#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/36/2203610.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_2203610
loop_
_publ_author_name
'Mikki Vinodu'
'Israel Goldberg'
_publ_section_title
;
 catena-Poly[[bis(pyridine-κN)cobalt(II)]-μ-oxalato]
 0.25-hydrate]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m527
_journal_page_last               m529
_journal_paper_doi               10.1107/S1600536804007512
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C2 O4) (C5 H5 N)2], 0.25H2 O'
_chemical_formula_moiety         'C12 H10 Co N2 O4, 0.25H2 O'
_chemical_formula_sum            'C12 H10.5 Co N2 O4.25'
_chemical_formula_weight         309.65
_chemical_name_systematic
;
catena-Poly[[bis(pyridine-\kN)cobalt(II)]-μ-oxalato] 0.25-hydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.369(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4320(3)
_cell_length_b                   9.1810(4)
_cell_length_c                   14.9370(5)
_cell_measurement_reflns_used    2213
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.47
_cell_volume                     1289.71(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        DENZO
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and
MERCURY (Bruno et al., 2002)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1° 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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9965
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.8781
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.768
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0389
_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)+(0.0729P)²+0.0368P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                2213
_reflns_number_total             2884
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg6032.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2203610
_cod_database_fobs_code          2203610
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.24978(2) 0.15117(3) -0.004522(16) 0.01569(14) Uani d . 1 Co
O2 0.06943(15) 0.14140(15) 0.06838(10) 0.0169(3) Uani d . 1 O
O3 0.43149(15) 0.13499(16) -0.07360(10) 0.0178(3) Uani d . 1 O
O4 0.13332(15) -0.01654(16) -0.07461(9) 0.0189(3) Uani d . 1 O
O5 0.36296(15) -0.01383(16) 0.07210(9) 0.0179(3) Uani d . 1 O
C6 0.5203(2) 0.0429(2) -0.04229(12) 0.0160(4) Uani d . 1 C
C7 -0.0189(2) 0.0461(2) 0.04156(12) 0.0162(4) Uani d . 1 C
N8 0.16213(19) 0.3060(2) -0.10054(12) 0.0185(4) Uani d . 1 N
C9 0.0459(2) 0.3829(2) -0.08569(14) 0.0233(5) Uani d . 1 C
H9 0.0012 0.3653 -0.0318 0.028 Uiso calc R 1 H
C10 -0.0129(2) 0.4867(3) -0.14447(14) 0.0266(5) Uani d . 1 C
H10 -0.0954 0.5392 -0.1309 0.032 Uiso calc R 1 H
C11 0.0509(2) 0.5127(2) -0.22363(14) 0.0247(5) Uani d . 1 C
H11 0.0135 0.5838 -0.2652 0.030 Uiso calc R 1 H
C12 0.1697(2) 0.4331(3) -0.24061(14) 0.0277(5) Uani d . 1 C
H12 0.2152 0.4477 -0.2945 0.033 Uiso calc R 1 H
C13 0.2220(2) 0.3316(3) -0.17801(14) 0.0257(5) Uani d . 1 C
H13 0.3041 0.2775 -0.1903 0.031 Uiso calc R 1 H
N14 0.33091(18) 0.3130(2) 0.08869(11) 0.0179(4) Uani d . 1 N
C15 0.3387(2) 0.2806(3) 0.17672(13) 0.0246(5) Uani d . 1 C
H15 0.3152 0.1847 0.1943 0.029 Uiso calc R 1 H
C16 0.3797(3) 0.3812(3) 0.24277(15) 0.0284(5) Uani d . 1 C
H16 0.3830 0.3546 0.3044 0.034 Uiso calc R 1 H
C17 0.4156(3) 0.5202(3) 0.21822(15) 0.0288(5) Uani d . 1 C
H17 0.4456 0.5905 0.2623 0.035 Uiso calc R 1 H
C18 0.4068(3) 0.5554(3) 0.12776(15) 0.0301(5) Uani d . 1 C
H18 0.4297 0.6506 0.1087 0.036 Uiso calc R 1 H
C19 0.3639(2) 0.4487(2) 0.06548(14) 0.0248(5) Uani d . 1 C
H19 0.3578 0.4734 0.0035 0.030 Uiso calc R 1 H
O20 0.3061(8) 0.7150(8) -0.0786(5) 0.051(2) Uani d P 0.25 O
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'
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'
N N 0.0061 0.0033 '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
O3 Co1 O2 . . 173.27(6) yes
O3 Co1 O4 . . 96.84(6) yes
O2 Co1 O4 . . 79.32(5) yes
O3 Co1 O5 . . 79.47(5) yes
O2 Co1 O5 . . 94.81(5) yes
O4 Co1 O5 . . 88.19(6) yes
O3 Co1 N14 . . 96.06(6) yes
O2 Co1 N14 . . 87.46(6) yes
O4 Co1 N14 . . 166.50(6) yes
O5 Co1 N14 . . 90.25(7) yes
O3 Co1 N8 . . 90.33(6) yes
O2 Co1 N8 . . 95.13(6) yes
O4 Co1 N8 . . 89.56(7) yes
O5 Co1 N8 . . 169.22(6) yes
N14 Co1 N8 . . 94.35(8) yes
C7 O2 Co1 . . 114.27(12) ?
C6 O3 Co1 . . 114.62(12) ?
C7 O4 Co1 3 . 113.14(12) ?
C6 O5 Co1 3_655 . 112.29(12) ?
O5 C6 O3 3_655 . 126.38(17) ?
O5 C6 C6 3_655 3_655 117.3(2) ?
O3 C6 C6 . 3_655 116.3(2) ?
O4 C7 O2 3 . 126.75(18) ?
O4 C7 C7 3 3 116.8(2) ?
O2 C7 C7 . 3 116.5(2) ?
C9 N8 C13 . . 116.94(19) ?
C9 N8 Co1 . . 121.30(14) ?
C13 N8 Co1 . . 121.76(15) ?
N8 C9 C10 . . 123.57(19) ?
N8 C9 H9 . . 118.2 ?
C10 C9 H9 . . 118.2 ?
C9 C10 C11 . . 118.7(2) ?
C9 C10 H10 . . 120.6 ?
C11 C10 H10 . . 120.6 ?
C12 C11 C10 . . 118.5(2) ?
C12 C11 H11 . . 120.7 ?
C10 C11 H11 . . 120.7 ?
C11 C12 C13 . . 119.1(2) ?
C11 C12 H12 . . 120.5 ?
C13 C12 H12 . . 120.5 ?
N8 C13 C12 . . 123.2(2) ?
N8 C13 H13 . . 118.4 ?
C12 C13 H13 . . 118.4 ?
C19 N14 C15 . . 117.59(19) ?
C19 N14 Co1 . . 123.92(14) ?
C15 N14 Co1 . . 118.27(15) ?
N14 C15 C16 . . 122.7(2) ?
N14 C15 H15 . . 118.6 ?
C16 C15 H15 . . 118.6 ?
C17 C16 C15 . . 119.3(2) ?
C17 C16 H16 . . 120.4 ?
C15 C16 H16 . . 120.4 ?
C16 C17 C18 . . 118.5(2) ?
C16 C17 H17 . . 120.7 ?
C18 C17 H17 . . 120.7 ?
C17 C18 C19 . . 118.8(2) ?
C17 C18 H18 . . 120.6 ?
C19 C18 H18 . . 120.6 ?
N14 C19 C18 . . 123.0(2) ?
N14 C19 H19 . . 118.5 ?
C18 C19 H19 . . 118.5 ?
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 O3 . 2.0721(15) yes
Co1 O2 . 2.0903(14) yes
Co1 O4 . 2.1209(15) yes
Co1 O5 . 2.1350(14) yes
Co1 N14 . 2.1375(18) yes
Co1 N8 . 2.1400(18) yes
O2 C7 . 1.252(2) yes
O3 C6 . 1.255(3) yes
O4 C7 3 1.251(2) yes
O5 C6 3_655 1.247(2) yes
C6 O5 3_655 1.248(2) yes
C6 C6 3_655 1.561(4) yes
C7 O4 3 1.251(2) yes
C7 C7 3 1.566(4) yes
N8 C9 . 1.337(3) ?
N8 C13 . 1.346(3) ?
C9 C10 . 1.383(3) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.388(3) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.377(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.384(3) ?
C12 H12 . 0.9500 ?
C13 H13 . 0.9500 ?
N14 C19 . 1.337(3) ?
N14 C15 . 1.345(3) ?
C15 C16 . 1.385(3) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.377(3) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.385(3) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.389(3) ?
C18 H18 . 0.9500 ?
C19 H19 . 0.9500 ?
