#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/37/2213766.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_2213766
loop_
_publ_author_name
'Han, Ke-Fei'
'Chen, He-Yan'
'Wang, Zhong-Ming'
_publ_section_title
;
 trans-Tetraaquabis(1,3-di-4-pyridylpropane-κN)cobalt(II)
 naphthalene-1,5-disulfonate monohydrate
;
_journal_coeditor_code           FJ2023
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1695
_journal_page_last               m1696
_journal_paper_doi               10.1107/S1600536807023446
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Co (C13 H14 N2)2 (H2 O)4](C10 H6 O6 S2), H2 O'
_chemical_formula_moiety
;
C26 H36 Co N4 O4 2+, C10 H6 O6 S2 2-, H2 O
;
_chemical_formula_sum            'C36 H44 Co N4 O11 S2'
_chemical_formula_weight         849.82
_chemical_name_systematic
;
trans-Tetraaquabis(1,3-di-4-pyridylpropane-κN)cobalt(II)
naphthalene-1,5-disulfonate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.844(2)
_cell_length_b                   8.3912(17)
_cell_length_c                   20.035(4)
_cell_measurement_reflns_used    17625
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.73
_cell_volume                     1973.9(7)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku 2001)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 1997b) and Mercury (Macrae et al.,
2006)
;
_computing_publication_material
;
SHELXL97 and WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-axis Rapid IP area-detector'
_diffrn_measurement_method       'ω Oscillation'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17625
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.8067
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.43
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0633P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                3259
_reflns_number_total             4418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fj2023.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213766
_cod_database_fobs_code          2213766
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0 0 0 0.03243(4) Uani d S 1 . .
S S1 0.747491(16) 0.35189(3) 0.086588(11) 0.04424(6) Uani d . 1 . .
N N1 0.05768(5) 0.16358(9) 0.07838(3) 0.03629(17) Uani d . 1 A .
N N2 0.71693(6) 0.35709(11) 0.35647(4) 0.0559(2) Uani d . 1 . .
O O1 0.09129(4) -0.18980(7) 0.05235(3) 0.04155(16) Uani d . 1 . .
O O2 -0.14437(5) -0.05367(8) 0.04662(3) 0.04633(17) Uani d . 1 . .
O O6 0.76383(6) 0.47271(9) 0.13864(3) 0.0592(2) Uani d . 1 . .
O O4 0.76400(5) 0.19127(8) 0.11191(4) 0.0585(2) Uani d . 1 . .
O O5 0.81263(5) 0.38569(8) 0.03177(3) 0.05015(18) Uani d . 1 . .
C C1 0.04884(7) 0.12998(12) 0.14243(4) 0.0447(2) Uani d . 1 . .
H H1 0.0158 0.0337 0.1523 0.054 Uiso calc R 1 . .
C C2 0.08631(7) 0.23099(13) 0.19450(5) 0.0498(3) Uani d . 1 A .
H H2 0.0775 0.203 0.2384 0.06 Uiso calc R 1 . .
C C3 0.13715(6) 0.37430(12) 0.18186(4) 0.0434(2) Uani d . 1 . .
C C4 0.14654(7) 0.40891(12) 0.11582(5) 0.0459(2) Uani d . 1 A .
H H4 0.1805 0.5036 0.1048 0.055 Uiso calc R 1 . .
C C5 0.10545(7) 0.30265(11) 0.06603(4) 0.0423(2) Uani d . 1 . .
H H5 0.1113 0.3292 0.0216 0.051 Uiso calc R 1 A .
