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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 5| May 2010| Page m575
https://doi.org/10.1107/S1600536810014200

Redetermination of di-μ-hydrido-hexa­hydrido­tetra­kis(tetra­hydro­furan)dialuminium(III)magnesium(II)

Hima Kumar Lingam,a Xuenian Chen,b Teshome Yisgedu,a Zhenguo Huang,a Ji-Cheng Zhaoa* and Sheldon G. Shoreb

aDepartment of Materials Science and Engineering, The Ohio State University, Columbus, OH 43210, USA, and bDepartment of Chemistry, The Ohio State University, Columbus, OH 43210, USA
*Correspondence e-mail: zhao.199@osu.edu

(Received 23 February 2010; accepted 18 April 2010; online 28 April 2010)

The structure of the title compound, [Mg(AlH4)2(C4H8O)4], has been redetermined at 150 K. The MgII ion is hexa­coordinated to four tetra­hydro­furan (THF) ligands, and two AlH4− anions through bridging H atoms. The Al—H distances are more precise compared to those previously determined [Nöth et al. (1995[Nöth, H., Schmidt, M. & Treitl, A. (1995). Chem. Ber. 128, 999-1006.]). Chem. Ber. 128, 999–1006; Fichtner & Fuhr (2002[Fichtner, M. & Fuhr, O. (2002). J. Alloys Compd, 345, 286-296.]). J. Alloys Compd, 345, 386–396]. The mol­ecule has twofold rotation symmetry.

Related literature

For the synthesis of Mg(AlH4)2·4THF, see: Ashby et al. (1970[Ashby, E. C., Schwartz, R. D. & James, B. D. (1970). Inorg. Chem. 9, 325-332.]); Shen & Che (1991[Shen, P. & Che, Y. (1991). Faming ZhuanliShenqing Gongkai Shuomingshu, CN1051179, p. 7.]); Nöth et al. (1995[Nöth, H., Schmidt, M. & Treitl, A. (1995). Chem. Ber. 128, 999-1006.]). For the synthesis of AlH4MgBH4, see: Ashby & Goel (1977[Ashby, E. C. & Goel, A. B. (1977). Inorg. Chem. 16, 2082-2085.]). For previous determinations of the crystal structure of Mg(AlH4)2·4THF, see: Noth et al. (1995[Nöth, H., Schmidt, M. & Treitl, A. (1995). Chem. Ber. 128, 999-1006.]); Fichtner & Fuhr (2002[Fichtner, M. & Fuhr, O. (2002). J. Alloys Compd, 345, 286-296.]). For the thermal decomposition properties of Mg(AlH4)2·4THF, see: Dilts & Ashby (1972[Dilts, J. A. & Ashby, E. C. (1972). Inorg. Chem. 11, 1230-1236.]). For other alanate structures, see: Sklar & Post (1967[Sklar, N. & Post, B. (1967). Inorg. Chem. 6, 669-671.]); Lauher et al. (1979[Lauher, J. W., Dougherty, D. & Herley, P. J. (1979). Acta Cryst. B35, 1454-1456.]); Fichtner & Fuhr (2002[Fichtner, M. & Fuhr, O. (2002). J. Alloys Compd, 345, 286-296.]); Fichtner et al. (2004[Fichtner, M., Frommen, C. & Fuhr, O. (2004). Inorg. Chem. 44, 3479-3484.]).

[Scheme 1]

Experimental

Crystal data

  • [Al2MgH8(C4H8O)4]

  • Mr = 374.75

  • Orthorhombic, P c n b

  • a = 10.161 (2) Å

  • b = 14.027 (3) Å

  • c = 16.429 (3) Å

  • V = 2341.6 (8) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.16 mm−1

  • T = 150 K

  • 0.38 × 0.31 × 0.19 mm
Data collection

  • Nonius Kappa CCD diffractometer

  • Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) Tmin = 0.940, Tmax = 0.969

  • 5018 measured reflections

  • 2687 independent reflections

  • 1973 reflections with I > 2σ(I)

  • Rint = 0.017
Refinement

  • R[F2 > 2σ(F2)] = 0.041

  • wR(F2) = 0.119

  • S = 1.07

  • 2687 reflections

  • 122 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.30 e Å−3

  • Δρmin = −0.30 e Å−3

Data collection: COLLECT (Nonius, 1998[Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: SCALEPACK (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: DENZO (Otwinowski & Minor 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810014200/ci5044sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810014200/ci5044Isup2.hkl

checkCIF report


Comment top

Mg(AlH4)2.4THF, (I), is a starting material for the synthesis of Mg(AlH4)2 which is an interesting candidate for hydrogen storage applications because of its high theoretical hydrogen storage capacity. Ashby et al. (1970) reported the synthesis of (I) by the metathesis reaction between NaAlH4 and MgCl2. Noth et al. (1995) and recently Fichtner & Fuhr (2002) reported the crystal structure of (I), but neither of the groups obtained high quality single crystal X-ray diffraction data. In the present work good quality single crystals were obtained from reaction between NaAlH4 and ClMgBH4 where the product, AlH4MgBH4.THF disproportionated to form (I). The crystal structure was determined using single crystal X-ray diffraction and compared with the previously reported data.

In general, the present crystal structure determination confirms the previous results. As previously described by Noth et al. (1995) and Fichtner & Fuhr (2002), the structure of (I) consists of discrete octahedral building blocks where four THF molecules and two tetrahedral AlH4– units are connected to a Mg central atom. Fichtner & Fuhr (2002) reported only lattice parameters without coordinates of the atoms. Noth et al. (1995) reported the Al—H(t) and Al—H(b) bond lengths as 1.214 and 1.528 Å, respectively, which are shorter than expected. Moreover, the structure was only refined to a final R value of 0.065. We have redetermined this crystal structure at 150 K, with a final R value of 0.040 to obtain more precise data. In the present work, the Al—H(t) and Al—H(b) bond lengths were found to be 1.524 and 1.573 Å, respectively, which are close to the Al—H bond distance in other alanates. Al—H distances reported in other alanates with AlH4– tetrahedral are 1.547 Å (at 8 K) for LiAlH4 (Sklar & Post, 1967), 1.532 Å (at 296 K) for NaAlH4 (Lauher et al., 1979), 1.55 Å (at 200 K) for Mg(AlH4)2.Et2O (Fichtner & Fuhr, 2002) and 1.65 Å (at 230 K) for Ca(AlH4)2.4THF (Fichtner et al., 2004).

Related literature top

For the synthesis of Mg(AlH4)2.4THF, see: Ashby et al. (1970); Shen et al. (1991); Noth et al. (1995). For the synthesis of AlH4.MgBH4, see: Ashby & Goel (1977). For the crystal structue of Mg(AlH4)2.4THF, see: Noth et al. (1995); Fichtner & Fuhr (2002). For the thermal decomposition properties of Mg(AlH4)2.4THF, see: Dilts & Ashby (1972). For other alanate structures, see: Sklar & Post (1967); Lauher et al. (1979); Fichtner & Fuhr (2002); Fichtner et al. (2004).

Experimental top

All the manipulations were carried out in high vacuum lines and an Ar filled glove box to avoid the compounds reacting with oxygen and moisture. Solvents were dried by vacuum distillation from sodium benzophenone ketyl. Precursor ClMgBH4 was synthesized by ball milling MgCl2 and Mg(BH4)2 in 1:1 mole ratio in a high energy ball mill for 1 h. AlH4MgBH4 was prepared by the procedure reported by Ashby & Goel (1977). In a typical procedure, a clear solution of NaAlH4 in THF was added to a solution of ClMgBH4 in THF with rapid stirring for 60 min at room temperature. After completion of reaction, NaCl was filtered out from the solution and the solvent was removed from the filtrate under dynamic vacuum. The obtained AlH4MgBH4.THF powder was dissolved in benzene, filtered, concentrated, and aged for 2 days. AlH4MgBH4.THF slowly disproportionated to give colourless crystals of (I).

Refinement top

H atoms bonded to aluminium atoms were located and refined isotropically. The range of refined Al–H distances is 1.50 (2)–1.573 (18) Å. The remaining H atoms were placed in calculated positions [C–H = 0.99 Å] and refined using a rigid model with Uiso(H) = 1.2Ueq(C).

Structure description top

Mg(AlH4)2.4THF, (I), is a starting material for the synthesis of Mg(AlH4)2 which is an interesting candidate for hydrogen storage applications because of its high theoretical hydrogen storage capacity. Ashby et al. (1970) reported the synthesis of (I) by the metathesis reaction between NaAlH4 and MgCl2. Noth et al. (1995) and recently Fichtner & Fuhr (2002) reported the crystal structure of (I), but neither of the groups obtained high quality single crystal X-ray diffraction data. In the present work good quality single crystals were obtained from reaction between NaAlH4 and ClMgBH4 where the product, AlH4MgBH4.THF disproportionated to form (I). The crystal structure was determined using single crystal X-ray diffraction and compared with the previously reported data.

In general, the present crystal structure determination confirms the previous results. As previously described by Noth et al. (1995) and Fichtner & Fuhr (2002), the structure of (I) consists of discrete octahedral building blocks where four THF molecules and two tetrahedral AlH4– units are connected to a Mg central atom. Fichtner & Fuhr (2002) reported only lattice parameters without coordinates of the atoms. Noth et al. (1995) reported the Al—H(t) and Al—H(b) bond lengths as 1.214 and 1.528 Å, respectively, which are shorter than expected. Moreover, the structure was only refined to a final R value of 0.065. We have redetermined this crystal structure at 150 K, with a final R value of 0.040 to obtain more precise data. In the present work, the Al—H(t) and Al—H(b) bond lengths were found to be 1.524 and 1.573 Å, respectively, which are close to the Al—H bond distance in other alanates. Al—H distances reported in other alanates with AlH4– tetrahedral are 1.547 Å (at 8 K) for LiAlH4 (Sklar & Post, 1967), 1.532 Å (at 296 K) for NaAlH4 (Lauher et al., 1979), 1.55 Å (at 200 K) for Mg(AlH4)2.Et2O (Fichtner & Fuhr, 2002) and 1.65 Å (at 230 K) for Ca(AlH4)2.4THF (Fichtner et al., 2004).

For the synthesis of Mg(AlH4)2.4THF, see: Ashby et al. (1970); Shen et al. (1991); Noth et al. (1995). For the synthesis of AlH4.MgBH4, see: Ashby & Goel (1977). For the crystal structue of Mg(AlH4)2.4THF, see: Noth et al. (1995); Fichtner & Fuhr (2002). For the thermal decomposition properties of Mg(AlH4)2.4THF, see: Dilts & Ashby (1972). For other alanate structures, see: Sklar & Post (1967); Lauher et al. (1979); Fichtner & Fuhr (2002); Fichtner et al. (2004).

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor 1997) and SCALEPACK; 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 molecular structure of [Mg(AlH4)2(C4H8O)4], showing 50% probability displacement ellipsoids and the atomic numbering scheme. Atoms labelled with the suffix A are generated by the symmetry operation (-x, 1/2-y, z).
Di-µ-hydrido-hexahydridotetrakis(tetrahydrofuran)dialuminium(III)magnesium(II) top
Crystal data top
[Al2MgH8(C4H8O)4]F(000) = 824
Mr = 374.75Dx = 1.063 Mg m−3
Orthorhombic, PcnbMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2b 2acCell parameters from 2687 reflections
a = 10.161 (2) Åθ = 2.4–27.5°
b = 14.027 (3) ŵ = 0.16 mm−1
c = 16.429 (3) ÅT = 150 K
V = 2341.6 (8) Å3Cube, colourless
Z = 40.38 × 0.31 × 0.19 mm
Data collection top
Nonius Kappa CCD
diffractometer		2687 independent reflections
Radiation source: fine-focus sealed tube1973 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)		h = −13→13
Tmin = 0.940, Tmax = 0.969k = −18→18
5018 measured reflectionsl = −21→21
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.119H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0615P)2 + 0.6568P]
where P = (Fo2 + 2Fc2)/3
2687 reflections(Δ/σ)max = 0.001
122 parametersΔρmax = 0.30 e Å−3
0 restraintsΔρmin = −0.30 e Å−3
Crystal data top
[Al2MgH8(C4H8O)4]V = 2341.6 (8) Å3
Mr = 374.75Z = 4
Orthorhombic, PcnbMo Kα radiation
a = 10.161 (2) ŵ = 0.16 mm−1
b = 14.027 (3) ÅT = 150 K
c = 16.429 (3) Å0.38 × 0.31 × 0.19 mm
Data collection top
Nonius Kappa CCD
diffractometer		2687 independent reflections
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)		1973 reflections with I > 2σ(I)
Tmin = 0.940, Tmax = 0.969Rint = 0.017
5018 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.119H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 0.30 e Å−3
2687 reflectionsΔρmin = −0.30 e Å−3
122 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Al10.22387 (5)0.44321 (4)0.13620 (3)0.03294 (17)
Mg10.00000.25000.13728 (4)0.02116 (19)
O10.16625 (10)0.16699 (8)0.13767 (6)0.0298 (3)
O30.00000.25000.01068 (8)0.0269 (3)
O20.00000.25000.26391 (8)0.0270 (3)
C8−0.06993 (19)0.23112 (14)−0.12525 (9)0.0429 (5)
H8A−0.13410.2828−0.13560.052*
H8B−0.08150.1806−0.16670.052*
C40.27768 (17)0.17950 (14)0.19205 (12)0.0439 (5)
H4A0.25880.15150.24610.053*
H4B0.29820.24800.19910.053*
C50.02463 (19)0.33286 (12)0.31515 (9)0.0370 (4)
H5A−0.02850.38800.29670.044*
H5B0.11890.35070.31360.044*
C7−0.08466 (18)0.19178 (13)−0.04047 (9)0.0382 (4)
H7A−0.17730.1962−0.02220.046*
H7B−0.05700.1242−0.03860.046*
C6−0.0151 (2)0.30305 (13)0.39968 (10)0.0445 (5)
H6A−0.10980.31510.40940.053*
H6B0.03730.33700.44150.053*
C20.3257 (2)0.05289 (16)0.10336 (13)0.0573 (6)
H2A0.37810.03960.05380.069*
H2B0.3177−0.00660.13540.069*
C30.3878 (2)0.1296 (2)0.15261 (16)0.0763 (8)
H3A0.44800.10220.19380.092*
H3B0.43820.17370.11740.092*
C10.1945 (2)0.09039 (16)0.08170 (14)0.0587 (6)
H1A0.19450.11430.02500.070*
H1B0.12720.03960.08650.070*
H10.1142 (17)0.3641 (12)0.1382 (9)0.034 (5)*
H20.2892 (19)0.4426 (13)0.2215 (13)0.055 (6)*
H30.3167 (19)0.4126 (16)0.0687 (13)0.063 (6)*
H40.156 (2)0.5361 (18)0.1206 (14)0.076 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.0350 (3)0.0315 (3)0.0323 (3)−0.0085 (2)−0.0024 (2)0.0047 (2)
Mg10.0227 (4)0.0223 (4)0.0184 (3)0.0009 (3)0.0000.000
O10.0284 (6)0.0313 (6)0.0297 (6)0.0073 (5)−0.0075 (4)−0.0111 (4)
O30.0292 (8)0.0336 (8)0.0178 (7)−0.0037 (6)0.0000.000
O20.0401 (9)0.0208 (7)0.0200 (7)−0.0038 (7)0.0000.000
C80.0587 (12)0.0459 (11)0.0243 (8)0.0041 (9)−0.0085 (8)−0.0006 (7)
C40.0391 (10)0.0438 (10)0.0488 (11)0.0098 (8)−0.0215 (8)−0.0096 (9)
C50.0550 (11)0.0294 (9)0.0268 (8)−0.0089 (8)0.0003 (7)−0.0075 (7)
C70.0442 (10)0.0455 (10)0.0249 (8)−0.0094 (8)−0.0090 (7)−0.0014 (7)
C60.0556 (12)0.0522 (12)0.0257 (8)−0.0139 (9)0.0049 (8)−0.0098 (8)
C20.0657 (14)0.0601 (14)0.0462 (11)0.0366 (11)−0.0033 (10)−0.0097 (10)
C30.0344 (12)0.107 (2)0.0876 (17)0.0248 (12)−0.0139 (11)−0.0386 (16)
C10.0526 (12)0.0554 (13)0.0681 (14)0.0211 (10)−0.0125 (10)−0.0379 (11)
Geometric parameters (Å, º) top
Al1—H11.573 (18)C4—C31.471 (3)
Al1—H21.55 (2)C4—H4A0.99
Al1—H31.52 (2)C4—H4B0.99
Al1—H41.50 (2)C5—C61.505 (2)
Mg1—O1i2.0517 (11)C5—H5A0.99
Mg1—O12.0518 (11)C5—H5B0.99
Mg1—O32.0800 (15)C7—H7A0.99
Mg1—O22.0804 (15)C7—H7B0.99
Mg1—H11.977 (18)C6—C6i1.519 (4)
O1—C11.443 (2)C6—H6A0.99
O1—C41.4529 (19)C6—H6B0.99
O3—C7i1.4537 (17)C2—C11.477 (3)
O3—C71.4537 (17)C2—C31.487 (3)
O2—C51.4567 (17)C2—H2A0.99
O2—C5i1.4567 (17)C2—H2B0.99
C8—C71.506 (2)C3—H3A0.99
C8—C8i1.517 (4)C3—H3B0.99
C8—H8A0.99C1—H1A0.99
C8—H8B0.99C1—H1B0.99
H1—Al1—H2106.3 (9)O2—C5—C6105.40 (13)
H1—Al1—H3104.8 (10)O2—C5—H5A110.7
H2—Al1—H3113.1 (11)C6—C5—H5A110.7
H1—Al1—H4107.0 (11)O2—C5—H5B110.7
H2—Al1—H4110.9 (11)C6—C5—H5B110.7
H3—Al1—H4114.0 (12)H5A—C5—H5B108.8
O1i—Mg1—O1179.65 (6)O3—C7—C8105.66 (13)
O1i—Mg1—O390.18 (3)O3—C7—H7A110.6
O1—Mg1—O390.18 (3)C8—C7—H7A110.6
O1i—Mg1—O289.82 (3)O3—C7—H7B110.6
O1—Mg1—O289.82 (3)C8—C7—H7B110.6
O3—Mg1—O2180.0H7A—C7—H7B108.7
O1i—Mg1—H191.4 (5)C5—C6—C6i102.59 (11)
O1—Mg1—H188.6 (5)C5—C6—H6A111.2
O3—Mg1—H190.4 (4)C6i—C6—H6A111.2
O2—Mg1—H189.6 (4)C5—C6—H6B111.2
C1—O1—C4109.08 (13)C6i—C6—H6B111.2
C1—O1—Mg1125.75 (10)H6A—C6—H6B109.2
C4—O1—Mg1125.10 (10)C1—C2—C3104.88 (16)
C7i—O3—C7109.37 (16)C1—C2—H2A110.8
C7i—O3—Mg1125.32 (8)C3—C2—H2A110.8
C7—O3—Mg1125.32 (8)C1—C2—H2B110.8
C5—O2—C5i109.39 (16)C3—C2—H2B110.8
C5—O2—Mg1125.30 (8)H2A—C2—H2B108.8
C5i—O2—Mg1125.30 (8)C4—C3—C2105.13 (18)
C7—C8—C8i102.78 (11)C4—C3—H3A110.7
C7—C8—H8A111.2C2—C3—H3A110.7
C8i—C8—H8A111.2C4—C3—H3B110.7
C7—C8—H8B111.2C2—C3—H3B110.7
C8i—C8—H8B111.2H3A—C3—H3B108.8
H8A—C8—H8B109.1O1—C1—C2106.93 (15)
O1—C4—C3105.34 (15)O1—C1—H1A110.3
O1—C4—H4A110.7C2—C1—H1A110.3
C3—C4—H4A110.7O1—C1—H1B110.3
O1—C4—H4B110.7C2—C1—H1B110.3
C3—C4—H4B110.7H1A—C1—H1B108.6
H4A—C4—H4B108.8
Symmetry code: (i) −x, −y+1/2, z.

Experimental details

Crystal data
Chemical formula[Al2MgH8(C4H8O)4]
Mr374.75
Crystal system, space groupOrthorhombic, Pcnb
Temperature (K)150
a, b, c (Å)10.161 (2), 14.027 (3), 16.429 (3)
V (Å3)2341.6 (8)
Z4
Radiation typeMo Kα
µ (mm−1)0.16
Crystal size (mm)0.38 × 0.31 × 0.19
Data collection
DiffractometerNonius Kappa CCD
Absorption correctionMulti-scan
(SCALEPACK; Otwinowski & Minor, 1997)
Tmin, Tmax0.940, 0.969
No. of measured, independent and
observed [I > 2σ(I)] reflections		5018, 2687, 1973
Rint0.017
(sin θ/λ)max (Å−1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.119, 1.07
No. of reflections2687
No. of parameters122
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.30, −0.30

Computer programs: COLLECT (Nonius, 1998), SCALEPACK (Otwinowski & Minor, 1997), DENZO (Otwinowski & Minor 1997) and SCALEPACK, SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

This work was funded by the US Department of Energy, the Office of Energy Efficiency and Renewable Energy (EERE) under Contract No. DE-FC3605GO15062 as part of the DOE Metal Hydride Center of Excellence.

References

First citationAshby, E. C. & Goel, A. B. (1977). Inorg. Chem. 16, 2082–2085.  CrossRef CAS Web of Science Google Scholar
 First citationAshby, E. C., Schwartz, R. D. & James, B. D. (1970). Inorg. Chem. 9, 325–332.  CrossRef CAS Web of Science Google Scholar
 First citationDilts, J. A. & Ashby, E. C. (1972). Inorg. Chem. 11, 1230–1236.  CrossRef CAS Web of Science Google Scholar
 First citationFichtner, M., Frommen, C. & Fuhr, O. (2004). Inorg. Chem. 44, 3479–3484.  Web of Science CSD CrossRef Google Scholar
 First citationFichtner, M. & Fuhr, O. (2002). J. Alloys Compd, 345, 286–296.  Web of Science CSD CrossRef CAS Google Scholar
 First citationLauher, J. W., Dougherty, D. & Herley, P. J. (1979). Acta Cryst. B35, 1454–1456.  CrossRef CAS IUCr Journals Web of Science Google Scholar
 First citationNonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.  Google Scholar
 First citationNöth, H., Schmidt, M. & Treitl, A. (1995). Chem. Ber. 128, 999–1006.  Google Scholar
 First citationOtwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationShen, P. & Che, Y. (1991). Faming ZhuanliShenqing Gongkai Shuomingshu, CN1051179, p. 7.  Google Scholar
 First citationSklar, N. & Post, B. (1967). Inorg. Chem. 6, 669–671.  CrossRef CAS Web of Science Google Scholar

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ISSN: 2056-9890
Volume 66| Part 5| May 2010| Page m575
https://doi.org/10.1107/S1600536810014200
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