Tri(2-furyl)phosphine (PFu3) reacts with [Ru4(μ-H)4(CO)12] (1) in refluxing THF to give,
apart from an isomeric pair of the substituton products [Ru4(μ-H)4(CO)10(PFu3)2] (2a and
2b), the μ-phosphido cluster [Ru4(μ-H)2(CO)8(PFu3)2(μ-PFu2)(μ-η
1,η
2-C4H3O)] (3) and a series
of μ
3- and μ
4-phosphinidene clusters [Ru4(μ-H)2(CO)12
-
x
(PFu3)
x
(μ
3-PFu)] (x = 0 (4), 2 (5), 3
(6)) and [Ru4(μ-H)2(CO)9(PFu3)2(μ
4-PFu)(μ
3-η
1,η
1,η
2-C4H2O)] (7). In this one-pot reaction, the
excellent facility for PFu3 to act as rich sources of furyl, furyne, phosphide (μ-PR2), and
phosphinidene (μ
3-PR and μ
4-PR) fragments on tetrametallic frameworks has been demonstrated. The single-crystal X-ray structures of all new molecules have been determined. The
structure of 7 represents the first structurally characterized example of stable furyne-containing cluster complexes of ruthenium. The electrochemical behavior and molecular
orbital calculations of these metallophosphorus clusters have been examined as a function
of the coordination modes of the phosphorus-containing moieties.
Treatment of [Os3(CO)10(NCMe)2] with platinum bis(alkynyl) complexes cis‐[Pt(C≡CPh)2(L)] [L = 4,4′‐dimethyl‐2,2′‐bipyridine (Me2bipy), 4,4′‐bis(tert‐butyl)‐2,2′‐bipyridine (tBu2bipy)] at room temperature readily affords the novel, spiked‐triangular heterometallic cluster complexes [Os3Pt(CO)9(μ4‐η2‐C≡CPh)(η1‐C≡CPh)(L)] (L = Me2bipy 1, tBu2bipy 2) in moderate yields. X‐ray analysis of both complexes reveals that one alkynyl moiety is coordinated to the metal atoms in a μ4‐η2(||) mode, accompanied by a concomitant transfer of an η1‐C≡CPh group from the platinum centre to the osmium atom to give a metal framework with an osmium atom apically bonded to an Os2Pt triangle.
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