supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers Open access

hb2722 scheme

Acta Cryst. (2008). E64, m694    [ doi:10.1107/S1600536808010878 ]

Hexaaquacadmium(II) bis[4-(2-hydroxybenzylideneamino)benzenesulfonate] dihydrate

X.-S. Tai, J. Xu, Y.-M. Feng and Z.-P. Liang

Abstract top

In the title compound, [Cd(H2O)6](C13H10NO4S)2·2H2O, the Cd atom (site symmetry \overline{1}) adopts a regular octahedral coordination and the anion is stabilized by an intramolecular O-H...N hydrogen bond. O-H...O hydrogen bonds involving the coordinated and uncoordinated water molecules lead to a three-dimensional network.

Comment top

As part of our ongoing studies of the synthesis and coordination chemistry of Schiff-base ligands (e.g. Tai et al., 2008), we now report the synthesis and structure of the title compound, (I), (Fig. 1), in which the organic species does not coordiate to the metal and a hydrated molecular salt arises.

The Cd atom (site symmetry 1) in (I) is bonded to six water molecules (Table 1). The anion is stablisied by an intramolecular O-H···N hydrogen bond (Table 2), which perhaps correlates with the fact that the aromatic rings are almost co-planar [dihedral angle = 4.09 (14)°].

The water molecules, both bound and unbound, participate in O-H···O hydrogen bonds to link the component speices into a three-dimensional network.

Related literature top

For related literature, see: Tai et al. (2008).

Experimental top

1 mmol of cadmium nitrate was added to a solution of salicylaldehyde-4-aminobenzene sulfonic acid (1 mmol) in 10 ml of 95% ethanol. The mixture was stirred for 2 h at refluxing temperature. Evaporating some ethanol, clear blocks of (I) were obtained after one weeks.

Refinement top

The H atoms were placed geometrically (C—H = 0.93–0.96 Å, O—H = 0.85Å) and refined as riding with Uiso(H) = 1.2Ueq(carrier).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); 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. The molecular structure of (I) showing 50% displacement ellipsoids (arbitrary spheres for the H atoms). The hydrogen bonds are indicated by double-dashed lines. Symmetry code: (i) 1-x, 1-y, 1-z.
Hexaaquacadmium(II) bis[4-(2-hydroxybenzylideneamino)benzenesulfonate] dihydrate top
Crystal data top
[Cd(H2O)6](C13H10NO4S)2·2H2OF000 = 828
Mr = 809.09Dx = 1.626 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4564 reflections
a = 18.464 (2) Åθ = 2.6–27.9º
b = 6.1488 (8) ŵ = 0.86 mm−1
c = 14.5701 (12) ÅT = 298 (2) K
β = 92.226 (2)ºBlock, colourless
V = 1652.9 (3) Å30.48 × 0.45 × 0.18 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer		2904 independent reflections
Radiation source: fine-focus sealed tube2447 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.035
T = 298(2) Kθmax = 25.0º
ω scansθmin = 2.2º
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −21→21
Tmin = 0.682, Tmax = 0.860k = −7→5
7936 measured reflectionsl = −17→16
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)] = 0.028H-atom parameters constrained
wR(F2) = 0.075  w = 1/[σ2(Fo2) + (0.0376P)2 + 0.6281P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
2904 reflectionsΔρmax = 0.28 e Å−3
214 parametersΔρmin = −0.60 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Cd(H2O)6](C13H10NO4S)2·2H2OV = 1652.9 (3) Å3
Mr = 809.09Z = 2
Monoclinic, P21/cMo Kα
a = 18.464 (2) ŵ = 0.86 mm−1
b = 6.1488 (8) ÅT = 298 (2) K
c = 14.5701 (12) Å0.48 × 0.45 × 0.18 mm
β = 92.226 (2)º
Data collection top
Bruker SMART CCD
diffractometer		2904 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		2447 reflections with I > 2σ(I)
Tmin = 0.682, Tmax = 0.860Rint = 0.035
7936 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028214 parameters
wR(F2) = 0.075H-atom parameters constrained
S = 1.06Δρmax = 0.28 e Å−3
2904 reflectionsΔρmin = −0.60 e Å−3
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
Cd10.50000.50000.50000.03115 (11)
N10.00853 (11)0.8935 (4)0.61988 (16)0.0392 (5)
O10.35962 (10)0.9727 (3)0.59697 (14)0.0419 (5)
O20.34686 (10)0.9949 (3)0.76142 (14)0.0424 (5)
O30.33264 (10)1.3176 (3)0.66883 (14)0.0425 (5)
O4−0.09042 (11)0.6152 (4)0.56383 (17)0.0655 (7)
H4−0.04930.66180.57420.098*
O50.50034 (11)0.1696 (3)0.56929 (14)0.0472 (5)
H5A0.45730.12740.57790.057*
H5B0.52350.17500.62080.057*
O60.46644 (10)0.3400 (3)0.36324 (12)0.0425 (5)
H6A0.49970.35700.32510.051*
H6B0.42790.39870.34120.051*
O70.38005 (10)0.5588 (3)0.52336 (13)0.0415 (5)
H7A0.37450.68860.54180.050*
H7B0.36630.47360.56520.050*
O80.42645 (10)0.6168 (3)0.76420 (13)0.0462 (5)
H8A0.40350.73660.76460.055*
H8B0.40000.52300.73620.055*
S10.32404 (3)1.08214 (11)0.67158 (5)0.03098 (16)
C10.23015 (14)1.0294 (4)0.65692 (18)0.0296 (6)
C20.18127 (14)1.1822 (5)0.6840 (2)0.0463 (8)
H20.19761.31250.70980.056*
C30.10786 (15)1.1428 (5)0.6730 (2)0.0523 (9)
H30.07491.24700.69120.063*
C40.08304 (14)0.9485 (5)0.63495 (19)0.0343 (6)
C50.13250 (15)0.7954 (5)0.6086 (2)0.0447 (7)
H50.11630.66470.58300.054*
C60.20627 (14)0.8343 (5)0.6199 (2)0.0440 (7)
H60.23950.72960.60270.053*
C7−0.04225 (15)1.0304 (5)0.6320 (2)0.0406 (7)
H7−0.03021.17090.65070.049*
C8−0.11807 (14)0.9738 (4)0.61762 (19)0.0368 (7)
C9−0.13909 (15)0.7700 (5)0.5839 (2)0.0437 (7)
C10−0.21291 (15)0.7219 (5)0.5712 (2)0.0522 (8)
H10−0.22730.58610.54910.063*
C11−0.26382 (16)0.8743 (6)0.5911 (2)0.0521 (8)
H11−0.31270.84030.58260.063*
C12−0.24418 (16)1.0779 (6)0.6235 (2)0.0529 (8)
H12−0.27931.18080.63610.064*
C13−0.17160 (15)1.1260 (5)0.6369 (2)0.0464 (7)
H13−0.15801.26230.65920.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03180 (16)0.03028 (17)0.03128 (16)0.00014 (11)0.00026 (11)−0.00045 (11)
N10.0266 (12)0.0439 (14)0.0467 (14)−0.0041 (11)−0.0031 (10)−0.0035 (11)
O10.0316 (10)0.0456 (12)0.0490 (12)−0.0008 (8)0.0082 (9)−0.0114 (9)
O20.0331 (10)0.0496 (13)0.0438 (12)−0.0010 (8)−0.0079 (9)0.0034 (9)
O30.0378 (10)0.0300 (10)0.0600 (13)−0.0074 (8)0.0050 (9)−0.0035 (9)
O40.0424 (12)0.0513 (14)0.102 (2)−0.0018 (11)−0.0095 (12)−0.0244 (14)
O50.0534 (12)0.0412 (12)0.0463 (12)−0.0071 (10)−0.0058 (9)0.0082 (9)
O60.0426 (11)0.0443 (11)0.0399 (11)0.0034 (9)−0.0062 (9)−0.0043 (9)
O70.0358 (10)0.0384 (11)0.0508 (12)0.0016 (9)0.0067 (9)−0.0007 (9)
O80.0505 (12)0.0381 (12)0.0492 (12)0.0031 (9)−0.0094 (9)−0.0032 (9)
S10.0249 (3)0.0302 (3)0.0378 (4)−0.0031 (3)0.0007 (3)−0.0016 (3)
C10.0258 (13)0.0322 (15)0.0306 (13)−0.0012 (11)0.0004 (10)−0.0005 (11)
C20.0330 (15)0.0418 (17)0.064 (2)−0.0024 (13)−0.0032 (14)−0.0210 (15)
C30.0283 (14)0.052 (2)0.076 (2)0.0050 (14)−0.0011 (14)−0.0259 (17)
C40.0285 (14)0.0411 (16)0.0332 (14)−0.0034 (12)−0.0013 (11)−0.0016 (12)
C50.0329 (14)0.0346 (16)0.066 (2)−0.0045 (13)−0.0012 (13)−0.0125 (14)
C60.0294 (14)0.0326 (16)0.070 (2)−0.0018 (12)0.0036 (13)−0.0113 (14)
C70.0344 (15)0.0415 (17)0.0458 (17)−0.0083 (13)0.0000 (13)0.0011 (13)
C80.0274 (14)0.0446 (18)0.0384 (15)−0.0035 (12)−0.0001 (11)0.0035 (12)
C90.0354 (15)0.0475 (18)0.0477 (17)−0.0032 (14)−0.0036 (13)0.0003 (14)
C100.0398 (17)0.055 (2)0.061 (2)−0.0140 (15)−0.0127 (14)0.0020 (16)
C110.0293 (15)0.076 (3)0.0501 (19)−0.0080 (16)−0.0062 (13)0.0125 (17)
C120.0331 (16)0.069 (2)0.057 (2)0.0102 (16)0.0052 (14)0.0098 (17)
C130.0389 (16)0.0487 (19)0.0517 (18)0.0001 (14)0.0025 (13)0.0026 (14)
Geometric parameters (Å, °) top
Cd1—O52.2684 (19)C1—C21.371 (4)
Cd1—O5i2.2684 (19)C1—C61.380 (4)
Cd1—O72.2826 (18)C2—C31.380 (4)
Cd1—O7i2.2826 (18)C2—H20.9300
Cd1—O6i2.2862 (17)C3—C41.388 (4)
Cd1—O62.2862 (17)C3—H30.9300
N1—C71.278 (4)C4—C51.377 (4)
N1—C41.425 (3)C5—C61.386 (4)
O1—S11.4565 (19)C5—H50.9300
O2—S11.462 (2)C6—H60.9300
O3—S11.4570 (19)C7—C81.450 (4)
O4—C91.349 (4)C7—H70.9300
O4—H40.8200C8—C91.395 (4)
O5—H5A0.8499C8—C131.398 (4)
O5—H5B0.8501C9—C101.400 (4)
O6—H6A0.8500C10—C111.366 (4)
O6—H6B0.8501C10—H100.9300
O7—H7A0.8500C11—C121.381 (5)
O7—H7B0.8500C11—H110.9300
O8—H8A0.8499C12—C131.379 (4)
O8—H8B0.8499C12—H120.9300
S1—C11.768 (3)C13—H130.9300
O5—Cd1—O5i180.0C1—C2—C3120.1 (3)
O5—Cd1—O793.52 (7)C1—C2—H2120.0
O5i—Cd1—O786.48 (7)C3—C2—H2120.0
O5—Cd1—O7i86.48 (7)C2—C3—C4120.3 (3)
O5i—Cd1—O7i93.52 (7)C2—C3—H3119.8
O7—Cd1—O7i180.0C4—C3—H3119.8
O5—Cd1—O6i90.09 (7)C5—C4—C3119.2 (2)
O5i—Cd1—O6i89.91 (7)C5—C4—N1116.2 (2)
O7—Cd1—O6i91.93 (7)C3—C4—N1124.6 (3)
O7i—Cd1—O6i88.07 (7)C4—C5—C6120.5 (3)
O5—Cd1—O689.91 (7)C4—C5—H5119.7
O5i—Cd1—O690.09 (7)C6—C5—H5119.7
O7—Cd1—O688.07 (7)C1—C6—C5119.6 (3)
O7i—Cd1—O691.93 (7)C1—C6—H6120.2
O6i—Cd1—O6180.0C5—C6—H6120.2
C7—N1—C4122.1 (2)N1—C7—C8122.1 (3)
C9—O4—H4109.5N1—C7—H7119.0
Cd1—O5—H5A110.6C8—C7—H7119.0
Cd1—O5—H5B110.5C9—C8—C13118.9 (3)
H5A—O5—H5B108.8C9—C8—C7121.4 (3)
Cd1—O6—H6A109.8C13—C8—C7119.7 (3)
Cd1—O6—H6B110.0O4—C9—C8122.1 (2)
H6A—O6—H6B108.4O4—C9—C10118.4 (3)
Cd1—O7—H7A109.0C8—C9—C10119.5 (3)
Cd1—O7—H7B109.2C11—C10—C9120.1 (3)
H7A—O7—H7B107.9C11—C10—H10120.0
H8A—O8—H8B108.3C9—C10—H10120.0
O1—S1—O3112.68 (12)C10—C11—C12121.4 (3)
O1—S1—O2112.09 (12)C10—C11—H11119.3
O3—S1—O2111.19 (12)C12—C11—H11119.3
O1—S1—C1107.08 (12)C13—C12—C11118.9 (3)
O3—S1—C1106.63 (11)C13—C12—H12120.5
O2—S1—C1106.74 (12)C11—C12—H12120.5
C2—C1—C6120.2 (2)C12—C13—C8121.2 (3)
C2—C1—S1119.5 (2)C12—C13—H13119.4
C6—C1—S1120.2 (2)C8—C13—H13119.4
O1—S1—C1—C2−148.3 (2)S1—C1—C6—C5−179.8 (2)
O3—S1—C1—C2−27.4 (3)C4—C5—C6—C1−0.8 (5)
O2—S1—C1—C291.5 (2)C4—N1—C7—C8−179.3 (3)
O1—S1—C1—C632.8 (3)N1—C7—C8—C9−4.2 (4)
O3—S1—C1—C6153.7 (2)N1—C7—C8—C13176.4 (3)
O2—S1—C1—C6−87.4 (2)C13—C8—C9—O4−180.0 (3)
C6—C1—C2—C3−1.0 (5)C7—C8—C9—O40.6 (4)
S1—C1—C2—C3−179.9 (3)C13—C8—C9—C10−0.7 (4)
C1—C2—C3—C40.2 (5)C7—C8—C9—C10179.9 (3)
C2—C3—C4—C50.3 (5)O4—C9—C10—C11179.7 (3)
C2—C3—C4—N1−179.3 (3)C8—C9—C10—C110.5 (5)
C7—N1—C4—C5−172.3 (3)C9—C10—C11—C120.3 (5)
C7—N1—C4—C37.3 (5)C10—C11—C12—C13−0.8 (5)
C3—C4—C5—C60.0 (5)C11—C12—C13—C80.5 (5)
N1—C4—C5—C6179.6 (3)C9—C8—C13—C120.2 (4)
C2—C1—C6—C51.3 (4)C7—C8—C13—C12179.6 (3)
Symmetry codes: (i) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N10.821.892.611 (3)147
O5—H5A···O1ii0.852.072.909 (3)170
O5—H5B···O8iii0.851.922.750 (3)167
O6—H6A···O8i0.851.932.778 (3)177
O6—H6B···O2iv0.851.972.802 (3)166
O7—H7A···O10.851.952.793 (3)174
O7—H7B···O3ii0.851.912.757 (3)172
O8—H8A···O20.851.902.750 (3)176
O8—H8B···O3ii0.852.002.851 (3)176
Symmetry codes: (ii) x, y−1, z; (iii) −x+1, y−1/2, −z+3/2; (i) −x+1, −y+1, −z+1; (iv) x, −y+3/2, z−1/2.
Table 1
Selected geometric parameters (Å) top
Cd1—O52.2684 (19)Cd1—O62.2862 (17)
Cd1—O72.2826 (18)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N10.821.892.611 (3)147
O5—H5A···O1i0.852.072.909 (3)170
O5—H5B···O8ii0.851.922.750 (3)167
O6—H6A···O8iii0.851.932.778 (3)177
O6—H6B···O2iv0.851.972.802 (3)166
O7—H7A···O10.851.952.793 (3)174
O7—H7B···O3i0.851.912.757 (3)172
O8—H8A···O20.851.902.750 (3)176
O8—H8B···O3i0.852.002.851 (3)176
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+3/2; (iii) −x+1, −y+1, −z+1; (iv) x, −y+3/2, z−1/2.
Acknowledgements top

The authors thank the National Natural Science Foundation of China (grant No. 20671073), the National Natural Science Foundation of Shandong (grant No. Y2007B60), the Science and Technology Foundation of Weifang and Weifang University for research grants.

references
References top

Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Tai, X.-S., Feng, Y.-M. & Zhang, H.-X. (2008). Acta Cryst. E64, m502.