A new synthesis for trithiophosphonates from primary phosphines, nBuLi (or nBu(2)Mg) and elemental sulfur is presented and its mechanism investigated; the lithium and magnesium salts of cyclohexyltrithiophosphonate have been fully characterised to reveal dimers in the solid state in which all three of the trithiophosphonate sulfurs are involved in metal bonding.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
Hexafluorobut-2-yne (hfb) reacts (u.v.) with buta-1,3-diene(tricarbonyl)iron, tricarbonyl(2.3-dimethylbuta-1.3- diene)iron, or tricarbonyl(diphenyl-o-styrylphosphine) iron to form FeII 1 : 1 adducts in which the acetylene links the iron and dienes as in, for example, CH2[graphic omitted](CO)3. Similar reactions with 3,3,3-trifluoroprop-1-yne gave the corresponding adducts, in which the arrangement FeC(CF3)CH– is present. In contrast tricarbonyl(cyclohexa-1,3-diene)ruthenium forms on irradiation with hfb a 1 : 2 adduct. Replacement of co-ordinated CO in the adduct by P(OCH2)3CMe gave crystals of (9)[Ru(CO)2{P(OCH2)3CMe}(C6H8)(C4F6)2] suitable for X-ray crystallography. Crystals of (9) are monoclinic, space group P21/c, with Z= 4 in a unit cell of drmensions: a= 8.875(5), b= 17.841 (9), c= 16.517(5)Å, β= 94.51(3)°. The X-ray diffraction study (R 0.078, 2 418 observed intensities, measured by diffractometer) shows that formal insertion of a hfb molecule has occurred between the Ru atom and each carbon atom of one of the original olefinic bonds of the cyclohexadiene system. A new seven-membered ruthenacyclohepta-1,5-diene ring is generated. The co-ordination state of the Ru atom is close to octahedral, the ring system occupying three facial sites.Reaction of CH2[graphic omitted](CO)3 with carbon monoxide affords an acyl species; however, with heat in the absence of CO an interesting reductive–elimination reaction occurs with formation of a substituted tricarbonyl(cyclohexa-1,3-diene)iron complex. A similar ring closure reaction occurs with the adduct from [Fe(1,3-C4H6)(CO)3] and hfb.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
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