Complexes of ligands containing phenyl and cyclopentadienyl rings. Synthesis, characterization and spectroscopic studies on tricarbonylmanganese tricarbonylchromium derivatives
“…2 reacted with [Mn(CO) 4 Br] 2 to produce compound 18 , Cr(CO) 3 (η 6 ,η 5 -C 6 H 5 C 5 H 4 )Mn(CO) 3 . The synthesis of 18 has been completed through route I shown in Scheme by two groups. , Compared with their methods, our synthetic method is superior in the following aspects: mild reaction conditions, easy manipulation, and high yield. In addition, when [Mn(CO) 4 Br] 2 was treated with 4 , a heterobimetallic compound with the bridging phenylindenyl ligand ((tricarbonylchromio)-η 6 ,η 5 -phenylindenyl))tricarbonylmanganese ( 19 ) was obtained (Scheme ).…”
Section: Resultsmentioning
confidence: 99%
“…There are three possible synthetic routes (as shown in Scheme ). Compared with route III, routes I and II are more complicated and forcing reaction conditions are needed. − We will introduce later in this paper that route III is a general method for the syntheses of these compounds, with advantages of easy manipulation, mild reaction conditions, and moderate to high yields. 2 …”
A new synthetic method of heterobimetallic complexes bridging with a pi,pi-phenylcyclopentadienyl ligand, tricarbonylchromium-eta(6),eta(5)-phenylcyclopentadienyl-transition metal complexes, was developed through the reactions of (eta(6)-C(6)H(5)C(5)H(5))Cr(CO)(3) or its sodium salt with transition metal complexes. The method is suitable for most transition metal elements with the advantages of easy manipulation, mild reaction conditions, and moderate to high yields. As indicated by (1)H NMR spectra, the interactions between the two pi systems of phenyl and cyclopentadienyl rings were weak. X-ray crystal structures of seven complexes were studied. Compound 23, [eta(6)-C(6)H(5)Cr(CO)(3)](2)C(10)H(10), crystallizes in orthorhombic space group Pbca with cell constants a = 29.616(8) Å, b = 12.861(5) Å, c = 12.397(7) Å, V = 4721(6) Å(3), Z = 8, R = 0.045, and R(w) = 0.045. Compound 3, (eta(6)-C(6)H(5)C(9)H(7))Cr(CO)(3), crystallizes in monoclinic space group P2(1)/c with cell constants a = 7.901(3) Å, b = 14.799(2) Å, c = 12.917(2) Å, beta = 99.72(2) degrees, V = 1488.7(4) Å(3), Z = 4, R = 0.044, and R(w) = 0.051. Compound 7, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Ti(CO)(2)(eta(5)-C(5)H(5)), crystallizes in monoclinic space group P2(1)/c with cell constants a = 12.361(4) Å, b = 12.487(6) Å, c = 12.531(7) Å, beta = 93.48(4) degrees, V = 1930 Å(3), Z = 4, R = 0.047, and R(w) = 0.048. Compound 13, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Mo(CO)(3)Br, crystallizes in monoclinic space group P2(1)/c with cell constants a = 14.685(2) Å, b = 8.509(3) Å, c = 14.960(3) Å, beta = 104.46(1) degrees, V = 1810.0(7) Å(3), Z = 4, R = 0.037, and R(w) = 0.037. Compound 19, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(9)H(6))Mn(CO)(3), crystallizes in triclinic space group P(-)(1) with cell constants a = 11.660(4) Å, b = 12.578(5) Å, c = 6.987(2) Å, alpha = 100.03(3) degrees, beta = 104.19(2) degrees, gamma = 71.99(3) degrees, V = 939.3(6) Å(3), Z = 2, R = 0.048, and R(w) = 0.065. Compound 21, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Ru(PPh(3))(2)Cl, crystallizes with one molecule of EtOH in triclinic space group P(-)(1) with cell constants a = 14.033(4) Å, b = 16.163(6) Å, c = 10.411(3) Å, alpha = 104.22(3) degrees, beta = 103.50(2) degrees, gamma = 90.81(3) degrees, V = 2219(1) Å(3), Z = 2, R = 0.081, and R(w) = 0.096. Compound 22, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Co(CO)(2), crystallizes in orthorhombic space group P2(1)2(1)2(1) with cell constants a = 15.083(5) Å, b = 16.391(5) Å, c = 6.351(4) Å, V = 1570(1) Å(3), Z = 4, R = 0.036, and R(w) = 0.039. The trans configurations of the two metal atoms in these molecules were found as expected; the phenyl and cyclopentadienyl or indenyl rings in the molecules were found to be not coplanar.
“…2 reacted with [Mn(CO) 4 Br] 2 to produce compound 18 , Cr(CO) 3 (η 6 ,η 5 -C 6 H 5 C 5 H 4 )Mn(CO) 3 . The synthesis of 18 has been completed through route I shown in Scheme by two groups. , Compared with their methods, our synthetic method is superior in the following aspects: mild reaction conditions, easy manipulation, and high yield. In addition, when [Mn(CO) 4 Br] 2 was treated with 4 , a heterobimetallic compound with the bridging phenylindenyl ligand ((tricarbonylchromio)-η 6 ,η 5 -phenylindenyl))tricarbonylmanganese ( 19 ) was obtained (Scheme ).…”
Section: Resultsmentioning
confidence: 99%
“…There are three possible synthetic routes (as shown in Scheme ). Compared with route III, routes I and II are more complicated and forcing reaction conditions are needed. − We will introduce later in this paper that route III is a general method for the syntheses of these compounds, with advantages of easy manipulation, mild reaction conditions, and moderate to high yields. 2 …”
A new synthetic method of heterobimetallic complexes bridging with a pi,pi-phenylcyclopentadienyl ligand, tricarbonylchromium-eta(6),eta(5)-phenylcyclopentadienyl-transition metal complexes, was developed through the reactions of (eta(6)-C(6)H(5)C(5)H(5))Cr(CO)(3) or its sodium salt with transition metal complexes. The method is suitable for most transition metal elements with the advantages of easy manipulation, mild reaction conditions, and moderate to high yields. As indicated by (1)H NMR spectra, the interactions between the two pi systems of phenyl and cyclopentadienyl rings were weak. X-ray crystal structures of seven complexes were studied. Compound 23, [eta(6)-C(6)H(5)Cr(CO)(3)](2)C(10)H(10), crystallizes in orthorhombic space group Pbca with cell constants a = 29.616(8) Å, b = 12.861(5) Å, c = 12.397(7) Å, V = 4721(6) Å(3), Z = 8, R = 0.045, and R(w) = 0.045. Compound 3, (eta(6)-C(6)H(5)C(9)H(7))Cr(CO)(3), crystallizes in monoclinic space group P2(1)/c with cell constants a = 7.901(3) Å, b = 14.799(2) Å, c = 12.917(2) Å, beta = 99.72(2) degrees, V = 1488.7(4) Å(3), Z = 4, R = 0.044, and R(w) = 0.051. Compound 7, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Ti(CO)(2)(eta(5)-C(5)H(5)), crystallizes in monoclinic space group P2(1)/c with cell constants a = 12.361(4) Å, b = 12.487(6) Å, c = 12.531(7) Å, beta = 93.48(4) degrees, V = 1930 Å(3), Z = 4, R = 0.047, and R(w) = 0.048. Compound 13, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Mo(CO)(3)Br, crystallizes in monoclinic space group P2(1)/c with cell constants a = 14.685(2) Å, b = 8.509(3) Å, c = 14.960(3) Å, beta = 104.46(1) degrees, V = 1810.0(7) Å(3), Z = 4, R = 0.037, and R(w) = 0.037. Compound 19, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(9)H(6))Mn(CO)(3), crystallizes in triclinic space group P(-)(1) with cell constants a = 11.660(4) Å, b = 12.578(5) Å, c = 6.987(2) Å, alpha = 100.03(3) degrees, beta = 104.19(2) degrees, gamma = 71.99(3) degrees, V = 939.3(6) Å(3), Z = 2, R = 0.048, and R(w) = 0.065. Compound 21, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Ru(PPh(3))(2)Cl, crystallizes with one molecule of EtOH in triclinic space group P(-)(1) with cell constants a = 14.033(4) Å, b = 16.163(6) Å, c = 10.411(3) Å, alpha = 104.22(3) degrees, beta = 103.50(2) degrees, gamma = 90.81(3) degrees, V = 2219(1) Å(3), Z = 2, R = 0.081, and R(w) = 0.096. Compound 22, Cr(CO)(3)(eta(6),eta(5)-C(6)H(5)C(5)H(4))Co(CO)(2), crystallizes in orthorhombic space group P2(1)2(1)2(1) with cell constants a = 15.083(5) Å, b = 16.391(5) Å, c = 6.351(4) Å, V = 1570(1) Å(3), Z = 4, R = 0.036, and R(w) = 0.039. The trans configurations of the two metal atoms in these molecules were found as expected; the phenyl and cyclopentadienyl or indenyl rings in the molecules were found to be not coplanar.
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