The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized fr...The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4) 3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.展开更多
The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction ana...The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction analysis were obtained from n pentane diffused to CH 2Cl 2 solution. The crystal {(PPh 3) 2ClRu( μ Cl)Ru(PPh 3)B 10 H 7〔OCH(CH 3) 2〕 3}·0.4(H 2O) is monoclinic , space group P2 1/n , M r= 1359.47, with a=19.434(4), b =14.340(4), c=25.865(9) , β= 95.48(3)°, V=7175(4) 3, D c =1.258 g/cm 3, Z=4, λ (Mo Kα )=0.71073, μ=6.03 cm -1 , F(000)=2784, R=0.0631, wR 2 = 0.1425, S =1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh 3)RuB 10 H 7〔OCH(CH 3) 2〕 3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.展开更多
The title compound (Ⅰ) has been synthesized by the reaction of [RuCl2(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. The re-action gave two main products Ⅰ and Ⅱ. Crystals of the title compound ...The title compound (Ⅰ) has been synthesized by the reaction of [RuCl2(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. The re-action gave two main products Ⅰ and Ⅱ. Crystals of the title compound (Ⅰ) suitable fora single crystal X-ray diffraction analysis were recrystailized from n-pentane/CH2Cl2 so-lution. Its structure was determined by X-ray crystallography analysis. The crystal of{(PPh3)2RuB10 H8 [(CH3)2CHO]2} (Ⅰ) is monoclinic, space group P21/n, Mr =860. 01, with a= 12. 927(2), b= 23. 672(6), c= 14. 090(4) A, β=93. 22(2)°, V=4305 A3, Dc= 1. 327 g/cm3, Z= 4, λ(MoKα) =0. 71073A, μ=4. 6 cm-1, F(000) =1776, R = 0. 059, Rw = 0. 075, S = 2. 62. The cluster structure is based on a closoeleven-vertex {RuB10 } polyhedron skeleton with two replacing isopropoxy and twoPPh3 groups.展开更多
The title compound has been synthesized by the reaction of [RuCl2-(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. Crystalsof the title compound suitable for a single crystal X-ray diffraction analy...The title compound has been synthesized by the reaction of [RuCl2-(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. Crystalsof the title compound suitable for a single crystal X-ray diffraction analysis were recrystallized from n-pentane/CH2Cl2 solution. The crystal is monoclinic, space group P21,/n,Mr=1294. 19, with a=11. 591 (6), b=23. 993(4), c=24. 900(4) A, β=90. 52(2), V= 6925(4) A3, Dc= 1.241 g/cm3, Z=4, A(MoKa) =0. 71073 A, P=6. 2cm-1, F(000)=2640, R=0. 046, wR2=0. 083, S=1. 09. The cluster is a bimetallicspecies in which the second ruthenium center is bound exopolyhedrally to the compound{(PPh3)2RuB10H8[OCH (CH3)2]2 } via an Ru (1) -C;(1)-Ru (2) bridge and Ru (2) B(6) and Ru(2)-B(7) bonds.展开更多
The title platinaborane, [(P (2) Ph 3)Pt (1) ( μ 2 B (11) (B (9) OC^(CH 3) 3 B 10 ~H 10 ))Pt (7) (P (1) Ph 3)] 2, a triple cluster, which is a binuclear Pt complex dimme...The title platinaborane, [(P (2) Ph 3)Pt (1) ( μ 2 B (11) (B (9) OC^(CH 3) 3 B 10 ~H 10 ))Pt (7) (P (1) Ph 3)] 2, a triple cluster, which is a binuclear Pt complex dimmer, was prepared. Single crystal X ray diffraction analysis shows that a Pt (7) atom served as a common vertex between cluster {PtB 10 } and {Pt 4}. The {Pt 4} cluster is of parallelogram.展开更多
文摘The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4) 3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.
文摘The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction analysis were obtained from n pentane diffused to CH 2Cl 2 solution. The crystal {(PPh 3) 2ClRu( μ Cl)Ru(PPh 3)B 10 H 7〔OCH(CH 3) 2〕 3}·0.4(H 2O) is monoclinic , space group P2 1/n , M r= 1359.47, with a=19.434(4), b =14.340(4), c=25.865(9) , β= 95.48(3)°, V=7175(4) 3, D c =1.258 g/cm 3, Z=4, λ (Mo Kα )=0.71073, μ=6.03 cm -1 , F(000)=2784, R=0.0631, wR 2 = 0.1425, S =1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh 3)RuB 10 H 7〔OCH(CH 3) 2〕 3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.
文摘The title compound (Ⅰ) has been synthesized by the reaction of [RuCl2(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. The re-action gave two main products Ⅰ and Ⅱ. Crystals of the title compound (Ⅰ) suitable fora single crystal X-ray diffraction analysis were recrystailized from n-pentane/CH2Cl2 so-lution. Its structure was determined by X-ray crystallography analysis. The crystal of{(PPh3)2RuB10 H8 [(CH3)2CHO]2} (Ⅰ) is monoclinic, space group P21/n, Mr =860. 01, with a= 12. 927(2), b= 23. 672(6), c= 14. 090(4) A, β=93. 22(2)°, V=4305 A3, Dc= 1. 327 g/cm3, Z= 4, λ(MoKα) =0. 71073A, μ=4. 6 cm-1, F(000) =1776, R = 0. 059, Rw = 0. 075, S = 2. 62. The cluster structure is based on a closoeleven-vertex {RuB10 } polyhedron skeleton with two replacing isopropoxy and twoPPh3 groups.
文摘The title compound has been synthesized by the reaction of [RuCl2-(PPh3)3], closo-[B10H10]2- and PhCH(OH)COOH in (CH3)2CHOH solution. Crystalsof the title compound suitable for a single crystal X-ray diffraction analysis were recrystallized from n-pentane/CH2Cl2 solution. The crystal is monoclinic, space group P21,/n,Mr=1294. 19, with a=11. 591 (6), b=23. 993(4), c=24. 900(4) A, β=90. 52(2), V= 6925(4) A3, Dc= 1.241 g/cm3, Z=4, A(MoKa) =0. 71073 A, P=6. 2cm-1, F(000)=2640, R=0. 046, wR2=0. 083, S=1. 09. The cluster is a bimetallicspecies in which the second ruthenium center is bound exopolyhedrally to the compound{(PPh3)2RuB10H8[OCH (CH3)2]2 } via an Ru (1) -C;(1)-Ru (2) bridge and Ru (2) B(6) and Ru(2)-B(7) bonds.
文摘The title platinaborane, [(P (2) Ph 3)Pt (1) ( μ 2 B (11) (B (9) OC^(CH 3) 3 B 10 ~H 10 ))Pt (7) (P (1) Ph 3)] 2, a triple cluster, which is a binuclear Pt complex dimmer, was prepared. Single crystal X ray diffraction analysis shows that a Pt (7) atom served as a common vertex between cluster {PtB 10 } and {Pt 4}. The {Pt 4} cluster is of parallelogram.
