New mono- and di- substituted derivatives of Fe3 (CO) 9(μ3 - S) 2 were synthesized by reac- tion of C6H5NCS with Fe3 (CO) 1 2 atroom temperature.Their structure were characterized by means of IR(νCO) ,MS,1 H NMR,1 3...New mono- and di- substituted derivatives of Fe3 (CO) 9(μ3 - S) 2 were synthesized by reac- tion of C6H5NCS with Fe3 (CO) 1 2 atroom temperature.Their structure were characterized by means of IR(νCO) ,MS,1 H NMR,1 3 C NMR,elemental analysis and X- ray four cycle diffrac- tometer.The results showed that the formulas of the cluster compounds are Fe3 (CO) 8 (CNC6H5) (μ3 - S) 2 and Fe3 (CO) 7(CNC6H5) 2 (μ3 - S) 2 respectively.展开更多
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
The reaction of μ alkyne bridged dimolybdenum compound 〔Mo 2( μ C 2HPh)(CO) 4( η 5 C 5H 4C(O)Me) 2〕 1 with Co 2(CO) 8 in refluxing toluene gave a new butterfly compound 〔Co 2Mo 2( μ 4 C 2HPh)( μ CO) 4(CO) 4( ...The reaction of μ alkyne bridged dimolybdenum compound 〔Mo 2( μ C 2HPh)(CO) 4( η 5 C 5H 4C(O)Me) 2〕 1 with Co 2(CO) 8 in refluxing toluene gave a new butterfly compound 〔Co 2Mo 2( μ 4 C 2HPh)( μ CO) 4(CO) 4( η 5 C 5H 4C(O)Me) 2〕 2 which was fully characterized by elemental analysis, IR, 1H NMR and X ray single crystal diffraction techniques. 2 crystallized in monoclinic system, C 30 H 20 Co 2Mo 2O 10 , M r =850.23, space group P2 1/a(#14), a=14.165(5), b=12.498(2), c=16.204(2) , β = 96 50(2)°, V = 2850(1) 3, Z = 4, D c = 1.981 g cm -3 , F(000)=1672, μ (Mo Kα )=20.41 cm -1 , final R=0.030, R w =0.039 for 4831 observable reflections with I>2σ(I ). The structure contains a Co 2Mo 2 butterfly core, and each Mo-Co bond is spanned by an asymmetric semi bridging carbonyl ligand.展开更多
The reaction of dipropargyl phthalate C6H41,2(CO2CH2C2H)2 1 with octacarbonyldicobalt 2 resulted in the formation of red complex C6H41,2(CO2CH2C2H)2Co2(CO)62 3, in which each Co2(CO)6 group coordinates to one of t...The reaction of dipropargyl phthalate C6H41,2(CO2CH2C2H)2 1 with octacarbonyldicobalt 2 resulted in the formation of red complex C6H41,2(CO2CH2C2H)2Co2(CO)62 3, in which each Co2(CO)6 group coordinates to one of the two CC bonds of 1. Molecular structure of complex 3 was determined by single crystal Xray analyses. The crystal belongs to the monoclinic system, space group P21/a with the following crystallographic parameters: a=8.521(2), b=29.143(6), c=12.918(7) , = 100.12(3),V=3158(2) 3, Z=4, Mr=814.09, Dc=1712 g.cm-3, F(000)=1608, (MoK)=21.37 cm-1 and final R=0.044 for 3151 observations.展开更多
The chiral cluster RuCoMo（CO）8 （μ3-Se）C5H4C （O）C6H4C （O）OCH3was synthesizgd by the thermal reaction of the precursor （μ3-Se）RuCo2（Co）9 with ’thefunctionally substituted cyclopentadienyl tricarbonyl meta...The chiral cluster RuCoMo（CO）8 （μ3-Se）C5H4C （O）C6H4C （O）OCH3was synthesizgd by the thermal reaction of the precursor （μ3-Se）RuCo2（Co）9 with ’thefunctionally substituted cyclopentadienyl tricarbonyl metal complex anions [Mo（CO）3（η5-C5H4） C （O）C6H4C （O） OCH3]- in THF. It was characterized by C/H elementalanalysis, IR, 1H/13C-NMR and MS （FAB）, and its crystal structure has also beensolved by single-crystal X-ray diffraction. Crystal data: Mr=786. 23, triclinic, spacegroup P1, a =8. 200（2）, b= 19. 631 （7）, c=7.997（2） , a=92. 50（2）, β=108. 66 （2）, γ=88. 97（2）°, V= 1218. 5（6） , Z=2, Dc=2. 143g/cm3, F（000） =756. 00, μ= 33. 44cm-1, the final R =0. 054 and R.= 0. 077 for 2644 observationswith （I≥3.0σ（I） ）.展开更多
文摘New mono- and di- substituted derivatives of Fe3 (CO) 9(μ3 - S) 2 were synthesized by reac- tion of C6H5NCS with Fe3 (CO) 1 2 atroom temperature.Their structure were characterized by means of IR(νCO) ,MS,1 H NMR,1 3 C NMR,elemental analysis and X- ray four cycle diffrac- tometer.The results showed that the formulas of the cluster compounds are Fe3 (CO) 8 (CNC6H5) (μ3 - S) 2 and Fe3 (CO) 7(CNC6H5) 2 (μ3 - S) 2 respectively.
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The reaction of μ alkyne bridged dimolybdenum compound 〔Mo 2( μ C 2HPh)(CO) 4( η 5 C 5H 4C(O)Me) 2〕 1 with Co 2(CO) 8 in refluxing toluene gave a new butterfly compound 〔Co 2Mo 2( μ 4 C 2HPh)( μ CO) 4(CO) 4( η 5 C 5H 4C(O)Me) 2〕 2 which was fully characterized by elemental analysis, IR, 1H NMR and X ray single crystal diffraction techniques. 2 crystallized in monoclinic system, C 30 H 20 Co 2Mo 2O 10 , M r =850.23, space group P2 1/a(#14), a=14.165(5), b=12.498(2), c=16.204(2) , β = 96 50(2)°, V = 2850(1) 3, Z = 4, D c = 1.981 g cm -3 , F(000)=1672, μ (Mo Kα )=20.41 cm -1 , final R=0.030, R w =0.039 for 4831 observable reflections with I>2σ(I ). The structure contains a Co 2Mo 2 butterfly core, and each Mo-Co bond is spanned by an asymmetric semi bridging carbonyl ligand.
文摘The reaction of dipropargyl phthalate C6H41,2(CO2CH2C2H)2 1 with octacarbonyldicobalt 2 resulted in the formation of red complex C6H41,2(CO2CH2C2H)2Co2(CO)62 3, in which each Co2(CO)6 group coordinates to one of the two CC bonds of 1. Molecular structure of complex 3 was determined by single crystal Xray analyses. The crystal belongs to the monoclinic system, space group P21/a with the following crystallographic parameters: a=8.521(2), b=29.143(6), c=12.918(7) , = 100.12(3),V=3158(2) 3, Z=4, Mr=814.09, Dc=1712 g.cm-3, F(000)=1608, (MoK)=21.37 cm-1 and final R=0.044 for 3151 observations.
文摘The chiral cluster RuCoMo（CO）8 （μ3-Se）C5H4C （O）C6H4C （O）OCH3was synthesizgd by the thermal reaction of the precursor （μ3-Se）RuCo2（Co）9 with ’thefunctionally substituted cyclopentadienyl tricarbonyl metal complex anions [Mo（CO）3（η5-C5H4） C （O）C6H4C （O） OCH3]- in THF. It was characterized by C/H elementalanalysis, IR, 1H/13C-NMR and MS （FAB）, and its crystal structure has also beensolved by single-crystal X-ray diffraction. Crystal data: Mr=786. 23, triclinic, spacegroup P1, a =8. 200（2）, b= 19. 631 （7）, c=7.997（2） , a=92. 50（2）, β=108. 66 （2）, γ=88. 97（2）°, V= 1218. 5（6） , Z=2, Dc=2. 143g/cm3, F（000） =756. 00, μ= 33. 44cm-1, the final R =0. 054 and R.= 0. 077 for 2644 observationswith （I≥3.0σ（I） ）.
