TY - JOUR
T1 - Synthesis and Characterization of Molybdenum Complexes Containing both End-on Organohydrazido(1−) and Organohydrazido(2−) Ligands. X-ray Crystal Structures of [Mo(NHNPh2)(NNPh2)(acac)Cl2] and [Mo(NHNMePh)(NNMePh)(acac)Cl2]
AU - Bustos, Carlos
AU - Manzur, Carolina
AU - Carrillo, David
AU - Robert, Francis
AU - Gouzerh, Pierre
PY - 1994/3/1
Y1 - 1994/3/1
N2 - In acetonitrile, bis(acetylacetonato)dioxomolybdenum(VI), [MoO2(acac)2], reacts with disubstituted hydrazine hydrohalides (RR′NNH3+X−: R = R′ = Ph; R = Ph, R′ = Me; X = Cl, Br, I) to yield a new series of complexes, which have been characterized by elemental analysis, electrochemistry and spectroscopy (IR, UV-visible, and 1H NMR) and formulated as [Mo(NHNPh2)(NNPh2)(acac)X2] (X = Cl (1), Br (2), I (3)) and [Mo(NHNMePh)- (NNMePh)(acac)X2] (X = Cl (4), Br (5), I (6)). The X-ray crystal structures of 1 and 4 are reported. Crystals of 1 are monoclinic, space group P21/a, with a = 9.352(1) Å,b = 31.320(2) Å, c = 9.612(1) Å, β = 95.35(1)°, and Z = 4. The structure was solved using 3833 unique reflections, and refinement gave final R and Rw values of 0.037 and 0.052, respectively. Crystals of 4 are triclinic, space group P1, with a = 7.765(1) Å, b = 7.715(2) Å, c=17.910(2) Å, α = 89.18(1)°, β=91.35(1)°, γ = 92.64(1)°, and Z = 2. The structure was solved using 4515 unique reflections, and refinement gave final R and Rw values of 0.032 and 0.033, respectively. Both complexes display similar distorted octahedral geometries. The coordination sphere consists of two mutually cis organohydrazido ligands, two mutually trans chloro ligands and one chelated acetylacetonato ligand. The organohydrazido(2−) and organohydrazido(1−) ligands adopt the linear and bent “end-on” conformations, respectively.
AB - In acetonitrile, bis(acetylacetonato)dioxomolybdenum(VI), [MoO2(acac)2], reacts with disubstituted hydrazine hydrohalides (RR′NNH3+X−: R = R′ = Ph; R = Ph, R′ = Me; X = Cl, Br, I) to yield a new series of complexes, which have been characterized by elemental analysis, electrochemistry and spectroscopy (IR, UV-visible, and 1H NMR) and formulated as [Mo(NHNPh2)(NNPh2)(acac)X2] (X = Cl (1), Br (2), I (3)) and [Mo(NHNMePh)- (NNMePh)(acac)X2] (X = Cl (4), Br (5), I (6)). The X-ray crystal structures of 1 and 4 are reported. Crystals of 1 are monoclinic, space group P21/a, with a = 9.352(1) Å,b = 31.320(2) Å, c = 9.612(1) Å, β = 95.35(1)°, and Z = 4. The structure was solved using 3833 unique reflections, and refinement gave final R and Rw values of 0.037 and 0.052, respectively. Crystals of 4 are triclinic, space group P1, with a = 7.765(1) Å, b = 7.715(2) Å, c=17.910(2) Å, α = 89.18(1)°, β=91.35(1)°, γ = 92.64(1)°, and Z = 2. The structure was solved using 4515 unique reflections, and refinement gave final R and Rw values of 0.032 and 0.033, respectively. Both complexes display similar distorted octahedral geometries. The coordination sphere consists of two mutually cis organohydrazido ligands, two mutually trans chloro ligands and one chelated acetylacetonato ligand. The organohydrazido(2−) and organohydrazido(1−) ligands adopt the linear and bent “end-on” conformations, respectively.
UR - http://www.scopus.com/inward/record.url?scp=0001225081&partnerID=8YFLogxK
U2 - 10.1021/ic00085a035
DO - 10.1021/ic00085a035
M3 - Article
AN - SCOPUS:0001225081
SN - 0020-1669
VL - 33
SP - 1427
EP - 1433
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 7
ER -