Poly[[triaqua­tri-μ5-tartrato-dilanthanum(III)] dihydrate]

Shi-Zhu, L.

doi:10.1107/S160053680801756X

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 7| July 2008| Page m933

doi:10.1107/S160053680801756X

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Poly[[triaquatri-μ₅-tartrato-dilanthanum(III)] dihydrate]

Liu Shi-Zhu ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China
^*Correspondence e-mail: liushizhu521@126.com

(Received 18 April 2008; accepted 11 June 2008; online 19 June 2008)

In the title polymer, {[La₂(C₄H₄O₆)₃(H₂O)₃]·2H₂O}_n, two symmetry-independent La^III ions are nine-coordinated and display a distorted monocapped square-antiprismatic geometry. One is coordinated by seven O atoms from four tartrate ligands and two water molecules, the other by eight O atoms from five tartrate ligands and one water molecule. The three tartrate ligands in the asymmetric unit act identically as μ₅-ligands, which link lanthanum centres to form a three-dimensional coordination framework. An extensive network of hydrogen bonds is observed in the crystal structure, involving two uncoordinated water molecules, one of which is disordered over two positions, with occupancies of 0.550 (13) and 0.450 (13).

Related literature

For related literature, see: Yaghi et al. (1998 , 2003 ); Serre et al. (2004 ); James et al. (2003 ).

Experimental

Crystal data

[La₂(C₄H₄O₆)₃(H₂O)₃]·2H₂O
M_r = 812.12
Monoclinic, P 2₁ /c
a = 12.6271 (2) Å
b = 12.9273 (2) Å
c = 16.6556 (3) Å
β = 127.801 (1)°
V = 2148.22 (6) Å³
Z = 4
Mo Kα radiation
μ = 4.04 mm⁻¹
T = 296 (2) K
0.25 × 0.21 × 0.18 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.372, T_max = 0.480
19115 measured reflections
3771 independent reflections
3226 reflections with I > 2σ(I)
R_int = 0.047

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.057
S = 1.05
3771 reflections
344 parameters
H-atom parameters constrained
Δρ_max = 0.87 e Å⁻³
Δρ_min = −0.65 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3A⋯O8ⁱ	0.82	1.87	2.677 (4)	169
O4—H4⋯O18ⁱⁱ	0.82	1.80	2.619 (4)	174
O9—H9⋯O16	0.82	2.46	3.177 (5)	147
O10—H10A⋯O8ⁱⁱⁱ	0.82	1.94	2.745 (4)	167
O15—H15⋯O2ⁱ	0.82	1.82	2.632 (4)	175
O16—H16⋯O4WA	0.82	1.89	2.667 (9)	158
O16—H16⋯O4WB	0.82	1.94	2.708 (9)	157
Symmetry codes: (i) $[-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) -x, -y+2, -z+2.

Data collection: SMART (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680801756X/bh2174sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680801756X/bh2174Isup2.hkl

checkCIF report

Comment top

The use of multifunctional organic linker molecules to polymerize metal centers into open-framework materials has led to the development of a rich field of chemistry (Yaghi et al., 1998, 2003; Serre et al., 2004; James, 2003) owing to the potential applications of these materials in catalysis, separation, gas storage and molecular recognition. Among such novel open-framework materials, lanthanide oxalates are particularly noteworthy. The wide variety of coordination modes of the tartarate anion permits the use of metal-tartarate units as excellent building blocks to construct a great diversity of frameworks ranging from discrete oligomeric entities to one-, two- and three-dimensional networks. Recently, we obtained the title La^III polymer, (I), and its crystal structure is reported here.

In the asymmetric unit of (I), two symmetry independent La^III ions are nine-coordinated and display a distorted monocapped square antiprism geometry. One is coordinated by seven O atoms from four tartarate ligands and two coordinated water molecules, the other is defined by eight O atoms from five tartarate ligands and one coordinated water molecule (Fig. 1). All three unique tartarate ligands only act as one type of coordination mode, which link lanthanum centres to form a three-dimensional coordination framework (Fig. 2). The shortest La···La separations in the solid are 6.207 (2), 6.520 (3) and 6.535 (2) Å. The voids between the individual metal complex units are filled with classical hydrogen bonded (Table 1) interstitial disordered water molecules.

Related literature top

For related literature, see: Yaghi et al. (1998, 2003); Serre et al. (2004); James et al. (2003).

Experimental top

A mixture of La₂O₃ (0.5 mmol), tartaric acid (1.5 mmol) and H₂O (10 ml) in the presence of HClO₄ (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 to 433 K and maintained at this temperature for 7 days, and then cooled to room temperature at 5 K.h^-1. The crystals were obtained in ca. 46% yield based on La.

Computing details top

Data collection: SMART (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

	Fig. 1. The structure of (I), showing the atomic numbering scheme. Non-H atoms are shown with 30% probability displacement ellipsoids.
	Fig. 2. A packing view of (I), showing the inter and intramolecular hydrogen bonds.

Poly[[triaquatri-µ₅-tartrato-dilanthanum(III)] dihydrate] top

Crystal data top

[La₂(C₄H₄O₆)₃(H₂O)₃]·2H₂O	F(000) = 1568
M_r = 812.12	D_x = 2.511 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 15678 reflections
a = 12.6271 (2) Å	θ = 1.4–28.0°
b = 12.9273 (2) Å	µ = 4.04 mm⁻¹
c = 16.6556 (3) Å	T = 296 K
β = 127.801 (1)°	Block, colourless
V = 2148.22 (6) Å³	0.25 × 0.21 × 0.18 mm
Z = 4

Data collection top

Bruker APEXII area-detector diffractometer	3771 independent reflections
Radiation source: fine-focus sealed tube	3226 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.047
ϕ and ω scans	θ_max = 25.2°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→15
T_min = 0.372, T_max = 0.480	k = −15→14
19115 measured reflections	l = −19→19

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.057	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0203P)² + 3.8165P] where P = (F_o² + 2F_c²)/3
3771 reflections	(Δ/σ)_max = 0.001
344 parameters	Δρ_max = 0.87 e Å⁻³
0 restraints	Δρ_min = −0.65 e Å⁻³

Crystal data top

[La₂(C₄H₄O₆)₃(H₂O)₃]·2H₂O	V = 2148.22 (6) Å³
M_r = 812.12	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 12.6271 (2) Å	µ = 4.04 mm⁻¹
b = 12.9273 (2) Å	T = 296 K
c = 16.6556 (3) Å	0.25 × 0.21 × 0.18 mm
β = 127.801 (1)°

Data collection top

Bruker APEXII area-detector diffractometer	3771 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3226 reflections with I > 2σ(I)
T_min = 0.372, T_max = 0.480	R_int = 0.047
19115 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.05	Δρ_max = 0.87 e Å⁻³
3771 reflections	Δρ_min = −0.65 e Å⁻³
344 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1	−0.0900 (4)	0.9566 (4)	0.5698 (3)	0.0155 (10)
C2	−0.1083 (4)	0.8523 (4)	0.5199 (3)	0.0177 (10)
H2	−0.0295	0.8416	0.5224	0.021*
C3	−0.2308 (4)	0.8455 (4)	0.4086 (3)	0.0176 (10)
H3	−0.2432	0.9136	0.3782	0.021*
C4	−0.2140 (4)	0.7672 (4)	0.3482 (3)	0.0174 (10)
C5	0.0357 (5)	1.0235 (4)	0.9197 (3)	0.0183 (10)
C6	0.1840 (4)	0.9984 (4)	0.9767 (3)	0.0184 (10)
H6	0.2249	1.0587	0.9697	0.022*
C7	0.2635 (4)	0.9782 (3)	1.0918 (3)	0.0165 (10)
H7	0.2333	1.0265	1.1193	0.020*
C8	0.4144 (4)	0.9950 (4)	1.1463 (3)	0.0172 (10)
C9	0.2706 (4)	0.7265 (4)	0.8239 (3)	0.0171 (10)
C10	0.2636 (4)	0.6536 (4)	0.8918 (3)	0.0152 (10)
H10	0.2424	0.5841	0.8623	0.018*
C11	0.3977 (4)	0.6497 (3)	0.9974 (3)	0.0150 (10)
H11	0.4687	0.6446	0.9899	0.018*
C12	0.4096 (4)	0.5570 (3)	1.0589 (3)	0.0137 (10)
La1	−0.02226 (2)	0.81431 (2)	0.77118 (2)	0.01422 (8)
La2	−0.54797 (2)	0.73846 (2)	0.22545 (2)	0.01381 (8)
O1	−0.0471 (3)	0.9566 (3)	0.6612 (2)	0.0248 (8)
O2	−0.1144 (3)	1.0376 (2)	0.5208 (2)	0.0207 (7)
O3	−0.1053 (3)	0.7743 (2)	0.5816 (2)	0.0221 (7)
H3A	−0.0661	0.7267	0.5776	0.033*
O4	−0.3519 (3)	0.8206 (2)	0.3936 (2)	0.0184 (7)
H4	−0.3650	0.8645	0.4222	0.028*
O5	−0.3178 (3)	0.7172 (2)	0.2791 (2)	0.0221 (8)
O6	−0.1040 (3)	0.7609 (3)	0.3649 (2)	0.0232 (8)
O7	−0.0495 (3)	0.9637 (3)	0.8484 (2)	0.0255 (8)
O8	0.0074 (3)	1.1045 (2)	0.9438 (3)	0.0226 (8)
O9	0.1947 (3)	0.9140 (3)	0.9266 (3)	0.0294 (8)
H9	0.2372	0.8703	0.9710	0.044*
O10	0.2457 (3)	0.8752 (2)	1.1112 (2)	0.0237 (8)
H10A	0.1714	0.8711	1.0973	0.036*
O11	0.4892 (3)	0.9167 (2)	1.1844 (2)	0.0214 (7)
O12	0.4517 (3)	1.0853 (2)	1.1460 (2)	0.0213 (7)
O13	0.1759 (3)	0.7910 (3)	0.7713 (3)	0.0256 (8)
O14	0.3687 (3)	0.7181 (3)	0.8235 (2)	0.0235 (8)
O15	0.1587 (3)	0.6864 (2)	0.8953 (2)	0.0197 (7)
H15	0.1438	0.6427	0.9228	0.030*
O16	0.4191 (3)	0.7419 (2)	1.0529 (2)	0.0212 (7)
H16	0.4526	0.7832	1.0370	0.032*
O17	0.4440 (3)	0.5724 (2)	1.1455 (2)	0.0238 (8)
O18	0.3836 (3)	0.4696 (2)	1.0164 (2)	0.0194 (7)
O1W	−0.2694 (3)	0.8479 (3)	0.6519 (3)	0.0322 (9)
H1W	−0.3029	0.8425	0.6809	0.048*
H2W	−0.3074	0.8967	0.6129	0.048*
O2W	−0.1015 (3)	0.6276 (3)	0.7134 (2)	0.0307 (8)
H4W	−0.1775	0.6138	0.6932	0.046*
H3W	−0.0543	0.5815	0.7543	0.046*
O3W	−0.7660 (3)	0.6479 (3)	0.1489 (3)	0.0363 (10)
H6W	−0.8076	0.6421	0.1715	0.054*
H5W	−0.8025	0.6085	0.1004	0.054*
O5W	0.6940 (6)	0.5141 (5)	0.6746 (7)	0.139 (3)
H10W	0.6504	0.5618	0.6312	0.208*
H9W	0.6446	0.4937	0.6900	0.208*
O4WA	0.4665 (13)	0.9039 (8)	0.9799 (8)	0.056 (5)	0.450 (13)
H4WA	0.4304	0.8494	0.9818	0.084*	0.450 (13)
H4WB	0.4877	0.8889	0.9417	0.084*	0.450 (13)
O4WB	0.5902 (11)	0.8436 (8)	1.0338 (7)	0.072 (4)	0.550 (13)
H4WC	0.5854	0.8295	0.9818	0.108*	0.550 (13)
H4WD	0.5400	0.8961	1.0169	0.108*	0.550 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.008 (2)	0.020 (3)	0.017 (3)	−0.0002 (18)	0.008 (2)	0.000 (2)
C2	0.018 (2)	0.019 (3)	0.019 (2)	−0.0007 (19)	0.013 (2)	0.001 (2)
C3	0.014 (2)	0.018 (3)	0.019 (3)	−0.0001 (18)	0.010 (2)	−0.001 (2)
C4	0.018 (3)	0.020 (3)	0.016 (2)	−0.0001 (19)	0.011 (2)	0.002 (2)
C5	0.026 (3)	0.015 (3)	0.017 (2)	0.000 (2)	0.015 (2)	0.005 (2)
C6	0.023 (2)	0.016 (3)	0.018 (2)	−0.0038 (19)	0.013 (2)	−0.003 (2)
C7	0.025 (3)	0.010 (2)	0.019 (2)	0.0028 (19)	0.015 (2)	0.003 (2)
C8	0.025 (3)	0.015 (3)	0.013 (2)	0.000 (2)	0.012 (2)	−0.002 (2)
C9	0.019 (3)	0.020 (3)	0.013 (2)	−0.0007 (19)	0.010 (2)	−0.001 (2)
C10	0.015 (2)	0.015 (3)	0.020 (2)	0.0020 (18)	0.013 (2)	0.0033 (19)
C11	0.020 (2)	0.014 (2)	0.016 (2)	0.0004 (18)	0.013 (2)	−0.0021 (19)
C12	0.010 (2)	0.016 (3)	0.018 (2)	0.0019 (18)	0.0102 (19)	−0.002 (2)
La1	0.01520 (14)	0.01340 (16)	0.01582 (14)	0.00137 (10)	0.01041 (12)	0.00210 (11)
La2	0.01507 (14)	0.01329 (15)	0.01485 (14)	−0.00060 (10)	0.01008 (12)	−0.00145 (11)
O1	0.035 (2)	0.024 (2)	0.0153 (18)	−0.0022 (15)	0.0153 (16)	−0.0006 (15)
O2	0.0321 (19)	0.0115 (18)	0.0204 (18)	0.0018 (14)	0.0170 (16)	0.0048 (14)
O3	0.0296 (19)	0.0142 (18)	0.0211 (18)	0.0049 (14)	0.0148 (16)	0.0042 (14)
O4	0.0148 (16)	0.0217 (19)	0.0211 (18)	−0.0020 (13)	0.0123 (14)	−0.0078 (14)
O5	0.0188 (18)	0.027 (2)	0.0230 (18)	−0.0058 (14)	0.0140 (15)	−0.0108 (15)
O6	0.0202 (18)	0.031 (2)	0.0234 (19)	−0.0026 (14)	0.0158 (15)	−0.0061 (15)
O7	0.0218 (18)	0.025 (2)	0.0244 (19)	−0.0017 (14)	0.0116 (16)	−0.0084 (16)
O8	0.0267 (18)	0.0119 (18)	0.034 (2)	−0.0001 (14)	0.0208 (16)	−0.0045 (15)
O9	0.0268 (19)	0.033 (2)	0.0237 (19)	0.0059 (15)	0.0129 (16)	−0.0087 (16)
O10	0.0199 (17)	0.0202 (19)	0.033 (2)	0.0000 (14)	0.0170 (16)	0.0073 (16)
O11	0.0196 (17)	0.0160 (18)	0.0259 (18)	−0.0002 (14)	0.0126 (15)	0.0017 (15)
O12	0.0273 (18)	0.0150 (19)	0.0174 (17)	−0.0051 (14)	0.0115 (15)	−0.0027 (14)
O13	0.0247 (19)	0.031 (2)	0.028 (2)	0.0126 (15)	0.0197 (16)	0.0147 (16)
O14	0.0207 (18)	0.033 (2)	0.0245 (19)	0.0064 (15)	0.0181 (16)	0.0072 (16)
O15	0.0174 (17)	0.0201 (19)	0.0271 (19)	0.0030 (13)	0.0164 (15)	0.0106 (15)
O16	0.0309 (19)	0.0135 (18)	0.0235 (18)	−0.0071 (14)	0.0189 (16)	−0.0049 (14)
O17	0.037 (2)	0.0175 (19)	0.0171 (18)	0.0001 (15)	0.0166 (16)	0.0003 (15)
O18	0.0267 (18)	0.0165 (19)	0.0195 (17)	−0.0007 (14)	0.0164 (15)	−0.0011 (14)
O1W	0.0219 (19)	0.051 (2)	0.028 (2)	0.0068 (16)	0.0173 (16)	0.0164 (18)
O2W	0.035 (2)	0.022 (2)	0.0256 (19)	−0.0047 (16)	0.0143 (17)	−0.0026 (16)
O3W	0.027 (2)	0.052 (3)	0.039 (2)	−0.0224 (17)	0.0246 (18)	−0.0308 (19)
O5W	0.117 (5)	0.100 (5)	0.255 (10)	0.012 (4)	0.142 (6)	0.041 (6)
O4WA	0.103 (11)	0.045 (7)	0.053 (7)	−0.036 (7)	0.064 (8)	−0.019 (5)
O4WB	0.090 (9)	0.075 (8)	0.056 (6)	−0.033 (7)	0.047 (6)	0.005 (5)

Geometric parameters (Å, º) top

C1—O2	1.245 (5)	La1—O2W	2.563 (3)
C1—O1	1.266 (5)	La1—O9	2.679 (3)
C1—C2	1.525 (6)	La1—O3	2.698 (3)
C2—O3	1.424 (5)	La2—O5	2.478 (3)
C2—C3	1.524 (6)	La2—O14ⁱⁱ	2.488 (3)
C2—H2	0.9800	La2—O17ⁱⁱⁱ	2.496 (3)
C3—O4	1.427 (5)	La2—O3W	2.505 (3)
C3—C4	1.531 (6)	La2—O11ⁱⁱⁱ	2.529 (3)
C3—H3	0.9800	La2—O4	2.569 (3)
C4—O6	1.241 (5)	La2—O12^iv	2.606 (3)
C4—O5	1.269 (5)	La2—O16ⁱⁱⁱ	2.641 (3)
C5—O8	1.249 (5)	La2—O10ⁱⁱⁱ	2.730 (3)
C5—O7	1.265 (5)	O3—H3A	0.8187
C5—C6	1.527 (6)	O4—H4	0.8211
C6—O9	1.430 (5)	O6—La1^v	2.534 (3)
C6—C7	1.547 (6)	O9—H9	0.8167
C6—H6	0.9800	O10—La2^vi	2.730 (3)
C7—O10	1.420 (5)	O10—H10A	0.8180
C7—C8	1.543 (6)	O11—La2^vi	2.529 (3)
C7—H7	0.9800	O12—La2^vii	2.606 (3)
C8—O11	1.258 (5)	O14—La2^viii	2.488 (3)
C8—O12	1.260 (5)	O15—H15	0.8188
C9—O14	1.249 (5)	O16—La2^vi	2.641 (3)
C9—O13	1.268 (5)	O16—H16	0.8184
C9—C10	1.516 (6)	O17—La2^vi	2.496 (3)
C10—O15	1.426 (5)	O1W—H1W	0.8167
C10—C11	1.520 (6)	O1W—H2W	0.8174
C10—H10	0.9800	O2W—H4W	0.8180
C11—O16	1.429 (5)	O2W—H3W	0.8220
C11—C12	1.523 (6)	O3W—H6W	0.8155
C11—H11	0.9800	O3W—H5W	0.8177
C12—O17	1.241 (5)	O5W—H10W	0.8468
C12—O18	1.265 (5)	O5W—H9W	0.8478
La1—O7	2.458 (3)	O4WA—H4WA	0.8498
La1—O1	2.476 (3)	O4WA—H4WB	0.8499
La1—O1W	2.505 (3)	O4WA—H4WD	0.7409
La1—O13	2.519 (3)	O4WB—H4WC	0.8505
La1—O6ⁱ	2.534 (3)	O4WB—H4WD	0.8503
La1—O15	2.537 (3)

O2—C1—O1	122.7 (4)	O1—La1—O3	59.64 (10)
O2—C1—C2	119.5 (4)	O1W—La1—O3	72.73 (10)
O1—C1—C2	117.8 (4)	O13—La1—O3	69.61 (10)
O3—C2—C3	113.3 (4)	O6ⁱ—La1—O3	129.38 (10)
O3—C2—C1	107.7 (4)	O15—La1—O3	109.80 (10)
C3—C2—C1	114.6 (4)	O2W—La1—O3	66.30 (10)
O3—C2—H2	106.9	O9—La1—O3	131.08 (10)
C3—C2—H2	106.9	O5—La2—O14ⁱⁱ	131.51 (10)
C1—C2—H2	106.9	O5—La2—O17ⁱⁱⁱ	75.65 (10)
O4—C3—C2	113.9 (4)	O14ⁱⁱ—La2—O17ⁱⁱⁱ	130.47 (10)
O4—C3—C4	107.5 (4)	O5—La2—O3W	144.32 (11)
C2—C3—C4	113.1 (4)	O14ⁱⁱ—La2—O3W	70.40 (10)
O4—C3—H3	107.3	O17ⁱⁱⁱ—La2—O3W	69.74 (11)
C2—C3—H3	107.3	O5—La2—O11ⁱⁱⁱ	80.05 (10)
C4—C3—H3	107.3	O14ⁱⁱ—La2—O11ⁱⁱⁱ	101.25 (11)
O6—C4—O5	124.2 (4)	O17ⁱⁱⁱ—La2—O11ⁱⁱⁱ	126.38 (10)
O6—C4—C3	118.9 (4)	O3W—La2—O11ⁱⁱⁱ	128.09 (11)
O5—C4—C3	116.8 (4)	O5—La2—O4	61.24 (9)
O8—C5—O7	124.6 (4)	O14ⁱⁱ—La2—O4	72.79 (10)
O8—C5—C6	117.5 (4)	O17ⁱⁱⁱ—La2—O4	129.34 (10)
O7—C5—C6	117.8 (4)	O3W—La2—O4	140.56 (10)
O9—C6—C5	108.5 (4)	O11ⁱⁱⁱ—La2—O4	72.77 (10)
O9—C6—C7	111.8 (4)	O5—La2—O12^iv	76.47 (10)
C5—C6—C7	115.0 (4)	O14ⁱⁱ—La2—O12^iv	78.72 (10)
O9—C6—H6	107.0	O17ⁱⁱⁱ—La2—O12^iv	68.33 (10)
C5—C6—H6	107.0	O3W—La2—O12^iv	82.92 (11)
C7—C6—H6	107.0	O11ⁱⁱⁱ—La2—O12^iv	147.59 (10)
O10—C7—C8	108.0 (3)	O4—La2—O12^iv	76.44 (10)
O10—C7—C6	111.6 (4)	O5—La2—O16ⁱⁱⁱ	76.20 (10)
C8—C7—C6	109.6 (3)	O14ⁱⁱ—La2—O16ⁱⁱⁱ	149.60 (10)
O10—C7—H7	109.2	O17ⁱⁱⁱ—La2—O16ⁱⁱⁱ	60.38 (10)
C8—C7—H7	109.2	O3W—La2—O16ⁱⁱⁱ	93.63 (10)
C6—C7—H7	109.2	O11ⁱⁱⁱ—La2—O16ⁱⁱⁱ	67.75 (10)
O11—C8—O12	125.4 (4)	O4—La2—O16ⁱⁱⁱ	125.67 (9)
O11—C8—C7	117.3 (4)	O12^iv—La2—O16ⁱⁱⁱ	126.16 (9)
O12—C8—C7	117.2 (4)	O5—La2—O10ⁱⁱⁱ	136.93 (10)
O14—C9—O13	124.9 (4)	O14ⁱⁱ—La2—O10ⁱⁱⁱ	72.81 (10)
O14—C9—C10	117.5 (4)	O17ⁱⁱⁱ—La2—O10ⁱⁱⁱ	118.40 (10)
O13—C9—C10	117.6 (4)	O3W—La2—O10ⁱⁱⁱ	70.51 (11)
O15—C10—C9	109.0 (3)	O11ⁱⁱⁱ—La2—O10ⁱⁱⁱ	58.50 (9)
O15—C10—C11	111.5 (4)	O4—La2—O10ⁱⁱⁱ	111.26 (10)
C9—C10—C11	110.6 (4)	O12^iv—La2—O10ⁱⁱⁱ	146.07 (9)
O15—C10—H10	108.6	O16ⁱⁱⁱ—La2—O10ⁱⁱⁱ	77.54 (10)
C9—C10—H10	108.6	C1—O1—La1	131.0 (3)
C11—C10—H10	108.6	C2—O3—La1	121.9 (3)
O16—C11—C10	110.8 (4)	C2—O3—H3A	103.0
O16—C11—C12	108.7 (3)	La1—O3—H3A	114.7
C10—C11—C12	112.6 (4)	C3—O4—La2	119.8 (2)
O16—C11—H11	108.2	C3—O4—H4	108.6
C10—C11—H11	108.2	La2—O4—H4	121.1
C12—C11—H11	108.2	C4—O5—La2	127.0 (3)
O17—C12—O18	125.4 (4)	C4—O6—La1^v	135.2 (3)
O17—C12—C11	118.4 (4)	C5—O7—La1	131.3 (3)
O18—C12—C11	116.2 (4)	C6—O9—La1	121.6 (2)
O7—La1—O1	78.94 (11)	C6—O9—H9	104.2
O7—La1—O1W	76.88 (11)	La1—O9—H9	104.9
O1—La1—O1W	75.70 (11)	C7—O10—La2^vi	123.3 (2)
O7—La1—O13	123.42 (11)	C7—O10—H10A	108.1
O1—La1—O13	76.42 (10)	La2^vi—O10—H10A	126.4
O1W—La1—O13	140.85 (11)	C8—O11—La2^vi	131.4 (3)
O7—La1—O6ⁱ	74.88 (11)	C8—O12—La2^vii	133.4 (3)
O1—La1—O6ⁱ	145.67 (10)	C9—O13—La1	126.5 (3)
O1W—La1—O6ⁱ	77.03 (10)	C9—O14—La2^viii	143.6 (3)
O13—La1—O6ⁱ	137.11 (10)	C10—O15—La1	123.8 (2)
O7—La1—O15	115.51 (10)	C10—O15—H15	110.8
O1—La1—O15	136.82 (10)	La1—O15—H15	120.3
O1W—La1—O15	145.22 (10)	C11—O16—La2^vi	122.1 (2)
O13—La1—O15	61.51 (10)	C11—O16—H16	105.4
O6ⁱ—La1—O15	75.61 (10)	La2^vi—O16—H16	126.4
O7—La1—O2W	142.04 (11)	C12—O17—La2^vi	128.9 (3)
O1—La1—O2W	125.34 (11)	La1—O1W—H1W	111.2
O1W—La1—O2W	81.70 (12)	La1—O1W—H2W	127.1
O13—La1—O2W	92.68 (11)	H1W—O1W—H2W	105.8
O6ⁱ—La1—O2W	69.95 (11)	La1—O2W—H4W	116.7
O15—La1—O2W	69.01 (10)	La1—O2W—H3W	117.0
O7—La1—O9	60.31 (10)	H4W—O2W—H3W	104.7
O1—La1—O9	87.05 (11)	La2—O3W—H6W	128.7
O1W—La1—O9	136.24 (11)	La2—O3W—H5W	124.9
O13—La1—O9	68.26 (11)	H6W—O3W—H5W	105.5
O6ⁱ—La1—O9	98.66 (11)	H10W—O5W—H9W	105.7
O15—La1—O9	69.45 (10)	H4WA—O4WA—H4WB	105.2
O2W—La1—O9	138.45 (11)	H4WA—O4WA—H4WD	106.4
O7—La1—O3	133.15 (10)	H4WC—O4WB—H4WD	105.1

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O8^iv	0.82	1.87	2.677 (4)	169
O4—H4···O18^vii	0.82	1.80	2.619 (4)	174
O9—H9···O16	0.82	2.46	3.177 (5)	147
O10—H10A···O8^ix	0.82	1.94	2.745 (4)	167
O15—H15···O2^iv	0.82	1.82	2.632 (4)	175
O16—H16···O4WA	0.82	1.89	2.667 (9)	158
O16—H16···O4WB	0.82	1.94	2.708 (9)	157

Symmetry codes: (iv) −x, y−1/2, −z+3/2; (vii) −x, y+1/2, −z+3/2; (ix) −x, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[La₂(C₄H₄O₆)₃(H₂O)₃]·2H₂O
M_r	812.12
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	12.6271 (2), 12.9273 (2), 16.6556 (3)
β (°)	127.801 (1)
V (Å³)	2148.22 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	4.04
Crystal size (mm)	0.25 × 0.21 × 0.18

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.372, 0.480
No. of measured, independent and observed [I > 2σ(I)] reflections	19115, 3771, 3226
R_int	0.047
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.057, 1.05
No. of reflections	3771
No. of parameters	344
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.87, −0.65

Computer programs: SMART (Bruker, 2004), SAINT (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
O3—H3A···O8ⁱ	0.82	1.87	2.677 (4)	169.1
O4—H4···O18ⁱⁱ	0.82	1.80	2.619 (4)	174.2
O9—H9···O16	0.82	2.46	3.177 (5)	147.1
O10—H10A···O8ⁱⁱⁱ	0.82	1.94	2.745 (4)	166.5
O15—H15···O2ⁱ	0.82	1.82	2.632 (4)	175.2
O16—H16···O4WA	0.82	1.89	2.667 (9)	157.9
O16—H16···O4WB	0.82	1.94	2.708 (9)	157.2

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

Acknowledgements

The author acknowledges South China Normal University for supporting this work.

References

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