# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jie-Hui Yu' _publ_contact_author_email JIEHUIYU@YAHOO.COM.CN _publ_section_title ; 4-Carboxylphthalhydrzidate-bridged layered Pb(II) coordination polymers ; loop_ _publ_author_name 'Yu Hui' 'Qin Hou' 'Juan Jin' 'Yu Peng' 'Jiqing Xu' # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 752419' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H12 N4 O4 Pb' _chemical_formula_weight 591.54 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 21.5673(11) _cell_length_b 10.1496(5) _cell_length_c 16.1354(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.849(3) _cell_angle_gamma 90.00 _cell_volume 3519.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 9.628 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siements SMART CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12459 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.25 _reflns_number_total 4348 _reflns_number_gt 3340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4348 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.451360(11) 0.15757(2) 0.081676(14) 0.02997(10) Uani 1 1 d . . . N1 N 0.5374(2) -0.0187(5) 0.1371(3) 0.0323(12) Uani 1 1 d . . . N2 N 0.5705(3) 0.0053(5) 0.2131(3) 0.0310(12) Uani 1 1 d . . . H2A H 0.5747 0.0865 0.2276 0.037 Uiso 1 1 calc R . . N3 N 0.3725(2) 0.3311(5) 0.0057(3) 0.0300(12) Uani 1 1 d . . . N4 N 0.3575(2) 0.0665(5) -0.0234(3) 0.0313(12) Uani 1 1 d . . . O1 O 0.4987(2) -0.1626(4) 0.0394(3) 0.0366(11) Uani 1 1 d . . . O2 O 0.6259(2) -0.0502(4) 0.3329(3) 0.0414(11) Uani 1 1 d . . . O3 O 0.5143(3) -0.6462(4) 0.1058(4) 0.0517(14) Uani 1 1 d . . . O4 O 0.5754(3) -0.7151(5) 0.2174(4) 0.0553(14) Uani 1 1 d . . . C1 C 0.5408(3) -0.3833(6) 0.1419(4) 0.0266(12) Uani 1 1 d . . . H1A H 0.5172 -0.4028 0.0925 0.032 Uiso 1 1 calc R . . C2 C 0.5648(3) -0.4834(6) 0.1931(4) 0.0259(12) Uani 1 1 d . . . C3 C 0.6003(3) -0.4540(6) 0.2670(4) 0.0306(13) Uani 1 1 d . . . H3A H 0.6168 -0.5220 0.3005 0.037 Uiso 1 1 calc R . . C4 C 0.6112(3) -0.3243(5) 0.2910(4) 0.0299(13) Uani 1 1 d . . . H4A H 0.6346 -0.3055 0.3406 0.036 Uiso 1 1 calc R . . C5 C 0.5870(2) -0.2226(5) 0.2406(3) 0.0218(11) Uani 1 1 d . . . C6 C 0.5525(2) -0.2507(6) 0.1656(4) 0.0232(12) Uani 1 1 d . . . C7 C 0.5285(3) -0.1403(5) 0.1123(4) 0.0249(12) Uani 1 1 d . . . C8 C 0.5966(3) -0.0844(6) 0.2669(4) 0.0267(12) Uani 1 1 d . . . C9 C 0.5512(3) -0.6277(6) 0.1703(5) 0.0365(16) Uani 1 1 d . . . C10 C 0.3793(3) 0.4606(6) 0.0193(4) 0.0363(15) Uani 1 1 d . . . H10A H 0.4128 0.4893 0.0548 0.044 Uiso 1 1 calc R . . C11 C 0.3384(4) 0.5546(7) -0.0175(5) 0.0481(19) Uani 1 1 d . . . H11A H 0.3447 0.6436 -0.0060 0.058 Uiso 1 1 calc R . . C12 C 0.2890(4) 0.5151(7) -0.0707(5) 0.0474(18) Uani 1 1 d . . . H12A H 0.2606 0.5765 -0.0940 0.057 Uiso 1 1 calc R . . C13 C 0.2818(3) 0.3798(7) -0.0897(4) 0.0339(14) Uani 1 1 d . . . C14 