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Acta Crystallogr Sect E Struct Rep Online. 2009 November 1; 65(Pt 11): m1310.
Published online 2009 October 7. doi:  10.1107/S1600536809039774
PMCID: PMC2971040

Tetra­aqua­bis(2-oxo-1,2-dihydro­pyridine-5-sulfonato-κO 2)zinc(II)

Abstract

The metal atom in the title compound, [Zn(C5H4NO4S)2(H2O)4], lies on a center of inversion and is linked to the anionic ligand through the carbonyl O atom. In the crystal structure, the 2-oxo-1,2-dihydro­pyridine-5-sulfon­ate ligand inter­acts with other mol­ecules through N—H(...)O and O—H(...)O hydrogen bonds, forming a three-dimensional network structure.

Related literature

For the crystal structure of another zwitterionic tetra­aqua­bis(amide)–metalII complex, see: Gao et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1310-scheme1.jpg

Experimental

Crystal data

  • [Zn(C5H4NO4S)2(H2O)4]
  • M r = 485.74
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1310-efi1.jpg
  • a = 6.7701 (2) Å
  • b = 13.9725 (5) Å
  • c = 10.0343 (3) Å
  • β = 115.331 (2)°
  • V = 857.93 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.74 mm−1
  • T = 293 K
  • 0.21 × 0.16 × 0.16 mm

Data collection

  • Rigaku R-AXIS RAPID IP diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.711, T max = 0.768
  • 8224 measured reflections
  • 1951 independent reflections
  • 1866 reflections with I > 2σ(I)
  • R int = 0.021

Refinement

  • R[F 2 > 2σ(F 2)] = 0.023
  • wR(F 2) = 0.066
  • S = 1.06
  • 1951 reflections
  • 144 parameters
  • 5 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.37 e Å−3
  • Δρmin = −0.39 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 [triangle]); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2009 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809039774/xu2623sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809039774/xu2623Isup2.hkl

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

Acknowledgments

We thank the Natural Science Foundation of Heilongjiang Province (No. B200501), Heilongjiang University, China, and the University of Malaya for supporting this study.

supplementary crystallographic information

Experimental

Zinc carbonate (0.25 g, 2 mmol) was added to a hot aqueous solution of 2-hydroxypyridine 5-sulfonic acid (0.35 g, 2 mmol); the pH value was adjusted to 6 with 0.1 M sodium hydroxide. The solution was allowed to evaporate slowly. Colorless prismatic crystals were isolated after five days. CH&N elemental analysis. Calc. for C10H16N2O12S2Zn:C 24.73, H 3.32, N 5.77%; found: C 24.77, H 3.37, N 5.81%.

Refinement

Carbon-bound H-atoms were placed in calculated positions (C—H 0.93 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2U(C). The ammonium and water H-atoms were refined with a distance restraint of N–H = O–H 0.85±0.01 Å; their temperature factors were refined.

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of Zn(H2O)4(C5H4NO4S)2 at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.

Crystal data

[Zn(C5H4NO4S)2(H2O)4]F(000) = 496
Mr = 485.74Dx = 1.880 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7685 reflections
a = 6.7701 (2) Åθ = 3.3–27.5°
b = 13.9725 (5) ŵ = 1.74 mm1
c = 10.0343 (3) ÅT = 293 K
β = 115.331 (2)°Prism, colorles
V = 857.93 (5) Å30.21 × 0.16 × 0.16 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID IP diffractometer1951 independent reflections
Radiation source: fine-focus sealed tube1866 reflections with I > 2σ(I)
graphiteRint = 0.021
ω scansθmax = 27.5°, θmin = 3.3°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −8→8
Tmin = 0.711, Tmax = 0.768k = −17→18
8224 measured reflectionsl = −13→13

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.037P)2 + 0.5079P] where P = (Fo2 + 2Fc2)/3
1951 reflections(Δ/σ)max = 0.001
144 parametersΔρmax = 0.37 e Å3
5 restraintsΔρmin = −0.39 e Å3

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

xyzUiso*/Ueq
Zn10.50000.50000.50000.02207 (10)
S10.81951 (6)0.69216 (3)−0.07941 (4)0.01923 (11)
O10.4186 (2)0.54472 (10)0.28771 (14)0.0295 (3)
O30.9550 (2)0.77155 (9)0.00655 (14)0.0290 (3)
O20.95353 (19)0.61832 (9)−0.10431 (13)0.0264 (3)
O40.63570 (19)0.72213 (9)−0.21315 (13)0.0271 (3)
O1W0.20020 (19)0.43039 (9)0.40362 (13)0.0252 (2)
O2W0.3496 (2)0.62596 (11)0.53828 (17)0.0406 (3)
C20.7484 (3)0.55821 (12)0.25390 (18)0.0234 (3)
H20.83600.52710.34130.028*
C10.5190 (3)0.56850 (11)0.21274 (17)0.0214 (3)
N10.4007 (2)0.60683 (10)0.07675 (15)0.0229 (3)
C50.4880 (2)0.64352 (13)−0.01119 (17)0.0221 (3)
H50.39790.6715−0.10090.027*
C40.7072 (2)0.63937 (11)0.03179 (17)0.0201 (3)
C30.8395 (3)0.59340 (11)0.16668 (18)0.0227 (3)
H30.98910.58730.19560.027*
H10.2625 (16)0.6084 (16)0.045 (2)0.035 (6)*
H110.158 (4)0.4218 (18)0.3125 (12)0.048 (7)*
H120.166 (4)0.3815 (12)0.438 (3)0.045 (7)*
H210.223 (2)0.6479 (18)0.509 (3)0.051 (7)*
H220.431 (4)0.6538 (17)0.6168 (18)0.049 (7)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Zn10.02021 (15)0.02605 (16)0.02093 (15)−0.00103 (9)0.00973 (11)0.00145 (9)
S10.01744 (18)0.02194 (19)0.01890 (19)−0.00059 (13)0.00834 (14)0.00027 (13)
O10.0244 (6)0.0417 (7)0.0246 (6)−0.0023 (5)0.0125 (5)0.0061 (5)
O30.0276 (6)0.0281 (6)0.0320 (7)−0.0085 (5)0.0133 (5)−0.0060 (5)
O20.0222 (5)0.0329 (6)0.0252 (6)0.0046 (5)0.0111 (5)−0.0021 (5)
O40.0241 (6)0.0313 (6)0.0233 (6)0.0017 (5)0.0076 (5)0.0071 (5)
O1W0.0249 (6)0.0286 (6)0.0223 (6)−0.0043 (5)0.0104 (5)0.0014 (5)
O2W0.0268 (7)0.0401 (8)0.0447 (8)0.0077 (6)0.0056 (6)−0.0145 (6)
C20.0214 (7)0.0268 (8)0.0198 (7)0.0036 (6)0.0069 (6)0.0030 (6)
C10.0223 (7)0.0218 (7)0.0204 (7)−0.0023 (6)0.0094 (6)−0.0005 (6)
N10.0151 (6)0.0316 (7)0.0216 (7)−0.0009 (5)0.0074 (5)0.0019 (5)
C50.0203 (7)0.0264 (8)0.0190 (7)0.0007 (6)0.0079 (6)0.0024 (5)
C40.0198 (7)0.0215 (7)0.0204 (7)−0.0012 (6)0.0101 (6)−0.0006 (5)
C30.0178 (7)0.0266 (8)0.0229 (8)0.0021 (6)0.0078 (6)0.0001 (6)

Geometric parameters (Å, °)

Zn1—O1i2.0560 (12)O2W—H210.833 (10)
Zn1—O12.0560 (12)O2W—H220.838 (10)
Zn1—O1Wi2.0788 (12)C2—C31.360 (2)
Zn1—O1W2.0788 (12)C2—C11.434 (2)
Zn1—O2W2.1487 (14)C2—H20.9300
Zn1—O2Wi2.1487 (14)C1—N11.362 (2)
S1—O41.4477 (12)N1—C51.356 (2)
S1—O31.4626 (12)N1—H10.850 (10)
S1—O21.4643 (12)C5—C41.358 (2)
S1—C41.7588 (15)C5—H50.9300
O1—C11.2553 (19)C4—C31.418 (2)
O1W—H110.841 (10)C3—H30.9300
O1W—H120.841 (10)
O1i—Zn1—O1180.0Zn1—O1W—H12125.1 (18)
O1i—Zn1—O1Wi83.37 (5)H11—O1W—H12108 (2)
O1—Zn1—O1Wi96.63 (5)Zn1—O2W—H21137.0 (19)
O1i—Zn1—O1W96.63 (5)Zn1—O2W—H22112.2 (18)
O1—Zn1—O1W83.37 (5)H21—O2W—H22109 (3)
O1Wi—Zn1—O1W180.00 (6)C3—C2—C1120.81 (15)
O1i—Zn1—O2W90.07 (6)C3—C2—H2119.6
O1—Zn1—O2W89.93 (6)C1—C2—H2119.6
O1Wi—Zn1—O2W88.66 (5)O1—C1—N1117.88 (14)
O1W—Zn1—O2W91.34 (5)O1—C1—C2126.76 (15)
O1i—Zn1—O2Wi89.93 (6)N1—C1—C2115.35 (14)
O1—Zn1—O2Wi90.07 (6)C5—N1—C1124.58 (13)
O1Wi—Zn1—O2Wi91.34 (5)C5—N1—H1117.5 (16)
O1W—Zn1—O2Wi88.66 (5)C1—N1—H1118.0 (16)
O2W—Zn1—O2Wi180.0N1—C5—C4119.93 (14)
O4—S1—O3113.63 (8)N1—C5—H5120.0
O4—S1—O2113.28 (7)C4—C5—H5120.0
O3—S1—O2110.91 (7)C5—C4—C3118.76 (14)
O4—S1—C4106.01 (7)C5—C4—S1119.40 (12)
O3—S1—C4106.05 (7)C3—C4—S1121.84 (12)
O2—S1—C4106.28 (7)C2—C3—C4120.17 (14)
C1—O1—Zn1136.67 (11)C2—C3—H3119.9
Zn1—O1W—H11112.6 (17)C4—C3—H3119.9
O1Wi—Zn1—O1—C128.28 (18)N1—C5—C4—C32.1 (2)
O1W—Zn1—O1—C1−151.72 (18)N1—C5—C4—S1−177.08 (12)
O2W—Zn1—O1—C1116.92 (17)O4—S1—C4—C5−6.85 (15)
O2Wi—Zn1—O1—C1−63.08 (17)O3—S1—C4—C5114.25 (14)
Zn1—O1—C1—N1−171.26 (12)O2—S1—C4—C5−127.66 (13)
Zn1—O1—C1—C29.9 (3)O4—S1—C4—C3173.98 (13)
C3—C2—C1—O1−175.15 (17)O3—S1—C4—C3−64.92 (15)
C3—C2—C1—N16.0 (2)O2—S1—C4—C353.17 (15)
O1—C1—N1—C5173.90 (16)C1—C2—C3—C4−1.2 (2)
C2—C1—N1—C5−7.1 (2)C5—C4—C3—C2−3.0 (2)
C1—N1—C5—C43.2 (3)S1—C4—C3—C2176.21 (13)

Symmetry codes: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1···O2ii0.85 (1)1.99 (1)2.790 (2)157 (2)
O1w—H11···O2iii0.84 (1)1.98 (1)2.809 (2)171 (2)
O1w—H12···O3iv0.84 (1)1.93 (1)2.767 (2)172 (3)
O2w—H21···O3v0.83 (1)2.13 (1)2.926 (2)160 (3)
O2w—H22···O4vi0.84 (1)1.93 (1)2.765 (2)174 (3)

Symmetry codes: (ii) x−1, y, z; (iii) −x+1, −y+1, −z; (iv) −x+1, y−1/2, −z+1/2; (v) x−1, −y+3/2, z+1/2; (vi) x, y, z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU2623).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Gao, S., Zhang, Z.-Y., Huo, L.-H., Zhao, H. & Zhao, J.-G. (2004). Acta Cryst. E60, m1422–m1424.
  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Rigaku (1998). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  • Rigaku/MSC (2002). CrystalClear Rigaku/MSC Inc., The Woodlands, Texas, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2009). publCIF In preparation.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography