Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Previous article
Next article
Previous article
Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Next article

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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 9| September 2010| Page m1161
https://doi.org/10.1107/S1600536810033052

Poly[di­aqua-μ2-oxalato-di-μ4-terephthalato-diytterbium(III)]

Chun-Xiang Wanga and Zhi-Feng Lia*

aSchool of Materials & Chemical Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, People's Republic of China
*Correspondence e-mail: jxlzfeng@yahoo.com.cn

(Received 25 July 2010; accepted 17 August 2010; online 25 August 2010)

The crystal structure of the title complex, [Yb2(C8H4O4)2(C2O4)(H2O)2]n, features an extended three-dimensional framework made up of Yb3+ ions coordinated by terephthalate ligands, oxalate ligands and water mol­ecules. The Yb3+ ion has a distorted square-anti­prismatic coordination formed by one aqua ligand, two O atoms from an oxalate ligand and five O atoms belonging to four terephthalate anions. Two symmetry-independent terephthalate anions, as well as the oxalate anion, occupy special positions on inversion centers. The water molecule participates in O—H⋯O hydrogen bonding with both terephthalate anions.

Related literature

For isotypic structures, derivatives of Lu and Dy, see: Li & Wang (2009[Li, Z.-F. & Wang, C.-X. (2009). Acta Cryst. E65, m1157.]) and Li et al. (2009[Li, Z.-F., Cheng, Q., Chen, J.-Z. & Chen, Y. (2009). Z. Kristallogr. New Cryst. Struct. 224, 483-484.]), respectively.

[Scheme 1]

Experimental

Crystal data

  • [Yb2(C8H4O4)2(C2O4)(H2O)2]

  • Mr = 798.36

  • Triclinic, [P \overline 1]

  • a = 7.034 (2) Å

  • b = 7.583 (2) Å

  • c = 10.213 (3) Å

  • α = 75.372 (4)°

  • β = 70.851 (4)°

  • γ = 88.126 (4)°

  • V = 497.2 (2) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 9.43 mm−1

  • T = 295 K

  • 0.24 × 0.15 × 0.05 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003[Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.]) Tmin = 0.211, Tmax = 0.629

  • 2630 measured reflections

  • 1882 independent reflections

  • 1785 reflections with I > 2σ(I)

  • Rint = 0.025
Refinement

  • R[F2 > 2σ(F2)] = 0.046

  • wR(F2) = 0.120

  • S = 1.06

  • 1882 reflections

  • 154 parameters

  • H-atom parameters constrained

  • Δρmax = 4.45 e Å−3

  • Δρmin = −4.21 e Å−3

Table 1
Selected bond lengths (Å)

Yb—O1 2.790 (6)
Yb—O1i 2.315 (6)
Yb—O2 2.314 (6)
Yb—O3 2.264 (6)
Yb—O4ii 2.209 (6)
Yb—O5 2.310 (6)
Yb—O6iii 2.321 (6)
Yb—O7 2.293 (5)
Symmetry codes: (i) -x+1, -y, -z+2; (ii) -x+1, -y+1, -z+2; (iii) -x, -y+1, -z+2.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O7—H7A⋯O3i 0.85 1.92 2.751 (6) 167
O7—H7B⋯O2iv 0.85 1.91 2.754 (6) 178
Symmetry codes: (i) -x+1, -y, -z+2; (iv) -x, -y, -z+2.

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810033052/ya2126sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810033052/ya2126Isup2.hkl

checkCIF report


Comment top

The title compound is isostructural with its Lu and Dy analogues (Li & Wang, 2009; Li et al., 2009). As illustrated in Fig. 1, the Yb atoms is coordinated by two oxalate O atoms and five O atoms of four terephthalate anions; an aqua ligand completes a distorted square antiprismatic geometry. The Yb-O distances are in the range of 2.208 (6)–2.790 (6) Å, with an average Yb-O bond of 2.352 Å; these parameters are similar to M-O bonds found in the above mentioned previously reported isostructural complexes.

