| 165130-65-4

• CAS: 165130-65-4
• 化学式: C₁₆H₃₀B₂S₄Ti₂
• 分子量: 468.06
• InChiKey: YHEBPHXHZRYALU-UHFFFAOYSA-L

反应信息

• 作为反应物：
  描述：

  以 四氢呋喃 为溶剂， 以20%的产率得到cyclopenta-1,3-diene;propane-1,3-dithiolate;titanium(3+)
  参考文献：
  名称：

  Reductions of Cyclopentadienyltitanium Diolate and Dithiolate Species with Boron and Tin Hydrides

  摘要：

  Reactions of various CpTi diolate and thiolate complexes with boron and tin hydrides are examined. Reaction of the species (CpTiCl(2))(2)(OCH(2)CMe(2)CH(2)O) (6), generated in situ, with LiBH4 yields black crystals of [CpTi(BH4)(OCH(2)CMe(2)CH(2)O)](2)TiCp (7). This trimetallic product is paramagnetic and has been characterized crystallographically. The reaction of CpTiCl(SCH2CH2CH2S) (1) with LiBH4 performed in THF at room temperature affords black crystals of the diamagnetic species 8. NMR and crystallographic data confirmed the formulation of 8 as the dimeric species [CpTi(SCH2CH2CH2S)(BH4)](2). The similar reaction of 1 with NaBEt(3)H also yielded black crystals whose characterization via spectroscopic methods was precluded by insolubility. Nonetheless, X-ray crystallographic study confirmed the formulation of 9 as the dimeric compound [CpTi(SCH2CH2CH2S)](2). The reaction of 1 with Bu(3)SnH proceeds to yield black, insoluble crystals of 10. Repeated attempts to characterize 10 by X-ray crystallographic methods were made. Preliminary crystallographic data establish the connectivity and thus the formulation of 10 as Cp(3)Ti(3)S(2)(SCH2CH2CH2S)(2). The reaction of [CpTiCl(SCH2CH2S)](2) (2) with Bu(3)SnH led to uncharacterized paramagnetic and diamagnetic products, although a small amount of the known species CP5Ti5S6 (12) was isolated. The reaction of CpTiCl(SCH2CH2SCH2CH2S) (3) with Bu(3)SnH affords the dark, crystalline, sparingly soluble, product [CpTi(SCH2CH2SCH2CH2S)(2)](2) (11), which was formulated on the basis of X-ray crystallographic data. The structures of these products are described, and the implications of this chemistry are considered. X-ray data for the compounds presented herein are summarized below. Compound 7: P2(1)/a, a = 16.117(8) Angstrom, b = 9.889(5) Angstrom, c = 19.533(7) Angstrom, beta = 109.95(3)degrees, Z = 4, V = 2926(2) Angstrom(3). Compound 8: P2(1)/n, a = 15.863(9) Angstrom, b = 16.025(7) Angstrom, c = 8.411(3) Angstrom, b = 90.082(4)degrees, Z = 4, V = 2138(2) Angstrom(3). Compound 9: P2(1)/n, a = 8.750(2) Angstrom, b = 9.526(1) Angstrom, c = 11.732(2) Angstrom,beta = 110.33(1)degrees, Z = 4, V = 917.0(3) Angstrom(3). Compound 10: Cc, a = 15.080(9) Angstrom, b = 15.747(9) Angstrom, c = 10.776(4) Angstrom,beta = 91.26(7)degrees, Z = 4, V = 2559(2) Angstrom(3). Compound 11: Aba2, a = 19.684(10) Angstrom, b = 7.869(10) Angstrom, c = 14.408(6) Angstrom, Z = 4, V = 2232(4) Angstrom(3).

  DOI：

  10.1021/om00006a032
• 作为产物：
  描述：

  锂硼氢 、 (cyclopentadienyl)(1,3-propanedithiolate)titanium(IV) chloride 以 四氢呋喃 为溶剂， 以80%的产率得到
  参考文献：
  名称：

  Reductions of Cyclopentadienyltitanium Diolate and Dithiolate Species with Boron and Tin Hydrides

  摘要：

  Reactions of various CpTi diolate and thiolate complexes with boron and tin hydrides are examined. Reaction of the species (CpTiCl(2))(2)(OCH(2)CMe(2)CH(2)O) (6), generated in situ, with LiBH4 yields black crystals of [CpTi(BH4)(OCH(2)CMe(2)CH(2)O)](2)TiCp (7). This trimetallic product is paramagnetic and has been characterized crystallographically. The reaction of CpTiCl(SCH2CH2CH2S) (1) with LiBH4 performed in THF at room temperature affords black crystals of the diamagnetic species 8. NMR and crystallographic data confirmed the formulation of 8 as the dimeric species [CpTi(SCH2CH2CH2S)(BH4)](2). The similar reaction of 1 with NaBEt(3)H also yielded black crystals whose characterization via spectroscopic methods was precluded by insolubility. Nonetheless, X-ray crystallographic study confirmed the formulation of 9 as the dimeric compound [CpTi(SCH2CH2CH2S)](2). The reaction of 1 with Bu(3)SnH proceeds to yield black, insoluble crystals of 10. Repeated attempts to characterize 10 by X-ray crystallographic methods were made. Preliminary crystallographic data establish the connectivity and thus the formulation of 10 as Cp(3)Ti(3)S(2)(SCH2CH2CH2S)(2). The reaction of [CpTiCl(SCH2CH2S)](2) (2) with Bu(3)SnH led to uncharacterized paramagnetic and diamagnetic products, although a small amount of the known species CP5Ti5S6 (12) was isolated. The reaction of CpTiCl(SCH2CH2SCH2CH2S) (3) with Bu(3)SnH affords the dark, crystalline, sparingly soluble, product [CpTi(SCH2CH2SCH2CH2S)(2)](2) (11), which was formulated on the basis of X-ray crystallographic data. The structures of these products are described, and the implications of this chemistry are considered. X-ray data for the compounds presented herein are summarized below. Compound 7: P2(1)/a, a = 16.117(8) Angstrom, b = 9.889(5) Angstrom, c = 19.533(7) Angstrom, beta = 109.95(3)degrees, Z = 4, V = 2926(2) Angstrom(3). Compound 8: P2(1)/n, a = 15.863(9) Angstrom, b = 16.025(7) Angstrom, c = 8.411(3) Angstrom, b = 90.082(4)degrees, Z = 4, V = 2138(2) Angstrom(3). Compound 9: P2(1)/n, a = 8.750(2) Angstrom, b = 9.526(1) Angstrom, c = 11.732(2) Angstrom,beta = 110.33(1)degrees, Z = 4, V = 917.0(3) Angstrom(3). Compound 10: Cc, a = 15.080(9) Angstrom, b = 15.747(9) Angstrom, c = 10.776(4) Angstrom,beta = 91.26(7)degrees, Z = 4, V = 2559(2) Angstrom(3). Compound 11: Aba2, a = 19.684(10) Angstrom, b = 7.869(10) Angstrom, c = 14.408(6) Angstrom, Z = 4, V = 2232(4) Angstrom(3).

  DOI：

  10.1021/om00006a032