On the microstructure and symmetry of apparently hexagonal BaAl2O4

The P6₃ (a=2a_p, b=2b_p, c=c_p) crystal structure reported for BaAl₂O₄ at room temperature has been carefully re-investigated by a combined transmission electron microscopy and neutron powder diffraction study. It is shown that the poor fit of this P6₃ (a=2a_p, b=2b_p, c=c_p) structure model for BaAl₂O₄ to neutron powder diffraction data is primarily due to the failure to take into account coherent scattering between different domains related by enantiomorphic twinning of the P6₃22 parent sub-structure. Fast Fourier transformation of [0 0 1] lattice images from small localized real space regions (∼10 nm in diameter) are used to show that the P6₃ (a=2a_p, b=2b_p, c=c_p) crystal structure reported for BaAl₂O₄ is not correct on the local scale. The correct local symmetry of the very small nano-domains is most likely orthorhombic or monoclinic.     

Phase transitions in K3AlF6

Phase transitions in the elpasolite-type K₃AlF₆ complex fluoride were investigated using differential scanning calorimetry, electron diffraction and X-ray powder diffraction. Three phase transitions were identified with critical temperatures , and . The α-K₃AlF₆ phase is stable below T₁ and crystallizes in a monoclinic unit cell with a=18.8588(2)Å, b=34.0278(2)Å, c=18.9231(1)Å, β=90.453(1)° (a=2a_c−c_c, b=4b_c, c=a_c+2c_c; a_c, b_c, c_c—the basic lattice vectors of the face-centered cubic elpasolite structure) and space group I2/a or Ia. The intermediate β phase exists only in very narrow temperature interval between T₁ and T₂. The γ polymorph is stable in the T₂<T<T₃ temperature range and has an orthorhombic unit cell with a=36.1229(6)Å, b=17.1114(3)Å, c=12.0502(3)Å (a=3a_c−3c_c, b=2b_c, c=a_c+c_c) at 250 °C and space group Fddd. Above T₃ the cubic δ polymorph forms with a_c=8.5786(4)Å at 400 °C and space group . The similarity between the K₃AlF₆ and K₃MoO₃F₃ compounds is discussed.     

Assembly of diverse structural types of organotellurium compounds in the reactions of (4-MeO-C6H4)2TeO with pyridine carboxylic acids

The reactions of Ar₂TeO (Ar = 4-MeO-C₆H₄) with 2-, 3- and 4-pyridine carboxylic acids (LH) afforded different organotelluroxane structural types depending on the stoichiometry of the reactants and the conditions of the reaction. Ar₂Te(L)OH (1a-1c) are formed in a 1:1 reaction of Ar₂TeO with LH in the presence of water. On the other hand a 1:2 reaction under anhydrous conditions leads to the formation of Ar₂TeL₂ (2a-2c). A 2:2 reaction under anhydrous conditions affords the ditelluroxanes Ar₂Te(L)OTe(L)Ar₂ (3a-3c) while tritelluroxanes Ar₂Te(L)OTeAr₂OTe(L)Ar₂ (4a-4c) are formed in 3:2 reactions. Interestingly, 3a-3c are formed in the reaction of 2a-2c with Ar₂TeO. The former can be hydrolyzed to 1a-1c while the latter upon reaction with Ar₂TeO lead to the formation of the tritelluroxanes 4a-4c. Attempts to metalate 2a with PdCl₂(MeCN)₂ leads to a transfer of the carboxylate ligand to palladium affording Ar₂TeCl₂ and PdL₂. X-ray crystal structures of representative examples of the family of 1, 2 and 3 reveal interesting supramolecular structures and the formation of a novel [TeO]₂ structural unit. The latter results from intermolecular secondary Te?O interactions.     

Total synthesis of (±)-camphorataimides and (±)-himanimides by NaBH4/Ni(OAc)2 or Zn/AcOH stereoselective reduction

Maleic anhydride 1 of Antrodia camphorate, which can be isolated from Chinese herbal medicine, is achieved in which the longest linear sequence is only five steps, in 40% overall yield from commercially available succinic anhydride. The crucial antrodimides 3 and 2 can be readily transformed by the chemoselective reduction with Zn/AcOH and NaBH₄/Ni(OAc)₂·4H₂O to afford the naturally occurring camphorataimides, 4 and 5, in high yields as well, respectively. This synthetic strategy can also be modified to give access to a variety of different maleic acid derivatives, himanimides 6-8.     

Atom-efficient and environment-friendly multicomponent synthesis of amidoalkyl naphthols catalyzed by P2O5

An atom-efficient and environment-friendly approach for the synthesis of amidoalkyl naphthols (4a-x) via multicomponent one-pot reaction of 2-naphthol (1), aromatic aldehyde (2) and amide (3) catalyzed by P₂O₅ has been developed. The present approach offers several advantages such as reduced reaction times, moderate temperature, higher yields, eco-friendly reaction condition, easy purification and economic availability of the catalyst.     

Quantum chemistry studies on the Ru-M interactions and the P NMR in [Ru(CO)3(Ph2Ppy)2(MCl2)] (M = Zn, Cd, Hg)

To study the Ru-M interactions and their effects on ³¹P NMR, complexes [Ru(CO)₃(Ph₂Ppy)₂] (py = pyridine) (1) and [Ru(CO)₃(Ph₂Ppy)₂MCl₂] (M = Zn, 2; Cd, 3; Hg, 4) were calculated by density functional theory (DFT) PBE0 method. Moreover, the PBE0-GIAO method was employed to calculate the ³¹P chemical shifts in complexes. The calculated ³¹P chemical shifts in 1-3 follow 2 > 3 > 1 which are consistent to experimental results, proving that PBE0-GIAO method adopted in this study is reasonable. This method is employed to predict the ³¹P chemical shift in designed complex 4. Compared with 1, the ³¹P chemical shifts in 2-4 vary resulting from adjacent Ru-M interactions. The Ru → M or Ru ← M charge-transfer interactions in 2-4 are revealed by second-order perturbation theory. The strength order of Ru → M interactions is the same as that of the P-Ru → M delocalization with Zn > Cd > Hg, which coincides with the order of ³¹P NMR chemical shifts. The interaction of Ru → M, corresponding to the delocalization from 4d orbital of Ru to s valence orbital of M²⁺, results in the delocalization of P-Ru → M, which decreases the electron density of P nucleus and causes the downfield ³¹P chemical shifts. Except 2, the back-donation effect of Ru ← M, arising from the delocalization from s valence orbital of M²⁺ to the valence orbital of Ru, is against the P-Ru → M delocalization and results in the upfield ³¹P chemical shifts in 4. Meanwhile, the binding energies indicate that complex 4 is stable and can be synthesized experimentally. However, as complex [Ru(CO)₃(Ph₂Ppy)₂HgCl]⁺5 is more stable than 4, the reaction of 1 with HgCl₂ only gave 5 experimentally.     

A convergent total synthesis of antiplasmodial C2 symmetric (+)-ekeberin D4

The first concise total synthesis of C₂ symmetric (+)-ekeberin D₄ (1) that exhibits antiplasmodial activity has been achieved in total nine steps and 27% yield from the known diol 4. The efficient synthetic method features the regio- and diastereoselective epoxidation of 4 and convergent coupling between half fragments 2 and 3 by taking into account the C₂ symmetric property.     

[Cu4OCl6(DABCO)2]·0.5DABCO·4CH3OH (“MFU-5”): Modular synthesis of a zeolite-like metal-organic framework constructed from tetrahedral {Cu4OCl6} secondary building units and linear organic linkers

A novel metal-organic framework (MOF) based on a tetranuclear copper cluster and a linear organic ligand formulated as [Cu₄OCl₆(DABCO)₂]·0.5DABCO·4CH₃OH (denoted as MFU-5, MFU=Metal-Organic Framework, Ulm University; DABCO=1,4-diazabicyclo[2.2.2]octane), was prepared via solvothermal synthesis. In contrast with common MOF synthesis strategies, MFU-5 is assembled from pre-defined molecular secondary building units, i.e. {Cu₄OCl₆} moieties, which become the nodes of the coordination framework. The title compound was characterized by single crystal X-ray diffraction, variable temperature powder diffraction (VT-XRPD), thermal analysis, as well as IR- and UV/Vis spectroscopy. Crystal data for MFU-5: hexagonal, P6/mcc (no. 192), a=25.645(9), c=17.105(11) Å, V=9742(8) Å³, Z=12, 1690 structure factors, R[F²>2σ(F²)]=0.049. MFU-5 is a 3D metal-organic framework with 1D channels running along the c-axis hosting DABCO and methanol solvent molecules. The framework displays a zeolite-like structure constructed from mso cages, which represents the composite building units in the zeolites SSF, MSO and SZR. Two-fold interpenetration is observed between these building units. TG/DTA-MS and VT-XRPD characterization reveal a stepwise release of methanol and DABCO molecules upon heating, eventually resulting in a structural change into a non-porous material.     

Synthesis, crystal structure, infrared and Raman spectra of Sr4Cu3(AsO4)2(AsO3OH)4·3H2O and Ba2Cu4(AsO4)2(AsO3OH)3

The two new compounds, Sr₄Cu₃(AsO₄)₂(AsO₃OH)₄·3H₂O (1) and Ba₂Cu₄(AsO₄)₂(AsO₃OH)₃(2), were synthesized under hydrothermal conditions. They represent previously unknown structure types and are the first compounds synthesized in the systems SrO/BaO-CuO-As₂O₅-H₂O. Their crystal structures were determined by single-crystal X-ray diffraction [space group C2/c, a=18.536(4) Å, b=5.179(1) Å, c=24.898(5) Å, β=93.67(3)°, V=2344.0(8) Å³, Z=4 for 1; space group P4₂/n, a=7.775(1) Å, c=13.698(3) Å, V=828.1(2) Å³, Z=2 for 2]. The crystal structure of 1 is related to a group of compounds formed by Cu²⁺-(XO₄)³⁻ layers (X=P⁵⁺, As⁵⁺) linked by M cations (M=alkali, alkaline earth, Pb²⁺, or Ag⁺) and partly by hydrogen bonds. In 1, worth mentioning is the very short hydrogen bond length, D···A=2.477(3) Å. It is one of the examples of extremely short hydrogen bonds, where the donor and acceptor are crystallographically different. Compound 2 represents a layered structure consisting of Cu₂O₈ centrosymmetric dimers crosslinked by As1φ₄ tetrahedra, where φ is O or OH, which are interconnected by Ba, As2 and hydrogen bonds to form a three-dimensional network. The layers are formed by Cu₂O₈ centrosymmetric dimers of CuO₅ edge-sharing polyhedra, crosslinked by As1O₄ tetrahedra. Vibrational spectra (FTIR and Raman) of both compounds are described. The spectroscopic manifestation of the very short hydrogen bond in 1, and ABC-like spectra in 2 were discussed.     

Supramolecular nanostructured assemblies of different types of porphyrins with fullerene using TiO2 nanoparticles for light energy conversion

TiO₂ nanoparticles were modified with porphyrin derivatives, 5-[4-benzoic acid]-10,15,20-tris[3,5-di-tert-butylphenyl]-21H,23H-porphyrin (Ar-H₂P-COOH), 5-[4-benzoic acid]-10,20-tris[3,5-di-tert-butylphenyl]-21H,23H-porphyrin (H-H₂P-COOH), and 5,10,15,20-tetra[4-benzoic acid]-21H,23H-porphyrin (H₂P-4COOH). The porphyrin-modified TiO₂ nanoparticles were deposited on nanostructured OTE/SnO₂ electrode together with nanoclusters of fullerene (C₆₀) in acetonitrile-toluene (3/1, v/v) using an electrophoretic deposition technique to afford the porphyrin-modified TiO₂ composite electrode denoted as OTE/SnO₂/(porphyrin-modified TiO₂ nanoparticle+C₆₀)_n. The porphyrin-modified TiO₂ composite electrodes have efficient light absorbing properties in the visible region, exhibiting the photoactive response under visible light excitation using redox couple. The incident photon-to-photocurrent efficiency (IPCE) values of supramolecular nanostructured electrodes of porphyrin-modified TiO₂ nanoparticles with fullerene [OTE/SnO₂/(Ar-H₂P-COO-TiO₂+C₆₀)_n, OTE/SnO₂/(H-H₂P-COO-TiO₂+C₆₀)_n, and OTE/SnO₂/(H₂P-4COO-TiO₂+C₆₀)_n] are much larger than those of the reference systems of porphyrin-modified TiO₂ nanoparticles without C₆₀ [OTE/SnO₂/(Ar-H₂P-COO-TiO₂)_n, OTE/SnO₂/(H-H₂P-COO-TiO₂)_n, and OTE/SnO₂/(H₂P-4COO-TiO₂)_n]. In particular, the maximum IPCE value (41%) is obtained for OTE/SnO₂/(H-H₂P-COO-TiO₂+C₆₀)_n under the bias potential of 0.2 V versus SCE. This indicates that the formation of supramolecular complexes between porphyrins and fullerene on TiO₂ nanoparticles plays an important role in improvement of the light energy conversion properties.     

Stereoconvergent synthesis of C1-C17 and C18-C25 fragments of bafilomycin A1

The effective syntheses of the enantiomerically pure C1-C17 2 and C18-C25 3 fragments as promising synthetic intermediates of bafilomycin A₁, 1 have been achieved.     

A highly stereoselective preparation of CF3-substituted 1-aryl-1,2-diphenylethenes: application to the synthesis of panomifene

β-CF₃-α,β-diphenylvinyl sulfide 3a was prepared stereoselectively in 77% yield from the reaction of 2 with phenyllithium at room temperature for 5 h. Oxidation of 3a with MCPBA afforded the corresponding vinyl sulfone 4a, in which (E)-4a can be crystallized in a mixture of CH₂Cl₂ and hexane. The addition-elimination reaction of (E)-4a with phenyllithium having substituents on the benzene ring provided 5a-j in 51-82% yields stereospecifically. Similarly, the treatment of (E)-4a with p-chloroethoxyphenyllithium in the presence of 12-crown-4 (20 mol %) at −10 °C, followed by slowly warming to room temperature, resulted in the formation of the corresponding panomifene precursor 6 in 82% yield.     

Novel solvent-free reaction of C60 with active methylene compounds in the presence of Na2CO3 under high-speed vibration milling

Inorganic base, Na₂CO₃, was utilized to replace organic base, DBU, in the Bingel reaction employing diethyl bromomalonate under the mechanochemical ‘high-speed vibration milling’ conditions to give the cyclopropanated C₆₀1 in high yield. In contrast, reactions of C₆₀ with diethyl malonate and ethyl acetoacetate in the presence of Na₂CO₃ under HSVM conditions afforded 1,4-bisadduct 2 and dihydrofuran-fused C₆₀ derivative 3, respectively.     

Comparative structural study of the complexation behaviour of silver(I), cadmium(II), mercury(II), and palladium(II) with a 17-membered N3O2-donor macrocycle

A comparative investigation of the coordination behaviour of the 17-membered, N₃O₂-donor macrocycle, 1,12,15-triaza-3,4:9,10-dibenzo-5,8-dioxacycloheptadecane, L, with the soft metal ions Ag(I), Cd(II), Hg(II), and Pd(II) is reported. The X-ray structures of 12 complexes have been determined and a range of structural types, including both mononuclear and dinuclear species, shown to occur. In particular cases the effect of anion variation on the resulting structures has been investigated; L reacts with AgX (X = NO₃, ClO₄, PF₆, OTf and CN) to yield related 2:2 (metal:ligand) complexes of types [Ag₂L₂(NO₃)₂] (1), [Ag₂L₂](ClO₄)₂ · 2DMF (2), [Ag₂L₂](PF₆)₂ · 2DMF (3), [Ag₂L₂](OTf)₂ (4) and [Ag₂L₂(μ-CN)][Ag(CN)₂] · H₂O (5). In all five complexes the ether oxygens of each ring are unbound. In 1–4 the macrocycles are present in sandwich-like arrangements that shield the dinuclear silver centres, with each silver bonded to two nitrogen donors from one L and one nitrogen from a second L. A Ag···Ag contact is present between each metal centre such that both centres can be described as showing distorted tetrahedral geometries. In the case of 5 a rare single μ₂-κC:κC symmetrically bridging two-electron-donating cyano bridge links silver ions [Ag···Ag distance, 2.7437(10) Å]; the macrocyclic ligands are orientated away from the dinuclear metal centres. In contrast to the behaviour of silver, reaction of cadmium(II) perchlorate with L resulted in a mononuclear sandwich-like complex of type [CdL₂](ClO₄)₂ · CH₃CN (6). Again, the ether oxygens do not coordinate, with each L binding to the cadmium centre only via its three nitrogen donors in a facial arrangement such that a distorted octahedral coordination geometry is attained. Reaction of L with HgX₂ (X = ClO₄, SCN and I) yielded the monomeric species [HgL(ClO₄)₂] (7), [HgL(SCN)₂]·CH₃CN (8) and [Hg₂L₂](HgI₄)₂ · 2L (9), in which all five donors of L are bound to the respective mercury centres. However, reaction of L with Hg(NO₃)₂ in dichloromethane/methanol gave a mononuclear sandwich-like complex [HgL₂](NO₃)₂ · 2CH₃OH (10) without anion coordination. Reaction of K₂PdCl₄ and Pd(NO₃)₂ with L yielded the 1:1 complexes [PdLCl]Cl · H₂O (11) and [PdL(NO₃)]NO₃ · CH₃OH (12), respectively, in which the metal is bound to three nitrogen donors from L along with the corresponding chloride or nitrate anion. Each palladium adopts a distorted square-planar coordination geometry; once again the ether oxygens are not coordinated.     

Thermal decomposition of iron(VI) oxides, K2FeO4 and BaFeO4, in an inert atmosphere

The thermal decomposition of solid samples of iron(VI) oxides, K₂FeO₄·0.088 H₂O (1) and BaFeO₄·0.25H₂O (2) in inert atmosphere has been examined using simultaneous thermogravimetry and differential thermal analysis (TG/DTA), in combination with in situ analysis of the evolved gases by online coupled mass spectrometer (EGA-MS). The final decomposition products were characterized by ⁵⁷Fe Mössbauer spectroscopy. Water molecules were released first, followed by a distinct decomposition step with endothermic DTA peak of 1 and 2 at 273 and 248 °C, respectively, corresponding to the evolution of molecular oxygen as confirmed by EGA-MS. The released amounts of O₂ were determined as 0.42 and 0.52 mol pro formula of 1 and 2, respectively. The decomposition product of K₂FeO₄ at 250 °C was determined as Fe(III) species in the form of KFeO₂. Formation of an amorphous mixture of superoxide, peroxide, and oxide of potassium may be other products of the thermal conversion of iron(VI) oxide 1 to account for less than expected released oxygen. The thermogravimetric and Mössbauer data suggest that barium iron perovskite with the intermediate valence state of iron (between III and IV) was the product of thermal decomposition of iron(VI) oxide 2.     

Synthesis of water-soluble 2-alkylcyclodextrin-C60 conjugates and their inclusion complexation in aqueous solution

Two β-cyclodextrin-C₆₀ conjugates (3 and 4) with a flexible linker at the secondary face of cyclodextrin are synthesized by a single reaction of 2-(ω-azidoundecanyl)-2-O-heptakis (2,3,6-tri-O-methyl)-β-cyclodextrin (2) and C₆₀, both of which display satisfactory water solubility. Structural analyses show that 3 is a closed [5,6] aziridinofullerene, whereas 4 is a bis-adduct derivative. Using rhodamine B (RhB) as a guest molecule, the inclusion complexation behavior of 3 was investigated in aqueous solution.     

Chemically modified oximato complexes of titanium(IV) isopropoxide as new precursors for the sol-gel preparation of nano-sized titania: Crystal and molecular structure of [Ti{ONC10H16}4·2CH2Cl2]

Reactions of [Ti(OPrⁱ)₄] with various oximes, in anhydrous refluxing benzene yielded complexes of the type [Ti{OPrⁱ}_4−n{L}_n], where, n = 1-4 and LH = (CH₃)₂CNOH (1-4), C₉H₁₆CNOH (5-8) and C₉H₁₈CNOH (9-12). The compounds were characterized by elemental analyses, molecular weight measurements, FAB-mass, FT-IR and NMR (¹H, ¹³C{¹H}) spectral studies. The FAB-mass spectra of mono- (1), and di- (2), (6), (10) substituted products indicate their dimeric nature and that of tri- (3) and tetra- (4), (8) substituted derivatives suggest their monomeric nature. Crystal and molecular structure of [Ti{ONC₁₀H₁₆}₄·2CH₂Cl₂] (8A) suggests that the oximato ligands bind the metal in a dihapto η²-(N, O) manner, leading to the formation of an eight coordinated species. Thermogravimetric curves of (3), (6) and (10) exhibit multi-step decomposition with the formation of TiO₂ as the final product in each case, at 900 °C. Low temperature (∼600 °C) sol-gel transformations of (2), (3), (4), (6), (7) and (8) yielded nano-sized titania (a), (b), (c), (d), (e) and (f), respectively. Formation of anatase phase in all the titania samples was confirmed by powder XRD patterns, FT-IR and Raman spectroscopy. SEM images of (a), (b), (c), (d), (e) and (f) exhibit formation of nano-grains with agglomer like surface morphologies. Compositions of all the titania samples were investigated by EDX analyses. The absorption spectra of the two representative samples, (a) and (f) indicate an energy band gap of 3.17 eV and 3.75 eV, respectively.     

Synthesis and characterisation of six Fe(II or III), Co(II) or Zr(IV) complexes containing the ligand [CH(SiMe2R)P(Ph)2NSiMe3] (R = Me, NEt2) and of [Co{N(SiMe3)C(Ph)C(H)P(Ph)2NSiMe3}2]

The C,N-(trimethylsilyliminodiphenylphosphoranyl)silylmethylmetal complexes [Fe(L)₂] (3), [Co(L)₂] (4), [ZrCl₃(L)]·0.83CH₂Cl₂ (5), [Fe(L)₃] (6), [Fe(L′)₂] (7) and [Co(L′)₂] (8) have been prepared from the lithium compound Li[CH(SiMe₂R)P(Ph)₂NSiMe₃] [1a, (R = Me) {≡ Li(L)}; 1b, (R = NEt₂) {≡ Li(L′)}] and the appropriate metal chloride (or for 7, FeCl₃). From Li[N(SiMe₃)C(Ph)C(H)P(Ph)₂NSiMe₃] [≡ Li(L″)] (2), prepared in situ from Li(L) (1a) and PhCN, and CoCl₂ there was obtained bis(3-trimethylsilylimino- diphenylphosphoranyl-2-phenyl-N-trimethylsilyl-1-azaallyl-N,N′)cobalt(II) (9). These crystalline complexes 3-9 were characterised by their mass spectra, microanalyses, high spin magnetic moments (not 5) and for 5 multinuclear NMR solution spectra. The X-ray structure of 3 showed it to be a pseudotetrahedral bis(chelate), the iron atom at the spiro junction.     

Synthesis and characterization of some novel cadmium(II) complexes with 3-hydroxypicolinic acid (3-OHpicH): Crystal and molecular structures of [CdI(3-OHpic)(3-OHpicH)(H2O)]2, [Cd(3-OHpic)2(H2O)2] and [Cd(3-OHpic)2]n

Cadmium(II) complexes of 3-hydroxypicolinic acid, namely [CdI(3-OHpic)(3-OHpicH)(H₂O)]₂ (1), [Cd(3-OHpic)₂(H₂O)₂] (2) and [Cd(3-OHpic)₂]_n (3) were prepared and characterized by spectroscopic methods (IR, NMR) and their molecular and crystal structures were determined by X-ray crystal structure analysis. Complexes 1 and 2 were prepared in similar reaction conditions using different cadmium(II) salts: cadmium(II) iodide and cadmium(II) acetate dihydrate, respectively, while 3 was prepared by recrystallization of 2 from N,N-dimethylformamide solution. Various coordination modes of 3-OHpicH in 1–3 were established in the solid state: bidentate N,O-chelated mode in 1 and 2, monodentate mode through the carboxylate O atom from zwitterionic ligand in 1 and bidentate N,O-chelated and bridging mode in 3. In the DMF solution of all prepared complexes, only monodentate mode of 3-OHpicH binding to cadmium(II) through the carboxylate O atom was established by ¹H, ¹³C, ¹⁵N and ¹¹³Cd NMR spectroscopy.     

Magnetic behavior of MnPS3 phases intercalated by [Zn2L] (LH2: macrocyclic ligand obtained by condensation of 2-hydroxy-5-methyl-1,3-benzenedicarbaldehyde and 1,2-diaminobenzene)

The intercalation of the cationic binuclear macrocyclic complex [Zn₂L]²⁺ (LH₂: macrocyclic ligand obtained by the template condensation of 2-hydroxy-5-methyl-1,3-benzenedicarbaldehyde and 1,2-diaminobenzene) was achieved by a cationic exchange process, using K_0.4Mn_0.8PS₃ as a precursor. Three intercalated materials were obtained and characterized: (Zn₂L)_0.05K_0.3Mn_0.8PS₃(1), (Zn₂L)_0.1K_0.2Mn_0.8PS₃(2) and (Zn₂L)_0.05K_0.3Mn_0.8PS₃(3), the latter phase being obtained by an assisted microwave radiation process. The magnetic data permit to estimate the Weiss temperature θ of ≈−130 K for (1); ≈−155 K for (2) and ≈−130 K for (3). The spin canting present in the potassium precursor remains unperturbed in composite (3), and spontaneous magnetization is observed under 50 K in both materials. However composites (1) and (2) do not present this spontaneous magnetization at low temperatures.The electronic properties of the intercalates do not appear to be significantly altered. The reflectance spectra of the intercalated phases (1), (2) and (3) show a gap value between 1.90 and 1.80 eV, lower than the value observed for the K_0.4Mn_0.8PS₃ precursor of 2.8 eV.