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In the crystal structure of the polymeric title compound, (C2H8N)[Eu(C2O4)2(H2O)]·3H2O, the independent oxalate that lies on a general position chelates to two Eu atoms, as do the other two oxalates that lie on different centres of inversion, the bridging mode of the oxalates giving rise to a three-dimensional anionic network. The water-coordinated Eu atom exists in a tricapped trigonal–prismatic geometry. The cations and solvent water mol­ecules occupy the cavities of the network and are involved in hydrogen bonding with each other and with the network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805027467/bt6728sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805027467/bt6728Isup2.hkl
Contains datablock I

CCDC reference: 287467

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.026
  • wR factor = 0.062
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N1 PLAT417_ALERT_2_B Short Inter D-H..H-D H1W2 .. H2W1 .. 2.08 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.55 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.56 Ang. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C3 - C3_c ... 1.54 Ang. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C4 - C4_d ... 1.55 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O2W -H2W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H3W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat O3W -H3W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O4W -H4W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O4W -H4W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat N1 -H1N1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Rat N1 -H1N2 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 111(5), Rep 111(2) ...... 2.50 su-Rat H2W1 -O2W -H2W2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 111(5), Rep 111(2) ...... 2.50 su-Rat H3W1 -O3W -H3W2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(5), Rep 109(2) ...... 2.50 su-Rat H4W1 -O4W -H4W2 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O3W -H5# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat O3W -H6# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O4W -H7# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat O4W -H8# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat N1 -H9# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.850(10) ...... 4.00 su-Rat N1 -H10# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.92(3), Rep 1.920(10) ...... 3.00 su-Rat H1# -O2W 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.12(4), Rep 2.120(10) ...... 4.00 su-Rat H8# -O3 1.555 2.545 PLAT736_ALERT_1_C H...A Calc 1.96(3), Rep 1.960(10) ...... 3.00 su-Rat H9# -O3W 1.555 1.555
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 29 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 24 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

Some rare earth/monovalent-cation oxalates contain water, and the compounds that are formulated as [M][(C2O4)2La].nH2O have been studied in order to understand the nature of the water molecules, as water is crucial to their applications. Such double oxalates have been structurally authenticated by both single-crystal and powder-diffraction methods; the ammonium derivative is a monohydrate, and the water molecule is involved in coordination to the Y atom in [NH4][(C2O4)2(H2O)Y] (MacDonald & Spink, 1967). The nine-coordinate metal atom displays capped trigonal–prismatic coordination. The caesium analogue also has the rare earth atom in such a geometry (Bataille et al., 2000), as does the trihydrated sodium salt (Bataille & Louër, 1999). Another aquadioxalatoyttrate, a propyl-1,2-diammonium salt, has two solvent water molecules that interact with the cation (Vaidhyanathan et al., 2001). Double salts with other nine-coordinate water-coordinated rare earths include the erbium (Steinfink & Brunton, 1970), lanthanum (Fourcade-Cavillou & Trombe, 2002), neodymium (Fourcade-Cavillou & Trombe, 2002; Kahwa et al., 1984), samarium, europium, gadolinium and terbium (Kahwa et al., 1984) complexes.

The title dimethylammonium aquadioxalatoeuropate(III) exists as the trihydrate, (I) (Fig. 1). The Eu atom is surrounded by the eight atoms of four oxalates and the water molecule in a capped trigonal–prismatic environment (Fig. 2). The cations and solvent water molecules interact with each other along the channels of the polymeric anion (Fig. 3); extensive hydrogen bonds (Table 2) give rise to a tightly held network structure that has no solvent-accessible cavities.

Experimental top

A mixture of dieuropium trioxalate xhydrate (0.012 g, 0.02 mmol), 1,3,5-benzenetricarboxylic acid (0.011 g, 0.05 mmol) and water (4 ml) was heated to 333 K, and to this mixture was added di-n-propylethylamine (0.04 g, 0.05 mmol). The solution was placed in a Teflon-lined Parr bomb, which was heated to 453 K for 48 h. It was cooled at a rate of 5 K h−1 to 333 K to yield colourless crystals of (I). As benzenetricarboxylic acid was not incorporated into the product, the reaction is essentially between dieuropium trixoxalate and dipropylethylamine; the dimethylammonium cation in the product probably results from the decomposition of dipropylethylamine.

Refinement top

The C-bound H atoms were placed in calculated positions, with C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C), and were included in the refinement in the riding-model approximation. Water and ammonium H atoms were located in difference Fourier maps, and were refined with distance restraints of O—H = N—H = 0.85 (1) Å and H···H = 1.39 (1) Å and with Uiso(H) = 1.2Ueq(O,N). The short H1W2···H2W1 distance of 2.08 Å is probably a consequence of some disorder in atom O2W, but the disorder could not be resolved. The largest peak in the final difference Fourier map of 1.08 e Å−3 was about 1 Å from Eu1.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of a portion of the three-dimensional motif, showing the geometry of the Eu atom in polymeric (I). Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) 3/2 − x, y − 1/2, 1/2 − z; (ii) 1 − x, 1 − y, 1 − z; (iii) 2 − x, 1 − y, 1 − z.]
[Figure 2] Fig. 2. The trigonal–prismatic geometry of the Eu atom in (I).
[Figure 3] Fig. 3. A view of the polymeric [(C2O4)2(H2O)Eu] network in (I).
Poly[dimethylammonium aquadi-µ-oxalato-europate(III) trihydrate] top
Crystal data top
(C2H8N)[Eu(C2O4)2(H2O)]·3H2OF(000) = 872
Mr = 446.16Dx = 2.143 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 885 reflections
a = 9.674 (1) Åθ = 2.4–27.2°
b = 11.761 (1) ŵ = 4.60 mm1
c = 12.315 (2) ÅT = 295 K
β = 99.285 (2)°Block, colourless
V = 1382.8 (3) Å30.06 × 0.05 × 0.05 mm
Z = 4
Data collection top
Bruker SMART 1000 area-detector
diffractometer
3113 independent reflections
Radiation source: fine-focus sealed tube2578 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ϕ and ω scansθmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 127
Tmin = 0.702, Tmax = 0.803k = 1514
8455 measured reflectionsl = 1515
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)] = 0.026Hydrogen site location: difference Fourier map
wR(F2) = 0.062H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0359P)2]
where P = (Fo2 + 2Fc2)/3
3113 reflections(Δ/σ)max = 0.001
212 parametersΔρmax = 1.07 e Å3
15 restraintsΔρmin = 0.42 e Å3
Crystal data top
(C2H8N)[Eu(C2O4)2(H2O)]·3H2OV = 1382.8 (3) Å3
Mr = 446.16Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.674 (1) ŵ = 4.60 mm1
b = 11.761 (1) ÅT = 295 K
c = 12.315 (2) Å0.06 × 0.05 × 0.05 mm
β = 99.285 (2)°
Data collection top
Bruker SMART 1000 area-detector
diffractometer
3113 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2578 reflections with I > 2σ(I)
Tmin = 0.702, Tmax = 0.803Rint = 0.026
8455 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02615 restraints
wR(F2) = 0.062H atoms treated by a mixture of independent and constrained refinement
S = 0.99Δρmax = 1.07 e Å3
3113 reflectionsΔρmin = 0.42 e Å3
212 parameters
Special details top

Experimental. A dimensionless value of 2r*µ = 0.30 was used in the SADABS step.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Eu10.71368 (2)0.51552 (1)0.33081 (1)0.02102 (7)
O10.8070 (3)0.6409 (2)0.2055 (2)0.0272 (6)
O20.8660 (3)0.8194 (2)0.1726 (2)0.0253 (6)
O30.6396 (3)0.7159 (2)0.3435 (2)0.0288 (6)
O40.6851 (3)0.8950 (2)0.3006 (2)0.0318 (6)
O50.6813 (3)0.5115 (2)0.5224 (2)0.0305 (6)
O60.5335 (3)0.4854 (2)0.6428 (2)0.0263 (6)
O70.9160 (3)0.6182 (2)0.4341 (2)0.0306 (6)
O81.1006 (3)0.6088 (2)0.5673 (2)0.0347 (7)
O1W0.5452 (3)0.5236 (3)0.1537 (2)0.0374 (7)
O2W0.4196 (5)0.3424 (3)0.0340 (3)0.066 (1)
O3W0.1705 (6)0.5038 (4)0.0076 (3)0.079 (1)
O4W0.0859 (5)0.2816 (4)0.0322 (4)0.077 (1)
N10.2682 (5)0.6312 (4)0.1956 (4)0.051 (1)
C10.8002 (4)0.7455 (3)0.2175 (3)0.0220 (7)
C20.6990 (4)0.7897 (3)0.2946 (3)0.0225 (8)
C30.5625 (4)0.4992 (3)0.5474 (3)0.0219 (7)
C41.0046 (4)0.5657 (3)0.4997 (3)0.0256 (8)
C50.1511 (7)0.6242 (7)0.2548 (5)0.084 (2)
C60.3064 (8)0.7458 (6)0.1680 (5)0.087 (2)
H1W10.514 (5)0.462 (2)0.122 (3)0.045*
H1W20.572 (4)0.568 (2)0.107 (2)0.045*
H2W10.334 (2)0.355 (4)0.014 (5)0.079*
H2W20.435 (5)0.273 (1)0.046 (5)0.079*
H3W10.160 (6)0.543 (4)0.051 (3)0.095*
H3W20.121 (6)0.445 (3)0.001 (5)0.095*
H4W10.077 (6)0.253 (5)0.032 (2)0.093*
H4W20.017 (4)0.262 (5)0.063 (4)0.093*
H1N10.252 (5)0.589 (3)0.139 (2)0.061*
H1N20.338 (4)0.605 (4)0.240 (3)0.061*
H5A0.17560.65990.32540.127*
H5B0.12830.54590.26460.127*
H5C0.07170.66230.21370.127*
H6A0.22600.78350.12800.130*
H6B0.37920.74240.12360.130*
H6C0.33940.78710.23440.130*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu10.0240 (1)0.0177 (1)0.0222 (1)0.0001 (1)0.0063 (1)0.0002 (1)
O10.039 (2)0.016 (1)0.030 (1)0.001 (1)0.015 (1)0.001 (1)
O20.024 (2)0.021 (1)0.033 (2)0.001 (1)0.010 (1)0.004 (1)
O30.035 (2)0.021 (1)0.035 (2)0.001 (1)0.019 (1)0.003 (1)
O40.048 (2)0.018 (1)0.034 (2)0.001 (1)0.020 (1)0.001 (1)
O50.023 (1)0.043 (2)0.026 (1)0.003 (1)0.005 (1)0.001 (1)
O60.025 (1)0.034 (1)0.020 (1)0.002 (1)0.004 (1)0.002 (1)
O70.032 (2)0.023 (1)0.036 (2)0.003 (1)0.001 (1)0.007 (1)
O80.032 (2)0.023 (1)0.045 (2)0.002 (1)0.006 (1)0.007 (1)
O1W0.043 (2)0.042 (2)0.028 (2)0.006 (1)0.005 (1)0.001 (1)
O2W0.093 (3)0.038 (2)0.068 (3)0.000 (2)0.010 (2)0.007 (2)
O3W0.124 (4)0.073 (3)0.045 (2)0.021 (3)0.023 (3)0.002 (2)
O4W0.113 (4)0.059 (3)0.072 (3)0.018 (2)0.051 (3)0.013 (2)
N10.043 (3)0.065 (3)0.046 (3)0.019 (2)0.011 (2)0.011 (2)
C10.024 (2)0.024 (2)0.018 (2)0.000 (1)0.002 (2)0.002 (1)
