Poly[[diaqua-hemi-μ(4)-oxalato-μ(2)-oxalato-praseodymium(III)] monohydrate].

In the title complex, {[Pr(C(2)O(4))(1.5)(H(2)O)(2)]·H(2)O}(n), the Pr(III) ion, which lies on a crystallographic inversion centre, is coordinated by seven O atoms from four oxalate ligands and two O atoms from two water ligands; further Pr-O coordination from tetra-dentate oxalate ligands forms a three-dimensional structure. The compound crystallized as a monohydrate, the water mol-ecule occupying space in small voids and being secured by O-H⋯O hydrogen bonding as an acceptor from ligand water H atoms and as a donor to oxalate O-acceptor sites.

Related literature

For background to lanthanide oxalates and their preparation, see: Hansson (1970 ▶, 1972 ▶, 1973a ▶, 1973b ▶); Michaelides et al. (1988 ▶); Ollendorf & Weigel (1969 ▶); Steinfink & Brunton (1970 ▶); Trollet et al. (1998 ▶); Trombe (2003 ▶); Unaleroglu et al. (1997 ▶). For related structures, see: Trombe et al. (2004 ▶); Barrett Adams et al. (1998 ▶); Beagley et al. (1988 ▶).

Experimental

Crystal data

[Pr(C2O4)1.5(H2O)2]·H2O

M = 326.99

Triclinic,

a = 6.0367 (12) Å

b = 7.6222 (15) Å

c = 8.9353 (18) Å

α = 98.330 (4)°

β = 99.814 (3)°

γ = 96.734 (4)°

V = 396.58 (14) Å3

Z = 2

Mo Kα radiation

μ = 6.17 mm−1

T = 273 K

0.18 × 0.16 × 0.10 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.341, T max = 0.542

2140 measured reflections

1521 independent reflections

1450 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.075

S = 1.00

1521 reflections

118 parameters

H-atom parameters constrained

Δρmax = 0.80 e Å−3

Δρmin = −1.50 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809033947/nk2001sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809033947/nk2001Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pr(C2O4)1.5(H2O)2]·H2O	Z = 2
Mr = 326.99	F(000) = 310
Triclinic, P1	Dx = 2.738 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.0367 (12) Å	Cell parameters from 905 reflections
b = 7.6222 (15) Å	θ = 3.3–28.3°
c = 8.9353 (18) Å	µ = 6.17 mm−1
α = 98.330 (4)°	T = 273 K
β = 99.814 (3)°	Block, green
γ = 96.734 (4)°	0.18 × 0.16 × 0.10 mm
V = 396.58 (14) Å3

Bruker SMART APEX CCD diffractometer	1521 independent reflections
Radiation source: fine-focus sealed tube	1450 reflections with I > 2σ(I)
graphite	Rint = 0.020
φ and ω scans	θmax = 26.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −7→7
Tmin = 0.341, Tmax = 0.542	k = −9→8
2140 measured reflections	l = −10→11

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075	H-atom parameters constrained
S = 1.00	w = 1/[σ2(Fo2) + (0.049P)2 + 1.09P] where P = (Fo2 + 2Fc2)/3
1521 reflections	(Δ/σ)max = 0.001
118 parameters	Δρmax = 0.80 e Å−3
0 restraints	Δρmin = −1.49 e Å−3

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.

	x	y	z	Uiso*/Ueq
Pr1	1.00780 (5)	0.80762 (4)	0.29489 (3)	0.01182 (13)
C1	1.4452 (9)	1.0278 (7)	0.5703 (6)	0.0155 (11)
C2	1.0808 (10)	0.5659 (7)	−0.0322 (7)	0.0163 (12)
C3	0.8789 (9)	0.5155 (7)	0.5109 (6)	0.0157 (11)
O1	1.2322 (6)	0.9964 (5)	0.5514 (4)	0.0156 (8)
O2	1.5785 (7)	1.1009 (6)	0.6910 (5)	0.0220 (9)
O3	1.1296 (7)	0.7232 (5)	0.0431 (5)	0.0195 (9)
O4	1.1455 (7)	0.5077 (5)	−0.1515 (5)	0.0217 (9)
O5	0.8004 (7)	0.6413 (5)	0.4552 (5)	0.0195 (9)
O6	0.7818 (7)	0.4116 (6)	0.5849 (5)	0.0230 (9)
O1W	0.6751 (7)	0.8292 (7)	0.0928 (5)	0.0310 (11)
H1WA	0.5581	0.8534	0.1260	0.046*
H1WB	0.6299	0.7771	0.0011	0.046*
O2W	1.0612 (8)	1.0993 (6)	0.2071 (5)	0.0288 (10)
H2WA	1.1653	1.1872	0.2227	0.043*
H2WB	0.9752	1.1029	0.1239	0.043*
O3W	0.4213 (9)	0.3694 (7)	0.2101 (6)	0.0420 (13)
H3WA	0.4103	0.4339	0.2922	0.063*
H3WB	0.5590	0.3823	0.2031	0.063*

