Thermal properties and crystallization of MgO–FeO<Subscript>x</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript> glasses

Five novel bridged heptaphenyl polyhedral oligomeric silsesquioxanes (POSSs), in which two identical silicon cages R₇(SiO_1.5)₈ (with R = Phenyl) are linked to various aliphatic [(CH₂) _n with n = 2, 6 and 10] and aromatic (Ar–Ar and Ar–O–Ar, where Ar = p-C₆H₄) bridges, were synthesized. The obtained compounds were characterized by elemental analysis and ¹ H NMR spectroscopy, and the results were in very good agreement with those of expected products. The synthesized heptaphenyl POSSs were thermally degraded, in dynamic heating conditions (25–700 °C), in both flowing nitrogen and static air atmosphere. The temperatures at 5% mass loss (T _5%) and residues at 700 °C were thus determined to evaluate their resistance to thermal degradation, but no substantial difference was found between the values in the two studied environments. The obtained T _5% values were much higher than those of the corresponding isobutyl and cyclopentyl POSSs we investigated in the past. Also, the T _5% values of the phenyl POSSs with aliphatic bridges decreased quite linearly on increasing the number of bridge carbon atoms (n _C). This behaviour was interpreted and attributed to the presence of the external corona formed by voluminous phenyl groups. The residue at 700 °C, which was largely higher than those of the corresponding isobutyl and cyclopentyl POSSs, was a further confirmation of the better thermal stability of the compounds here studied.     

Catalytic activity of amines in the oxidation of anthrone

The rate of non-radical oxidation of anthrone with molecular oxygen, catalyzed by aliphatic amines with different substituents, amino acids, aromatic amines, and compounds possessing several basic centers, was measured. The catalytic activity of amines decreases in the series RO(CH₂) _n NH₂ > RNH₂ > morpholine derivatives > RR′N(CH₂) _n NH₂ > guanidine > RR′NH > RR′R″N > 1,4-diazabicyclo[2.2.2]octane > amino acids > (R)PhNH₂. A relation was found between proton affinities and structural parameters of the amines and their catalytic activity in the title reaction.     

Pulsed electrochemical deposition of nickel oxides on multi-walled carbon nanotubes from EDTA alkaline solutions: a SEM,XPS, and voltammetric characterization

A study regarding the electrodeposition of nickel oxide particles on the activated multi-walled carbon nanotubes from 2 M NaOH solution containing Ni(NO₃)₂ and EDTA was carried out. The electrodeposition process was carried out using an optimized double-pulse sequence of potentials: E ₁ = ?0.2 V vs. SCE (t ₁ = 0.3 s) and E ₂ = 0.7 V vs. SCE (t ₂ = 0.03 s). Spectroscopic XPS investigations and SEM analysis were used in order to characterize the surface and morphology of the studied modified electrode. Cyclic voltammetry and chronoamperometry were used in order to evaluate the electrochemical/amperometric performance of the GC/MWCNT-Ni electrode toward the oxidation of some aliphatic alcohols in strong alkaline medium.     

Syntheses,structures, and catalytic activity in Friedel–Crafts acylations of substituted tetramethylcyclopentadienyl molybdenum carbonyl complexes

Reactions of the substituted tetramethylcyclopentadienes [C₅HMe₄R] [R =  ^t Bu, Ph, CH₂CH₂C(CH₃)₃] with Mo(CO)₃(CH₃CN)₃ in refluxing xylene gave a series of dinuclear molybdenum carbonyl complexes [(η⁵-C₅Me₄R)Mo(CO)₃]₂ [R =  ^t Bu (1), Ph (2), CH₂CH₂C(CH₃)₃ (3)], [(η⁵-C₅Me ^t Bu)Mo(μ-CO)₂]₂ (4)], and [(η⁵-C₅Me₄) ^t Bu]₂Mo₂O₄(μ-O) (5)], respectively. Complexes 1–5 were characterized by elemental analysis, IR, ¹H NMR, and ¹³C NMR spectroscopy. In addition, their crystal structures were determined by X-ray crystal diffraction analysis. The catalytic activities of complexes 1–3 in Friedel–Crafts acylation in the presence of o-chloranil has also been investigated; the reactions were achieved under mild conditions to give the corresponding products in moderate yields.     

