Poly[tris-(dimethyl-formamide)(μ3-2,4,6-triiodobenzene-1,3,5-tricarboxyl-ato)samarium(III)].

In the title compound, [Sm(C9I3O6)(C3H7NO)3] n , the Sm(III) atom is coordinated by nine O atoms, viz. six carboxyl-ate O atoms from three 2,4,6-triiodobenzene-1,3,5-tricarboxyl-ate (I3BTC) ligands and three O atoms from three N,N-dimethyl-formamide (DMF) mol-ecules. Each I3BTC ligand bridges three Sm(III) atoms, generating a three-dimensional metal-organic framework structure. The asymmetric unit contains one Sm(III) ion and one I3BTC anion, both situated on a threefold axis, and one DMF mol-ecule in a general position.

Related literature

For applications of compounds with metal-organic framework structures (MOFs), see: Nakanishi & Tanaka (2007 ▶); Phan et al. (2010 ▶); Suib et al. (2008 ▶). For related structures, see: Daiguebonne et al. (2002 ▶); Han et al. (2012 ▶); Lu et al. (2008 ▶); Serre et al. (2004 ▶).

Experimental

Crystal data

[Sm(C9I3O6)(C3H7NO)3]

M = 954.43

Cubic,

a = 14.1341 (16) Å

V = 2823.6 (6) Å3

Z = 4

Mo Kα radiation

μ = 5.41 mm−1

T = 295 K

0.16 × 0.15 × 0.15 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.478, T max = 0.498

5119 measured reflections

2143 independent reflections

2026 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.049

S = 1.03

2143 reflections

106 parameters

H-atom parameters constrained

Δρmax = 0.72 e Å−3

Δρmin = −0.62 e Å−3

Absolute structure: Flack (1983 ▶), 943 Friedel pairs

Flack parameter: 0.02 (2)

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: WinGX (Farrugia, 2012 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813003358/cv5378sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813003358/cv5378Isup2.hkl

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

[Sm(C9I3O6)(C3H7NO)3]	Dx = 2.245 Mg m−3
Mr = 954.43	Mo Kα radiation, λ = 0.71073 Å
Cubic, P213	Cell parameters from 2685 reflections
Hall symbol: P 2ac 2ab 3	θ = 3.2–27.2°
a = 14.1341 (16) Å	µ = 5.41 mm−1
V = 2823.6 (6) Å3	T = 295 K
Z = 4	Prism, yellow
F(000) = 1772	0.16 × 0.15 × 0.15 mm

Bruker APEXII CCD area-detector diffractometer	2143 independent reflections
Radiation source: fine-focus sealed tube	2026 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 27.4°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −12→7
Tmin = 0.478, Tmax = 0.498	k = 0→18
5119 measured reflections	l = −16→12

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.021	w = 1/[σ2(Fo2) + (0.0236P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.049	(Δ/σ)max = 0.002
S = 1.03	Δρmax = 0.72 e Å−3
2143 reflections	Δρmin = −0.62 e Å−3
106 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints	Extinction coefficient: 0.00049 (7)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 943 Friedel pairs
Secondary atom site location: difference Fourier map	Flack parameter: 0.02 (2)

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. SHELXTL (Sheldrick, 2008)

	x	y	z	Uiso*/Ueq
O2	0.9837 (2)	−0.17185 (19)	0.4744 (2)	0.0341 (7)
C1	0.9099 (3)	−0.1640 (3)	0.4268 (3)	0.0219 (8)
C2	0.8710 (2)	−0.2536 (3)	0.3796 (3)	0.0227 (8)
C3	0.9151 (3)	−0.2914 (3)	0.2996 (3)	0.0236 (8)
C4	0.8963 (4)	0.2099 (3)	0.4875 (4)	0.0464 (12)
H4	0.9575	0.2290	0.5023	0.056*
C5	0.8521 (6)	0.3734 (5)	0.5058 (7)	0.125 (4)
H5A	0.8541	0.4090	0.4479	0.187*
H5B	0.9125	0.3772	0.5367	0.187*
H5C	0.8042	0.3990	0.5465	0.187*
C6	0.7318 (5)	0.2501 (7)	0.4593 (7)	0.126 (4)
H6A	0.7297	0.1860	0.4370	0.189*
H6B	0.7099	0.2918	0.4103	0.189*
H6C	0.6920	0.2564	0.5139	0.189*
I1	1.03806 (2)	−0.22509 (2)	0.248693 (19)	0.03739 (10)
N1	0.8303 (4)	0.2748 (3)	0.4848 (4)	0.0687 (14)
O1	0.8674 (2)	−0.08834 (19)	0.4139 (2)	0.0304 (6)
O3	0.8828 (2)	0.1250 (2)	0.4717 (2)	0.0428 (8)
Sm1	0.999507 (13)	0.000493 (13)	0.500493 (13)	0.01931 (8)

