Zirconium(IV) dilanthanum(III) penta­sulfide

Raw, A.D.; Ibers, J.A.

doi:10.1107/S1600536811045193

inorganic compounds

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Volume 67| Part 12| December 2011| Page i70

https://doi.org/10.1107/S1600536811045193

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Zirconium(IV) dilanthanum(III) pentasulfide

Adam D. Raw ^a and James A. Ibers ^a ^*

^aDepartment of Chemistry, Northwestern University, 2145 Sheridan Rd, Evanston, IL 60208-3113, USA
^*Correspondence e-mail: ibers@chem.northwestern.edu

(Received 20 October 2011; accepted 27 October 2011; online 5 November 2011)

Zirconium(IV) dilanthanum(III) pentasulfide, ZrLa₂S₅, crystallizes with four formula units in the space group Pnma in the U₃S₅ structure type. The asymmetric unit comprises one Zr, one La and four S atoms. The Zr and three S atoms are situated on mirror planes. The structure consists of LaS₈ face-sharing bicapped distorted trigonal prisms and ZrS₇ edge-sharing monocapped octahedra.

Related literature

The cell parameters of ZrLa₂S₅ were previously reported from X-ray powder diffraction measurements (Kokhno & Serebrennikov, 1977 ). In a separate study, single-crystal X-ray diffraction measurements were used to determine the lattice parameters but not the structural parameters (Donohue & Jeitschko, 1974 ). Given that these lattice parameters, the space group, and the stoichiometry are similar to those of U₃S₅, it was assumed that ZrLa₂S₅ and U₃S₅ are isotypic (Donohue & Jeitschko, 1974). For analogous structures, see: Du Pont de Nemours (1976 ) and Potel et al. (1972 ). Physical property measurements of this and related compounds have been reported. For optical properties, see: Alekseeva et al. (1980 ); for electrical properties, see: Senova et al. (1984 ). For synthetic details, see: Jin et al. (2009 ). For ionic radii, see: Shannon (1976 ). For standardization of structural data, see: Gelato & Parthé (1987 ).

Experimental

Crystal data

ZrLa₂S₅
M_r = 529.34
Orthorhombic, P n m a
a = 11.4784 (4) Å
b = 8.2010 (3) Å
c = 7.3799 (3) Å
V = 694.70 (5) Å³
Z = 4
Mo Kα radiation
μ = 14.93 mm⁻¹
T = 100 K
0.12 × 0.11 × 0.09 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: numerical [face indexed (SADABS; Bruker, 2009 )] T_min = 0.263, T_max = 0.340
8134 measured reflections
890 independent reflections
877 reflections with I > 2σ(I)
R_int = 0.018

Refinement

R[F² > 2σ(F²)] = 0.017
wR(F²) = 0.056
S = 2.51
890 reflections
44 parameters
Δρ_max = 2.20 e Å⁻³
Δρ_min = −0.54 e Å⁻³

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2009 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811045193/wm2549sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811045193/wm2549Isup2.hkl

checkCIF report

Comment top

Single crystals of ZrLa₂S₅ resulted from attempts to synthesize zirconium analogues of the uranium lanthanide oxysulfide compound UYb₂O₂S₃ (Jin et al., 2009).

ZrLa₂S₅ adopts the U₃S₅ structure type (Potel et al., 1972). The unit-cell dimensions have been previously reported from single-crystal X-ray diffraction data (Donohue & Jeitschko, 1974) and from powder X-ray diffraction data (Kokhno & Serebrennikov, 1977). Unit-cell dimensions for ZrLa₂S₅ from the two single-crystal determinations compare favorably: a = 11.4864 (5), b = 8.2167 (5), c = 7.3894 (3) Å at room temperature (Donohue & Jeitschko, 1974) versus a = 11.4784 (4), b = 8.2010 (3), c = 7.3799 (3) Å from the present study at 100 K. (See also Kokhno & Serebrennikov, 1977). Isostructural compounds have been previously reported based on X-ray powder diffraction measurements for all trivalent lanthanides and yttrium excluding promethium, europium and ytterbium (Du Pont de Nemours, 1976).

