#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/52/2225221.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_2225221
loop_
_publ_author_name
'Yang, Li-Qing'
'Li, Xin-Hua'
_publ_section_title
;
 Poly[[(2,2'-bipyridine)(μ₃-2-sulfonatobenzoato)lead(II)] dihydrate]
;
_journal_coeditor_code           DN2537
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m310
_journal_page_last               m311
_journal_paper_doi               10.1107/S1600536810005763
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C7 H4 O5 S) (C10 H8 N2)], 2H2 O'
_chemical_formula_moiety         'C17 H12 N2 O5 Pb S, 2(H2 O)'
_chemical_formula_sum            'C17 H16 N2 O7 Pb S'
_chemical_formula_weight         599.57
_chemical_name_systematic
;
Poly[[(2,2'-bipyridine)(μ₃-2-sulfonatobenzoato)lead(II)] dihydrate]
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.6290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3464(11)
_cell_length_b                   6.9951(5)
_cell_length_c                   17.2844(12)
_cell_measurement_reflns_used    3318
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.37
_cell_volume                     1843.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '600 frames, delta omega = 2 dgr'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9382
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.311
_exptl_absorpt_correction_T_max  0.26
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.831
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0286P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                2944
_reflns_number_total             3318
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            dn2537.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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               2225221
_cod_database_fobs_code          2225221
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_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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.402858(9) 0.234749(19) -0.017420(8) 0.03015(7) Uani d . 1 . .
S S1 0.25615(7) -0.17058(17) -0.11614(6) 0.0407(3) Uani d . 1 . .
O O1 0.43147(15) -0.1252(4) 0.00541(15) 0.0333(6) Uani d . 1 . .
O O2 0.42527(16) -0.4252(4) 0.04577(16) 0.0393(7) Uani d . 1 . .
O O3 0.3148(2) -0.3281(5) -0.12513(18) 0.0558(8) Uani d . 1 . .
O O4 0.1728(2) -0.1882(5) -0.16536(18) 0.0566(8) Uani d . 1 . .
O O5 0.29504(18) 0.0181(4) -0.12329(15) 0.0503(8) Uani d . 1 . .
N N1 0.4155(2) 0.1825(5) 0.12289(17) 0.0307(7) Uani d . 1 . .
N N2 0.2610(2) 0.2622(4) 0.0397(2) 0.0351(8) Uani d . 1 . .
C C1 0.4933(2) 0.1312(5) 0.1606(2) 0.0352(9) Uani d . 1 . .
H H1 0.5424 0.1327 0.1337 0.042 Uiso calc R 1 . .
C C2 0.5031(3) 0.0765(6) 0.2376(2) 0.0443(10) Uani d . 1 . .
H H2 0.5576 0.0398 0.2622 0.053 Uiso calc R 1 . .
C C3 0.4304(3) 0.0773(6) 0.2774(2) 0.0499(11) Uani d . 1 . .
H H3 0.4351 0.0400 0.3294 0.060 Uiso calc R 1 . .
C C4 0.3511(3) 0.1333(6) 0.2399(2) 0.0476(11) Uani d . 1 . .
H H4 0.3018 0.1355 0.2665 0.057 Uiso calc R 1 . .
C C5 0.3442(3) 0.1870(5) 0.1619(2) 0.0340(9) Uani d . 1 . .
C C6 0.2604(3) 0.2435(5) 0.1169(3) 0.0382(11) Uani d . 1 . .
C C7 0.1840(4) 0.2756(6) 0.1507(4) 0.0584(15) Uani d . 1 . .
H H7 0.1837 0.2637 0.2042 0.070 Uiso calc R 1 . .
C C8 0.1089(3) 0.3251(8) 0.1042(4) 0.0723(17) Uani d . 1 . .
H H8 0.0572 0.3459 0.1262 0.087 Uiso calc R 1 . .
C C9 0.1097(3) 0.3439(7) 0.0258(4) 0.0638(15) Uani d . 1 . .
