supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportcited insimilar papers Open access

hb5188 scheme

Acta Cryst. (2009). E65, m1548    [ doi:10.1107/S1600536809046583 ]

Hexaaquacobalt(II) bis(4-amino-3-methylbenzenesulfonate)

W. Zhang and Y.-T. Chen

Abstract top

In the title molecular salt, [Co(H2O)6](C7H8NO3S)2, the Co2+ cation lies on an inversion centre. In the crystal, the components are linked by N-H...O and O-H...O hydrogen bonds, thereby generating sheets parallel to (001).

Related literature top

For background to hydrogen-bonded networks, see: Tai et al. (2007).

Experimental top

A solution of 1.0 mmol 4-amino-3-methyl-benzenesulfonic acid and 1.0 mmol NaOH in 10 ml ethanol was added to a solution of 0.5 mmol Co(CH3COO)24H2O in 5 ml e thanol at room temperature. The mixture was refluxed for 4 h with stirring, then the resulting precipitate was filtered, washed, and dried in vacuo over P4O10 for 48 h. Pink blocks of (I) were obtained by slowly evaporating from methanol at room temperature.

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. Atosm with suffix A are generated by the symmetry operation (1–x, 1–y, –z).
Hexaaquacobalt(II) bis(4-amino-3-methylbenzenesulfonate) top
Crystal data top
[Co(H2O)6](C7H8NO3S)2F(000) = 562
Mr = 539.43Dx = 1.664 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3103 reflections
a = 6.309 (1) Åθ = 3.3–28.3°
b = 7.0513 (11) ŵ = 1.06 mm−1
c = 24.262 (4) ÅT = 293 K
β = 94.080 (2)°Block, pink
V = 1076.6 (3) Å30.21 × 0.16 × 0.12 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer		1921 independent reflections
Radiation source: fine-focus sealed tube1690 reflections with I > 2σ(I)
graphiteRint = 0.019
φ and ω scansθmax = 25.1°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −7→7
Tmin = 0.809, Tmax = 0.884k = −8→6
5530 measured reflectionsl = −25→28
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.073 w = 1/[σ2(Fo2) + (0.035P)2 + 0.4723P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
1921 reflectionsΔρmax = 0.42 e Å−3
143 parametersΔρmin = −0.32 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0268 (16)
Crystal data top
[Co(H2O)6](C7H8NO3S)2V = 1076.6 (3) Å3
Mr = 539.43Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.309 (1) ŵ = 1.06 mm−1
b = 7.0513 (11) ÅT = 293 K
c = 24.262 (4) Å0.21 × 0.16 × 0.12 mm
β = 94.080 (2)°
Data collection top
Bruker SMART CCD
diffractometer		1921 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		1690 reflections with I > 2σ(I)
Tmin = 0.809, Tmax = 0.884Rint = 0.019
5530 measured reflectionsθmax = 25.1°
Refinement top
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.073Δρmax = 0.42 e Å−3
S = 1.10Δρmin = −0.32 e Å−3
1921 reflectionsAbsolute structure: ?
143 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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
Co10.50000.50000.00000.02153 (14)
S10.59383 (7)0.51047 (6)0.403529 (19)0.02233 (15)
O10.5037 (2)0.66812 (19)0.43304 (5)0.0324 (3)
O20.5014 (2)0.32921 (19)0.41856 (5)0.0315 (3)
O30.8256 (2)0.50668 (17)0.41067 (6)0.0311 (3)
O40.3989 (2)0.73519 (19)0.04326 (6)0.0363 (3)
H70.27750.77620.05060.054*
H80.48880.81560.05670.054*
O50.4048 (2)0.3100 (2)0.05939 (6)0.0365 (4)
H90.28420.25600.05890.055*
H100.49240.22010.06640.055*
O60.7970 (2)0.50949 (18)0.04025 (7)0.0418 (4)
H120.86840.60540.05190.063*
H110.87060.41340.05070.063*
N10.3463 (3)0.6380 (3)0.16739 (7)0.0474 (5)
H1A0.22290.68450.15800.057*
H1B0.43200.61150.14250.057*
C10.5244 (3)0.5467 (2)0.33285 (7)0.0232 (4)
C20.6647 (3)0.5036 (2)0.29306 (8)0.0247 (4)
H20.79800.45450.30390.030*
C30.6088 (3)0.5326 (2)0.23743 (8)0.0260 (4)
C40.4060 (3)0.6062 (3)0.22179 (8)0.0289 (4)
C50.2676 (3)0.6489 (3)0.26221 (8)0.0307 (4)
H50.13410.69850.25180.037*
C60.3248 (3)0.6188 (3)0.31715 (8)0.0289 (4)
H60.23010.64670.34370.035*
C70.7578 (4)0.4865 (3)0.19380 (9)0.0360 (5)
H7A0.88880.43870.21100.054*
H7B0.78540.59910.17330.054*
H7C0.69450.39230.16930.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0198 (2)0.0217 (2)0.0232 (2)−0.00091 (13)0.00196 (14)−0.00005 (12)
S10.0203 (3)0.0220 (3)0.0245 (3)−0.00008 (16)−0.00023 (18)0.00040 (16)
O10.0316 (7)0.0326 (7)0.0328 (7)0.0041 (6)0.0005 (6)−0.0082 (6)
O20.0299 (7)0.0284 (7)0.0359 (8)−0.0036 (6)0.0002 (6)0.0071 (6)
O30.0220 (7)0.0343 (8)0.0362 (8)0.0004 (5)−0.0024 (6)0.0012 (5)
O40.0278 (7)0.0340 (8)0.0476 (9)−0.0019 (6)0.0072 (6)−0.0164 (6)
O50.0270 (7)0.0361 (8)0.0474 (9)0.0027 (6)0.0088 (6)0.0160 (7)
O60.0311 (8)0.0281 (8)0.0633 (11)−0.0004 (6)−0.0171 (7)−0.0025 (6)
N10.0528 (12)0.0596 (13)0.0288 (9)0.0205 (10)−0.0043 (8)0.0047 (9)
C10.0247 (9)0.0198 (8)0.0248 (9)−0.0011 (7)−0.0006 (7)0.0021 (7)
C20.0236 (9)0.0197 (9)0.0307 (10)0.0007 (7)0.0009 (8)0.0008 (7)
C30.0304 (10)0.0196 (9)0.0283 (10)−0.0003 (7)0.0041 (8)−0.0009 (7)
C40.0375 (11)0.0222 (9)0.0263 (10)0.0008 (8)−0.0019 (8)0.0025 (7)
C50.0268 (10)0.0306 (10)0.0338 (11)0.0077 (8)−0.0042 (8)0.0003 (8)
C60.0261 (10)0.0307 (10)0.0299 (10)0.0031 (8)0.0031 (8)−0.0011 (8)
C70.0418 (12)0.0335 (11)0.0334 (11)0.0050 (9)0.0085 (10)0.0004 (8)
Geometric parameters (Å, °) top
Co1—O6i2.0515 (14)N1—C41.365 (2)
Co1—O62.0515 (14)N1—H1A0.8600
Co1—O4i2.0866 (13)N1—H1B0.8600
Co1—O42.0866 (13)C1—C61.386 (2)
Co1—O52.0868 (13)C1—C21.389 (3)
Co1—O5i2.0868 (13)C2—C31.386 (3)
S1—O11.4593 (13)C2—H20.9300
S1—O31.4603 (14)C3—C41.407 (3)
S1—O21.4617 (13)C3—C71.500 (3)
S1—C11.7580 (18)C4—C51.392 (3)
O4—H70.8498C5—C61.372 (3)
O4—H80.8498C5—H50.9300
O5—H90.8500C6—H60.9300
