#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/74/2017458.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_2017458
loop_
_publ_author_name
'Xie, Cheng-Zhi'
'Qiao, Xin'
'Xue, Fei'
'Xu, Jing-Yuan'
_publ_section_title
Poly[bis(μ₃-5'-carboxy-2,2'-bipyridine-5-carboxylato-κ⁴O:N,N':O')lead(II)]
_journal_coeditor_code           SQ3226
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m491
_journal_page_last               m493
_journal_paper_doi               10.1107/S0108270109047015
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pb (C12 H7 N2 O4)2]'
_chemical_formula_moiety         'C24 H14 N4 O8 Pb'
_chemical_formula_sum            'C24 H14 N4 O8 Pb'
_chemical_formula_weight         693.58
_chemical_name_systematic
;
Poly[bis(μ₃-5'-carboxy-2,2'-bipyridine-5-carboxylato-
κ⁴O:N,N':O')lead(II)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.4470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1836(17)
_cell_length_b                   11.3719(13)
_cell_length_c                   13.5342(16)
_cell_measurement_reflns_used    5931
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.33
_cell_volume                     2110.2(4)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Berndt, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(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       'φ and ω'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7034
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    8.061
_exptl_absorpt_correction_T_max  0.5649
_exptl_absorpt_correction_T_min  0.2955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0284P)²+3.5386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                1909
_reflns_number_total             1977
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3226.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017458
_cod_database_fobs_code          2017458
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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 1.0000 -0.185023(14) 0.2500 0.02158(8) Uani d S 1 . .
O O1 1.35482(18) 0.0450(3) 0.3027(3) 0.0431(7) Uani d . 1 . .
O O2 1.33990(19) 0.2374(3) 0.2601(3) 0.0427(7) Uani d . 1 . .
O O3 0.53033(17) 0.0145(2) -0.1189(3) 0.0393(7) Uani d . 1 . .
H H3 0.4765 -0.0169 -0.1437 0.059 Uiso calc R 1 . .
O O4 0.5826(2) -0.1696(2) -0.0702(3) 0.0365(7) Uani d . 1 . .
N N1 1.05914(19) -0.0069(2) 0.1651(2) 0.0234(6) Uani d . 1 . .
N N2 0.86879(19) -0.0556(3) 0.0862(2) 0.0242(6) Uani d . 1 . .
C C1 1.1553(2) 0.0136(3) 0.2098(3) 0.0228(7) Uani d . 1 . .
H H1 1.1972 -0.0493 0.2416 0.027 Uiso calc R 1 . .
C C2 1.1966(2) 0.1240(3) 0.2116(3) 0.0214(7) Uani d . 1 . .
C C3 1.1322(3) 0.2174(3) 0.1641(3) 0.0302(8) Uani d . 1 . .
H H3A 1.1560 0.2932 0.1663 0.036 Uiso calc R 1 . .
C C4 1.0322(3) 0.1960(3) 0.1134(4) 0.0305(9) Uani d . 1 . .
H H4 0.9887 0.2567 0.0792 0.037 Uiso calc R 1 . .
C C5 0.9984(2) 0.0825(3) 0.1147(3) 0.0212(7) Uani d . 1 . .
C C6 0.8921(2) 0.0515(3) 0.0612(3) 0.0210(7) Uani d . 1 . .
C C7 0.8212(2) 0.1262(3) -0.0118(3) 0.0278(8) Uani d . 1 . .
H H7 0.8387 0.1984 -0.0302 0.033 Uiso calc R 1 . .
C C8 0.7239(2) 0.0916(3) -0.0568(3) 0.0283(8) Uani d . 1 . .
H H8 0.6755 0.1413 -0.1042 0.034 Uiso calc R 1 . .
C C9 0.6999(2) -0.0179(3) -0.0302(3) 0.0231(7) Uani d . 1 . .
C C10 0.7750(2) -0.0891(3) 0.0406(3) 0.0243(7) Uani d . 1 . .
H H10 0.7595 -0.1634 0.0570 0.029 Uiso calc R 1 . .
C C11 1.3063(2) 0.1379(3) 0.2624(3) 0.0245(7) Uani d . 1 . .
C C12 0.5974(2) -0.0649(3) -0.0754(3) 0.0255(7) Uani d . 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'
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
O2 Pb1 O2 3_445 4_745 141.03(13) yes
O2 Pb1 N1 3_445 2_755 75.17(9) ?
O2 Pb1 N1 4_745 2_755 139.69(9) ?
O2 Pb1 N1 3_445 . 139.69(9) yes
O2 Pb1 N1 4_745 . 75.17(9) yes
N1 Pb1 N1 2_755 . 81.17(12) yes
O2 Pb1 N2 3_445 2_755 120.73(10) ?
O2 Pb1 N2 4_745 2_755 81.58(9) ?
N1 Pb1 N2 2_755 2_755 59.82(8) ?
N1 Pb1 N2 . 2_755 70.89(9) ?
O2 Pb1 N2 3_445 . 81.58(9) yes
O2 Pb1 N2 4_745 . 120.73(10) yes
N1 Pb1 N2 2_755 . 70.89(9) yes
N1 Pb1 N2 . . 59.82(8) yes
N2 Pb1 N2 2_755 . 113.75(12) yes
O2 Pb1 O4 3_445 7_645 76.46(10) yes
O2 Pb1 O4 4_745 7_645 80.46(9) yes
N1 Pb1 O4 2_755 7_645 136.50(8) ?
N1 Pb1 O4 . 7_645 100.65(9) yes
N2 Pb1 O4 2_755 7_645 161.64(9) ?
N2 Pb1 O4 . 7_645 72.90(9) yes
O2 Pb1 O4 3_445 8_546 80.46(9) ?
O2 Pb1 O4 4_745 8_546 76.46(10) ?
N1 Pb1 O4 2_755 8_546 100.65(9) ?
N1 Pb1 O4 . 8_546 136.50(8) yes
N2 Pb1 O4 2_755 8_546 72.90(9) ?
N2 Pb1 O4 . 8_546 161.64(9) yes
O4 Pb1 O4 7_645 8_546 106.36(12) yes
C11 O2 Pb1 . 3 134.3(2) ?
C12 O3 H3 . . 109.5 ?
C12 O4 Pb1 . 7_645 124.0(3) ?
C1 N1 C5 . . 118.4(3) ?
C1 N1 Pb1 . . 116.2(2) ?
C5 N1 Pb1 . . 120.5(2) ?
C10 N2 C6 . . 118.8(3) ?
C10 N2 Pb1 . . 119.1(2) ?
C6 N2 Pb1 . . 121.2(2) ?
N1 C1 C2 . . 123.8(3) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C1 C2 C3 . . 117.0(3) ?
C1 C2 C11 . . 119.9(3) ?
C3 C2 C11 . . 123.0(3) ?
C4 C3 C2 . . 119.5(3) ?
C4 C3 H3A . . 120.3 ?
C2 C3 H3A . . 120.3 ?
C5 C4 C3 . . 119.1(3) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N1 C5 C4 . . 122.1(3) ?
N1 C5 C6 . . 115.4(3) ?
C4 C5 C6 . . 122.5(3) ?
N2 C6 C7 . . 121.4(3) ?
N2 C6 C5 . . 115.7(3) ?
C7 C6 C5 . . 122.8(3) ?
C8 C7 C6 . . 119.3(3) ?
C8 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
C9 C8 C7 . . 119.2(3) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 118.2(3) ?
C8 C9 C12 . . 123.7(3) ?
C10 C9 C12 . . 118.1(3) ?
N2 C10 C9 . . 123.0(3) ?
N2 C10 H10 . . 118.5 ?
C9 C10 H10 . . 118.5 ?
O2 C11 O1 . . 126.7(3) ?
O2 C11 C2 . . 117.8(3) ?
O1 C11 C2 . . 115.5(3) ?
O4 C12 O3 . . 125.3(3) ?
O4 C12 C9 . . 120.5(3) ?
O3 C12 C9 . . 114.2(3) ?
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 O2 3_445 2.644(3) yes
Pb1 O2 4_745 2.644(3) ?
Pb1 N1 2_755 2.667(3) ?
Pb1 N1 . 2.667(3) yes
Pb1 N2 2_755 2.694(3) ?
Pb1 N2 . 2.694(3) yes
Pb1 O4 7_645 2.758(3) ?
Pb1 O4 8_546 2.758(3) yes
O1 C11 . 1.269(5) yes
O2 C11 . 1.247(5) yes
O2 Pb1 3 2.644(3) ?
O3 C12 . 1.298(4) yes
O3 H3 . 0.8200 ?
O4 C12 . 1.219(4) yes
O4 Pb1 7_645 2.758(3) ?
N1 C1 . 1.339(4) ?
N1 C5 . 1.345(4) ?
N2 C10 . 1.341(4) ?
N2 C6 . 1.351(4) ?
C1 C2 . 1.398(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.399(5) ?
C2 C11 . 1.513(4) ?
C3 C4 . 1.392(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.392(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.500(4) ?
C6 C7 . 1.394(5) ?
C7 C8 . 1.391(5) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.387(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.391(5) ?
C9 C12 . 1.505(4) ?
C10 H10 . 0.9300 ?
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
O2 Pb1 N1 C1 3_445 . . . 160.3(2) ?
O2 Pb1 N1 C1 4_745 . . . -41.1(2) ?
N1 Pb1 N1 C1 2_755 . . . 106.0(3) ?