H H9 0.0592 0.3776 -0.0063 0.077 Uiso calc R 1 . .
C C10 0.1878(3) 0.3116(6) -0.0047(3) 0.0500(12) Uani d . 1 . .
H H10 0.1892 0.3248 -0.0581 0.060 Uiso calc R 1 . .
C C11 0.3901(3) -0.2673(5) 0.0288(2) 0.0274(9) Uani d . 1 . .
C C12 0.2956(3) -0.2376(4) 0.0411(3) 0.0308(9) Uani d . 1 . .
C C13 0.2730(3) -0.2575(5) 0.1167(3) 0.0389(11) Uani d . 1 . .
H H13 0.3152 -0.2949 0.1568 0.047 Uiso calc R 1 . .
C C14 0.1877(3) -0.2215(6) 0.1319(3) 0.0491(13) Uani d . 1 . .
H H14 0.1731 -0.2319 0.1825 0.059 Uiso calc R 1 . .
C C15 0.1244(3) -0.1702(6) 0.0723(3) 0.0477(11) Uani d . 1 . .
H H15 0.0674 -0.1455 0.0829 0.057 Uiso calc R 1 . .
C C16 0.1451(2) -0.1554(6) -0.0030(3) 0.0412(10) Uani d . 1 . .
H H16 0.1019 -0.1232 -0.0431 0.049 Uiso calc R 1 . .
C C17 0.2304(2) -0.1884(5) -0.0192(2) 0.0316(8) Uani d . 1 . .
O O6 0.0809(3) 0.4682(6) -0.1967(3) 0.1033(15) Uani d . 1 . .
H H6A 0.1149 0.5621 -0.1834 0.155 Uiso d R 1 . .
H H6B 0.0420 0.5073 -0.2324 0.155 Uiso d R 1 . .
O O7 0.0420(2) 0.0904(6) -0.1850(2) 0.0793(11) Uani d . 1 . .
H H7A 0.0845 0.0127 -0.1844 0.119 Uiso d R 1 . .
H H7B 0.0594 0.2030 -0.1938 0.119 Uiso d R 1 . .
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'
S S 0.1246 0.1234 '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
N1 Pb1 N2 . . 65.91(11) ?
N1 Pb1 O1 . . 73.07(9) ?
N2 Pb1 O1 . . 98.94(8) ?
N1 Pb1 O2 . 1_565 74.35(9) ?
N2 Pb1 O2 . 1_565 81.04(9) ?
O1 Pb1 O2 . 1_565 144.08(8) ?
N1 Pb1 O1 . 3_655 85.01(9) ?
N2 Pb1 O1 . 3_655 150.00(10) ?
O1 Pb1 O1 . 3_655 63.85(9) ?
O2 Pb1 O1 1_565 3_655 98.72(7) ?
O3 S1 O4 . . 112.87(19) ?
O3 S1 O5 . . 114.6(2) ?
O4 S1 O5 . . 111.53(19) ?
O3 S1 C17 . . 104.97(19) ?
O4 S1 C17 . . 105.67(19) ?
O5 S1 C17 . . 106.38(17) ?
C11 O1 Pb1 . . 136.9(2) ?
C11 O1 Pb1 . 3_655 105.1(2) ?
Pb1 O1 Pb1 . 3_655 116.15(9) ?
C11 O2 Pb1 . 1_545 132.2(2) ?
C1 N1 C5 . . 119.4(3) ?
C1 N1 Pb1 . . 119.2(2) ?
C5 N1 Pb1 . . 121.1(3) ?
C10 N2 C6 . . 119.8(4) ?
C10 N2 Pb1 . . 120.6(3) ?
C6 N2 Pb1 . . 119.4(3) ?
N1 C1 C2 . . 122.4(4) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C3 C2 C1 . . 118.5(4) ?
C3 C2 H2 . . 120.7 ?
C1 C2 H2 . . 120.7 ?
C4 C3 C2 . . 119.5(4) ?
C4 C3 H3 . . 120.3 ?
C2 C3 H3 . . 120.3 ?
C3 C4 C5 . . 120.0(4) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
N1 C5 C4 . . 120.1(4) ?
N1 C5 C6 . . 116.7(4) ?
C4 C5 C6 . . 123.1(4) ?
N2 C6 C7 . . 120.3(5) ?
N2 C6 C5 . . 116.4(4) ?
C7 C6 C5 . . 123.3(5) ?
C8 C7 C6 . . 119.3(6) ?
C8 C7 H7 . . 120.4 ?
C6 C7 H7 . . 120.4 ?
C9 C8 C7 . . 120.2(5) ?
C9 C8 H8 . . 119.9 ?
C7 C8 H8 . . 119.9 ?
C8 C9 C10 . . 118.2(5) ?
C8 C9 H9 . . 120.9 ?
C10 C9 H9 . . 120.9 ?
N2 C10 C9 . . 122.2(5) ?
N2 C10 H10 . . 118.9 ?
C9 C10 H10 . . 118.9 ?
O2 C11 O1 . . 123.2(4) ?
O2 C11 C12 . . 119.1(3) ?
O1 C11 C12 . . 117.6(3) ?
C13 C12 C17 . . 119.1(4) ?
C13 C12 C11 . . 117.8(4) ?
C17 C12 C11 . . 123.2(4) ?
C14 C13 C12 . . 120.1(5) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C15 C14 C13 . . 120.2(4) ?
C15 C14 H14 . . 119.9 ?
C13 C14 H14 . . 119.9 ?
C16 C15 C14 . . 120.3(4) ?
C16 C15 H15 . . 119.8 ?
C14 C15 H15 . . 119.8 ?
C15 C16 C17 . . 120.2(4) ?
C15 C16 H16 . . 119.9 ?
C17 C16 H16 . . 119.9 ?
C16 C17 C12 . . 120.0(4) ?
C16 C17 S1 . . 119.8(3) ?
C12 C17 S1 . . 120.1(3) ?
H6A O6 H6B . . 107.6 ?
H7A O7 H7B . . 109.7 ?
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 N1 . 2.438(3) ?
Pb1 N2 . 2.499(4) ?
Pb1 O1 . 2.579(3) ?
Pb1 O2 1_565 2.623(3) ?
Pb1 O1 3_655 2.640(2) ?
S1 O3 . 1.442(3) ?
S1 O4 . 1.457(3) ?
S1 O5 . 1.460(3) ?
S1 C17 . 1.770(4) ?
O1 C11 . 1.270(4) ?
O1 Pb1 3_655 2.640(2) ?
O2 C11 . 1.250(4) ?
O2 Pb1 1_545 2.623(3) ?
N1 C1 . 1.341(5) ?
N1 C5 . 1.350(5) ?
N2 C10 . 1.331(6) ?
N2 C6 . 1.343(6) ?
C1 C2 . 1.377(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.376(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.369(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.392(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.477(6) ?
C6 C7 . 1.387(7) ?
C7 C8 . 1.371(8) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.362(7) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.382(6) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.503(5) ?
C12 C13 . 1.397(7) ?
C12 C17 . 1.402(6) ?
C13 C14 . 1.389(7) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.380(7) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.379(6) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.388(5) ?
C16 H16 . 0.9300 ?
O6 H6A . 0.8533 ?
O6 H6B . 0.8532 ?
O7 H7A . 0.8484 ?
O7 H7B . 0.8510 ?
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
O6 H6A O4 1_565 0.85 1.97 2.808(5) 167.5
O6 H6B O7 2_554 0.85 1.90 2.752(6) 177.8
O7 H7A O4 . 0.85 1.95 2.791(5) 168.7
O7 H7B O6 . 0.85 1.89 2.722(6) 167.0
