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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 μ4-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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807057303/ci2484sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807057303/ci2484Isup2.hkl
Contains datablock I

CCDC reference: 672662

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.024
  • wR factor = 0.066
  • Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.77 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.30 Ratio
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.773 Tmax scaled 0.281 Tmin scaled 0.150 PLAT794_ALERT_5_G Check Predicted Bond Valency for Nd1 (2) 2.10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

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]·H2OF(000) = 1320
Mr = 690.74Dx = 2.429 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 28 reflections
a = 19.966 (4) Åθ = 5.2–12.4°
b = 7.8761 (9) ŵ = 5.51 mm1
c = 13.9861 (8) ÅT = 295 K
β = 120.81 (1)°Block, purple
V = 1889.0 (5) Å30.37 × 0.35 × 0.23 mm
Z = 4
Data collection top
Siemens P4
diffractometer
1759 reflections with I > 2σ(I)
Radiation source: medium-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 26.0°, θmin = 2.4°
ω–2θ scansh = 124
Absorption correction: ψ scan
(North et al., 1968)
k = 19
Tmin = 0.194, Tmax = 0.364l = 1715
2342 measured reflections3 standard reflections every 97 reflections
1859 independent reflections intensity decay: <1%
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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0385P)2 + 5.3046P]
where P = (Fo2 + 2Fc2)/3
1859 reflections(Δ/σ)max = 0.001
132 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 1.53 e Å3
Crystal data top
[Nd2(C4H4O4)3(H2O)2]·H2OV = 1889.0 (5) Å3
Mr = 690.74Z = 4
Monoclinic, C2/cMo Kα radiation
a = 19.966 (4) ŵ = 5.51 mm1
b = 7.8761 (9) ÅT = 295 K
c = 13.9861 (8) Å0.37 × 0.35 × 0.23 mm
β = 120.81 (1)°
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 every 97 reflections
2342 measured reflections intensity decay: <1%
1859 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.066H-atom parameters constrained
S = 1.03Δρmax = 0.71 e Å3
1859 reflectionsΔρmin = 1.53 e Å3
132 parameters
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, º) 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—C1147.9 (4)O1—Nd1—O6—Nd1iv69.23 (11)
O6—Nd1—O1—C136.2 (4)O5—Nd1—O6—Nd1iv173.16 (16)
O5—Nd1—O1—C181.6 (4)O4ii—Nd1—O6—Nd1iv33.06 (13)
O4ii—Nd1—O1—C175.3 (4)O1w—Nd1—O6—Nd1iv91.53 (11)
O1w—Nd1—O1—C16.0 (5)O3ii—Nd1—O6—Nd1iv14.02 (9)
O3ii—Nd1—O1—C132.1 (4)C5—Nd1—O6—Nd1iv169.9 (2)
C5—Nd1—O1—C158.6 (4)C4ii—Nd1—O6—Nd1iv23.57 (11)
C4ii—Nd1—O1—C153.9 (4)Nd1iv—O2—C1—O14.1 (8)
Nd1iv—Nd1—O1—C12.3 (3)Nd1iv—O2—C1—C2176.0 (3)
O2i—Nd1—O5—C5148.6 (2)Nd1—O1—C1—O24.1 (6)
O6i—Nd1—O5—C5147.99 (19)Nd1—O1—C1—C2176.0 (3)
O3iii—Nd1—O5—C5134.3 (2)O2—C1—C2—C31.8 (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—C574.7 (3)Nd1v—O4—C4—O30.5 (3)
O1w—Nd1—O5—C574.7 (2)Nd1v—O4—C4—C3177.4 (3)
O3ii—Nd1—O5—C517.9 (3)Nd1iii—O3—C4—O4159.2 (4)
C4ii—Nd1—O5—C540.4 (3)Nd1v—O3—C4—O40.5 (3)
Nd1iv—Nd1—O5—C50.4 (2)Nd1iii—O3—C4—C322.8 (7)
O2i—Nd1—O6—C535.2 (2)Nd1v—O3—C4—C3177.4 (3)
O6i—Nd1—O6—C5129.7 (2)Nd1iii—O3—C4—Nd1v159.8 (6)
O3iii—Nd1—O6—C551.89 (19)C2—C3—C4—O4115.1 (4)
O1—Nd1—O6—C5120.8 (2)C2—C3—C4—O367.0 (4)
O5—Nd1—O6—C53.23 (19)Nd1—O5—C5—O65.9 (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—C615.7 (6)
Nd1iv—Nd1—O6—C5169.9 (2)Nd1—O6—C5—C6175.0 (3)
O2i—Nd1—O6—Nd1iv134.70 (11)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x, y+1, z1/2; (iii) x+1/2, y+3/2, z+1; (iv) x+1/2, y1/2, z+1/2; (v) x, y+1, z+1/2; (vi) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) 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: (i) x+1/2, y+1/2, z+1/2; (iv) x+1/2, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Nd2(C4H4O4)3(H2O)2]·H2O
Mr690.74
Crystal system, space groupMonoclinic, C2/c
Temperature (K)295
a, b, c (Å)19.966 (4), 7.8761 (9), 13.9861 (8)
β (°) 120.81 (1)
V3)1889.0 (5)
Z4
Radiation typeMo Kα
µ (mm1)5.51
Crystal size (mm)0.37 × 0.35 × 0.23
Data collection
DiffractometerSiemens P4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.194, 0.364
No. of measured, independent and
observed [I > 2σ(I)] reflections
2342, 1859, 1759
Rint0.019
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.066, 1.03
No. of reflections1859
No. of parameters132
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.71, 1.53

Computer programs: XSCANS (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).

Selected bond lengths (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, z1/2; (iii) x+1/2, y+3/2, z+1.
Hydrogen-bond geometry (Å, º) 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: (i) x+1/2, y+1/2, z+1/2; (iv) x+1/2, y1/2, z+1/2.
 

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