Poly[diaqua­(μ-oxalato)(μ-2-oxido­pyridinium-3-carboxyl­ato)praseo­dymium(III)]

Xu, Y.-J.; Yang, X.-X.; Zhao, H.-B.

doi:10.1107/S160053680900542X

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 3| March 2009| Page m310

doi:10.1107/S160053680900542X

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Poly[diaqua(μ-oxalato)(μ-2-oxidopyridinium-3-carboxylato)praseodymium(III)]

Yong-Jun Xu,^a ^* Xiao-Xi Yang ^a and Hong-Bin Zhao ^a

^aCollege of Chemistry and Environmental Engineering, Dongguan University of Technology, Dongguan 523808, Guangdong, People's Republic of China
^*Correspondence e-mail: xuyj2009@yahoo.com.cn

(Received 1 February 2009; accepted 16 February 2009; online 21 February 2009)

In the title complex, [Pr(C₆H₄NO₃)(C₂O₄)(H₂O)₂]_n, each Pr^III ion is coordinated by eight O atoms from two 2-oxynicotinate ligands, two oxalate ligands and two water molecules, displaying a distorted bicapped square-antiprismatic geometry. The carboxylate groups link adjacent praseodymium metal centres, forming layers parallel to the bc plane. The crystal packing is stabilized by intermolecular O—H⋯O and N—H⋯O hydrogen bonds.

Related literature

For a general background on the molecular self-assembly of supramolecular architectures, see: Mou et al. (2008 ); Moulton & Zaworotko (2001 ); Zeng et al. (2007 ).

Experimental

Crystal data

[Pr(C₆H₄NO₃)(C₂O₄)(H₂O)₂]
M_r = 403.06
Triclinic, $[P \overline 1]$
a = 7.5820 (19) Å
b = 8.643 (2) Å
c = 9.375 (4) Å
α = 108.992 (4)°
β = 103.925 (4)°
γ = 102.043 (3)°
V = 535.6 (3) Å³
Z = 2
Mo Kα radiation
μ = 4.60 mm⁻¹
T = 296 K
0.19 × 0.17 × 0.16 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.435, T_max = 0.485
2751 measured reflections
1888 independent reflections
1753 reflections with I > 2σ(I)
R_int = 0.024

Refinement

R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.080
S = 1.10
1888 reflections
187 parameters
8 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.06 e Å⁻³
Δρ_min = −1.66 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2W—H4W⋯O3	0.83 (3)	2.56 (2)	3.306 (6)	149 (4)
O2W—H3W⋯O7ⁱ	0.84 (5)	1.95 (6)	2.764 (6)	164 (7)
O2W—H4W⋯O2Wⁱⁱ	0.83 (3)	2.37 (2)	2.820 (8)	114 (2)
O1W—H2W⋯O2ⁱⁱ	0.85 (6)	2.49 (4)	3.280 (7)	157 (8)
O1W—H1W⋯O3	0.84 (5)	2.34 (6)	2.760 (6)	111 (5)
O1W—H1W⋯O6ⁱⁱⁱ	0.84 (5)	2.24 (3)	3.002 (6)	151 (6)
N1—H1⋯O4ⁱⁱⁱ	0.86 (6)	2.12 (4)	2.878 (7)	146 (6)
Symmetry codes: (i) x, y-1, z; (ii) -x+1, -y+1, -z+2; (iii) -x+1, -y+2, -z+2.

Data collection: APEX2 (Bruker, 2004 ); cell refinement: APEX2; 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: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680900542X/rz2293sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680900542X/rz2293Isup2.hkl

checkCIF report

Comment top

Molecular self-assembly of supramolecular architectures has received much attention during recent decades (Zeng et al., 2007; Moulton & Zaworotko, 2001; Mou et al., 2008). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. Recently, we obtained the title coordination polymer, which was synthesized under hydrothermal conditions.

As illustrated in Fig. 1, in the structure of the title compound each Pr^III centre is in a distorted bicapped square antiprismatic geometry, defined by eight oxygen atoms from two 2-oxynicotinate ligands, two oxalate ligands, and two water molecules The Pr^III ions are linked by 2-oxynicotinate ligands and oxalate ligands to form layers parallel to the bc plane (Fig. 2), with separations between adjacent Pr^III metal centres of 4.410 (4), 6.505 (5) and 6.551 (3) Å. Intermolecular O—H···O and N—H···O hydrogen bonding interactions (Table 1) involving the 2-oxynicotinate ligands, the oxalate ligands and the water molecules assemble neighboring layers to form a three-dimensional supramolecular network motif.

Related literature top

For a general background on the molecular self-assembly of supramolecular architectures, see: Mou et al. (2008); Moulton & Zaworotko (2001); Zeng et al. (2007).

Experimental top

A mixture of Pr₂O₃ (0.330 g; 1.0 mmol), 2-oxynicotinic acid (0.127 g; 1 mmol), oxalic acid(0.09 g; 1 mmol), water (10 ml) in the presence of HNO₃ (0.024 g; 0.385 mmol) was stirred vigorously for 20 min and then sealed in a Teflon-lined stainless-steel autoclave (20 ml, capacity). The autoclave was heated and maintained at 443 K for 3 days. After cooling to room temperature at 5 K h^-1, colourless block crystals of the title compound were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 (Bruker, 2004); data reduction: APEX2 (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: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure of the title compound showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (i) -x, 1 - y, 2 - z; (ii) -x, 1 - y, 1 - z; (iii) -x, 2 - y, 2 - z.
	Fig. 2. Crystal structure of the title compound viewed approximately along the a axis.

Poly[diaqua(µ-oxalato)(µ-2-oxidopyridinium-3- carboxylato)praseodymium(III)] top

Crystal data top

[Pr(C₆H₄NO₃)(C₂O₄)(H₂O)₂]	Z = 2
M_r = 403.06	F(000) = 388
Triclinic, P1	D_x = 2.499 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.5820 (19) Å	Cell parameters from 2183 reflections
b = 8.643 (2) Å	θ = 2.6–28.0°
c = 9.375 (4) Å	µ = 4.60 mm⁻¹
α = 108.992 (4)°	T = 296 K
β = 103.925 (4)°	Block, colourless
γ = 102.043 (3)°	0.19 × 0.17 × 0.16 mm
V = 535.6 (3) Å³

Data collection top

Bruker APEXII area-detector diffractometer	1888 independent reflections
Radiation source: fine-focus sealed tube	1753 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
ϕ and ω scans	θ_max = 25.2°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→8
T_min = 0.435, T_max = 0.485	k = −6→10
2751 measured reflections	l = −11→10

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.080	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ²(F_o²) + (0.0483P)² + 0.01P] where P = (F_o² + 2F_c²)/3
1888 reflections	(Δ/σ)_max = 0.001
187 parameters	Δρ_max = 1.06 e Å⁻³
8 restraints	Δρ_min = −1.66 e Å⁻³

Crystal data top

[Pr(C₆H₄NO₃)(C₂O₄)(H₂O)₂]	γ = 102.043 (3)°
M_r = 403.06	V = 535.6 (3) Å³
Triclinic, P1	Z = 2
a = 7.5820 (19) Å	Mo Kα radiation
b = 8.643 (2) Å	µ = 4.60 mm⁻¹
c = 9.375 (4) Å	T = 296 K
α = 108.992 (4)°	0.19 × 0.17 × 0.16 mm
β = 103.925 (4)°

Data collection top

Bruker APEXII area-detector diffractometer	1888 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1753 reflections with I > 2σ(I)
T_min = 0.435, T_max = 0.485	R_int = 0.024
2751 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	8 restraints
wR(F²) = 0.080	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	Δρ_max = 1.06 e Å⁻³
1888 reflections	Δρ_min = −1.66 e Å⁻³
187 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

	x	y	z	U_iso*/U_eq
Pr1	0.13688 (4)	0.65736 (3)	0.88899 (3)	0.01199 (13)
O1	0.1360 (5)	0.5899 (6)	1.1378 (4)	0.0209 (9)
O2	0.2431 (6)	0.4573 (6)	1.2882 (5)	0.0292 (10)
O3	0.4163 (6)	0.8435 (6)	1.1280 (4)	0.0255 (10)
O4	0.0792 (6)	0.7141 (5)	0.6359 (4)	0.0210 (9)
O5	−0.0653 (6)	0.5985 (5)	0.3701 (5)	0.0240 (9)
O6	0.1917 (5)	0.9740 (5)	0.9339 (5)	0.0211 (9)
O7	0.0683 (6)	1.1925 (5)	0.9755 (5)	0.0221 (9)
N1	0.6714 (7)	0.9795 (7)	1.3550 (6)	0.0213 (11)
H1	0.709 (9)	1.056 (6)	1.320 (7)	0.026*
C1	0.2690 (8)	0.5814 (8)	1.2460 (6)	0.0184 (12)
C2	0.4526 (7)	0.7259 (7)	1.3291 (6)	0.0155 (11)
C3	0.5671 (8)	0.7451 (8)	1.4747 (7)	0.0226 (13)
H3	0.5331	0.6633	1.5160	0.027*
C4	0.7339 (8)	0.8845 (9)	1.5629 (7)	0.0268 (14)
H4	0.8106	0.8963	1.6620	0.032*
C5	0.7816 (8)	1.0019 (8)	1.5011 (7)	0.0260 (14)
H5	0.8900	1.0978	1.5591	0.031*
C6	0.5042 (8)	0.8480 (8)	1.2612 (6)	0.0176 (12)
C7	0.0043 (7)	0.5910 (7)	0.5025 (6)	0.0169 (12)
C8	0.0756 (7)	1.0482 (7)	0.9731 (6)	0.0132 (11)
O1W	0.4579 (6)	0.7364 (7)	0.8300 (6)	0.0344 (11)
H1W	0.526 (8)	0.825 (6)	0.912 (6)	0.052*
H2W	0.532 (7)	0.703 (9)	0.781 (7)	0.052*
O2W	0.3042 (6)	0.4283 (6)	0.9073 (5)	0.0256 (9)
H3W	0.253 (9)	0.355 (5)	0.938 (6)	0.038*
H4W	0.362 (3)	0.520 (3)	0.987 (4)	0.038*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pr1	0.01204 (18)	0.0123 (2)	0.01350 (19)	0.00367 (13)	0.00302 (12)	0.00841 (14)
O1	0.0147 (19)	0.030 (3)	0.0152 (19)	0.0010 (18)	−0.0001 (16)	0.0128 (18)
O2	0.030 (2)	0.023 (3)	0.031 (2)	−0.003 (2)	0.0026 (19)	0.019 (2)
O3	0.0211 (19)	0.029 (3)	0.019 (2)	−0.0046 (18)	−0.0042 (16)	0.0153 (19)
O4	0.031 (2)	0.015 (2)	0.0137 (19)	0.0041 (18)	0.0044 (17)	0.0060 (17)
O5	0.040 (2)	0.016 (2)	0.016 (2)	0.0109 (19)	0.0039 (18)	0.0103 (18)
O6	0.0183 (19)	0.019 (2)	0.035 (2)	0.0104 (18)	0.0150 (17)	0.0138 (19)
O7	0.027 (2)	0.013 (2)	0.036 (2)	0.0079 (18)	0.0173 (18)	0.0158 (19)
N1	0.019 (2)	0.019 (3)	0.025 (3)	0.002 (2)	0.003 (2)	0.012 (2)
C1	0.023 (3)	0.019 (3)	0.013 (3)	0.006 (3)	0.005 (2)	0.006 (2)
C2	0.015 (2)	0.018 (3)	0.015 (3)	0.004 (2)	0.006 (2)	0.008 (2)
C3	0.026 (3)	0.028 (4)	0.018 (3)	0.009 (3)	0.007 (2)	0.016 (3)
C4	0.020 (3)	0.035 (4)	0.019 (3)	0.005 (3)	−0.003 (2)	0.012 (3)
C5	0.015 (3)	0.025 (4)	0.029 (3)	0.003 (3)	0.001 (2)	0.006 (3)
C6	0.019 (3)	0.021 (3)	0.015 (3)	0.008 (2)	0.008 (2)	0.006 (2)
C7	0.017 (3)	0.017 (3)	0.019 (3)	0.005 (2)	0.005 (2)	0.011 (2)
C8	0.014 (2)	0.011 (3)	0.013 (3)	0.003 (2)	0.000 (2)	0.005 (2)
O1W	0.025 (2)	0.035 (3)	0.034 (3)	0.000 (2)	0.0112 (19)	0.007 (2)
O2W	0.025 (2)	0.030 (3)	0.033 (2)	0.015 (2)	0.0120 (18)	0.021 (2)

Geometric parameters (Å, º) top

Pr1—O3	2.458 (4)	O7—C8	1.253 (7)
Pr1—O4	2.532 (4)	O7—Pr1ⁱ	2.537 (4)
Pr1—O7ⁱ	2.537 (4)	N1—C5	1.350 (8)
Pr1—O5ⁱⁱ	2.540 (4)	N1—C6	1.372 (8)
Pr1—O1ⁱⁱⁱ	2.543 (4)	N1—H1	0.86 (6)
Pr1—O6	2.555 (4)	C1—C2	1.491 (8)
Pr1—O1	2.583 (4)	C1—Pr1ⁱⁱⁱ	3.018 (6)
Pr1—O2W	2.593 (4)	C2—C3	1.367 (8)
Pr1—O1W	2.626 (4)	C2—C6	1.434 (8)
Pr1—O2ⁱⁱⁱ	2.734 (4)	C3—C4	1.396 (8)
Pr1—C1ⁱⁱⁱ	3.018 (6)	C3—H3	0.9300
Pr1—H4W	2.44 (4)	C4—C5	1.352 (9)
O1—C1	1.280 (7)	C4—H4	0.9300
O1—Pr1ⁱⁱⁱ	2.543 (4)	C5—H5	0.9300
O2—C1	1.253 (7)	C7—C7ⁱⁱ	1.546 (11)
O2—Pr1ⁱⁱⁱ	2.734 (4)	C8—C8ⁱ	1.555 (10)
O3—C6	1.251 (7)	O1W—H1W	0.84 (5)
O4—C7	1.248 (7)	O1W—H2W	0.84 (5)
O5—C7	1.255 (6)	O2W—H3W	0.84 (5)
O5—Pr1ⁱⁱ	2.540 (4)	O2W—H4W	0.83 (3)
O6—C8	1.249 (6)

O3—Pr1—O4	120.86 (13)	O4—Pr1—H4W	127.8 (11)
O3—Pr1—O7ⁱ	88.47 (14)	O7ⁱ—Pr1—H4W	129.5 (10)
O4—Pr1—O7ⁱ	102.37 (13)	O5ⁱⁱ—Pr1—H4W	81.2 (5)
O3—Pr1—O5ⁱⁱ	137.09 (15)	O1ⁱⁱⁱ—Pr1—H4W	88.8 (9)
O4—Pr1—O5ⁱⁱ	63.36 (13)	O6—Pr1—H4W	129.1 (6)
O7ⁱ—Pr1—O5ⁱⁱ	134.11 (14)	O1—Pr1—H4W	60.0 (11)
O3—Pr1—O1ⁱⁱⁱ	127.58 (12)	O2W—Pr1—H4W	18.7 (8)
O4—Pr1—O1ⁱⁱⁱ	111.40 (13)	O1W—Pr1—H4W	67.4 (11)
O7ⁱ—Pr1—O1ⁱⁱⁱ	76.36 (13)	O2ⁱⁱⁱ—Pr1—H4W	134.2 (6)
O5ⁱⁱ—Pr1—O1ⁱⁱⁱ	70.57 (14)	C1ⁱⁱⁱ—Pr1—H4W	111.2 (8)
O3—Pr1—O6	69.27 (14)	C1—O1—Pr1ⁱⁱⁱ	98.8 (3)
O4—Pr1—O6	65.37 (13)	C1—O1—Pr1	131.9 (3)
O7ⁱ—Pr1—O6	63.08 (12)	Pr1ⁱⁱⁱ—O1—Pr1	118.71 (14)
O5ⁱⁱ—Pr1—O6	128.42 (12)	C1—O2—Pr1ⁱⁱⁱ	90.5 (3)
O1ⁱⁱⁱ—Pr1—O6	136.28 (12)	C6—O3—Pr1	140.0 (4)
O3—Pr1—O1	66.31 (12)	C7—O4—Pr1	119.9 (3)
O4—Pr1—O1	170.59 (12)	C7—O5—Pr1ⁱⁱ	120.3 (4)
O7ⁱ—Pr1—O1	70.75 (13)	C8—O6—Pr1	120.7 (3)
O5ⁱⁱ—Pr1—O1	116.45 (13)	C8—O7—Pr1ⁱ	121.3 (3)
O1ⁱⁱⁱ—Pr1—O1	61.29 (14)	C5—N1—C6	125.6 (5)
O6—Pr1—O1	115.03 (13)	C5—N1—H1	116 (5)
O3—Pr1—O2W	81.72 (14)	C6—N1—H1	118 (4)
O4—Pr1—O2W	117.75 (13)	O2—C1—O1	120.7 (5)
O7ⁱ—Pr1—O2W	137.99 (13)	O2—C1—C2	119.7 (5)
O5ⁱⁱ—Pr1—O2W	63.32 (13)	O1—C1—C2	119.5 (5)
O1ⁱⁱⁱ—Pr1—O2W	77.80 (13)	O2—C1—Pr1ⁱⁱⁱ	65.0 (3)
O6—Pr1—O2W	144.55 (13)	O1—C1—Pr1ⁱⁱⁱ	56.4 (3)
O1—Pr1—O2W	67.88 (13)	C2—C1—Pr1ⁱⁱⁱ	168.4 (4)
O3—Pr1—O1W	65.67 (14)	C3—C2—C6	120.3 (5)
O4—Pr1—O1W	69.36 (14)	C3—C2—C1	119.0 (5)
O7ⁱ—Pr1—O1W	139.13 (15)	C6—C2—C1	120.6 (5)
O5ⁱⁱ—Pr1—O1W	79.60 (14)	C2—C3—C4	121.5 (6)
O1ⁱⁱⁱ—Pr1—O1W	144.47 (15)	C2—C3—H3	119.2
O6—Pr1—O1W	77.88 (14)	C4—C3—H3	119.2
O1—Pr1—O1W	120.06 (14)	C5—C4—C3	118.5 (5)
O2W—Pr1—O1W	71.70 (15)	C5—C4—H4	120.7
O3—Pr1—O2ⁱⁱⁱ	153.63 (15)	C3—C4—H4	120.7
O4—Pr1—O2ⁱⁱⁱ	67.95 (13)	N1—C5—C4	119.8 (6)
O7ⁱ—Pr1—O2ⁱⁱⁱ	65.16 (14)	N1—C5—H5	120.1
O5ⁱⁱ—Pr1—O2ⁱⁱⁱ	69.19 (14)	C4—C5—H5	120.1
O1ⁱⁱⁱ—Pr1—O2ⁱⁱⁱ	49.16 (12)	O3—C6—N1	118.7 (5)
O6—Pr1—O2ⁱⁱⁱ	96.62 (13)	O3—C6—C2	127.0 (5)
O1—Pr1—O2ⁱⁱⁱ	102.91 (12)	N1—C6—C2	114.3 (5)
O2W—Pr1—O2ⁱⁱⁱ	117.69 (14)	O4—C7—O5	127.0 (5)
O1W—Pr1—O2ⁱⁱⁱ	135.00 (14)	O4—C7—C7ⁱⁱ	117.4 (6)
O3—Pr1—C1ⁱⁱⁱ	147.53 (14)	O5—C7—C7ⁱⁱ	115.7 (6)
O4—Pr1—C1ⁱⁱⁱ	88.65 (14)	O6—C8—O7	127.4 (5)
O7ⁱ—Pr1—C1ⁱⁱⁱ	70.79 (14)	O6—C8—C8ⁱ	116.4 (6)
O5ⁱⁱ—Pr1—C1ⁱⁱⁱ	65.76 (14)	O7—C8—C8ⁱ	116.2 (6)
O1ⁱⁱⁱ—Pr1—C1ⁱⁱⁱ	24.77 (14)	Pr1—O1W—H1W	103 (4)
O6—Pr1—C1ⁱⁱⁱ	118.47 (14)	Pr1—O1W—H2W	148 (5)
O1—Pr1—C1ⁱⁱⁱ	83.03 (13)	H1W—O1W—H2W	107 (6)
O2W—Pr1—C1ⁱⁱⁱ	96.95 (15)	Pr1—O2W—H3W	116 (5)
O1W—Pr1—C1ⁱⁱⁱ	144.76 (15)	Pr1—O2W—H4W	70 (3)
O2ⁱⁱⁱ—Pr1—C1ⁱⁱⁱ	24.54 (14)	H3W—O2W—H4W	108 (4)
O3—Pr1—H4W	63.2 (7)

Symmetry codes: (i) −x, −y+2, −z+2; (ii) −x, −y+1, −z+1; (iii) −x, −y+1, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H4W···O3	0.83 (3)	2.56 (2)	3.306 (6)	149 (4)
O2W—H3W···O7^iv	0.84 (5)	1.95 (6)	2.764 (6)	164 (7)
O2W—H4W···O2W^v	0.83 (3)	2.37 (2)	2.820 (8)	114 (2)
O1W—H2W···O2^v	0.85 (6)	2.49 (4)	3.280 (7)	157 (8)
O1W—H1W···O3	0.84 (5)	2.34 (6)	2.760 (6)	111 (5)
O1W—H1W···O6^vi	0.84 (5)	2.24 (3)	3.002 (6)	151 (6)
N1—H1···O4^vi	0.86 (6)	2.12 (4)	2.878 (7)	146 (6)

Symmetry codes: (iv) x, y−1, z; (v) −x+1, −y+1, −z+2; (vi) −x+1, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[Pr(C₆H₄NO₃)(C₂O₄)(H₂O)₂]
M_r	403.06
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	7.5820 (19), 8.643 (2), 9.375 (4)
α, β, γ (°)	108.992 (4), 103.925 (4), 102.043 (3)
V (Å³)	535.6 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	4.60
Crystal size (mm)	0.19 × 0.17 × 0.16

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.435, 0.485
No. of measured, independent and observed [I > 2σ(I)] reflections	2751, 1888, 1753
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.080, 1.10
No. of reflections	1888
No. of parameters	187
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.06, −1.66

Computer programs: APEX2 (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H4W···O3	0.83 (3)	2.56 (2)	3.306 (6)	149 (4)
O2W—H3W···O7ⁱ	0.84 (5)	1.95 (6)	2.764 (6)	164 (7)
O2W—H4W···O2Wⁱⁱ	0.83 (3)	2.37 (2)	2.820 (8)	114 (2)
O1W—H2W···O2ⁱⁱ	0.85 (6)	2.49 (4)	3.280 (7)	157 (8)
O1W—H1W···O3	0.84 (5)	2.34 (6)	2.760 (6)	111 (5)
O1W—H1W···O6ⁱⁱⁱ	0.84 (5)	2.24 (3)	3.002 (6)	151 (6)
N1—H1···O4ⁱⁱⁱ	0.86 (6)	2.12 (4)	2.878 (7)	146 (6)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z+2; (iii) −x+1, −y+2, −z+2.

Acknowledgements

The authors gratefully acknowledge the financial support from the Emphasis Project sponsored by the Department of Education of Guangdong Province (No. [2007]129).

References

Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Mou, J.-X., Zeng, R.-H., Qiu, Y.-C., Zhang, W.-G., Deng, H. & Zeller, M. (2008). Inorg. Chem. Commun. 11, 1347–1351. Web of Science CSD CrossRef CAS Google Scholar
Moulton, B. & Zaworotko, M. J. (2001). Chem. Rev. 101, 1629–1658. Web of Science CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zeng, R.-H., Qiu, Y.-C., Cai, Y.-P., Wu, J.-Z. & Deng, H. (2007). Acta Cryst. E63, m1666. Web of Science CSD CrossRef IUCr Journals Google Scholar

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Volume 65| Part 3| March 2009| Page m310

doi:10.1107/S160053680900542X

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

Poly[di­aqua­(μ-oxalato)(μ-2-oxido­pyridinium-3-carboxyl­ato)praseo­dymium(III)]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Poly[diaqua(μ-oxalato)(μ-2-oxidopyridinium-3-carboxylato)praseodymium(III)]