Characterization by X-ray

Na[Sb(OH)g], respectively. The latter compound is one of the least soluble sodium salts known and is useful in sodium analysis. Numerous polyantimonate(V) derivatives are prepared by heat treatment of mixtures of antimony trioxide and other metal oxides or carbonates. Of these, K Sb O [12056-59-6] and K Sb O [52015-49-3] have been characterized by x-ray. These consist of three-dimensional networks of SbO in which corners and edges are shared with K" ions located in tunnels through the network (23). Simple species such as SbO and Sb20 2, analogous to orthophosphate and pyrophosphate, apparendy do not exist. 

CH2CN)4Yb[( J.-H)2BH]2, and (CgH N)4Yb[( J.-H)2BH4]2 have been stmcturally characterized by x-ray crystallography and shown to contain ytterbium to boron hydride Yb—H—B linkages. Thermal decomposition of lanthanaboranes can be used to generate lanthanide metal borides. 

Returning briefly to CO2 as a ligand in addition to the various mono-C02 complexes referred to above, several bis(rj -CO2) transition-metal adducts are known, e.g. /ran -[Mo( ) -C02)2(PMe3)4] (5) and trans.mer-[Mo( 2-C02)2(PMc3)3(CNPr )].< 22 The first homo-bimetallic bridging-C02 complex has also been structurally characterized by X-ray analysis, viz. [(dppp)(CO)2Re(/x, j 0,0 j C)Re(CO)3(dppp)] (6) [dppp = l,3-bis(diphenyl-phosphino)propanc]. 0 3)... 

IF7 has been shown to act as a weak Lewis acid towards CsF and NOF, and the compounds CsIFg and NOIFg have been characterized by X-ray powder patterns and by Raman spectroscopy they are believed to contain the IFg anion. 

The first (white) product has been characterized by X-ray diffraction at —55° and features a linear F-Xe-N group and a planar N atom (Fig. 18.4). " ° On the basis of Raman and F nmr data, the cation of the final (pale yellow) product is believed to be essentially like the V-shaped [Xe2F3]+ cation but with the 2 terminal F atoms replaced by... 

Several chiral BOX-copper(II) catalysts 27a-c, 28a,b [31h, 38] and chiral BOX-copper(II) substrate/hydrolyzed enone complexes 29a,b [31f 39] have been characterized by X-ray structure analysis (Scheme 4.24). 

This is paramagnetic (one unpaired electron fj, = 1.77 /xB). A similar benzoate [Ru30(0C0Ph)6py3]PF6 has been characterized by X-ray diffraction (the central Ru-O distance is short, at 1.935 A). The structure of [Ru30(0Ac)6(H20)3]C104 is similar [103],... 

Two forms of the methyl complex have been characterized by X-ray diffraction the Rh-C distances differ slightly at 1.97 and 2.01 A, though the sp coordination geometry is the same. 

As well as the neutral compounds, also cationic complexes are available from chlorosilyl compounds by chloride abstraction. One example 12 has been characterized by x-ray structure analysis (Fig. 2). 

A structurally characterized gold complex with a C5HPh4 ligand Au(r C5HPh4)(PPh3) (46a) was reported [66], An unusual trinuclear cluster 46b derived therefrom was also characterized by X-ray structural analysis. 

A certain jr-facial selectivity was achieved when MCpCl2 (M = Ti, Zr) fragments were coordinated to the optically active fused cyclopentadienyl ligands. For instance, reaction of ZrCpCl3 with the lithium derivative of 126 at —78 °C gave predominantly 133 which was characterized by X-ray structural analysis [152]. 

The second complex has been characterized by X-ray crystallography223. The ruthenium(II) atom is coordinated to three Me2SO molecules via the oxygen atom and to three via the sulphur atom to give the irregular octahedral geometry as shown in Scheme 18. 

In contrast, the same substrate (76) gave only the monomeric palladium complex (78), characterized by X-ray analysis and spectra [MePdBr(OPPhMe2)2, THF, 20°C >95%]. ... 

Complexation via amidinate units was found in ruthenium complexes containing tri- and pentacyclic trifluoromethylaryl-substituted quinoxalines. The complex fragment [(tbbpy)2Ru] (tbbpy = bis(4,4 -di-ferf-butyl-2,2 -bipyridine) has been employed in these compounds which have all been structurally characterized by X-ray diffraction. ... 

---