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Reactions of [Ge(OPri)4] with internally functionalised oximes in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded complexes of the type [Ge(OPri)4-n{ONC(CH3)C4H3O-2}n] (1, 2); [Ge(OPri)4-n{ONC(CH3)C4H3S-2}n] (3, 4); [Ge(OPri)4-n{ONC(CH3)C5H4N-2}n] (5, 6); [Ge(OPri)4-n{ONC(H)C4H3O-2}n] (7, 8); [Ge(OPri)4-n{ONC(H)C4H3S-2}n] (9, 10); [Ge(OPri)4-n{ONC(H)C5H4N-2}n] (11, 12)(where n= 1 or 2), All the above monomeric complexes are soluble in organic solvents and have been characterised by elemental analyses and spectroscopy. Thermal and hydrolytic studies of complexes 2, 4and 8suggest them to be potential molecular precursors for the synthesis of pure GeO2at low temperatures by the sol-gel technique. Powder X-ray diffraction, IR spectral studies as well as SEM images of the GeO2indicate formation of pure nano-crystalline hexagonal (α-quartz) germania at 550°C.

A variety of heteroleptic complexes of the type [Sn(acac)2Cl2-n(L)n] [where L = {O(CH2)3N=C(Me)Ar} and {ON=C(R)Ar}; R = Me, H; Ar = 2–C5H4N, 2–C4H3O or 2–C4H3S; n= 1 or 2] have been synthesised in quantitative yields by the metathetical reaction of cis-[Sn(acac)2Cl2] with the sodium salt of the ligands in anhydrous methanol–benzene mixture. Corresponding bis(acetylacetonato)methyloximatotin(IV) complexes have also been prepared by a similar reaction of cis-[Sn(acac)2IMe] with the potassium salt of the oximes. Absence of any significant shift in the hetero-aryl ring carbon/proton resonances of all the derivatives of internally functionalised ligands indicates non-participation of the hetero-atom of the ring on coordination to the tin atom. Spectroscopic data suggest retention of the cis-octahedral configuation for all these derivatives. Hydrolysis of [Sn(acac)2{ON=C(Me)C4H3O}Cl], followed by sintering at 650°C yielded pure SnO2microcrystals, which were characterised by XRD and SEM analyses.

Reactions of bis(acetylacetonato)aluminum(III)‐di‐μ‐isopropoxo‐di‐isopropoxo aluminum(III), [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(OPri)2] with aminoalcohols, (HORNR1R2) in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded binuclear complexes of the types [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(ORNR1R2)(OPri)] and [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(ORNR1R2)2] (R  (CH2)3, R1= R2= H; R = CH2C(CH3)2, R1= R2= H; R = (CH2)2, R1= H, R2= CH3; and R  (CH2)2, R1= R2= CH3), respectively. All these compounds are soluble in common organic solvents and exhibit sharp melting points. Molecular weight determinations reveal their binuclear nature in refluxing benzene. Plausible structures have been proposed on the basis of elemental analysis, molecular weight measurements, IR, NMR (1H, 13C, and 27Al), and FAB mass spectral studies. 27Al NMR spectra show the presence of both five‐ and six‐coordinated aluminum sites. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:518–522, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10184

Reactions of bis(acetylacetonato)aluminum(III)-di-μ-isopropoxo-di-isopropoxo aluminum(III), [(CH3COCHCOCH3)2Al(μ-OPrⁱ)2Al(OPrⁱ)2] with aminoalcohols, (HO&bond;R&bond;NR¹R²) in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded binuclear complexes of the types [(CH3COCHCOCH3)2Al(μ-OPrⁱ)2Al(O&bond;R&bond;NR¹R²)(OPrⁱ)] and [(CH3COCHCOCH3)2Al(μ-OPrⁱ)2Al(O&bond;R&bond;NR¹R²)2] (R &dbond; &bond;(CH2)3&bond;, R¹ = R² = H; R = &bond;CH2C(CH3)2&bond;, R¹ = R² = H; R = &bond;(CH2)2&bond;, R¹ = H, R² = &bond;CH3; and R &dbond; &bond;(CH2)2&bond;, R¹ = R² = CH3), respectively. All these compounds are soluble in common organic solvents and exhibit sharp melting points. Molecular weight determinations reveal their binuclear nature in refluxing benzene. Plausible structures have been proposed on the basis of elemental analysis, molecular weight measurements, IR, NMR (¹H, ¹³C, and ²⁷Al), and FAB mass spectral studies. ²⁷Al NMR spectra show the presence of both five- and six-coordinated aluminum sites. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:518–522, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10184