C 0.2331(3) 0.3309(7) -0.1493(5) 0.0414(17) Uani 1 1 d . . . H14A H 0.2041 0.3889 -0.1748 0.050 Uiso 1 1 calc R . . C15 C 0.2300(3) 0.2030(8) -0.1674(4) 0.0413(16) Uani 1 1 d . . . H15A H 0.1995 0.1741 -0.2076 0.050 Uiso 1 1 calc R . . C16 C 0.2712(3) 0.1091(7) -0.1281(4) 0.0345(14) Uani 1 1 d . . . C17 C 0.2692(3) -0.0278(7) -0.1451(5) 0.0412(16) Uani 1 1 d . . . H17A H 0.2393 -0.0608 -0.1846 0.049 Uiso 1 1 calc R . . C18 C 0.3102(4) -0.1110(8) -0.1045(5) 0.0473(18) Uani 1 1 d . . . H18A H 0.3101 -0.2001 -0.1181 0.057 Uiso 1 1 calc R . . C19 C 0.3531(3) -0.0616(6) -0.0417(5) 0.0393(16) Uani 1 1 d . . . H19A H 0.3794 -0.1204 -0.0118 0.047 Uiso 1 1 calc R . . C20 C 0.3245(3) 0.2903(6) -0.0481(4) 0.0279(13) Uani 1 1 d . . . C21 C 0.3174(3) 0.1505(6) -0.0663(4) 0.0285(13) 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 0.03390(14) 0.02577(14) 0.02824(14) 0.00419(9) -0.00907(9) -0.00213(10) N1 0.041(3) 0.028(3) 0.027(3) 0.002(2) -0.005(2) 0.013(2) N2 0.042(3) 0.018(2) 0.031(3) -0.002(2) -0.003(2) 0.002(2) N3 0.032(3) 0.028(3) 0.029(3) 0.000(2) -0.001(2) 0.001(2) N4 0.027(3) 0.026(3) 0.039(3) 0.003(2) -0.003(2) 0.001(2) O1 0.040(3) 0.044(3) 0.024(2) 0.0027(19) -0.0095(19) 0.007(2) O2 0.052(3) 0.033(2) 0.036(3) -0.006(2) -0.014(2) -0.006(2) O3 0.070(4) 0.033(3) 0.050(4) -0.007(2) -0.008(3) -0.021(2) O4 0.072(4) 0.020(2) 0.071(4) 0.001(3) -0.011(3) 0.001(2) C1 0.022(3) 0.025(3) 0.032(3) -0.004(3) -0.001(2) -0.004(2) C2 0.024(3) 0.023(3) 0.031(3) -0.006(2) 0.001(2) -0.003(2) C3 0.028(3) 0.026(3) 0.036(3) 0.002(3) -0.006(3) 0.004(2) C4 0.029(3) 0.030(3) 0.029(3) -0.002(2) -0.007(2) 0.000(2) C5 0.022(3) 0.020(3) 0.024(3) -0.001(2) 0.000(2) -0.002(2) C6 0.021(3) 0.022(3) 0.026(3) 0.000(2) -0.004(2) -0.002(2) C7 0.025(3) 0.026(3) 0.022(3) 0.001(2) -0.006(2) 0.003(2) C8 0.028(3) 0.026(3) 0.026(3) -0.001(2) -0.001(2) -0.004(2) C9 0.035(4) 0.026(3) 0.050(5) -0.011(3) 0.007(3) -0.008(3) C10 0.045(4) 0.029(3) 0.035(4) 0.002(3) 0.002(3) -0.004(3) C11 0.070(5) 0.025(4) 0.048(5) -0.003(3) 0.001(4) 0.004(3) C12 0.056(5) 0.032(4) 0.055(5) 0.006(3) 0.007(4) 0.011(3) C13 0.032(3) 0.033(3) 0.037(4) 0.008(3) 0.007(3) 0.007(3) C14 0.029(3) 0.047(4) 0.046(4) 0.013(3) -0.007(3) 0.006(3) C15 0.030(4) 0.053(4) 0.040(4) 0.008(3) -0.009(3) -0.006(3) C16 0.027(3) 0.040(4) 0.036(4) 0.005(3) 0.001(3) -0.007(3) C17 0.033(4) 0.046(4) 0.044(4) -0.003(3) -0.003(3) -0.010(3) C18 0.043(4) 0.033(4) 0.064(5) -0.003(4) -0.001(4) -0.011(3) C19 0.038(4) 0.029(3) 0.050(4) 0.005(3) -0.007(3) 0.001(3) C20 0.027(3) 0.028(3) 0.030(3) 0.007(3) 0.007(2) -0.001(2) C21 0.023(3) 0.030(3) 0.032(3) 0.006(3) 0.002(2) 0.000(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 O1 2.310(5) 5_655 ? Pb1 O3 2.423(4) 1_565 ? Pb1 N3 2.673(5) . ? Pb1 N1 2.677(5) . ? Pb1 N4 2.691(5) . ? N1 C7 1.306(7) . ? N1 N2 1.387(8) . ? N2 C8 1.348(8) . ? N3 C10 1.338(7) . ? N3 C20 1.360(8) . ? N4 C19 1.336(8) . ? N4 C21 1.362(8) . ? O1 C7 1.312(7) . ? O1 Pb1 2.310(5) 5_655 ? O2 C8 1.242(7) . ? O3 C9 1.271(9) . ? O3 Pb1 2.423(4) 1_545 ? O4 C9 1.252(9) . ? C1 C2 1.382(9) . ? C1 C6 1.417(8) . ? C2 C3 1.393(9) . ? C2 C9 1.532(8) . ? C3 C4 1.386(8) . ? C4 C5 1.388(8) . ? C5 C6 1.394(8) . ? C5 C8 1.475(8) . ? C6 C7 1.480(8) . ? C10 C11 1.397(10) . ? C11 C12 1.372(11) . ? C12 C13 1.413(10) . ? C13 C20 1.421(9) . ? C13 C14 1.449(10) . ? C14 C15 1.332(10) . ? C15 C16 1.417(10) . ? C16 C21 1.413(9) . ? C16 C17 1.416(10) . ? C17 C18 1.351(11) . ? C18 C19 1.405(10) . ? C20 C21 1.454(8) . ? 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 O3 79.78(18) 5_655 1_565 ? O1 Pb1 N3 85.50(16) 5_655 . ? O3 Pb1 N3 81.83(18) 1_565 . ? O1 Pb1 N1 86.43(15) 5_655 . ? O3 Pb1 N1 97.62(19) 1_565 . ? N3 Pb1 N1 171.89(16) . . ? O1 Pb1 N4 81.63(16) 5_655 . ? O3 Pb1 N4 139.87(18) 1_565 . ? N3 Pb1 N4 61.46(15) . . ? N1 Pb1 N4 116.37(16) . . ? C7 N1 N2 119.2(5) . . ? C7 N1 Pb1 116.7(4) . . ? N2 N1 Pb1 117.9(4) . . ? C8 N2 N1 127.3(5) . . ? C10 N3 C20 118.1(6) . . ? C10 N3 Pb1 121.1(4) . . ? C20 N3 Pb1 120.9(4) . . ? C19 N4 C21 117.8(6) . . ? C19 N4 Pb1 120.7(4) . . ? C21 N4 Pb1 121.1(4) . . ? C7 O1 Pb1 121.8(4) . 5_655 ? C9 O3 Pb1 123.9(4) . 1_545 ? C2 C1 C6 119.1(6) . . ? C1 C2 C3 120.3(5) . . ? C1 C2 C9 120.3(6) . . ? C3 C2 C9 119.3(6) . . ? C4 C3 C2 120.7(6) . . ? C3 C4 C5 119.7(6) . . ? C4 C5 C6 120.1(5) . . ? C4 C5 C8 120.1(5) . . ? C6 C5 C8 119.7(5) . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C7 118.9(5) . . ? C1 C6 C7 121.1(5) . . ? N1 C7 O1 119.1(5) . . ? N1 C7 C6 120.2(5) . . ? O1 C7 C6 120.7(5) . . ? O2 C8 N2 121.2(6) . . ? O2 C8 C5 124.2(5) . . ? N2 C8 C5 114.6(5) . . ? O4 C9 O3 126.3(6) . . ? O4 C9 C2 118.1(7) . . ? O3 C9 C2 115.6(6) . . ? N3 C10 C11 123.0(7) . . ? C12 C11 C10 119.7(7) . . ? C11 C12 C13 119.0(7) . . ? C12 C13 C20 117.6(7) . . ? C12 C13 C14 122.5(6) . . ? C20 C13 C14 119.9(6) . . ? C15 C14 C13 120.0(6) . . ? C14 C15 C16 122.6(7) . . ? C21 C16 C17 115.9(6) . . ? C21 C16 C15 119.6(6) . . ? C17 C16 C15 124.4(7) . . ? C18 C17 C16 120.8(7) . . ? C17 C18 C19 119.3(7) . . ? N4 C19 C18 122.6(7) . . ? N3 C20 C13 122.4(6) . . ? N3 C20 C21 119.2(6) . . ? C13 C20 C21 118.4(6) . . ? N4 C21 C16 123.5(6) . . ? N4 C21 C20 117.2(6) . . ? C16 C21 C20 119.2(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.599 _refine_diff_density_min -2.279 _refine_diff_density_rms 0.202 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 752420' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24 N6 O19 Pb4' _chemical_formula_weight 1565.28 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 10.594(2) _cell_length_b 10.716(2) _cell_length_c 14.990(3) _cell_angle_alpha 85.91(3) _cell_angle_beta 80.52(3) _cell_angle_gamma 89.68(3) _cell_volume 1674.