The La—S interatomic distances (Table 1, Fig. 1) in the face-sharing bicapped distorted trigonal prisms LaS₈ (Fig. 2) range from 2.8861 (8) to 3.0698 (9) Å. The Zr—S distances range from 2.5704 (8) to 2.7421 (11) Å. These values are close to the distances of 3.00 Å for La—S and 2.62 Å for Zr—S calculated from the summed ionic radii (Shannon, 1976).

Physical property measurements of ZrLa₂S₅ have been reported by Alekseeva et al. (1980) and Senova et al. (1984).

Related literature top

The cell parameters of ZrLa₂S₅ were previously reported from X-ray powder diffraction measurements (Kokhno & Serebrennikov, 1977). In a separate study, single-crystal X-ray diffraction measurements were used to determine the lattice parameters but not the structural parameters (Donohue & Jeitschko, 1974). Given that these lattice parameters, the space group, and the stoichiometry are similar to those of U₃S₅, it was assumed that ZrLa₂S₅ and U₃S₅ are isotypic (Donohue & Jeitschko, 1974). For analogous structures, see: Du Pont de Nemours (1976) and Potel et al. (1972). Physical property measurements of this and related compounds have been reported. For optical properties, see: Alekseeva et al. (1980); for electrical properties, see: Senova et al. (1984). For synthetic details, see: Jin et al. (2009). For ionic radii, see: Shannon (1976). For standardization of structural data, see: Gelato & Parthé (1987).

Experimental top

ZrO₂ (99.99%, Aldrich) and La₂S₃ (99.9%, Strem) were used as received. Sb₂S₃ was synthesized from the elements. ZrLa₂S₅ was crystallized in a two step reaction in carbon-coated fused-silica tubes that had been evacuated to 10 ^-4 Torr. In the first step, 0.02 g (0.16 mmol) ZrO₂ and 0.3 g (0.08 mmol) La₂S₃ were heated at 1273 K for 99 h and cooled to 298 K in 14 h. The resulting powder was combined with 0.02 g (0.06 mmol) Sb₂S₃ and heated at 1273 K for 99 h then cooled to 873 K at a rate of 2 K/h before cooling to 298 K over 10 h. The resulting ZrLa₂S₅ formed black prismatic crystals in low yield (<5 wt%). These were mechanically separated from the remaining powder.

Structure description top

Single crystals of ZrLa₂S₅ resulted from attempts to synthesize zirconium analogues of the uranium lanthanide oxysulfide compound UYb₂O₂S₃ (Jin et al., 2009).

Physical property measurements of ZrLa₂S₅ have been reported by Alekseeva et al. (1980) and Senova et al. (1984).

The cell parameters of ZrLa₂S₅ were previously reported from X-ray powder diffraction measurements (Kokhno & Serebrennikov, 1977). In a separate study, single-crystal X-ray diffraction measurements were used to determine the lattice parameters but not the structural parameters (Donohue & Jeitschko, 1974). Given that these lattice parameters, the space group, and the stoichiometry are similar to those of U₃S₅, it was assumed that ZrLa₂S₅ and U₃S₅ are isotypic (Donohue & Jeitschko, 1974). For analogous structures, see: Du Pont de Nemours (1976) and Potel et al. (1972). Physical property measurements of this and related compounds have been reported. For optical properties, see: Alekseeva et al. (1980); for electrical properties, see: Senova et al. (1984). For synthetic details, see: Jin et al. (2009). For ionic radii, see: Shannon (1976). For standardization of structural data, see: Gelato & Parthé (1987).

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2009); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of ZrLa₂S₅. Displacement ellipsoids are displayed at the 95% probability level.
	Fig. 2. The ZrLa₂S₅ structure. La atoms are blue, Zr atoms are black, S atoms are yellow

Zirconium(IV) dilanthanum(III) pentasulfide top

Crystal data top

ZrLa₂S₅	D_x = 5.061 Mg m⁻³
M_r = 529.34	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 6255 reflections
a = 11.4784 (4) Å	θ = 3.1–27.9°
b = 8.2010 (3) Å	µ = 14.93 mm⁻¹
c = 7.3799 (3) Å	T = 100 K
V = 694.70 (5) Å³	Prism, black
Z = 4	0.12 × 0.11 × 0.09 mm
F(000) = 936

Data collection top

Bruker APEXII CCD diffractometer	890 independent reflections
Radiation source: fine-focus sealed tube	877 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
φ and ω scans	θ_max = 27.9°, θ_min = 3.3°
Absorption correction: numerical [face indexed (SADABS; Bruker, 2009)]	h = −14→15
T_min = 0.263, T_max = 0.340	k = −10→6
8134 measured reflections	l = −9→9

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.017	[1.00000 + 0.00000exp(0.00(sinθ/λ)²)]/ [σ²(F_o²) + 0.0000 + 0.0000*P + (0.0158P)² + 0.0000sinθ/λ] where P = 1.00000F_o² + 0.00000F_c²
wR(F²) = 0.056	(Δ/σ)_max = 0.001
S = 2.51	Δρ_max = 2.20 e Å⁻³
890 reflections	Δρ_min = −0.54 e Å⁻³
44 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0015 (2)

Crystal data top

ZrLa₂S₅	V = 694.70 (5) Å³
M_r = 529.34	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 11.4784 (4) Å	µ = 14.93 mm⁻¹
b = 8.2010 (3) Å	T = 100 K
c = 7.3799 (3) Å	0.12 × 0.11 × 0.09 mm

Data collection top

Bruker APEXII CCD diffractometer	890 independent reflections
Absorption correction: numerical [face indexed (SADABS; Bruker, 2009)]	877 reflections with I > 2σ(I)
T_min = 0.263, T_max = 0.340	R_int = 0.018
8134 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.017	44 parameters
wR(F²) = 0.056	0 restraints
S = 2.51	Δρ_max = 2.20 e Å⁻³
890 reflections	Δρ_min = −0.54 e Å⁻³

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

	x	y	z	U_iso*/U_eq
La1	0.328759 (18)	0.501789 (17)	0.44160 (3)	0.00537 (12)
Zr1	0.01001 (3)	0.2500	0.42914 (5)	0.00286 (13)
S1	0.29147 (10)	0.2500	0.15995 (15)	0.0061 (2)
S2	0.07363 (7)	0.53474 (10)	0.32234 (11)	0.00812 (18)
S3	0.19311 (10)	0.2500	0.64058 (15)	0.0063 (2)
S4	0.00443 (9)	0.2500	0.05768 (14)	0.0073 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La1	0.00643 (17)	0.00439 (17)	0.00529 (17)	0.00023 (5)	−0.00022 (6)	−0.00036 (5)
Zr1	0.0030 (2)	0.0028 (2)	0.0028 (2)	0.000	−0.00063 (13)	0.000
S1	0.0073 (5)	0.0053 (5)	0.0056 (5)	0.000	−0.0013 (4)	0.000
S2	0.0102 (4)	0.0080 (3)	0.0062 (4)	0.0004 (3)	0.0007 (3)	−0.0005 (3)
S3	0.0086 (5)	0.0051 (5)	0.0051 (5)	0.000	0.0008 (4)	0.000
S4	0.0066 (6)	0.0062 (5)	0.0090 (6)	0.000	0.0007 (4)	0.000

Geometric parameters (Å, º) top

La1—S4ⁱ	2.8861 (8)	Zr1—S2^viii	2.7206 (9)
La1—S4ⁱⁱ	2.9230 (7)	Zr1—S2^ix	2.7206 (9)
La1—S1ⁱⁱ	2.9402 (8)	Zr1—S4	2.7421 (11)
La1—S1	2.9610 (8)	S1—Zr1ⁱ	2.5932 (12)
La1—S3	2.9740 (8)	S1—La1^x	2.9402 (8)
La1—S3ⁱⁱⁱ	3.0235 (8)	S1—La1ⁱⁱⁱ	2.9402 (8)
La1—S2ⁱⁱ	3.0398 (8)	S1—La1^vi	2.9609 (8)
La1—S2	3.0698 (9)	S2—Zr1^viii	2.7206 (9)
La1—La1^iv	4.0247 (4)	S2—La1ⁱⁱⁱ	3.0398 (8)
La1—La1^v	4.0712 (3)	S3—La1^vi	2.9739 (8)
La1—La1ⁱⁱⁱ	4.1092 (2)	S3—La1ⁱⁱ	3.0235 (8)
La1—La1ⁱⁱ	4.1092 (2)	S3—La1^xi	3.0235 (8)
Zr1—S2^vi	2.5704 (8)	S4—La1^xii	2.8861 (8)
Zr1—S2	2.5705 (8)	S4—La1^vii	2.8861 (8)
Zr1—S1^vii	2.5932 (12)	S4—La1ⁱⁱⁱ	2.9230 (7)
Zr1—S3	2.6176 (12)	S4—La1^x	2.9230 (7)

