############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_global _audit_creation_method 'PLATON option' _journal_date_recd_electronic 2010-12-16 _journal_date_accepted 2011-01-05 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2011 _journal_volume 67 _journal_issue 2 _journal_page_first m163 _journal_page_last m164 _journal_paper_category QM _journal_coeditor_code XU5124 _publ_contact_author_name ; Shen, Fwu Ming ; _publ_contact_author_address ; Department of Biotechnology Yuanpei University No.306, Yuanpei St., HsinChu 30015 Taiwan ; _publ_contact_author_email fmshen@mail.ypu.edu.tw _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; Poly[(\m~4~-pyridine-2,3-dicarboxylato)lead(II)] ; loop_ _publ_author_name _publ_author_address 'Lush, Shie Fu' ; Department of General Education Center Yuanpei University HsinChu 30015 Taiwan ; 'Shen, Fwu Ming' ; Department of Biotechnology Yuanpei University HsinChu 30015 Taiwan ; data_I _chemical_name_systematic ; Poly[(\m~4~-pyridine-2,3-dicarboxylato)lead(II)] ; _chemical_name_common ? _chemical_formula_moiety 'C7 H3 N O4 Pb' _chemical_formula_sum 'C7 H3 N O4 Pb' _chemical_formula_structural ? _chemical_formula_iupac '[Pb (C7 H3 N O4)]' _chemical_formula_weight 372.30 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 11.6943(9) _cell_length_b 4.5392(4) _cell_length_c 14.1636(12) _cell_angle_alpha 90 _cell_angle_beta 90.046(2) _cell_angle_gamma 90 _cell_volume 751.84(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2856 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.00 _cell_measurement_temperature 297 _cell_special_details ; ; _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 3.289 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 22.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; Elemental analysis: calculated for C~7~H~3~NO~4~Pb: (Mr=372.29) C, 22.56; H, 0.81; N, 3.76%. Found:C,22.47; H, 0.89; N, 3.85%. IR data (cm^-1^): 3429(s), 1602(s), 1579(s), 1551(s), 1459(w), 1385(s), 1276(w), 1236(w), 1105(m), 871(m), 825(m), 779(m), 711(s), 700(m), 660(m), 603(w), 534(w), 443(w). ; _diffrn_ambient_temperature 297 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 4013 _diffrn_reflns_av_R_equivalents 0.1249 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > \s(F^2^) is used only for calculating -R-factor-obs 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. ; _reflns_number_total 1484 _reflns_number_gt 1336 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_gt 0.1982 _refine_ls_wR_factor_ref 0.2035 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_number_reflns 1484 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1477P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 4.555 _refine_diff_density_min -5.059 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb Pb -3.3944 10.1111 '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' N N 0.0061 0.0033 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'PLATON (Spek, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Pb Pb 0.60762(4) 0.01636(10) 0.85892(3) 0.0213(3) Uani . . 1.000 O O1 0.6007(6) 0.3400(19) 0.5591(4) 0.035(2) Uani . . 1.000 O O2 0.5381(7) 0.120(2) 0.6883(5) 0.037(3) Uani . . 1.000 O O3 0.6905(9) -0.061(2) 0.4106(6) 0.032(3) Uani . . 1.000 O O4 0.8222(6) 0.2863(17) 0.4294(4) 0.038(2) Uani . . 1.000 N N 0.7437(6) -0.1315(19) 0.7170(5) 0.024(2) Uani . . 1.000 C C1 0.7208(12) -0.0178(18) 0.6321(9) 0.021(4) Uani . . 1.000 C C2 0.7951(11) -0.058(3) 0.5526(9) 0.021(3) Uani . . 1.000 C C3 0.8932(8) -0.216(2) 0.5715(6) 0.027(3) Uani . . 1.000 C C4 0.9192(9) -0.325(3) 0.6603(7) 0.038(4) Uani . . 1.000 C C5 0.8383(9) -0.288(3) 0.7300(6) 0.036(3) Uani . . 1.000 C C6 0.6141(8) 0.163(3) 0.6231(6) 0.023(3) Uani . . 1.000 C C7 0.7687(9) 0.068(2) 0.4580(7) 0.019(3) Uani . . 1.000 H H3A 0.94410 -0.25180 0.52240 0.0320 Uiso calc R 1.000 H H4A 0.98820 -0.41980 0.67230 0.0450 Uiso calc R 1.000 H H5A 0.85060 -0.37490 0.78850 0.0430 Uiso calc R 1.000 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pb 0.0207(5) 0.0242(5) 0.0189(5) -0.00310(10) -0.0051(3) -0.00160(10) O1 0.035(4) 0.045(5) 0.026(3) 0.015(4) 0.007(3) 0.012(3) O2 0.027(4) 0.061(6) 0.024(3) 0.017(5) 0.001(3) 0.013(4) O3 0.039(5) 0.031(4) 0.027(4) 0.006(4) -0.022(4) -0.013(4) O4 0.044(4) 0.041(5) 0.030(3) -0.007(4) -0.010(3) 0.009(3) N 0.018(4) 0.032(5) 0.021(3) 0.004(3) -0.003(3) 0.004(3) C1 0.018(7) 0.028(6) 0.017(6) -0.002(3) 0.000(5) -0.001(3) C2 0.006(5) 0.037(5) 0.021(5) 0.002(4) -0.004(4) -0.010(5) C3 0.023(5) 0.032(6) 0.026(4) 0.006(4) 0.003(4) 0.003(4) C4 0.029(6) 0.054(8) 0.031(5) 0.018(6) -0.013(4) 0.010(5) C5 0.041(6) 0.046(7) 0.021(4) 0.009(5) -0.009(4) 0.011(4) C6 0.018(5) 0.031(5) 0.021(4) 0.006(4) -0.005(3) 0.002(4) C7 0.008(5) 0.030(5) 0.019(4) 0.006(4) -0.007(4) 0.004(4) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb N . . 2.651(7) yes Pb O1 . 2_646 2.816(7) yes Pb O1 . 4_555 2.911(6) yes Pb O2 . . 2.592(7) yes Pb O2 . 2_646 2.566(9) yes Pb O3 . 4_545 2.397(9) yes Pb O3 . 4_555 2.754(9) yes Pb O4 . 4_555 2.845(7) yes O1 C6 . . 1.221(13) no O2 C6 . . 1.297(12) no O3 C7 . . 1.276(14) no O4 C7 . . 1.240(12) no N C1 . . 1.336(14) no N C5 . . 1.327(14) no C1 C2 . . 1.435(18) no C1 C6 . . 1.499(17) no C2 C3 . . 1.379(16) no C2 C7 . . 1.489(16) no C3 C4 . . 1.385(14) no C4 C5 . . 1.378(14) no C3 H3A . . 0.9300 no C4 H4A . . 0.9300 no C5 H5A . . 0.9300 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 Pb N . . . 61.8(2) no O1 Pb O2 2_646 . . 99.5(2) no O2 Pb O2 . . 2_646 71.1(3) no O2 Pb O3 . . 4_545 124.6(3) no O1 Pb O2 4_555 . . 149.2(2) no O2 Pb O3 . . 4_555 101.2(3) no O2 Pb O4 . . 