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5123 _exptl_crystal_size_mid 0.4265 _exptl_crystal_size_min 0.0892 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 20.149 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1225 _exptl_absorpt_correction_T_max 0.5 _exptl_absorpt_process_details ;Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16597 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7579 _reflns_number_gt 6602 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.5669P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7579 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.92857(3) 0.64673(3) 0.269490(18) 0.01779(9) Uani 1 1 d . . . Pb2 Pb -1.00076(3) 0.98859(3) 0.36943(2) 0.02039(10) Uani 1 1 d . . . Pb3 Pb -0.91982(3) 1.34010(3) 0.446725(18) 0.01667(9) Uani 1 1 d . . . Pb4 Pb -0.98274(3) 1.26542(3) 0.16719(2) 0.02531(10) Uani 1 1 d . . . N1 N -0.6528(7) 0.5772(6) 0.1615(4) 0.0198(14) Uani 1 1 d . . . N2 N -0.5381(7) 0.5962(7) 0.1027(4) 0.0246(16) Uani 1 1 d . . . H2A H -0.5444 0.6238 0.0483 0.029 Uiso 1 1 calc R . . N3 N -0.7158(7) 0.9084(7) 0.1661(5) 0.0238(16) Uani 1 1 d . . . N4 N -0.5977(7) 0.9375(7) 0.1096(4) 0.0250(16) Uani 1 1 d . . . H4A H -0.6023 0.9744 0.0574 0.030 Uiso 1 1 calc R . . N5 N -0.7483(7) 1.2462(7) 0.1643(5) 0.0239(16) Uani 1 1 d . . . N6 N -0.6373(6) 1.2720(7) 0.1047(5) 0.0259(17) Uani 1 1 d . . . H6A H -0.6448 1.3035 0.0515 0.031 Uiso 1 1 calc R . . O1 O -0.7508(5) 0.5176(6) 0.3026(4) 0.0265(14) Uani 1 1 d . . . O2 O -0.3252(6) 0.6054(6) 0.0602(4) 0.0299(15) Uani 1 1 d . . . O3 O -0.0559(6) 0.4292(5) 0.2882(4) 0.0245(13) Uani 1 1 d . . . O4 O -0.1549(6) 0.3679(6) 0.4271(4) 0.0268(13) Uani 1 1 d . . . O5 O -0.8144(5) 0.8264(5) 0.3020(4) 0.0249(13) Uani 1 1 d . . . O6 O -0.3847(6) 0.9427(6) 0.0679(4) 0.0336(16) Uani 1 1 d . . . O7 O -0.1245(6) 0.7957(6) 0.3136(4) 0.0286(14) Uani 1 1 d . . . O8 O -0.2323(7) 0.7110(8) 0.4445(5) 0.0440(19) Uani 1 1 d . . . O9 O -0.8533(6) 1.1835(6) 0.3000(4) 0.0262(14) Uani 1 1 d . . . O10 O -0.4239(6) 1.2831(6) 0.0624(4) 0.0305(15) Uani 1 1 d . . . O11 O -0.1539(6) 1.1390(6) 0.2922(4) 0.0325(16) Uani 1 1 d . . . O12 O -0.2429(6) 1.0367(6) 0.4202(4) 0.0300(14) Uani 1 1 d . . . OH1 O -1.0161(6) 1.1401(5) 0.4874(3) 0.0201(12) Uani 1 1 d . . . OH2 O -0.9528(5) 0.6042(5) 0.4189(3) 0.0209(12) Uani 1 1 d . . . OW1 O -0.8970(9) 1.2469(12) -0.0132(6) 0.092(4) Uani 1 1 d . . . OW2 O -0.9492(8) 1.0274(7) 0.1573(5) 0.051(2) Uani 1 1 d . . . OW3 O 0.8573(10) -0.0030(13) 0.0606(6) 0.099(4) Uani 1 1 d . . . OW4 O 0.8358(10) 0.2704(16) 0.0387(8) 0.138(6) Uani 1 1 d . . . OW5 O -0.8716(9) 1.4916(7) 0.0874(5) 0.056(2) Uani 1 1 d . . . C1 C -0.5218(8) 0.5042(7) 0.2728(5) 0.0154(15) Uani 1 1 d . . . C2 C -0.4102(7) 0.5250(7) 0.2111(5) 0.0140(15) Uani 1 1 d . . . C3 C -0.2910(8) 0.4971(7) 0.2351(5) 0.0193(17) Uani 1 1 d . . . H3B H -0.2166 0.5114 0.1931 0.023 Uiso 1 1 calc R . . C4 