Poly[μ6-adipato-diaquadi-μ2-oxalato-digadolinium(III)]

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

doi:10.1107/S1600536810036111

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 10| October 2010| Page m1263

doi:10.1107/S1600536810036111

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Poly[μ₆-adipato-diaquadi-μ₂-oxalato-digadolinium(III)]

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

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

(Received 26 August 2010; accepted 8 September 2010; online 15 September 2010)

In the centrosymmetric title compound, [Gd₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]_n, the Gd³⁺ cations are each coordinated by nine O atoms, three from adipate anions, two from oxalate anions and one from an aqua ligand, completing a distorted tricapped trigonal-prismatic geometry. These tricapped trigonal prisms are bridged by the adipate ligands, generating layers lying parallel to (010). The coordination polymer layers are linked into a three-dimensional framework by the rigid oxalate ligands. The adipate and oxalate ions are all located on centers of inversion. A part of the adipate anion is disordered over two positions in a 0.75:0.25 ratio.

Related literature

For structures involving adipate ligands and lanthanide ions, see: Dimos et al. (2002 ). For structures involving oxalate ligands and lanthanide ions, see: Trombe & Mohanu (2004 ).

Experimental

Crystal data

[Gd₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]
M_r = 670.70
Triclinic, $[P \overline 1]$
a = 6.815 (4) Å
b = 6.982 (4) Å
c = 8.997 (7) Å
α = 104.759 (10)°
β = 108.11 (1)°
γ = 104.320 (7)°
V = 367.8 (4) Å³
Z = 1
Mo Kα radiation
μ = 9.02 mm⁻¹
T = 295 K
0.23 × 0.11 × 0.08 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.241, T_max = 0.491
1751 measured reflections
1236 independent reflections
1157 reflections with I > 2σ(I)
R_int = 0.013

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.059
S = 1.05
1236 reflections
127 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.56 e Å⁻³
Δρ_min = −1.41 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O3ⁱ	0.84 (6)	2.00 (5)	2.799 (4)	160
O7—H7B⋯O6ⁱⁱ	0.83 (7)	2.07 (7)	2.888 (5)	168
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x, -y+1, -z.

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/S1600536810036111/su2209sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810036111/su2209Isup2.hkl

checkCIF report

Comment top

As shown in Fig. 1 the asymmetric unit of the title compound consists of one Gd³⁺ cation, half of an adipate anion, two half oxalate anions and one aqua ligand. The Gd atom is coordinated by nine oxygen atoms, in which four oxygen atoms are from three adipate anions, four from two oxalate anions and one from a water molecule, to form a SmO₉ polyhedron with a distorted tricapped trigonal-prismatic geometry. The Gd—O(adipate) distances vary in the range of 2.430 (4)–2.575 (4) Å (average 2.512 (4) Å), which is nearly identical to the value of 2.425 (8)–2.611 (8) Å (average 2.471 (8) Å) observed in Gd₂(C₆H₈O₄)₃(H₂O)₄ (Dimos et al., 2002). The Gd—O(oxalate) distances are in the range of 2.385 (4)–2.540 (4) Å, which are usual for lanthanide oxalates complexes (Trombe & Mohanu, 2004). In the title complex, the adipate anions are located on inversion centers and atom C3 is positionally disordered (C3A and C3B; occupancies 0.75/0.25). Two carboxylate oxygen atoms chelate one Gd atom with each oxygen atom additionally bonded to another Gd atom. To the best of our knowledge, this η²,µ₃-η²,µ₃-chelating-bridging octadentate coordination mode of the adipate ligand has not been reported previously.

Through the terminal carboxylato bridging interactions, the GdO₉ polyhedra are edged-shared to generate metal-oxygen chains extending infinitely along [100], in which the adjacent Gd···Gd distances are 4.23 (3) Å and 4.25 (2) Å, respectively. Along [001] the chains are linked by the adipate anions into layers parallel to (010) (Fig. 2). Two symmetry independent oxalate ions are also located on centers of inversion and act as double bidentate (tetradentate) ligands in a linear chain, which connect Gd atoms to form zigzag chains along [001]. Through the oxalate and adipate ligand bridging interactions, the Gd atoms build up a three-dimensional open framework with the channels propagating in [001] (Fig. 3). The aqua ligand provides H-bond donors which participate in O-H···O hydrogen bonds with the oxalate atoms O3 and O6 (Table 1).

Related literature top

For structures involving adipate ligands and lanthanide ions, see: Dimos et al. (2002). For structures involving oxalate ligands and lanthanide ions, see: Trombe & Mohanu (2004).

Experimental top

A mixture of GdCl₃.6H₂O(1.00 mmol, 0.36 g), oxalic acid (0.50 mmol, 0.05 g), adipic acid (0.50 mmol, 0.07 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. On cooling a small amount of colorless plate-like crystals were obtained.They were filtered off and washed with water and acetone.

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 fragment of the molecuar structure of the title compound, with the atom-numbering scheme. Displacement ellipsoidsare drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. Symmetry codes: (i) -x, 1 - y, 1 - z; (ii) 1 - x, 1 - y, 1 - z; (iii) -x, - y, 1- z; (iv) - x, - y, -z; (v) 1 - x, 1 - y, 2 - z.
	Fig. 2. A view along the b-axis of the two-dimensional layer structure formed by the connectivity between the Gd atoms and the adipate moieties present in the title compound [the C-bound H-atoms and atom C3B have been omitted for clarity].
	Fig. 3. A view along the c-axis of the three-dimensional framework of the title compound [the C-bound H-atoms and atom C3B have been omitted for clarity].

Poly[µ₆-adipato-diaquadi-µ₂-oxalato-digadolinium(III)] top

Crystal data top

[Gd₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]	Z = 1
M_r = 670.70	F(000) = 312
Triclinic, P1	D_x = 3.028 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.815 (4) Å	Cell parameters from 238 reflections
b = 6.982 (4) Å	θ = 2.6–28.3°
c = 8.997 (7) Å	µ = 9.02 mm⁻¹
α = 104.759 (10)°	T = 295 K
β = 108.11 (1)°	Plate, colorless
γ = 104.320 (7)°	0.23 × 0.11 × 0.08 mm
V = 367.8 (4) Å³

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	1236 independent reflections
Radiation source: fine-focus sealed tube	1157 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.013
ϕ and ω scans	θ_max = 25.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −7→8
T_min = 0.241, T_max = 0.491	k = −7→8
1751 measured reflections	l = −9→10

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0451P)²] where P = (F_o² + 2F_c²)/3
1236 reflections	(Δ/σ)_max < 0.001
127 parameters	Δρ_max = 1.56 e Å⁻³
2 restraints	Δρ_min = −1.41 e Å⁻³

Crystal data top

[Gd₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]	γ = 104.320 (7)°
M_r = 670.70	V = 367.8 (4) Å³
Triclinic, P1	Z = 1
a = 6.815 (4) Å	Mo Kα radiation
b = 6.982 (4) Å	µ = 9.02 mm⁻¹
c = 8.997 (7) Å	T = 295 K
α = 104.759 (10)°	0.23 × 0.11 × 0.08 mm
β = 108.11 (1)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	1236 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	1157 reflections with I > 2σ(I)
T_min = 0.241, T_max = 0.491	R_int = 0.013
1751 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	2 restraints
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	Δρ_max = 1.56 e Å⁻³
1236 reflections	Δρ_min = −1.41 e Å⁻³
127 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	Occ. (<1)
Gd	0.15528 (4)	0.34583 (3)	0.36187 (3)	0.01206 (12)
O1	0.1523 (6)	0.5226 (6)	0.6494 (4)	0.0175 (8)
O2	0.4788 (6)	0.5964 (5)	0.6393 (4)	0.0156 (8)
O3	0.2680 (6)	0.1539 (6)	0.5394 (4)	0.0168 (8)
O4	0.1538 (6)	−0.0817 (6)	0.6500 (5)	0.0191 (8)
O5	−0.0130 (7)	0.2517 (6)	0.0669 (4)	0.0191 (8)
O6	−0.1324 (7)	0.0169 (6)	−0.1924 (5)	0.0210 (9)
O7	0.2703 (7)	0.6881 (6)	0.3356 (5)	0.0218 (9)
H7A	0.403 (5)	0.763 (10)	0.370 (8)	0.033*
H7B	0.218 (12)	0.757 (10)	0.281 (8)	0.033*
C1	0.3614 (9)	0.6107 (8)	0.7255 (7)	0.0144 (11)
C2	0.4651 (10)	0.7225 (9)	0.9107 (7)	0.0193 (12)
H2A	0.4012	0.8285	0.9405	0.023*	0.75
H2B	0.6218	0.7953	0.9448	0.023*	0.75
H2C	0.3517	0.7421	0.9503	0.023*	0.25
H2D	0.5696	0.8616	0.9373	0.023*	0.25
C3A	0.4343 (15)	0.5720 (14)	1.0070 (10)	0.0262 (17)	0.75
H3A1	0.4800	0.6550	1.1242	0.031*	0.75
H3A2	0.2790	0.4864	0.9633	0.031*	0.75
C3B	0.588 (4)	0.598 (4)	1.005 (3)	0.0262 (17)	0.25
H3B1	0.6830	0.5544	0.9531	0.031*	0.25
H3B2	0.6791	0.6879	1.1213	0.031*	0.25
C4	0.1222 (8)	0.0203 (8)	0.5547 (6)	0.0140 (11)
C5	−0.0433 (9)	0.0774 (8)	−0.0367 (7)	0.0143 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd	0.00971 (18)	0.01274 (17)	0.00989 (17)	0.00183 (12)	0.00225 (12)	0.00217 (11)
O1	0.016 (2)	0.0173 (19)	0.0148 (19)	0.0059 (16)	0.0033 (16)	0.0017 (16)
O2	0.013 (2)	0.0160 (19)	0.0132 (19)	0.0034 (16)	0.0050 (16)	0.0007 (15)
O3	0.011 (2)	0.0182 (19)	0.0161 (19)	0.0011 (16)	0.0029 (16)	0.0050 (16)
O4	0.013 (2)	0.021 (2)	0.020 (2)	0.0031 (17)	0.0015 (16)	0.0105 (17)
O5	0.021 (2)	0.018 (2)	0.0131 (19)	0.0066 (17)	0.0035 (16)	0.0023 (16)
O6	0.027 (2)	0.021 (2)	0.014 (2)	0.0086 (18)	0.0061 (18)	0.0053 (17)
O7	0.017 (2)	0.020 (2)	0.029 (2)	0.0045 (18)	0.0081 (19)	0.0134 (18)
C1	0.016 (3)	0.011 (2)	0.013 (3)	0.006 (2)	0.002 (2)	0.005 (2)
C2	0.015 (3)	0.020 (3)	0.018 (3)	0.003 (2)	0.006 (2)	0.003 (2)
C3A	0.026 (4)	0.037 (4)	0.016 (4)	0.013 (4)	0.009 (3)	0.007 (4)
C3B	0.026 (4)	0.037 (4)	0.016 (4)	0.013 (4)	0.009 (3)	0.007 (4)
C4	0.009 (3)	0.016 (3)	0.012 (3)	0.003 (2)	0.002 (2)	0.001 (2)
C5	0.008 (3)	0.016 (3)	0.016 (3)	0.001 (2)	0.004 (2)	0.003 (2)

Geometric parameters (Å, º) top

Gd—O1	2.575 (4)	O7—H7B	0.83 (7)
Gd—O1ⁱ	2.473 (4)	C1—C2	1.489 (8)
Gd—O2	2.569 (4)	C2—C3A	1.538 (10)
Gd—O2ⁱⁱ	2.430 (4)	C2—C3B	1.57 (3)
Gd—O3	2.403 (4)	C2—H2A	0.9700
Gd—O4ⁱⁱⁱ	2.385 (4)	C2—H2B	0.9700
Gd—O5	2.374 (4)	C2—H2C	0.9700
Gd—O6^iv	2.540 (4)	C2—H2D	0.9700
Gd—O7	2.420 (4)	C3A—C3A^v	1.510 (16)
O1—C1	1.274 (7)	C3A—H3A1	0.9700
O2—C1	1.279 (6)	C3A—H3A2	0.9700
O3—C4	1.252 (7)	C3B—C3B^v	1.54 (5)
O4—C4	1.249 (6)	C3B—H3B1	0.9700
O5—C5	1.253 (6)	C3B—H3B2	0.9700
O6—C5	1.246 (7)	C4—C4ⁱⁱⁱ	1.558 (10)
O7—H7A	0.84 (6)	C5—C5^iv	1.546 (10)

O5—Gd—O4ⁱⁱⁱ	89.95 (13)	C4—O3—Gd	118.6 (3)
O5—Gd—O3	133.53 (13)	C4—O4—Gdⁱⁱⁱ	119.1 (3)
O4ⁱⁱⁱ—Gd—O3	68.29 (13)	C5—O5—Gd	123.7 (3)
O5—Gd—O7	78.95 (14)	C5—O6—Gd^iv	117.9 (3)
O4ⁱⁱⁱ—Gd—O7	142.92 (13)	Gd—O7—H7A	122 (5)
O3—Gd—O7	141.60 (14)	Gd—O7—H7B	139 (5)
O5—Gd—O2ⁱⁱ	92.50 (13)	H7A—O7—H7B	97 (7)
O4ⁱⁱⁱ—Gd—O2ⁱⁱ	142.01 (12)	O1—C1—O2	118.3 (5)
O3—Gd—O2ⁱⁱ	83.07 (12)	O1—C1—C2	120.4 (5)
O7—Gd—O2ⁱⁱ	74.35 (13)	O2—C1—C2	121.2 (5)
O5—Gd—O1ⁱ	81.91 (12)	O1—C1—Gd	59.4 (3)
O4ⁱⁱⁱ—Gd—O1ⁱ	69.18 (13)	O2—C1—Gd	59.1 (3)
O3—Gd—O1ⁱ	122.76 (12)	C2—C1—Gd	174.0 (4)
O7—Gd—O1ⁱ	74.25 (14)	C1—C2—C3A	112.9 (5)
O2ⁱⁱ—Gd—O1ⁱ	148.60 (13)	C1—C2—C3B	112.6 (10)
O5—Gd—O6^iv	65.44 (13)	C1—C2—H2A	109.0
O4ⁱⁱⁱ—Gd—O6^iv	70.90 (14)	C3A—C2—H2A	109.0
O3—Gd—O6^iv	68.66 (13)	C3B—C2—H2A	135.3
O7—Gd—O6^iv	131.77 (14)	C1—C2—H2B	109.0
O2ⁱⁱ—Gd—O6^iv	75.79 (13)	C3A—C2—H2B	109.0
O1ⁱ—Gd—O6^iv	127.57 (13)	C3B—C2—H2B	73.4
O5—Gd—O2	147.43 (13)	H2A—C2—H2B	107.8
O4ⁱⁱⁱ—Gd—O2	122.50 (13)	C1—C2—H2C	109.1
O3—Gd—O2	69.27 (13)	C3A—C2—H2C	73.3
O7—Gd—O2	73.02 (13)	C3B—C2—H2C	109.1
O2ⁱⁱ—Gd—O2	64.38 (14)	H2B—C2—H2C	136.9
O1ⁱ—Gd—O2	105.56 (12)	C1—C2—H2D	109.1
O6^iv—Gd—O2	124.28 (12)	C3A—C2—H2D	134.9
O5—Gd—O1	147.09 (13)	C3B—C2—H2D	109.1
O4ⁱⁱⁱ—Gd—O1	80.01 (13)	H2C—C2—H2D	107.8
O3—Gd—O1	71.21 (13)	C3A^v—C3A—C2	112.2 (8)
O7—Gd—O1	90.34 (13)	C3A^v—C3A—H2C	148.3
O2ⁱⁱ—Gd—O1	114.63 (12)	C3A^v—C3A—H3A1	109.2
O1ⁱ—Gd—O1	65.20 (14)	C2—C3A—H3A1	109.2
O6^iv—Gd—O1	136.78 (12)	H2C—C3A—H3A1	91.7
O2—Gd—O1	50.45 (12)	C3A^v—C3A—H3A2	109.2
O5—Gd—C1	159.72 (13)	C2—C3A—H3A2	109.2
O4ⁱⁱⁱ—Gd—C1	100.86 (14)	H2C—C3A—H3A2	85.5
O3—Gd—C1	66.75 (14)	H3A1—C3A—H3A2	107.9
O7—Gd—C1	82.15 (15)	C3B^v—C3B—C2	108 (2)
O2ⁱⁱ—Gd—C1	89.45 (14)	C3B^v—C3B—H3B1	110.1
O1ⁱ—Gd—C1	85.94 (14)	C2—C3B—H3B1	110.1
O6^iv—Gd—C1	134.31 (13)	C3B^v—C3B—H3B2	110.1
O2—Gd—C1	25.31 (13)	C2—C3B—H3B2	110.1
O1—Gd—C1	25.21 (14)	H3B1—C3B—H3B2	108.4
C1—O1—Gdⁱ	133.0 (3)	O4—C4—O3	126.3 (5)
C1—O1—Gd	95.4 (3)	O4—C4—C4ⁱⁱⁱ	117.1 (6)
Gdⁱ—O1—Gd	114.80 (14)	O3—C4—C4ⁱⁱⁱ	116.6 (6)
C1—O2—Gdⁱⁱ	147.7 (3)	O6—C5—O5	127.0 (5)
C1—O2—Gd	95.5 (3)	O6—C5—C5^iv	116.6 (6)
Gdⁱⁱ—O2—Gd	115.62 (14)	O5—C5—C5^iv	116.4 (6)

O5—Gd—O1—C1	−140.5 (3)	O3—Gd—O5—C5	−8.0 (5)
O4ⁱⁱⁱ—Gd—O1—C1	145.4 (3)	O7—Gd—O5—C5	148.3 (4)
O3—Gd—O1—C1	75.1 (3)	O2ⁱⁱ—Gd—O5—C5	74.8 (4)
O7—Gd—O1—C1	−70.5 (3)	O1ⁱ—Gd—O5—C5	−136.2 (4)
O2ⁱⁱ—Gd—O1—C1	2.4 (3)	O6^iv—Gd—O5—C5	1.7 (4)
O1ⁱ—Gd—O1—C1	−143.0 (4)	O2—Gd—O5—C5	117.5 (4)
O6^iv—Gd—O1—C1	97.7 (3)	O1—Gd—O5—C5	−138.6 (4)
O2—Gd—O1—C1	−3.1 (3)	C1—Gd—O5—C5	170.0 (4)
O5—Gd—O1—Gdⁱ	2.5 (3)	Gdⁱ—O1—C1—O2	−126.2 (4)
O4ⁱⁱⁱ—Gd—O1—Gdⁱ	−71.57 (16)	Gd—O1—C1—O2	5.5 (5)
O3—Gd—O1—Gdⁱ	−141.88 (18)	Gdⁱ—O1—C1—C2	55.3 (6)
O7—Gd—O1—Gdⁱ	72.44 (17)	Gd—O1—C1—C2	−173.1 (4)
O2ⁱⁱ—Gd—O1—Gdⁱ	145.34 (15)	Gdⁱ—O1—C1—Gd	−131.6 (4)
O1ⁱ—Gd—O1—Gdⁱ	−0.001 (2)	Gdⁱⁱ—O2—C1—O1	−170.9 (4)
O6^iv—Gd—O1—Gdⁱ	−119.29 (18)	Gd—O2—C1—O1	−5.5 (5)
O2—Gd—O1—Gdⁱ	139.9 (2)	Gdⁱⁱ—O2—C1—C2	7.6 (9)
C1—Gd—O1—Gdⁱ	143.0 (4)	Gd—O2—C1—C2	173.0 (4)
O5—Gd—O2—C1	139.9 (3)	Gdⁱⁱ—O2—C1—Gd	−165.4 (6)
O4ⁱⁱⁱ—Gd—O2—C1	−34.5 (3)	O5—Gd—C1—O1	86.4 (5)
O3—Gd—O2—C1	−79.2 (3)	O4ⁱⁱⁱ—Gd—C1—O1	−34.7 (3)
O7—Gd—O2—C1	108.2 (3)	O3—Gd—C1—O1	−95.2 (3)
O2ⁱⁱ—Gd—O2—C1	−171.4 (4)	O7—Gd—C1—O1	107.9 (3)
O1ⁱ—Gd—O2—C1	40.5 (3)	O2ⁱⁱ—Gd—C1—O1	−177.9 (3)
O6^iv—Gd—O2—C1	−122.4 (3)	O1ⁱ—Gd—C1—O1	33.2 (3)
O1—Gd—O2—C1	3.1 (3)	O6^iv—Gd—C1—O1	−108.5 (3)
O5—Gd—O2—Gdⁱⁱ	−48.6 (3)	O2—Gd—C1—O1	174.4 (5)
O4ⁱⁱⁱ—Gd—O2—Gdⁱⁱ	136.96 (15)	O5—Gd—C1—O2	−88.0 (5)
O3—Gd—O2—Gdⁱⁱ	92.21 (16)	O4ⁱⁱⁱ—Gd—C1—O2	150.9 (3)
O7—Gd—O2—Gdⁱⁱ	−80.42 (17)	O3—Gd—C1—O2	90.4 (3)
O2ⁱⁱ—Gd—O2—Gdⁱⁱ	0.0	O7—Gd—C1—O2	−66.5 (3)
O1ⁱ—Gd—O2—Gdⁱⁱ	−148.11 (15)	O2ⁱⁱ—Gd—C1—O2	7.7 (3)
O6^iv—Gd—O2—Gdⁱⁱ	49.0 (2)	O1ⁱ—Gd—C1—O2	−141.2 (3)
O1—Gd—O2—Gdⁱⁱ	174.5 (2)	O6^iv—Gd—C1—O2	77.1 (3)
C1—Gd—O2—Gdⁱⁱ	171.4 (4)	O1—Gd—C1—O2	−174.4 (5)
O5—Gd—O3—C4	−72.7 (4)	O1—C1—C2—C3A	66.3 (7)
O4ⁱⁱⁱ—Gd—O3—C4	−5.0 (4)	Gdⁱⁱⁱ—O4—C4—O3	−175.4 (4)
O7—Gd—O3—C4	146.7 (3)	Gdⁱⁱⁱ—O4—C4—C4ⁱⁱⁱ	5.3 (7)
O2ⁱⁱ—Gd—O3—C4	−159.5 (4)	Gd—O3—C4—O4	−175.0 (4)
O1ⁱ—Gd—O3—C4	39.7 (4)	Gd—O3—C4—C4ⁱⁱⁱ	4.3 (7)
O6^iv—Gd—O3—C4	−82.1 (4)	Gd^iv—O6—C5—O5	178.4 (4)
O2—Gd—O3—C4	135.3 (4)	Gd^iv—O6—C5—C5^iv	−0.3 (7)
O1—Gd—O3—C4	81.5 (4)	Gd—O5—C5—O6	179.1 (4)
C1—Gd—O3—C4	108.1 (4)	Gd—O5—C5—C5^iv	−2.1 (8)
O4ⁱⁱⁱ—Gd—O5—C5	−67.3 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O3ⁱⁱ	0.84 (6)	2.00 (5)	2.799 (4)	160
O7—H7B···O6^vi	0.83 (7)	2.07 (7)	2.888 (5)	168

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

Experimental details

Crystal data
Chemical formula	[Gd₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]
M_r	670.70
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	6.815 (4), 6.982 (4), 8.997 (7)
α, β, γ (°)	104.759 (10), 108.11 (1), 104.320 (7)
V (Å³)	367.8 (4)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	9.02
Crystal size (mm)	0.23 × 0.11 × 0.08

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.241, 0.491
No. of measured, independent and observed [I > 2σ(I)] reflections	1751, 1236, 1157
R_int	0.013
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.059, 1.05
No. of reflections	1236
No. of parameters	127
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.56, −1.41

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O3ⁱ	0.84 (6)	2.00 (5)	2.799 (4)	160
O7—H7B···O6ⁱⁱ	0.83 (7)	2.07 (7)	2.888 (5)	168

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

Acknowledgements

This work was supported by the Jiangxi Provincial Educational Foundation (GJJ09227).

References

Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dimos, A., Tsaousis, D., Michaelides, A. & Skoulika, S. (2002). Chem. Mater. 14, 2616–2622. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Trombe, J. C. & Mohanu, A. (2004). Solid State Sci. 6, 1403–1419. Web of Science CSD CrossRef CAS Google Scholar