#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/93/2209351.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_2209351
loop_
_publ_author_name
'Hao, Zhi-Feng'
'Li, Hai-Feng'
'Chen, Yao-Wen'
'Zhang, Yao-Fang'
_publ_section_title
;(μ-p-Phenylenediaminetetraacetato)bis[aqua(2,2'-bipyridine)cobalt(II)]
 tetrahydrate
;
_journal_coeditor_code           XU2028
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1346
_journal_page_last               m1347
_journal_paper_doi               10.1107/S1600536806015753
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Co2 (C14 H12 N2 O8) (C10 H8 N2)2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C34 H32 Co2 N6 O10, 4H2 O'
_chemical_formula_sum            'C34 H40 Co2 N6 O14'
_chemical_formula_weight         874.58
_chemical_name_systematic
;
Diaqua-bis(2,2'-bipyridine)-dicobalt(II)
(μ-p-phenylenediamine-N,N,N',N'-tetraacetato)
tetrahydrate
;
_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                66.108(2)
_cell_angle_beta                 75.257(2)
_cell_angle_gamma                86.508(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8813(9)
_cell_length_b                   9.9042(9)
_cell_length_c                   10.8240(10)
_cell_measurement_reflns_used    1700
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.1
_cell_volume                     935.58(15)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker APEX area-dectector'
_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  0.016
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6768
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.031
_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)+(0.0423P)²+0.2519P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.076
_refine_ls_wR_factor_ref         0.078
_reflns_number_gt                2976
_reflns_number_total             3278
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2028.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        935.59(15)
_cod_database_code               2209351
_cod_database_fobs_code          2209351
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
O O6 0.7527(2) 0.3088(3) 0.6459(2) 0.0620(5) Uani d D 1
Co Co1 0.77246(3) 0.84133(3) 0.70566(3) 0.02853(11) Uani d . 1
O O1 0.80423(16) 0.88843(16) 0.86295(15) 0.0377(4) Uani d . 1
O O4 0.97254(14) 0.78061(15) 0.64011(15) 0.0368(4) Uani d . 1
O O5W 0.80799(17) 1.06175(17) 0.56758(17) 0.0411(4) Uani d D 1
N N2 0.55431(17) 0.87833(19) 0.75897(18) 0.0334(4) Uani d . 1
N N1 0.78332(16) 0.60972(18) 0.87061(17) 0.0290(4) Uani d . 1
N N3 0.68953(18) 0.77378(19) 0.57546(18) 0.0334(4) Uani d . 1
C C2 0.6421(2) 0.5481(2) 0.9384(2) 0.0293(4) Uani d . 1
C C4 0.9964(2) 0.6426(2) 0.6836(2) 0.0365(5) Uani d . 1
H H4 0.626 0.431 0.825 0.043 Uiso d . 1
C C13 0.5492(2) 0.7755(2) 0.5950(2) 0.0346(5) Uani d . 1
C C1 0.5777(2) 0.4616(2) 0.8945(2) 0.0361(5) Uani d . 1
H H1 0.601 0.641 1.079 0.043 Uiso d . 1
C C18 0.8756(2) 0.5374(2) 0.7874(2) 0.0348(5) Uani d . 1
H H18A 0.8224 0.5075 0.7380 0.042 Uiso calc R 1
H H18B 0.9116 0.4495 0.8489 0.042 Uiso calc R 1
O O3 0.8945(2) 0.8112(2) 1.0454(2) 0.0649(5) Uani d . 1
O O2 1.10696(17) 0.59163(19) 0.64410(19) 0.0596(5) Uani d . 1
C C12 0.4731(2) 0.8328(2) 0.6997(2) 0.0359(5) Uani d . 1
C C6 0.8506(2) 0.7899(2) 0.9585(2) 0.0356(5) Uani d . 1
C C3 0.5621(2) 0.5850(2) 1.0447(2) 0.0363(5) Uani d . 1
C C19 0.8569(2) 0.6345(2) 0.9632(2) 0.0341(5) Uani d . 1
H H19A 0.9544 0.6123 0.9380 0.041 Uiso calc R 1
H H19B 0.8168 0.5656 1.0585 0.041 Uiso calc R 1
C C11 0.3294(3) 0.8440(3) 0.7325(3) 0.0575(7) Uani d . 1
H H11 0.2743 0.8111 0.6913 0.069 Uiso calc R 1
C C14 0.4830(3) 0.7301(3) 0.5199(3) 0.0512(6) Uani d . 1
H H14 0.3859 0.7294 0.5369 0.061 Uiso calc R 1
C C8 0.4932(2) 0.9372(3) 0.8493(3) 0.0465(6) Uani d . 1
H H8 0.5495 0.9697 0.8897 0.056 Uiso calc R 1
C C17 0.7641(2) 0.7311(3) 0.4766(2) 0.0426(5) Uani d . 1
H H17 0.8611 0.7313 0.4615 0.051 Uiso calc R 1
C C15 0.5617(3) 0.6860(3) 0.4194(3) 0.0559(7) Uani d . 1
H H15 0.5183 0.6559 0.3674 0.067 Uiso calc R 1
C C16 0.7045(3) 0.6870(3) 0.3966(3) 0.0519(6) Uani d . 1
H H16 0.7597 0.6584 0.3286 0.062 Uiso calc R 1
C C10 0.2687(3) 0.9042(4) 0.8264(3) 0.0639(8) Uani d . 1
H H10 0.1721 0.9122 0.8494 0.077 Uiso calc R 1
C C9 0.3512(3) 0.9523(3) 0.8855(3) 0.0580(7) Uani d . 1
H H9 0.3123 0.9941 0.9488 0.070 Uiso calc R 1
O O7 0.0594(2) 0.8327(2) 0.2079(2) 0.0695(6) Uani d D 1
H H5WA 0.783(3) 1.123(3) 0.603(3) 0.065(9) Uiso d D 1
H H5WB 0.8838(18) 1.097(3) 0.506(2) 0.067(9) Uiso d D 1
H H6WA 0.812(2) 0.279(3) 0.693(3) 0.058(9) Uiso d D 1
H H6WB 0.801(3) 0.361(3) 0.5646(18) 0.093(13) Uiso d D 1
H H7WB 0.017(3) 0.826(4) 0.153(3) 0.081(11) Uiso d D 1
H H7WA 0.089(3) 0.9218(15) 0.173(3) 0.079(11) Uiso d 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
H6WA O6 H6WB . . 104(3) ?
O1 Co1 O4 . . 97.82(6) yes
O1 Co1 O5W . . 91.47(6) yes
O4 Co1 O5W . . 95.18(6) yes
O1 Co1 N3 . . 165.84(6) yes
O4 Co1 N3 . . 93.84(6) yes
O5W Co1 N3 . . 95.47(7) yes
O1 Co1 N2 . . 91.37(6) yes
O4 Co1 N2 . . 169.70(6) yes
O5W Co1 N2 . . 89.20(7) yes
N3 Co1 N2 . . 76.44(7) yes
O1 Co1 N1 . . 78.75(6) yes
O4 Co1 N1 . . 75.90(6) yes
O5W Co1 N1 . . 165.56(6) yes
N3 Co1 N1 . . 96.44(6) yes
N2 Co1 N1 . . 101.52(6) yes
C6 O1 Co1 . . 118.95(13) ?
C4 O4 Co1 . . 118.27(13) ?
Co1 O5W H5WA . . 115(2) ?
Co1 O5W H5WB . . 124(2) ?
H5WA O5W H5WB . . 107(3) ?
C8 N2 C12 . . 118.31(19) ?
C8 N2 Co1 . . 125.32(16) ?
C12 N2 Co1 . . 116.32(14) ?
C2 N1 C18 . . 117.09(16) ?
C2 N1 C19 . . 114.13(16) ?
C18 N1 C19 . . 110.06(16) ?
C2 N1 Co1 . . 107.95(12) ?
C18 N1 Co1 . . 102.15(12) ?
C19 N1 Co1 . . 103.86(11) ?
C17 N3 C13 . . 117.94(19) ?
C17 N3 Co1 . . 125.82(15) ?
C13 N3 Co1 . . 116.24(14) ?
C1 C2 C3 . . 117.59(19) ?
C1 C2 N1 . . 122.48(18) ?
C3 C2 N1 . . 119.73(18) ?
O2 C4 O4 . . 124.7(2) ?
O2 C4 C18 . . 118.93(19) ?
O4 C4 C18 . . 116.33(17) ?
N3 C13 C14 . . 121.6(2) ?
N3 C13 C12 . . 115.44(18) ?
C14 C13 C12 . . 122.9(2) ?
C2 C1 C3 . 2_667 120.5(2) ?
C2 C1 H4 . . 122.2 ?
C3 C1 H4 2_667 . 117.3 ?
N1 C18 C4 . . 110.16(17) ?
N1 C18 H18A . . 109.6 ?
C4 C18 H18A . . 109.6 ?
N1 C18 H18B . . 109.6 ?
C4 C18 H18B . . 109.6 ?
H18A C18 H18B . . 108.1 ?
N2 C12 C11 . . 121.2(2) ?
N2 C12 C13 . . 115.21(18) ?
C11 C12 C13 . . 123.6(2) ?
O3 C6 O1 . . 124.9(2) ?
O3 C6 C19 . . 117.3(2) ?
O1 C6 C19 . . 117.76(18) ?
C1 C3 C2 2_667 . 121.9(2) ?
C1 C3 H1 2_667 . 117.5 ?
C2 C3 H1 . . 120.6 ?
N1 C19 C6 . . 114.87(17) ?
N1 C19 H19A . . 108.5 ?
C6 C19 H19A . . 108.5 ?
N1 C19 H19B . . 108.5 ?
C6 C19 H19B . . 108.5 ?
H19A C19 H19B . . 107.5 ?
C10 C11 C12 . . 119.5(2) ?
C10 C11 H11 . . 120.3 ?
C12 C11 H11 . . 120.3 ?
C15 C14 C13 . . 119.4(2) ?
C15 C14 H14 . . 120.3 ?
C13 C14 H14 . . 120.3 ?
N2 C8 C9 . . 123.2(2) ?
N2 C8 H8 . . 118.4 ?
C9 C8 H8 . . 118.4 ?
N3 C17 C16 . . 123.2(2) ?
N3 C17 H17 . . 118.4 ?
C16 C17 H17 . . 118.4 ?
C16 C15 C14 . . 119.4(2) ?
C16 C15 H15 . . 120.3 ?
C14 C15 H15 . . 120.3 ?
C15 C16 C17 . . 118.4(2) ?
C15 C16 H16 . . 120.8 ?
C17 C16 H16 . . 120.8 ?
C9 C10 C11 . . 119.4(2) ?
C9 C10 H10 . . 120.3 ?
C11 C10 H10 . . 120.3 ?
C10 C9 C8 . . 118.3(2) ?
C10 C9 H9 . . 120.8 ?
C8 C9 H9 . . 120.8 ?
H7WB O7 H7WA . . 106(3) ?
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 N1 . 2.2828(17) yes
Co1 N2 . 2.1345(17) yes
Co1 N3 . 2.1268(17) yes
Co1 O1 . 2.0366(15) yes
Co1 O4 . 2.0642(14) yes
Co1 O5W . 2.0752(16) yes
O1 C6 . 1.265(3) ?
O4 C4 . 1.281(3) ?
O5W H5WA . 0.84(3) ?
O5W H5WB . 0.846(19) ?
N2 C8 . 1.334(3) ?
N2 C12 . 1.341(3) ?
N1 C2 . 1.441(2) ?
N1 C18 . 1.477(3) ?
N1 C19 . 1.479(3) ?
N3 C17 . 1.339(3) ?
N3 C13 . 1.348(3) ?
C2 C1 . 1.384(3) ?
C2 C3 . 1.387(3) ?
C4 O2 . 1.226(3) ?
C4 C18 . 1.515(3) ?
C13 C14 . 1.376(3) ?
C13 C12 . 1.486(3) ?
C1 C3 2_667 1.387(3) ?
C1 H4 . 0.9300 ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
O3 C6 . 1.224(3) ?
C12 C11 . 1.382(3) ?
C6 C19 . 1.517(3) ?
C3 C1 2_667 1.387(3) ?
C3 H1 . 0.9300 ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
C11 C10 . 1.373(4) ?
C11 H11 . 0.9300 ?
C14 C15 . 1.375(4) ?
C14 H14 . 0.9300 ?
C8 C9 . 1.374(3) ?
C8 H8 . 0.9300 ?
C17 C16 . 1.374(3) ?
C17 H17 . 0.9300 ?
C15 C16 . 1.369(4) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
C10 C9 . 1.364(4) ?
C10 H10 . 0.9300 ?
C9 H9 . 0.9300 ?
O6 H6WA . 0.84(2) ?
O6 H6WB . 0.85(2) ?
O7 H7WB . 0.83(3) ?
O7 H7WA . 0.84(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
O5W H5WA O6 1_565 0.84(3) 2.06(3) 2.879(4) 166(3)
O5W H5WB O4 2_776 0.846(19) 1.87(2) 2.699(2) 165(3)
O6 H6WA O7 2_666 0.84(2) 1.88(3) 2.701(3) 165(3)
O6 H6WB O2 2_766 0.85(2) 2.073(19) 2.862(3) 155(3)
O7 H7WA O1 2_676 0.84(2) 2.06(2) 2.871(3) 161(3)
O7 H7WB O3 1_454 0.83(3) 1.93(3) 2.757(3) 172(3)
