Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Nag, K.' 'Adhikary, Bibhutosh' 'Bag, Pradip' 'Dutta, Bula' 'Florke, Ulrich' _publ_contact_author_name 'Prof K Nag' _publ_contact_author_address ; Dept of Inorganic Chemistry Indian Association of the Cultivati Culcutta 700032 INDIA ; _publ_contact_author_email ICKN@MAHENDRA.IACS.RES.IN _publ_contact_author_fax '+49 5251 60 3423' _publ_contact_author_phone '+49 5251 60 2496' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Organized assemblies of lead (II) complexes of a tetraiminodiphenol macrocyclic ligand: Manifestation of weak metal-anion interaction and directional influence of anion. ; _publ_contact_letter ; DATE 13-02-2002 Paper Ref.: B201608G This is the CIF file with crystallographic data for the compounds 1, 2, 3 from the manuscript ; data_1 _database_code_CSD 179593 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H28 N4 O2 Pb)(Cl O4)2' _chemical_formula_sum 'C24 H28 Cl2 N4 O10 Pb' _chemical_formula_weight 810.59 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Hexagonal' _symmetry_space_group_name_H-M 'R-3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 35.124(5) _cell_length_b 35.124(5) _cell_length_c 12.095(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12922(4) _cell_formula_units_Z 18 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.57 _cell_measurement_theta_max 12.75 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7128 _exptl_absorpt_coefficient_mu 6.122 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.382 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 3 _diffrn_reflns_number 6919 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.2542 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.49 _reflns_number_total 5831 _reflns_number_gt 1501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000043(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5831 _refine_ls_number_parameters 371 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2748 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2227 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.869 _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 0.10826(3) 0.14098(3) -0.09861(8) 0.0819(4) Uani 1 1 d . . . O1 O 0.1781(5) 0.1924(5) -0.0219(11) 0.080(4) Uani 1 1 d . . . O2 O 0.0956(4) 0.1942(4) -0.0149(10) 0.072(4) Uani 1 1 d . . . N1 N 0.1638(6) 0.1631(6) -0.2545(15) 0.079(6) Uani 1 1 d . . . N2 N 0.0877(5) 0.1747(7) -0.2513(15) 0.078(5) Uani 1 1 d . . . N3 N 0.1161(5) 0.2277(6) 0.1855(14) 0.067(5) Uani 1 1 d . . . H3A H 0.1080 0.2046 0.1445 0.081 Uiso 1 1 calc R . . N4 N 0.2016(6) 0.2188(6) 0.1777(15) 0.084(6) Uani 1 1 d . . . H4A H 0.1800 0.2017 0.1341 0.100 Uiso 1 1 calc R . . C1 C 0.1449(8) 0.1412(7) -0.3582(18) 0.098(8) Uani 1 1 d . . . H1A H 0.1251 0.1099 -0.3439 0.117 Uiso 1 1 calc R . . H1B H 0.1686 0.1439 -0.4064 0.117 Uiso 1 1 calc R . . C2 C 0.1196(8) 0.1595(8) -0.4185(19) 0.100(8) Uani 1 1 d . . . H2A H 0.1385 0.1914 -0.4266 0.120 Uiso 1 1 calc R . . H2B H 0.1121 0.1467 -0.4928 0.120 Uiso 1 1 calc R . . C3 C 0.0785(8) 0.1503(8) -0.3600(19) 0.105(8) Uani 1 1 d . . . H3B H 0.0607 0.1186 -0.3461 0.126 Uiso 1 1 calc R . . H3C H 0.0614 0.1588 -0.4076 0.126 Uiso 1 1 calc R . . C4 C 0.0868(7) 0.2093(9) -0.2513(19) 0.082(7) Uani 1 1 d . . . H4B H 0.0779 0.2160 -0.3183 0.098 Uiso 1 1 calc R . . C5 C 0.0975(6) 0.2413(7) -0.1635(18) 0.066(6) Uani 1 1 d . . . C6 C 0.1041(6) 0.2823(9) -0.190(2) 0.091(8) Uani 1 1 d . . . H6A H 0.1019 0.2883 -0.2648 0.109 Uiso 1 1 calc R . . C7 C 0.1138(7) 0.3158(8) -0.112(2) 0.077(7) Uani 1 1 d . . . C8 C 0.1183(6) 0.3592(7) -0.1514(19) 0.095(8) Uani 1 1 d . . . H8A H 0.1255 0.3790 -0.0890 0.142 Uiso 1 1 calc R . . H8B H 0.0908 0.3538 -0.1841 0.142 Uiso 1 1 calc R . . H8C H 0.1416 0.3724 -0.2061 0.142 Uiso 1 1 calc R . . C9 C 0.1200(7) 0.3071(8) -0.004(2) 0.087(7) Uani 1 1 d . . . H9A H 0.1285 0.3294 0.0488 0.105 Uiso 1 1 calc R . . C10 C 0.1141(5) 0.2666(5) 0.0282(17) 0.051(5) Uani 1 1 d . . . C11 C 0.1025(6) 0.2320(7) -0.0493(17) 0.056(5) Uani 1 1 d . . . C12 C 0.1217(6) 0.2628(7) 0.1401(16) 0.065(6) Uani 1 1 d . . . H12A H 0.1316 0.2879 0.1847 0.078 Uiso 1 1 calc R . . C13 C 0.1226(7) 0.2247(7) 0.3039(16) 0.082(7) Uani 1 1 d . . . H13A H 0.1053 0.1939 0.3271 0.098 Uiso 1 1 calc R . . H13B H 0.1117 0.2415 0.3446 0.098 Uiso 1 1 calc R . . C14 C 0.1712(7) 0.2423(7) 0.3343(17) 0.078(6) Uani 1 1 d . . . H14A H 0.1882 0.2717 0.3018 0.094 Uiso 1 1 calc R . . H14B H 0.1737 0.2460 0.4147 0.094 Uiso 1 1 calc R . . C15 C 0.1938(6) 0.2161(6) 0.3013(15) 0.064(5) Uani 1 1 d . . . H15A H 0.2219 0.2280 0.3402 0.077 Uiso 1 1 calc R . . H15B H 0.1753 0.1853 0.3232 0.077 Uiso 1 1 calc R . . C16 C 0.2382(8) 0.2449(7) 0.1365(19) 0.072(6) Uani 1 1 d . . . H16A H 0.2601 0.2647 0.1849 0.087 Uiso 1 1 calc R . . C17 C 0.2497(7) 0.2472(7) 0.0221(18) 0.064(6) Uani 1 1 d . . . C18 C 0.2942(7) 0.2764(7) -0.014(2) 0.086(7) Uani 1 1 d . . . H18A H 0.3151 0.2957 0.0367 0.103 Uiso 1 1 calc R . . C19 C 0.3062(8) 0.2764(8) -0.121(2) 0.077(7) Uani 1 1 d . . . C20 C 0.3569(7) 0.3065(8) -0.150(2) 0.116(9) Uani 1 1 d . . . H20A H 0.3723 0.3244 -0.0860 0.174 Uiso 1 1 calc R . . H20B H 0.3601 0.3253 -0.2117 0.174 Uiso 1 1 calc R . . H20C H 0.3692 0.2881 -0.1687 0.174 Uiso 1 1 calc R . . C21 C 0.2768(8) 0.2481(8) -0.192(2) 0.082(7) Uani 1 1 d . . . H21A H 0.2865 0.2473 -0.2640 0.098 Uiso 1 1 calc R . . C22 C 0.2319(8) 0.2190(8) -0.167(2) 0.079(7) Uani 1 1 d . . . C23 C 0.2181(8) 0.2182(8) -0.058(2) 0.076(7) Uani 1 1 d . . . C24 C 0.2043(10) 0.1913(8) -0.256(2) 0.092(8) Uani 1 1 d . . . H24A H 0.2184 0.1948 -0.3243 0.110 Uiso 1 1 calc R . . Cl10 Cl 0.2361(2) 0.3676(2) 0.1761(5) 0.099(2) Uani 1 1 d D . . O11 O 0.2306(5) 0.3326(4) 0.1120(12) 0.132(7) Uani 1 1 d D . . O12 O 0.2302(5) 0.3583(5) 0.2890(10) 0.141(7) Uani 1 1 d D . . O13 O 0.2023(5) 0.3782(5) 0.1434(13) 0.139(7) Uani 1 1 d D . . O14 O 0.2767(4) 0.4060(4) 0.1559(11) 0.100(5) Uani 1 1 d D . . Cl20 Cl -0.0241(3) 0.0797(3) -0.1943(8) 0.175(4) Uani 1 1 d D . . O21 O -0.0636(5) 0.0427(6) -0.1540(19) 0.296(19) Uani 1 1 d D . . O22 O -0.0261(6) 0.0831(7) -0.3132(12) 0.188(10) Uani 1 1 d D . . O23 O 0.0145(5) 0.0776(6) -0.1605(16) 0.204(12) Uani 1 1 d D . . O24 O -0.0208(7) 0.1199(5) -0.1447(15) 0.183(10) Uani 1 1 d 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 0.1014(8) 0.0691(7) 0.0748(6) 0.0019(6) -0.0029(6) 0.0422(6) O1 0.082(11) 0.105(12) 0.054(9) -0.001(9) -0.005(9) 0.047(10) O2 0.088(10) 0.080(10) 0.055(9) -0.002(8) 0.002(8) 0.047(9) N1 0.096(14) 0.068(13) 0.072(13) -0.030(11) -0.001(13) 0.040(12) N2 0.063(12) 0.115(16) 0.073(13) -0.002(13) -0.012(10) 0.057(12) N3 0.057(11) 0.073(12) 0.067(12) 0.003(10) 0.009(10) 0.029(10) N4 0.087(15) 0.118(17) 0.075(14) 0.014(13) 0.003(12) 0.073(14) C1 0.16(2) 0.081(17) 0.062(16) -0.029(14) 0.001(16) 0.064(18) C2 0.12(2) 0.11(2) 0.065(16) -0.011(15) 0.001(17) 0.053(19) C3 0.12(2) 0.13(2) 0.074(18) -0.028(17) -0.043(17) 0.067(19) C4 0.083(17) 0.12(2) 0.065(16) 0.020(16) 0.017(13) 0.067(17) C5 0.071(15) 0.083(16) 0.063(15) 0.012(13) 0.019(12) 0.053(13) C6 0.074(16) 0.12(2) 0.11(2) 0.035(19) 0.003(15) 0.067(17) C7 0.068(15) 0.082(18) 0.11(2) 0.022(17) 0.017(15) 0.057(15) C8 0.065(15) 0.099(18) 0.11(2) 0.039(16) 0.019(14) 0.037(14) C9 0.069(16) 0.10(2) 0.090(19) 0.006(16) 0.002(15) 0.039(15) C10 0.047(12) 0.027(10) 0.073(15) 0.009(11) -0.003(11) 0.014(9) C11 0.050(12) 0.066(14) 0.066(14) 0.002(12) -0.016(11) 0.039(12) C12 0.088(16) 0.067(15) 0.049(13) -0.011(12) -0.009(12) 0.045(13) C13 0.080(17) 0.102(18) 0.051(14) -0.002(13) -0.009(13) 0.037(14) C14 0.102(18) 0.081(16) 0.059(14) -0.008(12) 0.008(13) 0.052(14) C15 0.062(13) 0.082(15) 0.049(12) 0.014(11) 0.018(11) 0.038(12) C16 0.087(18) 0.075(16) 0.069(16) -0.004(13) -0.007(14) 0.051(15) C17 0.068(15) 0.070(15) 0.068(15) -0.026(13) -0.024(13) 0.045(13) C18 0.058(15) 0.092(18) 0.10(2) 0.036(16) -0.002(14) 0.032(14) C19 0.11(2) 0.082(17) 0.075(17) 0.014(15) 0.011(17) 0.072(17) C20 0.085(18) 0.16(2) 0.11(2) 0.016(19) 0.055(16) 0.059(18) C21 0.074(17) 0.103(19) 0.085(18) -0.013(16) 0.009(15) 0.055(15) C22 0.084(19) 0.077(17) 0.10(2) -0.004(16) -0.002(17) 0.059(16) C23 0.095(19) 0.086(18) 0.078(18) 0.019(15) -0.003(16) 0.067(17) C24 0.15(3) 0.065(17) 0.09(2) 0.002(16) 0.01(2) 0.073(18) Cl10 0.104(5) 0.098(5) 0.070(4) -0.004(4) -0.010(4) 0.032(4) O11 0.198(19) 0.108(14) 0.121(15) -0.010(12) 0.003(14) 0.100(14) O12 0.159(18) 0.136(16) 0.096(14) 0.037(13) -0.007(13) 0.052(13) O13 0.127(15) 0.192(19) 0.119(16) -0.007(14) -0.024(13) 0.096(15) O14 0.079(11) 0.085(11) 0.097(12) 0.021(10) 0.020(10) 0.012(9) Cl20 0.190(11) 0.194(11) 0.137(9) 0.011(8) -0.001(8) 0.093(9) O21 0.118(19) 0.26(3) 0.33(4) 0.09(3) 0.08(2) -0.044(19) O22 0.18(2) 0.32(3) 0.083(15) -0.016(18) -0.010(15) 0.15(2) O23 0.121(17) 0.26(3) 0.21(3) 0.04(2) -0.047(18) 0.078(18) O24 0.32(3) 0.159(19) 0.143(18) -0.030(16) 0.022(19) 0.18(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 Pb1 O2 2.356(13) . ? Pb1 O1 2.388(14) . ? Pb1 N2 2.488(17) . ? Pb1 N1 2.539(18) . ? O1 C23 1.31(2) . ? O2 C11 1.29(2) . ? N1 C24 1.26(3) . ? N1 C1 1.45(2) . ? N2 C4 1.23(2) . ? N2 C3 1.51(3) . ? N3 C12 1.27(2) . ? N3 C13 1.46(2) . ? N4 C16 1.25(2) . ? N4 C15 1.51(2) . ? C1 C2 1.52(3) . ? C2 C3 1.49(3) . ? C4 C5 1.45(3) . ? C5 C6 1.38(3) . ? C5 C11 1.45(2) . ? C6 C7 1.41(3) . ? C7 C9 1.38(3) . ? C7 C8 1.53(3) . ? C9 C10 1.39(2) . ? C10 C12 1.40(2) . ? C10 C11 1.42(2) . ? C13 C14 1.54(2) . ? C14 C15 1.54(2) . ? C16 C17 1.43(3) . ? C17 C23 1.44(3) . ? C17 C18 1.44(3) . ? C18 C19 1.36(3) . ? C19 C21 1.33(3) . ? C19 C20 1.59(3) . ? C21 C22 1.42(3) . ? C22 C23 1.40(3) . ? C22 C24 1.45(3) . ? Cl10 O11 1.382(11) . ? Cl10 O12 1.395(12) . ? Cl10 O14 1.410(11) . ? Cl10 O13 1.466(12) . ? Cl20 O21 1.430(13) . ? Cl20 O22 1.447(13) . ? Cl20 O23 1.454(13) . ? Cl20 O24 1.485(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 Pb1 O1 76.3(5) . . ? O2 Pb1 N2 74.1(6) . . ? O1 Pb1 N2 111.2(5) . . ? O2 Pb1 N1 119.8(5) . . ? O1 Pb1 N1 73.5(5) . . ? N2 Pb1 N1 70.4(6) . . ? C23 O1 Pb1 137.2(14) . . ? C11 O2 Pb1 131.6(13) . . ? C24 N1 C1 116(2) . . ? C24 N1 Pb1 129.9(17) . . ? C1 N1 Pb1 113.8(14) . . ? C4 N2 C3 117(2) . . ? C4 N2 Pb1 128.8(17) . . ? C3 N2 Pb1 114.0(14) . . ? C12 N3 C13 122.6(19) . . ? C16 N4 C15 122(2) . . ? N1 C1 C2 113.6(18) . . ? C3 C2 C1 113(2) . . ? C2 C3 N2 112.3(19) . . ? N2 C4 C5 130(2) . . ? C6 C5 C11 119(2) . . ? C6 C5 C4 119(2) . . ? C11 C5 C4 122.3(19) . . ? C5 C6 C7 124(2) . . ? C9 C7 C6 116(2) . . ? C9 C7 C8 124(3) . . ? C6 C7 C8 119(2) . . ? C7 C9 C10 122(2) . . ? C9 C10 C12 116(2) . . ? C9 C10 C11 121.3(19) . . ? C12 C10 C11 123.0(17) . . ? O2 C11 C10 119.4(18) . . ? O2 C11 C5 123.8(19) . . ? C10 C11 C5 116.8(18) . . ? N3 C12 C10 124.4(19) . . ? N3 C13 C14 112.8(17) . . ? C15 C14 C13 119.9(18) . . ? N4 C15 C14 110.6(15) . . ? N4 C16 C17 126(2) . . ? C16 C17 C23 121(2) . . ? C16 C17 C18 121(2) . . ? C23 C17 C18 118(2) . . ? C19 C18 C17 121(2) . . ? C21 C19 C18 119(2) . . ? C21 C19 C20 123(2) . . ? C18 C19 C20 117(2) . . ? C19 C21 C22 125(2) . . ? C23 C22 C21 117(2) . . ? C23 C22 C24 125(2) . . ? C21 C22 C24 117(3) . . ? O1 C23 C22 125(2) . . ? O1 C23 C17 116(2) . . ? C22 C23 C17 119(2) . . ? N1 C24 C22 129(3) . . ? O11 Cl10 O12 113.8(9) . . ? O11 Cl10 O14 112.2(8) . . ? O12 Cl10 O14 110.8(8) . . ? O11 Cl10 O13 107.7(8) . . ? O12 Cl10 O13 106.2(8) . . ? O14 Cl10 O13 105.6(8) . . ? O21 Cl20 O22 110.4(10) . . ? O21 Cl20 O23 111.4(10) . . ? O22 Cl20 O23 111.7(10) . . ? O21 Cl20 O24 107.8(10) . . ? O22 Cl20 O24 107.8(9) . . ? O23 Cl20 O24 107.6(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.342 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.151 #===END data_2 _database_code_CSD 179594 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H28 N4 O2 Pb)(N O3)2' _chemical_formula_sum 'C24 H28 N6 O8 Pb' _chemical_formula_weight 735.71 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.277(1) _cell_length_b 17.922(3) _cell_length_c 14.368(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.08(1) _cell_angle_gamma 90.00 _cell_volume 2644.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 7.572 _cell_measurement_theta_max 17.562 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 6.439 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% '<1' _diffrn_reflns_number 7520 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6082 _reflns_number_gt 4298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00068(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6082 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 0.17002(2) 0.197771(11) 0.611042(14) 0.02791(8) Uani 1 1 d . . . N1 N -0.0531(4) 0.1362(2) 0.5749(3) 0.0290(11) Uani 1 1 d . . . N2 N -0.0048(4) 0.2449(2) 0.7190(3) 0.0283(10) Uani 1 1 d . . . N3 N 0.4599(4) 0.1126(2) 0.8110(3) 0.0282(10) Uani 1 1 d . . . H3C H 0.4202 0.1402 0.7691 0.034 Uiso 1 1 calc R . . N4 N 0.3991(4) -0.0122(2) 0.6718(3) 0.0300(11) Uani 1 1 d . . . H4A H 0.3677 0.0322 0.6610 0.036 Uiso 1 1 calc R . . O1 O 0.1902(4) 0.0670(2) 0.6329(3) 0.0405(11) Uani 1 1 d . . . O2 O 0.2539(3) 0.1919(2) 0.7662(2) 0.0325(8) Uani 1 1 d . . . C1 C -0.1502(5) 0.1913(3) 0.5412(4) 0.0332(12) Uani 1 1 d . . . H1A H -0.2213 0.1653 0.5075 0.040 Uiso 1 1 calc R . . H1B H -0.1095 0.2254 0.4975 0.040 Uiso 1 1 calc R . . C2 C -0.2057(5) 0.2363(3) 0.6201(4) 0.0345(14) Uani 1 1 d . . . H2A H -0.2779 0.2667 0.5946 0.041 Uiso 1 1 calc R . . H2B H -0.2417 0.2016 0.6652 0.041 Uiso 1 1 calc R . . C3 C -0.1097(5) 0.2873(3) 0.6712(4) 0.0322(13) Uani 1 1 d . . . H3A H -0.0719 0.3217 0.6266 0.039 Uiso 1 1 calc R . . H3B H -0.1557 0.3169 0.7169 0.039 Uiso 1 1 calc R . . C4 C -0.0176(6) 0.2293(3) 0.8043(4) 0.0348(14) Uani 1 1 d . . . H4 H -0.0913 0.2492 0.8323 0.042 Uiso 1 1 calc R . . C5 C 0.0685(5) 0.1840(3) 0.8637(4) 0.0308(13) Uani 1 1 d . . . C6 C 0.0205(6) 0.1578(3) 0.9466(4) 0.0387(15) Uani 1 1 d . . . H6 H -0.0635 0.1730 0.9623 0.046 Uiso 1 1 calc R . . C7 C 0.0886(6) 0.1103(3) 1.0084(4) 0.0383(15) Uani 1 1 d . . . C8 C 0.0292(7) 0.0815(4) 1.0952(4) 0.0565(19) Uani 1 1 d . . . H8A H -0.0591 0.1000 1.0987 0.085 Uiso 1 1 calc R . . H8B H 0.0804 0.0984 1.1493 0.085 Uiso 1 1 calc R . . H8C H 0.0281 0.0274 1.0939 0.085 Uiso 1 1 calc R . . C9 C 0.2145(6) 0.0932(3) 0.9849(4) 0.0347(14) Uani 1 1 d . . . H9 H 0.2648 0.0625 1.0252 0.042 Uiso 1 1 calc R . . C10 C 0.2698(6) 0.1194(3) 0.9040(4) 0.0270(12) Uani 1 1 d . . . C11 C 0.1988(6) 0.1666(3) 0.8400(4) 0.0303(13) Uani 1 1 d . . . C12 C 0.4002(6) 0.0961(3) 0.8857(4) 0.0302(13) Uani 1 1 d . . . H12 H 0.4447 0.0669 0.9309 0.036 Uiso 1 1 calc R . . C13 C 0.5931(5) 0.0866(3) 0.7942(4) 0.0347(14) Uani 1 1 d . . . H13A H 0.6488 0.0974 0.8493 0.042 Uiso 1 1 calc R . . H13B H 0.6272 0.1146 0.7418 0.042 Uiso 1 1 calc R . . C14 C 0.6004(6) 0.0038(3) 0.7729(4) 0.0375(14) Uani 1 1 d . . . H14A H 0.5574 -0.0234 0.8223 0.045 Uiso 1 1 calc R . . H14B H 0.6923 -0.0111 0.7752 0.045 Uiso 1 1 calc R . . C15 C 0.5398(5) -0.0204(3) 0.6795(4) 0.0361(14) Uani 1 1 d . . . H15A H 0.5786 0.0091 0.6302 0.043 Uiso 1 1 calc R . . H15B H 0.5619 -0.0728 0.6689 0.043 Uiso 1 1 calc R . . C16 C 0.3175(5) -0.0665(3) 0.6800(3) 0.0269(12) Uani 1 1 d . . . H16 H 0.3523 -0.1134 0.6964 0.032 Uiso 1 1 calc R . . C17 C 0.1797(5) -0.0617(3) 0.6663(3) 0.0241(12) Uani 1 1 d . . . C18 C 0.1070(5) -0.1266(3) 0.6751(3) 0.0272(12) Uani 1 1 d . . . H18 H 0.1495 -0.1705 0.6951 0.033 Uiso 1 1 calc R . . C19 C -0.0241(5) -0.1286(3) 0.6555(3) 0.0267(12) Uani 1 1 d . . . C20 C -0.1005(6) -0.2001(3) 0.6664(4) 0.0401(14) Uani 1 1 d . . . H20A H -0.1913 -0.1913 0.6490 0.060 Uiso 1 1 calc R . . H20B H -0.0934 -0.2165 0.7307 0.060 Uiso 1 1 calc R . . H20C H -0.0658 -0.2383 0.6264 0.060 Uiso 1 1 calc R . . C21 C -0.0830(5) -0.0624(3) 0.6263(3) 0.0269(12) Uani 1 1 d . . . H21 H -0.1729 -0.0633 0.6118 0.032 Uiso 1 1 calc R . . C22 C -0.0180(5) 0.0046(3) 0.6172(3) 0.0288(12) Uani 1 1 d . . . C23 C 0.1206(5) 0.0068(3) 0.6385(3) 0.0273(12) Uani 1 1 d . . . C24 C -0.0916(5) 0.0691(3) 0.5834(4) 0.0310(13) Uani 1 1 d . . . H24 H -0.1791 0.0600 0.5655 0.037 Uiso 1 1 calc R . . N10 N 0.4556(5) 0.1444(3) 0.5288(3) 0.0347(11) Uani 1 1 d . . . O11 O 0.4366(4) 0.1578(3) 0.6130(3) 0.0453(11) Uani 1 1 d . . . O12 O 0.5572(5) 0.1138(3) 0.5073(3) 0.0654(15) Uani 1 1 d . . . O13 O 0.3692(4) 0.1592(3) 0.4686(3) 0.0509(12) Uani 1 1 d . . . N20 N 0.1573(5) 0.3769(3) 0.5607(4) 0.0397(13) Uani 1 1 d . . . O21 O 0.1471(7) 0.3343(3) 0.4956(3) 0.105(3) Uani 1 1 d . . . O22 O 0.1199(6) 0.4403(3) 0.5497(4) 0.093(2) Uani 1 1 d . . . O23 O 0.2029(5) 0.3548(3) 0.6361(3) 0.0603(14) 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 0.03211(11) 0.02351(10) 0.02828(11) 0.00349(11) 0.00337(7) 0.00191(13) N1 0.033(3) 0.026(2) 0.028(2) -0.002(2) -0.001(2) 0.009(2) N2 0.031(3) 0.025(2) 0.029(2) -0.001(2) 0.003(2) -0.001(2) N3 0.034(3) 0.026(2) 0.024(2) -0.0039(19) -0.005(2) -0.003(2) N4 0.029(3) 0.026(2) 0.035(3) -0.003(2) 0.001(2) 0.002(2) O1 