(5) 7_575 ? O5 C2 1.24(3) . ? C1 C5 1.44(3) . ? C2 C7 1.51(3) . ? C3 C4 1.40(3) . ? C3 C8 1.50(3) . ? C4 C5 1.44(3) . ? C4 H4B 0.9500 . ? C5 C6 1.41(3) . ? C6 C7 1.39(3) . ? C6 H6A 0.9500 . ? C7 C8 1.35(3) . ? C8 H8A 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 Pb1 Pb1 O1 127(10) 2_655 . ? Pb1 Pb1 O1 48(10) 2_655 2_655 ? O1 Pb1 O1 96.2(8) . 2_655 ? Pb1 Pb1 O4 128(10) 2_655 8_576 ? O1 Pb1 O4 71.2(10) . 8_576 ? O1 Pb1 O4 86.2(15) 2_655 8_576 ? Pb1 Pb1 O4 48(10) 2_655 7_575 ? O1 Pb1 O4 85.8(15) . 7_575 ? O1 Pb1 O4 66.4(10) 2_655 7_575 ? O4 Pb1 O4 142.2(8) 8_576 7_575 ? O2 Pb2 O1 96.4(6) . 3_445 ? O2 Pb2 O4 73.2(6) . 6_576 ? O1 Pb2 O4 68.8(5) 3_445 6_576 ? C3 O1 Pb1 136(2) . . ? C3 O1 Pb2 112.3(14) . 3 ? Pb1 O1 Pb2 111.7(14) . 3 ? C3 O1 Pb1 132.3(19) . 2_655 ? Pb1 O1 Pb1 4.5(16) . 2_655 ? Pb2 O1 Pb1 115.3(14) 3 2_655 ? C1 O2 Pb2 108.0(15) . . ? C2 O4 Pb1 154.7(19) . 8_475 ? C2 O4 Pb2 100.9(14) . 6_575 ? Pb1 O4 Pb2 101.9(13) 8_475 6_575 ? C2 O4 Pb1 150.7(18) . 7_575 ? Pb1 O4 Pb1 4(2) 8_475 7_575 ? Pb2 O4 Pb1 105.1(12) 6_575 7_575 ? O2 C1 O3 120(2) . . ? O2 C1 C5 120(2) . . ? O3 C1 C5 120(2) . . ? O5 C2 O4 120(2) . . ? O5 C2 C7 121(2) . . ? O4 C2 C7 119(2) . . ? O1 C3 C4 123(2) . . ? O1 C3 C8 120(2) . . ? C4 C3 C8 117(2) . . ? C3 C4 C5 122(2) . . ? C3 C4 H4B 119.2 . . ? C5 C4 H4B 119.2 . . ? C6 C5 C4 119(2) . . ? C6 C5 C1 123(2) . . ? C4 C5 C1 117(2) . . ? C7 C6 C5 119(2) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C8 C7 C6 124(2) . . ? C8 C7 C2 116(2) . . ? C6 C7 C2 120(2) . . ? C7 C8 C3 119(2) . . ? C7 C8 H8A 120.4 . . ? C3 C8 H8A 120.4 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.688 _refine_diff_density_min -7.988 _refine_diff_density_rms 1.309