# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Cheng-Yong Su' _publ_contact_author_email cesscy@mail.sysu.edu.cn _publ_author_name 'Cheng-Yong Su' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 854707' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 N6 O16 Pb' _chemical_formula_weight 975.92 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 24.1114(16) _cell_length_b 22.9404(16) _cell_length_c 7.5513(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.250(3) _cell_angle_gamma 90.00 _cell_volume 4143.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3788 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 25.99 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 4.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5612 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16450 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4071 _reflns_number_gt 3785 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated water molecules show typical large thermal displacement due to their freedom in the void framework channels. Constrained refinement ISOR was applied for all water solvents to approximate to isotropic behavior, which gives 30 restraints. O1w, O4w and O5w were treated as disordered fractional sites with arbitrary occupancies of 0.25 or 0.5. H atoms of solvated water molecules were not added. The largest residual density peak of 4.499 appears adjacent to Pb1 atom, indicating strong absorption of such heavy metal atom, although empirical absorption corrections were applied to reflections by use of the ABSCOR program. 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^)+(0.0697P)^2^+45.5859P] 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 4071 _refine_ls_number_parameters 259 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.068 _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 0.0000 0.454856(12) 0.2500 0.01665(13) Uani 1 2 d S . . O1 O 0.1161(2) 0.4444(2) 0.3325(8) 0.0344(12) Uani 1 1 d . . . O2 O 0.05810(18) 0.3687(2) 0.3163(7) 0.0300(11) Uani 1 1 d . . . O3 O 0.3627(2) 0.2909(2) 0.2727(8) 0.0380(13) Uani 1 1 d . . . O4 O 0.4755(2) 0.0608(2) 0.0542(7) 0.0278(10) Uani 1 1 d . . . N1 N 0.2854(2) 0.2325(3) 0.2504(8) 0.0269(12) Uani 1 1 d . . . H1A H 0.2744 0.1961 0.2345 0.032 Uiso 1 1 calc R . . N2 N 0.4426(2) 0.1038(2) 0.1001(7) 0.0245(12) Uani 1 1 d . . . C1 C 0.1071(3) 0.3908(3) 0.3279(9) 0.0239(13) Uani 1 1 d . . . C2 C 0.1549(2) 0.3490(3) 0.3203(9) 0.0220(13) Uani 1 1 d . . . C3 C 0.2098(3) 0.3692(3) 0.3383(11) 0.0338(16) Uani 1 1 d . . . H3A H 0.2170 0.4093 0.3621 0.041 Uiso 1 1 calc R . . C4 C 0.2541(3) 0.3320(3) 0.3223(12) 0.0361(17) Uani 1 1 d . . . H4A H 0.2914 0.3463 0.3402 0.043 Uiso 1 1 calc R . . C5 C 0.2439(3) 0.2736(3) 0.2799(9) 0.0252(14) Uani 1 1 d . . . C6 C 0.1890(3) 0.2523(3) 0.2701(10) 0.0287(15) Uani 1 1 d . . . H6A H 0.1818 0.2121 0.2475 0.034 Uiso 1 1 calc R . . C7 C 0.1455(3) 0.2896(3) 0.2931(9) 0.0253(14) Uani 1 1 d . . . H7A H 0.1087 0.2746 0.2903 0.030 Uiso 1 1 calc R . . C8 C 0.3402(3) 0.2435(3) 0.2442(9) 0.0270(14) Uani 1 1 d . . . C9 C 0.3749(3) 0.1920(3) 0.1975(9) 0.0232(13) Uani 1 1 d . . . C10 C 0.3612(3) 0.1337(3) 0.2183(9) 0.0274(14) Uani 1 1 d . . . H10A H 0.3276 0.1239 0.2648 0.033 Uiso 1 1 calc R . . C11 C 0.3955(3) 0.0904(3) 0.1726(9) 0.0271(14) Uani 1 1 d . . . H11A H 0.3864 0.0508 0.1917 0.032 Uiso 1 1 calc R . . C12 C 0.4579(3) 0.1603(3) 0.0754(9) 0.0267(14) Uani 1 1 d . . . H12A H 0.4913 0.1690 0.0260 0.032 Uiso 1 1 calc R . . C13 C 0.4238(3) 0.2045(3) 0.1237(10) 0.0276(14) Uani 1 1 d . . . H13A H 0.4338 0.2440 0.1064 0.033 Uiso 1 1 calc R . . O5 O 0.2728(2) 0.3760(2) -0.1752(9) 0.0461(15) Uani 1 1 d . . . N3 N 0.3273(3) 0.4327(4) 0.0141(13) 0.060(2) Uani 1 1 d . . . C14 C 0.3309(6) 0.4753(8) 0.155(2) 0.107(6) Uani 1 1 d . . . H14A H 0.2933 0.4892 0.1701 0.161 Uiso 1 1 calc R . . H14B H 0.3539 0.5082 0.1254 0.161 Uiso 1 1 calc R . . H14C H 0.3480 0.4574 0.2671 0.161 Uiso 1 1 calc R . . C15 C 0.3793(4) 0.4064(6) -0.024(2) 0.084(4) Uani 1 1 d . . . H15A H 0.3714 0.3777 -0.1201 0.125 Uiso 1 1 calc R . . H15B H 0.3977 0.3871 0.0833 0.125 Uiso 1 1 calc R . . H15C H 0.4040 0.4367 -0.0616 0.125 Uiso 1 1 calc R . . C16 C 0.2794(4) 0.4131(5) -0.0690(15) 0.055(2) Uani 1 1 d . . . H16 H 0.2464 0.4313 -0.0386 0.066 Uiso 1 1 calc R . . O1W O 0.0000 0.0037(13) 0.2500 0.097(8) Uani 0.50 2 d SPU A 1 O2W O 0.4703(5) 0.3234(6) 0.418(2) 0.143(5) Uani 1 1 d U B 1 O3W O 0.1875(3) 0.5039(3) 0.1199(9) 0.0549(16) Uani 1 1 d U C 1 O4W O 0.0000 0.2396(9) 0.2500 0.149(7) Uani 1 2 d SU D 1 O5W O 0.0455(13) 0.0653(14) 0.517(5) 0.069(8) Uani 0.25 1 d PU E 2 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 0.01655(18) 0.01489(19) 0.01852(19) 0.000 0.00218(12) 0.000 O1 0.022(2) 0.025(2) 0.056(4) -0.001(2) 0.003(2) 0.0071(19) O2 0.018(2) 0.025(2) 0.047(3) 0.003(2) 0.005(2) 0.0028(18) O3 0.026(2) 0.029(3) 0.060(4) -0.004(3) 0.009(2) 0.001(2) O4 0.031(3) 0.027(2) 0.028(3) -0.003(2) 0.016(2) 0.005(2) N1 0.021(3) 0.028(3) 0.031(3) 0.001(3) 0.001(2) 0.003(2) N2 0.024(3) 0.026(3) 0.023(3) 0.005(2) 0.001(2) 0.009(2) C1 0.022(3) 0.025(3) 0.024(3) 0.001(3) 0.000(2) 0.006(2) C2 0.018(3) 0.025(3) 0.024(3) 0.002(3) 0.006(2) 0.005(2) C3 0.027(3) 0.022(3) 0.052(5) -0.003(3) 0.005(3) 0.001(3) C4 0.020(3) 0.030(4) 0.058(5) -0.002(4) 0.005(3) 