#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/69/2016919.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_2016919
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 H10 N2) (H2 O)2] , C12 H10 N2'
_chemical_formula_moiety         'C22 H16 Co N2 O10, C12 H12 N2)'
_chemical_formula_sum            'C34 H28 Co N4 O10'
_chemical_formula_weight         711.53
_chemical_name_systematic
;
poly[[diaqua-μ-2,5-dicarboxybenzene-1,4-dicarboxylato-
μ-1,2-di-4-pyridylethene-cobalt(II)] 1,2-di-4-pyridylethene 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                93.1051(14)
_cell_angle_beta                 113.8441(13)
_cell_angle_gamma                106.2234(14)
_cell_formula_units_Z            1
_cell_length_a                   9.0283(2)
_cell_length_b                   9.6152(2)
_cell_length_c                   10.1064(3)
_cell_measurement_reflns_used    6054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.22
_cell_volume                     756.41(3)
_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 0.926
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12370
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             367
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0298
_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          0.0766
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                3132
_reflns_number_total             3331
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3070.cif
_cod_data_source_block           I
_cod_database_code               2016919
_cod_database_fobs_code          2016919
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 0.01298(9) Uani d S 1 . .
N N11 1.01957(16) 0.65228(13) 0.67162(13) 0.0167(2) Uani d . 1 . .
C C11 1.03383(19) 0.61342(16) 0.80048(16) 0.0192(3) Uani d . 1 . .
H H11 1.0383 0.5174 0.8141 0.023 Uiso calc R 1 . .
C C21 1.0424(2) 0.70658(17) 0.91461(16) 0.0201(3) Uani d . 1 . .
H H21 1.0567 0.6758 1.0055 0.024 Uiso calc R 1 . .
C C31 1.02991(19) 0.84579(16) 0.89522(16) 0.0180(3) Uani d . 1 . .
C C41 1.0187(2) 0.88780(16) 0.76216(16) 0.0190(3) Uani d . 1 . .
H H41 1.0136 0.9830 0.7453 0.023 Uiso calc R 1 . .
C C51 1.01496(19) 0.78910(16) 0.65568(16) 0.0191(3) Uani d . 1 . .
H H51 1.0088 0.8195 0.5662 0.023 Uiso calc R 1 . .
C C61 1.0239(2) 0.94025(17) 1.01034(16) 0.0199(3) Uani d . 1 . .
H H61 1.0560 0.9150 1.1052 0.024 Uiso calc R 1 . .
N N12 0.62629(16) 0.59521(14) 0.84960(14) 0.0199(3) Uani d . 1 . .
C C12 0.5584(2) 0.68283(18) 0.76311(18) 0.0270(3) Uani d . 1 . .
H H12 0.5330 0.6643 0.6617 0.032 Uiso calc R 1 . .
C C22 0.5238(2) 0.79944(18) 0.81624(18) 0.0279(4) Uani d . 1 . .
H H22 0.4767 0.8604 0.7521 0.034 Uiso calc R 1 . .
C C32 0.55852(19) 0.82723(17) 0.96460(17) 0.0208(3) Uani d . 1 . .
C C42 0.6294(2) 0.73470(18) 1.05249(17) 0.0257(3) Uani d . 1 . .
H H42 0.6558 0.7500 1.1543 0.031 Uiso calc R 1 . .
C C52 0.6615(2) 0.62079(18) 0.99221(18) 0.0245(3) Uani d . 1 . .
H H52 0.7101 0.5587 1.0539 0.029 Uiso calc R 1 . .
C C62 0.5236(2) 0.94623(18) 1.03210(18) 0.0240(3) Uani d . 1 . .
H H62 0.5360 0.9462 1.1300 0.029 Uiso calc R 1 . .
C C13 0.65820(18) 0.11433(15) 0.55886(15) 0.0143(3) Uani d . 1 . .
C C23 0.51484(18) 0.14047(15) 0.56273(15) 0.0151(3) Uani d . 1 . .
C C33 0.35838(18) 0.02575(15) 0.50243(15) 0.0158(3) Uani d . 1 . .
H H33 0.2603 0.0436 0.5032 0.019 Uiso calc R 1 . .
C C43 0.82592(18) 0.23614(15) 0.60063(15) 0.0151(3) Uani d . 1 . .
C C53 0.52051(18) 0.28671(16) 0.63096(16) 0.0172(3) Uani d . 1 . .
O O13 0.81410(13) 0.34150(11) 0.53333(11) 0.0168(2) Uani d . 1 . .
O O23 0.96182(13) 0.21851(12) 0.68884(12) 0.0217(2) Uani d . 1 . .
O O33 0.65657(14) 0.35861(12) 0.74754(12) 0.0219(2) Uani d . 1 . .
H H33A 0.642(4) 0.485(3) 0.799(3) 0.077(9) Uiso d . 1 . .
O O43 0.39350(15) 0.32596(13) 0.57317(14) 0.0306(3) Uani d . 1 . .
O O1W 1.19427(14) 0.43673(12) 0.66059(12) 0.0178(2) Uani d . 1 . .
H H1WB 1.258(3) 0.410(3) 0.635(3) 0.041(6) Uiso d . 1 . .
H H1WA 1.136(3) 0.361(3) 0.675(2) 0.036(6) 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(5) ?
O13 Co1 O1W . 2_766 89.99(4) ?
O13 Co1 O1W 2_766 2_766 90.01(4) ?
O13 Co1 O1W . . 90.01(4) y
O13 Co1 O1W 2_766 . 89.99(4) ?
O1W Co1 O1W 2_766 . 180.0 ?
O13 Co1 N11 . . 88.87(4) y
O13 Co1 N11 2_766 . 91.13(4) ?
O1W Co1 N11 2_766 . 91.65(4) ?
O1W Co1 N11 . . 88.35(4) y
O13 Co1 N11 . 2_766 91.13(4) ?
O13 Co1 N11 2_766 2_766 88.87(4) ?
O1W Co1 N11 2_766 2_766 88.35(4) ?
O1W Co1 N11 . 2_766 91.65(4) ?
N11 Co1 N11 . 2_766 180.0 ?
C11 N11 C51 . . 117.22(12) ?
C11 N11 Co1 . . 120.58(10) ?
C51 N11 Co1 . . 122.19(10) ?
N11 C11 C21 . . 123.09(14) ?
N11 C11 H11 . . 118.5 ?
C21 C11 H11 . . 118.5 ?
C11 C21 C31 . . 119.47(14) ?
C11 C21 H21 . . 120.3 ?
C31 C21 H21 . . 120.3 ?
C21 C31 C41 . . 117.52(13) ?
C21 C31 C61 . . 119.91(13) ?
C41 C31 C61 . . 122.54(13) ?
C51 C41 C31 . . 119.05(14) ?
C51 C41 H41 . . 120.5 ?
C31 C41 H41 . . 120.5 ?
N11 C51 C41 . . 123.55(14) ?
N11 C51 H51 . . 118.2 ?
C41 C51 H51 . . 118.2 ?
C61 C61 C31 2_777 . 123.80(18) ?
C61 C61 H61 2_777 . 118.1 ?
C31 C61 H61 . . 118.1 ?
C12 N12 C52 . . 118.97(13) ?
C12 N12 H33A . . 121.5(14) ?
C52 N12 H33A . . 119.2(14) ?
N12 C12 C22 . . 122.19(15) ?
N12 C12 H12 . . 118.9 ?
C22 C12 H12 . . 118.9 ?
C12 C22 C32 . . 119.67(15) ?
C12 C22 H22 . . 120.2 ?
C32 C22 H22 . . 120.2 ?
C42 C32 C22 . . 117.08(14) ?
C42 C32 C62 . . 118.69(14) ?
C22 C32 C62 . . 124.24(14) ?
C52 C42 C32 . . 120.15(15) ?
C52 C42 H42 . . 119.9 ?
C32 C42 H42 . . 119.9 ?
N12 C52 C42 . . 121.93(15) ?
N12 C52 H52 . . 119.0 ?
C42 C52 H52 . . 119.0 ?
C62 C62 C32 2_677 . 125.63(19) ?
C62 C62 H62 2_677 . 117.2 ?
C32 C62 H62 . . 117.2 ?
C33 C13 C23 2_656 . 119.33(13) ?
C33 C13 C43 2_656 . 117.50(12) ?
C23 C13 C43 . . 122.71(12) ?
C33 C23 C13 . . 118.83(13) ?
C33 C23 C53 . . 117.70(12) ?
C13 C23 C53 . . 123.47(13) ?
C13 C33 C23 2_656 . 121.83(13) ?
C13 C33 H33 2_656 . 119.1 ?
C23 C33 H33 . . 119.1 ?
O13 C43 O23 . . 126.62(13) ?
O13 C43 C13 . . 114.91(12) ?
O23 C43 C13 . . 118.26(12) ?
O43 C53 O33 . . 125.13(13) ?
O43 C53 C23 . . 118.05(13) ?
O33 C53 C23 . . 116.80(12) ?
C43 O13 Co1 . . 130.15(9) ?
C53 O33 H33A . . 110.3(13) ?
Co1 O1W H1WB . . 117.5(17) ?
Co1 O1W H1WA . . 100.8(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 . 2.0824(10) y
Co1 O13 2_766 2.0824(10) ?
Co1 O1W 2_766 2.1171(11) ?
Co1 O1W . 2.1171(11) y
Co1 N11 . 2.1251(12) y
Co1 N11 2_766 2.1251(12) ?
N11 C11 . 1.3403(19) ?
N11 C51 . 1.3440(19) ?
C11 C21 . 1.384(2) ?
C11 H11 . 0.9500 ?
C21 C31 . 1.392(2) ?
C21 H21 . 0.9500 ?
C31 C41 . 1.398(2) ?
C31 C61 . 1.465(2) ?
C41 C51 . 1.379(2) ?
C41 H41 . 0.9500 ?
C51 H51 . 0.9500 ?
C61 C61 2_777 1.334(3) ?
C61 H61 . 0.9500 ?
N12 C12 . 1.336(2) ?
N12 C52 . 1.336(2) ?
N12 H33A . 1.22(3) ?
C12 C22 . 1.382(2) ?
C12 H12 . 0.9500 ?
C22 C32 . 1.396(2) ?
C22 H22 . 0.9500 ?
C32 C42 . 1.391(2) ?
C32 C62 . 1.471(2) ?
C42 C52 . 1.379(2) ?
C42 H42 . 0.9500 ?
C52 H52 . 0.9500 ?
C62 C62 2_677 1.330(3) ?
C62 H62 . 0.9500 ?
C13 C33 2_656 1.3936(19) ?
C13 C23 . 1.4006(19) ?
C13 C43 . 1.5105(19) ?
C23 C33 . 1.394(2) ?
C23 C53 . 1.5105(19) ?
C33 C13 2_656 1.3936(19) ?
C33 H33 . 0.9500 ?
C43 O13 . 1.2557(17) ?
C43 O23 . 1.2558(18) ?
C53 O43 . 1.2340(19) ?
C53 O33 . 1.2814(18) ?
O33 H33A . 1.35(3) ?
O1W H1WB . 0.81(3) ?
O1W H1WA . 0.83(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 . 1.35(3) 1.22(3) 2.5759(16) 177(3)
O1W H1WB O43 1_655 0.81(3) 1.92(3) 2.7210(16) 174(2)
O1W H1WA O23 . 0.83(2) 1.83(2) 2.6414(16) 165(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 . . . . 47.47(11) ?
O13 Co1 N11 C11 2_766 . . . -132.53(11) ?
O1W Co1 N11 C11 2_766 . . . 137.42(11) ?
O1W Co1 N11 C11 . . . . -42.58(11) ?
O13 Co1 N11 C51 . . . . -131.22(12) ?
O13 Co1 N11 C51 2_766 . . . 48.78(12) ?
O1W Co1 N11 C51 2_766 . . . -41.26(12) ?
O1W Co1 N11 C51 . . . . 138.74(12) ?
C51 N11 C11 C21 . . . . 0.5(2) ?
Co1 N11 C11 C21 . . . . -178.23(11) ?
N11 C11 C21 C31 . . . . 2.3(2) ?
C11 C21 C31 C41 . . . . -3.5(2) ?
C11 C21 C31 C61 . . . . 174.74(14) ?
C21 C31 C41 C51 . . . . 2.0(2) ?
C61 C31 C41 C51 . . . . -176.16(14) ?
C11 N11 C51 C41 . . . . -2.1(2) ?
Co1 N11 C51 C41 . . . . 176.61(11) ?
C31 C41 C51 N11 . . . . 0.8(2) ?
C21 C31 C61 C61 . . . 2_777 -165.20(19) ?
C41 C31 C61 C61 . . . 2_777 12.9(3) ?
C52 N12 C12 C22 . . . . 0.2(3) ?
N12 C12 C22 C32 . . . . -0.7(3) ?
C12 C22 C32 C42 . . . . 0.8(3) ?
C12 C22 C32 C62 . . . . -178.72(16) ?
C22 C32 C42 C52 . . . . -0.4(2) ?
C62 C32 C42 C52 . . . . 179.10(16) ?
C12 N12 C52 C42 . . . . 0.2(2) ?
C32 C42 C52 N12 . . . . -0.1(3) ?
C42 C32 C62 C62 . . . 2_677 171.3(2) ?
C22 C32 C62 C62 . . . 2_677 -9.2(3) ?
C33 C13 C23 C33 2_656 . . . -1.2(2) ?
C43 C13 C23 C33 . . . . 170.81(13) ?
C33 C13 C23 C53 2_656 . . . 177.99(13) ?
C43 C13 C23 C53 . . . . -10.0(2) ?
C13 C23 C33 C13 . . . 2_656 1.2(2) ?
C53 C23 C33 C13 . . . 2_656 -178.01(13) ?
C33 C13 C43 O13 2_656 . . . 118.33(14) ?
C23 C13 C43 O13 . . . . -53.78(18) ?
C33 C13 C43 O23 2_656 . . . -56.73(18) ?
C23 C13 C43 O23 . . . . 131.16(15) ?
C33 C23 C53 O43 . . . . -35.65(19) ?
C13 C23 C53 O43 . . . . 145.19(15) ?
C33 C23 C53 O33 . . . . 142.57(14) ?
C13 C23 C53 O33 . . . . -36.6(2) ?
O23 C43 O13 Co1 . . . . 15.1(2) ?
C13 C43 O13 Co1 . . . . -159.49(9) ?
O1W Co1 O13 C43 2_766 . . . 167.20(12) ?
O1W Co1 O13 C43 . . . . -12.80(12) ?
N11 Co1 O13 C43 . . . . -101.15(12) ?
N11 Co1 O13 C43 2_766 . . . 78.85(12) ?