4_555 123.1(2) no O2 Pb C7 . . 4_555 121.1(3) no O1 Pb N 2_646 . . 139.5(2) no O2 Pb N 2_646 . . 91.4(2) no O3 Pb N 4_545 . . 76.7(3) no O1 Pb N 4_555 . . 144.3(2) no O3 Pb N 4_555 . . 102.6(3) no O4 Pb N 4_555 . . 79.4(2) no N Pb C7 . . 4_555 97.8(3) no O1 Pb O2 2_646 . 2_646 48.2(2) no O1 Pb O3 2_646 . 4_545 88.8(3) no O1 Pb O1 2_646 . 4_555 68.73(19) no O1 Pb O3 2_646 . 4_555 116.7(3) no O1 Pb O4 2_646 . 4_555 135.08(17) no O1 Pb C7 2_646 . 4_555 121.8(2) no O2 Pb O3 2_646 . 4_545 75.1(3) no O1 Pb O2 4_555 . 2_646 113.1(2) no O2 Pb O3 2_646 . 4_555 158.7(3) no O2 Pb O4 2_646 . 4_555 153.8(2) no O2 Pb C7 2_646 . 4_555 167.3(2) no O1 Pb O3 4_555 . 4_545 84.7(3) no O3 Pb O3 4_545 . 4_555 123.4(3) no O3 Pb O4 4_545 . 4_555 78.9(3) no O3 Pb C7 4_545 . 4_555 98.4(3) no O1 Pb O3 4_555 . 4_555 63.3(2) no O1 Pb O4 4_555 . 4_555 67.22(18) no O1 Pb C7 4_555 . 4_555 54.8(2) no O3 Pb O4 4_555 . 4_555 46.7(3) no O3 Pb C7 4_555 . 4_555 25.1(3) no O4 Pb C7 4_555 . 4_555 24.2(2) no Pb O1 C6 2_656 . . 89.5(6) no Pb O1 C6 4_554 . . 150.1(7) no Pb O1 Pb 2_656 . 4_554 111.3(2) no Pb O2 C6 . . . 118.5(6) no Pb O2 Pb . . 2_656 125.3(3) no Pb O2 C6 2_656 . . 99.5(7) no Pb O3 C7 4_544 . . 147.7(8) no Pb O3 C7 4_554 . . 88.8(6) no Pb O3 Pb 4_544 . 4_554 123.4(4) no Pb O4 C7 4_554 . . 85.5(6) no Pb N C1 . . . 117.7(7) no Pb N C5 . . . 122.1(6) no C1 N C5 . . . 119.9(9) no N C1 C2 . . . 122.4(11) no N C1 C6 . . . 117.0(10) no C2 C1 C6 . . . 120.5(10) no C1 C2 C3 . . . 114.7(11) no C1 C2 C7 . . . 122.2(11) no C3 C2 C7 . . . 123.1(10) no C2 C3 C4 . . . 123.0(10) no C3 C4 C5 . . . 117.2(10) no N C5 C4 . . . 122.6(9) no O1 C6 O2 . . . 122.7(10) no O1 C6 C1 . . . 122.0(9) no O2 C6 C1 . . . 115.3(10) no O3 C7 O4 . . . 123.8(9) no O3 C7 C2 . . . 116.4(9) no Pb C7 O3 4_554 . . 66.1(6) no O4 C7 C2 . . . 119.8(9) no Pb C7 O4 4_554 . . 70.3(5) no Pb C7 C2 4_554 . . 142.1(7) no C2 C3 H3A . . . 119.00 no C4 C3 H3A . . . 118.00 no C3 C4 H4A . . . 121.00 no C5 C4 H4A . . . 121.00 no N C5 H5A . . . 119.00 no C4 C5 H5A . . . 119.00 no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N Pb O2 C6 . . . . -27.3(8) no N Pb O2 Pb . . . 2_656 -155.1(5) no O1 Pb O2 C6 2_646 . . . -169.0(9) no O1 Pb O2 Pb 2_646 . . 2_656 63.2(4) no O2 Pb O2 C6 2_646 . . . -129.5(9) no O2 Pb O2 Pb 2_646 . . 2_656 102.7(4) no O3 Pb O2 C6 4_545 . . . -73.9(10) no O3 Pb O2 Pb 4_545 . . 2_656 158.3(4) no O1 Pb O2 C6 4_555 . . . 126.9(9) no O1 Pb O2 Pb 4_555 . . 2_656 -0.9(7) no O3 Pb O2 C6 4_555 . . . 71.1(9) no O3 Pb O2 Pb 4_555 . . 2_656 -56.7(4) no O4 Pb O2 C6 4_555 . . . 25.9(10) no O4 Pb O2 Pb 4_555 . . 2_656 -101.9(4) no C7 Pb O2 C6 4_555 . . . 54.5(10) no C7 Pb O2 Pb 4_555 . . 2_656 -73.3(5) no O2 Pb N C1 . . . . 15.4(7) no O2 Pb N C5 . . . . -171.4(9) no O1 Pb N C1 2_646 . . . 85.5(8) no O1 Pb N C5 2_646 . . . -101.3(8) no O2 Pb N C1 2_646 . . . 83.0(7) no O2 Pb N C5 2_646 . . . -103.8(9) no O3 Pb N C1 4_545 . . . 157.4(8) no O3 Pb N C5 4_545 . . . -29.4(9) no O1 Pb N C1 4_555 . . . -142.1(7) no O1 Pb N C5 4_555 . . . 31.1(10) no O3 Pb N C1 4_555 . . . -80.8(7) no O3 Pb N C5 4_555 . . . 92.4(9) no O4 Pb N C1 4_555 . . . -121.6(7) no O4 Pb N C5 4_555 . . . 51.6(8) no C7 Pb N C1 4_555 . . . -105.8(7) no C7 Pb N C5 4_555 . . . 67.4(9) no O2 Pb O1 C6 . . 2_646 2_646 51.7(7) no O2 Pb O1 Pb . . 2_646 3_657 -150.3(3) no N Pb O1 C6 . . 2_646 2_646 -5.4(8) no N Pb O1 Pb . . 2_646 3_657 152.5(3) no O2 Pb O2 Pb . . 2_646 2_646 14.6(4) no O2 Pb O2 C6 . . 2_646 2_646 -120.6(7) no N Pb O2 Pb . . 2_646 2_646 -44.8(4) no N Pb O2 C6 . . 2_646 2_646 179.9(7) no O2 Pb O3 C7 . . 4_545 4_545 136.3(13) no N Pb O3 C7 . . 4_545 4_545 95.1(14) no O2 Pb O1 Pb . . 4_555 3_657 72.2(6) no O2 Pb O1 C6 . . 4_555 4_555 -59.0(14) no N Pb O1 Pb . . 4_555 3_657 -149.1(3) no N Pb O1 C6 . . 4_555 4_555 79.8(14) no O2 Pb O3 C7 . . 4_555 4_555 -144.8(6) no N Pb O3 C7 . . 4_555 4_555 -81.6(6) no O2 Pb O4 C7 . . 4_555 4_555 93.1(6) no N Pb O4 C7 . . 4_555 4_555 138.9(6) no O2 Pb C7 O3 . . 4_555 4_555 41.3(7) no O2 Pb C7 O4 . . 4_555 4_555 -102.4(5) no O2 Pb C7 C2 . . 4_555 4_555 144.2(11) no N Pb C7 O3 . . 4_555 4_555 102.9(6) no N Pb C7 O4 . . 4_555 4_555 -40.7(6) no N Pb C7 C2 . . 4_555 4_555 -154.2(12) no Pb O1 C6 O2 4_554 . . . -131.7(11) no Pb O1 C6 C1 2_656 . . . -175.5(10) no Pb O1 C6 O2 2_656 . . . 3.8(11) no Pb O1 C6 C1 4_554 . . . 49.0(19) no Pb O2 C6 C1 2_656 . . . 175.1(8) no Pb O2 C6 C1 . . . . 36.0(13) no Pb O2 C6 O1 . . . . -143.4(9) no Pb O2 C6 O1 2_656 . . . -4.2(12) no Pb O3 C7 O4 4_544 . . . 136.7(11) no Pb O3 C7 O4 4_554 . . . -42.2(10) no Pb O3 C7 C2 4_544 . . . -43.1(19) no Pb O3 C7 C2 4_554 . . . 138.0(9) no Pb O3 C7 Pb 4_544 . . 4_554 178.9(15) no Pb O4 C7 O3 4_554 . . . 40.7(10) no Pb O4 C7 C2 4_554 . . . -139.5(9) no C5 N C1 C2 . . . . 0.1(16) no Pb N C1 C2 . . . . 173.5(8) no Pb N C1 C6 . . . . -5.1(12) no C1 N C5 C4 . . . . 4.1(17) no C5 N C1 C6 . . . . -178.5(10) no Pb N C5 C4 . . . . -169.0(9) no C6 C1 C2 C3 . . . . 176.8(10) no N C1 C2 C3 . . . . -1.7(16) no N C1 C2 C7 . . . . 179.7(10) no C6 C1 C2 C7 . . . . -1.9(17) no N C1 C6 O1 . . . . 159.4(10) no N C1 C6 O2 . . . . -20.0(15) no C2 C1 C6 O1 . . . . -19.2(17) no C2 C1 C6 O2 . . . . 161.5(10) no C1 C2 C3 C4 . . . . -0.7(17) no C7 C2 C3 C4 . . . . 177.9(11) no C1 C2 C7 O3 . . . . -74.7(15) no C1 C2 C7 O4 . . . . 105.5(13) no C1 C2 C7 Pb . . . 4_554 10(2) no C3 C2 C7 O3 . . . . 106.7(13) no C3 C2 C7 O4 . . . . -73.0(15) no C3 C2 C7 Pb . . . 4_554 -168.9(8) no C2 C3 C4 C5 . . . . 4.5(18) no C3 C4 C5 N . . . . -6.3(18) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C5 H5A O3 4_545 0.93 2.57 3.164(13) 122 yes