Synthesis,spectral characterization and antibacterial activity of O,O’-dialkyl and alkylene dithiophosphatogold (III)dichloride; crystal structure of [S2POCMe2CMe2O]AuCl2

Abstract

O, O’-Dialkyl and alkylene dithiophosphatogold (III)dichloride complexes of the type [(RO)₂PS₂]AuCl₂ and [S₂POGO]AuCl₂, where R?=?Et, nPr, iPr, iBu, Ph, cyclohexyl and cyclopentyl, where G?=?CMe₂CMe₂-, have been synthesized in 80-90% yields by reaction of the corresponding acid or sodium salts of the appropriate dithiophosphoric acids in 1:1 ratio with gold (III) chloride in dry dichloromethane at room temperature. The compounds have been characterized by elemental analyses, IR and (¹H, ^l3C, and ³¹P) NMR. The crystal structure of [S₂POCMe₂CMe₂O]AuCl₂, was determined. These new complexes have shown their growth inhibiting potential against various bacterial strains with moderate to good activity.     

X-ray crystal structure of [VO(DPA)(H2O)2]·2H2O (DPA=Dipicolinate dianion)

The X-ray crystal structure of the trans-diaqua complex [VO(DPA)(H2O2)]·2H2O (1) (DPA=dipicolinate dianion) has been determined. Comparison with the known structure of [VO(DPA)(o-phen)]·3H2O (2), obtained from (1) by displacement of the two coordinated aqua molecules, shows that the coordination sphere around vanadium is reorganised during this reaction.     

Synthesis,characterization and crystal structure of a 1D heteropolytungstate [4,4′-bipyH2]2[4,4′-bipyH][PCoW11O39]·H2O

A chain-like structure compound [4,4′-bipyH₂]₂[4,4′-bipyH][PCoW₁₁O₃₉]?·?H₂O, in which lacunary polyoxoanions are joined by a Co–O–W bridge, was prepared through the hydrothermal method and characterized by IR, and X-ray crystallography. The title compound crystallizes in a monoclinic lattice, P2₁/n space group, with a?=?13.643 (3), b?=?27.052(5), c?=?15.180(3)?Å, β?=?100.63(3)°, V?=?5506.2(19)?ų, Z?=?4, R ₁?=?0.0792, wR ₂?=?0.1532. Cobalt-substituted Keggin-type subunits are connected via Co–O–W bridges to form a 1D, chainlike, polymolecular Keggin POM. TG-DTA analysis indicates the title compound decomposes at 553°C.     

Hydrothermal synthesis of a mixed-valence hexamolybdate cluster: crystal structure of [HN(CH2CH2)3N]2[HMoVMoVI5O19]·[N(CH2CH2)3N]

The hydrothermal reaction of MoO₃, V, Na₂WO₄· 2H₂O, [N(CH₂CH₂)₃N](1,4-diazabicyclo[2.2.2] octane), and H₂O at 160°C for 90h gave dark-brown crystals of [HN(CH₂CH₂)₃N]₂[HMo^VMo^VI ₅O¹⁹]·[N(CH₂CH₂)₃N], (1), in 40% yield. Complex (1) is the first one-electron reduced mixed-valence hexamolybdate to be crystallized and structurally characterized. The crystal structure of (1) consists of discrete [HMo^VMo^VI ₅O₁₉]^2– anions, [HN-(CH₂CH₂)₃N]⁺ cations, and neutral [N(CH₂CH₂)₃N] molecules of crystallization.     

Synthesis and crystal structure of the coordination polymer of silver with 4,4′-bipyridylethylene [Ag(Bpe)](NO3)·3H2O

The compound [Ag(Bpe)](NO₃)·3H₂O (Bpe = 4,4′-bipyridylethylene, C₁₂H₁₀N₂) is prepared and its crystal structure is determined. The crystals are triclinic: a = 9.073(2) Å, b = 10.074(2) Å, c = 10.391(2) Å, α = 61.18(3)°, β = 72.11(3)°, γ = 68.62(3)°, space group P $\bar 1$ , V = 764.7(3) ų, ρ(calcd) = 1.764 g/cm³, Z = 2. The structure is composed of polymeric cationic chains, [Ag(Bpe)] _∞ ⁺ , NO ₃ ^? counterions, and water molecules. The Ag⁺ ions are bound to the two N atoms of two crystallographically nonequivalent Bpe ligands and form a nearly linear coordination (Ag(1)-N(1), 2.129 Å; Ag(1)-N(2), 2.120(4) Å; N(1)Ag(1)N(2), 169.9(2)°).     

Synthesis and Crystal Structure of K3[HO{VO(O2)2}2]·H2O

The title compound K3[HO{VO(O2)2}2]·H2O has been synthesized and its crystal structure was determined by X-ray diffraction method. The crystal is of monoclinic, space group P21/c with a = 6.7078(3), b = 9.9539(6), c = 15.8182(9)A, β = 93.702(3)0, V = 1053.96(10)A3, Mr = 414.20, Dc = 2.610 g/cm3, Z = 4, λ(MoKα) = 0.71073A, F(000) = 808, μ = 3.014 mm-1, the final R = 0.0173 and wR = 0.0466 for 2178 observed reflections with I > 2σ(I). X-ray diffraction reveals that the coordination polyhedra of V atoms are not chemically equivalent: the V(1) and V(2) polyhedra can be described as pentagonal pyramid and pentagonal bipyramid, respectively.     

{Cu[H2NC(CH2OH)3]2}{Pic}2·2H2O的合成与晶体结构

三羟甲基氨基甲烷与苦味酸Pic铜在乙醇水混合液中反应,制得少见的不对称氢键连接的超分子化合物{Cu[H2NC(CH2OH)3]2}{Pic}2·2H2O.晶体属三斜晶系,空间群为P ī,晶胞参数为a = 6.894(1),b = 8.219(1),c = 13.543(3) ', α = 79.290(1),β = 8 3.36(2), γ = 84.590(1)°,化学式为C20H30CuN8O22,V = 746.9(2) '3,Z = 1,Dc = 1.774 g/cm3,F000 = 411,μ = 0.844 mm-1,R = 0.0334,Rw = 0.0863.在配合物的结构单元中, Cu2+位于对称中心,分别与2个四齿配体三羟甲基氨基甲烷中的2个-OH,1个-NH2,三齿配位,呈笼状螯合.而另一个-OH,因配体和中心离子构型的限制,不参与配位.     

X-ray crystal structure and properties of the [Mo(CN)2O(acetam)] · 2.5H2O complex

The X-ray crystal structure and properties of the [Mo(CN)₂O(acetam)] · 2.5H₂O {acetam = N-[1-(pyridin-2-yl)-ethylidene]diethanetriamine} complex are described. The complex was prepared by the in situ reaction of [Mo(CN)₄O(H₂O)]^2–, 2-acetylpyridine and diethylenetriamine in aqueous solution. The complex is seven coordinated. The Mo atom having a distorted pentagonal bipyramid arrangement with a tetradentate 'half-unit' Schiff base and oxygen ligand in a plane. The properties of the salt, i.r., u.v.–vis. spectra and cyclic voltammetry measurements are described and compared with those of [Mo(CN)₂O(diaceen)] · H₂O {diaceen = N,N-bis[1-(pyridin-2-yl)ethylidene]ethane-1,2-diamine) having the same coordination number for the metal.     

Synthesis, crystal structure, and thermal analysis of hexahydrogen dodecavanadate of composition [NH3 · H2O]6 · H6[Ca4V12O40] · 6H2O

Dihydrogen dodecavanadate of composition [NH₃ · H₂O]₆ · H₆[Ca₄V₁₂O₄₀] · 6H₂O was synthe-sized and studied by X-ray crystallography and TGA analyses. The crystals are cubic, space group I $\bar 4$ 3m;; unit cell parameters: a = 13.518(2) ?, V = 2470.4(3) ?³, ??_calc = 2.2334 g/cm³, Z = 2.     

Crystal structure of a novel complex [Co(3,3′-bpbc)(H2O)3]·H2O

A novel coordination polymer constructed with [Co(3,3′-bpbc)(H₂O)₃]·H₂O(I) (3,3′-bpbc = 2,2′-bipyridine-3,3′-dicarboxylic acid) is successfully synthesized at room temperature and characterized by elemental analysis and IR spectra. The crystal structure of the complex is determined by single crystal X-ray diffraction. The unit cell parameters for complex I are: a = 9.9606(11) Å, b = 9.2552(10) Å, c = 16.0258(17) Å, β = 96.731(0)°, V = 1467.2(3) ų, Z = 4, space group P2(1)/n. In the crystal, the cobalt(II) ion adopts a hexa-coordinate environment, and the structure units aggregate together to give birth to infinite 1D chains. The 2D and 3D framework is constructed via intermolecular hydrogen bonds.     

Synthesis,crystal structure modeling and thermal decomposition of yttrium propionate [Y2(CH3CH2COO)6·H2O]·3.5H2O

An yttrium propionate complex was synthesized and characterized for its application as precursor for Y₂O₃ based oxide thin films deposition and YBa₂Cu₃O_7 − x superconducting thin films. The TG–DTA and FT-IR analyses have revealed the formation of an yttrium propionate complex with the formula [Y₂(CH₃CH₂COO)₆·H₂O]·3.5H₂O. The molecular structure of the yttrium propionate complex was determined by modeling the FT-IR spectra. The coordination numbers for the yttrium ions are eight and nine, respectively being coordinated by bridging bimetallic triconnective and chelating bidentate propionate groups.The thermal decomposition of yttrium propionate has been investigated by thermogravimetric (TG) and differential thermal analysis (DTA) coupled with quadrupole mass spectrometry (QMS), X-ray diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques.     

Synthesis and structure of [Re3S3.7Br4.3(PPh3)3]·0.5CH2Cl2

One of the products of the reaction between Re₃S₇Br₇ and PPh₃ has been isolated in crystalline state and characterized by single crystal X-ray diffraction (XRD), mass-spectrometry, and EPR spectroscopy. The crystalline phase obtained is a co-crystallization product of two cluster complexes: [Re₃(μ₃-S)₂(μ-S)₂(μ-Br)Br₃(PPh₃)₃] (1a) an [Re₃(μ₃-S)₂(μ-S)(μ-Br)₂Br₃(PPh₃)₃] (1b). The ratio 1a:1b in the investigated single crystal sample is ～7:3.     

Synthesis,Molecular Structure,and Thermal Properties of the Supramolecular Complex [Zn{NH(CH2)4O}{S2CN(C2H5)2}2]2 · CH2N(CH2)4O}2

The supramolecular complex [Zn{NH(CH₂)₄O}{S₂CN(C₂H₅)₂}₂]₂ · CH₂N(CH₂)₄O}₂ (I) has been synthesized and studied by X-ray crystallography and thermal analysis. The noncentrosymmetric complex is composed of two structurally nonequivalent molecules of the adduct of bis(diethyldithiocarbamato)zinc with morpholine, which are linked with the outer-sphere N,N’-dimorpholinomethane molecule through two hydrogen bonds N-H?O. The major differences between the adduct molecules are related to the strength of Zn-N bonds, spatial orientation of the coordinated morpholine heterocyclic rings, and the proportion between the contributions of the trigonal bipyramidal (TBP) and tetragonal pyramidal (TP) components to the geometry of zinc polyhedra. Calculations show that the geometry of the zinc polyhedra is almost halfway between TBP and TP. The thermal destruction of supramolecular compound I is accompanied by desorption of the outer-sphere and coordinated organic molecules. At the final stage, defragmentation of the “dithiocarbamate part” of the complex leads to the formation of ZnS.     

Synthesis and crystal structure of Cs7[BW12O40][Rh2(CH3COO)4Cl]2 · 8H2O

The binary salt Cs₇[BW₁₂O₄₀][Rh₂(CH₃COO)₄Cl]₂ · 8H₂O was obtained by heating of K₈[HBW₁₁O₃₉] · 13H₂O with [Rh₂(CH₃COO)₄(H₂O)₂] in water followed by crystallization in the presence of CsCl. The crystal structure of the salt was determined by X-ray diffraction. Its ionic structure consists of the Cs⁺ cations, the Keggin-type heteropoly anions [BW₁₂O₄₀]^5?, and the polymeric chain anions catena-[Rh₂(CH₃COO)₄Cl] _n ^n? .     

The crystal structure of tetraphenylphosphonium pentacyanonitridorhenate(V), (PPh4)3[ReN(CN)5]·7H2O

Summary The crystal structure of (PPh₄)₃[ReN(CN)₅]·7H₂O has been determined from three dimensional X-ray diffraction data. The orange crystals are triclinic, space group , with cell dimensions a=12.514(3), b=15.8514), c=19.030(3) Å, =77.62(2), =84.61(1) and =74.03(2)^o, z=2, D_obsd=1.40(1) g cm^–3 and D_calc=1.37(1) g cm^–3. The anisotropic refinement of 5861 observed reflections converged to R=0.049.The [ReN(CN)₅]^3– ion has a distorted octahedral geometry. Bond distances: ReN=1.68(1), Re–C_av (planar)=2.12(1), Re–C (axial)=2.39(1) Å. The Re atom is displaced by 0.31 Å out of the plane formed by the four carbon atoms towards the nitrido ligand.