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

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ISSN: 2056-9890

Poly[tetra­aquadi-μ4-oxalato-potassium­ytterbium(III)]

aKey Laboratory of Functional Inorganic Materials Chemistry (MOE), School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China
*Correspondence e-mail: gmli_2000@163.com

(Received 17 October 2011; accepted 1 November 2011; online 9 November 2011)

In the title compound, [KYb(C2O4)2(H2O)4]n, the YbIII ion lies on a site of [\overline{4}] symmetry in a dodeca­hedral environment defined by eight O atoms from four oxalate ligands. The K atom lies on a different [\overline{4}] axis and is coordinated by four O atoms from four oxalate ligands and four water O atoms. The oxalate ligand has an inversion center at the mid-point of the C—C bond. The metal ions are linked by the oxalate ligands into a three-dimensional framework. O—H⋯O hydrogen bonding is present in the crystal structure.

Related literature

For related structures, see: Camara et al. (2003[Camara, M., Daiguebonne, C., Boubekeur, K., Roisnel, T., Gérault, Y., Baux, C., Dret, F. L. & Guillou, O. (2003). Compt. Rend. Chim. 6, 405-415.]); Zhang et al. (2009[Zhang, X.-J., Xing, Y.-H., Wang, C.-G., Han, J., Li, J., Ge, M.-F., Zeng, X.-Q. & Niu, S.-Y. (2009). Inorg. Chim. Acta, 362, 1058-1064.]).

[Scheme 1]

Experimental

Crystal data
  • [KYb(C2O4)2(H2O)4]

  • Mr = 460.24

  • Tetragonal, I 41 /a

  • a = 11.3502 (16) Å

  • c = 8.9142 (18) Å

  • V = 1148.4 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 8.57 mm−1

  • T = 293 K

  • 0.08 × 0.07 × 0.07 mm

Data collection
  • Rigaku R-AXIS RAPID diffractometer

  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.562, Tmax = 0.606

  • 5407 measured reflections

  • 648 independent reflections

  • 585 reflections with I > 2σ(I)

  • Rint = 0.051

Refinement
  • R[F2 > 2σ(F2)] = 0.017

  • wR(F2) = 0.039

  • S = 0.94

  • 648 reflections

  • 41 parameters

  • 3 restraints

  • H-atom parameters constrained

  • Δρmax = 0.55 e Å−3

  • Δρmin = −0.43 e Å−3

Table 1
Selected bond lengths (Å)

K1—O1 2.8402 (19)
K1—O3 2.871 (3)
Yb1—O1 2.3629 (19)
Yb1—O2i 2.304 (2)
Symmetry code: (i) -x, -y+1, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H1⋯O3ii 0.85 2.08 2.899 (3) 163
O3—H2⋯O2iii 0.85 2.06 2.837 (3) 152
Symmetry codes: (ii) [-y+{\script{5\over 4}}, x+{\script{3\over 4}}, z-{\script{1\over 4}}]; (iii) [-y+{\script{3\over 4}}, x+{\script{3\over 4}}, -z+{\script{3\over 4}}].

Data collection: RAPID-AUTO (Rigaku, 1998[Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002[Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.]); 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: DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Lanthanide complexes with spectroscopic and magnetic properties are currently of considerable interest. Oxalate ligand can serve as bridging ligand in high dimensional frameworks (Camara et al., 2003; Zhang et al., 2009). In this paper, we present the synthesis and crystal structure of the title compound.

The title compound was obtained as a byproduct by the decomposition of 1,3,5-triazine-2,4,6-tricarboxylate ligand. In the title compound, [YbK(C2O4)2(H2O)4]n, the eight-coordinated YbIII ion lies on a 4 site symmetry in a distorted dodecahedral geometry defined by eight O atoms from four oxalate ligands. The eight-coordinated K ion is also locate on another site of 4 symmetry in a distorted dodecahedral geometry defined by four O atoms from oxalate ligands and four O atoms from water molecules (Fig. 1, Table 1).

In the crystal, each oxalate ligand links two Yb and two K atoms, forming a three-dimensional framework (Fig. 2). O—H···O hydrogen bonds are present (Table 2).

Related literature top

For related structures, see: Camara et al. (2003); Zhang et al. (2009).

Experimental top

The title compound was obtained as a byproduct caused by the decomposition of 1,3,5-triazine-2,4,6-tricarboxylate ligand. Yb(NO3)3.6H2O (14.01 mg, 0.03 mmol) and potassium salt of 1,3,5-triazine-2,4,6-tricarboxylate (9.8 mg, 0.03 mmol) were dissolved in 15 ml water. After stirring at room temperature for 0.5 h, the solution was allowed to stand for about one week. Colorless block crystals were obtained in 36% yield.

Refinement top

Water H atoms were initially located in a differece Fourier map and were treated as riding atoms, with O—H = 0.85 Å and with Uiso(H) = 1.5Ueq(O).

Structure description top

Lanthanide complexes with spectroscopic and magnetic properties are currently of considerable interest. Oxalate ligand can serve as bridging ligand in high dimensional frameworks (Camara et al., 2003; Zhang et al., 2009). In this paper, we present the synthesis and crystal structure of the title compound.

The title compound was obtained as a byproduct by the decomposition of 1,3,5-triazine-2,4,6-tricarboxylate ligand. In the title compound, [YbK(C2O4)2(H2O)4]n, the eight-coordinated YbIII ion lies on a 4 site symmetry in a distorted dodecahedral geometry defined by eight O atoms from four oxalate ligands. The eight-coordinated K ion is also locate on another site of 4 symmetry in a distorted dodecahedral geometry defined by four O atoms from oxalate ligands and four O atoms from water molecules (Fig. 1, Table 1).

In the crystal, each oxalate ligand links two Yb and two K atoms, forming a three-dimensional framework (Fig. 2). O—H···O hydrogen bonds are present (Table 2).

For related structures, see: Camara et al. (2003); Zhang et al. (2009).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound, showing displacement ellipsoids at the 50% probability level. [Symmetry codes: (i) -x, 1-y, -z; (ii) 1/4-y, 3/4+x, -1/4+z; (iii) -3/4+y, 3/4-x, -1/4-z; (iv) 3/4-y, 3/4+x, -1/4-z; (v) -1/4+y, 3/4-x, -1/4+z; (vi) x, 1/2+y, z; (vii) -x, 3/2-y, z; (viii) 3/4-y, 3/4+x, 3/4-z; (ix) -3/4+y, 3/4-x, 3/4-z.]
[Figure 2] Fig. 2. A packing view along [001], showing the three-dimensional framework.
Poly[tetraaquadi-µ4-oxalato-potassiumytterbium(III)] top
Crystal data top
[KYb(C2O4)2(H2O)4]Dx = 2.662 Mg m3
Mr = 460.24Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/aCell parameters from 4696 reflections
Hall symbol: -I 4adθ = 3.6–27.4°
a = 11.3502 (16) ŵ = 8.57 mm1
c = 8.9142 (18) ÅT = 293 K
V = 1148.4 (3) Å3Block, colorless
Z = 40.08 × 0.07 × 0.07 mm
F(000) = 868
Data collection top
Rigaku R-AXIS RAPID
diffractometer
648 independent reflections
Radiation source: fine-focus sealed tube585 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ω scanθmax = 27.4°, θmin = 3.6°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1414
Tmin = 0.562, Tmax = 0.606k = 1314
5407 measured reflectionsl = 1011
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.039H-atom parameters constrained
S = 0.94 w = 1/[σ2(Fo2) + (0.P)2]
where P = (Fo2 + 2Fc2)/3
648 reflections(Δ/σ)max < 0.001
41 parametersΔρmax = 0.55 e Å3
3 restraintsΔρmin = 0.43 e Å3
Crystal data top
[KYb(C2O4)2(H2O)4]Z = 4
Mr = 460.24Mo Kα radiation
Tetragonal, I41/aµ = 8.57 mm1
a = 11.3502 (16) ÅT = 293 K
c = 8.9142 (18) Å0.08 × 0.07 × 0.07 mm
V = 1148.4 (3) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
648 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
585 reflections with I > 2σ(I)
Tmin = 0.562, Tmax = 0.606Rint = 0.051
5407 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0173 restraints
wR(F2) = 0.039H-atom parameters constrained
S = 0.94Δρmax = 0.55 e Å3
648 reflectionsΔρmin = 0.43 e Å3
41 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.0038 (3)0.5244 (3)0.0802 (3)0.0159 (6)
K10.00000.75000.37500.0296 (4)
O10.0084 (2)0.63272 (19)0.0937 (2)0.0209 (5)
O20.0045 (2)0.44765 (18)0.1836 (2)0.0224 (5)
O30.2057 (3)0.8934 (3)0.3322 (3)0.0509 (8)
H10.23630.91250.24860.076*
H20.25200.84730.37870.076*
Yb10.00000.75000.12500.01065 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0188 (16)0.0154 (15)0.0136 (12)0.0004 (12)0.0010 (11)0.0004 (11)
K10.0345 (6)0.0345 (6)0.0198 (7)0.0000.0000.000
O10.0346 (14)0.0125 (11)0.0156 (9)0.0003 (10)0.0013 (8)0.0017 (8)
O20.0399 (14)0.0122 (11)0.0150 (9)0.0010 (10)0.0009 (9)0.0006 (8)
O30.0374 (17)0.075 (2)0.0402 (13)0.0106 (16)0.0038 (12)0.0195 (15)
Yb10.01004 (12)0.01004 (12)0.01186 (15)0.0000.0000.000
Geometric parameters (Å, º) top
C1—O11.236 (4)Yb1—O12.3629 (19)
C1—O21.269 (4)Yb1—O2i2.304 (2)
C1—C1i1.536 (5)O3—H10.8500
K1—O12.8402 (19)O3—H20.8499
K1—O32.871 (3)
O1—C1—O2127.7 (3)O2i—Yb1—O1v137.29 (7)
O1—C1—C1i116.9 (3)O2ii—Yb1—O1vi137.29 (7)
O2—C1—C1i115.4 (3)O2iii—Yb1—O1vi82.21 (8)
O1—K1—O396.95 (7)O2iv—Yb1—O1vi68.87 (7)
C1—O1—Yb1118.53 (17)O2i—Yb1—O1vi76.19 (8)
C1—O1—K1123.44 (17)O1v—Yb1—O1vi132.92 (6)
Yb1—O1—K1117.59 (8)O2ii—Yb1—O176.19 (8)
C1—O2—Yb1i120.27 (18)O2iii—Yb1—O1137.29 (7)
K1—O3—H1126.4O2iv—Yb1—O182.21 (8)
K1—O3—H295.1O2i—Yb1—O168.87 (7)
H1—O3—H2109.3O1v—Yb1—O168.77 (10)
O2ii—Yb1—O2iii92.95 (2)O1vi—Yb1—O1132.92 (6)
O2ii—Yb1—O2iv153.79 (9)O2ii—Yb1—O1vii68.87 (7)
O2iii—Yb1—O2iv92.95 (2)O2iii—Yb1—O1vii76.19 (8)
O2ii—Yb1—O2i92.95 (2)O2iv—Yb1—O1vii137.29 (7)
O2iii—Yb1—O2i153.79 (9)O2i—Yb1—O1vii82.21 (8)
O2iv—Yb1—O2i92.95 (2)O1v—Yb1—O1vii132.92 (6)
O2ii—Yb1—O1v82.21 (8)O1vi—Yb1—O1vii68.77 (10)
O2iii—Yb1—O1v68.87 (7)O1—Yb1—O1vii132.92 (6)
O2iv—Yb1—O1v76.19 (8)
Symmetry codes: (i) x, y+1, z; (ii) y1/4, x+3/4, z1/4; (iii) x, y+1/2, z; (iv) y+1/4, x+3/4, z1/4; (v) x, y+3/2, z; (vi) y3/4, x+3/4, z1/4; (vii) y+3/4, x+3/4, z1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H1···O3viii0.852.082.899 (3)163
O3—H2···O2ix0.852.062.837 (3)152
Symmetry codes: (viii) y+5/4, x+3/4, z1/4; (ix) y+3/4, x+3/4, z+3/4.

Experimental details

Crystal data
Chemical formula[KYb(C2O4)2(H2O)4]
Mr460.24
Crystal system, space groupTetragonal, I41/a
Temperature (K)293
a, c (Å)11.3502 (16), 8.9142 (18)
V3)1148.4 (3)
Z4
Radiation typeMo Kα
µ (mm1)8.57
Crystal size (mm)0.08 × 0.07 × 0.07
Data collection
DiffractometerRigaku R-AXIS RAPID
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.562, 0.606
No. of measured, independent and
observed [I > 2σ(I)] reflections
5407, 648, 585
Rint0.051
(sin θ/λ)max1)0.648
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.017, 0.039, 0.94
No. of reflections648
No. of parameters41
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.55, 0.43

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999).

Selected bond lengths (Å) top
K1—O12.8402 (19)Yb1—O12.3629 (19)
K1—O32.871 (3)Yb1—O2i2.304 (2)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H1···O3ii0.852.082.899 (3)163
O3—H2···O2iii0.852.062.837 (3)152
Symmetry codes: (ii) y+5/4, x+3/4, z1/4; (iii) y+3/4, x+3/4, z+3/4.
 

Acknowledgements

This work was supported financially by the National Natural Science Foundation of China (Nos. 20872030 and 20972043), Heilongjiang Province (Nos. 2009RFXXG201, GC09A402 and 2010 t d03) and Heilongjiang University.

References

First citationBrandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationCamara, M., Daiguebonne, C., Boubekeur, K., Roisnel, T., Gérault, Y., Baux, C., Dret, F. L. & Guillou, O. (2003). Compt. Rend. Chim. 6, 405–415.  Web of Science CSD CrossRef CAS Google Scholar
First citationHigashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationZhang, X.-J., Xing, Y.-H., Wang, C.-G., Han, J., Li, J., Ge, M.-F., Zeng, X.-Q. & Niu, S.-Y. (2009). Inorg. Chim. Acta, 362, 1058–1064.  Web of Science CSD CrossRef CAS Google Scholar

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ISSN: 2056-9890
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