Poly[diaqua-μ(2)-isonicotinato-μ(2)-oxalato-terbium(III)].

In the crystal structure of the title complex, [Tb(C(6)H(4)NO(2))(C(2)O(4))(H(2)O)(2)](n), the Tb(III) ion is coordinated by two O atoms from two isonicotinate (inic) anions, four O atoms of two oxalate anions, and two water mol-ecules, displaying a distorted square-antiprismatic geometry. The Tb(III) ion, the inic anion and the water mol-ecules occupy general positions. One of the two crystallographically independent oxalate anions is located on a center of inversion, whereas the second is located on the twofold rotation axis. The carboxyl-ate groups of the inic and oxalate anions link the terbium metal centres into layers. These layers are connected by O-H⋯O and N-H⋯O hydrogen bonding into a three-dimensional network.

Related literature

For background, see: Eddaoudi et al. (2001 ▶); Rizk et al. (2005 ▶). An independent determination of this structure is reported in the preceeding paper, see: Song et al. (2009 ▶).

Experimental

Crystal data

[Tb(C6H4NO2)(C2O4)(H2O)2]

M = 405.07

Monoclinic,

a = 17.7919 (18) Å

b = 9.9259 (10) Å

c = 12.9670 (13) Å

β = 112.4140 (10)°

V = 2117.0 (4) Å3

Z = 8

Mo Kα radiation

μ = 6.72 mm−1

T = 296 (2) K

0.23 × 0.22 × 0.20 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (APEX2; Bruker, 2004 ▶) T min = 0.241, T max = 0.272

5243 measured reflections

1907 independent reflections

1674 reflections with I > 2σ(I)

R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.063

S = 1.01

1907 reflections

163 parameters

6 restraints

H-atom parameters constrained

Δρmax = 1.40 e Å−3

Δρmin = −1.31 e Å−3

Data collection: APEX2 (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: PLATON (Spek, 2003 ▶) and SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808042682/nc2118sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808042682/nc2118Isup2.hkl

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

[Tb(C6H4NO2)(C2O4)(H2O)2]	F(000) = 1536
Mr = 405.07	Dx = 2.542 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 17.7919 (18) Å	Cell parameters from 2410 reflections
b = 9.9259 (10) Å	θ = 2.4–27.7°
c = 12.9670 (13) Å	µ = 6.72 mm−1
β = 112.414 (1)°	T = 296 K
V = 2117.0 (4) Å3	Block, colourless
Z = 8	0.23 × 0.22 × 0.20 mm

Bruker APEXII area-detector diffractometer	1674 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.031
φ and ω scans	θmax = 25.2°, θmin = 2.4°
Absorption correction: multi-scan (APEX2; Bruker, 2004)	h = −21→20
Tmin = 0.241, Tmax = 0.272	k = −5→11
5243 measured reflections	l = −15→15
1907 independent reflections

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063	H-atom parameters constrained
S = 1.01	w = 1/[σ2(Fo2) + (0.0363P)2] where P = (Fo2 + 2Fc2)/3
1907 reflections	(Δ/σ)max = 0.002
163 parameters	Δρmax = 1.40 e Å−3
6 restraints	Δρmin = −1.31 e Å−3

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 > 2sigma(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
Tb1	0.824056 (12)	0.03238 (2)	0.574780 (18)	0.01553 (10)
O5	0.9618 (2)	−0.0185 (4)	0.6050 (3)	0.0289 (9)
O2	0.6877 (2)	0.0558 (4)	0.4672 (3)	0.0326 (9)
O3	0.8029 (2)	−0.1491 (3)	0.4403 (3)	0.0239 (8)
C8	1.0149 (3)	−0.0110 (5)	0.7019 (4)	0.0192 (11)
O6	1.0905 (2)	−0.0055 (4)	0.7291 (3)	0.0272 (9)
C1	0.6278 (3)	0.1294 (5)	0.4198 (4)	0.0215 (11)
C2	0.5442 (3)	0.0692 (5)	0.3902 (4)	0.0172 (10)
C3	0.4756 (3)	0.1501 (6)	0.3627 (4)	0.0264 (12)
H3	0.4800	0.2434	0.3618	0.032*
C6	0.5336 (3)	−0.0690 (5)	0.3874 (4)	0.0241 (11)
H6	0.5781	−0.1263	0.4050	0.029*
C4	0.4010 (3)	0.0890 (6)	0.3366 (4)	0.0315 (13)
H4	0.3556	0.1438	0.3206	0.038*
C5	0.4563 (3)	−0.1211 (5)	0.3584 (5)	0.0314 (13)
H5	0.4500	−0.2142	0.3564	0.038*
N1	0.3903 (3)	−0.0438 (5)	0.3330 (4)	0.0309 (11)
C7	0.7582 (3)	−0.2447 (5)	0.4457 (4)	0.0201 (11)
O4	0.7261 (2)	−0.3320 (3)	0.3724 (3)	0.0252 (8)
O1	0.6308 (2)	0.2507 (4)	0.3926 (3)	0.0334 (9)
O1W	0.75857 (19)	0.1250 (3)	0.6941 (3)	0.0228 (8)
H1W	0.7146	0.0877	0.6885	0.034*
H2W	0.7794	0.1546	0.7598	0.034*
O2W	0.8300 (2)	0.1188 (4)	0.4029 (3)	0.0312 (9)
H3W	0.8554	0.0794	0.3691	0.047*
H4W	0.8051	0.1834	0.3631	0.047*

	U11	U22	U33	U12	U13	U23
Tb1	0.01241 (14)	0.01564 (15)	0.01830 (15)	−0.00225 (9)	0.00558 (10)	−0.00106 (9)
O5	0.0153 (18)	0.048 (2)	0.023 (2)	0.0038 (17)	0.0067 (16)	−0.0063 (18)
O2	0.0144 (18)	0.052 (3)	0.028 (2)	0.0001 (18)	0.0045 (16)	0.001 (2)
O3	0.0271 (19)	0.0201 (18)	0.0287 (19)	−0.0097 (16)	0.0153 (16)	−0.0047 (16)
C8	0.017 (3)	0.018 (2)	0.019 (3)	0.003 (2)	0.003 (2)	0.000 (2)
O6	0.0132 (18)	0.040 (2)	0.027 (2)	0.0019 (16)	0.0068 (16)	−0.0024 (17)
C1	0.019 (3)	0.031 (3)	0.016 (2)	−0.006 (2)	0.009 (2)	−0.007 (2)
C2	0.017 (2)	0.021 (3)	0.014 (2)	−0.005 (2)	0.0058 (19)	0.001 (2)
C3	0.023 (3)	0.028 (3)	0.033 (3)	0.004 (2)	0.017 (2)	0.008 (2)
C6	0.019 (3)	0.022 (3)	0.031 (3)	−0.003 (2)	0.010 (2)	0.001 (2)
C4	0.019 (3)	0.049 (4)	0.030 (3)	0.007 (3)	0.014 (2)	0.008 (3)
C5	0.036 (3)	0.022 (3)	0.040 (3)	−0.013 (3)	0.018 (3)	−0.004 (3)
N1	0.023 (2)	0.044 (3)	0.026 (2)	−0.009 (2)	0.010 (2)	−0.001 (2)
C7	0.019 (2)	0.017 (3)	0.023 (3)	0.004 (2)	0.006 (2)	0.002 (2)
O4	0.033 (2)	0.0225 (18)	0.0218 (18)	−0.0081 (16)	0.0128 (16)	−0.0050 (16)
O1	0.038 (2)	0.027 (2)	0.041 (2)	−0.0189 (18)	0.0211 (19)	−0.0120 (19)
O1W	0.0180 (17)	0.027 (2)	0.0260 (18)	−0.0064 (15)	0.0116 (15)	−0.0071 (16)
O2W	0.049 (2)	0.024 (2)	0.029 (2)	0.0045 (18)	0.0241 (18)	0.0045 (17)

Tb1—O1i	2.280 (3)	C2—C3	1.389 (7)
Tb1—O2	2.303 (3)	C3—C4	1.379 (7)
Tb1—O5	2.383 (3)	C3—H3	0.9300
Tb1—O4ii	2.385 (3)	C6—C5	1.380 (7)
Tb1—O2W	2.427 (3)	C6—H6	0.9300
Tb1—O3	2.435 (3)	C4—N1	1.330 (8)
Tb1—O6iii	2.443 (4)	C4—H4	0.9300
Tb1—O1W	2.443 (3)	C5—N1	1.335 (7)
O5—C8	1.254 (6)	C5—H5	0.9300
O2—C1	1.244 (6)	C7—O4	1.251 (6)
O3—C7	1.259 (6)	C7—C7ii	1.545 (10)
C8—O6	1.256 (6)	O4—Tb1ii	2.385 (3)
C8—C8iii	1.529 (10)	O1—Tb1i	2.280 (3)
O6—Tb1iii	2.443 (4)	O1W—H1W	0.8429
C1—O1	1.261 (6)	O1W—H2W	0.8420
C1—C2	1.511 (6)	O2W—H3W	0.8367
C2—C6	1.383 (7)	O2W—H4W	0.8365
O1i—Tb1—O2	103.43 (14)	O6—C8—C8iii	116.0 (5)
O1i—Tb1—O5	84.39 (13)	C8—O6—Tb1iii	118.3 (3)
O2—Tb1—O5	154.22 (14)	O2—C1—O1	125.4 (5)
O1i—Tb1—O4ii	151.43 (12)	O2—C1—C2	117.9 (5)
O2—Tb1—O4ii	80.50 (13)	O1—C1—C2	116.7 (5)
O5—Tb1—O4ii	104.46 (13)	C6—C2—C3	118.0 (4)
O1i—Tb1—O2W	72.60 (12)	C6—C2—C1	120.7 (4)
O2—Tb1—O2W	79.21 (13)	C3—C2—C1	121.3 (5)
O5—Tb1—O2W	79.88 (13)	C4—C3—C2	118.6 (5)
O4ii—Tb1—O2W	135.25 (12)	C4—C3—H3	120.7
O1i—Tb1—O3	141.11 (12)	C2—C3—H3	120.7
O2—Tb1—O3	78.56 (13)	C5—C6—C2	119.4 (5)
O5—Tb1—O3	80.16 (12)	C5—C6—H6	120.3
O4ii—Tb1—O3	67.43 (11)	C2—C6—H6	120.3
O2W—Tb1—O3	69.67 (11)	N1—C4—C3	123.8 (5)
O1i—Tb1—O6iii	85.24 (13)	N1—C4—H4	118.1
O2—Tb1—O6iii	137.67 (13)	C3—C4—H4	118.1
O5—Tb1—O6iii	66.65 (12)	N1—C5—C6	122.9 (5)
O4ii—Tb1—O6iii	74.06 (12)	N1—C5—H5	118.6
O2W—Tb1—O6iii	141.48 (12)	C6—C5—H5	118.6
O3—Tb1—O6iii	119.77 (12)	C4—N1—C5	117.4 (4)
O1i—Tb1—O1W	75.34 (12)	O4—C7—O3	126.5 (5)
O2—Tb1—O1W	72.48 (13)	O4—C7—C7ii	117.1 (5)
O5—Tb1—O1W	133.16 (12)	O3—C7—C7ii	116.4 (5)
O4ii—Tb1—O1W	79.12 (11)	C7—O4—Tb1ii	118.1 (3)
O2W—Tb1—O1W	130.27 (12)	C1—O1—Tb1i	154.0 (4)
O3—Tb1—O1W	138.71 (11)	Tb1—O1W—H1W	115.5
O6iii—Tb1—O1W	69.91 (12)	Tb1—O1W—H2W	129.8
C8—O5—Tb1	119.1 (3)	H1W—O1W—H2W	106.0
C1—O2—Tb1	149.9 (4)	Tb1—O2W—H3W	122.5
C7—O3—Tb1	116.5 (3)	Tb1—O2W—H4W	129.8
O5—C8—O6	127.0 (5)	H3W—O2W—H4W	107.4
O5—C8—C8iii	117.0 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···O3iv	0.84	2.22	2.992 (5)	153
O2W—H4W···O1Wi	0.84	2.19	3.003 (5)	163
O1W—H1W···N1v	0.84	1.83	2.661 (5)	167
O2W—H3W···O6vi	0.84	2.01	2.836 (5)	172

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W⋯O3i	0.84	2.22	2.992 (5)	153
O2W—H4W⋯O1Wii	0.84	2.19	3.003 (5)	163
O1W—H1W⋯N1iii	0.84	1.83	2.661 (5)	167
O2W—H3W⋯O6iv	0.84	2.01	2.836 (5)	172

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