0.035(2) 0.022(2) 0.064(3) 0.0048(19) -0.005(2) -0.0015(19) O2 0.037(2) 0.035(2) 0.0252(18) 0.0022(19) 0.0023(16) 0.002(2) C1 0.032(3) 0.033(3) 0.035(3) 0.005(3) -0.002(2) 0.003(3) C2 0.033(3) 0.026(3) 0.044(3) 0.007(3) 0.005(3) 0.009(3) C3 0.033(3) 0.021(3) 0.043(3) -0.002(2) 0.000(3) 0.008(2) C4 0.040(3) 0.032(3) 0.034(3) -0.009(3) 0.007(3) 0.006(3) C5 0.040(3) 0.025(3) 0.028(3) -0.006(2) 0.000(2) 0.000(3) C6 0.038(3) 0.050(4) 0.029(3) -0.008(3) 0.006(3) -0.001(3) C7 0.047(4) 0.045(4) 0.024(3) -0.002(3) 0.005(3) -0.005(3) C8 0.064(5) 0.067(5) 0.039(4) 0.005(4) 0.010(3) -0.003(4) C9 0.044(4) 0.030(3) 0.030(3) 0.001(3) -0.008(3) -0.010(3) C10 0.038(3) 0.017(3) 0.026(3) -0.002(2) 0.003(2) -0.002(3) C11 0.039(3) 0.025(3) 0.027(3) -0.011(2) 0.002(3) -0.005(3) C12 0.039(3) 0.022(3) 0.030(3) -0.005(2) -0.005(3) 0.003(3) C13 0.027(3) 0.038(3) 0.038(3) -0.007(3) -0.004(3) -0.001(3) C14 0.031(3) 0.041(4) 0.041(3) -0.003(3) -0.005(3) 0.006(3) C15 0.027(3) 0.036(3) 0.045(4) -0.003(3) -0.001(3) 0.006(3) C16 0.032(3) 0.022(3) 0.027(3) -0.002(2) -0.001(2) 0.006(3) C17 0.030(3) 0.022(3) 0.020(3) -0.001(2) -0.010(2) 0.001(2) C18 0.032(3) 0.025(3) 0.024(3) -0.001(2) -0.004(2) 0.005(3) C19 0.031(3) 0.028(3) 0.021(3) -0.001(2) 0.004(2) -0.002(3) C20 0.043(3) 0.034(3) 0.044(3) 0.008(3) 0.002(3) -0.007(3) C21 0.030(3) 0.031(3) 0.019(3) -0.006(2) 0.001(2) 0.001(3) C22 0.032(3) 0.031(3) 0.023(3) 0.000(2) 0.003(2) 0.004(3) C23 0.032(3) 0.026(3) 0.024(3) -0.001(2) -0.003(2) 0.000(3) C24 0.027(3) 0.036(3) 0.030(3) -0.005(3) 0.001(2) 0.005(3) N10 0.036(3) 0.032(3) 0.037(3) 0.002(2) 0.004(2) -0.004(2) O11 0.043(3) 0.067(3) 0.026(2) -0.001(2) 0.0040(19) 0.002(2) O12 0.044(3) 0.089(4) 0.064(3) -0.019(3) 0.007(2) 0.010(3) O13 0.059(3) 0.064(3) 0.029(2) 0.006(2) -0.006(2) 0.015(3) N20 0.053(3) 0.020(3) 0.046(3) -0.003(2) 0.000(3) 0.002(2) O21 0.234(8) 0.040(3) 0.038(3) -0.008(2) -0.035(4) 0.043(4) O22 0.117(5) 0.032(3) 0.126(5) -0.013(3) -0.052(4) 0.013(3) O23 0.097(4) 0.045(3) 0.038(3) 0.004(2) -0.023(3) -0.015(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 2.363(3) . ? Pb1 O1 2.373(4) . ? Pb1 N2 2.559(4) . ? Pb1 N1 2.580(5) . ? Pb1 O11 2.831(4) . ? Pb1 O23 2.855(5) . ? Pb1 O21 2.960(5) . ? Pb1 O13 3.027(4) . ? N1 C24 1.274(7) . ? N1 C1 1.473(6) . ? N2 C4 1.269(6) . ? N2 C3 1.469(6) . ? N3 C12 1.290(6) . ? N3 C13 1.474(7) . ? N4 C16 1.292(6) . ? N4 C15 1.454(6) . ? O1 C23 1.299(6) . ? O2 C11 1.302(6) . ? C1 C2 1.519(7) . ? C2 C3 1.515(7) . ? C4 C5 1.454(7) . ? C5 C6 1.387(7) . ? C5 C11 1.429(8) . ? C6 C7 1.399(8) . ? C7 C9 1.384(8) . ? C7 C8 1.501(8) . ? C9 C10 1.394(7) . ? C10 C11 1.430(7) . ? C10 C12 1.437(7) . ? C13 C14 1.517(7) . ? C14 C15 1.522(7) . ? C16 C17 1.426(7) . ? C17 C18 1.389(7) . ? C17 C23 1.420(7) . ? C18 C19 1.367(7) . ? C19 C21 1.390(7) . ? C19 C20 1.513(7) . ? C21 C22 1.384(7) . ? C22 C23 1.447(7) . ? C22 C24 1.454(7) . ? N10 O12 1.229(6) . ? N10 O13 1.246(6) . ? N10 O11 1.255(6) . ? N20 O22 1.209(6) . ? N20 O21 1.209(6) . ? N20 O23 1.231(6) . ? 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 O1 78.70(13) . . ? O2 Pb1 N2 71.51(13) . . ? O1 Pb1 N2 107.81(14) . . ? O2 Pb1 N1 117.52(13) . . ? O1 Pb1 N1 71.17(13) . . ? N2 Pb1 N1 67.98(13) . . ? O2 Pb1 O11 70.11(11) . . ? O1 Pb1 O11 70.65(13) . . ? N2 Pb1 O11 141.07(12) . . ? N1 Pb1 O11 138.27(13) . . ? O2 Pb1 O23 83.54(12) . . ? O1 Pb1 O23 161.32(13) . . ? N2 Pb1 O23 71.39(14) . . ? N1 Pb1 O23 123.17(14) . . ? O11 Pb1 O23 97.94(14) . . ? O2 Pb1 O21 125.77(13) . . ? O1 Pb1 O21 153.52(14) . . ? N2 Pb1 O21 91.37(16) . . ? N1 Pb1 O21 100.86(17) . . ? O11 Pb1 O21 105.78(17) . . ? O23 Pb1 O21 42.53(12) . . ? O2 Pb1 O13 113.28(12) . . ? O1 Pb1 O13 78.78(13) . . ? N2 Pb1 O13 172.82(12) . . ? N1 Pb1 O13 112.56(13) . . ? O11 Pb1 O13 43.18(11) . . ? O23 Pb1 O13 103.34(13) . . ? O21 Pb1 O13 81.48(15) . . ? C24 N1 C1 117.1(5) . . ? C24 N1 Pb1 131.4(4) . . ? C1 N1 Pb1 111.5(3) . . ? C4 N2 C3 117.7(5) . . ? C4 N2 Pb1 127.8(4) . . ? C3 N2 Pb1 114.0(3) . . ? C12 N3 C13 122.4(5) . . ? C16 N4 C15 124.3(5) . . ? C23 O1 Pb1 141.6(3) . . ? C11 O2 Pb1 129.1(3) . . ? N1 C1 C2 112.3(4) . . ? C3 C2 C1 115.2(5) . . ? N2 C3 C2 111.7(4) . . ? N2 C4 C5 127.4(5) . . ? C6 C5 C11 119.7(5) . . ? C6 C5 C4 117.7(5) . . ? C11 