#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/65/2206592.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_2206592
loop_
_publ_author_name
'Deng, Qian-Jun'
'Liu, Zhuang-Tian'
'Zeng, Ming-Hua'
_publ_section_title
;
 Bis(imidazolium)
 diaquabis(pyridine-2,5-dicarboxylato-κ²N,O)cobaltate(II)
 tetrahydrate
;
_journal_coeditor_code           WW6403
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1514
_journal_page_last               m1516
_journal_paper_doi               10.1107/S1600536805021380
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'(C3 H5 N2)2 [Co (C7 H3 N O4)2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         '2C3 H5 N2 +, C14 H10 Co N2 O10 2-, 4H2 O'
_chemical_formula_sum            'C20 H28 Co N6 O14'
_chemical_formula_weight         635.41
_chemical_name_systematic
;
Bis(imidazolium) diaquabis(pyridine-2,5-dicarboxylato-κ²N,O)cobaltate(II)
tetrahydrate
;
_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                97.70(3)
_cell_angle_beta                 116.80(3)
_cell_angle_gamma                93.26(3)
_cell_formula_units_Z            1
_cell_length_a                   8.844(5)
_cell_length_b                   9.062(4)
_cell_length_c                   9.635(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7
_cell_measurement_theta_min      2
_cell_volume                     677.0(6)
_computing_cell_refinement       'R3m Software'
_computing_data_collection       'R3m Software (Siemens, 1990)'
_computing_data_reduction        'R3m Software'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens R3m'
_diffrn_measurement_method       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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3153
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.8198
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             329
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.510
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0526
_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)+(0.0964P)²+0.3143P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                2532
_reflns_number_total             2959
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww6403.cif
_cod_data_source_block           I
_cod_database_code               2206592
_cod_database_fobs_code          2206592
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
Co1 0.0000 1.0000 0.0000 0.02994(19) Uani d S 1 Co
C1 0.2736(3) 0.8200(3) 0.0206(3) 0.0299(5) Uani d . 1 C
C2 0.4307(3) 0.7754(3) 0.0503(3) 0.0329(6) Uani d . 1 C
H2A 0.4375 0.6804 0.0049 0.039 Uiso calc R 1 H
C3 0.5788(3) 0.8748(3) 0.1494(3) 0.0321(6) Uani d . 1 C
H3B 0.6856 0.8467 0.1710 0.038 Uiso calc R 1 H
C4 0.5652(3) 1.0167(3) 0.2156(3) 0.0294(5) Uani d . 1 C
C5 0.4020(3) 1.0539(3) 0.1756(3) 0.0311(5) Uani d . 1 C
H5A 0.3920 1.1494 0.2172 0.037 Uiso calc R 1 H
C6 0.1052(3) 0.7173(3) -0.0814(3) 0.0327(6) Uani d . 1 C
C7 0.7189(3) 1.1315(3) 0.3274(3) 0.0319(6) Uani d . 1 C
C8 0.7564(5) 0.5958(4) 0.3782(5) 0.0538(8) Uani d . 1 C
H8A 0.8088 0.5334 0.3334 0.065 Uiso calc R 1 H
C9 0.5654(4) 0.6883(5) 0.4383(5) 0.0542(9) Uani d . 1 C
H9A 0.4629 0.7005 0.4409 0.065 Uiso calc R 1 H
C10 0.7137(5) 0.7796(4) 0.5225(4) 0.0519(8) Uani d . 1 C
H10A 0.7332 0.8666 0.5947 0.062 Uiso calc R 1 H
N1 0.2578(3) 0.9595(2) 0.0800(3) 0.0301(5) Uani d . 1 N
N2 0.8303(3) 0.7213(3) 0.4826(3) 0.0468(6) Uani d . 1 N
H2B 0.9351 0.7598 0.5194 0.056 Uiso calc R 1 H
N3 0.5929(4) 0.5746(3) 0.3483(4) 0.0511(7) Uani d . 1 N
H3A 0.5177 0.5013 0.2831 0.061 Uiso calc R 1 H
O1 -0.0304(2) 0.7744(2) -0.1042(2) 0.0361(4) Uani d . 1 O
O2 0.1123(3) 0.5860(2) -0.1318(3) 0.0467(5) Uani d . 1 O
O3 0.8647(3) 1.0970(3) 0.3553(3) 0.0483(6) Uani d . 1 O
O4 0.6911(3) 1.2515(2) 0.3855(3) 0.0505(6) Uani d . 1 O
O1W 0.0070(3) 0.9328(3) 0.2012(3) 0.0440(5) Uani d . 1 O
H1A -0.040(6) 0.967(5) 0.236(6) 0.066 Uiso d . 1 H
H1B 0.024(6) 0.843(5) 0.219(5) 0.066 Uiso d . 1 H
O2W 0.1152(4) 0.6748(3) 0.2941(4) 0.0704(9) Uani d . 1 O
H2C 0.174(8) 0.686(6) 0.408(8) 0.106 Uiso d . 1 H
H2D 0.056(8) 0.592(7) 0.256(7) 0.106 Uiso d . 1 H
O3W 0.3018(3) 0.4042(3) 0.0960(4) 0.0625(8) Uani d . 1 O
H3C 0.217(7) 0.357(6) 0.113(6) 0.094 Uiso d . 1 H
H3D 0.249(8) 0.457(7) 0.046(7) 0.094 Uiso d . 1 H
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'
Co Co 0.3494 0.9721 '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
O1W Co1 O1 . 2_575 89.90(9) yes
O1W Co1 O1 . . 90.10(9) yes
O1W Co1 N1 2_575 . 91.08(10) yes
O1W Co1 N1 . . 88.92(10) yes
O1W Co1 N1 . 2_575 91.07(10) yes
O1 Co1 N1 2_575 . 101.77(9) yes
O1 Co1 N1 . . 78.23(9) yes
N1 C1 C2 . . 122.3(2) ?
N1 C1 C6 . . 114.9(2) ?
C2 C1 C6 . . 122.9(2) ?
C1 C2 C3 . . 119.1(2) ?
C1 C2 H2A . . 120.4 ?
C3 C2 H2A . . 120.4 ?
C4 C3 C2 . . 119.4(2) ?
C4 C3 H3B . . 120.3 ?
C2 C3 H3B . . 120.3 ?
C5 C4 C3 . . 117.8(2) ?
C5 C4 C7 . . 119.0(2) ?
C3 C4 C7 . . 123.3(2) ?
N1 C5 C4 . . 123.6(2) ?
N1 C5 H5A . . 118.2 ?
C4 C5 H5A . . 118.2 ?
O2 C6 O1 . . 125.9(2) ?
O2 C6 C1 . . 117.7(2) ?
O1 C6 C1 . . 116.4(2) ?
O4 C7 O3 . . 125.1(3) ?
O4 C7 C4 . . 117.4(2) ?
O3 C7 C4 . . 117.4(2) ?
N2 C8 N3 . . 107.8(3) ?
N2 C8 H8A . . 126.1 ?
N3 C8 H8A . . 126.1 ?
C10 C9 N3 . . 107.2(3) ?
C10 C9 H9A . . 126.4 ?
N3 C9 H9A . . 126.4 ?
C9 C10 N2 . . 107.3(3) ?
C9 C10 H10A . . 126.3 ?
N2 C10 H10A . . 126.3 ?
C5 N1 C1 . . 117.8(2) ?
C5 N1 Co1 . . 128.65(18) ?
C1 N1 Co1 . . 113.50(17) ?
C8 N2 C10 . . 109.0(3) ?
C8 N2 H2B . . 125.5 ?
C10 N2 H2B . . 125.5 ?
C8 N3 C9 . . 108.7(3) ?
C8 N3 H3A . . 125.7 ?
C9 N3 H3A . . 125.7 ?
C6 O1 Co1 . . 116.87(17) ?
Co1 O1W H1A . . 120(4) ?
Co1 O1W H1B . . 122(3) ?
H1A O1W H1B . . 113(5) ?
H2C O2W H2D . . 109(5) ?
H3C O3W H3D . . 97(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1W 2.085(2) yes
Co1 O1 2.098(2) yes
Co1 N1 2.124(2) yes
C1 N1 1.358(3) ?
