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81.
The neutral technetium(V) phosphoraneimine complex [TcNCl2(Ph2PNH)2] is formed when (Bu4N)[TcOCl4] reacts with Me3SiNPPh3 in dichloromethane. Distances of 2.078(4) and 2.102(4) Å have been found between Tc and the neutral triphenylphosphoraneimine ligands. The Tc‐N‐P angles are 133.7(3) and 134.8(3)°. The terminal nitrido ligand is formed by decomposition of an additional molecule of Me3SiNPPh3. The protons which are used for the protonation of the organic ligands are released during the decomposition of CH2Cl2. The same reaction yields the [TcNCl4]— anion when it is performed in acetonitrile. 相似文献
82.
Synthesis and Structure of [(Me2PhP)3Cl2ReN]2NbCl4 and [Re3N3Cl5(PMe2Ph)6][NbCl6] The reaction of ReNCl2(PMe2Ph)3 with NbCl5 in toluene yields the trinuclear complexes [(Me2PhP)3Cl2ReN]2‐ NbCl4 (1) and [Re3N3Cl5(PMe2Ph)6][NbCl6] ( 2 ). 1 forms triclinic crystals with the composition 1 · 2 C7H8 (P 1, a = 1074.5(1), b = 1289.1(2), c = 1299.3(2) pm, α = 85.25(2)°, β = 81.04(2)°, γ = 86.02(1)°, Z = 1). In the centrosymmetric compound 1 two complexes ReNCl2(PMe2Ph)3 coordinate with their nitrido ligands a square planar, central unit NbCl4 to form an almost linear arrangement Re≡N–Nb–N≡Re. The length of the Re–N triple bonds is 172,2 pm, and the Nb–N distances of 216.0 pm correspond to coordinative single bonds. 2 forms orthorhombic crystals with the space group P212121 and a = 1286.0(1), b = 2109.2(4), c = 2436.2(3) pm, Z = 4. The three Re atoms are located at the corners of a triangle. They are connected by two asymmetric nitrido bridges and two asymmetric chloro bridges. The weakly bent nitrido bridges (Re–N–Re = 152° and 157°) are characterized by Re–N distances of 169 und 207 pm as well as 171 and 207 pm. Re1, in addition, binds a terminal nitrido ligand with Re1–N1 = 166 pm. 相似文献
83.
Synthesis and Structure of [(Me2PhP)3Cl2ReN]2ReCl4, [(Me2PhP)3Cl2ReN]2ReCl4 · 2 SbCl3 and [Re(NH)Cl2(PMe2Ph)3][SbCl6] The reaction of ReNCl2(PMePh)3 with SbCl5 in toluene yields the trinuclear complex [(Me2PhP)3Cl2Re≡N]2ReCl4 · 2 SbCl3 ( 1 · 2 SbCl3). It forms triclinic crystals with the composition 1 · 2 SbCl3, as well as monoclinic crystals 1 · 2 SbCl3 · 4 C7H8. The monoclinic crystals with the space group P21/c, and a = 1212.3(2), b = 2098.5(4), c = 1827.7(3) pm, β = 95.51(1)°, Z = 2, have been used for a crystal structure determination. In the centrosymmetric complex 1 two complexes ReNCl2(PMe2Ph)3 coordinate with their nitrido ligands a square planar, central unit ReCl4. The SbCl3 molecules are coordinated by chlorine bridges to Cl atoms of 1 , and, in addition, connect the complexes 1 with each other. The SbCl3 free compound 1 is obtained in good yield by the reaction of ReNCl2(PMePh)3 with ReCl4(NCEt)2. It crystallizes in the triclinic space group P1 with a = 1037.7(3), b = 1153.0(2), c = 1393.8(3) pm, α = 72.31(2)°, β = 74.06(2)°, γ = 67.94(2)°, and Z = 1. The bond lengths of the Re–N triple bonds are 172 pm in 1 and 170 pm in 1 · 2 SbCl3. By the reaction of ReNCl2(PMePh)3 with SbCl5 in CH2Cl2 the solvent is decomposed forming HCl which protonates the nitrido ligand to afford the imido complex [Re(NH)Cl2(PMe2Ph)3][SbCl6] ( 2 ) crystallizing in the monoclinic space group P21/n with a = 1221.4(2), b = 1358.6(2), c = 2177.3(1) pm, β = 92,72(1)° and Z = 4. The Re–N distance in the almost linear unit Re≡N–H is 169,1 pm. 相似文献
84.
Guilhem Claude Dominik Weh Dr. Adelheid Hagenbach Prof. Joshua S. Figueroa Prof. Ulrich Abram 《无机化学与普通化学杂志》2023,649(1):e202200320
p-Fluorophenylisocyanide (CNPhpF) reacts with [Re(CO)5Br] under stepwise exchange of the carbonyl ligands depending on the conditions applied. The reaction stops with the formation of fac-[Re(CO)3Br(CNPhpF)2] in boiling THF. An ongoing carbonyl exchange is observed at higher temperatures, e. g. in refluxing toluene, with the final formation of the [Re(CNPhpF)6]+ cation. The progress of the reactions has been studied by 19F NMR spectroscopy and the structures of [Re(CO)Br(CNPhpF)4] and [Re(CNPhpF)6](BPh4) have been elucidated by X-ray diffraction. 相似文献
85.
Dr. Federico Salsi Dr. Shuai Wang Dr. Christian Teutloff Marvin Busse Dr. Michael L. Neville Dr. Adelheid Hagenbach Prof. Dr. Robert Bittl Prof. Dr. Joshua S. Figueroa Prof. Dr. Ulrich Abram 《Angewandte Chemie (International ed. in English)》2023,62(19):e202300254
The first consistent series of mononuclear 17-electron complexes of three Group 7 elements has been isolated in crystalline form and studied by X-ray diffraction and spectroscopic methods. The paramagnetic compounds have a composition of [M0(CO)(CNp-F-ArDArF2)4] (M=Mn, Tc, Re; ArDArF2=2,6-(3,5-(CF3)2C6H3)2C6H2F) and are stabilized by four sterically encumbering isocyanides, which prevent the metalloradicals from dimerization. They have a square pyramidal structure with the carbonyl ligands as apexes. The frozen-solution EPR spectra of the rhenium and technetium compounds are clearly anisotropic with large 99Tc and 185,187Re hyperfine interactions for one component. High-field EPR (Q band and W band) has been applied for the elucidation of the EPR parameters of the manganese(0) complex. 相似文献