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dried in air. Yield 85%. Anal. Found: C, 61.0; H, 7.7;
N, 14.4; S 11.7. C15H23N3OS Anal. Calc.: C, 61.4; H,
7.9; N, 14.3; S, 11.9%. IR: w(CꢀS) 845 m cm−1; w(CꢀN)
3.2.9. [Pt{C6H4C(CH3(CH2)10)ꢀNNꢀC(S)NH2}]4 (1d)
Yield 60%. Anal. Found: C, 43.4; H, 5.4; N, 7.7; S,
6.1. C76H116N12S4Pt4 Anal. Calc.: C, 43.3; H, 5.5; N,
1620 s cm−1
.
8.0; S 6.1%. IR: w(CꢀN) 1610 s cm−1
.
Thiosemicarbazones b–e were prepared following a
similar procedure.
3.2.10. [Pt{4-MeC6H3C(Me)ꢀNNꢀC(S)NHMe}]4 (1e)
Yield 50%. Anal. Found: C, 31.9; H, 3.1; N, 10.2; S,
7.6. C44H52N12S4Pt4 Anal. Calc.: C, 31.9; H, 3.2; N,
10.1; S 7.7%. IR: w(CꢀN) 1615 s cm−1
.
3.2.2. 4-MeC6H4C(Me)ꢀNN(H)ꢀC(S)NH2 (b)
Yield 80%. Anal. Found: C, 58.3; H, 6.3; N, 20.3; S
15.6. C10H13N3S Anal. Calc.: C, 57.9; H, 6.3; N, 20.3; S,
15.5%. IR: w(CꢀS) 820 m cm−1; w(CꢀN) 1615 sh, s
3.2.11. Preparation of [Pt{3-CH3(CH2)5OC6H3C-
(Me)ꢀNNꢀC(S)NH2}(PPh3)] (2a)
cm−1
.
PPh3 (27.0 mg, 0.103 mmol) was added to a suspen-
sion of 1a (50.0 mg, 0.026 mmol) in acetone (15 cm3).
The solution was stirred for 4 h, the solvent removed in
vacuo and the resulting yellow solid recrystallised from
acetone–n-hexane. Yield 75%. Anal. Found: C, 52.9;
H, 4.7; N, 5.7; S, 4.2. C33H36N3OSPtP Anal. Calc.: C,
3.2.3. C6H5C(Et)ꢀNN(H)ꢀC(S)NH2 (c)
Yield 75%. Anal. Found: C, 58.1; H, 6.5; N, 20.3; S
15.6. C10H13N3S Anal. Calc.: C, 57.9; H, 6.3; N, 20.3; S,
15.5%. IR: w(CꢀS) 820 m cm−1; w(CꢀN) 1620 s cm−1
.
52.9; H, 4.8; N, 5.6; S, 4.3%. IR: w(CꢀN) 1620 s cm−1
.
3.2.4. C6H5C{CH3(CH2)10}ꢀNN(H)ꢀC(S)NH2 (d)
3.2.12. [Pt{4-MeC6H3C(Me)ꢀNNꢀC(S)NH2}(PPh3)]
(2b)
Compound 2b was synthesised following a similar
procedure to that for 2a, but after stirring the cy-
clometallated compound–phosphine mixture, an or-
ange precipitate appeared which was filtered off and
dried in vacuo.
Yield 50%. Anal. Found: C, 68.1; H, 9.3; N, 12.8; S,
9.9. C19H31N3S Anal. Calc.: C, 68.4; H, 9.4; N, 12.6; S,
9.6%. IR: w(CꢀS) 825 m cm−1; w(CꢀN) 1620 sh, s
cm−1
.
3.2.5. 4-MeC6H4C(Me)ꢀNN(H)ꢀC(S)NHMe (e)
Yield 85%. Anal. Found: C, 59.5; H, 6.8; N, 18.9; S
14.6. C11H15N3S Anal. Calc.: C, 59.7; H, 6.8; N, 19.0; S,
Yield 80%. Anal. Found: C, 50.5; H, 4.0; N, 6.5; S,
4.7. C28H26N3SPtP Anal. Calc.: C, 50.7; H,3.9; N, 6.3;
S, 4.8%. IR: w(CꢀN) 1605 sh, s cm−1
.
14.5%. IR: w(CꢀS) 825 s cm−1; w(CꢀS) 1620 m cm−1
.
Compounds 3a and 2e were synthesised following a
similar procedure to that for 2a as orange solids.
Compounds 2c and 2d were synthesised following a
similar procedure to that for 2b as orange solids.
3.2.6. Preparation of
[Pt{3-CH3(CH2)5OC6H3C(Me)ꢀNNꢀC(S)NH2}]4 (1a)
To a stirred solution of potassium tetrachloroplati-
nate (200 mg, 0.48 mmol) in water (3 cm3), ethanol was
added (27 cm3). The fine yellow suspension of potas-
sium tetrachloroplatinate obtained was treated with
3-CH3(CH2)5OC6H4C(Me)ꢀNN(H)C(ꢀS)NH2 (a) (160
mg, 0.55 mmol). The mixture was stirred for 48 h at
60°C. After cooling to room temperature, the orange
precipitate formed was filtered off, washed with ethanol
and dried in air. Yield 71%. Anal. Found: C, 37.0; H,
4.0; N, 8.4; S 6.5. C60H84N12O4S4Pt4 Anal. Calc.: C,
3.2.13. [Pt{C6H4C(Et)ꢀNNꢀC(S)NH2}(PPh3)] (2c)
Yield 80%. Anal. Found: C, 50.5; H, 4.2; N, 6.6; S,
4.7. C28H26N3SPtP Anal. Calc.: C, 50.7; H, 3.9; N, 6.3;
S, 4.8%. IR: w(CꢀN) 1580 s cm−1
.
3.2.14. [Pt{C6H4C(CH3(CH2)10)ꢀNNꢀC(S)NH2}(PPh3)]
(2d)
Yield 50%. Anal. Found: C, 57.0; H, 4.0; N, 5.4; S,
4.1. C37H34N3SPtP Anal. Calc.: C, 57.1; H, 4.4; N, 5.4;
37.0; H, 4.3; N, 8.6; S, 6.6%. IR: w(CꢀN) 1620 s cm−1
Compounds 1b–1e were obtained following a similar
.
S, 4.1%. IR: w(CꢀN) 1605 s cm−1
.
procedure as orange solids.
3.2.15. [Pt{4-MeC6H3C(Me)ꢀNNꢀC(S)NHMe}(PPh3)]
(2e)
Yield 30%. Anal. Found: C, 51.5; H, 4.2; N, 6.2; S,
3.2.7. [Pt{4-MeC6H3C(Me)ꢀNNꢀC(S)NH2}]4 (1b)
Yield 66%. Anal. Found: C, 30.2; H, 2.9; N, 10.0; S,
8.4. C40H44N12S4Pt4 Anal. Calc.: C, 30.0; H, 2.8; N,
4.6. C29H28N3SPtP Anal. Calc.: C, 51.5; H, 4.2; N, 6.2;
S, 4.7%. IR: w(CꢀN) 1580 s cm−1
.
10.5; S 8.0%. IR: w(CꢀN) 1610 sh, m cm−1
.
3.2.16. [Pt{3-CH3(CH2)5OC6H3C(Me)ꢀNNꢀC(S)NH2}-
(P(4-MeOC6H4)3)] (3a)
Yield 60%. Anal. Found: C, 51.5; H, 5.2; N, 5.2; S,
3.2.8. [Pt{C6H4C(Et)ꢀNNꢀC(S)NH2}]4 (1c)
Yield 70%. Anal. Found: C, 30.4; H,3.0; N, 10.0; S,
8.2. C40H44N12S4Pt4 Anal. Calc.: C, 30.0; H, 2.8; N,
3.9. C36H42N3O4SPtP Anal. Calc.: C, 51.5; H, 5.0; N,
10.5; S 8.0%. IR: w(CꢀN) 1610 sh, s cm−1
.
5.0; S, 3.8%. IR: w(CꢀN) 1615 s cm−1
.