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

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ISSN: 2056-9890

catena-Poly[[di­aquacadmium(II)]bis­­(μ-pyridine-3-sulfonato)-κ2N:O;κ2O:N]

aCollege of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, People's Republic of China, bFaculty of Earth Sciences, China University of Geosciences, Wuhan 430074, People's Republic of China, and cDepartment of Resources and Environmental Engineering, Guilin University of Technology, Guilin 541004, People's Republic of China
*Correspondence e-mail: zhihuiqiu299@yahoo.com.cn

(Received 5 March 2008; accepted 21 March 2008; online 29 March 2008)

In the title polymeric complex, [Cd(C5H4NO3S)2(H2O)2]n, the Cd atom is located on a centre of inversion and is coordinated by two O atoms and two N atoms, derived from four different pyridine-3-sulfonate ligands, and two O atoms derived from two water mol­ecules, forming a distorted trans-N2O4 octa­hedral geometry. The topology of the polymer is a one-dimensional chain mediated by bridging pyridine-3-sulfonate anions. These are connected into a three-dimensional architecture via hydrogen bonds.

Related literature

For related literature, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]). For related structures, see: Brodersen et al. (1980[Brodersen, K., Dolling, R. & Liehr, G. (1980). Z. Anorg. Allg. Chem. 464, 17-22.]); Chandrasekhar (1977[Chandrasekhar, K. (1977). Acta Cryst. B33, 143-145.]); Cotton et al. (1992a[Cotton, F. A., Daniels, L. M. & Murillo, C. A. (1992a). Polyhedron, 11, 2475-2481.],b[Cotton, F. A., Daniels, L. M., Montero, M. L. & Murillo, C. A. (1992b). Polyhedron, 11, 2767-2774.]); van der Lee & Barboiu (2004[Lee, A. van der & Barboiu, M. (2004). Acta Cryst. E60, m421-m423.]); Mäkinen et al. (2001[Mäkinen, S. K., Melcer, N. J., Parvez, M. & Shimizu, G. K. H. (2001). Chem. Eur. J. 7, 5176-5182.]); Walsh & Hathaway (1980[Walsh, B. & Hathaway, B. J. (1980). J. Chem. Soc. Dalton Trans. pp. 681-689.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd(C5H4NO3S)2(H2O)2]

  • Mr = 464.74

  • Monoclinic, P 21 /c

  • a = 7.7480 (11) Å

  • b = 13.264 (2) Å

  • c = 7.3291 (11) Å

  • β = 97.081 (2)°

  • V = 747.47 (19) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.78 mm−1

  • T = 294 (2) K

  • 0.26 × 0.22 × 0.18 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 1998[Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.674, Tmax = 0.740

  • 4111 measured reflections

  • 1520 independent reflections

  • 1396 reflections with I > 2σ(I)

  • Rint = 0.023

Refinement
  • R[F2 > 2σ(F2)] = 0.021

  • wR(F2) = 0.053

  • S = 1.10

  • 1520 reflections

  • 115 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.42 e Å−3

  • Δρmin = −0.73 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C5—H5⋯O3i 0.93 2.39 3.256 (3) 155
C4—H4⋯O2ii 0.93 2.55 3.422 (3) 157
O4—H4B⋯O3iii 0.79 (3) 1.99 (4) 2.780 (3) 176 (3)
O4—H4A⋯O2iv 0.81 (3) 1.98 (3) 2.773 (3) 168 (3)
Symmetry codes: (i) [x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (ii) [-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (iii) [-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]; (iv) -x+1, -y+1, -z+2.

Data collection: SMART (Bruker, 1998[Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1998[Bruker (1998). SMART, SAINT and SADABS. 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

Complexes or salts based on pyridinesulfonate are very rare in the Cambridge Structural Database (CSD; Version 5.25; Allen, 2002). A six-coordinate complex with pyridine-3-sulfonate ligands that is closely related to the title complex, (I), has been reported (Walsh & Hathaway, 1980). Other pyridine-3-sulfonate complexes are also available (Brodersen et al., 1980; Cotton et al., 1992a, b; Mäkinen et al., 2001; van der Lee & Barboiu, 2004), as well as that of the acid (Chandrasekhar, 1977).

In (I), Fig. 1, the Cd atom is located on a centre of inversion and is six-coordinated by two N atoms and two O atoms derived from four different pyridine-3-sulfonate molecules, and two O atoms derived from two water molecules. The resulting trans-N2O4 donor sets defines a distorted octahedral environment for Cd with angles ranging from 84.76 (7) to 180°, Cd—O distances in the range 2.2872 (18) to 2.3113 (17) Å, and Cd—N distances of 2.3233 (18) and 2.3234 (18) Å.

The molecules aggregate via bridging pyridine-3-sulfonate anions to form a chain. In the crystal structure, chains are linked into a 3-D architecture via hydrogen bonding interactions, Table 1 & Fig. 2.

Related literature top

For related literature, see: Allen (2002). For related structures, see: Brodersen et al. (1980); Chandrasekhar (1977); Cotton et al. (1992a,b); van der Lee & Barboiu (2004); Mäkinen et al. (2001); Walsh & Hathaway (1980).

Experimental top

Pyridine-3-sulfonate, (1 mmol, 159 mg) was dissolved in methanol (A.R., 99.9%) (10 ml). To the resulting clear solution was added CdCl2.6H2O (0.5 mmol, 149 mg) in methanol (10 ml). After keeping the resulting mixture in air to evaporate about half of the solvent, colourless blocks of (I) were deposited. The crystals were isolated, washed with ethanol three times (Yield 74%). Analysis: found: C, 25.98; H, 2.66; N, 6.08; S, 13.84; C10H12CdN2O8S2 requires: C, 25.82; H, 2.58; N, 6.02; S, 14.27.

Refinement top

The C-bound H atoms were included in the riding model approximation with C—H = 0.93–0.96 Å, and with Uiso(H)= 1.2Ueq(C)-1.5Ueq(C). The water-bound H atoms were located in difference Fourier maps and the O—H distances were refined without constraint, see Table 1 for distances.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); 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. Extended structure in (I) showing the coordination geometry for the Cd atom, the atom labelling scheme and displacement ellipsoids at the 50% probability level. The Cd atom is located at a center of inversion.
[Figure 2] Fig. 2. Crystal packing of (I) viewed approximately down the a-direction showing the hydrogen bonding interactions as dashed lines.
catena-Poly[[diaquacadmium(II)]bis(µ-pyridine-3-sulfonato)- κ2N:O;κ2O:N] top
Crystal data top
[Cd(C5H4NO3S)2(H2O)2]F(000) = 460
Mr = 464.74Dx = 2.065 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3022 reflections
a = 7.7480 (11) Åθ = 3.1–26.3°
b = 13.264 (2) ŵ = 1.78 mm1
c = 7.3291 (11) ÅT = 294 K
β = 97.081 (2)°Block, colourless
V = 747.47 (19) Å30.26 × 0.22 × 0.18 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
1520 independent reflections
Radiation source: fine-focus sealed tube1396 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ϕ and ο scansθmax = 26.3°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 96
Tmin = 0.674, Tmax = 0.740k = 1615
4111 measured reflectionsl = 49
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)] = 0.021H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.053 w = 1/[σ2(Fo2) + (0.0952P)2 + 1.5031P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
1520 reflectionsΔρmax = 0.42 e Å3
115 parametersΔρmin = 0.73 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.087 (3)
Crystal data top
[Cd(C5H4NO3S)2(H2O)2]V = 747.47 (19) Å3
Mr = 464.74Z = 2
Monoclinic, P21/cMo Kα radiation
a = 7.7480 (11) ŵ = 1.78 mm1
b = 13.264 (2) ÅT = 294 K
c = 7.3291 (11) Å0.26 × 0.22 × 0.18 mm
β = 97.081 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
1520 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
1396 reflections with I > 2σ(I)
Tmin = 0.674, Tmax = 0.740Rint = 0.023
4111 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0210 restraints
wR(F2) = 0.053H atoms treated by a mixture of independent and constrained refinement
S = 1.10Δρmax = 0.42 e Å3
1520 reflectionsΔρmin = 0.73 e Å3
115 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
Cd10.00000.50000.50000.02008 (12)
S10.71583 (7)0.62259 (4)0.77922 (8)0.02183 (15)
N10.2044 (2)0.62074 (14)0.6090 (3)0.0246 (4)
O10.7687 (2)0.57880 (16)0.6122 (3)0.0449 (5)
O20.7069 (2)0.54880 (14)0.9231 (3)0.0392 (5)
O30.8146 (2)0.71095 (13)0.8402 (3)0.0377 (4)
C10.3697 (3)0.59388 (16)0.6647 (3)0.0234 (5)
H10.39790.52570.67220.028*
C20.4994 (3)0.66450 (17)0.7113 (3)0.0202 (4)
C30.4585 (3)0.76576 (17)0.7005 (4)0.0276 (5)
H30.54390.81430.73000.033*
C40.2885 (3)0.79362 (18)0.6450 (4)0.0317 (5)
H40.25720.86130.63800.038*
C50.1657 (3)0.71933 (18)0.6000 (3)0.0268 (5)
H50.05140.73850.56190.032*
O40.0841 (3)0.40325 (16)0.7537 (3)0.0359 (4)
H4A0.140 (4)0.426 (2)0.845 (5)0.046 (10)*
H4B0.113 (4)0.348 (3)0.733 (5)0.043 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01370 (15)0.02211 (16)0.02355 (16)0.00007 (8)0.00117 (9)0.00150 (8)
S10.0152 (3)0.0238 (3)0.0254 (3)0.0008 (2)0.0021 (2)0.0035 (2)
N10.0181 (9)0.0241 (9)0.0305 (10)0.0004 (8)0.0018 (8)0.0032 (8)
O10.0238 (9)0.0694 (14)0.0411 (11)0.0142 (9)0.0027 (8)0.0210 (10)
O20.0327 (10)0.0345 (10)0.0475 (12)0.0032 (8)0.0070 (8)0.0145 (9)
O30.0270 (9)0.0304 (9)0.0518 (11)0.0079 (7)0.0107 (8)0.0012 (9)
C10.0191 (11)0.0197 (10)0.0301 (12)0.0014 (8)0.0016 (9)0.0018 (9)
C20.0173 (10)0.0245 (11)0.0189 (10)0.0005 (8)0.0022 (8)0.0020 (8)
C30.0231 (11)0.0207 (11)0.0391 (13)0.0044 (9)0.0049 (10)0.0049 (10)
C40.0297 (13)0.0211 (11)0.0444 (15)0.0042 (10)0.0047 (11)0.0008 (10)
C50.0187 (11)0.0296 (12)0.0313 (12)0.0056 (9)0.0001 (9)0.0007 (10)
O40.0454 (11)0.0315 (10)0.0280 (10)0.0043 (9)0.0059 (8)0.0025 (8)
Geometric parameters (Å, º) top
Cd1—O4i2.2872 (18)O1—Cd1iv2.3113 (17)
Cd1—O42.2873 (18)C1—C21.386 (3)
Cd1—O1ii2.3113 (17)C1—H10.9300
Cd1—O1iii2.3113 (17)C2—C31.380 (3)
Cd1—N1i2.3233 (18)C3—C41.380 (4)
Cd1—N12.3234 (18)C3—H30.9300
S1—O31.4404 (18)C4—C51.382 (3)
S1—O21.4466 (19)C4—H40.9300
S1—O11.4587 (19)C5—H50.9300
S1—C21.779 (2)O4—H4A0.81 (3)
N1—C51.341 (3)O4—H4B0.79 (3)
N1—C11.344 (3)
O4i—Cd1—O4180C5—N1—Cd1121.09 (15)
O4i—Cd1—O1ii83.10 (8)C1—N1—Cd1120.36 (15)
O4—Cd1—O1ii96.90 (8)S1—O1—Cd1iv142.09 (12)
O4i—Cd1—O1iii96.90 (8)N1—C1—C2122.1 (2)
O4—Cd1—O1iii83.10 (8)N1—C1—H1119.0
O1ii—Cd1—O1iii180C2—C1—H1119.0
O4i—Cd1—N1i89.62 (7)C3—C2—C1119.3 (2)
O4—Cd1—N1i90.38 (7)C3—C2—S1121.48 (17)
O1ii—Cd1—N1i84.76 (7)C1—C2—S1119.21 (17)
O1iii—Cd1—N1i95.24 (7)C4—C3—C2118.8 (2)
O4i—Cd1—N190.37 (7)C4—C3—H3120.6
O4—Cd1—N189.63 (7)C2—C3—H3120.6
O1ii—Cd1—N195.24 (7)C3—C4—C5118.9 (2)
O1iii—Cd1—N184.76 (7)C3—C4—H4120.5
N1i—Cd1—N1180C5—C4—H4120.5
O3—S1—O2113.30 (12)N1—C5—C4122.7 (2)
O3—S1—O1113.01 (13)N1—C5—H5118.6
O2—S1—O1112.70 (13)C4—C5—H5118.6
O3—S1—C2106.20 (11)Cd1—O4—H4A122 (2)
O2—S1—C2106.70 (11)Cd1—O4—H4B115 (2)
O1—S1—C2104.03 (10)H4A—O4—H4B112 (3)
C5—N1—C1118.18 (19)
O4i—Cd1—N1—C542.65 (19)N1—C1—C2—S1178.71 (18)
O4—Cd1—N1—C5137.35 (19)O3—S1—C2—C38.3 (2)
O1ii—Cd1—N1—C540.45 (19)O2—S1—C2—C3129.5 (2)
O1iii—Cd1—N1—C5139.55 (19)O1—S1—C2—C3111.2 (2)
O4i—Cd1—N1—C1130.30 (18)O3—S1—C2—C1173.02 (19)
O4—Cd1—N1—C149.70 (18)O2—S1—C2—C151.9 (2)
O1ii—Cd1—N1—C1146.60 (18)O1—S1—C2—C167.5 (2)
O1iii—Cd1—N1—C133.40 (18)C1—C2—C3—C40.6 (4)
O3—S1—O1—Cd1iv65.4 (2)S1—C2—C3—C4179.29 (19)
O2—S1—O1—Cd1iv64.7 (2)C2—C3—C4—C50.8 (4)
C2—S1—O1—Cd1iv179.9 (2)C1—N1—C5—C40.2 (4)
C5—N1—C1—C20.4 (3)Cd1—N1—C5—C4172.90 (19)
Cd1—N1—C1—C2172.76 (16)C3—C4—C5—N10.4 (4)
N1—C1—C2—C30.0 (3)
Symmetry codes: (i) x, y+1, z+1; (ii) x1, y, z; (iii) x+1, y+1, z+1; (iv) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···O3v0.932.393.256 (3)155
C4—H4···O2vi0.932.553.422 (3)157
O4—H4B···O3vii0.79 (3)1.99 (4)2.780 (3)176 (3)
O4—H4A···O2viii0.81 (3)1.98 (3)2.773 (3)168 (3)
Symmetry codes: (v) x1, y+3/2, z1/2; (vi) x+1, y+1/2, z+3/2; (vii) x+1, y1/2, z+3/2; (viii) x+1, y+1, z+2.

Experimental details

Crystal data
Chemical formula[Cd(C5H4NO3S)2(H2O)2]
Mr464.74
Crystal system, space groupMonoclinic, P21/c
Temperature (K)294
a, b, c (Å)7.7480 (11), 13.264 (2), 7.3291 (11)
β (°) 97.081 (2)
V3)747.47 (19)
Z2
Radiation typeMo Kα
µ (mm1)1.78
Crystal size (mm)0.26 × 0.22 × 0.18
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.674, 0.740
No. of measured, independent and
observed [I > 2σ(I)] reflections
4111, 1520, 1396
Rint0.023
(sin θ/λ)max1)0.623
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.053, 1.10
No. of reflections1520
No. of parameters115
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.42, 0.73

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···O3i0.932.393.256 (3)155
C4—H4···O2ii0.932.553.422 (3)157
O4—H4B···O3iii0.79 (3)1.99 (4)2.780 (3)176 (3)
O4—H4A···O2iv0.81 (3)1.98 (3)2.773 (3)168 (3)
Symmetry codes: (i) x1, y+3/2, z1/2; (ii) x+1, y+1/2, z+3/2; (iii) x+1, y1/2, z+3/2; (iv) x+1, y+1, z+2.
 

Acknowledgements

This work was supported by the Natural Science Foundation of Guangxi (GuiKeJi0639031), People's Republic of China. This research was also sponsored by the Program for Hundred Outstanding Young Teachers in Higher Education Institutions of Guangxi, People's Republic of China.

References

First citationAllen, F. H. (2002). Acta Cryst. B58, 380–388.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationBrodersen, K., Dolling, R. & Liehr, G. (1980). Z. Anorg. Allg. Chem. 464, 17–22.  CSD CrossRef CAS Web of Science Google Scholar
First citationBruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
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First citationCotton, F. A., Daniels, L. M., Montero, M. L. & Murillo, C. A. (1992b). Polyhedron, 11, 2767–2774.  CSD CrossRef CAS Web of Science Google Scholar
First citationCotton, F. A., Daniels, L. M. & Murillo, C. A. (1992a). Polyhedron, 11, 2475–2481.  CSD CrossRef CAS Web of Science Google Scholar
First citationLee, A. van der & Barboiu, M. (2004). Acta Cryst. E60, m421–m423.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationMäkinen, S. K., Melcer, N. J., Parvez, M. & Shimizu, G. K. H. (2001). Chem. Eur. J. 7, 5176–5182.  CrossRef PubMed CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWalsh, B. & Hathaway, B. J. (1980). J. Chem. Soc. Dalton Trans. pp. 681–689.  CSD CrossRef Web of Science Google Scholar

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