Selective,metal-free oxidation of sulfides to sulfoxides Using 30% hydrogen peroxide catalyzed with <Emphasis Type="Italic">N</Emphasis>-bromosuccinimide (NBS) under neutral buffered reaction conditions

Various types of aromatic and aliphatic sulfides are selectively oxidized to the corresponding sulfoxides in good to excellent yields using 30% H₂O₂ in the presence of catalytic amounts of N-bromosuccinimide (NBS) in buffered aqueous acetonitrile solution (pH =7.00). The results showed that acid sensitive functional groups such as double bonds, and O,O-acetals remained intact under the described reaction conditions     

Effect of mixed thiols on the adsorption,capacitive and hybridization performance of DNA self-assembled monolayers on gold

In this article, we investigated the effect of mixed thiols (HS(CH₂)₅CH₃, HS(CH₂)₆OH and HS(CH₂)₂NH₂) on the adsorption, capacitive and hybridization performance of thiol-modified probe DNA self-assembled monolayers on gold by chronocoulometry (CC) and cyclic voltammetry (CV). Co-assembly of HS(CH₂)₅CH₃ with probe DNA availed DNA surface adsorption on gold more than HS(CH₂)₆OH and HS(CH₂)₂NH₂. With the increase of the assembly concentration ratio of probe DNA and mixed thiols (C _DNA/C _thiols), DNA surface coverage (Γ _m) was almost constant for DNA/HS(CH₂)₅CH₃ mixed SAMs and increased gradually for DNA/HS(CH₂)₆OH or DNA/HS(CH₂)₂NH₂ mixed SAMs. Interfacial capacitance (C _d) value of DNA/thiol-mixed SAMs on gold mainly depended on the capacitance of thiols SAMs. DNA hybridization almost did not change the capacitance value of DNA/thiol-mixed SAMs on gold. Hybridization experiments indicated that the maximal DNA hybridization density (H _D) was 1.2 × 10^?11 and 1.1 × 10^?11 mol cm^?2 with HS(CH₂)₅CH₃ or HS(CH₂)₆OH as mixed thiols respectively, much bigger than that with short-chain thiols (HS(CH₂)₂NH₂). The size fitting coefficient d _c/d _t values for the optimal hybridization of DNA/HS(CH₂)₅CH₃ and DNA/HS(CH₂)₆OH mixed SAMs were 0.70 and 0.93, respectively. This indicated that probe DNA with much bigger Γ _m should be co-assembled with HS(CH₂)₅CH₃ on gold to obtain the biggest H _D than with HS(CH₂)₆OH. These conclusions provided the important reference for optimally designing DNA sensor.     

Chemical looping combustion characteristics of coal with Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> oxygen carrier

Chemical looping combustion (CLC) by direct use of coal as fuel is promising with its prominent advantages, but insufficient conversion of coal in the CLC system is a great limitation. In this research, in order to explore the limiting factor inherent for coal conversion in the CLC system, from the perspective of chemical structure of coal, reaction of a selected Chinese typical coal (designated as LZ) with Fe₂O₃ was systematically investigated. Thermogravimetric investigation of LZ coal reaction with Fe₂O₃ at the oxygen excess number Φ = 1.0 indicated that after dehydration, there existed three discernible reaction stages as observed, which were attributed to the combined reactions of Fe₂O₃ with the primary and secondary gaseous products evolved from LZ coal. Meanwhile, the Fe₂O₃ provided should be controlled around Φ = 1.0 aiming at effective conversion of LZ coal and simultaneous proper utilization of Fe₂O₃. And then, both gaseous Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy analysis of the gaseous and solid products formed from reaction of LZ coal with Fe₂O₃ at Φ = 1.0 indicated that full conversion of LZ coal was not reached with a little unconverted CO occurring, though partial Fe₂O₃ was over reduced to lower valence of oxides than Fe₃O₄. Furthermore, in order to explore the insufficient conversion of LZ coal at the molecular scale, X-ray photoelectron spectroscopy analysis revealed the distribution and evolution of the carbon functional groups involved in LZ coal after its reaction with Fe₂O₃ and further found that effective conversion of the aromatic/aliphatic C=C/C–H groups in LZ coal was the rate-limited step at the molecular scale with the relative content of these groups still dominated around 59% after LZ coal reaction with Fe₂O₃. Finally, solid IR (infrared) analysis and quantitative evaluation of the solid products of LZ coal reaction with Fe₂O₃ indicated that the length of aliphatic C–H groups decreased due to its partial disintegration, while the aromatization of the residual char was aggravated with the higher relative IR intensity ratio of the aromatic C=C groups, which reduced the reactivity of LZ residual char and hindered the full conversion of LZ coal.     

Synthesis and catalytic activity of rhenium carbonyl complexes containing alkyl-substituted tetramethylcyclopentadienyl ligands

A series of six alkyl-substituted tetramethylcyclopentadienyl mononuclear metal carbonyl complexes [(η ⁵-C₅Me₄R)Re(CO)₃] [R = allyl (1), i-Pr (2), n-butyl (3), t-butyl (4), benzyl (5), CH(CH₂)₄ (6)] have been synthesized by treating the corresponding ligands (C₅Me₄R) [R = allyl, i-Pr, n-butyl, t-butyl, benzyl, CH(CH₂)₄] with Re₂(CO)₁₀ in refluxing xylene. The six new complexes were characterized by elemental analysis, IR, ¹H NMR and ¹³C NMR spectroscopy. The crystal structures of all six complexes were determined by X-ray crystal diffraction analysis, showing that they have similar molecular structures, being mononuclear carbonyl complexes. In each of these complexes, the Re atom is η ⁵ -coordinated to the cyclopentadienyl ring. Complexes 1–5 have significant catalytic activity in Friedel–Crafts reactions of aromatic compounds with alkylation reagents. Compared with traditional catalysts, these mononuclear rhenium carbonyl complexes have obvious advantages such as lower amounts of catalyst, mild reaction conditions and environmentally friendly chemistry.     

Features of the First and Second Order Electrospray Ionization Mass Spectra for Salt-Like Products Derived from Monools and Diols Using Combined Reagents Based on ω-Bromoacyl Chlorides and Nitrogen Bases

Derivatization by composite reagents based on ω-bromoacyl chlorides [ClCO(C₂) _n Br (n = 1–4)] and pyridine was applied to study aliphatic and alicyclic alcohols and diols by ordinary and tandem electrospray ionization (ESI) mass spectrometry. The applied derivatization involves the simultaneous acylation of hydroxyl groups with an acyl chloride moiety and the quaternization of pyridine with a terminal bromoalkyl group. Under the ESI conditions, quaternary salts produce corresponding mono and diammonium cations, which are detected in the first-order mass spectra. Collision-induced dissociation (CID) of primary cations generated from monool derivatives gives rise to ammonium cations of the corresponding acids HOOC(CH₂) _n –N⁺(C₅H₅). The CID of primary dications affords the same cations which are also eliminated from dications to form mono-charged fragments.     

Extraction Properties of Oligoethylene Glycol Bis[(2-Diphenylphosphinylmethyl-4-methyl)phenyl] Ethers

Extraction of Ln(III), Sc(III), Ga(III), and Re(VII) ions by solutions of phosphorylated monopodands having [ortho-(diphenylphosphinylmethyl)-para-methyl]phenyl terminal groups, 2-Ph₂P(O)CH₂(4-Me)C₆H₃(OCH₂CH₂) _n OC₆H₃(Me-4)CH₂P(O)Ph₂-2 (n = 1–5), in organic solvents has been studied. The stoichiometries of extractable complexes were determined. The effect of the aqueous phase, organic solvent, and phosphorylated podand structure on the efficacy of metal-ion recovery into organic phase has been considered.     

Synthesis and characterization of crystallizable aliphatic thermoplastic poly(ester urethane) elastomers through a non-isocyanate route

A simple non-isocyanate route is developed for synthesizing crystallizable aliphatic thermoplastic poly(ester urethane) elastomers(TPEURs) with good thermal and mechanical properties. Three prepolymers of1,6-bis(hydroxyethyloxycarbonylamino) hexane(BHCH), i.e. Pre PBHCHs, were prepared through the self-transurethane polycondensation of BHCH. A poly(butylene adipate) prepolymer(Pre PBA) with terminal HO― groups was prepared and used as a polyester glycol. A series of TPEURs were prepared by the co-polycondensation of the Pre PBHCHs with Pre PBA at 170 ℃ under a reduced pressure of 399 Pa. The TPEURs were characterized by gel permeation chromatography, FTIR,1H-NMR, differential scanning calorimetry, thermogravimetric analysis, wide-angle X-ray diffraction, atomic force microscopy, and tensile test. The TPEURs exhibited M_n up to 23300 g/mol, M_w up to 51100 g/mol, Tg ranging from-33.8 ℃ to-3.1 ℃, T_m from 94.3 ℃ to 111.9 ℃, initial decomposition temperature over 274.7 ℃, tensile strength up to18.8 MPa with a strain at break of 450.0%, and resilience up to 77.5%. TPU elastomers with good crystallization and mechanical properties were obtained through a non-isocyanate route.     

Syntheses,crystal structures and in vitro anticancer activities of oxovanadium(IV) complexes of amino acid Schiff base and 1,10-phenanthroline ligands

Four oxovanadium(IV) complexes, namely [VO(desa-met)(phen)]·MeOH·2H₂O (1) (desa-met = Schiff base derived from 4-(diethylamino)salicylaldehyde and dl-methionine, phen = 1,10-phenanthroline), [VO(o-van-met) (phen)]·MeOH·CH₂Cl₂·3H₂O (2) (o-van-met = Schiff base derived from o-vanillin and dl-methionine), [VO(dtbs-napa)(phen)]·2H₂O (3) (dtbs-napa = Schiff base derived from 3,5-di-tert-butyl salicylaldehyde and 3-(1-naphthyl)-l-alanine) and [VO(hyna-napa)(phen)]·1.5H₂O (4) (hyna-napa = Schiff base derived from 2-hydroxy-1-naphthaldehyde and 3-(1-naphthyl)-l-alanine), were synthesized and characterized by IR, HRMS, UV–vis spectra, molar conductance and single-crystal X-ray diffraction (XRD). X-ray structural analysis showed that the V(IV) atoms in all four complexes are six-coordinated in a distorted octahedral environment. In the crystals of complexes 1 and 2, π–π stacking interactions together with hydrogen bonds connect the molecular units into 2D networks. Meanwhile, CH–π stacking interactions are observed between the aromatic rings in the crystals of 1 and 4, while the π–π stacking interactions between aromatic rings in the crystals of 2 and 3 are arranged with a face-to-face mode. The in vitro anticancer activities of these complexes against A-549 and HeGp2 cells were tested by MTT assay.     

Effect of alkali metal salts on decomposition of ionic liquid like organic salt

N ¹,N ¹,N ²,N ²-tetramethylethane-1,2-diamine-based ionic salts (TMEDA), N ¹,N ¹,N ¹,N ²,N ²,N ²-hexamethylethane-1,2-diaminium dicyanamide (HMEDA-(DCA)₂) were prepared following the quaternization and subsequent ion exchange. The chemical structure of the HMEDA-(DCA)₂ was confirmed using ¹³C NMR spectrum and elemental analysis. The corresponding viscosity of its 60 wt% solution was found to be lower than 5 cP at room temperature, which was critical for propellant application. The ignition delay of 40 wt% HMEDA-(DCA)₂ solution was decreased to 20–30 ms dramatically using alkali metal salts, Li(CH₃COO), Mg(CH₃COO)₂, and Ca(CH₃COO)₂ as a co-catalyst when white fume nitric acid was utilized as an oxidizer.     

Abraham Model Expressions for Describing Water-to-Diethylene Glycol and Gas-to-Diethylene Glycol Solute Transfer Processes at 298.15 K

A gas chromatographic headspace analysis method was used to experimentally determine gas-to-liquid partition coefficients and infinite dilution activity dilution for 14 different aliphatic and cyclic hydrocarbons (alkanes, cycloalkanes, alkenes, alkynes), eight different aromatic compounds (benzene, alkylbenzenes, halobenzenes), five different chloroalkanes (dichloromethane, trichloromethane, 1-chlorobutane, 1,2-dichloropropane, isopropylbromide), tetrahydrofuran, butyl acetate, and acetonitrile dissolved in diethylene glycol at 298.15 K. Solubilities were also measured at 298.15 K for 31 crystalline nonelectrolyte organic solutes including several polycyclic aromatic hydrocarbons and substituted benzoic acid derivatives. The experimental results of the headspace chromatographic and spectroscopic solubility measurements were converted to gas-to-diethylene glycol and water-to-diethylene glycol partition coefficients, and molar solubility ratios using standard thermodynamic relationships. Expressions were derived for solute transfer into diethylene glycol from the calculated partition coefficients and solubility ratios. Mathematical correlations based on the Abraham model describe the observed partition coefficient and solubility data to within 0.14 log₁₀ units (or less).     

Pyrolysis of pine needles: effects of process parameters on products yield and analysis of products

Pyrolysis of pine needles was carried out in a semi-batch reactor. The effects of pyrolysis parameters such as temperature (350–650 °C), heating rate (10 and 50 °C min^?1), nitrogen flow rate (50–200 cm³ min^?1) and biomass particle size (0.25–1.7 mm) were examined on products yield. Maximum bio-oil yield of 43.76% was obtained at pyrolysis temperature of 550 °C with a heating rate of 50 °C min^?1, nitrogen flow rate of 100 cm³ min^?1 for biomass particle size of 0.6 < d _p < 1 mm. The characterization of pyrolysis products (bio-oil, bio-char) has been made through different instrumental methods like Fourier transform infrared spectroscopy, gas chromatography–mass spectrometry, nuclear magnetic resonance spectroscopy (¹H NMR), X-ray powder diffraction, field emission scanning electron microscope and Brunauer–Emmett–Teller surface area analysis. The empirical formula of the bio-oil and bio-char was found as CH_1.47O_0.36N_0.005 and CH_0.56O_0.28N_0.013 with heating value of 26.25 and 25.50 MJ kg^?1, respectively. Results show that bio-oil can be potentially valuable as a renewable fuel after upgrading and can be used as a feedstock for valuable chemicals production. The properties of bio-char reveal that it can be used as solid fuels, as a cheap adsorbent and as a feedstock for activated carbon production.     

Theoretical investigation of carboranylpyrrole structures and the thermal resistance and conducting properties of carboranylpyrrole polymers

The carboranylpyrrole polymers are functional materials with superior thermal resistance and conducting performances. The carboranylpyrrole structures and Laplacian bond order (LBO) of carborane moiety, as well as the thermal resistance and conducting properties of carboranylpyrrole dimers or polymers, were investigated theoretically. The ¹¹B NMR chemical shifts of 3-(2-methyl-o-carboranyl)alkyl-1H-pyrrole monomers (CP-1 to CP-5) were calculated and analyzed. The average LBO values of some characteristic chemical bonds in the carborane cages of CP-1 to CP-5 molecules were calculated. It is found that the average LBO values of carborane moieties change slightly with the increase in alkyl chain length. The temperature resulting in about 15–20 % weight loss for CP-1, CP-3, CP-4 and CP-5 polymers is predicted to be more than 700 °C. Apart from the C–C bonds in carborane moieties of 3-(2-R-o-carboranyl)propyl-1H-pyrrole (R = CH₂OH, CH₂OCH₃, CN, COCl, Ph) substituents, the LBO values of other bonds in these cages change slightly relative to that in the molecule of 3-(2-methyl-o-carboranyl)propyl-1H-pyrrole (CP-3). The C–C bond LBO values in the carborane cages of these substituents with electron-donating groups (R = CH₂OH, CH₂OCH₃) are bigger than that in CP-3, while those values in those substituents with electron-withdrawing groups (R = CN, COCl, Ph) are smaller than that in CP-3. The polymerization activity calculated for CP-1 to CP-5 monomers increases with the increase in alkyl chain length. The calculated orbital energy gap (?E _LUMO?HOMO) of CP-1 to CP-5 dimers decreases with the increase in alkyl chain length, and accordingly, the electronic conductivity has the potential to increase. In addition, the calculated band gaps of CP-1 to CP-5 dimers cell models also decrease with the increase in alkyl chain length.     

New functionalization opportunities for <Emphasis Type="Italic">peri</Emphasis>-hydroxynaphthoyl and <Emphasis Type="Italic">peri</Emphasis>-fused heterocyclic compounds

A capability was studied of hydrogenated α-pyrone heterocycle in 7-methoxy-4-(4-methoxy-phenyl)-3,4-dihydro-2H-benzo[h]chromen-2-one to undergo aminolysis under the treatment with hydrazine hydrate, primary and secondary aliphatic and aromatic amines. A new approach was developed to the preparation of perihydroxyketone of naphthalene series containing a specific functional substituent in the ortho-position with respect to hydroxy group. The effect was revealed of an acetyl group in the position 9 of 7-methoxy-4-(4-methoxyphenyl)-3,4-dihydro-2H-benzo[h]chromen-2-one on the reaction of this compound with aliphatic amines and hydrazine hydrate. 9-Methoxy-1-(4-methoxyphenyl)-6-methyl-3H-benzo[de]pyrido[3,2,1-if]cinnolin-3-one [9-methyl-6-methoxy-3-(4-methoxyphenyl)-10,10a-diazapyren-1-one] was obtained, a new bis-peri-fused heteroaromatic system.     

Synthesis of water soluble metalloporphyrin-cored amphiphilic star block copolymer photocatalysts for an environmental application

Two series of water-soluble metalloporphyrin-cored amphiphilic star block copolymers were synthesized by controlled radical polymerizations such as atom transfer radical polymerization (ATRP) and reversible addition fragmentation chain transfer (RAFT), which gave eight amphiphilic block copolymer arm chains consisting of poly(n-butyl acrylate-b-poly(ethylene glycol) methyl ether methacylate) (PnBA-b-PEGMEMA, M_n,GPC = 78,000, M_w/M_n = 1.2, 70 wt% of PPEGMEMA) and poly(styrene-b-2-dimethylamino ethyl acrylate) (PS-b-PDMAEA, M_n,GPC = 83,000, M_w/M_n = 1.2, 67 wt% of PDMAEA), yielding porphyrin(Pd)-(PnBA-b-PPEGMEMA)₈ and porphyrin(Pd)-(PS-b-PDMAEA)₈, respectively. Obtained metalloporphyrin polymer photocatalysts were homogeneously solubilized in water to apply to the removal of chlorophenols in water, and was distinguished from conventional water-insoluble small molecular metalloporphyrin photocatalysts. Notably, we found that the water-soluble star block copolymers with hydrophobic–hydrophilic core–shell structures more effectively decomposed the chlorophenol, 2,4,6-trichlorophenol (2,4,6-TCP), in water under visible light irradiation (k = 1.39 h^?1, t_1/2 = 0.5 h) in comparison to the corresponding water-soluble star homopolymer, because the hydrophobic core near the metalloporphyrin effectively captured and decomposed the hydrophobic chlorophenols in water.     

Channel inclusion of primary alcohols in isostructural solvates of the antiretroviral nevirapine: an X-ray and thermal analysis study

X-ray structural and thermoanalytical data for a series of solvates 2–7 of the anti-HIV drug nevirapine containing primary alcohols CH₃(CH₂) _n OH with n = 2–7 are reported. The structures of 2–7 are based on a common isostructural framework comprising centrosymmetric hydrogen-bonded nevirapine dimers and contain a common channel parallel to the crystal b-axis whose repeat length spans a narrow range (~8.43–8.52 Å) in the series and accommodates the various solvent molecules in 2–7. Thermogravimetry yielded a guest–host ratio close to 0.5 for the 1-butanol solvate 3 and a steady decrease in this ratio from 0.43 to 0.32 for the solvates 4–7. This anomalous stoichiometric variation was resolved following successful X-ray analysis of solvate 3 which revealed that the length spanned by the disordered 1-butanol molecule is commensurate with the channel periodicity b, resulting in a stoichiometric compound. Instead, solvates 5–7, for which single crystal X-ray data were available, showed significant disorder for the solvent molecules, attributed to their increasing chain lengths being incommensurate with the parameter b.     

Stereoisomerism of Octahedral Titanium <Emphasis Type="Italic">cis</Emphasis>-Tetrafluoro Complexes with Ph<Subscript>2</Subscript>P(O)CH<Subscript>2</Subscript>CH(OH)Me Enantiomers According to <Superscript>19</Superscript>F NMR Data

Effect of enantiomers of a monodentate ligand on the stereoisomerism of mixed octahedral cis-tetrafluoro complexes of d⁰ transition metals has been studied by ¹⁹F{¹H} and ³¹P{¹H} NMR by the example of TiF₄ complexation in CH₂Cl₂ with Ph₂P(O)CH₂CH(OH)Me (L) containing asymmetric carbon atom in the aliphatic hydrocarbon group that constitutes a racemic mixture of enantiomers. Composition of complexes formed in solution has been determined, conclusion has been drawn on the relative stereochemical configuration of the chiral and meso stereoisomers of octahedral complex cis-TiF₄L₂ on the basis of analysis of ¹⁹F NMR spectra, using the heterotropism concept.