Poly[bis­(μ4-benzene-1,4-dicarboxyl­ato)(μ4-succinato)diterbium(III)]

Yu, C.-H.

doi:10.1107/S1600536808011355

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 5| May 2008| Page m735

doi:10.1107/S1600536808011355

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Poly[bis(μ₄-benzene-1,4-dicarboxylato)(μ₄-succinato)diterbium(III)]

Chun-Hui Yu ^a ^*

^aDepartment of Chemistry, College of Chemistry and Biology, Beihua University, Jilin City 132013, People's Republic of China
^*Correspondence e-mail: jlschy@126.com

(Received 15 April 2008; accepted 21 April 2008; online 30 April 2008)

In the title compound, [Tb₂(C₄H₄O₄)(C₈H₄O₄)₂]_n, the coordination around each Tb atom is distorted square-antiprismatic. The benzene-1,4-dicarboxylate and succinate anions bridge the antiprisms, forming a three-dimensional network. The succinate anion is located on a centre of inversion. The structure is isomorphous with the Dy, Gd, Er and Nd complexes.

Related literature

For isomorphous structures, see: Wang & Li (2005 ) He et al. (2006 ); Li & Wang (2005 ); Li et al. (2006 ).

Experimental

Crystal data

[Tb₂(C₄H₄O₄)(C₈H₄O₄)₂]
M_r = 381.07
Orthorhombic, P b c a
a = 13.948 (3) Å
b = 6.8724 (14) Å
c = 21.844 (4) Å
V = 2093.9 (7) Å³
Z = 8
Mo Kα radiation
μ = 6.77 mm⁻¹
T = 293 (2) K
0.29 × 0.27 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.121, T_max = 0.257
18548 measured reflections
2376 independent reflections
2135 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.017
wR(F²) = 0.041
S = 1.07
2376 reflections
154 parameters
H-atom parameters constrained
Δρ_max = 1.09 e Å⁻³
Δρ_min = −0.44 e Å⁻³

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808011355/bt2699sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808011355/bt2699Isup2.hkl

checkCIF report

Comment top

Lanthanide complexes usually exhibit interesting framework structures and intense luminescence. In all types of rare-earth compounds, carboxylate anions with aromatic rings are widely used in the construction of high-dimensional lanthanide coordination polymers because these anions are able to act as bridging ligands in various ligating modes. However, rare-earth coordination polymers with mixed aromatic and fatty carboxylates are rarely studied (Wang & Li, 2005). In this paper, we present a new mixed carboxylate complex, namely [Tb₂(1,4-bdc)₂(suc)]_n (I), where 1,4-bdc=benzene-1,4-dicarboxylate and suc= succinate.

In (I), each Tb(III) center is coordinated by eight O atoms from 1,4-bdc and suc anions in a distorted square antiprism (Fig. 1). Each carboxylate moiety of the 1,4-bdc bridges two Tb(III) atoms, whereas each carboxylate group of suc links four Tb(III) atoms. In these modes, the central Tb(III) atoms are linked by 1,4-bdc and suc ligands, resulting in a rare three-dimensional framework structure (Fig. 2). The succinate anion is located on a centre of inversion. The structure of the title compound is isomorphous with the Dy (Li & Wang, 2005) Gd (Wang & Li, 2005), Er (He et al., 2006) and the Nd (Li et al., 2006) complex.

Related literature top

For isomorphous structures, see: Wang & Li (2005) He et al. (2006); Li & Wang (2005); Li et al. (2006).

Experimental top

A mixture of 1,4-H₂bdc (0.5 mmol), H₂suc (0.5 mmol), NaOH (1 mmol) and TbCl₃^.6H₂O (0.5 mmol) was suspended in 12 ml of deionized water and sealed in a 20-ml Teflon-lined autoclave. Upon heating at 185°C for ten days, the autoclave was slowly cooled to room temperature. The crystals were collected, washed with deionized water and dried.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. The structure of (I), showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Symmetry codes: (i) 0.5 - x, y - 1/2, z; (ii) 0.5 - x, -y, z + 1/2; (iii) x + 1/2, y, 0.5 - z; (iv) x, y - 1, z; (v) 1 - x, 1 - y, 1 - z.

Poly[bis(µ₄-benzene-1,4-dicarboxylato)(µ₄-succinato)diterbium(III)] top

Crystal data top

[Tb₂(C₄H₄O₄)(C₈H₄O₄)₂]	F(000) = 1432
M_r = 381.07	D_x = 2.418 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 15551 reflections
a = 13.948 (3) Å	θ = 3.0–27.5°
b = 6.8724 (14) Å	µ = 6.77 mm⁻¹
c = 21.844 (4) Å	T = 293 K
V = 2093.9 (7) Å³	Block, colorless
Z = 8	0.29 × 0.27 × 0.20 mm

Data collection top

Rigaku R-AXIS RAPID diffractometer	2376 independent reflections
Radiation source: rotating anode	2135 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
Detector resolution: 10.0 pixels mm^-1	θ_max = 27.5°, θ_min = 3.4°
ω scans	h = −18→18
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −8→8
T_min = 0.121, T_max = 0.257	l = −28→28
18548 measured reflections

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)] = 0.017	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.041	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0163P)² + 4.6062P] where P = (F_o² + 2F_c²)/3
2376 reflections	(Δ/σ)_max = 0.001
154 parameters	Δρ_max = 1.10 e Å⁻³
0 restraints	Δρ_min = −0.44 e Å⁻³

Crystal data top

[Tb₂(C₄H₄O₄)(C₈H₄O₄)₂]	V = 2093.9 (7) Å³
M_r = 381.07	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 13.948 (3) Å	µ = 6.77 mm⁻¹
b = 6.8724 (14) Å	T = 293 K
c = 21.844 (4) Å	0.29 × 0.27 × 0.20 mm

Data collection top

Rigaku R-AXIS RAPID diffractometer	2376 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2135 reflections with I > 2σ(I)
T_min = 0.121, T_max = 0.257	R_int = 0.027
18548 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.017	0 restraints
wR(F²) = 0.041	H-atom parameters constrained
S = 1.07	Δρ_max = 1.10 e Å⁻³
2376 reflections	Δρ_min = −0.44 e Å⁻³
154 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
C1	0.1795 (2)	0.2005 (4)	0.33571 (13)	0.0204 (6)
C2	0.1524 (2)	0.1513 (4)	0.27097 (13)	0.0187 (6)
C3	0.0612 (2)	0.1987 (5)	0.24969 (14)	0.0253 (7)
H3	0.0170	0.2563	0.2759	0.030*
C4	0.0363 (2)	0.1603 (5)	0.18965 (13)	0.0231 (7)
H4	−0.0247	0.1919	0.1756	0.028*
C5	0.1021 (2)	0.0744 (4)	0.15012 (12)	0.0148 (5)
C6	0.1935 (2)	0.0297 (5)	0.17129 (14)	0.0223 (6)
H6	0.2382	−0.0253	0.1449	0.027*
C7	0.2183 (2)	0.0667 (5)	0.23162 (14)	0.0242 (7)
H7	0.2792	0.0348	0.2457	0.029*
C8	0.3754 (2)	0.5305 (4)	0.46896 (15)	0.0202 (6)
C9	0.4829 (2)	0.5423 (5)	0.46975 (14)	0.0238 (7)
H9A	0.5034	0.6766	0.4660	0.029*
H9B	0.5095	0.4688	0.4358	0.029*
C10	0.0752 (2)	0.0328 (4)	0.08488 (12)	0.0126 (5)
O1	0.25854 (17)	0.1379 (4)	0.35567 (9)	0.0256 (5)
O2	0.12255 (18)	0.3032 (3)	0.36600 (10)	0.0274 (5)
O3	0.33421 (15)	0.3741 (3)	0.45414 (10)	0.0200 (4)
O4	0.32547 (15)	0.6772 (3)	0.48303 (9)	0.0178 (4)
O5	0.13755 (15)	−0.0398 (3)	0.05016 (9)	0.0173 (4)
O6	−0.00860 (15)	0.0752 (3)	0.06791 (9)	0.0184 (4)
Tb1	0.331426 (9)	0.019240 (18)	0.445275 (6)	0.01157 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0303 (17)	0.0194 (14)	0.0114 (13)	−0.0055 (12)	−0.0067 (12)	−0.0008 (12)
C2	0.0266 (16)	0.0182 (14)	0.0113 (13)	0.0008 (12)	−0.0074 (12)	−0.0024 (11)
C3	0.0226 (16)	0.0388 (19)	0.0146 (14)	0.0067 (13)	−0.0006 (12)	−0.0092 (14)
C4	0.0151 (14)	0.0381 (18)	0.0162 (14)	0.0072 (13)	−0.0058 (12)	−0.0084 (13)
C5	0.0169 (13)	0.0180 (13)	0.0094 (12)	−0.0011 (11)	−0.0012 (10)	−0.0023 (11)
C6	0.0173 (14)	0.0318 (17)	0.0179 (15)	0.0030 (12)	−0.0059 (11)	−0.0072 (13)
C7	0.0241 (16)	0.0305 (17)	0.0180 (14)	0.0078 (13)	−0.0104 (12)	−0.0039 (13)
C8	0.0167 (14)	0.0154 (14)	0.0285 (16)	0.0013 (11)	−0.0058 (12)	−0.0014 (12)
C9	0.0238 (16)	0.0236 (16)	0.0240 (16)	−0.0028 (12)	−0.0007 (13)	0.0018 (13)
C10	0.0161 (13)	0.0135 (13)	0.0082 (12)	−0.0042 (10)	−0.0014 (10)	0.0017 (10)
O1	0.0288 (12)	0.0363 (13)	0.0116 (9)	−0.0006 (10)	−0.0090 (9)	0.0023 (9)
O2	0.0365 (14)	0.0298 (12)	0.0159 (10)	0.0018 (10)	−0.0071 (10)	−0.0108 (10)
O3	0.0136 (10)	0.0126 (9)	0.0338 (12)	0.0003 (8)	−0.0069 (9)	−0.0015 (9)
O4	0.0175 (10)	0.0150 (9)	0.0209 (10)	0.0014 (8)	−0.0025 (8)	−0.0017 (8)
O5	0.0184 (10)	0.0253 (11)	0.0083 (9)	0.0039 (8)	0.0010 (7)	0.0000 (8)
O6	0.0134 (10)	0.0294 (11)	0.0123 (9)	−0.0010 (9)	−0.0036 (8)	−0.0009 (8)
Tb1	0.01146 (7)	0.01367 (7)	0.00960 (7)	−0.00056 (5)	−0.00011 (5)	−0.00135 (5)

Geometric parameters (Å, º) top

C1—O2	1.252 (4)	C9—H9A	0.9700
C1—O1	1.261 (4)	C9—H9B	0.9700
C1—C2	1.503 (4)	C10—O5	1.257 (3)
C2—C7	1.386 (4)	C10—O6	1.260 (3)
C2—C3	1.393 (4)	O1—Tb1	2.352 (2)
C3—C4	1.382 (4)	O2—Tb1ⁱ	2.370 (2)
C3—H3	0.9300	O3—Tb1	2.447 (2)
C4—C5	1.391 (4)	O3—Tb1ⁱ	2.524 (2)
C4—H4	0.9300	O4—Tb1ⁱⁱⁱ	2.492 (2)
C5—C6	1.392 (4)	O4—Tb1ⁱ	2.578 (2)
C5—C10	1.501 (4)	O5—Tb1^iv	2.3359 (19)
C6—C7	1.386 (4)	O6—Tb1^v	2.283 (2)
C6—H6	0.9300	Tb1—O6^vi	2.283 (2)
C7—H7	0.9300	Tb1—O5^vii	2.3359 (19)
C8—O3	1.261 (4)	Tb1—O2^viii	2.370 (2)
C8—O4	1.263 (4)	Tb1—O4^ix	2.492 (2)
C8—C9	1.501 (4)	Tb1—O3^viii	2.524 (2)
C8—Tb1ⁱ	2.932 (3)	Tb1—O4^viii	2.578 (2)
C9—C9ⁱⁱ	1.521 (6)	Tb1—C8^viii	2.932 (3)

O2—C1—O1	124.4 (3)	C8—O4—Tb1ⁱⁱⁱ	130.8 (2)
O2—C1—C2	117.7 (3)	C8—O4—Tb1ⁱ	93.10 (17)
O1—C1—C2	117.9 (3)	Tb1ⁱⁱⁱ—O4—Tb1ⁱ	108.64 (7)
C7—C2—C3	119.8 (3)	C10—O5—Tb1^iv	134.11 (18)
C7—C2—C1	120.7 (3)	C10—O6—Tb1^v	154.76 (19)
C3—C2—C1	119.4 (3)	O6^vi—Tb1—O5^vii	86.13 (7)
C4—C3—C2	120.1 (3)	O6^vi—Tb1—O1	105.02 (8)
C4—C3—H3	120.0	O5^vii—Tb1—O1	151.11 (8)
C2—C3—H3	120.0	O6^vi—Tb1—O2^viii	75.44 (8)
C3—C4—C5	120.3 (3)	O5^vii—Tb1—O2^viii	134.79 (8)
C3—C4—H4	119.8	O1—Tb1—O2^viii	74.10 (9)
C5—C4—H4	119.8	O6^vi—Tb1—O3	80.00 (7)
C4—C5—C6	119.5 (3)	O5^vii—Tb1—O3	81.91 (7)
C4—C5—C10	120.4 (3)	O1—Tb1—O3	74.17 (8)
C6—C5—C10	120.2 (3)	O2^viii—Tb1—O3	132.69 (8)
C7—C6—C5	120.3 (3)	O6^vi—Tb1—O4^ix	103.49 (7)
C7—C6—H6	119.9	O5^vii—Tb1—O4^ix	74.84 (7)
C5—C6—H6	119.9	O1—Tb1—O4^ix	126.02 (8)
C6—C7—C2	120.1 (3)	O2^viii—Tb1—O4^ix	70.12 (8)
C6—C7—H7	120.0	O3—Tb1—O4^ix	156.11 (7)
C2—C7—H7	120.0	O6^vi—Tb1—O3^viii	166.21 (7)
O3—C8—O4	119.4 (3)	O5^vii—Tb1—O3^viii	96.79 (7)
O3—C8—C9	120.2 (3)	O1—Tb1—O3^viii	78.76 (8)
O4—C8—C9	120.3 (3)	O2^viii—Tb1—O3^viii	93.23 (8)
O3—C8—Tb1ⁱ	58.93 (15)	O3—Tb1—O3^viii	113.73 (5)
O4—C8—Tb1ⁱ	61.42 (15)	O4^ix—Tb1—O3^viii	64.62 (7)
C9—C8—Tb1ⁱ	170.4 (2)	O6^vi—Tb1—O4^viii	143.04 (7)
C8—C9—C9ⁱⁱ	107.6 (3)	O5^vii—Tb1—O4^viii	79.52 (7)
C8—C9—H9A	110.2	O1—Tb1—O4^viii	75.72 (8)
C9ⁱⁱ—C9—H9A	110.2	O2^viii—Tb1—O4^viii	136.68 (8)
C8—C9—H9B	110.2	O3—Tb1—O4^viii	64.43 (7)
C9ⁱⁱ—C9—H9B	110.2	O4^ix—Tb1—O4^viii	105.25 (6)
H9A—C9—H9B	108.5	O3^viii—Tb1—O4^viii	50.58 (6)
O5—C10—O6	123.8 (2)	O6^vi—Tb1—C8^viii	168.43 (8)
O5—C10—C5	118.4 (2)	O5^vii—Tb1—C8^viii	90.44 (8)
O6—C10—C5	117.8 (2)	O1—Tb1—C8^viii	73.28 (9)
C1—O1—Tb1	141.6 (2)	O2^viii—Tb1—C8^viii	114.33 (9)
C1—O2—Tb1ⁱ	124.6 (2)	O3—Tb1—C8^viii	88.58 (7)
C8—O3—Tb1	151.30 (19)	O4^ix—Tb1—C8^viii	86.20 (8)
C8—O3—Tb1ⁱ	95.72 (17)	O3^viii—Tb1—C8^viii	25.35 (7)
Tb1—O3—Tb1ⁱ	111.92 (8)	O4^viii—Tb1—C8^viii	25.48 (7)

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

Experimental details

Crystal data
Chemical formula	[Tb₂(C₄H₄O₄)(C₈H₄O₄)₂]
M_r	381.07
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	293
a, b, c (Å)	13.948 (3), 6.8724 (14), 21.844 (4)
V (Å³)	2093.9 (7)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	6.77
Crystal size (mm)	0.29 × 0.27 × 0.20

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.121, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	18548, 2376, 2135
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.017, 0.041, 1.07
No. of reflections	2376
No. of parameters	154
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.10, −0.44

Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Acknowledgements

The author thanks the Beihua University for supporting this work.

References

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