catena-Poly[diaqua­tris(μ3-biphenyl-2,2-dicarboxyl­ato)disamarium(III)]

Wei, D.-Y.; Zhang, Y.-G.; Wang, M.-L.; Zhu, Z.-K.

doi:10.1107/S1600536809046625

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 12| December 2009| Pages m1553-m1554

doi:10.1107/S1600536809046625

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catena-Poly[diaquatris(μ₃-biphenyl-2,2-dicarboxylato)disamarium(III)]

Dan-Yi Wei,^a ^* Yan-Guang Zhang,^a Mei-Li Wang ^a and Zhen-Ke Zhu ^a

^aState Key Laboratory Base of Novel Functional Materials and Preparation Science, Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211, People's Republic of China
^*Correspondence e-mail: weidanyi@nbu.edu.cn

(Received 9 July 2009; accepted 5 November 2009; online 11 November 2009)

The title compound, [Sm₂(C₁₄H₈O₄)₃(H₂O)₂]_n, is composed of one-dimensional chains and is isostructural with previously reported compounds [Wang et al. (2003 ). Eur. J. Inorg. Chem. pp. 1355–1360]. The asymmetric unit contains two Sm atoms, each of which lies on a crystallographic twofold axis. Both crystallographically independent Sm atoms are coordinated by eight O atoms in a distorted dodecahedral arrangement. The polymeric chains run along [001]. Adjacent chains are connected through π–π interactions [centroid–centroid distance = 3.450 (2) Å], forming a two-dimensional supramolecular network.

Related literature

For background to the design and syntheses of lanthanide complexes and their potential applications as fluorescent probes, magnetic materials and catalysts, see: Barta et al. (2008 ); de Bettencourt-Dias et al. (2005 ), (2005); Chen et al. (2008 ); Fujita et al. (1994 ); Taniguchi & Takahei (1993 ). For the effect of the organic ligands on the structural framework of lanthanide complexes, see: Liu & Xu (2005 ); Wang et al. (2007 ); Yigit et al. (2006 ). For the use of multidentate O-donor ligands as organic spacers in the construction of these complexes, see: Lin et al. (2005 ); Zheng et al. (2008 ). For the coordination behaviour of 2,2′-biphenyldicarboxylate, see: Thirumurugan et al. (2003 ); Xu et al. (2006 ); Rui et al. (2007 ).

Experimental

Crystal data

[Sm₂(C₁₄H₈O₄)₃(H₂O)₂]
M_r = 1057.34
Monoclinic, C 2/c
a = 20.776 (4) Å
b = 21.441 (4) Å
c = 8.2660 (17) Å
β = 103.94 (3)°
V = 3573.7 (13) Å³
Z = 4
Mo Kα radiation
μ = 3.33 mm⁻¹
T = 293 K
0.39 × 0.34 × 0.27 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.261, T_max = 0.409
15001 measured reflections
3962 independent reflections
3238 reflections with I > 2σ(I)
R_int = 0.067

Refinement

R[F² > 2σ(F²)] = 0.066
wR(F²) = 0.130
S = 1.18
3962 reflections
263 parameters
H-atom parameters constrained
Δρ_max = 2.31 e Å⁻³
Δρ_min = −1.91 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809046625/jh2091sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809046625/jh2091Isup2.hkl

checkCIF report

Comment top

Design and syntheses of lanthanide complexes are of great interest due to their various topological networks and potential applications in fluorescent probes, magnetic materials, catalysts (Barta et al., 2008; Bettencout-de Dias, 2005; Chen et al., 2008; Fujita et al., 1994; Taniguchi & Takahei, 1993). As reported in literature, the geometries and properties of organic ligands have great effect on structural framework of lanthanide complexes. So much effort has been devoted to modify the building blocks to control the products by selection of appropriate organic ligands (Liu & Xu, 2005; Wang et al., 2007; Yigit et al., 2006). Multidentae O donor ligands have been employed extensively as organic spacers in the construction of these complexes, such as α,ω-dicarboxylate and 1,3,5-benzenetricarboxylate (Lin et al., 2005; Zheng et al., 2008). Recently, research suggests that 2,2'-biphenyldicarboxylate (dpdc) possesses intriguing coordination behaviors to afford new coordination polymers (Thirumurugan et al., 2003; Xu, et al., 2006; Rui, et al., 2007). In this articles, we will report a new coordination polymers [Sm₂(C₁₄H₈O₄)₃(H₂O)₂]_n.