C5 C4 122.6(5) . . ? C5 C6 C7 124.5(6) . . ? C9 C7 C6 115.6(5) . . ? C9 C7 C8 122.5(6) . . ? C6 C7 C8 121.9(6) . . ? C7 C9 C10 122.8(6) . . ? C9 C10 C11 121.5(5) . . ? C9 C10 C12 117.8(5) . . ? C11 C10 C12 120.7(5) . . ? O2 C11 C5 123.8(5) . . ? O2 C11 C10 120.2(5) . . ? C5 C11 C10 115.9(5) . . ? N3 C12 C10 124.1(5) . . ? N3 C13 C14 113.3(5) . . ? C13 C14 C15 115.7(5) . . ? N4 C15 C14 114.4(5) . . ? N4 C16 C17 126.0(5) . . ? C18 C17 C23 121.5(5) . . ? C18 C17 C16 118.2(5) . . ? C23 C17 C16 120.2(5) . . ? C19 C18 C17 122.2(5) . . ? C18 C19 C21 117.0(5) . . ? C18 C19 C20 120.9(5) . . ? C21 C19 C20 122.1(5) . . ? C22 C21 C19 124.3(5) . . ? C21 C22 C23 118.6(5) . . ? C21 C22 C24 118.3(5) . . ? C23 C22 C24 123.1(5) . . ? O1 C23 C17 120.4(5) . . ? O1 C23 C22 123.3(5) . . ? C17 C23 C22 116.4(5) . . ? N1 C24 C22 128.5(5) . . ? O12 N10 O13 120.7(5) . . ? O12 N10 O11 119.4(5) . . ? O13 N10 O11 119.8(5) . . ? N10 O11 Pb1 102.9(3) . . ? N10 O13 Pb1 93.5(3) . . ? O22 N20 O21 118.3(6) . . ? O22 N20 O23 121.8(6) . . ? O21 N20 O23 119.8(5) . . ? N20 O21 Pb1 94.9(4) . . ? N20 O23 Pb1 99.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.952 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.132 #===END data_3 _database_code_CSD 179595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H26 N4 O2 Pb2)(N O3)2' _chemical_formula_sum 'C24 H26 N6 O8 Pb2' _chemical_formula_weight 940.89 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.582(1) _cell_length_b 9.531(1) _cell_length_c 18.285(2) _cell_angle_alpha 95.30(1) _cell_angle_beta 91.00(1) _cell_angle_gamma 92.69(1) _cell_volume 1313.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 7.809 _cell_measurement_theta_max 16.961 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 12.858 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 13 _diffrn_reflns_number 7234 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6010 _reflns_number_gt 4626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0734P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6010 _refine_ls_number_parameters 362 _refine_ls_number_restraints 570 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 0.985 _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 0.74171(4) 0.46035(3) 0.026755(17) 0.01815(11) Uani 1 1 d U . . O1 O 0.5322(8) 0.4599(6) -0.0695(3) 0.0200(12) Uani 1 1 d U . . N1 N 0.7201(10) 0.2177(8) -0.0364(4) 0.0205(14) Uani 1 1 d U . . N2 N 0.6481(10) 0.3184(7) 0.1335(4) 0.0220(15) Uani 1 1 d U . . C1 C 0.7834(12) 0.1020(9) 0.0062(5) 0.0231(18) Uani 1 1 d U . . H1A H 0.9050 0.1259 0.0236 0.028 Uiso 1 1 calc R . . H1B H 0.7836 0.0143 -0.0263 0.028 Uiso 1 1 calc R . . C2 C 0.6677(13) 0.0789(9) 0.0717(5) 0.0249(19) Uani 1 1 d U . . H2A H 0.5446 0.0908 0.0573 0.030 Uiso 1 1 calc R . . H2B H 0.6768 -0.0189 0.0833 0.030 Uiso 1 1 calc R . . C3 C 0.7119(14) 0.1752(10) 0.1401(5) 0.028(2) Uani 1 1 d U . . H3A H 0.6573 0.1359 0.1824 0.034 Uiso 1 1 calc R . . H3B H 0.8401 0.1816 0.1486 0.034 Uiso 1 1 calc R . . C4 C 0.5732(12) 0.3747(9) 0.1887(5) 0.0219(17) Uani 1 1 d U . . H4A H 0.5604 0.3203 0.2287 0.026 Uiso 1 1 calc R . . C5 C 0.5040(11) 0.5149(9) 0.1973(5) 0.0180(16) Uani 1 1 d U . . C6 C 0.4833(12) 0.5723(10) 0.2703(5) 0.0221(18) Uani 1 1 d U . . H6A H 0.5108 0.5172 0.3087 0.027 Uiso 1 1 calc R . . C7 C 0.4501(12) 0.5919(9) 0.1395(4) 0.0189(17) Uani 1 1 d U . . C8 C 0.5899(13) 0.2339(10) -0.3668(5) 0.029(2) Uani 1 1 d U . . H8A H 0.6341 0.1398 -0.3681 0.043 Uiso 1 1 calc R . . H8B H 0.6706 0.2938 -0.3921 0.043 Uiso 1 1 calc R . . H8C H 0.4744 0.2293 -0.3908 0.043 Uiso 1 1 calc R . . C9 C 0.5755(11) 0.2939(10) -0.2881(5) 0.0216(17) Uani 1 1 d U . . C10 C 0.6227(11) 0.2184(9) -0.2304(5) 0.0204(17) Uani 1 1 d U . . H10A H 0.6587 0.1259 -0.2411 0.024 Uiso 1 1 calc R . . C11 C 0.6192(12) 0.2739(9) -0.1561(5) 0.0192(16) Uani 1 1 d U . . C12 C 0.6786(11) 0.1832(9) -0.1033(5) 0.0178(16) Uani 1 1 d U . . H12A H 0.6878 0.0877 -0.1202 0.021 Uiso 1 1 calc R . . N10 N 0.8185(10) 0.7178(7) -0.0796(4) 0.0257(16) Uani 1 1 d DU . . O11 O 0.8002(11) 0.8004(8) -0.1278(4) 0.0433(19) Uani 1 1 d DU . . O12 O 0.7495(11) 0.7446(7) -0.0181(4) 0.0395(18) Uani 1 1 d DU . . O13 O 0.9089(9) 0.6112(7) -0.0906(4) 0.0333(15) Uani 1 1 d DU . . Pb2 