Di-, hexa- and poly-nuclear molybdenum(II) carboxylates containing quadruply bonded [Mo2]4+ units: crystal structures of [Mo2(O2CCHF2)2(bpy)2 (MeCN)(BF4)][BF4] and [Mo6(O2CCHF2)12(bpy)4 ] (bpy = 2,2′-bipyridine)
Abstract
The reaction of [Mo
2
(O
2
CMe)
4
] with
an excess of CHF
2
CO
2
H resulted in the formation of
[Mo
2
(O
2
CCHF
2
)
4
]·MeCN
1. Treatment of 1 with Et
3
O
+
gave
[Mo
2
(O
2
CCHF
2
)
2
(MeCN)
4
][BF
4
]
2
2, which was converted into
[Mo
2
(O
2
CCHF
2
)
2
(bpy)
2
(MeCN)(BF
4
)][BF
4
] 3 on addition of
2,2′-bipyridine (bpy). The reaction of 1 and 3 (1∶2) in the
presence of CHF
2
CO
2
-
gave the
`trimer-of-dimers' complex
[Mo
6
(O
2
CCHF
2
)
12
(bpy)
4
] 4 in which two
[Mo
2
(O
2
CCHF
2
)
4
(bpy)
2
] units are the two axial ligands to a central
[Mo
2
(O
2
CCHF
2
)
4
] unit. The
related reaction of 1 and 3 at a 1∶1 ratio in the presence of
CHF
2
CO
2
-
gave
[Mo
4
(O
2
CCHF
2
)
8
(bpy)
2
]
n
5, which was concluded to be a
one-dimensional polymer consisting of alternating
[Mo
2
(O
2
CCHF
2
)
4
(bpy)
2
] and [Mo
2
(O
2
CCHF
2
)
4
]
units identical to those in 4.
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