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Acta Cryst. (2008). E64, m1348    [ doi:10.1107/S1600536808031036 ]

Poly[aqua[[mu]3-N'-(carboxymethyl)ethylenediamine-N,N,N'-triacetato]samarium(III)]

G.-Y. Zhou, G.-R. Wu, Z.-Y. Deng and X.-T. Chen

Abstract top

In the title coordination polymer, [Sm(C10H13N2O8)(H2O)]n, each samarium(III) centre is nine-coordinated by six O and two N atoms from three N'-(carboxymethyl)ethylenediamine-N,N,N'-triacetate ligands and one O atom of a water molecule, forming polymeric chains running parallel to the a axis. The packing is governed by intermolecular O-H...O hydrogen-bonding interactions.

Comment top

Research on metal–organic frameworks has been expanding rapidly, due to their interesting structural motifs (Dakanali et al., 2003) and other potential applications (Kitaura et al., 2002; Rowsell et al., 2004) in molecular-based materials. Ethylenediaminetetraacetic acid (H4edta) is a good example of a bridging ligand that can link metal centres into extended networks. Herein, we report a new samarium complex obtained by the hydrothermal treatment of Sm2O3 and H4edta in the presence of HClO4.

The samarium(III) metal centre is nine-coordinated by six oxygen and two nitrogen atoms from three different N'-(carboxymethyl)ethylenediamine-N,N,N'-triacetato ligands and one water molecule (Fig. 1) to form a polymeric chain running parallel to the crystallographic a axis (Fig. 2). The Sm···Sm separations between adjacent metal centres are 4.2461 (6) and 6.6506 (8) Å. The polymeric chains self-assemble via intermolecular O—H···O hydrogen bonding interactions (Table 1) to form a three-dimensional supramolecular network. The title compound is isostructural with the corresponding neodymium polymeric complex (Huang et al., 2008).

Related literature top

For the corresponding neodymium polymeric complex, see: Huang et al. (2008). For related literature, see: Dakanali et al. (2003); Kitaura et al. (2002); Rowsell et al. (2004).

Experimental top

A mixture of Sm2O3 (0.5 mmol), ethylenediaminetetraacetic acid (H4edta) (0.5 mmol), HClO4 (0.2 mmol) and H2O (10 ml) was placed in a 23 ml Teflon reactor, which was heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h-1. The crystals obtained were washed with water and dryed in air.

Refinement top

Water H atoms were tentatively located in difference Fourier maps and were refined with distance restraints of O—H = 0.82 Å and H···H = 1.20 Å, each within a standard deviation of 0.01 Å, and with Uiso(H) = 1.5Ueq(O). Other H atoms were placed in calculated positions (C—H = 0.97 Å and O—H = 0.82 Å) and refined using a riding model, with Uiso(H) = 1.2Ueq(C, O).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 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: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of the title compound, showing the atomic numbering scheme. Non-H atoms are shown as 30% probability displacement ellipsoids. Symmetry codes: (i: 1+x, y, z; ii: 2-x, 1-y, 1-z).
[Figure 2] Fig. 2. The one-dimensional polymeric chain of the title compound.
Poly[aqua[µ3-N'-(carboxymethyl)ethylenediamine-N,N,N'-triacetato] samarium(III)] top
Crystal data top
[Sm(C10H13N2O8)(H2O)]F(000) = 1784
Mr = 457.60Dx = 2.394 Mg m−3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 3600 reflections
a = 6.6506 (7) Åθ = 1.7–28.0°
b = 14.7051 (16) ŵ = 4.68 mm−1
c = 25.967 (3) ÅT = 296 K
V = 2539.5 (5) Å3Block, colourless
Z = 80.23 × 0.19 × 0.18 mm
Data collection top
Bruker APEXII area-detector
diffractometer		2637 independent reflections
Radiation source: fine-focus sealed tube2289 reflections with I > 2σ(I)
graphiteRint = 0.035
φ and ω scanθmax = 26.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −8→5
Tmin = 0.355, Tmax = 0.433k = −16→18
13066 measured reflectionsl = −32→32
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0288P)2 + 6.2721P]
where P = (Fo2 + 2Fc2)/3
2637 reflections(Δ/σ)max = 0.002
206 parametersΔρmax = 0.94 e Å−3
3 restraintsΔρmin = −1.21 e Å−3
Crystal data top
[Sm(C10H13N2O8)(H2O)]V = 2539.5 (5) Å3
Mr = 457.60Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 6.6506 (7) ŵ = 4.68 mm−1
b = 14.7051 (16) ÅT = 296 K
c = 25.967 (3) Å0.23 × 0.19 × 0.18 mm
Data collection top
Bruker APEXII area-detector
diffractometer		2637 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2289 reflections with I > 2σ(I)
Tmin = 0.355, Tmax = 0.433Rint = 0.035
13066 measured reflectionsθmax = 26.5°
Refinement top
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.064Δρmax = 0.94 e Å−3
S = 1.03Δρmin = −1.21 e Å−3
2637 reflectionsAbsolute structure: ?
206 parametersFlack parameter: ?
3 restraintsRogers parameter: ?
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
xyzUiso*/Ueq
Sm11.07590 (3)0.506856 (12)0.420681 (7)0.01387 (8)
C11.2133 (6)0.3523 (3)0.33453 (14)0.0168 (8)
C21.0904 (6)0.2870 (3)0.36651 (15)0.0186 (8)
H2A1.01700.24670.34370.022*
H2B1.18070.25000.38700.022*
C30.7461 (6)0.3440 (3)0.37554 (15)0.0197 (8)
H3A0.65430.37390.39910.024*
H3B0.69180.28430.36780.024*
C40.7586 (6)0.3985 (3)0.32648 (14)0.0193 (8)
H4A0.85800.37130.30390.023*
H4B0.62970.39650.30900.023*
C50.9165 (6)0.5334 (3)0.29164 (15)0.0186 (8)
H5A0.81890.54860.26520.022*
H5B1.00970.48930.27740.022*
C61.0293 (6)0.6179 (3)0.30788 (15)0.0178 (8)
C70.6310 (6)0.5491 (3)0.34790 (15)0.0199 (9)
H7A0.51630.52050.33150.024*
H7B0.64670.60910.33290.024*
C80.5880 (6)0.5592 (3)0.40475 (15)0.0166 (8)
C90.9173 (6)0.2796 (3)0.44879 (15)0.0194 (9)
H9A1.02770.23690.45220.023*
H9B0.79420.24470.44580.023*
C100.9064 (6)0.3372 (3)0.49695 (15)0.0173 (8)
N10.9459 (5)0.3332 (2)0.40114 (12)0.0164 (7)
N20.8138 (5)0.4946 (2)0.33643 (12)0.0173 (7)
O11.2293 (4)0.43367 (18)0.34962 (10)0.0207 (6)
O21.2980 (5)0.32419 (18)0.29435 (10)0.0235 (7)
O31.0724 (4)0.63138 (19)0.35307 (11)0.0232 (7)
O41.0758 (5)0.6717 (2)0.27029 (11)0.0292 (7)
H41.11820.71990.28190.044*
O50.9074 (4)0.42346 (18)0.49227 (10)0.0203 (6)
O60.7369 (4)0.5605 (2)0.43483 (10)0.0233 (6)
O70.4107 (4)0.57144 (19)0.41872 (11)0.0211 (6)
O80.9000 (5)0.2985 (2)0.53938 (11)0.0294 (7)
O1W1.3250 (5)0.3977 (2)0.46232 (11)0.0271 (7)
H2W1.350 (8)0.3428 (10)0.4613 (15)0.041*
H1W1.348 (8)0.412 (3)0.4922 (7)0.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.01036 (12)0.01782 (12)0.01343 (12)0.00028 (8)0.00067 (7)−0.00100 (8)
C10.0145 (19)0.021 (2)0.0153 (18)0.0028 (16)0.0001 (15)−0.0005 (15)
C20.019 (2)0.0179 (19)0.019 (2)0.0032 (17)0.0014 (16)0.0000 (16)
C30.016 (2)0.0196 (19)0.023 (2)−0.0039 (17)−0.0008 (18)−0.0007 (16)
C40.017 (2)0.022 (2)0.0197 (19)−0.0027 (16)−0.0040 (17)−0.0026 (15)
C50.019 (2)0.022 (2)0.0152 (19)−0.0017 (17)−0.0002 (16)−0.0008 (16)
C60.0142 (19)0.018 (2)0.021 (2)0.0000 (16)0.0007 (16)0.0010 (16)
C70.016 (2)0.026 (2)0.018 (2)0.0035 (17)0.0008 (16)0.0034 (17)
C80.014 (2)0.0157 (18)0.020 (2)−0.0015 (15)0.0019 (16)−0.0007 (15)
C90.025 (2)0.017 (2)0.016 (2)0.0001 (17)0.0005 (17)0.0022 (15)
C100.0102 (19)0.024 (2)0.0176 (19)−0.0010 (16)0.0031 (15)0.0005 (16)
N10.0181 (18)0.0169 (16)0.0143 (16)0.0004 (14)0.0019 (13)0.0000 (13)
N20.0138 (16)0.0193 (17)0.0187 (16)0.0011 (14)0.0008 (13)0.0005 (14)
O10.0174 (15)0.0206 (14)0.0242 (14)−0.0011 (12)0.0052 (12)−0.0055 (12)
O20.0319 (18)0.0201 (14)0.0186 (14)0.0006 (13)0.0078 (12)−0.0020 (12)
O30.0277 (17)0.0257 (16)0.0163 (14)−0.0039 (13)−0.0037 (12)0.0008 (12)
O40.046 (2)0.0227 (16)0.0190 (15)−0.0149 (15)0.0017 (14)0.0007 (12)
O50.0218 (16)0.0184 (14)0.0209 (15)−0.0051 (12)0.0034 (12)−0.0039 (11)
O60.0133 (14)0.0355 (17)0.0211 (14)0.0051 (13)−0.0039 (12)−0.0038 (12)
O70.0115 (14)0.0224 (15)0.0295 (16)−0.0004 (11)0.0016 (12)−0.0047 (12)
O80.0337 (19)0.0355 (18)0.0189 (15)0.0007 (15)0.0027 (13)0.0061 (13)
O1W0.0303 (18)0.0290 (17)0.0221 (16)0.0045 (15)−0.0043 (14)0.0029 (13)
Geometric parameters (Å, °) top
Sm1—O12.367 (3)C5—C61.512 (5)
Sm1—O62.416 (3)C5—H5A0.9700
Sm1—O7i2.421 (3)C5—H5B0.9700
Sm1—O5ii2.484 (3)C6—O31.224 (5)
Sm1—O52.493 (3)C6—O41.294 (5)
Sm1—O32.537 (3)C7—N21.486 (5)
Sm1—O1W2.548 (3)C7—C81.511 (5)
Sm1—N12.744 (3)C7—H7A0.9700
Sm1—N22.803 (3)C7—H7B0.9700
C1—O21.256 (4)C8—O71.247 (5)
C1—O11.263 (5)C8—O61.261 (5)
C1—C21.510 (5)C9—N11.479 (5)
C2—N11.481 (5)C9—C101.512 (5)
C2—H2A0.9700C9—H9A0.9700
C2—H2B0.9700C9—H9B0.9700
C3—N11.494 (5)C10—O81.241 (5)
C3—C41.507 (5)C10—O51.274 (5)
C3—H3A0.9700O4—H40.8200
C3—H3B0.9700O5—Sm1ii2.484 (3)
C4—N21.483 (5)O7—Sm1iii2.421 (3)
C4—H4A0.9700O1W—H2W0.823 (10)
C4—H4B0.9700O1W—H1W0.820 (10)
C5—N21.464 (5)
O1—Sm1—O6131.98 (9)N2—C4—H4B109.2
O1—Sm1—O7i76.45 (9)C3—C4—H4B109.2
O6—Sm1—O7i137.16 (10)H4A—C4—H4B107.9
O1—Sm1—O5ii151.34 (10)N2—C5—C6109.3 (3)
O6—Sm1—O5ii76.64 (9)N2—C5—H5A109.8
O7i—Sm1—O5ii79.40 (9)C6—C5—H5A109.8
O1—Sm1—O5123.46 (9)N2—C5—H5B109.8
O6—Sm1—O568.14 (9)C6—C5—H5B109.8
O7i—Sm1—O5128.46 (9)H5A—C5—H5B108.3
O5ii—Sm1—O562.91 (10)O3—C6—O4124.6 (4)
O1—Sm1—O378.03 (9)O3—C6—C5121.1 (4)
O6—Sm1—O382.03 (9)O4—C6—C5114.2 (3)
O7i—Sm1—O373.18 (9)N2—C7—C8113.8 (3)
O5ii—Sm1—O3109.41 (9)N2—C7—H7A108.8
O5—Sm1—O3150.11 (9)C8—C7—H7A108.8
O1—Sm1—O1W76.36 (9)N2—C7—H7B108.8
O6—Sm1—O1W138.39 (10)C8—C7—H7B108.8
O7i—Sm1—O1W70.02 (10)H7A—C7—H7B107.7
O5ii—Sm1—O1W81.07 (10)O7—C8—O6124.1 (4)
O5—Sm1—O1W70.48 (10)O7—C8—C7118.5 (3)
O3—Sm1—O1W138.98 (10)O6—C8—C7117.2 (3)
O1—Sm1—N164.43 (9)N1—C9—C10113.6 (3)
O6—Sm1—N192.16 (10)N1—C9—H9A108.9
O7i—Sm1—N1130.62 (9)C10—C9—H9A108.9
O5ii—Sm1—N1124.49 (9)N1—C9—H9B108.9
O5—Sm1—N162.50 (9)C10—C9—H9B108.9
O3—Sm1—N1122.76 (9)H9A—C9—H9B107.7
O1W—Sm1—N172.34 (10)O8—C10—O5122.8 (4)
O1—Sm1—N268.30 (10)O8—C10—C9118.6 (4)
O6—Sm1—N263.86 (9)O5—C10—C9118.6 (3)
O7i—Sm1—N2125.50 (9)C9—N1—C2110.3 (3)
O5ii—Sm1—N2139.87 (9)C9—N1—C3108.3 (3)
O5—Sm1—N2105.71 (9)C2—N1—C3110.8 (3)
O3—Sm1—N260.04 (9)C9—N1—Sm1112.4 (2)
O1W—Sm1—N2134.02 (10)C2—N1—Sm1109.5 (2)
N1—Sm1—N266.42 (9)C3—N1—Sm1105.3 (2)
O2—C1—O1122.1 (4)C5—N2—C4110.4 (3)
O2—C1—C2119.3 (3)C5—N2—C7109.3 (3)
O1—C1—C2118.5 (3)C4—N2—C7110.2 (3)
N1—C2—C1113.2 (3)C5—N2—Sm1107.8 (2)
N1—C2—H2A108.9C4—N2—Sm1110.6 (2)
C1—C2—H2A108.9C7—N2—Sm1108.5 (2)
N1—C2—H2B108.9C1—O1—Sm1129.5 (2)
C1—C2—H2B108.9C6—O3—Sm1123.3 (3)
H2A—C2—H2B107.8C6—O4—H4109.5
N1—C3—C4112.6 (3)C10—O5—Sm1ii108.9 (2)
N1—C3—H3A109.1C10—O5—Sm1124.3 (2)
C4—C3—H3A109.1Sm1ii—O5—Sm1117.09 (10)
N1—C3—H3B109.1C8—O6—Sm1129.3 (2)
C4—C3—H3B109.1C8—O7—Sm1iii145.0 (3)
H3A—C3—H3B107.8Sm1—O1W—H2W137 (3)
N2—C4—C3111.9 (3)Sm1—O1W—H1W111 (3)
N2—C4—H4A109.2H2W—O1W—H1W104 (4)
C3—C4—H4A109.2
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) x−1, y, z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O4—H4···O2iv0.821.662.474 (4)170.
O1W—H1W···O6ii0.82 (1)2.02 (2)2.771 (4)153.(2)
O1W—H2W···O8v0.82 (1)2.10 (2)2.928 (4)177.(2)
Symmetry codes: (iv) −x+5/2, y+1/2, z; (ii) −x+2, −y+1, −z+1; (v) x+1/2, −y+1/2, −z+1.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O4—H4···O2i0.821.662.474 (4)170.
O1W—H1W···O6ii0.82 (1)2.02 (2)2.771 (4)153.(2)
O1W—H2W···O8iii0.82 (1)2.10 (2)2.928 (4)177.(2)
Symmetry codes: (i) −x+5/2, y+1/2, z; (ii) −x+2, −y+1, −z+1; (iii) x+1/2, −y+1/2, −z+1.
Acknowledgements top

The authors acknowledge Hezhou University for supporting this work.

references
References top

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