TY - JOUR
T1 - [o-Phenylenebis(dimethylarsine)]heptacarbonyldiiron. Preparation, Crystal Structure, and Fluxionality in Solution
AU - Bailey, Webb I.
AU - Bino, Avi
AU - Cotton, F. Albert
AU - Kolthammer, Brian W.S.
AU - Lahuerta, Pascual
AU - Puebla, P.
AU - Uson, R.
PY - 1982
Y1 - 1982
N2 - The reaction of Fe2(CO)9 with o-phenylenebis(dimethylarsine), diars, in an atmosphere of CO gives yellow (diars) Fe2(CO)8 and red (diars)Fe2(CO)7, separable by chromatography on silica. The red compound crystallizes in space group [formula omitted] with Z = 2 and the following unit cell dimensions: a = 9.706 (4) Å b = 11.876 (3) Å c = 9.576 (3) Å β = 92.41 (2)°; β = 104.81 (2)°; γ = 91.25 (2)°; V = 1066 (1) Å3. The structure consists of dinuclear molecules in which diars is chelated on one iron atom (Fe(1)) to which are also bound two terminal CO groups. Fe(1) also forms a metal-metal bond, 2.566 (1) Å, to Fe(2), which bears three strictly terminal CO groups. Of the remaining two CO groups, one forms a nearly symmetrical bridge while the other is semibridging with its short bond, 1.894 (7) Å, to Fe(2) and its long bond, 2.103 (7) Å, to Fe(1). The 13C NMR spectrum is highly temperature dependent, changing from a five-line spectrum (1:2:2:1:1) at −132 °C to a single-line spectrum at 11°C. A three-stage process for equivalencing all of the CO's is proposed.
AB - The reaction of Fe2(CO)9 with o-phenylenebis(dimethylarsine), diars, in an atmosphere of CO gives yellow (diars) Fe2(CO)8 and red (diars)Fe2(CO)7, separable by chromatography on silica. The red compound crystallizes in space group [formula omitted] with Z = 2 and the following unit cell dimensions: a = 9.706 (4) Å b = 11.876 (3) Å c = 9.576 (3) Å β = 92.41 (2)°; β = 104.81 (2)°; γ = 91.25 (2)°; V = 1066 (1) Å3. The structure consists of dinuclear molecules in which diars is chelated on one iron atom (Fe(1)) to which are also bound two terminal CO groups. Fe(1) also forms a metal-metal bond, 2.566 (1) Å, to Fe(2), which bears three strictly terminal CO groups. Of the remaining two CO groups, one forms a nearly symmetrical bridge while the other is semibridging with its short bond, 1.894 (7) Å, to Fe(2) and its long bond, 2.103 (7) Å, to Fe(1). The 13C NMR spectrum is highly temperature dependent, changing from a five-line spectrum (1:2:2:1:1) at −132 °C to a single-line spectrum at 11°C. A three-stage process for equivalencing all of the CO's is proposed.
UR - http://www.scopus.com/inward/record.url?scp=33751401915&partnerID=8YFLogxK
U2 - 10.1021/ic00131a054
DO - 10.1021/ic00131a054
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AN - SCOPUS:33751401915
SN - 0020-1669
VL - 21
SP - 289
EP - 294
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 1
ER -