N2 Pb1 N1 C1 2_755 . . . 45.0(2) ?
N2 Pb1 N1 C1 . . . . 179.0(3) ?
O4 Pb1 N1 C1 7_645 . . . -118.1(2) ?
O4 Pb1 N1 C1 8_546 . . . 9.8(3) ?
O2 Pb1 N1 C5 3_445 . . . 5.6(3) ?
O2 Pb1 N1 C5 4_745 . . . 164.2(3) ?
N1 Pb1 N1 C5 2_755 . . . -48.7(2) ?
N2 Pb1 N1 C5 2_755 . . . -109.7(3) ?
N2 Pb1 N1 C5 . . . . 24.3(2) ?
O4 Pb1 N1 C5 7_645 . . . 87.2(3) ?
O4 Pb1 N1 C5 8_546 . . . -144.9(2) ?
O2 Pb1 N2 C10 3_445 . . . -18.9(3) ?
O2 Pb1 N2 C10 4_745 . . . 126.9(2) ?
N1 Pb1 N2 C10 2_755 . . . -96.0(3) ?
N1 Pb1 N2 C10 . . . . 173.2(3) ?
N2 Pb1 N2 C10 2_755 . . . -138.8(3) ?
O4 Pb1 N2 C10 7_645 . . . 59.5(3) ?
O4 Pb1 N2 C10 8_546 . . . -31.0(4) ?
O2 Pb1 N2 C6 3_445 . . . 150.3(3) ?
O2 Pb1 N2 C6 4_745 . . . -64.0(3) ?
N1 Pb1 N2 C6 2_755 . . . 73.1(2) ?
N1 Pb1 N2 C6 . . . . -17.6(2) ?
N2 Pb1 N2 C6 2_755 . . . 30.3(2) ?
O4 Pb1 N2 C6 7_645 . . . -131.4(3) ?
O4 Pb1 N2 C6 8_546 . . . 138.1(3) ?
C5 N1 C1 C2 . . . . 3.0(5) ?
Pb1 N1 C1 C2 . . . . -152.3(3) ?
N1 C1 C2 C3 . . . . 0.5(5) ?
N1 C1 C2 C11 . . . . -179.0(3) ?
C1 C2 C3 C4 . . . . -3.1(6) ?
C11 C2 C3 C4 . . . . 176.3(4) ?
C2 C3 C4 C5 . . . . 2.3(6) ?
C1 N1 C5 C4 . . . . -3.9(5) ?
Pb1 N1 C5 C4 . . . . 150.3(3) ?
C1 N1 C5 C6 . . . . 176.7(3) ?
Pb1 N1 C5 C6 . . . . -29.1(4) ?
C3 C4 C5 N1 . . . . 1.3(6) ?
C3 C4 C5 C6 . . . . -179.3(4) ?
C10 N2 C6 C7 . . . . -1.0(5) ?
Pb1 N2 C6 C7 . . . . -170.2(3) ?
C10 N2 C6 C5 . . . . -179.6(3) ?
Pb1 N2 C6 C5 . . . . 11.2(4) ?
N1 C5 C6 N2 . . . . 11.3(4) ?
C4 C5 C6 N2 . . . . -168.1(3) ?
N1 C5 C6 C7 . . . . -167.2(3) ?
C4 C5 C6 C7 . . . . 13.4(5) ?
N2 C6 C7 C8 . . . . 2.4(5) ?
C5 C6 C7 C8 . . . . -179.1(3) ?
C6 C7 C8 C9 . . . . -1.7(6) ?
C7 C8 C9 C10 . . . . -0.3(5) ?
C7 C8 C9 C12 . . . . -179.1(3) ?
C6 N2 C10 C9 . . . . -1.1(5) ?
Pb1 N2 C10 C9 . . . . 168.3(3) ?
C8 C9 C10 N2 . . . . 1.7(5) ?
C12 C9 C10 N2 . . . . -179.4(3) ?
Pb1 O2 C11 O1 3 . . . 30.4(6) ?
Pb1 O2 C11 C2 3 . . . -149.1(3) ?
C1 C2 C11 O2 . . . . 178.5(3) ?
C3 C2 C11 O2 . . . . -0.9(5) ?
C1 C2 C11 O1 . . . . -1.0(5) ?
C3 C2 C11 O1 . . . . 179.6(4) ?
Pb1 O4 C12 O3 7_645 . . . 65.8(5) ?
Pb1 O4 C12 C9 7_645 . . . -113.6(3) ?
C8 C9 C12 O4 . . . . 162.9(4) ?
C10 C9 C12 O4 . . . . -15.9(5) ?
C8 C9 C12 O3 . . . . -16.6(5) ?
C10 C9 C12 O3 . . . . 164.6(3) ?
