#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/58/2225854.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_2225854
loop_
_publ_author_name
'Starosta, Wojciech'
'Leciejewicz, Janusz'
_publ_section_title
;
 Poly[aqua(μ-pyrazine-2-carboxylato-κ³N,O:O)(μ-pyrazine-2-carboxylato-κ³N,O:O')lead(II)]
;
_journal_coeditor_code           HB5383
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m525
_journal_page_last               m526
_journal_paper_doi               10.1107/S1600536810013188
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C5 H3 N2 O2)2 (H2 O)]'
_chemical_formula_moiety         'C10 H8 N4 O5 Pb'
_chemical_formula_sum            'C10 H8 N4 O5 Pb'
_chemical_formula_weight         471.39
_chemical_name_common            'Lead pyrazinate monohydrate'
_chemical_name_systematic
;
Poly[aqua(μ-pyrazine-2-carboxylato-κ³N,O:O)(μ-
pyrazine-2-carboxylato-κ³N,O:O')lead(II)]
;
_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                 114.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.098(2)
_cell_length_b                   10.382(2)
_cell_length_c                   11.678(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     1228.0(5)
_computing_cell_refinement       'KM-4 software (Kuma, 1996)'
_computing_data_collection       'KM-4 software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Kuma KM-4 four-circle diffractometer'
_diffrn_measurement_method       'profile data from ω/2θ 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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3579
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        20.24
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.766
_exptl_absorpt_correction_T_max  0.251
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         6.450
_refine_diff_density_min         -5.858
_refine_ls_extinction_coef       0.0154(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0578
_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)+(0.1217P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                2230
_reflns_number_total             3411
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb5383.cif
_cod_data_source_block           I
_cod_original_cell_volume        1228.0(4)
_cod_original_sg_symbol_Hall     ' -P 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225854
_cod_database_fobs_code          2225854
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 0.47863(3) 0.12876(4) 0.35712(3) 0.02848(19) Uani d . 1 . .
O O11 0.3570(7) -0.0031(8) 0.4636(8) 0.0413(18) Uani d . 1 . .
C C22 0.6620(9) 0.3784(10) 0.5171(10) 0.034(2) Uani d . 1 . .
O O21 0.4811(9) 0.2586(8) 0.5220(8) 0.0399(18) Uani d . 1 . .
N N21 0.6655(8) 0.2972(9) 0.4344(8) 0.0327(18) Uani d . 1 . .
C C12 0.1581(9) 0.1152(9) 0.3625(10) 0.0299(19) Uani d . 1 . .
C C13 0.0296(11) 0.1383(11) 0.3473(11) 0.039(2) Uani d . 1 . .
H H13 -0.0039 0.0957 0.3980 0.047 Uiso calc R 1 . .
C C27 0.5599(12) 0.3532(11) 0.5717(12) 0.040(2) Uani d . 1 . .
N N22 0.8312(12) 0.5089(11) 0.5106(13) 0.059(3) Uani d . 1 . .
C C26 0.7546(11) 0.3203(12) 0.3893(12) 0.039(2) Uani d . 1 . .
H H26 0.7616 0.2642 0.3303 0.047 Uiso calc R 1 . .
N N11 0.2083(9) 0.1695(10) 0.2906(9) 0.0362(19) Uani d . 1 . .
C C16 0.1307(12) 0.2491(12) 0.2013(12) 0.045(3) Uani d . 1 . .
H H16 0.1628 0.2889 0.1481 0.054 Uiso calc R 1 . .
C C23 0.7440(13) 0.4853(12) 0.5559(14) 0.050(3) Uani d . 1 . .
H H23 0.7365 0.5409 0.6151 0.060 Uiso calc R 1 . .
O O1 0.4080(11) 0.3287(10) 0.2149(9) 0.056(2) Uani d D 1 . .
H H1 0.378(11) 0.402(7) 0.218(10) 0.084 Uiso d D 1 . .
H H2 0.385(8) 0.312(13) 0.138(3) 0.084 Uiso d D 1 . .
O O12 0.2045(8) -0.0170(9) 0.5394(8) 0.0445(19) Uani d . 1 . .
C C17 0.2455(9) 0.0251(9) 0.4646(9) 0.0275(18) Uani d . 1 . .
N N12 -0.0479(10) 0.2225(11) 0.2591(11) 0.050(3) Uani d . 1 . .
C C15 0.0023(12) 0.2730(13) 0.1871(12) 0.047(3) Uani d . 1 . .
H H15 -0.0500 0.3278 0.1230 0.056 Uiso calc R 1 . .
C C25 0.8376(14) 0.4253(14) 0.4272(15) 0.055(3) Uani d . 1 . .
H H25 0.8995 0.4379 0.3935 0.066 Uiso calc R 1 . .
O O22 0.5643(12) 0.4168(10) 0.6610(9) 0.054(2) 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
O21 Pb1 O11 . 3_656 81.6(3) ?
O21 Pb1 O1 . . 88.0(3) ?
O11 Pb1 O1 3_656 . 152.2(3) n
O21 Pb1 O11 . . 75.0(3) ?
O11 Pb1 O11 3_656 . 70.5(3) n
O1 Pb1 O11 . . 131.3(3) ?
O21 Pb1 N21 . . 65.4(3) n
O11 Pb1 N21 3_656 . 81.6(3) ?
O1 Pb1 N21 . . 70.6(3) ?
O11 Pb1 N21 . . 134.3(3) ?
O21 Pb1 N11 . . 78.0(3) ?
O11 Pb1 N11 3_656 . 129.8(3) ?
O1 Pb1 N11 . . 72.0(3) n
O11 Pb1 N11 . . 60.1(3) n
N21 Pb1 N11 . . 127.6(3) ?
O21 Pb1 O22 . 4_565 149.2(3) ?
O11 Pb1 O22 3_656 4_565 102.5(3) n
O1 Pb1 O22 . 4_565 74.3(3) n
O11 Pb1 O22 . 4_565 135.4(3) ?
N21 Pb1 O22 . 4_565 84.8(3) ?
N11 Pb1 O22 . 4_565 118.2(3) ?
C17 O11 Pb1 . 3_656 119.3(6) ?
C17 O11 Pb1 . . 125.8(6) ?
Pb1 O11 Pb1 3_656 . 109.5(3) ?
N21 C22 C23 . . 123.2(11) ?
N21 C22 C27 . . 116.9(9) ?
C23 C22 C27 . . 119.9(11) ?
C27 O21 Pb1 . . 126.1(7) ?
C22 N21 C26 . . 115.8(10) ?
C22 N21 Pb1 . . 116.0(6) ?
C26 N21 Pb1 . . 127.7(8) ?
N11 C12 C13 . . 121.9(10) ?
N11 C12 C17 . . 117.9(8) ?
C13 C12 C17 . . 120.2(9) ?
N12 C13 C12 . . 120.6(11) ?
N12 C13 H13 . . 119.7 ?
C12 C13 H13 . . 119.7 ?
O22 C27 O21 . . 125.7(12) ?
O22 C27 C22 . . 119.1(10) ?
O21 C27 C22 . . 115.1(10) ?
C23 N22 C25 . . 116.5(11) ?
N21 C26 C25 . . 121.9(11) ?
N21 C26 H26 . . 119.0 ?
C25 C26 H26 . . 119.0 ?
C12 N11 C16 . . 117.4(10) ?
C12 N11 Pb1 . . 116.4(6) ?
C16 N11 Pb1 . . 125.8(8) ?
N11 C16 C15 . . 120.5(11) ?
N11 C16 H16 . . 119.8 ?
C15 C16 H16 . . 119.8 ?
N22 C23 C22 . . 121.0(13) ?
N22 C23 H23 . . 119.5 ?
C22 C23 H23 . . 119.5 ?
Pb1 O1 H1 . . 137(10) ?
Pb1 O1 H2 . . 113(9) ?
H1 O1 H2 . . 106(3) ?
O12 C17 O11 . . 124.8(9) ?
O12 C17 C12 . . 118.7(9) ?
O11 C17 C12 . . 116.5(8) ?
C15 N12 C13 . . 116.5(10) ?
N12 C15 C16 . . 122.9(11) ?
N12 C15 H15 . . 118.5 ?
C16 C15 H15 . . 118.5 ?
N22 C25 C26 . . 121.5(11) ?
N22 C25 H25 . . 119.2 ?
C26 C25 H25 . . 119.2 ?
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 O21 . 2.341(7) y
Pb1 O11 3_656 2.508(7) y
Pb1 O1 . 2.573(9) y
Pb1 O11 . 2.572(8) y
Pb1 N21 . 2.577(9) y
Pb1 N11 . 2.807(9) y
Pb1 O22 4_565 2.856(8) y
O11 C17 . 1.277(12) ?
O11 Pb1 3_656 2.508(7) ?
C22 N21 . 1.295(14) ?
C22 C23 . 1.389(15) ?
C22 C27 . 1.532(16) ?
O21 C27 . 1.285(14) ?
N21 C26 . 1.318(12) ?
C12 N11 . 1.310(13) ?
C12 C13 . 1.385(13) ?
C12 C17 . 1.513(13) ?
C13 N12 . 1.357(15) ?
C13 H13 . 0.9300 ?
C27 O22 . 1.217(15) ?
N22 C23 . 1.302(17) ?
N22 C25 . 1.328(19) ?
C26 C25 . 1.378(18) ?
C26 H26 . 0.9300 ?
N11 C16 . 1.334(14) ?
C16 C15 . 1.388(17) ?
C16 H16 . 0.9300 ?
C23 H23 . 0.9300 ?
O1 H1 . 0.84(2) ?
O1 H2 . 0.84(2) ?
O12 C17 . 1.219(12) ?
N12 C15 . 1.295(17) ?
C15 H15 . 0.9300 ?
C25 H25 . 0.9300 ?
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
O1 H2 O21 4_565 0.84(2) 2.17(5) 2.837(13) 136(7)
O1 H1 O22 3_666 0.84(2) 2.29(5) 2.969(15) 139(7)
O1 H1 O12 4_565 0.84(2) 2.49(7) 3.056(13) 126(7)
