Poly[[diaqua­hemi-μ4-oxalato-μ2-oxalato-praseodymium(III)] monohydrate]

Yang, T.-H.; Chen, Q.; Zhuang, W.; Wang, Z.; Yue, B.-Y.

doi:10.1107/S1600536809033947

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 9| September 2009| Pages m1152-m1153

doi:10.1107/S1600536809033947

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Poly[[diaquahemi-μ₄-oxalato-μ₂-oxalato-praseodymium(III)] monohydrate]

Ting-Hai Yang,^a ^* Qiang Chen,^a Wei Zhuang,^a Zhe Wang ^a and Bang-Yi Yue ^a

^aHigh-Tech Institute of Nangjing University, Changzhou 213164, People's Republic of China
^*Correspondence e-mail: tinghaiyang@gmail.com

(Received 9 August 2009; accepted 25 August 2009; online 29 August 2009)

In the title complex, {[Pr(C₂O₄)_1.5(H₂O)₂]·H₂O}_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 tetradentate oxalate ligands forms a three-dimensional structure. The compound crystallized as a monohydrate, the water molecule 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_r = 326.99
Triclinic, $[P \overline 1]$
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[F² > 2σ(F²)] = 0.029
wR(F²) = 0.075
S = 1.00
1521 reflections
118 parameters
H-atom parameters constrained
Δρ_max = 0.80 e Å⁻³
Δρ_min = −1.50 e Å⁻³

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⋯O3W^iv	0.84	1.98	2.807 (7)	166
O2W—H2WB⋯O3^v	0.84	2.20	2.919 (6)	144
O3W—H3WA⋯O6^vi	0.84	2.08	2.829 (7)	149
O3W—H3WB⋯O4^vii	0.84	2.03	2.833 (6)	159
Symmetry codes: (i) -x+2, -y+2, -z+1; (ii) x-1, y, z; (iii) -x+1, -y+1, -z; (iv) x+1, y+1, z; (v) -x+2, -y+2, -z; (vi) -x+1, -y+1, -z+1; (vii) -x+2, -y+1, -z.

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).

Supporting information

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

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

checkCIF report

Comment top

In the last decade considerable attention has been afforded to the structures and properties of lanthanide oxalates due to their ability to act as precursors of lanthanide oxides. Some single crystals of lanthanide oxalates, such as[Ln(C₂O₄)₃(H₂O)₄].(H₂O) (Ln = Sc or Yb), [Ln₂(C₂O₄)₃(H₂O)₆].4H₂O (Ln = La, Ce, Pr or Nd) and [Nd₂(C₂O₄)₃(H₂O)₆] have been obtained either in silica gel (Ollendorff & Weigel, 1969), by hydrothermal reaction (Michaelides et al., 1988) or by other methods (Hansson, 1970, 1972, 1973a,b; Unaleroglu et al., 1997; Trollet et al., 1998; Trombe, 2003). Crystals of [Ln(C₂O₄)(HC₂O₄)].4H₂O (Ln = Er or Tm) were prepared by saturating a boiling solution of oxalic acid in 3 M H₂SO₄ with the lanthanide oxide and then slowly cooling to 273 K (Steinfink & Brunton, 1970). However, a few praseodymium oxalate complex has been reported. The present paper is concerned with a new crystal structure of praseodymium oxalate complex with a three-dimensional network structure.

The asymmetric unit of the title compound, [Pr(C₂O₄)_1.5(H₂O)₂].(H₂O), (I), is shown in Fig. 1. The Pr atom lies on an inversion centre and is coordinated by seven O atoms [O1, O1^iv, O2ⁱⁱ, O3, O4ⁱⁱⁱ, O5 and O6ⁱ] from four oxlate ligands, and two O atoms from two aqua ligands, thereby forming a slightly distorted PrO₉ polyhedral coordination geometry. The Pr—O bond distances range from 2.451 (4) Å to 2.608 (3) Å, in agreement with those in compounds (Trombe et al. (2004); Barrett Adams et al. (1998)).

In the complex, the equivalent Pr atom are connected is coordinated by seven O atoms from four oxalate ligands and two O atoms from water ligands. Further Pr–O coordination from the tetradentate oxalate ligands forms a three-dimensional structure (Fig.2). The compound crystallized as a monohydrate; this water molecule occupies space in small voids and is 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 top

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 top

All solvents and chemicals were of analytical grade and were used without further purification. Pr(NO₃)₃^.6H₂O (0.05 mmol, 0.023 g), Na₂C₂O₄(0.075 mmol, 0.011 g), and deionized water (10 ml) were mixed together. The mixture was sealed in a Teflon-line autoclave and then heated at 443 K for 5 d under autogenous pressure and then cooled to room temperature. Green crystals were obtained.

Computing details top

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

Figures top

	Fig. 1. Molecular structure of (I), showing 50% probability displacement ellipsoids. [symmetry codes:(i) -x + 2,-y + 1,-z + 1; (ii) -x + 3,-y + 2,-z + 1; (iii) -x + 2,-y + 1,-z; (iv) -x + 2,-y + 2,-z + 1.
	Fig. 2. The unit cell packing diagram of (I).

Poly[[diaquahemi-µ₄-oxalato-µ₂-oxalato-praseodymium(III)] monohydrate] top

Crystal data top

[Pr(C₂O₄)_1.5(H₂O)₂]·H₂O	Z = 2
M_r = 326.99	F(000) = 310
Triclinic, P1	D_x = 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

Data collection top

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

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.075	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.049P)² + 1.09P] where P = (F_o² + 2F_c²)/3
1521 reflections	(Δ/σ)_max = 0.001
118 parameters	Δρ_max = 0.80 e Å⁻³
0 restraints	Δρ_min = −1.50 e Å⁻³

Crystal data top

[Pr(C₂O₄)_1.5(H₂O)₂]·H₂O	γ = 96.734 (4)°
M_r = 326.99	V = 396.58 (14) Å³
Triclinic, P1	Z = 2
a = 6.0367 (12) Å	Mo Kα radiation
b = 7.6222 (15) Å	µ = 6.17 mm⁻¹
c = 8.9353 (18) Å	T = 273 K
α = 98.330 (4)°	0.18 × 0.16 × 0.10 mm
β = 99.814 (3)°

Data collection top

Bruker SMART APEX CCD diffractometer	1521 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	1450 reflections with I > 2σ(I)
T_min = 0.341, T_max = 0.542	R_int = 0.020
2140 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	0 restraints
wR(F²) = 0.075	H-atom parameters constrained
S = 1.00	Δρ_max = 0.80 e Å⁻³
1521 reflections	Δρ_min = −1.50 e Å⁻³
118 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	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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—Pr1^iv	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—O1^iv	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—O1^iv	120.77 (14)
O5—Pr1—O6ⁱ	65.89 (14)	O2ⁱⁱ—Pr1—O1^iv	121.99 (13)
O2W—Pr1—O6ⁱ	142.54 (15)	O1W—Pr1—O1^iv	77.27 (13)
O5—Pr1—O2ⁱⁱ	131.79 (14)	O3—Pr1—O1^iv	146.78 (13)
O2W—Pr1—O2ⁱⁱ	71.54 (15)	O4ⁱⁱⁱ—Pr1—O1^iv	122.88 (13)
O6ⁱ—Pr1—O2ⁱⁱ	71.37 (14)	O1—Pr1—O1^iv	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—Pr1^iv	123.3 (3)
O6ⁱ—Pr1—O4ⁱⁱⁱ	69.96 (15)	Pr1—O1—Pr1^iv	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—O1^iv	67.14 (13)	H2WA—O2W—H2WB	107.3
O2W—Pr1—O1^iv	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—Pr1^iv	29.2 (8)	O2W—Pr1—O3—C2	−156.5 (4)
C1ⁱⁱ—C1—O1—Pr1^iv	−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)	O1^iv—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)
O1^iv—Pr1—O1—C1	−159.9 (5)	O6—C3—O5—Pr1	−174.3 (5)
O5—Pr1—O1—Pr1^iv	−66.72 (16)	C3ⁱ—C3—O5—Pr1	6.5 (8)
O2W—Pr1—O1—Pr1^iv	78.30 (17)	O2W—Pr1—O5—C3	−154.9 (4)
O6ⁱ—Pr1—O1—Pr1^iv	−132.92 (18)	O6ⁱ—Pr1—O5—C3	−6.5 (4)
O2ⁱⁱ—Pr1—O1—Pr1^iv	151.7 (2)	O2ⁱⁱ—Pr1—O5—C3	−36.2 (5)
O1W—Pr1—O1—Pr1^iv	30.1 (3)	O1W—Pr1—O5—C3	138.0 (4)
O3—Pr1—O1—Pr1^iv	144.93 (15)	O3—Pr1—O5—C3	61.9 (5)
O4ⁱⁱⁱ—Pr1—O1—Pr1^iv	−112.8 (2)	O4ⁱⁱⁱ—Pr1—O5—C3	69.7 (4)
O1^iv—Pr1—O1—Pr1^iv	0.0	O1—Pr1—O5—C3	−84.4 (4)
O1—C1—O2—Pr1ⁱⁱ	−171.6 (4)	O1^iv—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)

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+3, −y+2, −z+1; (iii) −x+2, −y+1, −z; (iv) −x+2, −y+2, −z+1.

Hydrogen-bond geometry (Å, º) top

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···O2^iv	0.84	1.96	2.694 (6)	146
O1W—H1WA···O3^v	0.84	2.60	3.235 (6)	133
O1W—H1WB···O3W^vi	0.84	2.00	2.833 (6)	169
O2W—H2WA···O3W^vii	0.84	1.98	2.807 (7)	166
O2W—H2WB···O3^viii	0.84	2.20	2.919 (6)	144
O3W—H3WA···O6^ix	0.84	2.08	2.829 (7)	149
O3W—H3WB···O4ⁱⁱⁱ	0.84	2.03	2.833 (6)	159

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

Experimental details

Crystal data
Chemical formula	[Pr(C₂O₄)_1.5(H₂O)₂]·H₂O
M_r	326.99
Crystal system, space group	Triclinic, P1
Temperature (K)	273
a, b, c (Å)	6.0367 (12), 7.6222 (15), 8.9353 (18)
α, β, γ (°)	98.330 (4), 99.814 (3), 96.734 (4)
V (Å³)	396.58 (14)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	6.17
Crystal size (mm)	0.18 × 0.16 × 0.10

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.341, 0.542
No. of measured, independent and observed [I > 2σ(I)] reflections	2140, 1521, 1450
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.075, 1.00
No. of reflections	1521
No. of parameters	118
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.80, −1.50

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H2WB···O1W	0.84	2.55	2.858 (7)	103.3
O1W—H1WA···O2ⁱ	0.84	1.96	2.694 (6)	145.6
O1W—H1WA···O3ⁱⁱ	0.84	2.60	3.235 (6)	133.4
O1W—H1WB···O3Wⁱⁱⁱ	0.84	2.00	2.833 (6)	168.6
O2W—H2WA···O3W^iv	0.84	1.98	2.807 (7)	166.3
O2W—H2WB···O3^v	0.84	2.20	2.919 (6)	144.3
O3W—H3WA···O6^vi	0.84	2.08	2.829 (7)	148.8
O3W—H3WB···O4^vii	0.84	2.03	2.833 (6)	158.6

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

Acknowledgements

The authors acknowledge the High-Tech Research Institute of Nanjing University for supporting this work.

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