Synthesis and structure of the dimeric organo-antimony (V) imido complex [Ph3Sb(μ-NCH2CH2Ph)]2

The amine PhCH₂CH₂NH₂ undergoes dimetallation by [Ph₃Sb(NMe₂)₂] (1) under mild conditions to give the first structurally authenticated example of an organo-Sb(V) imido complex, [Ph₃Sb(μ-NCH₂CH₂Ph)]₂ (2).     

Synthesis and X-ray crystal structure of a novel organometallic (μ3-oxido)(μ3-imido) trinuclear iridium complex

Reaction of the organometallic aqua ion [Cp*Ir(H(2)O)(3)](2+) with tert-butyl(trimethylsilyl)amine in acetone yielded a novel trinuclear (μ(3)-oxido)(μ(3)-imido)pentamethylcyclopentadienyliridium(III) complex, [(Cp*Ir)(3)(O)(N(t)Bu)](2+). Single crystal structure analyses show the complex can be isolated both in the double salt ((t)BuNH(3))[(Cp*Ir)(3)(O)(N(t)Bu)](CF(3)SO(3))(3) (1) and in the simple triflate [(Cp*Ir)(3)(O)(N(t)Bu)](CF(3)SO(3))(2) (2). The double salt is stabilized by hydrogen bonding between the tert-butylammonium ion and the three triflate anions. It is the first time that a trinuclear (μ(3)-oxido)(μ(3)-imido) transition metal complex has been structurally characterized.     

Synthesis and Crystal Structure of a Novel Mercapto-organotin Complex: [Et_3NH] [Ph_2SnCl(μ~2-SCH_2COO~-)]

Diorganotinmercaptoacetates,generallyusedforPVCstabilizer',havebeensynthesizedbythereactionofdiorganotindichloridesandmercaptoaceticacidinthepresenceofanorganicbase,butthereactionsbetweentriorganotinchloridesandmercaptoaceticacidhavebeenlittlestudied.Inthispaper,wereportanewdephenylationreactionandcrystalstructureofanunexpectedcomplex[Et3NH][Ph,SnCI(rf-SCHZCOO-)].WehaveexpectedtosynthesizePh3SnSCHZCOOSnph3bythereactionofPh3SnCIandHSCHZCOOHin2:lmolarratiointhepresenceoforganicba…     

Synthesis and crystal structure of a novel two-dimensional network complex [Mn(O_2CCH_2Cl)_2(phen)]_n

A novel two-dimensional network manganese(Ⅱ) polymer complex [Mn(O2CCH2CI)2-(phen)]n has been synthesized and characterized by elemental analysis and IR spectrum. The crystal structure of title complex has also been determined, which is in monoclinic of a space group P21/c with the following unit cell parameters at 294K: a =1.9738(4) nm, b =1.1384(2) nm, c =0.74915(14) nm, V=1.6795(5) nm3, Z= 2.     

Synthesis and molecular structure of the complex [Ph3Sb(NO3)]2O·Me2CO

The reaction of silver nitrate with Ph₃-SbBr₂ in an ethanol-acetone solution afforded the complex [Ph₃Sb(NO₃)]₂O·Me₂C=O (1). According to the data of X-ray diffraction study of crystals of1, molecule1 contains a nonlinear O-bridge, which links two Sb atoms. The Sb atoms have a trigonal-bipyramidal configuration. The NO₃ group and the bridging oxygen atom are in axial positions and the three Ph substituents are in equatorial positions. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 1, pp. 174–176, January, 1999.     

Synthesis and crystal structure of a trinuclear titanium(IV) β -diketonate complex with a six-membered [Ti–(μ-O)]3 ring

The trinuclear titanium(IV) β-diketonate complex, [Ti₃(μ-O)₃(dppd)₆]?·?(DMF)(0.5EtOH) (1) (H-dppd?=?1,3-diphenylpropane-1,3-dione) has been synthesized and its crystal structure and spectroscopic properties have been studied. Complex 1 crystallizes in monoclinic system with space group C2/c and a?=?20.954(5)?Å, b?=?18.705(4)?Å, c?=?24.617(6)?Å, β?=?111.957(4)°, Z?=?4. The complex consists of a six-membered [Ti–(μ-O)]₃ ring, of which three titanium(IV) ions are linked together by bridging oxygen atoms. Each titanium(IV) possesses an octahedral geometry, with four oxygen atoms from the two β-diketonate ligands and two bridging oxygen atoms.     

Synthesis and crystal structure of [MoH3(CCBut)(Ph2PCH2CH2PPh2)2], a trihydrido-alkynyl complex

Reaction of Bu^tCCH with trans-[Mo(N₂)₂(dppe)₂] (dppe = Ph₂PCH₂CH₂PPh₂) gives [MoH₃(CCBu^t)(dppe)₂], whose X-ray structure is reported.     

Synthesis, properties, and crystal structure of the tin(IV) complex with N-(2-hydroxyethyl)ethylenediaminetriacetic acid [Sn(μ-Hedtra)(μ-OH)SnCl3(H2O)] · 3H2O

The binuclear tin(IV) complex with N-(2-hydroxyethyl)ethylenediamine-N,N′,N′-triacetic acid (H₄Hedtra) is synthesized. The compound is characterized by elemental analysis, thermogravimetry, and IR spectroscopy. An X-ray diffraction analysis of complex Sn(μ-Hedtra)(μ-OH)SnCl₃(H₂O)] · 3H₂O (I) is carried out. Structure I is formed by the binuclear complexes and molecules of water of crystallization. One of the tin atoms coordinates six “active” sites Hedtra^4? (the alcohol branch is deprotonated and forms a bridge between two tin atoms) and the bridging hydroxo group. The polyhedron is a pentagonal bipyramid. The octahedral environment of the second tin atom is formed by two bridging oxygen atoms, three chlorine atoms (fac isomer), and a coordination water molecule.     

Synthesis and Structure of [Pd(NH3)4][cis-Pd(NH3)2(SO3)2][Pd(NH3)3(SO3)] · H2O

A new palladium compound [Pd(NH₃)₄][cis-Pd(NH₃)₂(SO₃)₂][Pd(NH₃)₃(SO₃)] · H₂O (I) was synthesized and its structure was studied by X-ray powder diffraction method. In the course of the synthesis, the initial trans-diamminesulfite anionic complex is transformed into the cis-configuration. Further heating in aqueous solution results in isomerization of a substance into a neutral complex [Pd(NH₃)₃(SO₃)]. Crystals I are triclinic: a = 10.3297(2) Å, b = 14.1062(3) Å, c = 6.8531(1) Å, = 101.36(0)°, = 92.74(0)°, = 92.71(0)°, space group P1¯. Structure I consists of the columns with alternating cis-[Pd(NH₃)₂(SO₃)₂]^2– and [Pd(NH₃)₃(SO₃)] complexes and [Pd(NH₃)₄]²⁺ ions between the columns.     

Synthesis and structure of novel dinitrosyl iron complexes [Fe2(μ-SCH2CH2NHR)2(NO)4]

Two novel dinitrosyl iron complexes with thiolate bridging ligands [Fe₂(μ-SCH₂CH₂NHR)₂(NO)₄] (R = Ac, Boc), derived from the cysteamine complex [Fe₂(μ-SCH₂CH₂NH₃)₂(NO)₄]²⁺ are described. The complex with acylated cysteamine is characterized by X-ray diffraction analysis. The cysteamine complex is a convenient precursor for modification of the bridging ligand.     

Synthesis and crystal structure of [UO2CrO4(C5NH5COO)] · 0.25H2O

[UO₂CrO₄(C₅NH₅COO)] · 0.25H₂O crystals have been synthesized and studied by X-ray diffraction and IR spectroscopy. The compound crystallizes in monoclinic system with the unit cell parameters a = 7.2362(3) ?, b = 13.8847(6) ?, c = 10.7204(5) ?, ?? = 90.037(2)°, space group P2₁/n, Z = 4, R = 0.0236. The structure consists of [UO₂CrO₄(C₅NH₅COO)] chains, which run in the direction [100] and correspond to the AT³B⁰¹ crystallochemical formula, where A = UO ₂ ²⁺ , T³ = CrO ₄ ^2? , and B⁰¹ is nicotinic acid molecules in the form of zwitter ions. The results of analyzing nonbonded interactions in the crystal structure by the method of molecular Voronoi-Dirichlet polyhedra (MMVDP) are presented.     

Synthesis and crystal structure of a novel mixed valence tri-iron complex salt: [hexakis(thiazole)iron(II)][μ-oxo- bis(trichloroiron(III))]

The title compound, [Fe(tz)₆][Fe₂OCl₆] (1) (tz = thiazole) has been synthesized under argon by the reaction of anhydrous FeCl₃ with thiazole in ethanol. 1 crystallises in the cubic space group (no. 205) with . 1 consists of a face-centered cubic array of [Fe(tz)₆]² cations, with the oxo-bridged [Fe₂OCl₆]²⁻ anion occupying the cell and edge centres.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Synthesis of Ph2LSn(μ-OH)Bu3SnCl. Trapping of monomeric triorganotin hydroxide Ph2LSnOH

The reaction of triorganotin(IV) compound Ph₂LSnCl (1), (L = 2,6-(t-BuOCH₂)₂C₆H₃), with (Bu₃Sn)₂O resulted to the isolation of Ph₂LSn(μ-OH)Bu₃SnCl (2), in which a monomeric triorganotin(IV) hydroxide Ph₂LSnOH intermolecularly coordinates Bu₃SnCl moiety. Compound 2 was characterized by combination of ¹H, ¹³C and ¹¹⁹Sn NMR spectroscopy, ESI/MS, elemental analysis and X-ray diffraction.     

Synthesis and structure of gold complexes [Ph3PR]+[Au(CN)2I2-trans]−, R = Et,CH2Ph,Ph

Russian Chemical Bulletin - Gold complexes [Ph3PR]+[Au(CN)2I2-trans]?, where R = Et (1), CH2Ph (2), Ph (3), were synthesized by the reaction of potassium dicyanodiiodoaurate with...     

Synthesis and characterisation of novel selenium-containing clusters; crystal structures of [Ru4(μ4-Se)2(CO)8(μ-CO)3] and [Ru3(μ3-Se)2(CO)7(Ph2P(CH2)3PPh2)]

The compound [Ru₄(μ-Se)₂(CO)₈(μ3-CO)₃] (1), has been obtained in good yield by vacuum pyrolysis of [RU₃(CO)₁₂] with [Ph₂Se₂] at 185°C. Reaction of 1 with 1,3-bis(diphenylphosphino)propane at room temperature affords the novel cluster [RU₃(μ₃-Se)₂(CO)₇(Ph₂P(CH₂)₃PPh₂)] (2). The structures of 1 and 2 have been determined by an X-ray diffraction study.     

Synthesis, crystal structure, magnetic property and thermal studies of [Ni(CH(3)COO)2·(NH2CH2Ph)4

[Ni(CH(3)COO)(2)·(NH(2)CH(2)Ph)(4)] complex was synthesized using benzylamine and nickel acetate. The molecular structure of this complex was obtained by single crystal X-ray diffraction and characterized by elemental analysis, IR spectrometry and thermal analysis. The complex crystallized in the monoclinic space group P2(1)/n with cell parameters a=11.234(4)?, b=6.459(2)?, c=22.647(8)?, α=90.00, β=91.149(4)°, γ=90.00, V=1642.8(10)?(3), Z=2. The structure has been solved by direct methods and refined to R(1)=0.0876 for 6377 observed reflections I>2σ(I). Magnetic studies for complex show the data over the whole temperature range 5-300 K are well fitted to the Curie-Weiss law with C=1.03 cm(3) K mol(-1) and θ=-1.38 K. This fitting indicates antiferromagnetic interaction between the Ni ions and the metal center exhibits distorted octahedral coordination geometries. The thermal analysis was carried out to understand the thermal stability of the title complex.     

Lithium and lanthanum complexes with acenaphthylene dianion. Molecular structure of [Li(Et2O)2]2μ2:η3[Li(η3:η3-C12H8)]2 complex

The lithium complex with the acenaphthylene dianion [Li(Et₂O)₂]₂₂:³[Li(³:³-C₁₂H₈)]₂ (1) was synthesized by the reduction of acenaphthylene with lithium in diethyl ether. According to the X-ray diffraction data, compound 1 has a reverse-sandwich structure with the bridging dianion ₂:³[Li(³:³-C₁₂H₈)]₂. Two lithium atoms in complex 1 are located between two coplanar acenaphthylene ligands of the ₂:³[Li(³:³-C₁₂H₈)]₂ ^2– dianion and are ³-coordinated with the five- and six-membered rings. The lanthanum complex with the acenaphthylene dianion [LaI₂(THF)₃]₂(₂-C₁₂H₈) (2) was synthesized by the reduction of acenaphthylene in THF with the lanthanum(iii) complex [LaI₂(THF)₃]₂(₂-C₁₀H₈) containing the naphthalene dianion. The ¹H NMR spectrum of complex 2 in THF-d₈ exhibits four signals of the acenaphthylene dianion, whose strong upfield shifts compared to those of free acenaphthylene indicate the dianionic character of the ligand. The highest upfield chemical shift belongs to the proton bound to the C atom on which, according to calculation, the maximum negative charge is concentrated.     

Synthesis,crystal structure and magnetic properties of an oxamato-bridged heterobinuclear NiIICuII complex [Ni(cyclam)Cu(opba)]2·3DMSO

An oxamato-bridged heterobinuclear Ni^IICu^II complex [Ni(cyclam)Cu(opba)]₂ · 3DMSO (1) has been synthesized, characterized by elemental analysis, infrared spectra and magnetic susceptibility, where cyclam is 1, 4, 8, 11-tetraazacyclotetradecane and opba is o-phenylenebis(oxamato). The complex crystallizes in the triclinic system, space group P 1 with a = 12.006(3) Å, b = 12.783(3) Å, c = 20.977(5) Å, α = 76.634(4)°, β = 75.172(4)°, γ = 80.818(4)° and Z = 2. According to X-ray crystallographic studies, the four-coordinate copper(II) atom is a slightly distorted planar geometry and is linked to nickel(II) through the exo-cis oxygen atoms of [Cu(opba)]^2?; the six-coordinate nickel(II) center lies in a highly distorted octahedral environment. Magnetic susceptibility measurements of the complex in the temperature range 2–300 K indicate that the heterobinuclear Ni^IICu^II units are coupled antiferromagnetically with J = ?57.38 cm^?1, g _Ni = 2.25 and g _Cu = 2.02.     

Synthesis and structure of a novel bis-μ-oxo rhenium(VI) dimer: Re2O2(μ-O)2(CH2CMe2Ph)4

The complex Re(O)Cl₃(PPh₃)₂ reacts with dialkyl zinc reagents in CH₂Cl₂ to give the novel bis-μ-oxo rhenium(VI) dimer [Re(O)(μ-O)R₂]₂. The molecular structure has been determined by single-crystal X-ray diffraction methods.