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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 10| October 2011| Pages m1433-m1434
https://doi.org/10.1107/S1600536811038347

Poly[di­aquabis­(μ4-fumarato-κ4O1:O1′:O4:O4′)(μ4-fumarato-κ6O1:O1,O1′:O4:O4,O4′)(μ2-fumaric acid-κ2O1:O4)dipraseodymium(III)]

Pei-lian Liu,a Wanwan Cao,a Jin Wang,a Rong-hua Zenga and Zhuo Zenga,b*

aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China, and bKey Laboratory of Organofluorine Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, 200032, People's Republic of China
*Correspondence e-mail: zhuosioc@yahoo.com.cn

(Received 30 August 2011; accepted 19 September 2011; online 30 September 2011)

The title complex, [Pr2(C4H2O4)3(C4H4O4)(H2O)2]n, was synthesized by reaction of praseodymium(III) nitrate hexa­hydrate with fumaric acid in a water–ethanol (4:1) solution. The asymmetric unit comprises a Pr3+ cation, one and a half fumarate dianions (L2−), one half-mol­ecule of fumaric acid (H2L) and one coordinated water mol­ecule. The carboxyl­ate groups of the fumarate dianion and fumaric acid exhibit different coordination modes. In one fumarate dianion, two carboxyl­ate groups are chelating with two Pr3+ cations, and the other two O atoms each coordinate a Pr3+ cation. Each O atom of the second fumarate dianion binds to a different Pr3+ cation. The fumaric acid employs one O atom at each end to bridge two Pr3+ cations. The Pr3+ cation is coordinated in a distorted tricapped trigonal–prismatic environment by eight O atoms of fumarate dianion or fumaric acid ligands and one water O atom. The PrO9 coordination polyhedra are edge-shared through one carboxyl­ate O atom and two carboxyl­ate groups, generating infinite praseodymium–oxygen chains, which are further connected by the ligands into a three-dimensional framework. The crystal structure is stabilized by O—H⋯O hydrogen-bond inter­actions between the coordin­ated water mol­ecule and the carboxyl­ate O atoms.

Related literature

For the structural diversity and potential use as superconductors and magnetic materials of metal complexes of carboxyl­ates, see: Kim et al. (2004[Kim, Y. J., Suh, M. & Jung, D. Y. (2004). Inorg. Chem. 43, 245-250.]); Ye et al. (2005[Ye, B.-H., Tong, M. L. & Chen, X. M. (2005). Coord. Chem. Rev. 249, 545-565.]). For applications of rare earth carboxyl­ates, see: Baggio & Perec (2004[Baggio, R. & Perec, M. (2004). Inorg. Chem. 43, 6965-6968.]); Seo et al. (2000[Seo, J. S., Whang, D., Lee, H., Jun, S. I., Oh, J., Jeon, Y. J. & Kim, K. (2000). Nature (London), 404, 982-986.]).

[Scheme 1]

Experimental

Crystal data

  • [Pr2(C4H2O4)3(C4H4O4)(H2O)2]]

  • Mr = 776.10

  • Monoclinic, P 21 /c

  • a = 8.3714 (3) Å

  • b = 14.6034 (6) Å

  • c = 8.7518 (4) Å

  • β = 103.118 (2)°

  • V = 1042.00 (7) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 4.72 mm−1

  • T = 298 K

  • 0.26 × 0.19 × 0.15 mm
Data collection

  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.355, Tmax = 0.493

  • 10102 measured reflections

  • 2394 independent reflections

  • 2175 reflections with I > 2σ(I)

  • Rint = 0.027
Refinement

  • R[F2 > 2σ(F2)] = 0.016

  • wR(F2) = 0.041

  • S = 1.05

  • 2394 reflections

  • 170 parameters

  • 3 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.44 e Å−3

  • Δρmin = −0.75 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C3—H3⋯O7 0.93 2.50 2.815 (3) 100
O1W—H2W⋯O7i 0.83 (1) 2.11 (1) 2.911 (2) 165 (2)
O2—H2A⋯O9ii 0.82 1.86 2.661 (2) 167
O1W—H1W⋯O5iii 0.82 (1) 2.09 (2) 2.816 (2) 147 (2)
Symmetry codes: (i) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) [x+1, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]; (iii) -x+1, -y, -z.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). 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: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536811038347/hg5089sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811038347/hg5089Isup2.hkl

checkCIF report


Comment top

Metal complexes of carboxylates have attracted much attention due to their wide range of structural diversities and potential use on superconductors and magnetic materials (Kim et al., 2004; Ye et al., 2005). What is more, a particularly attractive goal is the rare-earth carboxylates, because of their special application on the 4f-block elements and their unique f-f electronic transitions. (Seo et al., 2000; Baggio et al., 2004). In this paper, we report the title complex (scheme. 1), obtained by the reaction of praseodymium(III) nitrate hexahydrate with fumaric acid in a water-ethanol (4:1) solution.

The structure of the asymmetric unit of the title complex is shown in Fig. 1. It comprises a Pr3+ cation, 1.5 fumarate dianions (L2-), 0.5 fumaric acid (H2L) and one water ligand. The carboxylate groups of the fumarate dianion and fumaric acid exhibit different coordination modes. In one fumarate dianion, two carboxylate groups are chelating with two Pr3+ cations, and other two O atoms(O4 and O4iv) are coordinated with Pr3+ cation respectively. The other fumarate dianion bridges four Pr3+ cations with monodentate mode, and the fumaric acid bridges two Pr3+ cations with monodentate mode. In the crystallographic asymmetric unit, the Pr3+ cation is sited within a distorted tricapped trigonal prism defined by nine O atoms derived from seven different bridging ligands and a coordinated water molecule. One of the carboxylate groups, derived from L2-, is chelating, and the remaining six carboxylates coordinate in a monodentate mode. The Pr—O bond distances range from 2.4040 (15) to 2.7719 (16) Å. The O—Pr—O bond angles range from 72.35 (5) to 146.04 (5)°. The PrO9 coordination polyhedra are edge-shared through one carboxylate O atoms (O4) and two carboxylate groups (O8—C4—O9 and O6—C1—O7) to generate infinite praseodymium-oxygen chains (Fig. 2). The chains are further connected by the ligands to form a three-dimensional framework. The crystal is stabilized by hydrogen bond interactions between the coordinated water and carboxylate O atoms.

Related literature top

For the structural diversity and potential use as superconductors and magnetic materials of metal complexes of carboxylates, see: Kim et al. (2004); Ye et al. (2005). For applications of rare earth carboxylates, see: Baggio & Perec (2004); Seo et al. (2000).

Experimental top

Fumaric acid (0.5 mmol, 0.058 g), Praseodymium(III) nitrate hexahydrate(0.3 mmol, 0.13 g) was dissolved in a water-ethanol(4:1) solution(10 ml). The mixture was transferred to a 20 ml Teflon-lined stainless steel autoclave, which was heated at 413 K for 96 h. The reactor was cooled to room temperature over a period of 24 h. Blue crystals were obtained after filtrated, washed with water and vacuum dried.

Refinement top

Carbon-bound H atoms were included in the riding-model approximation, with C—H =0.93Å and with Uiso(H) = 1.2Ueq(C). H atom bound to carboxyl-O atom was initially located in a difference map but was then fixed in the riding-model approximation, with O—H = 0.82Å and with Uiso(H) = 1.5 Ueq(O). Water H atoms were tentatively located in difference Fourier maps and were refined with distance restraints of O—H = 0.82Å and H···H = 1.29 Å, and with Uiso(H) = 1.5 Ueq(O).

Structure description top

Metal complexes of carboxylates have attracted much attention due to their wide range of structural diversities and potential use on superconductors and magnetic materials (Kim et al., 2004; Ye et al., 2005). What is more, a particularly attractive goal is the rare-earth carboxylates, because of their special application on the 4f-block elements and their unique f-f electronic transitions. (Seo et al., 2000; Baggio et al., 2004). In this paper, we report the title complex (scheme. 1), obtained by the reaction of praseodymium(III) nitrate hexahydrate with fumaric acid in a water-ethanol (4:1) solution.

The structure of the asymmetric unit of the title complex is shown in Fig. 1. It comprises a Pr3+ cation, 1.5 fumarate dianions (L2-), 0.5 fumaric acid (H2L) and one water ligand. The carboxylate groups of the fumarate dianion and fumaric acid exhibit different coordination modes. In one fumarate dianion, two carboxylate groups are chelating with two Pr3+ cations, and other two O atoms(O4 and O4iv) are coordinated with Pr3+ cation respectively. The other fumarate dianion bridges four Pr3+ cations with monodentate mode, and the fumaric acid bridges two Pr3+ cations with monodentate mode. In the crystallographic asymmetric unit, the Pr3+ cation is sited within a distorted tricapped trigonal prism defined by nine O atoms derived from seven different bridging ligands and a coordinated water molecule. One of the carboxylate groups, derived from L2-, is chelating, and the remaining six carboxylates coordinate in a monodentate mode. The Pr—O bond distances range from 2.4040 (15) to 2.7719 (16) Å. The O—Pr—O bond angles range from 72.35 (5) to 146.04 (5)°. The PrO9 coordination polyhedra are edge-shared through one carboxylate O atoms (O4) and two carboxylate groups (O8—C4—O9 and O6—C1—O7) to generate infinite praseodymium-oxygen chains (Fig. 2). The chains are further connected by the ligands to form a three-dimensional framework. The crystal is stabilized by hydrogen bond interactions between the coordinated water and carboxylate O atoms.

For the structural diversity and potential use as superconductors and magnetic materials of metal complexes of carboxylates, see: Kim et al. (2004); Ye et al. (2005). For applications of rare earth carboxylates, see: Baggio & Perec (2004); Seo et al. (2000).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. View of the local coordination of praseodymium(III) with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i)x,1/2 - y,-1/2 + z; (ii)1 + x,y,z; (iii)1 + x,1/2 - y,-1/2 + z; (iv)1 - x,-y,1 - z; (v)2 - x,-y,1 - z.]
[Figure 2] Fig. 2. Perspective view of the crystal packing.
Poly[diaquabis(µ4-fumarato- κ4O1:O1':O4:O4')(µ4-fumarato- κ6O1:O1,O1':O4:O4,O4') (µ2-fumaric acid-κ2O1:O4)dipraseodymium(III)] top
Crystal data top
[Pr2(C4H2O4)3(C4H4O4)(H2O)2]F(000) = 744
Mr = 776.10Dx = 2.474 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7002 reflections
a = 8.3714 (3) Åθ = 2.5–27.5°
b = 14.6034 (6) ŵ = 4.72 mm−1
c = 8.7518 (4) ÅT = 298 K
β = 103.118 (2)°Block, blue
V = 1042.00 (7) Å30.26 × 0.19 × 0.15 mm
Z = 2
Data collection top
Bruker APEXII CCD area-detector
diffractometer		2394 independent reflections
Radiation source: fine-focus sealed tube2175 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
phi and ω scansθmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −9→10
Tmin = 0.355, Tmax = 0.493k = −16→18
10102 measured reflectionsl = −11→6
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)] = 0.016Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.041H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0212P)2 + 0.5013P]
where P = (Fo2 + 2Fc2)/3
2394 reflections(Δ/σ)max = 0.001
170 parametersΔρmax = 0.44 e Å−3
3 restraintsΔρmin = −0.75 e Å−3
Crystal data top
[Pr2(C4H2O4)3(C4H4O4)(H2O)2]V = 1042.00 (7) Å3
Mr = 776.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 8.3714 (3) ŵ = 4.72 mm−1
b = 14.6034 (6) ÅT = 298 K
c = 8.7518 (4) Å0.26 × 0.19 × 0.15 mm
β = 103.118 (2)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		2394 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2175 reflections with I > 2σ(I)
Tmin = 0.355, Tmax = 0.493Rint = 0.027
10102 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0163 restraints
wR(F2) = 0.041H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.44 e Å−3
2394 reflectionsΔρmin = −0.75 e Å−3
170 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
C10.3406 (3)0.31371 (13)0.2443 (3)0.0132 (5)
C20.1598 (3)0.31134 (14)0.2330 (3)0.0170 (5)
H20.09020.29740.13690.020*
C30.0955 (3)0.32820 (15)0.3540 (3)0.0155 (4)
H30.16650.34510.44760.019*
C4−0.0831 (3)0.32223 (14)0.3522 (3)0.0128 (4)
C50.5360 (3)0.10365 (14)0.3762 (2)0.0133 (4)
C60.5244 (3)0.04325 (14)0.5105 (3)0.0160 (4)
H60.55220.06680.61180.019*
C80.9749 (3)0.06063 (16)0.3044 (3)0.0191 (5)
O10.8615 (2)0.11349 (12)0.30016 (19)0.0244 (4)
O21.0535 (2)0.05332 (15)0.1918 (2)0.0356 (5)
H2A1.01060.08680.11870.053*
C71.0333 (3)−0.00121 (16)0.4388 (3)0.0199 (5)
H71.1178−0.04220.43690.024*
O40.5972 (2)0.18329 (9)0.40478 (19)0.0143 (3)
O50.4920 (2)0.07499 (11)0.23774 (17)0.0208 (4)
O60.39185 (18)0.27539 (11)0.13689 (17)0.0174 (3)
O70.43025 (18)0.35433 (10)0.36074 (17)0.0149 (3)
O8−0.1853 (2)0.30866 (10)0.2257 (2)0.0174 (4)
O9−0.1193 (2)0.33071 (11)0.48376 (19)0.0182 (3)
O1W0.6829 (2)0.02369 (11)0.02361 (19)0.0198 (4)
H2W0.645 (3)−0.0181 (14)0.068 (2)0.030*
H1W0.656 (3)0.0080 (17)−0.0692 (12)0.030*
Pr10.632685 (13)0.190489 (7)0.097718 (13)0.00921 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0123 (11)0.0141 (11)0.0138 (12)0.0023 (7)0.0040 (9)0.0036 (8)
C20.0118 (11)0.0233 (13)0.0153 (13)−0.0014 (8)0.0018 (10)−0.0034 (8)
C30.0116 (10)0.0221 (11)0.0132 (11)−0.0022 (8)0.0035 (9)−0.0013 (9)
C40.0139 (11)0.0108 (10)0.0139 (11)−0.0008 (8)0.0039 (9)−0.0009 (8)
C50.0156 (10)0.0123 (10)0.0139 (11)−0.0005 (8)0.0071 (9)−0.0005 (8)
C60.0226 (12)0.0147 (11)0.0117 (11)−0.0013 (9)0.0063 (9)0.0005 (8)
C80.0173 (11)0.0225 (12)0.0171 (12)0.0025 (9)0.0031 (10)0.0016 (9)
O10.0270 (9)0.0292 (10)0.0171 (9)0.0133 (7)0.0055 (8)0.0058 (7)
O20.0323 (11)0.0532 (13)0.0258 (10)0.0204 (9)0.0160 (9)0.0184 (9)
C70.0188 (11)0.0219 (12)0.0174 (12)0.0080 (9)0.0008 (9)0.0023 (9)
O40.0200 (8)0.0108 (7)0.0129 (8)−0.0021 (6)0.0054 (7)−0.0012 (6)
O50.0348 (10)0.0173 (8)0.0117 (8)−0.0093 (7)0.0082 (7)−0.0021 (6)
O60.0152 (8)0.0242 (8)0.0144 (8)0.0039 (6)0.0068 (7)−0.0032 (6)
O70.0135 (7)0.0168 (8)0.0136 (8)0.0011 (6)0.0013 (6)−0.0012 (6)
O80.0142 (8)0.0217 (9)0.0152 (9)−0.0037 (6)0.0013 (7)−0.0020 (6)
O90.0172 (8)0.0240 (8)0.0159 (9)−0.0035 (7)0.0089 (7)−0.0041 (7)
O1W0.0248 (9)0.0150 (8)0.0201 (9)−0.0034 (6)0.0057 (8)−0.0025 (7)
Pr10.00954 (7)0.01013 (7)0.00840 (8)0.00028 (4)0.00300 (5)0.00065 (4)
Geometric parameters (Å, º) top
C1—O61.251 (3)O1—Pr12.5560 (16)
C1—O71.268 (3)O2—H2A0.8200
C1—O71.268 (3)C7—C7ii1.316 (5)
C1—C21.495 (3)C7—H70.9300
C2—C31.315 (3)O4—Pr1iii2.4717 (14)
C2—H20.9300O4—Pr12.7719 (16)
C3—C41.495 (3)O5—Pr12.5278 (15)
C3—H30.9300O6—Pr12.4563 (14)
C4—O81.252 (3)O7—Pr1iii2.4508 (15)
C4—O91.261 (3)O8—Pr1iv2.4040 (15)
C5—O51.256 (2)O9—Pr1v2.5184 (15)
C5—O41.273 (2)O1W—Pr12.5795 (16)
C5—C61.490 (3)O1W—H2W0.825 (10)
C6—C6i1.328 (4)O1W—H1W0.824 (9)
C6—H60.9300Pr1—O8vi2.4040 (15)
C8—O11.218 (3)Pr1—O7vii2.4508 (15)
C8—O21.308 (3)Pr1—O4vii2.4717 (14)
C8—C71.475 (3)Pr1—O9viii2.5184 (15)
O6—C1—O7124.9 (2)H2W—O1W—H1W102.5 (14)
O6—C1—O7124.9 (2)O8vi—Pr1—O7vii146.04 (5)
O6—C1—C2117.1 (2)O8vi—Pr1—O691.49 (5)
O7—C1—C2118.04 (19)O7vii—Pr1—O679.69 (5)
O7—C1—C2118.04 (19)O8vi—Pr1—O4vii75.42 (5)
C3—C2—C1122.4 (2)O7vii—Pr1—O4vii70.62 (5)
C3—C2—H2118.8O6—Pr1—O4vii75.15 (5)
C1—C2—H2118.8O8vi—Pr1—O9viii77.32 (5)
C2—C3—C4124.9 (2)O7vii—Pr1—O9viii96.08 (5)
C2—C3—H3117.6O6—Pr1—O9viii153.38 (5)
C4—C3—H3117.6O4vii—Pr1—O9viii78.65 (5)
O8—C4—O9124.4 (2)O8vi—Pr1—O5124.67 (5)
O8—C4—C3120.0 (2)O7vii—Pr1—O585.60 (5)
O9—C4—C3115.6 (2)O6—Pr1—O577.38 (6)
O5—C5—O4120.73 (19)O4vii—Pr1—O5146.29 (5)
O5—C5—C6120.43 (19)O9viii—Pr1—O5128.82 (5)
O4—C5—C6118.78 (19)O8vi—Pr1—O172.35 (5)
C6i—C6—C5121.8 (3)O7vii—Pr1—O1137.28 (5)
C6i—C6—H6119.1O6—Pr1—O1129.43 (5)
C5—C6—H6119.1O4vii—Pr1—O1139.16 (5)
O1—C8—O2123.4 (2)O9viii—Pr1—O170.41 (5)
O1—C8—C7121.8 (2)O5—Pr1—O174.27 (5)
O2—C8—C7114.8 (2)O8vi—Pr1—O1W132.29 (5)
C8—O1—Pr1139.18 (16)O7vii—Pr1—O1W69.87 (5)
C8—O2—H2A109.5O6—Pr1—O1W134.22 (5)
C7ii—C7—C8120.5 (3)O4vii—Pr1—O1W122.25 (5)
C7ii—C7—H7119.7O9viii—Pr1—O1W65.70 (5)
C8—C7—H7119.7O5—Pr1—O1W67.18 (5)
C5—O4—Pr1iii142.77 (14)O1—Pr1—O1W67.64 (5)
C5—O4—Pr188.35 (12)O8vi—Pr1—O476.79 (5)
Pr1iii—O4—Pr1127.68 (5)O7vii—Pr1—O4127.21 (5)
C5—O5—Pr1100.28 (12)O6—Pr1—O467.16 (5)
C1—O6—Pr1139.76 (15)O4vii—Pr1—O4131.91 (3)
C1—O7—Pr1iii136.47 (13)O9viii—Pr1—O4131.20 (5)
C4—O8—Pr1iv139.42 (14)O5—Pr1—O448.73 (4)
C4—O9—Pr1v137.70 (14)O1—Pr1—O462.59 (5)
Pr1—O1W—H2W118.5 (18)O1W—Pr1—O4105.50 (5)
Pr1—O1W—H1W119.2 (19)
O6—C1—C2—C3162.7 (2)C1—O6—Pr1—O116.7 (3)
O7—C1—C2—C3−17.5 (3)C1—O6—Pr1—O1W113.2 (2)
O7—C1—C2—C3−17.5 (3)C1—O6—Pr1—O423.5 (2)
C1—C2—C3—C4−176.7 (2)C5—O5—Pr1—O8vi4.60 (16)
C2—C3—C4—O8−7.0 (3)C5—O5—Pr1—O7vii−158.77 (14)
C2—C3—C4—O9172.2 (2)C5—O5—Pr1—O6−78.37 (13)
O5—C5—C6—C6i3.3 (4)C5—O5—Pr1—O4vii−114.41 (14)
O4—C5—C6—C6i−173.9 (3)C5—O5—Pr1—O9viii106.95 (14)
O2—C8—O1—Pr129.0 (4)C5—O5—Pr1—O159.30 (13)
C7—C8—O1—Pr1−150.46 (18)C5—O5—Pr1—O1W131.23 (14)
O1—C8—C7—C7ii−2.2 (5)C5—O5—Pr1—O4−7.80 (12)
O2—C8—C7—C7ii178.3 (3)C8—O1—Pr1—O8vi−115.0 (3)
O5—C5—O4—Pr1iii153.25 (17)C8—O1—Pr1—O7vii44.8 (3)
C6—C5—O4—Pr1iii−29.5 (3)C8—O1—Pr1—O6168.1 (2)
O5—C5—O4—Pr1−13.4 (2)C8—O1—Pr1—O4vii−75.5 (3)
C6—C5—O4—Pr1163.80 (18)C8—O1—Pr1—O9viii−32.5 (2)
O4—C5—O5—Pr115.0 (2)C8—O1—Pr1—O5109.8 (3)
C6—C5—O5—Pr1−162.19 (17)C8—O1—Pr1—O1W38.5 (2)
O7—C1—O6—Pr133.2 (3)C8—O1—Pr1—O4161.1 (3)
O7—C1—O6—Pr133.2 (3)C5—O4—Pr1—O8vi−161.98 (13)
C2—C1—O6—Pr1−147.04 (17)Pr1iii—O4—Pr1—O8vi28.18 (8)
O6—C1—O7—O70.00 (13)C5—O4—Pr1—O7vii44.97 (14)
C2—C1—O7—O70.00 (7)Pr1iii—O4—Pr1—O7vii−124.87 (8)
O6—C1—O7—Pr1iii−70.6 (3)C5—O4—Pr1—O6100.68 (13)
O7—C1—O7—Pr1iii0 (100)Pr1iii—O4—Pr1—O6−69.17 (8)
C2—C1—O7—Pr1iii109.6 (2)C5—O4—Pr1—O4vii141.96 (10)
O9—C4—O8—Pr1iv−69.1 (3)Pr1iii—O4—Pr1—O4vii−27.89 (15)
C3—C4—O8—Pr1iv110.1 (2)C5—O4—Pr1—O9viii−102.32 (13)
O8—C4—O9—Pr1v9.8 (3)Pr1iii—O4—Pr1—O9viii87.84 (9)
C3—C4—O9—Pr1v−169.47 (15)C5—O4—Pr1—O57.57 (12)
C1—O6—Pr1—O8vi−51.5 (2)Pr1iii—O4—Pr1—O5−162.27 (11)
C1—O6—Pr1—O7vii161.5 (2)C5—O4—Pr1—O1−85.22 (13)
C1—O6—Pr1—O4vii−126.0 (2)Pr1iii—O4—Pr1—O1104.93 (9)
C1—O6—Pr1—O9viii−115.5 (2)C5—O4—Pr1—O1W−31.27 (13)
C1—O6—Pr1—O573.8 (2)Pr1iii—O4—Pr1—O1W158.88 (7)
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+2, −y, −z+1; (iii) x, −y+1/2, z+1/2; (iv) x−1, y, z; (v) x−1, −y+1/2, z+1/2; (vi) x+1, y, z; (vii) x, −y+1/2, z−1/2; (viii) x+1, −y+1/2, z−1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···O70.932.502.815 (3)100
O1W—H2W···O7ix0.83 (1)2.11 (1)2.911 (2)165 (2)
O2—H2A···O9viii0.821.862.661 (2)167
O1W—H1W···O5x0.82 (1)2.09 (2)2.816 (2)147 (2)
Symmetry codes: (viii) x+1, −y+1/2, z−1/2; (ix) −x+1, y−1/2, −z+1/2; (x) −x+1, −y, −z.

Experimental details

Crystal data
Chemical formula[Pr2(C4H2O4)3(C4H4O4)(H2O)2]
Mr776.10
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)8.3714 (3), 14.6034 (6), 8.7518 (4)
β (°) 103.118 (2)
V (Å3)1042.00 (7)
Z2
Radiation typeMo Kα
µ (mm−1)4.72
Crystal size (mm)0.26 × 0.19 × 0.15
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.355, 0.493
No. of measured, independent and
observed [I > 2σ(I)] reflections		10102, 2394, 2175
Rint0.027
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.016, 0.041, 1.05
No. of reflections2394
No. of parameters170
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.44, −0.75

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), SHELXTL97 (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···O70.932.502.815 (3)100.3
O1W—H2W···O7i0.825 (10)2.106 (12)2.911 (2)165 (2)
O2—H2A···O9ii0.821.862.661 (2)166.5
O1W—H1W···O5iii0.824 (9)2.087 (16)2.816 (2)147 (2)
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) x+1, −y+1/2, z−1/2; (iii) −x+1, −y, −z.
 

Acknowledgements

The authors gratefully acknowledge the support of the Department of Science and Technology, Guangdong Province [grant Nos. 2010 A020507001–76, 5300410, FIPL-05–003].

References

First citationBaggio, R. & Perec, M. (2004). Inorg. Chem. 43, 6965–6968.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationBruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationKim, Y. J., Suh, M. & Jung, D. Y. (2004). Inorg. Chem. 43, 245–250.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationSeo, J. S., Whang, D., Lee, H., Jun, S. I., Oh, J., Jeon, Y. J. & Kim, K. (2000). Nature (London), 404, 982–986.  PubMed CAS Google Scholar
 First citationSheldrick, G. M. (1996). 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
 First citationYe, B.-H., Tong, M. L. & Chen, X. M. (2005). Coord. Chem. Rev. 249, 545–565.  CrossRef CAS Google Scholar

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ISSN: 2056-9890
Volume 67| Part 10| October 2011| Pages m1433-m1434
https://doi.org/10.1107/S1600536811038347
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