The crystal structure of the title compound (I) consists of one-dimensional chains of [Sm₂(C₁₄H₈O₄)₃(H₂O)₂]_n. (Fig 1). The asymmetric unit consists of two Sm atoms, each of which lies on the crystallographic twofold axis. Both crystallographically independent Sm atoms are coordinated to eight oxygen atoms and have a distorted dodecahedral arrangement. The Sm(1)—O (carboxylate) distances fall in the range 2.320 (5)–2.615 (5) Å, and the O—Sm(1)—O bond angles are in the range 25.5 (2)–153.5 (2)°. While the Sm(2)—O (carboxylate) bond lengths vary from 2.301 (5) Å to 2.480 (5))Å, and the Sm(2)—O (aqua) distances are both 2.540 (6) Å. The O—Sm(2)—O bond angles range from 66.8 (2)–147.2 (2)°. The coordination environments of two Sm atoms are different. The Sm(1) is coordinated to one tetradentate dpdc ligand and four pentadentate dpdc ligands, however, the Sm(2) is bonded to two tetradentate dpdc ligands, two pentadentate dpdc ligands, and two coordinated water molecules. The Sm atoms are bridged by the two types dpdc ligands to afford one-dimensional infinite polymeric chain which run along the [001] direction. As reported in documents, the one-dimensional chain looks like a pinwheel, the Sm atoms are at the center of pinwheel. The parallel phenyl rings of adjacent chains are interdigitaed. The two-dimensional supramolecule networks are formed by π-π interactions between these phenyl rings.

Related literature top

For background to the design and syntheses of lanthanide complexes and their potential applications as fluorescent probes, magnetic materials and catalysts, see: Barta et al. (2008); de Bettencourt-Dias et al. (2005), (2005); Chen et al. (2008); Fujita et al. (1994); Taniguchi & Takahei (1993). For the effect of the organic ligands on the structural framework of lanthanide complexes, see: Liu & Xu (2005); Wang et al. (2007); Yigit et al. (2006). For the use of multidentate O-donor ligands as organic spacers in the construction of these complexes, see: Lin et al. (2005); Zheng et al. (2008). For the coordination behaviour of 2,2'-biphenyldicarboxylate, see: Thirumurugan et al. (2003); Xu et al. (2006); Rui et al. (2007).

Experimental top

A mixture of Sm(NO₃)₃.6H₂O (0.222 g, 0.5 mmol) and 2,2'-diphenldicarboxylic acid (0.126 g, 0.5 mmol), H₂O (5 ml), and H₂C₂O₄ (0.080 g, 1 mmol), NaOH (0.040 g, 1 mmol) was sealed in a 25-ml stainless-steel reactor with Teflon liner, heated to 180°C for 4 days, and then cooled to room temperature. The products were filtered and colorless block crystals are obtained.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. ORTEP view of complex molecule of (I). Displacement ellipsoids are drawn at the 45% probability level. (#1 = -x, y, 3/2 - z; #2 = x, y, z + 1; #3 = -x, y, 1/2 - z.)
	Fig. 2. two-dimensional supramolecular layer in (I).

catena-Poly[diaquatris(µ₃-biphenyl-2,2-dicarboxylato)disamarium(III)] top

Crystal data top

[Sm₂(C₁₄H₈O₄)₃(H₂O)₂]	F(000) = 2064
M_r = 1057.34	D_x = 1.965 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 12337 reflections
a = 20.776 (4) Å	θ = 3.0–27.7°
b = 21.441 (4) Å	µ = 3.33 mm⁻¹
c = 8.2660 (17) Å	T = 293 K
β = 103.94 (3)°	Block, colorless
V = 3573.7 (13) Å³	0.39 × 0.34 × 0.27 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	3962 independent reflections
Radiation source: fine-focus sealed tube	3238 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.067
Detector resolution: 0 pixels mm^-1	θ_max = 27.5°, θ_min = 3.0°
ω scans	h = −26→26
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −27→27
T_min = 0.261, T_max = 0.409	l = −10→10
15001 measured reflections

