#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/56/2015665.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_2015665
loop_
_publ_author_name
'Lah, Nina'
'Leban, Ivan'
_publ_section_title
;
 A dimeric cobalt(II)--suberate complex with 3-aminopyridine
;
_journal_coeditor_code           SK3064
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m550
_journal_page_last               m552
_journal_paper_doi               10.1107/S0108270106040935
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co2 (C5 H6 N2)4 (C H4 O)2 Cl2 (C8 H12 O4)]'
_chemical_formula_moiety         'C30 H44 Cl2 Co2 N8 O6'
_chemical_formula_sum            'C30 H44 Cl2 Co2 N8 O6'
_chemical_formula_weight         801.49
_chemical_name_systematic
;
 tetrakis(3-aminopyridine)dichloro-bis(methanol)-μ2-suberato-dicobalt(II)
;
_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                104.5050(10)
_cell_angle_beta                 106.0520(10)
_cell_angle_gamma                95.8880(10)
_cell_formula_units_Z            1
_cell_length_a                   7.3955(2)
_cell_length_b                   11.2390(3)
_cell_length_c                   11.7463(3)
_cell_measurement_reflns_used    3157
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.00
_cell_volume                     892.73(4)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO AND SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia,1997)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans at κ=55°'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6468
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0222P)²+0.7104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                3185
_reflns_number_total             3599
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3064.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2015665
_cod_database_fobs_code          2015665
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
Co Co1 0.83083(4) 0.36023(2) 0.26676(2) 0.01840(9) Uani d . 1
Cl Cl1 1.09870(7) 0.48057(5) 0.24732(4) 0.02239(12) Uani d . 1
O O1 0.92758(19) 0.32824(13) 0.44642(12) 0.0217(3) Uani d . 1
O O2 0.6284(2) 0.26129(13) 0.33218(13) 0.0246(3) Uani d . 1
C C1 0.7627(3) 0.26816(18) 0.42889(18) 0.0210(4) Uani d . 1
C C2 0.7289(3) 0.2055(2) 0.5226(2) 0.0262(5) Uani d . 1
H H2A 0.6108 0.1445 0.4846 0.031 Uiso calc R 1
H H2B 0.7131 0.2678 0.5913 0.031 Uiso calc R 1
C C3 0.8914(4) 0.1401(2) 0.5725(2) 0.0347(5) Uani d . 1
H H3A 1.0099 0.2009 0.6086 0.042 Uiso calc R 1
H H3B 0.8665 0.1097 0.6381 0.042 Uiso calc R 1
C C4 0.9180(4) 0.0319(2) 0.4762(2) 0.0348(5) Uani d . 1
H H4A 0.9394 0.0620 0.4096 0.042 Uiso calc R 1
H H4B 0.8005 -0.0297 0.4416 0.042 Uiso calc R 1
N N11 0.6291(2) 0.34125(15) 0.09381(15) 0.0220(4) Uani d . 1
C C12 0.4518(3) 0.36211(18) 0.0832(2) 0.0242(4) Uani d . 1
H H12 0.4129 0.3792 0.1535 0.029 Uiso calc R 1
C C13 0.3210(3) 0.35911(19) -0.0311(2) 0.0281(5) Uani d . 1
C C14 0.3824(3) 0.3329(2) -0.1349(2) 0.0328(5) Uani d . 1
H H14 0.3005 0.3310 -0.2115 0.039 Uiso calc R 1
C C15 0.5631(3) 0.3099(2) -0.1240(2) 0.0328(5) Uani d . 1
H H15 0.6048 0.2914 -0.1932 0.039 Uiso calc R 1
C C16 0.6838(3) 0.3144(2) -0.00876(19) 0.0274(5) Uani d . 1
H H16 0.8067 0.2983 -0.0019 0.033 Uiso calc R 1
N N12 0.1381(3) 0.37748(19) -0.0389(2) 0.0345(5) Uani d . 1
N N21 0.9065(2) 0.18399(15) 0.19406(15) 0.0206(4) Uani d . 1
C C22 1.0871(3) 0.16606(19) 0.22372(19) 0.0231(4) Uani d . 1
H H22 1.1840 0.2353 0.2676 0.028 Uiso calc R 1
C C23 1.1384(3) 0.0490(2) 0.19239(19) 0.0244(4) Uani d . 1
C C24 0.9901(3) -0.05349(19) 0.1266(2) 0.0269(5) Uani d . 1
H H24 1.0166 -0.1336 0.1039 0.032 Uiso calc R 1
C C25 0.8037(3) -0.0341(2) 0.0958(2) 0.0276(5) Uani d . 1
H H25 0.7035 -0.1012 0.0513 0.033 Uiso calc R 1
C C26 0.7663(3) 0.08437(19) 0.13102(19) 0.0249(5) Uani d . 1
H H26 0.6399 0.0959 0.1105 0.030 Uiso calc R 1
N N22 1.3262(3) 0.0353(2) 0.2280(2) 0.0361(5) Uani d . 1
O O1M 0.7753(2) 0.53724(14) 0.35736(13) 0.0205(3) Uani d . 1
C C1M 0.6415(3) 0.5548(2) 0.4250(2) 0.0319(5) Uani d . 1
H H1A 0.5157 0.5126 0.3716 0.048 Uiso calc R 1
H H1B 0.6414 0.6425 0.4550 0.048 Uiso calc R 1
H H1C 0.6775 0.5212 0.4938 0.048 Uiso calc R 1
H H1M 0.873(4) 0.574(3) 0.398(2) 0.035(8) Uiso d . 1
H H22A 1.407(4) 0.100(3) 0.253(3) 0.047(8) Uiso d . 1
H H12A 0.130(4) 0.419(3) 0.043(3) 0.062(9) Uiso d . 1
H H22B 1.354(4) -0.034(3) 0.196(3) 0.052(9) Uiso d . 1
H H12B 0.073(5) 0.413(3) -0.110(3) 0.070(10) 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'
Cl Cl 0.1484 0.1585 '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
N11 Co1 O1M . . 95.08(6) no
N11 Co1 N21 . . 90.75(6) no
O1M Co1 N21 . . 174.16(6) no
N11 Co1 O1 . . 154.37(6) no
O1M Co1 O1 . . 88.17(5) no
N21 Co1 O1 . . 86.44(6) no
N11 Co1 O2 . . 94.26(6) no
O1M Co1 O2 . . 90.97(6) no
N21 Co1 O2 . . 88.29(6) no
O1 Co1 O2 . . 60.21(5) no
N11 Co1 Cl1 . . 99.58(5) no
O1M Co1 Cl1 . . 85.16(4) no
N21 Co1 Cl1 . . 94.17(5) no
O1 Co1 Cl1 . . 106.03(4) no
O2 Co1 Cl1 . . 165.89(4) no
C1 O1 Co1 . . 90.65(11) no
C1 O2 Co1 . . 89.72(12) no
O2 C1 O1 . . 119.22(18) no
O2 C1 C2 . . 120.82(18) no
O1 C1 C2 . . 119.96(18) no
C1 C2 C3 . . 113.29(18) no
C1 C2 H2A . . 108.9 no
C3 C2 H2A . . 108.9 no
C1 C2 H2B . . 108.9 no
C3 C2 H2B . . 108.9 no
H2A C2 H2B . . 107.7 no
C4 C3 C2 . . 114.22(19) no
C4 C3 H3A . . 108.7 no
C2 C3 H3A . . 108.7 no
C4 C3 H3B . . 108.7 no
C2 C3 H3B . . 108.7 no
H3A C3 H3B . . 107.6 no
C3 C4 C4 . 2_756 114.8(2) no
C3 C4 H4A . . 108.6 no
C4 C4 H4A 2_756 . 108.6 no
C3 C4 H4B . . 108.6 no
C4 C4 H4B 2_756 . 108.6 no
H4A C4 H4B . . 107.5 no
C12 N11 C16 . . 118.68(18) no
C12 N11 Co1 . . 122.06(14) no
C16 N11 Co1 . . 119.15(14) no
N11 C12 C13 . . 122.3(2) no
N11 C12 H12 . . 118.9 no
C13 C12 H12 . . 118.9 no
N12 C13 C14 . . 121.7(2) no
N12 C13 C12 . . 120.5(2) no
C14 C13 C12 . . 117.7(2) no
C15 C14 C13 . . 119.9(2) no
C15 C14 H14 . . 120.1 no
C13 C14 H14 . . 120.1 no
C14 C15 C16 . . 119.2(2) no
C14 C15 H15 . . 120.4 no
C16 C15 H15 . . 120.4 no
N11 C16 C15 . . 122.2(2) no
N11 C16 H16 . . 118.9 no
C15 C16 H16 . . 118.9 no
C13 N12 H12A . . 110.8(18) no
C13 N12 H12B . . 115.0(18) no
H12A N12 H12B . . 116(3) no
C22 N21 C26 . . 118.41(18) no
C22 N21 Co1 . . 122.13(13) no
C26 N21 Co1 . . 118.80(14) no
N21 C22 C23 . . 123.50(19) no
N21 C22 H22 . . 118.2 no
C23 C22 H22 . . 118.2 no
N22 C23 C22 . . 121.1(2) no
N22 C23 C24 . . 121.7(2) no
C22 C23 C24 . . 117.09(19) no
C25 C24 C23 . . 119.0(2) no
C25 C24 H24 . . 120.5 no
C23 C24 H24 . . 120.5 no
C26 C25 C24 . . 119.9(2) no
C26 C25 H25 . . 120.0 no
C24 C25 H25 . . 120.0 no
N21 C26 C25 . . 122.0(2) no
N21 C26 H26 . . 119.0 no
C25 C26 H26 . . 119.0 no
C23 N22 H22A . . 116(2) no
C23 N22 H22B . . 118(2) no
H22A N22 H22B . . 120(3) no
C1M O1M Co1 . . 125.62(13) no
C1M O1M H1M . . 110(2) no
Co1 O1M H1M . . 104(2) no
O1M C1M H1A . . 109.5 no
O1M C1M H1B . . 109.5 no
H1A C1M H1B . . 109.5 no
O1M C1M H1C . . 109.5 no
H1A C1M H1C . . 109.5 no
H1B C1M H1C . . 109.5 no
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 N11 . 2.1070(16) yes
Co1 O1M . 2.1466(15) yes
Co1 N21 . 2.1470(17) yes
Co1 O1 . 2.1662(13) yes
Co1 O2 . 2.1887(14) yes
Co1 Cl1 . 2.3793(5) yes
O1 C1 . 1.268(2) no
O2 C1 . 1.264(2) no
C1 C2 . 1.508(3) no
C2 C3 . 1.529(3) no
C2 H2A . 0.9700 no
C2 H2B . 0.9700 no
C3 C4 . 1.510(3) no
C3 H3A . 0.9700 no
C3 H3B . 0.9700 no
C4 C4 2_756 1.516(5) no
C4 H4A . 0.9700 no
C4 H4B . 0.9700 no
N11 C12 . 1.334(3) no
N11 C16 . 1.348(3) no
C12 C13 . 1.411(3) no
C12 H12 . 0.9300 no
C13 N12 . 1.371(3) no
C13 C14 . 1.390(3) no
C14 C15 . 1.365(3) no
C14 H14 . 0.9300 no
C15 C16 . 1.386(3) no
C15 H15 . 0.9300 no
C16 H16 . 0.9300 no
N12 H12A . 0.98(3) no
N12 H12B . 1.04(3) no
N21 C22 . 1.334(3) no
N21 C26 . 1.341(3) no
C22 C23 . 1.396(3) no
C22 H22 . 0.9300 no
C23 N22 . 1.371(3) no
C23 C24 . 1.397(3) no
C24 C25 . 1.380(3) no
C24 H24 . 0.9300 no
C25 C26 . 1.372(3) no
C25 H25 . 0.9300 no
C26 H26 . 0.9300 no
N22 H22A . 0.83(3) no
N22 H22B . 0.85(3) no
O1M C1M . 1.430(3) no
O1M H1M . 0.75(3) no
C1M H1A . 0.9600 no
C1M H1B . 0.9600 no
C1M H1C . 0.9600 no
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
O1M H1M O1 2_766 0.75(3) 1.98(3) 2.683(2) 156(3)
N22 H22A O2 1_655 0.83(3) 2.13(3) 2.952(3) 175(3)
N12 H12A Cl1 1_455 0.98(3) 2.41(3) 3.375(2) 169(3)
N12 H12B Cl1 2_665 1.04(3) 2.40(3) 3.430(2) 169(3)