In the title complex, both symmetry independent terephthalate (tp) anions occupy special positions on the inversion centers; nevertheless they exhibit different modes of coordination of Yb atoms. The tp1 anion (O1 to O2, C1 to C4) functions as chelating-bridging tridentate ligand: two carboxylate oxygen atoms (O1 and O2) chelate one Yb atom; the O1 atom is additionally bonded to another Yb atom; the Yb···Yb separation is 4.232 (1) Å. Two edge-sharing [YbO8] polyhedra are bridged by the bidentate tp2 (O3 to O4, C5 to C8) ligands thus generating chains along the [010] direction. The chains are further linked by the tp1 and tp2 ligands into three-dimensional framework. The oxalate anion is also located on the inversion center and acts as a tetradentate ligand connecting the edge-sharing [YbO8] polyhedra along the [100] direction thus even further stabilizing the three-dimensional framework. The aqua ligand provides H-bond donors which participate in H-bonds with terephthalate oxygen atoms O2 and O3.

Related literature top

For isostructural/isotypic structures, derivatives of Lu and Dy, see: Li & Wang (2009) and Li et al. (2009), respectively.

Experimental top

A mixture of YbCl3.6H2O (1.00 mmol, 0.39 g), oxalic acid (0.50 mmol, 0.05 g), terephthalic acid (0.50 mmol, 0.09 g), NaOH (2.00 mmol, 0.08 g) and H2O (10.0 ml) was heated in a 23 ml stainless steel reactor with a Teflon liner at 453 K for 72 h. A small amount of colorless plate-like crystals were filtered and washed with water and acetone.

Refinement top

H atoms attached to C atoms were included at calculated positions and treated as riding atoms [C–H = 0.93 Å and Uiso(H) = 1.2Ueq(C)]. Water H atoms were located in difference Fourier maps placed at the idealized positions with O-H distance of 0.85 Å and included in the final refinement as fixed contribution with Uiso(H) = 1.5Ueq(O). The highest density peak and deepest hole are located at 0.87 Å and 1.09 Å from the Yb atom respectively.

Structure description top

The title compound is isostructural with its Lu and Dy analogues (Li & Wang, 2009; Li et al., 2009). As illustrated in Fig. 1, the Yb atoms is coordinated by two oxalate O atoms and five O atoms of four terephthalate anions; an aqua ligand completes a distorted square antiprismatic geometry. The Yb-O distances are in the range of 2.208 (6)–2.790 (6) Å, with an average Yb-O bond of 2.352 Å; these parameters are similar to M-O bonds found in the above mentioned previously reported isostructural complexes.

In the title complex, both symmetry independent terephthalate (tp) anions occupy special positions on the inversion centers; nevertheless they exhibit different modes of coordination of Yb atoms. The tp1 anion (O1 to O2, C1 to C4) functions as chelating-bridging tridentate ligand: two carboxylate oxygen atoms (O1 and O2) chelate one Yb atom; the O1 atom is additionally bonded to another Yb atom; the Yb···Yb separation is 4.232 (1) Å. Two edge-sharing [YbO8] polyhedra are bridged by the bidentate tp2 (O3 to O4, C5 to C8) ligands thus generating chains along the [010] direction. The chains are further linked by the tp1 and tp2 ligands into three-dimensional framework. The oxalate anion is also located on the inversion center and acts as a tetradentate ligand connecting the edge-sharing [YbO8] polyhedra along the [100] direction thus even further stabilizing the three-dimensional framework. The aqua ligand provides H-bond donors which participate in H-bonds with terephthalate oxygen atoms O2 and O3.

For isostructural/isotypic structures, derivatives of Lu and Dy, see: Li & Wang (2009) and Li et al. (2009), respectively.

Computing details top

Data collection: APEXII (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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 fragment of the structure of the title compound, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small circles of arbitrary radii. Symmetry codes: (i) 1 -x, -y, 2 - z; (ii) 1 - x, 1 - y, 2 - z; (iii) -x, 1 - y, 2 - z; (iv) 1 - x, -y, 1 - z; (v) 2 - x, 1 - y, 1 - z.
Poly[diaqua-µ2-oxalato-di-µ4-terephthalato-diytterbium(III)] top
Crystal data top
[Yb2(C8H4O4)2(C2O4)(H2O)2]Z = 1
Mr = 798.36F(000) = 372
Triclinic, P1Dx = 2.666 Mg m−3
Hall symbol: -p 1Mo Kα radiation, λ = 0.71073 Å
a = 7.034 (2) ÅCell parameters from 196 reflections
b = 7.583 (2) Åθ = 2.1–27.3°
c = 10.213 (3) ŵ = 9.43 mm−1
α = 75.372 (4)°T = 295 K
β = 70.851 (4)°Plate, colorless
γ = 88.126 (4)°0.24 × 0.15 × 0.05 mm
V = 497.2 (2) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		1882 independent reflections
Radiation source: fine-focus sealed tube1785 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
φ and ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		h = −8→8
Tmin = 0.211, Tmax = 0.629k = −8→9
2630 measured reflectionsl = −7→12
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0995P)2]
where P = (Fo2 + 2Fc2)/3
1882 reflections(Δ/σ)max < 0.001
154 parametersΔρmax = 4.45 e Å−3
0 restraintsΔρmin = −4.21 e Å−3
Crystal data top
[Yb2(C8H4O4)2(C2O4)(H2O)2]γ = 88.126 (4)°
Mr = 798.36V = 497.2 (2) Å3
Triclinic, P1Z = 1
a = 7.034 (2) ÅMo Kα radiation
b = 7.583 (2) ŵ = 9.43 mm−1
c = 10.213 (3) ÅT = 295 K
α = 75.372 (4)°0.24 × 0.15 × 0.05 mm
β = 70.851 (4)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		1882 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		1785 reflections with I > 2σ(I)
Tmin = 0.211, Tmax = 0.629Rint = 0.025
2630 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.120H-atom parameters constrained
S = 1.06Δρmax = 4.45 e Å−3
1882 reflectionsΔρmin = −4.21 e Å−3
154 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
Yb0.31071 (4)0.22186 (3)1.01498 (3)0.01504 (19)
C10.3854 (12)0.0294 (11)0.7912 (9)0.0203 (16)
C20.4409 (12)0.0093 (11)0.6438 (9)0.0202 (16)
C30.3229 (16)0.0805 (15)0.5592 (11)0.033 (2)
H30.20480.13550.59760.039*
C40.6198 (14)−0.0700 (13)0.5823 (10)0.030 (2)
H40.7015−0.11630.63700.036*
C50.7144 (12)0.4806 (10)0.7821 (9)0.0189 (16)
C60.8607 (13)0.4930 (11)0.6352 (10)0.0211 (18)
C70.8292 (13)0.3852 (12)0.5521 (10)0.0282 (19)
H70.71490.30660.58750.034*
C81.0353 (13)0.6070 (12)0.5820 (10)0.0275 (19)
H81.06020.67800.63740.033*
C9−0.0833 (11)0.4309 (10)1.0574 (9)0.0194 (16)
O10.4818 (8)−0.0459 (8)0.8752 (6)0.0228 (12)
O20.2462 (9)0.1353 (8)0.8314 (6)0.0228 (12)
O30.6140 (8)0.3311 (8)0.8501 (6)0.0224 (12)
O40.6994 (9)0.6187 (8)0.8296 (7)0.0248 (13)
O5−0.0295 (9)0.2697 (8)1.0944 (7)0.0246 (12)
O6−0.2511 (8)0.4911 (8)1.1074 (7)0.0254 (13)
O70.1351 (8)−0.0452 (7)1.1590 (7)0.0242 (13)
H7B0.0166−0.07401.16440.036*
H7A0.1979−0.14291.16720.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb0.0191 (3)0.0156 (3)0.0129 (3)0.00119 (15)−0.00688 (17)−0.00586 (17)
C10.024 (4)0.017 (4)0.023 (5)−0.008 (3)−0.009 (3)−0.007 (3)
C20.026 (4)0.020 (4)0.016 (4)0.003 (3)−0.008 (3)−0.004 (3)
C30.036 (5)0.043 (6)0.023 (5)0.015 (4)−0.014 (4)−0.012 (4)
C40.032 (4)0.039 (5)0.025 (5)0.015 (4)−0.015 (4)−0.015 (4)
C50.026 (4)0.017 (4)0.013 (4)0.001 (3)−0.007 (3)−0.002 (3)
C60.026 (4)0.017 (4)0.020 (5)−0.001 (3)−0.006 (4)−0.007 (3)
C70.030 (4)0.028 (4)0.024 (5)−0.015 (3)0.000 (4)−0.010 (4)
C80.034 (4)0.024 (4)0.028 (5)−0.014 (3)−0.007 (4)−0.014 (4)
C90.022 (4)0.017 (3)0.021 (4)0.004 (3)−0.009 (3)−0.006 (3)
O10.025 (3)0.031 (3)0.018 (3)0.002 (2)−0.014 (2)−0.008 (2)
O20.029 (3)0.028 (3)0.015 (3)0.007 (2)−0.008 (3)−0.013 (2)
O30.024 (3)0.022 (3)0.020 (3)0.002 (2)−0.004 (2)−0.007 (2)
O40.032 (3)0.026 (3)0.019 (3)−0.003 (2)−0.005 (3)−0.016 (3)
O50.030 (3)0.020 (3)0.023 (3)0.004 (2)−0.011 (3)−0.003 (2)
O60.023 (3)0.026 (3)0.019 (3)0.007 (2)−0.004 (2)0.003 (2)
O70.020 (3)0.017 (3)0.029 (3)−0.001 (2)−0.004 (3)−0.001 (2)
Geometric parameters (Å, º) top
Yb—O12.790 (6)C3—H30.9300
Yb—O1i2.315 (6)C4—H40.9300
Yb—O22.314 (6)C5—O41.249 (10)
Yb—O32.264 (6)C5—O31.264 (10)
Yb—O4ii2.209 (6)C5—C61.497 (12)
Yb—O52.310 (6)C6—C71.387 (13)
Yb—O6iii2.321 (6)C6—C81.395 (11)
Yb—O72.293 (5)C7—C8v1.377 (12)
Yb—Ybi4.2315 (10)C7—H70.9300
C1—O21.274 (10)C8—H80.9300
C1—O11.277 (10)C9—O61.245 (10)
C1—C21.473 (12)C9—O51.269 (9)
C2—C31.390 (13)C9—C9iii1.550 (15)
C2—C41.401 (12)O7—H7B0.85
C3—C4iv1.390 (13)O7—H7A0.85
O4ii—Yb—O398.9 (2)O1—Yb—Ybi30.57 (12)
O4ii—Yb—O7102.6 (2)C9iii—Yb—Ybi163.60 (15)
O3—Yb—O7141.9 (2)O2—C1—O1119.6 (8)
O4ii—Yb—O579.5 (2)O2—C1—C2118.4 (8)
O3—Yb—O5145.4 (2)O1—C1—C2121.8 (7)
O7—Yb—O570.19 (19)C3—C2—C4118.5 (8)
O4ii—Yb—O2159.4 (3)C3—C2—C1120.3 (8)
O3—Yb—O285.5 (2)C4—C2—C1121.1 (8)
O7—Yb—O285.2 (2)C4iv—C3—C2120.5 (9)
O5—Yb—O285.5 (2)C4iv—C3—H3119.8
O4ii—Yb—O1i82.5 (2)C2—C3—H3119.8
O3—Yb—O1i80.7 (2)C3iv—C4—C2121.0 (8)
O7—Yb—O1i71.5 (2)C3iv—C4—H4119.5
O5—Yb—O1i132.4 (2)C2—C4—H4119.5
O2—Yb—O1i118.1 (2)O4—C5—O3124.2 (7)
O4ii—Yb—O6iii79.2 (2)O4—C5—C6117.8 (7)
O3—Yb—O6iii75.4 (2)O3—C5—C6118.0 (7)
O7—Yb—O6iii139.4 (2)C7—C6—C8118.8 (8)
O5—Yb—O6iii70.34 (19)C7—C6—C5120.4 (8)
O2—Yb—O6iii82.5 (2)C8—C6—C5120.7 (8)
O1i—Yb—O6iii147.1 (2)C8v—C7—C6121.0 (7)
O4ii—Yb—O1150.1 (2)C8v—C7—H7119.5
O3—Yb—O170.77 (19)C6—C7—H7119.5
O7—Yb—O174.9 (2)C7v—C8—C6120.2 (9)
O5—Yb—O1125.1 (2)C7v—C8—H8119.9
O2—Yb—O150.14 (19)C6—C8—H8119.9
O1i—Yb—O168.4 (2)O6—C9—O5127.2 (8)
O6iii—Yb—O1122.4 (2)O6—C9—C9iii117.0 (8)
O4ii—Yb—C9iii72.4 (2)O5—C9—C9iii115.7 (8)
O3—Yb—C9iii96.2 (2)O5—C9—Ybiii166.7 (6)
O7—Yb—C9iii120.2 (2)C9iii—C9—Ybiii76.1 (5)
O5—Yb—C9iii50.05 (19)C1—O1—Ybi165.8 (6)
O2—Yb—C9iii87.2 (2)C1—O1—Yb82.4 (5)
O1i—Yb—C9iii154.0 (2)Ybi—O1—Yb111.6 (2)
O6iii—Yb—C9iii21.0 (2)C1—O2—Yb104.7 (5)
O1—Yb—C9iii135.19 (19)C5—O3—Yb140.5 (5)
O4ii—Yb—Ybi120.04 (17)C5—O4—Ybii157.0 (6)
O3—Yb—Ybi72.20 (14)C9—O5—Yb117.5 (5)
O7—Yb—Ybi69.81 (14)C9—O6—Ybiii117.0 (5)
O5—Yb—Ybi138.46 (14)Yb—O7—H7B123.8
O2—Yb—Ybi80.49 (15)Yb—O7—H7A118.8
O1i—Yb—Ybi37.81 (15)H7B—O7—H7A107.3
O6iii—Yb—Ybi144.33 (15)
O2—C1—C2—C3−10.1 (13)C2—C1—O2—Yb−155.3 (6)
O1—C1—C2—C3174.7 (9)O4ii—Yb—O2—C1161.8 (6)
O2—C1—C2—C4165.3 (8)O3—Yb—O2—C158.4 (5)
O1—C1—C2—C4−9.8 (12)O7—Yb—O2—C1−84.5 (5)
C4—C2—C3—C4iv1.1 (16)O5—Yb—O2—C1−155.0 (5)
C1—C2—C3—C4iv176.7 (8)O1i—Yb—O2—C1−18.5 (6)
C3—C2—C4—C3iv−1.1 (16)O6iii—Yb—O2—C1134.3 (5)
C1—C2—C4—C3iv−176.7 (8)O1—Yb—O2—C1−10.2 (5)
O4—C5—C6—C7−152.4 (9)C9iii—Yb—O2—C1154.9 (5)
O3—C5—C6—C727.6 (12)Ybi—Yb—O2—C1−14.2 (5)
O4—C5—C6—C830.4 (13)O4—C5—O3—Yb30.8 (14)
O3—C5—C6—C8−149.6 (9)C6—C5—O3—Yb−149.2 (7)
C8—C6—C7—C8v−1.5 (16)O4ii—Yb—O3—C5−46.7 (9)
C5—C6—C7—C8v−178.8 (8)O7—Yb—O3—C5−170.7 (8)
C7—C6—C8—C7v1.5 (16)O5—Yb—O3—C537.6 (11)
C5—C6—C8—C7v178.8 (8)O2—Yb—O3—C5113.0 (9)
O2—C1—O1—Ybi171.7 (17)O1i—Yb—O3—C5−127.6 (9)
C2—C1—O1—Ybi−13 (3)O6iii—Yb—O3—C529.6 (9)
O2—C1—O1—Yb−16.0 (7)O1—Yb—O3—C5162.2 (9)
C2—C1—O1—Yb159.1 (7)C9iii—Yb—O3—C526.3 (9)
O4ii—Yb—O1—C1−164.4 (5)Ybi—Yb—O3—C5−165.5 (9)
O3—Yb—O1—C1−90.6 (5)O3—C5—O4—Ybii50.2 (19)
O7—Yb—O1—C1106.3 (5)C6—C5—O4—Ybii−129.7 (12)
O5—Yb—O1—C154.5 (5)O6—C9—O5—Yb−166.9 (7)
O2—Yb—O1—C19.9 (4)C9iii—C9—O5—Yb9.8 (12)
O1i—Yb—O1—C1−178.0 (6)Ybiii—C9—O5—Yb160 (2)
O6iii—Yb—O1—C1−33.1 (5)O4ii—Yb—O5—C969.9 (6)
C9iii—Yb—O1—C1−11.5 (6)O3—Yb—O5—C9−20.5 (8)
Ybi—Yb—O1—C1−178.0 (6)O7—Yb—O5—C9177.6 (7)
O4ii—Yb—O1—Ybi13.6 (5)O2—Yb—O5—C9−95.9 (6)
O3—Yb—O1—Ybi87.4 (3)O1i—Yb—O5—C9139.5 (6)
O7—Yb—O1—Ybi−75.7 (3)O6iii—Yb—O5—C9−12.3 (6)
O5—Yb—O1—Ybi−127.5 (2)O1—Yb—O5—C9−128.6 (6)
O2—Yb—O1—Ybi−172.1 (4)C9iii—Yb—O5—C9−5.8 (7)
O1i—Yb—O1—Ybi0.000 (2)Ybi—Yb—O5—C9−166.1 (5)
O6iii—Yb—O1—Ybi144.9 (2)O5—C9—O6—Ybiii−169.3 (7)
C9iii—Yb—O1—Ybi166.5 (2)C9iii—C9—O6—Ybiii14.1 (12)
O1—C1—O2—Yb19.9 (9)
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1, −y+1, −z+2; (iii) −x, −y+1, −z+2; (iv) −x+1, −y, −z+1; (v) −x+2, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O3i0.851.922.751 (6)167
O7—H7B···O2vi0.851.912.754 (6)178
Symmetry codes: (i) −x+1, −y, −z+2; (vi) −x, −y, −z+2.

Experimental details

Crystal data
Chemical formula[Yb2(C8H4O4)2(C2O4)(H2O)2]
Mr798.36
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)7.034 (2), 7.583 (2), 10.213 (3)
α, β, γ (°)75.372 (4), 70.851 (4), 88.126 (4)
V (Å3)497.2 (2)
Z1
Radiation typeMo Kα
µ (mm−1)9.43
Crystal size (mm)0.24 × 0.15 × 0.05
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.211, 0.629
No. of measured, independent and
observed [I > 2σ(I)] reflections		2630, 1882, 1785
Rint0.025
(sin θ/λ)max (Å−1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.120, 1.06
No. of reflections1882
No. of parameters154
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)4.45, −4.21

Computer programs: APEXII (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Yb—O12.790 (6)Yb—O4ii2.209 (6)
Yb—O1i2.315 (6)Yb—O52.310 (6)
Yb—O22.314 (6)Yb—O6iii2.321 (6)
Yb—O32.264 (6)Yb—O72.293 (5)
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1, −y+1, −z+2; (iii) −x, −y+1, −z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O3i0.851.922.751 (6)167
O7—H7B···O2iv0.851.912.754 (6)178
Symmetry codes: (i) −x+1, −y, −z+2; (iv) −x, −y, −z+2.
 

Acknowledgements

This work was supported by the Jiangxi Provincial Educational Foundation (GJJ09227).

References

First citationBruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationLi, Z.-F., Cheng, Q., Chen, J.-Z. & Chen, Y. (2009). Z. Kristallogr. New Cryst. Struct. 224, 483–484.  CAS Google Scholar
 First citationLi, Z.-F. & Wang, C.-X. (2009). Acta Cryst. E65, m1157.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationSheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 9| September 2010| Page m1161
https://doi.org/10.1107/S1600536810033052
Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS