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Acta Crystallogr Sect E Struct Rep Online. 2008 September 1; 64(Pt 9): m1137.
Published online 2008 August 6. doi:  10.1107/S1600536808024720
PMCID: PMC2960514

catena-Poly[[diaqua­[(4-tolyl­sulfan­yl)acetato-κO]cadmium(II)]-μ-4,4′-bipyridine-κ2 N:N′]

Abstract

The title complex, [Cd(C9H9O2S)2(C10H8N2)(H2O)2]n, has a linear chain structure. The central CdII ion is in a slightly disorted octa­hedral environment, coordinated by two aqua ligands, two (4-tolyl­sulfan­yl)acetate ligands and two bridging 4,4′-bipyridine ligands. The CdII ion lies on a twofold rotation axis. Inter­molecular O—H(...)O hydrogen bonds connect adjacent chains, forming a layer structure. An intramolecular O—H(...)O hydrogen bond is also present.

Related literature

For related literature, see: Lin et al. (2006 [triangle]); Zheng et al. (2006 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1137-scheme1.jpg

Experimental

Crystal data

  • [Cd(C9H9O2S)2(C10H8N2)(H2O)2]
  • M r = 667.09
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1137-efi2.jpg
  • a = 21.659 (4) Å
  • b = 11.590 (2) Å
  • c = 11.137 (2) Å
  • β = 93.88 (3)°
  • V = 2789.3 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.98 mm−1
  • T = 296 (2) K
  • 0.40 × 0.35 × 0.17 mm

Data collection

  • Bruker APEXII area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.68, T max = 0.85
  • 12185 measured reflections
  • 3154 independent reflections
  • 2937 reflections with I > 2σ(I)
  • R int = 0.017

Refinement

  • R[F 2 > 2σ(F 2)] = 0.032
  • wR(F 2) = 0.112
  • S = 1.12
  • 3154 reflections
  • 184 parameters
  • 3 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.60 e Å−3
  • Δρmin = −0.37 e Å−3

Data collection: APEX2 (Bruker, 2006 [triangle]); cell refinement: SAINT (Bruker, 2006 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808024720/at2595sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808024720/at2595Isup2.hkl

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

supplementary crystallographic information

Comment

The title compound, (I), is isostructural with the NiII (Lin et al., 2006) and CoII analogues (Zheng et al., 2006). The structure of (I) (Fig.1) consists of linear chains formed through 4,4'-bipy ligands linking six-coordinated CdII ions which lie on twofold rotation axes. Intermolecular O—H···O hydrogen bonds link neighboring chains to form a two-dimensional network. It is notable that these chains are arranged alternately and the 4-tolysulfanyl groups are almost coplanar. There is no signifcant π-π interactions between the planes of adjacent chains with centroid-centroid distance of 6.19 (1)Å and plane-to-plane distance of 3.64 (1) Å.

Experimental

CdSO4.8/3H2O (0.128 g, 0.5 mmol), (4-tolylsulfanyl)acetic acid (0.091 g, 0.5 mmol), 4,4'-bipy (0.039 g, 0.25 mmol) and H2O (18 ml) were sealed in a 25 ml stainless-steel reactor with a Teflon-lined stainless steel reactor and the solution was heated at 433 K for 72 h and then cooled to room temperature over a period of 72 h. Colourless crystals suitable for X-ray analysis were obtained.

Refinement

The methyl groups were allowed to rotate to fit the electron density [C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C)]; the other H atoms were positioned geometrically [aromatic C—H = 0.93 Å and aliphatic C—H = 0.97 Å, Uiso(H) = 1.2Ueq(C)]. Water H atom H1WA was positioned geometrically, with O—H = 0.82 Å, and the other water H atoms H1WB was located from a difference Fourier map, and they were refined with distance restraints of O—H = 0.85 (2) Å and H···H = 1.30 (2) Å; their displacement parameters were set to 1.5Ueq(O).

Figures

Fig. 1.
A view of part of the title structure, showing 30% probability displacement ellipsoids. [Symmetry codes: (a) -x, y, -z+1/2; (b) x, y+1, z; (c) x, y-1, z.]
Fig. 2.
The chain structure of the title compound. All H atoms have been omitted for clarity.

Crystal data

[Cd(C9H9O2S)2(C10H8N2)(H2O)2]F000 = 1360
Mr = 667.09Dx = 1.589 Mg m3
Monoclinic, C2/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 7745 reflections
a = 21.659 (4) Åθ = 2.7–27.5º
b = 11.590 (2) ŵ = 0.98 mm1
c = 11.137 (2) ÅT = 296 (2) K
β = 93.88 (3)ºBlock, colourless
V = 2789.3 (9) Å30.40 × 0.35 × 0.17 mm
Z = 4

Data collection

Bruker APEXII area-detector diffractometer3154 independent reflections
Radiation source: fine-focus sealed tube2937 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.017
T = 296(2) Kθmax = 27.5º
ω scansθmin = 2.7º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −27→27
Tmin = 0.68, Tmax = 0.85k = −14→14
12185 measured reflectionsl = −14→14

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.112  w = 1/[σ2(Fo2) + (0.0658P)2 + 5.8321P] where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
3154 reflectionsΔρmax = 0.60 e Å3
184 parametersΔρmin = −0.37 e Å3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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)

xyzUiso*/Ueq
Cd10.00000.05131 (2)0.25000.03198 (12)
S10.14880 (4)0.21253 (9)−0.05125 (7)0.0514 (2)
O10.08144 (10)0.05635 (16)0.1325 (2)0.0353 (5)
O1W0.06445 (12)0.0644 (2)0.4169 (2)0.0415 (5)
H1WA0.09900.08360.39820.062*
H1WB0.0700 (14)0.012 (3)0.464 (3)0.047 (11)*
O20.15198 (12)0.1218 (3)0.2705 (2)0.0632 (8)
N10.0000−0.1422 (3)0.25000.0290 (6)
N20.0000−0.7537 (3)0.25000.0303 (7)
C10.16190 (13)0.3534 (3)0.0059 (3)0.0422 (7)
C20.19048 (16)0.3817 (4)0.1177 (3)0.0506 (9)
H2A0.20250.32340.17170.061*
C30.20102 (17)0.4945 (4)0.1488 (3)0.0544 (9)
H3A0.22100.51090.22340.065*
C40.18302 (16)0.5854 (4)0.0730 (3)0.0520 (8)
C50.15375 (18)0.5566 (3)−0.0382 (3)0.0508 (9)
H5A0.14070.6152−0.09100.061*
C60.14372 (16)0.4440 (3)−0.0715 (3)0.0469 (9)
H6A0.12450.4275−0.14680.056*
C70.1952 (2)0.7075 (5)0.1109 (4)0.0714 (12)
H7A0.23890.71860.12710.107*
H7B0.17420.72360.18220.107*
H7C0.18030.75860.04760.107*
C80.17850 (15)0.1165 (4)0.0670 (3)0.0495 (8)
H8A0.18790.04260.03160.059*
H8B0.21690.14810.10290.059*
C90.13410 (13)0.0967 (3)0.1664 (3)0.0385 (6)
C10−0.02550 (18)−0.2021 (3)0.3350 (3)0.0470 (8)
H10A−0.0435−0.16190.39590.056*
C11−0.02676 (18)−0.3207 (3)0.3379 (3)0.0441 (8)
H11A−0.0457−0.35840.39920.053*
C120.0000−0.3838 (3)0.25000.0259 (7)
C130.0000−0.5111 (3)0.25000.0250 (7)
C14−0.02533 (15)−0.5744 (3)0.3404 (3)0.0357 (6)
H14A−0.0432−0.53630.40290.043*
C15−0.02423 (15)−0.6931 (3)0.3382 (3)0.0365 (6)
H15A−0.0410−0.73310.40060.044*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.03971 (19)0.02551 (18)0.03160 (18)0.0000.00893 (12)0.000
S10.0526 (5)0.0682 (6)0.0343 (4)−0.0107 (4)0.0090 (3)0.0052 (4)
O10.0353 (11)0.0355 (11)0.0362 (11)−0.0019 (7)0.0104 (9)−0.0040 (8)
O1W0.0525 (13)0.0448 (12)0.0281 (10)0.0011 (10)0.0085 (9)0.0047 (9)
O20.0444 (13)0.107 (2)0.0385 (13)−0.0222 (15)0.0024 (10)0.0066 (14)
N10.0354 (16)0.0245 (15)0.0280 (15)0.0000.0076 (13)0.000
N20.0364 (16)0.0283 (16)0.0272 (15)0.0000.0089 (13)0.000
C10.0259 (13)0.071 (2)0.0310 (14)−0.0051 (13)0.0104 (11)0.0042 (14)
C20.0409 (16)0.080 (3)0.0311 (15)−0.0024 (17)0.0043 (12)0.0064 (16)
C30.0416 (17)0.088 (3)0.0336 (16)−0.0069 (19)0.0047 (13)−0.0062 (18)
C40.0392 (16)0.074 (2)0.0447 (18)−0.0076 (17)0.0169 (14)−0.0093 (18)
C50.0455 (19)0.068 (3)0.0399 (18)0.0016 (15)0.0091 (15)0.0059 (15)
C60.0368 (16)0.074 (3)0.0302 (15)−0.0021 (14)0.0025 (12)0.0062 (14)
C70.070 (3)0.080 (3)0.066 (3)−0.010 (2)0.023 (2)−0.014 (2)
C80.0342 (15)0.067 (2)0.0492 (18)0.0037 (15)0.0146 (13)0.0072 (16)
C90.0321 (13)0.0426 (16)0.0417 (16)0.0027 (12)0.0084 (12)0.0068 (13)
C100.073 (2)0.0307 (15)0.0411 (16)0.0028 (15)0.0315 (16)−0.0034 (13)
C110.069 (2)0.0292 (14)0.0374 (15)0.0012 (14)0.0306 (15)0.0021 (12)
C120.0284 (16)0.0253 (17)0.0245 (16)0.0000.0048 (13)0.000
C130.0260 (16)0.0236 (17)0.0259 (16)0.0000.0047 (13)0.000
C140.0510 (17)0.0298 (13)0.0289 (13)−0.0056 (12)0.0207 (12)−0.0053 (11)
C150.0506 (16)0.0293 (14)0.0320 (13)−0.0068 (12)0.0198 (12)−0.0030 (11)

Geometric parameters (Å, °)

Cd1—N12.243 (3)C4—C51.393 (5)
Cd1—O1W2.253 (2)C4—C71.495 (6)
Cd1—O1Wi2.253 (2)C5—C61.371 (5)
Cd1—N2ii2.259 (3)C5—H5A0.9300
Cd1—O12.267 (2)C6—H6A0.9300
Cd1—O1i2.267 (2)C7—H7A0.9600
S1—C11.769 (4)C7—H7B0.9600
S1—C81.809 (4)C7—H7C0.9600
O1—C91.266 (4)C8—C91.532 (4)
O1W—H1WA0.8200C8—H8A0.9700
O1W—H1WB0.805 (17)C8—H8B0.9700
O2—C91.232 (4)C10—C111.375 (4)
N1—C10i1.325 (3)C10—H10A0.9300
N1—C101.325 (3)C11—C121.381 (3)
N2—C151.343 (3)C11—H11A0.9300
N2—C15i1.343 (3)C12—C11i1.381 (3)
N2—Cd1iii2.259 (3)C12—C131.475 (5)
C1—C21.391 (5)C13—C14i1.389 (3)
C1—C61.398 (5)C13—C141.389 (3)
C2—C31.367 (7)C14—C151.376 (4)
C2—H2A0.9300C14—H14A0.9300
C3—C41.389 (6)C15—H15A0.9300
C3—H3A0.9300
N1—Cd1—O1W93.87 (6)C6—C5—H5A119.2
N1—Cd1—O1Wi93.87 (6)C4—C5—H5A119.2
O1W—Cd1—O1Wi172.26 (12)C5—C6—C1121.0 (3)
N1—Cd1—N2ii180.0C5—C6—H6A119.5
O1W—Cd1—N2ii86.13 (6)C1—C6—H6A119.5
O1Wi—Cd1—N2ii86.13 (6)C4—C7—H7A109.5
N1—Cd1—O191.48 (5)C4—C7—H7B109.5
O1W—Cd1—O190.67 (9)H7A—C7—H7B109.5
O1Wi—Cd1—O189.13 (9)C4—C7—H7C109.5
N2ii—Cd1—O188.52 (5)H7A—C7—H7C109.5
N1—Cd1—O1i91.48 (5)H7B—C7—H7C109.5
O1W—Cd1—O1i89.13 (9)C9—C8—S1114.1 (2)
O1Wi—Cd1—O1i90.67 (9)C9—C8—H8A108.7
N2ii—Cd1—O1i88.52 (5)S1—C8—H8A108.7
O1—Cd1—O1i177.04 (10)C9—C8—H8B108.7
C1—S1—C8105.40 (18)S1—C8—H8B108.7
C9—O1—Cd1123.9 (2)H8A—C8—H8B107.6
Cd1—O1W—H1WA109.5O2—C9—O1126.0 (3)
Cd1—O1W—H1WB123 (3)O2—C9—C8118.2 (3)
H1WA—O1W—H1WB105.7O1—C9—C8115.9 (3)
C10i—N1—C10116.8 (4)N1—C10—C11123.4 (3)
C10i—N1—Cd1121.62 (18)N1—C10—H10A118.3
C10—N1—Cd1121.62 (18)C11—C10—H10A118.3
C15—N2—C15i116.8 (4)C10—C11—C12120.2 (3)
C15—N2—Cd1iii121.58 (18)C10—C11—H11A119.9
C15i—N2—Cd1iii121.58 (18)C12—C11—H11A119.9
C2—C1—C6117.7 (4)C11i—C12—C11116.0 (4)
C2—C1—S1126.2 (3)C11i—C12—C13122.02 (18)
C6—C1—S1116.1 (3)C11—C12—C13122.02 (18)
C3—C2—C1120.6 (4)C14i—C13—C14116.2 (3)
C3—C2—H2A119.7C14i—C13—C12121.89 (17)
C1—C2—H2A119.7C14—C13—C12121.89 (17)
C2—C3—C4122.4 (3)C15—C14—C13120.4 (3)
C2—C3—H3A118.8C15—C14—H14A119.8
C4—C3—H3A118.8C13—C14—H14A119.8
C3—C4—C5116.8 (4)N2—C15—C14123.0 (3)
C3—C4—C7120.6 (4)N2—C15—H15A118.5
C5—C4—C7122.6 (4)C14—C15—H15A118.5
C6—C5—C4121.5 (4)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x, y+1, z; (iii) x, y−1, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O20.821.942.667 (4)148
O1W—H1WB···O1iv0.805 (17)2.04 (2)2.782 (3)154 (4)

Symmetry codes: (iv) x, −y, z+1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: AT2595).

References

  • Bruker (2006). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Lin, H., Su, H. & Feng, Y. (2006). Acta Cryst. E62, m747–m749.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Zheng, X.-Y., Su, H. & Feng, Y.-L. (2006). Acta Cryst. E62, m1393–m1394.

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