# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'F.J.Martinez Casado' ;Laboratorio de Estudios Cristalogr\'aficos, IACT, CSIC-UGR, Avenida de las Palmeras, 4 E-18100 Armilla, Granada (Spain) ; 'L.Canadillas Delgado' ;Institut Laue-Langevin (ILL) 6, rue Jules Horowitz BP 156 38042 Grenoble (France) ; F.Cucinotta ;Dipartimento di Scienze e Tecnologie Avanzate and Nano-SISTEMI Interdisciplinary Centre, Universit\'a del Piemonte Orientale "A. Avogadro" via Teresa Michel 11, I-15121 Alessandria, Italy ; ; A.Guerrero Martinez ; ;Departamento de Qu\'imica F\'isica, Universidad de Vigo E-36310 Vigo (Spain) ; 'M.Ramos Riesco' ;Dpto. Quimica Fisica I Fac. Ciencias Quimicas Universidad Complutense de Madrid Avda. Complutense s/n 28040 Madrid (Spain) ; L.Marchese ;Dipartimento di Scienze e Tecnologie Avanzate and Nano-SISTEMI Interdisciplinary Centre, Universit\'a del Piemonte Orientale "A. Avogadro" via Teresa Michel 11, I-15121 Alessandria, Italy ; 'J.A.Rodriguez Cheda' ;Dpto. Quimica Fisica I Fac. Ciencias Quimicas Universidad Complutense de Madrid Avda. Complutense s/n 28040 Madrid (Spain) ; _publ_contact_author_address ;Laboratorio de Estudios Cristalogr\'aficos, IACT, CSIC-UGR, Avenida de las Palmeras, 4 E-18100 Armilla, Granada (Spain) ; _publ_contact_author_email fmarcas@lec.csic.es _publ_contact_author_phone +34958230000 _publ_contact_author_name 'F. J. Martinez Casado' data_PbC4_4,4'-bipy_100K _database_code_depnum_ccdc_archive 'CCDC 849294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'aqua-4,4'-bipyridine-dilead(II) tetrabutyrate' ; _chemical_name_common "aqua-4,4'-bipyridine-dilead(II) tetrabutyrate" _chemical_melting_point ? _chemical_formula_moiety 2(Pb+2),4(C4O2H7-),(C10H8N2),(H2O) _chemical_formula_sum 'C26 H38 N2 O9 Pb2' _chemical_formula_weight 936.96 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 19.450(3) _cell_length_b 20.139(5) _cell_length_c 8.060(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.07(3) _cell_angle_gamma 90.00 _cell_volume 2965.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 11.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5705 _exptl_absorpt_correction_T_max 0.7503 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.73790 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean 9.77 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21052 _diffrn_reflns_av_R_equivalents 0.1243 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3196 _reflns_number_gt 2979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2. and ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+40.0861P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3196 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 N1 N 0.1729(5) 0.1431(4) 1.1337(9) 0.048(2) Uani 1 1 d . . . O2 O 0.1695(4) 0.0199(3) 0.6381(8) 0.0483(16) Uani 1 1 d . . . O4 O 0.0090(4) 0.1169(3) 0.5525(7) 0.0455(15) Uani 1 1 d . . . O3 O 0.0980(4) 0.1771(3) 0.7335(8) 0.0501(16) Uani 1 1 d . . . O1 O 0.2333(5) 0.0833(4) 0.8589(10) 0.0568(18) Uani 1 1 d . . . C5 C 0.1652(5) 0.1325(4) 1.2885(10) 0.0388(18) Uani 1 1 d . . . H5 H 0.1378 0.0949 1.3002 0.047 Uiso 1 1 calc R . . C15 C 0.0415(6) 0.1722(5) 0.6003(12) 0.046(2) Uani 1 1 d . . . C11 C 0.2291(5) 0.0452(5) 0.7311(12) 0.0431(19) Uani 1 1 d . . . C1 C 0.2129(11) 0.1931(8) 1.1259(14) 0.108(7) Uani 1 1 d . . . H1 H 0.2228 0.1998 1.0196 0.130 Uiso 1 1 calc R . . C2 C 0.2425(12) 0.2381(9) 1.2632(15) 0.127(9) Uani 1 1 d . . . H2 H 0.2686 0.2758 1.2463 0.153 Uiso 1 1 calc R . . C3 C 0.2337(6) 0.2276(5) 1.4246(11) 0.053(3) Uani 1 1 d . . . C4 C 0.1945(6) 0.1730(4) 1.4341(10) 0.042(2) Uani 1 1 d . . . H4 H 0.1872 0.1624 1.5417 0.051 Uiso 1 1 calc R . . C16 C 0.0085(10) 0.2358(7) 0.499(2) 0.088(5) Uani 1 1 d . . . H16A H -0.0154 0.2234 0.3739 0.105 Uiso 1 1 calc R . . H16B H -0.0308 0.2505 0.5431 0.105 Uiso 1 1 calc R . . C12 C 0.2954(7) 0.0311(8) 0.6885(19) 0.081(4) Uani 1 1 d . . . H12A H 0.3007 -0.0177 0.6840 0.097 Uiso 1 1 calc R . . H12B H 0.2878 0.0485 0.5686 0.097 Uiso 1 1 calc R . . C13 C 0.3642(11) 0.0580(17) 0.808(4) 0.187(16) Uani 1 1 d . . . H13A H 0.3732 0.0412 0.9293 0.225 Uiso 1 1 calc R . . H13B H 0.3611 0.1071 0.8109 0.225 Uiso 1 1 calc R . . C17 C 0.0538(14) 0.2926(7) 0.504(2) 0.116(8) Uani 1 1 d . . . H17A H 0.0266 0.3223 0.4052 0.139 Uiso 1 1 calc R . . H17B H 0.0978 0.2770 0.4801 0.139 Uiso 1 1 calc R . . C14 C 0.425(2) 0.038(2) 0.748(8) 0.26(2) Uani 1 1 d . . . H14A H 0.4703 0.0599 0.8222 0.385 Uiso 1 1 calc R . . H14B H 0.4139 0.0515 0.6250 0.385 Uiso 1 1 calc R . . H14C H 0.4313 -0.0101 0.7582 0.385 Uiso 1 1 calc R . . C18 C 0.078(2) 0.3326(10) 0.666(4) 0.181(16) Uani 1 1 d . . . H18A H 0.1071 0.3705 0.6497 0.272 Uiso 1 1 calc R . . H18B H 0.1090 0.3052 0.7644 0.272 Uiso 1 1 calc R . . H18C H 0.0358 0.3487 0.6926 0.272 Uiso 1 1 calc R . . O1W O 0.0000 -0.0434(4) 0.7500 0.0372(17) Uani 1 2 d S . . Pb1 Pb 0.110840(19) 0.068111(13) 0.86798(3) 0.0361(2) 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 N1 0.085(6) 0.045(4) 0.015(3) -0.008(3) 0.018(3) -0.028(4) O2 0.077(4) 0.036(3) 0.027(3) -0.007(3) 0.011(3) 0.003(3) O4 0.071(4) 0.047(4) 0.018(3) 0.002(2) 0.014(3) 0.006(3) O3 0.094(5) 0.034(3) 0.029(3) 0.002(2) 0.029(3) -0.009(3) O1 0.081(5) 0.054(4) 0.042(4) -0.015(3) 0.028(4) -0.021(4) C5 0.071(5) 0.027(4) 0.020(4) -0.005(3) 0.018(4) -0.013(4) C15 0.084(6) 0.037(5) 0.028(4) 0.012(4) 0.034(5) 0.010(4) C11 0.063(5) 0.035(4) 0.034(4) -0.005(4) 0.019(4) -0.002(4) C1 0.190(17) 0.120(12) 0.026(5) -0.035(7) 0.053(8) -0.116(13) C2 0.23(2) 0.135(14) 0.029(6) -0.048(7) 0.066(9) -0.147(15) C3 0.090(7) 0.055(6) 0.016(4) -0.010(4) 0.021(4) -0.034(5) C4 0.080(6) 0.034(4) 0.019(3) -0.004(3) 0.023(4) -0.014(4) C16 0.139(13) 0.062(8) 0.086(10) 0.047(8) 0.069(10) 0.044(8) C12 0.072(7) 0.102(11) 0.066(8) -0.029(8) 0.020(6) -0.001(7) C13 0.064(10) 0.35(5) 0.15(2) -0.07(2) 0.040(13) -0.057(17) C17 0.25(2) 0.045(7) 0.083(11) 0.021(7) 0.091(14) 0.029(10) C14 0.14(3) 0.24(4) 0.41(7) -0.03(5) 0.13(4) -0.09(3) C18 0.38(5) 0.069(11) 0.16(2) -0.010(13) 0.18(3) -0.033(19) O1W 0.060(5) 0.024(4) 0.026(4) 0.000 0.013(3) 0.000 Pb1 0.0677(3) 0.0254(3) 0.0144(2) -0.00248(8) 0.01303(17) -0.00985(11) _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 N1 C1 1.289(13) . ? N1 C5 1.324(10) . ? N1 Pb1 2.559(7) . ? O2 C11 1.253(12) . ? O2 Pb1 2.669(7) . ? O2 Pb1 2.735(6) 6 ? O4 C15 1.273(12) . ? O3 C15 1.249(13) . ? O3 Pb1 2.423(6) . ? O1 C11 1.265(11) . ? O1 Pb1 2.428(8) . ? C5 C4 1.380(11) . ? C5 H5 0.9500 . ? C15 C16 1.535(14) . ? C11 C12 1.471(16) . ? C1 C2 1.392(14) . ? C1 H1 0.9500 . ? C2 C3 1.385(12) . ? C2 H2 0.9500 . ? C3 C4 1.355(12) . ? C3 C3 1.471(16) 7_558 ? C4 H4 0.9500 . ? C16 C17 1.44(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C12 C13 1.46(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.48(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C17 C18 1.47(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Pb1 O2 2.735(6) 6_556 ? 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 C1 N1 C5 115.9(8) . . ? C1 N1 Pb1 122.7(6) . . ? C5 N1 Pb1 121.4(6) . . ? C11 O2 Pb1 88.0(5) . . ? C11 O2 Pb1 141.9(6) . 6 ? Pb1 O2 Pb1 128.9(3) . 6 ? C15 O3 Pb1 103.8(5) . . ? C11 O1 Pb1 99.1(6) . . ? N1 C5 C4 124.0(8) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? O3 C15 O4 121.9(8) . . ? O3 C15 C16 118.3(11) . . ? O4 C15 C16 119.7(11) . . ? O2 C11 O1 121.4(9) . . ? O2 C11 C12 119.2(9) . . ? O1 C11 C12 119.4(10) . . ? N1 C1 C2 124.1(9) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 119.8(10) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 115.4(8) . . ? C4 C3 C3 122.9(9) . 7_558 ? C2 C3 C3 121.7(10) . 7_558 ? C3 C4 C5 120.5(7) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C17 C16 C15 120.6(16) . . ? C17 C16 H16A 107.2 . . ? C15 C16 H16A 107.2 . . ? C17 C16 H16B 107.2 . . ? C15 C16 H16B 107.2 . . ? H16A C16 H16B 106.8 . . ? C13 C12 C11 116.8(15) . . ? C13 C12 H12A 108.1 . . ? C11 C12 H12A 108.1 . . ? C13 C12 H12B 108.1 . . ? C11 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C12 C13 C14 110(3) . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C16 C17 C18 117.9(15) . . ? C16 C17 H17A 107.8 . . ? C18 C17 H17A 107.8 . . ? C16 C17 H17B 107.8 . . ? C18 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 Pb1 O1 79.9(3) . . ? O3 Pb1 N1 77.7(2) . . ? O1 Pb1 N1 76.4(3) . . ? O3 Pb1 O2 91.3(2) . . ? O1 Pb1 O2 50.8(2) . . ? N1 Pb1 O2 127.2(3) . . ? O3 Pb1 O2 153.4(2) . 6_556 ? O1 Pb1 O2 87.7(3) . 6_556 ? N1 Pb1 O2 76.6(3) . 6_556 ? O2 Pb1 O2 98.98(16) . 6_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.373 _refine_diff_density_min -4.578 _refine_diff_density_rms 0.247 #END data_PbC4_4,4'-bipy_298K _database_code_depnum_ccdc_archive 'CCDC 849295' #TrackingRef 'PbC4_bipy_100K_298K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate' ; _chemical_name_common 'aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate' _chemical_melting_point ? _chemical_formula_moiety 2(Pb+2),4(C4O2H7-),(C12H10N2),(H2O) _chemical_formula_sum 'C28 H40 N2 O9 Pb2' _chemical_formula_weight 963.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0070 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0120 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.1460 10.7510 '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 18.479(4) _cell_length_b 22.360(5) _cell_length_c 8.2480(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.64(3) _cell_angle_gamma 90.00 _cell_volume 3349.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1831 _exptl_absorpt_coefficient_mu 10.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5300 _exptl_absorpt_correction_T_max 0.7742 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.73790 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean 9.77 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42581 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 29.00 _reflns_number_total 3973 _reflns_number_gt 3691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2. and ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+5.8167P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00227(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3973 _refine_ls_number_parameters 187 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 O4 O 0.4910(2) 0.3911(2) 0.4525(4) 0.0725(10) Uani 1 1 d . . . O1 O 0.33472(19) 0.47824(16) 0.4567(5) 0.0660(9) Uani 1 1 d . . . O3 O 0.4022(2) 0.33695(15) 0.3107(4) 0.0671(9) Uani 1 1 d . . . O2 O 0.2677(2) 0.4251(2) 0.2647(5) 0.0737(10) Uani 1 1 d . . . C6 C 0.2602(3) 0.3401(2) -0.0376(6) 0.0602(11) Uani 1 1 d . . . H6 H 0.2408 0.3393 0.0587 0.072 Uiso 1 1 calc R . . C11 C 0.2745(3) 0.4558(2) 0.3927(6) 0.0555(10) Uani 1 1 d . . . C15 C 0.4597(3) 0.3416(2) 0.4169(6) 0.0634(12) Uani 1 1 d . . . C16 C 0.5016(8) 0.2913(4) 0.5088(12) 0.186(7) Uani 1 1 d D . . H16A H 0.5532 0.2996 0.5099 0.223 Uiso 1 1 calc R . . H16B H 0.4946 0.2950 0.6221 0.223 Uiso 1 1 calc R . . C12 C 0.2081(3) 0.4659(4) 0.4708(9) 0.092(2) Uani 1 1 d . . . H12A H 0.2202 0.4517 0.5836 0.111 Uiso 1 1 calc R . . H12B H 0.2007 0.5088 0.4760 0.111 Uiso 1 1 calc R . . C17 C 0.4914(8) 0.2298(4) 0.4679(18) 0.319(14) Uani 1 1 d D . . H17A H 0.4894 0.2254 0.3501 0.383 Uiso 1 1 calc R . . H17B H 0.4441 0.2173 0.4914 0.383 Uiso 1 1 calc R . . C13 C 0.1394(6) 0.4401(7) 0.399(2) 0.214(10) Uani 1 1 d . . . H13A H 0.1435 0.3969 0.4077 0.257 Uiso 1 1 calc R . . H13B H 0.1289 0.4500 0.2821 0.257 Uiso 1 1 calc R . . C18 C 0.5478(7) 0.1901(5) 0.5539(18) 0.192(7) Uani 1 1 d D . . H18A H 0.5304 0.1496 0.5429 0.288 Uiso 1 1 calc R . . H18B H 0.5589 0.2007 0.6686 0.288 Uiso 1 1 calc R . . H18C H 0.5915 0.1936 0.5071 0.288 Uiso 1 1 calc R . . C14 C 0.0786(9) 0.4597(12) 0.473(4) 0.43(3) Uani 1 1 d . . . H14A H 0.0359 0.4360 0.4315 0.652 Uiso 1 1 calc R . . H14B H 0.0683 0.5010 0.4470 0.652 Uiso 1 1 calc R . . H14C H 0.0913 0.4550 0.5908 0.652 Uiso 1 1 calc R . . Pb1 Pb 0.386328(8) 0.437554(6) 0.195282(15) 0.04209(10) Uani 1 1 d . . . O1W O 0.5000 0.5399(2) 0.2500 0.0612(11) Uani 1 2 d S . . C5 C 0.2371(2) 0.2531(2) -0.4310(5) 0.0522(9) Uani 1 1 d . . . H5 H 0.2005 0.2269 -0.4118 0.063 Uiso 1 1 calc R . . C3 C 0.2627(2) 0.29900(18) -0.3061(5) 0.0454(8) Uani 1 1 d . . . C2 C 0.3148(2) 0.34214(19) -0.3202(5) 0.0493(9) Uani 1 1 d . . . H2 H 0.3339 0.3452 -0.4167 0.059 Uiso 1 1 calc R . . C1 C 0.3384(2) 0.38063(19) -0.1907(5) 0.0515(9) Uani 1 1 d . . . H1 H 0.3739 0.4089 -0.2023 0.062 Uiso 1 1 calc R . . N1 N 0.3129(2) 0.37945(17) -0.0494(4) 0.0514(8) Uani 1 1 d . . . C4 C 0.2332(3) 0.3009(2) -0.1610(6) 0.0589(11) Uani 1 1 d . . . H4 H 0.1950 0.2752 -0.1488 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O4 0.069(2) 0.099(3) 0.0471(18) -0.0015(18) 0.0044(16) 0.007(2) O1 0.0654(19) 0.068(2) 0.063(2) -0.0232(17) 0.0072(16) -0.0055(16) O3 0.086(2) 0.0556(18) 0.062(2) 0.0086(15) 0.0199(18) -0.0121(16) O2 0.064(2) 0.101(3) 0.057(2) -0.030(2) 0.0149(17) -0.0166(19) C6 0.073(3) 0.068(3) 0.043(2) -0.014(2) 0.019(2) -0.023(2) C11 0.062(2) 0.059(2) 0.045(2) -0.0017(19) 0.0105(19) 0.004(2) C15 0.079(3) 0.069(3) 0.046(2) 0.016(2) 0.025(2) 0.018(3) C16 0.290(17) 0.161(10) 0.123(8) 0.091(8) 0.079(10) 0.129(11) C12 0.067(3) 0.126(6) 0.089(4) -0.035(4) 0.026(3) 0.000(4) C17 0.56(4) 0.201(16) 0.223(18) 0.116(15) 0.15(2) 0.23(2) C13 0.089(6) 0.38(3) 0.189(14) -0.141(14) 0.069(8) -0.091(10) C18 0.248(15) 0.119(8) 0.234(15) 0.093(9) 0.108(12) 0.098(9) C14 0.174(16) 0.70(5) 0.50(5) -0.31(4) 0.22(3) -0.20(2) Pb1 0.05060(13) 0.04269(13) 0.03095(12) -0.00321(4) 0.00220(7) -0.00634(4) O1W 0.072(3) 0.056(2) 0.053(3) 0.000 0.005(2) 0.000 C5 0.062(2) 0.054(2) 0.0396(19) -0.0079(16) 0.0056(16) -0.0212(18) C3 0.055(2) 0.0442(19) 0.0361(18) -0.0066(15) 0.0056(15) -0.0106(16) C2 0.056(2) 0.057(2) 0.0361(18) -0.0041(16) 0.0108(16) -0.0122(18) C1 0.060(2) 0.051(2) 0.043(2) -0.0068(16) 0.0089(17) -0.0172(17) N1 0.063(2) 0.0536(19) 0.0365(16) -0.0093(14) 0.0067(15) -0.0142(16) C4 0.069(3) 0.065(3) 0.046(2) -0.013(2) 0.0182(19) -0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4 C15 1.258(7) . ? O4 Pb1 2.794(4) . ? O1 C11 1.246(6) . ? O1 Pb1 2.673(4) . ? O1 Pb1 2.763(3) 6_566 ? O3 C15 1.251(7) . ? O3 Pb1 2.439(3) . ? O2 C11 1.246(6) . ? O2 Pb1 2.382(4) . ? C6 N1 1.329(6) . ? C6 C4 1.366(6) . ? C6 H6 0.9300 . ? C11 C12 1.504(7) . ? C11 Pb1 2.887(5) . ? C15 C16 1.492(9) . ? C15 Pb1 2.977(5) . ? C16 C17 1.4190(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C12 C13 1.421(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C17 C18 1.452(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C13 C14 1.446(18) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? Pb1 N1 2.568(3) . ? Pb1 O1 2.763(3) 6_565 ? C5 C5 1.321(9) 7_554 ? C5 C3 1.469(5) . ? C5 H5 0.9300 . ? C3 C2 1.383(5) . ? C3 C4 1.404(6) . ? C2 C1 1.379(5) . ? C2 H2 0.9300 . ? C1 N1 1.335(5) . ? C1 H1 0.9300 . ? C4 H4 0.9300 . ? 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 C15 O4 Pb1 85.7(3) . . ? C11 O1 Pb1 86.9(3) . . ? C11 O1 Pb1 137.7(3) . 6_566 ? Pb1 O1 Pb1 132.75(14) . 6_566 ? C15 O3 Pb1 102.8(3) . . ? C11 O2 Pb1 100.7(3) . . ? N1 C6 C4 122.8(4) . . ? N1 C6 H6 118.6 . . ? C4 C6 H6 118.6 . . ? O1 C11 O2 121.5(5) . . ? O1 C11 C12 119.6(5) . . ? O2 C11 C12 118.9(5) . . ? O1 C11 Pb1 67.6(3) . . ? O2 C11 Pb1 54.2(3) . . ? C12 C11 Pb1 171.2(4) . . ? O3 C15 O4 122.1(4) . . ? O3 C15 C16 125.9(7) . . ? O4 C15 C16 111.9(7) . . ? O3 C15 Pb1 53.0(2) . . ? O4 C15 Pb1 69.3(3) . . ? C16 C15 Pb1 172.2(5) . . ? C17 C16 C15 125.2(9) . . ? C17 C16 H16A 106.0 . . ? C15 C16 H16A 106.0 . . ? C17 C16 H16B 106.0 . . ? C15 C16 H16B 106.0 . . ? H16A C16 H16B 106.3 . . ? C13 C12 C11 119.7(7) . . ? C13 C12 H12A 107.4 . . ? C11 C12 H12A 107.4 . . ? C13 C12 H12B 107.4 . . ? C11 C12 H12B 107.4 . . ? H12A C12 H12B 106.9 . . ? C16 C17 C18 115.1(8) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C12 C13 C14 113.7(12) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 Pb1 O3 81.23(15) . . ? O2 Pb1 N1 75.73(12) . . ? O3 Pb1 N1 81.27(12) . . ? O2 Pb1 O1 50.57(11) . . ? O3 Pb1 O1 91.94(12) . . ? N1 Pb1 O1 126.22(12) . . ? O2 Pb1 O1 92.24(14) . 6_565 ? O3 Pb1 O1 155.13(12) . 6_565 ? N1 Pb1 O1 73.86(12) . 6_565 ? O1 Pb1 O1 102.41(7) . 6_565 ? O2 Pb1 O4 108.22(14) . . ? O3 Pb1 O4 49.04(13) . . ? N1 Pb1 O4 126.89(13) . . ? O1 Pb1 O4 79.27(12) . . ? O1 Pb1 O4 153.34(12) 6_565 . ? O2 Pb1 C11 25.10(13) . . ? O3 Pb1 C11 87.53(13) . . ? N1 Pb1 C11 100.69(13) . . ? O1 Pb1 C11 25.53(12) . . ? O1 Pb1 C11 96.69(12) 6_565 . ? O4 Pb1 C11 95.25(13) . . ? O2 Pb1 C15 95.93(16) . . ? O3 Pb1 C15 24.19(14) . . ? N1 Pb1 C15 103.46(15) . . ? O1 Pb1 C15 86.57(12) . . ? O1 Pb1 C15 170.50(12) 6_565 . ? O4 Pb1 C15 24.92(14) . . ? C11 Pb1 C15 92.76(13) . . ? C5 C5 C3 123.8(5) 7_554 . ? C5 C5 H5 118.1 7_554 . ? C3 C5 H5 118.1 . . ? C2 C3 C4 115.9(4) . . ? C2 C3 C5 124.6(4) . . ? C4 C3 C5 119.5(4) . . ? C1 C2 C3 119.7(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C6 N1 C1 117.3(3) . . ? C6 N1 Pb1 124.4(3) . . ? C1 N1 Pb1 117.1(3) . . ? C6 C4 C3 120.6(4) . . ? C6 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.717 _refine_diff_density_min -1.453 _refine_diff_density_rms 0.168 # Attachment 'PbC4_bpe_150K_298K.cif' data_PbC4_bpe_150K _database_code_depnum_ccdc_archive 'CCDC 849296' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate' ; _chemical_name_common 'aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate' _chemical_melting_point ? _chemical_formula_moiety 2(Pb+2),4(C4O2H7-),(C12H10N2),(H2O) _chemical_formula_sum 'C28 H40 N2 O9 Pb2' _chemical_formula_weight 963.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0070 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0120 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.1460 10.7510 '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 18.037(4) _cell_length_b 22.430(5) _cell_length_c 8.1390(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.63(3) _cell_angle_gamma 90.00 _cell_volume 3236.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1831 _exptl_absorpt_coefficient_mu 11.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5773 _exptl_absorpt_correction_T_max 0.8367 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.73790 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean 9.77 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36017 _diffrn_reflns_av_R_equivalents 0.1589 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.50 _reflns_number_total 3668 _reflns_number_gt 3434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2. and ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+15.3466P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3668 _refine_ls_number_parameters 187 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 O4 O 0.4933(3) 0.3932(3) 0.4545(6) 0.0579(12) Uani 1 1 d . . . O1 O 0.3313(3) 0.4790(2) 0.4623(7) 0.0582(12) Uani 1 1 d . . . O3 O 0.4028(3) 0.3379(2) 0.3143(7) 0.0597(12) Uani 1 1 d . . . O2 O 0.2623(3) 0.4241(3) 0.2737(8) 0.0673(15) Uani 1 1 d . . . C6 C 0.2575(4) 0.3406(3) -0.0333(9) 0.0560(17) Uani 1 1 d . . . H6 H 0.2375 0.3399 0.0667 0.067 Uiso 1 1 calc R . . C11 C 0.2695(4) 0.4550(4) 0.4019(11) 0.0549(16) Uani 1 1 d . . . C15 C 0.4637(5) 0.3439(4) 0.4199(9) 0.0607(19) Uani 1 1 d . . . C16 C 0.5070(10) 0.2899(6) 0.4991(18) 0.127(6) Uani 1 1 d . . . H16A H 0.5563 0.2904 0.4617 0.152 Uiso 1 1 calc R . . H16B H 0.5179 0.2974 0.6210 0.152 Uiso 1 1 calc R . . C12 C 0.2035(5) 0.4646(6) 0.4932(15) 0.088(3) Uani 1 1 d . . . H12A H 0.2184 0.4496 0.6090 0.106 Uiso 1 1 calc R . . H12B H 0.1946 0.5080 0.5001 0.106 Uiso 1 1 calc R . . C17 C 0.4803(9) 0.2311(6) 0.478(3) 0.161(8) Uani 1 1 d D . . H17A H 0.4618 0.2238 0.3577 0.193 Uiso 1 1 calc R . . H17B H 0.4370 0.2267 0.5361 0.193 Uiso 1 1 calc R . . C13 C 0.1326(8) 0.4361(10) 0.417(3) 0.193(14) Uani 1 1 d D . . H13A H 0.1293 0.3977 0.4753 0.232 Uiso 1 1 calc R . . H13B H 0.1355 0.4267 0.2997 0.232 Uiso 1 1 calc R . . C18 C 0.5371(10) 0.1855(7) 0.542(3) 0.190(11) Uani 1 1 d D . . H18A H 0.5143 0.1458 0.5240 0.285 Uiso 1 1 calc R . . H18B H 0.5551 0.1918 0.6619 0.285 Uiso 1 1 calc R . . H18C H 0.5795 0.1886 0.4828 0.285 Uiso 1 1 calc R . . C14 C 0.062(2) 0.469(3) 0.417(8) 0.80(10) Uani 1 1 d D . . H14A H 0.0190 0.4427 0.3742 1.200 Uiso 1 1 calc R . . H14B H 0.0602 0.5039 0.3454 1.200 Uiso 1 1 calc R . . H14C H 0.0593 0.4811 0.5312 1.200 Uiso 1 1 calc R . . Pb1 Pb 0.384479(12) 0.438740(9) 0.19720(3) 0.04079(17) Uani 1 1 d . . . O1W O 0.5000 0.5382(3) 0.2500 0.0484(14) Uani 1 2 d S . . C5 C 0.2372(4) 0.2532(3) -0.4278(8) 0.0470(14) Uani 1 1 d . . . H5 H 0.2009 0.2252 -0.4050 0.056 Uiso 1 1 calc R . . C3 C 0.2607(4) 0.2993(3) -0.3048(8) 0.0445(13) Uani 1 1 d . . . C2 C 0.3133(4) 0.3430(3) -0.3213(8) 0.0488(14) Uani 1 1 d . . . H2 H 0.3329 0.3461 -0.4216 0.059 Uiso 1 1 calc R . . C1 C 0.3366(4) 0.3817(3) -0.1913(8) 0.0485(14) Uani 1 1 d . . . H1 H 0.3732 0.4111 -0.2040 0.058 Uiso 1 1 calc R . . N1 N 0.3103(3) 0.3802(3) -0.0466(7) 0.0475(12) Uani 1 1 d . . . C4 C 0.2302(5) 0.3005(3) -0.1566(10) 0.0527(15) Uani 1 1 d . . . H4 H 0.1910 0.2737 -0.1427 0.063 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 O4 0.059(3) 0.071(4) 0.041(3) 0.001(2) 0.004(2) 0.007(3) O1 0.057(3) 0.057(3) 0.058(3) -0.012(2) 0.002(2) 0.001(2) O3 0.083(3) 0.050(3) 0.051(3) 0.000(2) 0.024(3) -0.014(2) O2 0.059(3) 0.079(4) 0.063(4) -0.026(3) 0.008(3) -0.013(3) C6 0.063(4) 0.059(4) 0.047(4) -0.012(3) 0.013(3) -0.014(3) C11 0.051(4) 0.057(4) 0.058(4) -0.001(3) 0.015(3) 0.002(3) C15 0.085(5) 0.056(4) 0.045(4) 0.013(3) 0.022(4) 0.020(4) C16 0.194(16) 0.101(9) 0.095(9) 0.054(8) 0.051(10) 0.071(10) C12 0.065(5) 0.110(8) 0.095(7) -0.025(7) 0.028(5) 0.005(5) C17 0.155(15) 0.086(10) 0.24(2) 0.061(13) 0.038(15) 0.017(10) C13 0.068(8) 0.32(3) 0.21(2) -0.13(2) 0.077(12) -0.076(12) C18 0.193(18) 0.134(13) 0.28(3) 0.125(16) 0.140(18) 0.115(13) C14 0.77(14) 0.45(9) 0.92(18) 0.11(11) -0.53(14) 0.24(9) Pb1 0.0470(2) 0.0385(2) 0.0350(2) -0.00172(7) 0.00267(12) -0.00583(7) O1W 0.054(3) 0.046(3) 0.042(3) 0.000 0.003(3) 0.000 C5 0.048(3) 0.049(3) 0.042(3) -0.004(3) 0.004(2) -0.017(3) C3 0.047(3) 0.043(3) 0.042(3) -0.006(3) 0.005(2) -0.010(2) C2 0.053(3) 0.053(4) 0.041(3) -0.005(3) 0.009(3) -0.013(3) C1 0.055(3) 0.048(3) 0.041(3) -0.002(3) 0.006(3) -0.014(3) N1 0.054(3) 0.046(3) 0.042(3) -0.008(2) 0.008(2) -0.010(2) C4 0.059(4) 0.051(3) 0.048(4) -0.007(3) 0.009(3) -0.018(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 O4 C15 1.237(11) . ? O4 Pb1 2.787(5) . ? O4 Pb1 2.905(6) 2_655 ? O1 C11 1.254(9) . ? O1 Pb1 2.675(6) . ? O1 Pb1 2.702(5) 6_566 ? O3 C15 1.272(10) . ? O3 Pb1 2.454(5) . ? O2 C11 1.239(10) . ? O2 Pb1 2.421(6) . ? C6 N1 1.321(9) . ? C6 C4 1.371(10) . ? C6 H6 0.9500 . ? C11 C12 1.530(11) . ? C11 Pb1 2.912(8) . ? C15 C16 1.519(13) . ? C15 Pb1 2.983(7) . ? C16 C17 1.40(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C12 C13 1.462(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C17 C18 1.472(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C13 C14 1.470(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? Pb1 N1 2.544(5) . ? Pb1 O1 2.702(5) 6_565 ? Pb1 O4 2.905(6) 2_655 ? C5 C5 1.346(13) 7_554 ? C5 C3 1.447(8) . ? C5 H5 0.9500 . ? C3 C2 1.388(9) . ? C3 C4 1.415(10) . ? C2 C1 1.374(9) . ? C2 H2 0.9500 . ? C1 N1 1.350(9) . ? C1 H1 0.9500 . ? C4 H4 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 C15 O4 Pb1 86.7(4) . . ? C15 O4 Pb1 123.2(5) . 2_655 ? Pb1 O4 Pb1 92.06(16) . 2_655 ? C11 O1 Pb1 87.9(4) . . ? C11 O1 Pb1 138.1(5) . 6_566 ? Pb1 O1 Pb1 131.9(2) . 6_566 ? C15 O3 Pb1 101.6(4) . . ? C11 O2 Pb1 100.4(5) . . ? N1 C6 C4 123.3(7) . . ? N1 C6 H6 118.3 . . ? C4 C6 H6 118.3 . . ? O2 C11 O1 121.3(7) . . ? O2 C11 C12 121.1(8) . . ? O1 C11 C12 117.6(8) . . ? O2 C11 Pb1 54.8(4) . . ? O1 C11 Pb1 66.6(4) . . ? C12 C11 Pb1 174.3(7) . . ? O4 C15 O3 122.1(7) . . ? O4 C15 C16 116.7(10) . . ? O3 C15 C16 121.0(10) . . ? O4 C15 Pb1 68.8(4) . . ? O3 C15 Pb1 53.7(3) . . ? C16 C15 Pb1 167.9(7) . . ? C17 C16 C15 124.0(15) . . ? C17 C16 H16A 106.3 . . ? C15 C16 H16A 106.3 . . ? C17 C16 H16B 106.3 . . ? C15 C16 H16B 106.3 . . ? H16A C16 H16B 106.4 . . ? C13 C12 C11 115.5(10) . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C16 C17 C18 114.2(15) . . ? C16 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? C16 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C12 C13 C14 118(3) . . ? C12 C13 H13A 107.7 . . ? C14 C13 H13A 107.7 . . ? C12 C13 H13B 107.7 . . ? C14 C13 H13B 107.7 . . ? H13A C13 H13B 107.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 Pb1 O3 80.7(2) . . ? O2 Pb1 N1 75.97(19) . . ? O3 Pb1 N1 80.84(19) . . ? O2 Pb1 O1 50.17(17) . . ? O3 Pb1 O1 92.35(17) . . ? N1 Pb1 O1 126.02(18) . . ? O2 Pb1 O1 93.1(2) . 6_565 ? O3 Pb1 O1 155.36(18) . 6_565 ? N1 Pb1 O1 74.52(18) . 6_565 ? O1 Pb1 O1 101.93(11) . 6_565 ? O2 Pb1 O4 107.8(2) . . ? O3 Pb1 O4 49.04(18) . . ? N1 Pb1 O4 126.39(19) . . ? O1 Pb1 O4 79.94(16) . . ? O1 Pb1 O4 153.01(17) 6_565 . ? O2 Pb1 O4 149.34(18) . 2_655 ? O3 Pb1 O4 77.43(17) . 2_655 ? N1 Pb1 O4 79.53(17) . 2_655 ? O1 Pb1 O4 151.06(15) . 2_655 ? O1 Pb1 O4 97.91(16) 6_565 2_655 ? O4 Pb1 O4 72.89(18) . 2_655 ? O2 Pb1 C11 24.7(2) . . ? O3 Pb1 C11 87.3(2) . . ? N1 Pb1 C11 100.5(2) . . ? O1 Pb1 C11 25.48(19) . . ? O1 Pb1 C11 97.0(2) 6_565 . ? O4 Pb1 C11 95.3(2) . . ? O4 Pb1 C11 164.5(2) 2_655 . ? O2 Pb1 C15 95.9(2) . . ? O3 Pb1 C15 24.7(2) . . ? N1 Pb1 C15 103.3(2) . . ? O1 Pb1 C15 87.34(19) . . ? O1 Pb1 C15 169.92(19) 6_565 . ? O4 Pb1 C15 24.5(2) . . ? O4 Pb1 C15 72.02(18) 2_655 . ? C11 Pb1 C15 93.1(2) . . ? C5 C5 C3 125.1(8) 7_554 . ? C5 C5 H5 117.4 7_554 . ? C3 C5 H5 117.4 . . ? C2 C3 C4 116.7(6) . . ? C2 C3 C5 123.8(6) . . ? C4 C3 C5 119.5(6) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C6 N1 C1 117.6(6) . . ? C6 N1 Pb1 124.5(5) . . ? C1 N1 Pb1 116.7(4) . . ? C6 C4 C3 119.5(6) . . ? C6 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.480 _refine_diff_density_min -3.693 _refine_diff_density_rms 0.237 #END data_PbC4_4,4'-bipy_298K _database_code_depnum_ccdc_archive 'CCDC 849412' #TrackingRef 'PbC4_bipy_100K_298K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'aqua-4,4'-bipyridine-dilead(II) tetrabutyrate' ; _chemical_name_common "aqua-4,4'-bipyridine-dilead(II) tetrabutyrate" _chemical_melting_point ? _chemical_formula_moiety 2(Pb+2),4(C4O2H7-),(C10H8N2),(H2O) _chemical_formula_sum 'C26 H38 N2 O9 Pb2' _chemical_formula_weight 936.96 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 20.300(4) _cell_length_b 20.143(4) _cell_length_c 8.1470(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.71(3) _cell_angle_gamma 90.00 _cell_volume 3136.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 10.772 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.73790 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean 9.77 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48620 _diffrn_reflns_av_R_equivalents 0.1484 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.50 _reflns_number_total 3528 _reflns_number_gt 3423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2. and ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+5.1190P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3528 _refine_ls_number_parameters 178 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 N1 N 0.1661(2) 0.1473(2) 1.1371(5) 0.0508(9) Uani 1 1 d . . . O2 O 0.1647(2) 0.0178(2) 0.6532(5) 0.0666(10) Uani 1 1 d . . . O4 O 0.0141(2) 0.1165(2) 0.5563(4) 0.0623(9) Uani 1 1 d . . . O3 O 0.0946(2) 0.17766(18) 0.7419(5) 0.0660(9) Uani 1 1 d . . . O1 O 0.2226(2) 0.0848(2) 0.8618(6) 0.0707(11) Uani 1 1 d . . . C5 C 0.1610(2) 0.1358(2) 1.2930(6) 0.0496(9) Uani 1 1 d . . . H5 H 0.1347 0.0996 1.3053 0.060 Uiso 1 1 calc R . . C15 C 0.0432(3) 0.1714(3) 0.6052(6) 0.0531(10) Uani 1 1 d . . . C11 C 0.2199(3) 0.0444(3) 0.7411(6) 0.0541(10) Uani 1 1 d . . . C1 C 0.2032(5) 0.1989(4) 1.1239(7) 0.103(3) Uani 1 1 d . . . H1 H 0.2071 0.2080 1.0156 0.124 Uiso 1 1 calc R . . C2 C 0.2368(5) 0.2408(4) 1.2610(7) 0.107(4) Uani 1 1 d . . . H2 H 0.2624 0.2769 1.2441 0.128 Uiso 1 1 calc R . . C3 C 0.2321(2) 0.2284(2) 1.4234(5) 0.0472(10) Uani 1 1 d . . . C4 C 0.1927(2) 0.1745(2) 1.4371(5) 0.0492(9) Uani 1 1 d . . . H4 H 0.1875 0.1643 1.5433 0.059 Uiso 1 1 calc R . . C16 C 0.0155(5) 0.2335(4) 0.5033(12) 0.112(3) Uani 1 1 d . . . H16A H 0.0029 0.2215 0.3812 0.134 Uiso 1 1 calc R . . H16B H -0.0279 0.2438 0.5229 0.134 Uiso 1 1 calc R . . C12 C 0.2862(4) 0.0298(5) 0.7060(11) 0.100(3) Uani 1 1 d . . . H12A H 0.2943 -0.0176 0.7201 0.119 Uiso 1 1 calc R . . H12B H 0.2779 0.0399 0.5842 0.119 Uiso 1 1 calc R . . C13 C 0.3497(6) 0.0622(8) 0.806(3) 0.179(8) Uani 1 1 d . . . H13A H 0.3578 0.0553 0.9287 0.214 Uiso 1 1 calc R . . H13B H 0.3449 0.1096 0.7832 0.214 Uiso 1 1 calc R . . C17 C 0.0516(12) 0.2915(6) 0.523(3) 0.211(9) Uani 1 1 d D . . H17A H 0.0201 0.3228 0.4445 0.253 Uiso 1 1 calc R . . H17B H 0.0889 0.2834 0.4761 0.253 Uiso 1 1 calc R . . C14 C 0.4118(7) 0.0368(12) 0.762(3) 0.233(9) Uani 1 1 d . . . H14A H 0.4534 0.0593 0.8333 0.350 Uiso 1 1 calc R . . H14B H 0.4048 0.0450 0.6415 0.350 Uiso 1 1 calc R . . H14C H 0.4169 -0.0100 0.7847 0.350 Uiso 1 1 calc R . . C18 C 0.0830(14) 0.3265(12) 0.681(4) 0.47(4) Uani 1 1 d D . . H18A H 0.1107 0.3623 0.6621 0.705 Uiso 1 1 calc R . . H18B H 0.1124 0.2969 0.7675 0.705 Uiso 1 1 calc R . . H18C H 0.0472 0.3440 0.7217 0.705 Uiso 1 1 calc R . . O1W O 0.0000 -0.0433(2) 0.7500 0.0599(12) Uani 1 2 d S . . Pb1 Pb 0.106791(7) 0.069683(7) 0.876075(16) 0.03942(12) 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 N1 0.064(2) 0.058(2) 0.0268(16) -0.0097(15) 0.0114(15) -0.0216(19) O2 0.062(2) 0.076(2) 0.058(2) -0.0203(19) 0.0159(17) -0.0060(19) O4 0.074(2) 0.072(2) 0.0395(16) -0.0048(15) 0.0168(15) -0.0082(18) O3 0.082(2) 0.060(2) 0.0461(18) 0.0066(15) 0.0074(17) -0.0154(18) O1 0.062(2) 0.087(3) 0.068(3) -0.026(2) 0.028(2) -0.019(2) C5 0.064(2) 0.047(2) 0.039(2) -0.0087(16) 0.0184(18) -0.0187(19) C15 0.067(3) 0.058(3) 0.038(2) 0.0096(18) 0.022(2) -0.001(2) C11 0.056(2) 0.060(3) 0.048(2) -0.002(2) 0.021(2) 0.000(2) C1 0.165(7) 0.120(5) 0.032(2) -0.029(3) 0.044(3) -0.104(6) C2 0.173(8) 0.120(6) 0.038(3) -0.031(3) 0.049(4) -0.112(6) C3 0.062(2) 0.054(2) 0.0258(17) -0.0119(16) 0.0157(16) -0.0241(19) C4 0.067(2) 0.053(2) 0.0302(18) -0.0039(16) 0.0199(17) -0.018(2) C16 0.123(7) 0.097(6) 0.100(6) 0.058(5) 0.018(5) 0.009(5) C12 0.071(4) 0.137(7) 0.099(5) -0.030(5) 0.041(4) 0.004(4) C13 0.070(6) 0.29(2) 0.180(15) -0.036(11) 0.052(8) -0.015(7) C17 0.30(2) 0.077(7) 0.207(18) 0.054(8) 0.021(17) 0.006(10) C14 0.086(8) 0.36(3) 0.27(3) 0.02(2) 0.086(12) -0.012(13) C18 0.29(3) 0.18(2) 0.99(11) -0.19(5) 0.28(5) -0.07(2) O1W 0.084(3) 0.043(2) 0.046(2) 0.000 0.012(2) 0.000 Pb1 0.04626(16) 0.04155(16) 0.02688(14) -0.00548(4) 0.00765(9) -0.00719(4) _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 N1 C1 1.310(7) . ? N1 C5 1.328(6) . ? N1 Pb1 2.586(4) . ? O2 C11 1.231(6) . ? O2 Pb1 2.685(4) . ? O4 C15 1.254(6) . ? O3 C15 1.249(6) . ? O3 Pb1 2.409(4) . ? O1 C11 1.263(7) . ? O1 Pb1 2.411(4) . ? C5 C4 1.375(6) . ? C5 H5 0.9300 . ? C15 C16 1.502(8) . ? C11 C12 1.497(8) . ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.375(6) . ? C3 C3 1.493(7) 7_558 ? C4 H4 0.9300 . ? C16 C17 1.360(17) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C12 C13 1.428(15) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.51(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C17 C18 1.420(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 C1 N1 C5 116.6(4) . . ? C1 N1 Pb1 122.2(3) . . ? C5 N1 Pb1 121.1(3) . . ? C11 O2 Pb1 87.5(3) . . ? C15 O3 Pb1 103.9(3) . . ? C11 O1 Pb1 99.7(3) . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? O3 C15 O4 122.4(5) . . ? O3 C15 C16 117.0(6) . . ? O4 C15 C16 120.6(6) . . ? O2 C11 O1 121.7(5) . . ? O2 C11 C12 120.3(5) . . ? O1 C11 C12 118.0(5) . . ? N1 C1 C2 124.0(5) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 116.8(4) . . ? C4 C3 C3 121.6(4) . 7_558 ? C2 C3 C3 121.6(5) . 7_558 ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C17 C16 C15 124.3(10) . . ? C17 C16 H16A 106.3 . . ? C15 C16 H16A 106.3 . . ? C17 C16 H16B 106.3 . . ? C15 C16 H16B 106.3 . . ? H16A C16 H16B 106.4 . . ? C13 C12 C11 120.0(8) . . ? C13 C12 H12A 107.3 . . ? C11 C12 H12A 107.3 . . ? C13 C12 H12B 107.3 . . ? C11 C12 H12B 107.3 . . ? H12A C12 H12B 106.9 . . ? C12 C13 C14 112.2(14) . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C16 C17 C18 126.4(18) . . ? C16 C17 H17A 105.7 . . ? C18 C17 H17A 105.7 . . ? C16 C17 H17B 105.7 . . ? C18 C17 H17B 105.7 . . ? H17A C17 H17B 106.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 Pb1 O1 79.43(16) . . ? O3 Pb1 N1 77.03(13) . . ? O1 Pb1 N1 76.86(14) . . ? O3 Pb1 O2 92.63(14) . . ? O1 Pb1 O2 50.25(13) . . ? N1 Pb1 O2 127.09(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.327 _refine_diff_density_min -2.868 _refine_diff_density_rms 0.222