S4ⁱ—La1—S4ⁱⁱ	92.295 (9)	S2—La1—La1ⁱⁱ	80.696 (17)
S4ⁱ—La1—S1ⁱⁱ	145.31 (3)	La1^iv—La1—La1ⁱⁱ	103.733 (7)
S4ⁱⁱ—La1—S1ⁱⁱ	70.41 (3)	La1^v—La1—La1ⁱⁱ	90.408 (4)
S4ⁱ—La1—S1	66.63 (3)	La1ⁱⁱⁱ—La1—La1ⁱⁱ	127.785 (11)
S4ⁱⁱ—La1—S1	141.82 (3)	S2^vi—Zr1—S2	130.58 (4)
S1ⁱⁱ—La1—S1	143.100 (13)	S2^vi—Zr1—S1^vii	101.36 (2)
S4ⁱ—La1—S3	82.42 (2)	S2—Zr1—S1^vii	101.36 (2)
S4ⁱⁱ—La1—S3	132.98 (3)	S2^vi—Zr1—S3	87.40 (2)
S1ⁱⁱ—La1—S3	87.96 (2)	S2—Zr1—S3	87.40 (2)
S1—La1—S3	77.69 (2)	S1^vii—Zr1—S3	158.10 (3)
S4ⁱ—La1—S3ⁱⁱⁱ	122.76 (3)	S2^vi—Zr1—S2^viii	153.69 (2)
S4ⁱⁱ—La1—S3ⁱⁱⁱ	78.51 (2)	S2—Zr1—S2^viii	73.59 (3)
S1ⁱⁱ—La1—S3ⁱⁱⁱ	84.12 (2)	S1^vii—Zr1—S2^viii	80.19 (3)
S1—La1—S3ⁱⁱⁱ	86.66 (2)	S3—Zr1—S2^viii	83.19 (3)
S3—La1—S3ⁱⁱⁱ	141.885 (17)	S2^vi—Zr1—S2^ix	73.59 (3)
S4ⁱ—La1—S2ⁱⁱ	70.75 (3)	S2—Zr1—S2^ix	153.69 (2)
S4ⁱⁱ—La1—S2ⁱⁱ	63.66 (2)	S1^vii—Zr1—S2^ix	80.19 (3)
S1ⁱⁱ—La1—S2ⁱⁱ	74.61 (3)	S3—Zr1—S2^ix	83.19 (3)
S1—La1—S2ⁱⁱ	129.30 (2)	S2^viii—Zr1—S2^ix	80.92 (4)
S3—La1—S2ⁱⁱ	70.62 (3)	S2^vi—Zr1—S4	72.55 (2)
S3ⁱⁱⁱ—La1—S2ⁱⁱ	140.91 (2)	S2—Zr1—S4	72.55 (2)
S4ⁱ—La1—S2	136.89 (2)	S1^vii—Zr1—S4	73.97 (3)
S4ⁱⁱ—La1—S2	130.36 (2)	S3—Zr1—S4	127.93 (4)
S1ⁱⁱ—La1—S2	69.42 (3)	S2^viii—Zr1—S4	131.74 (2)
S1—La1—S2	73.87 (3)	S2^ix—Zr1—S4	131.74 (2)
S3—La1—S2	72.74 (3)	Zr1ⁱ—S1—La1^x	108.37 (3)
S3ⁱⁱⁱ—La1—S2	69.57 (3)	Zr1ⁱ—S1—La1ⁱⁱⁱ	108.37 (3)
S2ⁱⁱ—La1—S2	128.71 (2)	La1^x—S1—La1ⁱⁱⁱ	87.63 (3)
S4ⁱ—La1—La1^iv	46.526 (16)	Zr1ⁱ—S1—La1^vi	92.19 (3)
S4ⁱⁱ—La1—La1^iv	45.769 (15)	La1^x—S1—La1^vi	88.267 (9)
S1ⁱⁱ—La1—La1^iv	110.25 (2)	La1ⁱⁱⁱ—S1—La1^vi	159.29 (4)
S1—La1—La1^iv	106.65 (2)	Zr1ⁱ—S1—La1	92.19 (3)
S3—La1—La1^iv	113.61 (2)	La1^x—S1—La1	159.29 (4)
S3ⁱⁱⁱ—La1—La1^iv	104.09 (2)	La1ⁱⁱⁱ—S1—La1	88.267 (9)
S2ⁱⁱ—La1—La1^iv	56.031 (16)	La1^vi—S1—La1	88.43 (3)
S2—La1—La1^iv	173.643 (17)	Zr1—S2—Zr1^viii	106.41 (3)
S4ⁱ—La1—La1^v	135.682 (15)	Zr1—S2—La1ⁱⁱⁱ	107.38 (3)
S4ⁱⁱ—La1—La1^v	45.861 (14)	Zr1^viii—S2—La1ⁱⁱⁱ	144.80 (3)
S1ⁱⁱ—La1—La1^v	46.186 (15)	Zr1—S2—La1	95.92 (3)
S1—La1—La1^v	134.217 (15)	Zr1^viii—S2—La1	101.56 (3)
S3—La1—La1^v	133.973 (16)	La1ⁱⁱⁱ—S2—La1	84.53 (2)
S3ⁱⁱⁱ—La1—La1^v	47.682 (15)	Zr1—S3—La1^vi	97.24 (3)
S2ⁱⁱ—La1—La1^v	95.655 (16)	Zr1—S3—La1	97.24 (3)
S2—La1—La1^v	84.950 (15)	La1^vi—S3—La1	87.95 (3)
La1^iv—La1—La1^v	90.417 (4)	Zr1—S3—La1ⁱⁱ	111.80 (3)
S4ⁱ—La1—La1ⁱⁱⁱ	107.70 (2)	La1^vi—S3—La1ⁱⁱ	150.89 (4)
S4ⁱⁱ—La1—La1ⁱⁱⁱ	123.806 (19)	La1—S3—La1ⁱⁱ	86.491 (11)
S1ⁱⁱ—La1—La1ⁱⁱⁱ	106.89 (2)	Zr1—S3—La1^xi	111.80 (3)
S1—La1—La1ⁱⁱⁱ	45.659 (16)	La1^vi—S3—La1^xi	86.491 (11)
S3—La1—La1ⁱⁱⁱ	102.01 (2)	La1—S3—La1^xi	150.89 (4)
S3ⁱⁱⁱ—La1—La1ⁱⁱⁱ	46.251 (17)	La1ⁱⁱ—S3—La1^xi	84.64 (3)
S2ⁱⁱ—La1—La1ⁱⁱⁱ	172.533 (17)	Zr1—S4—La1^xii	90.83 (3)
S2—La1—La1ⁱⁱⁱ	47.425 (16)	Zr1—S4—La1^vii	90.83 (3)
La1^iv—La1—La1ⁱⁱⁱ	128.467 (9)	La1^xii—S4—La1^vii	91.36 (3)
La1^v—La1—La1ⁱⁱⁱ	90.409 (4)	Zr1—S4—La1ⁱⁱⁱ	106.12 (3)
S4ⁱ—La1—La1ⁱⁱ	107.50 (2)	La1^xii—S4—La1ⁱⁱⁱ	163.03 (4)
S4ⁱⁱ—La1—La1ⁱⁱ	91.72 (2)	La1^vii—S4—La1ⁱⁱⁱ	87.705 (9)
S1ⁱⁱ—La1—La1ⁱⁱ	46.074 (16)	Zr1—S4—La1^x	106.12 (3)
S1—La1—La1ⁱⁱ	124.18 (2)	La1^xii—S4—La1^x	87.705 (9)
S3—La1—La1ⁱⁱ	47.258 (17)	La1^vii—S4—La1^x	163.03 (4)
S3ⁱⁱⁱ—La1—La1ⁱⁱ	128.91 (2)	La1ⁱⁱⁱ—S4—La1^x	88.28 (3)
S2ⁱⁱ—La1—La1ⁱⁱ	48.044 (16)

Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) −x+1/2, −y+1, z+1/2; (iii) −x+1/2, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) x, −y+3/2, z; (vi) x, −y+1/2, z; (vii) x−1/2, y, −z+1/2; (viii) −x, −y+1, −z+1; (ix) −x, y−1/2, −z+1; (x) −x+1/2, y−1/2, z−1/2; (xi) −x+1/2, y−1/2, z+1/2; (xii) x−1/2, −y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	ZrLa₂S₅
M_r	529.34
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	100
a, b, c (Å)	11.4784 (4), 8.2010 (3), 7.3799 (3)
V (Å³)	694.70 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	14.93
Crystal size (mm)	0.12 × 0.11 × 0.09

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Numerical [face indexed (SADABS; Bruker, 2009)]
T_min, T_max	0.263, 0.340
No. of measured, independent and observed [I > 2σ(I)] reflections	8134, 890, 877
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.659

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.017, 0.056, 2.51
No. of reflections	890
No. of parameters	44
Δρ_max, Δρ_min (e Å⁻³)	2.20, −0.54

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), CrystalMaker (Palmer, 2009).

Acknowledgements

The research was kindly supported by the US Department of Energy, Basic Energy Sciences, Chemical Sciences, Biosciences, and Geosciences Division and Divison of Materials Science and Engineering grant ER-15522. Use was made of the IMSERC X-ray Facility at Northwestern University, supported by the International Institute of Nanotechnology (IIN)

References

Alekseeva, T. P., Senova, R. N., Cherkasova, T. G. & Kokhno, G. V. (1980). Khim. Khim. Tekhnol. Geol. Mater. Reg. Nauchno-Prakt. Konf. 3, 8–9. Google Scholar
Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Donohue, P. C. & Jeitschko, W. (1974). Mater. Res. Bull. 9, 1333–1336. CrossRef CAS Google Scholar
Du Pont de Nemours, E. I., and Co. (1976). US Patent No. 3 956 461. Google Scholar
Gelato, L. M. & Parthé, E. (1987). J. Appl. Cryst. 20, 139–143. CrossRef Web of Science IUCr Journals Google Scholar
Jin, G. B., Choi, E. S. & Ibers, J. A. (2009). Inorg. Chem. 48, 8227–8232. Web of Science CrossRef PubMed CAS Google Scholar
Kokhno, G. V. & Serebrennikov, V. V. (1977). Zh. Neorg. Khim. 22, 2111–2114. CAS Google Scholar
Palmer, D. (2009). CrystalMaker Software. CrystalMaker Software Ltd, Oxford, England. Google Scholar
Potel, M., Brochu, R., Padiou, J. & Grandjean, D. (1972). C. R. Seances Acad. Sci. Ser. C, 275, 1419–1421. CAS Google Scholar
Senova, R. N., Alekseeva, T. P., Cherkasova, T. G. & Kokhno, G. V. (1984). Sintez i Reakts, pp. 89–92. Tomsk: Sposobnost Veshchestv. Google Scholar
Shannon, R. D. (1976). Acta Cryst. A32, 751–767. CrossRef CAS IUCr Journals Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar