metal-organic compounds
0.2 mmol) and tetrahydrofuran (5 ml). The solution was heated under
re¯ux for 24 h, and the colour of the solution changed from orange to
yellow. Upon cooling to room temperature, hexane (10 ml) was
added to the mixture. The solid was ®ltered off and then recrys-
tallized from CH2Cl2/MeOH (1:5 v/v, 12 ml) (yield 160 mg, 77%; m.p.
541±542 K). Analysis calculated for C42H26Br2F10N4Pd: C 48.35, H
2.49, N 5.37%; found: C 47.60, H 1.96, N 5.36%. 1H NMR (CDCl3): ꢁ
5.91 (s, 4H, CH2C6H5), 6.07 (d, 4H, J = 10 Hz, CH2C6F5), 6.99±7.42
(m, 18H, Ar±H). 13C NMR (CDCl3): ꢁ 53.00 (CH2C6H5), 41.30
(CH2C6F5), 110.33 (d, J = 15.3 Hz), 111.96 (d, J = 10.7 Hz), 123.68,
127.40, 127.65, 128.88, 128.81, 134.56, 134.63, 134.76, 134.89, 135.11,
135.49 (Ar±C), 183.06 (CÐPd). 19F NMR (CDCl3): ꢁ 140.82 (2F,
Fo), 150.57 (1F, Fp), 159.44 (2F, Fm).
Table 2
The intra- and intermolecular hydrogen-bond interactions in (I) (A, ).
ꢀ
Ê
Cg1 and Cg2 are the centroids of the C2A±C7A and C22B±C27B rings,
respectively.
DÐHÁ Á ÁA
DÐH
HÁ Á ÁA
DÁ Á ÁA
DÐHÁ Á ÁA
C21AÐH21AÁ Á Á F1Ai
C11AÐH12AÁ Á ÁF1A
C11BÐH11BÁ Á ÁBr1Bii
C26BÐH26BÁ Á ÁF4Biii
C25BÐH25BÁ Á ÁCg1iv
C3AÐH3AÁ Á ÁCg2v
0.97
0.97
0.97
0.93
0.93
0.93
2.45
2.39
2.89
2.38
2.59
2.78
3.19 (1)
2.80 (1)
3.70 (1)
3.21 (1)
3.41 (1)
3.62 (1)
132
105
142
148
148
150
Symmetry codes: (iii) x 1; y; z; (iv) x 2; y; z 1; (v) x 1; y; z.
Crystal data
The authors acknowledge the Faculty of Arts and Sciences,
Ondokuz Mayõs University, Turkey, for the use of the Stoe
IPDS-II diffractometer (purchased under grant No. F.279 of
È
the University Research Fund) and Dokuz Eylul University
Research Funds (project No. 04.KB.FEN.100).
3
Ê
[PdBr2(C21H13F5N2)2]
Mr = 1042.89
Triclinic, P1
a = 11.6122 (8) A
Ê
b = 12.1401 (9) A
V = 1912.1 (2) A
Z = 2
3
Dx = 1.811 Mg m
Mo Kꢂ radiation
Ê
1
ꢅ = 2.66 mm
T = 293 (2) K
Ê
c = 13.6590 (11) A
ꢂ = 92.589 (6)ꢀ
ꢃ = 95.610 (6)ꢀ
ꢄ = 92.520 (6)ꢀ
Prism, colourless
0.18 Â 0.16 Â 0.09 mm
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: GD3050). Services for accessing these data are
described at the back of the journal.
Data collection
Stoe IPDS-II diffractometer
! scans
Absorption correction: integration
(X-RED32; Stoe & Cie, 2002)
Tmin = 0.646, Tmax = 0.796
23746 measured re¯ections
7493 independent re¯ections
3911 re¯ections with I > 2ꢆ(I)
Rint = 0.121
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91.1 (2)
88.9 (2)
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ꢁ
Acta Cryst. (2006). C62, m535±m537
GokËce et al. [PdBr2(C21H13F5N2)2] m537
È