15627-48-2Relevant academic research and scientific papers
Aminomethylene complexes of divalent tungsten and molybdenum
Cook, Darren J.,Hill, Anthony F.
, p. 5616 - 5617 (1997)
Convenient routes are reported to aminomethylene complexes of divalent molybdenum and tungsten: [M(=CHNiPr2)(CO)2(S2CA)2] (M = Mo, W; A = NMe2, NEt2, N(CH2)4, OEt).
Synthesis and Reactivity of the Paramagnetic Nitrosyl Complexes 2+ (M = Cr or Mo), and the Crystal Structures of and
Clamp, Sara,Connelly, Neil G.,Taylor, Graham E.,Louttit, Thomas S.
, p. 2162 - 2169 (1980)
Excess of Y (Y = BF4 or PF6) and in acetonitrile afford paramagnetic Y2.At room temperature (1; M = Cr) and (1-) yield (2; R = Me or ET) which affords cis- in refluxing toluene; only cis-(2-) is isolable from the reaction between (1; M = Cr) and Na2.A crystal-structure determination of (2; R = Et) has revealed the geometry about chromium to be pentagonal bipyramidal with the nitrosyl ligand in an axial position; crystals are triclinic, space group PI, with Z = 2, in a unit cell of dimensions a = 9.525(3), b = 9.903(5), c = 14.649(7) Angstroem, α = 103.8(4), β = 74.5(3), and γ = 107.4(3) degree.The structure has been solved from diffractometer data by the heavy-atom method, and refined to R = 0.040 for 3.033 observed reflections.With 1,2-bis(diphenylphosphino)ethane (dppe) in acetonitrile (1; M = Cr or Mo) affords Y2 (3; M = Cr) and Y (4; M = Mo) which is oxidised to (3; M = Mo) by Y.Dppe and (1; M = Cr) also give Y (5; X = F) which is reduced, as is (3; M = Cr), by Na in tetrahydrofuran to (6; X = F).The crystal structure of (6; X = F) has verified the trans disposition of the NO and F ligands; crystals are monoclinic, space group P21/n, with Z = 2, in a unit cell of dimensions a = 11.080(6), b = 16.352(6), c = 13.129(7) Angstroem, and β = 109.17(4) deg.The structure has been solved from diffractometer data by the heavy-atom method, and refined to R = 0.047 for 2633 observed reflections.Complexes (3) and (4) react with chloride ion to give Y (5; M = Cr or Mo, X = Cl) and (6; M = Mo, X = Cl) respectively, which are interconvertible by Y oxidation reduction .The redox properties of complexes (1)-(6) have also been studied, by cyclic voltammetry, and the retention during electron transfer of the mutually trans disposition of the dppe ligands of (3)-(6) verified by 31P NMR and e.s.r. spectroscopy.
Synthetic and structural study of cyclopentadienylchromium dithiocarbamate complexes and their thermolytic derivatives
Goh, Lai Yoong,Weng, Zhiqiang,Leong, Weng Kee,Leung, Pak Hing
, p. 4398 - 4407 (2008/10/08)
The reaction of [CpCr(CO)3]2 (1) with the tetraalkylthiuram disulfides [R2NC(S)S]2 (R = Me, Et, i-Pr) has been investigated. At ambient temperature, CpCr(CO)2(η2-S2CNR2) (3) was obtained as air-stable dark red crystals in 81-87% yields from reactions in solution and in quantitative yield from a reaction in the solid state (3a, R = Me); the precursor complex CpCr(CO)3(η1-S2CNMe2) (2a) crystallized out in a 1:1 admixture with 3a from a product solution after 3 days at -29 °C. At 90 °C for 2 h, the same reaction or the thermal degradation of 3 led to the isolation of the thiocarbenoid complex CpCr(CO)2(η2-SCNR2) (4) as dark red crystals (ca. 10%), double cubanes Cp6Cr8S8(η2:4-SCNR 2)2 (5a, R = Me; 5b, R = Et) as dark brown crystals (3-7%), Cp6Cr6S8(η1:η?2-S 2CNR) (6) as dark crystals (7-14%), Cr(η2-S2CNR2)3 (7) as dark blue crystals (16-21%), Cp2Cr2(CO)4S as dark green crystals (1-3%), and Cp4Cr4S4 (12-22%) as dark green solids. The crystal structures of 2-6 were reported. Unprecedented bridging modes were found in the double cubanes: in 5, two Cr4S4 cubane clusters were linked by a μ-η2:η4-dithiooxamide ligand as well as a Cr - Cr bridge with bond distances of 3.101 and 3.118 A? in the two independent molecules of the compound, and in 6, the cubanes were linked by two μ-η1:η2-dithiocarbamate ligands.
Chromium(III) Dithiocarbamates - A Thin Layer Chromatographic Study and Characterisation of Some New Binuclear Mixed Ligand Dithiocarbamates
Soundararajan, G.,Subbaiyan, M.
, p. 1058 - 1061 (2007/10/02)
When chromium(III) dithiocarbamates are prepared from chromium(VI) species by reduction and complexation with excess ligand, new mixed ligand binuclear dithiocarbamates are formed along with mononuclear chelates , where dtc = dithiocarbamate anion and tds = thiuram disulphide.These new complexes are characterised by different physical methods after separation from mononuclear chelates by preparative column chromatography.
