Poly[[triaqua­(μ3-4-oxidopyridine-2,6-dicarboxyl­ato)terbium(III)] monohydrate]

Lv, D.-Y.; Gao, Z.-Q.; Gu, J.-Z.

doi:10.1107/S1600536811005447

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 3| March 2011| Pages m357-m358

doi:10.1107/S1600536811005447

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Poly[[triaqua(μ₃-4-oxidopyridine-2,6-dicarboxylato)terbium(III)] monohydrate]

Dong-Yu Lv,^a ^* Zhu-Qing Gao ^b and Jin-Zhong Gu ^a

^aKey Laboratory of Nonferrous Metal Chemistry and Resources Utilization of Gansu Province, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, People's Republic of China, and ^bSchool of Chemistry and Biology Engineering, Taiyuan University of Science and Technology, Taiyuan 030021, People's Republic of China
^*Correspondence e-mail: lvdy@lzu.edu.cn

(Received 10 January 2011; accepted 14 February 2011; online 23 February 2011)

In the title coordination polymer, {[Tb(C₇H₂NO₅)(H₂O)₃]·H₂O}_n, the Tb^III atom is eight-coordinated by a tridentate 4-oxidopyridine-2,6-dicarboxylate trianion, two adjacent monodentate anions and three water molecules, forming a distorted bicapped trigonal–prismatic TbNO₇ coordination environment. The anions bridge adjacent Tb^III ions into double chains. Adjacent chains are further connected into sheets parallel to (10 $[\overline{1}]$ ). O—H⋯O hydrogen bonds involving both coordinated and uncoordinated water molecules 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 Tb^III, see: Chen et al. (2008 ); Ramya et al. (2010 ).

Experimental

Crystal data

[Tb(C₇H₂NO₅)(H₂O)₃]·H₂O
M_r = 411.08
Monoclinic, P 2₁ /n
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[F² > 2σ(F²)] = 0.019
wR(F²) = 0.051
S = 1.10
2080 reflections
196 parameters
12 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.34 e Å⁻³
Δρ_min = −0.60 e Å⁻³

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) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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⋯O5^iv	0.86 (4)	1.93 (3)	2.725 (3)	154 (3)
O7—H3W⋯O9^v	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⋯O2^vi	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⋯O2^vii	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) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) -x+1, -y+1, -z; (v) -x+1, -y+1, -z+1; (vi) -x+1, -y+2, -z; (vii) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

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 ).

Supporting information

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

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

checkCIF report

Comment top

The design and synthesis of luminescent lanthanide coordination polymers have achieved great progress during the last years owing to their potential applications in biomedical imaging, as luminescent sensors or as fluorescent probes (Kustaryono et al., 2010; He et al., 2010). Eu and Tb are the most useful lanthanides due to their good fluorescence properties (Li et al., 2008; Luo et al., 2008). Many multi-carboxylate or heterocylic carboxylic acids are used for designing such materials (Li et al., 2008; Luo et al., 2008). For lanthanide coordination polymers, 4-hydroxy-pyridine-2,6-dicarboxylic acid is an excellent bridging pyridine dicarboxylate ligand (Lv et al., 2010; Gao et al., 2008), which can provide at most one nitrogen atom and five O coordination sites. In order to extend the investigation in this field, we synthesized the lanthanide coordination polymer {[Tb(C₇H₂NO₅)(H₂O)₃]^.H₂O}, and report its structure here.

The title compound is isotypic with its Dy (Gao et al., 2006) and Eu (Lv et al., 2010) analogues. As shown in Fig.1, the asymmetric unit contains one Tb(III) ion, one 4-oxidopyridine-2,6-dicarboxylate anion, three coordinated water molecules, and one water molecule of crystallisation. The Tb atom is eight-coordinated by seven oxygen atoms from three anions and three coordinated water molecules and by one nitrogen atom from one tridentate anion (the other two anions are monodentate), forming a distorted bicapped trigonal-prismatic coordination environment.

Important bond distances and angles are presented in Table 1. The Tb—O bond lengths [2.3035 (19) to 2.424 (2) Å] are shorter than the Tb—N bond length [2.471 (2) Å], which is in agreement with the bond lengths observed in other Tb(III) complexes (Chen et al., 2008; Ramya et al., 2010). The anion adopts a µ₃-pentadentate coordination mode, as shown in Fig. 1. The anions bridge adjacent Tb^III ions to form infinite double chains (Fig. 2). Adjacent chains are further connected by the coordination of the anions and Tb(III) ions into a two-dimensional sheet parallel to (101) (Fig. 3), which are further extended into a three-dimensional framework through O—H···O hydrogen-bonding interactions including both coordinated and uncoordinated water molecules (Table 2).

Related literature top

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 Tb^III, see: Chen et al. (2008); Ramya et al. (2010).

Experimental top

To a solution of terbium(III) nitrate hexahydrate (0.136 g, 0.3 mmol) in water (5 ml) was added an aqueous solution (5 ml) of the ligand (0.060 g, 0.3 mmol) and a drop of triethylamine. The reactants were sealed in a 25-ml Teflon-lined stainless-steel Parr bomb. The bomb was heated at 433 K for 3 days. The cool solution contained single crystals in ca 60% yield. Anal. Calcd for C₇H₁₀TbNO₉: C, 20.45; H, 2.45; N, 3.41. Found: C, 20.16; H, 2.17; N, 3.74.

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

Figures top

	Fig. 1. Drawing of the asymmetric unit of the title compound, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level.
	Fig. 2. View along the b axis of the title compound, showing the double chain.
	Fig. 3. View approximately along the a axis, showing the sheet structure of {[Tb(C₇H₂NO₅)(H₂O)₃]^.H₂O}.

Poly[[triaqua(µ₃-4-oxidopyridine-2,6-dicarboxylato)terbium(III)] monohydrate] top

Crystal data top

[Tb(C₇H₂NO₅)(H₂O)₃]·H₂O	F(000) = 784
M_r = 411.08	D_x = 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

Data collection top

Bruker APEXII CCD diffractometer	2080 independent reflections
Radiation source: fine-focus sealed tube	1929 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ϕ and ω scans	θ_max = 25.5°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −12→11
T_min = 0.162, T_max = 0.247	k = −9→8
7828 measured reflections	l = −18→18

Refinement top

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(F_o²) + (0.0227P)² + 0.941P] where P = (F_o² + 2F_c²)/3
S = 1.10	(Δ/σ)_max = 0.001
2080 reflections	Δρ_max = 1.34 e Å⁻³
196 parameters	Δρ_min = −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)

Crystal data top

[Tb(C₇H₂NO₅)(H₂O)₃]·H₂O	V = 1120.9 (4) Å³
M_r = 411.08	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.953 (2) Å	µ = 6.35 mm⁻¹
b = 7.5454 (16) Å	T = 293 K
c = 15.461 (3) Å	0.30 × 0.25 × 0.22 mm
β = 105.126 (2)°

Data collection top

Bruker APEXII CCD diffractometer	2080 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	1929 reflections with I > 2σ(I)
T_min = 0.162, T_max = 0.247	R_int = 0.032
7828 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	12 restraints
wR(F²) = 0.051	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	Δρ_max = 1.34 e Å⁻³
2080 reflections	Δρ_min = −0.60 e Å⁻³
196 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
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—Tb1^iv	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—Tb1^iv	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)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H1W···O1^v	0.85 (4)	2.10 (3)	2.799 (3)	139 (3)
O6—H2W···O5^vi	0.86 (4)	1.93 (3)	2.725 (3)	154 (3)
O7—H3W···O9^vii	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···O2^viii	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···O2^ix	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) x+1/2, −y+3/2, z+1/2; (ii) −x+1/2, y+1/2, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) −x+1, −y+1, −z; (vii) −x+1, −y+1, −z+1; (viii) −x+1, −y+2, −z; (ix) x−1/2, −y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula	[Tb(C₇H₂NO₅)(H₂O)₃]·H₂O
M_r	411.08
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	9.953 (2), 7.5454 (16), 15.461 (3)
β (°)	105.126 (2)
V (Å³)	1120.9 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	6.35
Crystal size (mm)	0.30 × 0.25 × 0.22

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.162, 0.247
No. of measured, independent and observed [I > 2σ(I)] reflections	7828, 2080, 1929
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.051, 1.10
No. of reflections	2080
No. of parameters	196
No. of restraints	12
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.34, −0.60

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Putz, 2005), publCIF (Westrip, 2010).

Selected bond lengths (Å) top

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

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

Hydrogen-bond geometry (Å, º) top

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···O5^iv	0.86 (4)	1.93 (3)	2.725 (3)	154 (3)
O7—H3W···O9^v	0.875 (16)	1.84 (2)	2.687 (3)	162 (4)
O7—H4W···O9	0.85 (4)	2.23 (3)	2.995 (4)	151 (3)
O8—H5W···O2^vi	0.849 (19)	1.847 (19)	2.693 (3)	175 (4)
O8—H6W···O3ⁱⁱ	0.85 (4)	1.85 (4)	2.680 (3)	167 (4)
O9—H7W···O2^vii	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) x+1/2, −y+3/2, z+1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x+3/2, y−1/2, −z+1/2; (iv) −x+1, −y+1, −z; (v) −x+1, −y+1, −z+1; (vi) −x+1, −y+2, −z; (vii) x−1/2, −y+3/2, z+1/2.

References

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