[2.2.2]m,p,p- and [2.2.2]m,m,p-Cyclophane-Ag-triflate: new π-prismand complexes

Structure of recombinant Ves v 2 at 2.0 Å resolution: structural analysis of an allergenic hyaluronidase from wasp venom

“…Natural Ves v 2 and rVes v 2 were redissolved in 50 mM Tris-HCl pH 8.5, 0.2 M NaCl and 1 M urea and incubated with 3%(w/w) endoproteinase Lys-C (Wako GmbH, Richmond, VA, USA) and Asp-N (Calbiochem, Sunnyvale, CA, USA) at 310 K for 18 h (Seppala et al, 2005). Reduction and alkylation of rVes v 2 were performed as described in Seppala et al (2005).…”

“…Natural Ves v 2 and rVes v 2 were redissolved in 50 mM Tris-HCl pH 8.5, 0.2 M NaCl and 1 M urea and incubated with 3%(w/w) endoproteinase Lys-C (Wako GmbH, Richmond, VA, USA) and Asp-N (Calbiochem, Sunnyvale, CA, USA) at 310 K for 18 h (Seppala et al, 2005). Reduction and alkylation of rVes v 2 were performed as described in Seppala et al (2005). Assignment of the disulfide bridges in r Ves v 2 and the glycosylation sites in nVes v 2 were performed by enzymatic digestion employing 3%(w/w) trypsin (Sequencing Grade Modified Trypsin, Promega, Madison, WI, USA) in 50 mM Tris-HCl pH 8.5, 0.2 M NaCl and 1 M urea.…”

Small Hydrocarbon Cyclophanes: Synthesis, X-ray Analysis and Molecular Modelling

“…A member of the earlier reported family of hydrocarbon [2.2.2]cyclophanes, [9,10] namely [2.2.2]m,m,p-cyclophane (5) formed crystals by slow evaporation of a 1:1 dichloromethane/hexane mixture. Colourless crystals of the disulfides (16 and 17) were obtained by dissolving the crude products in dichloromethane and allowing the solvent to evaporate very slowly from each solution at room temperature, to give small well-diffracting crystals of 16 and 17.…”

“…The X-ray structure ( Figure 4) shows a very similar conformation to that present in the earlier hydrocarbon [2.2.2]cyclophanes. [5,9,10] The X-ray structure of its π-prismand Ag ϩ complex 9 has been reported earlier. [9,10] X-ray structures of similar cyclophane silver complexes have been reported by Hopf et al [20Ϫ23] Disulfides 16 and 17 crystallise in a monoclinic space group (P2 1 /n).…”

“…[5,9,10] The X-ray structure of its π-prismand Ag ϩ complex 9 has been reported earlier. [9,10] X-ray structures of similar cyclophane silver complexes have been reported by Hopf et al [20Ϫ23] Disulfides 16 and 17 crystallise in a monoclinic space group (P2 1 /n). The structures are strained and forced almost planar due to the very strained diphenyl parts of the molecules ( Figure 5 1)°indicating an almost ideal π-prismand geometry and a triangular shape.…”