9‐(Organothio)‐9‐borabicyclo[3.3.1]nonane — Herstellung und Charakterisierung

Abstract

Die PRS-9-BBN-Verbindungen [R = CH3 (la), C2Hs (lb), CH(CH3)2 ( 1 6 C4CH3h (la), CaHs (leh -CH2CHz-(If)] werden aus 9-Cl-9-BBN mit LiSR (la, b, d, e) oder aus (9-BBN), mit HSR (lc, f) hergestellt. Siimtiiche 9-RS-9-BBN-Verbindungen sind in &sung bei Raumtemperatur monomer ("B-NMR). Die n-C-und BC-Resonanzen des GH14B-Bicyclus sind in den "C-NMRSpektren von la-c und fbei bzw. unterhalb Raumtemperatur in jeweils zwei Sgtze aufgespalten (behinderte Rotation um die BSBindung). Vom festen Dimeren (lab iiegi eine R6ntgenstruktur-analyse vor. Die gemischten Dimeren la-9-BBN und lb-9-BBN bilden sicb in Liisung aus la bzw. l b mit (9-BBN (MS, "B-NMR-Spektren). (1ah reagiert mit AICla, Pyridin oder Trimethylphosphan unter Bildung der kristallisierten 1 :1 -Additionsverbindungen la-AlC13, Py-la bzw. TMP-la.

Trinuclear Early/Late‐Transition‐Metal Thiolate Complexes

“…Anhydrous CH 3 CN (H 2 O Ͻ 0.001 %) obtained from Aldrich was degassed, freshly distilled and stored over molecular sieves under nitrogen. LiSPh [67] was prepared according to a literature procedure. Anhydrous CoCl 2 and VCl 3 (Ͼ97 %) were purchased from Aldrich.…”

Syntheses, Structures, and Properties of Trinuclear Copper(I)/Titanium(IV) Thiolate Complexes

“…Anhydrous CH 3 CN (H 2 O Ͻ 0.001 %), CH 2 Cl 2 (H 2 O Ͻ 0.001 %), and DMF (H 2 O Ͻ 0.005 %) were obtained from Aldrich and degassed, freshly distilled, and stored over molecular sieves under nitrogen. TiCl 4 ·2thf [50] and LiSPh [51] were prepared according to literature procedures. CuCl was washed with HCl, CH 3 OH, and diethyl ether to remove traces of CuCl 2 , then dried under vacuum.…”

Syntheses, Structures and Theoretical Investigations of [Li(thf)4]2[Ti2Cu8S4(SPh)10] and [Ti2Ag6S6Cl2(PPhiPr2)6]

“…TiCl 4 ·2thf, [36] LiSPh [37] and S(SiMe 3 ) 2 [38] were prepared according to literature procedures. CuCl was washed with HCl, CH 3 OH, and diethyl ether to remove traces of CuCl 2 , and then dried under vacuum.…”