Penta­potassium praseodymium(III) dilithium deca­fluoride, K5PrLi2F10

Gagor, A.

doi:10.1107/S1600536809044043

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 11| November 2009| Page i81

https://doi.org/10.1107/S1600536809044043

Open

access

Pentapotassium praseodymium(III) dilithium decafluoride, K₅PrLi₂F₁₀

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 12 October 2009; accepted 23 October 2009; online 28 October 2009)

The crystal structure of K₅PrLi₂F₁₀ is isotypic with those of other K₅RELi₂F₁₀ compounds (RE = Eu, Nd). The lanthanoid ions are isolated in K₅PrLi₂F₁₀, with a mean separation between the Pr ions of 7.356 Å. It classifies this crystal as a so-called self-activated material containing lanthanoid ions within the matrix. Except for two K⁺ and two F⁻ ions, all atoms are located on sites with m symmetry. In the structure, distorted PrF₈ dodecahedra and two different LiF₄ tetrahedra share F atoms, forming sheets parallel to (100). The isolated PrF₈ dodecahedra exhibit a mean Pr—F distance of 2.406 Å. The K⁺ cations are located within and between these sheets, leading to highly irregular KF_x polyhedra with coordination numbers of eight and nine for the alkali metal cations.

Related literature

The structures of the isotypic Nd and Eu analogues have been reported by Hong & McCollum (1979 ) and 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

K₅PrLi₂F₁₀
M_r = 540.29
Orthorhombic, P n m a
a = 20.6492 (6) Å
b = 7.7903 (3) Å
c = 6.9255 (2) Å
V = 1114.06 (6) Å³
Z = 4
Mo Kα radiation
μ = 6.34 mm⁻¹
T = 295 K
0.35 × 0.13 × 0.05 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 = 0.40, T_max = 0.73
24749 measured reflections
4910 independent reflections
3709 reflections with I > 2σ(I)
R_int = 0.045

Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.045
S = 1.02
4910 reflections
98 parameters
Δρ_max = 1.17 e Å⁻³
Δρ_min = −2.04 e Å⁻³

Table 1
Selected bond lengths (Å)

Pr1—F5	2.3426 (12)
Pr1—F3ⁱ	2.3737 (8)
Pr1—F2	2.3751 (12)
Pr1—F1	2.4368 (11)
Pr1—F8ⁱⁱ	2.4463 (11)
Pr1—F4	2.4488 (8)
Li1—F6ⁱⁱⁱ	1.802 (4)
Li1—F1^iv	1.856 (4)
Li1—F3^v	1.8602 (19)
Li2—F7	1.796 (4)
Li2—F4ⁱⁱⁱ	1.819 (2)
Li2—F8	1.843 (4)
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/S1600536809044043/wm2268sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809044043/wm2268Isup2.hkl

checkCIF report

Comment top

The title crystal belongs to so-called self-activated materials containing lanthanoid ions within the matrix. An important 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.

In the structure, two different LiF₄ tetrahedra together with distorted PrF₈ dodecahedra form sheets expanding perpendicular to [100]. K1 atoms occupy cavities within the sheets and are surrounded by 9 F^- ions in a mean distance of 2.780 Å. The remaining potassium atoms are located between the sheets within a KF₉ and KF₈ environment. Each PrF₈ dodecahedron is surrounded by twelve others with a minimum and maximum Pr—Pr separation of 6.7656 (2) and 7.8684 (2) Å, and individual distances of: 2× 6.7656 (2), 2× 6.9169 (2), 2× 6.9255 (2), 2× 7.7903 (3) and 4× 7.8684 (2) Å.

The bond valence sums of all metal atoms have been calculated from the received structure model using the bond-valence method (Brown, 1992, 2002; Mattausch et al., 1991); Pr 2.86, K1 1.05, K2 0.98, K3 1.06, and Li 1.08 v.u. The Pr ion is slightly under-bonded which may be associated with the distorted surrounding of this cation. When such distortions occur, the equal-valence rule is not obeyed (Brown, 1992). The valences of K atoms are close to the formal charge of +1. The Li position is over-bonded with a 8.3% higher bond-valence sum than those expected from the formal charge of +1.

