#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/69/2016920.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_2016920
loop_
_publ_author_name
'Atria, Ana María'
'Corsini, Gino'
'Talamilla, Arlyn'
'Garland, Maria Teresa'
'Baggio, Ricardo'
_publ_section_title
;Two isomorphous cobalt(II) complexes:
 poly[[diaqua-μ-2,5-dicarboxybenzene-1,4-dicarboxylato-μ-1,2-di-4-pyridylethene-cobalt(II)]
 1,2-di-4-pyridylethene solvate] and the 1,2-di-4-pyridylethane analogue
;
_journal_coeditor_code           FG3070
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m24
_journal_page_last               m27
_journal_paper_doi               10.1107/S0108270108041541
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Co(C10 H4 O8) (C12 H12 N2) (H2 O)2] , C12 H12 N2'
_chemical_formula_moiety         'C22 H16 Co N2 O10, C12 H16 N2'
_chemical_formula_sum            'C34 H32 Co N4 O10'
_chemical_formula_weight         715.57
_chemical_name_systematic
;
poly[[diaqua-μ-2,5-dicarboxybenzene-1,4-dicarboxylato-
μ-1,2-di-4-pyridylethene-cobalt(II)] 1,2-di-4-pyridylethane solvate]
;
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                92.2999(7)
_cell_angle_beta                 111.9705(6)
_cell_angle_gamma                105.6443(7)
_cell_formula_units_Z            1
_cell_length_a                   9.0933(4)
_cell_length_b                   9.5887(5)
_cell_length_c                   10.0058(5)
_cell_measurement_reflns_used    6988
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.24
_cell_volume                     769.33(7)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0111
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16531
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             371
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0282
_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)+(0.0432P)²+0.4048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                3363
_reflns_number_total             3442
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3070.cif
_cod_data_source_block           II
_cod_database_code               2016920
_cod_database_fobs_code          2016920
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_disorder_assembly
_atom_site_disorder_group
Co Co1 1.0000 0.5000 0.5000 0.01268(8) Uani d S 1 . .
N N11 1.00772(14) 0.64830(12) 0.66911(12) 0.0166(2) Uani d . 1 . .
C C11 1.01890(18) 0.60773(15) 0.79794(15) 0.0206(3) Uani d . 1 . .
H H11 1.0145 0.5091 0.8099 0.025 Uiso calc R 1 . .
C C21 1.03664(18) 0.70288(15) 0.91484(15) 0.0221(3) Uani d . 1 . .
H H21 1.0469 0.6699 1.0052 0.026 Uiso calc R 1 . .
C C31 1.03933(18) 0.84696(15) 0.89905(15) 0.0205(3) Uani d . 1 . .
C C41 1.02532(19) 0.88863(15) 0.76420(15) 0.0228(3) Uani d . 1 . .
H H41 1.0255 0.9856 0.7480 0.027 Uiso calc R 1 . .
C C51 1.01111(18) 0.78745(15) 0.65403(15) 0.0199(3) Uani d . 1 . .
H H51 1.0034 0.8180 0.5631 0.024 Uiso calc R 1 . .
C C61 1.0565(2) 0.95237(17) 1.02381(15) 0.0267(3) Uani d . 1 . .
H H61A 1.1736 1.0161 1.0712 0.032 Uiso calc R 1 . .
H H61B 1.0303 0.8960 1.0971 0.032 Uiso calc R 1 . .
N N12 0.61075(15) 0.58527(13) 0.84643(13) 0.0207(2) Uani d . 1 . .
C C12 0.52451(19) 0.66391(16) 0.76178(16) 0.0248(3) Uani d . 1 . .
H H12 0.4868 0.6408 0.6589 0.030 Uiso calc R 1 . .
C C22 0.4878(2) 0.77847(16) 0.81846(16) 0.0276(3) Uani d . 1 . .
H H22 0.4253 0.8319 0.7549 0.033 Uiso calc R 1 . .
C C32 0.54274(17) 0.81441(15) 0.96850(15) 0.0207(3) Uani d . 1 . .
C C42 0.6322(2) 0.73079(16) 1.05508(15) 0.0251(3) Uani d . 1 . .
H H42 0.6719 0.7515 1.1583 0.030 Uiso calc R 1 . .
C C52 0.6632(2) 0.61772(16) 0.99128(16) 0.0257(3) Uani d . 1 . .
H H52 0.7237 0.5612 1.0521 0.031 Uiso calc R 1 . .
C C62 0.5060(2) 0.93506(16) 1.04066(16) 0.0266(3) Uani d . 1 . .
H H62A 0.5948 0.9711 1.1400 0.032 Uiso calc R 1 . .
H H62B 0.3996 0.8928 1.0511 0.032 Uiso calc R 1 . .
C C13 0.65325(16) 0.11282(13) 0.55581(13) 0.0145(2) Uani d . 1 . .
C C23 0.51056(16) 0.13905(13) 0.56013(14) 0.0154(2) Uani d . 1 . .
C C33 0.35951(16) 0.02621(14) 0.50310(14) 0.0159(2) Uani d . 1 . .
H H33 0.2625 0.0447 0.5045 0.019 Uiso calc R 1 . .
C C43 0.81693(16) 0.23255(13) 0.59562(13) 0.0149(2) Uani d . 1 . .
C C53 0.51163(17) 0.28302(14) 0.62758(15) 0.0176(3) Uani d . 1 . .
O O13 0.80913(11) 0.34027(10) 0.52823(10) 0.01647(19) Uani d . 1 . .
O O23 0.94715(12) 0.21110(11) 0.68265(11) 0.0219(2) Uani d . 1 . .
O O33 0.64417(12) 0.35290(11) 0.74026(11) 0.0221(2) Uani d . 1 . .
H H33A 0.636(3) 0.468(3) 0.791(3) 0.076(9) Uiso d . 1 . .
O O43 0.38682(13) 0.32279(12) 0.57544(13) 0.0301(3) Uani d . 1 . .
O O1W 1.17975(12) 0.42847(11) 0.65954(10) 0.01734(19) Uani d . 1 . .
H H1WB 1.248(3) 0.402(2) 0.632(2) 0.035(5) Uiso d . 1 . .
H H1WA 1.124(3) 0.356(2) 0.672(2) 0.033(5) Uiso d . 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'
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
O13 Co1 O13 . 2_766 180.00(4) ?
O13 Co1 O1W . 2_766 89.85(4) ?
O13 Co1 O1W 2_766 2_766 90.15(4) ?
O13 Co1 O1W . . 90.15(4) y
O13 Co1 O1W 2_766 . 89.85(4) ?
O1W Co1 O1W 2_766 . 180.0 ?
O13 Co1 N11 . . 89.34(4) y
O13 Co1 N11 2_766 . 90.66(4) ?
O1W Co1 N11 2_766 . 91.35(4) ?
O1W Co1 N11 . . 88.65(4) y
O13 Co1 N11 . 2_766 90.66(4) ?
O13 Co1 N11 2_766 2_766 89.34(4) ?
O1W Co1 N11 2_766 2_766 88.65(4) ?
O1W Co1 N11 . 2_766 91.35(4) ?
N11 Co1 N11 . 2_766 180.0000(10) ?
C11 N11 C51 . . 117.35(11) ?
C11 N11 Co1 . . 120.74(9) ?
C51 N11 Co1 . . 121.81(9) ?
N11 C11 C21 . . 123.04(12) ?
N11 C11 H11 . . 118.5 ?
C21 C11 H11 . . 118.5 ?
C11 C21 C31 . . 119.62(12) ?
C11 C21 H21 . . 120.2 ?
C31 C21 H21 . . 120.2 ?
C21 C31 C41 . . 117.31(12) ?
C21 C31 C61 . . 120.77(12) ?
C41 C31 C61 . . 121.92(12) ?
C51 C41 C31 . . 119.36(12) ?
C51 C41 H41 . . 120.3 ?
C31 C41 H41 . . 120.3 ?
N11 C51 C41 . . 123.29(12) ?
N11 C51 H51 . . 118.4 ?
C41 C51 H51 . . 118.4 ?
C31 C61 C61 . 2_777 112.98(15) ?
C31 C61 H61A . . 109.0 ?
C61 C61 H61A 2_777 . 109.0 ?
C31 C61 H61B . . 109.0 ?
C61 C61 H61B 2_777 . 109.0 ?
H61A C61 H61B . . 107.8 ?
C12 N12 C52 . . 118.67(12) ?
C12 N12 H33A . . 122.1(12) ?
C52 N12 H33A . . 119.1(12) ?
N12 C12 C22 . . 122.38(13) ?
N12 C12 H12 . . 118.8 ?
C22 C12 H12 . . 118.8 ?
C32 C22 C12 . . 119.64(13) ?
C32 C22 H22 . . 120.2 ?
C12 C22 H22 . . 120.2 ?
C22 C32 C42 . . 117.15(12) ?
C22 C32 C62 . . 123.61(13) ?
C42 C32 C62 . . 119.21(13) ?
C52 C42 C32 . . 120.14(13) ?
C52 C42 H42 . . 119.9 ?
C32 C42 H42 . . 119.9 ?
N12 C52 C42 . . 122.03(13) ?
N12 C52 H52 . . 119.0 ?
C42 C52 H52 . . 119.0 ?
C32 C62 C62 . 2_677 114.79(15) ?
C32 C62 H62A . . 108.6 ?
C62 C62 H62A 2_677 . 108.6 ?
C32 C62 H62B . . 108.6 ?
C62 C62 H62B 2_677 . 108.6 ?
H62A C62 H62B . . 107.5 ?
C33 C13 C23 2_656 . 118.93(11) ?
C33 C13 C43 2_656 . 117.48(11) ?
C23 C13 C43 . . 123.18(11) ?
C33 C23 C13 . . 119.16(11) ?
C33 C23 C53 . . 117.40(11) ?
C13 C23 C53 . . 123.41(11) ?
C13 C33 C23 2_656 . 121.90(12) ?
C13 C33 H33 2_656 . 119.1 ?
C23 C33 H33 . . 119.1 ?
O23 C43 O13 . . 126.34(12) ?
O23 C43 C13 . . 117.96(11) ?
O13 C43 C13 . . 115.47(11) ?
O43 C53 O33 . . 125.00(12) ?
O43 C53 C23 . . 118.74(12) ?
O33 C53 C23 . . 116.21(11) ?
C43 O13 Co1 . . 129.42(8) ?
C53 O33 H33A . . 112.8(13) ?
Co1 O1W H1WB . . 116.0(14) ?
Co1 O1W H1WA . . 101.5(15) ?
H1WB O1W H1WA . . 105(2) ?
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 O13 . 2.0990(9) y
Co1 O13 2_766 2.0991(9) ?
Co1 O1W 2_766 2.1049(9) ?
Co1 O1W . 2.1049(9) y
Co1 N11 . 2.1341(11) y
Co1 N11 2_766 2.1341(11) ?
N11 C11 . 1.3368(17) ?
N11 C51 . 1.3422(17) ?
C11 C21 . 1.3857(19) ?
C11 H11 . 0.9500 ?
C21 C31 . 1.3916(19) ?
C21 H21 . 0.9500 ?
C31 C41 . 1.3923(19) ?
C31 C61 . 1.5074(18) ?
C41 C51 . 1.3831(18) ?
C41 H41 . 0.9500 ?
C51 H51 . 0.9500 ?
C61 C61 2_777 1.514(3) ?
C61 H61A . 0.9900 ?
C61 H61B . 0.9900 ?
N12 C12 . 1.3320(19) ?
N12 C52 . 1.3384(19) ?
N12 H33A . 1.34(3) ?
C12 C22 . 1.389(2) ?
C12 H12 . 0.9500 ?
C22 C32 . 1.388(2) ?
C22 H22 . 0.9500 ?
C32 C42 . 1.3910(19) ?
C32 C62 . 1.5142(18) ?
C42 C52 . 1.3811(19) ?
C42 H42 . 0.9500 ?
C52 H52 . 0.9500 ?
C62 C62 2_677 1.521(3) ?
C62 H62A . 0.9900 ?
C62 H62B . 0.9900 ?
C13 C33 2_656 1.3930(17) ?
C13 C23 . 1.4020(17) ?
C13 C43 . 1.5133(17) ?
C23 C33 . 1.3948(18) ?
C23 C53 . 1.5082(17) ?
C33 C13 2_656 1.3930(17) ?
C33 H33 . 0.9500 ?
C43 O23 . 1.2557(16) ?
C43 O13 . 1.2594(15) ?
C53 O43 . 1.2297(17) ?
C53 O33 . 1.2883(17) ?
O33 H33A . 1.23(3) ?
O1W H1WB . 0.85(2) ?
O1W H1WA . 0.79(2) ?
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
O33 H33A N12 . 1.23(3) 1.34(3) 2.5695(15) 174(3)
O1W H1WB O43 1_655 0.85(2) 1.87(2) 2.7252(14) 174(2)
O1W H1WA O23 . 0.79(2) 1.86(2) 2.6265(14) 164(2)
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O13 Co1 N11 C11 . . . . 50.41(11) ?
O13 Co1 N11 C11 2_766 . . . -129.59(11) ?
O1W Co1 N11 C11 2_766 . . . 140.24(11) ?
O1W Co1 N11 C11 . . . . -39.76(11) ?
O13 Co1 N11 C51 . . . . -133.41(11) ?
O13 Co1 N11 C51 2_766 . . . 46.59(11) ?
O1W Co1 N11 C51 2_766 . . . -43.58(11) ?
O1W Co1 N11 C51 . . . . 136.42(11) ?
C51 N11 C11 C21 . . . . -1.2(2) ?
Co1 N11 C11 C21 . . . . 175.12(11) ?
N11 C11 C21 C31 . . . . 1.6(2) ?
C11 C21 C31 C41 . . . . -0.6(2) ?
C11 C21 C31 C61 . . . . 179.29(14) ?
C21 C31 C41 C51 . . . . -0.6(2) ?
C61 C31 C41 C51 . . . . 179.54(14) ?
C11 N11 C51 C41 . . . . 0.0(2) ?
Co1 N11 C51 C41 . . . . -176.34(11) ?
C31 C41 C51 N11 . . . . 0.9(2) ?
C21 C31 C61 C61 . . . 2_777 -138.30(18) ?
C41 C31 C61 C61 . . . 2_777 41.6(3) ?
C52 N12 C12 C22 . . . . 0.2(2) ?
N12 C12 C22 C32 . . . . 0.4(2) ?
C12 C22 C32 C42 . . . . -0.6(2) ?
C12 C22 C32 C62 . . . . -178.65(15) ?
C22 C32 C42 C52 . . . . 0.1(2) ?
C62 C32 C42 C52 . . . . 178.30(15) ?
C12 N12 C52 C42 . . . . -0.7(2) ?
C32 C42 C52 N12 . . . . 0.5(3) ?
C22 C32 C62 C62 . . . 2_677 -32.6(3) ?
C42 C32 C62 C62 . . . 2_677 149.39(18) ?
C33 C13 C23 C33 2_656 . . . -1.1(2) ?
C43 C13 C23 C33 . . . . 171.44(12) ?
C33 C13 C23 C53 2_656 . . . 177.10(12) ?
C43 C13 C23 C53 . . . . -10.34(19) ?
C13 C23 C33 C13 . . . 2_656 1.2(2) ?
C53 C23 C33 C13 . . . 2_656 -177.18(12) ?
C33 C13 C43 O23 2_656 . . . -56.23(16) ?
C23 C13 C43 O23 . . . . 131.12(13) ?
C33 C13 C43 O13 2_656 . . . 118.61(13) ?
C23 C13 C43 O13 . . . . -54.04(17) ?
C33 C23 C53 O43 . . . . -33.79(18) ?
C13 C23 C53 O43 . . . . 147.96(14) ?
C33 C23 C53 O33 . . . . 143.98(12) ?
C13 C23 C53 O33 . . . . -34.27(18) ?
O23 C43 O13 Co1 . . . . 13.17(19) ?
C13 C43 O13 Co1 . . . . -161.17(8) ?
O1W Co1 O13 C43 2_766 . . . 168.07(11) ?
O1W Co1 O13 C43 . . . . -11.93(11) ?
N11 Co1 O13 C43 . . . . -100.58(11) ?
N11 Co1 O13 C43 2_766 . . . 79.42(11) ?