Pb 0.76243(4) 0.54214(3) 0.530870(16) 0.01838(11) Uani 1 1 d U . . O2 O 0.9672(8) 0.5493(6) 0.4357(3) 0.0198(12) Uani 1 1 d U . . N3 N 0.8558(10) 0.6603(8) 0.6550(4) 0.0230(15) Uani 1 1 d U . . N4 N 0.7966(10) 0.7936(8) 0.5034(4) 0.0224(15) Uani 1 1 d U . . C13 C 0.7901(14) 0.8012(10) 0.6794(5) 0.0259(19) Uani 1 1 d U . . H13A H 0.8335 0.8300 0.7296 0.031 Uiso 1 1 calc R . . H13B H 0.6608 0.7948 0.6800 0.031 Uiso 1 1 calc R . . C14 C 0.8491(14) 0.9099(9) 0.6302(5) 0.0261(19) Uani 1 1 d U . . H14A H 0.9738 0.8977 0.6192 0.031 Uiso 1 1 calc R . . H14B H 0.8405 1.0034 0.6567 0.031 Uiso 1 1 calc R . . C15 C 0.7433(14) 0.9057(9) 0.5568(5) 0.0258(19) Uani 1 1 d U . . H15A H 0.6171 0.8915 0.5662 0.031 Uiso 1 1 calc R . . H15B H 0.7610 0.9966 0.5362 0.031 Uiso 1 1 calc R . . C16 C 0.8282(12) 0.8318(9) 0.4401(5) 0.0225(17) Uani 1 1 d U . . H16A H 0.8186 0.9285 0.4353 0.027 Uiso 1 1 calc R . . C17 C 0.8776(11) 0.7468(9) 0.3735(5) 0.0183(16) Uani 1 1 d U . . C18 C 0.8619(12) 0.8081(10) 0.3082(5) 0.0243(18) Uani 1 1 d U . . H18A H 0.8215 0.9001 0.3097 0.029 Uiso 1 1 calc R . . C19 C 0.9029(12) 0.7408(9) 0.2409(5) 0.0219(17) Uani 1 1 d U . . C20 C 0.8784(15) 0.8113(12) 0.1705(6) 0.035(2) Uani 1 1 d U . . H20A H 0.9138 0.7486 0.1291 0.053 Uiso 1 1 calc R . . H20B H 0.9506 0.8984 0.1732 0.053 Uiso 1 1 calc R . . H20C H 0.7552 0.8317 0.1643 0.053 Uiso 1 1 calc R . . C21 C 0.9677(12) 0.6068(10) 0.2409(5) 0.0228(18) Uani 1 1 d U . . H21A H 0.9964 0.5584 0.1958 0.027 Uiso 1 1 calc R . . C22 C 0.9916(12) 0.5414(9) 0.3053(5) 0.0204(17) Uani 1 1 d U . . C23 C 0.9447(11) 0.6087(9) 0.3749(5) 0.0187(16) Uani 1 1 d U . . C24 C 0.9348(13) 0.5988(9) 0.7036(5) 0.0233(18) Uani 1 1 d U . . H24A H 0.9477 0.6482 0.7504 0.028 Uiso 1 1 calc R . . N20 N 0.6783(11) 0.2588(8) 0.4054(4) 0.0300(17) Uani 1 1 d DU . . O21 O 0.6831(13) 0.1693(10) 0.3524(5) 0.063(3) Uani 1 1 d DU . . O22 O 0.5860(10) 0.3628(7) 0.4037(4) 0.0385(17) Uani 1 1 d DU . . O23 O 0.7650(11) 0.2420(8) 0.4615(4) 0.0451(19) Uani 1 1 d DU . . 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 0.02077(18) 0.01535(17) 0.01813(18) 0.00045(12) 0.00145(13) 0.00054(12) O1 0.024(3) 0.022(3) 0.013(3) 0.002(2) 0.003(2) 0.001(2) N1 0.026(4) 0.020(3) 0.016(3) 0.002(3) -0.008(3) 0.004(3) N2 0.029(4) 0.016(3) 0.021(3) 0.001(3) 0.004(3) 0.005(3) C1 0.031(5) 0.014(4) 0.026(4) 0.007(3) -0.003(4) 0.005(3) C2 0.036(5) 0.016(4) 0.024(4) 0.002(3) 0.001(4) 0.003(4) C3 0.042(6) 0.021(4) 0.021(4) -0.001(3) -0.008(4) 0.005(4) C4 0.024(4) 0.020(4) 0.022(4) 0.004(3) -0.001(3) -0.003(3) C5 0.019(4) 0.016(4) 0.019(4) 0.002(3) 0.005(3) -0.002(3) C6 0.024(4) 0.025(4) 0.017(4) 0.003(3) 0.004(4) 0.002(4) C7 0.024(4) 0.022(4) 0.010(4) -0.003(3) 0.002(3) 0.002(3) C8 0.032(5) 0.027(5) 0.026(4) -0.003(4) 0.007(4) 0.004(4) C9 0.016(4) 0.028(4) 0.019(4) -0.005(3) 0.000(3) -0.004(3) C10 0.018(4) 0.018(4) 0.024(4) -0.005(3) 0.003(3) -0.001(3) C11 0.024(4) 0.017(4) 0.016(4) -0.001(3) 0.004(3) -0.001(3) C12 0.017(4) 0.017(4) 0.018(4) -0.005(3) -0.001(3) 0.004(3) N10 0.035(4) 0.018(3) 0.023(4) 0.001(3) -0.001(3) -0.003(3) O11 0.061(5) 0.046(4) 0.026(4) 0.015(3) 0.001(4) 0.007(4) O12 0.068(5) 0.021(3) 0.031(4) 0.004(3) 0.020(4) 0.003(3) O13 0.034(4) 0.030(3) 0.036(4) 0.001(3) 0.008(3) 0.007(3) Pb2 0.02199(19) 0.01738(17) 0.01558(18) 0.00076(12) 0.00249(13) -0.00036(13) O2 0.028(3) 0.023(3) 0.009(3) 0.004(2) 0.005(2) 0.003(2) N3 0.026(4) 0.023(3) 0.019(3) 0.000(3) 0.006(3) -0.004(3) N4 0.028(4) 0.022(3) 0.017(3) -0.001(3) -0.006(3) 0.002(3) C13 0.037(5) 0.029(4) 0.013(4) 0.000(3) 0.007(4) 0.010(4) C14 0.040(5) 0.020(4) 0.018(4) -0.001(3) 0.001(4) 0.002(4) C15 0.040(5) 0.018(4) 0.019(4) -0.001(3) 0.001(4) 0.006(4) C16 0.030(5) 0.016(4) 0.021(4) -0.001(3) -0.003(4) 0.000(3) C17 0.018(4) 0.019(4) 0.019(4) 0.006(3) 0.003(3) 0.003(3) C18 0.023(4) 0.021(4) 0.030(4) 0.008(3) 0.002(4) 0.000(3) C19 0.026(4) 0.025(4) 0.015(4) 0.006(3) -0.004(3) -0.001(3) C20 0.041(6) 0.038(6) 0.029(5) 0.017(4) 0.001(5) 0.003(5) C21 0.026(5) 0.028(4) 0.015(4) 0.004(3) -0.001(3) 0.002(4) C22 0.027(4) 0.024(4) 0.009(3) 0.000(3) -0.002(3) -0.003(3) C23 0.020(4) 0.018(4) 0.018(4) -0.001(3) 0.000(3) -0.002(3) C24 0.033(5) 0.022(4) 0.013(4) -0.003(3) 0.001(3) -0.002(4) N20 0.034(4) 0.029(4) 0.027(4) -0.003(3) 0.001(3) 0.002(3) O21 0.069(6) 0.065(6) 0.049(5) -0.031(5) -0.002(5) 0.020(5) O22 0.038(4) 0.035(4) 0.041(4) -0.004(3) -0.008(3) 0.005(3) O23 0.063(5) 0.037(4) 0.035(4) 0.002(3) -0.009(4) 0.009(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 Pb1 O1 2.350(6) . ? Pb1 O1 2.366(6) 2_665 ? Pb1 N1 2.485(7) . ? Pb1 N2 2.567(7) . ? Pb1 O12 2.900(7) . ? Pb1 O13 2.962(7) . ? O1 C7 1.340(9) 2_665 ? O1 Pb1 2.366(6) 2_665 ? N1 C12 1.267(11) . ? N1 C1 1.499(10) . ? N2 C4 1.255(11) . ? N2 C3 1.483(11) . ? C1 C2 1.523(12) . ? C2 C3 1.506(12) . ? C4 C5 1.455(12) . ? C5 C7 1.406(12) . ? C5 C6 1.411(12) . ? C6 C9 1.383(13) 2_665 ? C7 O1 1.340(9) 2_665 ? C7 C11 1.415(12) 2_665 ? C8 C9 1.506(12) . ? C9 C6 1.383(13) 2_665 ? C9 C10 1.382(13) . ? C10 C11 1.414(12) . ? C11 C7 1.415(12) 2_665 ? C11 C12 1.435(12) . ? N10 O11 1.245(8) . ? N10 O13 1.254(8) . ? N10 O12 1.259(8) . ? Pb2 O2 2.355(6) . ? Pb2 O2 2.357(6) 2_766 ? Pb2 N4 2.496(8) . ? Pb2 N3 2.513(8) . ? Pb2 O22 3.010(7) . ? Pb2 O23 3.022(7) . ? O2 C23 1.305(10) . ? O2 Pb2 2.357(6) 2_766 ? N3 C24 1.266(12) . ? N3 C13 1.486(11) . ? N4 C16 1.269(12) . ? N4 C15 1.456(11) . ? C13 C14 1.493(13) . ? C14 C15 1.548(13) . ? C16 C17 1.463(12) . ? C17 C18 1.383(12) . ? C17 C23 1.436(12) . ? C18 C19 1.381(13) . ? C19 C21 1.390(13) . ? C19 C20 1.518(12) . ? C21 C22 1.396(12) . ? C22 C23 1.430(11) . ? C22 C24 1.469(12) 2_766 ? C24 C22 1.469(12) 2_766 ? N20 O21 1.233(9) . ? N20 O23 1.234(9) . ? N20 O22 1.243(9) . ? 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 O1 68.3(2) . 2_665 ? O1 Pb1 N1 72.9(2) . . ? O1 Pb1 N1 113.4(2) 2_665 . ? O1 Pb1 N2 115.4(2) . . ? O1 Pb1 N2 71.7(2) 2_665 . ? N1 Pb1 N2 79.4(2) . . ? O1 Pb1 O12 73.3(2) . . ? O1 Pb1 O12 78.3(2) 2_665 . ? N1 Pb1 O12 136.1(2) . . ? N2 Pb1 O12 141.4(2) . . ? O1 Pb1 O13 72.6(2) . . ? O1 Pb1 O13 116.90(19) 2_665 . ? N1 Pb1 O13 99.3(2) . . ? N2 Pb1 O13 170.6(2) . . ? O12 Pb1 O13 43.50(18) . . ? C7 O1 Pb1 126.9(5) 2_665 . ? C7 O1 Pb1 121.0(5) 2_665 2_665 ? Pb1 O1 Pb1 111.7(2) . 2_665 ? C12 N1 C1 116.1(7) . . ? C12 N1 Pb1 126.7(6) . . ? C1 N1 Pb1 116.8(5) . . ? C4 N2 C3 116.1(8) . . ? C4 N2 Pb1 121.6(6) . . ? C3 N2 Pb1 121.2(6) . . ? N1 C1 C2 112.0(7) . . ? C3 C2 C1 115.3(8) . . ? N2 C3 C2 111.1(8) . . ? N2 C4 C5 127.1(8) . . ? C7 C5 C6 119.0(8) . . ? C7 C5 C4 125.4(8) . . ? C6 C5 C4 115.6(8) . . ? C9 C6 C5 122.9(9) 2_665 . ? O1 C7 C5 120.3(8) 2_665 . ? O1 C7 C11 120.4(8) 2_665 2_665 ? C5 C7 C11 119.2(7) . 2_665 ? C6 C9 C10 117.0(8) 2_665 . ? C6 C9 C8 121.6(9) 2_665 . ? C10 C9 C8 121.4(8) . . ? C9 C10 C11 123.0(8) . . ? C10 C11 C7 118.5(8) . 2_665 ? C10 C11 C12 115.8(8) . . ? C7 C11 C12 125.6(8) 2_665 . ? N1 C12 C11 127.1(8) . . ? O11 N10 O13 121.2(7) . . ? O11 N10 O12 119.1(7) . . ? O13 N10 O12 119.7(7) . . ? N10 O12 Pb1 97.3(5) . . ? N10 O13 Pb1 94.5(5) . . ? O2 Pb2 O2 68.7(2) . 2_766 ? O2 Pb2 N4 73.5(2) . . ? O2 Pb2 N4 112.4(2) 2_766 . ? O2 Pb2 N3 117.5(2) . . ? O2 Pb2 N3 72.2(2) 2_766 . ? N4 Pb2 N3 79.0(2) . . ? O2 Pb2 O22 75.8(2) . . ? O2 Pb2 O22 111.13(19) 2_766 . ? N4 Pb2 O22 110.8(2) . . ? N3 Pb2 O22 166.0(2) . . ? O2 Pb2 O23 75.0(2) . . ? O2 Pb2 O23 72.5(2) 2_766 . ? N4 Pb2 O23 143.0(2) . . ? N3 Pb2 O23 133.7(2) . . ? O22 Pb2 O23 41.7(2) . . ? C23 O2 Pb2 125.6(5) . . ? C23 O2 Pb2 122.7(5) . 2_766 ? Pb2 O2 Pb2 111.3(2) . 2_766 ? C24 N3 C13 115.9(8) . . ? C24 N3 Pb2 123.6(6) . . ? C13 N3 Pb2 119.6(6) . . ? C16 N4 C15 114.8(8) . . ? C16 N4 Pb2 123.9(6) . . ? C15 N4 Pb2 120.1(6) . . ? N3 C13 C14 111.7(7) . . ? C13 C14 C15 114.8(8) . . ? N4 C15 C14 112.1(8) . . ? N4 C16 C17 129.2(8) . . ? C18 C17 C23 120.9(8) . . ? C18 C17 C16 116.5(8) . . ? C23 C17 C16 122.6(8) . . ? C19 C18 C17 123.2(9) . . ? C18 C19 C21 117.0(8) . . ? C18 C19 C20 121.1(9) . . ? C21 C19 C20 121.9(8) . . ? C19 C21 C22 122.3(8) . . ? C21 C22 C23 121.0(8) . . ? C21 C22 C24 115.9(7) . 2_766 ? C23 C22 C24 123.1(8) . 2_766 ? O2 C23 C22 121.7(8) . . ? O2 C23 C17 122.7(8) . . ? C22 C23 C17 115.5(8) . . ? N3 C24 C22 127.1(8) . 2_766 ? O21 N20 O23 118.6(8) . . ? O21 N20 O22 121.3(8) . . ? O23 N20 O22 120.0(7) . . ? N20 O22 Pb2 97.7(5) . . ? N20 O23 Pb2 97.3(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.871 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.293 # END of CIF