Related literature top

The structures of the isotypic Nd and Eu analogues have been reported by Hong & McCollum (1979) and 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

The K₅PrLi₂F₁₀ crystal was grown from commercially available KF, PrF₃ and LiF (Aldrich 99.99%, anhydrous) using the Bridgman method in a graphite crucible under argon atmosphere. The reagents were heated at 923 K (melting point 813 K). The pulling rate was 1mm/h, temperature gradient was 100°/cm.

Structure description top

The structures of the isotypic Nd and Eu analogues have been reported by Hong & McCollum (1979) and 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 of the K₅PrLi₂F₁₀ structure as seen down [010]. Displacement ellipsoids have been drawn at the 50% probability level.

Pentapotassium praseodymium(III) dilithium decafluoride top

Crystal data top

K₅PrLi₂F₁₀	F(000) = 1000
M_r = 540.29	D_x = 3.221 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 11195 reflections
a = 20.6492 (6) Å	θ = 2.6–47.0°
b = 7.7903 (3) Å	µ = 6.34 mm⁻¹
c = 6.9255 (2) Å	T = 295 K
V = 1114.06 (6) Å³	Rectangular prism, colourless
Z = 4	0.35 × 0.13 × 0.05 mm

Data collection top

Kuma KM-4 with CCD area-detector diffractometer	4910 independent reflections
Radiation source: fine-focus sealed tube	3709 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.045
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm^-1	θ_max = 47.1°, θ_min = 3.1°
ω scans	h = −19→42
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	k = −16→13
T_min = 0.40, T_max = 0.73	l = −13→11
24749 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)] = 0.029	w = 1/[σ²(F_o²) + (0.0151P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.045	(Δ/σ)_max = 0.001
S = 1.02	Δρ_max = 1.17 e Å⁻³
4910 reflections	Δρ_min = −2.04 e Å⁻³
98 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0319 (3)

Crystal data top

K₅PrLi₂F₁₀	V = 1114.06 (6) Å³
M_r = 540.29	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 20.6492 (6) Å	µ = 6.34 mm⁻¹
b = 7.7903 (3) Å	T = 295 K
c = 6.9255 (2) Å	0.35 × 0.13 × 0.05 mm

Data collection top

Kuma KM-4 with CCD area-detector diffractometer	4910 independent reflections
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	3709 reflections with I > 2σ(I)
T_min = 0.40, T_max = 0.73	R_int = 0.045
24749 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	98 parameters
wR(F²) = 0.045	0 restraints
S = 1.02	Δρ_max = 1.17 e Å⁻³
4910 reflections	Δρ_min = −2.04 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 F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > σ(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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	0.456661 (15)	0.97842 (4)	0.25210 (4)	0.01639 (5)
K2	0.283103 (15)	0.02682 (4)	0.42595 (5)	0.01786 (6)
K3	0.35981 (2)	0.2500	0.94040 (6)	0.01865 (8)
Pr1	0.107262 (4)	0.2500	0.239205 (12)	0.00794 (2)
Li1	0.92241 (16)	0.2500	0.9697 (5)	0.0140 (6)
Li2	0.67429 (16)	0.2500	0.8399 (5)	0.0138 (6)
F1	0.00854 (5)	0.2500	0.04643 (17)	0.0152 (2)
F2	0.01862 (6)	0.2500	0.45774 (17)	0.0189 (2)
F3	0.09014 (4)	0.95753 (10)	0.15779 (13)	0.01896 (17)
F4	0.14806 (4)	0.07426 (10)	0.50594 (12)	0.01643 (16)
F5	0.21956 (6)	0.2500	0.19130 (18)	0.0182 (2)
F6	0.37398 (6)	0.2500	0.31393 (18)	0.0170 (2)
F7	0.75970 (6)	0.2500	0.79114 (17)	0.0171 (2)
F8	0.63138 (6)	0.2500	0.60663 (16)	0.0160 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K1	0.01604 (12)	0.01537 (12)	0.01777 (13)	−0.00135 (9)	−0.00063 (10)	−0.00158 (10)
K2	0.01912 (13)	0.01524 (13)	0.01921 (14)	0.00175 (10)	−0.00062 (11)	−0.00098 (10)
K3	0.0311 (2)	0.01106 (17)	0.01382 (18)	0.000	−0.00294 (15)	0.000
Pr1	0.00890 (4)	0.00760 (4)	0.00733 (4)	0.000	−0.00056 (3)	0.000
Li1	0.0140 (15)	0.0148 (16)	0.0131 (15)	0.000	−0.0021 (12)	0.000
Li2	0.0128 (16)	0.0152 (16)	0.0132 (15)	0.000	0.0005 (12)	0.000
F1	0.0111 (5)	0.0188 (6)	0.0156 (5)	0.000	−0.0023 (4)	0.000
F2	0.0180 (6)	0.0243 (6)	0.0144 (5)	0.000	0.0026 (4)	0.000
F3	0.0249 (4)	0.0109 (4)	0.0211 (4)	0.0000 (3)	−0.0063 (3)	−0.0032 (3)
F4	0.0240 (4)	0.0101 (3)	0.0153 (4)	−0.0001 (3)	−0.0031 (3)	−0.0007 (3)
F5	0.0129 (5)	0.0237 (6)	0.0182 (5)	0.000	−0.0015 (4)	0.000
F6	0.0170 (5)	0.0210 (6)	0.0132 (5)	0.000	−0.0024 (4)	0.000
F7	0.0144 (5)	0.0210 (6)	0.0160 (5)	0.000	0.0017 (4)	0.000
F8	0.0155 (5)	0.0212 (6)	0.0112 (5)	0.000	−0.0015 (4)	0.000

Geometric parameters (Å, º) top

K1—F8ⁱ	2.7256 (9)	K3—F5^xv	3.3772 (13)
K1—F1ⁱⁱ	2.7514 (8)	Pr1—F5	2.3426 (12)
K1—F2ⁱⁱⁱ	2.7537 (10)	Pr1—F3^xviii	2.3737 (8)
K1—F6^iv	2.7521 (9)	Pr1—F3^xix	2.3737 (8)
K1—F4ⁱⁱⁱ	2.7841 (9)	Pr1—F2	2.3751 (12)
K1—F1^v	2.7996 (9)	Pr1—F1	2.4368 (11)
K1—F3^vi	2.8307 (10)	Pr1—F8^xx	2.4463 (11)
K1—F2ⁱⁱ	2.8679 (9)	Pr1—F4^xxi	2.4488 (8)
K1—Li1^vii	2.948 (2)	Pr1—F4	2.4488 (8)
K1—F3^viii	3.0127 (9)	Pr1—Li2^x	3.227 (3)
K1—Li2ⁱ	3.299 (3)	Li1—F6^xvii	1.802 (4)
K1—Li1^ix	3.416 (3)	Li1—F1^xxii	1.856 (4)
K2—F7^x	2.6636 (9)	Li1—F3ⁱ	1.8602 (19)
K2—F6	2.6733 (10)	Li1—F3^xxiii	1.8602 (19)
K2—F5	2.7176 (10)	Li1—K1^xxiv	2.948 (2)
K2—F7^xi	2.7735 (8)	Li1—K1^xxv	2.948 (2)
K2—F8^xi	2.7964 (8)	Li1—K3^xvii	3.120 (3)
K2—F5^xii	2.8338 (9)	Li1—K1^xxvi	3.416 (3)
K2—F4	2.8669 (9)	Li1—K1^xxvii	3.416 (3)
K2—Li2^xi	2.969 (2)	Li1—K2^xvii	3.438 (3)
K2—F3^v	3.0730 (10)	Li1—K2^xxviii	3.438 (3)
K2—Li2^x	3.271 (3)	Li2—F7	1.796 (4)
K2—F4^xiii	3.3319 (9)	Li2—F4^xvii	1.819 (2)
K2—Li1^x	3.438 (3)	Li2—F4^xxviii	1.819 (2)
K3—F4^xiv	2.5717 (8)	Li2—F8	1.843 (4)
K3—F4^xii	2.5717 (8)	Li2—K2^xi	2.969 (2)
K3—F6^xv	2.6035 (13)	Li2—K2^xxix	2.969 (2)
K3—F7^x	2.6161 (12)	Li2—Pr1^xvii	3.227 (3)
K3—F3^v	2.7409 (9)	Li2—K2^xxviii	3.271 (3)
K3—F3^xvi	2.7409 (9)	Li2—K2^xvii	3.271 (3)
K3—Li1^x	3.120 (3)	Li2—K1ⁱ	3.299 (3)
K3—F2^xvii	3.3544 (13)	Li2—K1^xxiii	3.299 (3)

F8ⁱ—K1—F1ⁱⁱ	125.43 (3)	F4^xxi—Pr1—F4	67.98 (4)
F8ⁱ—K1—F2ⁱⁱⁱ	88.14 (3)	F6^xvii—Li1—F1^xxii	107.07 (18)
F1ⁱⁱ—K1—F2ⁱⁱⁱ	143.14 (3)	F6^xvii—Li1—F3ⁱ	108.50 (12)
F8ⁱ—K1—F6^iv	91.85 (3)	F1^xxii—Li1—F3ⁱ	105.63 (12)
F1ⁱⁱ—K1—F6^iv	64.63 (3)	F6^xvii—Li1—F3^xxiii	108.50 (12)
F2ⁱⁱⁱ—K1—F6^iv	136.63 (3)	F1^xxii—Li1—F3^xxiii	105.63 (12)
F8ⁱ—K1—F4ⁱⁱⁱ	66.76 (3)	F3ⁱ—Li1—F3^xxiii	120.71 (19)
F1ⁱⁱ—K1—F4ⁱⁱⁱ	136.58 (3)	F7—Li2—F4^xvii	113.76 (13)
F2ⁱⁱⁱ—K1—F4ⁱⁱⁱ	66.13 (3)	F7—Li2—F4^xxviii	113.76 (13)
F6^iv—K1—F4ⁱⁱⁱ	74.14 (3)	F4^xvii—Li2—F4^xxviii	97.67 (17)
F8ⁱ—K1—F1^v	59.66 (3)	F7—Li2—F8	107.90 (19)
F1ⁱⁱ—K1—F1^v	91.123 (11)	F4^xvii—Li2—F8	111.81 (14)
F2ⁱⁱⁱ—K1—F1^v	94.63 (3)	F4^xxviii—Li2—F8	111.81 (14)
F6^iv—K1—F1^v	122.31 (3)	Li1^xxx—F1—Pr1	163.42 (12)
F4ⁱⁱⁱ—K1—F1^v	123.47 (3)	Li1^xxx—F1—K1^xxxi	76.83 (7)
F8ⁱ—K1—F3^vi	122.20 (3)	Pr1—F1—K1^xxxi	92.75 (3)
F1ⁱⁱ—K1—F3^vi	63.47 (3)	Li1^xxx—F1—K1^xxxii	76.83 (7)
F2ⁱⁱⁱ—K1—F3^vi	86.88 (3)	Pr1—F1—K1^xxxii	92.75 (3)
F6^iv—K1—F3^vi	127.87 (3)	K1^xxxi—F1—K1^xxxii	100.52 (4)
F4ⁱⁱⁱ—K1—F3^vi	151.98 (3)	Li1^xxx—F1—K1ⁱⁱⁱ	92.14 (9)
F1^v—K1—F3^vi	63.45 (3)	Pr1—F1—K1ⁱⁱⁱ	100.61 (3)
F8ⁱ—K1—F2ⁱⁱ	163.96 (3)	K1^xxxi—F1—K1ⁱⁱⁱ	88.877 (11)
F1ⁱⁱ—K1—F2ⁱⁱ	61.06 (3)	K1^xxxii—F1—K1ⁱⁱⁱ	163.31 (4)
F2ⁱⁱⁱ—K1—F2ⁱⁱ	91.081 (12)	Li1^xxx—F1—K1^xxxiii	92.14 (9)
F6^iv—K1—F2ⁱⁱ	77.79 (3)	Pr1—F1—K1^xxxiii	100.61 (3)
F4ⁱⁱⁱ—K1—F2ⁱⁱ	98.33 (3)	K1^xxxi—F1—K1^xxxiii	163.31 (4)
F1^v—K1—F2ⁱⁱ	136.33 (3)	K1^xxxii—F1—K1^xxxiii	88.877 (11)
F3^vi—K1—F2ⁱⁱ	73.73 (3)	K1ⁱⁱⁱ—F1—K1^xxxiii	78.93 (3)
F8ⁱ—K1—F3^viii	63.86 (3)	Pr1—F2—K1^xvi	109.20 (4)
F1ⁱⁱ—K1—F3^viii	61.62 (3)	Pr1—F2—K1^v	109.20 (4)
F2ⁱⁱⁱ—K1—F3^viii	148.97 (3)	K1^xvi—F2—K1^v	80.51 (3)
F6^iv—K1—F3^viii	61.87 (3)	Pr1—F2—K1^xxxi	91.20 (3)
F4ⁱⁱⁱ—K1—F3^viii	110.26 (3)	K1^xvi—F2—K1^xxxi	159.16 (5)
F1^v—K1—F3^viii	60.57 (3)	K1^v—F2—K1^xxxi	88.919 (12)
F3^vi—K1—F3^viii	96.68 (2)	Pr1—F2—K1^xxxii	91.20 (3)
F2ⁱⁱ—K1—F3^viii	119.57 (3)	K1^xvi—F2—K1^xxxii	88.919 (12)
Li1^vii—K1—F3^viii	36.35 (5)	K1^v—F2—K1^xxxii	159.16 (5)
F7^x—K2—F6	85.20 (3)	K1^xxxi—F2—K1^xxxii	95.07 (4)
F7^x—K2—F5	86.26 (3)	Pr1—F2—K3^x	152.55 (5)
F6—K2—F5	75.48 (3)	K1^xvi—F2—K3^x	91.46 (3)
F7^x—K2—F7^xi	148.04 (2)	K1^v—F2—K3^x	91.46 (3)
F6—K2—F7^xi	124.90 (3)	K1^xxxi—F2—K3^x	70.76 (3)
F5—K2—F7^xi	91.11 (3)	K1^xxxii—F2—K3^x	70.76 (3)
F7^x—K2—F8^xi	132.63 (3)	Li1ⁱ—F3—Pr1^iv	165.41 (10)
F6—K2—F8^xi	92.00 (3)	Li1ⁱ—F3—K3ⁱⁱⁱ	83.04 (9)
F5—K2—F8^xi	138.59 (3)	Pr1^iv—F3—K3ⁱⁱⁱ	109.90 (3)
F7^xi—K2—F8^xi	63.76 (3)	Li1ⁱ—F3—K1^xx	91.08 (11)
F7^x—K2—F5^xii	90.93 (3)	Pr1^iv—F3—K1^xx	92.15 (3)
F6—K2—F5^xii	134.17 (3)	K3ⁱⁱⁱ—F3—K1^xx	104.10 (3)
F5—K2—F5^xii	149.912 (14)	Li1ⁱ—F3—K1^xxxiv	69.92 (9)
F7^xi—K2—F5^xii	75.74 (3)	Pr1^iv—F3—K1^xxxiv	96.33 (3)
F8^xi—K2—F5^xii	58.52 (3)	K3ⁱⁱⁱ—F3—K1^xxxiv	152.20 (3)
F7^x—K2—F4	66.25 (3)	K1^xx—F3—K1^xxxiv	83.32 (2)
F6—K2—F4	130.92 (3)	Li1ⁱ—F3—K2ⁱⁱⁱ	84.56 (11)
F5—K2—F4	64.12 (3)	Pr1^iv—F3—K2ⁱⁱⁱ	87.66 (3)
F7^xi—K2—F4	83.97 (3)	K3ⁱⁱⁱ—F3—K2ⁱⁱⁱ	94.32 (3)
F8^xi—K2—F4	136.82 (3)	K1^xx—F3—K2ⁱⁱⁱ	160.43 (4)
F5^xii—K2—F4	87.36 (3)	K1^xxxiv—F3—K2ⁱⁱⁱ	77.26 (2)
F7^x—K2—F3^v	75.18 (3)	Li2^x—F4—Pr1	97.15 (9)
F6—K2—F3^v	61.83 (3)	Li2^x—F4—K3^xiii	149.53 (9)
F5—K2—F3^v	134.29 (3)	Pr1—F4—K3^xiii	113.22 (3)
F7^xi—K2—F3^v	125.84 (3)	Li2^x—F4—K1^v	89.01 (11)
F8^xi—K2—F3^v	62.28 (3)	Pr1—F4—K1^v	106.09 (3)
F5^xii—K2—F3^v	73.02 (3)	K3^xiii—F4—K1^v	85.08 (3)
F4—K2—F3^v	136.25 (3)	Li2^x—F4—K2	85.46 (11)
Li2^xi—K2—F3^v	95.76 (7)	Pr1—F4—K2	105.13 (3)
F7^x—K2—F4^xiii	150.90 (3)	K3^xiii—F4—K2	84.30 (3)
F6—K2—F4^xiii	66.48 (3)	K1^v—F4—K2	148.74 (3)
F5—K2—F4^xiii	80.51 (3)	Li2^x—F4—K2^xii	62.51 (9)
F7^xi—K2—F4^xiii	58.60 (3)	Pr1—F4—K2^xii	159.63 (3)
F8^xi—K2—F4^xiii	58.53 (3)	K3^xiii—F4—K2^xii	87.07 (3)
F5^xii—K2—F4^xiii	113.24 (3)	K1^v—F4—K2^xii	76.23 (2)
F4—K2—F4^xiii	127.88 (3)	K2—F4—K2^xii	73.936 (19)
Li2^xi—K2—F4^xiii	32.91 (5)	Pr1—F5—K2^xxi	113.16 (4)
F3^v—K2—F4^xiii	95.86 (2)	Pr1—F5—K2	113.16 (4)
Li2^x—K2—F4^xiii	148.36 (6)	K2^xxi—F5—K2	79.55 (4)
F4^xiv—K3—F4^xii	158.39 (4)	Pr1—F5—K2^xiii	94.16 (3)
F4^xiv—K3—F6^xv	80.31 (2)	K2^xxi—F5—K2^xiii	152.13 (5)
F4^xii—K3—F6^xv	80.31 (2)	K2—F5—K2^xiii	84.854 (11)
F4^xiv—K3—F7^x	93.34 (2)	Pr1—F5—K2^xxxv	94.16 (3)
F4^xii—K3—F7^x	93.34 (2)	K2^xxi—F5—K2^xxxv	84.854 (11)
F6^xv—K3—F7^x	134.26 (4)	K2—F5—K2^xxxv	152.13 (5)
F4^xiv—K3—F3^v	136.82 (3)	K2^xiii—F5—K2^xxxv	99.10 (4)
F4^xii—K3—F3^v	64.56 (3)	Pr1—F5—K3^xxxvi	157.18 (5)
F6^xv—K3—F3^v	131.85 (3)	K2^xxi—F5—K3^xxxvi	83.90 (3)
F7^x—K3—F3^v	81.97 (3)	K2—F5—K3^xxxvi	83.90 (3)
F4^xiv—K3—F3^xvi	64.56 (3)	K2^xiii—F5—K3^xxxvi	71.52 (3)
F4^xii—K3—F3^xvi	136.82 (3)	K2^xxxv—F5—K3^xxxvi	71.52 (3)
F6^xv—K3—F3^xvi	131.85 (3)	Li1^x—F6—K3^xxxvi	152.74 (12)
F7^x—K3—F3^xvi	81.97 (3)	Li1^x—F6—K2	98.53 (9)
F3^v—K3—F3^xvi	72.29 (4)	K3^xxxvi—F6—K2	102.09 (4)
F4^xiv—K3—F2^xvii	91.41 (2)	Li1^x—F6—K2^xxi	98.53 (9)
F4^xii—K3—F2^xvii	91.41 (2)	K3^xxxvi—F6—K2^xxi	102.09 (4)
F6^xv—K3—F2^xvii	71.40 (4)	K2—F6—K2^xxi	81.14 (4)
F7^x—K3—F2^xvii	154.34 (4)	Li1^x—F6—K1^xix	77.59 (7)
F3^v—K3—F2^xvii	77.38 (3)	K3^xxxvi—F6—K1^xix	85.13 (3)
F3^xvi—K3—F2^xvii	77.38 (3)	K2—F6—K1^xix	168.70 (4)
Li1^x—K3—F2^xvii	77.66 (7)	K2^xxi—F6—K1^xix	88.891 (10)
F4^xiv—K3—F5^xv	81.66 (2)	Li1^x—F6—K1^xviii	77.59 (7)
F4^xii—K3—F5^xv	81.66 (2)	K3^xxxvi—F6—K1^xviii	85.13 (3)
F6^xv—K3—F5^xv	65.49 (4)	K2—F6—K1^xviii	88.892 (10)
F7^x—K3—F5^xv	68.77 (3)	K2^xxi—F6—K1^xviii	168.70 (4)
F3^v—K3—F5^xv	133.69 (2)	K1^xix—F6—K1^xviii	100.48 (4)
F3^xvi—K3—F5^xv	133.69 (2)	Li2—F7—K3^xvii	153.04 (13)
Li1^x—K3—F5^xv	145.44 (7)	Li2—F7—K2^xxviii	92.28 (9)
F2^xvii—K3—F5^xv	136.89 (3)	K3^xvii—F7—K2^xxviii	107.91 (4)
F5—Pr1—F3^xviii	96.53 (2)	Li2—F7—K2^xvii	92.28 (9)
F5—Pr1—F3^xix	96.53 (2)	K3^xvii—F7—K2^xvii	107.91 (4)
F3^xviii—Pr1—F3^xix	147.44 (4)	K2^xxviii—F7—K2^xvii	81.49 (4)
F5—Pr1—F2	148.56 (4)	Li2—F7—K2^xi	77.81 (7)
F3^xviii—Pr1—F2	92.10 (2)	K3^xvii—F7—K2^xi	85.39 (3)
F3^xix—Pr1—F2	92.10 (2)	K2^xxviii—F7—K2^xi	164.59 (4)
F5—Pr1—F1	138.64 (4)	K2^xvii—F7—K2^xi	87.078 (7)
F3^xviii—Pr1—F1	75.24 (2)	Li2—F7—K2^xxix	77.81 (7)
F3^xix—Pr1—F1	75.24 (2)	K3^xvii—F7—K2^xxix	85.39 (3)
F2—Pr1—F1	72.81 (4)	K2^xxviii—F7—K2^xxix	87.078 (7)
F5—Pr1—F8^xx	70.11 (4)	K2^xvii—F7—K2^xxix	164.59 (4)
F3^xviii—Pr1—F8^xx	78.33 (2)	K2^xi—F7—K2^xxix	102.07 (4)
F3^xix—Pr1—F8^xx	78.33 (2)	Li2—F8—Pr1^vi	163.01 (13)
F2—Pr1—F8^xx	141.33 (4)	Li2—F8—K1ⁱ	90.34 (9)
F1—Pr1—F8^xx	68.53 (4)	Pr1^vi—F8—K1ⁱ	102.45 (3)
F5—Pr1—F4^xxi	76.48 (3)	Li2—F8—K1^xxiii	90.34 (9)
F3^xviii—Pr1—F4^xxi	140.09 (3)	Pr1^vi—F8—K1^xxiii	102.45 (3)
F3^xix—Pr1—F4^xxi	72.17 (3)	K1ⁱ—F8—K1^xxiii	81.52 (3)
F2—Pr1—F4^xxi	77.55 (3)	Li2—F8—K2^xxix	76.53 (7)
F1—Pr1—F4^xxi	134.52 (3)	Pr1^vi—F8—K2^xxix	92.84 (3)
F8^xx—Pr1—F4^xxi	131.95 (3)	K1ⁱ—F8—K2^xxix	162.49 (4)
F5—Pr1—F4	76.48 (3)	K1^xxiii—F8—K2^xxix	86.943 (11)
F3^xviii—Pr1—F4	72.17 (3)	Li2—F8—K2^xi	76.53 (7)
F3^xix—Pr1—F4	140.09 (3)	Pr1^vi—F8—K2^xi	92.84 (3)
F2—Pr1—F4	77.55 (3)	K1ⁱ—F8—K2^xi	86.943 (11)
F1—Pr1—F4	134.52 (3)	K1^xxiii—F8—K2^xi	162.49 (4)
F8^xx—Pr1—F4	131.95 (3)	K2^xxix—F8—K2^xi	100.92 (4)

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−1/2, y, −z+1/2; (xxi) x, −y+1/2, z; (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	K₅PrLi₂F₁₀
M_r	540.29
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	295
a, b, c (Å)	20.6492 (6), 7.7903 (3), 6.9255 (2)
V (Å³)	1114.06 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	6.34
Crystal size (mm)	0.35 × 0.13 × 0.05

Data collection
Diffractometer	Kuma KM-4 with CCD area-detector
Absorption correction	Multi-scan (CrysAlis RED; Oxford Diffraction, 2007)
T_min, T_max	0.40, 0.73
No. of measured, independent and observed [I > 2σ(I)] reflections	24749, 4910, 3709
R_int	0.045
(sin θ/λ)_max (Å⁻¹)	1.031

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.045, 1.02
No. of reflections	4910
No. of parameters	98
Δρ_max, Δρ_min (e Å⁻³)	1.17, −2.04

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

Pr1—F5	2.3426 (12)	Li1—F6ⁱⁱⁱ	1.802 (4)
Pr1—F3ⁱ	2.3737 (8)	Li1—F1^iv	1.856 (4)
Pr1—F2	2.3751 (12)	Li1—F3^v	1.8602 (19)
Pr1—F1	2.4368 (11)	Li2—F7	1.796 (4)
Pr1—F8ⁱⁱ	2.4463 (11)	Li2—F4ⁱⁱⁱ	1.819 (2)
Pr1—F4	2.4488 (8)	Li2—F8	1.843 (4)

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

Brandenburg, K. & Putz, H. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brown, I. D. (1992). Acta Cryst. B48, 553–572. CrossRef CAS Web of Science IUCr Journals Google Scholar
Brown, I. D. (2002). The Chemical Bond in Inorganic Chemistry - The Bond Valence Model. IUCr monographs on Crystallography 12. Oxford University Press. Google Scholar
Gagor, A. (2009). Acta Cryst. E65, i82. Web of Science CrossRef IUCr Journals Google Scholar
Hong, H. Y.-P. & McCollum, B. C. (1979). Mater. Res. Bull. 14, 137–142. CrossRef CAS Web of Science Google Scholar
Mattausch, H. J., Eger, R. & Simon, A. (1991). Z. Anorg. Allg. Chem. 597, 145–150. CrossRef CAS Web of Science Google Scholar
Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England. Google Scholar
Ryba-Romanowski, W., Solarz, P., Gusowski, M. & Dominiak-Dzik, G. (2007). Rad. Meas. 42, 798–802. Web of Science CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar