Poly[(μ(4)-benzene-1,3,5-tricarboxyl-ato)bis-(N,N-dimethyl-acetamide)-terbium(III)].

The title compound, [Tb(C(9)H(3)O(6))(C(4)H(9)NO)(2)], shows a rare-earth three-dimensional metal-organic framework structure. In this complex of an eight-coordinated Tb(3+) ion, the asymmetric unit contains one benzene-1,3,5-tricarb-oxy-lic ligand and two coordinated dimethyl-acetamide mol-ecules. Each Tb(3+) ion is coordinated by six O atoms from four carboxyl-ate groups of the benzene-1,3,5-tricarb-oxy-lic ligands and two O atoms from two terminal dimethyl-acetamide mol-ecules.

Related literature

For metal-organic framework compounds with adsorption, catalytic and fluorescence properties, see: Sun et al. (2006 ▶); Ravon et al. (2008 ▶); Allendorf et al. (2009 ▶). For isotypic rare earth complexes, see: Thirumurugan & Natarajan (2004 ▶) and for rare earth coordination polymers, see: Guo et al. (2006 ▶).

Experimental

Crystal data

[Tb(C9H3O6)(C4H9NO)2]

M = 540.28

Monoclinic,

a = 10.8924 (6) Å

b = 16.7740 (9) Å

c = 10.9631 (6) Å

β = 102.254 (1)°

V = 1957.42 (18) Å3

Z = 4

Mo Kα radiation

μ = 3.66 mm−1

T = 273 K

0.60 × 0.40 × 0.40 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ▶) T min = 0.218, T max = 0.322

10235 measured reflections

3433 independent reflections

2385 reflections with I > 2σ(I)

R int = 0.055

Refinement

R[F 2 > 2σ(F 2)] = 0.034

wR(F 2) = 0.066

S = 0.89

3433 reflections

259 parameters

24 restraints

H-atom parameters constrained

Δρmax = 1.52 e Å−3

Δρmin = −0.79 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b ▶); molecular graphics: SHELXTL (Sheldrick, 2008b ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812010264/go2045sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812010264/go2045Isup2.hkl

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

[Tb(C9H3O6)(C4H9NO)2]	F(000) = 1064
Mr = 540.28	Dx = 1.833 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.8924 (6) Å	Cell parameters from 2246 reflections
b = 16.7740 (9) Å	θ = 2.3–22.4°
c = 10.9631 (6) Å	µ = 3.66 mm−1
β = 102.254 (1)°	T = 273 K
V = 1957.42 (18) Å3	Rod, colourless
Z = 4	0.60 × 0.40 × 0.40 mm

