#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/85/2208577.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_2208577
loop_
_publ_author_name
'Heren, Zerrin'
'Ersanlı, Cem Cüneyt'
'Keser, Cem'
'Ocak Ískeleli, Nazan'
_publ_section_title
;
 Redetermination of
 trans-diaquabis(picolinato-κ²N,O)cobalt(II)
 dihydrate
;
_journal_coeditor_code           DN2006
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m796
_journal_page_last               m798
_journal_paper_doi               10.1107/S1600536806009081
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co (C6 H4 N O2)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C12 H12 Co N2 O6, 2H2 O'
_chemical_formula_sum            'C12 H16 Co N2 O8'
_chemical_formula_weight         375.20
_chemical_name_systematic
;
trans-diaquabis(picolinato-κ²N,O)cobalt(II) dihydrate
;
_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                 123.780(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8093(9)
_cell_length_b                   5.1846(3)
_cell_length_c                   17.5233(16)
_cell_measurement_reflns_used    14007
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.5
_cell_volume                     740.74(12)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-II'
_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  0.044
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12035
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.9
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1760
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0239
_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)+(0.0389P)²+0.0458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                1441
_reflns_number_total             1760
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2006.cif
_cod_data_source_block           I
_cod_original_cell_volume        740.74(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208577
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
Co Co1 0.5000 0.5000 0.5000 0.02541(9) Uani d S 1
O O1W 0.42241(14) 0.7409(2) 0.38364(8) 0.0348(2) Uani d D 1
H H1A 0.473(2) 0.884(3) 0.3993(15) 0.052 Uiso d D 1
H H1B 0.435(3) 0.663(4) 0.3457(12) 0.052 Uiso d D 1
O O1 0.43782(12) 0.7832(2) 0.55832(7) 0.0320(2) Uani d . 1
C C1 0.28721(18) 0.7910(3) 0.53122(10) 0.0294(3) Uani d . 1
N N1 0.24581(15) 0.4280(2) 0.43453(9) 0.0273(3) Uani d . 1
O O2 0.23001(15) 0.9384(3) 0.56192(9) 0.0430(3) Uani d . 1
C C2 0.17365(17) 0.6054(3) 0.45624(10) 0.0278(3) Uani d . 1
C C3 0.00540(19) 0.6215(4) 0.41267(12) 0.0354(4) Uani d . 1
H H3 -0.0413 0.7468 0.4293 0.043 Uiso calc R 1
C C4 -0.0916(2) 0.4463(4) 0.34374(13) 0.0412(4) Uani d . 1
H H4 -0.2052 0.4533 0.3125 0.049 Uiso calc R 1
C C5 -0.0181(2) 0.2613(4) 0.32182(12) 0.0408(4) Uani d . 1
H H5 -0.0813 0.1407 0.2761 0.049 Uiso calc R 1
C C6 0.15083(19) 0.2576(3) 0.36890(11) 0.0340(3) Uani d . 1
