Title compound,Mr=1273.16,was synthesized by a substitution reaction and its crystal' is triclinic belonging to space group P1 with cell parameters:a=13.944(2),b=14.143(7),c=14.233(3), A,a=77.35(3)°,β=69.94(...Title compound,Mr=1273.16,was synthesized by a substitution reaction and its crystal' is triclinic belonging to space group P1 with cell parameters:a=13.944(2),b=14.143(7),c=14.233(3), A,a=77.35(3)°,β=69.94(2)°,γ=63.50(3)°,V=2351(1)A^3,Z=2,D_c=1.799g cm^(-3).Room tem- perature,graphite-filtered Mo K_α,radiation(λ=0.71073A)was used for data collection.μ=14.988 cm^(-1),F(000)=1280,R=0.051 for 7025 observed reflections.The crystal consists of decrete cluster molecules containing a duster core[Mo_3(μ_3-S)]^(10+)with three μ-S,one μ-dtp(dtp=[S_2P(OC_2H_5)]^(2-), three x-dtp and one allylthioureo to form a local six-coordinated sphere around each Mo atom.The bónds of cluster skeleton[Mo_3(μ_3-S)(μ-S)_3]^(4+),Mo—Mo 2.744～2.766,Mo—(μ_3-S)2.340～2.342 and Mo—(μ-S)2.272～2.296 A,are comparable with those found in the related analogues.展开更多
The reaction of trinuclear molybdenum cluster{Mo_3S_4(μ-dtp)(dtp)_3(H_2O)}1[dtp= S_2P(OEt)_2]with RCO_2Na(R=H,CH_3)in the presence of Py gave the black compounds{Mo_3S_4(μ- O_2CR)(dtp)_3(Py)}(2,R=H,3,R=CH_3).Both co...The reaction of trinuclear molybdenum cluster{Mo_3S_4(μ-dtp)(dtp)_3(H_2O)}1[dtp= S_2P(OEt)_2]with RCO_2Na(R=H,CH_3)in the presence of Py gave the black compounds{Mo_3S_4(μ- O_2CR)(dtp)_3(Py)}(2,R=H,3,R=CH_3).Both compounds are characterized by X-ray crystallo- graphy.It is shown that crystals 2 and 3 belong to space group P with Z=2 and a=10.519(2),b= 12.121(2),c=15.757(2),α=93.27(1),β=94.63(1),γ=105.22(1)°,V=1925~3 for crystal 2,whereas a=9.556(2),b=14.067(7),c=15.914(9),α=101.41(4),β=101.44(4),γ=74.26(3)°,V=1994~3 for crystal 3.The final R factors are 0.041 and 0.048 for crystal 2 and 3 respectively.The structure analysis indicates that(O_2CR)^- ligand selectively substitutes the bridging(dtp)ligand.This type of Mo_3 cluster molecule where structure contains two species of bidentate ligand is for the first time to be obtained by us.展开更多
文摘Title compound,Mr=1273.16,was synthesized by a substitution reaction and its crystal' is triclinic belonging to space group P1 with cell parameters:a=13.944(2),b=14.143(7),c=14.233(3), A,a=77.35(3)°,β=69.94(2)°,γ=63.50(3)°,V=2351(1)A^3,Z=2,D_c=1.799g cm^(-3).Room tem- perature,graphite-filtered Mo K_α,radiation(λ=0.71073A)was used for data collection.μ=14.988 cm^(-1),F(000)=1280,R=0.051 for 7025 observed reflections.The crystal consists of decrete cluster molecules containing a duster core[Mo_3(μ_3-S)]^(10+)with three μ-S,one μ-dtp(dtp=[S_2P(OC_2H_5)]^(2-), three x-dtp and one allylthioureo to form a local six-coordinated sphere around each Mo atom.The bónds of cluster skeleton[Mo_3(μ_3-S)(μ-S)_3]^(4+),Mo—Mo 2.744～2.766,Mo—(μ_3-S)2.340～2.342 and Mo—(μ-S)2.272～2.296 A,are comparable with those found in the related analogues.
文摘The reaction of trinuclear molybdenum cluster{Mo_3S_4(μ-dtp)(dtp)_3(H_2O)}1[dtp= S_2P(OEt)_2]with RCO_2Na(R=H,CH_3)in the presence of Py gave the black compounds{Mo_3S_4(μ- O_2CR)(dtp)_3(Py)}(2,R=H,3,R=CH_3).Both compounds are characterized by X-ray crystallo- graphy.It is shown that crystals 2 and 3 belong to space group P with Z=2 and a=10.519(2),b= 12.121(2),c=15.757(2),α=93.27(1),β=94.63(1),γ=105.22(1)°,V=1925~3 for crystal 2,whereas a=9.556(2),b=14.067(7),c=15.914(9),α=101.41(4),β=101.44(4),γ=74.26(3)°,V=1994~3 for crystal 3.The final R factors are 0.041 and 0.048 for crystal 2 and 3 respectively.The structure analysis indicates that(O_2CR)^- ligand selectively substitutes the bridging(dtp)ligand.This type of Mo_3 cluster molecule where structure contains two species of bidentate ligand is for the first time to be obtained by us.
