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Acta Crystallogr Sect E Struct Rep Online. 2008 May 1; 64(Pt 5): m645.
Published online 2008 April 10. doi:  10.1107/S1600536808009422
PMCID: PMC2961243

Hexaaqua­cobalt(II) bis­[4-(2-hydroxy­benzyl­ideneamino)­benzene­sulfonate]

Abstract

In the cation of the title compound, [Co(H2O)6](C13H10NO4S)2, the Co atom lies on a centre of symmetry and its coordination geometry is octahedral. The crystal structure is stabilized by water–anion O—H(...)O hydrogen bonds. An intra­molecular O—H(...)N hydrogen bond occurs in the anion.

Related literature

For related literature, see: Allen et al. (1987 [triangle]); Tai & Feng (2008 [triangle]); Tai et al. (2003 [triangle]); Tai et al. (2008 [triangle]); Tai, Yin & Feng (2007 [triangle]); Tai, Yin & Hao (2007 [triangle]); Tai, Yin, Feng & Kong (2007 [triangle]); Wang et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m645-scheme1.jpg

Experimental

Crystal data

  • [Co(H2O)6](C13H10NO4S)2
  • M r = 719.59
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m645-efi1.jpg
  • a = 6.3216 (13) Å
  • b = 35.211 (3) Å
  • c = 6.9924 (15) Å
  • β = 90.186 (2)°
  • V = 1556.4 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 0.76 mm−1
  • T = 298 (2) K
  • 0.40 × 0.35 × 0.15 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2000 [triangle]) T min = 0.752, T max = 0.895
  • 7328 measured reflections
  • 2749 independent reflections
  • 2171 reflections with I > 2σ(I)
  • R int = 0.040

Refinement

  • R[F 2 > 2σ(F 2)] = 0.070
  • wR(F 2) = 0.141
  • S = 1.17
  • 2749 reflections
  • 205 parameters
  • H-atom parameters constrained
  • Δρmax = 0.34 e Å−3
  • Δρmin = −0.69 e Å−3

Data collection: SMART (Bruker, 2000 [triangle]); cell refinement: SAINT (Bruker, 2000 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808009422/at2558sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808009422/at2558Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors thank the National Natural Science Foundation of China (20671073), the National Natural Science Foundation of Shandong (Y2007B60), the Science and Technology Foundation of Weifang and Weifang University for research grants.

supplementary crystallographic information

Comment

As part of our ongoing studies of the coordination chemistry of Schiff base ligands (Xi-Shi & Yi-Min, 2008; Tai, Feng & Zhang, 2008; Tai, Yin & Feng, 2007; Tai, Yin, Feng & Kong, 2007; Tai, Yin & Hao, 2007; Wang et al., 2007; Tai et al., 2003), we now report the synthesis and structure of the title compound, (I), (Fig. 1).

In the molecule of (I), the Co (II) centre is six-coordinate with six O donors of the water molecules. The C7—N1 bond length of 1.281 (8) Å is close to double-bond. Otherwise, the geometrical parameters for (I) are in normal range (Allen et al., 1987). The dihedral angle between the two benzene ring is 33.5°, indicating that the molecule is non-planar, which perhaps correlates with the intramolecular and intermolecular hydrogen bonds (Table 1).

Experimental

1 mmol of Cobalt acetate was added to a solution of salicylaldehyde-4-aminobenzene sulfonic acid (1 mmol) in 10 ml of 95% ethanol. The mixture was stirred for 2 h at refluxing temperature. Evaporating some ethanol, clear blocks of (I) were obtained after one weeks.

Refinement

The H atoms were placed geometrically [C—H = 0.93 Å, O—H = 0.82 for hydroxy group and O—H = 0.85 Å for water molecules] and refined as riding with Uiso(H) = 1.2Ueq(carrier).

Figures

Fig. 1.
The molecular structure of (I) showing 30% displacement ellipsoids. [Symmetry code: (a) -x +2, -y, -z].

Crystal data

[Co(H2O)6](C13H10NO4S)2F000 = 746
Mr = 719.59Dx = 1.535 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2380 reflections
a = 6.3216 (13) Åθ = 2.4–25.3º
b = 35.211 (3) ŵ = 0.76 mm1
c = 6.9924 (15) ÅT = 298 (2) K
β = 90.186 (2)ºBlock, light purple
V = 1556.4 (5) Å30.40 × 0.35 × 0.15 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer2749 independent reflections
Radiation source: fine-focus sealed tube2171 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.040
T = 298(2) Kθmax = 25.0º
[var phi] and ω scansθmin = 2.3º
Absorption correction: multi-scan(SADABS; Bruker, 2000)h = −5→7
Tmin = 0.752, Tmax = 0.895k = −41→37
7328 measured reflectionsl = −8→8

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.071H-atom parameters constrained
wR(F2) = 0.141  w = 1/[σ2(Fo2) + (0.0118P)2 + 5.6103P] where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max < 0.001
2749 reflectionsΔρmax = 0.34 e Å3
205 parametersΔρmin = −0.69 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Co11.00000.00000.00000.0332 (3)
N10.4234 (9)0.23121 (15)0.5063 (8)0.0585 (14)
O10.5135 (6)0.05103 (11)0.3289 (6)0.0480 (10)
O20.5140 (6)0.05158 (12)0.6754 (6)0.0504 (11)
O30.8400 (5)0.06145 (11)0.5055 (5)0.0418 (9)
O40.1496 (8)0.28449 (14)0.5667 (7)0.0772 (15)
H40.19930.26320.58090.116*
O50.7065 (5)0.02585 (12)0.0016 (6)0.0496 (10)
H5A0.68390.0392−0.09780.060*
H5B0.68500.03890.10200.060*
O61.1038 (6)0.03462 (13)0.2207 (6)0.0571 (12)
H6A1.23320.03100.24840.069*
H6B1.02790.03250.32030.069*
O71.1055 (6)0.03864 (12)−0.2024 (6)0.0575 (12)
H7A1.02600.0392−0.30070.069*
H7B1.23260.0344−0.23550.069*
S10.61081 (19)0.06622 (4)0.50249 (19)0.0345 (3)
C10.5625 (8)0.11545 (15)0.4991 (7)0.0349 (12)
C20.3648 (9)0.12848 (17)0.4446 (9)0.0471 (15)
H20.26050.11150.40590.056*
C30.3241 (10)0.16694 (17)0.4483 (10)0.0542 (17)
H30.19070.17580.41400.065*
C40.4787 (10)0.19236 (17)0.5021 (10)0.0522 (15)
C50.6758 (10)0.17953 (18)0.5569 (9)0.0545 (17)
H50.77940.19670.59500.065*
C60.7197 (9)0.14085 (17)0.5552 (8)0.0471 (15)
H60.85270.13200.59110.056*
C70.5616 (11)0.25709 (18)0.4752 (10)0.0571 (17)
H70.69920.25000.44480.069*
C80.5093 (11)0.29731 (17)0.4862 (10)0.0542 (16)
C90.3064 (12)0.3093 (2)0.5366 (10)0.0624 (19)
C100.2661 (13)0.34768 (19)0.5538 (10)0.067 (2)
H100.13130.35570.58810.080*
C110.4190 (14)0.3740 (2)0.5216 (10)0.071 (2)
H110.38820.39970.53620.085*
C120.6230 (15)0.3628 (2)0.4664 (12)0.080 (2)
H120.72680.38080.43990.095*
C130.6654 (12)0.32435 (19)0.4525 (10)0.0661 (19)
H130.80090.31640.41990.079*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0218 (5)0.0452 (6)0.0327 (5)−0.0015 (5)−0.0018 (4)−0.0005 (5)
N10.063 (4)0.047 (3)0.066 (4)0.009 (3)−0.001 (3)−0.008 (3)
O10.032 (2)0.060 (3)0.051 (3)0.0021 (18)−0.0070 (18)−0.011 (2)
O20.035 (2)0.065 (3)0.051 (3)0.0022 (19)0.0071 (18)0.018 (2)
O30.0233 (18)0.057 (2)0.045 (2)0.0035 (17)0.0008 (16)0.0017 (19)
O40.081 (4)0.063 (3)0.087 (4)0.014 (3)0.020 (3)0.006 (3)
O50.037 (2)0.075 (3)0.037 (2)0.013 (2)−0.0008 (17)0.001 (2)
O60.028 (2)0.095 (3)0.048 (3)−0.002 (2)−0.0009 (18)−0.023 (2)
O70.028 (2)0.090 (3)0.055 (3)−0.002 (2)−0.0028 (18)0.026 (2)
S10.0233 (6)0.0456 (8)0.0348 (7)0.0022 (6)−0.0004 (5)0.0012 (6)
C10.028 (3)0.047 (3)0.030 (3)0.002 (2)−0.002 (2)−0.001 (2)
C20.033 (3)0.051 (4)0.058 (4)0.002 (3)−0.016 (3)−0.002 (3)
C30.041 (3)0.049 (4)0.072 (5)0.011 (3)−0.005 (3)−0.001 (3)
C40.053 (4)0.048 (3)0.056 (4)0.012 (3)0.001 (3)−0.003 (3)
C50.061 (4)0.045 (4)0.057 (4)−0.004 (3)−0.014 (3)−0.009 (3)
C60.038 (3)0.057 (4)0.046 (4)−0.001 (3)−0.014 (3)−0.003 (3)
C70.061 (4)0.053 (4)0.057 (4)0.012 (3)−0.001 (3)−0.007 (3)
C80.065 (4)0.049 (4)0.049 (4)0.002 (3)−0.003 (3)−0.013 (3)
C90.084 (5)0.057 (4)0.047 (4)0.007 (4)0.008 (4)−0.002 (3)
C100.104 (6)0.045 (4)0.051 (4)0.017 (4)0.008 (4)−0.003 (3)
C110.107 (6)0.046 (4)0.059 (5)0.019 (4)−0.010 (4)−0.002 (4)
C120.105 (7)0.045 (4)0.089 (6)0.000 (4)−0.009 (5)0.001 (4)
C130.067 (5)0.057 (4)0.075 (5)0.003 (4)−0.005 (4)−0.007 (4)

Geometric parameters (Å, °)

Co1—O52.067 (3)C1—C61.392 (7)
Co1—O5i2.067 (3)C2—C31.379 (8)
Co1—O62.072 (4)C2—H20.9300
Co1—O6i2.072 (4)C3—C41.377 (8)
Co1—O7i2.075 (4)C3—H30.9300
Co1—O72.075 (4)C4—C51.379 (8)
N1—C71.281 (8)C5—C61.390 (8)
N1—C41.412 (7)C5—H50.9300
O1—S11.460 (4)C6—H60.9300
O2—S11.452 (4)C7—C81.456 (8)
O3—S11.458 (3)C7—H70.9300
O4—C91.338 (8)C8—C131.392 (9)
O4—H40.8200C8—C91.397 (9)
O5—H5A0.8501C9—C101.381 (9)
O5—H5B0.8500C10—C111.359 (10)
O6—H6A0.8500C10—H100.9300
O6—H6B0.8500C11—C121.404 (10)
O7—H7A0.8500C11—H110.9300
O7—H7B0.8500C12—C131.384 (9)
S1—C11.760 (5)C12—H120.9300
C1—C21.384 (7)C13—H130.9300
O5—Co1—O5i180.0 (2)C3—C2—H2120.4
O5—Co1—O691.09 (15)C1—C2—H2120.4
O5i—Co1—O688.91 (15)C4—C3—C2120.8 (6)
O5—Co1—O6i88.91 (15)C4—C3—H3119.6
O5i—Co1—O6i91.09 (15)C2—C3—H3119.6
O6—Co1—O6i180.0 (2)C3—C4—C5120.2 (6)
O5—Co1—O7i89.69 (15)C3—C4—N1117.4 (6)
O5i—Co1—O7i90.31 (15)C5—C4—N1122.4 (6)
O6—Co1—O7i88.81 (17)C4—C5—C6119.9 (6)
O6i—Co1—O7i91.19 (17)C4—C5—H5120.0
O5—Co1—O790.31 (15)C6—C5—H5120.0
O5i—Co1—O789.69 (15)C5—C6—C1119.3 (5)
O6—Co1—O791.19 (17)C5—C6—H6120.3
O6i—Co1—O788.81 (17)C1—C6—H6120.3
O7i—Co1—O7180.0 (3)N1—C7—C8121.8 (6)
C7—N1—C4121.1 (6)N1—C7—H7119.1
C9—O4—H4109.5C8—C7—H7119.1
Co1—O5—H5A112.8C13—C8—C9119.2 (6)
Co1—O5—H5B112.9C13—C8—C7119.7 (6)
H5A—O5—H5B110.4C9—C8—C7121.1 (6)
Co1—O6—H6A112.5O4—C9—C10119.2 (7)
Co1—O6—H6B112.4O4—C9—C8121.6 (6)
H6A—O6—H6B110.2C10—C9—C8119.2 (7)
Co1—O7—H7A112.2C11—C10—C9121.5 (7)
Co1—O7—H7B112.2C11—C10—H10119.3
H7A—O7—H7B110.0C9—C10—H10119.3
O2—S1—O3111.6 (2)C10—C11—C12120.5 (7)
O2—S1—O1112.6 (2)C10—C11—H11119.7
O3—S1—O1112.7 (2)C12—C11—H11119.7
O2—S1—C1106.7 (2)C13—C12—C11118.2 (8)
O3—S1—C1106.6 (2)C13—C12—H12120.9
O1—S1—C1106.1 (2)C11—C12—H12120.9
C2—C1—C6120.5 (5)C12—C13—C8121.3 (7)
C2—C1—S1119.1 (4)C12—C13—H13119.3
C6—C1—S1120.4 (4)C8—C13—H13119.3
C3—C2—C1119.3 (5)
O2—S1—C1—C2−77.9 (5)C2—C1—C6—C50.4 (9)
O3—S1—C1—C2162.7 (4)S1—C1—C6—C5−178.0 (5)
O1—S1—C1—C242.4 (5)C4—N1—C7—C8−177.6 (6)
O2—S1—C1—C6100.5 (5)N1—C7—C8—C13179.6 (7)
O3—S1—C1—C6−18.9 (5)N1—C7—C8—C91.8 (11)
O1—S1—C1—C6−139.2 (5)C13—C8—C9—O4178.6 (6)
C6—C1—C2—C3−0.7 (9)C7—C8—C9—O4−3.6 (11)
S1—C1—C2—C3177.7 (5)C13—C8—C9—C10−0.7 (10)
C1—C2—C3—C41.2 (10)C7—C8—C9—C10177.1 (6)
C2—C3—C4—C5−1.3 (11)O4—C9—C10—C11−178.9 (7)
C2—C3—C4—N1−178.6 (6)C8—C9—C10—C110.4 (11)
C7—N1—C4—C3−150.6 (7)C9—C10—C11—C121.1 (11)
C7—N1—C4—C532.2 (10)C10—C11—C12—C13−2.2 (11)
C3—C4—C5—C60.9 (11)C11—C12—C13—C82.0 (11)
N1—C4—C5—C6178.2 (6)C9—C8—C13—C12−0.5 (11)
C4—C5—C6—C1−0.5 (10)C7—C8—C13—C12−178.3 (7)

Symmetry codes: (i) −x+2, −y, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O4—H4···N10.821.882.588 (7)143
O5—H5A···O2ii0.851.962.736 (6)151
O5—H5B···O10.851.972.744 (6)151
O6—H6A···O1iii0.851.992.757 (5)150
O6—H6B···O30.852.032.768 (5)144
O7—H7A···O3ii0.851.962.759 (5)157
O7—H7B···O2iv0.851.982.761 (5)152
C6—H6···O30.932.562.918 (7)104

Symmetry codes: (ii) x, y, z−1; (iii) x+1, y, z; (iv) x+1, y, z−1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: AT2558).

References

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  • Tai, X. S., Yin, J., Feng, Y. M. & Kong, F. Y. (2007). Chin. J. Inorg. Chem.23, 1812–1814.
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