Solid complex, preparation

The materials shown and described above were generally prepared from the nucleophilic phenoxide or alkoxide and the appropriate bromide. The syntheses of a variety of such compounds were detailed in a report which appeared in 1977. In the same report, complex stability and complexation kinetics are reported. Other, detailed studies, of a similar nature have recently appeared" . Vogtle and his collaborators have also demonstrated that solid complexes can be formed even from simple polyethylene glycol ethers . Crystal structures of such species are also available... 

The first xanthates of V(IV), [Cp2V(Rxanth)] (R = Me, Et, Pr , or Bu), isolated as purple solids were prepared by the same method (71). Kwoka et al. (70) were able to obtain an alkylenebis(dithiocarbamate) vanadyl complex, VO[SjjCNH(CH2) NHCS2] for n — 2, but not for... 

When L = 4-CNC5H4N (PK3 = 1.86), 2-CIC5H4N (pK = 2.81), or 4-PhCOC5H4N (pKj = 3.35) [Hg2L2] [C10412 can be isolated as solids. However, under the same conditions the more basic unsubstituted pyridine (pK, = 5.21) leads to disproportionation, and no complex can be isolated. Complexes of Hg(I) of these more basic substituted pyridines can be prepared under a N2 atmosphere in MeOH at -70°C. Table 1 shows some Hg(I) complexes prepared with N-donor ligands. The majority contain an Hg2 ion with each atom coordinated to one or two N atoms as in I or II. 

The experimental details are mentioned as they arise often air must be excluded from the reactions but there are many examples when this exclusion is not important (or may even be fatal ) to the reaction. A general point is that nearly all of these organocobalt(III) complexes are unstable to visible light, and so light should be excluded during the preparations at all times whenever the organocobalt(III) complex is in solution. The solid complexes are stable to visible light. 

While iron(III) complexes of thiosemicarbazones with different functional groups involving have been prepared from 2-acetylpyridine, substitution on the ring has been more popular with thiosemicarbazones derived from 2-formylpyridine. The only thiosemicarbazones in which the 2-acetylpyridine ring has been substituted are 15a and 15b, prepared from 6-methyl-2-acetyl-pyridine [120]. Both of these iron(III) complexes have rhombic spectra and values of g, are similar to those found for the 2-acetylpyridine thiosemicarbazones. Solution studies have been carried out on the iron(III) complex of 2,6-diacetylpyridine mono-thiosemicarbazone, but the solid complex was not isolated [143]. 

The monohydrate explodes at 109 -110° C during slow heating [ 1 ]. The solid complex exploded when manipulated on a glass sinter with a metal spatula [1]. Preparation on small scale and use of plastic equipment is recommended [2],... 

In preliminary studies various metal salts such as PdCl2 were attached to the ligands and the complexes characterized by NMR spectroscopy and X-ray crystallography. Typical examples are the palladium complexes (32)—(44) (Scheme 9).66 The catalytic profiles of these and other transition metal complexes prepared by this method still need to be defined. Moreover, solid-phase synthetic versions would be advantageous, and this may well be possible via the (protected) phenol function. 

A great many metal complexes are prepared by reactions carried out in aqueous solutions. Consequently, solid complexes are frequently obtained as hydrates. Water is also a potential ligand so various possibilities exist for compounds to be prepared with water held in both ways. For example, [Cr(H20)4Cl2]Cl-2ff20 and [Cr(H20)5Cl]Cl2-ff20 have the same formula, but they are obviously different compounds. In the first case, two chloride ions are coordinated and one is present as an anion, whereas in the second case the numbers are reversed. Many other examples of hydrate isomerism are known. 

The RPIA technology has been enhanced in the Stratus CS system by utilization of a dendrimer-antibody complex in which the analyte-specific capture antibody is covalenty coupled onto a dendrimer. The test packs in the Stratus CS system include dendrimer-capture antibody complex reagent, the alkaline phosphatase labeled antibody conjugate reagent, the substrate-wash reagent and a piece of glass fiber filter paper as the solid phase. Preparation and unique properties associated with these dendrimer-coupled antibody complexes are described below. 

Highly reactive calcium can be readily prepared by the reduction of calcium halides in tetrahydrofuran solution with preformed lithium biphenylide under an argon atmosphere at room temperature.5 This colored calcium species seems to be reasonably soluble in THF. However, the reactive calcium complex prepared from preformed lithium naphthalenide was insoluble in THF solution and precipitated out of solution to give a highly reactive black solid. The exact nature of this black calcium complex has not been determined. Acid hydrolysis of the black material releases naphthalene as well as THF. Accordingly, the most likely structure of the black material is a Ca-naphthalene-THF complex similar in nature to the soluble magnesium-anthracene complex recently reported.6... 

A preparative solid- gas phase synthesis of acetyl hypofluorite (1, R = Me) has been described it is based on the reaction of dilute fluorine (with air or nitrogen) with a solid complex of potassium acetate with acetic acid and can be also modified7 -9 for the preparation of acetyl... 

Uozumi, Y. Danjo, H. Hayashi, T. New Amphiphilic Palladium-Phosphine Complexes Bound to Solid Supports Preparation and Use for Catalytic Allylic Substitution in Aqueous Media, Tetrahedron Lett. 1997, 38, 3557. 

Oxovanadium(IV) complexes with (97) and (98) derived from alkyl aminoalcohols and Hsal or o-hydroxyacetophenone (and substituted derivatives), respectively, have been prepared as well as VOz+ complexes with (99) derived from 2-hydrazinoethanol and Hsal and substituted Hsal. Most of these and some properties are summarized in Table 42. Generally the complexes were prepared by adding an alcoholic solution of the SB, either previously obtained as a solid or prepared in situ, to alcoholic vanadyl acetate. The mixture is normally refluxed for several hours and the precipitates are collected by filtration as they are not soluble they are not recrystallized. 

Early solid complexes include [VO(oxine)2], [VO(oxine)2py] and [VO(5,7-X2oxine)2] (X = Br, I).357 [VOX(oxine)] (X = Cl, Br, OH) were also prepared with magnetic moments dependent on temperature.823 On the contrary, for brown [VO(oxine)2], prepared from V0S04 in aqueous solution,387 /4fr is near the spin-only value and v(V=0) = 979 cm-1.595 These values indicate a monomeric structure and this was confirmed for its 2-methyl derivative by X-ray diffraction (Figure 36).824... 

Bozis and McCormick prepared several green complexes with monothio-/3-diketones (153)-(155), formulated as monomeric square pyramidal [VOLJ.849 With (156) and (157), the complexes have a golden yellow colour, diffuse reflectance spectra differ from those with (153)-(155) and v(V=0) was at 868 and 876 cm-1 for [VO(ttmbs)2] and [VO(nebas)2], respectively.850 The solid complexes probably have a structure that involves —V—O—V— bridging, as found for [VO(salnpn)] (Figure 30). 

Numerous nickel(II) complexes with a variety of polydentate amines have been described. Selected examples of such complexes are collected in Table 42. In general, solid complexes have been easily obtained by direct synthesis from nickel salts and the appropriate ligand using H20, MeOH, EtOH or butanol as reaction medium. Most of the complexes with the fully TV-alkyl-substituted ligands are conveniently prepared under anhydrous conditions. 

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