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Volumn 25, Issue 25, 2006, Pages 5843-5846

Templated synthesis and intact coordination of a diorganotriselenane: [RuCl2(PPh3){κ3-Se,N,N′-Se(mt Se)2}] (mtSe = selenomethimazolyl)

(4) Dewhurst, Rian D a Hansen, Andrew R a Hill, Anthony F a Smith, Matthew K a

a AUSTRALIAN NATIONAL UNIVERSITY (Australia)

Author keywords

[No Author keywords available]

Indexed keywords

COMPLEXATION; COORDINATION REACTIONS; PARAFFINS; SELENIUM COMPOUNDS; SYNTHESIS (CHEMICAL);

BIDENTATE COMPOUNDS; DIORGANOTRISELENANE; METHIMAZOLE;

ORGANOMETALLICS;

EID: 33845887233 PISSN: 02767333 EISSN: None Source Type: Journal
DOI: 10.1021/om0608511 Document Type: Article

Times cited : (22)

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58
- 33845880468
- 4: [RuH(NCMe)2(CO)(PPh3)2]BF4 (250 mg, 0.31 mmol, HmtSe (50 mg, 0.31 mmol, and DBU (200 mg, 1.31 mmol) in CH2C12 (100 mL) were stirred anaerobically for 48 h, diluted with ethanol (100 mL, and slowly concentrated (ca. 50 mL) to provide pale orange crystals. Recrystallized (CH2Cl2/EtOH) yield 147 mg (59, Anal. Found: C, 60.01; H, 4.73; N, 3.60. Calcd for C 41H36N2OP2RuSe: C, 60.44; H, 4.45; N, 3.44. IR (Nujol, 1962w (νRuH, 1899vs (νCO) cm-1. NMR (CDCl3, 25°C) 1H: δH 7.70-7.22 (m, 30 H, C6H5, 5.74, 5.49 (d × 2, 1 H × 2, NCH=CH, 3JHH, 1.5, 2.70 (s, 3H, NCH3, 12.87 t, 1 H, 2JPH, 19.2 Hz, RuH, 31P-{1H, δP 49.79
- P 49.79.

59
- 33845878315
- 1) of the mt ligand: Foreman, M. R. St.-J.; Hill, A. F.; Smith, M. K. Manuscript in preparation.
- 1) of the mt ligand: Foreman, M. R. St.-J.; Hill, A. F.; Smith, M. K. Manuscript in preparation.

60
- 33845906429
- 5: Ethynyltoluene (100 mg, 0.86 mmol) and 4 (70 mg, 0.086 mmol) in toluene (5 mL) were stirred for 18 h and then diluted with methanol (30 mL) to precipitate the product. Recrystallized yield (acetone/Et2O, 29 mg (47, Anal. Found: C, 64.04; H, 4.61; N, 3.28. Calcd for C50H 44OP2- RuSe: C, 64.51; H, 4.76; N, 3.01. IR (Nujol, 1905vs (νCO) cm-1. NMR (CDCl3, 25°C) 1H: δH 7.83 (dt, l H, 3JHH =17.1, 3JPH not resolved, RuCH, 7.64, 7.46, 7.23 (m × 3, 30 H, C6H5, 6.82, 6.36 (d × 2, 2 H × 2, 3JHH, 7.4, C6H4, 6.27, 5.80 (s br × 2, 1 H × 2, NCHCH, 5.85 (d, 1 H, 3J HH, 16.8, RuCH=CH, 2.51 (s, 3 H, NCH3, 2.22 s, 3 H, CCH3, 31P{1H, δP 43.02
- P 43.02.

61
- 33845886472
- 6: [RuCl2(PPh3)3, 261 mg, 0.27 mmol, HmtSe, 87 mg, 0.55 mmol, Na2CO3 (51 mg, 0.48 mmol, and gray selenium (80 mg, l.01 g-atom) were stirred anaerobically in CH2Cl2 (50 mL) for 48 h, filtered through diatomaceous earth, concentrated to ca. 20 mL, layered with light petroleum, and cooled to -20°C overnight to provide black crystals. Yield: 142 mg (63, Anal. Found: C, 34.85; H, 2.97; N, 5.72. Calcd for C26H25N 4PCl2-RuSe3-CH2Cl2: C, 35.24; H, 3.18; N, 6.09. NMR (CDCl3, 25°C) 1H: δH 8, 15 (s br, 1 H, NCH=CH) 7.22 (d, l H, 3J HH, 2.1, NCH=CH, 6.91 (s br, 1 H, NCH=CH, 6.39 (d, l H, 3JHH, 1.5 Hz, NCH=CH, 7.86-7.18 (m, 15 H, C 6H5, 3.64, 3.43 s × 2, 3H × 2, NCH 3, 31P
- 2 = 0.138 [6141 reflections with I > 2σ(I), 2θ < 50.1°], 390 parameters; CCDC 620516.

62
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