C -0.2845(8) 0.4481(7) 0.3217(5) 0.0160(16) Uani 1 1 d . . . C5 C -0.3949(8) 0.4299(7) 0.3844(5) 0.0206(17) Uani 1 1 d . . . H5A H -0.3888 0.4003 0.4434 0.025 Uiso 1 1 calc R . . C6 C -0.5142(8) 0.4546(7) 0.3618(5) 0.0211(17) Uani 1 1 d . . . H6B H -0.5879 0.4389 0.4041 0.025 Uiso 1 1 calc R . . C7 C -0.6460(7) 0.5342(7) 0.2450(5) 0.0161(15) Uani 1 1 d . . . C8 C -0.4190(8) 0.5775(7) 0.1192(5) 0.0180(16) Uani 1 1 d . . . C9 C -0.1568(8) 0.4127(7) 0.3497(5) 0.0194(17) Uani 1 1 d . . . C10 C -0.5860(8) 0.8352(7) 0.2789(5) 0.0177(16) Uani 1 1 d . . . C11 C -0.4724(8) 0.8602(7) 0.2184(5) 0.0174(16) Uani 1 1 d . . . C12 C -0.3565(8) 0.8377(7) 0.2471(5) 0.0191(16) Uani 1 1 d . . . H12A H -0.2809 0.8568 0.2074 0.023 Uiso 1 1 calc R . . C13 C -0.3508(8) 0.7875(7) 0.3336(5) 0.0164(15) Uani 1 1 d . . . C14 C -0.4657(8) 0.7642(8) 0.3939(5) 0.0214(17) Uani 1 1 d . . . H14A H -0.4629 0.7331 0.4531 0.026 Uiso 1 1 calc R . . C15 C -0.5833(8) 0.7864(7) 0.3669(5) 0.0207(17) Uani 1 1 d . . . H15B H -0.6589 0.7691 0.4070 0.025 Uiso 1 1 calc R . . C16 C -0.7074(8) 0.8585(7) 0.2471(6) 0.0209(17) Uani 1 1 d . . . C17 C -0.4798(8) 0.9148(7) 0.1272(5) 0.0211(17) Uani 1 1 d . . . C18 C -0.2258(8) 0.7618(8) 0.3672(5) 0.0234(18) Uani 1 1 d . . . C19 C -0.6230(8) 1.1753(7) 0.2763(5) 0.0165(16) Uani 1 1 d . . . C20 C -0.5110(7) 1.2003(7) 0.2131(5) 0.0140(15) Uani 1 1 d . . . C21 C -0.3890(8) 1.1793(7) 0.2378(5) 0.0189(17) Uani 1 1 d . . . H21A H -0.3152 1.2002 0.1966 0.023 Uiso 1 1 calc R . . C22 C -0.3807(8) 1.1274(7) 0.3239(5) 0.0208(17) Uani 1 1 d . . . C23 C -0.4918(8) 1.1040(8) 0.3859(5) 0.0229(18) Uani 1 1 d . . . H23A H -0.4851 1.0713 0.4441 0.027 Uiso 1 1 calc R . . C24 C -0.6113(8) 1.1272(7) 0.3646(5) 0.0206(17) Uani 1 1 d . . . H24A H -0.6839 1.1113 0.4080 0.025 Uiso 1 1 calc R . . C25 C -0.7437(8) 1.2010(7) 0.2481(5) 0.0198(17) Uani 1 1 d . . . C26 C -0.5196(8) 1.2530(7) 0.1216(5) 0.0202(17) Uani 1 1 d . . . C27 C -0.2500(8) 1.1011(7) 0.3478(5) 0.0204(17) 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 0.01068(16) 0.02583(16) 0.01617(15) 0.00363(11) -0.00240(11) -0.00058(13) Pb2 0.01302(17) 0.02558(16) 0.02229(16) 0.00236(12) -0.00376(12) -0.00135(13) Pb3 0.01153(16) 0.02283(16) 0.01500(14) 0.00288(11) -0.00217(11) 0.00216(12) Pb4 0.01511(17) 0.03479(19) 0.02691(17) 0.00003(13) -0.00721(13) 0.00569(14) N1 0.013(4) 0.028(3) 0.018(3) 0.003(3) -0.003(3) 0.000(3) N2 0.013(4) 0.042(4) 0.018(3) 0.014(3) -0.003(3) 0.002(3) N3 0.009(3) 0.033(4) 0.028(4) 0.004(3) -0.003(3) 0.002(3) N4 0.008(3) 0.047(4) 0.020(3) 0.008(3) -0.006(3) 0.005(3) N5 0.008(3) 0.037(4) 0.026(3) 0.003(3) -0.001(3) -0.001(3) N6 0.006(3) 0.049(4) 0.022(3) 0.011(3) -0.006(3) -0.003(3) O1 0.003(3) 0.046(4) 0.028(3) 0.007(3) 0.002(2) 0.005(3) O2 0.017(3) 0.051(4) 0.020(3) 0.015(3) -0.005(2) 0.001(3) O3 0.014(3) 0.034(3) 0.027(3) -0.005(2) -0.005(2) -0.003(3) O4 0.019(3) 0.041(3) 0.021(3) 0.006(3) -0.010(2) 0.006(3) O5 0.006(3) 0.032(3) 0.035(3) -0.002(3) -0.002(2) 0.005(3) O6 0.018(3) 0.059(4) 0.021(3) 0.010(3) -0.003(3) 0.005(3) O7 0.012(3) 0.040(3) 0.035(3) 0.004(3) -0.010(3) 0.004(3) O8 0.017(4) 0.077(5) 0.037(4) 0.022(4) -0.016(3) 0.001(4) O9 0.008(3) 0.039(3) 0.027(3) 0.002(3) 0.008(2) -0.006(3) O10 0.009(3) 0.059(4) 0.020(3) 0.009(3) 0.003(2) 0.005(3) O11 0.013(3) 0.053(4) 0.028(3) 0.023(3) -0.006(3) -0.007(3) O12 0.015(3) 0.046(4) 0.029(3) 0.014(3) -0.012(3) 0.004(3) OH1 0.021(3) 0.019(3) 0.019(3) 0.006(2) -0.002(2) -0.001(2) OH2 0.014(3) 0.028(3) 0.018(3) 0.003(2) 0.001(2) 0.006(2) OW1 0.040(6) 0.168(11) 0.068(6) -0.026(7) -0.001(5) -0.038(7) OW2 0.047(5) 0.044(4) 0.065(5) 0.000(4) -0.025(4) 0.007(4) OW3 0.042(6) 0.201(13) 0.057(6) -0.001(7) -0.016(5) -0.029(7) OW4 0.035(6) 0.281(18) 0.089(8) 0.073(10) -0.019(6) -0.004(9) OW5 0.056(6) 0.055(5) 0.059(5) -0.004(4) -0.013(4) -0.002(4) C1 0.010(4) 0.021(4) 0.015(3) 0.002(3) -0.003(3) 0.000(3) C2 0.007(4) 0.020(3) 0.016(3) -0.001(3) -0.005(3) 0.003(3) C3 0.009(4) 0.029(4) 0.019(4) 0.001(3) -0.002(3) -0.007(3) C4 0.016(4) 0.020(4) 0.014(3) 0.003(3) -0.008(3) -0.005(3) C5 0.018(4) 0.025(4) 0.019(4) 0.009(3) -0.009(3) 0.000(4) C6 0.014(4) 0.028(4) 0.020(4) 0.003(3) 0.000(3) -0.001(4) C7 0.004(4) 0.021(4) 0.022(4) 0.002(3) -0.001(3) 0.004(3) C8 0.012(4) 0.025(4) 0.016(3) 0.004(3) -0.002(3) 0.000(3) C9 0.017(4) 0.020(4) 0.021(4) 0.007(3) -0.009(3) -0.006(3) C10 0.011(4) 0.017(4) 0.026(4) 0.004(3) -0.008(3) 0.001(3) C11 0.009(4) 0.023(4) 0.019(4) 0.000(3) -0.002(3) 0.002(3) C12 0.009(4) 0.022(4) 0.026(4) -0.001(3) 0.001(3) 0.001(3) C13 0.013(4) 0.017(3) 0.021(4) -0.002(3) -0.008(3) 0.002(3) C14 0.016(4) 0.028(4) 0.021(4) 0.004(3) -0.005(3) 0.001(4) C15 0.012(4) 0.028(4) 0.020(4) 0.002(3) 0.001(3) 0.003(4) C16 0.010(4) 0.019(4) 0.033(4) 0.003(3) -0.004(3) 0.001(3) C17 0.012(4) 0.022(4) 0.028(4) 0.007(3) -0.002(3) -0.002(3) C18 0.018(5) 0.031(4) 0.022(4) 0.001(3) -0.006(3) 0.009(4) C19 0.013(4) 0.016(3) 0.018(4) 0.002(3) 0.003(3) 0.000(3) C20 0.008(4) 0.023(4) 0.011(3) -0.001(3) -0.001(3) 0.003(3) C21 0.017(4) 0.021(4) 0.017(4) 0.006(3) -0.002(3) -0.006(3) C22 0.021(5) 0.024(4) 0.018(4) 0.000(3) -0.005(3) -0.001(4) C23 0.023(5) 0.026(4) 0.019(4) 0.007(3) -0.003(3) -0.005(4) C24 0.017(4) 0.022(4) 0.020(4) 0.004(3) 0.003(3) 0.000(4) C25 0.010(4) 0.024(4) 0.025(4) -0.001(3) -0.002(3) 0.000(3) C26 0.016(4) 0.026(4) 0.017(4) 0.008(3) -0.002(3) 0.007(3) C27 0.016(4) 0.023(4) 0.023(4) 0.003(3) -0.009(3) -0.003(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 OH2 2.226(5) . ? Pb1 O5 2.400(6) . ? Pb1 O1 2.426(6) . ? Pb1 O7 2.637(6) 1_455 ? Pb1 O3 2.673(6) 1_455 ? Pb2 OH1 2.470(5) . ? Pb2 OH1 2.498(5) 2_376 ? Pb2 O12 2.612(6) 1_455 ? Pb2 O11 2.626(6) 1_455 ? Pb2 O9 2.660(5) . ? Pb2 O7 2.707(6) 1_455 ? Pb2 O5 2.738(6) . ? Pb3 OH2 2.346(5) 2_376 ? Pb3 OH1 2.374(5) . ? Pb3 O8 2.507(7) 2_476 ? Pb3 O4 2.569(6) 1_465 ? Pb4 N5 2.484(7) . ? Pb4 OW2 2.584(7) . ? Pb4 O3 2.635(6) 1_465 ? Pb4 O11 2.680(5) 1_455 ? Pb4 O9 2.693(7) . ? Pb4 OW1 2.728(9) . ? N1 C7 1.316(10) . ? N1 N2 1.385(9) . ? N2 C8 1.336(11) . ? N3 C16 1.307(10) . ? N3 N4 1.414(9) . ? N4 C17 1.335(11) . ? N5 C25 1.322(10) . ? N5 N6 1.371(9) . ? N6 C26 1.325(11) . ? O1 C7 1.294(9) . ? O2 C8 1.239(9) . ? O3 C9 1.296(10) . ? O3 Pb4 2.635(6) 1_645 ? O3 Pb1 2.673(5) 1_655 ? O4 C9 1.228(9) . ? O4 Pb3 2.569(6) 1_645 ? O5 C16 1.318(9) . ? O6 C17 1.251(9) . ? O7 C18 1.269(10) . ? O7 Pb1 2.637(6) 1_655 ? O7 Pb2 2.707(6) 1_655 ? O8 C18 1.236(10) . ? O8 Pb3 2.507(7) 2_476 ? O9 C25 1.293(9) . ? O10 C26 1.259(9) . ? O11 C27 1.254(9) . ? O11 Pb2 2.626(6) 1_655 ? O11 Pb4 2.680(5) 1_655 ? O12 C27 1.256(9) . ? O12 Pb2 2.612(6) 1_655 ? OH1 Pb2 2.498(5) 2_376 ? OH2 Pb3 2.346(5) 2_376 ? C1 C2 1.384(10) . ? C1 C6 1.415(10) . ? C1 C7 1.472(11) . ? C2 C3 1.395(11) . ? C2 C8 1.468(10) . ? C3 C4 1.377(10) . ? C4 C5 1.380(11) . ? C4 C9 1.518(12) . ? C5 C6 1.381(12) . ? C10 C15 1.389(10) . ? C10 C11 1.397(10) . ? C10 C16 1.459(12) . ? C11 C12 1.381(12) . ? C11 C17 1.463(11) . ? C12 C13 1.378(11) . ? C13 C14 1.404(11) . ? C13 C18 1.509(12) . ? C14 C15 1.385(12) . ? C19 C20 1.405(10) . ? C19 C24 1.411(10) . ? C19 C25 1.430(12) . ? C20 C21 1.414(11) . ? C20 C26 1.462(10) . ? C21 C22 1.385(10) . ? C22 C23 1.386(11) . ? C22 C27 1.508(12) . ? C23 C24 1.373(12) . ? 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 OH2 Pb1 O5 83.4(2) . . ? OH2 Pb1 O1 71.7(2) . . ? O5 Pb1 O1 88.7(2) . . ? OH2 Pb1 O7 82.9(2) . 1_455 ? O5 Pb1 O7 81.04(19) . 1_455 ? O1 Pb1 O7 153.56(19) . 1_455 ? OH2 Pb1 O3 78.84(19) . 1_455 ? O5 Pb1 O3 162.15(19) . 1_455 ? O1 Pb1 O3 84.0(2) . 1_455 ? O7 Pb1 O3 98.51(18) 1_455 1_455 ? OH1 Pb2 OH1 74.98(19) . 2_376 ? OH1 Pb2 O12 72.3(2) . 1_455 ? OH1 Pb2 O12 93.46(18) 2_376 1_455 ? OH1 Pb2 O11 86.1(2) . 1_455 ? OH1 Pb2 O11 142.87(18) 2_376 1_455 ? O12 Pb2 O11 49.94(17) 1_455 1_455 ? OH1 Pb2 O9 72.87(17) . . ? OH1 Pb2 O9 125.96(19) 2_376 . ? O12 Pb2 O9 115.91(19) 1_455 . ? O11 Pb2 O9 75.74(19) 1_455 . ? OH1 Pb2 O7 143.15(18) . 1_455 ? OH1 Pb2 O7 89.10(18) 2_376 1_455 ? O12 Pb2 O7 75.8(2) 1_455 1_455 ? O11 Pb2 O7 87.4(2) 1_455 1_455 ? O9 Pb2 O7 139.65(18) . 1_455 ? OH1 Pb2 O5 133.38(19) . . ? OH1 Pb2 O5 81.06(18) 2_376 . ? O12 Pb2 O5 149.41(19) 1_455 . ? O11 Pb2 O5 132.74(19) 1_455 . ? O9 Pb2 O5 90.84(18) . . ? O7 Pb2 O5 74.01(18) 1_455 . ? OH2 Pb3 OH1 84.01(19) 2_376 . ? OH2 Pb3 O8 80.6(2) 2_376 2_476 ? OH1 Pb3 O8 88.8(2) . 2_476 ? OH2 Pb3 O4 68.5(2) 2_376 1_465 ? OH1 Pb3 O4 74.7(2) . 1_465 ? O8 Pb3 O4 146.1(2) 2_476 1_465 ? N5 Pb4 OW2 78.1(3) . . ? N5 Pb4 O3 104.4(2) . 1_465 ? OW2 Pb4 O3 140.2(2) . 1_465 ? N5 Pb4 O11 122.4(2) . 1_455 ? OW2 Pb4 O11 69.9(2) . 1_455 ? O3 Pb4 O11 76.1(2) 1_465 1_455 ? N5 Pb4 O9 50.41(19) . . ? OW2 Pb4 O9 72.1(2) . . ? O3 Pb4 O9 79.31(19) 1_465 . ? O11 Pb4 O9 74.31(17) 1_455 . ? N5 Pb4 OW1 78.6(3) . . ? OW2 Pb4 OW1 77.5(3) . . ? O3 Pb4 OW1 142.4(3) 1_465 . ? O11 Pb4 OW1 134.6(3) 1_455 . ? O9 Pb4 OW1 124.3(3) . . ? C7 N1 N2 117.0(7) . . ? C8 N2 N1 128.7(7) . . ? C16 N3 N4 115.4(7) . . ? C17 N4 N3 128.1(7) . . ? C25 N5 N6 120.1(7) . . ? C25 N5 Pb4 101.5(5) . . ? N6 N5 Pb4 138.3(5) . . ? C26 N6 N5 126.1(7) . . ? C7 O1 Pb1 114.9(5) . . ? C9 O3 Pb4 122.5(5) . 1_645 ? C9 O3 Pb1 119.7(5) . 1_655 ? Pb4 O3 Pb1 117.4(2) 1_645 1_655 ? C9 O4 Pb3 107.9(5) . 1_645 ? C16 O5 Pb1 117.7(5) . . ? C16 O5 Pb2 125.3(5) . . ? Pb1 O5 Pb2 104.9(2) . . ? C18 O7 Pb1 123.7(5) . 1_655 ? C18 O7 Pb2 113.7(5) . 1_655 ? Pb1 O7 Pb2 99.4(2) 1_655 1_655 ? C18 O8 Pb3 136.7(6) . 2_476 ? C25 O9 Pb2 136.6(5) . . ? C25 O9 Pb4 92.5(5) . . ? Pb2 O9 Pb4 99.0(2) . . ? C27 O11 Pb2 92.2(5) . 1_655 ? C27 O11 Pb4 166.8(6) . 1_655 ? Pb2 O11 Pb4 100.2(2) 1_655 1_655 ? C27 O12 Pb2 92.8(5) . 1_655 ? Pb3 OH1 Pb2 118.0(2) . . ? Pb3 OH1 Pb2 124.5(2) . 2_376 ? Pb2 OH1 Pb2 105.02(19) . 2_376 ? Pb1 OH2 Pb3 140.6(3) . 2_376 ? C2 C1 C6 119.3(7) . . ? C2 C1 C7 119.6(7) . . ? C6 C1 C7 121.1(7) . . ? C1 C2 C3 121.0(7) . . ? C1 C2 C8 118.9(7) . . ? C3 C2 C8 120.1(7) . . ? C4 C3 C2 119.3(7) . . ? C3 C4 C5 120.1(8) . . ? C3 C4 C9 120.9(7) . . ? C5 C4 C9 119.0(7) . . ? C4 C5 C6 121.6(7) . . ? C5 C6 C1 118.6(7) . . ? O1 C7 N1 118.9(7) . . ? O1 C7 C1 120.2(7) . . ? N1 C7 C1 120.9(7) . . ? O2 C8 N2 121.0(7) . . ? O2 C8 C2 124.1(8) . . ? N2 C8 C2 114.9(7) . . ? O4 C9 O3 124.0(8) . . ? O4 C9 C4 119.1(7) . . ? O3 C9 C4 116.9(7) . . ? C15 C10 C11 120.7(8) . . ? C15 C10 C16 120.7(7) . . ? C11 C10 C16 118.6(7) . . ? C12 C11 C10 119.4(7) . . ? C12 C11 C17 121.8(7) . . ? C10 C11 C17 118.7(7) . . ? C13 C12 C11 121.2(7) . . ? C12 C13 C14 118.7(8) . . ? C12 C13 C18 122.6(7) . . ? C14 C13 C18 118.7(7) . . ? C15 C14 C13 121.3(7) . . ? C14 C15 C10 118.7(7) . . ? N3 C16 O5 118.0(8) . . ? N3 C16 C10 123.3(7) . . ? O5 C16 C10 118.7(7) . . ? O6 C17 N4 120.0(8) . . ? O6 C17 C11 124.3(8) . . ? N4 C17 C11 115.7(7) . . ? O8 C18 O7 126.4(9) . . ? O8 C18 C13 116.9(8) . . ? O7 C18 C13 116.7(7) . . ? C20 C19 C24 118.6(8) . . ? C20 C19 C25 118.3(7) . . ? C24 C19 C25 123.1(7) . . ? C19 C20 C21 120.8(7) . . ? C19 C20 C26 120.0(7) . . ? C21 C20 C26 119.1(6) . . ? C22 C21 C20 119.2(7) . . ? C21 C22 C23 119.4(8) . . ? C21 C22 C27 118.5(7) . . ? C23 C22 C27 122.0(7) . . ? C24 C23 C22 122.5(8) . . ? C23 C24 C19 119.4(7) . . ? O9 C25 N5 115.5(8) . . ? O9 C25 C19 124.3(7) . . ? N5 C25 C19 120.2(7) . . ? O10 C26 N6 120.8(7) . . ? O10 C26 C20 123.9(8) . . ? N6 C26 C20 115.2(7) . . ? O11 C27 O12 123.5(8) . . ? O11 C27 C22 118.2(7) . . ? O12 C27 C22 118.2(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.616 _refine_diff_density_min -3.948 _refine_diff_density_rms 0.434