metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

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

aDepartment of Chemistry and Chemical Engineering, Weifang University, Weifang 261061, People's Republic of China
*Correspondence e-mail: taixishi@lzu.edu.cn

(Received 6 April 2008; accepted 7 April 2008; online 10 April 2008)

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[Allen, F. H., Kennard, O., Watson, D. G., Brammer, L., Orpen, A. G. & Taylor, R. (1987). J. Chem. Soc. Perkin Trans. 2, pp. S1-19.]); Tai & Feng (2008[Xi-Shi, T. & Yi-Min, F. (2008). Acta Cryst. E64, o707.]); Tai et al. (2003[Tai, X.-S., Yin, X.-H., Tan, M.-Y. & Li, Y.-Z. (2003). Acta Cryst. E59, o681-o682.]); Tai et al. (2008[Tai, X.-S., Feng, Y.-M. & Zhang, H.-X. (2008). Acta Cryst. E64, m502.]); Tai, Yin & Feng (2007[Tai, X. S., Yin, J. & Feng, Y. M. (2007). Z. Kristallogr. New Cryst. Struct. 222, 398-400.]); Tai, Yin & Hao (2007[Tai, X.-S., Yin, J. & Hao, M.-Y. (2007). Acta Cryst. E63, m1061-m1062.]); Tai, Yin, Feng & Kong (2007[Tai, X. S., Yin, J., Feng, Y. M. & Kong, F. Y. (2007). Chin. J. Inorg. Chem. 23, 1812-1814.]); Wang et al. (2007[Wang, L.-H., Yin, J. & Tai, X.-S. (2007). Acta Cryst. E63, m1664.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(H2O)6](C13H10NO4S)2

  • Mr = 719.59

  • Monoclinic, P 21 /n

  • 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[Bruker (2000). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.752, Tmax = 0.895

  • 7328 measured reflections

  • 2749 independent reflections

  • 2171 reflections with I > 2σ(I)

  • Rint = 0.040

Refinement
  • R[F2 > 2σ(F2)] = 0.070

  • wR(F2) = 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

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O4—H4⋯N1 0.82 1.88 2.588 (7) 143
O5—H5A⋯O2i 0.85 1.96 2.736 (6) 151
O5—H5B⋯O1 0.85 1.97 2.744 (6) 151
O6—H6A⋯O1ii 0.85 1.99 2.757 (5) 150
O6—H6B⋯O3 0.85 2.03 2.768 (5) 144
O7—H7A⋯O3i 0.85 1.96 2.759 (5) 157
O7—H7B⋯O2iii 0.85 1.98 2.761 (5) 152
C6—H6⋯O3 0.93 2.56 2.918 (7) 104
Symmetry codes: (i) x, y, z-1; (ii) x+1, y, z; (iii) x+1, y, z-1.

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

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).

Related literature top

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

Experimental top

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 top

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).

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) showing 30% displacement ellipsoids. [Symmetry code: (a) -x +2, -y, -z].
Hexaaquacobalt(II) bis[4-(2-hydroxybenzylideneamino)benzenesulfonate] top
Crystal data top
[Co(H2O)6](C13H10NO4S)2F(000) = 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 = 2.4–25.3°
b = 35.211 (3) ŵ = 0.76 mm1
c = 6.9924 (15) ÅT = 298 K
β = 90.186 (2)°Block, light purple
V = 1556.4 (5) Å30.40 × 0.35 × 0.15 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
2749 independent reflections
Radiation source: fine-focus sealed tube2171 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ϕ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 57
Tmin = 0.752, Tmax = 0.895k = 4137
7328 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.071Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.141H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0118P)2 + 5.6103P]
where P = (Fo2 + 2Fc2)/3
2749 reflections(Δ/σ)max < 0.001
205 parametersΔρmax = 0.34 e Å3
0 restraintsΔρmin = 0.70 e Å3
Crystal data top
[Co(H2O)6](C13H10NO4S)2V = 1556.4 (5) Å3
Mr = 719.59Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.3216 (13) ŵ = 0.76 mm1
b = 35.211 (3) ÅT = 298 K
c = 6.9924 (15) Å0.40 × 0.35 × 0.15 mm
β = 90.186 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
2749 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
2171 reflections with I > 2σ(I)
Tmin = 0.752, Tmax = 0.895Rint = 0.040
7328 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0710 restraints
wR(F2) = 0.141H-atom parameters constrained
S = 1.17Δρmax = 0.34 e Å3
2749 reflectionsΔρmin = 0.70 e Å3
205 parameters
Special details top

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) top
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)
H5A0.68390.03920.09780.060*
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)
H7A1.02600.03920.30070.069*
H7B1.23260.03440.23550.069*
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) top
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, º) top
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—C277.9 (5)C2—C1—C6—C50.4 (9)
O3—S1—C1—C2162.7 (4)S1—C1—C6—C5178.0 (5)
O1—S1—C1—C242.4 (5)C4—N1—C7—C8177.6 (6)
O2—S1—C1—C6100.5 (5)N1—C7—C8—C13179.6 (7)
O3—S1—C1—C618.9 (5)N1—C7—C8—C91.8 (11)
O1—S1—C1—C6139.2 (5)C13—C8—C9—O4178.6 (6)
C6—C1—C2—C30.7 (9)C7—C8—C9—O43.6 (11)
S1—C1—C2—C3177.7 (5)C13—C8—C9—C100.7 (10)
C1—C2—C3—C41.2 (10)C7—C8—C9—C10177.1 (6)
C2—C3—C4—C51.3 (11)O4—C9—C10—C11178.9 (7)
C2—C3—C4—N1178.6 (6)C8—C9—C10—C110.4 (11)
C7—N1—C4—C3150.6 (7)C9—C10—C11—C121.1 (11)
C7—N1—C4—C532.2 (10)C10—C11—C12—C132.2 (11)
C3—C4—C5—C60.9 (11)C11—C12—C13—C82.0 (11)
N1—C4—C5—C6178.2 (6)C9—C8—C13—C120.5 (11)
C4—C5—C6—C10.5 (10)C7—C8—C13—C12178.3 (7)
Symmetry code: (i) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
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, z1; (iii) x+1, y, z; (iv) x+1, y, z1.

Experimental details

Crystal data
Chemical formula[Co(H2O)6](C13H10NO4S)2
Mr719.59
Crystal system, space groupMonoclinic, P21/n
Temperature (K)298
a, b, c (Å)6.3216 (13), 35.211 (3), 6.9924 (15)
β (°) 90.186 (2)
V3)1556.4 (5)
Z2
Radiation typeMo Kα
µ (mm1)0.76
Crystal size (mm)0.40 × 0.35 × 0.15
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.752, 0.895
No. of measured, independent and
observed [I > 2σ(I)] reflections
7328, 2749, 2171
Rint0.040
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.071, 0.141, 1.17
No. of reflections2749
No. of parameters205
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.34, 0.70

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N10.821.882.588 (7)143
O5—H5A···O2i0.851.962.736 (6)151
O5—H5B···O10.851.972.744 (6)151
O6—H6A···O1ii0.851.992.757 (5)150
O6—H6B···O30.852.032.768 (5)144
O7—H7A···O3i0.851.962.759 (5)157
O7—H7B···O2iii0.851.982.761 (5)152
C6—H6···O30.932.562.918 (7)104
Symmetry codes: (i) x, y, z1; (ii) x+1, y, z; (iii) x+1, y, z1.
 

Acknowledgements

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.

References

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