Poly[[penta­aqua­(μ4-pyridine-2,4,6-tri­carboxyl­ato)(μ3-pyridine-2,4,6-tri­carboxyl­ato)disamarium(III)] mono­hydrate]

Jin, Y.-W.; Zhu, H.

doi:10.1107/S1600536812002462

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 3| March 2012| Page m287

doi:10.1107/S1600536812002462

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Poly[[pentaaqua(μ₄-pyridine-2,4,6-tricarboxylato)(μ₃-pyridine-2,4,6-tricarboxylato)disamarium(III)] monohydrate]

Yong-Wei Jin ^a and Hong-lin Zhu ^a ^*

^aCrystal Engineering Division, Center of Applied Solid State Chemistry Research, Ningbo University, Ningbo, Zhejiang 315211, People's Republic of China
^*Correspondence e-mail: zhuhonglin1@nbu.edu.cn

(Received 10 January 2012; accepted 19 January 2012; online 10 February 2012)

The asymmetric unit of the title compound, {[Sm₂(C₈H₂NO₆)₂(H₂O)₅]·H₂O}_n, contains two independent Sm^III ions, two pyridine-2,4,6-tricarboxylate (ptc) ligands, five aqua ligands and one lattice water molecule. One Sm^III ion is nine-coordinated by one N and five O atoms from the three ptc ligands and three aqua ligands in a distorted monocapped square antiprismatic geometry, and the other is eight-coordinated by one N and five O atoms from three ptc ligands and two aqua ligands in a 4,4′-bicapped trigonal antiprismatic geometry. The ptc ligands brigde the Sm^III ions into a three-dimensional polymeric framework. Extensive O—H⋯O hydrogen bonding is observed in the crystal structure.

Related literature

For related compounds, see: Gao et al. (2006 ); Ghosh & Bharadwaj (2005 ); Li et al. (2008 ); Wang et al. (2007 ).

Experimental

Crystal data

[Sm₂(C₈H₂NO₆)₂(H₂O)₅]·H₂O
M_r = 825.01
Monoclinic, P 2₁ /n
a = 18.426 (4) Å
b = 6.9082 (14) Å
c = 18.583 (4) Å
β = 111.98 (3)°
V = 2193.6 (8) Å³
Z = 4
Mo Kα radiation
μ = 5.40 mm⁻¹
T = 293 K
0.43 × 0.28 × 0.21 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.177, T_max = 0.321
20300 measured reflections
4963 independent reflections
4776 reflections with I > 2σ(I)
R_int = 0.035

Refinement

R[F² > 2σ(F²)] = 0.018
wR(F²) = 0.041
S = 1.19
4963 reflections
344 parameters
H-atom parameters constrained
Δρ_max = 0.69 e Å⁻³
Δρ_min = −0.84 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O14ⁱ	0.82	1.87	2.686 (3)	172
O7—H7B⋯O2ⁱⁱ	0.86	1.80	2.645 (3)	165
O8—H8A⋯O12ⁱⁱⁱ	0.89	1.83	2.727 (3)	177
O8—H8B⋯O9^iv	0.87	2.38	2.831 (3)	113
O9—H9A⋯O6ⁱ	0.87	1.84	2.698 (3)	171
O9—H9B⋯O5ⁱ	0.93	2.55	3.052 (3)	114
O16—H16A⋯O4ⁱ	0.82	2.31	3.075 (3)	157
O16—H16B⋯O15^v	0.79	1.97	2.747 (3)	171
O17—H17A⋯O18^vi	0.84	1.86	2.697 (3)	176
O17—H17B⋯O5^vii	0.80	1.96	2.731 (3)	162
O18—H18A⋯O14^viii	0.85	2.06	2.905 (3)	174
O18—H18B⋯O13	0.82	1.93	2.736 (3)	168
Symmetry codes: (i) -x+1, -y, -z+1; (ii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) -x+1, -y+1, -z+1; (iv) x, y+1, z; (v) -x+1, -y, -z+2; (vi) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (vii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (viii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ .

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.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536812002462/cv5233sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812002462/cv5233Isup2.hkl

checkCIF report

Comment top

In recent years, research of lanthanide pyridine-2,4,6-tricarboxylate coordination polymers has been of great interest in the fields of molecule adsorption, host-guest interaction and luminescence materials (Gao et al., 2006; Li et al., 2008; Wang et al., 2007;) etc. The compound {[Pr(H₂O)₂(ptc)].2H₂O} reported by Ghosh et al. (2005) represents an example of three-dimensional MOF, which could potentially be utilized as an adsorption material. In this contribution, we report the structure of the title compound.

The asymmetric unit of title compound contains two Sm^III ions (Sm1, Sm2), two ptc ligands (denoted as ptc1 and ptc2 ligands, which contain N1 and N2 atoms, respectively) (H₃ptc = pyridine-2,4,6-tricarboxylate), five aqua ligands and one lattice water molecule as illustrated in Fig. 1. The Sm1 and Sm2 are respectively 9- and 8-coordinated with the ligating atoms occupying the corners of distorted monocapped square anti-prism and 4,4'-bicapped trigonal anti-prism, respectively. The bond distances about the Sm1 and Sm2 atoms fall in the regions 2.406-2.587 Å and 2.359-2.529 Å, the corresponding bond angles are in the regions 50.9-147.8° and 63.3-159.7°, respectively.

Each ptc1 ligand links four Sm^III centers with the 4-carboxylate bonded to two metal ions in syn-syn bridging fashion and the 2-carboxylate coordinated to two metal ions in anti-syn bridging fashion, while each ptc2 ligand connects three Sm^III centers with the 4-carboxylate chelating one metal ion and the 2-carboxylate bridging two metal ions in anti-anti bridging fashions.

Both ptc1 and ptc2 ligands coordinate Sm1 atoms to form a linear [Sm(ptc)₂] metallo-ligand, which, in turn, bridges the Sm2 atoms to generate one-dimensional ribbon-like chains with rectangular and 8-membered rhombic rings alternating (Fig. 2). Within the rectangular ring, the two adjacent ptc1 and ptc2 ligands orientate approximately parallelly to each other with a dihedral angle of 7.4° and the mean interplanar distance of 3.33 Å suggests significant intrachain π···π stacking interactions. The resulting one-dimensional chains donate carboxylate O atoms (O1 and O10) to coordinate with Sm atoms from two neighboring chains to construct a three-dimensional framework (Fig. 3).

Related literature top

For related compounds, see: Gao et al. (2006); Ghosh & Bharadwaj (2005); Li et al. (2008); Wang et al. (2007).

Experimental top

All chemicals were obtained from commerical sources and were used as obtained. A mixture of SmCl₃.nH₂O (0.60 mmol), pyridine-2,4,6-tricarboxylic acid (0.0537 g, 0.25 mmol), Malonic acid (0.0261 g, 0.25 mmol), NaOH (1 ml, 1 M) and H₂O (20 ml) was sealed into a 23 ml Teflon-lined stainless autoclave, which was heated up to 180°C, at which temperature the reactor was held for 3 days, and then cooled to room temperature. A mixture of brownish deposit and a small amount of colourless block-liked crystals were obtained.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. A portion of the crystal structure showing the atomic numbering and 45% probability dispalcement ellipsoids [symmetry codes: (i) 1/2-x, -1/2+y, 1/2-z; (ii) x, y, 1+z; (iii) 1-x, 1-y, 1-z; (iv) 1/2-x, -1/2+y, 3/2-z].
	Fig. 2. The one-dimensional chain with the rectangular and 8-membered rhombic rings.
	Fig. 3. The three-dimensional metal-organic framework in the title compound.

