Abstract:SummaryThe isocratic high-performance liquid chromatography of 1,1'-bis(diphenylphosphino)ferrocene (dppf), 1,1'-bis(diphenylphosphino)ruthenocene (dppr), bis(diphenylphosphino)methane (dppm) and triphenylphosphine (PPh3)-substituted heterometallic Au-Mn or AuRe carbonyl complexes is reported. A column packed with PGC (porous graphitic carbon) was used after preliminary experiments had shown that silica-and bonded-phase (silica-based) stationary phases were unsatisfactory for separation. The PGC column exhibit… Show more
“…The bite angle of dppr (99.63(6)°) is 2.1% larger than that of dppf (97.55(5)°), while the average M···Cp centroid (M = Fe, Ru) distance in dppr (1.805 Å) is 9.6% larger than in dppf (1.647 Å). The bite angle of a phosphine has been linked to the catalytic efficiency of its complexes. 5b, 2 Crystal structure of PtRu 3 (CO) 6 (μ-CO) 2 (η 2 -dppf)(μ 4 -S) 2 ( 5a ), with thermal ellipsoids at 50% probability. 3 Crystal structure of PtRu 3 (CO) 6 (μ-CO) 2 (η 2 -dppr)(μ 4 -S) 2 ( 5b ), with thermal ellipsoids at 50% probability.…”
Section: Resultsmentioning
confidence: 99%
“…All reactions were performed under pure dry argon using standard Schlenk techniques. Pt 2 (dba) 3 ( 1 ), dppf ( 2a ), dppr ( 2b ),5b and Ru 3 (CO) 9 ( μ 3 -S) 2 ( 4 ) 9 were prepared by literature methods. Solvents used were of reagent grade and were dried by published procedures and freshly distilled and degassed under argon before use.…”
Section: Methodsmentioning
confidence: 99%
“…The ease of M−M and M−S bond formation and cleavage also leads to a variety of fascinating but unpredictable cluster structures. Our interest in the metallocenyl diphosphines (P−P) such as dppf 4 ( 2a ) [dppf = 1,1‘-bis(diphenylphosphino)ferrocene] and dppr ( 2b ) [dppr = 1,1‘-bis(diphenylphosphino)ruthenocene] stems from their rich catalytic and electroactive potential. This approach would provide a simple entry into electroactive clusters if a precursor like Pt( η 2 -P−P)( η 2 -C 2 H 4 ) can be synthesized and isolated easily.…”
Two labile but air-stable Pt(0) complexes Pt(η 2 -P-P)(η 2 -dba) [dba ) dibenzylideneacetone; P-P ) 1,1′-bis(diphenylphosphino)ferrocene (dppf) (3a) or 1,1′-bis(diphenylphosphino)ruthenocene (dppr) (3b)] were prepared from Pt 2 (dba) 3 (1) and the corresponding metallocenyl diphosphine. Reductive addition of 3 to Ru 3 (CO) 9 (µ 3 -S) 2 (4) gave good yields of two novel square clusters PtRu 3 (CO) 6 (µ-CO) 2 (η 2 -P-P)(µ 4 -S) 2 [P-P ) dppf (5a) or dppr (5b)]. A one-pot reaction mixture containing 1, 4, and the diphosphine (2) gave Ru 3 (CO) 7 (µ-P-P)(µ 3 -S) 2 [P-P ) dppf (6a) or dppr (6b)] along with 5a and 5b. All products have been characterized by IR, 1 H, and 31 P{ 1 H} NMR. In addition, X-ray crystal analyses were also performed on complexes 3a, 5a, 5b, and 6a. 3a is a planar Pt(0)-olefin complex stabilized by chelating dppf and a trans,trans-dba moiety coordinated via a CdC functionality. Compounds 5a and 5b are rare examples of almost regularly octahedral heterometallic square clusters with two µ 4 -S ligands above and below the PtRu 3 plane.
“…The bite angle of dppr (99.63(6)°) is 2.1% larger than that of dppf (97.55(5)°), while the average M···Cp centroid (M = Fe, Ru) distance in dppr (1.805 Å) is 9.6% larger than in dppf (1.647 Å). The bite angle of a phosphine has been linked to the catalytic efficiency of its complexes. 5b, 2 Crystal structure of PtRu 3 (CO) 6 (μ-CO) 2 (η 2 -dppf)(μ 4 -S) 2 ( 5a ), with thermal ellipsoids at 50% probability. 3 Crystal structure of PtRu 3 (CO) 6 (μ-CO) 2 (η 2 -dppr)(μ 4 -S) 2 ( 5b ), with thermal ellipsoids at 50% probability.…”
Section: Resultsmentioning
confidence: 99%
“…All reactions were performed under pure dry argon using standard Schlenk techniques. Pt 2 (dba) 3 ( 1 ), dppf ( 2a ), dppr ( 2b ),5b and Ru 3 (CO) 9 ( μ 3 -S) 2 ( 4 ) 9 were prepared by literature methods. Solvents used were of reagent grade and were dried by published procedures and freshly distilled and degassed under argon before use.…”
Section: Methodsmentioning
confidence: 99%
“…The ease of M−M and M−S bond formation and cleavage also leads to a variety of fascinating but unpredictable cluster structures. Our interest in the metallocenyl diphosphines (P−P) such as dppf 4 ( 2a ) [dppf = 1,1‘-bis(diphenylphosphino)ferrocene] and dppr ( 2b ) [dppr = 1,1‘-bis(diphenylphosphino)ruthenocene] stems from their rich catalytic and electroactive potential. This approach would provide a simple entry into electroactive clusters if a precursor like Pt( η 2 -P−P)( η 2 -C 2 H 4 ) can be synthesized and isolated easily.…”
Two labile but air-stable Pt(0) complexes Pt(η 2 -P-P)(η 2 -dba) [dba ) dibenzylideneacetone; P-P ) 1,1′-bis(diphenylphosphino)ferrocene (dppf) (3a) or 1,1′-bis(diphenylphosphino)ruthenocene (dppr) (3b)] were prepared from Pt 2 (dba) 3 (1) and the corresponding metallocenyl diphosphine. Reductive addition of 3 to Ru 3 (CO) 9 (µ 3 -S) 2 (4) gave good yields of two novel square clusters PtRu 3 (CO) 6 (µ-CO) 2 (η 2 -P-P)(µ 4 -S) 2 [P-P ) dppf (5a) or dppr (5b)]. A one-pot reaction mixture containing 1, 4, and the diphosphine (2) gave Ru 3 (CO) 7 (µ-P-P)(µ 3 -S) 2 [P-P ) dppf (6a) or dppr (6b)] along with 5a and 5b. All products have been characterized by IR, 1 H, and 31 P{ 1 H} NMR. In addition, X-ray crystal analyses were also performed on complexes 3a, 5a, 5b, and 6a. 3a is a planar Pt(0)-olefin complex stabilized by chelating dppf and a trans,trans-dba moiety coordinated via a CdC functionality. Compounds 5a and 5b are rare examples of almost regularly octahedral heterometallic square clusters with two µ 4 -S ligands above and below the PtRu 3 plane.
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