Half-sandwich ruthenium phosphine complexes with sulfur-donor ligands. X-ray crystal structures of [Cp*RuH(SH)(PEt3)(2)][BPh4] and [Cp*Ru((S2COPr)-Pr-i)(PEt3)]

Coto A.; Puerta MC.; Valerga P.; Tenorio MJ.

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Half-sandwich ruthenium phosphine complexes with sulfur-donor ligands. X-ray crystal structures of [CpRuH(SH)(PEt3)(2)][BPh4] and [CpRu((S2COPr)-Pr-i)(PEt3)]

机译：具有硫供体配体的半三明治钌膦膦配合物。 [Cp * RuH（SH）（PEt3）（2）] [BPh4]和[Cp * Ru（（S2COPr）-Pr-i）（PEt3）]的X射线晶体结构

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The complexes [CpRuCl(PEt3)(2)] (1) and [CpRuCl((PMePr2)-Pr-i)(PPh3)] (2) react with H2S in EtOH in the presence of NaBPh4 furnishing the green persulfide derivatives [{CpRu(L)}(2)(mu-S-2)][BPh4](2) (L = (PEt3)(2), ((PMePr2)-Pr-i)(PPh3)), which were also obtained by reaction of 1 or 2 with elemental sulfur and NaBPh4 in MeOH. At variance with this, the reaction of [Cp*RuCl(PEt3)(2)] (3) with H2S in EtOH afforded the Ru-IV hydrido-metallothiol [Cp*RuH(SH)(PEt3)(2)][BPh4], which has been structurally characterized, derived from the oxidative addition of SH2 to the electron-rich Ru-II moiety {[Cp*Ru(PEt3)(2)](+)}. This compound is oxidized to yield the persulfide complex [{Cp*Ru(PEt3)(2)}(2)(mu-S-2)][BPh4](2), which was also obtained by reaction of 3 with elemental sulfur. The reaction of 1, 2, and 3 with 2-mercapto-pyridine (HSPy) in EtOH yielded cationic complexes in which HSPy is tautomerized to its 1H-pyridine-thione form as inferred from spectral data. Compound 1 reacts with potassium alkyl-xanthates KS2COR (R = Me, Et, Pr-i) yielding compounds of the type [CpRu(eta(1)-S2COR)(PEt3)(2)], whereas the reaction of 2 and 3 led respectively to the complexes [CpRu(eta(2)-S2COR)((PMePr2)-Pr-i)] and [Cp*Ru(eta(2)-S2COR)(PEt3)], which contain one bidentate xanthate and one phosphine. The X-ray crystal structure of [Cp*Ru((S2COPr)-Pr-i)(PEt3)] was determined. In analogous fashion, the reaction of 1 with sodium diethyldithiocarbamate yielded [CpRu(eta(1)-S2CNEt2)(PEt3)(2)], whereas 2 and 3 afforded the corresponding derivatives [CpRu(eta(2)-S2CNEt2)((PMePr2)-Pr-i)] and [Cp*Ru(eta(2)-S2CNEt2)(PEt3)]. [References: 52]

机译：络合物[CpRuCl（PEt3）（2）]（1）和[CpRuCl（（PMePr2）-Pr-i）（PPh3）]（2）在NaBPh4存在下与EtOH中的H2S反应，得到绿色的过硫化物衍生物[{ CpRu（L）}（2）（mu-S-2）] [BPh4]（2）（L =（PEt3）（2），（（（PMePr2）-Pr-1）（PPh3））） 1或2与元素硫和NaBPh4在MeOH中的反应。与此不同的是，[Cp * RuCl（PEt3）（2）]（3）与H2S在EtOH中的反应提供了Ru-IV氢化金属硫醇[Cp * RuH（SH）（PEt3）（2）] [BPh4 ]，其结构特征在于，它是由SH2氧化成富电子的Ru-II部分{[Cp * Ru（PEt3）（2）]（+）}衍生而来的。将该化合物氧化，生成过硫化物络合物[{Cp * Ru（PEt3）（2）}（2）（mu-S-2）] [BPh4]（2），也可通过3与元素硫反应获得。 1、2和3与2-巯基吡啶（HSPy）在EtOH中的反应生成阳离子络合物，其中HSPy被互变异构化为其1H-吡啶-硫酮形式，如光谱数据所示。化合物1与烷基黄原酸钾KS2COR（R = Me，Et，Pr-i）反应生成[CpRu（eta（1）-S2COR）（PEt3）（2）]类型的化合物，而2和3的反应分别导致[CpRu（eta（2）-S2COR）（（（PMePr2）-Pr-i）]和[Cp * Ru（eta（2）-S2COR）（PEt3）]的络合物，其中包含一个二齿黄药和一个膦。确定了[Cp * Ru（（S2COPr）-Pr-1）（PEt3）]的X射线晶体结构。以类似的方式，1与二乙基二硫代氨基甲酸钠反应生成[CpRu（eta（1）-S2CNEt2）（PEt3）（2）]，而2和3提供相应的衍生物[CpRu（eta（2）-S2CNEt2）（（ PMePr2）-Pr-i）]和[Cp * Ru（eta（2）-S2CNEt2）（PEt3）]。 [参考：52]

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《Organometallics》 |1998年第20期|共8页
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Coto A.; Puerta MC.; Valerga P.; Tenorio MJ.;
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1. Half-sandwich ruthenium phosphine complexes with sulfur-donor ligands. X-ray crystal structures of [Cp*RuH(SH)(PEt3)(2)][BPh4] and [Cp*Ru((S2COPr)-Pr-i)(PEt3)] [J] . Coto A., Puerta MC., Valerga P., Organometallics . 1998,第20期

机译：具有硫供体配体的半三明治钌膦膦配合物。 [Cp * RuH（SH）（PEt3）（2）] [BPh4]和[Cp * Ru（（S2COPr）-Pr-i）（PEt3）]的X射线晶体结构
2. Alternative Mechanisms of the Alkyne to Vinylidene Isomerization Promoted by Half-Sandwich Ruthenium Complexes. X-ray Crystal Structures of [Cp~*Ru=C=CHCOOMe(dippe)][BPh_4] and [Cp~*RuH(C≡ CCOOMe)(dippe)][BPh_4] (dippe = 1,2-bis(diisopropylphosphino) [J] . Isaac de los Rios, Manuel Jimenez Tenorio, M. Carmen Puerta Journal of the American Chemical Society . 1997,第28期

机译：半夹心钌配合物促进炔烃向亚乙烯基异构化的替代机制。 [Cp〜* Ru = C = CHCOOMe（dippe）] [BPh_4]和[Cp〜* RuH（C≡CCOOMe）（dippe）] [BPh_4]的X射线晶体结构（dippe = 1,2-bis（diisopropylphosphino））
3. Reactivity of the electron-rich allenylidene-ruthenium complexes [Cp*Ru{=C=C=C(R)Ph}(dippe)][BPh4] (R = H, Ph). X-ray crystal structure of a novel dicationic ruthenium carbyne (CP* = C5Me5; dippe=1,2-bis(diisopropylphosphine)ethane) [J] . Bustelo E., Jimenez-Tenorio M., Mereiter K., Organometallics . 2002,第9期

机译：富电子的亚烯基-钌络合物[Cp * Ru {= C = C = C（R）Ph}（dippe）] [BPh4]（R = H，Ph）的反应性。新型双金属钌卡宾（CP * = C5Me5; dippe = 1,2-双（二异丙基膦）乙烷）的X射线晶体结构
4. Controlled Radical Polymerization Catalyzed by Ruthenium Complexes: Variations on Ru-Cp~# [C] . Sebastien Delfosse, Aurore Richel, Francois Simal, American Chemical Society symposium on advances in controlled/living radical polymerization . 2003

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Half-sandwich ruthenium phosphine complexes with sulfur-donor ligands. X-ray crystal structures of [Cp*RuH(SH)(PEt3)(2)][BPh4] and [Cp*Ru((S2COPr)-Pr-i)(PEt3)]

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Half-sandwich ruthenium phosphine complexes with sulfur-donor ligands. X-ray crystal structures of [CpRuH(SH)(PEt3)(2)][BPh4] and [CpRu((S2COPr)-Pr-i)(PEt3)]