Poly[[triaqua-(μ(3)-pyridine-2,4,6-tri-car-boxyl-ato)gadolinium(III)] monohydrate].

The title compound, {[Gd(C(8)H(2)NO(6))(H(2)O)(3)]·H(2)O}(n), was obtained in water under hydro-thermal conditions. The Gd(III) ions are nine-coordinated by two O and one N atoms from one pyridine-2,4,6-tricarboxyl-ate ligand, two O atoms from another ligand, one O atom from a third ligand and three coordinated water mol-ecules. 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 pan class="Chemical">lanthanide-organic frameworks and their properties, see: Parker (2000 ▶); Tobisch (2005 ▶); Pan et al. (2003 ▶).

Experimental

Crystal data

[Gd(C8H2NO6)(H2O)3]·H2O

M = 437.42

Monoclinic,

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[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.049

S = 1.04

2776 reflections

206 parameters

8 restraints

pan class="Disease">H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.64 e Å−3

Δρmin = −1.29 e Å−3

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 ▶).

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

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809038793/zq2008Isup2.hkl

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

[Gd(C8H2NO6)(H2O)3]·H2O	F(000) = 836
Mr = 437.42	Dx = 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

Rigaku Saturn diffractometer	2776 independent reflections
Radiation source: rotating anode	2366 reflections with I > 2σ(I)
confocal	Rint = 0.038
Detector resolution: 7.31 pixels mm-1	θmax = 27.9°, θmin = 1.7°
ω scans	h = −15→15
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −8→9
Tmin = 0.544, Tmax = 0.655	l = −17→17
10599 measured 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)] = 0.021	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(Fo2) + (0.0242P)2] where P = (Fo2 + 2Fc2)/3
2776 reflections	(Δ/σ)max = 0.001
206 parameters	Δρmax = 0.64 e Å−3
8 restraints	Δρmin = −1.29 e Å−3

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.

	x	y	z	Uiso*/Ueq
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)

	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)

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—Gd1iv	2.530 (2)	C3—C7	1.492 (4)
O4—C7	1.261 (4)	C4—C5	1.374 (4)
O4—Gd1iv	2.517 (2)	C4—H4	0.9500
O5—C8	1.269 (4)	C5—C8	1.513 (4)
O6—C8	1.245 (4)	C7—Gd1iv	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—Gd1iv	92.69 (17)
O2i—Gd1—O1	75.39 (7)	C7—O4—Gd1iv	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—Gd1iv	60.73 (15)
O7—Gd1—C7ii	144.11 (8)	O3—C7—Gd1iv	61.32 (15)
O8—Gd1—C7ii	143.83 (9)	C3—C7—Gd1iv	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)	Gd1iv—O4—C7—O3	0.5 (3)
O4ii—Gd1—N1—C5	88.6 (2)	Gd1iv—O4—C7—C3	−176.1 (3)
O3ii—Gd1—N1—C5	119.2 (2)	Gd1iv—O3—C7—O4	−0.5 (3)
C7ii—Gd1—N1—C5	103.6 (2)	Gd1iv—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)

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···O3v	0.83 (2)	1.97 (2)	2.795 (3)	175 (4)
O8—H8A···O6vi	0.82 (3)	1.80 (3)	2.621 (3)	171 (4)
O8—H8B···O4vii	0.75 (2)	2.22 (3)	2.933 (3)	158 (4)
O9—H9A···O6vi	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···O8vii	0.81 (2)	2.24 (3)	3.051 (4)	173 (4)
O10—H10B···O9viii	0.82 (3)	2.45 (3)	3.169 (4)	148 (4)

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⋯O4iv	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⋯O8iv	0.81 (2)	2.24 (3)	3.051 (4)	173 (4)
O10—H10B⋯O9v	0.82 (3)	2.45 (3)	3.169 (4)	148 (4)

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