#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/37/2013747.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013747 loop_ _publ_author_name 'Dale, Sophie H.' 'Elsegood, Mark R. J.' 'Kainth, Sarita' _publ_section_title ; Poly[lead(II)-\m~2~-aqua-\m~4~-terephthalato] ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m76 _journal_page_last m78 _journal_paper_doi 10.1107/S0108270103029573 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Pb (C8 H4 O4) (H2 O)]' _chemical_formula_moiety 'C8 H6 O5 Pb' _chemical_formula_sum 'C8 H6 O5 Pb' _chemical_formula_weight 389.32 _chemical_name_systematic ; Poly[lead(II)-\m~2~-aqua-\m~3~-terephthalato] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens 'Geom except OH coords refined with restraints' _atom_sites_solution_primary direct _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 109.404(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.6661(7) _cell_length_b 7.5042(5) _cell_length_c 11.1260(8) _cell_measurement_reflns_used 3310 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.89 _cell_measurement_theta_min 3.34 _cell_volume 839.95(10) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4408 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.02 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 20.077 _exptl_absorpt_correction_T_max 0.300 _exptl_absorpt_correction_T_min 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2001)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 3.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Column _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.629 _refine_diff_density_min -2.110 _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 134 _refine_ls_number_reflns 1637 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0228 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.2788P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0570 _reflns_number_gt 1496 _reflns_number_total 1637 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bm1557.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2013747 _cod_database_fobs_code 2013747 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pb1 1.031682(18) 0.02918(3) 0.699144(18) 0.01008(11) Uani d D 1 . . Pb C1 0.6240(5) 0.1435(7) 0.7082(5) 0.0099(11) Uani d . 1 . . C C2 0.5292(5) 0.0668(7) 0.7534(5) 0.0104(11) Uani d . 1 . . C H2 0.5554 0.0156 0.8361 0.012 Uiso calc R 1 . . H C3 0.3961(5) 0.0655(8) 0.6770(6) 0.0146(12) Uani d . 1 . . C H3 0.3316 0.0138 0.7081 0.018 Uiso calc R 1 . . H C4 0.3570(5) 0.1393(7) 0.5557(5) 0.0099(11) Uani d . 1 . . C C5 0.4509(5) 0.2214(7) 0.5129(5) 0.0118(11) Uani d . 1 . . C H5 0.4237 0.2777 0.4318 0.014 Uiso calc R 1 . . H C6 0.5846(5) 0.2218(7) 0.5879(5) 0.0119(11) Uani d . 1 . . C H6 0.6487 0.2754 0.5571 0.014 Uiso calc R 1 . . H C7 0.7671(5) 0.1342(7) 0.7905(5) 0.0110(11) Uani d . 1 . . C O1 0.8542(3) 0.1999(5) 0.7482(3) 0.0122(8) Uani d . 1 . . O O2 0.7939(4) 0.0603(5) 0.8988(4) 0.0168(9) Uani d . 1 . . O C8 0.2154(5) 0.1169(7) 0.4704(5) 0.0140(12) Uani d . 1 . . C O3 0.1400(4) 0.0149(5) 0.5068(4) 0.0157(9) Uani d . 1 . . O O4 0.1760(3) 0.1879(5) 0.3620(3) 0.0154(8) Uani d . 1 . . O O5 1.0015(3) 0.3415(5) 0.6003(3) 0.0131(8) Uani d D 1 . . O H5A 0.936(3) 0.354(3) 0.5219(15) 0.020 Uiso d D 1 . . H H5B 1.063(3) 0.381(3) 0.568(3) 0.020 Uiso d D 1 . . H 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 Pb1 0.00812(14) 0.01156(16) 0.00969(16) -0.00022(7) 0.00181(9) -0.00037(7) C1 0.011(2) 0.008(3) 0.009(3) -0.001(2) 0.001(2) -0.002(2) C2 0.010(3) 0.016(3) 0.005(3) -0.002(2) 0.002(2) -0.001(2) C3 0.010(3) 0.018(3) 0.019(3) 0.001(2) 0.009(2) 0.003(2) C4 0.010(2) 0.007(3) 0.012(3) 0.002(2) 0.002(2) 0.000(2) C5 0.014(3) 0.013(3) 0.007(3) 0.005(2) 0.002(2) -0.001(2) C6 0.012(2) 0.010(3) 0.014(3) 0.001(2) 0.006(2) 0.001(2) C7 0.007(2) 0.010(3) 0.016(3) 0.001(2) 0.004(2) -0.006(2) O1 0.0081(17) 0.013(2) 0.016(2) 0.0005(15) 0.0042(15) 0.0014(16) O2 0.0120(19) 0.022(2) 0.015(2) 0.0007(16) 0.0024(16) 0.0019(17) C8 0.015(3) 0.013(3) 0.012(3) 0.001(2) 0.002(2) -0.004(2) O3 0.010(2) 0.026(2) 0.013(2) -0.0062(16) 0.0074(17) -0.0033(16) O4 0.0125(18) 0.018(2) 0.012(2) -0.0003(15) -0.0002(15) -0.0006(16) O5 0.0110(18) 0.017(2) 0.0106(19) -0.0012(15) 0.0030(15) 0.0013(16) 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' 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' 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_3 _geom_angle _geom_angle_publ_flag O3 Pb1 O1 3_656 . 83.53(12) ? O3 Pb1 O5 3_656 . 76.84(12) ? O1 Pb1 O5 . . 68.13(11) y O3 Pb1 O4 3_656 3_656 51.07(12) y O1 Pb1 O4 . 3_656 74.99(12) ? O5 Pb1 O4 . 3_656 118.47(11) ? O3 Pb1 O1 3_656 2_746 102.80(12) ? O1 Pb1 O1 . 2_746 137.33(9) ? O5 Pb1 O1 . 2_746 154.54(11) ? O4 Pb1 O1 3_656 2_746 76.94(11) ? O3 Pb1 O3 3_656 1_655 68.98(15) ? O1 Pb1 O3 . 1_655 137.41(12) ? O5 Pb1 O3 . 1_655 74.18(11) ? O4 Pb1 O3 3_656 1_655 107.91(12) ? O1 Pb1 O3 2_746 1_655 81.90(11) ? O3 Pb1 O5 3_656 2_746 115.69(12) ? O1 Pb1 O5 . 2_746 76.97(11) y O5 Pb1 O5 . 2_746 141.45(10) ? O4 Pb1 O5 3_656 2_746 64.72(11) ? O1 Pb1 O5 2_746 2_746 62.12(11) y O3 Pb1 O5 1_655 2_746 144.00(11) ? C6 C1 C2 . . 119.8(5) ? C6 C1 C7 . . 121.8(5) ? C2 C1 C7 . . 118.3(5) ? C3 C2 C1 . . 119.9(5) ? C3 C2 H2 . . 120.1 ? C1 C2 H2 . . 120.1 ? C4 C3 C2 . . 120.5(5) ? C4 C3 H3 . . 119.8 ? C2 C3 H3 . . 119.8 ? C5 C4 C3 . . 119.5(5) ? C5 C4 C8 . . 121.4(5) ? C3 C4 C8 . . 118.9(5) ? C4 C5 C6 . . 120.5(5) ? C4 C5 H5 . . 119.8 ? C6 C5 H5 . . 119.8 ? C5 C6 C1 . . 119.8(5) ? C5 C6 H6 . . 120.1 ? C1 C6 H6 . . 120.1 ? O2 C7 O1 . . 124.0(5) ? O2 C7 C1 . . 117.6(5) ? O1 C7 C1 . . 118.5(5) ? C7 O1 Pb1 . . 125.7(3) ? C7 O1 Pb1 . 2_756 126.8(3) ? Pb1 O1 Pb1 . 2_756 101.25(11) ? O4 C8 O3 . . 121.1(5) ? O4 C8 C4 . . 120.3(5) ? O3 C8 C4 . . 118.4(5) ? C8 O3 Pb1 . 3_656 98.0(3) ? C8 O3 Pb1 . 1_455 134.3(3) ? Pb1 O3 Pb1 3_656 1_455 111.02(15) ? C8 O4 Pb1 . 3_656 88.3(3) ? Pb1 O5 Pb1 . 2_756 98.71(11) ? Pb1 O5 H5A . . 116.7(16) ? Pb1 O5 H5A 2_756 . 116.9(15) ? Pb1 O5 H5B . . 117.7(16) ? Pb1 O5 H5B 2_756 . 117.7(16) ? H5A O5 H5B . . 90.7(17) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 O1 . 2.492(3) y Pb1 O1 2_746 2.731(4) y Pb1 O3 3_656 2.434(4) y Pb1 O3 1_655 2.751(4) y Pb1 O4 3_656 2.650(4) y Pb1 O5 . 2.563(4) y Pb1 O5 2_746 2.759(4) y C1 C6 . 1.393(7) ? C1 C2 . 1.394(7) ? C1 C7 . 1.498(6) ? C2 C3 . 1.391(7) ? C2 H2 . 0.9500 ? C3 C4 . 1.388(8) ? C3 H3 . 0.9500 ? C4 C5 . 1.388(7) ? C4 C8 . 1.503(7) ? C5 C6 . 1.393(7) ? C5 H5 . 0.9500 ? C6 H6 . 0.9500 ? C7 O2 . 1.269(7) ? C7 O1 . 1.272(6) ? C8 O4 . 1.256(6) ? C8 O3 . 1.270(7) ? O5 H5A . 0.92(2) ? O5 H5B . 0.90(2) ? 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 O5 H5B O2 2_756 0.90(2) 1.97(2) 2.728(5) 140(2) O5 H5A O2 4_565 0.92(2) 1.79(2) 2.678(5) 160(2) 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_4 _geom_torsion C6 C1 C2 C3 . . 1.4(8) C7 C1 C2 C3 . . -177.0(5) C1 C2 C3 C4 . . 0.3(8) C2 C3 C4 C5 . . -2.7(8) C2 C3 C4 C8 . . 173.0(5) C3 C4 C5 C6 . . 3.4(8) C8 C4 C5 C6 . . -172.2(5) C4 C5 C6 C1 . . -1.7(8) C2 C1 C6 C5 . . -0.7(8) C7 C1 C6 C5 . . 177.6(5) C6 C1 C7 O2 . . -179.9(5) C2 C1 C7 O2 . . -1.6(7) C6 C1 C7 O1 . . -0.1(8) C2 C1 C7 O1 . . 178.2(5) O2 C7 O1 Pb1 . . 64.4(6) C1 C7 O1 Pb1 . . -115.4(4) O2 C7 O1 Pb1 . 2_756 -82.5(6) C1 C7 O1 Pb1 . 2_756 97.7(5) O3 Pb1 O1 C7 3_656 . 86.3(4) O5 Pb1 O1 C7 . . 164.7(4) O4 Pb1 O1 C7 3_656 . 35.0(4) O1 Pb1 O1 C7 2_746 . -15.6(4) O3 Pb1 O1 C7 1_655 . 135.3(4) O5 Pb1 O1 C7 2_746 . -32.0(4) O3 Pb1 O1 Pb1 3_656 2_756 -120.14(13) O5 Pb1 O1 Pb1 . 2_756 -41.75(11) O4 Pb1 O1 Pb1 3_656 2_756 -171.51(14) O1 Pb1 O1 Pb1 2_746 2_756 137.98(14) O3 Pb1 O1 Pb1 1_655 2_756 -71.20(18) O5 Pb1 O1 Pb1 2_746 2_756 121.56(12) C5 C4 C8 O4 . . -7.0(8) C3 C4 C8 O4 . . 177.4(5) C5 C4 C8 O3 . . 168.1(5) C3 C4 C8 O3 . . -7.6(7) O4 C8 O3 Pb1 . 3_656 13.2(6) C4 C8 O3 Pb1 . 3_656 -161.8(4) O4 C8 O3 Pb1 . 1_455 -116.9(5) C4 C8 O3 Pb1 . 1_455 68.1(6) O3 C8 O4 Pb1 . 3_656 -12.0(5) C4 C8 O4 Pb1 . 3_656 162.9(4) O3 Pb1 O5 Pb1 3_656 2_756 129.07(13) O1 Pb1 O5 Pb1 . 2_756 40.84(10) O4 Pb1 O5 Pb1 3_656 2_756 98.49(13) O1 Pb1 O5 Pb1 2_746 2_756 -138.7(2) O3 Pb1 O5 Pb1 1_655 2_756 -159.39(14) O5 Pb1 O5 Pb1 2_746 2_756 14.2(2)