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 title compound Fe_3 (CO)_8(CN)S_2 was synthesized by the reaction of C_6H_5NCS cleaving fragments with Fe_3 (CO)_(12) at room temperature. Crystal data: C_9Fe_3NO_8S_2, Mr=481. 76, triclinic , space group P1,a= 9....The title compound Fe_3 (CO)_8(CN)S_2 was synthesized by the reaction of C_6H_5NCS cleaving fragments with Fe_3 (CO)_(12) at room temperature. Crystal data: C_9Fe_3NO_8S_2, Mr=481. 76, triclinic , space group P1,a= 9. 436 (3), b=10. 210(2), c=9. 14l(3) A, a =90. 63(2), β=117. 55(3), γ=96. 66(2)°, V=773. 5(4) A ̄3 , Z=2, D_c= 2. 068 g/cm ̄3, μ(MoKa)=30. 78 cm ̄(-1), F(000)=470 .T= 293K , final R=0. 030 and R_w=0. 041 for 2314 observed reflections with I>3. 00 σ(I).The monosubstituted ligand(CN)in Fe_3 (CO)_8 (CN)S_2 is linked to basal Fe (3) atom of the distorted tetragonal pyramid Fe_3S_2 framework.展开更多
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 title compound Fe_3 (CO)_8(CN)S_2 was synthesized by the reaction of C_6H_5NCS cleaving fragments with Fe_3 (CO)_(12) at room temperature. Crystal data: C_9Fe_3NO_8S_2, Mr=481. 76, triclinic , space group P1,a= 9. 436 (3), b=10. 210(2), c=9. 14l(3) A, a =90. 63(2), β=117. 55(3), γ=96. 66(2)°, V=773. 5(4) A ̄3 , Z=2, D_c= 2. 068 g/cm ̄3, μ(MoKa)=30. 78 cm ̄(-1), F(000)=470 .T= 293K , final R=0. 030 and R_w=0. 041 for 2314 observed reflections with I>3. 00 σ(I).The monosubstituted ligand(CN)in Fe_3 (CO)_8 (CN)S_2 is linked to basal Fe (3) atom of the distorted tetragonal pyramid Fe_3S_2 framework.