C C6 0.18164(8) 0.48559(13) 0.23797(5) 0.0579(3) Uani d P 0.5 A 1
H H6A 0.1227 0.5047 0.2664 0.069 Uiso calc PR 0.5 A 1
H H6B 0.2013 0.5869 0.2192 0.069 Uiso calc PR 0.5 A 1
C C7 0.28932(14) 0.4136(3) 0.28140(9) 0.0529(5) Uani d P 0.5103(12) A 1
H H7A 0.3116 0.4813 0.3201 0.063 Uiso calc PR 0.5103(12) A 1
H H7B 0.2712 0.309 0.2976 0.063 Uiso calc PR 0.5103(12) A 1
C C8 0.38620(15) 0.4003(2) 0.24030(10) 0.0507(4) Uiso d P 0.5103(12) A 1
H H8A 0.3953 0.4995 0.2168 0.061 Uiso calc PR 0.5103(12) A 1
H H8B 0.3711 0.3159 0.2072 0.061 Uiso calc PR 0.5103(12) A 1
C C6' 0.18164(8) 0.48559(13) 0.23797(5) 0.0579(3) Uani d P 0.5 A 2
H H6'A 0.1556 0.449 0.2793 0.069 Uiso calc PR 0.5 A 2
H H6'B 0.1496 0.5907 0.228 0.069 Uiso calc PR 0.5 A 2
C C7' 0.31428(14) 0.4992(2) 0.24959(10) 0.0461(5) Uani d P 0.4897(12) A 2
H H7'A 0.3413 0.5425 0.2097 0.055 Uiso calc PR 0.4897(12) A 2
H H7'B 0.3376 0.5707 0.2869 0.055 Uiso calc PR 0.4897(12) A 2
C C8' 0.36579(16) 0.3346(3) 0.26491(11) 0.0546(5) Uiso d P 0.4897(12) A 2
H H8'A 0.3555 0.2683 0.2249 0.066 Uiso calc PR 0.4897(12) A 2
H H8'B 0.3299 0.2828 0.3 0.066 Uiso calc PR 0.4897(12) A 2
C C9 0.49568(8) 0.36248(15) 0.28889(6) 0.0698(3) Uani d . 1 . .
C C10 0.51811(9) 0.31754(17) 0.35430(6) 0.0756(4) Uani d . 1 A .
H H10 0.4588 0.2874 0.3777 0.091 Uiso calc R 1 . .
C C11 0.62792(9) 0.31639(16) 0.38596(6) 0.0682(4) Uani d . 1 . .
H H11 0.6405 0.2851 0.4309 0.082 Uiso calc R 1 A .
C C12 0.69455(9) 0.39956(14) 0.29287(5) 0.0620(3) Uani d . 1 . .
H H12 0.7553 0.4277 0.2703 0.074 Uiso calc R 1 A .
C C13 0.58737(9) 0.40483(16) 0.25804(6) 0.0714(4) Uani d . 1 A .
H H13 0.5769 0.4373 0.2133 0.086 Uiso calc R 1 . .
C C14 0.53333(7) 0.23713(12) 0.06039(5) 0.0537(3) Uani d . 1 . .
H H14 0.5629 0.1496 0.0853 0.064 Uiso calc R 1 . .
C C15 0.60165(6) 0.36363(11) 0.05135(4) 0.0416(2) Uani d . 1 . .
C C16 0.55874(6) 0.50062(10) 0.01431(4) 0.0402(2) Uani d . 1 . .
C C17 0.62546(7) 0.63484(12) 0.00435(5) 0.0509(3) Uani d . 1 . .
H H17 0.7014 0.6369 0.0233 0.061 Uiso calc R 1 . .
C C18 0.58165(8) 0.76140(13) -0.03229(6) 0.0604(3) Uani d . 1 . .
H H18 0.6281 0.8479 -0.0389 0.072 Uiso calc R 1 . .
O O3 0.91963(6) 0.70891(10) 0.13413(4) 0.0646(2) Uani d . 1 . .
H H1B 0.1124(8) -0.2462(12) 0.0288(5) 0.056(3) Uiso d . 1 . .
H H2B -0.1361(8) -0.1205(13) 0.0732(5) 0.069(3) Uiso d . 1 . .
H H1A 0.1499(9) -0.1651(14) 0.0826(6) 0.079(4) Uiso d . 1 . .
H H3A 0.9564(10) 0.6867(17) 0.1185(7) 0.091(4) Uiso d . 1 . .
H H2A -0.1742(8) 0.0219(12) 0.0639(5) 0.054(3) Uiso d . 1 . .
H H3B 0.8764(11) 0.6151(19) 0.1378(7) 0.105(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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O2 Co1 O2 3 . 180.00(3)
O2 Co1 O1 3 . 89.37(3)
O2 Co1 O1 . . 90.63(3)
O2 Co1 O1 3 3 90.63(3)
O2 Co1 O1 . 3 89.37(3)
O1 Co1 O1 . 3 180.00(4)
O2 Co1 N1 3 3 90.64(3)
O2 Co1 N1 . 3 89.36(3)
O1 Co1 N1 . 3 88.50(3)
O1 Co1 N1 3 3 91.50(3)
O2 Co1 N1 3 . 89.36(3)
O2 Co1 N1 . . 90.64(3)
O1 Co1 N1 . . 91.50(3)
O1 Co1 N1 3 . 88.50(3)
N1 Co1 N1 3 . 180.00(4)
O4 S1 O6 . . 113.64(5)
O4 S1 O5 . . 112.80(4)
O6 S1 O5 . . 111.97(4)
O4 S1 C15 . . 105.68(4)
O6 S1 C15 . . 106.11(5)
O5 S1 C15 . . 105.89(4)
C1 N1 C5 . . 116.94(7)
C1 N1 Co1 . . 121.07(6)
C5 N1 Co1 . . 121.99(6)
C12 N2 C11 . . 115.63(9)
Co1 O1 H1B . . 111.1(7)
Co1 O1 H1A . . 117.8(7)
H1B O1 H1A . . 106.7(10)
Co1 O2 H2B . . 115.2(8)
Co1 O2 H2A . . 116.1(7)
H2B O2 H2A . . 107.0(11)
N1 C1 C2 . . 122.92(9)
N1 C1 H1 . . 118.5
C2 C1 H1 . . 118.5
C1 C2 C3 . . 120.20(9)
C1 C2 H2 . . 119.9
C3 C2 H2 . . 119.9
C4 C3 C2 . . 116.92(8)
C4 C3 C6 . . 121.64(9)
C2 C3 C6 . . 121.44(8)
C3 C4 C5 . . 119.66(9)
C3 C4 H4 . . 120.2
C5 C4 H4 . . 120.2
N1 C5 C4 . . 123.34(8)
N1 C5 H5 . . 118.3
C4 C5 H5 . . 118.3
C3 C6 C7 . . 110.84(11)
C3 C6 H6A . . 109.5
C7 C6 H6A . . 109.5
C3 C6 H6B . . 109.5
C7 C6 H6B . . 109.5
H6A C6 H6B . . 108.1
C8 C7 C6 . . 110.43(14)
C8 C7 H7A . . 109.6
C6 C7 H7A . . 109.6
C8 C7 H7B . . 109.6
C6 C7 H7B . . 109.6
H7A C7 H7B . . 108.1
C7 C8 C9 . . 107.91(14)
C7 C8 H8A . . 110.1
C9 C8 H8A . . 110.1
C7 C8 H8B . . 110.1
C9 C8 H8B . . 110.1
H8A C8 H8B . . 108.4
C8' C7' H7'A . . 109.8
C8' C7' H7'B . . 109.8
H7'A C7' H7'B . . 108.3
C7' C8' C9 . . 106.09(15)
C7' C8' H8'A . . 110.5
C9 C8' H8'A . . 110.5
C7' C8' H8'B . . 110.5
C9 C8' H8'B . . 110.5
H8'A C8' H8'B . . 108.7
C10 C9 C13 . . 116.33(10)
C10 C9 C8 . . 134.91(12)
C13 C9 C8 . . 108.20(12)
C10 C9 C8' . . 108.32(12)
C13 C9 C8' . . 134.99(13)
C9 C10 C11 . . 120.18(11)
C9 C10 H10 . . 119.9
C11 C10 H10 . . 119.9
N2 C11 C10 . . 123.83(11)
N2 C11 H11 . . 118.1
C10 C11 H11 . . 118.1
N2 C12 C13 . . 123.95(11)
N2 C12 H12 . . 118
C13 C12 H12 . . 118
C9 C13 C12 . . 120.08(11)
C9 C13 H13 . . 120
C12 C13 H13 . . 120
C15 C14 C18 . 3_665 120.14(9)
C15 C14 H14 . . 119.9
C18 C14 H14 3_665 . 119.9
C14 C15 C16 . . 121.39(7)
C14 C15 S1 . . 117.82(7)
C16 C15 S1 . . 120.79(6)
C17 C16 C15 . . 123.49(7)
C17 C16 C16 . 3_665 118.91(10)
C15 C16 C16 . 3_665 117.60(10)
C18 C17 C16 . . 121.52(8)
C18 C17 H17 . . 119.2
C16 C17 H17 . . 119.2
C17 C18 C14 . 3_665 120.42(9)
C17 C18 H18 . . 119.8
C14 C18 H18 3_665 . 119.8
H3A O3 H3B . . 102.7(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O2 3 2.1022(8)
Co1 O2 . 2.1022(8)
Co1 O1 . 2.1230(7)
Co1 O1 3 2.1230(7)
Co1 N1 3 2.1294(8)
Co1 N1 . 2.1294(8)
S1 O4 . 1.4444(8)
S1 O6 . 1.4491(8)
S1 O5 . 1.4508(8)
S1 C15 . 1.7807(9)
N1 C1 . 1.3314(11)
N1 C5 . 1.3341(12)
N2 C12 . 1.3161(13)
N2 C11 . 1.3193(14)
O1 H1B . 0.735(10)
O1 H1A . 0.884(10)
O2 H2B . 0.771(11)
O2 H2A . 0.823(10)
C1 C2 . 1.3718(13)
C1 H1 . 0.93
C2 C3 . 1.3831(14)
C2 H2 . 0.93
C3 C4 . 1.3732(13)
C3 C6 . 1.5026(13)
C4 C5 . 1.3782(13)
C4 H4 . 0.93
C5 H5 . 0.93
C6 C7 . 1.567(2)
C6 H6A . 0.97
C6 H6B . 0.97
C7 C8 . 1.502(3)
C7 H7A . 0.97
C7 H7B . 0.97
C8 C9 . 1.548(2)
C8 H8A . 0.97
C8 H8B . 0.97
C7' C8' . 1.525(3)
C7' H7'A . 0.97
C7' H7'B . 0.97
C8' C9 . 1.568(2)
C8' H8'A . 0.97
C8' H8'B . 0.97
C9 C10 . 1.3559(17)
C9 C13 . 1.3654(17)
C10 C11 . 1.3700(15)
C10 H10 . 0.93
C11 H11 . 0.93
C12 C13 . 1.3665(15)
C12 H12 . 0.93
C13 H13 . 0.93
C14 C15 . 1.3612(13)
C14 C18 3_665 1.4036(13)
C14 H14 . 0.93
C15 C16 . 1.4252(12)
C16 C17 . 1.4051(13)
C16 C16 3_665 1.4336(15)
C17 C18 . 1.3549(14)
C17 H17 . 0.93
C18 C14 3_665 1.4036(13)
C18 H18 . 0.93
O3 H3A . 0.599(14)
O3 H3B . 0.947(15)
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
_geom_hbond_publ_flag
O3 H3B O6 . 0.947(15) 1.792(14) 2.7176(11) 164.8(13) y
O3 H3A O1 1_665 0.599(14) 2.436(14) 2.9013(12) 136.6(16) y
O2 H2A O4 1_455 0.823(10) 1.916(10) 2.7363(11) 174.6(10) y
O1 H1B O5 3_655 0.735(10) 1.979(10) 2.7096(10) 173.1(10) y
O1 H1A N2 2_645 0.884(10) 1.872(10) 2.7495(12) 171.3(11) y
O2 H2B O3 1_445 0.771(11) 1.940(11) 2.6959(11) 166.8(11) y
