The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1...The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1H/13C--NMR. Theproposal concerning mechanism was discussed herewith and the structure was reportedas well. Crystallographic data: Mr= 563. 85, monoclinicl P21/n(# 14); a= 8. 009(2), b= 17. 600(5), c=12. 003(4) A; β=95. 91(2)°; V= 1683. 0 (9) A3; Z=4;Dc=2. 22 g. cm-3; F(000) = 1048, μ=89. 27 cm-1 ; final R=0. 039 and Rw=0. 049for 2121 observable reflections with (I≥3. cσ(I) ). The crystal structure determinationshows that S atom coordinates to all three metal (W,Fe,Co) atoms in a μ3,-fashion,thetitle cluster core has the tetrahedral skeleton.展开更多
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 complex [Et4N][(Ph3P)2{CuS2WS2Fe} Br2] (1 ), C44, H50NBr2CuFeP2S4W, M4= 1246. 13, has been obtained by reaction of [Et4N]2[WS4] andFeBr2 with Cu (Ph3P )3I in MeCN/CH2Cl2. Crystal data for [Et4N][(Ph3P)2{CuS2WS2Fe)...The complex [Et4N][(Ph3P)2{CuS2WS2Fe} Br2] (1 ), C44, H50NBr2CuFeP2S4W, M4= 1246. 13, has been obtained by reaction of [Et4N]2[WS4] andFeBr2 with Cu (Ph3P )3I in MeCN/CH2Cl2. Crystal data for [Et4N][(Ph3P)2{CuS2WS2Fe) Br2] (1): triclinic, P1, Z = 2, a= 13. 495 (7), b = 15. 322 (5), c =12. 361 (4), a=105. 32(3), β=93. 19(4), γ=101. 35(4) and V=2401. 2 The bond lengths of W-Fe bond and the W-Cu distance are 2. 793(2) A and 2. 823(2), respectively. Three kind metal atoms of the title structure [Et4N][(Ph3P)2{CuS2WS2Fe}Br2] (1) are nearly distributed along a line, and along which three metalatoms (W, Cu, Fe) are approximately tetrahedral coordination.展开更多
文摘The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1H/13C--NMR. Theproposal concerning mechanism was discussed herewith and the structure was reportedas well. Crystallographic data: Mr= 563. 85, monoclinicl P21/n(# 14); a= 8. 009(2), b= 17. 600(5), c=12. 003(4) A; β=95. 91(2)°; V= 1683. 0 (9) A3; Z=4;Dc=2. 22 g. cm-3; F(000) = 1048, μ=89. 27 cm-1 ; final R=0. 039 and Rw=0. 049for 2121 observable reflections with (I≥3. cσ(I) ). The crystal structure determinationshows that S atom coordinates to all three metal (W,Fe,Co) atoms in a μ3,-fashion,thetitle cluster core has the tetrahedral skeleton.
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 complex [Et4N][(Ph3P)2{CuS2WS2Fe} Br2] (1 ), C44, H50NBr2CuFeP2S4W, M4= 1246. 13, has been obtained by reaction of [Et4N]2[WS4] andFeBr2 with Cu (Ph3P )3I in MeCN/CH2Cl2. Crystal data for [Et4N][(Ph3P)2{CuS2WS2Fe) Br2] (1): triclinic, P1, Z = 2, a= 13. 495 (7), b = 15. 322 (5), c =12. 361 (4), a=105. 32(3), β=93. 19(4), γ=101. 35(4) and V=2401. 2 The bond lengths of W-Fe bond and the W-Cu distance are 2. 793(2) A and 2. 823(2), respectively. Three kind metal atoms of the title structure [Et4N][(Ph3P)2{CuS2WS2Fe}Br2] (1) are nearly distributed along a line, and along which three metalatoms (W, Cu, Fe) are approximately tetrahedral coordination.
