0000000000132282
AUTHOR
Angeles Monge
ChemInform Abstract: Formation in Solution, Synthesis and Crystal Structure of μ-Oxalatobis(bis(2-pyridylcarbonyl)amido)dicopper(II).
Abstract The compound μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II), [Cu 2 {(NCsH 5 CO) 2 N} 2 - (C 2 O 4 )] was synthesized and characterized by spectroscopy, EPR and diffraction methods. It crystallizes in the triclinic space group P 1 with cell constants: a =7.6793(6), b =9.238(2), c =10.007(2) A, α=83.80(1), β=68.37(1) and γ=69.44(1)°; V =617.7(3) A 3 , D (calc., Z =2)=1.80 g cm −3 , M r =667.6, F (000)=336, λ, (Mo Kα)=0.71069 A, μ (Mo Kα)=17.895 cm −1 and T =295 K. A total of 3587 data were collected over the range of 1 ⩽ θ ⩽ 30°; of these, 2391 (independent and with I⩾2σ( I )) were used in the structural analysis. The final R and R w residuals were 0.049 and 0.053, respective…
Synthesis and magnetic properties of bis(μ-hydroxo)bis[(2,2 ′-bipyridyl)copper(II)] squarate. Crystal structure of bis(μ-hydroxo)bis[(2,2′-bipyridyl)copper(II)] squarate tetrahydrate
Abstract The compound [Cu2(bipy)2(OH)2](C4O4)·5.5H2O, where bipy and C4O42− correspond to 2,2′-bipyridyl and squarate (dianion of 3,4-dihydroxy-3-cyclo- butene-1,3-dione) respectively, has been synthesized. Its magnetic properties have been investigated in the 2–300 K temperature range. The ground state is a spin-triplet state, with a singlet-triplet separation of 145 cm−1. The EPR powder spectrum confirms the nature of the ground state. Well-formed single crystals of the tetrahydrate, [Cu2(bipy)2(OH)2](C4O4)·4H2O, were grown from aqueous solutions and characterized by X-ray diffraction. The system is triclinic, space group P 1 , with a = 9.022(2), b = 9.040(2), c = 8.409(2) A, α = 103.51(2…
ChemInform Abstract: Synthesis and Magnetic Properties of Bis(μ-hydroxo)bis((2,2′-bipyridyl)copper(II)) Squarate. Crystal Structure of Bis(μ-hydroxo)bis((2,2′-bipyridyl)copper(II)) Squarate Tetrahydrate.
Abstract The compound [Cu2(bipy)2(OH)2](C4O4)·5.5H2O, where bipy and C4O42− correspond to 2,2′-bipyridyl and squarate (dianion of 3,4-dihydroxy-3-cyclo- butene-1,3-dione) respectively, has been synthesized. Its magnetic properties have been investigated in the 2–300 K temperature range. The ground state is a spin-triplet state, with a singlet-triplet separation of 145 cm−1. The EPR powder spectrum confirms the nature of the ground state. Well-formed single crystals of the tetrahydrate, [Cu2(bipy)2(OH)2](C4O4)·4H2O, were grown from aqueous solutions and characterized by X-ray diffraction. The system is triclinic, space group P 1 , with a = 9.022(2), b = 9.040(2), c = 8.409(2) A, α = 103.51(2…
Formation in solution, synthesis and crystal structure of μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II)
Abstract The compound μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II), [Cu 2 {(NCsH 5 CO) 2 N} 2 - (C 2 O 4 )] was synthesized and characterized by spectroscopy, EPR and diffraction methods. It crystallizes in the triclinic space group P 1 with cell constants: a =7.6793(6), b =9.238(2), c =10.007(2) A, α=83.80(1), β=68.37(1) and γ=69.44(1)°; V =617.7(3) A 3 , D (calc., Z =2)=1.80 g cm −3 , M r =667.6, F (000)=336, λ, (Mo Kα)=0.71069 A, μ (Mo Kα)=17.895 cm −1 and T =295 K. A total of 3587 data were collected over the range of 1 ⩽ θ ⩽ 30°; of these, 2391 (independent and with I⩾2σ( I )) were used in the structural analysis. The final R and R w residuals were 0.049 and 0.053, respective…
Effects of substitutions on cyclopentadienyl rings in complexes with molybdenum-mercury bonds. 95Mo and 199Hg NMR studies
NMR data for 95Mo and 199Hg nuclei have been obtained for new di- and trimetallic complexes Cp′(CO)3MoHgX containing molybdenum-mercury bonds and bulky and/or potentially bifunctional substituted cyclopentadienyl ligands; Cp′=C5HMe2Ph2, C5Me4Bz, C5Bz5, C5H4PPh2 and C5Me4PPh2 (Bz=CH2C6H5; Me =CH3; Ph=C6H5); X=Cp′(CO)3Mo, Cl, Br, 1, SCN. They are discussed within the context of our earlier results reported for analogous complexes with the cyclopentadienyl ligands bearing methyl groups. With the exception of phenyl substituted rings, a rather narrow range of 95Mo chemical shifts is found for the compounds with the same number of different substituents on cyclopentadienyl ligands. An outstandin…
Isolation of enantiomerically pure organometallic palladium compounds: synthesis of the triangles prepared from enantiopure [cis-Pd2(C6H4PPh2)2(NCCH3)4]2+
Reaction of the racemic [Pd(C(6)H(4)PPh(2))Br](4) () with the silver salt of 1R-(1alpha,2beta,3alpha)]-3-methyl-2-(nitromethyl)-5-oxocyclopentaneacetate, (R)-AgO(2)CR*, results in the formation of a mixture of diastereoisomers (RRR)- and (SRR)- of the formula Pd(2)(C(6)H(4)PPh(2))(2)(O(2)CR*)(2) that were separated by standard chromatographic methods. Each diastereoisomer was readily converted into the tetrametallic stereoisomers (SS)- and (RR)-, of the formula [Pd(C(6)H(4)PPh(2))Br](4) that were isolated and characterized by X-ray crystallography. The R enantiomer of the solvated cationic species [cis-Pd(2)(C(6)H(4)PPh(2))(2)(NCCH(3))(4)](2+), obtained from (RR)-, was reacted with ammonium…
Diastereospecific control in the synthesis of enantiomerically pure bis-equatorial rhodium(II) catalysts by chiral phosphanes
The reaction of Rh2(O2CR)4 [R = CH3, CF3] with the chiral phosphane (1S,2S,5R)-(2-hydroxy-5-isopropenyl-2-methylcyclohexyl)(diphenyl)phosphane, (+)PPh2(CH−R*−OH) or its enantiomer (1R,2R,5S)-(2-hydroxy-5-isopropenyl-2-methylcyclohexyl)(diphenyl)phosphane, (−)-PPh2(CH−R*−OH), results in the specific formation of the products (P)-Rh2(μ-O2CR)2(η1-O2CR)2{η2-(+)PPh2(CH−R*−OH)}2 [P(+)1, R = CH3; P(+)2 R = CF3] and (M)-Rh2(μ-O2CR)2(η1-O2CR)2{η2-(−)-PPh2(CH−R*−OH)}2 [M(−)1, R = CH3; M(−)2, R = CF3] in a high yield. Their synthesis, characterisation and catalytic behaviour in metal−carbenoid reactions are reported. X-ray analysis of P(+)2 and M(−)2 shows, in each case, a Rh24+ unit supported by two …