H H6 0.2003 0.1316 0.3543 0.041 Uiso calc R 1
O O2W 0.4257(2) 0.4866(3) 0.24435(9) 0.0568(4) Uani d D 1
H H2A 0.461(3) 0.337(3) 0.2598(18) 0.085 Uiso d D 1
H H2B 0.361(3) 0.498(5) 0.1870(7) 0.085 Uiso d D 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.02300(14) 0.02569(15) 0.02698(14) -0.00044(12) 0.01355(11) -0.00255(12)
O1W 0.0386(6) 0.0320(6) 0.0331(6) -0.0038(5) 0.0196(5) 0.0002(5)
O1 0.0273(5) 0.0316(6) 0.0360(5) -0.0024(4) 0.0170(5) -0.0088(5)
C1 0.0305(7) 0.0305(8) 0.0283(7) 0.0010(6) 0.0170(6) -0.0006(6)
N1 0.0253(6) 0.0269(6) 0.0282(6) -0.0011(5) 0.0139(5) -0.0002(5)
O2 0.0375(6) 0.0493(8) 0.0437(6) 0.0031(5) 0.0235(5) -0.0130(5)
C2 0.0269(7) 0.0302(7) 0.0279(7) 0.0003(6) 0.0162(6) 0.0015(6)
C3 0.0293(8) 0.0394(9) 0.0393(9) 0.0022(7) 0.0201(7) 0.0003(7)
C4 0.0258(7) 0.0503(11) 0.0422(9) -0.0039(7) 0.0156(7) -0.0013(8)
C5 0.0331(8) 0.0409(9) 0.0376(8) -0.0094(7) 0.0128(7) -0.0074(8)
C6 0.0338(8) 0.0309(8) 0.0350(8) -0.0018(7) 0.0177(7) -0.0037(7)
O2W 0.0774(10) 0.0468(8) 0.0381(6) 0.0087(8) 0.0272(7) 0.0012(7)
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'
Co Co 0.3494 0.9721 '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'
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
O1 Co1 O1 . 3_666 180.0
O1 Co1 N1 . 3_666 100.91(5)
O1 Co1 N1 . . 79.09(5)
N1 Co1 N1 3_666 . 180.0
O1 Co1 O1W . 3_666 89.42(5)
O1 Co1 O1W 3_666 3_666 90.58(5)
N1 Co1 O1W 3_666 3_666 84.19(5)
N1 Co1 O1W . 3_666 95.81(5)
O1 Co1 O1W . . 90.58(5)
O1 Co1 O1W 3_666 . 89.42(5)
N1 Co1 O1W 3_666 . 95.81(5)
N1 Co1 O1W . . 84.19(5)
O1W Co1 O1W 3_666 . 180.00(5)
Co1 O1W H1A . . 111.6(16)
Co1 O1W H1B . . 110.0(15)
H1A O1W H1B . . 111.1(17)
C1 O1 Co1 . . 115.96(10)
O2 C1 O1 . . 124.76(14)
O2 C1 C2 . . 118.75(14)
O1 C1 C2 . . 116.49(13)
C6 N1 C2 . . 118.29(13)
C6 N1 Co1 . . 129.11(11)
C2 N1 Co1 . . 111.98(10)
N1 C2 C3 . . 122.81(15)
N1 C2 C1 . . 115.83(13)
C3 C2 C1 . . 121.35(14)
C4 C3 C2 . . 118.22(16)
C4 C3 H3 . . 120.9
C2 C3 H3 . . 120.9
C5 C4 C3 . . 119.30(15)
C5 C4 H4 . . 120.4
C3 C4 H4 . . 120.4
C4 C5 C6 . . 118.90(16)
C4 C5 H5 . . 120.5
C6 C5 H5 . . 120.5
N1 C6 C5 . . 122.46(15)
N1 C6 H6 . . 118.8
C5 C6 H6 . . 118.8
H2A O2W H2B . . 111(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 O1 2.0652(10)
Co1 N1 2.1193(13)
Co1 O1W 2.1379(11)
O1W H1A 0.847(9)
O1W H1B 0.84(2)
O1 C1 1.2765(18)
C1 O2 1.2344(19)
C1 C2 1.505(2)
N1 C6 1.334(2)
N1 C2 1.338(2)
C2 C3 1.383(2)
C3 C4 1.382(3)
C3 H3 0.9300
C4 C5 1.376(3)
C4 H4 0.9300
C5 C6 1.381(2)
C5 H5 0.9300
C6 H6 0.9300
O2W H2A 0.832(10)
O2W H2B 0.841(10)
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
O1W H1A O1 3_676 0.847(9) 1.892(10) 2.7300(17) 169.9(19)
O1W H1B O2W . 0.84(2) 1.956(10) 2.7900(19) 171(2)
O2W H2A O2W 2_645 0.832(10) 2.150(15) 2.9264(18) 155(3)
O2W H2B O2 4_575 0.841(10) 1.853(10) 2.6891(19) 173(3)
C3 H3 O2 3_576 0.93 2.54 3.447(2) 166
