Poly[diaqua­tris(μ4-isophthalato)dilanthanum(III)]

Fan, L.-Q.; Wu, J.-H.

doi:10.1107/S1600536809054543

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 2| February 2010| Page m240

https://doi.org/10.1107/S1600536809054543

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Poly[diaquatris(μ₄-isophthalato)dilanthanum(III)]

Le-Qing Fan ^a ^* and Ji-Huai Wu ^a

^aInstitute of Materials Physical Chemistry and the Key Laboratory for Functional Materials of Fujian Higher Education, Huaqiao University, Quanzhou, Fujian 362021, People's Republic of China
^*Correspondence e-mail: lqfan@hqu.edu.cn

(Received 14 December 2009; accepted 18 December 2009; online 30 January 2010)

In the title coordination polymer, [La₂(C₈H₄O₄)₃(H₂O)₂]_n, there are two independent La^III atoms which are coordinated differently in slightly distorted pentagonal-bipyramidal and slightly disorted bicapped trigonal-prismatic environments. The La^III ions are bridged by μ₄-isophthalate ligands, forming two-dimensional layers. In the crystal structure, these layers are connected by intermolecular O—H⋯O hydrogen bonds into a three-dimensional network.

Related literature

For background information on lanthanide coordination polymers, see: Cheng et al. (2007 ); Dorweiler et al. (2009 ); Mondal et al. (2009 ) and for the use of multicarboxyl group ligands in this type of polymer, see: Mahata et al. (2007 ); Zhou et al. (2008 ).

Experimental

Crystal data

[La₂(C₈H₄O₄)₃(H₂O)₂]
M_r = 806.19
Monoclinic, P 2₁ /n
a = 13.3956 (12) Å
b = 14.4877 (8) Å
c = 13.5754 (11) Å
β = 103.998 (5)°
V = 2556.4 (3) Å³
Z = 4
Mo Kα radiation
μ = 3.37 mm⁻¹
T = 293 K
0.20 × 0.15 × 0.10 mm

Data collection

Rigaku Mercury diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007 ) T_min = 0.717, T_max = 1.000
19411 measured reflections
5841 independent reflections
5111 reflections with I > 2σ(I)
R_int = 0.042

Refinement

R[F² > 2σ(F²)] = 0.048
wR(F²) = 0.139
S = 1.08
5841 reflections
361 parameters
18 restraints
H-atom parameters constrained
Δρ_max = 2.72 e Å⁻³
Δρ_min = −1.33 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O13—H13A⋯O2ⁱ	0.85	2.27	2.814 (8)	122
O13—H13B⋯O11ⁱ	0.85	2.20	2.976 (8)	152
O14—H14B⋯O10ⁱⁱ	0.85	1.97	2.795 (8)	162
O14—H14A⋯O7ⁱⁱⁱ	0.85	2.10	2.656 (8)	122
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) -x+1, -y, -z+1.

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004 ); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536809054543/lh2972sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809054543/lh2972Isup2.hkl

checkCIF report

Comment top

Investigations of the constructions of coordination polymers based on lanthanide metals have attracted great interests not only for their diverse structures but also for their luminescent and magnetic properties (Cheng et al., 2007; Dorweiler et al., 2009; Mondal et al., 2009). Because ligands containing multicarboxyl groups can give rise to abundant coordination modes, they have been selected to build lanthanide coordination polymers (Mahata et al., 2007; Zhou et al., 2008). We report herein the crystal structure of the title La(III) compound, (I).

As shown in Fig.1, the asymmetric unit of (I) contains two independent La^III ions, three isophthalato (ip) ligands, and two coordinated water molecules. Atom La1 is coordinated by seven O atoms in a slightly distorted pentagonal bipyramidal environment. The pentagonal plane is occupied by four oxygen atoms from four ip ligands and one oxygen atom from a water molecule, and the two apical sites are occupied by another two oxygen atoms from two ip ligands. The coordination geometry of La2 is a slightly disortoted bi-capped trigonal prism. The La^III ions are bridged by µ₄-isophthalato ligands to form two-dimensional layers (Fig. 2). In the crystal structure, these layers are connected by intermolecular O—H···O hydrogen bonds to form a three-dimensional network.

Related literature top

For background information on lanthanide coordination polymers, see: Cheng et al. (2007); Dorweiler et al. (2009); Mondal et al. (2009) and for the use of multicarboxyl group ligands in this type of polymer, see: Mahata et al. (2007); Zhou et al. (2008).

Experimental top

A mixture of La₂O₃ (0.163 g, 0.5 mmol), isophthalic acid (0.166 g, 1 mmol) and H₂O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 443 K for 7 days and then cooled to room temperature at a rate of 0.2 K h^—1. The colorless crystals obtained were washed with water and dried in air (yield 16% based on La).

Structure description top

For background information on lanthanide coordination polymers, see: Cheng et al. (2007); Dorweiler et al. (2009); Mondal et al. (2009) and for the use of multicarboxyl group ligands in this type of polymer, see: Mahata et al. (2007); Zhou et al. (2008).

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. The asymmetric unit of (I), showing the atom-numbering scheme. H atoms are not included and displacement ellipsoids are drawn at the 30% probability level. Additional symmetry related atoms are included to complete the coordination geomtry around the La atoms [Symmetry codes: (A) 1.5 — x, —0.5 + y, 0.5 — z; (B) 0.5 + x, 0.5 — y, —0.5 + z; (C) 1.5 — x, 0.5 + y, 0.5 — z; (D) 1 — x, — y, 1 — z].

Fig. 2. View of part of the two-dimensional layer of (I). H atoms are not included.

Poly[diaquatris(µ₄-isophthalato)dilanthanum(III)] top

Crystal data top

[La₂(C₈H₄O₄)₃(H₂O)₂]	F(000) = 1544
M_r = 806.19	D_x = 2.095 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 6025 reflections
a = 13.3956 (12) Å	θ = 3.1–27.5°
b = 14.4877 (8) Å	µ = 3.37 mm⁻¹
c = 13.5754 (11) Å	T = 293 K
β = 103.998 (5)°	Prism, colorless
V = 2556.4 (3) Å³	0.20 × 0.15 × 0.10 mm
Z = 4

Data collection top

Rigaku Mercury diffractometer	5841 independent reflections
Radiation source: fine-focus sealed tube	5111 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.042
ω scans	θ_max = 27.5°, θ_min = 2.1°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007)	h = −17→16
T_min = 0.717, T_max = 1.000	k = −18→18
19411 measured reflections	l = −17→17

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)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.139	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0811P)² + 4.3612P] where P = (F_o² + 2F_c²)/3
5841 reflections	(Δ/σ)_max = 0.001
361 parameters	Δρ_max = 2.72 e Å⁻³
18 restraints	Δρ_min = −1.33 e Å⁻³

Crystal data top

[La₂(C₈H₄O₄)₃(H₂O)₂]	V = 2556.4 (3) Å³
M_r = 806.19	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 13.3956 (12) Å	µ = 3.37 mm⁻¹
b = 14.4877 (8) Å	T = 293 K
c = 13.5754 (11) Å	0.20 × 0.15 × 0.10 mm
β = 103.998 (5)°

Data collection top

Rigaku Mercury diffractometer	5841 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007)	5111 reflections with I > 2σ(I)
T_min = 0.717, T_max = 1.000	R_int = 0.042
19411 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.048	18 restraints
wR(F²) = 0.139	H-atom parameters constrained
S = 1.08	Δρ_max = 2.72 e Å⁻³
5841 reflections	Δρ_min = −1.33 e Å⁻³
361 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
La1	0.84385 (2)	0.31714 (2)	0.38814 (2)	0.02027 (12)
La2	0.61501 (2)	0.06678 (2)	0.32769 (2)	0.02238 (12)
O1	0.6774 (3)	0.2657 (3)	0.2958 (3)	0.0358 (10)
O2	0.5239 (4)	0.2049 (3)	0.2615 (4)	0.0375 (11)
O3	0.7107 (4)	0.5678 (4)	0.1326 (5)	0.0545 (15)
O4	0.5900 (4)	0.6718 (3)	0.1260 (5)	0.0510 (14)
O5	0.7672 (4)	0.2617 (4)	0.5144 (4)	0.0463 (13)
O6	0.6532 (4)	0.1469 (4)	0.4850 (4)	0.0463 (13)
O7	0.5312 (4)	0.0136 (3)	0.7733 (4)	0.0383 (11)
O8	0.5033 (4)	0.1180 (3)	0.8868 (3)	0.0392 (11)
O9	0.8372 (4)	0.3771 (3)	0.2105 (3)	0.0359 (10)
O10	0.8799 (4)	0.4248 (3)	0.0703 (4)	0.0395 (11)
O11	0.6533 (4)	0.0748 (3)	0.1637 (4)	0.0437 (12)
O12	0.7235 (4)	−0.0402 (3)	0.0943 (4)	0.0482 (13)
O13	0.9519 (5)	0.3449 (5)	0.5562 (4)	0.071 (2)
H13B	1.0027	0.3819	0.5703	0.085*
H13A	0.9312	0.3119	0.5991	0.085*
O14	0.4569 (4)	0.0722 (3)	0.3964 (4)	0.0454 (13)
H14A	0.4165	0.0455	0.3466	0.054*
H14B	0.4465	0.0688	0.4557	0.054*
C1	0.5822 (5)	0.2719 (5)	0.2627 (5)	0.0319 (13)
C2	0.6223 (5)	0.5905 (5)	0.1368 (5)	0.0381 (15)
C3	0.7040 (5)	0.2086 (5)	0.5416 (5)	0.0373 (15)
C4	0.5455 (5)	0.0912 (5)	0.8170 (5)	0.0318 (13)
C5	0.8589 (4)	0.3606 (4)	0.1257 (4)	0.0265 (12)
C6	0.7158 (6)	0.0436 (5)	0.1157 (5)	0.0366 (15)
C7	0.5369 (5)	0.3625 (5)	0.2226 (6)	0.0409 (16)
C8	0.5967 (5)	0.4312 (4)	0.1954 (6)	0.0365 (15)
H8A	0.6664	0.4201	0.2018	0.044*
C9	0.5563 (6)	0.5166 (5)	0.1589 (7)	0.0497 (19)
C10	0.4527 (8)	0.5310 (7)	0.1490 (10)	0.082 (3)
H10A	0.4231	0.5864	0.1219	0.099*
C11	0.3917 (9)	0.4641 (9)	0.1789 (11)	0.098 (4)
H11A	0.3229	0.4759	0.1765	0.118*
C12	0.4353 (7)	0.3788 (6)	0.2126 (9)	0.072 (3)
H12A	0.3939	0.3324	0.2285	0.086*
C13	0.6907 (5)	0.2169 (5)	0.6486 (5)	0.0353 (14)
C14	0.6329 (5)	0.1517 (5)	0.6845 (5)	0.0339 (14)
H14C	0.6048	0.1024	0.6431	0.041*
C15	0.6156 (5)	0.1586 (5)	0.7833 (5)	0.0320 (13)
C16	0.6589 (6)	0.2315 (6)	0.8462 (5)	0.0457 (18)
H16A	0.6474	0.2371	0.9108	0.055*
C17	0.7189 (6)	0.2949 (6)	0.8120 (6)	0.0466 (19)
H17A	0.7495	0.3426	0.8546	0.056*
C18	0.7350 (6)	0.2888 (5)	0.7121 (6)	0.0428 (16)
H18A	0.7751	0.3327	0.6896	0.051*
C19	0.8584 (5)	0.2627 (4)	0.0888 (5)	0.0320 (13)
C20	0.7905 (5)	0.2005 (4)	0.1165 (5)	0.0337 (14)
H20A	0.7471	0.2201	0.1564	0.040*
C21	0.7878 (5)	0.1090 (5)	0.0845 (6)	0.0399 (16)
C22	0.8536 (7)	0.0792 (5)	0.0250 (7)	0.056 (2)
H22A	0.8520	0.0182	0.0033	0.067*
C23	0.9201 (7)	0.1409 (5)	−0.0010 (7)	0.059 (2)
H23A	0.9649	0.1210	−0.0393	0.071*
C24	0.9221 (6)	0.2322 (5)	0.0284 (6)	0.0427 (17)
H24A	0.9662	0.2734	0.0078	0.051*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La1	0.02440 (19)	0.01671 (19)	0.02177 (19)	0.00019 (11)	0.00959 (13)	0.00025 (11)
La2	0.0265 (2)	0.0186 (2)	0.02394 (19)	−0.00009 (12)	0.00989 (14)	0.00050 (11)
O1	0.033 (2)	0.039 (3)	0.034 (2)	0.000 (2)	0.0058 (19)	0.001 (2)
O2	0.039 (3)	0.024 (2)	0.049 (3)	−0.003 (2)	0.009 (2)	0.008 (2)
O3	0.035 (3)	0.046 (3)	0.083 (4)	−0.002 (2)	0.015 (3)	0.017 (3)
O4	0.047 (3)	0.027 (3)	0.079 (4)	−0.002 (2)	0.016 (3)	0.008 (2)
O5	0.051 (3)	0.058 (3)	0.035 (3)	−0.018 (3)	0.021 (2)	0.001 (2)
O6	0.047 (3)	0.058 (3)	0.036 (3)	−0.018 (3)	0.014 (2)	−0.009 (2)
O7	0.038 (3)	0.039 (3)	0.041 (3)	−0.005 (2)	0.015 (2)	−0.002 (2)
O8	0.041 (3)	0.048 (3)	0.031 (2)	−0.001 (2)	0.0141 (19)	−0.003 (2)
O9	0.040 (2)	0.039 (3)	0.031 (2)	−0.007 (2)	0.0132 (19)	−0.0029 (19)
O10	0.056 (3)	0.029 (2)	0.036 (3)	−0.008 (2)	0.017 (2)	0.0010 (19)
O11	0.057 (3)	0.040 (3)	0.043 (3)	−0.011 (2)	0.027 (2)	−0.003 (2)
O12	0.060 (3)	0.030 (3)	0.061 (3)	−0.002 (2)	0.027 (3)	−0.003 (2)
O13	0.068 (4)	0.105 (5)	0.035 (3)	−0.049 (4)	0.006 (3)	0.004 (3)
O14	0.046 (3)	0.058 (3)	0.039 (3)	−0.007 (2)	0.024 (2)	−0.013 (2)
C1	0.038 (3)	0.031 (3)	0.027 (3)	−0.005 (3)	0.008 (2)	0.001 (2)
C2	0.034 (4)	0.032 (4)	0.047 (4)	0.001 (3)	0.008 (3)	0.008 (3)
C3	0.035 (3)	0.043 (4)	0.036 (3)	−0.007 (3)	0.013 (3)	−0.004 (3)
C4	0.025 (3)	0.039 (4)	0.030 (3)	0.002 (3)	0.004 (2)	0.000 (3)
C5	0.025 (3)	0.024 (3)	0.031 (3)	0.000 (2)	0.008 (2)	0.004 (2)
C6	0.049 (4)	0.031 (3)	0.034 (3)	−0.003 (3)	0.016 (3)	0.000 (3)
C7	0.033 (3)	0.029 (4)	0.057 (4)	−0.004 (3)	0.005 (3)	0.006 (3)
C8	0.032 (3)	0.033 (4)	0.046 (4)	−0.001 (3)	0.012 (3)	0.005 (3)
C9	0.034 (4)	0.035 (4)	0.077 (6)	0.003 (3)	0.009 (4)	0.011 (4)
C10	0.055 (5)	0.046 (5)	0.149 (8)	0.009 (4)	0.029 (5)	0.036 (5)
C11	0.060 (6)	0.079 (6)	0.160 (9)	0.010 (5)	0.034 (6)	0.044 (6)
C12	0.051 (5)	0.041 (4)	0.127 (7)	−0.003 (4)	0.029 (5)	0.023 (5)
C13	0.037 (3)	0.041 (4)	0.032 (3)	−0.007 (3)	0.017 (3)	−0.006 (3)
C14	0.033 (3)	0.040 (4)	0.032 (3)	−0.004 (3)	0.012 (2)	−0.003 (3)
C15	0.031 (3)	0.039 (4)	0.028 (3)	−0.002 (3)	0.011 (2)	−0.001 (3)
C16	0.052 (4)	0.057 (5)	0.029 (3)	−0.017 (4)	0.012 (3)	−0.011 (3)
C17	0.046 (4)	0.055 (5)	0.045 (4)	−0.026 (4)	0.023 (3)	−0.022 (4)
C18	0.046 (4)	0.042 (4)	0.045 (4)	−0.008 (3)	0.019 (3)	−0.004 (3)
C19	0.036 (3)	0.027 (3)	0.034 (3)	0.000 (3)	0.011 (3)	−0.001 (3)
C20	0.044 (4)	0.026 (3)	0.034 (3)	−0.006 (3)	0.017 (3)	0.002 (3)
C21	0.043 (4)	0.033 (4)	0.050 (4)	−0.008 (3)	0.022 (3)	−0.004 (3)
C22	0.073 (6)	0.032 (4)	0.078 (6)	−0.013 (4)	0.049 (5)	−0.005 (4)
C23	0.081 (6)	0.034 (4)	0.083 (6)	−0.006 (4)	0.061 (5)	−0.012 (4)
C24	0.044 (4)	0.036 (4)	0.055 (4)	−0.004 (3)	0.027 (3)	−0.002 (3)

Geometric parameters (Å, º) top

La1—O12ⁱ	2.291 (5)	C1—C7	1.492 (9)
La1—O4ⁱⁱ	2.310 (5)	C2—C9	1.465 (10)
La1—O8ⁱⁱⁱ	2.338 (5)	C3—C13	1.510 (9)
La1—O5	2.343 (5)	C4—C15	1.500 (9)
La1—O1	2.396 (4)	C5—C19	1.504 (9)
La1—O13	2.422 (5)	C5—La2ⁱ	3.056 (6)
La1—O9	2.545 (4)	C6—C21	1.486 (10)
La2—O3ⁱⁱ	2.266 (5)	C7—C12	1.356 (11)
La2—O6	2.376 (5)	C7—C8	1.383 (9)
La2—O2	2.402 (4)	C8—C9	1.392 (10)
La2—O7^iv	2.403 (5)	C8—H8A	0.9300
La2—O11	2.405 (5)	C9—C10	1.377 (12)
La2—O10ⁱⁱ	2.471 (5)	C10—C11	1.391 (14)
La2—O14	2.514 (5)	C10—H10A	0.9300
La2—O9ⁱⁱ	2.897 (5)	C11—C12	1.395 (14)
O1—C1	1.250 (8)	C11—H11A	0.9300
O2—C1	1.243 (8)	C12—H12A	0.9300
O3—C2	1.244 (9)	C13—C14	1.382 (9)
O3—La2ⁱ	2.266 (5)	C13—C18	1.391 (10)
O4—C2	1.251 (8)	C14—C15	1.418 (9)
O4—La1ⁱ	2.310 (5)	C14—H14C	0.9300
O5—C3	1.263 (8)	C15—C16	1.394 (10)
O6—C3	1.264 (8)	C16—C17	1.373 (10)
O7—C4	1.265 (8)	C16—H16A	0.9300
O7—La2^iv	2.403 (5)	C17—C18	1.426 (10)
O8—C4	1.276 (8)	C17—H17A	0.9300
O8—La1^v	2.338 (5)	C18—H18A	0.9300
O9—C5	1.276 (7)	C19—C24	1.391 (9)
O9—La2ⁱ	2.897 (5)	C19—C20	1.395 (9)
O10—C5	1.269 (7)	C20—C21	1.393 (9)
O10—La2ⁱ	2.471 (5)	C20—H20A	0.9300
O11—C6	1.262 (8)	C21—C22	1.400 (10)
O12—C6	1.258 (8)	C22—C23	1.367 (10)
O12—La1ⁱⁱ	2.291 (5)	C22—H22A	0.9300
O13—H13B	0.8500	C23—C24	1.379 (11)
O13—H13A	0.8501	C23—H23A	0.9300
O14—H14A	0.8500	C24—H24A	0.9300
O14—H14B	0.8501

O12ⁱ—La1—O4ⁱⁱ	178.4 (2)	C7—C1—La2	164.5 (5)
O12ⁱ—La1—O8ⁱⁱⁱ	91.26 (18)	O3—C2—O4	123.4 (7)
O4ⁱⁱ—La1—O8ⁱⁱⁱ	89.77 (18)	O3—C2—C9	116.3 (6)
O12ⁱ—La1—O5	88.85 (19)	O4—C2—C9	120.3 (7)
O4ⁱⁱ—La1—O5	89.6 (2)	O5—C3—O6	123.5 (6)
O8ⁱⁱⁱ—La1—O5	134.94 (17)	O5—C3—C13	118.4 (6)
O12ⁱ—La1—O1	89.71 (19)	O6—C3—C13	118.0 (6)
O4ⁱⁱ—La1—O1	90.01 (18)	O7—C4—O8	125.1 (6)
O8ⁱⁱⁱ—La1—O1	148.99 (15)	O7—C4—C15	118.1 (6)
O5—La1—O1	76.07 (17)	O8—C4—C15	116.8 (6)
O12ⁱ—La1—O13	85.0 (2)	O10—C5—O9	121.9 (6)
O4ⁱⁱ—La1—O13	94.3 (2)	O10—C5—C19	118.6 (5)
O8ⁱⁱⁱ—La1—O13	66.51 (17)	O9—C5—C19	119.5 (5)
O5—La1—O13	68.62 (19)	O10—C5—La2ⁱ	51.4 (3)
O1—La1—O13	144.36 (18)	O9—C5—La2ⁱ	70.7 (3)
O12ⁱ—La1—O9	82.32 (17)	C19—C5—La2ⁱ	169.2 (4)
O4ⁱⁱ—La1—O9	99.13 (19)	O12—C6—O11	124.5 (6)
O8ⁱⁱⁱ—La1—O9	71.23 (15)	O12—C6—C21	117.0 (6)
O5—La1—O9	152.80 (17)	O11—C6—C21	118.5 (6)
O1—La1—O9	78.20 (15)	C12—C7—C8	118.7 (7)
O13—La1—O9	135.42 (17)	C12—C7—C1	120.0 (7)
O3ⁱⁱ—La2—O6	78.3 (2)	C8—C7—C1	121.4 (6)
O3ⁱⁱ—La2—O2	119.00 (18)	C7—C8—C9	122.3 (7)
O6—La2—O2	84.73 (19)	C7—C8—H8A	118.9
O3ⁱⁱ—La2—O7^iv	142.19 (18)	C9—C8—H8A	118.9
O6—La2—O7^iv	135.92 (17)	C10—C9—C8	117.8 (7)
O2—La2—O7^iv	85.41 (16)	C10—C9—C2	120.8 (7)
O3ⁱⁱ—La2—O11	77.4 (2)	C8—C9—C2	121.4 (7)
O6—La2—O11	139.53 (17)	C9—C10—C11	121.0 (9)
O2—La2—O11	79.43 (17)	C9—C10—H10A	119.5
O7^iv—La2—O11	79.77 (17)	C11—C10—H10A	119.5
O3ⁱⁱ—La2—O10ⁱⁱ	89.1 (2)	C10—C11—C12	119.0 (10)
O6—La2—O10ⁱⁱ	86.12 (17)	C10—C11—H11A	120.5
O2—La2—O10ⁱⁱ	147.73 (16)	C12—C11—H11A	120.5
O7^iv—La2—O10ⁱⁱ	79.90 (17)	C7—C12—C11	121.2 (9)
O11—La2—O10ⁱⁱ	125.15 (16)	C7—C12—H12A	119.4
O3ⁱⁱ—La2—O14	145.5 (2)	C11—C12—H12A	119.4
O6—La2—O14	70.65 (17)	C14—C13—C18	119.0 (6)
O2—La2—O14	73.46 (17)	C14—C13—C3	119.4 (6)
O7^iv—La2—O14	65.34 (16)	C18—C13—C3	121.6 (6)
O11—La2—O14	136.85 (18)	C13—C14—C15	121.3 (6)
O10ⁱⁱ—La2—O14	74.30 (17)	C13—C14—H14C	119.4
O3ⁱⁱ—La2—O9ⁱⁱ	77.81 (16)	C15—C14—H14C	119.4
O6—La2—O9ⁱⁱ	128.00 (17)	C16—C15—C14	119.6 (6)
O2—La2—O9ⁱⁱ	146.91 (15)	C16—C15—C4	120.3 (6)
O7^iv—La2—O9ⁱⁱ	67.88 (15)	C14—C15—C4	120.0 (6)
O11—La2—O9ⁱⁱ	76.96 (15)	C17—C16—C15	119.3 (7)
O10ⁱⁱ—La2—O9ⁱⁱ	48.19 (14)	C17—C16—H16A	120.3
O14—La2—O9ⁱⁱ	109.79 (15)	C15—C16—H16A	120.3
C1—O1—La1	154.9 (4)	C16—C17—C18	121.1 (7)
C1—O2—La2	112.7 (4)	C16—C17—H17A	119.5
C2—O3—La2ⁱ	158.2 (6)	C18—C17—H17A	119.5
C2—O4—La1ⁱ	137.7 (5)	C13—C18—C17	119.7 (7)
C3—O5—La1	150.0 (5)	C13—C18—H18A	120.1
C3—O6—La2	149.2 (5)	C17—C18—H18A	120.1
C4—O7—La2^iv	135.1 (4)	C24—C19—C20	119.2 (6)
C4—O8—La1^v	134.3 (4)	C24—C19—C5	122.8 (6)
C5—O9—La1	145.9 (4)	C20—C19—C5	118.1 (6)
C5—O9—La2ⁱ	84.7 (3)	C21—C20—C19	120.0 (6)
La1—O9—La2ⁱ	122.32 (17)	C21—C20—H20A	120.0
C5—O10—La2ⁱ	105.0 (4)	C19—C20—H20A	120.0
C6—O11—La2	141.0 (5)	C20—C21—C22	120.1 (6)
C6—O12—La1ⁱⁱ	142.2 (5)	C20—C21—C6	119.2 (6)
La1—O13—H13B	125.4	C22—C21—C6	120.7 (6)
La1—O13—H13A	109.3	C23—C22—C21	119.1 (7)
H13B—O13—H13A	125.2	C23—C22—H22A	120.4
La2—O14—H14A	96.9	C21—C22—H22A	120.4
La2—O14—H14B	134.0	C22—C23—C24	121.4 (7)
H14A—O14—H14B	120.6	C22—C23—H23A	119.3
O2—C1—O1	122.1 (6)	C24—C23—H23A	119.3
O2—C1—C7	118.9 (6)	C23—C24—C19	120.2 (7)
O1—C1—C7	119.0 (6)	C23—C24—H24A	119.9
O2—C1—La2	45.6 (3)	C19—C24—H24A	119.9
O1—C1—La2	76.5 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O2^vi	0.85	2.27	2.814 (8)	122
O13—H13B···O11^vi	0.85	2.20	2.976 (8)	152
O14—H14B···O10^v	0.85	1.97	2.795 (8)	162
O14—H14A···O7^iv	0.85	2.10	2.656 (8)	122

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

Experimental details

Crystal data
Chemical formula	[La₂(C₈H₄O₄)₃(H₂O)₂]
M_r	806.19
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	13.3956 (12), 14.4877 (8), 13.5754 (11)
β (°)	103.998 (5)
V (Å³)	2556.4 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.37
Crystal size (mm)	0.20 × 0.15 × 0.10

Data collection
Diffractometer	Rigaku Mercury diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2007)
T_min, T_max	0.717, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	19411, 5841, 5111
R_int	0.042
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.048, 0.139, 1.08
No. of reflections	5841
No. of parameters	361
No. of restraints	18
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.72, −1.33

Computer programs: CrystalClear (Rigaku, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2004), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O2ⁱ	0.85	2.268	2.814 (8)	122.19
O13—H13B···O11ⁱ	0.85	2.199	2.976 (8)	151.85
O14—H14B···O10ⁱⁱ	0.85	1.974	2.795 (8)	162.09
O14—H14A···O7ⁱⁱⁱ	0.85	2.104	2.656 (8)	122.2

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

Acknowledgements

This work was supported financially by the Young Talent Fund of Fujian Province (No. 2007 F3060).

References

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