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

In the title coordination polymer, {[Tb(C(7)H(2)NO(5))(H(2)O)(3)]·H(2)O}(n), the Tb(III) atom is eight-coordinated by a tridentate 4-oxidopyridine-2,6-dicarboxyl-ate trianion, two adjacent monodentate anions and three water mol-ecules, forming a distorted bicapped trigonal-prismatic TbNO(7) coordination environment. The anions bridge adjacent Tb(III) ions into double chains. Adjacent chains are further connected into sheets parallel to (10). O-H⋯O hydrogen bonds involving both coordinated and uncoordinated water mol-ecules generate a three-dimensional network.

Related literature

For structures and properties of luminescent lanthanide coordination compounds, see: Kustaryono et al. (2010 ▶); He et al. (2010 ▶); Li et al. (2008 ▶); Luo et al. (2008 ▶). For the use of multi-carboxyl­ate and heterocyclic acids in coordination chemistry, see: Li et al. (2008 ▶); Luo et al. (2008 ▶). For the dicarboxyl­ate ligand 4-oxido-pyridine-2,6-dicarboxyl­ate, see: Gao et al. (2008 ▶). For the isotypic structures of the Dy and Eu analogues, see: Gao et al. (2006 ▶) and Lv et al. (2010 ▶), respectively. For bond lengths and angles in other complexes with eight-coordinate TbIII, see: Chen et al. (2008 ▶); Ramya et al. (2010 ▶).

Experimental

Crystal data

[Tb(C7H2NO5)(H2O)3]·H2O

M = 411.08

Monoclinic,

a = 9.953 (2) Å

b = 7.5454 (16) Å

c = 15.461 (3) Å

β = 105.126 (2)°

V = 1120.9 (4) Å3

Z = 4

Mo Kα radiation

μ = 6.35 mm−1

T = 293 K

0.30 × 0.25 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.162, T max = 0.247

7828 measured reflections

2080 independent reflections

1929 reflections with I > 2σ(I)

R int = 0.032

Refinement

R[F 2 > 2σ(F 2)] = 0.019

wR(F 2) = 0.051

S = 1.10

2080 reflections

196 parameters

12 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 1.34 e Å−3

Δρmin = −0.60 e Å−3

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 ▶) and DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811005447/wm2449sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811005447/wm2449Isup2.hkl

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

[Tb(C7H2NO5)(H2O)3]·H2O	F(000) = 784
Mr = 411.08	Dx = 2.436 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5700 reflections
a = 9.953 (2) Å	θ = 2.2–28.3°
b = 7.5454 (16) Å	µ = 6.35 mm−1
c = 15.461 (3) Å	T = 293 K
β = 105.126 (2)°	Block, colorless
V = 1120.9 (4) Å3	0.30 × 0.25 × 0.22 mm
Z = 4

Bruker APEXII CCD diffractometer	2080 independent reflections
Radiation source: fine-focus sealed tube	1929 reflections with I > 2σ(I)
graphite	Rint = 0.032
φ and ω scans	θmax = 25.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −12→11
Tmin = 0.162, Tmax = 0.247	k = −9→8
7828 measured reflections	l = −18→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)] = 0.019	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.051	w = 1/[σ2(Fo2) + (0.0227P)2 + 0.941P] where P = (Fo2 + 2Fc2)/3
S = 1.10	(Δ/σ)max = 0.001
2080 reflections	Δρmax = 1.34 e Å−3
196 parameters	Δρmin = −0.60 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: 0.0244 (6)

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
Tb1	0.499147 (11)	0.823001 (18)	0.253250 (7)	0.01168 (10)
C1	0.5913 (3)	0.8297 (4)	0.06235 (18)	0.0145 (6)
C2	0.4542 (3)	0.7331 (4)	0.03360 (17)	0.0137 (6)
C3	0.3928 (3)	0.6833 (4)	−0.05345 (18)	0.0157 (6)
H3	0.4367	0.7069	−0.0984	0.019*
C4	0.2628 (3)	0.5961 (4)	−0.07393 (17)	0.0150 (6)
C5	0.2059 (3)	0.5615 (4)	−0.00148 (17)	0.0166 (6)
H5	0.1218	0.5012	−0.0109	0.020*
C6	0.2739 (3)	0.6163 (4)	0.08284 (17)	0.0149 (6)
C7	0.2160 (3)	0.5940 (4)	0.16200 (17)	0.0176 (6)
H1W	0.685 (3)	0.519 (5)	0.3081 (14)	0.033 (10)*
H2W	0.678 (4)	0.555 (5)	0.2179 (17)	0.049 (12)*
H3W	0.507 (4)	0.547 (2)	0.394 (2)	0.049 (13)*
H4W	0.477 (4)	0.706 (4)	0.433 (2)	0.039 (12)*
H5W	0.378 (3)	1.090 (5)	0.1149 (12)	0.032 (10)*
H6W	0.339 (4)	1.121 (5)	0.196 (2)	0.051 (13)*
H7W	0.348 (2)	0.664 (5)	0.544 (3)	0.051 (14)*
H8W	0.457 (5)	0.756 (7)	0.608 (3)	0.11 (2)*
N1	0.3970 (3)	0.7017 (3)	0.10190 (15)	0.0144 (5)
O1	0.6315 (2)	0.8714 (3)	0.14414 (12)	0.0198 (5)
O2	0.6576 (2)	0.8598 (3)	0.00587 (13)	0.0232 (5)
O3	0.2780 (2)	0.6745 (3)	0.23225 (14)	0.0273 (6)
O4	0.1088 (2)	0.5009 (3)	0.15414 (12)	0.0222 (5)
O5	0.1971 (2)	0.5510 (3)	−0.15625 (12)	0.0191 (5)
O6	0.6360 (2)	0.5619 (3)	0.25964 (14)	0.0286 (5)
O7	0.5014 (3)	0.6624 (3)	0.38879 (14)	0.0254 (5)
O8	0.3974 (3)	1.0761 (3)	0.17129 (14)	0.0294 (6)
O9	0.4360 (3)	0.6777 (3)	0.5670 (2)	0.0376 (6)

	U11	U22	U33	U12	U13	U23
Tb1	0.00900 (13)	0.01520 (14)	0.01068 (12)	−0.00006 (5)	0.00229 (7)	−0.00069 (4)
C1	0.0132 (15)	0.0153 (15)	0.0153 (13)	0.0025 (11)	0.0043 (11)	0.0017 (10)
C2	0.0126 (15)	0.0137 (14)	0.0153 (12)	0.0009 (12)	0.0044 (11)	0.0017 (11)
C3	0.0146 (16)	0.0195 (16)	0.0137 (13)	0.0016 (11)	0.0047 (11)	0.0008 (10)
C4	0.0133 (15)	0.0159 (15)	0.0145 (12)	0.0045 (12)	0.0013 (10)	−0.0021 (10)
C5	0.0121 (15)	0.0184 (15)	0.0186 (13)	−0.0034 (12)	0.0030 (11)	−0.0012 (11)
C6	0.0113 (14)	0.0165 (15)	0.0168 (13)	−0.0007 (12)	0.0036 (11)	0.0023 (11)
C7	0.0136 (15)	0.0219 (16)	0.0170 (13)	0.0004 (13)	0.0035 (11)	0.0018 (11)
N1	0.0099 (13)	0.0182 (13)	0.0148 (11)	−0.0016 (10)	0.0027 (9)	−0.0013 (9)
O1	0.0145 (11)	0.0288 (12)	0.0164 (10)	−0.0054 (9)	0.0048 (8)	−0.0030 (8)
O2	0.0189 (12)	0.0352 (13)	0.0178 (10)	−0.0049 (10)	0.0087 (8)	0.0022 (9)
O3	0.0229 (13)	0.0446 (16)	0.0165 (10)	−0.0167 (10)	0.0087 (9)	−0.0084 (9)
O4	0.0184 (12)	0.0307 (13)	0.0178 (9)	−0.0134 (10)	0.0050 (8)	−0.0016 (8)
O5	0.0155 (11)	0.0272 (12)	0.0126 (9)	0.0033 (9)	−0.0001 (8)	−0.0052 (8)
O6	0.0329 (14)	0.0328 (14)	0.0226 (11)	0.0189 (11)	0.0118 (10)	0.0066 (10)
O7	0.0338 (15)	0.0226 (14)	0.0218 (11)	0.0025 (10)	0.0107 (10)	0.0009 (9)
O8	0.0394 (15)	0.0339 (14)	0.0198 (11)	0.0178 (11)	0.0163 (10)	0.0098 (10)
O9	0.0222 (15)	0.0273 (15)	0.0595 (18)	0.0038 (11)	0.0041 (13)	0.0031 (12)

Tb1—O5i	2.3035 (19)	C5—C6	1.367 (4)
Tb1—O8	2.368 (2)	C5—H5	0.9300
Tb1—O6	2.383 (2)	C6—N1	1.347 (4)
Tb1—O4ii	2.4106 (19)	C6—C7	1.492 (4)
Tb1—O3	2.415 (2)	C7—O4	1.256 (3)
Tb1—O7	2.416 (2)	C7—O3	1.257 (3)
Tb1—O1	2.424 (2)	O4—Tb1iii	2.4106 (19)
Tb1—N1	2.471 (2)	O5—Tb1iv	2.3035 (19)
C1—O2	1.245 (3)	O6—H1W	0.85 (4)
C1—O1	1.263 (3)	O6—H2W	0.86 (4)
C1—C2	1.508 (4)	O7—H3W	0.875 (16)
C2—N1	1.345 (4)	O7—H4W	0.85 (4)
C2—C3	1.377 (4)	O8—H5W	0.849 (16)
C3—C4	1.412 (4)	O8—H6W	0.85 (4)
C3—H3	0.9300	O9—H7W	0.86 (4)
C4—O5	1.315 (3)	O9—H8W	0.85 (4)
C4—C5	1.405 (4)
O5i—Tb1—O8	99.83 (8)	C3—C2—C1	123.8 (2)
O5i—Tb1—O6	85.81 (8)	C2—C3—C4	119.5 (3)
O8—Tb1—O6	148.11 (7)	C2—C3—H3	120.2
O5i—Tb1—O4ii	81.52 (7)	C4—C3—H3	120.2
O8—Tb1—O4ii	70.97 (7)	O5—C4—C5	121.4 (3)
O6—Tb1—O4ii	140.77 (7)	O5—C4—C3	122.2 (2)
O5i—Tb1—O3	151.44 (7)	C5—C4—C3	116.4 (2)
O8—Tb1—O3	93.13 (9)	C6—C5—C4	120.1 (3)
O6—Tb1—O3	96.50 (8)	C6—C5—H5	120.0
O4ii—Tb1—O3	78.83 (7)	C4—C5—H5	120.0
O5i—Tb1—O7	82.37 (8)	N1—C6—C5	123.3 (3)
O8—Tb1—O7	140.75 (8)	N1—C6—C7	113.5 (2)
O6—Tb1—O7	70.95 (8)	C5—C6—C7	123.2 (3)
O4ii—Tb1—O7	70.65 (7)	O4—C7—O3	124.5 (3)
O3—Tb1—O7	71.68 (8)	O4—C7—C6	118.9 (2)
O5i—Tb1—O1	80.00 (7)	O3—C7—C6	116.5 (3)
O8—Tb1—O1	74.95 (7)	C2—N1—C6	117.4 (2)
O6—Tb1—O1	75.22 (8)	C2—N1—Tb1	121.61 (19)
O4ii—Tb1—O1	137.48 (7)	C6—N1—Tb1	120.69 (18)
O3—Tb1—O1	128.19 (7)	C1—O1—Tb1	124.88 (18)
O7—Tb1—O1	142.73 (8)	C7—O3—Tb1	124.41 (18)
O5i—Tb1—N1	143.47 (8)	C7—O4—Tb1iii	138.84 (17)
O8—Tb1—N1	77.25 (8)	C4—O5—Tb1iv	127.69 (17)
O6—Tb1—N1	79.77 (8)	Tb1—O6—H1W	123 (2)
O4ii—Tb1—N1	129.18 (8)	Tb1—O6—H2W	114 (3)
O3—Tb1—N1	64.24 (7)	H1W—O6—H2W	112 (3)
O7—Tb1—N1	122.96 (8)	Tb1—O7—H3W	124 (2)
O1—Tb1—N1	63.95 (7)	Tb1—O7—H4W	125 (2)
O2—C1—O1	124.7 (3)	H3W—O7—H4W	110 (3)
O2—C1—C2	119.1 (2)	Tb1—O8—H5W	127 (2)
O1—C1—C2	116.2 (2)	Tb1—O8—H6W	109 (3)
N1—C2—C3	123.2 (3)	H5W—O8—H6W	115 (3)
N1—C2—C1	112.9 (2)	H7W—O9—H8W	114 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H1W···O1v	0.85 (4)	2.10 (3)	2.799 (3)	139 (3)
O6—H2W···O5vi	0.86 (4)	1.93 (3)	2.725 (3)	154 (3)
O7—H3W···O9vii	0.88 (2)	1.84 (2)	2.687 (3)	162 (4)
O7—H4W···O9	0.85 (4)	2.23 (3)	2.995 (4)	151 (3)
O8—H5W···O2viii	0.85 (2)	1.85 (2)	2.693 (3)	175 (4)
O8—H6W···O3ii	0.85 (4)	1.85 (4)	2.680 (3)	167 (4)
O9—H7W···O2ix	0.86 (4)	1.84 (2)	2.699 (3)	175 (4)
O9—H8W···O4i	0.85 (4)	2.37 (4)	3.073 (4)	141 (5)

Table 1

Selected bond lengths (Å)

Tb1—O5i	2.3035 (19)
Tb1—O8	2.368 (2)
Tb1—O6	2.383 (2)
Tb1—O4ii	2.4106 (19)
Tb1—O3	2.415 (2)
Tb1—O7	2.416 (2)
Tb1—O1	2.424 (2)
Tb1—N1	2.471 (2)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H1W⋯O1iii	0.85 (4)	2.10 (3)	2.799 (3)	139 (3)
O6—H2W⋯O5iv	0.86 (4)	1.93 (3)	2.725 (3)	154 (3)
O7—H3W⋯O9v	0.88 (2)	1.84 (2)	2.687 (3)	162 (4)
O7—H4W⋯O9	0.85 (4)	2.23 (3)	2.995 (4)	151 (3)
O8—H5W⋯O2vi	0.85 (2)	1.85 (2)	2.693 (3)	175 (4)
O8—H6W⋯O3ii	0.85 (4)	1.85 (4)	2.680 (3)	167 (4)
O9—H7W⋯O2vii	0.86 (4)	1.84 (2)	2.699 (3)	175 (4)
O9—H8W⋯O4i	0.85 (4)	2.37 (4)	3.073 (4)	141 (5)

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