#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/09/2230914.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_2230914
loop_
_publ_author_name
'Zhu, Xian-Dong'
_publ_section_title
;
 catena-Poly[[[tetraaquacobalt(II)]-μ-4,4'-bipyridine-κ²N:N']
 pyridine-3,5-dicarboxylate trihydrate]
;
_journal_coeditor_code           XU5203
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m970
_journal_page_last               m971
_journal_paper_doi               10.1107/S1600536811023816
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Co (C10 H8 N2) (H2 O)4] (C7 H3 N O4), 3H2 O'
_chemical_formula_moiety         'C10 H16 Co N2 O4 2+, C7 H3 N O4 2-, 3(H2 O)'
_chemical_formula_sum            'C17 H25 Co N3 O11'
_chemical_formula_weight         506.33
_chemical_name_systematic
;
catena-Poly[[[tetraaquacobalt(II)]-μ-4,4'-bipyridine-
κ²N:N'] pyridine-3,5-dicarboxylate trihydrate]
;
_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           SHELXL-97
_cell_angle_alpha                105.352(4)
_cell_angle_beta                 92.837(4)
_cell_angle_gamma                94.624(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0053(18)
_cell_length_b                   11.449(3)
_cell_length_c                   14.077(4)
_cell_measurement_reflns_used    2942
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.0467
_cell_volume                     1082.2(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_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  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8332
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0325
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                4345
_reflns_number_total             4863
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu5203.cif
_cod_data_source_block           I
_cod_database_code               2230914
_cod_database_fobs_code          2230914
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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.38876(3) 0.627012(17) 0.230821(15) 0.02719(11) Uani d . 1 1 . .
O O1 0.88432(18) 0.45647(11) 0.17193(9) 0.0357(3) Uani d . 1 1 . .
O O2 0.8709(2) 0.31057(12) 0.02985(9) 0.0457(3) Uani d . 1 1 . .
O O3 0.8583(2) 0.32631(11) 0.48551(9) 0.0457(3) Uani d . 1 1 . .
O O4 0.8299(3) 0.12902(13) 0.47420(10) 0.0588(4) Uani d . 1 1 . .
N N1 0.3885(2) 0.43762(12) 0.23107(10) 0.0289(3) Uani d . 1 1 . .
N N2 0.3821(2) -0.18489(12) 0.23179(10) 0.0302(3) Uani d . 1 1 . .
N N3 0.8803(2) 0.03959(13) 0.17180(11) 0.0377(3) Uani d . 1 1 . .
C C1 0.3827(3) 0.40339(14) 0.31469(12) 0.0331(4) Uani d . 1 1 . .
H H1 0.3823 0.4648 0.3751 0.040 Uiso calc R 1 1 . .
C C2 0.3773(3) 0.28345(14) 0.31811(12) 0.0313(3) Uani d . 1 1 . .
H H2 0.3750 0.2645 0.3798 0.038 Uiso calc R 1 1 . .
C C3 0.3752(2) 0.19091(13) 0.23145(11) 0.0252(3) Uani d . 1 1 . .
C C4 0.3781(3) 0.22635(14) 0.14371(12) 0.0312(3) Uani d . 1 1 . .
H H4 0.3747 0.1666 0.0821 0.037 Uiso calc R 1 1 . .
C C5 0.3860(3) 0.34851(15) 0.14656(12) 0.0326(3) Uani d . 1 1 . .
H H5 0.3898 0.3704 0.0861 0.039 Uiso calc R 1 1 . .
C C6 0.3733(2) 0.06074(13) 0.23155(11) 0.0261(3) Uani d . 1 1 . .
C C7 0.3486(3) 0.02297(15) 0.31603(13) 0.0380(4) Uani d . 1 1 . .
H H7 0.3283 0.0807 0.3761 0.046 Uiso calc R 1 1 . .
C C8 0.3531(3) -0.09846(15) 0.31378(13) 0.0402(4) Uani d . 1 1 . .
H H8 0.3349 -0.1217 0.3729 0.048 Uiso calc R 1 1 . .
C C9 0.4037(3) -0.14903(14) 0.14960(13) 0.0331(4) Uani d . 1 1 . .
H H9 0.4233 -0.2086 0.0905 0.040 Uiso calc R 1 1 . .
C C10 0.3990(3) -0.02929(14) 0.14642(12) 0.0326(4) Uani d . 1 1 . .
H H10 0.4135 -0.0088 0.0859 0.039 Uiso calc R 1 1 . .
C C11 0.8681(3) 0.07055(16) 0.26959(13) 0.0338(4) Uani d . 1 1 . .
H H11 0.8642 0.0075 0.3020 0.041 Uiso calc R 1 1 . .
C C12 0.8609(2) 0.18844(15) 0.32658(11) 0.0288(3) Uani d . 1 1 . .
C C13 0.8678(2) 0.28087(14) 0.27885(11) 0.0274(3) Uani d . 1 1 . .
H H13 0.8659 0.3633 0.3155 0.033 Uiso calc R 1 1 . .
C C14 0.8773(2) 0.25103(14) 0.17736(11) 0.0262(3) Uani d . 1 1 . .
C C15 0.8837(2) 0.12965(15) 0.12731(12) 0.0327(3) Uani d . 1 1 . .
H H15 0.8908 0.1093 0.0577 0.039 Uiso calc R 1 1 . .
C C16 0.8777(2) 0.34712(14) 0.12216(11) 0.0288(3) Uani d . 1 1 . .
C C17 0.8465(3) 0.21575(15) 0.43678(12) 0.0356(4) Uani d . 1 1 . .
O O1W 0.19781(18) 0.56791(11) 0.10504(8) 0.0357(3) Uani d . 1 1 . .
H H1A 0.1813 0.6024 0.0591 0.043 Uiso d R 1 1 . .
H H1B 0.0898 0.5339 0.1132 0.043 Uiso d R 1 1 . .
O O2W 0.6205(2) 0.61273(12) 0.14338(12) 0.0472(3) Uani d . 1 1 . .
H H2A 0.7040 0.5672 0.1545 0.057 Uiso d R 1 1 . .
H H2B 0.6924 0.6702 0.1320 0.057 Uiso d R 1 1 . .
O O3W 0.14285(19) 0.63665(11) 0.31403(9) 0.0380(3) Uani d . 1 1 . .
H H3A 0.0450 0.5866 0.2905 0.046 Uiso d R 1 1 . .
H H3B 0.1477 0.6495 0.3764 0.046 Uiso d R 1 1 . .
O O4W 0.5585(2) 0.68048(12) 0.36252(11) 0.0510(4) Uani d . 1 1 . .
H H4A 0.6317 0.7466 0.3793 0.061 Uiso d R 1 1 . .
H H4B 0.6193 0.6310 0.3850 0.061 Uiso d R 1 1 . .
O O5W 0.8025(3) 0.87961(16) 0.43207(17) 0.0859(7) Uani d . 1 1 . .
H H5A 0.7997 0.9560 0.4422 0.103 Uiso d R 1 1 . .
H H5B 0.9151 0.8574 0.4258 0.103 Uiso d R 1 1 . .
O O6W 0.8252(2) 0.78607(12) 0.08166(12) 0.0575(4) Uani d . 1 1 . .
H H6A 0.8500 0.8610 0.1118 0.069 Uiso d R 1 1 . .
H H6B 0.9238 0.7623 0.0522 0.069 Uiso d R 1 1 . .
O O7W 0.7707(2) 0.55000(13) 0.45807(11) 0.0552(4) Uani d . 1 1 . .
H H7A 0.8792 0.5902 0.4781 0.066 Uiso d R 1 1 . .
H H7B 0.7806 0.4780 0.4623 0.066 Uiso d R 1 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'
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
_geom_angle_publ_flag
O4W Co1 O2W . . 94.18(7) ?
O4W Co1 O1W . . 174.82(5) ?
O2W Co1 O1W . . 90.62(6) ?
O4W Co1 O3W . . 88.56(6) ?
O2W Co1 O3W . . 177.17(5) ?
O1W Co1 O3W . . 86.62(5) ?
O4W Co1 N2 . 1_565 89.64(5) ?
O2W Co1 N2 . 1_565 90.37(5) ?
O1W Co1 N2 . 1_565 92.30(5) ?
O3W Co1 N2 . 1_565 90.39(5) ?
O4W Co1 N1 . . 90.65(5) ?
O2W Co1 N1 . . 90.96(5) ?
O1W Co1 N1 . . 87.30(5) ?
O3W Co1 N1 . . 88.27(5) ?
N2 Co1 N1 1_565 . 178.62(5) ?
C1 N1 C5 . . 116.80(14) ?
C1 N1 Co1 . . 121.68(11) ?
C5 N1 Co1 . . 121.46(11) ?
C9 N2 C8 . . 116.73(14) ?
C9 N2 Co1 . 1_545 121.19(11) ?
C8 N2 Co1 . 1_545 122.07(11) ?
C11 N3 C15 . . 117.02(15) ?
N1 C1 C2 . . 123.67(15) ?
N1 C1 H1 . . 118.2 ?
C2 C1 H1 . . 118.2 ?
C3 C2 C1 . . 120.00(15) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 116.44(14) ?
C2 C3 C6 . . 121.95(15) ?
C4 C3 C6 . . 121.61(15) ?
C5 C4 C3 . . 120.09(15) ?
C5 C4 H4 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
N1 C5 C4 . . 122.99(15) ?
N1 C5 H5 . . 118.5 ?
C4 C5 H5 . . 118.5 ?
C7 C6 C10 . . 116.35(14) ?
C7 C6 C3 . . 122.19(15) ?
C10 C6 C3 . . 121.46(15) ?
C6 C7 C8 . . 120.48(16) ?
C6 C7 H7 . . 119.8 ?
C8 C7 H7 . . 119.8 ?
N2 C8 C7 . . 122.99(16) ?
N2 C8 H8 . . 118.5 ?
C7 C8 H8 . . 118.5 ?
N2 C9 C10 . . 123.27(16) ?
N2 C9 H9 . . 118.4 ?
C10 C9 H9 . . 118.4 ?
C9 C10 C6 . . 120.15(15) ?
C9 C10 H10 . . 119.9 ?
C6 C10 H10 . . 119.9 ?
N3 C11 C12 . . 124.18(15) ?
N3 C11 H11 . . 117.9 ?
C12 C11 H11 . . 117.9 ?
C11 C12 C13 . . 117.76(15) ?
C11 C12 C17 . . 120.90(14) ?
C13 C12 C17 . . 121.34(15) ?
C14 C13 C12 . . 119.21(15) ?
C14 C13 H13 . . 120.4 ?
C12 C13 H13 . . 120.4 ?
C13 C14 C15 . . 118.25(14) ?
C13 C14 C16 . . 121.12(14) ?
C15 C14 C16 . . 120.63(14) ?
N3 C15 C14 . . 123.56(15) ?
N3 C15 H15 . . 118.2 ?
C14 C15 H15 . . 118.2 ?
O2 C16 O1 . . 125.59(15) ?
O2 C16 C14 . . 116.60(14) ?
O1 C16 C14 . . 117.81(14) ?
O4 C17 O3 . . 124.16(16) ?
O4 C17 C12 . . 118.32(16) ?
O3 C17 C12 . . 117.48(14) ?
Co1 O1W H1A . . 127.7 ?
Co1 O1W H1B . . 115.7 ?
H1A O1W H1B . . 107.9 ?
Co1 O2W H2A . . 116.1 ?
Co1 O2W H2B . . 127.7 ?
H2A O2W H2B . . 100.5 ?
Co1 O3W H3A . . 118.3 ?
Co1 O3W H3B . . 124.0 ?
H3A O3W H3B . . 107.1 ?
Co1 O4W H4A . . 122.4 ?
Co1 O4W H4B . . 122.6 ?
H4A O4W H4B . . 104.3 ?
H5A O5W H5B . . 113.0 ?
H6A O6W H6B . . 107.7 ?
H7A O7W H7B . . 106.9 ?
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 O1W . 2.0898(12) y
Co1 O2W . 2.0764(14) y
Co1 O3W . 2.1245(13) y
Co1 O4W . 2.0709(14) y
Co1 N1 . 2.1692(14) y
Co1 N2 1_565 2.1543(14) y
O1 C16 . 1.258(2) ?
O2 C16 . 1.252(2) ?
O3 C17 . 1.264(2) ?
O4 C17 . 1.242(2) ?
N1 C1 . 1.337(2) ?
N1 C5 . 1.345(2) ?
N2 C9 . 1.337(2) ?
N2 C8 . 1.343(2) ?
N3 C11 . 1.336(2) ?
N3 C15 . 1.340(2) ?
C1 C2 . 1.384(2) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.386(2) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.399(2) ?
C3 C6 . 1.490(2) ?
C4 C5 . 1.385(2) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 C7 . 1.383(2) ?
C6 C10 . 1.389(2) ?
C7 C8 . 1.385(2) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
C9 C10 . 1.386(2) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
C11 C12 . 1.382(2) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.395(2) ?
C12 C17 . 1.509(2) ?
C13 C14 . 1.385(2) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.387(2) ?
C14 C16 . 1.505(2) ?
C15 H15 . 0.9500 ?
O1W H1A . 0.8501 ?
O1W H1B . 0.8499 ?
O2W H2A . 0.8501 ?
O2W H2B . 0.8499 ?
O3W H3A . 0.8500 ?
O3W H3B . 0.8500 ?
O4W H4A . 0.8498 ?
O4W H4B . 0.8499 ?
O5W H5A . 0.8500 ?
O5W H5B . 0.8500 ?
O6W H6A . 0.8499 ?
O6W H6B . 0.8499 ?
O7W H7A . 0.8501 ?
O7W H7B . 0.8499 ?
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 O2 2_665 0.85 1.84 2.6813(19) 173
O1W H1B O1 1_455 0.85 1.96 2.780(2) 162
O2W H2A O1 . 0.85 1.91 2.760(2) 176
O2W H2B O6W . 0.85 1.87 2.707(2) 168
O3W H3A O1 1_455 0.85 2.12 2.897(2) 152
O3W H3B O3 2_666 0.85 1.89 2.7408(19) 176
O4W H4A O5W . 0.85 1.82 2.665(3) 171
O4W H4B O7W . 0.85 1.90 2.734(2) 168
O5W H5A O4 1_565 0.85 1.90 2.747(3) 172
O5W H5B O4 2_766 0.85 2.19 2.856(3) 135
O6W H6A N3 1_565 0.85 1.98 2.829(2) 173
O6W H6B O2 2_765 0.85 1.99 2.830(2) 172
O7W H7A O3 2_766 0.85 1.98 2.828(2) 175
O7W H7B O3 . 0.85 1.96 2.800(2) 168