	U11	U22	U33	U12	U13	U23
O2	0.0346 (17)	0.0259 (14)	0.0419 (17)	0.0000 (12)	−0.0116 (13)	−0.0055 (12)
C1	0.0222 (19)	0.0212 (19)	0.0224 (19)	−0.0053 (15)	0.0077 (15)	−0.0030 (15)
C2	0.0207 (19)	0.022 (2)	0.025 (2)	−0.0016 (15)	−0.0020 (14)	−0.0003 (15)
C3	0.0211 (19)	0.026 (2)	0.0234 (19)	−0.0046 (15)	0.0047 (15)	0.0007 (15)
C4	0.050 (3)	0.042 (3)	0.047 (3)	0.022 (2)	0.000 (2)	0.005 (2)
C5	0.170 (9)	0.061 (5)	0.143 (8)	0.061 (5)	−0.040 (7)	−0.039 (5)
C6	0.072 (5)	0.147 (10)	0.160 (9)	0.056 (6)	−0.011 (5)	−0.011 (6)
I1	0.03269 (16)	0.04066 (18)	0.03881 (18)	−0.01484 (12)	0.01194 (11)	−0.00927 (13)
N1	0.086 (4)	0.053 (3)	0.067 (3)	0.046 (3)	0.003 (3)	−0.007 (2)
O1	0.0303 (16)	0.0243 (15)	0.0365 (17)	0.0005 (12)	−0.0038 (13)	−0.0024 (12)
O3	0.0369 (18)	0.0390 (19)	0.053 (2)	0.0154 (14)	0.0044 (15)	0.0053 (16)
Sm1	0.01931 (8)	0.01931 (8)	0.01931 (8)	0.00093 (7)	0.00093 (7)	−0.00093 (7)

