Poly[[triaqua­(μ3-pyridine-2,4,6-tri­car­boxyl­ato)gadolinium(III)] monohydrate]

Wang, H.-S.; Zhang, W.-Q.

doi:10.1107/S1600536809038793

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 11| November 2009| Page m1271

https://doi.org/10.1107/S1600536809038793

Open

access

Poly[[triaqua(μ₃-pyridine-2,4,6-tricarboxylato)gadolinium(III)] monohydrate]

Hong-Sheng Wang ^a ^* and Wan-Qiang Zhang ^a

^aCollege of Chemistry and Chemical Engineering, Xuchang University, Xuchang, Henan Province 461000, People's Republic of China
^*Correspondence e-mail: xcuwaller@163.com

(Received 10 September 2009; accepted 25 September 2009; online 3 October 2009)

The title compound, {[Gd(C₈H₂NO₆)(H₂O)₃]·H₂O}_n, was obtained in water under hydrothermal conditions. The Gd^III ions are nine-coordinated by two O and one N atoms from one pyridine-2,4,6-tricarboxylate ligand, two O atoms from another ligand, one O atom from a third ligand and three coordinated water molecules. Each ligand binds three metal centers. Two-dimensional layers are formed through the Gd—O bonds and the layers are linked by O—H⋯O hydrogen bonds, forming a three-dimensional network.

Related literature

For related structures, see: Gao et al. (2006 ); Ghosh & Bharadwaj (2005 ); Wang et al. (2007 ); Fu & Xu (2008 ); Li et al. (2008 ). For general background to lanthanide-organic frameworks and their properties, see: Parker (2000 ); Tobisch (2005 ); Pan et al. (2003 ).

Experimental

Crystal data

[Gd(C₈H₂NO₆)(H₂O)₃]·H₂O
M_r = 437.42
Monoclinic, P 2₁ /c
a = 11.896 (3) Å
b = 7.2696 (14) Å
c = 13.505 (3) Å
β = 96.259 (3)°
V = 1160.9 (4) Å³
Z = 4
Mo Kα radiation
μ = 5.77 mm⁻¹
T = 113 K
0.12 × 0.10 × 0.08 mm

Data collection

Rigaku Saturn diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ) T_min = 0.544, T_max = 0.655
10599 measured reflections
2776 independent reflections
2366 reflections with I > 2σ(I)
R_int = 0.038

Refinement

R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.049
S = 1.04
2776 reflections
206 parameters
8 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.64 e Å⁻³
Δρ_min = −1.29 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O1ⁱ	0.82 (2)	2.02 (3)	2.794 (3)	157 (4)
O7—H7B⋯O3ⁱⁱ	0.83 (2)	1.97 (2)	2.795 (3)	175 (4)
O8—H8A⋯O6ⁱⁱⁱ	0.82 (3)	1.80 (3)	2.621 (3)	171 (4)
O8—H8B⋯O4^iv	0.75 (2)	2.22 (3)	2.933 (3)	158 (4)
O9—H9A⋯O6ⁱⁱⁱ	0.82 (2)	2.01 (3)	2.800 (3)	161 (4)
O9—H9B⋯O10	0.83 (2)	1.91 (3)	2.723 (3)	166 (4)
O10—H10A⋯O8^iv	0.81 (2)	2.24 (3)	3.051 (4)	173 (4)
O10—H10B⋯O9^v	0.82 (3)	2.45 (3)	3.169 (4)	148 (4)
Symmetry codes: (i) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) x, y-1, z; (iii) $[-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (v) -x, -y+1, -z+1.

Data collection: CrystalClear (Rigaku/MSC, 2005 ); cell refinement: CrystalClear; data reduction: CrystalClear; 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: CrystalStructure (Rigaku/MSC, 2005).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536809038793/zq2008sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809038793/zq2008Isup2.hkl

checkCIF report

Comment top

The preparation and property researching of metal-organic frameworks have attracted widespread interest in recent years due to their potential application in the areas of magnetism, luminescence, adsorption, catalysis and so on (Parker, 2000; Tobisch, 2005; Pan et al., 2003). Multicarboxylic acids containing pyridyl rings were widely used and many 1-D, 2-D and 3-D coordination polymers with novel structures have been reported. Especially, complexes with pyridine-2,4,6-tricarboxylato (H₃pta = pyridine-2,4,6-tricarboxylic acid) ligands have been recently reported (Li et al., 2008; Wang et al., 2007; Fu et al., 2008.). The title compound is a new Gd^III complex built with pta ligands and prepared under hydrothermal conditions.

As shown in Fig. 1, the local geometry of Gd^III ion is a distorted monocapped antitetragonal prism. Each pta ligand connects three Gd^III ions with oxgen atoms of the carboxyl groups and the nitrogen atom. There are three coordination water molecules on each Gd^III ion. A two-dimentional layer is constructed by the bonding among oxygen atoms and Gd^III ions (see Fig. 2). In addition, a lattice water molecule per asymmetric unit is in the crystal structure. Many O—H···O hydrogen bonds are formed between the oxygen atoms of water molecules and the oxygen atoms of caboxyl groups. As a result, the three-dimensional network formed by hydrogen bonds is shown in Fig. 3.

Related literature top

For related crystal structures, see: Gao et al. (2006); Ghosh & Bharadwaj (2005); Wang et al. (2007); Fu et al. (2008); Li et al. (2008). For general background to lanthanide-organic frameworks and their properties, see: Parker (2000); Tobisch (2005); Pan et al. (2003).

Experimental top

A mixture of H₃pta (0.0422 g, 0.2 mmol), GdCl₃.6H₂O (0.0743 g, 0.2 mmol) and deionized water (15 ml) was put in a teflon-lined steel bomb and heated at 453 K for 3 days, then cooled the bomb at a rate of 2 K/hour. The colorless crystals suitable for X-ray diffraction measurements were obtained. Spectroscopic analysis: IR (KBr, ν cm^-1): 3606, 3382, 1631, 1608, 1582, 1549, 1445, 1395, 1352, 1277, 1235, 1110, 1025, 950, 931, 818, 791, 740, 664, 623, 587, 543, 479, 435. Elemental analysis, calculated for C₈H₁₀GdNO₁₀: C, 21.97; H, 2.30; N, 3.20.%; found: C, 22.18; H, 2.11; N, 3.54%.

Structure description top

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97 (Sheldrick, 2008); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2005).

Figures top

	Fig. 1. The molecular structure of (I), with atom labels and 30% probability displacement ellipsoids for non-H atoms.
	Fig. 2. The packing of (I), showing the two-dimensional layers formed by Gd—O bonds.
	Fig. 3. View of the three-dimensional network constructed by O—H···O hydrogen bonds (dashed lines). All H atoms were omitted for clarity.

Poly[[triaqua(µ₃-pyridine-2,4,6-tricarboxylato)gadolinium(III)] monohydrate] top

Crystal data top

[Gd(C₈H₂NO₆)(H₂O)₃]·H₂O	F(000) = 836
M_r = 437.42	D_x = 2.503 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybc	Cell parameters from 3775 reflections
a = 11.896 (3) Å	θ = 1.7–28.7°
b = 7.2696 (14) Å	µ = 5.77 mm⁻¹
c = 13.505 (3) Å	T = 113 K
β = 96.259 (3)°	Block, colourless
V = 1160.9 (4) Å³	0.12 × 0.10 × 0.08 mm
Z = 4

Data collection top

Rigaku Saturn diffractometer	2776 independent reflections
Radiation source: rotating anode	2366 reflections with I > 2σ(I)
Confocal monochromator	R_int = 0.038
Detector resolution: 7.31 pixels mm^-1	θ_max = 27.9°, θ_min = 1.7°
ω scans	h = −15→15
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −8→9
T_min = 0.544, T_max = 0.655	l = −17→17
10599 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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.049	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0242P)²] where P = (F_o² + 2F_c²)/3
2776 reflections	(Δ/σ)_max = 0.001
206 parameters	Δρ_max = 0.64 e Å⁻³
8 restraints	Δρ_min = −1.29 e Å⁻³

Crystal data top

[Gd(C₈H₂NO₆)(H₂O)₃]·H₂O	V = 1160.9 (4) Å³
M_r = 437.42	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.896 (3) Å	µ = 5.77 mm⁻¹
b = 7.2696 (14) Å	T = 113 K
c = 13.505 (3) Å	0.12 × 0.10 × 0.08 mm
β = 96.259 (3)°

Data collection top

Rigaku Saturn diffractometer	2776 independent reflections
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	2366 reflections with I > 2σ(I)
T_min = 0.544, T_max = 0.655	R_int = 0.038
10599 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	8 restraints
wR(F²) = 0.049	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.64 e Å⁻³
2776 reflections	Δρ_min = −1.29 e Å⁻³
206 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
Gd1	0.283337 (12)	0.28362 (2)	0.703522 (11)	0.00496 (6)
O1	0.46782 (18)	0.4287 (3)	0.74763 (16)	0.0085 (5)
O2	0.58731 (18)	0.5825 (3)	0.85710 (16)	0.0080 (4)
O3	0.3449 (2)	1.0594 (3)	1.05119 (16)	0.0101 (5)
O4	0.25022 (19)	0.8881 (3)	1.14877 (16)	0.0111 (5)
O5	0.10951 (19)	0.3347 (3)	0.77338 (17)	0.0118 (5)
O6	0.00718 (19)	0.4715 (3)	0.88248 (16)	0.0105 (5)
O7	0.3762 (2)	0.1238 (3)	0.85200 (17)	0.0109 (5)
H7A	0.425 (3)	0.051 (4)	0.838 (3)	0.016*
H7B	0.369 (3)	0.110 (5)	0.9117 (19)	0.016*
O8	0.1937 (2)	−0.0211 (3)	0.71872 (18)	0.0117 (5)
H8A	0.129 (2)	−0.034 (5)	0.690 (3)	0.018*
H8B	0.225 (3)	−0.109 (4)	0.709 (3)	0.018*
O9	0.1329 (2)	0.2581 (3)	0.56658 (18)	0.0135 (5)
H9A	0.081 (3)	0.185 (4)	0.571 (3)	0.020*
H9B	0.121 (3)	0.314 (5)	0.513 (2)	0.020*
O10	0.0781 (2)	0.4862 (3)	0.40873 (19)	0.0194 (6)
H10A	0.106 (4)	0.505 (6)	0.357 (2)	0.029*
H10B	0.016 (3)	0.531 (5)	0.392 (3)	0.029*
N1	0.2963 (2)	0.4907 (3)	0.85098 (19)	0.0060 (5)
C1	0.3938 (3)	0.5761 (4)	0.8822 (2)	0.0055 (6)
C2	0.4007 (3)	0.7107 (4)	0.9553 (2)	0.0073 (6)
H2	0.4699	0.7730	0.9744	0.009*
C3	0.3035 (3)	0.7525 (4)	1.0003 (2)	0.0082 (6)
C4	0.2043 (3)	0.6563 (4)	0.9712 (2)	0.0073 (6)
H4	0.1385	0.6761	1.0037	0.009*
C5	0.2035 (3)	0.5320 (4)	0.8944 (2)	0.0070 (6)
C6	0.4912 (3)	0.5242 (4)	0.8255 (2)	0.0068 (6)
C7	0.3007 (3)	0.9081 (4)	1.0720 (2)	0.0077 (6)
C8	0.0974 (3)	0.4387 (4)	0.8469 (2)	0.0072 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd1	0.00489 (8)	0.00531 (9)	0.00486 (9)	0.00011 (6)	0.00130 (6)	−0.00021 (6)
O1	0.0066 (11)	0.0089 (11)	0.0103 (12)	−0.0013 (8)	0.0017 (9)	−0.0024 (9)
O2	0.0051 (11)	0.0103 (11)	0.0082 (11)	−0.0021 (8)	−0.0006 (9)	0.0004 (8)
O3	0.0137 (12)	0.0071 (11)	0.0099 (12)	−0.0012 (9)	0.0034 (9)	−0.0026 (9)
O4	0.0143 (13)	0.0104 (12)	0.0094 (12)	−0.0038 (9)	0.0059 (9)	−0.0025 (9)
O5	0.0075 (12)	0.0142 (11)	0.0142 (12)	−0.0027 (9)	0.0030 (9)	−0.0062 (9)
O6	0.0054 (11)	0.0150 (12)	0.0111 (12)	0.0014 (9)	0.0015 (9)	−0.0024 (9)
O7	0.0132 (13)	0.0111 (12)	0.0086 (12)	0.0047 (9)	0.0023 (10)	0.0035 (9)
O8	0.0084 (12)	0.0096 (12)	0.0166 (13)	0.0008 (9)	−0.0005 (10)	−0.0012 (10)
O9	0.0135 (13)	0.0173 (13)	0.0088 (12)	−0.0061 (9)	−0.0027 (10)	0.0041 (9)
O10	0.0237 (16)	0.0199 (13)	0.0141 (14)	0.0057 (11)	0.0010 (12)	0.0048 (11)
N1	0.0057 (13)	0.0058 (12)	0.0065 (13)	0.0006 (9)	0.0012 (10)	0.0008 (10)
C1	0.0072 (15)	0.0040 (14)	0.0056 (15)	−0.0021 (11)	0.0024 (12)	0.0023 (11)
C2	0.0071 (15)	0.0054 (14)	0.0094 (16)	−0.0029 (11)	0.0015 (12)	0.0004 (12)
C3	0.0097 (17)	0.0102 (16)	0.0042 (15)	0.0004 (11)	−0.0011 (12)	0.0011 (11)
C4	0.0061 (15)	0.0070 (14)	0.0092 (16)	0.0013 (11)	0.0026 (12)	0.0021 (12)
C5	0.0059 (15)	0.0073 (15)	0.0083 (16)	0.0010 (11)	0.0021 (12)	0.0009 (12)
C6	0.0095 (16)	0.0038 (14)	0.0071 (16)	0.0000 (11)	0.0007 (12)	0.0014 (11)
C7	0.0054 (15)	0.0101 (15)	0.0070 (16)	0.0018 (11)	−0.0017 (12)	0.0000 (12)
C8	0.0065 (16)	0.0060 (15)	0.0095 (16)	−0.0008 (11)	0.0023 (12)	0.0021 (12)

Geometric parameters (Å, º) top

Gd1—O2ⁱ	2.335 (2)	O7—H7B	0.83 (2)
Gd1—O5	2.393 (2)	O8—H8A	0.82 (3)
Gd1—O9	2.437 (3)	O8—H8B	0.75 (2)
Gd1—O1	2.449 (2)	O9—H9A	0.82 (2)
Gd1—O7	2.471 (2)	O9—H9B	0.83 (2)
Gd1—O8	2.477 (2)	O10—H10A	0.81 (2)
Gd1—N1	2.488 (2)	O10—H10B	0.82 (3)
Gd1—O4ⁱⁱ	2.517 (2)	N1—C5	1.339 (4)
Gd1—O3ⁱⁱ	2.530 (2)	N1—C1	1.342 (4)
Gd1—C7ⁱⁱ	2.880 (3)	C1—C2	1.386 (4)
O1—C6	1.266 (4)	C1—C6	1.504 (4)
O2—C6	1.250 (4)	C2—C3	1.397 (4)
O2—Gd1ⁱⁱⁱ	2.335 (2)	C2—H2	0.9500
O3—C7	1.264 (4)	C3—C4	1.391 (4)
O3—Gd1^iv	2.530 (2)	C3—C7	1.492 (4)
O4—C7	1.261 (4)	C4—C5	1.374 (4)
O4—Gd1^iv	2.517 (2)	C4—H4	0.9500
O5—C8	1.269 (4)	C5—C8	1.513 (4)
O6—C8	1.245 (4)	C7—Gd1^iv	2.880 (3)
O7—H7A	0.82 (2)

O2ⁱ—Gd1—O5	150.00 (8)	C6—O1—Gd1	123.22 (19)
O2ⁱ—Gd1—O9	98.27 (8)	C6—O2—Gd1ⁱⁱⁱ	134.9 (2)
O5—Gd1—O9	73.52 (8)	C7—O3—Gd1^iv	92.69 (17)
O2ⁱ—Gd1—O1	75.39 (7)	C7—O4—Gd1^iv	93.35 (18)
O5—Gd1—O1	128.84 (7)	C8—O5—Gd1	125.3 (2)
O9—Gd1—O1	141.45 (7)	Gd1—O7—H7A	112 (3)
O2ⁱ—Gd1—O7	74.73 (7)	Gd1—O7—H7B	140 (3)
O5—Gd1—O7	94.71 (8)	H7A—O7—H7B	107 (4)
O9—Gd1—O7	143.75 (8)	Gd1—O8—H8A	117 (3)
O1—Gd1—O7	72.28 (7)	Gd1—O8—H8B	121 (3)
O2ⁱ—Gd1—O8	77.00 (7)	H8A—O8—H8B	106 (4)
O5—Gd1—O8	73.01 (8)	Gd1—O9—H9A	119 (3)
O9—Gd1—O8	72.98 (8)	Gd1—O9—H9B	131 (3)
O1—Gd1—O8	138.37 (7)	H9A—O9—H9B	109 (4)
O7—Gd1—O8	70.78 (8)	H10A—O10—H10B	98 (4)
O2ⁱ—Gd1—N1	132.39 (8)	C5—N1—C1	118.9 (3)
O5—Gd1—N1	64.62 (8)	C5—N1—Gd1	120.3 (2)
O9—Gd1—N1	129.04 (8)	C1—N1—Gd1	120.47 (19)
O1—Gd1—N1	64.48 (7)	N1—C1—C2	122.2 (3)
O7—Gd1—N1	69.63 (8)	N1—C1—C6	114.3 (3)
O8—Gd1—N1	117.68 (8)	C2—C1—C6	123.4 (3)
O2ⁱ—Gd1—O4ⁱⁱ	125.38 (7)	C1—C2—C3	118.4 (3)
O5—Gd1—O4ⁱⁱ	81.63 (7)	C1—C2—H2	120.8
O9—Gd1—O4ⁱⁱ	76.75 (8)	C3—C2—H2	120.8
O1—Gd1—O4ⁱⁱ	76.74 (7)	C4—C3—C2	119.0 (3)
O7—Gd1—O4ⁱⁱ	136.55 (8)	C4—C3—C7	119.1 (3)
O8—Gd1—O4ⁱⁱ	144.83 (8)	C2—C3—C7	121.7 (3)
N1—Gd1—O4ⁱⁱ	69.84 (8)	C5—C4—C3	118.7 (3)
O2ⁱ—Gd1—O3ⁱⁱ	74.76 (7)	C5—C4—H4	120.7
O5—Gd1—O3ⁱⁱ	126.13 (8)	C3—C4—H4	120.7
O9—Gd1—O3ⁱⁱ	70.79 (8)	N1—C5—C4	122.7 (3)
O1—Gd1—O3ⁱⁱ	70.88 (7)	N1—C5—C8	113.8 (3)
O7—Gd1—O3ⁱⁱ	136.76 (8)	C4—C5—C8	123.4 (3)
O8—Gd1—O3ⁱⁱ	129.52 (7)	O2—C6—O1	125.4 (3)
N1—Gd1—O3ⁱⁱ	112.32 (8)	O2—C6—C1	117.9 (3)
O4ⁱⁱ—Gd1—O3ⁱⁱ	51.91 (7)	O1—C6—C1	116.7 (3)
O2ⁱ—Gd1—C7ⁱⁱ	100.19 (8)	O4—C7—O3	122.0 (3)
O5—Gd1—C7ⁱⁱ	104.20 (8)	O4—C7—C3	119.5 (3)
O9—Gd1—C7ⁱⁱ	71.79 (8)	O3—C7—C3	118.4 (3)
O1—Gd1—C7ⁱⁱ	72.09 (8)	O4—C7—Gd1^iv	60.73 (15)
O7—Gd1—C7ⁱⁱ	144.11 (8)	O3—C7—Gd1^iv	61.32 (15)
O8—Gd1—C7ⁱⁱ	143.83 (9)	C3—C7—Gd1^iv	176.6 (2)
N1—Gd1—C7ⁱⁱ	91.16 (8)	O6—C8—O5	126.3 (3)
O4ⁱⁱ—Gd1—C7ⁱⁱ	25.92 (7)	O6—C8—C5	117.7 (3)
O3ⁱⁱ—Gd1—C7ⁱⁱ	25.99 (7)	O5—C8—C5	116.0 (3)

O2ⁱ—Gd1—O1—C6	−147.2 (2)	Gd1—N1—C1—C2	171.2 (2)
O5—Gd1—O1—C6	12.7 (3)	C5—N1—C1—C6	−177.8 (3)
O9—Gd1—O1—C6	127.9 (2)	Gd1—N1—C1—C6	−4.0 (3)
O7—Gd1—O1—C6	−68.8 (2)	N1—C1—C2—C3	2.6 (4)
O8—Gd1—O1—C6	−97.2 (2)	C6—C1—C2—C3	177.5 (3)
N1—Gd1—O1—C6	6.5 (2)	C1—C2—C3—C4	0.9 (4)
O4ⁱⁱ—Gd1—O1—C6	80.3 (2)	C1—C2—C3—C7	−173.7 (3)
O3ⁱⁱ—Gd1—O1—C6	134.2 (2)	C2—C3—C4—C5	−4.3 (5)
C7ⁱⁱ—Gd1—O1—C6	106.8 (2)	C7—C3—C4—C5	170.5 (3)
O2ⁱ—Gd1—O5—C8	133.9 (2)	C1—N1—C5—C4	−1.1 (4)
O9—Gd1—O5—C8	−148.4 (3)	Gd1—N1—C5—C4	−174.9 (2)
O1—Gd1—O5—C8	−4.4 (3)	C1—N1—C5—C8	175.1 (3)
O7—Gd1—O5—C8	66.6 (2)	Gd1—N1—C5—C8	1.3 (3)
O8—Gd1—O5—C8	134.8 (3)	C3—C4—C5—N1	4.6 (5)
N1—Gd1—O5—C8	1.8 (2)	C3—C4—C5—C8	−171.3 (3)
O4ⁱⁱ—Gd1—O5—C8	−69.8 (2)	Gd1ⁱⁱⁱ—O2—C6—O1	62.9 (4)
O3ⁱⁱ—Gd1—O5—C8	−98.3 (2)	Gd1ⁱⁱⁱ—O2—C6—C1	−115.0 (3)
C7ⁱⁱ—Gd1—O5—C8	−82.7 (2)	Gd1—O1—C6—O2	171.1 (2)
O2ⁱ—Gd1—N1—C5	−151.4 (2)	Gd1—O1—C6—C1	−11.0 (3)
O5—Gd1—N1—C5	−1.5 (2)	N1—C1—C6—O2	−172.4 (3)
O9—Gd1—N1—C5	36.4 (3)	C2—C1—C6—O2	12.4 (4)
O1—Gd1—N1—C5	173.1 (2)	N1—C1—C6—O1	9.6 (4)
O7—Gd1—N1—C5	−107.4 (2)	C2—C1—C6—O1	−165.6 (3)
O8—Gd1—N1—C5	−53.6 (2)	Gd1^iv—O4—C7—O3	0.5 (3)
O4ⁱⁱ—Gd1—N1—C5	88.6 (2)	Gd1^iv—O4—C7—C3	−176.1 (3)
O3ⁱⁱ—Gd1—N1—C5	119.2 (2)	Gd1^iv—O3—C7—O4	−0.5 (3)
C7ⁱⁱ—Gd1—N1—C5	103.6 (2)	Gd1^iv—O3—C7—C3	176.1 (3)
O2ⁱ—Gd1—N1—C1	34.9 (3)	C4—C3—C7—O4	45.8 (4)
O5—Gd1—N1—C1	−175.3 (2)	C2—C3—C7—O4	−139.6 (3)
O9—Gd1—N1—C1	−137.4 (2)	C4—C3—C7—O3	−131.0 (3)
O1—Gd1—N1—C1	−0.6 (2)	C2—C3—C7—O3	43.6 (4)
O7—Gd1—N1—C1	78.9 (2)	Gd1—O5—C8—O6	177.7 (2)
O8—Gd1—N1—C1	132.6 (2)	Gd1—O5—C8—C5	−1.8 (4)
O4ⁱⁱ—Gd1—N1—C1	−85.1 (2)	N1—C5—C8—O6	−179.3 (3)
O3ⁱⁱ—Gd1—N1—C1	−54.5 (2)	C4—C5—C8—O6	−3.1 (4)
C7ⁱⁱ—Gd1—N1—C1	−70.1 (2)	N1—C5—C8—O5	0.2 (4)
C5—N1—C1—C2	−2.6 (4)	C4—C5—C8—O5	176.4 (3)

Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) x, −y+3/2, z−1/2; (iii) −x+1, y+1/2, −z+3/2; (iv) x, −y+3/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O1ⁱ	0.82 (2)	2.02 (3)	2.794 (3)	157 (4)
O7—H7B···O3^v	0.83 (2)	1.97 (2)	2.795 (3)	175 (4)
O8—H8A···O6^vi	0.82 (3)	1.80 (3)	2.621 (3)	171 (4)
O8—H8B···O4^vii	0.75 (2)	2.22 (3)	2.933 (3)	158 (4)
O9—H9A···O6^vi	0.82 (2)	2.01 (3)	2.800 (3)	161 (4)
O9—H9B···O10	0.83 (2)	1.91 (3)	2.723 (3)	166 (4)
O10—H10A···O8^vii	0.81 (2)	2.24 (3)	3.051 (4)	173 (4)
O10—H10B···O9^viii	0.82 (3)	2.45 (3)	3.169 (4)	148 (4)

Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (v) x, y−1, z; (vi) −x, y−1/2, −z+3/2; (vii) x, −y+1/2, z−1/2; (viii) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Gd(C₈H₂NO₆)(H₂O)₃]·H₂O
M_r	437.42
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	113
a, b, c (Å)	11.896 (3), 7.2696 (14), 13.505 (3)
β (°)	96.259 (3)
V (Å³)	1160.9 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.77
Crystal size (mm)	0.12 × 0.10 × 0.08

Data collection
Diffractometer	Rigaku Saturn
Absorption correction	Multi-scan (REQAB; Jacobson, 1998)
T_min, T_max	0.544, 0.655
No. of measured, independent and observed [I > 2σ(I)] reflections	10599, 2776, 2366
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.658

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.049, 1.04
No. of reflections	2776
No. of parameters	206
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.64, −1.29

Computer programs: CrystalClear (Rigaku/MSC, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), CrystalStructure (Rigaku/MSC, 2005).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O1ⁱ	0.82 (2)	2.02 (3)	2.794 (3)	157 (4)
O7—H7B···O3ⁱⁱ	0.83 (2)	1.97 (2)	2.795 (3)	175 (4)
O8—H8A···O6ⁱⁱⁱ	0.82 (3)	1.80 (3)	2.621 (3)	171 (4)
O8—H8B···O4^iv	0.75 (2)	2.22 (3)	2.933 (3)	158 (4)
O9—H9A···O6ⁱⁱⁱ	0.82 (2)	2.01 (3)	2.800 (3)	161 (4)
O9—H9B···O10	0.83 (2)	1.91 (3)	2.723 (3)	166 (4)
O10—H10A···O8^iv	0.81 (2)	2.24 (3)	3.051 (4)	173 (4)
O10—H10B···O9^v	0.82 (3)	2.45 (3)	3.169 (4)	148 (4)

Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) x, y−1, z; (iii) −x, y−1/2, −z+3/2; (iv) x, −y+1/2, z−1/2; (v) −x, −y+1, −z+1.

Acknowledgements

This work was supported by the Education Department of Henan Province (2009B150026).

References

Fu, D.-W. & Xu, H.-J. (2008). Acta Cryst. E64, m35. Web of Science CSD CrossRef IUCr Journals Google Scholar
Gao, H. L., Yi, L., Ding, B., Wang, H. S., Cheng, P., Liao, D. Z. & Yan, S. P. (2006). Inorg. Chem. 45, 481–483. Web of Science CSD CrossRef PubMed CAS Google Scholar
Ghosh, S. K. & Bharadwaj, P. K. (2005). Eur. J. Inorg. Chem. 24, 4886–4889. Web of Science CSD CrossRef Google Scholar
Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. Google Scholar
Li, C. J., Peng, M. X., Leng, J. D., Yang, M. M., Lin, Z. J. & Tong, M. L. (2008). CrystEngComm, 10, 1645–1652. Web of Science CSD CrossRef CAS Google Scholar
Pan, L., Adams, K. M., Hernandez, H. E., Wang, X., Zheng, C., Hattori, Y. & Kaneko, K. (2003). J. Am. Chem. Soc. 125, 3062–3063. Web of Science CSD CrossRef PubMed CAS Google Scholar
Parker, D. (2000). Coord. Chem. Rev. 205, 109–115. Web of Science CrossRef CAS Google Scholar
Rigaku/MSC (2005). CrystalStructure and CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tobisch, S. (2005). J. Am. Chem. Soc. 127, 11979–11980. Web of Science CrossRef PubMed CAS Google Scholar
Wang, H. S., Zhao, B., Zhai, B., Shi, W., Cheng, P., Liao, D. Z. & Yan, S. P. (2007). Cryst. Growth Des. 7, 1851–1857. Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.