	U11	U22	U33	U12	U13	U23
Pr1	0.01064 (19)	0.01179 (18)	0.01243 (18)	0.00024 (12)	0.00360 (12)	−0.00045 (12)
C1	0.012 (3)	0.016 (3)	0.019 (3)	0.001 (2)	0.005 (2)	0.001 (2)
C2	0.015 (3)	0.016 (3)	0.018 (3)	0.002 (2)	0.005 (2)	0.002 (2)
C3	0.016 (3)	0.016 (3)	0.014 (3)	0.002 (2)	0.004 (2)	0.000 (2)
O1	0.0075 (19)	0.019 (2)	0.020 (2)	0.0013 (15)	0.0047 (15)	−0.0003 (16)
O2	0.013 (2)	0.032 (2)	0.016 (2)	−0.0027 (17)	0.0036 (16)	−0.0062 (18)
O3	0.023 (2)	0.016 (2)	0.017 (2)	−0.0029 (16)	0.0072 (17)	−0.0033 (16)
O4	0.025 (2)	0.018 (2)	0.020 (2)	−0.0062 (17)	0.0118 (17)	−0.0028 (17)
O5	0.021 (2)	0.019 (2)	0.023 (2)	0.0084 (17)	0.0089 (17)	0.0085 (17)
O6	0.017 (2)	0.026 (2)	0.031 (2)	0.0070 (18)	0.0095 (18)	0.0138 (19)
O1W	0.015 (2)	0.053 (3)	0.023 (2)	0.010 (2)	0.0049 (18)	−0.005 (2)
O2W	0.029 (3)	0.021 (2)	0.035 (3)	−0.0021 (19)	0.001 (2)	0.013 (2)
O3W	0.029 (3)	0.050 (3)	0.038 (3)	−0.013 (2)	0.013 (2)	−0.017 (2)

