# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author ; Fan,Yong College of Chemistry Jilin University Changchun, 130012 P. R. China ; _publ_contact_author_phone 86-431-85167469 _publ_contact_author_fax 86-431-85168439 _publ_contact_author_email jiayin_sun@yahoo.com.cn _publ_requested_coeditor_name ? #========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Hydrothermal Synthesis and Crystal Structure of a Novel Lead Complex :[Pb4(OH)4(C8N8H4)2]2H2O ; loop_ _publ_author_address ; College of Chemistry Jilin University Changchun, 130012 P. R. China ; ; College of Chemistry Jilin University Changchun, 130012 P. R. China ; _publ_contact_author_name 'JiaYin Sun' _publ_author_name 'Yong Fan' #================================================= data_1 _database_code_depnum_ccdc_archive 'CCDC 849344' #TrackingRef 'CCDC-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H8 N16 O6 Pb4 ' _chemical_formula_sum 'C16 H8 N16 O6 Pb4' _chemical_formula_weight 1349.14 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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_space_group_name_Hall 'P 2c -2ac ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 25.361(5) _cell_length_b 7.8374(16) _cell_length_c 12.844(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2552.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 26.369 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'Bruker AXS SMART APEX CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24202 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5382 _reflns_number_gt 5050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997-2002)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2003)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+7.3682P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(11) _refine_ls_number_reflns 5382 _refine_ls_number_parameters 379 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 O6 O 0.3533(3) 0.5691(14) 0.7887(7) 0.046(2) Uani 1 1 d . . . C8 C 0.1898(4) 1.0707(14) 0.5586(8) 0.024(2) Uani 1 1 d . . . C4 C 0.1018(4) 1.2026(15) 0.5734(9) 0.025(2) Uani 1 1 d . . . H4 H 0.0964 1.1852 0.5026 0.030 Uiso 1 1 calc R . . C3 C 0.1504(3) 1.1503(13) 0.6191(9) 0.0179(18) Uani 1 1 d . . . C2 C 0.1576(4) 1.1911(15) 0.7253(8) 0.023(2) Uani 1 1 d . . . H2 H 0.1896 1.1643 0.7567 0.027 Uiso 1 1 calc R . . C16 C 0.2732(3) 0.5077(15) 0.0363(8) 0.024(2) Uani 1 1 d . . . C12 C 0.3098(3) 0.5961(14) 0.1060(9) 0.023(2) Uani 1 1 d . . . C11 C 0.3632(4) 0.6191(15) 0.0764(8) 0.025(2) Uani 1 1 d . . . H11 H 0.3751 0.5769 0.0129 0.030 Uiso 1 1 calc R . . C13 C 0.2947(4) 0.6481(18) 0.2023(9) 0.036(3) Uani 1 1 d . . . H13 H 0.2602 0.6291 0.2242 0.043 Uiso 1 1 calc R . . C14 C 0.3305(4) 0.7306(15) 0.2694(8) 0.025(2) Uani 1 1 d . . . H14 H 0.3193 0.7680 0.3344 0.030 Uiso 1 1 calc R . . C9 C 0.3820(4) 0.7563(14) 0.2398(8) 0.022(2) Uani 1 1 d . . . C10 C 0.3972(4) 0.7030(16) 0.1410(9) 0.029(3) Uani 1 1 d . . . H10 H 0.4313 0.7252 0.1183 0.035 Uiso 1 1 calc R . . C5 C 0.0624(4) 1.2786(15) 0.6319(8) 0.027(2) Uani 1 1 d . . . H5 H 0.0304 1.3058 0.6008 0.033 Uiso 1 1 calc R . . C6 C 0.0703(3) 1.3149(13) 0.7371(8) 0.020(2) Uani 1 1 d . . . C1 C 0.1191(4) 1.2689(15) 0.7842(8) 0.023(2) Uani 1 1 d . . . H1 H 0.1249 1.2912 0.8544 0.028 Uiso 1 1 calc R . . C15 C 0.4199(4) 0.8378(15) 0.3103(8) 0.021(2) Uani 1 1 d . . . C7 C 0.0303(4) 1.4017(15) 0.7981(8) 0.023(2) Uani 1 1 d . . . O5 O 0.4139(3) 0.4922(12) 0.5896(7) 0.044(2) Uani 1 1 d . . . N1 N 0.1821(3) 1.0057(13) 0.4633(7) 0.026(2) Uani 1 1 d . . . N2 N 0.2280(3) 0.9309(13) 0.4353(7) 0.027(2) Uani 1 1 d . . . N3 N 0.2639(3) 0.9591(15) 0.5103(7) 0.034(2) Uani 1 1 d . . . N4 N 0.2406(3) 1.0453(13) 0.5874(7) 0.029(2) Uani 1 1 d . . . N5 N -0.0161(3) 1.4569(13) 0.7586(7) 0.028(2) Uani 1 1 d . . . N6 N -0.0407(3) 1.5232(13) 0.8433(8) 0.031(2) Uani 1 1 d . . . N7 N -0.0127(4) 1.5086(16) 0.9237(8) 0.040(3) Uani 1 1 d . . . N8 N 0.0328(4) 1.4332(16) 0.9013(8) 0.037(3) Uani 1 1 d . . . N9 N 0.4693(3) 0.8932(13) 0.2787(7) 0.028(2) Uani 1 1 d . . . N10 N 0.4902(3) 0.9675(13) 0.3647(7) 0.027(2) Uani 1 1 d . . . N11 N 0.4565(3) 0.9560(14) 0.4399(7) 0.031(2) Uani 1 1 d . . . N12 N 0.4127(3) 0.8759(14) 0.4104(7) 0.030(2) Uani 1 1 d . . . N13 N 0.2845(3) 0.4615(15) -0.0607(7) 0.032(2) Uani 1 1 d . . . N14 N 0.2421(4) 0.3783(13) -0.0972(8) 0.033(2) Uani 1 1 d . . . N15 N 0.2066(3) 0.3728(14) -0.0249(8) 0.035(2) Uani 1 1 d . . . N16 N 0.2248(3) 0.4563(17) 0.0600(7) 0.041(3) Uani 1 1 d . . . O1 O 0.3256(3) 0.9198(9) 0.7413(5) 0.0224(16) Uani 1 1 d . . . O2 O 0.4026(2) 1.1706(10) 0.7759(6) 0.0218(15) Uani 1 1 d . . . O3 O 0.4306(2) 0.8712(9) 0.6712(6) 0.0212(15) Uani 1 1 d . . . O4 O 0.3637(2) 1.1096(9) 0.5765(5) 0.0202(15) Uani 1 1 d . . . Pb1 Pb 0.350566(13) 0.79167(6) 0.57610(3) 0.02365(10) Uani 1 1 d . . . Pb2 Pb 0.310604(15) 1.21572(6) 0.71046(3) 0.02752(10) Uani 1 1 d . . . Pb3 Pb 0.453418(14) 1.14531(6) 0.61743(3) 0.02288(9) Uani 1 1 d . . . Pb4 Pb 0.400383(14) 0.89968(5) 0.84895(3) 0.02156(9) 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 O6 0.043(5) 0.053(7) 0.041(5) 0.010(5) 0.001(4) -0.001(4) C8 0.024(5) 0.017(6) 0.032(6) -0.004(5) -0.003(4) -0.005(4) C4 0.030(5) 0.028(7) 0.018(5) -0.009(5) 0.000(4) -0.002(4) C3 0.020(4) 0.007(5) 0.027(4) 0.000(4) 0.004(5) -0.004(4) C2 0.018(4) 0.030(7) 0.019(5) -0.003(4) -0.003(4) 0.002(4) C16 0.019(4) 0.028(7) 0.024(5) -0.004(4) -0.001(4) -0.001(4) C12 0.020(4) 0.020(6) 0.030(6) 0.000(5) 0.000(4) 0.006(4) C11 0.019(4) 0.035(7) 0.022(5) -0.008(5) 0.009(4) -0.001(4) C13 0.020(5) 0.055(9) 0.033(6) -0.016(6) -0.008(5) -0.002(5) C14 0.024(5) 0.035(7) 0.016(5) 0.000(4) 0.008(4) 0.002(4) C9 0.021(4) 0.021(6) 0.023(5) 0.002(4) -0.001(4) 0.003(4) C10 0.019(4) 0.034(8) 0.035(7) 0.009(5) 0.005(4) -0.003(4) C5 0.025(5) 0.032(7) 0.024(6) -0.005(5) -0.004(4) -0.001(4) C6 0.020(4) 0.011(5) 0.029(6) 0.003(4) -0.006(4) -0.002(4) C1 0.023(5) 0.026(7) 0.021(5) 0.014(4) -0.011(4) 0.001(4) C15 0.018(4) 0.021(6) 0.024(5) -0.001(4) -0.004(4) 0.004(4) C7 0.028(5) 0.025(7) 0.015(5) -0.001(4) 0.000(4) 0.004(4) O5 0.052(5) 0.034(6) 0.046(5) -0.010(4) 0.002(4) 0.010(4) N1 0.016(4) 0.029(6) 0.033(5) -0.011(4) -0.008(3) 0.004(3) N2 0.018(4) 0.031(6) 0.033(5) -0.007(4) -0.009(4) 0.004(4) N3 0.018(4) 0.045(7) 0.039(6) -0.011(5) -0.011(4) 0.008(4) N4 0.021(4) 0.037(6) 0.027(5) -0.009(4) 0.002(4) 0.005(4) N5 0.022(4) 0.031(6) 0.031(5) -0.005(4) -0.002(4) 0.002(4) N6 0.032(4) 0.023(6) 0.037(5) -0.004(5) 0.008(4) 0.000(4) N7 0.042(6) 0.047(8) 0.032(6) -0.002(5) 0.004(5) 0.005(5) N8 0.036(5) 0.046(8) 0.029(5) -0.013(5) -0.002(4) 0.016(5) N9 0.023(4) 0.036(7) 0.025(4) -0.004(4) 0.007(4) -0.002(4) N10 0.021(4) 0.032(6) 0.029(5) -0.009(4) -0.002(4) -0.001(4) N11 0.031(4) 0.033(6) 0.029(5) -0.019(4) 0.008(4) -0.007(4) N12 0.019(4) 0.043(7) 0.028(5) -0.011(4) 0.001(4) -0.003(4) N13 0.031(5) 0.038(7) 0.027(5) 0.000(5) -0.008(4) -0.008(4) N14 0.032(4) 0.027(6) 0.039(5) -0.009(4) -0.002(4) -0.001(4) N15 0.026(4) 0.042(7) 0.035(5) -0.006(5) -0.004(4) -0.009(4) N16 0.028(4) 0.075(9) 0.021(5) -0.005(5) 0.003(4) -0.017(5) O1 0.019(3) 0.024(5) 0.025(4) -0.002(3) 0.000(3) -0.003(3) O2 0.020(3) 0.015(4) 0.030(4) -0.001(3) 0.000(3) -0.003(3) O3 0.020(3) 0.016(4) 0.028(4) -0.003(3) 0.000(3) 0.003(3) O4 0.016(3) 0.023(4) 0.022(3) -0.005(3) 0.002(3) -0.004(2) Pb1 0.01954(16) 0.0226(2) 0.02883(19) -0.00915(18) -0.00242(16) -0.00127(15) Pb2 0.02791(18) 0.0266(3) 0.0281(2) -0.00944(19) -0.00613(17) 0.01121(16) Pb3 0.02130(16) 0.0253(2) 0.02204(17) 0.00107(18) 0.00020(15) -0.00757(15) Pb4 0.02533(16) 0.0203(2) 0.01899(16) 0.00335(17) -0.00256(15) 0.00146(15) _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 C8 N1 1.341(13) . ? C8 N4 1.355(12) . ? C8 C3 1.412(14) . ? C4 C5 1.385(15) . ? C4 C3 1.426(14) . ? C3 C2 1.412(14) . ? C2 C1 1.377(15) . ? C16 N16 1.327(12) . ? C16 N13 1.329(13) . ? C16 C12 1.465(14) . ? C12 C13 1.357(16) . ? C12 C11 1.418(12) . ? C11 C10 1.365(15) . ? C13 C14 1.410(15) . ? C14 C9 1.373(13) . ? C9 C10 1.390(15) . ? C9 C15 1.468(14) . ? C5 C6 1.395(14) . ? C6 C1 1.424(13) . ? C6 C7 1.451(14) . ? C15 N12 1.333(13) . ? C15 N9 1.387(13) . ? C7 N8 1.349(13) . ? C7 N5 1.353(13) . ? N1 N2 1.352(12) . ? N1 Pb4 2.688(8) 4_554 ? N2 N3 1.343(12) . ? N3 N4 1.335(13) . ? N3 Pb1 2.697(9) . ? N4 Pb2 2.727(8) . ? N5 N6 1.358(13) . ? N6 N7 1.257(13) . ? N7 N8 1.329(13) . ? N9 N10 1.356(12) . ? N10 N11 1.291(12) . ? N11 N12 1.333(12) . ? N11 Pb3 2.721(9) . ? N12 Pb1 2.729(9) . ? N13 N14 1.343(13) . ? N14 N15 1.294(13) . ? N15 N16 1.353(14) . ? O1 Pb4 2.352(7) . ? O1 Pb2 2.384(7) . ? O1 Pb1 2.431(7) . ? O2 Pb4 2.322(8) . ? O2 Pb3 2.417(7) . ? O2 Pb2 2.504(6) . ? O3 Pb3 2.330(7) . ? O3 Pb4 2.418(7) . ? O3 Pb1 2.449(6) . ? O4 Pb2 2.338(7) . ? O4 Pb3 2.353(6) . ? O4 Pb1 2.513(7) . ? Pb4 N1 2.688(8) 4 ? 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 N1 C8 N4 109.3(9) . . ? N1 C8 C3 124.6(9) . . ? N4 C8 C3 126.1(9) . . ? C5 C4 C3 121.6(10) . . ? C8 C3 C2 122.7(9) . . ? C8 C3 C4 120.8(10) . . ? C2 C3 C4 116.4(9) . . ? C1 C2 C3 122.6(9) . . ? N16 C16 N13 109.4(9) . . ? N16 C16 C12 126.1(10) . . ? N13 C16 C12 124.4(9) . . ? C13 C12 C11 118.5(10) . . ? C13 C12 C16 121.3(9) . . ? C11 C12 C16 120.1(9) . . ? C10 C11 C12 120.0(10) . . ? C12 C13 C14 120.8(10) . . ? C9 C14 C13 120.7(10) . . ? C14 C9 C10 118.2(9) . . ? C14 C9 C15 121.0(9) . . ? C10 C9 C15 120.8(9) . . ? C11 C10 C9 121.7(9) . . ? C4 C5 C6 120.7(10) . . ? C5 C6 C1 119.0(10) . . ? C5 C6 C7 121.2(9) . . ? C1 C6 C7 119.8(9) . . ? C2 C1 C6 119.7(9) . . ? N12 C15 N9 109.7(9) . . ? N12 C15 C9 127.0(9) . . ? N9 C15 C9 123.3(9) . . ? N8 C7 N5 110.5(9) . . ? N8 C7 C6 125.7(9) . . ? N5 C7 C6 123.7(9) . . ? C8 N1 N2 106.4(8) . . ? C8 N1 Pb4 136.9(6) . 4_554 ? N2 N1 Pb4 113.0(6) . 4_554 ? N3 N2 N1 108.7(8) . . ? N4 N3 N2 108.4(7) . . ? N4 N3 Pb1 112.0(6) . . ? N2 N3 Pb1 134.1(8) . . ? N3 N4 C8 107.0(8) . . ? N3 N4 Pb2 113.0(6) . . ? C8 N4 Pb2 134.8(7) . . ? C7 N5 N6 102.8(8) . . ? N7 N6 N5 111.4(8) . . ? N6 N7 N8 110.6(10) . . ? N7 N8 C7 104.7(9) . . ? N10 N9 C15 104.4(8) . . ? N11 N10 N9 108.8(7) . . ? N10 N11 N12 111.8(8) . . ? N10 N11 Pb3 127.4(7) . . ? N12 N11 Pb3 118.1(6) . . ? C15 N12 N11 105.4(8) . . ? C15 N12 Pb1 141.1(8) . . ? N11 N12 Pb1 111.9(6) . . ? C16 N13 N14 106.6(9) . . ? N15 N14 N13 108.9(9) . . ? N14 N15 N16 108.9(8) . . ? C16 N16 N15 106.1(9) . . ? Pb4 O1 Pb2 107.0(3) . . ? Pb4 O1 Pb1 106.0(3) . . ? Pb2 O1 Pb1 107.4(3) . . ? Pb4 O2 Pb3 106.1(3) . . ? Pb4 O2 Pb2 104.0(3) . . ? Pb3 O2 Pb2 103.1(3) . . ? Pb3 O3 Pb4 105.9(3) . . ? Pb3 O3 Pb1 107.0(3) . . ? Pb4 O3 Pb1 103.4(2) . . ? Pb2 O4 Pb3 110.5(3) . . ? Pb2 O4 Pb1 106.1(3) . . ? Pb3 O4 Pb1 104.3(3) . . ? O1 Pb1 O3 71.0(2) . . ? O1 Pb1 O4 67.9(2) . . ? O3 Pb1 O4 68.7(2) . . ? O1 Pb1 N3 82.0(3) . . ? O3 Pb1 N3 135.1(3) . . ? O4 Pb1 N3 68.0(3) . . ? O1 Pb1 N12 137.0(3) . . ? O3 Pb1 N12 81.3(2) . . ? O4 Pb1 N12 71.7(3) . . ? N3 Pb1 N12 96.2(3) . . ? O4 Pb2 O1 71.6(2) . . ? O4 Pb2 O2 70.2(2) . . ? O1 Pb2 O2 70.0(2) . . ? O4 Pb2 N4 76.9(2) . . ? O1 Pb2 N4 74.0(3) . . ? O2 Pb2 N4 137.0(3) . . ? O3 Pb3 O4 73.5(2) . . ? O3 Pb3 O2 72.2(3) . . ? O4 Pb3 O2 71.5(2) . . ? O3 Pb3 N11 75.7(3) . . ? O4 Pb3 N11 77.1(2) . . ? O2 Pb3 N11 140.0(3) . . ? O2 Pb4 O1 73.8(2) . . ? O2 Pb4 O3 72.3(3) . . ? O1 Pb4 O3 72.9(2) . . ? O2 Pb4 N1 87.5(3) . 4 ? O1 Pb4 N1 70.9(2) . 4 ? O3 Pb4 N1 142.3(2) . 4 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.248 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.218 #================================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 849345' #TrackingRef 'CCDC-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 N8 O3 Pb2' _chemical_formula_sum 'C8 H6 N8 O3 Pb2' _chemical_formula_weight 676.61 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 tetragonal _symmetry_space_group_name_H-M 'P 42/m b c' _symmetry_space_group_name_Hall '-P 4c 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'x-1/2, -y-1/2, z' 'y-1/2, x-1/2, z-1/2' _cell_length_a 13.4523(10) _cell_length_b 13.4523(10) _cell_length_c 14.5250(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2628.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2367 _exptl_absorpt_coefficient_mu 25.611 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'Bruker AXS SMART APEX CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17320 _diffrn_reflns_av_R_equivalents 0.1895 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.49 _reflns_number_total 1717 _reflns_number_gt 1074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997-2002)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2003)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+59.0226P] 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 1717 _refine_ls_number_parameters 96 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Pb1 Pb 0.14516(3) -0.01121(3) 0.65958(5) 0.0243(2) Uani 1 1 d . . . O1 O 0.1021(7) -0.0164(6) 0.8198(8) 0.025(3) Uani 1 1 d . . . O2 O 0.1473(10) 0.1082(10) 0.5000 0.039(5) Uani 1 2 d S . . H10A H 0.0896 0.1515 0.5000 0.047 Uiso 1 2 calc SR . . H10B H 0.2064 0.1495 0.5000 0.047 Uiso 1 2 calc SR . . N1 N 0.2512(9) 0.1337(9) 0.7363(12) 0.040(4) Uani 1 1 d . . . N2 N 0.2087(9) 0.2247(9) 0.7421(13) 0.047(5) Uani 1 1 d . . . N3 N 0.1834(12) -0.2866(11) 0.5000 0.033(5) Uani 1 2 d S . . N4 N 0.1909(12) -0.1880(11) 0.5000 0.031(5) Uani 1 2 d S . . N5 N 0.1034(12) -0.1465(12) 0.5000 0.030(3) Uani 1 2 d S . . N6 N 0.0325(12) -0.2203(13) 0.5000 0.030(3) Uani 1 2 d S . . C1 C 0.3488(11) 0.1512(11) 0.7500 0.029(5) Uani 1 2 d SU . . C2 C 0.4256(11) 0.0744(11) 0.7500 0.046(5) Uani 1 2 d S . . C3 C 0.4026(11) -0.0252(10) 0.7511(17) 0.046(5) Uani 1 1 d . . . H3 H 0.3362 -0.0443 0.7535 0.055 Uiso 1 1 calc R . . C4 C 0.0857(15) -0.3055(13) 0.5000 0.031(6) Uani 1 2 d S . . C5 C 0.0422(14) -0.4046(14) 0.5000 0.025(3) Uani 1 2 d SU . . C6 C 0.1006(17) -0.4881(15) 0.5000 0.045(8) Uani 1 2 d S . . H6 H 0.1694 -0.4809 0.5000 0.053 Uiso 1 2 calc SR . . C7 C -0.0607(14) -0.4177(13) 0.5000 0.025(3) Uani 1 2 d S . . H7 H -0.1024 -0.3625 0.5000 0.030 Uiso 1 2 calc SR . . 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 0.0105(2) 0.0155(3) 0.0469(4) -0.0019(3) 0.0022(3) 0.00108(16) O1 0.012(4) 0.009(4) 0.055(9) 0.002(4) -0.004(5) 0.000(3) O2 0.023(7) 0.013(6) 0.082(15) 0.000 0.000 0.004(6) N1 0.020(6) 0.024(6) 0.074(12) -0.002(7) -0.013(7) -0.004(5) N2 0.025(6) 0.020(6) 0.095(14) -0.010(8) -0.006(8) -0.001(5) N3 0.020(8) 0.007(7) 0.071(16) 0.000 0.000 -0.003(6) N4 0.017(8) 0.009(7) 0.067(16) 0.000 0.000 0.004(6) N5 0.015(5) 0.018(6) 0.058(10) 0.000 0.000 -0.011(5) N6 0.015(5) 0.018(6) 0.058(10) 0.000 0.000 -0.011(5) C1 0.022(5) 0.022(5) 0.044(10) -0.004(5) -0.004(5) -0.012(6) C2 0.017(4) 0.017(4) 0.104(14) 0.002(5) 0.002(5) -0.010(5) C3 0.017(4) 0.017(4) 0.104(14) 0.002(5) 0.002(5) -0.010(5) C4 0.024(10) 0.006(8) 0.06(2) 0.000 0.000 -0.003(7) C5 0.018(6) 0.009(5) 0.048(8) 0.000 0.000 -0.003(4) C6 0.015(10) 0.020(10) 0.10(3) 0.000 0.000 0.006(8) C7 0.018(6) 0.009(5) 0.048(8) 0.000 0.000 -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 O1 2.327(9) 12_557 ? Pb1 O1 2.398(12) . ? Pb1 O1 2.512(9) 10_557 ? Pb1 N1 2.660(13) . ? Pb1 O2 2.820(8) . ? Pb1 Pb1 3.8172(11) 10_557 ? Pb1 Pb1 3.8172(11) 12_557 ? Pb1 Pb1 3.9170(9) 3 ? O1 Pb1 2.327(9) 10_557 ? O1 Pb1 2.512(8) 12_557 ? O2 Pb1 2.820(8) 11_556 ? O2 H10A 0.9700 . ? O2 H10B 0.9700 . ? N1 C1 1.348(16) . ? N1 N2 1.354(16) . ? N2 N2 1.29(3) 8_556 ? N3 N4 1.33(2) . ? N3 C4 1.34(3) . ? N4 N5 1.30(2) . ? N5 N6 1.38(2) . ? N5 Pb1 3.000(10) 11_556 ? N6 C4 1.35(2) . ? C1 N1 1.348(16) 8_556 ? C1 C2 1.46(3) . ? C2 C3 1.376(17) 8_556 ? C2 C3 1.376(17) . ? C3 C3 1.37(3) 6_546 ? C3 H3 0.9300 . ? C4 C5 1.46(2) . ? C5 C6 1.37(3) . ? C5 C7 1.40(3) . ? C6 C7 1.38(3) 9_546 ? C6 H6 0.9300 . ? C7 C6 1.38(3) 9_546 ? C7 H7 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 Pb1 O1 73.4(4) 12_557 . ? O1 Pb1 O1 70.1(4) 12_557 10_557 ? O1 Pb1 O1 70.2(4) . 10_557 ? O1 Pb1 N1 82.3(4) 12_557 . ? O1 Pb1 N1 75.2(4) . . ? O1 Pb1 N1 140.4(4) 10_557 . ? O1 Pb1 O2 75.0(4) 12_557 . ? O1 Pb1 O2 144.7(3) . . ? O1 Pb1 O2 112.6(4) 10_557 . ? N1 Pb1 O2 85.5(4) . . ? O1 Pb1 Pb1 79.1(3) 12_557 10_557 ? O1 Pb1 Pb1 35.5(2) . 10_557 ? O1 Pb1 Pb1 37.9(3) 10_557 10_557 ? N1 Pb1 Pb1 110.7(4) . 10_557 ? O2 Pb1 Pb1 147.1(3) . 10_557 ? O1 Pb1 Pb1 36.8(3) 12_557 12_557 ? O1 Pb1 Pb1 40.1(2) . 12_557 ? O1 Pb1 Pb1 77.2(2) 10_557 12_557 ? N1 Pb1 Pb1 64.0(3) . 12_557 ? O2 Pb1 Pb1 104.9(2) . 12_557 ? Pb1 Pb1 Pb1 61.738(19) 10_557 12_557 ? O1 Pb1 Pb1 37.6(2) 12_557 3 ? O1 Pb1 Pb1 76.2(2) . 3 ? O1 Pb1 Pb1 34.4(2) 10_557 3 ? N1 Pb1 Pb1 118.6(3) . 3 ? O2 Pb1 Pb1 88.1(3) . 3 ? Pb1 Pb1 Pb1 59.131(10) 10_557 3 ? Pb1 Pb1 Pb1 59.131(10) 12_557 3 ? Pb1 O1 Pb1 107.8(4) 10_557 . ? Pb1 O1 Pb1 108.0(4) 10_557 12_557 ? Pb1 O1 Pb1 102.0(4) . 12_557 ? Pb1 O2 Pb1 110.6(4) 11_556 . ? Pb1 O2 H10A 109.5 11_556 . ? Pb1 O2 H10A 109.5 . . ? Pb1 O2 H10B 109.5 11_556 . ? Pb1 O2 H10B 109.5 . . ? H10A O2 H10B 108.1 . . ? C1 N1 N2 104.1(12) . . ? C1 N1 Pb1 135.4(11) . . ? N2 N1 Pb1 117.5(9) . . ? N2 N2 N1 110.2(7) 8_556 . ? N4 N3 C4 105.3(15) . . ? N5 N4 N3 111.0(15) . . ? N4 N5 N6 108.5(15) . . ? N4 N5 Pb1 95.2(7) . 11_556 ? N6 N5 Pb1 124.5(5) . 11_556 ? C4 N6 N5 104.2(15) . . ? N1 C1 N1 111.3(19) . 8_556 ? N1 C1 C2 124.4(9) . . ? N1 C1 C2 124.4(9) 8_556 . ? C3 C2 C3 116(2) 8_556 . ? C3 C2 C1 122.0(10) 8_556 . ? C3 C2 C1 122.0(10) . . ? C3 C3 C2 122.0(10) 6_546 . ? C3 C3 H3 119.0 6_546 . ? C2 C3 H3 119.0 . . ? N3 C4 N6 111.0(15) . . ? N3 C4 C5 124.6(17) . . ? N6 C4 C5 124.4(18) . . ? C6 C5 C7 117.8(17) . . ? C6 C5 C4 121.3(18) . . ? C7 C5 C4 120.9(17) . . ? C5 C6 C7 122(2) . 9_546 ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 9_546 . ? C6 C7 C5 120.2(18) 9_546 . ? C6 C7 H7 119.9 9_546 . ? C5 C7 H7 119.9 . . ? 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 O2 H10B N4 0.97 2.59 3.50(2) 157.2 13_665 O2 H10B N3 0.97 1.71 2.68(2) 175.2 13_665 O2 H10A N5 0.97 2.60 3.41(2) 141.6 9_556 O2 H10A N6 0.97 1.89 2.85(2) 172.4 9_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.549 _refine_diff_density_min -2.598 _refine_diff_density_rms 0.398