#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/59/2225985.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_2225985
loop_
_publ_author_name
'Chen, Xiang'
'Liu, Hai-Cheng'
_publ_section_title
;
 Poly[diaquabis(μ₂-5-carboxy-2-propyl-1H-imidazole-4-carboxylato-κ³N³,O⁴:O⁵)lead(II)]
;
_journal_coeditor_code           SJ2771
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m543
_journal_paper_doi               10.1107/S1600536810013735
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C8 H9 N2 O4)2 (H2 O)2]'
_chemical_formula_moiety         'C16 H22 N4 O10 Pb'
_chemical_formula_sum            'C16 H22 N4 O10 Pb'
_chemical_formula_weight         637.57
_chemical_name_systematic
;
Poly[diaquabis(μ₂-5-carboxy-2-propyl-1H-imidazole-4-carboxylato-
κ³N³,O⁴:O⁵)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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.531(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1201(15)
_cell_length_b                   13.2929(16)
_cell_length_c                   11.5910(13)
_cell_measurement_reflns_used    2051
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.917
_cell_measurement_theta_min      2.483
_cell_volume                     1999.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4884
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.504
_exptl_absorpt_correction_T_max  0.4044
_exptl_absorpt_correction_T_min  0.1144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.689
_refine_ls_extinction_coef       0.00501(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0192
_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/[σ²(Fo²)+0.1700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                1640
_reflns_number_total             1751
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj2771.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2225985
_cod_database_fobs_code          2225985
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 0.5000 0.585420(12) 0.7500 0.02187(10) Uani d S 1 . .
N N1 0.36101(17) 0.72953(19) 0.7416(2) 0.0206(6) Uani d . 1 . .
N N2 0.26176(19) 0.8636(2) 0.7255(2) 0.0245(6) Uani d . 1 . .
H H2 0.2380 0.9221 0.7040 0.029 Uiso calc R 1 . .
O O1 0.33533(16) 0.55121(18) 0.8607(2) 0.0288(6) Uani d . 1 . .
O O2 0.20043(17) 0.61233(19) 0.9317(2) 0.0346(6) Uani d . 1 . .
O O3 0.09662(17) 0.7669(2) 0.9230(2) 0.0400(7) Uani d . 1 . .
H H3 0.1304 0.7149 0.9245 0.060 Uiso calc R 1 . .
O O4 0.0980(2) 0.9168(2) 0.8428(3) 0.0521(9) Uani d . 1 . .
O O5 0.43915(18) 0.6096(2) 0.5232(2) 0.0374(6) Uani d . 1 . .
H H5C 0.4120 0.5656 0.4750 0.045 Uiso d R 1 . .
H H5D 0.4830 0.6427 0.4915 0.045 Uiso d R 1 . .
C C1 0.2736(2) 0.6209(3) 0.8716(3) 0.0240(7) Uani d . 1 . .
C C2 0.2842(2) 0.7169(2) 0.8095(3) 0.0204(7) Uani d . 1 . .
C C3 0.2221(2) 0.8003(3) 0.7997(3) 0.0228(8) Uani d . 1 . .
C C4 0.1323(3) 0.8316(3) 0.8572(3) 0.0314(9) Uani d . 1 . .
C C5 0.3450(2) 0.8188(2) 0.6912(3) 0.0230(8) Uani d . 1 . .
C C6 0.4039(2) 0.8661(3) 0.6046(3) 0.0285(8) Uani d . 1 . .
H H6A 0.4688 0.8309 0.6062 0.034 Uiso calc R 1 . .
H H6B 0.4193 0.9353 0.6274 0.034 Uiso calc R 1 . .
C C7 0.3461(3) 0.8646(3) 0.4806(3) 0.0355(9) Uani d . 1 . .
H H7A 0.3380 0.7954 0.4541 0.043 Uiso calc R 1 . .
H H7B 0.2779 0.8928 0.4803 0.043 Uiso calc R 1 . .
C C8 0.4016(3) 0.9236(3) 0.3967(4) 0.0408(10) Uani d . 1 . .
H H8A 0.4129 0.9913 0.4246 0.061 Uiso calc R 1 . .
H H8B 0.3604 0.9245 0.3210 0.061 Uiso calc R 1 . .
H H8C 0.4667 0.8923 0.3914 0.061 Uiso calc 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'
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'
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
N1 Pb1 N1 . 2_656 86.81(11) ?
N1 Pb1 O5 . 2_656 93.06(8) ?
N1 Pb1 O5 2_656 2_656 76.75(8) ?
N1 Pb1 O5 . . 76.75(8) ?
N1 Pb1 O5 2_656 . 93.06(8) ?
O5 Pb1 O5 2_656 . 166.09(11) ?
N1 Pb1 O1 . . 62.85(7) ?
N1 Pb1 O1 2_656 . 134.44(7) ?
O5 Pb1 O1 2_656 . 72.23(7) ?
O5 Pb1 O1 . . 110.24(7) ?
N1 Pb1 O1 . 2_656 134.44(7) ?
N1 Pb1 O1 2_656 2_656 62.85(7) ?
O5 Pb1 O1 2_656 2_656 110.23(7) ?
O5 Pb1 O1 . 2_656 72.23(7) ?
O1 Pb1 O1 . 2_656 160.68(10) ?
N1 Pb1 O4 . 3_545 153.57(9) ?
N1 Pb1 O4 2_656 3_545 107.45(9) ?
O5 Pb1 O4 2_656 3_545 69.71(9) ?
O5 Pb1 O4 . 3_545 123.10(9) ?
O1 Pb1 O4 . 3_545 92.16(8) ?
O1 Pb1 O4 2_656 3_545 71.71(8) ?
N1 Pb1 O4 . 4_546 107.46(9) ?
N1 Pb1 O4 2_656 4_546 153.56(9) ?
O5 Pb1 O4 2_656 4_546 123.10(9) ?
O5 Pb1 O4 . 4_546 69.70(9) ?
O1 Pb1 O4 . 4_546 71.72(8) ?
O1 Pb1 O4 2_656 4_546 92.16(8) ?
O4 Pb1 O4 3_545 4_546 69.29(14) ?
C5 N1 C2 . . 106.2(3) ?
C5 N1 Pb1 . . 136.9(2) ?
C2 N1 Pb1 . . 116.79(19) ?
C5 N2 C3 . . 108.3(3) ?
C5 N2 H2 . . 125.9 ?
C3 N2 H2 . . 125.9 ?
C1 O1 Pb1 . . 119.8(2) ?
C4 O3 H3 . . 109.5 ?
C4 O4 Pb1 . 3_455 163.7(3) ?
Pb1 O5 H5C . . 127.1 ?
Pb1 O5 H5D . . 111.6 ?
H5C O5 H5D . . 108.5 ?
O1 C1 O2 . . 122.8(3) ?
O1 C1 C2 . . 118.7(3) ?
O2 C1 C2 . . 118.4(3) ?
C3 C2 N1 . . 109.3(3) ?
C3 C2 C1 . . 129.8(3) ?
N1 C2 C1 . . 120.8(3) ?
N2 C3 C2 . . 106.0(3) ?
N2 C3 C4 . . 120.6(3) ?
C2 C3 C4 . . 133.3(3) ?
O4 C4 O3 . . 122.8(3) ?
O4 C4 C3 . . 119.8(4) ?
O3 C4 C3 . . 117.3(3) ?
N1 C5 N2 . . 110.3(3) ?
N1 C5 C6 . . 127.6(3) ?
N2 C5 C6 . . 122.1(3) ?
C5 C6 C7 . . 113.2(3) ?
C5 C6 H6A . . 108.9 ?
C7 C6 H6A . . 108.9 ?
C5 C6 H6B . . 108.9 ?
C7 C6 H6B . . 108.9 ?
H6A C6 H6B . . 107.8 ?
C8 C7 C6 . . 112.3(3) ?
C8 C7 H7A . . 109.1 ?
C6 C7 H7A . . 109.1 ?
C8 C7 H7B . . 109.1 ?
C6 C7 H7B . . 109.1 ?
H7A C7 H7B . . 107.9 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
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 . 2.637(2) ?
Pb1 N1 2_656 2.637(2) ?
Pb1 O5 2_656 2.651(3) ?
Pb1 O5 . 2.652(3) ?
Pb1 O1 . 2.710(2) ?
Pb1 O1 2_656 2.710(2) ?
Pb1 O4 3_545 2.725(3) ?
Pb1 O4 4_546 2.725(3) ?
N1 C5 . 1.326(4) ?
N1 C2 . 1.377(4) ?
N2 C5 . 1.354(4) ?
N2 C3 . 1.361(5) ?
N2 H2 . 0.8600 ?
O1 C1 . 1.249(4) ?
O2 C1 . 1.273(4) ?
O3 C4 . 1.284(4) ?
O3 H3 . 0.8200 ?
O4 C4 . 1.221(4) ?
O4 Pb1 3_455 2.725(3) ?
O5 H5C . 0.8500 ?
O5 H5D . 0.8500 ?
C1 C2 . 1.481(5) ?
C2 C3 . 1.370(4) ?
C3 C4 . 1.496(5) ?
C5 C6 . 1.494(5) ?
C6 C7 . 1.522(4) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.517(5) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
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 H5D O4 8_565 0.85 2.58 3.182(4) 129.1
O5 H5D O3 8_565 0.85 2.16 3.004(3) 175.7
O5 H5C O1 6_565 0.85 2.19 3.035(3) 175.8
O3 H3 O2 . 0.82 1.64 2.459(3) 178.1
N2 H2 O1 4_556 0.86 2.05 2.909(4) 172.0
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
N1 Pb1 N1 C5 2_656 . . . 39.1(3) ?
O5 Pb1 N1 C5 2_656 . . . 115.6(3) ?
O5 Pb1 N1 C5 . . . . -54.8(3) ?
O1 Pb1 N1 C5 . . . . -176.2(3) ?
O1 Pb1 N1 C5 2_656 . . . -6.9(3) ?
O4 Pb1 N1 C5 3_545 . . . 163.3(3) ?
O4 Pb1 N1 C5 4_546 . . . -118.2(3) ?
N1 Pb1 N1 C2 2_656 . . . -137.1(2) ?
O5 Pb1 N1 C2 2_656 . . . -60.6(2) ?
O5 Pb1 N1 C2 . . . . 129.0(2) ?
O1 Pb1 N1 C2 . . . . 7.63(19) ?
O1 Pb1 N1 C2 2_656 . . . 176.89(18) ?
O4 Pb1 N1 C2 3_545 . . . -12.9(3) ?
O4 Pb1 N1 C2 4_546 . . . 65.6(2) ?
N1 Pb1 O1 C1 . . . . -8.6(2) ?
N1 Pb1 O1 C1 2_656 . . . 45.2(3) ?
O5 Pb1 O1 C1 2_656 . . . 94.6(2) ?
O5 Pb1 O1 C1 . . . . -70.9(2) ?
O1 Pb1 O1 C1 2_656 . . . -164.9(2) ?
O4 Pb1 O1 C1 3_545 . . . 162.5(2) ?
O4 Pb1 O1 C1 4_546 . . . -130.2(2) ?
Pb1 O1 C1 O2 . . . . -173.4(2) ?
Pb1 O1 C1 C2 . . . . 8.3(4) ?
C5 N1 C2 C3 . . . . -0.4(3) ?
Pb1 N1 C2 C3 . . . . 176.90(19) ?
C5 N1 C2 C1 . . . . 175.1(3) ?
Pb1 N1 C2 C1 . . . . -7.6(3) ?
O1 C1 C2 C3 . . . . 174.0(3) ?
O2 C1 C2 C3 . . . . -4.4(5) ?
O1 C1 C2 N1 . . . . -0.5(4) ?
O2 C1 C2 N1 . . . . -178.9(3) ?
C5 N2 C3 C2 . . . . 0.4(4) ?
C5 N2 C3 C4 . . . . 176.8(3) ?
N1 C2 C3 N2 . . . . 0.0(3) ?
C1 C2 C3 N2 . . . . -175.0(3) ?
N1 C2 C3 C4 . . . . -175.8(3) ?
C1 C2 C3 C4 . . . . 9.3(6) ?
Pb1 O4 C4 O3 3_455 . . . -108.0(9) ?
Pb1 O4 C4 C3 3_455 . . . 74.0(10) ?
N2 C3 C4 O4 . . . . -4.3(5) ?
C2 C3 C4 O4 . . . . 171.0(4) ?
N2 C3 C4 O3 . . . . 177.7(3) ?
C2 C3 C4 O3 . . . . -7.1(6) ?
C2 N1 C5 N2 . . . . 0.7(3) ?
Pb1 N1 C5 N2 . . . . -175.8(2) ?
C2 N1 C5 C6 . . . . -176.9(3) ?
Pb1 N1 C5 C6 . . . . 6.7(5) ?
C3 N2 C5 N1 . . . . -0.7(4) ?
C3 N2 C5 C6 . . . . 177.0(3) ?
N1 C5 C6 C7 . . . . 105.0(4) ?
N2 C5 C6 C7 . . . . -72.3(4) ?
C5 C6 C7 C8 . . . . 173.3(3) ?
