# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Ali Morsali' _publ_contact_author_email 'MORSALI A@YAHOO.COM' _publ_section_title ; Dynamic Crystal-to-Crystal Conversion of a 3D-3D Coordination polymer by De- and Rehydration ; loop_ _publ_author_name 'Ali Morsali' 'Alireza Aslani' 'Matthias Zeller' # Attachment 'SH-542_readyfordeposit.cif' data_SH-542 _database_code_depnum_ccdc_archive 'CCDC 660709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C6 H4 N O2)2 Pb' _chemical_formula_sum 'C12 H8 N2 O4 Pb' _chemical_formula_weight 451.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bcn' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 16.595(1) _cell_length_b 10.028(1) _cell_length_c 14.635(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2435.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19872 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description needdle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 13.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0305 _exptl_absorpt_correction_T_max 0.0905 _exptl_absorpt_process_details 'Sortav, Blessing Acta A51 33-70' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa-CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37528 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3553 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.4500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3553 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb -0.435654(8) 0.379691(14) -0.384065(10) 0.02561(6) Uani 1 1 d . . . O1 O -0.31492(17) 0.3274(3) -0.2955(2) 0.0336(7) Uani 1 1 d . . . O2 O -0.41167(19) 0.3575(3) -0.1938(2) 0.0403(7) Uani 1 1 d . . . O3 O -0.3906(3) 0.6154(3) -0.3450(3) 0.0535(10) Uani 1 1 d . . . O4 O -0.4899(2) 0.6336(3) -0.4451(2) 0.0422(8) Uani 1 1 d . . . N1 N -0.1797(2) 0.1780(4) -0.0082(3) 0.0353(8) Uani 1 1 d . . . N2 N -0.4439(3) 0.1097(4) -0.3574(4) 0.0441(10) Uani 1 1 d . . . C1 C -0.3422(2) 0.3237(4) -0.2154(3) 0.0294(9) Uani 1 1 d . . . C2 C -0.2858(2) 0.2701(4) -0.1424(3) 0.0283(9) Uani 1 1 d . . . C3 C -0.2217(3) 0.1889(4) -0.1641(3) 0.0329(9) Uani 1 1 d . . . H3 H -0.2127 0.1644 -0.2245 0.040 Uiso 1 1 calc R . . C4 C -0.1712(3) 0.1444(5) -0.0965(3) 0.0348(10) Uani 1 1 d . . . H4 H -0.1289 0.0882 -0.1127 0.042 Uiso 1 1 calc R . . C5 C -0.2423(3) 0.2562(5) 0.0123(3) 0.0382(10) Uani 1 1 d . . . H5 H -0.2499 0.2802 0.0731 0.046 Uiso 1 1 calc R . . C6 C -0.2962(3) 0.3035(5) -0.0518(3) 0.0351(10) Uani 1 1 d . . . H6 H -0.3391 0.3573 -0.0340 0.042 Uiso 1 1 calc R . . C7 C -0.4428(3) 0.6830(5) -0.3877(3) 0.0314(9) Uani 1 1 d . . . C8 C -0.4455(3) 0.8305(5) -0.3719(3) 0.0311(9) Uani 1 1 d . . . C9 C -0.3783(3) 0.8985(4) -0.3416(4) 0.0400(11) Uani 1 1 d . . . H9 H -0.3324 0.8517 -0.3243 0.048 Uiso 1 1 calc R . . C10 C -0.3792(3) 0.0358(4) -0.3371(4) 0.0445(12) Uani 1 1 d . . . H10 H -0.3324 0.0793 -0.3190 0.053 Uiso 1 1 calc R . . C11 C -0.5111(3) 0.0431(5) -0.3829(4) 0.0456(12) Uani 1 1 d . . . H11 H -0.5577 0.0916 -0.3947 0.055 Uiso 1 1 calc R . . C12 C -0.5135(3) 0.9062(5) -0.3921(4) 0.0433(12) Uani 1 1 d . . . H12 H -0.5605 0.8646 -0.4118 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.02591(9) 0.02371(9) 0.02721(9) 0.00030(6) -0.00097(6) 0.00058(5) O1 0.0298(15) 0.0431(16) 0.0278(16) 0.0007(13) -0.0001(13) 0.0021(13) O2 0.0261(14) 0.057(2) 0.0375(19) 0.0020(16) 0.0022(13) 0.0079(14) O3 0.065(3) 0.0277(17) 0.068(3) -0.0017(16) -0.031(2) -0.0005(16) O4 0.0472(19) 0.0316(16) 0.048(2) -0.0078(14) -0.0136(16) 0.0024(14) N1 0.0299(19) 0.044(2) 0.032(2) 0.0039(16) -0.0028(15) 0.0030(16) N2 0.048(3) 0.027(2) 0.058(3) 0.0005(17) 0.000(2) 0.0017(17) C1 0.028(2) 0.029(2) 0.032(2) -0.0012(17) -0.0037(17) -0.0039(16) C2 0.025(2) 0.035(2) 0.025(2) 0.0004(16) -0.0013(16) -0.0015(16) C3 0.036(2) 0.038(2) 0.024(2) -0.0003(18) 0.0000(18) 0.0048(18) C4 0.026(2) 0.039(2) 0.040(3) -0.0009(19) -0.0035(18) 0.0036(18) C5 0.039(2) 0.050(3) 0.025(2) -0.003(2) 0.0002(19) 0.003(2) C6 0.030(2) 0.044(2) 0.032(2) 0.0028(19) -0.0003(18) 0.0088(19) C7 0.033(2) 0.028(2) 0.033(2) -0.0041(17) -0.0029(19) -0.0020(16) C8 0.033(2) 0.029(2) 0.032(2) -0.0031(17) -0.0032(17) 0.0003(17) C9 0.043(3) 0.027(2) 0.050(3) -0.0014(19) -0.013(2) -0.0031(19) C10 0.045(3) 0.033(2) 0.056(3) -0.004(2) -0.013(2) -0.008(2) C11 0.040(3) 0.034(2) 0.063(4) -0.002(2) -0.002(2) 0.008(2) C12 0.038(3) 0.035(2) 0.058(3) -0.002(2) -0.005(2) -0.003(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 Pb O1 2.443(3) . ? Pb O3 2.544(3) . ? Pb N1 2.701(4) 2_454 ? Pb N2 2.739(4) . ? O1 C1 1.258(5) . ? O2 C1 1.242(5) . ? O3 C7 1.265(6) . ? O4 C7 1.251(5) . ? N1 C5 1.336(6) . ? N1 C4 1.343(6) . ? N1 Pb 2.701(4) 2_455 ? N2 C10 1.338(6) . ? N2 C11 1.351(7) . ? C1 C2 1.519(6) . ? C2 C3 1.377(6) . ? C2 C6 1.378(6) . ? C3 C4 1.371(6) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.380(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.497(6) . ? C8 C9 1.381(6) . ? C8 C12 1.392(7) . ? C9 C10 1.378(6) 1_565 ? C9 H9 0.9300 . ? C10 C9 1.378(6) 1_545 ? C10 H10 0.9300 . ? C11 C12 1.380(6) 1_545 ? C11 H11 0.9300 . ? C12 C11 1.380(6) 1_565 ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb O3 80.73(11) . . ? O1 Pb N1 74.32(10) . 2_454 ? O3 Pb N1 98.14(14) . 2_454 ? O1 Pb N2 75.73(12) . . ? O3 Pb N2 154.30(13) . . ? N1 Pb N2 85.40(13) 2_454 . ? C1 O1 Pb 101.9(2) . . ? C7 O3 Pb 100.7(3) . . ? C5 N1 C4 116.4(4) . . ? C5 N1 Pb 121.7(3) . 2_455 ? C4 N1 Pb 121.3(3) . 2_455 ? C10 N2 C11 116.6(4) . . ? C10 N2 Pb 122.6(3) . . ? C11 N2 Pb 119.4(3) . . ? O2 C1 O1 124.3(4) . . ? O2 C1 C2 119.3(4) . . ? O1 C1 C2 116.4(4) . . ? C3 C2 C6 117.6(4) . . ? C3 C2 C1 121.5(4) . . ? C6 C2 C1 120.9(4) . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? N1 C4 C3 123.3(4) . . ? N1 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? N1 C5 C6 123.6(4) . . ? N1 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C2 C6 C5 119.3(4) . . ? C2 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O4 C7 O3 123.2(4) . . ? O4 C7 C8 118.4(4) . . ? O3 C7 C8 118.3(4) . . ? C9 C8 C12 117.0(4) . . ? C9 C8 C7 120.9(4) . . ? C12 C8 C7 122.0(4) . . ? C10 C9 C8 120.0(5) 1_565 . ? C10 C9 H9 120.0 1_565 . ? C8 C9 H9 120.0 . . ? N2 C10 C9 123.5(5) . 1_545 ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 1_545 . ? N2 C11 C12 122.9(5) . 1_545 ? N2 C11 H11 118.6 . . ? C12 C11 H11 118.6 1_545 . ? C11 C12 C8 119.8(5) 1_565 . ? C11 C12 H12 120.1 1_565 . ? C8 C12 H12 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Pb O1 C1 87.5(3) . . . . ? N1 Pb O1 C1 -171.3(3) 2_454 . . . ? N2 Pb O1 C1 -82.1(3) . . . . ? O1 Pb O3 C7 176.9(3) . . . . ? N1 Pb O3 C7 104.4(3) 2_454 . . . ? N2 Pb O3 C7 -159.3(3) . . . . ? O1 Pb N2 C10 -21.1(4) . . . . ? O3 Pb N2 C10 -45.4(7) . . . . ? N1 Pb N2 C10 53.9(5) 2_454 . . . ? O1 Pb N2 C11 172.6(4) . . . . ? O3 Pb N2 C11 148.3(4) . . . . ? N1 Pb N2 C11 -112.5(4) 2_454 . . . ? Pb O1 C1 O2 -8.3(5) . . . . ? Pb O1 C1 C2 169.9(3) . . . . ? O2 C1 C2 C3 156.5(4) . . . . ? O1 C1 C2 C3 -21.9(6) . . . . ? O2 C1 C2 C6 -24.9(6) . . . . ? O1 C1 C2 C6 156.8(4) . . . . ? C6 C2 C3 C4 0.1(6) . . . . ? C1 C2 C3 C4 178.8(4) . . . . ? C5 N1 C4 C3 1.6(7) . . . . ? Pb N1 C4 C3 -169.7(3) 2_455 . . . ? C2 C3 C4 N1 -1.3(7) . . . . ? C4 N1 C5 C6 -0.7(7) . . . . ? Pb N1 C5 C6 170.5(4) 2_455 . . . ? C3 C2 C6 C5 0.7(7) . . . . ? C1 C2 C6 C5 -178.0(4) . . . . ? N1 C5 C6 C2 -0.4(8) . . . . ? Pb O3 C7 O4 -11.8(6) . . . . ? Pb O3 C7 C8 171.3(3) . . . . ? O4 C7 C8 C9 -153.0(5) . . . . ? O3 C7 C8 C9 24.0(7) . . . . ? O4 C7 C8 C12 23.1(7) . . . . ? O3 C7 C8 C12 -159.9(5) . . . . ? C12 C8 C9 C10 -3.4(7) . . . 1_565 ? C7 C8 C9 C10 172.9(5) . . . 1_565 ? C11 N2 C10 C9 0.4(9) . . . 1_545 ? Pb N2 C10 C9 -166.3(4) . . . 1_545 ? C10 N2 C11 C12 -2.9(8) . . . 1_545 ? Pb N2 C11 C12 164.3(4) . . . 1_545 ? C9 C8 C12 C11 1.1(7) . . . 1_565 ? C7 C8 C12 C11 -175.2(5) . . . 1_565 ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max 1.093 _refine_diff_density_min -1.723 _refine_diff_density_rms .238 # Attachment '315-A_07mz536_0m.cif' data_07mz536_0m _database_code_depnum_ccdc_archive 'CCDC 671943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 N2 O5 Pb' _chemical_formula_weight 469.42 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 Cc 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' _cell_length_a 10.8842(16) _cell_length_b 18.437(3) _cell_length_c 7.0724(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.218(2) _cell_angle_gamma 90.00 _cell_volume 1323.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3335 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 31.68 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 12.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.069 _exptl_absorpt_correction_T_max 0.114 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 6202 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3170 _reflns_number_gt 2992 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'Apex2 v2.1-4' _computing_data_reduction 'Apex2 v2.1-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1520 Friedel pairs' _refine_ls_abs_structure_Flack 0.005(8) _refine_ls_number_reflns 3170 _refine_ls_number_parameters 188 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.844 _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 C1 C 0.6559(5) 0.4532(3) 0.0287(8) 0.0142(10) Uani 1 1 d . . . C2 C 0.5215(5) 0.4633(3) -0.1312(8) 0.0147(11) Uani 1 1 d . . . C3 C 0.4729(5) 0.5321(3) -0.1931(8) 0.0184(11) Uani 1 1 d . . . H3 H 0.5255 0.5737 -0.1396 0.022 Uiso 1 1 calc R . . C4 C 0.3458(6) 0.5395(3) -0.3350(8) 0.0226(12) Uani 1 1 d . . . H4 H 0.3128 0.5871 -0.3743 0.027 Uiso 1 1 calc R . . C5 C 0.3145(6) 0.4170(4) -0.3577(9) 0.0259(14) Uani 1 1 d . . . H5 H 0.2593 0.3767 -0.4159 0.031 Uiso 1 1 calc R . . C6 C 0.4387(6) 0.4037(3) -0.2146(9) 0.0225(12) Uani 1 1 d . . . H6 H 0.4673 0.3556 -0.1738 0.027 Uiso 1 1 calc R . . C7 C 0.5321(7) 0.1749(4) 0.7291(11) 0.0155(14) Uani 1 1 d . . . C8 C 0.6157(5) 0.2249(3) 0.6542(9) 0.0159(11) Uani 1 1 d . . . C9 C 0.6196(7) 0.2186(3) 0.4611(9) 0.0248(15) Uani 1 1 d . . . H9 H 0.5719 0.1815 0.3714 0.030 Uiso 1 1 calc R . . C10 C 0.6954(7) 0.2681(3) 0.4024(8) 0.0242(13) Uani 1 1 d . . . H10 H 0.6983 0.2635 0.2703 0.029 Uiso 1 1 calc R . . C11 C 0.7602(6) 0.3267(3) 0.7091(8) 0.0180(11) Uani 1 1 d . . . H11 H 0.8082 0.3643 0.7964 0.022 Uiso 1 1 calc R . . C12 C 0.6891(6) 0.2792(3) 0.7776(10) 0.0184(13) Uani 1 1 d . . . H12 H 0.6902 0.2838 0.9121 0.022 Uiso 1 1 calc R . . N1 N 0.2683(5) 0.4837(3) -0.4181(7) 0.0273(12) Uani 1 1 d . . . N2 N 0.7643(6) 0.3216(3) 0.5207(9) 0.0181(13) Uani 1 1 d . . . O1 O 0.7334(4) 0.5070(2) 0.0744(5) 0.0164(8) Uani 1 1 d . . . O2 O 0.6831(4) 0.3924(2) 0.1166(6) 0.0184(8) Uani 1 1 d . . . O3 O 0.5139(5) 0.1921(2) 0.8882(7) 0.0298(11) Uani 1 1 d . . . O4 O 0.4858(4) 0.1175(2) 0.6312(5) 0.0213(9) Uani 1 1 d . . . O5 O 0.5282(4) 0.0435(2) 0.3252(6) 0.0207(9) Uani 1 1 d D . . H5A H 0.531(8) 0.073(3) 0.418(7) 0.031 Uiso 1 1 d D . . H5B H 0.597(4) 0.021(3) 0.388(9) 0.031 Uiso 1 1 d D . . Pb1 Pb 0.88347(2) 0.423661(7) 0.39704(3) 0.01037(5) 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 C1 0.012(2) 0.016(3) 0.017(3) -0.003(2) 0.007(2) -0.003(2) C2 0.009(2) 0.025(3) 0.010(2) 0.000(2) 0.004(2) -0.001(2) C3 0.015(3) 0.028(3) 0.014(3) 0.002(2) 0.008(2) 0.004(2) C4 0.021(3) 0.032(3) 0.018(3) 0.003(2) 0.010(2) 0.013(3) C5 0.018(3) 0.044(4) 0.018(3) -0.009(3) 0.009(2) -0.004(3) C6 0.019(3) 0.025(3) 0.021(3) -0.004(2) 0.004(2) -0.001(2) C7 0.013(3) 0.012(3) 0.021(4) 0.006(2) 0.006(3) 0.005(2) C8 0.018(3) 0.014(3) 0.016(3) -0.001(2) 0.006(2) -0.003(2) C9 0.042(4) 0.014(3) 0.018(3) -0.005(2) 0.011(3) -0.008(3) C10 0.043(4) 0.020(3) 0.016(3) 0.000(2) 0.018(3) -0.005(3) C11 0.020(3) 0.022(3) 0.009(3) -0.001(2) 0.002(2) -0.004(2) C12 0.020(3) 0.018(3) 0.018(3) -0.003(2) 0.008(3) -0.002(2) N1 0.018(3) 0.050(4) 0.017(3) 0.001(2) 0.010(2) 0.004(2) N2 0.023(3) 0.016(3) 0.019(3) 0.002(2) 0.012(3) -0.003(2) O1 0.0156(19) 0.019(2) 0.0147(18) 0.0004(15) 0.0051(15) -0.0031(15) O2 0.018(2) 0.020(2) 0.0156(19) -0.0011(16) 0.0038(16) -0.0025(16) O3 0.046(3) 0.019(2) 0.040(3) -0.006(2) 0.035(3) -0.010(2) O4 0.027(2) 0.021(2) 0.0163(19) 0.0012(16) 0.0080(17) -0.0122(18) O5 0.014(2) 0.022(2) 0.021(2) -0.0016(17) 0.0009(17) -0.0020(17) Pb1 0.01102(7) 0.01042(7) 0.01034(7) 0.00016(17) 0.00467(5) 0.00010(18) _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 C1 O2 1.264(7) . ? C1 O1 1.266(6) . ? C1 C2 1.501(7) . ? C2 C3 1.383(8) . ? C2 C6 1.409(8) . ? C3 C4 1.391(7) . ? C3 H3 0.9500 . ? C4 N1 1.326(8) . ? C4 H4 0.9500 . ? C5 N1 1.339(8) . ? C5 C6 1.386(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O3 1.253(8) . ? C7 O4 1.264(8) . ? C7 C8 1.519(8) . ? C8 C12 1.379(8) . ? C8 C9 1.386(8) . ? C9 C10 1.390(9) . ? C9 H9 0.9500 . ? C10 N2 1.335(8) . ? C10 H10 0.9500 . ? C11 N2 1.352(8) . ? C11 C12 1.368(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? N2 Pb1 2.610(6) . ? O1 Pb1 2.713(4) 2_564 ? O1 Pb1 2.746(4) . ? O2 Pb1 2.427(4) . ? O3 Pb1 2.577(4) 4_455 ? O4 Pb1 2.620(4) 4_455 ? O5 H5A 0.84(2) . ? O5 H5B 0.83(2) . ? Pb1 O3 2.577(4) 4_554 ? Pb1 O4 2.620(4) 4_554 ? Pb1 O1 2.713(4) 2_565 ? 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 C1 O1 123.6(5) . . ? O2 C1 C2 118.1(5) . . ? O1 C1 C2 118.2(5) . . ? C3 C2 C6 118.0(5) . . ? C3 C2 C1 120.6(5) . . ? C6 C2 C1 121.3(5) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? N1 C4 C3 123.4(6) . . ? N1 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? N1 C5 C6 123.3(6) . . ? N1 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C2 118.4(6) . . ? C5 C6 H6 120.8 . . ? C2 C6 H6 120.8 . . ? O3 C7 O4 122.9(6) . . ? O3 C7 C8 118.0(6) . . ? O4 C7 C8 119.2(6) . . ? C12 C8 C9 117.9(5) . . ? C12 C8 C7 120.2(6) . . ? C9 C8 C7 121.9(5) . . ? C8 C9 C10 118.2(5) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 123.8(5) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N2 C11 C12 122.0(6) . . ? N2 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C8 120.9(6) . . ? C11 C12 H12 119.6 . . ? C8 C12 H12 119.6 . . ? C4 N1 C5 117.8(5) . . ? C10 N2 C11 117.3(6) . . ? C10 N2 Pb1 123.9(4) . . ? C11 N2 Pb1 118.5(4) . . ? C1 O1 Pb1 135.1(3) . 2_564 ? C1 O1 Pb1 85.1(3) . . ? Pb1 O1 Pb1 111.79(13) 2_564 . ? C1 O2 Pb1 99.9(3) . . ? C7 O3 Pb1 94.5(4) . 4_455 ? C7 O4 Pb1 92.2(4) . 4_455 ? H5A O5 H5B 97(6) . . ? O2 Pb1 O3 97.08(15) . 4_554 ? O2 Pb1 N2 72.19(16) . . ? O3 Pb1 N2 75.86(17) 4_554 . ? O2 Pb1 O4 80.46(13) . 4_554 ? O3 Pb1 O4 50.33(13) 4_554 4_554 ? N2 Pb1 O4 115.03(16) . 4_554 ? O2 Pb1 O1 88.65(12) . 2_565 ? O3 Pb1 O1 146.18(13) 4_554 2_565 ? N2 Pb1 O1 74.29(15) . 2_565 ? O4 Pb1 O1 162.12(11) 4_554 2_565 ? O2 Pb1 O1 50.61(12) . . ? O3 Pb1 O1 127.64(14) 4_554 . ? N2 Pb1 O1 117.63(16) . . ? O4 Pb1 O1 81.11(12) 4_554 . ? O1 Pb1 O1 81.02(8) 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 162.5(5) . . . . ? O1 C1 C2 C3 -14.4(8) . . . . ? O2 C1 C2 C6 -14.2(8) . . . . ? O1 C1 C2 C6 169.0(5) . . . . ? C6 C2 C3 C4 -0.4(8) . . . . ? C1 C2 C3 C4 -177.2(5) . . . . ? C2 C3 C4 N1 -1.3(8) . . . . ? N1 C5 C6 C2 -1.2(9) . . . . ? C3 C2 C6 C5 1.6(8) . . . . ? C1 C2 C6 C5 178.3(5) . . . . ? O3 C7 C8 C12 12.2(9) . . . . ? O4 C7 C8 C12 -166.8(6) . . . . ? O3 C7 C8 C9 -166.7(6) . . . . ? O4 C7 C8 C9 14.3(9) . . . . ? C12 C8 C9 C10 -1.0(10) . . . . ? C7 C8 C9 C10 177.9(6) . . . . ? C8 C9 C10 N2 -0.3(10) . . . . ? N2 C11 C12 C8 -1.5(9) . . . . ? C9 C8 C12 C11 1.9(10) . . . . ? C7 C8 C12 C11 -177.1(6) . . . . ? C3 C4 N1 C5 1.7(8) . . . . ? C6 C5 N1 C4 -0.4(9) . . . . ? C9 C10 N2 C11 0.8(10) . . . . ? C9 C10 N2 Pb1 -172.4(5) . . . . ? C12 C11 N2 C10 0.1(9) . . . . ? C12 C11 N2 Pb1 173.6(5) . . . . ? O2 C1 O1 Pb1 107.9(5) . . . 2_564 ? C2 C1 O1 Pb1 -75.5(6) . . . 2_564 ? O2 C1 O1 Pb1 -8.4(5) . . . . ? C2 C1 O1 Pb1 168.3(4) . . . . ? O1 C1 O2 Pb1 9.6(6) . . . . ? C2 C1 O2 Pb1 -167.1(4) . . . . ? O4 C7 O3 Pb1 2.4(7) . . . 4_455 ? C8 C7 O3 Pb1 -176.5(5) . . . 4_455 ? O3 C7 O4 Pb1 -2.3(7) . . . 4_455 ? C8 C7 O4 Pb1 176.6(5) . . . 4_455 ? C1 O2 Pb1 O3 -138.7(3) . . . 4_554 ? C1 O2 Pb1 N2 148.6(4) . . . . ? C1 O2 Pb1 O4 -91.0(3) . . . 4_554 ? C1 O2 Pb1 O1 74.7(3) . . . 2_565 ? C1 O2 Pb1 O1 -4.8(3) . . . . ? C10 N2 Pb1 O2 34.4(5) . . . . ? C11 N2 Pb1 O2 -138.6(5) . . . . ? C10 N2 Pb1 O3 -68.0(5) . . . 4_554 ? C11 N2 Pb1 O3 119.0(5) . . . 4_554 ? C10 N2 Pb1 O4 -35.6(6) . . . 4_554 ? C11 N2 Pb1 O4 151.4(4) . . . 4_554 ? C10 N2 Pb1 O1 128.1(5) . . . 2_565 ? C11 N2 Pb1 O1 -44.9(4) . . . 2_565 ? C10 N2 Pb1 O1 57.4(6) . . . . ? C11 N2 Pb1 O1 -115.6(4) . . . . ? C1 O1 Pb1 O2 4.7(3) . . . . ? Pb1 O1 Pb1 O2 -132.3(2) 2_564 . . . ? C1 O1 Pb1 O3 69.1(3) . . . 4_554 ? Pb1 O1 Pb1 O3 -67.9(2) 2_564 . . 4_554 ? C1 O1 Pb1 N2 -24.1(4) . . . . ? Pb1 O1 Pb1 N2 -161.06(17) 2_564 . . . ? C1 O1 Pb1 O4 89.6(3) . . . 4_554 ? Pb1 O1 Pb1 O4 -47.39(14) 2_564 . . 4_554 ? C1 O1 Pb1 O1 -91.0(3) . . . 2_565 ? Pb1 O1 Pb1 O1 132.02(18) 2_564 . . 2_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O4 0.84(2) 1.93(3) 2.736(6) 159(7) . O5 H5B N1 0.83(2) 2.00(2) 2.812(6) 168(7) 3_546 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.110 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.128