Pr1—O5	2.448 (4)	C2—C2iii	1.555 (11)
Pr1—O2W	2.466 (4)	C3—O5	1.248 (7)
Pr1—O6i	2.472 (4)	C3—O6	1.258 (7)
Pr1—O2ii	2.490 (4)	C3—C3i	1.548 (11)
Pr1—O1W	2.500 (4)	O1—Pr1iv	2.609 (4)
Pr1—O3	2.504 (4)	O2—Pr1ii	2.490 (4)
Pr1—O4iii	2.541 (4)	O4—Pr1iii	2.541 (4)
Pr1—O1	2.586 (4)	O6—Pr1i	2.472 (4)
Pr1—O1iv	2.609 (4)	O1W—H1WA	0.8413
C1—O2	1.243 (7)	O1W—H1WB	0.8417
C1—O1	1.258 (7)	O2W—H2WA	0.8412
C1—C1ii	1.546 (11)	O2W—H2WB	0.8372
C2—O4	1.238 (7)	O3W—H3WA	0.8386
C2—O3	1.263 (7)	O3W—H3WB	0.8400
O5—Pr1—O2W	142.99 (15)	O6i—Pr1—O1iv	120.77 (14)
O5—Pr1—O6i	65.89 (14)	O2ii—Pr1—O1iv	121.99 (13)
O2W—Pr1—O6i	142.54 (15)	O1W—Pr1—O1iv	77.27 (13)
O5—Pr1—O2ii	131.79 (14)	O3—Pr1—O1iv	146.78 (13)
O2W—Pr1—O2ii	71.54 (15)	O4iii—Pr1—O1iv	122.88 (13)
O6i—Pr1—O2ii	71.37 (14)	O1—Pr1—O1iv	65.40 (14)
O5—Pr1—O1W	97.65 (15)	O2—C1—O1	126.7 (5)
O2W—Pr1—O1W	70.26 (16)	O2—C1—C1ii	116.0 (6)
O6i—Pr1—O1W	142.27 (16)	O1—C1—C1ii	117.3 (6)
O2ii—Pr1—O1W	130.26 (15)	O4—C2—O3	126.8 (5)
O5—Pr1—O3	133.93 (13)	O4—C2—C2iii	117.5 (6)
O2W—Pr1—O3	78.07 (15)	O3—C2—C2iii	115.7 (6)
O6i—Pr1—O3	92.40 (14)	O5—C3—O6	126.5 (5)
O2ii—Pr1—O3	67.24 (13)	O5—C3—C3i	117.1 (6)
O1W—Pr1—O3	74.66 (14)	O6—C3—C3i	116.4 (6)
O5—Pr1—O4iii	70.30 (13)	C1—O1—Pr1	118.7 (3)
O2W—Pr1—O4iii	132.32 (15)	C1—O1—Pr1iv	123.3 (3)
O6i—Pr1—O4iii	69.96 (15)	Pr1—O1—Pr1iv	114.60 (14)
O2ii—Pr1—O4iii	114.58 (14)	C1—O2—Pr1ii	123.5 (4)
O1W—Pr1—O4iii	72.53 (15)	C2—O3—Pr1	121.8 (4)
O3—Pr1—O4iii	64.03 (13)	C2—O4—Pr1iii	120.5 (4)
O5—Pr1—O1	85.86 (13)	C3—O5—Pr1	120.4 (4)
O2W—Pr1—O1	81.79 (14)	C3—O6—Pr1i	119.7 (4)
O6i—Pr1—O1	77.20 (14)	Pr1—O1W—H1WA	115.2
O2ii—Pr1—O1	63.42 (12)	Pr1—O1W—H1WB	132.7
O1W—Pr1—O1	137.77 (14)	H1WA—O1W—H1WB	106.2
O3—Pr1—O1	130.36 (13)	Pr1—O2W—H2WA	136.4
O4iii—Pr1—O1	145.06 (13)	Pr1—O2W—H2WB	113.6
O5—Pr1—O1iv	67.14 (13)	H2WA—O2W—H2WB	107.3
O2W—Pr1—O1iv	76.00 (14)	H3WA—O3W—H3WB	107.4
O2—C1—O1—Pr1	−172.7 (5)	C2iii—C2—O3—Pr1	6.3 (8)
C1ii—C1—O1—Pr1	8.0 (8)	O5—Pr1—O3—C2	1.9 (5)
O2—C1—O1—Pr1iv	29.2 (8)	O2W—Pr1—O3—C2	−156.5 (4)
C1ii—C1—O1—Pr1iv	−150.1 (5)	O6i—Pr1—O3—C2	60.1 (4)
O5—Pr1—O1—C1	133.4 (4)	O2ii—Pr1—O3—C2	128.7 (5)
O2W—Pr1—O1—C1	−81.6 (4)	O1W—Pr1—O3—C2	−83.9 (4)
O6i—Pr1—O1—C1	67.2 (4)	O4iii—Pr1—O3—C2	−6.2 (4)
O2ii—Pr1—O1—C1	−8.2 (4)	O1—Pr1—O3—C2	135.3 (4)
O1W—Pr1—O1—C1	−129.8 (4)	O1iv—Pr1—O3—C2	−117.2 (4)
O3—Pr1—O1—C1	−15.0 (5)	O3—C2—O4—Pr1iii	−174.2 (5)
O4iii—Pr1—O1—C1	87.3 (4)	C2iii—C2—O4—Pr1iii	4.8 (9)
O1iv—Pr1—O1—C1	−159.9 (5)	O6—C3—O5—Pr1	−174.3 (5)
O5—Pr1—O1—Pr1iv	−66.72 (16)	C3i—C3—O5—Pr1	6.5 (8)
O2W—Pr1—O1—Pr1iv	78.30 (17)	O2W—Pr1—O5—C3	−154.9 (4)
O6i—Pr1—O1—Pr1iv	−132.92 (18)	O6i—Pr1—O5—C3	−6.5 (4)
O2ii—Pr1—O1—Pr1iv	151.7 (2)	O2ii—Pr1—O5—C3	−36.2 (5)
O1W—Pr1—O1—Pr1iv	30.1 (3)	O1W—Pr1—O5—C3	138.0 (4)
O3—Pr1—O1—Pr1iv	144.93 (15)	O3—Pr1—O5—C3	61.9 (5)
O4iii—Pr1—O1—Pr1iv	−112.8 (2)	O4iii—Pr1—O5—C3	69.7 (4)
O1iv—Pr1—O1—Pr1iv	0.0	O1—Pr1—O5—C3	−84.4 (4)
O1—C1—O2—Pr1ii	−171.6 (4)	O1iv—Pr1—O5—C3	−149.4 (4)
C1ii—C1—O2—Pr1ii	7.8 (9)	O5—C3—O6—Pr1i	−173.9 (4)
O4—C2—O3—Pr1	−174.7 (5)	C3i—C3—O6—Pr1i	5.3 (8)

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H2WB···O1W	0.84	2.55	2.858 (7)	103
O1W—H1WA···O2iv	0.84	1.96	2.694 (6)	146
O1W—H1WA···O3v	0.84	2.60	3.235 (6)	133
O1W—H1WB···O3Wvi	0.84	2.00	2.833 (6)	169
O2W—H2WA···O3Wvii	0.84	1.98	2.807 (7)	166
O2W—H2WB···O3viii	0.84	2.20	2.919 (6)	144
O3W—H3WA···O6ix	0.84	2.08	2.829 (7)	149
O3W—H3WB···O4iii	0.84	2.03	2.833 (6)	159

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2W—H2WB⋯O1W	0.84	2.55	2.858 (7)	103
O1W—H1WA⋯O2i	0.84	1.96	2.694 (6)	146
O1W—H1WA⋯O3ii	0.84	2.60	3.235 (6)	133
O1W—H1WB⋯O3Wiii	0.84	2.00	2.833 (6)	169
O2W—H2WA⋯O3Wiv	0.84	1.98	2.807 (7)	166
O2W—H2WB⋯O3v	0.84	2.20	2.919 (6)	144
O3W—H3WA⋯O6vi	0.84	2.08	2.829 (7)	149
O3W—H3WB⋯O4vii	0.84	2.03	2.833 (6)	159

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .