#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/27/2232779.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_2232779
loop_
_publ_author_name
'Boyko, Alexander N.'
'Golenya, Irina A.'
'Izotova, Yulia A.'
'Haukka, Matti'
'Prisyazhnaya, Elena V.'
_publ_section_title
;
 Poly[di-μ₂-aqua-μ₅-(pyridine-2,6-dicarboxylato)-μ₃-(pyridine-2,6-dicarboxylato)-cobalt(II)disodium]
;
_journal_coeditor_code           HY2486
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1782
_journal_page_last               m1783
_journal_paper_doi               10.1107/S1600536811048252
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co Na2 (C7 H3 N O4)2 (H2 O)2]'
_chemical_formula_moiety         'C14 H10 Co N2 Na2 O10'
_chemical_formula_sum            'C14 H10 Co N2 Na2 O10'
_chemical_formula_weight         471.15
_chemical_name_systematic
;
Poly[di-μ₂-aqua-μ₅-(pyridine-2,6-dicarboxylato)-μ₃-(pyridine-
2,6-dicarboxylato)-cobalt(II)disodium]
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9540(3)
_cell_length_b                   13.2187(3)
_cell_length_c                   15.1475(3)
_cell_measurement_reflns_used    14413
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1592.63(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22979
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_correction_T_min  0.8258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.322
_refine_ls_abs_structure_details 'Flack (1983), 1749 Friedel pairs'
_refine_ls_abs_structure_Flack   0.017(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0227
_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)+(0.0247P)²+0.3490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                3388
_reflns_number_total             3640
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2486.cif
_cod_data_source_block           I
_cod_database_code               2232779
_cod_database_fobs_code          2232779
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, 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
_atom_site_symmetry_multiplicity
Co Co1 -0.05451(3) -0.010675(17) 0.25557(2) 0.01076(7) Uani d . 1 1
Na Na1 -0.07221(11) 0.28100(6) 0.49042(5) 0.01966(19) Uani d . 1 1
Na Na2 -0.26548(10) 0.06445(7) 0.52208(6) 0.0212(2) Uani d . 1 1
O O1 -0.24152(18) 0.05370(10) 0.34732(9) 0.0146(3) Uani d . 1 1
O O2 0.1115(2) 0.00400(10) 0.14651(11) 0.0163(4) Uani d . 1 1
O O3 0.1244(2) -0.00136(10) 0.36280(10) 0.0141(3) Uani d . 1 1
O O4 -0.21550(19) -0.09844(10) 0.16519(10) 0.0158(3) Uani d . 1 1
O O5 -0.30854(18) 0.20122(10) 0.41058(9) 0.0162(3) Uani d . 1 1
O O6 0.18157(18) 0.10750(11) 0.03583(9) 0.0183(3) Uani d . 1 1
O O7 0.23230(19) -0.09423(11) 0.47351(9) 0.0180(3) Uani d . 1 1
O O8 -0.2541(2) -0.25677(11) 0.11508(9) 0.0188(3) Uani d . 1 1
O O9 -0.55522(17) 0.05090(11) 0.53885(10) 0.0160(3) Uani d . 1 1
H H9A -0.5987 0.0012 0.5123 0.024 Uiso d R 1 1
H H9B -0.6164 0.0561 0.5846 0.024 Uiso d R 1 1
O O10 0.01645(19) 0.11758(10) 0.49835(10) 0.0164(3) Uani d . 1 1
H H10A 0.0629 0.0876 0.4541 0.025 Uiso d R 1 1
H H10B 0.0745 0.0949 0.5461 0.025 Uiso d R 1 1
N N1 -0.0691(2) 0.13931(12) 0.22358(10) 0.0109(3) Uani d . 1 1
N N2 -0.0236(2) -0.15690(12) 0.29271(11) 0.0112(3) Uani d . 1 1
C C1 -0.1490(2) 0.20301(14) 0.27769(12) 0.0120(4) Uani d . 1 1
C C2 -0.2419(2) 0.14940(15) 0.35081(13) 0.0126(4) Uani d . 1 1
C C3 -0.1404(2) 0.30715(14) 0.26432(15) 0.0158(4) Uani d . 1 1
H H3 -0.1946 0.3527 0.3036 0.019 Uiso calc R 1 1
C C4 -0.0503(3) 0.34270(15) 0.19181(14) 0.0153(4) Uani d . 1 1
H H4 -0.0429 0.4134 0.1812 0.018 Uiso calc R 1 1
C C5 0.0285(3) 0.27576(16) 0.13529(14) 0.0151(4) Uani d . 1 1
H H5 0.0879 0.2992 0.0849 0.018 Uiso calc R 1 1
C C6 0.0182(3) 0.17334(15) 0.15435(13) 0.0121(4) Uani d . 1 1
C C7 0.1110(3) 0.09008(15) 0.10677(13) 0.0136(4) Uani d . 1 1
C C8 0.0704(3) -0.17728(16) 0.36365(13) 0.0121(4) Uani d . 1 1
C C9 0.1491(3) -0.08438(15) 0.40480(13) 0.0136(4) Uani d . 1 1
C C10 0.0974(3) -0.27604(15) 0.39155(14) 0.0153(4) Uani d . 1 1
H H10 0.1621 -0.2900 0.4429 0.018 Uiso calc R 1 1
C C11 0.0270(3) -0.35394(15) 0.34216(13) 0.0149(4) Uani d . 1 1
H H11 0.0446 -0.4222 0.3594 0.018 Uiso calc R 1 1
C C12 -0.0685(2) -0.33259(14) 0.26795(15) 0.0148(4) Uani d . 1 1
H H12 -0.1161 -0.3854 0.2335 0.018 Uiso calc R 1 1
C C13 -0.0928(2) -0.23155(14) 0.24533(14) 0.0120(4) Uani d . 1 1
C C14 -0.1961(3) -0.19475(15) 0.16881(13) 0.0131(4) Uani d . 1 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'
Na Na 0.0362 0.0249 '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
N2 Co1 N1 . . 175.53(7)
N2 Co1 O2 . . 103.15(6)
N1 Co1 O2 . . 76.24(6)
N2 Co1 O3 . . 76.47(6)
N1 Co1 O3 . . 99.21(6)
O2 Co1 O3 . . 99.78(5)
N2 Co1 O4 . . 75.00(6)
N1 Co1 O4 . . 109.28(6)
O2 Co1 O4 . . 85.76(6)
O3 Co1 O4 . . 151.46(5)
N2 Co1 O1 . . 105.94(6)
N1 Co1 O1 . . 74.76(6)
O2 Co1 O1 . . 150.91(5)
O3 Co1 O1 . . 87.05(6)
O4 Co1 O1 . . 101.68(5)
O10 Na1 O9 . 4 149.94(7)
O10 Na1 O8 . 3_455 86.51(6)
O9 Na1 O8 4 3_455 89.09(5)
O10 Na1 O5 . 4 81.42(6)
O9 Na1 O5 4 4 90.82(5)
O8 Na1 O5 3_455 4 155.57(6)
O10 Na1 O5 . . 81.75(5)
O9 Na1 O5 4 . 126.98(6)
O8 Na1 O5 3_455 . 81.84(5)
O5 Na1 O5 4 . 116.98(6)
O9 Na2 O10 . . 166.94(6)
O9 Na2 O6 . 2 101.24(6)
O10 Na2 O6 . 2 91.77(5)
O9 Na2 O2 . 2 112.79(7)
O10 Na2 O2 . 2 75.58(6)
O6 Na2 O2 2 2 55.47(5)
O9 Na2 O5 . . 89.64(6)
O10 Na2 O5 . . 79.24(5)
O6 Na2 O5 2 . 142.14(6)
O2 Na2 O5 2 . 149.95(6)
O9 Na2 O1 . . 100.12(6)
O10 Na2 O1 . . 78.32(5)
O6 Na2 O1 2 . 90.91(5)
O2 Na2 O1 2 . 135.93(6)
O5 Na2 O1 . . 51.32(4)
O9 Na2 O8 . 3_455 93.80(6)
O10 Na2 O8 . 3_455 76.74(5)
O6 Na2 O8 2 3_455 139.38(6)
O2 Na2 O8 2 3_455 83.92(6)
O5 Na2 O8 . 3_455 74.50(5)
O1 Na2 O8 . 3_455 123.43(5)
C7 Na2 O8 2 3_455 112.28(6)
C2 O1 Co1 . . 114.40(12)
C2 O1 Na2 . . 84.54(11)
Co1 O1 Na2 . . 134.13(6)
C7 O2 Co1 . . 116.28(13)
C7 O2 Na2 . 2_554 88.16(12)
Co1 O2 Na2 . 2_554 152.28(7)
C9 O3 Co1 . . 115.10(13)
C14 O4 Co1 . . 115.19(13)
C2 O5 Na1 . 4_455 140.98(13)
C2 O5 Na1 . . 105.37(12)
Na1 O5 Na1 4_455 . 111.79(6)
C2 O5 Na2 . . 92.00(12)
Na1 O5 Na2 4_455 . 81.48(5)
Na1 O5 Na2 . . 82.74(5)
C7 O6 Na2 . 2_554 91.47(12)
C14 O8 Na1 . 3_444 126.37(13)
C14 O8 Na2 . 3_444 151.48(14)
Na1 O8 Na2 3_444 3_444 78.94(5)
Na2 O9 Na1 . 4_455 87.13(5)
Na2 O9 H9A . . 114.5
Na1 O9 H9A 4_455 . 124.4
Na2 O9 H9B . . 130.6
Na1 O9 H9B 4_455 . 98.4
H9A O9 H9B . . 102.5
Na1 O10 Na2 . . 89.78(6)
Na1 O10 H10A . . 121.9
Na2 O10 H10A . . 112.7
Na1 O10 H10B . . 120.8
Na2 O10 H10B . . 105.1
H10A O10 H10B . . 104.4
C6 N1 C1 . . 121.13(17)
C6 N1 Co1 . . 118.90(13)
C1 N1 Co1 . . 119.52(13)
C8 N2 C13 . . 120.84(17)
C8 N2 Co1 . . 118.88(14)
C13 N2 Co1 . . 120.26(13)
N1 C1 C3 . . 120.67(17)
N1 C1 C2 . . 112.81(17)
C3 C1 C2 . . 126.53(17)
O5 C2 O1 . . 125.27(18)
O5 C2 C1 . . 118.75(17)
O1 C2 C1 . . 115.96(17)
C1 C3 C4 . . 118.24(18)
C1 C3 H3 . . 120.9
C4 C3 H3 . . 120.9
C5 C4 C3 . . 120.39(19)
C5 C4 H4 . . 119.8
C3 C4 H4 . . 119.8
C4 C5 C6 . . 118.01(19)
C4 C5 H5 . . 121.0
C6 C5 H5 . . 121.0
N1 C6 C5 . . 121.52(19)
N1 C6 C7 . . 112.57(17)
C5 C6 C7 . . 125.74(19)
O6 C7 O2 . . 124.80(19)
O6 C7 C6 . . 120.17(18)
O2 C7 C6 . . 115.02(17)
N2 C8 C10 . . 121.37(19)
N2 C8 C9 . . 113.53(17)
C10 C8 C9 . . 125.01(19)
O7 C9 O3 . . 125.97(19)
O7 C9 C8 . . 118.77(18)
O3 C9 C8 . . 115.24(17)
C8 C10 C11 . . 118.04(19)
C8 C10 H10 . . 121.0
C11 C10 H10 . . 121.0
C12 C11 C10 . . 120.42(18)
C12 C11 H11 . . 119.8
C10 C11 H11 . . 119.8
C11 C12 C13 . . 118.10(19)
C11 C12 H12 . . 121.0
C13 C12 H12 . . 121.0
N2 C13 C12 . . 121.21(18)
N2 C13 C14 . . 113.58(16)
C12 C13 C14 . . 125.21(18)
O8 C14 O4 . . 125.53(19)
O8 C14 C13 . . 119.63(17)
O4 C14 C13 . . 114.84(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 N2 . 2.0281(16)
Co1 N1 . 2.0443(17)
Co1 O2 . 2.1235(17)
Co1 O3 . 2.1631(17)
Co1 O4 . 2.2044(15)
Co1 O1 . 2.2065(14)
Na1 O10 . 2.2757(16)
Na1 O9 4 2.3439(16)
Na1 O8 3_455 2.3924(16)
Na1 O5 4 2.4324(16)
Na1 O5 . 2.4715(16)
Na2 O9 . 2.3254(16)
Na2 O10 . 2.3772(17)
Na2 O6 2 2.3780(17)
Na2 O2 2 2.4232(18)
Na2 O5 . 2.4978(16)
Na2 O1 . 2.6579(17)
Na2 O8 3_455 2.7557(17)
O1 C2 . 1.266(2)
O2 C7 . 1.287(2)
O3 C9 . 1.284(2)
O4 C14 . 1.284(2)
O5 C2 . 1.253(2)
O6 C7 . 1.234(2)
O7 C9 . 1.240(2)
O8 C14 . 1.244(2)
O9 H9A . 0.8440
O9 H9B . 0.8492
O10 H10A . 0.8618
O10 H10B . 0.9091
N1 C6 . 1.336(3)
N1 C1 . 1.336(2)
N2 C8 . 1.337(3)
N2 C13 . 1.339(2)
C1 C3 . 1.393(3)
C1 C2 . 1.508(3)
C3 C4 . 1.393(3)
C3 H3 . 0.9500
C4 C5 . 1.382(3)
C4 H4 . 0.9500
C5 C6 . 1.387(3)
C5 H5 . 0.9500
C6 C7 . 1.508(3)
C8 C10 . 1.389(3)
C8 C9 . 1.513(3)
C10 C11 . 1.391(3)
C10 H10 . 0.9500
C11 C12 . 1.386(3)
C11 H11 . 0.9500
C12 C13 . 1.392(3)
C12 H12 . 0.9500
C13 C14 . 1.502(3)
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
O9 H9A O7 1_455 0.84 1.94 2.742(2) 159
O9 H9B O4 2_455 0.85 1.90 2.717(2) 162
O10 H10A O3 . 0.86 1.88 2.725(2) 166
O10 H10B O4 2 0.91 2.12 2.993(2) 159