Reactions of bis(β-diketonato)aluminium(III)-di-μ-isopropoxo-di-isopropoxoaluminium(III), [(CH3COCHCOR)2Al-(μ-OPr-i)2Al(OPr-i)2] with 2-pyridylmethanol, (C5H4N-2-CH2OH) in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene resulted in the synthesis of [(CH3COCHCOR)2Al(μ-OPr-i)2Al(OCH2-2-C5H4N)(OPr-i)] [where R=CH3 (1), -OC2-H5 (3), and -C6H5 (5)] and [(CH3COCHCOR)2Al(μ-OPr-i)2Al(OCH2-2-C5H4N)2] [where R=CH3 (2), -OC2H5 (4), and -C6H5 (6)], respectively. All of these compounds are sharp melting solids and are soluble in a variety of organic solvents (e.g., benzene, chloroform and dimethyl sulfoxide) except [(CH3COCHCOOC2H5)2Al(μ-OPr-i)2Al(OCH2-2-C5H4N)2], which is insoluble in benzene but soluble in chloroform and dimethylsulfoxide. All of these derivatives show a dinuclear structure in benzene. All of the above derivatives have been characterized by elemental analyses, molecular weight determinations, IR and NMR (1H, 13C and 27Al) and FAB mass spectral studies.

The crystal structure of the title compound PhAs(S2COPri)2 has been determined by single crystal X-ray diffraction and refined by full matrix least squares analysis with anisotropic temperature factors. The crystal is monoclinic, space groupP21/c,a=8.889(6),b=16.174(19),c=13.506(14) Å,ß=102.02(7)°,V=1899.2 Å3,Z=4,Dc=1.478 g cm-3, monochromated Mo-Ka radiation, ?=0.71069 Å,µ=22.07 cm-1.

The title compound is triclinic, space group P¯1,a=10.670(5)b=13.053(3),c=8.944(5) Å,a=100.18(3),ß=92.16(4),?=80.88(3)°,Z=1,V=1210.4 Å3, andR=0.043 for 2579 reflections. The molecule has two distorted octahedra sharing a corner occupied by an oxygen (bridging) atom, the Mo-Ob-Mo angle being 180°. The two molybdenum-oxygen bond lengths Mo-Ob (bridging) and Mo-O1, (terminal) are 1.92 and 1.62 Å, respectively. Except the Mo-S bondtrans to the terminal oxygen atom which has a bond length 2.81 Å, all other Mo-S bonds have an average length of 2.50 Å.

Bismuth tris(2,2-diethyltrimethylene dithiophosphate), [image omitted] M = 884.8, monoclinic, P2,/c, a = 9.591(3), b = 10.059(1), c = 36.170(5) Å, β = 90.51(2)°, V = 3489.5 Å3, Z = 4, Dc = 1.68 g cm-3, (MoKα) = 0.71069 Å, μ = 55.5 cm-1, F(000) = 880, T = 295 K. Final R = 0.122 for 3183 reflections. The coordination geometry around bismuth is slightly distorted octahedral with three short and three long Bi-S bonds (average lengths, 2.74 and 2.85 Å, respectively); 1,3,2Dioxaphosphorinane rings are present in chair form.Preliminary data have also been obtained for bismuth tris(2,3-butylene dithiophosphate), [image omitted] M = 758.6, monoclinic, C2/c, a = 16.684(8), b = 13.682(6), c = 11.930(6) Å, β = 98.45(2), V = 2693.8 Å3, Z = 4, T = 295 K, Dc = 1.87 g cm-3,μ = 69.1 cm-1 and R = 0.052 for 1073 reflections. The chelation is symmetrical in this compound with Bi-S bond lengths of 2.76 and 2.79 Å.

Tris-derivatives of Sb(III) with nine 1,3-diketones have been synthesized and characterized by elemental analysis and spectral studies. In these monomeric compounds the usual mode of bonding, i.e., through carbonyl oxygens, has been observed in which the antimony atom attains a coordination number six. Attempts have also been made to elucidate with the help of IR and PMR data the effect of different substituents at 1 and 3 positions on the chelating ability of the ring. A cis configuration has been proposed for the tris-complexes containing unsymmetrical ligands.

The reaction of ClSO2N = PPh2Cl () with NH3 yields H2NSO2N = PPh2NH2 (2).This compound is converted to Me3Si(H)NSO2N = PPh2N(H)SiMe3 (3) by Me3SiNMe2. 3reacts with WOCl4 under elimination of (Me3Si)2O and ClSO2NH2 to yield the eight-membered ring system (Cl3WNPPh2N)2 (4).The molecular structure of 4was investigated by an X-ray structure analysis.

Reaction of Sb(OPri)3 and HOC(Me)2C(Me)2OH in 1:2 molar ratio yields [image omitted]. Further reaction of (1) with alkali metal methoxides in 1:1 molar ratio in methanol yields bimetallic heterocycles, [image omitted] where (M = Li, Na or K). Reaction of [image omitted] with NiCl2.MeOH in 1:1 and 2:1 molar ratio in methanol forms [image omitted] and [image omitted]. These moisture sensitive, monomelic derivatives are solids and are soluble in DMSO, DMF, MeOH and CHC13. Conductivity measurements as well as IR and NMR (1H and 13C) spectral studies indicate terra-coordination around antimony in these complexes.

Reactions of triethoxyarsine and stibine with phenyl-and γ-naphthylisocyanates were carried out to study the cleavage of As-O and Sb-O bonds. The products were characterised by i. r. and elemental analysis.

A few bimetallic alkoxides of the types [MSn(OR)3], [Sb(Sn(OR)3)3] and [Pb(Sb(OR)4)2] [M = Na, K, R = CH3, C2H7, n and i-C3H7, n and i-C4H9 and i-C5H11] have been prepared and characterized. These are generally coloured solids or viscous liquids. These are monomeric and covalent in nature and are hydrolytically unstable to atmospheric moisture. IR, 1H and 13C and 119Sn NMR studies suggest 3-coordination around tin in these derivatives.

2-Iminoxy and 2-diethylaminoxy-1,3,2-dioxaarsacyclo-pentanes and-cyclohexanes have been synthesised by several routes as volatile liquids. Attempts have been made to throw light on the structures of these derivatives by studies of i. r. and p. m.r. spectra, refractive indices and molecular weights.

Twelve new octahedral complexes of the type Ph3Sb(Cl)(OC6H4CR=NR') (where R = H and R' = Me, Et, Pr, Bu, Ph and p-tolyl; R = Me and R' = Me, Bu and Bu') and Ph3Sb(OMe)-(OC6H4CR=NR')(R = H and R' = Me; R = R' = Me) have been synthesized and characterized after purification by recrystallization. The results of the i.r. and 1H n.m.r. spectra of these complexes suggest coordination of azomethine nitrogen to the antimony atom.

Centring of a lens or mirror is a very important operation. Generally centring of a lens is done by reflection or refraction method seeing the image stationary in both the cases. Centring & edging of large size lenses and mirrors are done using large milling machines. Suitable arrangements are made on the milling machine to see the reflected image. Using such machines & suitable arrangements, large size lenses and mirrors are centered and edged. This method is difficult as well as time consuming. A simple and quick method has been devised for the centring & edging of large size lenses/mirrors. In the suggested method the extent of the amount of off-centring in lens/mirror is worked out taking into consideration the actual radius of curvature and edge thickness on the centring cup so that edge thickness of the finished component comes equal all around. Lens/mirror is made off-centered on the cup by the calculated value using dial indicator. Then edging is carried out. Using the suggested method, edge thickness of 315 mm diameter polished lenses were made equal all around to .001 mm. Components are being used in one of the telescope.

X‐ray structure analysis of the synthesized title compound (III) (space group P1, Z=4) confirms intermolecular hydrogen bridges between its molecules resulting in a distorted trigonal‐bipyramidal coordination.

The alkoxides (IV), (VI), and (VIII) mentioned in the title are prepared by consecutive treatment of tin dichloride (I) with potassium (II) in the alcohols (III), antimony trichloride (V), and lead dichloride (VII) via transmetalation steps.