0.003(3) C5 0.024(3) 0.028(3) 0.024(3) -0.001(3) 0.002(3) 0.005(3) C6 0.026(3) 0.022(3) 0.038(4) -0.004(3) 0.005(3) 0.002(3) C7 0.019(3) 0.027(3) 0.029(3) 0.005(3) 0.003(3) 0.001(2) C8 0.024(3) 0.027(3) 0.029(3) -0.003(3) -0.002(3) 0.004(3) C9 0.020(3) 0.027(3) 0.022(3) -0.002(3) 0.002(2) 0.005(2) C10 0.023(3) 0.028(3) 0.030(3) 0.001(3) 0.000(3) 0.004(3) C11 0.019(3) 0.034(4) 0.028(3) 0.002(3) 0.001(3) 0.005(3) C12 0.024(3) 0.028(3) 0.029(3) -0.003(3) 0.006(3) -0.003(3) C13 0.022(3) 0.028(3) 0.032(4) -0.005(3) 0.001(3) 0.001(3) O5 0.036(3) 0.030(3) 0.070(4) -0.013(3) -0.001(3) 0.002(2) N3 0.049(5) 0.056(5) 0.072(6) -0.002(5) -0.006(4) -0.017(4) C14 0.071(9) 0.137(13) 0.116(13) -0.075(11) 0.021(8) -0.038(9) C15 0.039(5) 0.074(8) 0.136(13) 0.031(8) 0.002(6) -0.002(5) C16 0.045(5) 0.059(6) 0.064(6) -0.006(5) 0.014(5) -0.004(4) O1W 0.094(11) 0.098(11) 0.100(11) 0.000 0.012(9) 0.000 O2W 0.103(7) 0.154(8) 0.167(9) -0.020(7) -0.006(6) -0.001(6) O3W 0.050(3) 0.057(4) 0.059(4) 0.004(3) 0.008(3) -0.002(3) O4W 0.133(10) 0.162(10) 0.154(11) 0.000 0.027(8) 0.000 O5W 0.061(10) 0.067(11) 0.080(11) 0.001(9) 0.015(9) 0.006(8) _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 2.438(5) 2 ? Pb1 O2 2.438(5) . ? Pb1 O4 2.470(5) 7 ? Pb1 O4 2.470(5) 8_456 ? O1 C1 1.249(8) . ? O2 C1 1.277(8) . ? O3 C8 1.222(9) . ? O4 N2 1.337(7) . ? O4 Pb1 2.470(5) 7 ? N1 C8 1.352(9) . ? N1 C5 1.412(8) . ? N1 H1A 0.8800 . ? N2 C11 1.357(8) . ? N2 C12 1.367(9) . ? C1 C2 1.507(8) . ? C2 C7 1.390(9) . ? C2 C3 1.394(9) . ? C3 C4 1.384(10) . ? C3 H3A 0.9500 . ? C4 C5 1.392(10) . ? C4 H4A 0.9500 . ? C5 C6 1.404(9) . ? C6 C7 1.382(9) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.514(9) . ? C9 C10 1.391(10) . ? C9 C13 1.397(9) . ? C10 C11 1.364(9) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.383(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O5 C16 1.167(11) . ? N3 C16 1.322(12) . ? N3 C14 1.441(16) . ? N3 C15 1.455(14) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 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 O2 Pb1 O2 71.7(2) 2 . ? O2 Pb1 O4 83.68(17) 2 7 ? O2 Pb1 O4 82.77(17) . 7 ? O2 Pb1 O4 82.77(17) 2 8_456 ? O2 Pb1 O4 83.68(17) . 8_456 ? O4 Pb1 O4 163.3(2) 7 8_456 ? C1 O2 Pb1 101.2(4) . . ? N2 O4 Pb1 124.6(4) . 7 ? C8 N1 C5 126.6(6) . . ? C8 N1 H1A 116.7 . . ? C5 N1 H1A 116.7 . . ? O4 N2 C11 119.4(6) . . ? O4 N2 C12 119.0(5) . . ? C11 N2 C12 121.6(6) . . ? O1 C1 O2 123.3(6) . . ? O1 C1 C2 119.7(6) . . ? O2 C1 C2 116.7(6) . . ? C7 C2 C3 118.4(6) . . ? C7 C2 C1 121.2(6) . . ? C3 C2 C1 120.5(6) . . ? C4 C3 C2 121.3(7) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.9(7) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 119.0(6) . . ? C4 C5 N1 124.8(6) . . ? C6 C5 N1 116.2(6) . . ? C7 C6 C5 120.2(6) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C2 120.9(6) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? O3 C8 N1 125.0(6) . . ? O3 C8 C9 119.3(6) . . ? N1 C8 C9 115.7(6) . . ? C10 C9 C13 117.8(6) . . ? C10 C9 C8 125.3(6) . . ? C13 C9 C8 116.9(6) . . ? C11 C10 C9 120.8(6) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? N2 C11 C10 120.1(7) . . ? N2 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? N2 C12 C13 118.7(6) . . ? N2 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C12 C13 C9 121.0(6) . . ? C12 C13 H13A 119.5 . . ? C9 C13 H13A 119.5 . . ? C16 N3 C14 123.4(10) . . ? C16 N3 C15 119.3(10) . . ? C14 N3 C15 117.0(10) . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 N3 127.5(10) . . ? O5 C16 H16 116.2 . . ? N3 C16 H16 116.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.499 _refine_diff_density_min -2.239 _refine_diff_density_rms 0.198 #================================# data_compd2 _database_code_depnum_ccdc_archive 'CCDC 854708' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 N5 O11 Pb' _chemical_formula_weight 830.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.0753 8.5060 '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 43.753(3) _cell_length_b 7.7050(3) _cell_length_c 28.326(2) _cell_angle_alpha 90.00 _cell_angle_beta 129.724(12) _cell_angle_gamma 90.00 _cell_volume 7344.5(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4028 _cell_measurement_theta_min 2.6239 _cell_measurement_theta_max 62.5945 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 9.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2541 _exptl_absorpt_correction_T_max 0.4521 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10303 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 62.64 _reflns_number_total 5758 _reflns_number_gt 4093 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated DMF and water molecules show typical large thermal displacement due to their freedom in the void framework channels. Constrained refinement ISOR/SIMU was applied for all solvents to approximate to isotropic behaviors, which gives 30/84 restraints. O2w and O3w were treated as disordered fractional sites with arbitrary occupancy of 0.5. H atoms of solvated water molecules were not added. The solvated DMF molecule was further modelled by DFIX and FLAT to make it chemically sensible, causing 6 and 2 restraints. The residual density peaks more than 2 all appears adjacent to Pb1 atom, indicating strong adsorption of such heavy metal atom, although empirical absorption corrections were applied to reflections by use of the SCALE3 ABSPACK program. 