O5—H100.8499C7—H7A0.9600
O6—H120.8499C7—H7B0.9600
O6—H110.8499C7—H7C0.9600
O6i—Co1—O6180.0H12—O6—H11105.7
O6i—Co1—O4i92.07 (6)C4—N1—H1A120.0
O6—Co1—O4i87.93 (6)C4—N1—H1B120.0
O6i—Co1—O487.93 (6)H1A—N1—H1B120.0
O6—Co1—O492.07 (6)C6—C1—C2120.05 (17)
O4i—Co1—O4180.0C6—C1—S1118.67 (14)
O6i—Co1—O590.56 (6)C2—C1—S1121.28 (14)
O6—Co1—O589.44 (6)C3—C2—C1120.94 (17)
O4i—Co1—O587.15 (6)C3—C2—H2119.5
O4—Co1—O592.85 (6)C1—C2—H2119.5
O6i—Co1—O5i89.44 (6)C2—C3—C4118.72 (17)
O6—Co1—O5i90.56 (6)C2—C3—C7121.77 (18)
O4i—Co1—O5i92.85 (6)C4—C3—C7119.51 (17)
O4—Co1—O5i87.15 (6)N1—C4—C5120.13 (17)
O5—Co1—O5i180.0N1—C4—C3120.29 (18)
O1—S1—O3112.18 (8)C5—C4—C3119.58 (17)
O1—S1—O2111.56 (9)C6—C5—C4121.08 (17)
O3—S1—O2111.60 (7)C6—C5—H5119.5
O1—S1—C1106.81 (8)C4—C5—H5119.5
O3—S1—C1107.24 (8)C5—C6—C1119.63 (17)
O2—S1—C1107.10 (8)C5—C6—H6120.2
Co1—O4—H7133.5C1—C6—H6120.2
Co1—O4—H8120.2C3—C7—H7A109.5
H7—O4—H8106.2C3—C7—H7B109.5
Co1—O5—H9125.3H7A—C7—H7B109.5
Co1—O5—H10113.7C3—C7—H7C109.5
H9—O5—H10103.7H7A—C7—H7C109.5
Co1—O6—H12129.0H7B—C7—H7C109.5
Co1—O6—H11125.2
O1—S1—C1—C6−38.02 (17)C2—C3—C4—N1179.47 (17)
O3—S1—C1—C6−158.47 (14)C7—C3—C4—N1−0.9 (3)
O2—S1—C1—C681.62 (16)C2—C3—C4—C50.3 (3)
O1—S1—C1—C2142.30 (14)C7—C3—C4—C5179.96 (17)
O3—S1—C1—C221.85 (16)N1—C4—C5—C6−179.70 (19)
O2—S1—C1—C2−98.06 (15)C3—C4—C5—C6−0.6 (3)
C6—C1—C2—C30.4 (3)C4—C5—C6—C10.7 (3)
S1—C1—C2—C3−179.97 (13)C2—C1—C6—C5−0.6 (3)
C1—C2—C3—C4−0.2 (3)S1—C1—C6—C5179.75 (15)
C1—C2—C3—C7−179.85 (17)
Symmetry codes: (i) −x+1, −y+1, −z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2ii0.862.473.214 (2)145
N1—H1B···O40.862.563.129 (2)125
O4—H7···O2ii0.852.002.8300 (19)167
O4—H8···O3iii0.851.922.7675 (19)176
O5—H9···O1iv0.851.942.7828 (19)170
O5—H10···O3v0.851.952.7963 (19)174
O6—H11···O1v0.851.932.7711 (19)169
O6—H12···O2iii0.851.902.7419 (19)173
Symmetry codes: (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2.
Table 1
Selected geometric parameters (Å) top
Co1—O62.0515 (14)Co1—O52.0868 (13)
Co1—O42.0866 (13)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2i0.862.473.214 (2)145
N1—H1B···O40.862.563.129 (2)125
O4—H7···O2i0.852.002.8300 (19)167
O4—H8···O3ii0.851.922.7675 (19)176
O5—H9···O1iii0.851.942.7828 (19)170
O5—H10···O3iv0.851.952.7963 (19)174
O6—H11···O1iv0.851.932.7711 (19)169
O6—H12···O2ii0.851.902.7419 (19)173
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+3/2, y+1/2, −z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+1/2.
Acknowledgements top

The authors would like to thank the Program for New Century Excellent Talents in Universities for a research grant.

references
References top

Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Tai, X. S., Yin, J., Feng, Y. M. & Kong, F. Y. (2007). Chin. J. Inorg. Chem. 24, 1812–1814.