A novel structural rearrangement reaction of dialkylated derivatives of [Pt _2(μ-S) _2(PPh _3) _4] involving Pt-C bond formation

Ujam O.T.; Devoy S.M.; Henderson W.; Nicholson B.K.; Hor T.S.A.

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A novel structural rearrangement reaction of dialkylated derivatives of [Pt _2(μ-S) _2(PPh _3) _4] involving Pt-C bond formation

机译：[Pt _2（μ-S）_2（PPh _3）_4]的二烷基化衍生物的新型结构重排反应，涉及Pt-C键的形成

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Reaction of [Pt _2(μ-S) _2(PPh _3) _4] with the dialkylating agents ClCH _2C(O)CH _2Cl or ClCH _2C(NNHC(O)NH _2)CH _2Cl gives the dicationic di-μ-thiolate complexes [Pt _2{μ-SCH _2C(O)CH _2S)(PPh _3) _4] ~(2+) or [Pt _2{μ-SCH _2C(NNHC(O)NH _2)CH _2S} (PPh _3) _4] ~(2+), isolated as BPh _4 ~- salts and characterised by ESI mass spectrometry, NMR spectroscopy and single-crystal X-ray crystallography. Treatment of the complex [Pt _2{μ-SCH _2C(O)CH _2S)(PPh _3) _4] ~(2+), which contains a [6.6.4] bicyclic system, with hydroxide ions results in deprotonation of a CH _2 group and rearrangement of the resulting monocation, giving [Pt _2(μ-SCH _2C(O)CHS}(PPh _3) _4] ~+, isolated as its PF _6 ~- salt. An X-ray structure determination shows the complex to have a novel rearranged [6.5.5] bicyclic system containing a Pt-S-Pt-S-C five-membered ring with a Pt-C bond. The alkyl ligand has a high trans-influence, manifest in a long trans Pt-P bond and small ~1J(PtP) coupling constant to the trans PPh _3 ligand. Reaction of [Pt _2(μ-S) _2(PPh _3) _4] with the 2,4-dinitrophenylhydrazone derivative of 1,3-dichloroacetone leads to the closely related complex [Pt _2{μ-SCH _2C(NNHAr)CHS} (PPh _3) _3Cl] [Ar = C _6H _3(NO _2) _2] in which a PPh _3 ligand is substituted by a chloride.

机译：[Pt _2（μ-S）_2（PPh _3）_4]与二烷基化剂ClCH _2C（O）CH _2Cl或ClCH _2C（NNHC（O）NH _2）CH _2Cl的反应生成二官能双-硫醇盐配合物[Pt _2 {μ-SCH_2C（O）CH _2S）（PPh _3）_4]〜（2+）或[Pt _2 {μ-SCH_2C（NNHC（O）NH _2）CH _2S}（PPh _3）_4 ]〜（2+），分离为BPh_4〜-盐，并通过ESI质谱，NMR光谱和单晶X射线晶体学进行表征。用氢氧根离子处理包含[6.6.4]双环系统的复合物[Pt _2 {μ-SCH_2C（O）CH _2S）（PPh _3）_4]〜（2+）会导致CH的去质子化_2基团和所得单阳离子的重排，得到[Pt _2（μ-SCH_2C（O）CHS}（PPh _3）_4]〜+，分离为其PF _6〜-盐。X射线结构测定表明该络合物具有一个新的重排[6.5.5]双环系统，该系统包含带有Pt-C键的Pt-S-Pt-SC五元环，烷基配体具有高反式影响，表现为长反式Pt-P反式PPh _3配体具有键和小的〜1J（PtP）偶联常数。[Pt _2（μ-S）_2（PPh _3）_4]与1,3-二氯丙酮的2,4-二硝基苯基hydr衍生物反应紧密相关的络合物[Pt _2 {μ-SCH_2C（NNHAr）CHS}（PPh _3）_3Cl] [Ar = C _6H _3（NO _2）_2]，其中PPh _3配体被氯取代。

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《Dalton transactions: An international journal of inorganic chemistry》 |2012年第41期|共8页
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Ujam O.T.; Devoy S.M.; Henderson W.; Nicholson B.K.; Hor T.S.A.;
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1. A novel structural rearrangement reaction of dialkylated derivatives of [Pt _2(μ-S) _2(PPh _3) _4] involving Pt-C bond formation [J] . Ujam O.T., Devoy S.M., Henderson W., Dalton transactions: An international journal of inorganic chemistry . 2012,第41期

机译：[Pt _2（μ-S）_2（PPh _3）_4]的二烷基化衍生物的新型结构重排反应，涉及Pt-C键的形成
2. Thermal skeletal rearrangement of a nido-ruthenacyclopentadiene complex involving reversible rupture and formation of a ruthenium-ruthenium bond [J] . Inagaki A., Takao T., Moriya M., Organometallics . 2003,第11期

机译：涉及可逆断裂和钌-钌键形成的Nido-钌-环戊二烯络合物的热骨架重排
3. The structural chemistry of triorganotin(IV) derivatives of 3-amino-5-mercapto-1,2,4-triazole: Supramolecular structures involving intermolecular N-H center dot center dot center dot N and N-H center dot center dot center dot S hydrogen bonding [J] . Ma CL, Li YX, Han YW, Inorganica Chimica Acta . 2008,第1期

机译：3-氨基-5-巯基-1,2,4-三唑的三有机锡（IV）衍生物的结构化学：涉及分子间N-H中心点中心点中心点N和N-H中心点中心点中心点S氢键的超分子结构
4. Reaction of α-Imino Thioesters and the Subsequent C-C Bond Formation with the Unexpected Alkylthio Rearrangement [C] . Isao Mizota, Makoto Shimizu 日本化学会春季年会講演予稿集 . 2018

机译：α-氨基氨基氨基氨基铵和随后的C-C键形成与意外的烷硫基重排反应
5. I. Stereochemistry of cyclopropane formation involving group (IV) organometallic complexes. II. Slower stoichiometric and faster catalytic reduction of aldehydes by the PPh(3) substituted hydroxycyclopentadienyl ruthenium hydride [2,5-Ph(2)-3,4-Tol(2)(eta(5)-C(4)COH)]Ru(CO)(PPh(3))H: A highly chemoselective catalyst for hydrogenation of aldehydes over ketones. [D] . Strotman, Neil Adham. 2005

机译：I.涉及（IV）族有机金属配合物的环丙烷形成的立体化学。二。由PPh（3）取代的羟基环戊二烯基氢化钌[2,5-Ph（2）-3,4-Tol（2）（eta（5）-C（4）COH）] Ru的化学计量较慢和较快的醛催化还原（CO）（PPh（3））H：一种高度化学选择性的催化剂，用于醛在酮上的氢化。
6. Front Cover: Trend‐Analysis of Solid‐State Structures: Low‐Energy Conformational ‘Reactions’ Involving Directed and Coupled Movements in Half‐Sandwich Compounds CpFe(CO){C(=O)R}PPh3 (ChemistryOpen 5/2018) [O] . Prof. Dr. Henri Brunner, Prof. Dr. Takashi Tsuno 2018

机译：封面：固态结构的趋势分析：涉及半夹心化合物CpFe（CO）{C（= O）R} PPh3的定向运动和耦合运动的低能构象反应（ChemistryOpen 5/2018）
7. Intramolecular rearrangements of sulphines co-ordinated to Pt involving insertion and reductive coupling reactions. X-Ray crystal and molecular structure of (E)-PtII(PhS)(PPh3)2(PhSCSO)·C6H6, a new type of heterocumulene–metal complex [O] . Johan W. Gosselink, Anja M. F. Brouwers, Gerard van Koten, 1979

机译：协调涉及插入和还原偶联反应的核指的分子分子重排。（e） - PTII（PHS）（PPH3）2（PHSCSO）·C6H6，一种新型杂芳烃 - 金属络合物的X射线晶体和分子结构
8. Simultaneous Conversion of Ni-PR3 and B-H to Ni-H and B-PR3 Linkages by Thermal Rearrangement of d8-Closo-Bis(triarylphosphine)Nickelacarboranes. Crystal and Molecular Structure of (Closo-3-mu-CO-8-PPh3-3,1,2-NiC2B9H10)2; a Dimeric Nickelacarborane Complex Containing a Metal-Metal Bond. [R] . King, R. E., Miller, S. B., Knobler, C. B., 1983

机译：通过d8-Closo-Bis（三芳基膦）Nickelacarboranes的热重排将Ni-pR3和B-H同时转化为Ni-H和B-pR3键。（Closo-3-mu-CO-8-pph3-3,1,2-NiC2B9H10）2的晶体和分子结构;含有金属 - 金属键的二聚体Nickelacarborane复合物。

A novel structural rearrangement reaction of dialkylated derivatives of [Pt _2(μ-S) _2(PPh _3) _4] involving Pt-C bond formation

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