#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/30/2203093.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_2203093
loop_
_publ_author_name
'Shiu, Kom-Bei'
'Yen, Chia-Hung'
'Liao, Fen-Ling'
'Wang, Sue-Lein'
_publ_section_title
;Hexaaquacobalt(II)
 trans-bis(η³-pyridine-2,6-dicarboxylato-κ³O,N,O')cobaltate(II)
 dihydrate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m35
_journal_page_last               m37
_journal_paper_doi               10.1107/S1600536803027491
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (H2 O)6] [Co (C7 H3 N O4)2], 2H2 O'
_chemical_formula_moiety         'H12 Co O6 2+, C14 H6 Co N2 O8 2-, (H2 O)2'
_chemical_formula_sum            'C14 H22 Co2 N2 O16'
_chemical_formula_weight         592.20
_chemical_name_systematic
;
Hexaaquacobalt(II) trans-bis(η³-pyridine-2,6-
dicarboxylato-κ³O,N,O')cobaltate(II) dihydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                108.694(11)
_cell_angle_beta                 99.900(12)
_cell_angle_gamma                98.089(13)
_cell_formula_units_Z            2
_cell_length_a                   8.258(6)
_cell_length_b                   11.615(8)
_cell_length_c                   12.873(9)
_cell_measurement_reflns_used    2061
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     1126.5(14)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0832
_diffrn_reflns_av_sigmaI/netI    0.1595
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11729
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.85633
_exptl_absorpt_correction_T_min  0.67755
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.840
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1887
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1003P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2278
_reflns_number_gt                2686
_reflns_number_total             5293
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob6327.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1126.6(13)
_cod_database_code               2203093
_cod_database_fobs_code          2203093
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 0.13678(14) 0.78395(10) 0.24512(8) 0.0333(3) Uani d . 1 Co
Co2 -0.5000 0.5000 0.5000 0.0289(4) Uani d S 1 Co
Co3 0.5000 1.0000 0.0000 0.0474(5) Uani d S 1 Co
O1 0.3179(7) 0.9405(5) 0.2462(4) 0.0358(13) Uani d . 1 O
O2 0.4653(7) 1.1293(5) 0.3514(4) 0.0440(15) Uani d . 1 O
O3 -0.0326(7) 0.7051(5) 0.3210(5) 0.0462(15) Uani d . 1 O
O4 -0.0792(7) 0.7114(6) 0.4888(5) 0.0510(16) Uani d . 1 O
O5 0.3134(7) 0.6686(5) 0.2785(4) 0.0427(14) Uani d . 1 O
O6 0.4431(8) 0.5230(6) 0.1907(5) 0.0534(17) Uani d . 1 O
O7 -0.0548(7) 0.8293(5) 0.1319(5) 0.0448(15) Uani d . 1 O
O8 -0.1324(8) 0.8077(6) -0.0488(5) 0.0580(18) Uani d . 1 O
O9 -0.6308(8) 0.6407(5) 0.4862(4) 0.0477(16) Uani d . 1 O
O10 -0.6450(7) 0.4713(5) 0.6125(4) 0.0457(15) Uani d . 1 O
O11 -0.6881(9) 0.3723(6) 0.3572(6) 0.066(2) Uani d . 1 O
O12 0.5336(10) 0.8420(8) 0.0474(7) 0.096(3) Uani d . 1 O
O13 0.3786(9) 0.8811(7) -0.1686(5) 0.070(2) Uani d . 1 O
O14 0.2697(7) 0.9892(5) 0.0470(5) 0.0486(15) Uani d . 1 O
O15 0.1131(16) 0.6459(10) 0.6583(9) 0.142(4) Uani d . 1 O
O16 -0.0081(13) 1.0959(7) 0.2047(6) 0.102(3) Uani d . 1 O
N1 0.1909(7) 0.9068(5) 0.4044(5) 0.0247(13) Uani d . 1 N
N2 0.1499(8) 0.6746(5) 0.0913(5) 0.0288(14) Uani d . 1 N
C1 0.3685(10) 1.0317(7) 0.3363(7) 0.0342(19) Uani d . 1 C
C2 0.2998(9) 1.0161(7) 0.4345(6) 0.0287(17) Uani d . 1 C
C3 0.3378(10) 1.0988(7) 0.5433(7) 0.0361(19) Uani d . 1 C
C4 0.2610(11) 1.0641(8) 0.6218(6) 0.041(2) Uani d . 1 C
C5 0.1517(10) 0.9538(8) 0.5901(6) 0.0350(19) Uani d . 1 C
C6 0.1185(9) 0.8751(7) 0.4794(6) 0.0270(17) Uani d . 1 C
C7 -0.0064(11) 0.7537(8) 0.4284(7) 0.040(2) Uani d . 1 C
C8 0.3454(11) 0.5938(8) 0.1906(7) 0.037(2) Uani d . 1 C
C9 0.2511(9) 0.5965(7) 0.0796(6) 0.0276(17) Uani d . 1 C
C10 0.2711(10) 0.5271(7) -0.0244(7) 0.038(2) Uani d . 1 C
C11 0.1815(11) 0.5448(9) -0.1172(7) 0.049(2) Uani d . 1 C
C12 0.0745(12) 0.6266(9) -0.1059(7) 0.049(2) Uani d . 1 C
C13 0.0598(9) 0.6908(7) 0.0014(6) 0.0306(18) Uani d . 1 C
C14 -0.0519(10) 0.7832(8) 0.0277(7) 0.039(2) Uani d . 1 C
H3A 0.4197 1.1849 0.5703 0.050 Uiso d . 1 H
H4A 0.2363 1.1181 0.6940 0.050 Uiso d . 1 H
H5A 0.0984 0.9276 0.6389 0.050 Uiso d . 1 H
H9A -0.6531 0.6461 0.4159 0.050 Uiso d . 1 H
H9B -0.5781 0.7214 0.5356 0.050 Uiso d . 1 H
H10A -0.5774 0.4616 0.6746 0.050 Uiso d . 1 H
H10B -0.7338 0.3921 0.5771 0.050 Uiso d . 1 H
H10C 0.3524 0.4624 -0.0211 0.050 Uiso d . 1 H
H11A -0.7566 0.2895 0.3378 0.050 Uiso d . 1 H
H11B -0.6911 0.4070 0.2966 0.050 Uiso d . 1 H
H11C 0.1906 0.5092 -0.1992 0.050 Uiso d . 1 H
H12A 0.4982 0.7665 -0.0012 0.050 Uiso d . 1 H
H12B 0.5812 0.8497 0.1147 0.050 Uiso d . 1 H
H12C -0.0019 0.6351 -0.1593 0.050 Uiso d . 1 H
H13A 0.4218 0.8751 -0.2416 0.050 Uiso d . 1 H
H13B 0.3223 0.8139 -0.2068 0.050 Uiso d . 1 H
H14A 0.2578 1.0774 0.0597 0.050 Uiso d . 1 H
H14B 0.2700 1.0011 0.1255 0.050 Uiso d . 1 H
H15A 0.0458 0.5553 0.6195 0.050 Uiso d . 1 H
H15B 0.0759 0.6877 0.5999 0.050 Uiso d . 1 H
H16A 0.0216 1.1063 0.1363 0.050 Uiso d . 1 H
H16B -0.0204 1.1803 0.2451 0.050 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
N2 Co1 N1 . . 164.6(2)
N2 Co1 O3 . . 115.7(2)
N1 Co1 O3 . . 76.6(2)
N2 Co1 O1 . . 93.5(2)
N1 Co1 O1 . . 74.9(2)
O3 Co1 O1 . . 150.8(2)
N2 Co1 O5 . . 75.5(2)
N1 Co1 O5 . . 95.9(2)
O3 Co1 O5 . . 90.8(2)
O1 Co1 O5 . . 98.4(2)
N2 Co1 O7 . . 77.1(2)
N1 Co1 O7 . . 112.1(2)
O3 Co1 O7 . . 95.9(2)
O1 Co1 O7 . . 88.9(2)
O5 Co1 O7 . . 152.0(2)
O10 Co2 O10 . 2_466 180.0000(10)
O10 Co2 O9 . . 87.8(2)
O10 Co2 O9 2_466 . 92.2(2)
O10 Co2 O9 . 2_466 92.2(2)
O10 Co2 O9 2_466 2_466 87.8(2)
O9 Co2 O9 . 2_466 180.0000(10)
O10 Co2 O11 . . 91.7(3)
O10 Co2 O11 2_466 . 88.3(2)
O9 Co2 O11 . . 87.5(2)
O9 Co2 O11 2_466 . 92.5(2)
O10 Co2 O11 . 2_466 88.3(2)
O10 Co2 O11 2_466 2_466 91.7(3)
O9 Co2 O11 . 2_466 92.5(2)
O9 Co2 O11 2_466 2_466 87.5(2)
O11 Co2 O11 . 2_466 180.0000(10)
O14 Co3 O14 . 2_675 180.0
O14 Co3 O13 . . 90.6(2)
O14 Co3 O13 2_675 . 89.4(2)
O14 Co3 O13 . 2_675 89.4(2)
O14 Co3 O13 2_675 2_675 90.6(2)
O13 Co3 O13 . 2_675 180.0(2)
O14 Co3 O12 . 2_675 91.7(3)
O14 Co3 O12 2_675 2_675 88.3(3)
O13 Co3 O12 . 2_675 89.1(3)
O13 Co3 O12 2_675 2_675 90.9(3)
O14 Co3 O12 . . 88.3(3)
O14 Co3 O12 2_675 . 91.7(3)
O13 Co3 O12 . . 90.9(3)
O13 Co3 O12 2_675 . 89.1(3)
O12 Co3 O12 2_675 . 180.0000(10)
C1 O1 Co1 . . 117.4(5)
C7 O3 Co1 . . 116.3(5)
C8 O5 Co1 . . 115.0(5)
C14 O7 Co1 . . 113.7(5)
Co2 O9 H9A . . 114.9
Co2 O9 H9B . . 115.1
H9A O9 H9B . . 105.5
Co2 O10 H10A . . 110.6
Co2 O10 H10B . . 112.2
H10A O10 H10B . . 105.0
Co2 O11 H11A . . 135.9
Co2 O11 H11B . . 106.7
H11A O11 H11B . . 116.9
Co3 O12 H12A . . 121.2
Co3 O12 H12B . . 122.1
H12A O12 H12B . . 116.7
Co3 O13 H13A . . 127.0
Co3 O13 H13B . . 144.5
H13A O13 H13B . . 83.6
Co3 O14 H14A . . 98.2
Co3 O14 H14B . . 118.4
H14A O14 H14B . . 90.8
H15A O15 H15B . . 103.1
H16A O16 H16B . . 100.5
C6 N1 C2 . . 121.2(6)
C6 N1 Co1 . . 118.0(5)
C2 N1 Co1 . . 120.8(5)
C9 N2 C13 . . 121.3(6)
C9 N2 Co1 . . 121.0(5)
C13 N2 Co1 . . 117.6(5)
O2 C1 O1 . . 126.5(7)
O2 C1 C2 . . 118.9(7)
O1 C1 C2 . . 114.7(7)
N1 C2 C3 . . 120.6(7)
N1 C2 C1 . . 112.2(6)
C3 C2 C1 . . 127.2(7)
C2 C3 C4 . . 117.7(7)
C2 C3 H3A . . 123.4
C4 C3 H3A . . 119.0
C5 C4 C3 . . 121.0(7)
C5 C4 H4A . . 105.3
C3 C4 H4A . . 129.7
C4 C5 C6 . . 118.4(7)
C4 C5 H5A . . 123.7
C6 C5 H5A . . 117.9
N1 C6 C5 . . 121.1(7)
N1 C6 C7 . . 113.3(6)
C5 C6 C7 . . 125.5(7)
O4 C7 O3 . . 125.6(8)
O4 C7 C6 . . 120.1(8)
O3 C7 C6 . . 114.3(7)
O6 C8 O5 . . 125.4(8)
O6 C8 C9 . . 119.8(7)
O5 C8 C9 . . 114.7(7)
N2 C9 C10 . . 122.1(7)
N2 C9 C8 . . 113.6(7)
C10 C9 C8 . . 124.3(7)
C9 C10 C11 . . 117.1(8)
C9 C10 H10C . . 113.7
C11 C10 H10C . . 129.2
C12 C11 C10 . . 121.3(8)
C12 C11 H11C . . 110.6
C10 C11 H11C . . 127.8
C11 C12 C13 . . 117.7(7)
C11 C12 H12C . . 128.5
C13 C12 H12C . . 112.8
N2 C13 C12 . . 120.5(7)
N2 C13 C14 . . 115.5(6)
C12 C13 C14 . . 124.1(7)
O8 C14 O7 . . 125.2(8)
O8 C14 C13 . . 119.7(7)
O7 C14 C13 . . 115.1(7)
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
Co1 N2 . 2.012(6) yes
Co1 N1 . 2.017(6) yes
Co1 O3 . 2.106(5) yes
Co1 O1 . 2.181(5) yes
Co1 O5 . 2.193(5) yes
Co1 O7 . 2.200(6) yes
Co2 O10 . 2.107(5) yes
Co2 O10 2_466 2.107(5) ?
Co2 O9 . 2.118(6) yes
Co2 O9 2_466 2.118(6) ?
Co2 O11 . 2.148(6) yes
Co2 O11 2_466 2.148(6) ?
Co3 O14 . 2.092(6) yes
Co3 O14 2_675 2.092(6) ?
Co3 O13 . 2.136(6) yes
Co3 O13 2_675 2.136(6) ?
Co3 O12 2_675 2.150(8) ?
Co3 O12 . 2.150(8) yes
O1 C1 . 1.251(9) ?
O2 C1 . 1.230(9) ?
O3 C7 . 1.280(10) ?
O4 C7 . 1.236(9) ?
O5 C8 . 1.282(9) ?
O6 C8 . 1.230(10) ?
O7 C14 . 1.281(9) ?
O8 C14 . 1.225(9) ?
O9 H9A . 0.9161 ?
O9 H9B . 0.9384 ?
O10 H10A . 0.9407 ?
O10 H10B . 1.0090 ?
O11 H11A . 0.9756 ?
O11 H11B . 0.9846 ?
O12 H12A . 0.8709 ?
O12 H12B . 0.8588 ?
O13 H13A . 1.0465 ?
O13 H13B . 0.7999 ?
O14 H14A . 1.0063 ?
O14 H14B . 0.9744 ?
O15 H15A . 1.0336 ?
O15 H15B . 1.0456 ?
O16 H16A . 0.9919 ?
O16 H16B . 0.9807 ?
N1 C6 . 1.339(8) ?
N1 C2 . 1.347(9) ?
N2 C9 . 1.309(9) ?
N2 C13 . 1.346(9) ?
C1 C2 . 1.523(10) ?
C2 C3 . 1.373(10) ?
C3 C4 . 1.412(11) ?
C3 H3A . 1.0417 ?
C4 C5 . 1.355(11) ?
C4 H4A . 1.0135 ?
C5 C6 . 1.379(10) ?
C5 H5A . 0.9274 ?
C6 C7 . 1.500(11) ?
C8 C9 . 1.517(10) ?
C9 C10 . 1.375(10) ?
C10 C11 . 1.384(12) ?
C10 H10C . 1.0811 ?
C11 C12 . 1.378(13) ?
C11 H11C . 1.0228 ?
C12 C13 . 1.379(11) ?
C12 H12C . 0.8897 ?
C13 C14 . 1.507(11) ?
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
O14 H14B O1 . 0.98 1.91 2.770(10) 147
O13 H13A O2 2_675 1.05 1.81 2.85(2) 169
O9 H9B O2 2_576 0.94 1.86 2.79(3) 172
O10 H10B O4 2_466 1.01 1.71 2.69(3) 163
O15 H15B O4 . 1.05 1.87 2.84(2) 154
O9 H9A O5 1_455 0.92 1.85 2.760(10) 176
O10 H10A O6 2_566 0.94 1.83 2.76(2) 168
O11 H11B O6 1_455 0.99 2.49 3.39(2) 153
O14 H14A O8 2_575 1.01 1.83 2.75(2) 152
O16 H16A O8 2_575 0.99 1.98 2.92(2) 156
O13 H13B O15 1_554 0.80 2.38 3.16(4) 165
O16 H16B O15 2_576 0.98 2.32 3.28(3) 166
C5 H5A O16 2_576 0.93 2.34 3.25(2) 166
