Poly[diaqua-μ2-oxalato-di-μ4-succinato-diyttrium(III)]

Li, Z.-F.; Wang, C.-X.; Wang, P.

doi:10.1107/S1600536809032085

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 9| September 2009| Page m1095

doi:10.1107/S1600536809032085

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Poly[diaqua-μ₂-oxalato-di-μ₄-succinato-diyttrium(III)]

Zhi-Feng Li,^a ^* Chun-Xiang Wang ^a and Ping Wang ^a

^aSchool of Materials and Chemical Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, People's Republic of China
^*Correspondence e-mail: jxlzfeng@yahoo.com.cn

(Received 8 August 2009; accepted 13 August 2009; online 19 August 2009)

In the title compound, [Y₂(C₄H₄O₄)₂(C₂O₄)(H₂O)₂]_n, the flexible succinate anion assumes a gauche conformation and bridges the eight-coordinated Y atoms, generating two-dimensional layers parallel to (010). The coordination polymer layers are linked into a three-dimensional framework by the rigid oxalate ligands. The oxalate ions are located on a center of inversion. Intermolecular O—H⋯O hydrogen bonds help to stabilize the crystal structure.

Related literature

The title compound is isostructural with [Nd₂(C₄H₄O₄)₂(C₂O₄)(H₂O)], see: Wang et al. (2007 ). For bond lengths and angles in succinate anions, see: Seguatni et al. (2004 ).

Experimental

Crystal data

[Y₂(C₄H₄O₄)₂(C₂O₄)(H₂O)₂]
M_r = 534.02
Triclinic, $[P \overline 1]$
a = 6.610 (2) Å
b = 7.689 (3) Å
c = 8.018 (3) Å
α = 101.589 (5)°
β = 101.843 (4)°
γ = 101.492 (5)°
V = 378.2 (2) Å³
Z = 1
Mo Kα radiation
μ = 7.71 mm⁻¹
T = 295 K
0.21 × 0.18 × 0.09 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.215, T_max = 0.505
2108 measured reflections
1482 independent reflections
1376 reflections with I > 2σ(I)
R_int = 0.016

Refinement

R[F² > 2σ(F²)] = 0.022
wR(F²) = 0.059
S = 1.08
1482 reflections
119 parameters
H-atom parameters constrained
Δρ_max = 0.60 e Å⁻³
Δρ_min = −0.54 e Å⁻³

Table 1
Selected bond lengths (Å)

Y—O1	2.4755 (18)
Y—O1ⁱ	2.3319 (19)
Y—O2	2.4658 (19)
Y—O3ⁱⁱ	2.303 (2)
Y—O4ⁱⁱⁱ	2.218 (2)
Y—O5	2.3876 (19)
Y—O6^iv	2.3583 (19)
Y—O7	2.391 (2)
Symmetry codes: (i) -x+1, -y+1, -z+2; (ii) x+1, y, z; (iii) -x, -y+1, -z+1; (iv) -x+1, -y+2, -z+2.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O2^v	0.85	2.02	2.867 (5)	175
O7—H7B⋯O5ⁱⁱ	0.85	1.96	2.812 (4)	175
Symmetry codes: (ii) x+1, y, z; (v) -x+1, -y+1, -z+1.

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: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809032085/jj2005sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809032085/jj2005Isup2.hkl

checkCIF report

Comment top

The title compound (I), is isostructural with [Nd₂(C₄H₄O₄)₂(C₂O₄)(H₂O)] [Wang et al., 2007]. As shown in Fig.1, the asymmetric unit consists of one Y³⁺ cation, one succinate anion, a half of oxalate anion and one aqua ligand. The Y atoms are each coordinated by eight oxygen atoms of four succinate anions, one oxalate anion and one aqua ligand to complete a distorted square antiprismatic geometry. The Y-O distances range from 2.218 (2) to 2.4755 (18) Å.

In (I), the succinate anions assume a gauche conformation, in which both carboxylate groups exhibit different coordination modes: a common bidentate bridging mode and a tridentate chelating-bridging mode. In this mode, the Y atoms are linked into a two-dimensional polymeric sheet parallel to the (010) plane. These sheets are in turn bridged via oxalate ligands. Both lengths and angles within the succinate anions exhibit normal values [Seguatni et al., 2004]. The oxalate ions locate on a center of inversion and act as double bidentate (tetradentate) ligands in a linear chain which connect two Y atoms in two different layers to form a 3D framework (Fig.2). The aqua ligands donate hydrogen atoms to carboxylate oxygen atoms O2 and O5 to form hydrogen bonds, which make a significant contribution to the stabilization of the crystal structure of the title yttrium compound.

Related literature top

The title compound is isostructural with [Nd₂(C₄H₄O₄)₂(C₂O₄)(H₂O)], see: Wang et al. (2007). For bond lengths and angles in succinate anions, see: Seguatni et al. (2004).

Experimental top

A mixture of YCl₃.6H₂O (1.00 mmol, 0.30 g), oxalic acid (0.50 mmol, 0.05 g), succinic acid (0.50 mmol, 0.06 g), NaOH (2.00 mmol, 0.08 g) and H₂O (10.0 ml) was heated in a 23 ml stainless steel reactor with a Teflon liner at 443 K for 48 h. The colorless plate-like crystals were filtered and washed with water and acetone. Yield: 26% based on Y.

Computing details top

Data collection: APEX2 (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 the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. Symmetry code: (i) 1 - x, 1 - y, 1 - z; (ii) x + 1, y, z; (iii) -x, 1 - y, 1 - z; (iv) 1 - x, 2 - y, 2 - z; (v) x - 1, y, z.
	Fig. 2. The three-dimensional framework of the title compound.

Poly[diaqua-µ₂-oxalato-di-µ₄-succinato-diyttrium(III)] top

Crystal data top

[Y₂(C₄H₄O₄)₂(C₂O₄)(H₂O)₂]	Z = 1
M_r = 534.02	F(000) = 262
Triclinic, P1	D_x = 2.345 Mg m⁻³
Hall symbol: -p 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.610 (2) Å	Cell parameters from 336 reflections
b = 7.689 (3) Å	θ = 2.1–27.8°
c = 8.018 (3) Å	µ = 7.71 mm⁻¹
α = 101.589 (5)°	T = 295 K
β = 101.843 (4)°	Plate, colorless
γ = 101.492 (5)°	0.21 × 0.18 × 0.09 mm
V = 378.2 (2) Å³

Data collection top

Bruker APEXII CCD area-detector diffractometer	1482 independent reflections
Radiation source: fine-focus sealed tube	1376 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.016
ϕ and ω scans	θ_max = 26.2°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −8→7
T_min = 0.215, T_max = 0.505	k = −6→9
2108 measured reflections	l = −9→9

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.022	H-atom parameters constrained
wR(F²) = 0.059	w = 1/[σ²(F_o²) + (0.0373P)²] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.001
1482 reflections	Δρ_max = 0.60 e Å⁻³
119 parameters	Δρ_min = −0.54 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.017 (3)

Crystal data top

[Y₂(C₄H₄O₄)₂(C₂O₄)(H₂O)₂]	γ = 101.492 (5)°
M_r = 534.02	V = 378.2 (2) Å³
Triclinic, P1	Z = 1
a = 6.610 (2) Å	Mo Kα radiation
b = 7.689 (3) Å	µ = 7.71 mm⁻¹
c = 8.018 (3) Å	T = 295 K
α = 101.589 (5)°	0.21 × 0.18 × 0.09 mm
β = 101.843 (4)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	1482 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	1376 reflections with I > 2σ(I)
T_min = 0.215, T_max = 0.505	R_int = 0.016
2108 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	0 restraints
wR(F²) = 0.059	H-atom parameters constrained
S = 1.08	Δρ_max = 0.60 e Å⁻³
1482 reflections	Δρ_min = −0.54 e Å⁻³
119 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
Y	0.53610 (4)	0.62226 (3)	0.80635 (3)	0.01351 (12)
C1	0.1559 (4)	0.3484 (3)	0.7710 (3)	0.0152 (5)
C2	−0.0273 (4)	0.1915 (4)	0.7540 (4)	0.0252 (6)
H2A	−0.0878	0.2200	0.8536	0.030*
H2B	0.0271	0.0844	0.7616	0.030*
C3	−0.2057 (4)	0.1422 (4)	0.5858 (4)	0.0216 (6)
H3B	−0.1424	0.1425	0.4868	0.026*
H3A	−0.2900	0.0186	0.5697	0.026*
C4	−0.3519 (4)	0.2691 (4)	0.5834 (3)	0.0181 (6)
C5	0.3783 (4)	0.9630 (4)	0.9836 (3)	0.0161 (5)
O1	0.2979 (3)	0.4094 (2)	0.9192 (2)	0.0192 (4)
O2	0.1803 (3)	0.4203 (3)	0.6480 (2)	0.0213 (4)
O3	−0.3798 (4)	0.3458 (3)	0.7273 (3)	0.0332 (5)
O4	−0.4457 (3)	0.2882 (3)	0.4388 (3)	0.0330 (5)
O5	0.3011 (3)	0.7981 (2)	0.8991 (3)	0.0214 (4)
O6	0.2800 (3)	1.0725 (2)	1.0435 (3)	0.0210 (4)
O7	0.8645 (3)	0.6937 (3)	0.7236 (3)	0.0280 (5)
H7A	0.8427	0.6564	0.6127	0.042*
H7B	0.9949	0.7307	0.7811	0.042*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Y	0.01401 (16)	0.01412 (16)	0.01224 (16)	0.00374 (10)	0.00208 (9)	0.00406 (10)
C1	0.0149 (12)	0.0151 (13)	0.0164 (12)	0.0070 (10)	0.0039 (10)	0.0029 (10)
C2	0.0170 (13)	0.0255 (16)	0.0329 (15)	0.0021 (11)	0.0000 (12)	0.0171 (12)
C3	0.0149 (13)	0.0161 (14)	0.0275 (15)	0.0002 (10)	0.0005 (11)	−0.0001 (11)
C4	0.0177 (13)	0.0132 (13)	0.0199 (13)	−0.0011 (10)	0.0002 (10)	0.0059 (10)
C5	0.0145 (13)	0.0172 (13)	0.0169 (12)	0.0033 (10)	0.0024 (10)	0.0071 (10)
O1	0.0187 (9)	0.0201 (10)	0.0139 (9)	−0.0003 (8)	−0.0016 (7)	0.0044 (7)
O2	0.0216 (10)	0.0232 (10)	0.0162 (9)	−0.0001 (8)	0.0013 (7)	0.0076 (8)
O3	0.0434 (13)	0.0273 (12)	0.0304 (11)	0.0170 (10)	0.0105 (10)	0.0013 (9)
O4	0.0275 (11)	0.0441 (14)	0.0311 (11)	0.0075 (10)	0.0012 (9)	0.0253 (10)
O5	0.0160 (9)	0.0153 (10)	0.0290 (10)	0.0017 (7)	0.0049 (8)	−0.0004 (8)
O6	0.0164 (9)	0.0165 (10)	0.0301 (10)	0.0051 (8)	0.0074 (8)	0.0036 (8)
O7	0.0167 (9)	0.0412 (13)	0.0207 (10)	0.0033 (9)	0.0032 (8)	0.0012 (9)

Geometric parameters (Å, º) top

Y—O1	2.4755 (18)	C2—H2A	0.9700
Y—O1ⁱ	2.3319 (19)	C2—H2B	0.9700
Y—O2	2.4658 (19)	C3—C4	1.504 (4)
Y—O3ⁱⁱ	2.303 (2)	C3—H3B	0.9700
Y—O4ⁱⁱⁱ	2.218 (2)	C3—H3A	0.9700
Y—O5	2.3876 (19)	C4—O4	1.249 (3)
Y—O6^iv	2.3583 (19)	C4—O3	1.253 (3)
Y—O7	2.391 (2)	C5—O6	1.243 (3)
Y—Yⁱ	4.0005 (11)	C5—O5	1.258 (3)
C1—O2	1.246 (3)	C5—C5^iv	1.544 (5)
C1—O1	1.287 (3)	O7—H7A	0.8495
C1—C2	1.491 (4)	O7—H7B	0.8503
C2—C3	1.522 (4)

O4ⁱⁱⁱ—Y—O3ⁱⁱ	106.90 (8)	O5—Y—Yⁱ	86.67 (5)
O4ⁱⁱⁱ—Y—O1ⁱ	165.91 (7)	O7—Y—Yⁱ	123.69 (5)
O3ⁱⁱ—Y—O1ⁱ	78.99 (7)	O2—Y—Yⁱ	84.57 (5)
O4ⁱⁱⁱ—Y—O6^iv	89.63 (8)	O1—Y—Yⁱ	32.56 (4)
O3ⁱⁱ—Y—O6^iv	137.24 (8)	C1—Y—Yⁱ	58.88 (5)
O1ⁱ—Y—O6^iv	77.83 (7)	O2—C1—O1	118.6 (2)
O4ⁱⁱⁱ—Y—O5	82.76 (8)	O2—C1—C2	123.3 (2)
O3ⁱⁱ—Y—O5	151.09 (8)	O1—C1—C2	118.1 (2)
O1ⁱ—Y—O5	98.21 (7)	O2—C1—Y	59.11 (13)
O6^iv—Y—O5	68.11 (6)	O1—C1—Y	59.69 (12)
O4ⁱⁱⁱ—Y—O7	76.30 (8)	C2—C1—Y	173.79 (19)
O3ⁱⁱ—Y—O7	74.60 (8)	C1—C2—C3	115.8 (2)
O1ⁱ—Y—O7	93.43 (7)	C1—C2—H2A	108.3
O6^iv—Y—O7	71.50 (7)	C3—C2—H2A	108.3
O5—Y—O7	134.23 (7)	C1—C2—H2B	108.3
O4ⁱⁱⁱ—Y—O2	74.88 (7)	C3—C2—H2B	108.3
O3ⁱⁱ—Y—O2	79.10 (7)	H2A—C2—H2B	107.4
O1ⁱ—Y—O2	119.12 (6)	C4—C3—C2	114.3 (2)
O6^iv—Y—O2	143.65 (7)	C4—C3—H3B	108.7
O5—Y—O2	77.31 (7)	C2—C3—H3B	108.7
O7—Y—O2	132.82 (7)	C4—C3—H3A	108.7
O4ⁱⁱⁱ—Y—O1	126.14 (7)	C2—C3—H3A	108.7
O3ⁱⁱ—Y—O1	75.63 (8)	H3B—C3—H3A	107.6
O1ⁱ—Y—O1	67.40 (7)	O4—C4—O3	123.0 (3)
O6^iv—Y—O1	125.61 (6)	O4—C4—C3	118.9 (3)
O5—Y—O1	76.79 (7)	O3—C4—C3	118.0 (2)
O7—Y—O1	147.15 (7)	O6—C5—O5	127.1 (2)
O2—Y—O1	52.31 (6)	O6—C5—C5^iv	116.6 (3)
O4ⁱⁱⁱ—Y—C1	100.33 (8)	O5—C5—C5^iv	116.3 (3)
O3ⁱⁱ—Y—C1	74.65 (8)	C1—O1—Yⁱ	151.33 (16)
O1ⁱ—Y—C1	93.56 (7)	C1—O1—Y	93.65 (15)
O6^iv—Y—C1	141.99 (7)	Yⁱ—O1—Y	112.60 (7)
O5—Y—C1	76.83 (7)	C1—O2—Y	95.19 (15)
O7—Y—C1	146.47 (7)	C4—O3—Y^v	129.0 (2)
O2—Y—C1	25.70 (7)	C4—O4—Yⁱⁱⁱ	165.24 (19)
O1—Y—C1	26.66 (7)	C5—O5—Y	118.76 (16)
O4ⁱⁱⁱ—Y—Yⁱ	158.49 (6)	C5—O6—Y^iv	120.22 (16)
O3ⁱⁱ—Y—Yⁱ	74.64 (6)	Y—O7—H7A	110.0
O1ⁱ—Y—Yⁱ	34.84 (4)	Y—O7—H7B	133.6
O6^iv—Y—Yⁱ	103.73 (5)	H7A—O7—H7B	115.4

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O2^vi	0.85	2.02	2.867 (5)	175
O7—H7B···O5ⁱⁱ	0.85	1.96	2.812 (4)	175

Symmetry codes: (ii) x+1, y, z; (vi) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Y₂(C₄H₄O₄)₂(C₂O₄)(H₂O)₂]
M_r	534.02
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	6.610 (2), 7.689 (3), 8.018 (3)
α, β, γ (°)	101.589 (5), 101.843 (4), 101.492 (5)
V (Å³)	378.2 (2)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	7.71
Crystal size (mm)	0.21 × 0.18 × 0.09

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.215, 0.505
No. of measured, independent and observed [I > 2σ(I)] reflections	2108, 1482, 1376
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.622

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.059, 1.08
No. of reflections	1482
No. of parameters	119
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.60, −0.54

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Y—O1	2.4755 (18)	Y—O4ⁱⁱⁱ	2.218 (2)
Y—O1ⁱ	2.3319 (19)	Y—O5	2.3876 (19)
Y—O2	2.4658 (19)	Y—O6^iv	2.3583 (19)
Y—O3ⁱⁱ	2.303 (2)	Y—O7	2.391 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O2^v	0.85	2.02	2.867 (5)	175
O7—H7B···O5ⁱⁱ	0.85	1.96	2.812 (4)	175

Symmetry codes: (ii) x+1, y, z; (v) −x+1, −y+1, −z+1.

Acknowledgements

This work is supported by the Jiangxi Provincial Educational foundation (GJJ09227) and the Jiangxi Provincial Natural Science Foundation (No. 0620018).

References

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