Cs3ScCl6

Ward, M.D.; Ibers, J.A.

doi:10.1107/S1600536814009799

inorganic compounds

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ISSN: 2056-9890

Volume 70| Part 6| June 2014| Page i25

doi:10.1107/S1600536814009799

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Cs₃ScCl₆

Matthew D. Ward ^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

Edited by M. Weil, Vienna University of Technology, Austria (Received 9 April 2014; accepted 30 April 2014; online 10 May 2014)

Crystals of tricaesium scandium(III) hexachloride were obtained as a side product from the reaction of U, SnCl₂, Sc, and S in a CsCl flux at 1073 K. Cs₃ScCl₆ crystallizes in the Rb₃YCl₆ structure type. The asymmetric unit comprises three Cs sites, two Sc sites, and six Cl sites, all of which have site symmetry 1, except for the two Sc sites that have site symmetries of 2 and -1, respectively. The structure is composed of isolated [ScCl₆]³⁻ octahedra that are surrounded by Cs⁺ cations. Two Cs⁺ cations have interactions with eight Cl⁻ anions, while the third has interactions with ten Cl⁻ anions.

CCDC reference: 1000441

Related literature

Cs₃ScCl₆ crystallizes in the Rb₃YCl₆ structure type (space group C2/c; Mattfeld & Meyer, 1992 ). Previously, a number of ternary scandium halides of the composition A₃ScX₆ were characterized by single-crystal X-ray diffraction or Rietveld refinements from powder data. These include Na₃ScF₆ (Dahlke & Babel, 1994 ), Na₃ScBr₆ (Bohnsack & Meyer, 1996 ), Li₃ScCl₆ (Bohnsack et al., 1997 ), Li₃ScF₆ (Tyagi et al., 2005 ), K₃ScCl₆ (Cerny et al., 2010a ), and Na₃ScCl₆ (Cerny et al., 2010b ). Except for Li₃ScCl₆, these compounds crystallize in one of two structure types: Na₃CrCl₆ (P $[\overline{3}]$ 1c; Friedrich et al., 1987 ) or Na₃AlF₆ (P2₁/n; Náray-Szabó & Sasvári, 1938 ). For other caesium scandium chloride compounds, see: Poeppelmeier et al. (1980 ). For standardization of structure data, see: Gelato & Parthé (1987 ).

Experimental

Crystal data

Cs₃ScCl₆
M_r = 656.39
Monoclinic, C 2/c
a = 26.3310 (5) Å
b = 7.9632 (2) Å
c = 12.7085 (3) Å
β = 100.006 (1)°
V = 2624.17 (10) Å³
Z = 8
Mo Kα radiation
μ = 9.93 mm⁻¹
T = 100 K
0.05 × 0.04 × 0.03 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: numerical (SADABS; Bruker, 2009 ) T_min = 0.341, T_max = 0.438
30195 measured reflections
6379 independent reflections
5631 reflections with I > 2σ(I)
R_int = 0.038

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.050
S = 1.33
6379 reflections
93 parameters
Δρ_max = 0.98 e Å⁻³
Δρ_min = −1.26 e Å⁻³

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT-Plus (Bruker, 2009); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL2014; molecular graphics: CrystalMaker (Palmer, 2013 ); software used to prepare material for publication: SHELXL2014.

Supporting information

CCDC reference: 1000441

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536814009799/wm5022sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814009799/wm5022Isup2.hkl

checkCIF report

Comment top

Ternary scandium halides of the composition A₃ScX₆ are known for A = Li, Na, K and X = F, Cl, Br. These compounds crystallize in either the Na₃CrCl₆ (P31c) (Friedrich et al., 1987) or the Na₃AlF₆ (P2₁/n) (Náray-Szabó & Sasvári, 1938) structure types, except for Li₃ScCl₆ which crystallizes in space group C2/m (Bohnsack et al., 1997). Single-crystal refinements have been carried out for Na₃ScF₆ (Dahlke & Babel, 1994), Na₃ScBr₆ (Bohnsack & Meyer, 1996), Li₃ScCl₆ (Bohnsack et al., 1997), and Li₃ScF₆ (Tyagi et al., 2005). The structures of K₃ScCl₆ (Cerny et al., 2010a) and Na₃ScCl₆ (Cerny et al., 2010b) were determined by Rietveld refinement of X-ray powder data. Cs₃ScCl₆ is the first Cs-containing compound of the A₃ScX₆ family. It crystallizes in the monoclinic space group C2/c in the Rb₃YCl₆ structure type (Mattfeld & Meyer, 1992).

The structure of Cs₃ScCl₆ is composed of isolated [ScCl₆]^3- octahedra that are surrounded by Cs⁺ cations. The asymmetric unit, comprising three Cs, two Sc, and six Cl sites, is shown in Fig. 1, and a packing diagram is shown in Fig. 2. The composition achieves charge balance by assigning formal oxidation states of +1, +3, and -1 to Cs, Sc, and Cl, respectively. The Sc—Cl distances range from 2.4718 (5) Å to 2.5072 (6) Å at 100 K. These distances compare favorably with those of 2.601 Å at 298 K in Cs₃Sc₂Cl₉ (Poeppelmeier et al., 1980). Another caesium scandium chloride compound is CsScCl₃ (Poeppelmeier et al., 1980), which reportedly contains Sc(II).

Related literature top

Cs₃ScCl₆ crystallizes in the Rb₃YCl₆ structure type (space group C2/c; Mattfeld & Meyer, 1992). Previously, a number of ternary scandium halides of the composition A₃ScX₆ were characterized by single-crystal X-ray diffraction or Rietveld refinements from powder data. These include Na₃ScF₆ (Dahlke & Babel, 1994), Na₃ScBr₆ (Bohnsack & Meyer, 1996), Li₃ScCl₆ (Bohnsack et al., 1997), Li₃ScF₆ (Tyagi et al., 2005), K₃ScCl₆ (Cerny et al., 2010a), and Na₃ScCl₆ (Cerny et al., 2010b). Except for Li₃ScCl₆, these compounds crystallize in one of two structure types: Na₃CrCl₆ (P31c; Friedrich et al., 1987) or Na₃AlF₆ (P2₁/n; Náray-Szabó & Sasvári, 1938). For other caesium scandium chloride compounds, see: Poeppelmeier et al. (1980). For standardization of structure data, see: Gelato & Parthé (1987).

Experimental top

A reaction mixture containing U (0.126 mmol), SnCl₂ (0.126 mmol), Sc (1.290 mmol), S (0.378 mmol), and CsCl (0.594 mmol) was loaded into a carbon-coated fused-silica tube under an inert Ar atmosphere. The tube was then evacuated to 10 ^-4 Torr, flame sealed, and placed in a computer-controlled furnace. The tube was heated to 1073 K in 12 h, held there for 96 h, cooled to 773 K at a rate of 2 K/h, and then cooled to 298 K over a further 48 h. The reaction yielded black rectangular prisms of ScU₈S₁₇, purple blocks of Cs₃ScCl₆, and excess CsCl flux. Crystals of Cs₃ScCl₆ were also found as side products in other reactions that contained Sc and a CsCl flux. Crystals of Cs₃ScCl₆ are soluble in water.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT-Plus (Bruker, 2009); data reduction: SAINT-Plus (Bruker, 2009); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2013); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of Cs₃ScCl₆. Displacement ellipsoids at the 99% probability level are shown. Caesium atoms are blue, scandium atoms are purple, and chlorine atoms are green.
	Fig. 2. Packing of Cs₃ScCl₆ viewed nearly along the b axis.

Tricaesium scandium(III) hexachloride top

Crystal data top

Cs₃ScCl₆	F(000) = 2304
M_r = 656.39	D_x = 3.323 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 26.3310 (5) Å	Cell parameters from 9931 reflections
b = 7.9632 (2) Å	θ = 3.1–36.3°
c = 12.7085 (3) Å	µ = 9.93 mm⁻¹
β = 100.006 (1)°	T = 100 K
V = 2624.17 (10) Å³	Block, purple
Z = 8	0.05 × 0.04 × 0.03 mm

Data collection top

Bruker APEXII CCD diffractometer	5631 reflections with I > 2σ(I)
ϕ and ω scans	R_int = 0.038
Absorption correction: numerical (SADABS; Bruker, 2009)	θ_max = 36.4°, θ_min = 1.6°
T_min = 0.341, T_max = 0.438	h = −39→43
30195 measured reflections	k = −13→12
6379 independent reflections	l = −20→21

Refinement top

Refinement on F²	93 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.023	w = 1/[σ²(F_o²) + (0.0114F_o²)²]
wR(F²) = 0.050	(Δ/σ)_max = 0.002
S = 1.33	Δρ_max = 0.98 e Å⁻³
6379 reflections	Δρ_min = −1.26 e Å⁻³

Crystal data top

Cs₃ScCl₆	V = 2624.17 (10) Å³
M_r = 656.39	Z = 8
Monoclinic, C2/c	Mo Kα radiation
a = 26.3310 (5) Å	µ = 9.93 mm⁻¹
b = 7.9632 (2) Å	T = 100 K
c = 12.7085 (3) Å	0.05 × 0.04 × 0.03 mm
β = 100.006 (1)°

Data collection top

Bruker APEXII CCD diffractometer	6379 independent reflections
Absorption correction: numerical (SADABS; Bruker, 2009)	5631 reflections with I > 2σ(I)
T_min = 0.341, T_max = 0.438	R_int = 0.038
30195 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	93 parameters
wR(F²) = 0.050	0 restraints
S = 1.33	Δρ_max = 0.98 e Å⁻³
6379 reflections	Δρ_min = −1.26 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cs1	0.16275 (2)	0.18961 (2)	0.30059 (2)	0.01108 (3)
Cs2	0.34717 (2)	0.18469 (2)	0.35501 (2)	0.01108 (3)
Cs3	0.44859 (2)	0.24984 (2)	0.06656 (2)	0.01686 (3)
Sc1	0.0000	0.22061 (6)	0.2500	0.00772 (8)
Sc2	0.2500	0.2500	0.0000	0.00814 (8)
Cl1	0.05410 (2)	0.00676 (6)	0.68924 (4)	0.01302 (9)
Cl2	0.05417 (2)	0.44314 (7)	0.18670 (4)	0.01398 (9)
Cl3	0.05588 (2)	0.22355 (7)	0.42769 (4)	0.01427 (9)
Cl4	0.18402 (2)	0.04527 (7)	0.03693 (4)	0.01557 (10)
Cl5	0.25017 (2)	0.38135 (6)	0.17777 (4)	0.01095 (8)
Cl6	0.32362 (2)	0.06505 (7)	0.07773 (4)	0.01453 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cs1	0.00923 (5)	0.01059 (5)	0.01374 (6)	0.00077 (4)	0.00290 (4)	0.00089 (4)
Cs2	0.01074 (5)	0.01019 (5)	0.01199 (5)	0.00125 (4)	0.00105 (4)	−0.00113 (4)
Cs3	0.01421 (6)	0.02189 (7)	0.01509 (6)	−0.00445 (5)	0.00429 (5)	−0.00546 (5)
Sc1	0.0070 (2)	0.0084 (2)	0.0079 (2)	0.000	0.00144 (15)	0.000
Sc2	0.0078 (2)	0.0085 (2)	0.0081 (2)	−0.00052 (17)	0.00125 (16)	0.00062 (15)
Cl1	0.0106 (2)	0.0126 (2)	0.0162 (2)	−0.00042 (16)	0.00327 (16)	0.00394 (16)
Cl2	0.0123 (2)	0.0132 (2)	0.0167 (2)	−0.00298 (17)	0.00332 (16)	0.00265 (16)
Cl3	0.0103 (2)	0.0224 (2)	0.00960 (19)	0.00063 (17)	0.00039 (15)	−0.00036 (16)
Cl4	0.0193 (2)	0.0146 (2)	0.0138 (2)	−0.00819 (18)	0.00558 (17)	−0.00093 (16)
Cl5	0.0111 (2)	0.01172 (19)	0.01018 (18)	−0.00123 (16)	0.00216 (14)	−0.00105 (14)
Cl6	0.0148 (2)	0.0147 (2)	0.0134 (2)	0.00510 (18)	0.00040 (16)	0.00119 (16)

Geometric parameters (Å, º) top

Cs1—Cl5ⁱ	3.3378 (5)	Cs3—Cl6	3.6297 (6)
Cs1—Cl1ⁱⁱ	3.3504 (5)	Cs3—Cl1^v	3.6702 (6)
Cs1—Cl6ⁱⁱⁱ	3.3564 (5)	Cs3—Cl3ⁱⁱⁱ	3.7752 (6)
Cs1—Cl5	3.3637 (5)	Cs3—Cl2^viii	3.8144 (6)
Cs1—Cl3	3.4900 (6)	Cs3—Cl1ⁱⁱⁱ	3.8312 (6)
Cs1—Cl4^iv	3.4998 (5)	Cs3—Cl4^vii	3.8714 (6)
Cs1—Cl2	3.5926 (5)	Cs3—Cl2ⁱ	3.9852 (6)
Cs1—Cl4	3.6762 (6)	Sc1—Cl3^ix	2.4718 (5)
Cs2—Cl4ⁱⁱⁱ	3.3463 (5)	Sc1—Cl3	2.4718 (5)
Cs2—Cl2ⁱ	3.3479 (5)	Sc1—Cl2^ix	2.4940 (6)
Cs2—Cl5	3.4714 (5)	Sc1—Cl2	2.4941 (6)
Cs2—Cl5ⁱ	3.4937 (5)	Sc1—Cl1^x	2.5072 (6)
Cs2—Cl3^v	3.4969 (5)	Sc1—Cl1ⁱⁱ	2.5072 (6)
Cs2—Cl6	3.5986 (5)	Sc2—Cl4^vii	2.4859 (5)
Cs2—Cl6^iv	3.6000 (6)	Sc2—Cl4	2.4859 (5)
Cs2—Cl1^v	3.6904 (5)	Sc2—Cl5	2.4889 (5)
Cs3—Cl1^vi	3.5216 (5)	Sc2—Cl5^vii	2.4889 (5)
Cs3—Cl2^vii	3.5559 (6)	Sc2—Cl6	2.4975 (5)
Cs3—Cl3^vi	3.5878 (6)	Sc2—Cl6^vii	2.4976 (5)

Cl5ⁱ—Cs1—Cl1ⁱⁱ	102.445 (13)	Cl1^x—Sc1—Cs3^xi	58.901 (12)
Cl5ⁱ—Cs1—Cl6ⁱⁱⁱ	126.886 (13)	Cl1ⁱⁱ—Sc1—Cs3^xi	126.341 (17)
Cl1ⁱⁱ—Cs1—Cl6ⁱⁱⁱ	128.714 (13)	Cs1—Sc1—Cs3^xi	108.888 (3)
Cl5ⁱ—Cs1—Cl5	81.739 (7)	Cs1^ix—Sc1—Cs3^xi	71.484 (3)
Cl1ⁱⁱ—Cs1—Cl5	128.226 (13)	Cl3^ix—Sc1—Cs3^vii	53.295 (13)
Cl6ⁱⁱⁱ—Cs1—Cl5	77.438 (13)	Cl3—Sc1—Cs3^vii	126.632 (13)
Cl5ⁱ—Cs1—Cl3	128.060 (13)	Cl2^ix—Sc1—Cs3^vii	122.186 (17)
Cl1ⁱⁱ—Cs1—Cl3	62.204 (12)	Cl2—Sc1—Cs3^vii	52.590 (12)
Cl6ⁱⁱⁱ—Cs1—Cl3	75.407 (14)	Cl1^x—Sc1—Cs3^vii	126.341 (17)
Cl5—Cs1—Cl3	148.367 (13)	Cl1ⁱⁱ—Sc1—Cs3^vii	58.901 (12)
Cl5ⁱ—Cs1—Cl4^iv	62.031 (12)	Cs1—Sc1—Cs3^vii	71.484 (3)
Cl1ⁱⁱ—Cs1—Cl4^iv	96.352 (14)	Cs1^ix—Sc1—Cs3^vii	108.888 (3)
Cl6ⁱⁱⁱ—Cs1—Cl4^iv	95.297 (13)	Cs3^xi—Sc1—Cs3^vii	173.961 (14)
Cl5—Cs1—Cl4^iv	128.348 (13)	Cl3^ix—Sc1—Cs3^xii	57.081 (16)
Cl3—Cs1—Cl4^iv	70.483 (13)	Cl3—Sc1—Cs3^xii	124.00 (2)
Cl5ⁱ—Cs1—Cl2	159.024 (12)	Cl2^ix—Sc1—Cs3^xii	128.462 (13)
Cl1ⁱⁱ—Cs1—Cl2	62.017 (12)	Cl2—Sc1—Cs3^xii	124.235 (13)
Cl6ⁱⁱⁱ—Cs1—Cl2	72.479 (13)	Cl1^x—Sc1—Cs3^xii	54.672 (15)
Cl5—Cs1—Cl2	96.823 (12)	Cl1ⁱⁱ—Sc1—Cs3^xii	51.268 (14)
Cl3—Cs1—Cl2	59.584 (12)	Cs1—Sc1—Cs3^xii	103.650 (8)
Cl4^iv—Cs1—Cl2	130.060 (13)	Cs1^ix—Sc1—Cs3^xii	70.532 (5)
Cl5ⁱ—Cs1—Cl4	68.521 (12)	Cs3^xi—Sc1—Cs3^xii	113.557 (8)
Cl1ⁱⁱ—Cs1—Cl4	73.931 (13)	Cs3^vii—Sc1—Cs3^xii	71.830 (5)
Cl6ⁱⁱⁱ—Cs1—Cl4	132.642 (13)	Cl3^ix—Sc1—Cs3ⁱ	124.00 (2)
Cl5—Cs1—Cl4	59.605 (12)	Cl3—Sc1—Cs3ⁱ	57.082 (16)
Cl3—Cs1—Cl4	135.140 (12)	Cl2^ix—Sc1—Cs3ⁱ	124.235 (13)
Cl4^iv—Cs1—Cl4	126.021 (7)	Cl2—Sc1—Cs3ⁱ	128.461 (13)
Cl2—Cs1—Cl4	92.585 (13)	Cl1^x—Sc1—Cs3ⁱ	51.268 (14)
Cl4ⁱⁱⁱ—Cs2—Cl2ⁱ	144.147 (14)	Cl1ⁱⁱ—Sc1—Cs3ⁱ	54.672 (15)
Cl4ⁱⁱⁱ—Cs2—Cl5	70.962 (12)	Cs1—Sc1—Cs3ⁱ	70.532 (5)
Cl2ⁱ—Cs2—Cl5	131.312 (13)	Cs1^ix—Sc1—Cs3ⁱ	103.650 (8)
Cl4ⁱⁱⁱ—Cs2—Cl5ⁱ	114.518 (14)	Cs3^xi—Sc1—Cs3ⁱ	71.830 (5)
Cl2ⁱ—Cs2—Cl5ⁱ	99.045 (13)	Cs3^vii—Sc1—Cs3ⁱ	113.557 (8)
Cl5—Cs2—Cl5ⁱ	78.039 (6)	Cs3^xii—Sc1—Cs3ⁱ	67.059 (8)
Cl4ⁱⁱⁱ—Cs2—Cl3^v	72.190 (13)	Cl4^vii—Sc2—Cl4	179.999 (18)
Cl2ⁱ—Cs2—Cl3^v	76.407 (13)	Cl4^vii—Sc2—Cl5	90.268 (17)
Cl5—Cs2—Cl3^v	140.539 (13)	Cl4—Sc2—Cl5	89.731 (17)
Cl5ⁱ—Cs2—Cl3^v	131.180 (12)	Cl4^vii—Sc2—Cl5^vii	89.730 (17)
Cl4ⁱⁱⁱ—Cs2—Cl6	128.042 (13)	Cl4—Sc2—Cl5^vii	90.271 (17)
Cl2ⁱ—Cs2—Cl6	72.498 (12)	Cl5—Sc2—Cl5^vii	180.0
Cl5—Cs2—Cl6	60.126 (12)	Cl4^vii—Sc2—Cl6	86.646 (19)
Cl5ⁱ—Cs2—Cl6	72.674 (12)	Cl4—Sc2—Cl6	93.354 (19)
Cl3^v—Cs2—Cl6	143.761 (13)	Cl5—Sc2—Cl6	90.573 (16)
Cl4ⁱⁱⁱ—Cs2—Cl6^iv	93.629 (13)	Cl5^vii—Sc2—Cl6	89.427 (16)
Cl2ⁱ—Cs2—Cl6^iv	92.949 (14)	Cl4^vii—Sc2—Cl6^vii	93.356 (19)
Cl5—Cs2—Cl6^iv	123.475 (13)	Cl4—Sc2—Cl6^vii	86.644 (19)
Cl5ⁱ—Cs2—Cl6^iv	59.259 (11)	Cl5—Sc2—Cl6^vii	89.427 (16)
Cl3^v—Cs2—Cl6^iv	72.323 (12)	Cl5^vii—Sc2—Cl6^vii	90.574 (16)
Cl6—Cs2—Cl6^iv	126.850 (7)	Cl6—Sc2—Cl6^vii	180.0
Cl4ⁱⁱⁱ—Cs2—Cl1^v	73.789 (14)	Cl4^vii—Sc2—Cs1ⁱⁱ	132.946 (12)
Cl2ⁱ—Cs2—Cl1^v	76.813 (13)	Cl4—Sc2—Cs1ⁱⁱ	47.055 (12)
Cl5—Cs2—Cl1^v	93.390 (12)	Cl5—Sc2—Cs1ⁱⁱ	136.773 (12)
Cl5ⁱ—Cs2—Cl1^v	164.523 (12)	Cl5^vii—Sc2—Cs1ⁱⁱ	43.228 (12)
Cl3^v—Cs2—Cl1^v	62.887 (12)	Cl6—Sc2—Cs1ⁱⁱ	92.711 (13)
Cl6—Cs2—Cl1^v	91.899 (13)	Cl6^vii—Sc2—Cs1ⁱⁱ	87.288 (13)
Cl6^iv—Cs2—Cl1^v	135.208 (12)	Cl4^vii—Sc2—Cs1ⁱⁱⁱ	47.054 (12)
Cl1^vi—Cs3—Cl2^vii	121.939 (13)	Cl4—Sc2—Cs1ⁱⁱⁱ	132.945 (12)
Cl1^vi—Cs3—Cl3^vi	63.717 (12)	Cl5—Sc2—Cs1ⁱⁱⁱ	43.227 (12)
Cl2^vii—Cs3—Cl3^vi	58.283 (12)	Cl5^vii—Sc2—Cs1ⁱⁱⁱ	136.772 (12)
Cl1^vi—Cs3—Cl6	148.943 (13)	Cl6—Sc2—Cs1ⁱⁱⁱ	87.289 (13)
Cl2^vii—Cs3—Cl6	89.091 (12)	Cl6^vii—Sc2—Cs1ⁱⁱⁱ	92.712 (13)
Cl3^vi—Cs3—Cl6	147.118 (12)	Cs1ⁱⁱ—Sc2—Cs1ⁱⁱⁱ	180.0
Cl1^vi—Cs3—Cl1^v	57.631 (15)	Sc1^x—Cl1—Cs1^iv	91.260 (16)
Cl2^vii—Cs3—Cl1^v	173.337 (13)	Sc1^x—Cl1—Cs3^xi	94.994 (16)
Cl3^vi—Cs3—Cl1^v	121.151 (12)	Cs1^iv—Cl1—Cs3^xi	173.698 (17)
Cl6—Cs3—Cl1^v	91.731 (12)	Sc1^x—Cl1—Cs3^v	91.457 (16)
Cl1^vi—Cs3—Cl3ⁱⁱⁱ	57.741 (11)	Cs1^iv—Cl1—Cs3^v	91.711 (12)
Cl2^vii—Cs3—Cl3ⁱⁱⁱ	116.971 (12)	Cs3^xi—Cl1—Cs3^v	87.364 (13)
Cl3^vi—Cs3—Cl3ⁱⁱⁱ	88.872 (13)	Sc1^x—Cl1—Cs2^v	168.727 (19)
Cl6—Cs3—Cl3ⁱⁱⁱ	111.892 (12)	Cs1^iv—Cl1—Cs2^v	78.623 (11)
Cl1^v—Cs3—Cl3ⁱⁱⁱ	56.679 (11)	Cs3^xi—Cl1—Cs2^v	95.079 (12)
Cl1^vi—Cs3—Cl2^viii	73.210 (12)	Cs3^v—Cl1—Cs2^v	83.964 (11)
Cl2^vii—Cs3—Cl2^viii	89.108 (12)	Sc1^x—Cl1—Cs3ⁱ	87.017 (15)
Cl3^vi—Cs3—Cl2^viii	69.717 (12)	Cs1^iv—Cl1—Cs3ⁱ	89.870 (13)
Cl6—Cs3—Cl2^viii	109.110 (12)	Cs3^xi—Cl1—Cs3ⁱ	91.227 (12)
Cl1^v—Cs3—Cl2^viii	96.862 (12)	Cs3^v—Cl1—Cs3ⁱ	177.828 (16)
Cl3ⁱⁱⁱ—Cs3—Cl2^viii	130.920 (11)	Cs2^v—Cl1—Cs3ⁱ	97.813 (13)
Cl1^vi—Cs3—Cl1ⁱⁱⁱ	88.772 (12)	Sc1—Cl2—Cs2ⁱⁱⁱ	164.21 (2)
Cl2^vii—Cs3—Cl1ⁱⁱⁱ	57.881 (12)	Sc1—Cl2—Cs3^vii	93.554 (16)
Cl3^vi—Cs3—Cl1ⁱⁱⁱ	56.711 (11)	Cs2ⁱⁱⁱ—Cl2—Cs3^vii	89.963 (13)
Cl6—Cs3—Cl1ⁱⁱⁱ	111.495 (11)	Sc1—Cl2—Cs1	86.012 (16)
Cl1^v—Cs3—Cl1ⁱⁱⁱ	115.801 (4)	Cs2ⁱⁱⁱ—Cl2—Cs1	78.554 (11)
Cl3ⁱⁱⁱ—Cs3—Cl1ⁱⁱⁱ	59.122 (11)	Cs3^vii—Cl2—Cs1	90.658 (13)
Cl2^viii—Cs3—Cl1ⁱⁱⁱ	125.895 (12)	Sc1—Cl2—Cs3^xiii	99.566 (17)
Cl1^vi—Cs3—Cl4^vii	120.934 (12)	Cs2ⁱⁱⁱ—Cl2—Cs3^xiii	95.760 (13)
Cl2^vii—Cs3—Cl4^vii	89.959 (12)	Cs3^vii—Cl2—Cs3^xiii	90.890 (12)
Cl3^vi—Cs3—Cl4^vii	123.282 (12)	Cs1—Cl2—Cs3^xiii	174.107 (16)
Cl6—Cs3—Cl4^vii	54.119 (11)	Sc1—Cl2—Cs3ⁱⁱⁱ	95.280 (17)
Cl1^v—Cs3—Cl4^vii	85.176 (11)	Cs2ⁱⁱⁱ—Cl2—Cs3ⁱⁱⁱ	83.870 (12)
Cl3ⁱⁱⁱ—Cs3—Cl4^vii	63.654 (11)	Cs3^vii—Cl2—Cs3ⁱⁱⁱ	167.614 (16)
Cl2^viii—Cs3—Cl4^vii	163.219 (12)	Cs1—Cl2—Cs3ⁱⁱⁱ	98.594 (12)
Cl1ⁱⁱⁱ—Cs3—Cl4^vii	66.677 (11)	Cs3^xiii—Cl2—Cs3ⁱⁱⁱ	79.100 (11)
Cl1^vi—Cs3—Cl2ⁱ	96.304 (12)	Sc1—Cl3—Cs1	88.641 (15)
Cl2^vii—Cs3—Cl2ⁱ	116.554 (5)	Sc1—Cl3—Cs2^v	163.83 (2)
Cl3^vi—Cs3—Cl2ⁱ	123.146 (12)	Cs1—Cl3—Cs2^v	81.079 (11)
Cl6—Cs3—Cl2ⁱ	65.179 (11)	Sc1—Cl3—Cs3^xi	93.175 (15)
Cl1^v—Cs3—Cl2ⁱ	69.674 (11)	Cs1—Cl3—Cs3^xi	177.893 (16)
Cl3ⁱⁱⁱ—Cs3—Cl2ⁱ	126.317 (11)	Cs2^v—Cl3—Cs3^xi	97.376 (13)
Cl2^viii—Cs3—Cl2ⁱ	53.436 (15)	Sc1—Cl3—Cs3ⁱ	89.577 (19)
Cl1ⁱⁱⁱ—Cs3—Cl2ⁱ	174.105 (11)	Cs1—Cl3—Cs3ⁱ	87.819 (13)
Cl4^vii—Cs3—Cl2ⁱ	112.763 (11)	Cs2^v—Cl3—Cs3ⁱ	102.381 (13)
Cl3^ix—Sc1—Cl3	178.91 (4)	Cs3^xi—Cl3—Cs3ⁱ	91.125 (13)
Cl3^ix—Sc1—Cl2^ix	90.284 (19)	Sc2—Cl4—Cs2ⁱ	150.42 (2)
Cl3—Sc1—Cl2^ix	88.945 (19)	Sc2—Cl4—Cs1ⁱⁱ	101.617 (17)
Cl3^ix—Sc1—Cl2	88.945 (19)	Cs2ⁱ—Cl4—Cs1ⁱⁱ	83.078 (12)
Cl3—Sc1—Cl2	90.28 (2)	Sc2—Cl4—Cs1	100.906 (16)
Cl2^ix—Sc1—Cl2	89.45 (3)	Cs2ⁱ—Cl4—Cs1	78.879 (11)
Cl3^ix—Sc1—Cl1^x	90.480 (19)	Cs1ⁱⁱ—Cl4—Cs1	157.264 (17)
Cl3—Sc1—Cl1^x	90.306 (19)	Sc2—Cl4—Cs3^vii	106.150 (17)
Cl2^ix—Sc1—Cl1^x	91.511 (18)	Cs2ⁱ—Cl4—Cs3^vii	103.290 (14)
Cl2—Sc1—Cl1^x	178.89 (2)	Cs1ⁱⁱ—Cl4—Cs3^vii	86.175 (12)
Cl3^ix—Sc1—Cl1ⁱⁱ	90.305 (19)	Cs1—Cl4—Cs3^vii	84.641 (13)
Cl3—Sc1—Cl1ⁱⁱ	90.479 (19)	Sc2—Cl5—Cs1ⁱⁱⁱ	106.063 (17)
Cl2^ix—Sc1—Cl1ⁱⁱ	178.89 (2)	Sc2—Cl5—Cs1	109.697 (16)
Cl2—Sc1—Cl1ⁱⁱ	91.510 (18)	Cs1ⁱⁱⁱ—Cl5—Cs1	144.225 (16)
Cl1^x—Sc1—Cl1ⁱⁱ	87.54 (3)	Sc2—Cl5—Cs2	106.525 (16)
Cl3^ix—Sc1—Cs1	124.476 (13)	Cs1ⁱⁱⁱ—Cl5—Cs2	82.000 (11)
Cl3—Sc1—Cs1	55.599 (13)	Cs1—Cl5—Cs2	88.842 (12)
Cl2^ix—Sc1—Cs1	127.855 (17)	Sc2—Cl5—Cs2ⁱⁱⁱ	107.265 (15)
Cl2—Sc1—Cs1	57.945 (12)	Cs1ⁱⁱⁱ—Cl5—Cs2ⁱⁱⁱ	88.886 (12)
Cl1^x—Sc1—Cs1	121.740 (17)	Cs1—Cl5—Cs2ⁱⁱⁱ	79.759 (11)
Cl1ⁱⁱ—Sc1—Cs1	52.385 (11)	Cs2—Cl5—Cs2ⁱⁱⁱ	146.210 (15)
Cl3^ix—Sc1—Cs1^ix	55.600 (13)	Sc2—Cl6—Cs1ⁱ	136.14 (2)
Cl3—Sc1—Cs1^ix	124.478 (13)	Sc2—Cl6—Cs2	102.768 (17)
Cl2^ix—Sc1—Cs1^ix	57.945 (12)	Cs1ⁱ—Cl6—Cs2	78.359 (11)
Cl2—Sc1—Cs1^ix	127.855 (17)	Sc2—Cl6—Cs2ⁱⁱ	104.044 (16)
Cl1^x—Sc1—Cs1^ix	52.385 (11)	Cs1ⁱ—Cl6—Cs2ⁱⁱ	81.426 (12)
Cl1ⁱⁱ—Sc1—Cs1^ix	121.740 (17)	Cs2—Cl6—Cs2ⁱⁱ	153.152 (16)
Cs1—Sc1—Cs1^ix	173.309 (14)	Sc2—Cl6—Cs3	113.085 (18)
Cl3^ix—Sc1—Cs3^xi	126.634 (13)	Cs1ⁱ—Cl6—Cs3	110.735 (14)
Cl3—Sc1—Cs3^xi	53.296 (13)	Cs2—Cl6—Cs3	85.863 (12)
Cl2^ix—Sc1—Cs3^xi	52.590 (13)	Cs2ⁱⁱ—Cl6—Cs3	84.957 (13)
Cl2—Sc1—Cs3^xi	122.185 (17)

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

Experimental details

Crystal data
Chemical formula	Cs₃ScCl₆
M_r	656.39
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	100
a, b, c (Å)	26.3310 (5), 7.9632 (2), 12.7085 (3)
β (°)	100.006 (1)
V (Å³)	2624.17 (10)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	9.93
Crystal size (mm)	0.05 × 0.04 × 0.03

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Numerical (SADABS; Bruker, 2009)
T_min, T_max	0.341, 0.438
No. of measured, independent and observed [I > 2σ(I)] reflections	30195, 6379, 5631
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.834

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.050, 1.33
No. of reflections	6379
No. of parameters	93
Δρ_max, Δρ_min (e Å⁻³)	0.98, −1.26

Computer programs: APEX2 (Bruker, 2009), SAINT-Plus (Bruker, 2009), SHELXS2014 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2008), CrystalMaker (Palmer, 2013).

Acknowledgements

Use was made of the IMSERC X-ray facility at Northwestern University, supported by the International Institute of Nanotechnology.

References

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