Poly[[triaqua-(μ(3)-4-oxidopyridine-2,6-dicarboxyl-ato)europium(III)] monohydrate].

In the title coordination polymer, {[Eu(C(7)H(2)NO(5))(H(2)O)(3)]·H(2)O}(n), the Eu(III) atom is eight-coordinated by a tridentate 4-oxidopyridine-2,6-dicarboxyl-ate (hpc) trianion, two monodentate hpc anions and three water mol-ecules, forming a distorted bicapped trigonal-prismatic coordination geometry. The hpc ligands bridge adjacent Eu(III) ions, forming infinite double chains. Adjacent chains are further connected by hpc ligands into sheets. O-H⋯O hydrogen bonds then generate a three-dimensional supra-molecular framework.

Related literature

For the structures and properties of lanthanide coordination compounds, see: He et al. (2010 ▶); Kustaryono et al. (2010 ▶); Zhu, Sun et al. (2009 ▶); Wong et al. (2006 ▶). For the use of multi-carboxyl­ate and n class="Chemical">heterocyclic acids in coordination chemistry, see: Li et al. (2008 ▶); Luo et al. (2008 ▶) and for the dicarboxyl­ate ligand H3CAM (H3CAM is 4-hy­droxy-pyridine-2,6-dicarb­oxy­lic acid), see: Gao et al. (2006 ▶, 2008 ▶). For the isotypic structure {[Dy(CAM)(H2O)3]·H2O}, see: Gao et al. (2006 ▶). For bond lengths and angles in other complexes with eight-coordinate EuIII, see: Li et al. (2008 ▶); Zhu, Ikarashi et al. (2009 ▶)

Experimental

Crystal data

[Eu(C7H2NO5)(H2O)3]·H2O

M = 404.12

Monoclinic,

a = 10.0041 (15) Å

b = 7.5456 (11) Å

c = 15.528 (2) Å

β = 104.890 (1)°

V = 1132.8 (3) Å3

Z = 4

Mo Kα radiation

μ = 5.58 mm−1

T = 296 K

0.35 × 0.32 × 0.31 mm

Data collection

Bruker APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 1997 ▶) T min = 0.246, T max = 0.277

4884 measured reflections

2023 independent reflections

1856 reflections with I > 2σ(I)

R int = 0.074

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.065

S = 1.06

2023 reflections

196 parameters

12 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.82 e Å−3

Δρmin = −1.69 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); 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 ▶.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810048518/hb5735sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810048518/hb5735Isup2.hkl

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

[Eu(C7H2NO5)(H2O)3]·H2O	F(000) = 776
Mr = 404.12	Dx = 2.370 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3455 reflections
a = 10.0041 (15) Å	θ = 2.8–28.3°
b = 7.5456 (11) Å	µ = 5.58 mm−1
c = 15.528 (2) Å	T = 296 K
β = 104.890 (1)°	Block, colorless
V = 1132.8 (3) Å3	0.35 × 0.32 × 0.31 mm
Z = 4

Bruker APEXII CCD diffractometer	2023 independent reflections
Radiation source: fine-focus sealed tube	1856 reflections with I > 2σ(I)
graphite	Rint = 0.074
φ and ω scans	θmax = 25.5°, θmin = 2.8°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −11→12
Tmin = 0.246, Tmax = 0.277	k = −9→7
4884 measured reflections	l = −14→18

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)] = 0.026	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.065	w = 1/[σ2(Fo2) + 0.5803P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max = 0.001
2023 reflections	Δρmax = 0.82 e Å−3
196 parameters	Δρmin = −1.69 e Å−3
12 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: 0.0273 (8)

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
Eu1	0.500412 (13)	0.82415 (2)	0.746168 (10)	0.01204 (13)
C1	0.7849 (3)	0.5972 (4)	0.8389 (2)	0.0179 (7)
C2	0.7266 (3)	0.6188 (4)	0.9168 (2)	0.0159 (7)
C3	0.7942 (3)	0.5648 (4)	1.0015 (2)	0.0168 (7)
H3	0.8789	0.5069	1.0112	0.020*
H5	0.5632	0.7067	1.0980	0.020*
C4	0.7362 (3)	0.5967 (4)	1.0731 (2)	0.0153 (7)
C5	0.6069 (3)	0.6829 (4)	1.0528 (2)	0.0164 (8)
C6	0.5456 (3)	0.7327 (4)	0.9664 (2)	0.0142 (7)
C7	0.4087 (3)	0.8280 (4)	0.9380 (2)	0.0163 (8)
H1W	0.492 (5)	0.543 (3)	0.609 (3)	0.073 (17)*
H2W	0.536 (5)	0.692 (5)	0.567 (3)	0.060 (17)*
H3W	0.327 (5)	0.552 (7)	0.785 (2)	0.08 (2)*
H4W	0.315 (4)	0.511 (6)	0.6919 (18)	0.071 (17)*
H5W	0.660 (4)	1.125 (6)	0.802 (2)	0.069 (17)*
H6W	0.623 (4)	1.093 (6)	0.8862 (12)	0.047 (13)*
H7W	0.034 (5)	0.735 (6)	0.899 (4)	0.11 (2)*
H8W	0.155 (2)	0.835 (6)	0.949 (4)	0.078 (19)*
N1	0.6033 (3)	0.7025 (3)	0.89845 (18)	0.0151 (6)
O1	0.7227 (3)	0.6764 (3)	0.76842 (16)	0.0270 (7)
O2	0.8922 (2)	0.5058 (3)	0.84687 (15)	0.0234 (6)
O3	0.3689 (2)	0.8704 (3)	0.85661 (15)	0.0211 (5)
O4	0.3426 (2)	0.8572 (3)	0.99465 (16)	0.0245 (6)
O5	0.8011 (2)	0.5511 (3)	1.15508 (14)	0.0202 (5)
O6	0.5004 (3)	0.6614 (3)	0.61007 (18)	0.0275 (6)
O7	0.3631 (3)	0.5587 (4)	0.73985 (19)	0.0323 (7)
O8	0.6026 (3)	1.0809 (4)	0.82870 (18)	0.0319 (7)
O9	0.0664 (3)	0.8216 (3)	0.9349 (2)	0.0367 (8)

	U11	U22	U33	U12	U13	U23
Eu1	0.01379 (17)	0.01728 (17)	0.00543 (16)	0.00006 (5)	0.00313 (11)	0.00080 (5)
C1	0.0194 (16)	0.0240 (17)	0.0107 (17)	0.0022 (14)	0.0047 (14)	−0.0012 (14)
C2	0.0192 (16)	0.0166 (16)	0.0130 (17)	0.0000 (13)	0.0060 (14)	0.0001 (14)
C3	0.0189 (16)	0.0193 (16)	0.0119 (16)	0.0030 (13)	0.0031 (14)	0.0014 (13)
C4	0.0194 (15)	0.0171 (16)	0.0079 (16)	−0.0042 (13)	0.0010 (13)	0.0026 (13)
C5	0.0186 (17)	0.0243 (18)	0.0094 (17)	−0.0032 (12)	0.0092 (14)	−0.0015 (13)
C6	0.0195 (17)	0.0153 (15)	0.0094 (16)	−0.0007 (13)	0.0068 (14)	−0.0007 (13)
C7	0.0180 (17)	0.0193 (17)	0.0109 (18)	−0.0021 (13)	0.0028 (15)	−0.0021 (13)
N1	0.0175 (14)	0.0206 (13)	0.0071 (14)	0.0027 (11)	0.0033 (12)	0.0021 (11)
O1	0.0276 (14)	0.0468 (17)	0.0090 (13)	0.0166 (11)	0.0092 (11)	0.0085 (11)
O2	0.0241 (13)	0.0330 (14)	0.0128 (12)	0.0135 (11)	0.0043 (10)	−0.0014 (11)
O3	0.0201 (11)	0.0338 (13)	0.0094 (12)	0.0077 (11)	0.0041 (10)	0.0031 (11)
O4	0.0236 (12)	0.0419 (15)	0.0110 (13)	0.0061 (11)	0.0097 (11)	−0.0009 (11)
O5	0.0206 (11)	0.0305 (13)	0.0087 (12)	−0.0030 (10)	0.0021 (10)	0.0042 (10)
O6	0.0423 (17)	0.0266 (15)	0.0169 (15)	−0.0036 (12)	0.0135 (14)	−0.0033 (11)
O7	0.0413 (16)	0.0376 (16)	0.0212 (15)	−0.0181 (13)	0.0141 (14)	−0.0058 (13)
O8	0.0451 (16)	0.0393 (16)	0.0164 (14)	−0.0194 (14)	0.0172 (13)	−0.0085 (12)
O9	0.0278 (16)	0.0311 (16)	0.049 (2)	0.0034 (12)	0.0062 (15)	0.0025 (13)

Eu1—O5i	2.327 (2)	C5—C6	1.377 (4)
Eu1—O8	2.401 (3)	C5—H5	0.9344
Eu1—O7	2.416 (3)	C6—N1	1.345 (4)
Eu1—O1	2.432 (2)	C6—C7	1.509 (4)
Eu1—O2ii	2.433 (2)	C7—O4	1.249 (4)
Eu1—O3	2.440 (2)	C7—O3	1.264 (4)
Eu1—O6	2.445 (3)	O2—Eu1iii	2.433 (2)
Eu1—N1	2.498 (3)	O5—Eu1iv	2.327 (2)
C1—O2	1.255 (4)	O6—H1W	0.895 (19)
C1—O1	1.262 (4)	O6—H2W	0.867 (19)
C1—C2	1.481 (5)	O7—H3W	0.871 (19)
C2—N1	1.350 (4)	O7—H4W	0.856 (19)
C2—C3	1.376 (4)	O8—H5W	0.855 (19)
C3—C4	1.402 (5)	O8—H6W	0.868 (18)
C3—H3	0.9300	O9—H7W	0.861 (19)
C4—O5	1.317 (3)	O9—H8W	0.861 (19)
C4—C5	1.410 (4)
O5i—Eu1—O8	100.29 (9)	O2—C1—C2	119.1 (3)
O5i—Eu1—O7	85.49 (9)	O1—C1—C2	116.5 (3)
O8—Eu1—O7	148.21 (10)	N1—C2—C3	122.6 (3)
O5i—Eu1—O1	151.83 (8)	N1—C2—C1	114.1 (3)
O8—Eu1—O1	92.61 (9)	C3—C2—C1	123.2 (3)
O7—Eu1—O1	96.63 (9)	C2—C3—C4	120.4 (3)
O5i—Eu1—O2ii	81.44 (8)	C2—C3—H3	119.8
O8—Eu1—O2ii	70.73 (9)	C4—C3—H3	119.8
O7—Eu1—O2ii	140.91 (9)	O5—C4—C3	121.4 (3)
O1—Eu1—O2ii	79.36 (8)	O5—C4—C5	122.2 (3)
O5i—Eu1—O3	80.61 (8)	C3—C4—C5	116.4 (3)
O8—Eu1—O3	75.04 (9)	C6—C5—C4	119.8 (3)
O7—Eu1—O3	75.15 (9)	C6—C5—H5	120.2
O1—Eu1—O3	127.18 (8)	C4—C5—H5	120.0
O2ii—Eu1—O3	137.46 (8)	N1—C6—C5	123.0 (3)
O5i—Eu1—O6	82.43 (9)	N1—C6—C7	113.1 (3)
O8—Eu1—O6	140.55 (10)	C5—C6—C7	123.9 (3)
O7—Eu1—O6	71.01 (10)	O4—C7—O3	124.9 (3)
O1—Eu1—O6	71.90 (9)	O4—C7—C6	118.9 (3)
O2ii—Eu1—O6	70.83 (9)	O3—C7—C6	116.2 (3)
O3—Eu1—O6	143.08 (9)	C6—N1—C2	117.8 (3)
O5i—Eu1—N1	143.53 (9)	C6—N1—Eu1	121.6 (2)
O8—Eu1—N1	77.05 (9)	C2—N1—Eu1	120.3 (2)
O7—Eu1—N1	79.95 (9)	C1—O1—Eu1	124.7 (2)
O1—Eu1—N1	63.77 (9)	C1—O2—Eu1iii	138.4 (2)
O2ii—Eu1—N1	129.18 (9)	C7—O3—Eu1	125.3 (2)
O3—Eu1—N1	63.42 (8)	C4—O5—Eu1iv	127.88 (19)
O6—Eu1—N1	122.83 (9)	Eu1—O6—H1W	119 (3)
O5i—Eu1—H5W	101.3 (10)	Eu1—O6—H2W	129 (3)
O8—Eu1—H5W	17.0 (6)	H1W—O6—H2W	108 (3)
O7—Eu1—H5W	164.4 (6)	Eu1—O7—H3W	111 (3)
O1—Eu1—H5W	84.1 (10)	Eu1—O7—H4W	125 (3)
O2ii—Eu1—H5W	54.6 (6)	H3W—O7—H4W	115 (3)
O3—Eu1—H5W	91.9 (6)	Eu1—O8—H5W	108 (3)
O6—Eu1—H5W	123.6 (6)	Eu1—O8—H6W	126 (3)
N1—Eu1—H5W	86.4 (8)	H5W—O8—H6W	116 (3)
O2—C1—O1	124.4 (3)	H7W—O9—H8W	116 (3)
O2—C1—C2—N1	−173.0 (3)	O6—Eu1—N1—C6	−143.3 (2)
O1—C1—C2—N1	8.2 (4)	O5i—Eu1—N1—C2	170.8 (2)
O2—C1—C2—C3	9.4 (5)	O8—Eu1—N1—C2	−99.4 (2)
O1—C1—C2—C3	−169.3 (3)	O7—Eu1—N1—C2	102.7 (2)
N1—C2—C3—C4	−0.4 (5)	O1—Eu1—N1—C2	0.1 (2)
C1—C2—C3—C4	177.0 (3)	O2ii—Eu1—N1—C2	−48.0 (3)
C2—C3—C4—O5	−177.9 (3)	O3—Eu1—N1—C2	−178.9 (3)
C2—C3—C4—C5	0.9 (5)	O6—Eu1—N1—C2	43.2 (3)
O5—C4—C5—C6	178.0 (3)	O2—C1—O1—Eu1	172.3 (2)
C3—C4—C5—C6	−0.8 (4)	C2—C1—O1—Eu1	−9.0 (4)
C4—C5—C6—N1	0.2 (5)	O5i—Eu1—O1—C1	−163.2 (2)
C4—C5—C6—C7	−179.0 (3)	O8—Eu1—O1—C1	79.2 (3)
N1—C6—C7—O4	177.2 (3)	O7—Eu1—O1—C1	−70.3 (3)
C5—C6—C7—O4	−3.5 (5)	O2ii—Eu1—O1—C1	149.0 (3)
N1—C6—C7—O3	−1.8 (4)	O3—Eu1—O1—C1	6.0 (3)
C5—C6—C7—O3	177.4 (3)	O6—Eu1—O1—C1	−137.8 (3)
C5—C6—N1—C2	0.3 (5)	N1—Eu1—O1—C1	5.0 (3)
C7—C6—N1—C2	179.6 (3)	O1—C1—O2—Eu1iii	−29.7 (5)
C5—C6—N1—Eu1	−173.3 (2)	C2—C1—O2—Eu1iii	151.6 (2)
C7—C6—N1—Eu1	6.0 (4)	O4—C7—O3—Eu1	177.6 (2)
C3—C2—N1—C6	−0.2 (5)	C6—C7—O3—Eu1	−3.4 (4)
C1—C2—N1—C6	−177.8 (3)	O5i—Eu1—O3—C7	178.4 (3)
C3—C2—N1—Eu1	173.5 (2)	O8—Eu1—O3—C7	−78.2 (3)
C1—C2—N1—Eu1	−4.1 (4)	O7—Eu1—O3—C7	90.6 (3)
O5i—Eu1—N1—C6	−15.8 (3)	O1—Eu1—O3—C7	3.6 (3)
O8—Eu1—N1—C6	74.1 (2)	O2ii—Eu1—O3—C7	−115.4 (2)
O7—Eu1—N1—C6	−83.8 (2)	O6—Eu1—O3—C7	114.7 (2)
O1—Eu1—N1—C6	173.6 (3)	N1—Eu1—O3—C7	4.6 (2)
O2ii—Eu1—N1—C6	125.5 (2)	C3—C4—O5—Eu1iv	69.8 (4)
O3—Eu1—N1—C6	−5.5 (2)	C5—C4—O5—Eu1iv	−108.9 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H1W···O9v	0.90 (2)	1.85 (3)	2.696 (3)	158 (4)
O6—H2W···O9vi	0.87 (2)	2.15 (3)	2.962 (4)	156 (4)
O7—H4W···O3v	0.86 (2)	2.09 (3)	2.805 (3)	141 (4)
O8—H5W···O1ii	0.86 (2)	1.84 (2)	2.684 (4)	168 (4)
O8—H6W···O4vii	0.87 (2)	1.83 (2)	2.696 (4)	173 (4)
O9—H7W···O2viii	0.86 (2)	2.26 (3)	3.059 (4)	155 (5)
O9—H8W···O4	0.86 (2)	1.84 (2)	2.692 (4)	172 (6)

Table 1

Selected bond lengths (Å)

Eu1—O5i	2.327 (2)
Eu1—O8	2.401 (3)
Eu1—O7	2.416 (3)
Eu1—O1	2.432 (2)
Eu1—O2ii	2.433 (2)
Eu1—O3	2.440 (2)
Eu1—O6	2.445 (3)
Eu1—N1	2.498 (3)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H1W⋯O9iii	0.90 (2)	1.85 (3)	2.696 (3)	158 (4)
O6—H2W⋯O9iv	0.87 (2)	2.15 (3)	2.962 (4)	156 (4)
O7—H4W⋯O3iii	0.86 (2)	2.09 (3)	2.805 (3)	141 (4)
O8—H5W⋯O1ii	0.86 (2)	1.84 (2)	2.684 (4)	168 (4)
O8—H6W⋯O4v	0.87 (2)	1.83 (2)	2.696 (4)	173 (4)
O9—H7W⋯O2vi	0.86 (2)	2.26 (3)	3.059 (4)	155 (5)
O9—H8W⋯O4	0.86 (2)	1.84 (2)	2.692 (4)	172 (6)

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