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^)+(0.0911P)^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 SHELXL _refine_ls_extinction_coef 0.000059(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5758 _refine_ls_number_parameters 425 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.075 _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 0.724221(10) -1.37372(5) 0.721690(16) 0.01648(17) Uani 1 1 d . . . C1 C 0.7126(3) -1.5498(13) 0.7991(4) 0.016(2) Uani 1 1 d U . . C2 C 0.7070(3) -1.6480(14) 0.8388(4) 0.022(2) Uani 1 1 d . . . C3 C 0.7065(3) -1.8295(13) 0.8382(5) 0.024(2) Uani 1 1 d . . . H3A H 0.7100 -1.8894 0.8127 0.029 Uiso 1 1 calc R . . C4 C 0.7010(3) -1.9221(14) 0.8728(5) 0.026(2) Uani 1 1 d . . . H4A H 0.6995 -2.0451 0.8699 0.031 Uiso 1 1 calc R . . C5 C 0.6977(3) -1.8345(13) 0.9138(5) 0.024(2) Uani 1 1 d . . . C6 C 0.6977(3) -1.6557(13) 0.9139(5) 0.027(3) Uani 1 1 d . . . H6A H 0.6949 -1.5955 0.9402 0.033 Uiso 1 1 calc R . . C7 C 0.7018(3) -1.5616(14) 0.8765(5) 0.027(3) Uani 1 1 d . . . H7A H 0.7010 -1.4384 0.8765 0.033 Uiso 1 1 calc R . . N1 N 0.6942(3) -1.9207(11) 0.9532(4) 0.026(2) Uani 1 1 d . . . H1A H 0.6880 -1.8547 0.9714 0.031 Uiso 1 1 calc R . . C9 C 0.7011(3) -2.1413(15) 1.0204(5) 0.029(3) Uani 1 1 d . . . C10 C 0.7108(4) -2.3129(14) 1.0403(5) 0.032(3) Uani 1 1 d . . . H10A H 0.7145 -2.3937 1.0189 0.039 Uiso 1 1 calc R . . C11 C 0.7152(3) -2.3654(14) 1.0900(5) 0.028(2) Uani 1 1 d . . . H11A H 0.7216 -2.4832 1.1026 0.033 Uiso 1 1 calc R . . C12 C 0.7004(3) -2.0879(13) 1.1034(5) 0.024(2) Uani 1 1 d . . . H12A H 0.6968 -2.0109 1.1257 0.028 Uiso 1 1 calc R . . C13 C 0.6952(3) -2.0293(15) 1.0529(5) 0.028(3) Uani 1 1 d . . . H13A H 0.6876 -1.9122 1.0400 0.033 Uiso 1 1 calc R . . C14 C 0.3599(3) -0.6422(15) 0.4018(5) 0.028(2) Uani 1 1 d . . . C15 C 0.4026(3) -0.6761(16) 0.4471(5) 0.034(3) Uani 1 1 d . . . C16 C 0.4264(3) -0.6559(14) 0.4310(5) 0.027(3) Uani 1 1 d . . . H16A H 0.4148 -0.6172 0.3909 0.032 Uiso 1 1 calc R . . C17 C 0.4673(3) -0.6915(15) 0.4729(5) 0.031(3) Uani 1 1 d . . . H17A H 0.4833 -0.6727 0.4616 0.038 Uiso 1 1 calc R . . C18 C 0.4842(3) -0.7543(19) 0.5308(5) 0.040(3) Uani 1 1 d . . . C19 C 0.4617(4) -0.775(2) 0.5487(7) 0.063(4) Uani 1 1 d U . . H19A H 0.4735 -0.8160 0.5888 0.075 Uiso 1 1 calc R . . C20 C 0.4205(4) -0.734(2) 0.5064(7) 0.062(4) Uani 1 1 d U . . H20A H 0.4048 -0.7470 0.5186 0.074 Uiso 1 1 calc R . . C21 C 0.5474(3) -0.8710(16) 0.6246(5) 0.033(3) Uani 1 1 d . . . C22 C 0.5895(3) -0.9086(14) 0.6506(5) 0.030(3) Uani 1 1 d . . . C23 C 0.6108(3) -0.8094(16) 0.6412(5) 0.030(3) Uani 1 1 d . . . H23A H 0.5998 -0.7056 0.6178 0.036 Uiso 1 1 calc R . . C24 C 0.6495(3) -0.8610(14) 0.6660(4) 0.022(2) Uani 1 1 d . . . H24A H 0.6648 -0.7902 0.6606 0.027 Uiso 1 1 calc R . . C25 C 0.6450(3) -1.1083(14) 0.7107(5) 0.025(2) Uani 1 1 d . . . H25A H 0.6570 -1.2097 0.7352 0.030 Uiso 1 1 calc R . . C26 C 0.6074(3) -1.0569(15) 0.6877(5) 0.029(3) Uani 1 1 d . . . H26A H 0.5936 -1.1229 0.6972 0.034 Uiso 1 1 calc R . . C8 C 0.6988(4) -2.0873(14) 0.9675(5) 0.034(3) Uani 1 1 d . . . N2 N 0.7106(2) -2.2564(11) 1.1215(4) 0.0206(19) Uani 1 1 d . . . N3 N 0.5254(3) -0.7948(15) 0.5703(5) 0.042(3) Uani 1 1 d . . . H3B H 0.5380 -0.7650 0.5567 0.051 Uiso 1 1 calc R . . N4 N 0.6644(2) -1.0089(11) 0.6971(4) 0.0208(19) Uani 1 1 d . . . O1 O 0.7071(2) -1.3885(9) 0.7928(3) 0.0232(15) Uani 1 1 d U . . O2 O 0.7244(2) -1.6291(9) 0.7744(3) 0.0234(15) Uani 1 1 d . . . O3 O 0.7017(4) -2.1984(13) 0.9396(5) 0.073(3) Uani 1 1 d U . . O4 O 0.7173(2) -2.3057(9) 1.1720(3) 0.0192(15) Uani 1 1 d . . . O5 O 0.34659(19) -0.5872(9) 0.3496(3) 0.0237(17) Uani 1 1 d . . . O6 O 0.3375(2) -0.6736(11) 0.4151(4) 0.036(2) Uani 1 1 d . . . O7 O 0.5357(2) -0.9157(13) 0.6519(4) 0.050(3) Uani 1 1 d U . . O8 O 0.7001(2) -1.0588(9) 0.7171(3) 0.0236(16) Uani 1 1 d . . . O9 O 0.4518(3) -0.2384(16) 0.5043(6) 0.080(3) Uani 1 1 d DU . . N5 N 0.4337(5) -0.2483(19) 0.5570(9) 0.155(6) Uani 1 1 d DU . . C27 C 0.4750(7) -0.265(4) 0.6119(9) 0.191(8) Uani 1 1 d DU . . H27A H 0.4908 -0.1744 0.6118 0.287 Uiso 1 1 calc R . . H27B H 0.4850 -0.3792 0.6125 0.287 Uiso 1 1 calc R . . H27C H 0.4772 -0.2511 0.6483 0.287 Uiso 1 1 calc R . . C28 C 0.3927(7) -0.240(4) 0.5378(13) 0.187(8) Uani 1 1 d DU . . H28A H 0.3781 -0.1422 0.5097 0.280 Uiso 1 1 calc R . . H28B H 0.3948 -0.2247 0.5741 0.280 Uiso 1 1 calc R . . H28C H 0.3785 -0.3483 0.5170 0.280 Uiso 1 1 calc R . . C29 C 0.4288(6) -0.2363(17) 0.5061(9) 0.123(6) Uani 1 1 d DU . . H29 H 0.4024 -0.2251 0.4685 0.148 Uiso 1 1 calc R . . O1W O 0.6580(2) 0.6661(10) 0.4826(4) 0.038(2) Uani 1 1 d U . . O2W O 0.5832(7) 0.710(3) 0.3631(12) 0.086(7) Uani 0.50 1 d PU . . O3W O 0.5770(7) 0.382(3) 0.2628(11) 0.078(6) Uani 0.50 1 d PU . . 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 0.0173(2) 0.0200(2) 0.0167(2) 0.00144(19) 0.01298(18) 0.00020(19) C1 0.018(5) 0.021(5) 0.019(5) -0.001(4) 0.017(4) -0.005(4) C2 0.023(5) 0.028(6) 0.019(5) -0.004(5) 0.016(5) -0.002(5) C3 0.031(6) 0.028(6) 0.021(5) -0.006(4) 0.020(5) -0.003(5) C4 0.032(6) 0.027(6) 0.025(6) 0.004(5) 0.022(5) 0.001(5) C5 0.026(6) 0.027(7) 0.025(6) 0.001(5) 0.019(5) -0.001(5) C6 0.041(7) 0.025(7) 0.030(6) -0.006(5) 0.028(6) -0.002(5) C7 0.044(7) 0.022(5) 0.032(6) -0.002(5) 0.031(6) -0.003(5) N1 0.046(6) 0.024(5) 0.029(5) -0.001(4) 0.034(5) 0.001(4) C9 0.042(7) 0.030(6) 0.029(6) -0.005(5) 0.029(6) -0.007(6) C10 0.058(8) 0.025(6) 0.039(7) 0.001(5) 0.043(7) 0.006(6) C11 0.044(7) 0.020(5) 0.038(6) 0.001(5) 0.035(6) 0.005(6) C12 0.038(6) 0.020(6) 0.030(6) 0.000(5) 0.030(5) 0.002(5) C13 0.036(7) 0.028(6) 0.026(6) 0.002(5) 0.023(6) 0.003(5) C14 0.032(6) 0.031(6) 0.029(6) -0.009(5) 0.023(5) -0.007(5) C15 0.028(6) 0.053(8) 0.023(6) 0.003(5) 0.017(5) 0.004(6) C16 0.022(5) 0.043(7) 0.021(5) 0.002(5) 0.016(5) -0.003(5) C17 0.034(7) 0.038(6) 0.035(7) -0.003(5) 0.028(6) -0.004(5) C18 0.014(6) 0.066(9) 0.027(7) 0.005(6) 0.008(5) 0.009(6) C19 0.028(6) 0.115(10) 0.043(7) 0.033(7) 0.022(6) 0.029(7) C20 0.029(6) 0.112(10) 0.052(8) 0.027(8) 0.029(6) 0.019(7) C21 0.021(5) 0.048(7) 0.028(6) 0.011(6) 0.015(5) 0.011(6) C22 0.026(6) 0.036(7) 0.029(6) -0.004(5) 0.018(5) -0.001(5) C23 0.021(6) 0.038(7) 0.024(6) 0.006(5) 0.011(5) 0.000(5) C24 0.022(5) 0.021(6) 0.023(5) -0.007(5) 0.014(5) -0.009(5) C25 0.021(5) 0.027(6) 0.030(6) -0.008(5) 0.018(5) -0.004(5) C26 0.022(6) 0.037(6) 0.029(6) 0.002(5) 0.018(5) 0.004(5) C8 0.067(9) 0.027(7) 0.032(6) -0.010(5) 0.042(7) -0.008(6) N2 0.023(5) 0.024(5) 0.022(5) 0.003(4) 0.018(4) -0.002(4) N3 0.021(5) 0.073(8) 0.038(6) 0.013(6) 0.021(5) 0.012(5) N4 0.022(5) 0.020(5) 0.018(4) 0.002(4) 0.012(4) 0.003(4) O1 0.028(4) 0.024(4) 0.028(4) 0.003(3) 0.022(3) 0.006(3) O2 0.032(4) 0.026(4) 0.024(4) 0.001(4) 0.024(3) -0.004(4) O3 0.158(10) 0.037(5) 0.076(7) 0.004(5) 0.099(8) 0.002(6) O4 0.022(4) 0.026(4) 0.017(4) 0.002(3) 0.016(3) 0.003(3) O5 0.009(3) 0.035(5) 0.019(4) 0.000(3) 0.005(3) -0.008(3) O6 0.024(4) 0.059(6) 0.037(5) 0.002(4) 0.025(4) 0.001(4) O7 0.028(4) 0.085(7) 0.044(5) 0.022(5) 0.026(4) 0.016(5) O8 0.019(4) 0.021(4) 0.034(4) -0.003(3) 0.019(4) 0.003(3) O9 0.069(6) 0.111(7) 0.104(6) 0.009(5) 0.075(5) 0.008(5) N5 0.150(9) 0.178(9) 0.164(9) -0.002(7) 0.114(8) 0.018(8) C27 0.177(10) 0.189(10) 0.186(10) -0.003(8) 0.106(7) 0.004(8) C28 0.175(10) 0.187(10) 0.185(10) 0.006(8) 0.109(7) 0.006(8) C29 0.108(9) 0.131(9) 0.129(9) 0.014(8) 0.075(7) 0.008(8) O1W 0.043(4) 0.044(5) 0.040(4) -0.004(4) 0.032(4) -0.006(4) O2W 0.070(10) 0.102(11) 0.090(11) 0.004(8) 0.052(8) -0.006(8) O3W 0.079(10) 0.080(10) 0.079(10) -0.034(8) 0.052(8) 0.008(8) _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 O5 2.402(6) 5_636 ? Pb1 O2 2.468(7) . ? Pb1 O1 2.562(6) . ? Pb1 O8 2.616(7) . ? C1 O1 1.257(12) . ? C1 O2 1.257(11) . ? C1 C2 1.502(13) . ? C2 C7 1.396(14) . ? C2 C3 1.398(15) . ? C3 C4 1.348(14) . ? C3 H3A 0.9500 . ? C4 C5 1.431(14) . ? C4 H4A 0.9500 . ? C5 C6 1.378(14) . ? C5 N1 1.390(13) . ? C6 C7 1.385(14) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? N1 C8 1.322(14) . ? N1 H1A 0.8800 . ? C9 C10 1.393(16) . ? C9 C13 1.402(15) . ? C9 C8 1.495(14) . ? C10 C11 1.357(14) . ? C10 H10A 0.9500 . ? C11 N2 1.330(13) . ? C11 H11A 0.9500 . ? C12 N2 1.363(13) . ? C12 C13 1.373(14) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 O5 1.266(13) . ? C14 O6 1.280(12) . ? C14 C15 1.465(15) . ? C15 C16 1.383(14) . ? C15 C20 1.400(18) . ? C16 C17 1.403(15) . ? C16 H16A 0.9500 . ? C17 C18 1.384(16) . ? C17 H17A 0.9500 . ? C18 C19 1.373(17) . ? C18 N3 1.424(14) . ? C19 C20 1.424(17) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 O7 1.219(13) . ? C21 N3 1.322(14) . ? C21 C22 1.510(14) . ? C22 C23 1.361(15) . ? C22 C26 1.404(15) . ? C23 C24 1.412(14) . ? C23 H23A 0.9500 . ? C24 N4 1.328(13) . ? C24 H24A 0.9500 . ? C25 N4 1.368(13) . ? C25 C26 1.385(14) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C8 O3 1.226(13) . ? N2 O4 1.319(10) . ? N3 H3B 0.8800 . ? N4 O8 1.333(10) . ? O5 Pb1 2.402(6) 5_636 ? O9 C29 1.040(15) . ? N5 C29 1.319(16) . ? N5 C27 1.452(14) . ? N5 C28 1.506(14) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 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 O5 Pb1 O2 85.0(2) 5_636 . ? O5 Pb1 O1 77.7(2) 5_636 . ? O2 Pb1 O1 51.5(2) . . ? O5 Pb1 O8 79.2(2) 5_636 . ? O2 Pb1 O8 127.9(2) . . ? O1 Pb1 O8 76.6(2) . . ? O1 C1 O2 120.9(9) . . ? O1 C1 C2 119.6(9) . . ? O2 C1 C2 119.4(9) . . ? C7 C2 C3 118.5(10) . . ? C7 C2 C1 121.2(9) . . ? C3 C2 C1 120.3(9) . . ? C4 C3 C2 122.0(10) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 119.8(10) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 N1 118.5(10) . . ? C6 C5 C4 118.2(10) . . ? N1 C5 C4 123.3(9) . . ? C5 C6 C7 121.5(10) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C6 C7 C2 119.9(10) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C8 N1 C5 129.5(9) . . ? C8 N1 H1A 115.2 . . ? C5 N1 H1A 115.2 . . ? C10 C9 C13 117.2(10) . . ? C10 C9 C8 118.5(10) . . ? C13 C9 C8 124.3(10) . . ? C11 C10 C9 120.4(10) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? N2 C11 C10 121.8(10) . . ? N2 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? N2 C12 C13 120.1(9) . . ? N2 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C9 120.3(10) . . ? C12 C13 H13A 119.9 . . ? C9 C13 H13A 119.9 . . ? O5 C14 O6 122.8(10) . . ? O5 C14 C15 117.3(9) . . ? O6 C14 C15 119.9(10) . . ? C16 C15 C20 118.0(11) . . ? C16 C15 C14 120.0(10) . . ? C20 C15 C14 121.9(10) . . ? C15 C16 C17 121.3(10) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C18 C17 C16 119.8(10) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C19 C18 C17 120.8(11) . . ? C19 C18 N3 122.1(11) . . ? C17 C18 N3 117.1(10) . . ? C18 C19 C20 118.9(13) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? C15 C20 C19 121.1(12) . . ? C15 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? O7 C21 N3 125.2(10) . . ? O7 C21 C22 120.8(10) . . ? N3 C21 C22 113.9(9) . . ? C23 C22 C26 118.5(10) . . ? C23 C22 C21 125.0(11) . . ? C26 C22 C21 116.5(10) . . ? C22 C23 C24 119.9(11) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? N4 C24 C23 119.8(10) . . ? N4 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? N4 C25 C26 118.1(10) . . ? N4 C25 H25A 120.9 . . ? C26 C25 H25A 120.9 . . ? C25 C26 C22 120.9(11) . . ? C25 C26 H26A 119.6 . . ? C22 C26 H26A 119.6 . . ? O3 C8 N1 122.6(10) . . ? O3 C8 C9 118.9(10) . . ? N1 C8 C9 118.5(9) . . ? O4 N2 C11 121.5(9) . . ? O4 N2 C12 118.3(8) . . ? C11 N2 C12 120.2(9) . . ? C21 N3 C18 128.7(10) . . ? C21 N3 H3B 115.7 . . ? C18 N3 H3B 115.7 . . ? C24 N4 O8 118.4(8) . . ? C24 N4 C25 122.4(9) . . ? O8 N4 C25 119.2(8) . . ? C1 O1 Pb1 91.5(5) . . ? C1 O2 Pb1 96.0(6) . . ? C14 O5 Pb1 108.8(6) . 5_636 ? N4 O8 Pb1 127.9(5) . . ? C29 N5 C27 113.4(16) . . ? C29 N5 C28 106.1(15) . . ? C27 N5 C28 141(2) . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 H28A 109.5 . . ? N5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 C29 N5 125(2) . . ? O9 C29 H29 117.7 . . ? N5 C29 H29 117.7 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 62.64 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.323 _refine_diff_density_min -2.975 _refine_diff_density_rms 0.228 #==========================# data_compd2' _database_code_depnum_ccdc_archive 'CCDC 854709' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H49 N8 O20 Pb2' _chemical_formula_weight 1592.43 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 43.3044(11) _cell_length_b 7.7682(2) _cell_length_c 28.6980(9) _cell_angle_alpha 90.00 _cell_angle_beta 128.5490(10) _cell_angle_gamma 90.00 _cell_volume 7550.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7112 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3108 _exptl_absorpt_coefficient_mu 4.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5455 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33268 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8540 _reflns_number_gt 7090 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The solvated benzene and water molecules show typical large thermal displacement due to their freedom in the void framework channels. Constrained refinement ISOR/SIMU was applied for all solvents to approximate to isotropic behaviors, which gives 42/72 restraints. O2w and O3w were treated as disordered fractional sites with arbitrary occupancy of 0.8 and 0.2. H atoms of solvated water molecules were not added. The solvated benzene molecule was further modelled by AFIX 66 to simulate a hexagon. 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^)+(0.0378P)^2^+18.5304P] 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 8540 _refine_ls_number_parameters 421 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.012 _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 0.223668(4) 1.115613(17) 0.222865(6) 0.02909(6) Uani 1 1 d . . . O1 O 0.22289(10) 0.8552(4) 0.27381(14) 0.0415(7) Uani 1 1 d . . . O2 O 0.20519(9) 1.0964(3) 0.29169(14) 0.0410(7) Uani 1 1 d . . . O3 O 0.2009(2) 0.2942(5) 0.4408(2) 0.1085(19) Uani 1 1 d . . . O4 O 0.21868(8) 0.2045(4) 0.67256(12) 0.0378(6) Uani 1 1 d . . . O5 O -0.16398(9) 1.8211(6) -0.09144(16) 0.0654(10) Uani 1 1 d . . . O6 O -0.15278(8) 1.9237(4) -0.15215(14) 0.0474(8) Uani 1 1 d . . . O7 O 0.02811(13) 1.5418(9) 0.1308(3) 0.131(2) Uani 1 1 d U . . O8 O 0.20044(8) 1.4331(4) 0.22035(14) 0.0426(7) Uani 1 1 d . . . N1 N 0.19588(13) 0.5742(5) 0.45581(19) 0.0525(10) Uani 1 1 d . . . H1A H 0.1917 0.6421 0.4760 0.063 Uiso 1 1 calc R . . N2 N 0.21240(9) 0.2515(4) 0.62326(15) 0.0344(7) Uani 1 1 d . . . N3 N 0.02319(11) 1.6914(6) 0.0596(2) 0.0629(12) Uani 1 1 d . . . H3A H 0.0370 1.7301 0.0488 0.076 Uiso 1 1 calc R . . N4 N 0.16360(9) 1.4807(4) 0.19638(15) 0.0375(8) Uani 1 1 d . . . C1 C 0.21135(11) 0.9365(5) 0.29857(17) 0.0328(8) Uani 1 1 d . . . C2 C 0.20588(11) 0.8388(5) 0.33832(18) 0.0340(8) Uani 1 1 d . . . C3 C 0.20294(15) 0.9267(6) 0.3775(2) 0.0468(11) Uani 1 1 d . . . H3B H 0.2035 1.0490 0.3785 0.056 Uiso 1 1 calc R . . C4 C 0.19919(16) 0.8352(6) 0.4154(2) 0.0516(12) Uani 1 1 d . . . H4A H 0.1973 0.8957 0.4423 0.062 Uiso 1 1 calc R . . C5 C 0.19813(14) 0.6569(6) 0.4143(2) 0.0442(10) Uani 1 1 d . . . C6 C 0.20037(15) 0.5681(6) 0.3741(2) 0.0467(11) Uani 1 1 d . . . H6A H 0.1991 0.4460 0.3721 0.056 Uiso 1 1 calc R . . C7 C 0.20448(13) 0.6616(6) 0.33712(19) 0.0415(10) Uani 1 1 d . . . H7A H 0.2064 0.6017 0.3101 0.050 Uiso 1 1 calc R . . C8 C 0.19921(18) 0.4051(6) 0.4688(2) 0.0562(13) Uani 1 1 d . . . C9 C 0.20212(15) 0.3575(6) 0.5222(2) 0.0452(11) Uani 1 1 d . . . C10 C 0.19741(14) 0.4717(6) 0.5546(2) 0.0455(11) Uani 1 1 d . . . H10A H 0.1908 0.5885 0.5424 0.055 Uiso 1 1 calc R . . C11 C 0.20225(13) 0.4160(5) 0.6046(2) 0.0406(10) Uani 1 1 d . . . H11A H 0.1984 0.4943 0.6260 0.049 Uiso 1 1 calc R . . C12 C 0.21609(16) 0.1385(6) 0.5916(2) 0.0505(12) Uani 1 1 d . . . H12A H 0.2221 0.0215 0.6039 0.061 Uiso 1 1 calc R . . C13 C 0.21126(17) 0.1903(6) 0.5418(2) 0.0558(13) Uani 1 1 d . . . H13A H 0.2143 0.1084 0.5204 0.067 Uiso 1 1 calc R . . C14 C -0.14157(12) 1.8574(6) -0.1033(2) 0.0461(11) Uani 1 1 d . . . C15 C -0.09789(12) 1.8170(7) -0.0590(2) 0.0490(11) Uani 1 1 d . . . C16 C -0.08253(16) 1.7373(11) -0.0051(3) 0.093(2) Uani 1 1 d U . . H16A H -0.0996 1.7120 0.0042 0.112 Uiso 1 1 calc R . . C17 C -0.04263(17) 1.6936(12) 0.0355(3) 0.103(3) Uani 1 1 d U . . H17A H -0.0326 1.6386 0.0720 0.123 Uiso 1 1 calc R . . C18 C -0.01758(13) 1.7319(8) 0.0217(2) 0.0589(14) Uani 1 1 d . . . C19 C -0.03265(13) 1.8145(7) -0.0318(2) 0.0524(12) Uani 1 1 d . . . H19A H -0.0157 1.8418 -0.0412 0.063 Uiso 1 1 calc R . . C20 C -0.07261(13) 1.8571(6) -0.0715(2) 0.0490(12) Uani 1 1 d . . . H20A H -0.0826 1.9145 -0.1077 0.059 Uiso 1 1 calc R . . C21 C 0.04307(15) 1.5998(8) 0.1105(3) 0.0675(17) Uani 1 1 d . . . C22 C 0.08624(12) 1.5666(7) 0.1412(2) 0.0495(12) Uani 1 1 d . . . C23 C 0.10412(13) 1.4297(7) 0.1803(2) 0.0510(12) Uani 1 1 d . . . H23A H 0.0896 1.3643 0.1887 0.061 Uiso 1 1 calc R . . C24 C 0.14234(13) 1.3875(5) 0.2068(2) 0.0439(11) Uani 1 1 d . . . H24A H 0.1541 1.2914 0.2329 0.053 Uiso 1 1 calc R . . C25 C 0.14854(12) 1.6231(5) 0.1622(2) 0.0408(10) Uani 1 1 d . . . H25A H 0.1645 1.6924 0.1575 0.049 Uiso 1 1 calc R . . C26 C 0.10939(13) 1.6679(7) 0.1337(2) 0.0512(12) Uani 1 1 d . . . H26A H 0.0985 1.7674 0.1092 0.061 Uiso 0.50 1 calc PR . . C27 C 0.0493(7) -0.004(2) 0.6839(7) 0.184(8) Uani 0.50 1 d PGU . . H27A H 0.0349 0.0683 0.6498 0.221 Uiso 0.50 1 calc PR . . C28 C 0.0295(4) -0.124(3) 0.6927(9) 0.214(9) Uani 0.50 1 d PGU . . H28A H 0.0016 -0.1330 0.6646 0.257 Uiso 0.50 1 calc PR . . C29 C 0.0506(7) -0.230(2) 0.7425(11) 0.197(8) Uani 0.50 1 d PGU . . H29A H 0.0370 -0.3117 0.7485 0.237 Uiso 0.50 1 calc PR . . C30 C 0.0914(7) -0.216(2) 0.7836(8) 0.204(9) Uani 0.50 1 d PGU . . H30A H 0.1058 -0.2890 0.8177 0.245 Uiso 0.50 1 calc PR . . C31 C 0.1112(4) -0.097(3) 0.7748(8) 0.183(9) Uani 0.50 1 d PGU . . H31A H 0.1392 -0.0877 0.8029 0.219 Uiso 0.50 1 calc PR . . C32 C 0.0902(7) 0.009(2) 0.7249(10) 0.157(7) Uani 0.50 1 d PGU . . H32A H 0.1037 0.0909 0.7189 0.188 Uiso 0.50 1 calc PR . . O1W O 0.15899(15) 0.8329(6) 0.4893(2) 0.0869(13) Uani 1 1 d U . . O2W O 0.0511(2) 1.7529(13) -0.0110(4) 0.154(3) Uani 0.80 1 d PU . . O3W O 0.0777(15) -0.565(6) 0.858(2) 0.210(19) Uani 0.20 1 d PU . . 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 0.02850(9) 0.03152(9) 0.02876(8) 0.00313(6) 0.01858(7) 0.00044(6) O1 0.0614(19) 0.0366(16) 0.0492(18) 0.0061(13) 0.0456(16) 0.0081(13) O2 0.0508(17) 0.0350(16) 0.0479(18) 0.0071(12) 0.0360(15) 0.0034(12) O3 0.249(6) 0.049(2) 0.111(4) 0.000(2) 0.153(4) 0.001(3) O4 0.0454(16) 0.0421(16) 0.0319(14) 0.0078(12) 0.0271(13) 0.0014(13) O5 0.0358(17) 0.103(3) 0.055(2) 0.021(2) 0.0275(16) 0.0110(19) O6 0.0267(14) 0.062(2) 0.0420(18) 0.0049(15) 0.0158(13) 0.0022(13) O7 0.051(2) 0.204(6) 0.142(5) 0.106(5) 0.063(3) 0.046(3) O8 0.0265(14) 0.0357(15) 0.0586(19) 0.0010(14) 0.0230(14) 0.0059(12) N1 0.089(3) 0.043(2) 0.055(2) 0.0004(18) 0.060(2) -0.002(2) N2 0.0363(17) 0.0377(19) 0.0334(17) 0.0027(14) 0.0238(15) -0.0015(14) N3 0.0270(19) 0.090(3) 0.061(3) 0.015(2) 0.0218(19) 0.014(2) N4 0.0262(16) 0.0365(19) 0.042(2) -0.0048(15) 0.0177(15) 0.0032(14) C1 0.0309(19) 0.038(2) 0.0295(19) 0.0018(16) 0.0189(17) -0.0003(16) C2 0.037(2) 0.039(2) 0.034(2) 0.0018(17) 0.0264(17) 0.0019(17) C3 0.073(3) 0.038(2) 0.055(3) 0.001(2) 0.053(3) 0.000(2) C4 0.086(4) 0.042(2) 0.056(3) -0.004(2) 0.059(3) -0.003(2) C5 0.062(3) 0.043(2) 0.043(2) -0.0003(19) 0.040(2) -0.006(2) C6 0.077(3) 0.036(2) 0.044(2) -0.0022(19) 0.046(2) -0.006(2) C7 0.057(3) 0.044(2) 0.038(2) -0.0012(18) 0.037(2) -0.002(2) C8 0.091(4) 0.048(3) 0.052(3) -0.001(2) 0.056(3) -0.004(3) C9 0.063(3) 0.044(3) 0.043(2) -0.0019(19) 0.040(2) -0.006(2) C10 0.062(3) 0.045(3) 0.042(2) 0.0046(19) 0.038(2) 0.003(2) C11 0.053(3) 0.036(2) 0.039(2) 0.0020(17) 0.032(2) 0.0041(19) C12 0.078(3) 0.039(3) 0.059(3) 0.008(2) 0.054(3) 0.011(2) C13 0.095(4) 0.039(3) 0.065(3) -0.002(2) 0.066(3) 0.002(3) C14 0.028(2) 0.054(3) 0.042(2) -0.001(2) 0.0148(19) 0.0031(19) C15 0.031(2) 0.066(3) 0.043(3) 0.002(2) 0.020(2) 0.007(2) C16 0.042(3) 0.172(7) 0.072(4) 0.059(4) 0.039(3) 0.037(4) C17 0.045(3) 0.195(7) 0.073(4) 0.064(5) 0.039(3) 0.040(4) C18 0.030(2) 0.082(4) 0.051(3) 0.009(3) 0.019(2) 0.014(2) C19 0.037(2) 0.059(3) 0.061(3) 0.004(2) 0.030(2) -0.001(2) C20 0.030(2) 0.061(3) 0.045(3) 0.006(2) 0.018(2) 0.003(2) C21 0.037(3) 0.086(4) 0.077(4) 0.027(3) 0.034(3) 0.014(3) C22 0.030(2) 0.060(3) 0.053(3) 0.009(2) 0.023(2) 0.008(2) C23 0.036(2) 0.058(3) 0.059(3) 0.011(2) 0.029(2) 0.006(2) C24 0.038(2) 0.039(2) 0.053(3) 0.0053(19) 0.028(2) 0.0050(18) C25 0.028(2) 0.040(2) 0.051(3) 0.0034(19) 0.0236(19) 0.0018(17) C26 0.036(2) 0.052(3) 0.057(3) 0.010(2) 0.024(2) 0.009(2) C27 0.211(13) 0.177(13) 0.175(12) -0.006(10) 0.126(10) -0.003(11) C28 0.210(13) 0.226(14) 0.210(13) -0.001(11) 0.132(10) -0.003(11) C29 0.199(12) 0.223(13) 0.208(13) 0.009(11) 0.146(10) 0.001(11) C30 0.210(13) 0.203(13) 0.197(13) -0.009(11) 0.125(10) 0.001(11) C31 0.183(12) 0.181(13) 0.181(13) -0.044(10) 0.113(10) -0.013(10) C32 0.185(12) 0.169(12) 0.170(12) -0.014(10) 0.137(10) -0.030(10) O1W 0.114(4) 0.081(3) 0.092(3) 0.010(2) 0.077(3) 0.017(3) O2W 0.103(5) 0.196(9) 0.158(8) 0.004(6) 0.079(5) 0.017(6) O3W 0.21(2) 0.21(2) 0.21(2) 0.032(17) 0.128(18) -0.031(17) _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 O6 2.423(3) 5_585 ? Pb1 O1 2.508(3) . ? Pb1 O2 2.556(3) . ? Pb1 O8 2.647(3) . ? O1 C1 1.264(5) . ? O2 C1 1.260(5) . ? O3 C8 1.209(6) . ? O4 N2 1.316(4) . ? O5 C14 1.245(6) . ? O6 C14 1.271(6) . ? O6 Pb1 2.423(3) 5_585 ? O7 C21 1.195(7) . ? O8 N4 1.337(4) . ? N1 C8 1.349(6) . ? N1 C5 1.409(6) . ? N1 H1A 0.8800 . ? N2 C12 1.342(6) . ? N2 C11 1.349(5) . ? N3 C21 1.347(7) . ? N3 C18 1.416(6) . ? N3 H3A 0.8800 . ? N4 C24 1.344(6) . ? N4 C25 1.347(5) . ? C1 C2 1.507(6) . ? C2 C7 1.377(6) . ? C2 C3 1.388(6) . ? C3 C4 1.390(6) . ? C3 H3B 0.9500 . ? C4 C5 1.386(6) . ? C4 H4A 0.9500 . ? C5 C6 1.399(6) . ? C6 C7 1.385(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.503(6) . ? C9 C13 1.373(7) . ? C9 C10 1.390(6) . ? C10 C11 1.384(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.369(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.515(6) . ? C15 C20 1.384(7) . ? C15 C16 1.389(7) . ? C16 C17 1.396(7) . ? C16 H16A 0.9500 . ? C17 C18 1.398(8) . ? C17 H17A 0.9500 . ? C18 C19 1.395(7) . ? C19 C20 1.395(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.512(6) . ? C22 C23 1.380(7) . ? C22 C26 1.393(7) . ? C23 C24 1.362(6) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.392(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 H31A 0.9500 . ? C32 H32A 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 O6 Pb1 O1 85.20(11) 5_585 . ? O6 Pb1 O2 78.26(11) 5_585 . ? O1 Pb1 O2 51.54(9) . . ? O6 Pb1 O8 80.39(10) 5_585 . ? O1 Pb1 O8 128.63(10) . . ? O2 Pb1 O8 77.23(9) . . ? C1 O1 Pb1 94.5(2) . . ? C1 O2 Pb1 92.4(2) . . ? C14 O6 Pb1 106.6(3) . 5_585 ? N4 O8 Pb1 125.7(2) . . ? C8 N1 C5 128.7(4) . . ? C8 N1 H1A 115.7 . . ? C5 N1 H1A 115.7 . . ? O4 N2 C12 120.9(3) . . ? O4 N2 C11 119.2(3) . . ? C12 N2 C11 119.9(4) . . ? C21 N3 C18 126.8(5) . . ? C21 N3 H3A 116.6 . . ? C18 N3 H3A 116.6 . . ? O8 N4 C24 120.0(3) . . ? O8 N4 C25 118.9(4) . . ? C24 N4 C25 121.2(4) . . ? O2 C1 O1 121.6(4) . . ? O2 C1 C2 119.9(4) . . ? O1 C1 C2 118.5(4) . . ? C7 C2 C3 119.2(4) . . ? C7 C2 C1 120.6(4) . . ? C3 C2 C1 120.2(4) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3B 120.1 . . ? C4 C3 H3B 120.1 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.5(4) . . ? C4 C5 N1 117.1(4) . . ? C6 C5 N1 123.4(4) . . ? C7 C6 C5 118.8(4) . . ? C7 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? C2 C7 C6 122.0(4) . . ? C2 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? O3 C8 N1 123.5(5) . . ? O3 C8 C9 119.9(5) . . ? N1 C8 C9 116.5(4) . . ? C13 C9 C10 116.9(4) . . ? C13 C9 C8 118.1(4) . . ? C10 C9 C8 124.9(4) . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? N2 C11 C10 120.6(4) . . ? N2 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? N2 C12 C13 120.6(4) . . ? N2 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C9 121.7(4) . . ? C12 C13 H13A 119.2 . . ? C9 C13 H13A 119.2 . . ? O5 C14 O6 124.5(4) . . ? O5 C14 C15 120.1(4) . . ? O6 C14 C15 115.4(4) . . ? C20 C15 C16 118.8(4) . . ? C20 C15 C14 120.7(4) . . ? C16 C15 C14 120.6(5) . . ? C15 C16 C17 121.5(5) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C18 119.2(6) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 N3 116.9(5) . . ? C17 C18 N3 123.4(5) . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C15 C20 C19 120.9(5) . . ? C15 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? O7 C21 N3 123.5(5) . . ? O7 C21 C22 120.0(5) . . ? N3 C21 C22 116.4(5) . . ? C23 C22 C26 117.9(4) . . ? C23 C22 C21 117.9(5) . . ? C26 C22 C21 124.2(4) . . ? C24 C23 C22 120.8(5) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? N4 C24 C23 120.5(4) . . ? N4 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? N4 C25 C26 119.5(4) . . ? N4 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? C25 C26 C22 119.9(4) . . ? C25 C26 H26A 120.0 . . ? C22 C26 H26A 120.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 H27A 120.0 . . ? C32 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.759 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.150 #===========# data_L _database_code_depnum_ccdc_archive 'CCDC 854710' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 N2 O5' _chemical_formula_weight 276.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 4.9278(5) _cell_length_b 13.3692(12) _cell_length_c 18.6056(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.237(3) _cell_angle_gamma 90.00 _cell_volume 1225.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2827 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9770 _exptl_absorpt_correction_T_max 0.9884 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11765 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2825 _reflns_number_gt 2022 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; H atoms of water and carboxylate group were refined freeely, but the O-H distances were constrained by DFIX to close to 0.82, which causes 3 restraints. 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^)+(0.0864P)^2^+0.2902P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2825 _refine_ls_number_parameters 193 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _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 O2 O -0.7651(3) 0.58265(9) 0.52035(7) 0.0238(3) Uani 1 1 d . . . O3 O 0.2442(3) 0.74551(9) 0.75862(7) 0.0243(3) Uani 1 1 d . . . O1 O -0.8395(3) 0.43419(10) 0.57301(7) 0.0240(3) Uani 1 1 d D . . O4 O 1.0500(3) 0.65144(10) 1.00985(7) 0.0266(3) Uani 1 1 d . . . N1 N 0.1012(3) 0.58551(11) 0.77974(8) 0.0187(3) Uani 1 1 d . . . H1A H 0.1249 0.5340 0.8085 0.022 Uiso 1 1 calc R . . N2 N 0.8632(3) 0.65291(11) 0.95882(8) 0.0208(4) Uani 1 1 d . . . O1W O 0.8712(3) 0.61295(10) 0.14748(8) 0.0285(4) Uani 1 1 d D . . C2 C -0.5019(4) 0.53815(13) 0.62308(9) 0.0186(4) Uani 1 1 d . . . C7 C -0.3487(4) 0.62592(13) 0.62046(10) 0.0212(4) Uani 1 1 d . . . H7A H -0.3820 0.6733 0.5834 0.025 Uiso 1 1 calc R . . C5 C -0.1011(4) 0.57448(13) 0.72577(9) 0.0177(4) Uani 1 1 d . . . C3 C -0.4547(4) 0.46887(13) 0.67781(10) 0.0198(4) Uani 1 1 d . . . H3A H -0.5604 0.4096 0.6803 0.024 Uiso 1 1 calc R . . C6 C -0.1479(4) 0.64488(13) 0.67149(10) 0.0212(4) Uani 1 1 d . . . H6A H -0.0442 0.7047 0.6695 0.025 Uiso 1 1 calc R . . C4 C -0.2537(4) 0.48665(13) 0.72843(9) 0.0199(4) Uani 1 1 d . . . H4A H -0.2196 0.4388 0.7651 0.024 Uiso 1 1 calc R . . C12 C 0.8215(4) 0.73790(13) 0.92032(10) 0.0215(4) Uani 1 1 d . . . H12A H 0.9275 0.7957 0.9301 0.026 Uiso 1 1 calc R . . C8 C 0.2635(4) 0.66635(13) 0.79240(9) 0.0180(4) Uani 1 1 d . . . C1 C -0.7136(3) 0.52058(13) 0.56773(9) 0.0180(4) Uani 1 1 d . . . C9 C 0.4689(4) 0.65666(13) 0.85176(9) 0.0184(4) Uani 1 1 d . . . C11 C 0.7173(4) 0.56901(14) 0.94384(10) 0.0229(4) Uani 1 1 d . . . H11A H 0.7521 0.5092 0.9699 0.027 Uiso 1 1 calc R . . C13 C 0.6268(4) 0.74070(13) 0.86724(10) 0.0209(4) Uani 1 1 d . . . H13A H 0.5994 0.8006 0.8407 0.025 Uiso 1 1 calc R . . C10 C 0.5194(4) 0.56990(13) 0.89114(10) 0.0220(4) Uani 1 1 d . . . H10A H 0.4170 0.5111 0.8817 0.026 Uiso 1 1 calc R . . H1 H -0.963(5) 0.429(2) 0.5404(13) 0.063(9) Uiso 1 1 d D . . H1WA H 0.909(6) 0.637(2) 0.1064(11) 0.070(10) Uiso 1 1 d D . . H1WB H 0.834(6) 0.6613(17) 0.1731(15) 0.063(9) Uiso 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 O2 0.0241(7) 0.0258(7) 0.0214(7) 0.0043(5) -0.0056(5) -0.0027(5) O3 0.0294(8) 0.0204(7) 0.0230(7) 0.0027(5) -0.0054(6) -0.0007(5) O1 0.0245(7) 0.0243(7) 0.0232(7) 0.0023(6) -0.0074(6) -0.0048(6) O4 0.0275(8) 0.0310(7) 0.0212(7) -0.0008(6) -0.0104(6) 0.0008(6) N1 0.0203(8) 0.0186(7) 0.0171(7) 0.0006(6) -0.0043(6) 0.0011(6) N2 0.0227(8) 0.0241(8) 0.0154(7) -0.0019(6) -0.0038(6) 0.0014(6) O1W 0.0412(9) 0.0217(7) 0.0227(7) 0.0000(6) -0.0047(7) -0.0012(6) C2 0.0151(8) 0.0231(9) 0.0174(9) -0.0042(7) -0.0021(7) 0.0024(7) C7 0.0242(10) 0.0207(9) 0.0185(9) 0.0006(7) -0.0029(7) 0.0013(7) C5 0.0172(9) 0.0195(9) 0.0164(8) -0.0044(7) -0.0017(7) 0.0029(7) C3 0.0195(9) 0.0200(9) 0.0200(9) -0.0012(7) 0.0000(7) 0.0003(7) C6 0.0220(9) 0.0200(9) 0.0217(9) -0.0001(7) -0.0033(7) -0.0015(7) C4 0.0229(9) 0.0199(9) 0.0171(8) 0.0004(7) -0.0014(7) 0.0036(7) C12 0.0223(10) 0.0199(9) 0.0223(9) -0.0016(7) -0.0030(8) 0.0007(7) C8 0.0183(9) 0.0197(8) 0.0160(8) -0.0032(7) -0.0008(7) 0.0022(7) C1 0.0141(8) 0.0223(9) 0.0176(9) -0.0014(7) -0.0006(7) 0.0011(7) C9 0.0188(9) 0.0215(9) 0.0150(8) -0.0032(7) 0.0008(7) 0.0014(7) C11 0.0261(10) 0.0215(9) 0.0210(9) 0.0031(7) -0.0032(8) 0.0002(7) C13 0.0237(10) 0.0195(9) 0.0195(9) -0.0004(7) -0.0038(7) 0.0029(7) C10 0.0212(9) 0.0230(9) 0.0218(9) 0.0003(7) -0.0029(8) -0.0031(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C1 1.236(2) . ? O3 C8 1.234(2) . ? O1 C1 1.315(2) . ? O1 H1 0.860(18) . ? O4 N2 1.320(2) . ? N1 C8 1.364(2) . ? N1 C5 1.420(2) . ? N1 H1A 0.8800 . ? N2 C12 1.358(2) . ? N2 C11 1.361(2) . ? O1W H1WA 0.853(18) . ? O1W H1WB 0.825(17) . ? C2 C3 1.395(3) . ? C2 C7 1.396(3) . ? C2 C1 1.482(2) . ? C7 C6 1.392(3) . ? C7 H7A 0.9500 . ? C5 C6 1.399(3) . ? C5 C4 1.395(3) . ? C3 C4 1.385(3) . ? C3 H3A 0.9500 . ? C6 H6A 0.9500 . ? C4 H4A 0.9500 . ? C12 C13 1.374(3) . ? C12 H12A 0.9500 . ? C8 C9 1.501(2) . ? C9 C10 1.394(3) . ? C9 C13 1.396(3) . ? C11 C10 1.380(3) . ? C11 H11A 0.9500 . ? C13 H13A 0.9500 . ? C10 H10A 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 C1 O1 H1 110(2) . . ? C8 N1 C5 127.86(15) . . ? C8 N1 H1A 116.1 . . ? C5 N1 H1A 116.1 . . ? O4 N2 C12 119.70(15) . . ? O4 N2 C11 120.10(15) . . ? C12 N2 C11 120.18(17) . . ? H1WA O1W H1WB 105(3) . . ? C3 C2 C7 119.66(17) . . ? C3 C2 C1 121.11(16) . . ? C7 C2 C1 119.23(16) . . ? C2 C7 C6 120.82(17) . . ? C2 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C6 C5 C4 120.29(17) . . ? C6 C5 N1 123.64(16) . . ? C4 C5 N1 116.06(15) . . ? C4 C3 C2 119.93(17) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C7 C6 C5 118.98(17) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C3 C4 C5 120.30(17) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N2 C12 C13 120.36(17) . . ? N2 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? O3 C8 N1 123.19(17) . . ? O3 C8 C9 119.94(16) . . ? N1 C8 C9 116.86(15) . . ? O2 C1 O1 123.19(16) . . ? O2 C1 C2 122.07(16) . . ? O1 C1 C2 114.74(15) . . ? C10 C9 C13 117.60(17) . . ? C10 C9 C8 125.24(16) . . ? C13 C9 C8 117.14(16) . . ? N2 C11 C10 120.65(17) . . ? N2 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C12 C13 C9 120.87(17) . . ? C12 C13 H13A 119.6 . . ? C9 C13 H13A 119.6 . . ? C11 C10 C9 120.30(17) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.422 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.067 #==========================END