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Acta Cryst. (2008). E64, m1137    [ doi:10.1107/S1600536808024720 ]

catena-Poly[[diaqua[(4-tolylsulfanyl)acetato-[kappa]O]cadmium(II)]-[mu]-4,4'-bipyridine-[kappa]2N:N']

W.-X. Cai, X.-Y. Zheng, X.-H. Geng and Y.-L. Feng

Abstract top

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.

Comment top

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.

Related literature top

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

Experimental top

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 top

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).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); 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. 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.]
[Figure 2] Fig. 2. The chain structure of the title compound. All H atoms have been omitted for clarity.
catena-Poly[[diaqua[(4-tolylsulfanyl)acetato-κO]cadmium(II)]- µ-4,4'-bipyridine-κ2N:N'] top
Crystal data top
[Cd(C9H9O2S)2(C10H8N2)(H2O)2]F000 = 1360
Mr = 667.09Dx = 1.589 Mg m−3
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 mm−1
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 top
Bruker APEXII area-detector
diffractometer		3154 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 top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H 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 Å−3
184 parametersΔρmin = −0.37 e Å−3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Cd(C9H9O2S)2(C10H8N2)(H2O)2]V = 2789.3 (9) Å3
Mr = 667.09Z = 4
Monoclinic, C2/cMo Kα
a = 21.659 (4) ŵ = 0.98 mm−1
b = 11.590 (2) ÅT = 296 (2) K
c = 11.137 (2) Å0.40 × 0.35 × 0.17 mm
β = 93.88 (3)º
Data collection top
Bruker APEXII area-detector
diffractometer		3154 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2937 reflections with I > 2σ(I)
Tmin = 0.68, Tmax = 0.85Rint = 0.017
12185 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0323 restraints
wR(F2) = 0.112H atoms treated by a mixture of
independent and constrained refinement
S = 1.12Δρmax = 0.60 e Å−3
3154 reflectionsΔρmin = −0.37 e Å−3
184 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
Cd10.00000.05131 (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) top
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, °) top
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, °) top
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.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O20.821.942.667 (4)148
O1W—H1WB···O1i0.805 (17)2.04 (2)2.782 (3)154 (4)
Symmetry codes: (i) x, −y, z+1/2.
references
References top

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.

Zheng, X.-Y., Su, H. & Feng, Y.-L. (2006). Acta Cryst. E62, m1393–m1394.