C20.025 (2)0.021 (2)0.021 (2)0.002 (1)0.004 (2)0.000 (1)
C30.026 (2)0.017 (2)0.023 (2)0.001 (1)0.005 (2)0.000 (1)
C40.024 (2)0.027 (2)0.027 (2)0.001 (2)0.009 (2)0.002 (2)
C50.061 (4)0.136 (7)0.060 (4)0.029 (4)0.019 (3)0.019 (4)
C60.098 (6)0.063 (4)0.097 (5)0.002 (4)0.007 (4)0.019 (4)
Geometric parameters (Å, º) top
Eu1—O12.412 (2)C1—C21.560 (5)
Eu1—O2i2.430 (2)C3—C3ii1.540 (7)
Eu1—O32.476 (2)C4—C4iii1.547 (8)
Eu1—O4i2.469 (2)O1W—H1W10.85 (1)
Eu1—O52.430 (3)O1W—H1W20.85 (1)
Eu1—O6ii2.465 (3)O2W—H2W10.84 (1)
Eu1—O72.471 (3)O2W—H2W20.85 (1)
Eu1—O8iii2.492 (3)O3W—H3W10.85 (1)
Eu1—O1W2.505 (3)O3W—H3W20.84 (1)
O1—C11.242 (4)O4W—H4W10.85 (1)
O2—C11.257 (4)O4W—H4W20.85 (1)
O3—C21.247 (4)N1—H1N10.85 (1)
O4—C21.249 (4)N1—H1N20.85 (1)
O5—C31.245 (4)C5—H5A0.96
O6—C31.261 (4)C5—H5B0.96
O7—C41.244 (4)C5—H5C0.96
O8—C41.250 (4)C6—H6A0.96
N1—C51.445 (7)C6—H6B0.96
N1—C61.452 (8)C6—H6C0.96
O1—Eu1—O2i136.0 (1)C3—O5—Eu1120.8 (2)
O1—Eu1—O366.4 (1)C3—O6—Eu1ii119.3 (2)
O1—Eu1—O4i72.7 (1)C4—O7—Eu1119.8 (2)
O1—Eu1—O5138.9 (1)C4—O8—Eu1iii119.7 (2)
O1—Eu1—O6ii123.9 (1)C5—N1—C6114.9 (5)
O1—Eu1—O771.5 (1)O1—C1—O2126.4 (3)
O1—Eu1—O8iii111.5 (1)O1—C1—C2116.9 (3)
O1—Eu1—O1W71.2 (1)O2—C1—C2116.7 (3)
O2i—Eu1—O3144.2 (1)O3—C2—O4126.8 (3)
O2i—Eu1—O4i66.5 (1)O3—C2—C1116.4 (3)
O2i—Eu1—O584.7 (1)O4—C2—C1116.7 (3)
O2i—Eu1—O6ii71.7 (1)O5—C3—O6126.8 (3)
O2i—Eu1—O7134.1 (1)O5—C3—C3ii117.0 (4)
O2i—Eu1—O8iii69.7 (1)O6—C3—C3ii116.3 (4)
O2i—Eu1—O1W82.0 (1)O7—C4—O8126.2 (4)
O3—Eu1—O4i137.5 (1)O7—C4—C4iii117.7 (4)
O3—Eu1—O582.7 (1)O8—C4—C4iii116.1 (4)
O3—Eu1—O6ii72.5 (1)Eu1—O1W—H1W1120 (3)
O3—Eu1—O773.5 (1)Eu1—O1W—H1W2113 (3)
O3—Eu1—O8iii136.0 (1)H1W1—O1W—H1W2110 (2)
O3—Eu1—O1W82.2 (1)H2W1—O2W—H2W2111 (2)
O4i—Eu1—O5138.7 (1)H3W1—O3W—H3W2111 (2)
O4i—Eu1—O6ii125.4 (1)H4W1—O4W—H4W2109 (2)
O4i—Eu1—O7104.7 (1)C5—N1—H1N1109 (4)
O4i—Eu1—O8iii70.3 (1)C6—N1—H1N1112 (4)
O4i—Eu1—O1W73.9 (1)C5—N1—H1N2105 (4)
O5—Eu1—O6ii65.9 (1)C6—N1—H1N2106 (4)
O5—Eu1—O774.1 (1)H1N1—N1—H1N2110 (2)
O5—Eu1—O8iii72.3 (1)N1—C5—H5A109.5
O5—Eu1—O1W132.7 (1)N1—C5—H5B109.5
O6ii—Eu1—O7129.7 (1)H5A—C5—H5B109.5
O6ii—Eu1—O8iii124.5 (1)N1—C5—H5C109.5
O6ii—Eu1—O1W66.8 (1)H5A—C5—H5C109.5
O7—Eu1—O8iii65.2 (1)H5B—C5—H5C109.5
O7—Eu1—O1W141.2 (1)N1—C6—H6A109.5
O8iii—Eu1—O1W140.9 (1)N1—C6—H6B109.5
C1—O1—Eu1119.8 (2)H6A—C6—H6B109.5
C1—O2—Eu1iv118.9 (2)N1—C6—H6C109.5
C2—O3—Eu1118.1 (2)H6A—C6—H6C109.5
C2—O4—Eu1iv118.3 (2)H6B—C6—H6C109.5
O5—Eu1—O1—C131.3 (3)O6ii—Eu1—O7—C4105.3 (3)
O2i—Eu1—O1—C1158.8 (2)O4i—Eu1—O7—C469.8 (3)
O6ii—Eu1—O1—C160.0 (3)O3—Eu1—O7—C4154.4 (3)
O4i—Eu1—O1—C1178.5 (3)O8iii—Eu1—O7—C410.0 (3)
O7—Eu1—O1—C165.9 (3)O1W—Eu1—O7—C4152.2 (2)
O3—Eu1—O1—C113.6 (3)Eu1—O1—C1—O2165.9 (3)
O8iii—Eu1—O1—C1118.6 (3)Eu1—O1—C1—C214.9 (4)
O1W—Eu1—O1—C1103.1 (3)Eu1iv—O2—C1—O1163.0 (3)
O1—Eu1—O3—C210.8 (3)Eu1iv—O2—C1—C216.2 (4)
O5—Eu1—O3—C2141.3 (3)Eu1—O3—C2—O4172.5 (3)
O2i—Eu1—O3—C2148.2 (2)Eu1—O3—C2—C17.9 (4)
O6ii—Eu1—O3—C2151.7 (3)Eu1iv—O4—C2—O3169.7 (3)
O4i—Eu1—O3—C227.9 (3)Eu1iv—O4—C2—C19.9 (4)
O7—Eu1—O3—C265.9 (3)O1—C1—C2—O34.4 (5)
O8iii—Eu1—O3—C286.4 (3)O2—C1—C2—O3176.3 (3)
O1W—Eu1—O3—C283.6 (3)Eu1iv—C1—C2—O3172.8 (3)
O1—Eu1—O5—C3122.0 (2)O1—C1—C2—O4175.2 (3)
O2i—Eu1—O5—C365.0 (3)O2—C1—C2—O44.1 (5)
O6ii—Eu1—O5—C37.3 (2)Eu1iv—C1—C2—O46.8 (3)
O4i—Eu1—O5—C3109.7 (3)Eu1—O5—C3—O6173.0 (3)
O7—Eu1—O5—C3156.1 (3)Eu1—O5—C3—C3ii6.8 (5)
O3—Eu1—O5—C381.3 (3)Eu1ii—O6—C3—O5173.3 (3)
O8iii—Eu1—O5—C3135.4 (3)Eu1ii—O6—C3—C3ii6.8 (5)
O1W—Eu1—O5—C39.0 (3)Eu1—O7—C4—O8169.8 (3)
O1—Eu1—O7—C4135.5 (3)Eu1—O7—C4—C4iii9.1 (5)
O5—Eu1—O7—C467.4 (3)Eu1iii—O8—C4—O7170.6 (3)
O2i—Eu1—O7—C41.6 (3)Eu1iii—O8—C4—C4iii10.4 (5)
Symmetry codes: (i) x+3/2, y1/2, z+1/2; (ii) x+1, y+1, z+1; (iii) x+2, y+1, z+1; (iv) x+3/2, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2W0.85 (1)1.92 (1)2.759 (5)169 (4)
O1W—H1W2···O2Wv0.85 (1)2.05 (2)2.862 (5)162 (4)
O2W—H2W2···O7i0.85 (1)2.30 (2)3.071 (5)151 (4)
O2W—H2W2···O8i0.85 (1)2.37 (4)3.011 (4)133 (5)
O3W—H3W1···O4vi0.85 (1)2.02 (2)2.838 (5)162 (7)
O3W—H3W2···O4W0.84 (1)2.00 (3)2.770 (6)151 (5)
O4W—H4W1···O2v0.85 (1)2.08 (2)2.893 (4)159 (5)
O4W—H4W2···O3vii0.85 (1)2.12 (1)2.962 (5)173 (5)
N1—H1N1···O3W0.85 (1)1.96 (1)2.792 (6)167 (4)
N1—H1N2···O6ii0.85 (1)2.05 (2)2.879 (5)165 (5)
Symmetry codes: (i) x+3/2, y1/2, z+1/2; (ii) x+1, y+1, z+1; (v) x+1, y+1, z; (vi) x1/2, y+3/2, z1/2; (vii) x+1/2, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula(C2H8N)[Eu(C2O4)2(H2O)]·3H2O
Mr446.16
Crystal system, space groupMonoclinic, P21/n
Temperature (K)295
a, b, c (Å)9.674 (1), 11.761 (1), 12.315 (2)
β (°) 99.285 (2)
V3)1382.8 (3)
Z4
Radiation typeMo Kα
µ (mm1)4.60
Crystal size (mm)0.06 × 0.05 × 0.05
Data collection
DiffractometerBruker SMART 1000 area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.702, 0.803
No. of measured, independent and
observed [I > 2σ(I)] reflections
8455, 3113, 2578
Rint0.026
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.062, 0.99
No. of reflections3113
No. of parameters212
No. of restraints15
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.07, 0.42

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Eu1—O12.412 (2)Eu1—O6ii2.465 (3)
Eu1—O2i2.430 (2)Eu1—O72.471 (3)
Eu1—O32.476 (2)Eu1—O8iii2.492 (3)
Eu1—O4i2.469 (2)Eu1—O1W2.505 (3)
Eu1—O52.430 (3)
O1—Eu1—O2i136.0 (1)O3—Eu1—O773.5 (1)
O1—Eu1—O366.4 (1)O3—Eu1—O8iii136.0 (1)
O1—Eu1—O4i72.7 (1)O3—Eu1—O1W82.2 (1)
O1—Eu1—O5138.9 (1)O4i—Eu1—O5138.7 (1)
O1—Eu1—O6ii123.9 (1)O4i—Eu1—O6ii125.4 (1)
O1—Eu1—O771.5 (1)O4i—Eu1—O7104.7 (1)
O1—Eu1—O8iii111.5 (1)O4i—Eu1—O8iii70.3 (1)
O1—Eu1—O1W71.2 (1)O4i—Eu1—O1W73.9 (1)
O2i—Eu1—O3144.2 (1)O5—Eu1—O6ii65.9 (1)
O2i—Eu1—O4i66.5 (1)O5—Eu1—O774.1 (1)
O2i—Eu1—O584.7 (1)O5—Eu1—O8iii72.3 (1)
O2i—Eu1—O6ii71.7 (1)O5—Eu1—O1W132.7 (1)
O2i—Eu1—O7134.1 (1)O6ii—Eu1—O7129.7 (1)
O2i—Eu1—O8iii69.7 (1)O6ii—Eu1—O8iii124.5 (1)
O2i—Eu1—O1W82.0 (1)O6ii—Eu1—O1W66.8 (1)
O3—Eu1—O4i137.5 (1)O7—Eu1—O8iii65.2 (1)
O3—Eu1—O582.7 (1)O7—Eu1—O1W141.2 (1)
O3—Eu1—O6ii72.5 (1)O8iii—Eu1—O1W140.9 (1)
Symmetry codes: (i) x+3/2, y1/2, z+1/2; (ii) x+1, y+1, z+1; (iii) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2W0.85 (1)1.92 (1)2.759 (5)169 (4)
O1W—H1W2···O2Wiv0.85 (1)2.05 (2)2.862 (5)162 (4)
O2W—H2W2···O7i0.85 (1)2.30 (2)3.071 (5)151 (4)
O2W—H2W2···O8i0.85 (1)2.37 (4)3.011 (4)133 (5)
O3W—H3W1···O4v0.85 (1)2.02 (2)2.838 (5)162 (7)
O3W—H3W2···O4W0.84 (1)2.00 (3)2.770 (6)151 (5)
O4W—H4W1···O2iv0.85 (1)2.08 (2)2.893 (4)159 (5)
O4W—H4W2···O3vi0.85 (1)2.12 (1)2.962 (5)173 (5)
N1—H1N1···O3W0.85 (1)1.96 (1)2.792 (6)167 (4)
N1—H1N2···O6ii0.85 (1)2.05 (2)2.879 (5)165 (5)
Symmetry codes: (i) x+3/2, y1/2, z+1/2; (ii) x+1, y+1, z+1; (iv) x+1, y+1, z; (v) x1/2, y+3/2, z1/2; (vi) x+1/2, y1/2, z+1/2.
 

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