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Acta Cryst. (2007). E63, m3019    [ doi:10.1107/S1600536807057303 ]

Poly[[diaquatri-[mu]4-succinato-dineodymium(III)] monohydrate]

Y.-K. He, X.-F. Wang, L.-T. Zhang, Z.-B. Han and S. W. Ng

Abstract top

Carboxylate bridging in the title neodymium(III) coordination polymer, {[Nd2(C4H4O4)3(H2O)2]·H2O}n, leads to a three-dimensional network architecture. One of the two independent succinate groups lies on a centre of inversion whereas the other lies on a general position; both engage in [mu]4-bridging. The motif is consolidated by hydrogen bonds that involve the coordinated water molecule. The uncoordinated water molecule, which lies on a twofold rotation axis, is only weakly hydrogen bonded to the network. The NdIII atom shows tricapped trigonal prismatic coordination.

Comment top

The holonium ion reacts with succinic acid under hydrothermal conditions to form polymeric [Ho2(C4H4O4)3(H2O)4·6H2O] and [Ho2(C4H4O4)3(H2O)2·H2O] (Bernini et al., 2007). The latter compound is a dihydrate. With the neodymium cation in place of the holonium cation, the reaction yields the title compound, which has the corresponding formulation.

The title compound is polymeric owing to carboxylate bridging; the geometry of the metal atom is a tricapped trigonal prism (Fig. 2).

Related literature top

For the structure of [Ho2(C4H4O4)3(H2O)2·H2O], see: Bernini et al. (2007).

Experimental top

Neodymium nitrate hexahydrate (0.4 mmol, 0.175 g), succinic acid (1 mmol, 0.118 g), sodium hydroxide (1 mmol, 0.04 g) and water (10 ml) were placed in a 23-ml Teflon-lined Parr bomb. The bomb was heated at 453 K for 3 d and then cooled to room temperature at a rate of 5 K h−1 (yield 70%). CH&N elemental analysis for C12H18Nd2O15 (found%/calc%): C 20.79/20.87, H 2.57/2.63.

Refinement top

The methylene H atoms were placed at calculated positions (C—H = 0.97 Å) in the riding model approximation, with their Uiso values set to 1.2 times Ueq of the parent atoms. The H atoms of O1w were placed in chemically sensible positions on the basis of hydrogen bonds but were not refined (O—H = 0.85 Å). The H atom on O2w, which lies on a twofold axis, was similarly placed; however, O2w is only a weak hydrogen bond donor to O1w. The final difference Fourier map had a deep hole in the vicinity of Nd1 but was otherwise featureless.

Computing details top

Data collection: XSCANS (Bruker, 2000); cell refinement: XSCANS (Bruker, 2000); data reduction: XSCANS (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. Part of the polymeric structure of the title compound. Displacement ellipsoids are drawn at the 70% probability level, and H atoms as spheres of arbitrary radii. Symmetry codes are given in Table 1.
[Figure 2] Fig. 2. Geometry of the neodymium atom in the title compound.
Poly[[diaquatri-µ4-succinato-dineodymium(III)] monohydrate] top
Crystal data top
[Nd2(C4H4O4)3(H2O)2]·H2OF000 = 1320
Mr = 690.74Dx = 2.429 Mg m−3
Monoclinic, C2/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 28 reflections
a = 19.966 (4) Åθ = 5.2–12.4º
b = 7.8761 (9) ŵ = 5.51 mm−1
c = 13.9861 (8) ÅT = 295 (2) K
β = 120.81 (1)ºBlock, purple
V = 1889.0 (5) Å30.37 × 0.35 × 0.23 mm
Z = 4
Data collection top
Siemens P4
diffractometer		Rint = 0.019
Radiation source: medium-focus sealed tubeθmax = 26.0º
Monochromator: graphiteθmin = 2.4º
T = 295(2) Kh = −1→24
ω–2θ scansk = −1→9
Absorption correction: ψ scan
(North et al., 1968)		l = −17→15
Tmin = 0.194, Tmax = 0.3643 standard reflections
2342 measured reflections every 97 reflections
1859 independent reflections intensity decay: <1%
1759 reflections with I > 2σ(I)
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.066  w = 1/[σ2(Fo2) + (0.0385P)2 + 5.3046P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
1859 reflectionsΔρmax = 0.71 e Å−3
132 parametersΔρmin = −1.53 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Nd2(C4H4O4)3(H2O)2]·H2OV = 1889.0 (5) Å3
Mr = 690.74Z = 4
Monoclinic, C2/cMo Kα
a = 19.966 (4) ŵ = 5.51 mm−1
b = 7.8761 (9) ÅT = 295 (2) K
c = 13.9861 (8) Å0.37 × 0.35 × 0.23 mm
β = 120.81 (1)º
Data collection top
Siemens P4
diffractometer		1759 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)		Rint = 0.019
Tmin = 0.194, Tmax = 0.3643 standard reflections
2342 measured reflections every 97 reflections
1859 independent reflections intensity decay: <1%
Refinement top
R[F2 > 2σ(F2)] = 0.024132 parameters
wR(F2) = 0.066H-atom parameters constrained
S = 1.03Δρmax = 0.71 e Å−3
1859 reflectionsΔρmin = −1.53 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.269282 (10)0.78357 (2)0.230560 (14)0.01147 (10)
O10.1961 (2)0.7564 (4)0.3297 (3)0.0262 (7)
O20.17965 (17)0.4808 (3)0.3430 (2)0.0255 (6)
O30.18625 (14)0.4811 (3)0.6347 (2)0.0201 (5)
O40.17029 (17)0.2677 (3)0.5265 (2)0.0201 (6)
O50.40816 (16)0.7251 (3)0.3807 (2)0.0217 (6)
O60.32606 (13)0.5160 (3)0.3399 (2)0.0181 (5)
O1w0.33554 (16)0.6094 (3)0.1495 (2)0.0234 (6)
H110.32180.64600.08480.035*
H120.32230.50590.14540.035*
O2w0.50000.5101 (10)0.25000.079 (2)
H210.52030.57100.22060.118*
C10.1697 (2)0.6327 (4)0.3572 (3)0.0167 (7)
C20.1225 (2)0.6721 (5)0.4117 (3)0.0200 (7)
H2A0.07920.74480.36240.024*
H2B0.15510.73500.47980.024*
C30.0903 (2)0.5144 (5)0.4397 (3)0.0184 (7)
H3A0.05080.54980.45630.022*
H3B0.06550.44090.37500.022*
C40.15256 (18)0.4147 (5)0.5375 (3)0.0142 (6)
C50.39642 (19)0.5743 (5)0.3931 (3)0.0158 (7)
C60.4604 (2)0.4567 (5)0.4686 (3)0.0259 (8)
H6A0.46300.36390.42500.031*
H6B0.44830.40880.52190.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.01244 (14)0.00748 (15)0.01412 (14)0.00056 (6)0.00653 (10)0.00027 (6)
O10.0398 (18)0.0149 (11)0.0377 (18)−0.0004 (13)0.0298 (16)0.0011 (13)
O20.0356 (15)0.0124 (12)0.0414 (16)0.0014 (12)0.0290 (14)−0.0003 (12)
O30.0197 (12)0.0181 (13)0.0159 (12)0.0023 (11)0.0043 (10)−0.0034 (10)
O40.0293 (15)0.0117 (12)0.0159 (13)−0.0006 (11)0.0091 (12)0.0003 (10)
O50.0138 (13)0.0126 (13)0.0298 (15)−0.0002 (10)0.0046 (12)0.0014 (10)
O60.0103 (11)0.0192 (13)0.0193 (11)−0.0015 (10)0.0035 (10)0.0041 (10)
O1w0.0341 (15)0.0168 (13)0.0270 (13)0.0020 (12)0.0213 (12)0.0018 (11)
O2w0.053 (3)0.094 (5)0.087 (5)0.0000.033 (3)0.000
C10.0182 (17)0.0142 (16)0.0167 (16)0.0018 (13)0.0082 (14)0.0006 (13)
C20.0279 (19)0.0160 (16)0.0225 (18)0.0049 (16)0.0174 (16)0.0037 (15)
C30.0148 (15)0.0210 (17)0.0168 (16)−0.0009 (14)0.0062 (13)0.0010 (14)
C40.0118 (15)0.0158 (16)0.0163 (16)−0.0045 (14)0.0081 (13)0.0010 (14)
C50.0156 (16)0.0173 (16)0.0132 (15)−0.0016 (14)0.0064 (13)−0.0024 (14)
C60.0139 (18)0.0179 (18)0.034 (2)−0.0009 (16)0.0033 (16)0.0052 (16)
Geometric parameters (Å, °) top
Nd1—O12.486 (3)O6—C51.291 (4)
Nd1—O2i2.363 (3)O6—Nd1iv2.455 (2)
Nd1—O3ii2.572 (3)O1w—H110.85
Nd1—O3iii2.463 (2)O1w—H120.85
Nd1—O4ii2.537 (3)O2w—H210.86
Nd1—O52.519 (3)C1—C21.518 (5)
Nd1—O62.508 (2)C2—C31.538 (5)
Nd1—O6i2.455 (2)C2—H2A0.97
Nd1—O1w2.540 (3)C2—H2B0.97
O1—C11.258 (5)C3—C41.513 (5)
O2—C11.245 (4)C3—H3A0.97
O2—Nd1iv2.363 (3)C3—H3B0.97
O3—C41.278 (4)C4—Nd1v2.952 (3)
O3—Nd1iii2.463 (2)C5—C61.491 (5)
O3—Nd1v2.572 (3)C6—C6vi1.522 (7)
O4—C41.243 (4)C6—H6A0.97
O4—Nd1v2.537 (3)C6—H6B0.97
O5—C51.240 (4)
O2i—Nd1—O6i75.74 (9)C4—O4—Nd1v96.7 (2)
O2i—Nd1—O3iii76.80 (9)C5—O5—Nd194.9 (2)
O6i—Nd1—O3iii69.35 (9)C5—O6—Nd1iv152.6 (2)
O2i—Nd1—O1143.84 (10)C5—O6—Nd194.1 (2)
O6i—Nd1—O174.43 (10)Nd1iv—O6—Nd1111.50 (9)
O3iii—Nd1—O173.88 (10)Nd1—O1w—H11109.5
O2i—Nd1—O6131.05 (9)Nd1—O1w—H12109.5
O6i—Nd1—O6152.50 (3)H11—O1w—H12109.5
O3iii—Nd1—O6107.01 (8)O2—C1—O1124.7 (3)
O1—Nd1—O678.39 (9)O2—C1—C2117.9 (3)
O2i—Nd1—O586.97 (10)O1—C1—C2117.4 (3)
O6i—Nd1—O5140.11 (8)C1—C2—C3114.2 (3)
O3iii—Nd1—O571.83 (8)C1—C2—H2A108.7
O1—Nd1—O5103.28 (11)C3—C2—H2A108.7
O6—Nd1—O551.47 (8)C1—C2—H2B108.7
O2i—Nd1—O4ii82.89 (10)C3—C2—H2B108.7
O6i—Nd1—O4ii70.72 (8)H2A—C2—H2B107.6
O3iii—Nd1—O4ii138.47 (8)C4—C3—C2113.1 (3)
O1—Nd1—O4ii105.77 (11)C4—C3—H3A109.0
O6—Nd1—O4ii113.63 (8)C2—C3—H3A109.0
O5—Nd1—O4ii143.08 (10)C4—C3—H3B109.0
O2i—Nd1—O1w73.82 (9)C2—C3—H3B109.0
O6i—Nd1—O1w134.24 (8)H3A—C3—H3B107.8
O3iii—Nd1—O1w133.01 (9)O4—C4—O3119.0 (3)
O1—Nd1—O1w142.34 (9)O4—C4—C3121.7 (3)
O6—Nd1—O1w69.04 (8)O3—C4—C3119.3 (3)
O5—Nd1—O1w70.79 (9)O4—C4—Nd1v58.60 (18)
O4ii—Nd1—O1w72.30 (9)O3—C4—Nd1v60.36 (18)
O2i—Nd1—O3ii127.75 (9)C3—C4—Nd1v177.8 (2)
O6i—Nd1—O3ii103.59 (8)O5—C5—O6119.2 (3)
O3iii—Nd1—O3ii153.22 (2)O5—C5—C6122.6 (3)
O1—Nd1—O3ii79.34 (9)O6—C5—C6118.1 (3)
O6—Nd1—O3ii66.82 (8)O5—C5—Nd159.91 (19)
O5—Nd1—O3ii115.27 (8)O6—C5—Nd159.57 (17)
O4ii—Nd1—O3ii50.33 (8)C6—C5—Nd1175.1 (3)
O1w—Nd1—O3ii70.94 (9)C5—C6—C6vi113.0 (4)
C1—O1—Nd1134.0 (3)C5—C6—H6A109.0
C1—O2—Nd1iv147.2 (2)C6vi—C6—H6A109.0
C4—O3—Nd1iii155.3 (2)C5—C6—H6B109.0
C4—O3—Nd1v94.0 (2)C6vi—C6—H6B109.0
Nd1iii—O3—Nd1v109.12 (9)H6A—C6—H6B107.8
O2i—Nd1—O1—C1175.0 (3)O6i—Nd1—O6—Nd1iv60.36 (18)
O6i—Nd1—O1—C1139.6 (4)O3iii—Nd1—O6—Nd1iv138.18 (10)
O3iii—Nd1—O1—C1−147.9 (4)O1—Nd1—O6—Nd1iv69.23 (11)
O6—Nd1—O1—C1−36.2 (4)O5—Nd1—O6—Nd1iv−173.16 (16)
O5—Nd1—O1—C1−81.6 (4)O4ii—Nd1—O6—Nd1iv−33.06 (13)
O4ii—Nd1—O1—C175.3 (4)O1w—Nd1—O6—Nd1iv−91.53 (11)
O1w—Nd1—O1—C1−6.0 (5)O3ii—Nd1—O6—Nd1iv−14.02 (9)
O3ii—Nd1—O1—C132.1 (4)C5—Nd1—O6—Nd1iv−169.9 (2)
C5—Nd1—O1—C1−58.6 (4)C4ii—Nd1—O6—Nd1iv−23.57 (11)
C4ii—Nd1—O1—C153.9 (4)Nd1iv—O2—C1—O1−4.1 (8)
Nd1iv—Nd1—O1—C1−2.3 (3)Nd1iv—O2—C1—C2176.0 (3)
O2i—Nd1—O5—C5−148.6 (2)Nd1—O1—C1—O24.1 (6)
O6i—Nd1—O5—C5147.99 (19)Nd1—O1—C1—C2−176.0 (3)
O3iii—Nd1—O5—C5134.3 (2)O2—C1—C2—C3−1.8 (5)
O1—Nd1—O5—C566.5 (2)O1—C1—C2—C3178.3 (3)
O6—Nd1—O5—C53.36 (19)C1—C2—C3—C472.9 (4)
O4ii—Nd1—O5—C5−74.7 (3)Nd1v—O4—C4—O30.5 (3)
O1w—Nd1—O5—C5−74.7 (2)Nd1v—O4—C4—C3−177.4 (3)
O3ii—Nd1—O5—C5−17.9 (3)Nd1iii—O3—C4—O4159.2 (4)
C4ii—Nd1—O5—C5−40.4 (3)Nd1v—O3—C4—O4−0.5 (3)
Nd1iv—Nd1—O5—C5−0.4 (2)Nd1iii—O3—C4—C3−22.8 (7)
O2i—Nd1—O6—C535.2 (2)Nd1v—O3—C4—C3177.4 (3)
O6i—Nd1—O6—C5−129.7 (2)Nd1iii—O3—C4—Nd1v159.8 (6)
O3iii—Nd1—O6—C5−51.89 (19)C2—C3—C4—O4−115.1 (4)
O1—Nd1—O6—C5−120.8 (2)C2—C3—C4—O367.0 (4)
O5—Nd1—O6—C5−3.23 (19)Nd1—O5—C5—O6−5.9 (3)
O4ii—Nd1—O6—C5136.87 (19)Nd1—O5—C5—C6175.1 (3)
O1w—Nd1—O6—C578.41 (19)Nd1iv—O6—C5—O5165.2 (3)
O3ii—Nd1—O6—C5155.9 (2)Nd1—O6—C5—O55.9 (3)
C4ii—Nd1—O6—C5146.4 (2)Nd1iv—O6—C5—C6−15.7 (6)
Nd1iv—Nd1—O6—C5169.9 (2)Nd1—O6—C5—C6−175.0 (3)
O2i—Nd1—O6—Nd1iv−134.70 (11)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x, −y+1, z−1/2; (iii) −x+1/2, −y+3/2, −z+1; (iv) −x+1/2, y−1/2, −z+1/2; (v) x, −y+1, z+1/2; (vi) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H12···O1iv0.852.062.899 (4)168
O1W—H11···O4i0.851.902.709 (4)158
Symmetry codes: (iv) −x+1/2, y−1/2, −z+1/2; (i) −x+1/2, y+1/2, −z+1/2.
Table 1
Selected geometric parameters (Å) top
Nd1—O12.486 (3)Nd1—O52.519 (3)
Nd1—O2i2.363 (3)Nd1—O62.508 (2)
Nd1—O3ii2.572 (3)Nd1—O6i2.455 (2)
Nd1—O3iii2.463 (2)Nd1—O1w2.540 (3)
Nd1—O4ii2.537 (3)
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x, −y+1, z−1/2; (iii) −x+1/2, −y+3/2, −z+1.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H12···O1iv0.852.062.899 (4)168
O1W—H11···O4i0.851.902.709 (4)158
Symmetry codes: (iv) −x+1/2, y−1/2, −z+1/2; (i) −x+1/2, y+1/2, −z+1/2.
Acknowledgements top

The authors thank the Program for Liaoning Excellent Talents in Liaoning University (grant No. RC-05–11) and the University of Malaya for supporting this study.

references
References top

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.

Bernini, M.-C., Brusau, E.-V., Narda, G.-E., Echeverria, G.-E., Pozzi, C.-G., Punte, G. & Lehmann, C.-W. (2007). Eur. J. Inorg. Chem. pp. 684–693.

Bruker (2000). XSCANS. Bruker AXS Inc., Madison, Wisconsin, USA.

North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351–359.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Westrip, S. P. (2007). publCIF. In preparation.