O2—C1	1.245 (5)	C5—H5C	0.9600
O2—Sm1	2.474 (3)	C6—N1	1.480 (10)
C1—O1	1.240 (5)	C6—H6A	0.9600
C1—C2	1.534 (5)	C6—H6B	0.9600
C1—Sm1	2.844 (4)	C6—H6C	0.9600
C2—C3i	1.393 (5)	O1—Sm1	2.562 (3)
C2—C3	1.397 (5)	O3—Sm1	2.446 (3)
C3—C2ii	1.393 (5)	Sm1—O3iii	2.446 (3)
C3—I1	2.101 (4)	Sm1—O3iv	2.446 (3)
C4—O3	1.236 (6)	Sm1—O2iv	2.474 (3)
C4—N1	1.309 (6)	Sm1—O2iii	2.474 (3)
C4—H4	0.9300	Sm1—O1iii	2.562 (3)
C5—N1	1.458 (9)	Sm1—O1iv	2.562 (3)
C5—H5A	0.9600	Sm1—C1iv	2.844 (4)
C5—H5B	0.9600	Sm1—C1iii	2.844 (4)
C1—O2—Sm1	93.9 (2)	O3iv—Sm1—O1	73.51 (10)
O1—C1—O2	124.2 (4)	O2iv—Sm1—O1	133.46 (10)
O1—C1—C2	118.3 (3)	O2—Sm1—O1	51.69 (9)
O2—C1—C2	117.5 (3)	O2iii—Sm1—O1	71.50 (9)
O1—C1—Sm1	64.2 (2)	O3iii—Sm1—O1iii	77.37 (10)
O2—C1—Sm1	60.20 (19)	O3—Sm1—O1iii	73.51 (10)
C2—C1—Sm1	173.6 (2)	O3iv—Sm1—O1iii	142.72 (11)
C3i—C2—C3	118.3 (4)	O2iv—Sm1—O1iii	71.50 (9)
C3i—C2—C1	121.2 (3)	O2—Sm1—O1iii	133.46 (10)
C3—C2—C1	120.5 (3)	O2iii—Sm1—O1iii	51.69 (9)
C2ii—C3—C2	121.7 (4)	O1—Sm1—O1iii	118.13 (3)
C2ii—C3—I1	119.9 (3)	O3iii—Sm1—O1iv	73.51 (10)
C2—C3—I1	118.4 (3)	O3—Sm1—O1iv	142.72 (11)
O3—C4—N1	124.4 (5)	O3iv—Sm1—O1iv	77.37 (10)
O3—C4—H4	117.8	O2iv—Sm1—O1iv	51.69 (9)
N1—C4—H4	117.8	O2—Sm1—O1iv	71.50 (9)
N1—C5—H5A	109.5	O2iii—Sm1—O1iv	133.46 (10)
N1—C5—H5B	109.5	O1—Sm1—O1iv	118.13 (3)
H5A—C5—H5B	109.5	O1iii—Sm1—O1iv	118.13 (3)
N1—C5—H5C	109.5	O3iii—Sm1—C1	152.70 (11)
H5A—C5—H5C	109.5	O3—Sm1—C1	103.10 (11)
H5B—C5—H5C	109.5	O3iv—Sm1—C1	77.91 (10)
N1—C6—H6A	109.5	O2iv—Sm1—C1	110.46 (10)
N1—C6—H6B	109.5	O2—Sm1—C1	25.90 (10)
H6A—C6—H6B	109.5	O2iii—Sm1—C1	77.28 (10)
N1—C6—H6C	109.5	O1—Sm1—C1	25.84 (10)
H6A—C6—H6C	109.5	O1iii—Sm1—C1	128.98 (10)
H6B—C6—H6C	109.5	O1iv—Sm1—C1	95.43 (10)
C4—N1—C5	120.9 (6)	O3iii—Sm1—C1iv	77.91 (10)
C4—N1—C6	120.8 (6)	O3—Sm1—C1iv	152.70 (11)
C5—N1—C6	118.3 (5)	O3iv—Sm1—C1iv	103.10 (11)
C1—O1—Sm1	89.9 (2)	O2iv—Sm1—C1iv	25.90 (10)
C4—O3—Sm1	124.4 (3)	O2—Sm1—C1iv	77.28 (10)
O3iii—Sm1—O3	75.35 (12)	O2iii—Sm1—C1iv	110.46 (10)
O3iii—Sm1—O3iv	75.35 (12)	O1—Sm1—C1iv	128.98 (10)
O3—Sm1—O3iv	75.35 (12)	O1iii—Sm1—C1iv	95.43 (10)
O3iii—Sm1—O2iv	82.62 (10)	O1iv—Sm1—C1iv	25.84 (10)
O3—Sm1—O2iv	141.85 (10)	C1—Sm1—C1iv	103.16 (9)
O3iv—Sm1—O2iv	128.50 (10)	O3iii—Sm1—C1iii	103.10 (11)
O3iii—Sm1—O2	141.85 (10)	O3—Sm1—C1iii	77.91 (10)
O3—Sm1—O2	128.50 (10)	O3iv—Sm1—C1iii	152.70 (11)
O3iv—Sm1—O2	82.62 (10)	O2iv—Sm1—C1iii	77.28 (10)
O2iv—Sm1—O2	87.46 (10)	O2—Sm1—C1iii	110.46 (10)
O3iii—Sm1—O2iii	128.50 (10)	O2iii—Sm1—C1iii	25.90 (10)
O3—Sm1—O2iii	82.62 (10)	O1—Sm1—C1iii	95.43 (10)
O3iv—Sm1—O2iii	141.85 (10)	O1iii—Sm1—C1iii	25.84 (10)
O2iv—Sm1—O2iii	87.46 (10)	O1iv—Sm1—C1iii	128.98 (10)
O2—Sm1—O2iii	87.46 (10)	C1—Sm1—C1iii	103.16 (9)
O3iii—Sm1—O1	142.72 (11)	C1iv—Sm1—C1iii	103.16 (9)
O3—Sm1—O1	77.37 (10)
Sm1—O2—C1—O1	−5.3 (4)	C1—O1—Sm1—O3iv	−96.3 (2)
Sm1—O2—C1—C2	173.3 (3)	C1—O1—Sm1—O2iv	31.5 (3)
O1—C1—C2—C3i	−76.0 (5)	C1—O1—Sm1—O2	−2.7 (2)
O2—C1—C2—C3i	105.3 (4)	C1—O1—Sm1—O2iii	99.1 (2)
Sm1—C1—C2—C3i	172 (2)	C1—O1—Sm1—O1iii	122.17 (19)
O1—C1—C2—C3	104.2 (4)	C1—O1—Sm1—O1iv	−31.0 (3)
O2—C1—C2—C3	−74.4 (5)	C1—O1—Sm1—C1iv	−2.6 (3)
Sm1—C1—C2—C3	−8 (3)	C1—O1—Sm1—C1iii	109.2 (3)
C3i—C2—C3—C2ii	2.2 (7)	O1—C1—Sm1—O3iii	88.8 (3)
C1—C2—C3—C2ii	−178.0 (3)	O2—C1—Sm1—O3iii	−86.3 (3)
C3i—C2—C3—I1	−177.81 (18)	C2—C1—Sm1—O3iii	−156 (2)
C1—C2—C3—I1	2.0 (5)	O1—C1—Sm1—O3	5.5 (3)
O3—C4—N1—C5	179.1 (7)	O2—C1—Sm1—O3	−169.7 (2)
O3—C4—N1—C6	−1.6 (9)	C2—C1—Sm1—O3	120 (2)
O2—C1—O1—Sm1	5.1 (4)	O1—C1—Sm1—O3iv	77.1 (2)
C2—C1—O1—Sm1	−173.4 (3)	O2—C1—Sm1—O3iv	−98.1 (2)
N1—C4—O3—Sm1	−170.0 (4)	C2—C1—Sm1—O3iv	−168 (2)
C4—O3—Sm1—O3iii	33.2 (4)	O1—C1—Sm1—O2iv	−156.1 (2)
C4—O3—Sm1—O3iv	111.6 (4)	O2—C1—Sm1—O2iv	28.8 (2)
C4—O3—Sm1—O2iv	−23.6 (5)	C2—C1—Sm1—O2iv	−41 (2)
C4—O3—Sm1—O2	179.4 (4)	O1—C1—Sm1—O2	175.1 (4)
C4—O3—Sm1—O2iii	−99.8 (4)	C2—C1—Sm1—O2	−70 (2)
C4—O3—Sm1—O1	−172.4 (4)	O1—C1—Sm1—O2iii	−73.7 (2)
C4—O3—Sm1—O1iii	−47.7 (4)	O2—C1—Sm1—O2iii	111.1 (3)
C4—O3—Sm1—O1iv	67.3 (4)	C2—C1—Sm1—O2iii	41 (2)
C4—O3—Sm1—C1	−174.9 (4)	O2—C1—Sm1—O1	−175.1 (4)
C4—O3—Sm1—C1iv	21.3 (5)	C2—C1—Sm1—O1	115 (2)
C4—O3—Sm1—C1iii	−74.0 (4)	O1—C1—Sm1—O1iii	−73.78 (19)
C1—O2—Sm1—O3iii	132.2 (2)	O2—C1—Sm1—O1iii	111.1 (2)
C1—O2—Sm1—O3	12.9 (3)	C2—C1—Sm1—O1iii	41 (2)
C1—O2—Sm1—O3iv	77.5 (2)	O1—C1—Sm1—O1iv	152.9 (2)
C1—O2—Sm1—O2iv	−153.2 (2)	O2—C1—Sm1—O1iv	−22.3 (2)
C1—O2—Sm1—O2iii	−65.6 (3)	C2—C1—Sm1—O1iv	−92 (2)
C1—O2—Sm1—O1	2.7 (2)	O1—C1—Sm1—C1iv	177.9 (2)
C1—O2—Sm1—O1iii	−91.8 (3)	O2—C1—Sm1—C1iv	2.8 (3)
C1—O2—Sm1—O1iv	156.6 (2)	C2—C1—Sm1—C1iv	−67 (2)
C1—O2—Sm1—C1iv	−177.2 (3)	O1—C1—Sm1—C1iii	−75.0 (3)
C1—O2—Sm1—C1iii	−77.76 (18)	O2—C1—Sm1—C1iii	109.90 (18)
C1—O1—Sm1—O3iii	−130.8 (2)	C2—C1—Sm1—C1iii	40 (2)
C1—O1—Sm1—O3	−174.6 (3)