supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportcited insimilar papers  retraction buy article online

Acta Cryst. (2007). E63, m3054    [ doi:10.1107/S1600536807058527 ]

Hexaaquacobalt(II) bis(4-aminobenzenesulfonate)

H. Zhong, H.-L. Xie and C.-J. Luo

Abstract top

The asymmetric unit of the title compound, [Co(H2O)6](C6H6NO3S)2, contains one half-cation and one anion; the Co atom lies on an inversion centre. In the crystal structure, intermolecular O-H...O and O-H...S hydrogen bonds result in the formation of a supramolecular network. The conformation of the anion is stabilized by an intramolecular C-H...O hydrogen-bonding interaction.

Comment top

The crystal structure of hexaaquanickel(II) bis(4-aminobenzenesulfonate), (II), has previously been reported (Zhong et al., 2007). The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with that of (II). We report herein the crystal structure of (I).

In the molecule of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). The title compound, [Co(H2O)6](C6H6NO3S)2, contains one half-cation and one anion; the Co atom lies on an inversion centre, as in (II).

In the crystal structure, intermolecular O—H···O and O—H···S hydrogen bonds (Fig. 2 and Table 2) result in the formation of a supramolecular network structure. The conformation of the anion is stabilized by an intramolecular C—H···O hydrogen-bonding interaction., as in (II).

The both compounds, (I) and (II), are isostructural.

Related literature top

For a related structure, see: Zhong et al. (2007). For bond-length data, see: Allen et al. (1987).

Experimental top

Crystals of the title compound were synthesized using hydrothermal method in a 23 ml Teflon-lined Parr bomb, which was then sealed. Europium (III) nitrate pentahydrate (213.9 mg, 0.5 mmol), cobalt nitrate hexahydrate (145.9 mg, 0.5 mmol), p-aminobenzenesulfonic acid (346.4 mg, 2 mmol), ammonia (0.5 mol/l, 4 ml) and distilled water (8 g) were placed into the bomb and sealed. The bomb was then heated under autogenous pressure up to 453 K over the course of 7 d and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colourless solution was decanted from small pink crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.