C1 C2 1.383(4) ?
C1 C6 1.526(4) ?
C2 C3 1.395(4) ?
C2 H2A 0.9300 ?
C3 C4 1.393(4) ?
C3 H3B 0.9300 ?
C4 C5 1.390(4) ?
C4 C7 1.520(4) ?
C5 N1 1.347(3) ?
C5 H5A 0.9300 ?
C6 O2 1.240(3) ?
C6 O1 1.272(3) ?
C7 O4 1.245(3) ?
C7 O3 1.260(3) ?
C8 N2 1.322(5) ?
C8 N3 1.338(5) ?
C8 H8A 0.9300 ?
C9 C10 1.342(5) ?
C9 N3 1.361(5) ?
C9 H9A 0.9300 ?
C10 N2 1.362(4) ?
C10 H10A 0.9300 ?
N2 H2B 0.8600 ?
N3 H3A 0.8600 ?
O1W H1A 0.70(5) ?
O1W H1B 0.86(5) ?
O2W H2C 0.97(6) ?
O2W H2D 0.82(7) ?
O3W H3C 0.93(6) ?
O3W H3D 0.75(6) ?
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
_geom_hbond_publ_flag
O1W H1A O3 1_455 0.70(5) 2.01(5) 2.703(3) 169(5) yes
O1W H1B O2W . 0.86(5) 1.85(5) 2.688(4) 166(4) yes
O2W H2C O4 2_676 0.97(6) 1.78(7) 2.731(4) 165(5) yes
O2W H2D O2 2_565 0.82(7) 1.96(7) 2.777(4) 169(6) yes
O3W H3C O1 2_565 0.93(6) 1.94(6) 2.855(4) 167(5) yes
O3W H3D O2 . 0.75(6) 2.14(6) 2.882(4) 168(6) yes
N2 H2B O3 2_776 0.86 1.92 2.726(4) 157 yes
N3 H3A O3W . 0.86 1.99 2.797(4) 156 yes
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
N1 C1 C2 C3 . 2.4(4)
C6 C1 C2 C3 . -177.9(3)
C1 C2 C3 C4 . -0.2(4)
C2 C3 C4 C5 . -1.7(4)
C2 C3 C4 C7 . 178.7(2)
C3 C4 C5 N1 . 1.6(4)
C7 C4 C5 N1 . -178.7(2)
N1 C1 C6 O2 . -176.2(3)
C2 C1 C6 O2 . 4.1(4)
N1 C1 C6 O1 . 2.4(4)
C2 C1 C6 O1 . -177.3(3)
C5 C4 C7 O4 . 4.0(4)
C3 C4 C7 O4 . -176.4(3)
C5 C4 C7 O3 . -176.7(3)
C3 C4 C7 O3 . 3.0(4)
N3 C9 C10 N2 . 0.3(4)
C4 C5 N1 C1 . 0.4(4)
C4 C5 N1 Co1 . -177.45(19)
C2 C1 N1 C5 . -2.5(4)
C6 C1 N1 C5 . 177.7(2)
C2 C1 N1 Co1 . 175.7(2)
C6 C1 N1 Co1 . -4.0(3)
O1W Co1 N1 C5 2_575 91.7(2)
O1W Co1 N1 C5 . -88.3(2)
O1 Co1 N1 C5 2_575 1.3(2)
O1 Co1 N1 C5 . -178.7(2)
O1W Co1 N1 C1 2_575 -86.3(2)
O1W Co1 N1 C1 . 93.7(2)
O1 Co1 N1 C1 2_575 -176.64(18)
O1 Co1 N1 C1 . 3.36(18)
N3 C8 N2 C10 . 1.2(4)
C9 C10 N2 C8 . -0.9(4)
N2 C8 N3 C9 . -1.0(4)
C10 C9 N3 C8 . 0.4(4)
O2 C6 O1 Co1 . 179.1(2)
C1 C6 O1 Co1 . 0.6(3)
O1W Co1 O1 C6 2_575 89.0(2)
O1W Co1 O1 C6 . -91.0(2)
N1 Co1 O1 C6 . -2.1(2)
N1 Co1 O1 C6 2_575 177.9(2)
