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

The asymmetric unit of the title compound, {[Tb(C(8)H(2)NO(6))(H(2)O)(3)]·H(2)O}(n), contains one Tb(III) ion, one pyridine-2,4,6-tricarboxyl-ate (ptc) anion, three aqua ligands and one lattice water mol-ecule. The Tb(III) ion is nine coordinated by one N and five O atoms from three ptc ligands and by three O atoms from the three aqua ligands in a distorted bicapped trigonal-prismatic geometry. The ptc ligands bridge the Tb(III) ions into a two-dimensional polymeric framework parallel to (100). An extensive O-H⋯O hydrogen-bonding network consolidates the crystal packing.

Related literature

For the crystal structures of related complexes, see: Das et al. (2009 ▶); Wang & Zhang (2009 ▶); Wang et al. (2010 ▶); Lin et al. (2011 ▶); Jin et al. (2012 ▶).

Experimental

Crystal data

[Tb(C8H2NO6)(H2O)3]·H2O

M = 439.09

Monoclinic,

a = 11.936 (2) Å

b = 7.3343 (15) Å

c = 13.516 (3) Å

β = 96.43 (3)°

V = 1175.8 (4) Å3

Z = 4

Mo Kα radiation

μ = 6.07 mm−1

T = 293 K

0.32 × 0.30 × 0.28 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.164, T max = 0.183

10998 measured reflections

2664 independent reflections

2528 reflections with I > 2σ(I)

R int = 0.066

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.067

S = 1.06

2664 reflections

182 parameters

H-atom parameters constrained

Δρmax = 2.18 e Å−3

Δρmin = −1.11 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ▶); 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: SHELXL97.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812028929/cv5315sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812028929/cv5315Isup2.hkl

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

[Tb(C8H2NO6)(H2O)3]·H2O	F(000) = 840
Mr = 439.09	Dx = 2.480 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9883 reflections
a = 11.936 (2) Å	θ = 3.0–27.4°
b = 7.3343 (15) Å	µ = 6.07 mm−1
c = 13.516 (3) Å	T = 293 K
β = 96.43 (3)°	Block, colorless
V = 1175.8 (4) Å3	0.32 × 0.30 × 0.28 mm
Z = 4

Rigaku R-AXIS RAPID diffractometer	2664 independent reflections
Radiation source: fine-focus sealed tube	2528 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.066
Detector resolution: 0 pixels mm-1	θmax = 27.4°, θmin = 3.0°
ω scan	h = −15→15
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −9→9
Tmin = 0.164, Tmax = 0.183	l = −17→15
10998 measured reflections

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)] = 0.028	H-atom parameters constrained
wR(F2) = 0.067	w = 1/[σ2(Fo2) + (0.0172P)2 + 1.9544P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max = 0.001
2664 reflections	Δρmax = 2.18 e Å−3
182 parameters	Δρmin = −1.11 e Å−3
0 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: 0.0031 (4)

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
Tb	0.285028 (12)	1.21386 (2)	0.704284 (11)	0.01088 (9)
N	0.2959 (2)	1.0044 (4)	0.8499 (2)	0.0132 (5)
C1	0.3926 (3)	0.9190 (5)	0.8812 (2)	0.0140 (6)
C2	0.3992 (3)	0.7853 (5)	0.9547 (3)	0.0165 (7)
H2A	0.4669	0.7266	0.9750	0.020*
C3	0.3023 (3)	0.7424 (5)	0.9978 (3)	0.0167 (7)
C4	0.2025 (3)	0.8380 (5)	0.9689 (3)	0.0160 (7)
H4A	0.1382	0.8183	1.0000	0.019*
C5	0.2033 (3)	0.9641 (5)	0.8917 (2)	0.0141 (7)
C6	0.4904 (3)	0.9703 (4)	0.8255 (2)	0.0137 (6)
O1	0.4681 (2)	1.0675 (4)	0.74843 (18)	0.0186 (5)
O2	0.58643 (19)	0.9109 (3)	0.85646 (18)	0.0168 (5)
C7	0.2986 (3)	0.5894 (5)	1.0710 (2)	0.0162 (7)
O3	0.3445 (2)	0.4402 (4)	1.05122 (18)	0.0209 (5)
O4	0.2479 (2)	0.6092 (4)	1.14653 (19)	0.0238 (6)
C8	0.0984 (3)	1.0619 (5)	0.8451 (3)	0.0163 (7)
O5	0.0075 (2)	1.0267 (4)	0.8774 (2)	0.0250 (6)
O6	0.1127 (2)	1.1688 (4)	0.7744 (2)	0.0228 (6)
O7	0.1990 (2)	1.5188 (4)	0.7163 (2)	0.0262 (6)
H7A	0.1317	1.5476	0.7166	0.031*
H7B	0.2563	1.5872	0.7231	0.031*
O8	0.1356 (3)	1.2471 (4)	0.5676 (2)	0.0296 (7)
H8A	0.0844	1.3275	0.5632	0.050*
H8B	0.1167	1.1746	0.5237	0.050*
O9	0.3781 (2)	1.3706 (4)	0.85261 (19)	0.0243 (6)
H9A	0.4225	1.4272	0.8240	0.029*
H9B	0.3690	1.3909	0.9095	0.029*
O10	0.0703 (4)	0.4780 (5)	0.9079 (3)	0.0481 (9)
H10A	0.0413	0.4022	0.8662	0.058*
H10B	0.1358	0.4736	0.8891	0.058*

	U11	U22	U33	U12	U13	U23
Tb	0.00838 (12)	0.01147 (13)	0.01279 (13)	−0.00008 (5)	0.00110 (8)	0.00033 (5)
N	0.0100 (13)	0.0133 (13)	0.0162 (13)	−0.0010 (11)	0.0007 (11)	0.0008 (11)
C1	0.0118 (15)	0.0129 (16)	0.0164 (15)	0.0003 (12)	−0.0022 (13)	−0.0011 (12)
C2	0.0119 (17)	0.0182 (19)	0.0188 (18)	0.0026 (12)	−0.0008 (15)	0.0034 (12)
C3	0.0205 (18)	0.0126 (15)	0.0168 (18)	0.0009 (14)	0.0015 (16)	0.0023 (13)
C4	0.0133 (16)	0.0159 (17)	0.0200 (17)	0.0012 (13)	0.0073 (14)	0.0029 (14)
C5	0.0141 (15)	0.0150 (17)	0.0127 (15)	0.0000 (12)	0.0000 (13)	0.0005 (12)
C6	0.0140 (15)	0.0084 (15)	0.0185 (16)	0.0013 (12)	0.0015 (13)	−0.0025 (12)
O1	0.0135 (11)	0.0220 (13)	0.0209 (12)	0.0040 (10)	0.0048 (10)	0.0084 (10)
O2	0.0109 (11)	0.0172 (13)	0.0215 (12)	0.0043 (9)	−0.0015 (10)	−0.0011 (10)
C7	0.0151 (16)	0.0159 (17)	0.0173 (16)	−0.0001 (13)	0.0001 (14)	0.0042 (13)
O3	0.0251 (13)	0.0172 (13)	0.0209 (12)	0.0047 (10)	0.0049 (11)	0.0059 (10)
O4	0.0320 (15)	0.0197 (14)	0.0214 (13)	0.0071 (11)	0.0108 (12)	0.0069 (10)
C8	0.0132 (15)	0.0160 (16)	0.0200 (16)	0.0008 (13)	0.0027 (14)	0.0017 (13)
O5	0.0092 (11)	0.0335 (16)	0.0321 (14)	−0.0009 (10)	0.0022 (11)	0.0106 (12)
O6	0.0162 (12)	0.0288 (15)	0.0242 (14)	0.0063 (11)	0.0052 (11)	0.0133 (11)
O7	0.0150 (12)	0.0184 (14)	0.0441 (17)	0.0012 (10)	−0.0016 (12)	0.0001 (12)
O8	0.0257 (16)	0.0348 (16)	0.0257 (16)	0.0121 (12)	−0.0084 (14)	−0.0057 (12)
O9	0.0280 (14)	0.0269 (15)	0.0180 (12)	−0.0104 (12)	0.0029 (11)	−0.0044 (11)
O10	0.067 (2)	0.041 (2)	0.0368 (17)	0.0117 (18)	0.0046 (18)	−0.0032 (15)

Tb—O2i	2.324 (2)	C5—C8	1.518 (4)
Tb—O6	2.382 (3)	C6—O2	1.253 (4)
Tb—O8	2.432 (3)	C6—O1	1.266 (4)
Tb—O1	2.448 (2)	O2—Tbiii	2.324 (2)
Tb—O9	2.465 (3)	C7—O4	1.253 (4)
Tb—O7	2.474 (3)	C7—O3	1.266 (4)
Tb—N	2.488 (3)	C7—Tbiv	2.878 (3)
Tb—O4ii	2.518 (3)	O3—Tbiv	2.528 (3)
Tb—O3ii	2.528 (3)	O4—Tbiv	2.518 (3)
Tb—C7ii	2.878 (3)	C8—O5	1.241 (4)
N—C5	1.329 (4)	C8—O6	1.263 (4)
N—C1	1.340 (4)	O7—H7A	0.8302
C1—C2	1.392 (5)	O7—H7B	0.8454
C1—C6	1.506 (5)	O8—H8A	0.8470
C2—C3	1.387 (6)	O8—H8B	0.8095
C2—H2A	0.9293	O9—H9A	0.8057
C3—C4	1.400 (5)	O9—H9B	0.8018
C3—C7	1.500 (5)	O10—H10A	0.8390
C4—C5	1.396 (5)	O10—H10B	0.8498
C4—H4A	0.9271
O2i—Tb—O6	149.38 (9)	C5—N—C1	119.3 (3)
O2i—Tb—O8	97.26 (11)	C5—N—Tb	120.1 (2)
O6—Tb—O8	73.97 (11)	C1—N—Tb	120.3 (2)
O2i—Tb—O1	75.64 (9)	N—C1—C2	122.2 (3)
O6—Tb—O1	128.99 (8)	N—C1—C6	114.5 (3)
O8—Tb—O1	141.98 (10)	C2—C1—C6	123.2 (3)
O2i—Tb—O9	75.06 (9)	C3—C2—C1	118.5 (3)
O6—Tb—O9	94.10 (10)	C3—C2—H2A	120.6
O8—Tb—O9	142.78 (10)	C1—C2—H2A	120.9
O1—Tb—O9	72.40 (10)	C2—C3—C4	119.5 (3)
O2i—Tb—O7	75.90 (9)	C2—C3—C7	122.3 (3)
O6—Tb—O7	73.49 (10)	C4—C3—C7	118.2 (3)
O8—Tb—O7	71.63 (10)	C5—C4—C3	117.6 (3)
O1—Tb—O7	138.26 (9)	C5—C4—H4A	121.2
O9—Tb—O7	71.18 (9)	C3—C4—H4A	121.2
O2i—Tb—N	133.27 (9)	N—C5—C4	122.7 (3)
O6—Tb—N	64.57 (9)	N—C5—C8	113.9 (3)
O8—Tb—N	129.16 (11)	C4—C5—C8	123.3 (3)
O1—Tb—N	64.56 (9)	O2—C6—O1	124.9 (3)
O9—Tb—N	70.47 (9)	O2—C6—C1	118.5 (3)
O7—Tb—N	119.42 (10)	O1—C6—C1	116.6 (3)
O2i—Tb—O4ii	125.16 (9)	C6—O1—Tb	123.2 (2)
O6—Tb—O4ii	82.13 (10)	C6—O2—Tbiii	135.5 (2)
O8—Tb—O4ii	76.72 (10)	O4—C7—O3	122.2 (3)
O1—Tb—O4ii	77.54 (9)	O4—C7—C3	120.2 (3)
O9—Tb—O4ii	137.60 (9)	O3—C7—C3	117.6 (3)
O7—Tb—O4ii	144.19 (9)	O4—C7—Tbiv	60.86 (18)
N—Tb—O4ii	69.89 (9)	O3—C7—Tbiv	61.32 (18)
O2i—Tb—O3ii	74.43 (9)	C3—C7—Tbiv	177.3 (2)
O6—Tb—O3ii	126.72 (10)	C7—O3—Tbiv	92.6 (2)
O8—Tb—O3ii	70.88 (10)	C7—O4—Tbiv	93.4 (2)
O1—Tb—O3ii	71.25 (9)	O5—C8—O6	126.4 (3)
O9—Tb—O3ii	137.04 (9)	O5—C8—C5	118.0 (3)
O7—Tb—O3ii	127.92 (9)	O6—C8—C5	115.6 (3)
N—Tb—O3ii	112.14 (9)	C8—O6—Tb	125.7 (2)
O4ii—Tb—O3ii	51.80 (9)	Tb—O7—H7A	129.7
O2i—Tb—C7ii	100.00 (10)	Tb—O7—H7B	101.9
O6—Tb—C7ii	104.70 (10)	H7A—O7—H7B	128.4
O8—Tb—C7ii	71.93 (10)	Tb—O8—H8A	125.8
O1—Tb—C7ii	72.68 (9)	Tb—O8—H8B	127.7
O9—Tb—C7ii	144.85 (10)	H8A—O8—H8B	105.4
O7—Tb—C7ii	142.43 (9)	Tb—O9—H9A	96.4
N—Tb—C7ii	90.95 (10)	Tb—O9—H9B	140.3
O4ii—Tb—C7ii	25.75 (10)	H9A—O9—H9B	122.1
O3ii—Tb—C7ii	26.05 (9)	H10A—O10—H10B	95.6

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O5v	0.83	1.98	2.642 (4)	136
O7—H7B···O4vi	0.84	2.45	2.966 (4)	120
O8—H8A···O5v	0.85	2.04	2.822 (4)	152
O8—H8B···O10ii	0.81	1.95	2.760 (5)	174
O9—H9A···O1i	0.81	2.00	2.808 (4)	179
O9—H9B···O3vii	0.81	2.00	2.805 (4)	179
O10—H10A···O6viii	0.84	2.33	2.977 (5)	134
O10—H10B···O7viii	0.85	2.55	3.169 (5)	130

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O5i	0.83	1.98	2.642 (4)	136
O7—H7B⋯O4ii	0.84	2.45	2.966 (4)	120
O8—H8A⋯O5i	0.85	2.04	2.822 (4)	152
O8—H8B⋯O10iii	0.81	1.95	2.760 (5)	174
O9—H9A⋯O1iv	0.81	2.00	2.808 (4)	179
O9—H9B⋯O3v	0.81	2.00	2.805 (4)	179
O10—H10A⋯O6vi	0.84	2.33	2.977 (5)	134
O10—H10B⋯O7vi	0.85	2.55	3.169 (5)	130

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