Refinement top

H atoms (for H2O) were located in difference syntheses and refined isotropically. The H atoms were positioned geometrically, with N—H = 0.86 Å (for NH2) and C—H = 0.93 Å for aromatic H, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C,N).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level [symmetry code (A): −x + 3/2, y + 1/2, −z + 1/2].
[Figure 2] Fig. 2. A packing diagram of (I). Hydrogen bonds are shown as dashed lines.
Hexaaquacobalt(II) bis(4-aminobenzenesulfonate) top
Crystal data top
[Co(H2O)6](C6H6NO3S)2F(000) = 530
Mr = 511.38Dx = 1.550 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5606 reflections
a = 7.110 (2) Åθ = 2.2–26.5°
b = 6.1905 (17) ŵ = 1.03 mm−1
c = 24.9016 (11) ÅT = 273 K
β = 91.005 (4)°Prism, pink
V = 1095.9 (5) Å30.51 × 0.39 × 0.19 mm
Z = 2
Data collection top
Bruker APEX-II area-detector
diffractometer		2164 independent reflections
Radiation source: fine-focus sealed tube1869 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 26.4°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −8→8
Tmin = 0.623, Tmax = 0.829k = −7→7
6730 measured reflectionsl = −31→30
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)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0305P)2 + 0.444P]
where P = (Fo2 + 2Fc2)/3
2164 reflections(Δ/σ)max = 0.001
157 parametersΔρmax = 0.25 e Å−3
9 restraintsΔρmin = −0.25 e Å−3
Crystal data top
[Co(H2O)6](C6H6NO3S)2V = 1095.9 (5) Å3
Mr = 511.38Z = 2
Monoclinic, P21/nMo Kα radiation
a = 7.110 (2) ŵ = 1.03 mm−1
b = 6.1905 (17) ÅT = 273 K
c = 24.9016 (11) Å0.51 × 0.39 × 0.19 mm
β = 91.005 (4)°
Data collection top
Bruker APEX-II area-detector
diffractometer		2164 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		1869 reflections with I > 2σ(I)
Tmin = 0.623, Tmax = 0.829Rint = 0.023
6730 measured reflectionsθmax = 26.4°
Refinement top
R[F2 > 2σ(F2)] = 0.029H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.072Δρmax = 0.25 e Å−3
S = 1.01Δρmin = −0.25 e Å−3
2164 reflectionsAbsolute structure: ?
157 parametersFlack parameter: ?
9 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
Co10.50000.00000.00000.03904 (12)
S1−0.01463 (7)0.60843 (8)0.90518 (2)0.04647 (15)
O10.7236 (3)−0.1026 (3)0.04780 (9)0.0786 (6)
O20.5086 (3)0.2884 (3)0.03500 (7)0.0603 (4)
O30.3031 (3)−0.1035 (3)0.05312 (9)0.0796 (6)
O40.1552 (2)0.5138 (2)0.93055 (7)0.0599 (4)
O5−0.0146 (2)0.8390 (2)0.90902 (7)0.0584 (4)
O6−0.1924 (2)0.5169 (2)0.92380 (7)0.0604 (4)
N10.0301 (5)0.3770 (7)0.67180 (12)0.1339 (13)
H1AA0.00320.47070.64740.161*
H1BB0.06730.25000.66290.161*
C1−0.0035 (3)0.5452 (4)0.83690 (9)0.0506 (5)
C2−0.0538 (4)0.6917 (5)0.79840 (11)0.0691 (7)
H2−0.09320.82940.80810.083*
C3−0.0458 (4)0.6342 (6)0.74494 (11)0.0801 (8)
H3−0.08130.73440.71880.096*
C40.0125 (4)0.4347 (6)0.72937 (11)0.0725 (7)
C50.0607 (4)0.2900 (5)0.76906 (11)0.0765 (8)
H50.09980.15210.75950.092*
C60.0527 (4)0.3427 (4)0.82191 (10)0.0654 (6)
H60.08550.24120.84800.078*
H1A0.755 (3)−0.224 (3)0.0515 (11)0.071 (8)*
H2A0.608 (3)0.340 (5)0.0485 (12)0.095 (11)*
H3A0.278 (4)−0.224 (3)0.0590 (11)0.077 (9)*
H1B0.811 (3)−0.023 (3)0.0581 (12)0.079 (9)*
H2B0.418 (3)0.340 (5)0.0524 (11)0.096 (11)*
H3B0.212 (3)−0.027 (4)0.0615 (13)0.089 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0496 (2)0.0268 (2)0.0507 (2)0.00076 (14)0.00183 (14)0.00170 (15)
S10.0485 (3)0.0343 (3)0.0567 (3)0.0006 (2)0.0030 (2)−0.0004 (2)
O10.0800 (13)0.0383 (10)0.1157 (16)0.0055 (9)−0.0434 (11)0.0001 (10)
O20.0558 (9)0.0415 (9)0.0836 (12)−0.0008 (7)0.0051 (9)−0.0138 (8)
O30.0875 (13)0.0375 (10)0.1156 (16)0.0007 (9)0.0521 (12)0.0059 (10)
O40.0676 (10)0.0444 (9)0.0674 (10)0.0052 (7)−0.0115 (8)−0.0026 (7)
O50.0633 (9)0.0349 (8)0.0772 (10)0.0000 (7)0.0057 (8)−0.0016 (7)
O60.0649 (10)0.0434 (9)0.0736 (10)−0.0041 (7)0.0177 (8)−0.0022 (7)
N10.140 (3)0.190 (4)0.0716 (18)0.007 (3)0.0108 (17)−0.012 (2)
C10.0461 (11)0.0467 (12)0.0591 (12)−0.0006 (9)0.0015 (9)0.0040 (10)
C20.0734 (15)0.0650 (17)0.0691 (16)0.0113 (13)0.0055 (12)0.0130 (13)
C30.0765 (17)0.098 (2)0.0656 (16)0.0088 (16)0.0003 (13)0.0245 (16)
C40.0611 (15)0.097 (2)0.0593 (15)−0.0067 (14)0.0024 (12)−0.0012 (14)
C50.0886 (19)0.0746 (19)0.0665 (16)0.0056 (15)0.0039 (13)−0.0151 (14)
C60.0834 (17)0.0534 (14)0.0593 (13)0.0107 (12)−0.0002 (12)−0.0029 (11)
Geometric parameters (Å, º) top
Co1—O12.0690 (17)O3—H3B0.831 (17)
Co1—O21.9872 (16)N1—C41.485 (4)
Co1—O32.0456 (17)N1—H1AA0.8600
Co1—O2i1.9872 (16)N1—H1BB0.8600
Co1—O3i2.0456 (17)C1—C21.363 (3)
Co1—O1i2.0690 (17)C1—C61.369 (3)
S1—O51.4307 (16)C2—C31.380 (4)
S1—O61.4676 (17)C2—H20.9300
S1—O41.4740 (17)C3—C41.361 (4)
S1—C11.748 (2)C3—H30.9300
O1—H1A0.790 (16)C4—C51.373 (4)
O1—H1B0.827 (17)C5—C61.358 (4)
O2—H2A0.842 (17)C5—H50.9300
O2—H2B0.845 (17)C6—H60.9300
O3—H3A0.784 (17)
O1—Co1—O1i180.00 (14)H2A—O2—H2B107 (2)
O1—Co1—O290.33 (8)Co1—O3—H3A125 (2)
O1i—Co1—O289.67 (8)Co1—O3—H3B122 (2)
O1i—Co1—O386.58 (10)H3A—O3—H3B109 (2)
O1—Co1—O393.42 (10)C4—N1—H1AA120.0
O2—Co1—O2i180.00 (10)C4—N1—H1BB120.0
O2—Co1—O3i89.20 (8)H1AA—N1—H1BB120.0
O2i—Co1—O3i90.80 (8)C2—C1—C6119.5 (2)
O3i—Co1—O3180.00 (10)C2—C1—S1121.28 (19)
O2—Co1—O390.80 (8)C6—C1—S1119.25 (17)
O2i—Co1—O389.20 (8)C1—C2—C3119.5 (3)
O1—Co1—O2i89.67 (8)C1—C2—H2120.3
O1i—Co1—O2i90.33 (8)C3—C2—H2120.3
O1i—Co1—O3i93.42 (10)C4—C3—C2121.8 (3)
O1—Co1—O3i86.58 (10)C4—C3—H3119.1
O5—S1—O6111.29 (10)C2—C3—H3119.1
O5—S1—O4111.62 (10)C3—C4—C5117.4 (3)
O6—S1—O4114.49 (10)C3—C4—N1121.6 (3)
O5—S1—C1106.78 (10)C5—C4—N1120.9 (3)
O6—S1—C1105.95 (10)C6—C5—C4121.8 (3)
O4—S1—C1106.10 (10)C6—C5—H5119.1
Co1—O1—H1A124.8 (18)C4—C5—H5119.1
Co1—O1—H1B124.0 (19)C5—C6—C1120.1 (2)
H1A—O1—H1B109 (2)C5—C6—H6119.9
Co1—O2—H2A122 (2)C1—C6—H6119.9
Co1—O2—H2B123 (2)
Symmetry code: (i) −x+1, −y, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2···O50.932.572.910 (3)102
O1—H1B···S1ii0.83 (2)3.08 (2)3.863 (2)159 (2)
O1—H1A···O4iii0.79 (2)1.95 (2)2.738 (2)173 (3)
O1—H1B···O5ii0.83 (2)2.01 (2)2.832 (3)174 (3)
O2—H2A···O4ii0.84 (2)1.97 (2)2.807 (2)171 (3)
O2—H2B···O6iv0.85 (2)1.94 (2)2.764 (2)167 (3)
O3—H3A···S1v0.78 (2)3.17 (2)3.890 (2)155 (2)
O3—H3B···O5iv0.83 (2)1.98 (2)2.801 (2)172 (3)
O3—H3A···O6v0.78 (2)1.96 (2)2.742 (2)174 (3)
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x, −y+1, −z+1; (v) −x, −y, −z+1.
Selected geometric parameters (Å, º) top
Co1—O12.0690 (17)Co1—O32.0456 (17)
Co1—O21.9872 (16)
O1—Co1—O1i180.00 (14)O2—Co1—O2i180.00 (10)
O1—Co1—O290.33 (8)O2—Co1—O3i89.20 (8)
O1i—Co1—O289.67 (8)O2i—Co1—O3i90.80 (8)
O1i—Co1—O386.58 (10)O3i—Co1—O3180.00 (10)
O1—Co1—O393.42 (10)
Symmetry code: (i) −x+1, −y, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2···O50.932.572.910 (3)102
O1—H1B···S1ii0.827 (17)3.080 (17)3.863 (2)159 (2)
O1—H1A···O4iii0.790 (16)1.953 (17)2.738 (2)173 (3)
O1—H1B···O5ii0.827 (17)2.008 (18)2.832 (3)174 (3)
O2—H2A···O4ii0.842 (17)1.973 (18)2.807 (2)171 (3)
O2—H2B···O6iv0.845 (17)1.935 (18)2.764 (2)167 (3)
O3—H3A···S1v0.784 (17)3.17 (2)3.890 (2)155 (2)
O3—H3B···O5iv0.831 (17)1.976 (18)2.801 (2)172 (3)
O3—H3A···O6v0.784 (17)1.960 (17)2.742 (2)174 (3)
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x, −y+1, −z+1; (v) −x, −y, −z+1.
Acknowledgements top

We thank the Science and Technology Program of Jinggangshan University for financial support of this work (grant No. 2007).

references
References top

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.

Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Siemens (1996). SAINT and SHELXTL. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Zhong, H., Zhong, Q. Y., Xie, H.-L. & Luo, C.-J. (2007). Acta Cryst. E63, m2913–m2914.