#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/69/2216970.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_2216970
loop_
_publ_author_name
'Mustafa Tombul'
'Kutalmis Güven'
'Ingrid Svoboda'
_publ_section_title
;Poly[diaqua(μ₂-3-carboxypyrazine-2-carboxylato)(μ₂-pyrazine-2,3-dicarboxylic
 acid)potassium(I)]
;
_journal_coeditor_code           CF2158
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m246
_journal_page_last               m247
_journal_paper_doi               10.1107/S1600536807066202
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[K (C6 H3 N2 O4) (C6 H4 N2 O4) (H2 O)2]'
_chemical_formula_moiety         'C12 H11 K N4 O10'
_chemical_formula_sum            'C12 H11 K N4 O10'
_chemical_formula_weight         410.35
_chemical_name_systematic
;
Poly[diaqua(μ₂-3-carboxypyrazine-2-carboxylato)(μ₂-pyrazine-
2,3-dicarboxylic acid)potassium(I)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.39(2)
_cell_angle_beta                 81.180(10)
_cell_angle_gamma                64.24(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4171(11)
_cell_length_b                   8.0252(12)
_cell_length_c                   8.1153(13)
_cell_measurement_reflns_used    2574
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.684
_cell_volume                     404.46(14)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2006).
;
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      303(2)
_diffrn_detector_area_resol_mean 8.4012
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
with Sapphire CCD detector
;
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4541
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.8579
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[using a multifaceted crystal model based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             210
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.243
_refine_ls_extinction_coef       0.043(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1639
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0293
_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)+(0.0664P)²+0.1925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                1357
_reflns_number_total             1639
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2158.cif
_cod_data_source_block           I
_cod_original_cell_volume        404.43(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2216970
_cod_database_fobs_code          2216970
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C C1 0.2243(2) -0.0442(2) 0.6857(2) 0.0317(4) Uani d . 1
H H1A 0.0951 -0.0140 0.6552 0.038 Uiso calc R 1
C C2 0.3500(2) -0.2386(2) 0.7694(2) 0.0335(4) Uani d . 1
H H2 0.3046 -0.3358 0.7905 0.040 Uiso calc R 1
C C3 0.5925(2) -0.1443(2) 0.78702(18) 0.0249(3) Uani d . 1
C C4 0.4681(2) 0.0507(2) 0.69820(18) 0.0236(3) Uani d . 1
C C5 0.5421(2) 0.2104(2) 0.6487(2) 0.0289(3) Uani d . 1
C C6 0.8033(2) -0.2156(2) 0.8493(2) 0.0277(3) Uani d . 1
N N1 0.28268(17) 0.10040(18) 0.64756(16) 0.0281(3) Uani d . 1
N N2 0.53451(18) -0.28984(18) 0.82048(17) 0.0310(3) Uani d . 1
O O1 0.41860(17) 0.38402(16) 0.56448(17) 0.0394(3) Uani d . 1
H H1 0.476(7) 0.455(6) 0.533(5) 0.039(11) Uiso d P 0.50
O O2 0.94651(16) -0.29530(18) 0.77161(16) 0.0392(3) Uani d . 1
O O3 0.14687(17) 0.66521(18) 0.15762(17) 0.0407(3) Uani d D 1
H H3A 0.195(3) 0.727(3) 0.190(3) 0.057(6) Uiso d D 1
H H3B 0.245(2) 0.563(2) 0.149(3) 0.057(6) Uiso d D 1
O O4 0.71570(17) 0.16296(17) 0.68558(19) 0.0476(4) Uani d . 1
O O5 0.80518(19) -0.1943(2) 1.00104(17) 0.0504(4) Uani d . 1
H H5 0.925(4) -0.241(4) 1.038(3) 0.065(7) Uiso d . 1
K K1 0.0000 0.5000 0.5000 0.0471(2) Uani d S 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'
K K 0.2009 0.2494 '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
N1 C1 C2 . . 121.91(13)
N1 C1 H1A . . 119.0
C2 C1 H1A . . 119.0
N2 C2 C1 . . 121.64(14)
N2 C2 H2 . . 119.2
C1 C2 H2 . . 119.2
N2 C3 C4 . . 121.58(13)
N2 C3 C6 . . 113.19(12)
C4 C3 C6 . . 125.20(13)
N1 C4 C3 . . 121.03(13)
N1 C4 C5 . . 118.15(13)
C3 C4 C5 . . 120.76(13)
O4 C5 O1 . . 125.67(14)
O4 C5 C4 . . 118.05(13)
O1 C5 C4 . . 116.21(13)
O2 C6 O5 . . 126.25(14)
O2 C6 C3 . . 121.86(13)
O5 C6 C3 . . 111.63(13)
C1 N1 C4 . . 117.01(13)
C1 N1 K1 . . 119.50(9)
C4 N1 K1 . . 123.12(9)
C2 N2 C3 . . 116.78(13)
C5 O1 K1 . . 125.42(10)
C5 O1 H1 . . 109(3)
K1 O1 H1 . . 126(3)
C6 O2 K1 . 1_645 132.38(10)
K1 O3 H3A . . 96.3(15)
K1 O3 H3B . . 99.8(15)
H3A O3 H3B . . 106.6(13)
C6 O5 H5 . . 111.0(16)
N1 K1 N1 2_566 . 180.0
N1 K1 O3 2_566 2_566 107.16(4)
N1 K1 O3 . 2_566 72.84(4)
N1 K1 O3 2_566 . 72.84(4)
N1 K1 O3 . . 107.16(4)
O3 K1 O3 2_566 . 180.0
N1 K1 O1 2_566 2_566 55.92(4)
N1 K1 O1 . 2_566 124.08(4)
O3 K1 O1 2_566 2_566 76.02(4)
O3 K1 O1 . 2_566 103.98(4)
N1 K1 O1 2_566 . 124.08(4)
N1 K1 O1 . . 55.92(4)
O3 K1 O1 2_566 . 103.98(4)
O3 K1 O1 . . 76.02(4)
O1 K1 O1 2_566 . 180.0000(10)
N1 K1 O2 2_566 2_656 107.44(4)
N1 K1 O2 . 2_656 72.56(4)
O3 K1 O2 2_566 2_656 116.00(3)
O3 K1 O2 . 2_656 64.00(3)
O1 K1 O2 2_566 2_656 81.35(3)
O1 K1 O2 . 2_656 98.65(4)
N1 K1 O2 2_566 1_465 72.56(4)
N1 K1 O2 . 1_465 107.44(4)
O3 K1 O2 2_566 1_465 64.00(3)
O3 K1 O2 . 1_465 116.00(3)
O1 K1 O2 2_566 1_465 98.65(4)
O1 K1 O2 . 1_465 81.35(4)
O2 K1 O2 2_656 1_465 180.00(2)
N1 K1 H3A 2_566 . 70.6(3)
N1 K1 H3A . . 109.4(3)
O3 K1 H3A 2_566 . 164.1(2)
O3 K1 H3A . . 15.9(2)
O1 K1 H3A 2_566 . 112.9(3)
O1 K1 H3A . . 67.1(3)
O2 K1 H3A 2_656 . 79.1(2)
O2 K1 H3A 1_465 . 100.9(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
C1 N1 . 1.327(2) ?
C1 C2 . 1.383(2) ?
C1 H1A . 0.9300 ?
C2 N2 . 1.331(2) ?
C2 H2 . 0.9300 ?
C3 N2 . 1.3381(19) ?
C3 C4 . 1.392(2) ?
C3 C6 . 1.5097(19) ?
C4 N1 . 1.3397(18) ?
C4 C5 . 1.507(2) ?
C5 O4 . 1.2248(18) ?
C5 O1 . 1.2760(19) ?
C6 O2 . 1.1983(19) ?
C6 O5 . 1.3073(19) ?
N1 K1 . 2.8655(15) yes
O1 K1 . 2.8995(12) yes
O1 H1 . 0.80(4) ?
O3 K1 . 2.8771(15) yes
O3 H3A . 0.85(2) ?
O3 H3B . 0.848(9) ?
O5 H5 . 0.86(3) ?
K1 N1 2_566 2.8655(15) yes
K1 O3 2_566 2.8771(15) yes
K1 O1 2_566 2.8995(12) yes
K1 O2 2_656 3.0897(13) yes
K1 O2 1_465 3.0897(13) yes
K1 H3A . 3.09(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
O3 H3A O4 2_666 0.85(2) 1.899(10) 2.7334(17) 167(2)
O3 H3B N2 2_656 0.848(9) 2.035(10) 2.8701(19) 168(2)
O5 H5 O3 1_646 0.86(3) 1.76(3) 2.5994(17) 168(2)
O1 H1 O1 2_666 0.80(4) 1.68(4) 2.480(2) 171(5)
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_4
_geom_torsion
N1 C1 C2 N2 . 1.9(2)
N2 C3 C4 N1 . 2.1(2)
C6 C3 C4 N1 . 179.87(13)
N2 C3 C4 C5 . -174.99(13)
C6 C3 C4 C5 . 2.8(2)
N1 C4 C5 O4 . -175.63(14)
C3 C4 C5 O4 . 1.5(2)
N1 C4 C5 O1 . 1.5(2)
C3 C4 C5 O1 . 178.67(13)
N2 C3 C6 O2 . 74.92(18)
C4 C3 C6 O2 . -103.06(18)
N2 C3 C6 O5 . -99.65(16)
C4 C3 C6 O5 . 82.37(18)
C2 C1 N1 C4 . -1.8(2)
C2 C1 N1 K1 . -174.99(12)
C3 C4 N1 C1 . -0.1(2)
C5 C4 N1 C1 . 177.00(12)
C3 C4 N1 K1 . 172.82(10)
C5 C4 N1 K1 . -10.06(17)
C1 C2 N2 C3 . 0.0(2)
C4 C3 N2 C2 . -1.9(2)
C6 C3 N2 C2 . -179.99(12)
O4 C5 O1 K1 . -175.29(12)
C4 C5 O1 K1 . 7.78(19)
O5 C6 O2 K1 1_645 154.68(13)
C3 C6 O2 K1 1_645 -19.1(2)
C1 N1 K1 O3 2_566 61.01(11)
C4 N1 K1 O3 2_566 -111.76(11)
C1 N1 K1 O3 . -118.99(11)
C4 N1 K1 O3 . 68.24(11)
C1 N1 K1 O1 2_566 1.94(12)
C4 N1 K1 O1 2_566 -170.83(10)
C1 N1 K1 O1 . -178.06(12)
C4 N1 K1 O1 . 9.17(10)
C1 N1 K1 O2 2_656 -64.29(11)
C4 N1 K1 O2 2_656 122.94(11)
C1 N1 K1 O2 1_465 115.71(11)
C4 N1 K1 O2 1_465 -57.06(11)
C5 O1 K1 N1 2_566 171.23(11)
C5 O1 K1 N1 . -8.77(11)
C5 O1 K1 O3 2_566 48.85(13)
C5 O1 K1 O3 . -131.15(13)
C5 O1 K1 O2 2_656 -70.80(13)
C5 O1 K1 O2 1_465 109.20(13)