Poly[[pentaaqua(µ₄-pyridine-2,4,6-tricarboxylato)(µ₃-pyridine-2,4,6- tricarboxylato)disamarium(III)] monohydrate] top

Crystal data top

[Sm₂(C₈H₂NO₆)₂(H₂O)₅]·H₂O	F(000) = 1576
M_r = 825.01	D_x = 2.498 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 19369 reflections
a = 18.426 (4) Å	θ = 3.2–27.5°
b = 6.9082 (14) Å	µ = 5.40 mm⁻¹
c = 18.583 (4) Å	T = 293 K
β = 111.98 (3)°	Block, colorless
V = 2193.6 (8) Å³	0.43 × 0.28 × 0.21 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	4963 independent reflections
Radiation source: fine-focus sealed tube	4776 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
Detector resolution: 0 pixels mm^-1	θ_max = 27.5°, θ_min = 3.2°
ω scans	h = −23→23
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −8→8
T_min = 0.177, T_max = 0.321	l = −24→22
20300 measured reflections

Refinement top

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)] = 0.018	H-atom parameters constrained
wR(F²) = 0.041	w = 1/[σ²(F_o²) + (0.0066P)² + 3.5019P] where P = (F_o² + 2F_c²)/3
S = 1.19	(Δ/σ)_max = 0.002
4963 reflections	Δρ_max = 0.69 e Å⁻³
344 parameters	Δρ_min = −0.84 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: 0.00244 (6)

Crystal data top

[Sm₂(C₈H₂NO₆)₂(H₂O)₅]·H₂O	V = 2193.6 (8) Å³
M_r = 825.01	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 18.426 (4) Å	µ = 5.40 mm⁻¹
b = 6.9082 (14) Å	T = 293 K
c = 18.583 (4) Å	0.43 × 0.28 × 0.21 mm
β = 111.98 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	4963 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	4776 reflections with I > 2σ(I)
T_min = 0.177, T_max = 0.321	R_int = 0.035
20300 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.018	0 restraints
wR(F²) = 0.041	H-atom parameters constrained
S = 1.19	Δρ_max = 0.69 e Å⁻³
4963 reflections	Δρ_min = −0.84 e Å⁻³
344 parameters

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.

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

	x	y	z	U_iso*/U_eq
Sm1	0.373309 (7)	0.222784 (18)	0.378119 (7)	0.01049 (4)
Sm2	0.374965 (8)	0.250031 (17)	0.896720 (7)	0.01111 (5)
N1	0.42996 (13)	0.3322 (3)	0.27802 (12)	0.0125 (4)
C1	0.38355 (15)	0.4105 (3)	0.21147 (15)	0.0127 (5)
C2	0.40694 (15)	0.4323 (3)	0.14877 (15)	0.0139 (5)
H2A	0.3735	0.4861	0.1023	0.017*
C3	0.48176 (15)	0.3710 (3)	0.15774 (15)	0.0125 (5)
C4	0.53246 (15)	0.3029 (4)	0.22948 (15)	0.0136 (5)
H4A	0.5840	0.2707	0.2377	0.016*
C5	0.50357 (15)	0.2846 (3)	0.28859 (15)	0.0119 (5)
C6	0.30319 (15)	0.4640 (4)	0.20964 (15)	0.0145 (5)
O1	0.26044 (11)	0.5719 (3)	0.15807 (11)	0.0185 (4)
O2	0.28618 (11)	0.3912 (3)	0.26427 (11)	0.0206 (4)
C7	0.50797 (15)	0.3719 (3)	0.08959 (14)	0.0124 (5)
O3	0.45938 (12)	0.3160 (3)	0.02671 (11)	0.0219 (4)
O4	0.57737 (11)	0.4236 (3)	0.10278 (11)	0.0172 (4)
C8	0.55086 (16)	0.2082 (4)	0.36836 (16)	0.0146 (5)
O5	0.62134 (12)	0.1852 (3)	0.38807 (12)	0.0278 (5)
O6	0.51110 (11)	0.1716 (3)	0.41069 (11)	0.0183 (4)
O7	0.36682 (12)	−0.0503 (3)	0.29113 (11)	0.0220 (4)
H7B	0.3178	−0.0743	0.2654	0.026*
H7A	0.3869	−0.0502	0.2585	0.026*
O8	0.40849 (13)	0.5640 (3)	0.39790 (13)	0.0267 (5)
H8A	0.4563	0.6135	0.4218	0.032*
H8B	0.3682	0.5986	0.4083	0.032*
O9	0.37653 (13)	−0.0753 (3)	0.45208 (12)	0.0232 (4)
H9A	0.4159	−0.0992	0.4946	0.028*
H9B	0.3363	−0.1166	0.4672	0.028*
N2	0.38147 (13)	0.2822 (3)	0.76366 (13)	0.0126 (4)
C9	0.31935 (15)	0.3494 (3)	0.70511 (15)	0.0136 (5)
C10	0.31717 (16)	0.3588 (4)	0.62931 (15)	0.0164 (5)
H10A	0.2726	0.4017	0.5888	0.020*
C11	0.38335 (16)	0.3023 (4)	0.61614 (15)	0.0144 (5)
C12	0.44856 (17)	0.2360 (3)	0.67751 (16)	0.0142 (5)
H12A	0.4938	0.2004	0.6699	0.017*
C13	0.44461 (16)	0.2242 (3)	0.75073 (16)	0.0135 (5)
C14	0.25231 (16)	0.4146 (4)	0.72805 (15)	0.0148 (5)
O10	0.19320 (12)	0.4815 (3)	0.67583 (11)	0.0210 (4)
O11	0.26175 (12)	0.3950 (3)	0.79795 (11)	0.0232 (4)
C15	0.38312 (17)	0.3038 (4)	0.53467 (15)	0.0157 (5)
O12	0.44658 (13)	0.2832 (3)	0.52504 (12)	0.0221 (4)
O13	0.31898 (12)	0.3173 (3)	0.47848 (11)	0.0212 (4)
C16	0.50960 (15)	0.1461 (3)	0.82233 (15)	0.0134 (5)
O14	0.57112 (12)	0.0880 (3)	0.81788 (11)	0.0206 (4)
O15	0.49458 (12)	0.1467 (3)	0.88390 (11)	0.0198 (4)
O16	0.39568 (13)	−0.0498 (3)	0.97353 (11)	0.0244 (4)
H16B	0.4251	−0.0676	1.0162	0.029*
H16A	0.3898	−0.1564	0.9530	0.029*
O17	0.28096 (12)	0.3100 (3)	0.95460 (13)	0.0283 (5)
H17B	0.2358	0.3132	0.9261	0.034*
H17A	0.2806	0.2465	0.9929	0.034*
O18	0.21204 (15)	0.6072 (3)	0.41898 (14)	0.0374 (6)
H18B	0.2389	0.5106	0.4367	0.045*
H18A	0.1688	0.5550	0.3908	0.045*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm1	0.00985 (8)	0.01369 (7)	0.00821 (7)	0.00008 (4)	0.00368 (6)	0.00015 (4)
Sm2	0.00839 (8)	0.01720 (7)	0.00731 (7)	−0.00064 (4)	0.00243 (6)	−0.00005 (4)
N1	0.0109 (11)	0.0167 (10)	0.0101 (10)	0.0002 (8)	0.0040 (9)	0.0003 (8)
C1	0.0095 (12)	0.0143 (11)	0.0133 (12)	0.0001 (9)	0.0032 (10)	0.0017 (9)
C2	0.0132 (13)	0.0169 (11)	0.0101 (12)	−0.0002 (9)	0.0026 (10)	0.0028 (9)
C3	0.0128 (13)	0.0136 (11)	0.0118 (12)	−0.0032 (9)	0.0055 (10)	−0.0006 (9)
C4	0.0108 (13)	0.0162 (11)	0.0144 (13)	−0.0015 (9)	0.0055 (11)	−0.0011 (10)
C5	0.0115 (13)	0.0128 (10)	0.0111 (12)	−0.0005 (9)	0.0041 (11)	0.0002 (9)
C6	0.0113 (13)	0.0184 (12)	0.0133 (12)	0.0010 (9)	0.0042 (10)	−0.0015 (10)
O1	0.0137 (10)	0.0243 (9)	0.0164 (10)	0.0060 (7)	0.0045 (8)	0.0061 (8)
O2	0.0128 (10)	0.0339 (10)	0.0171 (10)	0.0053 (8)	0.0079 (8)	0.0105 (8)
C7	0.0137 (13)	0.0127 (10)	0.0105 (12)	0.0009 (9)	0.0044 (10)	0.0024 (9)
O3	0.0208 (11)	0.0313 (10)	0.0112 (10)	−0.0046 (8)	0.0031 (9)	−0.0038 (8)
O4	0.0150 (10)	0.0224 (9)	0.0158 (9)	−0.0015 (7)	0.0077 (8)	0.0010 (7)
C8	0.0127 (13)	0.0158 (11)	0.0140 (13)	0.0001 (9)	0.0036 (11)	−0.0002 (10)
O5	0.0108 (11)	0.0466 (13)	0.0235 (12)	0.0054 (9)	0.0035 (9)	0.0103 (10)
O6	0.0137 (10)	0.0295 (10)	0.0121 (9)	0.0051 (8)	0.0053 (8)	0.0073 (8)
O7	0.0143 (10)	0.0353 (11)	0.0188 (10)	−0.0037 (8)	0.0090 (9)	−0.0115 (9)
O8	0.0268 (12)	0.0190 (9)	0.0329 (12)	−0.0045 (8)	0.0098 (10)	−0.0050 (8)
O9	0.0273 (12)	0.0248 (10)	0.0169 (10)	0.0035 (8)	0.0074 (9)	0.0062 (8)
N2	0.0114 (11)	0.0163 (9)	0.0095 (11)	0.0000 (8)	0.0033 (9)	0.0004 (8)
C9	0.0136 (13)	0.0157 (11)	0.0113 (12)	0.0018 (9)	0.0044 (10)	0.0009 (9)
C10	0.0168 (14)	0.0197 (12)	0.0111 (13)	0.0039 (10)	0.0034 (11)	0.0030 (10)
C11	0.0173 (14)	0.0152 (11)	0.0114 (13)	0.0001 (9)	0.0062 (11)	−0.0017 (10)
C12	0.0137 (14)	0.0169 (12)	0.0128 (13)	0.0007 (9)	0.0058 (12)	−0.0007 (9)
C13	0.0131 (14)	0.0140 (11)	0.0133 (13)	−0.0002 (9)	0.0049 (11)	−0.0013 (9)
C14	0.0139 (13)	0.0171 (11)	0.0126 (12)	0.0028 (9)	0.0039 (10)	0.0006 (10)
O10	0.0170 (11)	0.0284 (10)	0.0149 (10)	0.0110 (8)	0.0029 (8)	0.0043 (8)
O11	0.0167 (11)	0.0417 (12)	0.0124 (10)	0.0096 (9)	0.0067 (9)	0.0040 (8)
C15	0.0216 (14)	0.0164 (11)	0.0105 (13)	0.0019 (10)	0.0076 (11)	−0.0003 (10)
O12	0.0175 (11)	0.0370 (11)	0.0136 (10)	0.0003 (8)	0.0077 (9)	−0.0027 (8)
O13	0.0180 (11)	0.0347 (11)	0.0099 (9)	0.0068 (8)	0.0042 (8)	−0.0007 (8)
C16	0.0129 (13)	0.0135 (11)	0.0132 (12)	−0.0016 (9)	0.0042 (10)	0.0001 (9)
O14	0.0137 (10)	0.0303 (10)	0.0194 (10)	0.0067 (8)	0.0079 (9)	0.0014 (8)
O15	0.0152 (10)	0.0336 (10)	0.0113 (9)	0.0068 (8)	0.0057 (8)	0.0043 (8)
O16	0.0297 (12)	0.0225 (10)	0.0140 (10)	0.0053 (8)	0.0002 (9)	0.0034 (8)
O17	0.0111 (11)	0.0532 (13)	0.0215 (11)	0.0062 (9)	0.0071 (9)	0.0058 (10)
O18	0.0347 (15)	0.0383 (13)	0.0323 (13)	0.0133 (10)	0.0046 (11)	−0.0015 (10)

Geometric parameters (Å, º) top

Sm1—O6	2.406 (2)	O3—Sm2^vi	2.377 (2)
Sm1—O2	2.422 (2)	O4—Sm2^iv	2.4185 (18)
Sm1—O8	2.436 (2)	C8—O5	1.221 (3)
Sm1—O7	2.4582 (19)	C8—O6	1.285 (3)
Sm1—O9	2.4642 (19)	O7—H7B	0.8654
Sm1—O13	2.5110 (18)	O7—H7A	0.8193
Sm1—O1ⁱ	2.5243 (19)	O8—H8A	0.8930
Sm1—N1	2.564 (2)	O8—H8B	0.8667
Sm1—O12	2.587 (2)	O9—H9A	0.8662
Sm1—C15	2.901 (3)	O9—H9B	0.9304
Sm2—O10ⁱⁱ	2.3600 (19)	N2—C9	1.333 (3)
Sm2—O3ⁱⁱⁱ	2.377 (2)	N2—C13	1.335 (3)
Sm2—O17	2.3925 (19)	C9—C10	1.396 (3)
Sm2—O15	2.4120 (19)	C9—C14	1.518 (3)
Sm2—O4^iv	2.4185 (19)	C10—C11	1.387 (3)
Sm2—O11	2.420 (2)	C10—H10A	0.9300
Sm2—O16	2.463 (2)	C11—C12	1.389 (4)
Sm2—N2	2.530 (2)	C11—C15	1.512 (3)
N1—C1	1.327 (3)	C12—C13	1.392 (4)
N1—C5	1.337 (3)	C12—H12A	0.9300
C1—C2	1.394 (3)	C13—C16	1.518 (4)
C1—C6	1.514 (3)	C14—O10	1.245 (3)
C2—C3	1.391 (4)	C14—O11	1.252 (3)
C2—H2A	0.9300	O10—Sm2^vii	2.3600 (19)
C3—C4	1.393 (4)	C15—O13	1.254 (3)
C3—C7	1.515 (3)	C15—O12	1.256 (3)
C4—C5	1.394 (3)	C16—O14	1.234 (3)
C4—H4A	0.9300	C16—O15	1.274 (3)
C5—C8	1.506 (4)	O16—H16B	0.7852
C6—O1	1.237 (3)	O16—H16A	0.8179
C6—O2	1.273 (3)	O17—H17B	0.8023
O1—Sm1^v	2.5243 (19)	O17—H17A	0.8383
C7—O3	1.238 (3)	O18—H18B	0.8223
C7—O4	1.260 (3)	O18—H18A	0.8524

O6—Sm1—O2	125.63 (6)	C2—C1—C6	124.1 (2)
O6—Sm1—O8	84.72 (7)	C3—C2—C1	118.0 (2)
O2—Sm1—O8	73.68 (8)	C3—C2—H2A	121.0
O6—Sm1—O7	80.78 (7)	C1—C2—H2A	121.0
O2—Sm1—O7	86.62 (7)	C2—C3—C4	119.8 (2)
O8—Sm1—O7	141.88 (7)	C2—C3—C7	120.7 (2)
O6—Sm1—O9	86.22 (7)	C4—C3—C7	119.5 (2)
O2—Sm1—O9	139.32 (7)	C3—C4—C5	117.9 (2)
O8—Sm1—O9	140.81 (7)	C3—C4—H4A	121.1
O7—Sm1—O9	73.17 (7)	C5—C4—H4A	121.1
O6—Sm1—O13	121.87 (7)	N1—C5—C4	121.8 (2)
O2—Sm1—O13	101.87 (6)	N1—C5—C8	114.3 (2)
O8—Sm1—O13	78.10 (7)	C4—C5—C8	123.8 (2)
O7—Sm1—O13	138.87 (7)	O1—C6—O2	125.5 (2)
O9—Sm1—O13	74.70 (7)	O1—C6—C1	119.9 (2)
O6—Sm1—O1ⁱ	147.10 (6)	O2—C6—C1	114.6 (2)
O2—Sm1—O1ⁱ	72.76 (7)	C6—O1—Sm1^v	136.93 (16)
O8—Sm1—O1ⁱ	128.16 (7)	C6—O2—Sm1	127.30 (17)
O7—Sm1—O1ⁱ	72.87 (6)	O3—C7—O4	126.5 (2)
O9—Sm1—O1ⁱ	67.72 (7)	O3—C7—C3	116.3 (2)
O13—Sm1—O1ⁱ	71.60 (7)	O4—C7—C3	117.1 (2)
O6—Sm1—N1	63.12 (7)	C7—O3—Sm2^vi	170.38 (18)
O2—Sm1—N1	62.70 (7)	C7—O4—Sm2^iv	127.27 (16)
O8—Sm1—N1	70.53 (7)	O5—C8—O6	125.2 (3)
O7—Sm1—N1	71.46 (6)	O5—C8—C5	120.0 (2)
O9—Sm1—N1	136.02 (6)	O6—C8—C5	114.8 (2)
O13—Sm1—N1	147.78 (7)	C8—O6—Sm1	127.38 (17)
O1ⁱ—Sm1—N1	123.39 (7)	Sm1—O7—H7B	107.1
O6—Sm1—O12	70.93 (7)	Sm1—O7—H7A	124.1
O2—Sm1—O12	139.30 (7)	H7B—O7—H7A	104.9
O8—Sm1—O12	71.36 (7)	Sm1—O8—H8A	127.1
O7—Sm1—O12	134.07 (7)	Sm1—O8—H8B	95.7
O9—Sm1—O12	69.64 (7)	H8A—O8—H8B	123.4
O13—Sm1—O12	50.94 (7)	Sm1—O9—H9A	120.4
O1ⁱ—Sm1—O12	114.82 (7)	Sm1—O9—H9B	124.7
N1—Sm1—O12	121.65 (7)	H9A—O9—H9B	99.0
O6—Sm1—C15	96.45 (8)	C9—N2—C13	119.8 (2)
O2—Sm1—C15	123.75 (7)	C9—N2—Sm2	119.21 (16)
O8—Sm1—C15	75.45 (7)	C13—N2—Sm2	120.87 (18)
O7—Sm1—C15	140.98 (7)	N2—C9—C10	122.1 (2)
O9—Sm1—C15	67.82 (7)	N2—C9—C14	114.5 (2)
O13—Sm1—C15	25.51 (7)	C10—C9—C14	123.4 (2)
O1ⁱ—Sm1—C15	92.01 (7)	C11—C10—C9	118.0 (2)
N1—Sm1—C15	141.37 (7)	C11—C10—H10A	121.0
O12—Sm1—C15	25.64 (7)	C9—C10—H10A	121.0
O10ⁱⁱ—Sm2—O3ⁱⁱⁱ	137.50 (7)	C10—C11—C12	119.7 (2)
O10ⁱⁱ—Sm2—O17	94.18 (8)	C10—C11—C15	120.1 (2)
O3ⁱⁱⁱ—Sm2—O17	79.54 (8)	C12—C11—C15	120.1 (2)
O10ⁱⁱ—Sm2—O15	91.23 (7)	C11—C12—C13	118.5 (2)
O3ⁱⁱⁱ—Sm2—O15	83.25 (7)	C11—C12—H12A	120.8
O17—Sm2—O15	159.69 (7)	C13—C12—H12A	120.8
O10ⁱⁱ—Sm2—O4^iv	148.20 (7)	N2—C13—C12	121.8 (3)
O3ⁱⁱⁱ—Sm2—O4^iv	73.67 (7)	N2—C13—C16	113.8 (2)
O17—Sm2—O4^iv	99.20 (7)	C12—C13—C16	124.4 (2)
O15—Sm2—O4^iv	86.13 (7)	O10—C14—O11	126.2 (2)
O10ⁱⁱ—Sm2—O11	76.61 (8)	O10—C14—C9	117.2 (2)
O3ⁱⁱⁱ—Sm2—O11	137.89 (7)	O11—C14—C9	116.6 (2)
O17—Sm2—O11	72.89 (7)	C14—O10—Sm2^vii	149.34 (19)
O15—Sm2—O11	127.43 (6)	C14—O11—Sm2	125.26 (16)
O4^iv—Sm2—O11	79.98 (7)	O13—C15—O12	121.9 (2)
O10ⁱⁱ—Sm2—O16	66.67 (7)	O13—C15—C11	118.9 (2)
O3ⁱⁱⁱ—Sm2—O16	70.83 (7)	O12—C15—C11	119.2 (3)
O17—Sm2—O16	82.31 (7)	O13—C15—Sm1	59.59 (13)
O15—Sm2—O16	81.90 (7)	O12—C15—Sm1	63.06 (14)
O4^iv—Sm2—O16	143.57 (7)	C11—C15—Sm1	168.04 (17)
O11—Sm2—O16	133.64 (7)	C15—O12—Sm1	91.30 (17)
O10ⁱⁱ—Sm2—N2	73.77 (7)	C15—O13—Sm1	94.91 (15)
O3ⁱⁱⁱ—Sm2—N2	136.39 (7)	O14—C16—O15	125.1 (3)
O17—Sm2—N2	137.00 (8)	O14—C16—C13	120.0 (2)
O15—Sm2—N2	63.27 (7)	O15—C16—C13	114.9 (2)
O4^iv—Sm2—N2	76.81 (6)	C16—O15—Sm2	127.11 (17)
O11—Sm2—N2	64.22 (7)	Sm2—O16—H16B	128.1
O16—Sm2—N2	125.92 (7)	Sm2—O16—H16A	121.5
C1—N1—C5	120.1 (2)	H16B—O16—H16A	104.5
C1—N1—Sm1	120.05 (16)	Sm2—O17—H17B	117.1
C5—N1—Sm1	119.15 (16)	Sm2—O17—H17A	121.9
N1—C1—C2	122.0 (2)	H17B—O17—H17A	103.8
N1—C1—C6	113.8 (2)	H18B—O18—H18A	100.8

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O14^viii	0.82	1.87	2.686 (3)	172
O7—H7B···O2ⁱ	0.86	1.80	2.645 (3)	165
O8—H8A···O12^iv	0.89	1.83	2.727 (3)	177
O8—H8B···O9^ix	0.87	2.38	2.831 (3)	113
O9—H9A···O6^viii	0.87	1.84	2.698 (3)	171
O9—H9B···O5^viii	0.93	2.55	3.052 (3)	114
O16—H16A···O4^viii	0.82	2.31	3.075 (3)	157
O16—H16B···O15^x	0.79	1.97	2.747 (3)	171
O17—H17A···O18ⁱⁱ	0.84	1.86	2.697 (3)	176
O17—H17B···O5^xi	0.80	1.96	2.731 (3)	162
O18—H18A···O14^xii	0.85	2.06	2.905 (3)	174
O18—H18B···O13	0.82	1.93	2.736 (3)	168

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

Experimental details

Crystal data
Chemical formula	[Sm₂(C₈H₂NO₆)₂(H₂O)₅]·H₂O
M_r	825.01
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	18.426 (4), 6.9082 (14), 18.583 (4)
β (°)	111.98 (3)
V (Å³)	2193.6 (8)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.40
Crystal size (mm)	0.43 × 0.28 × 0.21

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.177, 0.321
No. of measured, independent and observed [I > 2σ(I)] reflections	20300, 4963, 4776
R_int	0.035
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.018, 0.041, 1.19
No. of reflections	4963
No. of parameters	344
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.69, −0.84

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O14ⁱ	0.82	1.87	2.686 (3)	172
O7—H7B···O2ⁱⁱ	0.86	1.80	2.645 (3)	165
O8—H8A···O12ⁱⁱⁱ	0.89	1.83	2.727 (3)	177
O8—H8B···O9^iv	0.87	2.38	2.831 (3)	113
O9—H9A···O6ⁱ	0.87	1.84	2.698 (3)	171
O9—H9B···O5ⁱ	0.93	2.55	3.052 (3)	114
O16—H16A···O4ⁱ	0.82	2.31	3.075 (3)	157
O16—H16B···O15^v	0.79	1.97	2.747 (3)	171
O17—H17A···O18^vi	0.84	1.86	2.697 (3)	176
O17—H17B···O5^vii	0.80	1.96	2.731 (3)	162
O18—H18A···O14^viii	0.85	2.06	2.905 (3)	174
O18—H18B···O13	0.82	1.93	2.736 (3)	168

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

Acknowledgements

This project was supported by the Scientific Research Fund of Ningbo University (grant Nos. XKL11058 and XYL11005). Sincere thanks are also extended to the K. C. Wong Magna Fund of Ningbo University.

References

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