I. A. Baidina

γ-Halogenated iridium(III) acetylacetonates

Abstract γ-Halogenated iridium(III) acetylacetonates of the general formula Ir(acacX) n (acac) 3− n (where acacX is CH 3 –CO–CX–CO–CH 3 , acac is CH 3 –CO–CH–CO–CH 3 , n =1,2,3, X=F, Cl, Br, I) have been synthesized, purified and characterized. Spectroscopic and thermogravimetric studies have been carried out, as well as study of the relative volatility and thermal stability of the complexes. For a series of compounds, X-ray diffraction studies have been conducted and crystallographic characteristics have been obtained. The structures of Ir(acac) 3 , Ir(acacCl) 3 , Ir(acacBr) 3 , and Ir(acacI) 3 complexes have been determined.

Study of nitrosation of hexaammineruthenium(II): Crystal structure of trans-[RuNO(NH3)4Cl]Cl2

The nitrosation of [Ru(NH3)6]2+ in hydrochloric acid and alkaline ammonia media has been studied; the patterns of interconversion of ruthenium complexes in reaction solutions have been proposed. In both cases, nitrogen(II) oxide acts as the nitrosation agent. The procedure for the synthesis of [Ru(NO)(NH3)5]Cl3 · H2O (yield 75–80%), the main nitrosation product of [Ru(NH3)6]2+, has been optimized. Thermolysis of [Ru(NO)(NH3)5]Cl3 · H2O in a helium atmosphere has been studied; the intermediates have been identified. One of these products is polyamidodichloronitrosoruthenium(II) whose subsequent decomposition gives an equimolar mixture of ruthenium metal and dioxide. The structure of trans-[RuNO(NH3)4Cl]Cl2, formed in the second stage of thermolysis and as a by-product in the nitrosation of [Ru(NH3)6]Cl2, has been determined by X-ray diffraction.

Saturated Vapor Pressure and Crystal Structure of Bis-(2-imino-4-pentanonato)copper(II)

A comprehensive study of copper(II) bis-ketoiminate including tensimetric analysis of sublimation and structure solution has been carried out. The temperature dependence of saturated vapor pressure over Cu(ki)2 crystals derived by the flow method is expressed by the equation lnP(atm)} = 25.31-13750/T, ΔHsubl = -114.2 ± 1.3 kJ· mole-1,Δ Ssubl =210.2 ± 3.0> J· mole-1 · K-1. Crystal data for CuO2N2C10H16: a=15.143(3), b=16.681(8), c=13.795(32) Å, space group Ccca, Z=12, dcalc = 1.47 g/cm3, R=0.029. The structure is molecular and consists of crystallographically independent Cu(ki)2 complexes of two types, one with a cis structure and the other with a cis–trans disordering. The copper atom has a plane square environment of two oxygen and two nitrogen atoms. In the cis isomer, Cu–O 1.938 and Cu–N 1.895 Å; in the disordered complex, all four Cu–O(N) distances are 1.901 Å.

Synthesis, crystal structure, and thermal properties of [Pd(NH3)4][AuCl4]2

AbstractThe double complex salt [Pd(NH3)4][AuCl4]2 was synthesized and studied by X-ray diffraction: a = 7.5234(6) Å, b = 7.7909(5) Å, c = 8.0247(6) Å, α = 108.483(2)°, β = 106.497(2)°, γ = 99.972(3)°, V = 409.43(5) Å3, space group P % MathType!MTEF!2!1!+-% feaafiart1ev1aaatCvAUfeBSjuyZL2yd9gzLbvyNv2CaerbuLwBLn% hiov2DGi1BTfMBaeXatLxBI9gBaerbd9wDYLwzYbItLDharqqtubsr% 4rNCHbGeaGqiVy0df9qqqrpepC0xbbL8F4rqqrFfpeea0xe9Lq-Jc9% vqaqpepm0xbba9pwe9Q8fs0-yqaqpepae9pg0FirpepeKkFr0xfr-x% fr-xb9adbaqaaeGaciGaaiaabeqaamaabaabaaGcbaWaa0aaaeaaca% aIXaaaaaaa!361B!

Speciation of platinum(IV) in nitric acid solutions.

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Reaction of trans-[RuNO(NH3)4(OH)]Cl2 with nitric acid and synthesis of ammine(nitrato)nitrosoruthenium complexes

, Z = 1, ρcalod = 3.456 g/cm3, R = 0.0267. The compound was characterized by powder X-ray diffraction, thermal analysis, and IR and Raman spectroscopy. The metal products of thermolysis of the complex were studied by powder X-ray diffraction.

Complex salts [Pd(NH3)4](ReO4)2 and [Pd(NH3)4](MnO4)2: Synthesis, structure, and thermal properties

Abstract The reaction between [RuNO(NH 3 ) 4 OH]Cl 2 and an excess of 2 M H 2 SO 4 leads to the protonation of the starting complex and crystallisation of the title complex with sulphate and hydrosulphate anions. The crystal structure of the product has been determined. The linear nitroso group and water molecule are coordinated in trans positions.

Syntheses of [Rh(NH3)5Cl][MCl6] (M = Re, Os, Ir) and Investigation of Their Thermolysis Products. Crystal Structure of [Rh(NH3)5Cl][OsCl6]

The speciation of platinum(IV) ions in nitric acid (6-15.8 M) solutions of H2[Pt(OH)6] has been studied by (195)Pt NMR and Raman spectroscopy. Series of aqua-hydroxo-nitrato complexes [Pt(L)(x)(NO3)(6-x)] (L = H2O or OH(-); x = 0, ..., 6) were found to exist in such solutions. The pair additivity model of chemical shifts and statistical theory were used to assign signals in NMR spectra to particular [Pt(L)(x)(NO3)(6-x)] species. Mononuclear hexanitratoplatinates(IV) have been isolated in solid state in substantial yield as pyridinium salt (PyH)2[Pt(NO3)6] and characterized by single-crystal X-ray diffraction. Aging of the platinum nitric acid solutions for more than 5-6 h results in oligomerization of [Pt(L)(x)(NO3)(6-x)] species and the formation of oligonuclear aqua-hydroxo-nitrato complexes with OH(-) and NO3(-) bridging ligands. Oligomeric platinum(IV) complexes with two and four nuclei were unambiguously detected by NMR on (195)Pt -enriched samples. Oligomers with even higher nuclearity were also detected. Dimeric anions [Pt2(μ-OH)2(NO3)8](2-) have been isolated as single crystals of tetramethylammonium salt and characterized by X-ray diffraction.