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

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ISSN: 2056-9890

Poly[[μ4-tartrato-cadmium(II)] 0.167-hydrate]

aDepartment of Chemistry, Jining Normal College, Wulanchabu, Inner Mongolia 012000, People's Republic of China, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 1 May 2009; accepted 5 May 2009; online 14 May 2009)

The title compound, {[Cd(C4H4O6)]·0.167H2O}n, adopts a three-dimensional network structure in which each CdII ion is chelated by two pairs of carboxyl­ate and hydroxyl O atoms from two tartrate anions, and is additionally linked to two O atoms of two carboxyl­ate groups that are not involved in chelation. The asymmetric unit has four independent cadmium atoms, two of which lie on special positions of 2 site symmetry. The tartrate anions all lie on general positions. All hydroxyl groups are engaged in O—H⋯O hydrogen-bonds, one of which is also bifurcated. The non-coordinating water molecule is situated on a site with half-occupation.

Related literature

For the structure of cadmium tartrate trihydrate, see: González-Silgo et al. (1999[González-Silgo, C., González-Platas, J., Ruiz-Pérez, C., López, T. & Torres, M. E. (1999). Acta Cryst. C55, 710-712.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd(C4H4O6)]·0.167H2O

  • Mr = 263.47

  • Orthorhombic, C 2221

  • a = 10.7901 (4) Å

  • b = 11.1995 (5) Å

  • c = 30.588 (1) Å

  • V = 3696.3 (3) Å3

  • Z = 24

  • Mo Kα radiation

  • μ = 3.53 mm−1

  • T = 293 K

  • 0.37 × 0.22 × 0.15 mm

Data collection
  • Bruker APEXII area-detector difractometer diffractometer

  • Absorption correction: multi-scan (SADABS, Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.505, Tmax = 0.780 (expected range = 0.382–0.589)

  • 13041 measured reflections

  • 4095 independent reflections

  • 4073 reflections with I > 2σ(I)

  • Rint = 0.018

Refinement
  • R[F2 > 2σ(F2)] = 0.022

  • wR(F2) = 0.060

  • S = 1.02

  • 4095 reflections

  • 308 parameters

  • 6 restraints

  • H-atom parameters constrained

  • Δρmax = 1.34 e Å−3

  • Δρmin = −1.18 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1733 Friedel pairs

  • Flack parameter: −0.02 (2)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3⋯O18i 0.82 1.96 2.740 (4) 159
O4—H4⋯O10ii 0.82 2.50 3.236 (6) 149
O9—H9⋯O11iii 0.82 2.17 2.797 (5) 134
O9—H9⋯O1w 0.82 2.12 2.68 (2) 125
O10—H10⋯O15ii 0.82 2.15 2.938 (4) 160
O15—H15⋯O1iv 0.82 2.13 2.717 (4) 128
O16—H16⋯O7v 0.82 1.84 2.609 (4) 155
O1W—H1W1⋯O14iii 0.82 2.26 3.034 (19) 157
Symmetry codes: (i) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (ii) [x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]; (iii) [x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]; (iv) [x-{\script{1\over 2}}, y-{\script{1\over 2}}, z]; (v) x-1, y, z.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. 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: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supporting information


Related literature top

For the structure of cadmium tartrate trihydrate, see: González-Silgo et al. (1999).

Experimental top

Cadmium chloride 2.5 hydrate (0.23 g), R,R-tartaric acid (0.48 g), sodium hydroxide (0.39 g), imidazole (0.12 g) and water (0.4 ml) were sealed in a 25-ml Teflon-lined stainless-steel vessel. This was heated at 393 K for 3 d. The colourless crystals found in the cooled vessel were picked out manually.

Refinement top

C-bound H-atoms were placed in calculated positions (C-H = 0.98 Å) and were included in the refinement in the riding model approximation, with U(H) fixed at 1.2U(C). The hydroxy H-atoms were generated geometrically by assuming an sp3 type of hybridization (O-H = 0.82 Å); these were included in the refinement. At this stage, the difference Fourier map had a peak at about 1.5 Å from hydroxyl H9 atom and it was refined as a water molecule of half-site occupancy as the peak was 2.5 Å from the symmetry-related atom. The two water H atoms were placed in chemically sensible positions; only one of these H atom forms a hydrogen bond to an acceptor oxygen atom. The final difference Fourier map had a peak at 2 Å from O1W and hole at 1.2 Å from Cd1.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (Barbour, 2001) of a portion of polymeric cadmium tartrate 1/6 hydrate at the 70% probability level; H atoms are drawn as spheres of arbitrary radius. The disordered water molecule is not shown.
Poly[[µ4-tartrato-cadmium(II)] 0.167-hydrate] top
Crystal data top
[Cd(C4H4O6)]·0.167H2OF(000) = 3016
Mr = 263.47Dx = 2.841 Mg m3
Orthorhombic, C2221Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c 2Cell parameters from 4135 reflections
a = 10.7901 (4) Åθ = 2.3–27.2°
b = 11.1995 (5) ŵ = 3.53 mm1
c = 30.588 (1) ÅT = 293 K
V = 3696.3 (3) Å3Block, colourless
Z = 240.37 × 0.22 × 0.15 mm
Data collection top
Bruker APEXII area-detector difractometer
diffractometer
4095 independent reflections
Radiation source: fine-focus sealed tube4073 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
ϕ and ω scansθmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS, Sheldrick, 1996)
h = 1312
Tmin = 0.505, Tmax = 0.780k = 1414
13041 measured reflectionsl = 3839
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)] = 0.022H-atom parameters constrained
wR(F2) = 0.060 w = 1/[σ2(Fo2) + (0.0411P)2 + 9.1485P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
4095 reflectionsΔρmax = 1.34 e Å3
308 parametersΔρmin = 1.18 e Å3
6 restraintsAbsolute structure: Flack (1983), 1733 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (2)
Crystal data top
[Cd(C4H4O6)]·0.167H2OV = 3696.3 (3) Å3
Mr = 263.47Z = 24
Orthorhombic, C2221Mo Kα radiation
a = 10.7901 (4) ŵ = 3.53 mm1
b = 11.1995 (5) ÅT = 293 K
c = 30.588 (1) Å0.37 × 0.22 × 0.15 mm
Data collection top
Bruker APEXII area-detector difractometer
diffractometer
4095 independent reflections
Absorption correction: multi-scan
(SADABS, Sheldrick, 1996)
4073 reflections with I > 2σ(I)
Tmin = 0.505, Tmax = 0.780Rint = 0.018
13041 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.022H-atom parameters constrained
wR(F2) = 0.060Δρmax = 1.34 e Å3
S = 1.02Δρmin = 1.18 e Å3
4095 reflectionsAbsolute structure: Flack (1983), 1733 Friedel pairs
308 parametersAbsolute structure parameter: 0.02 (2)
6 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd11.00000.70141 (4)0.75000.01735 (8)
Cd20.95531 (3)0.81768 (3)0.578406 (9)0.02161 (7)
Cd30.41091 (3)0.79800 (2)0.601933 (8)0.01865 (7)
Cd40.00000.19902 (4)0.75000.03003 (11)
O11.0079 (3)0.7619 (3)0.67881 (10)0.0233 (6)
O21.1079 (3)0.8548 (3)0.62512 (10)0.0302 (7)
O31.1495 (3)0.8566 (3)0.74078 (9)0.0208 (6)
H31.21300.83670.75360.031*
O41.0508 (4)1.0602 (3)0.69188 (15)0.0482 (11)
H41.03371.09160.66840.072*
O51.3661 (3)1.0768 (3)0.72008 (12)0.0317 (7)
O61.1993 (3)1.1322 (3)0.75792 (11)0.0293 (7)
O70.9280 (3)0.6190 (3)0.58705 (11)0.0295 (7)
O80.8178 (3)0.4562 (3)0.57088 (11)0.0253 (6)
O90.7827 (3)0.7584 (3)0.53809 (12)0.0310 (7)
H90.79440.77710.51250.047*
O100.6037 (3)0.6797 (2)0.59740 (9)0.0195 (5)
H100.66300.72350.60230.029*
O110.4479 (3)0.7476 (3)0.53234 (10)0.0320 (7)
O120.5479 (4)0.6380 (4)0.48342 (11)0.0463 (10)
O130.2972 (3)0.6471 (3)0.62762 (11)0.0276 (7)
O140.3822 (3)0.5056 (3)0.58715 (11)0.0327 (8)
O150.2955 (3)0.3293 (3)0.63798 (9)0.0199 (5)
H150.32050.29180.65920.030*
O160.0760 (3)0.4462 (2)0.61037 (9)0.0213 (6)
H160.04930.51090.60210.032*
O170.0251 (2)0.3105 (3)0.67293 (9)0.0217 (5)
O180.1216 (3)0.3518 (3)0.72046 (10)0.0273 (7)
O1W0.6901 (17)0.9073 (17)0.4779 (6)0.145 (7)0.50
H1W10.73560.91330.45650.218*0.50
H1W20.68780.97110.49100.218*0.50
C11.0921 (4)0.8279 (3)0.66460 (12)0.0178 (7)
C21.1821 (3)0.8874 (3)0.69695 (12)0.0160 (7)
H2C1.26660.85990.69090.019*
C31.1755 (4)1.0224 (4)0.69036 (15)0.0257 (9)
H3C1.21031.04230.66170.031*
C41.2533 (4)1.0834 (3)0.72602 (13)0.0220 (8)
C50.8399 (4)0.5650 (4)0.56782 (13)0.0168 (7)
C60.7517 (4)0.6364 (3)0.53935 (12)0.0174 (7)
H6C0.75580.60470.50950.021*
C70.6197 (3)0.6243 (3)0.55551 (12)0.0160 (7)
H7C0.60160.53900.55880.019*
C80.5297 (4)0.6755 (4)0.52122 (13)0.0234 (8)
C90.3210 (4)0.5408 (4)0.61868 (13)0.0191 (8)
C100.2672 (3)0.4479 (3)0.65126 (12)0.0155 (7)
H10C0.30200.46220.68040.019*
C110.1258 (4)0.4612 (3)0.65322 (13)0.0168 (7)
H11C0.10540.54150.66380.020*
C120.0704 (4)0.3690 (3)0.68453 (12)0.0175 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01892 (17)0.01774 (17)0.01540 (16)0.0000.00203 (12)0.000
Cd20.02609 (15)0.01939 (14)0.01935 (13)0.00727 (12)0.00123 (10)0.00092 (10)
Cd30.02465 (14)0.01520 (12)0.01611 (12)0.00012 (11)0.00171 (9)0.00103 (11)
Cd40.0214 (2)0.0270 (2)0.0417 (2)0.0000.00595 (16)0.000
O10.0222 (14)0.0262 (14)0.0216 (13)0.0078 (12)0.0076 (11)0.0021 (11)
O20.0414 (19)0.0331 (17)0.0163 (13)0.0116 (15)0.0006 (12)0.0019 (12)
O30.0218 (14)0.0251 (14)0.0156 (13)0.0048 (11)0.0076 (10)0.0027 (11)
O40.043 (2)0.0263 (16)0.075 (3)0.0144 (16)0.039 (2)0.0157 (17)
O50.0260 (16)0.0282 (16)0.0409 (19)0.0114 (13)0.0012 (14)0.0064 (15)
O60.0278 (16)0.0292 (15)0.0308 (17)0.0002 (13)0.0033 (12)0.0115 (13)
O70.0274 (17)0.0166 (12)0.0447 (19)0.0003 (12)0.0195 (14)0.0032 (13)
O80.0229 (14)0.0149 (13)0.0383 (18)0.0001 (12)0.0082 (12)0.0011 (12)
O90.0288 (18)0.0210 (14)0.0432 (19)0.0068 (12)0.0084 (14)0.0166 (13)
O100.0226 (13)0.0196 (12)0.0162 (11)0.0005 (11)0.0020 (10)0.0045 (11)
O110.0330 (17)0.0416 (18)0.0213 (14)0.0254 (15)0.0083 (13)0.0069 (13)
O120.047 (2)0.069 (3)0.0224 (15)0.038 (2)0.0175 (15)0.0207 (16)
O130.0279 (16)0.0182 (14)0.0366 (17)0.0058 (12)0.0073 (13)0.0002 (13)
O140.042 (2)0.0219 (14)0.0345 (17)0.0030 (14)0.0219 (15)0.0005 (13)
O150.0222 (14)0.0177 (13)0.0200 (13)0.0019 (11)0.0014 (10)0.0040 (11)
O160.0235 (15)0.0197 (13)0.0206 (13)0.0014 (11)0.0066 (11)0.0055 (10)
O170.0200 (14)0.0240 (14)0.0211 (12)0.0063 (12)0.0015 (10)0.0025 (12)
O180.0236 (16)0.0360 (17)0.0223 (14)0.0060 (13)0.0009 (11)0.0037 (13)
O1W0.130 (10)0.170 (10)0.136 (10)0.007 (8)0.010 (8)0.065 (8)
C10.0201 (17)0.0161 (16)0.0172 (16)0.0026 (15)0.0031 (13)0.0002 (14)
C20.0157 (16)0.0166 (17)0.0156 (17)0.0012 (14)0.0003 (13)0.0013 (14)
C30.036 (2)0.0153 (18)0.026 (2)0.0032 (16)0.0151 (17)0.0011 (16)
C40.028 (2)0.0134 (16)0.0244 (19)0.0045 (16)0.0079 (16)0.0042 (15)
C50.0158 (18)0.0179 (17)0.0167 (17)0.0023 (14)0.0004 (12)0.0023 (14)
C60.0195 (18)0.0172 (17)0.0156 (16)0.0016 (15)0.0008 (13)0.0016 (13)
C70.0149 (18)0.0166 (16)0.0165 (17)0.0009 (14)0.0041 (13)0.0034 (14)
C80.023 (2)0.027 (2)0.0199 (17)0.0100 (17)0.0087 (14)0.0056 (16)
C90.0132 (17)0.0214 (19)0.0228 (19)0.0043 (15)0.0052 (14)0.0020 (16)
C100.0140 (17)0.0171 (16)0.0154 (16)0.0027 (14)0.0022 (13)0.0002 (13)
C110.0162 (18)0.0117 (15)0.0224 (19)0.0016 (14)0.0006 (13)0.0008 (14)
C120.0182 (19)0.0187 (16)0.0157 (16)0.0001 (14)0.0046 (13)0.0041 (14)
Geometric parameters (Å, º) top
Cd1—O5i2.207 (3)O8—Cd3xi2.247 (3)
Cd1—O5ii2.207 (3)O9—C61.408 (5)
Cd1—O12.282 (3)O9—H90.82
Cd1—O1iii2.282 (3)O10—C71.434 (4)
Cd1—O32.388 (3)O10—H100.82
Cd1—O3iii2.388 (3)O11—C81.245 (5)
Cd2—O12iv2.196 (3)O12—C81.245 (5)
Cd2—O22.220 (3)O12—Cd2xii2.196 (3)
Cd2—O72.260 (3)O13—C91.248 (5)
Cd2—O14v2.264 (3)O14—C91.233 (5)
Cd2—O92.330 (3)O14—Cd2i2.264 (3)
Cd2—O15v2.512 (3)O15—C101.422 (5)
Cd3—O132.232 (3)O15—Cd2i2.512 (3)
Cd3—O112.238 (3)O15—H150.82
Cd3—O8vi2.247 (3)O16—C111.426 (4)
Cd3—O17v2.283 (3)O16—Cd3i2.449 (3)
Cd3—O16v2.449 (3)O16—H160.82
Cd3—O102.470 (3)O17—C121.272 (5)
Cd4—O6vii2.290 (3)O17—Cd3i2.283 (3)
Cd4—O6viii2.290 (3)O18—C121.245 (5)
Cd4—O182.338 (3)O1W—H1W10.82
Cd4—O18ix2.338 (3)O1W—H1W20.82
Cd4—O4viii2.424 (4)C1—C21.538 (5)
Cd4—O4vii2.424 (4)C2—C31.526 (5)
O1—C11.250 (5)C2—H2C0.98
O2—C11.257 (5)C3—C41.536 (5)
O3—C21.428 (5)C3—H3C0.98
O3—H30.82C5—C61.518 (5)
O4—C31.412 (6)C6—C71.514 (5)
O4—Cd4x2.424 (4)C6—H6C0.98
O4—H40.82C7—C81.540 (5)
O5—C41.233 (6)C7—H7C0.98
O5—Cd1v2.207 (3)C9—C101.554 (5)
O6—C41.261 (5)C10—C111.534 (5)
O6—Cd4x2.290 (3)C10—H10C0.98
O7—C51.271 (5)C11—C121.530 (5)
O8—C51.246 (5)C11—H11C0.98
O5i—Cd1—O5ii101.55 (19)C6—O9—H9108.1
O5i—Cd1—O179.43 (12)Cd2—O9—H9108.1
O5ii—Cd1—O1123.99 (12)C7—O10—Cd3112.6 (2)
O5i—Cd1—O1iii123.99 (12)C7—O10—H10109.1
O5ii—Cd1—O1iii79.43 (12)Cd3—O10—H10109.1
O1—Cd1—O1iii145.46 (15)C8—O11—Cd3123.4 (3)
O5i—Cd1—O3148.58 (11)C8—O12—Cd2xii130.7 (3)
O5ii—Cd1—O393.84 (12)C9—O13—Cd3122.1 (3)
O1—Cd1—O369.28 (10)C9—O14—Cd2i125.2 (3)
O1iii—Cd1—O385.51 (10)C10—O15—Cd2i113.8 (2)
O5i—Cd1—O3iii93.84 (12)C10—O15—H15108.8
O5ii—Cd1—O3iii148.58 (11)Cd2i—O15—H15108.8
O1—Cd1—O3iii85.51 (10)C11—O16—Cd3i116.8 (2)
O1iii—Cd1—O3iii69.28 (9)C11—O16—H16108.1
O3—Cd1—O3iii86.61 (15)Cd3i—O16—H16108.1
O12iv—Cd2—O2100.04 (13)C12—O17—Cd3i122.8 (2)
O12iv—Cd2—O7112.50 (14)C12—O18—Cd4101.8 (3)
O2—Cd2—O7101.90 (11)H1W1—O1W—H1W2109.7
O12iv—Cd2—O14v92.86 (14)O1—C1—O2125.1 (4)
O2—Cd2—O14v90.47 (13)O1—C1—C2119.5 (3)
O7—Cd2—O14v148.89 (13)O2—C1—C2115.4 (3)
O12iv—Cd2—O988.41 (13)O3—C2—C3110.6 (3)
O2—Cd2—O9170.78 (11)O3—C2—C1110.1 (3)
O7—Cd2—O971.16 (10)C3—C2—C1108.3 (3)
O14v—Cd2—O992.81 (13)O3—C2—H2C109.3
O12iv—Cd2—O15v157.71 (14)C3—C2—H2C109.3
O2—Cd2—O15v91.88 (10)C1—C2—H2C109.3
O7—Cd2—O15v82.91 (12)O4—C3—C2109.7 (4)
O14v—Cd2—O15v68.10 (10)O4—C3—C4111.3 (4)
O9—Cd2—O15v81.37 (11)C2—C3—C4108.8 (3)
O13—Cd3—O11104.01 (13)O4—C3—H3C109.0
O13—Cd3—O8vi119.99 (12)C2—C3—H3C109.0
O11—Cd3—O8vi82.89 (12)C4—C3—H3C109.0
O13—Cd3—O17v82.97 (11)O5—C4—O6126.6 (4)
O11—Cd3—O17v150.04 (10)O5—C4—C3114.1 (4)
O8vi—Cd3—O17v119.27 (11)O6—C4—C3119.4 (4)
O13—Cd3—O16v151.21 (11)O8—C5—O7125.0 (4)
O11—Cd3—O16v98.13 (12)O8—C5—C6116.0 (3)
O8vi—Cd3—O16v80.54 (10)O7—C5—C6119.0 (4)
O17v—Cd3—O16v68.79 (10)O9—C6—C7108.6 (3)
O13—Cd3—O1094.40 (11)O9—C6—C5112.2 (3)
O11—Cd3—O1070.20 (10)C7—C6—C5110.8 (3)
O8vi—Cd3—O10140.87 (11)O9—C6—H6C108.4
O17v—Cd3—O1080.31 (9)C7—C6—H6C108.4
O16v—Cd3—O1075.93 (9)C5—C6—H6C108.4
O6vii—Cd4—O6viii141.86 (17)O10—C7—C6111.5 (3)
O6vii—Cd4—O18136.50 (11)O10—C7—C8111.8 (3)
O6viii—Cd4—O1875.69 (12)C6—C7—C8109.7 (3)
O6vii—Cd4—O18ix75.69 (12)O10—C7—H7C107.9
O6viii—Cd4—O18ix136.50 (11)C6—C7—H7C107.9
O18—Cd4—O18ix85.92 (17)C8—C7—H7C107.9
O6vii—Cd4—O4viii85.73 (13)O11—C8—O12125.8 (4)
O6viii—Cd4—O4viii69.85 (11)O11—C8—C7120.2 (3)
O18—Cd4—O4viii93.37 (14)O12—C8—C7114.1 (4)
O18ix—Cd4—O4viii151.60 (11)O14—C9—O13125.9 (4)
O6vii—Cd4—O4vii69.85 (11)O14—C9—C10119.2 (4)
O6viii—Cd4—O4vii85.73 (13)O13—C9—C10114.9 (4)
O18—Cd4—O4vii151.60 (11)O15—C10—C11108.4 (3)
O18ix—Cd4—O4vii93.37 (14)O15—C10—C9111.2 (3)
O4viii—Cd4—O4vii100.2 (2)C11—C10—C9109.4 (3)
C1—O1—Cd1122.3 (2)O15—C10—H10C109.3
C1—O2—Cd2118.2 (3)C11—C10—H10C109.3
C2—O3—Cd1116.9 (2)C9—C10—H10C109.3
C2—O3—H3108.1O16—C11—C12110.4 (3)
Cd1—O3—H3108.1O16—C11—C10109.1 (3)
C3—O4—Cd4x115.6 (3)C12—C11—C10110.3 (3)
C3—O4—H4108.4O16—C11—H11C109.0
Cd4x—O4—H4108.4C12—C11—H11C109.0
C4—O5—Cd1v123.2 (3)C10—C11—H11C109.0
C4—O6—Cd4x119.6 (3)O18—C12—O17121.7 (4)
C5—O7—Cd2120.8 (3)O18—C12—C11118.9 (3)
C5—O8—Cd3xi135.9 (3)O17—C12—C11119.3 (3)
C6—O9—Cd2116.9 (2)
O5i—Cd1—O1—C1165.4 (3)C1—C2—C3—C4173.4 (3)
O5ii—Cd1—O1—C168.6 (3)Cd1v—O5—C4—O623.0 (6)
O1iii—Cd1—O1—C157.5 (3)Cd1v—O5—C4—C3158.2 (3)
O3—Cd1—O1—C111.7 (3)Cd4x—O6—C4—O5155.8 (3)
O3iii—Cd1—O1—C199.8 (3)Cd4x—O6—C4—C325.5 (5)
O12iv—Cd2—O2—C1173.2 (3)O4—C3—C4—O5163.6 (4)
O7—Cd2—O2—C157.5 (3)C2—C3—C4—O575.5 (5)
O14v—Cd2—O2—C193.8 (3)O4—C3—C4—O617.6 (5)
O15v—Cd2—O2—C125.7 (3)C2—C3—C4—O6103.4 (4)
O5i—Cd1—O3—C26.4 (4)Cd3xi—O8—C5—O76.2 (7)
O5ii—Cd1—O3—C2113.2 (3)Cd3xi—O8—C5—C6175.0 (3)
O1—Cd1—O3—C211.8 (2)Cd2—O7—C5—O8179.7 (3)
O1iii—Cd1—O3—C2167.7 (3)Cd2—O7—C5—C60.9 (5)
O3iii—Cd1—O3—C298.3 (3)Cd2—O9—C6—C7123.0 (3)
O12iv—Cd2—O7—C579.3 (4)Cd2—O9—C6—C50.1 (4)
O2—Cd2—O7—C5174.4 (3)O8—C5—C6—O9179.4 (4)
O14v—Cd2—O7—C563.0 (4)O7—C5—C6—O90.5 (5)
O9—Cd2—O7—C50.7 (3)O8—C5—C6—C757.8 (5)
O15v—Cd2—O7—C583.9 (3)O7—C5—C6—C7121.1 (4)
O12iv—Cd2—O9—C6114.1 (3)Cd3—O10—C7—C6136.4 (2)
O7—Cd2—O9—C60.4 (3)Cd3—O10—C7—C813.1 (4)
O14v—Cd2—O9—C6153.1 (3)O9—C6—C7—O1056.7 (4)
O15v—Cd2—O9—C685.8 (3)C5—C6—C7—O1067.0 (4)
O13—Cd3—O10—C791.5 (2)O9—C6—C7—C867.8 (4)
O11—Cd3—O10—C711.8 (2)C5—C6—C7—C8168.5 (3)
O8vi—Cd3—O10—C761.3 (3)Cd3—O11—C8—O12174.4 (4)
O17v—Cd3—O10—C7173.6 (2)Cd3—O11—C8—C75.6 (6)
O16v—Cd3—O10—C7116.0 (2)Cd2xii—O12—C8—O112.3 (9)
O13—Cd3—O11—C880.2 (4)Cd2xii—O12—C8—C7177.7 (3)
O8vi—Cd3—O11—C8160.6 (4)O10—C7—C8—O116.3 (6)
O17v—Cd3—O11—C820.2 (5)C6—C7—C8—O11130.6 (4)
O16v—Cd3—O11—C881.3 (4)O10—C7—C8—O12173.7 (4)
O10—Cd3—O11—C89.5 (4)C6—C7—C8—O1249.5 (5)
O11—Cd3—O13—C941.6 (4)Cd2i—O14—C9—O13167.6 (3)
O8vi—Cd3—O13—C9131.4 (3)Cd2i—O14—C9—C1012.1 (5)
O17v—Cd3—O13—C9108.7 (3)Cd3—O13—C9—O1421.2 (6)
O16v—Cd3—O13—C997.5 (4)Cd3—O13—C9—C10158.5 (2)
O10—Cd3—O13—C929.0 (3)Cd2i—O15—C10—C11132.7 (2)
O6vii—Cd4—O18—C1225.4 (3)Cd2i—O15—C10—C912.4 (3)
O6viii—Cd4—O18—C12130.2 (3)O14—C9—C10—O151.9 (5)
O18ix—Cd4—O18—C1289.6 (3)O13—C9—C10—O15178.3 (3)
O4viii—Cd4—O18—C1261.9 (3)O14—C9—C10—C11121.7 (4)
O4vii—Cd4—O18—C12179.1 (3)O13—C9—C10—C1158.6 (4)
Cd1—O1—C1—O2172.9 (3)Cd3i—O16—C11—C125.5 (4)
Cd1—O1—C1—C210.0 (5)Cd3i—O16—C11—C10126.9 (3)
Cd2—O2—C1—O114.3 (6)O15—C10—C11—O1663.9 (4)
Cd2—O2—C1—C2162.9 (2)C9—C10—C11—O1657.6 (4)
Cd1—O3—C2—C3130.8 (3)O15—C10—C11—C1257.6 (4)
Cd1—O3—C2—C111.1 (4)C9—C10—C11—C12179.0 (3)
O1—C1—C2—O31.4 (5)Cd4—O18—C12—O171.1 (4)
O2—C1—C2—O3176.0 (3)Cd4—O18—C12—C11177.6 (3)
O1—C1—C2—C3122.5 (4)Cd3i—O17—C12—O18161.8 (3)
O2—C1—C2—C354.9 (5)Cd3i—O17—C12—C1116.8 (5)
Cd4x—O4—C3—C2118.3 (3)O16—C11—C12—O18164.7 (3)
Cd4x—O4—C3—C42.1 (5)C10—C11—C12—O1844.1 (5)
O3—C2—C3—O469.3 (4)O16—C11—C12—O1714.0 (5)
C1—C2—C3—O451.5 (5)C10—C11—C12—O17134.7 (4)
O3—C2—C3—C452.7 (5)
Symmetry codes: (i) x1/2, y1/2, z; (ii) x+5/2, y1/2, z+3/2; (iii) x+2, y, z+3/2; (iv) x+1/2, y+3/2, z+1; (v) x+1/2, y+1/2, z; (vi) x1/2, y+1/2, z; (vii) x+1, y1, z+3/2; (viii) x1, y1, z; (ix) x, y, z+3/2; (x) x+1, y+1, z; (xi) x+1/2, y1/2, z; (xii) x1/2, y+3/2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O18xiii0.821.962.740 (4)159
O4—H4···O10v0.822.503.236 (6)149
O9—H9···O11iv0.822.172.797 (5)134
O9—H9···O1w0.822.122.68 (2)125
O10—H10···O15v0.822.152.938 (4)160
O15—H15···O1i0.822.132.717 (4)128
O16—H16···O7xiv0.821.842.609 (4)155
O1W—H1W1···O14iv0.822.263.034 (19)157
Symmetry codes: (i) x1/2, y1/2, z; (iv) x+1/2, y+3/2, z+1; (v) x+1/2, y+1/2, z; (xiii) x+3/2, y+1/2, z+3/2; (xiv) x1, y, z.

Experimental details

Crystal data
Chemical formula[Cd(C4H4O6)]·0.167H2O
Mr263.47
Crystal system, space groupOrthorhombic, C2221
Temperature (K)293
a, b, c (Å)10.7901 (4), 11.1995 (5), 30.588 (1)
V3)3696.3 (3)
Z24
Radiation typeMo Kα
µ (mm1)3.53
Crystal size (mm)0.37 × 0.22 × 0.15
Data collection
DiffractometerBruker APEXII area-detector difractometer
diffractometer
Absorption correctionMulti-scan
(SADABS, Sheldrick, 1996)
Tmin, Tmax0.505, 0.780
No. of measured, independent and
observed [I > 2σ(I)] reflections
13041, 4095, 4073
Rint0.018
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.060, 1.02
No. of reflections4095
No. of parameters308
No. of restraints6
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.34, 1.18
Absolute structureFlack (1983), 1733 Friedel pairs
Absolute structure parameter0.02 (2)

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O18i0.821.962.740 (4)159
O4—H4···O10ii0.822.503.236 (6)149
O9—H9···O11iii0.822.172.797 (5)134
O9—H9···O1w0.822.122.68 (2)125
O10—H10···O15ii0.822.152.938 (4)160
O15—H15···O1iv0.822.132.717 (4)128
O16—H16···O7v0.821.842.609 (4)155
O1W—H1W1···O14iii0.822.263.034 (19)157
Symmetry codes: (i) x+3/2, y+1/2, z+3/2; (ii) x+1/2, y+1/2, z; (iii) x+1/2, y+3/2, z+1; (iv) x1/2, y1/2, z; (v) x1, y, z.
 

Acknowledgements

We acknowledge support from the Scientific Research Projects of Higher Education of Inner Mongolia (NJzy08217) and the University of Malaya.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS
First citationBruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals
First citationGonzález-Silgo, C., González-Platas, J., Ruiz-Pérez, C., López, T. & Torres, M. E. (1999). Acta Cryst. C55, 710–712.  Web of Science CSD CrossRef IUCr Journals
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationWestrip, S. P. (2009). publCIF. In preparation.

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