Refinement top

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)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.130	H-atom parameters constrained
S = 1.18	w = 1/[σ²(F_o²) + 89.0505P] where P = (F_o² + 2F_c²)/3
3962 reflections	(Δ/σ)_max = 0.005
263 parameters	Δρ_max = 2.31 e Å⁻³
0 restraints	Δρ_min = −1.91 e Å⁻³

Crystal data top

[Sm₂(C₁₄H₈O₄)₃(H₂O)₂]	V = 3573.7 (13) Å³
M_r = 1057.34	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 20.776 (4) Å	µ = 3.33 mm⁻¹
b = 21.441 (4) Å	T = 293 K
c = 8.2660 (17) Å	0.39 × 0.34 × 0.27 mm
β = 103.94 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	3962 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	3238 reflections with I > 2σ(I)
T_min = 0.261, T_max = 0.409	R_int = 0.067
15001 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.066	0 restraints
wR(F²) = 0.130	H-atom parameters constrained
S = 1.18	w = 1/[σ²(F_o²) + 89.0505P] where P = (F_o² + 2F_c²)/3
3962 reflections	Δρ_max = 2.31 e Å⁻³
263 parameters	Δρ_min = −1.91 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Sm1	0.0000	0.20641 (2)	0.7500	0.01913 (15)
Sm2	0.0000	0.28693 (2)	0.2500	0.01920 (15)
O1	0.0507 (3)	0.1479 (3)	0.5795 (7)	0.0347 (14)
O2	0.0696 (3)	0.2088 (2)	0.3778 (7)	0.0270 (12)
O3	0.0595 (3)	0.2463 (3)	0.0471 (7)	0.0272 (12)
O4	0.0957 (3)	0.1637 (3)	−0.0570 (7)	0.0371 (15)
O5	0.0340 (3)	0.3549 (3)	0.4988 (7)	0.0314 (14)
O6	0.0664 (3)	0.2896 (2)	0.7115 (7)	0.0253 (12)
C1	0.0717 (4)	0.1566 (4)	0.4500 (9)	0.0219 (15)
C2	0.0997 (4)	0.1010 (4)	0.3809 (10)	0.0261 (17)
C3	0.0705 (5)	0.0434 (4)	0.3985 (11)	0.038 (2)
H3A	0.0340	0.0418	0.4451	0.045*
C4	0.0948 (6)	−0.0106 (4)	0.3481 (12)	0.047 (3)
H4A	0.0750	−0.0487	0.3608	0.056*
C5	0.1484 (6)	−0.0084 (5)	0.2790 (11)	0.051 (3)
H5A	0.1650	−0.0448	0.2430	0.062*
C6	0.1774 (5)	0.0479 (5)	0.2632 (12)	0.043 (2)
H6A	0.2147	0.0484	0.2194	0.051*
C7	0.1542 (4)	0.1042 (4)	0.3090 (10)	0.0303 (19)
C8	0.1910 (4)	0.1616 (4)	0.2945 (10)	0.0290 (18)
C9	0.2548 (5)	0.1680 (5)	0.3969 (12)	0.043 (2)
H9A	0.2710	0.1377	0.4768	0.051*
C10	0.2938 (5)	0.2178 (5)	0.3824 (14)	0.049 (3)
H10A	0.3359	0.2209	0.4529	0.059*
C11	0.2722 (5)	0.2637 (6)	0.2657 (14)	0.047 (3)
H11A	0.2996	0.2971	0.2555	0.057*
C12	0.2084 (5)	0.2593 (5)	0.1633 (10)	0.037 (2)
H12A	0.1926	0.2902	0.0849	0.045*
C13	0.1687 (4)	0.2091 (4)	0.1778 (11)	0.0307 (19)
C14	0.1034 (4)	0.2052 (4)	0.0510 (10)	0.0277 (17)
C15	0.0564 (4)	0.3429 (3)	0.6499 (10)	0.0226 (16)
C16	0.0779 (4)	0.3973 (3)	0.7700 (9)	0.0246 (17)
C17	0.1438 (4)	0.3978 (4)	0.8573 (10)	0.0294 (18)
H17A	0.1715	0.3649	0.8458	0.035*
C18	0.1689 (5)	0.4476 (5)	0.9620 (12)	0.040 (2)
H18A	0.2131	0.4478	1.0206	0.048*
C19	0.1282 (5)	0.4962 (4)	0.9784 (11)	0.041 (2)
H19A	0.1452	0.5300	1.0458	0.049*
C20	0.0622 (5)	0.4954 (4)	0.8956 (11)	0.034 (2)
H20A	0.0348	0.5282	0.9097	0.041*
C21	0.0358 (5)	0.4454 (3)	0.7900 (10)	0.0278 (18)
O7	0.0919 (4)	0.3610 (3)	0.2356 (8)	0.0474 (18)
H7B	0.1218	0.3708	0.3270	0.050*
H7A	0.1034	0.3561	0.1493	0.075*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm1	0.0230 (3)	0.0164 (3)	0.0182 (3)	0.000	0.0054 (2)	0.000
Sm2	0.0226 (3)	0.0174 (3)	0.0179 (3)	0.000	0.0056 (2)	0.000
O1	0.054 (4)	0.025 (3)	0.033 (3)	0.009 (3)	0.025 (3)	0.005 (2)
O2	0.025 (3)	0.023 (3)	0.033 (3)	0.005 (2)	0.009 (2)	0.002 (2)
O3	0.029 (3)	0.031 (3)	0.023 (3)	0.005 (2)	0.009 (2)	−0.001 (2)
O4	0.041 (4)	0.032 (3)	0.032 (3)	0.013 (3)	−0.004 (3)	−0.007 (2)
O5	0.047 (4)	0.027 (3)	0.022 (3)	−0.007 (3)	0.012 (3)	−0.003 (2)
O6	0.022 (3)	0.019 (3)	0.037 (3)	−0.004 (2)	0.011 (2)	0.001 (2)
C1	0.017 (4)	0.025 (4)	0.024 (4)	0.004 (3)	0.007 (3)	−0.002 (3)
C2	0.031 (4)	0.023 (4)	0.023 (4)	0.012 (3)	0.004 (3)	0.000 (3)
C3	0.051 (6)	0.028 (4)	0.034 (5)	0.002 (4)	0.010 (4)	0.000 (3)
C4	0.077 (8)	0.024 (5)	0.036 (6)	0.004 (5)	0.007 (5)	0.000 (4)
C5	0.090 (9)	0.038 (5)	0.018 (5)	0.029 (6)	−0.001 (5)	−0.008 (4)
C6	0.042 (6)	0.047 (6)	0.037 (5)	0.025 (5)	0.004 (4)	−0.009 (4)
C7	0.033 (5)	0.035 (5)	0.018 (4)	0.014 (4)	−0.002 (3)	−0.004 (3)
C8	0.021 (4)	0.039 (5)	0.029 (4)	0.010 (3)	0.009 (3)	−0.010 (3)
C9	0.031 (5)	0.057 (6)	0.038 (5)	0.022 (5)	0.005 (4)	−0.015 (4)
C10	0.022 (5)	0.069 (7)	0.054 (7)	0.004 (5)	0.006 (4)	−0.028 (5)
C11	0.032 (5)	0.058 (7)	0.053 (7)	−0.015 (5)	0.015 (5)	−0.023 (5)
C12	0.043 (6)	0.061 (6)	0.010 (4)	−0.005 (5)	0.012 (4)	−0.007 (3)
C13	0.019 (4)	0.037 (5)	0.036 (5)	0.005 (3)	0.006 (3)	−0.008 (3)
C14	0.030 (4)	0.027 (4)	0.026 (4)	−0.004 (3)	0.006 (3)	0.003 (3)
C15	0.018 (4)	0.021 (4)	0.032 (4)	0.000 (3)	0.013 (3)	−0.005 (3)
C16	0.034 (5)	0.019 (4)	0.022 (4)	−0.006 (3)	0.010 (3)	−0.002 (3)
C17	0.034 (5)	0.033 (4)	0.026 (4)	−0.001 (4)	0.017 (4)	−0.004 (3)
C18	0.035 (5)	0.048 (6)	0.037 (5)	−0.009 (4)	0.011 (4)	−0.016 (4)
C19	0.055 (6)	0.040 (5)	0.031 (5)	−0.017 (5)	0.016 (4)	−0.017 (4)
C20	0.049 (6)	0.019 (4)	0.043 (5)	−0.006 (4)	0.026 (4)	−0.009 (3)
C21	0.047 (5)	0.015 (3)	0.027 (4)	−0.007 (3)	0.019 (4)	−0.001 (3)
O7	0.053 (4)	0.052 (4)	0.043 (4)	−0.026 (4)	0.023 (3)	−0.018 (3)

Geometric parameters (Å, º) top

Sm1—O1ⁱ	2.321 (6)	C4—H4A	0.9300
Sm1—O1	2.321 (6)	C5—C6	1.370 (15)
Sm1—O6	2.322 (5)	C5—H5A	0.9300
Sm1—O6ⁱ	2.322 (5)	C6—C7	1.386 (11)
Sm1—O4ⁱⁱ	2.410 (6)	C6—H6A	0.9300
Sm1—O4ⁱⁱⁱ	2.410 (6)	C7—C8	1.469 (13)
Sm1—O3ⁱⁱⁱ	2.613 (5)	C8—C9	1.397 (12)
Sm1—O3ⁱⁱ	2.613 (5)	C8—C13	1.403 (12)
Sm1—C14ⁱⁱⁱ	2.869 (8)	C9—C10	1.362 (15)
Sm1—C14ⁱⁱ	2.869 (8)	C9—H9A	0.9300
Sm2—O2ⁱⁱ	2.298 (5)	C10—C11	1.375 (16)
Sm2—O2	2.298 (5)	C10—H10A	0.9300
Sm2—O3ⁱⁱ	2.469 (6)	C11—C12	1.394 (13)
Sm2—O3	2.469 (6)	C11—H11A	0.9300
Sm2—O5	2.480 (5)	C12—C13	1.377 (13)
Sm2—O5ⁱⁱ	2.480 (5)	C12—H12A	0.9300
Sm2—O7	2.509 (6)	C13—C14	1.503 (11)
Sm2—O7ⁱⁱ	2.509 (6)	C14—Sm1^iv	2.869 (8)
O1—C1	1.264 (9)	C15—C16	1.527 (10)
O2—C1	1.263 (9)	C16—C17	1.387 (12)
O3—C14	1.264 (10)	C16—C21	1.388 (11)
O3—Sm1^iv	2.613 (5)	C17—C18	1.394 (12)
O4—C14	1.244 (10)	C17—H17A	0.9300
O4—Sm1^iv	2.410 (6)	C18—C19	1.369 (14)
O5—C15	1.250 (10)	C18—H18A	0.9300
O6—C15	1.248 (9)	C19—C20	1.376 (14)
C1—C2	1.498 (10)	C19—H19A	0.9300
C2—C3	1.399 (12)	C20—C21	1.407 (11)
C2—C7	1.402 (12)	C20—H20A	0.9300
C3—C4	1.369 (13)	C21—C21ⁱ	1.477 (18)
C3—H3A	0.9300	O7—H7B	0.8798
C4—C5	1.370 (16)	O7—H7A	0.8122

O1ⁱ—Sm1—O1	114.5 (3)	C14—O3—Sm2	134.8 (5)
O1ⁱ—Sm1—O6	150.4 (2)	C14—O3—Sm1^iv	88.3 (5)
O1—Sm1—O6	87.7 (2)	Sm2—O3—Sm1^iv	123.6 (2)
O1ⁱ—Sm1—O6ⁱ	87.7 (2)	C14—O4—Sm1^iv	98.4 (5)
O1—Sm1—O6ⁱ	150.4 (2)	C15—O5—Sm2	132.1 (5)
O6—Sm1—O6ⁱ	79.7 (3)	C15—O6—Sm1	135.5 (5)
O1ⁱ—Sm1—O4ⁱⁱ	76.9 (2)	O2—C1—O1	123.5 (7)
O1—Sm1—O4ⁱⁱ	79.4 (2)	O2—C1—C2	119.8 (7)
O6—Sm1—O4ⁱⁱ	128.6 (2)	O1—C1—C2	116.7 (7)
O6ⁱ—Sm1—O4ⁱⁱ	87.7 (2)	C3—C2—C7	120.1 (8)
O1ⁱ—Sm1—O4ⁱⁱⁱ	79.4 (2)	C3—C2—C1	116.4 (8)
O1—Sm1—O4ⁱⁱⁱ	76.9 (2)	C7—C2—C1	123.4 (7)
O6—Sm1—O4ⁱⁱⁱ	87.7 (2)	C4—C3—C2	121.0 (10)
O6ⁱ—Sm1—O4ⁱⁱⁱ	128.6 (2)	C4—C3—H3A	119.5
O4ⁱⁱ—Sm1—O4ⁱⁱⁱ	135.3 (3)	C2—C3—H3A	119.5
O1ⁱ—Sm1—O3ⁱⁱⁱ	77.7 (2)	C3—C4—C5	119.7 (10)
O1—Sm1—O3ⁱⁱⁱ	124.5 (2)	C3—C4—H4A	120.2
O6—Sm1—O3ⁱⁱⁱ	73.45 (19)	C5—C4—H4A	120.2
O6ⁱ—Sm1—O3ⁱⁱⁱ	77.39 (19)	C6—C5—C4	119.4 (9)
O4ⁱⁱ—Sm1—O3ⁱⁱⁱ	151.0 (2)	C6—C5—H5A	120.3
O4ⁱⁱⁱ—Sm1—O3ⁱⁱⁱ	51.29 (18)	C4—C5—H5A	120.3
O1ⁱ—Sm1—O3ⁱⁱ	124.5 (2)	C5—C6—C7	123.5 (11)
O1—Sm1—O3ⁱⁱ	77.7 (2)	C5—C6—H6A	118.2
O6—Sm1—O3ⁱⁱ	77.39 (19)	C7—C6—H6A	118.2
O6ⁱ—Sm1—O3ⁱⁱ	73.45 (19)	C6—C7—C2	116.3 (9)
O4ⁱⁱ—Sm1—O3ⁱⁱ	51.29 (18)	C6—C7—C8	119.1 (9)
O4ⁱⁱⁱ—Sm1—O3ⁱⁱ	151.0 (2)	C2—C7—C8	124.4 (7)
O3ⁱⁱⁱ—Sm1—O3ⁱⁱ	141.8 (2)	C9—C8—C13	117.0 (9)
O1ⁱ—Sm1—C14ⁱⁱⁱ	79.8 (2)	C9—C8—C7	118.0 (8)
O1—Sm1—C14ⁱⁱⁱ	99.6 (2)	C13—C8—C7	124.9 (7)
O6—Sm1—C14ⁱⁱⁱ	77.3 (2)	C10—C9—C8	121.4 (10)
O6ⁱ—Sm1—C14ⁱⁱⁱ	103.5 (2)	C10—C9—H9A	119.3
O4ⁱⁱ—Sm1—C14ⁱⁱⁱ	153.7 (2)	C8—C9—H9A	119.3
O4ⁱⁱⁱ—Sm1—C14ⁱⁱⁱ	25.4 (2)	C9—C10—C11	121.5 (9)
O3ⁱⁱⁱ—Sm1—C14ⁱⁱⁱ	26.1 (2)	C9—C10—H10A	119.3
O3ⁱⁱ—Sm1—C14ⁱⁱⁱ	154.7 (2)	C11—C10—H10A	119.3
O1ⁱ—Sm1—C14ⁱⁱ	99.6 (2)	C10—C11—C12	118.6 (10)
O1—Sm1—C14ⁱⁱ	79.8 (2)	C10—C11—H11A	120.7
O6—Sm1—C14ⁱⁱ	103.5 (2)	C12—C11—H11A	120.7
O6ⁱ—Sm1—C14ⁱⁱ	77.3 (2)	C13—C12—C11	120.2 (10)
O4ⁱⁱ—Sm1—C14ⁱⁱ	25.4 (2)	C13—C12—H12A	119.9
O4ⁱⁱⁱ—Sm1—C14ⁱⁱ	153.7 (2)	C11—C12—H12A	119.9
O3ⁱⁱⁱ—Sm1—C14ⁱⁱ	154.7 (2)	C12—C13—C8	121.4 (8)
O3ⁱⁱ—Sm1—C14ⁱⁱ	26.1 (2)	C12—C13—C14	116.2 (8)
C14ⁱⁱⁱ—Sm1—C14ⁱⁱ	179.0 (3)	C8—C13—C14	122.1 (8)
O2ⁱⁱ—Sm2—O2	86.4 (3)	O4—C14—O3	120.9 (8)
O2ⁱⁱ—Sm2—O3ⁱⁱ	72.10 (19)	O4—C14—C13	118.7 (8)
O2—Sm2—O3ⁱⁱ	78.1 (2)	O3—C14—C13	120.2 (7)
O2ⁱⁱ—Sm2—O3	78.1 (2)	O4—C14—Sm1^iv	56.2 (4)
O2—Sm2—O3	72.10 (19)	O3—C14—Sm1^iv	65.5 (4)
O3ⁱⁱ—Sm2—O3	138.7 (3)	C13—C14—Sm1^iv	164.9 (6)
O2ⁱⁱ—Sm2—O5	146.3 (2)	O6—C15—O5	125.6 (7)
O2—Sm2—O5	91.4 (2)	O6—C15—C16	116.1 (7)
O3ⁱⁱ—Sm2—O5	74.51 (19)	O5—C15—C16	118.2 (7)
O3—Sm2—O5	132.9 (2)	C17—C16—C21	120.2 (7)
O2ⁱⁱ—Sm2—O5ⁱⁱ	91.4 (2)	C17—C16—C15	116.3 (7)
O2—Sm2—O5ⁱⁱ	146.3 (2)	C21—C16—C15	123.5 (7)
O3ⁱⁱ—Sm2—O5ⁱⁱ	132.9 (2)	C16—C17—C18	120.3 (8)
O3—Sm2—O5ⁱⁱ	74.51 (19)	C16—C17—H17A	119.9
O5—Sm2—O5ⁱⁱ	108.0 (3)	C18—C17—H17A	119.9
O2ⁱⁱ—Sm2—O7	147.4 (2)	C19—C18—C17	119.8 (9)
O2—Sm2—O7	94.7 (2)	C19—C18—H18A	120.1
O3ⁱⁱ—Sm2—O7	140.0 (2)	C17—C18—H18A	120.1
O3—Sm2—O7	71.3 (2)	C18—C19—C20	120.4 (8)
O5—Sm2—O7	66.4 (2)	C18—C19—H19A	119.8
O5ⁱⁱ—Sm2—O7	69.9 (2)	C20—C19—H19A	119.8
O2ⁱⁱ—Sm2—O7ⁱⁱ	94.7 (2)	C19—C20—C21	120.7 (9)
O2—Sm2—O7ⁱⁱ	147.4 (2)	C19—C20—H20A	119.6
O3ⁱⁱ—Sm2—O7ⁱⁱ	71.3 (2)	C21—C20—H20A	119.6
O3—Sm2—O7ⁱⁱ	140.0 (2)	C16—C21—C20	118.6 (8)
O5—Sm2—O7ⁱⁱ	69.9 (2)	C16—C21—C21ⁱ	122.8 (6)
O5ⁱⁱ—Sm2—O7ⁱⁱ	66.4 (2)	C20—C21—C21ⁱ	118.5 (7)
O7—Sm2—O7ⁱⁱ	101.4 (4)	Sm2—O7—H7B	119.9
C1—O1—Sm1	137.2 (5)	Sm2—O7—H7A	110.3
C1—O2—Sm2	144.0 (5)	H7B—O7—H7A	119.3

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

Experimental details

Crystal data
Chemical formula	[Sm₂(C₁₄H₈O₄)₃(H₂O)₂]
M_r	1057.34
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	20.776 (4), 21.441 (4), 8.2660 (17)
β (°)	103.94 (3)
V (Å³)	3573.7 (13)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.33
Crystal size (mm)	0.39 × 0.34 × 0.27

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.261, 0.409
No. of measured, independent and observed [I > 2σ(I)] reflections	15001, 3962, 3238
R_int	0.067
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.066, 0.130, 1.18
No. of reflections	3962
No. of parameters	263
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + 89.0505P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	2.31, −1.91

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976).

Acknowledgements

This project was sponsored by K. C. Wong Magna Fund in Ningbo University and supported by the Zhejiang Provincial Science and Technology Agency project (2007 F70009).

References

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