TY - JOUR
T1 - Preparation and Characterization of Bis[(μ-acetato)halo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes
AU - Arnold, Deirdre I.
AU - Cotton, F. Albert
AU - Kühn, Fritz E.
PY - 1996
Y1 - 1996
N2 - Molecules of the formula Mo2X2(OAc)2(μ-dppa)2 (X = Cl (2), Br (3), I (4); dppa = bis(diphenylphosphino)-amine; OAc = CH3COO-) can be synthesized by the reaction of Mo2(OAc)4 (1) with dppa and (CH3)3SiX. All three compounds were characterized by IR and UV-visible spectroscopy, mass spectrometry, and 31P{1H} NMR spectroscopy. Single-crystal diffraction studies yield the following pertinent crystal data: for 2·2EtOH, orthorhombic Pbca (No. 61), a = 16.830(2) Å, b = 20.310(4) Å, c = 16.751(2) Å V = 5726(2) Å3, Z = 4; for 3·2(toluene), monoclinic C2lc (No. 15), a = 22.481(2) Å, b = 19.151(9) Å, c = 14.358(2) Å, β = 95.19(2)°, V = 6156(3) Å3, Z = 4; for 4·EtOH·CH3CN, monoclinic P21/c (No. 14), a = 20.607(9)Å, b = 16.020(3) Å, c = 17.189(5) Å, β = 95.81(2)°, V = 5645(3) Å3, Z = 4. The Mo-Mo distances for compounds 2-4 are 2.158(1), 2.176(1), and 2.164(1) Å, respectively. Both crystallographic data and physical measurements indicate that 2 and 3 have nearly identical Mo-X bond distances while those in 3 and 4 differ more significantly; the spectroscopic data bear this out. The Mo-O and Mo-P distances are very similar in all three of the complexes reported.
AB - Molecules of the formula Mo2X2(OAc)2(μ-dppa)2 (X = Cl (2), Br (3), I (4); dppa = bis(diphenylphosphino)-amine; OAc = CH3COO-) can be synthesized by the reaction of Mo2(OAc)4 (1) with dppa and (CH3)3SiX. All three compounds were characterized by IR and UV-visible spectroscopy, mass spectrometry, and 31P{1H} NMR spectroscopy. Single-crystal diffraction studies yield the following pertinent crystal data: for 2·2EtOH, orthorhombic Pbca (No. 61), a = 16.830(2) Å, b = 20.310(4) Å, c = 16.751(2) Å V = 5726(2) Å3, Z = 4; for 3·2(toluene), monoclinic C2lc (No. 15), a = 22.481(2) Å, b = 19.151(9) Å, c = 14.358(2) Å, β = 95.19(2)°, V = 6156(3) Å3, Z = 4; for 4·EtOH·CH3CN, monoclinic P21/c (No. 14), a = 20.607(9)Å, b = 16.020(3) Å, c = 17.189(5) Å, β = 95.81(2)°, V = 5645(3) Å3, Z = 4. The Mo-Mo distances for compounds 2-4 are 2.158(1), 2.176(1), and 2.164(1) Å, respectively. Both crystallographic data and physical measurements indicate that 2 and 3 have nearly identical Mo-X bond distances while those in 3 and 4 differ more significantly; the spectroscopic data bear this out. The Mo-O and Mo-P distances are very similar in all three of the complexes reported.
UR - http://www.scopus.com/inward/record.url?scp=0000019209&partnerID=8YFLogxK
U2 - 10.1021/ic9514758
DO - 10.1021/ic9514758
M3 - Article
AN - SCOPUS:0000019209
SN - 0020-1669
VL - 35
SP - 4733
EP - 4737
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 16
ER -