14
Ζ. Kristallogr. N C S 2 1 4 ( 1 9 9 9 )© b y R. O l d e n b o u r g V e r l a g , M ü n c h e n
C r y s t a l s t r u c t u r e o f t h e c l a t h r a t e C s s I n s G e ^ s
H. Menke, W. Carrillo-Cabrera, Κ. Peters, E.-M. Peters and H. G. von Schnering
Max-Planck-Institut f ü r Festkörperforschung, Heisenbergstr. 1, D-70569 Stuttgart, Germany
Received August 26, 1998, transferred to 1 st update of database ICSD in 1999, CSD-No. 409367
dò Abstract _
Cs8Ge38ln8, cubic, Prriin ( N o . 2 2 3 ) , a = 1 1 . 0 7 9 ( 2 ) Â ,
V= 1 3 5 9 . 9 Â3, Z = 1, Rgt(F) = 0 . 0 4 8 , R^F2) = 0 . 1 0 2 , T = 2 9 3 K.
Source of material
S t o i c h i o m e t r i c m i x t u r e s o f t h e e l e m e n t s w e r e s e a l e d i n N b c a p s u - l e s u n d e r Ar, h e a t e d u p t o 1 2 7 0 Κ ( 3 h ) , a n n e a l e d at 9 7 0 Κ ( 2 d ) a n d c o o l e d d o w n . T h e g r e y brittle c o m p o u n d i s a d i a m a g n e t i c s e m i c o n d u c t o r ; it d o e s n ' t r e a c t w i t h d i l u t e a c i d s and b a s e s [ 1 ] ,
Discussion
T h e r e f i n e m e n t o f the s i t e o c c u p a n c i e s r e s u l t s i n t h e c o m p o s i t i o n C s s I n « G c 4 6 - n w i t h η = 8 . 2 ± 0 . 6 . B o n d l e n g t h s in t h e E46 n e t ( f i g u r e ) : dl = 2 . 5 1 2 ( 3 ) Â , d2 = 2 . 5 3 3 ( 1 ) Â , di = 2 . 6 0 6 Â , d 4 = 2 . 6 4 1 Â .
Table 1. Data collection and handling.
Crystal:
Wavelength:
μ;
Diffractometer, scan mode:
26max:
N(hkl)measured. WfAWjunique:
Criterion for /0bs, N(hkl)gC N(param) refined:
Program:
grey, metallic luster, irregular, size 0 . 1 0 x 0 . 1 0 x 0 . 1 4 m m M o Ka radiation (0.71073 À) 292.17 cm~'_
SYNTEX P I , ω 62.16°
4 2 0 , 4 2 0
lobs > 2 a(/obs), 343 IS
SHELXL-93 [2]
Table 2. Atomic coordinates and displacement parameters (in À ).
Atom Site X y ζ U H C/22 C/33 U12 U13 C/23
Csl 2 a 0 0 0 0.0069(5) C/ll C/11 0 0 0
Cs2 6d 1/4 1/2 0 0.0099(8) 0.0206(6) C/22 0 0 0
E l (In) 6c 0.77(2) 1/4 0 1/2 0.011(1) 0.0080(7) C/22 0 0 0
E l ( G e ) 6c 0.23 1/4 0 1/2 0.011 0.0080 C/22 0 0 0
E2(Ge) 16 i 0.18456(8) X χ 0.0071(4) C/11 C/11 - 0 . 0 0 0 7 ( 3 ) C/12 C/12
E3(In) 24k 0.15(2) 0 0.3018(1) 0.1176(1) 0.0071(6) 0.0076(6) 0.0090(6) 0 0 0.0000(5)
E3(Ge) 24 k 0.85 0 0.3018 0.1176 0.0071 0.0076 0.0090 0 0 0.0000
Acknowledgment. W e thank the Fonds der Chemischen Industrie for financial support.
References
1. Kröner, R.: Zintl-Phasen der Alkalimetalle und des Bariums mit Cla- thratstruktur. Dissertation, Universität Stuttgart, 1989.
2. Sheldrick, G. M.: SHELXL-93, a program for refining crystal structures.
University of Göttingen 1993.
