Penta­potassium europium(III) dilithium deca­fluoride, K5EuLi2F10

Gagor, A.

doi:10.1107/S1600536809044055

inorganic compounds

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Volume 65| Part 11| November 2009| Page i82

https://doi.org/10.1107/S1600536809044055

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Pentapotassium europium(III) dilithium decafluoride, K₅EuLi₂F₁₀

Anna Gagor ^a ^*

^aW. Trzebiatowski Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Okólna str. 2, PO Box 1410, 50-950 Wrocław, Poland
^*Correspondence e-mail: a.gagor@int.pan.wroc.pl

(Received 13 October 2009; accepted 23 October 2009; online 28 October 2009)

The title compound, K₅EuLi₂F₁₀, belongs to so-called self-activated materials containing lanthanoid ions within the matrix. A common feature of these systems is a large separation between the closest lanthanoid ions, which is one of the crucial factors governing the self-quenching of luminescence. The crystal structure of K₅EuLi₂F₁₀ is isotypic with other K₅RELi₂F₁₀ compounds (RE = Nd, Pr). As expected from the lanthanoid contraction, the unit-cell volume for crystal with Eu³⁺ ions is the smallest of the three structures. Accordingly, the corresponding interatomic RE—RE distances are shorter. In the structure, distorted EuF₈ dodecahedra and two different LiF₄ tetrahedra, all with m symmetry, are present, forming sheets parallel to (100). The isolated EuF₈ dodecahedra exhibit a mean Eu—F distance of 2.356 Å. The K⁺ cations are located within and between the sheets, leading to highly irregular KF_x polyhedra (x = 8–9) around the alkali metal cations.

Related literature

The structure of the isotypic Nd analogue was reported by Hong & McCollum (1979 ); for the structure of the Pr analogue, see: Gagor (2009 ). For background to bond-valence calculations, see: Brown (1992 , 2002 ); Mattausch et al. (1991 ). Synthetic details were described by Ryba-Romanowski et al. (2007 ).

Experimental

Crystal data

K₅EuLi₂F₁₀
M_r = 551.35
Orthorhombic, P n m a
a = 20.5539 (6) Å
b = 7.7356 (2) Å
c = 6.8721 (2) Å
V = 1092.64 (5) Å³
Z = 4
Mo Kα radiation
μ = 7.75 mm⁻¹
T = 295 K
0.35 × 0.20 × 0.15 mm

Data collection

Kuma KM-4 with CCD area-detector diffractometer
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.146, T_max = 0.310
23852 measured reflections
4895 independent reflections
3564 reflections with I > 2σ(I)
R_int = 0.034

Refinement

R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.039
S = 0.83
4895 reflections
98 parameters
Δρ_max = 2.35 e Å⁻³
Δρ_min = −3.02 e Å⁻³

Table 1
Selected bond lengths (Å)

Eu1—F5	2.2923 (11)
Eu1—F2	2.3236 (11)
Eu1—F3ⁱ	2.3262 (7)
Eu1—F1	2.3918 (10)
Eu1—F4	2.3954 (7)
Eu1—F8ⁱⁱ	2.3996 (10)
Li1—F6ⁱⁱⁱ	1.804 (3)
Li1—F1^iv	1.862 (3)
Li1—F3^v	1.8669 (16)
Li2—F7	1.801 (4)
Li2—F4ⁱⁱⁱ	1.817 (2)
Li2—F8	1.844 (3)
Symmetry codes: (i) x, y-1, z; (ii) $[x-{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iii) $[x+{\script{1\over 2}}, y, -z+{\script{3\over 2}}]$ ; (iv) x+1, y, z+1; (v) -x+1, -y+1, -z+1.

Data collection: CrysAlis CCD (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2006 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536809044055/wm2269sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809044055/wm2269Isup2.hkl

checkCIF report

Comment top

Two different LiF₄ tetrahedra together with EuF₈ dodecahedra form sheets expanding perpendicular to [100]. Fig. 1 illustrates the crystal packing of K₅EuLi₂F₁₀ as seen down [001]. K1 atoms occupy cavities within the sheets and are surrounded by 9 F^- ions in a mean distance of 2.792 Å. Remaining potassium atoms are located between the sheets, leading to KF₉ and KF₈ polyhedra. The valence sums of K atoms are close to the formal charge of +1, with a slight tendency to over-bonding. The K2 ion in the K₅EuLi₂F₁₀ structure is slightly under-bonded (S = 0.977 v.u.), whereas the Li position is over-bonded, with a 15.6% higher bond-valence sum than those expected from the formal charge of +1.

Each EuF₈ dodecahedron is surrounded by twelve others with a shortest and longest Eu—Eu distance of 6.6968 (2) and 7.8353 (2) Å, respectively. The mean distance of Eu—Eu is 7.309 Å, with individual distances of 2× 6.6968 (2), 2× 6.8805 (2), 2× 6.8721 (2), 2× 7.7356 (2) and 4× 7.8353 (2) Å. The bond valence sums of all metal atoms have been calculated from the received structure model on the basis of the bond-valence method (Brown, 1992, 2002; Mattausch et al., 1991)]: Eu 2.81, K1 1.06, K2 1.00, K3 1.09 and Li 1.16 v.u. The Eu ion is slightly under-bonded. The lower value of Eu valence may be associated with the distorted surrounding of this cation. When such distortions occur, the equal-valence rule is not strictly obeyed (Brown, 1992).

Related literature top

The structure of the isotypic Nd analogue was reported by Hong & McCollum (1979); for the structure of the Pr analogue, see: Gagor (2009). For background to bond-valence calculations, see: Brown (1992, 2002); Mattausch et al. (1991). Synthetic details were described by Ryba-Romanowski et al. (2007).

Experimental top

Preparation details were taken from Ryba-Romanowski et al. (2007). The K₅EuLi₂F₁₀ crystal was grown from commercially available KF, EuF3 and LiF (Aldrich 99.99%, anhydrous) using the Bridgman method. The reagents were heated at 923 K (melting point 813 K) in a graphite crucible under argon atmosphere. The pulling rate was 1mm/h, the temperature gradient 100 %/cm.

Structure description top

The structure of the isotypic Nd analogue was reported by Hong & McCollum (1979); for the structure of the Pr analogue, see: Gagor (2009). For background to bond-valence calculations, see: Brown (1992, 2002); Mattausch et al. (1991). Synthetic details were described by Ryba-Romanowski et al. (2007).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. Crystal packing in K₅EuLi₂F₁₀ as seen down the c axis. The thermal ellipsoids have been drawn at the 50% probability level.

Pentapotassium europium(III) dilithium decafluoride top

Crystal data top

K₅EuLi₂F₁₀	F(000) = 1016
M_r = 551.35	D_x = 3.352 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 12717 reflections
a = 20.5539 (6) Å	θ = 2.8–47.0°
b = 7.7356 (2) Å	µ = 7.75 mm⁻¹
c = 6.8721 (2) Å	T = 295 K
V = 1092.64 (5) Å³	Rectangular prism, colorless
Z = 4	0.35 × 0.20 × 0.15 mm

Data collection top

Kuma KM-4 with CCD area-detector diffractometer	4895 independent reflections
Radiation source: fine-focus sealed tube	3564 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm^-1	θ_max = 47.2°, θ_min = 3.1°
ω scans	h = −42→27
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	k = −11→15
T_min = 0.146, T_max = 0.310	l = −14→9
23852 measured reflections

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)] = 0.021	w = 1/[σ²(F_o²) + (0.02P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.039	(Δ/σ)_max = 0.001
S = 0.83	Δρ_max = 2.35 e Å⁻³
4895 reflections	Δρ_min = −3.02 e Å⁻³
98 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0234 (3)

Crystal data top

K₅EuLi₂F₁₀	V = 1092.64 (5) Å³
M_r = 551.35	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 20.5539 (6) Å	µ = 7.75 mm⁻¹
b = 7.7356 (2) Å	T = 295 K
c = 6.8721 (2) Å	0.35 × 0.20 × 0.15 mm

Data collection top

Kuma KM-4 with CCD area-detector diffractometer	4895 independent reflections
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	3564 reflections with I > 2σ(I)
T_min = 0.146, T_max = 0.310	R_int = 0.034
23852 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	98 parameters
wR(F²) = 0.039	0 restraints
S = 0.83	Δρ_max = 2.35 e Å⁻³
4895 reflections	Δρ_min = −3.02 e Å⁻³

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.

To eliminate the weak reflections measured at high theta angles a 2theta limit was applied during structure refinement. The refinement on the whole data set (2theta = 47°) only slightly improved the standard deviations. Concluding, it was decided to refine the structure using a maximum measured 2theta limit. For completeness calculations the 2theta threshold was set to 28.

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

	x	y	z	U_iso*/U_eq
K1	0.457104 (13)	0.97833 (4)	0.25084 (4)	0.01525 (4)
K2	0.282845 (14)	0.02578 (4)	0.42686 (4)	0.01675 (5)
K3	0.36036 (2)	0.2500	0.93720 (6)	0.01762 (7)
Eu1	0.106855 (4)	0.2500	0.236787 (10)	0.00739 (2)
Li1	0.92238 (15)	0.2500	0.9701 (4)	0.0131 (5)
Li2	0.67290 (16)	0.2500	0.8419 (5)	0.0143 (6)
F1	0.00915 (5)	0.2500	0.04773 (15)	0.01369 (18)
F2	0.01991 (5)	0.2500	0.45288 (15)	0.0174 (2)
F3	0.09032 (4)	0.96151 (9)	0.15506 (12)	0.01698 (15)
F4	0.14639 (4)	0.07571 (10)	0.49951 (11)	0.01549 (14)
F5	0.21739 (5)	0.2500	0.19250 (16)	0.0167 (2)
F6	0.37353 (6)	0.2500	0.31189 (16)	0.01580 (19)
F7	0.75888 (5)	0.2500	0.79160 (15)	0.0160 (2)
F8	0.63085 (5)	0.2500	0.60493 (14)	0.01447 (19)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K1	0.01483 (10)	0.01435 (10)	0.01657 (10)	−0.00139 (8)	−0.00065 (9)	−0.00117 (9)
K2	0.01782 (11)	0.01449 (11)	0.01795 (10)	0.00145 (9)	−0.00036 (9)	−0.00152 (9)
K3	0.0292 (2)	0.01074 (15)	0.01291 (14)	0.000	−0.00250 (14)	0.000
Eu1	0.00789 (3)	0.00732 (3)	0.00696 (3)	0.000	−0.00052 (3)	0.000
Li1	0.0131 (13)	0.0150 (14)	0.0112 (12)	0.000	0.0005 (11)	0.000
Li2	0.0160 (15)	0.0147 (14)	0.0121 (12)	0.000	0.0002 (11)	0.000
F1	0.0096 (4)	0.0171 (5)	0.0144 (4)	0.000	−0.0018 (4)	0.000
F2	0.0163 (5)	0.0221 (5)	0.0138 (4)	0.000	0.0025 (4)	0.000
F3	0.0219 (4)	0.0108 (3)	0.0183 (3)	−0.0001 (3)	−0.0047 (3)	−0.0029 (3)
F4	0.0222 (4)	0.0104 (3)	0.0139 (3)	−0.0007 (3)	−0.0029 (3)	−0.0009 (3)
F5	0.0106 (4)	0.0228 (5)	0.0168 (4)	0.000	−0.0014 (4)	0.000
F6	0.0150 (5)	0.0197 (5)	0.0127 (4)	0.000	−0.0028 (4)	0.000
F7	0.0129 (5)	0.0203 (5)	0.0147 (4)	0.000	0.0011 (4)	0.000
F8	0.0134 (4)	0.0205 (5)	0.0095 (4)	0.000	−0.0012 (4)	0.000

Geometric parameters (Å, º) top

K1—F8ⁱ	2.7148 (9)	Eu1—F5	2.2923 (11)
K1—F1ⁱⁱ	2.7344 (7)	Eu1—F2	2.3236 (11)
K1—F2ⁱⁱⁱ	2.7451 (9)	Eu1—F3^xviii	2.3262 (7)
K1—F6^iv	2.7465 (8)	Eu1—F3^xix	2.3262 (7)
K1—F4ⁱⁱⁱ	2.7718 (8)	Eu1—F1	2.3918 (10)
K1—F1^v	2.7863 (8)	Eu1—F4^xx	2.3954 (7)
K1—F3^vi	2.8163 (9)	Eu1—F4	2.3954 (7)
K1—F2ⁱⁱ	2.8359 (8)	Eu1—F8^xxi	2.3996 (10)
K1—Li1^vii	2.933 (2)	Eu1—Li2^x	3.198 (3)
K1—F3^viii	2.9804 (8)	Li1—F6^xvii	1.804 (3)
K1—Li2ⁱ	3.266 (3)	Li1—F1^xxii	1.862 (3)
K1—Li1^ix	3.395 (3)	Li1—F3ⁱ	1.8669 (16)
K2—F7^x	2.6446 (8)	Li1—F3^xxiii	1.8669 (16)
K2—F6	2.6658 (10)	Li1—K1^xxiv	2.933 (2)
K2—F5	2.7225 (9)	Li1—K1^xxv	2.933 (2)
K2—F7^xi	2.7460 (7)	Li1—K3^xvii	3.076 (3)
K2—F8^xi	2.7831 (7)	Li1—K1^xxvi	3.395 (3)
K2—F5^xii	2.8078 (8)	Li1—K1^xxvii	3.395 (3)
K2—F4	2.8748 (8)	Li1—K2^xvii	3.426 (3)
K2—Li2^xi	2.965 (2)	Li1—K2^xxviii	3.426 (3)
K2—F3^v	3.0440 (9)	Li2—F7	1.801 (4)
K2—Li2^x	3.262 (3)	Li2—F4^xvii	1.817 (2)
K2—F4^xiii	3.3700 (8)	Li2—F4^xxviii	1.817 (2)
K2—Li1^x	3.426 (3)	Li2—F8	1.844 (3)
K3—F4^xii	2.5594 (8)	Li2—K2^xi	2.965 (2)
K3—F4^xiv	2.5594 (8)	Li2—K2^xxix	2.965 (2)
K3—F6^xv	2.5891 (11)	Li2—Eu1^xvii	3.198 (3)
K3—F7^x	2.6119 (11)	Li2—K2^xxviii	3.262 (3)
K3—F3^v	2.7320 (8)	Li2—K2^xvii	3.262 (3)
K3—F3^xvi	2.7320 (8)	Li2—K1ⁱ	3.266 (3)
K3—Li1^x	3.076 (3)	Li2—K1^xxiii	3.266 (3)
K3—F2^xvii	3.3652 (12)

F8ⁱ—K1—F1ⁱⁱ	125.15 (3)	F3ⁱ—Li1—F3^xxiii	122.43 (17)
F8ⁱ—K1—F2ⁱⁱⁱ	88.19 (3)	F7—Li2—F4^xvii	114.17 (13)
F1ⁱⁱ—K1—F2ⁱⁱⁱ	143.59 (3)	F7—Li2—F4^xxviii	114.17 (13)
F8ⁱ—K1—F6^iv	91.46 (3)	F4^xvii—Li2—F4^xxviii	95.80 (16)
F1ⁱⁱ—K1—F6^iv	65.12 (3)	F7—Li2—F8	106.88 (17)
F2ⁱⁱⁱ—K1—F6^iv	135.55 (3)	F4^xvii—Li2—F8	112.90 (13)
F8ⁱ—K1—F4ⁱⁱⁱ	67.56 (3)	F4^xxviii—Li2—F8	112.90 (13)
F1ⁱⁱ—K1—F4ⁱⁱⁱ	137.02 (3)	F7—Li2—K2^xi	65.12 (8)
F2ⁱⁱⁱ—K1—F4ⁱⁱⁱ	64.55 (3)	F4^xvii—Li2—K2^xi	86.08 (4)
F6^iv—K1—F4ⁱⁱⁱ	74.37 (3)	F4^xxviii—Li2—K2^xi	178.10 (12)
F8ⁱ—K1—F1^v	59.07 (3)	F8—Li2—K2^xi	66.01 (8)
F1ⁱⁱ—K1—F1^v	91.096 (10)	F7—Li2—K2^xxix	65.12 (8)
F2ⁱⁱⁱ—K1—F1^v	95.48 (2)	F4^xvii—Li2—K2^xxix	178.10 (12)
F6^iv—K1—F1^v	121.93 (3)	F4^xxviii—Li2—K2^xxix	86.08 (4)
F4ⁱⁱⁱ—K1—F1^v	123.48 (2)	F8—Li2—K2^xxix	66.01 (8)
F8ⁱ—K1—F3^vi	122.24 (3)	K2^xi—Li2—K2^xxix	92.03 (9)
F1ⁱⁱ—K1—F3^vi	62.54 (2)	Li1^xxx—F1—Eu1	163.75 (11)
F2ⁱⁱⁱ—K1—F3^vi	88.52 (3)	Li1^xxx—F1—K1^xxxi	76.71 (6)
F6^iv—K1—F3^vi	127.47 (3)	Eu1—F1—K1^xxxi	93.07 (3)
F4ⁱⁱⁱ—K1—F3^vi	151.91 (2)	Li1^xxx—F1—K1^xxxii	76.71 (6)
F1^v—K1—F3^vi	63.93 (3)	Eu1—F1—K1^xxxii	93.07 (3)
F8ⁱ—K1—F2ⁱⁱ	164.89 (3)	K1^xxxi—F1—K1^xxxii	100.45 (3)
F1ⁱⁱ—K1—F2ⁱⁱ	60.15 (3)	Li1^xxx—F1—K1ⁱⁱⁱ	91.64 (8)
F2ⁱⁱⁱ—K1—F2ⁱⁱ	91.732 (11)	Eu1—F1—K1ⁱⁱⁱ	100.88 (3)
F6^iv—K1—F2ⁱⁱ	78.06 (3)	K1^xxxi—F1—K1ⁱⁱⁱ	88.904 (10)
F4ⁱⁱⁱ—K1—F2ⁱⁱ	98.83 (3)	K1^xxxii—F1—K1ⁱⁱⁱ	162.80 (4)
F1^v—K1—F2ⁱⁱ	135.88 (3)	Li1^xxx—F1—K1^xxxiii	91.64 (8)
F3^vi—K1—F2ⁱⁱ	72.85 (3)	Eu1—F1—K1^xxxiii	100.88 (3)
F8ⁱ—K1—F3^viii	62.84 (2)	K1^xxxi—F1—K1^xxxiii	162.80 (4)
F1ⁱⁱ—K1—F3^viii	62.36 (3)	K1^xxxii—F1—K1^xxxiii	88.904 (10)
F2ⁱⁱⁱ—K1—F3^viii	148.43 (2)	K1ⁱⁱⁱ—F1—K1^xxxiii	78.68 (3)
F6^iv—K1—F3^viii	62.20 (3)	Eu1—F2—K1^xvi	110.14 (3)
F4ⁱⁱⁱ—K1—F3^viii	110.69 (2)	Eu1—F2—K1^v	110.14 (3)
F1^v—K1—F3^viii	59.86 (2)	K1^xvi—F2—K1^v	80.09 (3)
F3^vi—K1—F3^viii	96.38 (2)	Eu1—F2—K1^xxxi	91.98 (3)
F2ⁱⁱ—K1—F3^viii	119.55 (2)	K1^xvi—F2—K1^xxxi	157.42 (4)
Li1^vii—K1—F3^viii	36.79 (4)	K1^v—F2—K1^xxxi	88.268 (11)
F8ⁱ—K1—Li2ⁱ	34.37 (6)	Eu1—F2—K1^xxxii	91.98 (3)
F7^x—K2—F6	85.43 (3)	K1^xvi—F2—K1^xxxii	88.268 (11)
F7^x—K2—F5	85.58 (3)	K1^v—F2—K1^xxxii	157.42 (4)
F6—K2—F5	75.86 (3)	K1^xxxi—F2—K1^xxxii	95.64 (3)
F7^x—K2—F7^xi	148.354 (19)	Eu1—F2—K3^x	153.25 (4)
F6—K2—F7^xi	124.18 (3)	K1^xvi—F2—K3^x	90.02 (3)
F5—K2—F7^xi	90.98 (2)	K1^v—F2—K3^x	90.02 (3)
F7^x—K2—F8^xi	132.75 (3)	K1^xxxi—F2—K3^x	70.57 (2)
F6—K2—F8^xi	91.71 (2)	K1^xxxii—F2—K3^x	70.57 (2)
F5—K2—F8^xi	139.19 (3)	Li1ⁱ—F3—Eu1^iv	166.53 (9)
F7^xi—K2—F8^xi	63.94 (3)	Li1ⁱ—F3—K3ⁱⁱⁱ	81.61 (9)
F7^x—K2—F5^xii	91.28 (2)	Eu1^iv—F3—K3ⁱⁱⁱ	110.42 (3)
F6—K2—F5^xii	133.49 (3)	Li1ⁱ—F3—K1^xxi	90.59 (10)
F5—K2—F5^xii	150.205 (12)	Eu1^iv—F3—K1^xxi	92.43 (3)
F7^xi—K2—F5^xii	76.39 (3)	K3ⁱⁱⁱ—F3—K1^xxi	103.03 (3)
F8^xi—K2—F5^xii	57.98 (3)	Li1ⁱ—F3—K1^xxxiv	70.22 (9)
F7^x—K2—F4	66.62 (3)	Eu1^iv—F3—K1^xxxiv	97.07 (3)
F6—K2—F4	130.25 (2)	K3ⁱⁱⁱ—F3—K1^xxxiv	151.20 (3)
F5—K2—F4	62.29 (3)	K1^xxi—F3—K1^xxxiv	83.62 (2)
F7^xi—K2—F4	83.95 (3)	Li1ⁱ—F3—K2ⁱⁱⁱ	84.87 (10)
F8^xi—K2—F4	137.60 (2)	Eu1^iv—F3—K2ⁱⁱⁱ	88.18 (3)
F5^xii—K2—F4	89.28 (3)	K3ⁱⁱⁱ—F3—K2ⁱⁱⁱ	93.85 (3)
F7^x—K2—F3^v	76.20 (3)	K1^xxi—F3—K2ⁱⁱⁱ	161.70 (3)
F6—K2—F3^v	62.15 (3)	K1^xxxiv—F3—K2ⁱⁱⁱ	78.16 (2)
F5—K2—F3^v	135.02 (2)	Li2^x—F4—Eu1	97.82 (8)
F7^xi—K2—F3^v	125.05 (3)	Li2^x—F4—K3^xiii	147.88 (8)
F8^xi—K2—F3^v	61.27 (2)	Eu1—F4—K3^xiii	114.18 (3)
F5^xii—K2—F3^v	72.01 (3)	Li2^x—F4—K1^v	88.18 (11)
F4—K2—F3^v	137.88 (2)	Eu1—F4—K1^v	107.11 (3)
Li2^xi—K2—F3^v	94.67 (7)	K3^xiii—F4—K1^v	85.08 (2)
F7^x—K2—F4^xiii	150.54 (2)	Li2^x—F4—K2	84.91 (11)
F6—K2—F4^xiii	65.89 (2)	Eu1—F4—K2	106.00 (3)
F5—K2—F4^xiii	81.15 (3)	K3^xiii—F4—K2	83.77 (2)
F7^xi—K2—F4^xiii	58.49 (3)	K1^v—F4—K2	146.79 (3)
F8^xi—K2—F4^xiii	58.53 (2)	Li2^x—F4—K2^xii	61.37 (8)
F5^xii—K2—F4^xiii	112.98 (2)	Eu1—F4—K2^xii	159.13 (3)
F4—K2—F4^xiii	127.14 (2)	K3^xiii—F4—K2^xii	86.55 (2)
Li2^xi—K2—F4^xiii	32.54 (5)	K1^v—F4—K2^xii	75.704 (19)
F3^v—K2—F4^xiii	94.98 (2)	K2—F4—K2^xii	72.480 (17)
Li2^x—K2—F4^xiii	147.93 (5)	Eu1—F5—K2^xx	114.28 (3)
F4^xii—K3—F4^xiv	159.74 (4)	Eu1—F5—K2	114.28 (3)
F4^xii—K3—F6^xv	80.751 (19)	K2^xx—F5—K2	79.15 (3)
F4^xiv—K3—F6^xv	80.751 (19)	Eu1—F5—K2^xiii	94.85 (3)
F4^xii—K3—F7^x	93.29 (2)	K2^xx—F5—K2^xiii	150.40 (4)
F4^xiv—K3—F7^x	93.29 (2)	K2—F5—K2^xiii	84.342 (11)
F6^xv—K3—F7^x	133.01 (4)	Eu1—F5—K2^xxxv	94.85 (3)
F4^xii—K3—F3^v	63.21 (2)	K2^xx—F5—K2^xxxv	84.342 (11)
F4^xiv—K3—F3^v	136.75 (3)	K2—F5—K2^xxxv	150.40 (4)
F6^xv—K3—F3^v	131.84 (3)	K2^xiii—F5—K2^xxxv	98.89 (4)
F7^x—K3—F3^v	82.48 (3)	Li1^x—F6—K3^xxxvi	152.17 (12)
F4^xii—K3—F3^xvi	136.75 (3)	Li1^x—F6—K2^xx	98.23 (8)
F4^xiv—K3—F3^xvi	63.21 (2)	K3^xxxvi—F6—K2^xx	102.81 (3)
F6^xv—K3—F3^xvi	131.84 (3)	Li1^x—F6—K2	98.23 (8)
F7^x—K3—F3^xvi	82.48 (3)	K3^xxxvi—F6—K2	102.81 (3)
F3^v—K3—F3^xvi	73.58 (3)	K2^xx—F6—K2	81.18 (4)
F4^xii—K3—F2^xvii	90.874 (19)	Li1^x—F6—K1^xviii	77.21 (7)
F4^xiv—K3—F2^xvii	90.874 (19)	K3^xxxvi—F6—K1^xviii	85.04 (3)
F6^xv—K3—F2^xvii	71.03 (3)	K2^xx—F6—K1^xviii	168.64 (4)
F7^x—K3—F2^xvii	155.96 (3)	K2—F6—K1^xviii	89.126 (9)
F3^v—K3—F2^xvii	78.33 (3)	Li1^x—F6—K1^xix	77.21 (7)
F3^xvi—K3—F2^xvii	78.33 (3)	K3^xxxvi—F6—K1^xix	85.04 (3)
Li1^x—K3—F2^xvii	78.49 (6)	K2^xx—F6—K1^xix	89.126 (9)
F5—Eu1—F2	147.91 (4)	K2—F6—K1^xix	168.64 (4)
F5—Eu1—F3^xviii	96.48 (2)	K1^xviii—F6—K1^xix	99.84 (4)
F2—Eu1—F3^xviii	92.40 (2)	Li2—F7—K3^xvii	154.06 (11)
F5—Eu1—F3^xix	96.48 (2)	Li2—F7—K2^xxviii	92.42 (8)
F2—Eu1—F3^xix	92.40 (2)	K3^xvii—F7—K2^xxviii	106.96 (3)
F3^xviii—Eu1—F3^xix	147.22 (4)	Li2—F7—K2^xvii	92.42 (8)
F5—Eu1—F1	139.47 (4)	K3^xvii—F7—K2^xvii	106.96 (3)
F2—Eu1—F1	72.63 (4)	K2^xxviii—F7—K2^xvii	81.97 (3)
F3^xviii—Eu1—F1	75.29 (2)	Li2—F7—K2^xi	78.37 (7)
F3^xix—Eu1—F1	75.30 (2)	K3^xvii—F7—K2^xi	85.43 (3)
F5—Eu1—F4^xx	76.34 (3)	K2^xxviii—F7—K2^xi	165.38 (4)
F2—Eu1—F4^xx	77.25 (3)	K2^xvii—F7—K2^xi	87.055 (6)
F3^xviii—Eu1—F4^xx	140.49 (3)	Li2—F7—K2^xxix	78.37 (7)
F3^xix—Eu1—F4^xx	72.04 (3)	K3^xvii—F7—K2^xxix	85.43 (3)
F1—Eu1—F4^xx	133.97 (2)	K2^xxviii—F7—K2^xxix	87.055 (6)
F5—Eu1—F4	76.34 (3)	K2^xvii—F7—K2^xxix	165.38 (4)
F2—Eu1—F4	77.25 (3)	K2^xi—F7—K2^xxix	101.95 (4)
F3^xviii—Eu1—F4	72.04 (3)	Li2—F8—Eu1^vi	163.91 (12)
F3^xix—Eu1—F4	140.49 (3)	Li2—F8—K1ⁱ	89.41 (9)
F1—Eu1—F4	133.97 (2)	Eu1^vi—F8—K1ⁱ	102.73 (3)
F4^xx—Eu1—F4	68.51 (4)	Li2—F8—K1^xxiii	89.41 (9)
F5—Eu1—F8^xxi	70.51 (4)	Eu1^vi—F8—K1^xxiii	102.73 (3)
F2—Eu1—F8^xxi	141.59 (4)	K1ⁱ—F8—K1^xxiii	81.17 (3)
F3^xviii—Eu1—F8^xxi	78.10 (2)	Li2—F8—K2^xxix	76.74 (7)
F3^xix—Eu1—F8^xxi	78.10 (2)	Eu1^vi—F8—K2^xxix	93.11 (3)
F1—Eu1—F8^xxi	68.96 (4)	K1ⁱ—F8—K2^xxix	162.14 (4)
F4^xx—Eu1—F8^xxi	131.91 (2)	K1^xxiii—F8—K2^xxix	87.386 (10)
F4—Eu1—F8^xxi	131.91 (2)	Li2—F8—K2^xi	76.74 (7)
F6^xvii—Li1—F1^xxii	107.19 (16)	Eu1^vi—F8—K2^xi	93.11 (3)
F6^xvii—Li1—F3ⁱ	107.75 (11)	K1ⁱ—F8—K2^xi	87.386 (10)
F1^xxii—Li1—F3ⁱ	105.42 (11)	K1^xxiii—F8—K2^xi	162.14 (4)
F6^xvii—Li1—F3^xxiii	107.75 (11)	K2^xxix—F8—K2^xi	100.09 (4)
F1^xxii—Li1—F3^xxiii	105.42 (11)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1/2, y+1, −z+1/2; (iii) −x+1/2, −y+1, z−1/2; (iv) x, y+1, z; (v) −x+1/2, −y+1, z+1/2; (vi) x+1/2, y, −z+1/2; (vii) x−1/2, y+1, −z+3/2; (viii) −x+1/2, −y+2, z+1/2; (ix) −x+3/2, −y+1, z−1/2; (x) x−1/2, y, −z+3/2; (xi) −x+1, −y, −z+1; (xii) −x+1/2, −y, z+1/2; (xiii) −x+1/2, −y, z−1/2; (xiv) −x+1/2, y+1/2, z+1/2; (xv) x, y, z+1; (xvi) −x+1/2, y−1/2, z+1/2; (xvii) x+1/2, y, −z+3/2; (xviii) x, y−1, z; (xix) x, −y+3/2, z; (xx) x, −y+1/2, z; (xxi) x−1/2, y, −z+1/2; (xxii) x+1, y, z+1; (xxiii) −x+1, y−1/2, −z+1; (xxiv) x+1/2, −y+3/2, −z+3/2; (xxv) x+1/2, y−1, −z+3/2; (xxvi) −x+3/2, −y+1, z+1/2; (xxvii) −x+3/2, y−1/2, z+1/2; (xxviii) x+1/2, −y+1/2, −z+3/2; (xxix) −x+1, y+1/2, −z+1; (xxx) x−1, y, z−1; (xxxi) x−1/2, y−1, −z+1/2; (xxxii) x−1/2, −y+3/2, −z+1/2; (xxxiii) −x+1/2, y−1/2, z−1/2; (xxxiv) −x+1/2, −y+2, z−1/2; (xxxv) −x+1/2, y+1/2, z−1/2; (xxxvi) x, y, z−1.

Experimental details

Crystal data
Chemical formula	K₅EuLi₂F₁₀
M_r	551.35
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	295
a, b, c (Å)	20.5539 (6), 7.7356 (2), 6.8721 (2)
V (Å³)	1092.64 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	7.75
Crystal size (mm)	0.35 × 0.20 × 0.15

Data collection
Diffractometer	Kuma KM-4 with CCD area-detector
Absorption correction	Multi-scan (CrysAlis RED; Oxford Diffraction, 2007)
T_min, T_max	0.146, 0.310
No. of measured, independent and observed [I > 2σ(I)] reflections	23852, 4895, 3564
R_int	0.034
(sin θ/λ)_max (Å⁻¹)	1.032

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.039, 0.83
No. of reflections	4895
No. of parameters	98
Δρ_max, Δρ_min (e Å⁻³)	2.35, −3.02

Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2006).

Selected bond lengths (Å) top

Eu1—F5	2.2923 (11)	Li1—F6ⁱⁱⁱ	1.804 (3)
Eu1—F2	2.3236 (11)	Li1—F1^iv	1.862 (3)
Eu1—F3ⁱ	2.3262 (7)	Li1—F3^v	1.8669 (16)
Eu1—F1	2.3918 (10)	Li2—F7	1.801 (4)
Eu1—F4	2.3954 (7)	Li2—F4ⁱⁱⁱ	1.817 (2)
Eu1—F8ⁱⁱ	2.3996 (10)	Li2—F8	1.844 (3)

Symmetry codes: (i) x, y−1, z; (ii) x−1/2, y, −z+1/2; (iii) x+1/2, y, −z+3/2; (iv) x+1, y, z+1; (v) −x+1, −y+1, −z+1.

References

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