Poly[aqua-(μ(5)-2-oxido-4-sulfonato-benzoato)lanthanum(III)].

The title compound, [La(C(7)H(3)O(6)S)(H(2)O)](n), forms a three-dimensional framework in which the asymmetric unit contains one La(III) atom, one 5-sulfosalicylate (2-oxido-4-sulfonatobenzoate) ligand and one coordinated water mol-ecule. The La(III) atom is coordinated by nine O atoms from three carboxyl-ate, three sulfonate and two hydroxyl groups, and one water mol-ecule, forming a distorted trigonal-prismatic square-face tricapped geometry.

Related literature

For the use of rigid carboxyl­ate ligands in the design and synthesis of a variety of structures, see: Cao et al. (2002 ▶); Li et al. (2004 ▶, 2005 ▶). For the structure of the isotypic Nd compound, see: Wang et al. (2004 ▶).

Experimental

Crystal data

[La(C7H3O6S)(H2O)]

M = 372.08

Triclinic,

a = 6.2297 (7) Å

b = 8.2390 (8) Å

c = 9.9157 (9) Å

α = 111.587 (2)°

β = 94.325 (2)°

γ = 93.785 (2)°

V = 469.47 (8) Å3

Z = 2

Mo Kα radiation

μ = 4.79 mm−1

T = 293 K

0.24 × 0.16 × 0.12 mm

Data collection

Siemens SMART CCD area-detector diffractometer

Absorption correction: multi-scan (; Sheldrick, 1996 ▶) T min = 0.415, T max = 0.563

2457 measured reflections

1633 independent reflections

1527 reflections with I > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.035

wR(F 2) = 0.090

S = 1.07

1633 reflections

145 parameters

H-atom parameters constrained

Δρmax = 0.79 e Å−3

Δρmin = −1.66 e Å−3

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1994 ▶); 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.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809007879/is2373sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809007879/is2373Isup2.hkl

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

[La(C7H3O6S)(H2O)]	Z = 2
Mr = 372.08	F(000) = 352
Triclinic, P1	Dx = 2.632 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.2297 (7) Å	Cell parameters from 2088 reflections
b = 8.2390 (8) Å	θ = 2.2–25.1°
c = 9.9157 (9) Å	µ = 4.79 mm−1
α = 111.587 (2)°	T = 293 K
β = 94.325 (2)°	Block, colorless
γ = 93.785 (2)°	0.24 × 0.16 × 0.12 mm
V = 469.47 (8) Å3

Siemens SMART CCD area-detector diffractometer	1633 independent reflections
Radiation source: fine-focus sealed tube	1527 reflections with I > 2σ(I)
graphite	Rint = 0.029
ω scans	θmax = 25.1°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −4→7
Tmin = 0.415, Tmax = 0.563	k = −9→9
2457 measured reflections	l = −11→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)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.0456P)2 + 4.598P] where P = (Fo2 + 2Fc2)/3
1633 reflections	(Δ/σ)max < 0.001
145 parameters	Δρmax = 0.79 e Å−3
0 restraints	Δρmin = −1.66 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
La1	0.76441 (5)	0.64763 (5)	0.46004 (4)	0.01280 (16)
S1	0.9837 (3)	0.8865 (2)	0.28204 (17)	0.0167 (4)
O1	0.4823 (8)	0.4571 (7)	−0.2043 (5)	0.0258 (12)
O2	0.5737 (8)	0.5722 (7)	−0.3605 (5)	0.0215 (11)
O3	1.0224 (7)	0.6040 (6)	−0.3536 (5)	0.0139 (9)
O4	1.0612 (9)	0.7528 (6)	0.3353 (5)	0.0229 (11)
O5	0.7603 (9)	0.9023 (8)	0.3122 (6)	0.0360 (14)
O6	1.1278 (9)	1.0487 (6)	0.3439 (5)	0.0237 (11)
O7	0.4427 (9)	0.8190 (7)	0.5052 (7)	0.0332 (13)
H7A	0.3472	0.7722	0.4375	0.040*
H7B	0.4185	0.9029	0.5766	0.040*
C1	0.6163 (12)	0.5488 (9)	−0.2412 (7)	0.0181 (14)
C2	0.8185 (11)	0.6385 (9)	−0.1475 (7)	0.0150 (13)
C3	0.8153 (11)	0.7035 (9)	0.0033 (7)	0.0153 (13)
H3A	0.6938	0.6777	0.0437	0.018*
C4	0.9937 (11)	0.8069 (9)	0.0930 (7)	0.0168 (14)
C5	1.1779 (12)	0.8448 (10)	0.0340 (7)	0.0210 (15)
H5A	1.2964	0.9148	0.0953	0.025*
C6	1.1846 (11)	0.7790 (9)	−0.1142 (8)	0.0192 (14)
H6A	1.3085	0.8041	−0.1526	0.023*
C7	1.0069 (11)	0.6740 (8)	−0.2089 (7)	0.0141 (13)

	U11	U22	U33	U12	U13	U23
La1	0.0098 (2)	0.0143 (2)	0.0121 (2)	−0.00092 (15)	0.00131 (14)	0.00277 (16)
S1	0.0185 (8)	0.0174 (8)	0.0098 (8)	−0.0033 (7)	0.0027 (6)	0.0005 (6)
O1	0.023 (3)	0.034 (3)	0.019 (3)	−0.016 (2)	−0.001 (2)	0.012 (2)
O2	0.017 (2)	0.031 (3)	0.016 (3)	−0.009 (2)	−0.005 (2)	0.012 (2)
O3	0.015 (2)	0.015 (2)	0.009 (2)	0.0004 (18)	0.0007 (18)	0.0012 (18)
O4	0.034 (3)	0.019 (2)	0.017 (3)	−0.002 (2)	0.005 (2)	0.009 (2)
O5	0.025 (3)	0.047 (4)	0.022 (3)	0.001 (3)	0.008 (2)	−0.004 (3)
O6	0.031 (3)	0.014 (2)	0.020 (3)	−0.010 (2)	−0.001 (2)	0.001 (2)
O7	0.023 (3)	0.030 (3)	0.037 (3)	0.010 (2)	0.003 (2)	0.000 (3)
C1	0.024 (4)	0.014 (3)	0.014 (3)	0.000 (3)	0.004 (3)	0.002 (3)
C2	0.014 (3)	0.018 (3)	0.014 (3)	0.004 (3)	0.003 (3)	0.005 (3)
C3	0.017 (3)	0.019 (3)	0.012 (3)	0.003 (3)	0.007 (3)	0.007 (3)
C4	0.022 (3)	0.018 (3)	0.008 (3)	−0.002 (3)	0.001 (3)	0.003 (3)
C5	0.019 (3)	0.028 (4)	0.010 (3)	−0.003 (3)	−0.001 (3)	0.001 (3)
C6	0.017 (3)	0.020 (3)	0.017 (3)	−0.003 (3)	0.008 (3)	0.002 (3)
C7	0.019 (3)	0.014 (3)	0.008 (3)	−0.001 (3)	0.002 (3)	0.003 (3)

La1—O1i	2.676 (5)	O2—C1	1.279 (9)
La1—O2ii	2.449 (5)	O3—C7	1.349 (8)
La1—O2i	2.561 (5)	O7—H7A	0.8200
La1—O3iii	2.478 (4)	O7—H7B	0.8200
La1—O3ii	2.499 (4)	C1—C2	1.480 (10)
La1—O4	2.573 (5)	C2—C3	1.393 (9)
La1—O5	2.970 (7)	C2—C7	1.424 (9)
La1—O6iv	2.548 (5)	C3—C4	1.385 (10)
La1—O7	2.501 (5)	C3—H3A	0.9300
S1—O4	1.478 (5)	C4—C5	1.395 (10)
S1—O5	1.450 (6)	C5—C6	1.372 (10)
S1—O6	1.457 (5)	C5—H5A	0.9300
S1—C4	1.751 (7)	C6—C7	1.405 (10)
O1—C1	1.251 (9)	C6—H6A	0.9300
O2ii—La1—O3iii	103.65 (16)	O6—S1—O4	110.7 (3)
O2ii—La1—O3ii	68.47 (15)	O5—S1—C4	109.1 (3)
O3iii—La1—O3ii	67.24 (16)	O6—S1—C4	107.0 (3)
O2ii—La1—O7	72.75 (19)	O4—S1—C4	107.5 (3)
O3iii—La1—O7	158.70 (17)	C1—O1—La1i	93.1 (4)
O3ii—La1—O7	127.17 (17)	C1—O2—La1v	139.2 (4)
O2ii—La1—O6iv	87.98 (17)	C1—O2—La1i	97.8 (4)
O3iii—La1—O6iv	131.23 (16)	La1v—O2—La1i	116.49 (18)
O3ii—La1—O6iv	74.06 (16)	C7—O3—La1iii	121.3 (4)
O7—La1—O6iv	70.05 (18)	C7—O3—La1v	123.5 (4)
O2ii—La1—O2i	63.51 (18)	La1iii—O3—La1v	112.76 (16)
O3iii—La1—O2i	86.88 (16)	S1—O4—La1	110.1 (3)
O3ii—La1—O2i	116.96 (15)	S1—O5—La1	93.3 (3)
O7—La1—O2i	72.64 (18)	S1—O6—La1iv	151.0 (3)
O6iv—La1—O2i	138.33 (17)	La1—O7—H7A	109.5
O2ii—La1—O4	162.22 (17)	La1—O7—H7B	130.5
O3iii—La1—O4	73.55 (15)	H7A—O7—H7B	119.7
O3ii—La1—O4	94.76 (16)	O1—C1—O2	119.2 (6)
O7—La1—O4	116.21 (18)	O1—C1—C2	122.1 (6)
O6iv—La1—O4	81.48 (16)	O2—C1—C2	118.6 (6)
O2i—La1—O4	132.71 (16)	C3—C2—C7	120.0 (6)
O2ii—La1—O1i	110.68 (15)	C3—C2—C1	118.6 (6)
O3iii—La1—O1i	88.69 (16)	C7—C2—C1	121.1 (6)
O3ii—La1—O1i	154.12 (16)	C4—C3—C2	119.7 (6)
O7—La1—O1i	73.65 (18)	C4—C3—H3A	120.1
O6iv—La1—O1i	131.55 (17)	C2—C3—H3A	120.1
O2i—La1—O1i	49.19 (15)	C3—C4—C5	120.7 (6)
O4—La1—O1i	86.95 (15)	C3—C4—S1	118.5 (5)
O2ii—La1—O5	139.80 (16)	C5—C4—S1	120.8 (5)
O3iii—La1—O5	115.64 (15)	C6—C5—C4	120.1 (6)
O3ii—La1—O5	134.13 (15)	C6—C5—H5A	120.0
O7—La1—O5	67.57 (18)	C4—C5—H5A	120.0
O6iv—La1—O5	72.93 (16)	C5—C6—C7	120.9 (6)
O2i—La1—O5	108.88 (15)	C5—C6—H6A	119.5
O4—La1—O5	49.58 (16)	C7—C6—H6A	119.5
O1i—La1—O5	64.08 (16)	O3—C7—C6	119.5 (6)
O5—S1—O6	115.5 (3)	O3—C7—C2	122.0 (6)
O5—S1—O4	106.9 (3)	C6—C7—C2	118.4 (6)

Table 1

Selected bond lengths (Å)

La1—O1i	2.676 (5)
La1—O2ii	2.449 (5)
La1—O2i	2.561 (5)
La1—O3iii	2.478 (4)
La1—O3ii	2.499 (4)
La1—O4	2.573 (5)
La1—O5	2.970 (7)
La1—O6iv	2.548 (5)
La1—O7	2.501 (5)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .