Poly[tris­(dimethyl­formamide)(μ3-2,4,6-triiodobenzene-1,3,5-tricarboxyl­ato)samarium(III)]

Yan, B.; Sheng, D.; Yang, Y.

doi:10.1107/S1600536813003358

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 3| March 2013| Page m149

doi:10.1107/S1600536813003358

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Poly[tris(dimethylformamide)(μ₃-2,4,6-triiodobenzene-1,3,5-tricarboxylato)samarium(III)]

Bin Yan,^a ^* Daopeng Sheng ^a ^* and Yanzhao Yang ^a ^*

^aKey Laboratory for Special Functional Aggregated Materials of the Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan, Shandong 250100, People's Republic of China
^*Correspondence e-mail: wl-yanbin@163.com, sdp1214@gmail.com, yzhyang@sdu.edu.cn

(Received 23 December 2012; accepted 1 February 2013; online 13 February 2013)

In the title compound, [Sm(C₉I₃O₆)(C₃H₇NO)₃]_n, the Sm^III atom is coordinated by nine O atoms, viz. six carboxylate O atoms from three 2,4,6-triiodobenzene-1,3,5-tricarboxylate (I₃BTC) ligands and three O atoms from three N,N-dimethylformamide (DMF) molecules. 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 molecule 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_r = 954.43
Cubic, P 2₁ 3
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[F² > 2σ(F²)] = 0.021
wR(F²) = 0.049
S = 1.03
2143 reflections
106 parameters
H-atom parameters constrained
Δρ_max = 0.72 e Å⁻³
Δρ_min = −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 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536813003358/cv5378sup1.cif

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

checkCIF report

Comment top

Metal-organic framework (MOF) compounds have attracted considerable interest because of their potential applications in a variety of areas, including catalysis, shape-selective adsorption, gas storage, photochemistry, and materials with magnetic properties (Nakanishi et al., 2007; Phan et al., 2010; Suib et al., 2008). The design and synthesis of MOFs with great potential for chemical and structural diversity, is one of the major current challenges in inorganic chemistry. To the best of our knowledge, MOF structure of the I₃BTC ligand is not reported so far. The I₃BTC ligand, besides three iodine atoms at the 2,4,6-sites of benzene ring, is same as 1,3,5- benzenetricarboxylic acid (H₃BTC). Although the coordinated ability of carbonylic O atoms is influenced by the electronic properties of iodine atoms to some extent, its coordinated mode is almost no change (Daiguebonne et al., 2002). In recent years, the construction of MOFs based on H₃BTC ligand has been widely investigated owing to their fascinating coordination modes (Han et al., 2012; Lu et al., 2008; Serre et al., 2004). Herein we report the hydrothermal synthesis and crystal structure of the title compound (I).

In (I), the asymmetric unit contains one Sm^III ion and one I₃BTC anion, both situated on a threefold axis, and one DMF molecule in general position. As shown in Fig. 1, each Sm center is coordinated by nine O atoms -six carboxylate O atoms from three ligands and three O atoms from three DMF molecules. The Sm1–O bond lengths fall in the range of 2.446 (3)–2.562 (3) Å, and the O–Sm–O angles varying from 51.702 (88)–142.712 (91)°, thus falling in the expected region. Each ligand I₃BTC bridges three Sm atoms to produce a three-dimensional metal organic framework structure, while coordinated solvent molecules (DMF) exist among the pore canals by coordinating O atoms to central metal ions.

Related literature top

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 top

The title compound was prepared by the solvothermal reaction of Sm(NO₃)₃.6H₂O (100 mg), 2,4,6-triiodobenzene-1,3,5-tricarboxylic acid (100 mg), DMF (4 ml) and ethanol (4 ml) at 90 °C for 72 h. The autoclave was subsequently allowed to cool to room temperature. After washing with ethanol, colourless block crystals were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); 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).

Figures top

Fig. 1. A portion of the crystal structure of (I) showing the coordination environment of Sm1, 30% probability displacement ellipsoids and atomic numbering [symmetry codes: (i) 1 - x, 1/2 + y, 3/2 - z; (ii) 3/2 - x, 1 - y, -1/2 + z; (iii) 3/2 - x, 1 - y, -1/2 + z; (iv) 1/2 - x, -y, 1/2 + z].

Poly[tris(dimethylformamide)(µ₃-2,4,6-triiodobenzene-1,3,5-tricarboxylato)samarium(III)] top

Crystal data top

[Sm(C₉I₃O₆)(C₃H₇NO)₃]	D_x = 2.245 Mg m⁻³
M_r = 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

Data collection top

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

Refinement top

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(F_o²) + (0.0236P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.049	(Δ/σ)_max = 0.002
S = 1.03	Δρ_max = 0.72 e Å⁻³
2143 reflections	Δρ_min = −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	Absolute structure parameter: 0.02 (2)

Crystal data top

[Sm(C₉I₃O₆)(C₃H₇NO)₃]	Z = 4
M_r = 954.43	Mo Kα radiation
Cubic, P2₁3	µ = 5.41 mm⁻¹
a = 14.1341 (16) Å	T = 295 K
V = 2823.6 (6) Å³	0.16 × 0.15 × 0.15 mm

Data collection top

Bruker APEXII CCD area-detector diffractometer	2143 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2005)	2026 reflections with I > 2σ(I)
T_min = 0.478, T_max = 0.498	R_int = 0.020
5119 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	H-atom parameters constrained
wR(F²) = 0.049	Δρ_max = 0.72 e Å⁻³
S = 1.03	Δρ_min = −0.62 e Å⁻³
2143 reflections	Absolute structure: Flack (1983), 943 Friedel pairs
106 parameters	Absolute structure parameter: 0.02 (2)
0 restraints

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. SHELXTL (Sheldrick, 2008)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—O3^iv	2.446 (3)
C4—O3	1.236 (6)	Sm1—O2^iv	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—O1^iv	2.562 (3)
C5—H5A	0.9600	Sm1—C1^iv	2.844 (4)
C5—H5B	0.9600	Sm1—C1ⁱⁱⁱ	2.844 (4)

C1—O2—Sm1	93.9 (2)	O3^iv—Sm1—O1	73.51 (10)
O1—C1—O2	124.2 (4)	O2^iv—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)	O3^iv—Sm1—O1ⁱⁱⁱ	142.72 (11)
C3ⁱ—C2—C3	118.3 (4)	O2^iv—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—O1^iv	73.51 (10)
C2—C3—I1	118.4 (3)	O3—Sm1—O1^iv	142.72 (11)
O3—C4—N1	124.4 (5)	O3^iv—Sm1—O1^iv	77.37 (10)
O3—C4—H4	117.8	O2^iv—Sm1—O1^iv	51.69 (9)
N1—C4—H4	117.8	O2—Sm1—O1^iv	71.50 (9)
N1—C5—H5A	109.5	O2ⁱⁱⁱ—Sm1—O1^iv	133.46 (10)
N1—C5—H5B	109.5	O1—Sm1—O1^iv	118.13 (3)
H5A—C5—H5B	109.5	O1ⁱⁱⁱ—Sm1—O1^iv	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	O3^iv—Sm1—C1	77.91 (10)
N1—C6—H6A	109.5	O2^iv—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	O1^iv—Sm1—C1	95.43 (10)
C4—N1—C5	120.9 (6)	O3ⁱⁱⁱ—Sm1—C1^iv	77.91 (10)
C4—N1—C6	120.8 (6)	O3—Sm1—C1^iv	152.70 (11)
C5—N1—C6	118.3 (5)	O3^iv—Sm1—C1^iv	103.10 (11)
C1—O1—Sm1	89.9 (2)	O2^iv—Sm1—C1^iv	25.90 (10)
C4—O3—Sm1	124.4 (3)	O2—Sm1—C1^iv	77.28 (10)
O3ⁱⁱⁱ—Sm1—O3	75.35 (12)	O2ⁱⁱⁱ—Sm1—C1^iv	110.46 (10)
O3ⁱⁱⁱ—Sm1—O3^iv	75.35 (12)	O1—Sm1—C1^iv	128.98 (10)
O3—Sm1—O3^iv	75.35 (12)	O1ⁱⁱⁱ—Sm1—C1^iv	95.43 (10)
O3ⁱⁱⁱ—Sm1—O2^iv	82.62 (10)	O1^iv—Sm1—C1^iv	25.84 (10)
O3—Sm1—O2^iv	141.85 (10)	C1—Sm1—C1^iv	103.16 (9)
O3^iv—Sm1—O2^iv	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)	O3^iv—Sm1—C1ⁱⁱⁱ	152.70 (11)
O3^iv—Sm1—O2	82.62 (10)	O2^iv—Sm1—C1ⁱⁱⁱ	77.28 (10)
O2^iv—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)
O3^iv—Sm1—O2ⁱⁱⁱ	141.85 (10)	O1ⁱⁱⁱ—Sm1—C1ⁱⁱⁱ	25.84 (10)
O2^iv—Sm1—O2ⁱⁱⁱ	87.46 (10)	O1^iv—Sm1—C1ⁱⁱⁱ	128.98 (10)
O2—Sm1—O2ⁱⁱⁱ	87.46 (10)	C1—Sm1—C1ⁱⁱⁱ	103.16 (9)
O3ⁱⁱⁱ—Sm1—O1	142.72 (11)	C1^iv—Sm1—C1ⁱⁱⁱ	103.16 (9)
O3—Sm1—O1	77.37 (10)

Sm1—O2—C1—O1	−5.3 (4)	C1—O1—Sm1—O3^iv	−96.3 (2)
Sm1—O2—C1—C2	173.3 (3)	C1—O1—Sm1—O2^iv	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—O1^iv	−31.0 (3)
O2—C1—C2—C3	−74.4 (5)	C1—O1—Sm1—C1^iv	−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—O3^iv	77.1 (2)
C2—C1—O1—Sm1	−173.4 (3)	O2—C1—Sm1—O3^iv	−98.1 (2)
N1—C4—O3—Sm1	−170.0 (4)	C2—C1—Sm1—O3^iv	−168 (2)
C4—O3—Sm1—O3ⁱⁱⁱ	33.2 (4)	O1—C1—Sm1—O2^iv	−156.1 (2)
C4—O3—Sm1—O3^iv	111.6 (4)	O2—C1—Sm1—O2^iv	28.8 (2)
C4—O3—Sm1—O2^iv	−23.6 (5)	C2—C1—Sm1—O2^iv	−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—O1^iv	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—C1^iv	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—O3^iv	77.5 (2)	O1—C1—Sm1—O1^iv	152.9 (2)
C1—O2—Sm1—O2^iv	−153.2 (2)	O2—C1—Sm1—O1^iv	−22.3 (2)
C1—O2—Sm1—O2ⁱⁱⁱ	−65.6 (3)	C2—C1—Sm1—O1^iv	−92 (2)
C1—O2—Sm1—O1	2.7 (2)	O1—C1—Sm1—C1^iv	177.9 (2)
C1—O2—Sm1—O1ⁱⁱⁱ	−91.8 (3)	O2—C1—Sm1—C1^iv	2.8 (3)
C1—O2—Sm1—O1^iv	156.6 (2)	C2—C1—Sm1—C1^iv	−67 (2)
C1—O2—Sm1—C1^iv	−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)

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

Experimental details

Crystal data
Chemical formula	[Sm(C₉I₃O₆)(C₃H₇NO)₃]
M_r	954.43
Crystal system, space group	Cubic, P2₁3
Temperature (K)	295
a (Å)	14.1341 (16)
V (Å³)	2823.6 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.41
Crystal size (mm)	0.16 × 0.15 × 0.15

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.478, 0.498
No. of measured, independent and observed [I > 2σ(I)] reflections	5119, 2143, 2026
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.646

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.049, 1.03
No. of reflections	2143
No. of parameters	106
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.72, −0.62
Absolute structure	Flack (1983), 943 Friedel pairs
Absolute structure parameter	0.02 (2)

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), WinGX (Farrugia, 2012).

Acknowledgements

The authors acknowledge financial support from the National Natural Science Foundation of China (grant Nos. 21276142 and 21076115).

References

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