Bruker APEXII CCD diffractometer	3433 independent reflections
Radiation source: fine-focus sealed tube	2385 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.055
Detector resolution: 8.33 pixels mm-1	θmax = 25.0°, θmin = 2.3°
phi and ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	k = −17→19
Tmin = 0.218, Tmax = 0.322	l = −13→13
10235 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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066	H-atom parameters constrained
S = 0.89	w = 1/[σ2(Fo2) + (0.0188P)2] where P = (Fo2 + 2Fc2)/3
3433 reflections	(Δ/σ)max = 0.002
259 parameters	Δρmax = 1.52 e Å−3
24 restraints	Δρmin = −0.79 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
Tb1	0.65099 (3)	0.112365 (17)	−0.08321 (3)	0.02780 (11)
C1	0.6570 (6)	0.2120 (4)	0.1214 (6)	0.0390 (17)
C2	0.6452 (6)	0.2784 (4)	0.2122 (6)	0.0344 (16)
C3	0.7451 (6)	0.3279 (3)	0.2632 (6)	0.0337 (16)
H3	0.8227	0.3194	0.2428	0.040*
C4	0.7325 (5)	0.3896 (4)	0.3438 (5)	0.0283 (14)
C5	0.6154 (5)	0.4017 (3)	0.3746 (5)	0.0326 (16)
H5	0.6065	0.4423	0.4298	0.039*
C6	0.5112 (6)	0.3539 (4)	0.3241 (6)	0.0324 (16)
C7	0.5287 (6)	0.2932 (4)	0.2434 (6)	0.0372 (17)
H7	0.4607	0.2610	0.2087	0.045*
C8	0.8415 (6)	0.4454 (4)	0.3953 (6)	0.0311 (15)
C9	0.3875 (6)	0.3652 (4)	0.3574 (6)	0.0303 (16)
C10	0.5469 (7)	0.2846 (5)	−0.2411 (8)	0.062 (2)
C11	0.5890 (9)	0.2864 (5)	−0.3628 (8)	0.097 (3)
H11A	0.6323	0.2377	−0.3727	0.145*
H11B	0.6446	0.3307	−0.3633	0.145*
H11C	0.5172	0.2918	−0.4302	0.145*
C12	0.4520 (11)	0.3475 (6)	−0.0923 (11)	0.138 (5)
H12A	0.4480	0.2935	−0.0647	0.208*
H12B	0.3688	0.3694	−0.1135	0.208*
H12C	0.5023	0.3786	−0.0267	0.208*
C13	0.4954 (11)	0.4249 (6)	−0.2661 (10)	0.131 (4)
H13A	0.5156	0.4176	−0.3464	0.196*
H13B	0.5519	0.4630	−0.2189	0.196*
H13C	0.4107	0.4440	−0.2767	0.196*
C14	0.6376 (9)	−0.0207 (8)	−0.3242 (9)	0.094 (4)
C15	0.5893 (11)	−0.0955 (5)	−0.2590 (11)	0.131 (5)
H15A	0.6059	−0.1434	−0.3006	0.197*
H15B	0.5005	−0.0907	−0.2640	0.197*
H15C	0.6321	−0.0977	−0.1730	0.197*
C16	0.6552 (11)	−0.1129 (6)	−0.4926 (10)	0.140 (5)
H16A	0.6042	−0.1519	−0.4627	0.211*
H16B	0.7388	−0.1334	−0.4849	0.211*
H16C	0.6200	−0.1013	−0.5787	0.211*
C17	0.7101 (10)	0.0352 (7)	−0.4836 (10)	0.141 (5)
H17A	0.6452	0.0544	−0.5505	0.211*
H17B	0.7820	0.0201	−0.5159	0.211*
H17C	0.7332	0.0764	−0.4224	0.211*
N1	0.5073 (8)	0.3492 (5)	−0.1998 (8)	0.091 (2)
N2	0.6593 (8)	−0.0410 (5)	−0.4200 (8)	0.098 (3)
O1	0.7562 (4)	0.2041 (3)	0.0827 (4)	0.0467 (13)
O2	0.5632 (4)	0.1690 (3)	0.0810 (4)	0.0504 (13)
O3	0.3021 (4)	0.3156 (2)	0.3202 (4)	0.0395 (12)
O4	0.3703 (4)	0.4242 (2)	0.4224 (4)	0.0410 (12)
O5	0.8182 (4)	0.5022 (2)	0.4600 (4)	0.0447 (12)
O6	0.9428 (4)	0.4319 (2)	0.3650 (4)	0.0344 (11)
O7	0.5483 (4)	0.2215 (3)	−0.1834 (5)	0.0544 (14)
O8	0.6406 (5)	0.0438 (3)	−0.2719 (5)	0.0551 (14)

	U11	U22	U33	U12	U13	U23
Tb1	0.01970 (16)	0.02548 (17)	0.04074 (19)	0.00104 (17)	0.01207 (13)	0.00197 (17)
C1	0.034 (4)	0.037 (4)	0.049 (5)	−0.005 (3)	0.016 (4)	−0.011 (3)
C2	0.026 (4)	0.033 (4)	0.046 (4)	−0.007 (3)	0.011 (3)	−0.009 (3)
C3	0.023 (4)	0.031 (4)	0.052 (4)	0.000 (3)	0.020 (3)	−0.007 (3)
C4	0.022 (3)	0.028 (3)	0.036 (4)	0.000 (3)	0.007 (3)	−0.003 (3)
C5	0.030 (4)	0.033 (4)	0.038 (4)	0.001 (3)	0.015 (3)	−0.006 (3)
C6	0.029 (4)	0.033 (4)	0.039 (4)	−0.006 (3)	0.016 (3)	−0.007 (3)
C7	0.028 (4)	0.034 (4)	0.049 (4)	−0.009 (3)	0.009 (3)	−0.007 (3)
C8	0.023 (4)	0.035 (4)	0.036 (4)	0.002 (3)	0.009 (3)	0.001 (3)
C9	0.025 (4)	0.029 (4)	0.040 (4)	0.003 (3)	0.013 (3)	−0.003 (3)
C10	0.036 (5)	0.059 (6)	0.078 (7)	0.003 (4)	−0.014 (5)	−0.001 (5)
C11	0.092 (8)	0.111 (8)	0.079 (7)	0.000 (6)	−0.002 (6)	0.046 (6)
C12	0.152 (12)	0.108 (9)	0.145 (11)	0.077 (8)	0.008 (10)	−0.025 (8)
C13	0.145 (6)	0.109 (5)	0.126 (6)	−0.013 (4)	0.001 (4)	0.011 (4)
C14	0.058 (6)	0.152 (10)	0.068 (7)	0.016 (7)	0.005 (6)	−0.041 (7)
C15	0.163 (13)	0.065 (8)	0.179 (12)	−0.028 (7)	0.066 (10)	0.019 (7)
C16	0.156 (12)	0.139 (10)	0.125 (9)	0.008 (9)	0.027 (9)	−0.099 (8)
C17	0.126 (11)	0.195 (13)	0.117 (10)	−0.008 (9)	0.058 (9)	0.065 (9)
N1	0.099 (5)	0.066 (4)	0.095 (4)	0.008 (4)	−0.011 (4)	0.006 (4)
N2	0.093 (5)	0.103 (5)	0.094 (4)	0.015 (4)	0.013 (4)	−0.025 (4)
O1	0.025 (3)	0.058 (3)	0.062 (3)	−0.006 (2)	0.021 (3)	−0.025 (2)
O2	0.041 (3)	0.053 (3)	0.063 (3)	−0.018 (3)	0.025 (3)	−0.029 (3)
O3	0.026 (3)	0.036 (3)	0.061 (3)	−0.008 (2)	0.019 (2)	−0.016 (2)
O4	0.024 (3)	0.040 (3)	0.064 (3)	−0.004 (2)	0.022 (2)	−0.014 (2)
O5	0.026 (3)	0.041 (3)	0.068 (3)	−0.009 (2)	0.014 (3)	−0.028 (2)
O6	0.018 (2)	0.032 (3)	0.054 (3)	0.003 (2)	0.010 (2)	−0.006 (2)
O7	0.034 (3)	0.037 (3)	0.095 (4)	0.007 (2)	0.020 (3)	0.032 (3)
O8	0.055 (3)	0.054 (3)	0.062 (4)	−0.014 (3)	0.024 (3)	−0.026 (3)

Tb1—O5i	2.271 (4)	C11—H11A	0.9600
Tb1—O7	2.299 (4)	C11—H11B	0.9600
Tb1—O6ii	2.339 (4)	C11—H11C	0.9600
Tb1—O8	2.348 (5)	C12—N1	1.433 (11)
Tb1—O2	2.406 (4)	C12—H12A	0.9600
Tb1—O4iii	2.454 (4)	C12—H12B	0.9600
Tb1—O3iii	2.456 (4)	C12—H12C	0.9600
Tb1—O1	2.471 (4)	C13—N1	1.454 (10)
C1—O1	1.248 (7)	C13—H13A	0.9600
C1—O2	1.253 (7)	C13—H13B	0.9600
C1—C2	1.517 (8)	C13—H13C	0.9600
C2—C3	1.388 (8)	C14—N2	1.175 (10)
C2—C7	1.405 (8)	C14—O8	1.221 (11)
C3—C4	1.387 (7)	C14—C15	1.589 (13)
C3—H3	0.9300	C15—H15A	0.9600
C4—C5	1.402 (7)	C15—H15B	0.9600
C4—C8	1.523 (8)	C15—H15C	0.9600
C5—C6	1.403 (8)	C16—N2	1.440 (10)
C5—H5	0.9300	C16—H16A	0.9600
C6—C7	1.389 (8)	C16—H16B	0.9600
C6—C9	1.481 (8)	C16—H16C	0.9600
C7—H7	0.9300	C17—N2	1.609 (11)
C8—O6	1.238 (6)	C17—H17A	0.9600
C8—O5	1.246 (6)	C17—H17B	0.9600
C9—O3	1.250 (7)	C17—H17C	0.9600
C9—O4	1.257 (6)	O3—Tb1iv	2.456 (4)
C10—O7	1.232 (9)	O4—Tb1iv	2.454 (4)
C10—N1	1.285 (10)	O5—Tb1v	2.271 (4)
C10—C11	1.500 (11)	O6—Tb1vi	2.338 (4)
O5i—Tb1—O7	158.01 (15)	C6—C9—Tb1iv	179.1 (5)
O5i—Tb1—O6ii	84.24 (14)	O7—C10—N1	120.8 (9)
O7—Tb1—O6ii	77.77 (15)	O7—C10—C11	120.1 (8)
O5i—Tb1—O8	95.69 (17)	N1—C10—C11	119.1 (9)
O7—Tb1—O8	92.37 (18)	C10—C11—H11A	109.5
O6ii—Tb1—O8	76.59 (15)	C10—C11—H11B	109.5
O5i—Tb1—O2	84.73 (16)	H11A—C11—H11B	109.5
O7—Tb1—O2	79.21 (17)	C10—C11—H11C	109.5
O6ii—Tb1—O2	77.74 (14)	H11A—C11—H11C	109.5
O8—Tb1—O2	154.14 (16)	H11B—C11—H11C	109.5
O5i—Tb1—O4iii	76.21 (14)	N1—C12—H12A	109.5
O7—Tb1—O4iii	125.67 (15)	N1—C12—H12B	109.5
O6ii—Tb1—O4iii	144.63 (14)	H12A—C12—H12B	109.5
O8—Tb1—O4iii	76.37 (16)	N1—C12—H12C	109.5
O2—Tb1—O4iii	128.27 (16)	H12A—C12—H12C	109.5
O5i—Tb1—O3iii	128.97 (14)	H12B—C12—H12C	109.5
O7—Tb1—O3iii	72.82 (14)	N1—C13—H13A	109.5
O6ii—Tb1—O3iii	139.07 (14)	N1—C13—H13B	109.5
O8—Tb1—O3iii	76.85 (15)	H13A—C13—H13B	109.5
O2—Tb1—O3iii	122.52 (15)	N1—C13—H13C	109.5
O4iii—Tb1—O3iii	52.85 (13)	H13A—C13—H13C	109.5
O5i—Tb1—O1	94.68 (16)	H13B—C13—H13C	109.5
O7—Tb1—O1	87.62 (17)	N2—C14—O8	133.4 (13)
O6ii—Tb1—O1	130.58 (13)	N2—C14—C15	108.7 (11)
O8—Tb1—O1	151.84 (15)	O8—C14—C15	117.8 (9)
O2—Tb1—O1	53.07 (14)	C14—C15—H15A	109.5
O4iii—Tb1—O1	80.81 (14)	C14—C15—H15B	109.5
O3iii—Tb1—O1	76.26 (14)	H15A—C15—H15B	109.5
O1—C1—O2	121.3 (6)	C14—C15—H15C	109.5
O1—C1—C2	120.0 (6)	H15A—C15—H15C	109.5
O2—C1—C2	118.5 (6)	H15B—C15—H15C	109.5
C3—C2—C7	117.8 (6)	N2—C16—H16A	109.5
C3—C2—C1	122.3 (5)	N2—C16—H16B	109.5
C7—C2—C1	119.8 (6)	H16A—C16—H16B	109.5
C4—C3—C2	121.9 (5)	N2—C16—H16C	109.5
C4—C3—H3	119.1	H16A—C16—H16C	109.5
C2—C3—H3	119.1	H16B—C16—H16C	109.5
C3—C4—C5	118.7 (6)	N2—C17—H17A	109.5
C3—C4—C8	121.3 (5)	N2—C17—H17B	109.5
C5—C4—C8	120.0 (5)	H17A—C17—H17B	109.5
C4—C5—C6	121.5 (5)	N2—C17—H17C	109.5
C4—C5—H5	119.2	H17A—C17—H17C	109.5
C6—C5—H5	119.2	H17B—C17—H17C	109.5
C7—C6—C5	117.5 (5)	C10—N1—C12	120.3 (9)
C7—C6—C9	120.4 (6)	C10—N1—C13	124.1 (10)
C5—C6—C9	122.1 (5)	C12—N1—C13	114.8 (9)
C6—C7—C2	122.6 (6)	C14—N2—C16	138.5 (11)
C6—C7—H7	118.7	C14—N2—C17	108.0 (10)
C2—C7—H7	118.7	C16—N2—C17	113.5 (9)
O6—C8—O5	126.4 (6)	C1—O1—Tb1	90.9 (4)
O6—C8—C4	117.2 (6)	C1—O2—Tb1	93.8 (4)
O5—C8—C4	116.3 (5)	C9—O3—Tb1iv	93.0 (3)
O3—C9—O4	121.3 (5)	C9—O4—Tb1iv	92.9 (4)
O3—C9—C6	119.2 (5)	C8—O5—Tb1v	159.8 (4)
O4—C9—C6	119.5 (6)	C8—O6—Tb1vi	150.0 (4)
O3—C9—Tb1iv	60.7 (3)	C10—O7—Tb1	151.8 (5)
O4—C9—Tb1iv	60.6 (3)	C14—O8—Tb1	147.0 (7)
O1—C1—C2—C3	−5.5 (11)	O2—Tb1—O1—C1	−5.1 (4)
O2—C1—C2—C3	178.8 (7)	O4iii—Tb1—O1—C1	−160.2 (4)
O1—C1—C2—C7	172.2 (6)	O3iii—Tb1—O1—C1	146.0 (4)
O2—C1—C2—C7	−3.6 (10)	O1—C1—O2—Tb1	−9.5 (8)
C7—C2—C3—C4	0.7 (10)	C2—C1—O2—Tb1	166.2 (5)
C1—C2—C3—C4	178.4 (6)	O5i—Tb1—O2—C1	105.0 (5)
C2—C3—C4—C5	0.3 (9)	O7—Tb1—O2—C1	−90.1 (5)
C2—C3—C4—C8	−177.6 (6)	O6ii—Tb1—O2—C1	−169.7 (5)
C3—C4—C5—C6	−1.2 (9)	O8—Tb1—O2—C1	−162.8 (4)
C8—C4—C5—C6	176.8 (6)	O4iii—Tb1—O2—C1	37.2 (5)
C4—C5—C6—C7	0.8 (9)	O3iii—Tb1—O2—C1	−28.6 (5)
C4—C5—C6—C9	179.0 (6)	O1—Tb1—O2—C1	5.1 (4)
C5—C6—C7—C2	0.3 (10)	O4—C9—O3—Tb1iv	1.1 (6)
C9—C6—C7—C2	−177.9 (6)	C6—C9—O3—Tb1iv	−179.0 (5)
C3—C2—C7—C6	−1.1 (10)	O3—C9—O4—Tb1iv	−1.1 (6)
C1—C2—C7—C6	−178.8 (6)	C6—C9—O4—Tb1iv	179.0 (5)
C3—C4—C8—O6	−2.1 (9)	O6—C8—O5—Tb1v	−6.1 (17)
C5—C4—C8—O6	180.0 (5)	C4—C8—O5—Tb1v	177.0 (9)
C3—C4—C8—O5	175.2 (6)	O5—C8—O6—Tb1vi	74.9 (11)
C5—C4—C8—O5	−2.7 (9)	C4—C8—O6—Tb1vi	−108.2 (8)
C7—C6—C9—O3	5.8 (9)	N1—C10—O7—Tb1	−122.4 (11)
C5—C6—C9—O3	−172.3 (6)	C11—C10—O7—Tb1	59.0 (15)
C7—C6—C9—O4	−174.3 (6)	O5i—Tb1—O7—C10	165.9 (11)
C5—C6—C9—O4	7.6 (9)	O6ii—Tb1—O7—C10	−158.3 (12)
O7—C10—N1—C12	−6.3 (13)	O8—Tb1—O7—C10	−82.5 (12)
C11—C10—N1—C12	172.2 (9)	O2—Tb1—O7—C10	122.1 (12)
O7—C10—N1—C13	−176.0 (8)	O4iii—Tb1—O7—C10	−7.6 (13)
C11—C10—N1—C13	2.6 (14)	O3iii—Tb1—O7—C10	−7.1 (12)
O8—C14—N2—C16	−177.2 (11)	O1—Tb1—O7—C10	69.3 (12)
C15—C14—N2—C16	−0.4 (18)	N2—C14—O8—Tb1	−160.2 (9)
O8—C14—N2—C17	4.1 (17)	C15—C14—O8—Tb1	23.3 (16)
C15—C14—N2—C17	−179.2 (8)	O5i—Tb1—O8—C14	6.7 (11)
O2—C1—O1—Tb1	9.3 (7)	O7—Tb1—O8—C14	−152.8 (11)
C2—C1—O1—Tb1	−166.4 (6)	O6ii—Tb1—O8—C14	−76.0 (11)
O5i—Tb1—O1—C1	−85.0 (4)	O2—Tb1—O8—C14	−83.0 (12)
O7—Tb1—O1—C1	73.1 (4)	O4iii—Tb1—O8—C14	81.0 (11)
O6ii—Tb1—O1—C1	1.5 (5)	O3iii—Tb1—O8—C14	135.4 (11)
O8—Tb1—O1—C1	163.7 (4)	O1—Tb1—O8—C14	117.8 (10)