3

A new route for synthesis of [(η5-C5H5)L2Ru(μ-CN)RuL′2(η5-C5H5)]+X−(L, L′ PPh3, AsPh3 or SbPh3; L2, L′2 PPh2CH2CH2PPh2 or PPh2CH2PPh2; X− =BF4−, PF6− or BPh4−) using

Embed Size (px)

Citation preview

210

TABLE 1. Characterisation data of the complexes

Ligand?

Ll L2 L3 J-4

P P P P

P P P P

P P P P

Anion Colour , IR $-CsHs ‘H NMR Analyses: found (talc.) 31~ (‘H}NMR X- (melting point CC)) (cm-‘)

Yield (%) lC 2d C H N

PF6 Yb, (178-180) 60

2080 4.19 4.05

BF4 Y, (148) 56

Y, (152) 61

2060 4.18 4.06

BPh4 2085 4.18 4.05

63.8 4.22 0.87 (64.2) (4.51) (0.9)

67.3 4.8 1.12 (67.5) (4.7) (0.93)

74.1 5.6 0.79 (74.4) (5.2) (0.81)

60.1 4.5 0.90 (60.7) (4.27) (0.85)

62.6 4.7 1.21 (63.75) (4.4) (0.88)

71.0 4.7 0.72 (70.8) (4.96) (0.77)

58.0 4.12 0.88 (57.6) (4.05) (0.81)

60.1 4.51 1.1 (60.4) (4.2) (0.8)

67.9 4.3 0.69 (67.5) (4.73) (0.73)

52.8 3.7 0.78 (52.0) (3.65) (0.73)

54.1 3.51 1.2 (54.3) (3.76) (0.75)

61.2 4.6 0.70 (61.5) (4.3) (0.67)

57.2 4.53 1.16 (58.2) (4.45) (1.1)

60.3 4.3 1.18

(60.9) (4.67) (1.12) 70.2 5.6 1.01

(70.9) (5.29) (0.95)

57.1 4.6 1.2 (57.6) (4.24) (1.1)

60.9 4.7 1.19 (60.3) (4.45) (1.15)

71.0 5.2 0.90 (70.6) (5.1) (0.96)

47.3 41.6

47.4 41.5

47.6 41.6

46.9 40.8

47.0 40.6

46.8 40.7

A P A P PFe

A P A P

A P A P

A A A A

A A A A

A A A A

Sb Sb Sb Sb

Sb Sb Sb Sb

Sb Sb Sb Sb

dppe dppe

dppe dppe

dppe dppe

dppm dppm

dppm dppm

dppm dppm

BF4

BPh4

PF6

BF4

BPh4

PFe

BF4

BPh4

PFe

BF4

BPh4

PF6

BF4

BPh,,

Y, (175 59

Y, (153) 58

Y, (155) 62

Y, (172-175) 60

Y, (152) 58

Y, (149) 61

Y, (176) 60

Y, (157) 59

Y, (160) 61

Y, >235 60

Y, (220) 60

Y, (224) 58

Y, (172-175) 61

Y, (168) 57

Y, (159) 60

2080 4.19 4.06

2080 4.18 4.05

2090 4.20 4.07

2090 4.20 4.08

2070 4.18 4.06

2080 4.18 4.07

2085

2070

2085

2110

2100

2090

2090

2100

2100

4.36 4.10 4.22 4.08

4.33 4.09

4.21 3.9

4.35 4.09 4.22 4.0

4.35 4.17

4.36 4.15

4.35 4.16

4.30 4.16

4.32

4.30

4.15

4.17

82.1 79.7

82.3 79.8

82.2 79.7

81.8 78.1

81.6 78.3

81.7 78.2

aP = PPhs, A = AsPhs, Sb = SbPhs, dppe = 1,2-bis(diphenyIphosphino)ethane, dppm = bis(diphenylphosphino)methane. by=

yellow. c1, Cp linked with Ru-CN-. d2, Cp linked with Ru-NC-.

releasing one mole of NH3 and the resulting product subsequently interacts with another mole of [Ru- (r$-CsHs)b]’ forming a more stable CN bridged complex. The work on this and other reactions is under progress.

Acknowledgement

Thanks are due to CSIR, New Delhi for the award of a Senior Research Fellowship to one of the authors (A.M.).

211

References 5 C. W. Bird, Tetrahedron, 42 (1986) 89. 6 R. J. Boyd, Sai Cheng Choi and C. C. Hale, Chem. Phys.

E. M. Smolin and L. Rapoport, S-Triazine and Deriv- atives, The Chemistry of Heterocyclic Compounds, Interscience, New York, 1959. D. Martin, M. Bauer and V. A. Pankratov, Russ. Chem. Rev., 47 (1978) 10. Ch. Grundmann, Angew. Chem., Int. Ed, Engl., 2 (1963) 309. A. S. Gordetsov and Yu. I. Dergunov, Russ. Chem. Rev., 54 (1985) 2076.

L&r., Iii (1984) 136. 7 K. Jue.J. Ora. Chem.. 48 (1983) 1344. 8 M. MLot-Ne; (Mautner), j. Am. Chem. Sot., 10 (1979)

2396. 9 K. Mohan Rao, R. Prasad and U. C. Agarwala, Syn.

React. Inorg. Met. Org. Chem., 5 (1987) 469, and refs. therein.

10 G. J. Baird, S. G. Davies, S. D. Moon and S. J. Simpson, J. Chem. Sot. Dalton Trans., (1985) 1479, and refs. therein.