Mixed Solvent Of Methanol Research Articles

Synthesis of Unprotected Cyclic Peptide Methylene Dithioacetals by Rhodium-Catalyzed Oxidation of Methanol to Formaldehyde.

In the presence of a rhodium catalyst, unprotected peptide dithiols possessing two cysteine residues are efficiently converted to their corresponding cyclic methylene dithioacetals in a mixed solvent of methanol and water (4:1) under an oxygen atmosphere (1 atm). The slow formation of formaldehyde inhibits side reactions by maintaining its concentration at a low level, which is a key feature of this reaction. This method can be applied to peptide dithiols containing amino acids such as Gly, Ala, Ser, Lys, Met, Phe, Tyr, and His and provides cyclic methylene dithioacetals without being affected by other functional groups. Primary alcohols, such as ethanol and isopropanol, can also be employed. Oxytocin can be cyclized to provide a cyclic methylene dithioacetal.

Syntheses and crystal structures of four 4-(4-nitro-phen-yl)piperazinium salts with hydrogen succinate, 4-amino-benzoate, 2-(4-chloro-phen-yl)acetate and 2,3,4,5,6-penta-fluoro-benzoate anions.

The syntheses and crystal structures are presented for four organic salts of the 4-(4-nitro-phen-yl)piperazinium cation, namely, 4-(4-nitro-phen-yl)piperazinium hydrogen succinate, C10H14N3O2 +·C4H5O4 - (I), 4-(4-nitro-phen-yl)piperazinium 4-amino-benzoate monohydrate, C10H14N3O2 +·C7H6NO2 -·H2O (II), 4-(4-nitro-phen-yl)piperazinium 2-(4-chloro-phen-yl)acetate, C10H14N3O2 +·C8H6ClO2 - (III) and 4-(4-nitro-phen-yl)piperazinium 2,3,4,5,6-penta-fluoro-benzoate, C10H14N3O2 +·C7F5O2 - (IV). The salts form from mixtures of N-(4-nitro-phen-yl)piperazine and the corresponding acid [succinic acid (I), 4-amino-benzoic acid (II), 2-(4-chloro-phen-yl)acetic acid (III) and 2,3,4,5,6-penta-fluoro-benzoic acid (IV)] in mixed solvents of methanol and ethyl acetate. Salts I, III, and IV are anhydrous, whereas II is a monohydrate. In each structure, the overall conformation of the cation is determined by the disposition of the exocyclic N-C bond of the piperazine ring (either axial or equatorial) and twists about the N-C bond between the piperazine ring and its attached 4-nitro-phenyl ring. The packing motifs in each structure are quite different, though all are dominated by strong N-H⋯O hydrogen bonds, which are augmented in I and II by O-H⋯O hydrogen bonds, and in III by a π-π stacking inter-action between inversion-related 4-nitro-phenyl groups.

OPTIMIZING FLAVONOID EXTRACTION FROM Curcuma xanthorrhiza WITH A SIMPLEX CENTROID DESIGN

Curcuma xanthorrhiza is a species of the genus Curcuma which is a medicinal ingredient in high demand in Indonesia and other countries. Chemical compounds such as flavonoids and their diverse bioactivity have triggered research that prioritizes quality and efficiency. This study was designed to optimize the extraction solvent in producing flavonoids from the rhizome of C. xanthorrhiza based on a simplex centroid design using Design Expert 13.0. Extractor solvents (water, acetone, ethanol, and methanol), as well as their combinations, were studied to test the total flavonoid content using the calorimetric aluminum chloride method by spectrophotometer. The experimental results with the special cubic model are a good and reliable fit for recovering flavonoids. The optimal conditions obtained were highly accurate at the desirability value of 1.00 with a mixed solvent of methanol (0.445) and ethanol (0.555), which resulted in total flavonoid content of 144.665 mg quercetin equivalent per gram dry weight. Methanol and ethanol combined can be an effective solvent option for extracting high amounts of active compounds (especially flavonoids) in C. xanthorrhiza rhizome.

Crystal Structure, Theoretical Analyses and Thermodynamic Properties of a Ni(II) Complex Based on ONO Donor Tridentate Acylhydrazone

A novel complex [Ni(C10H8O5N3)2]and#183;H2Oand#183;(CH3OH) (1) (C10H9O5N3= 2-[(4-nitro- benzoyl)-hydrazone]-propionic acid) has been prepared by reaction of NiCl2 with C10H9O5N3 in mixed solvent of methanol and water. The Ni(II) complex in octahedral geometry was characterized by elemental analysis and X-ray single crystal diffraction. Isothermal titration calorimetry (ITC) was performed to observe the reactions between Ni(II) and C10H9O5N3 in methanol solvents. The results showed that the binding constant (Ka), enthalpy change (ΔH), entropy change (ΔS), and Gibbs free energy change (ΔG) of the system are 5.2and#215;105, -11.82 kJand#183;mol-1, 69.78 Jand#183;mol-1and#183;K-1 and -32.62 kJand#183;mol-1, respectively. In addition, the structure was optimized and frontier molecular orbital (FMO) of (1) were analyzed by B3LYP and HF methods with 6-31g level.

Dual Detection of Temperature And Chiral Amino Acid Using Triphenylamine‐Based Fluorescent Probes

AbstractAccuracy measurement of temperature is important in day‐to‐day life and scientific research. Chiral amino acids play an irreplaceable role in medicine, biochemistry, and other fields; however, the polarity solvents do easily disturb hydrogen bond formation between chiral amino acids and fluorescence probe. Herein, a fluorescent probe Tap‐S, using triphenylamine as fluorophore, is synthesized for dual detection of temperature and enantiomers of chiral amino acids in polarity aqueous solution. The fluorescence emission of Tap‐S to the temperature has a good response in the mixed solvent of methanol and glycerin over a wide temperature range (−45 to 50 °C). The gradient thermosensitivity, accuracy and reversibility of Tap‐S to the temperature in our strategy are achieved. Tap‐S can emit yellow fluorescence in the high‐viscosity mixed solution. By taking advantage of the viscosity measurement, the restricted intramolecular rotation mechanism of Tap‐S's fluorescence emission was effectively clarified. Furthermore, the potential use of Tap‐S to selective detect L‐phenylalanine of chiral amino acids has been successfully executed in the polarity aqueous solution at the room temperature (25 °C). The complex of Tap‐S and L‐phenylalanine can inhibit the rotation of the single bond of Tap‐S inducing the fluorescence emission. This work provides a novel strategy for the studies on not only the detection of temperature but also the enantiomers of chiral amino acids.

Synthesis, molecular structural, optical, thermal and third harmonic nonlinear optical analysis of Piperazine-1,4-diium bis(2-carboxy-6-nitrobenzoate) tetrahydrate single crystal

Structure and molecular interactions of the title molecular salt (NPP) were established by X-ray diffraction. The elucidated structure model assigns centrosymmetric triclinic arrangement for the molecules. Molecular packing was established through robust O–H⋯O, N–H⋯O and C–H⋯O hydrogen bond network revealing infinite chains, sheets and spiral ladder patterns. The molecular patterns were abridged through C–H … π and π – π linkages expressing several S and R graph set motifs. Single crystals of NPP with defined morphology were grown by the method of slow evaporation from solution from 1: 1 mixed solvent of methanol and water. FT- IR, FT - Raman spectra reinforced the functional groups and with NMR spectra, the protonated-deprotonated nature of the title molecule. UV–visible, Urbach plot, photoluminescence and fluorescence spectral profiles endorsed the electronic transitions and photophysical properties of NPP. Z-scan profile in the closed and open aperture modes was deployed to estimate the magnitude of the third-order nonlinear optical constants. Thermogravimetry coupled with Differential Scanning Calorimetry (DSC) declare the optimal thermal stability of the material till 71.8 °C.

Three-dimensional ordered macroporous imprinted polymer for bisphenol A recognition.

A novel kind of three-dimensional ordered macroporous molecular imprinted polymer (3DOM MIP) was prepared and studied. Monodisperse silica microspheres were used to form silica crystal template via simple centrifuge. In the presence of template molecule, acrylamide and trimethylolpropane trimethacrylate were co-polymerized in the interstices of crystal template bisphenol A (BPA). Hydrofluoric acid were employed to etch silica crystal and the mixed solvent of methanol with acetic acid were employed to extract template molecule. The results of SEM and FTIR confirmed the successful synthesis of 3DOM MIP. The obtained 3DOM MIP exhibited a rapid adsorption kinetics and a specific adsorption capacities toward template molecule because of the small size of MIP wall, which possessed much more effective imprinted cavies. Meanwhile, 3DOM MIP could selective recognized BPA from its structural analogues.

Preparation of a porphyrin-polyoxometalate hybrid and its photocatalytic degradation performance for mustard gas simulant 2-chloroethyl ethyl sulfide

By combining 5,10,15,20-tetra(4-chlorine)phenylporphyrin (TClPP) and α-Keggin polyoxometalate H5PV2Mo10O40 (H5PVMo) via a simple ion-exchange method, an organic-inorganic hybrid material [C44H28N4Cl4]1.5[H2PMo10V2O40]·2C2H6O (H2TClPP-H2PVMo) was prepared and thoroughly characterized by a variety of techniques. The homogeneous photocatalytic degradation of 2-chloroethyl ethyl sulfide (CEES) (5 µL) by H2TClPP-H2PVMo (1 × 10−6 mol/L) was studied in methanol and methanol-water mixed solvent (v/v = 1:1), in which the degradation rate of CEES reached 99.52% and 99.14%, respectively. The reaction followed first-order reaction kinetics, and the half-life and kinetic constant in methanol and the mixed solvent were respectively 33.0 min, −0.021 min−1 and 15.7 min, −0.043 min−1. Mechanism analysis indicated that under visible light irradiation in the air, CEES was degraded via oxidation and alcoholysis/hydrolysis in methanol and the mixed solvent. O2·− and 1O2 generated by H2TClPP-H2PVMo selectively oxidized CEES into a nontoxic sulfoxide. Singlet oxygen capture experiments showed that H2TClPP-H2PVMo (ϕ = 0.73) had a higher quantum yield of singlet oxygen than TClPP (ϕ = 0.35) under an air atmosphere and visible light irradiation.

Synthesis, DNA binding, apoptosis and molecular docking of a Mn(II) complex constructed by 2-(1,2,4-Triazol-1-yl)-4-picolinic acid

A new metal–organic complex (MOC), Mn(L)2·4H2O is successfully designed and synthesized by 2-(1,2,4-Triazol-1-yl)-4-picolinic acid ligand and Mn(NO3)2·4H2O in the mixed solvent of methanol and water. The complex was characterized by single-crystal X-ray diffraction, element analysis, Powder X-ray diffraction(PXRD). The binding constant between complex and DNA is 9.3 × 104, indicating that the complex and fish sperm DNA can bind well. Viscosity experiments prove that the complex interacts with DNA in an intercalation mode. Apoptosis and inverted microscope experiments show that the complex has obvious apoptotic effects on cancer cells. In general, the synthesized Mn(II) complex is of great significance to the treatment of cancer.

Antimalarial Activity of Sea Sponge Extract of Stylissa massa originating from waters of Rote Island

Research on the isolation, toxicity test, antimalarial test, and identification of the active compound from the ethyl acetate fraction of Stylissa massa sponge from Oenggae waters, Rote Island, has been conducted. This study aimed to investigate the antimalarial activity of the ethyl acetate fraction of the Stylissa massa sponge. Isolation was carried out by the extraction method using a mixed solvent of methanol: dichloromethane of 3: 2 (v/v), then the extract was partitioned in a solvent mixture of ethyl acetate: water of 1: 2 (v/v). The ethyl acetate extract obtained was separated by column chromatography using the gradient polarity system method. The toxicity test of each fraction was carried out by the Brine Shrimp Lethality Test (BSLT) method, and the antimalarial test was carried out by the haematin polymerization inhibition method. Identification of compounds from the active fraction in the antimalarial test was carried out using Liquid Chromatography-Mass Spectrometry (LC-MS). The extraction yield was 1.14 g (0.23%) of the ethyl acetate extract in the form of a dark brownish-yellow oily solid. Separation by column chromatography resulted in 15 fractions. Toxicity test results showed the four most active fractions with LC50 values, which are very promising for new drug discovery. The IC50 value in the antimalarial activity test of the four fractions indicated that the Stylissa massa sponge ethyl acetate extract was more active than the standard chloroquine compound (115 μg/mL). The LC-MS analysis indicates that fraction 11 contains two compounds that have been reported, and 1 compound is unknown. In contrast, fraction 14 indicates that it contains three compounds that have been reported and one unknown compound.

Experimental Measurement and Correlation of Solubilities of R-2[4-(6-Chloro-2-Benzoxazolyloxy)phenoxy]propanoic Acid in Methanol, Ethanol, and Methanol–Ethanol Mixed Solvents

The solubility of R-2[4-(6-chloro-2-benzoxazolyloxy)phenoxy]propanoic acid (abbreviated as Fenoxaprop-P) in methanol, ethanol and various methanol-ethanol mixed solvents have been experimentally measured in the temperature range from 273.15 to 323.15 K at atmospheric pressure using a laser monitoring observation technique. The experimental solubility of Fenoxaprop-P increases with increasing mole fraction of ethanol in the methanol–ethanol mixtures, which were analyzed by the solubility parameter. Experimental data were correlated with Buchowski–Ksiazczak λh equation and modified Apelblat equation. Computational results showed the Buchowski–Ksiazczak λh equation can fit the solubility data well. The dissolution enthalpy, entropy and Gibbs free energy of Fenoxaprop-P in methanol, ethanol and methanol-ethanol mixtures were also predicted by the Van’t Hoff and the Gibbs equation.

Construction of Metallacycle‐Linked Heteroarm Star Polymers via Orthogonal Post‐Assembly Polymerization and Their Intriguing Self‐Assembly into Large‐Area and Regular Nanocubes†

Summary of main observation and conclusionIn recent years, synthesis of hybrid heteroarm star polymer with precisely defined arms has evolved to be one of the most attractive topics within polymer chemistry. In this study, we present the successful synthesis of metallacycle‐linked heteroarm star polymers (HASPs) composed of crystalline poly(ε‐caprolactone) (PCL) and polyacrylate (poly (N‐isopropylacrylamide) (PNIPAM) segments via combination of ring‐opening polymerization (ROP) and reversible addition‐fragmentation chain transfer (RAFT) controlled radical polymerization. Firstly, a hexagonal metallacycle containing three hydroxy groups and three chain transfer agent moieties at the alternative vertexes was designed and synthesized based on the general principle of coordination‐driven self‐assembly. Subsequently, upon combination of two orthogonal post‐assembly polymerizations, a new family of HASPs containing a well‐defined hexagonal metallacycle with precisely controlled position of polymer arms was facilely prepared. Interestingly, the obtained HASPs could spontaneously self‐assemble into large‐area and regular cubic nanoparticles in tetrahydrofuran (THF)/methanol (MeOH) mixed solvents under specific conditions as confirmed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). This study provides a simple route to the controllable preparation of HASPs, and opens up a new way for further study on self‐assembly of different HASPs systems.

Stable Polyelectrolyte Humidity Sensors: Preparation and Application

Introduction Respiration monitoring is important for evaluating human health [1]. The human exhaled gas is always accompanied by high humidity, so humidity sensors are promising for respiration monitoring [2]. Importantly, a fast response to humidity change and good stability under high humidities must be guaranteed for the utilized humidity sensor. In order to achieve fast response and good stability, humidity sensors based on stable polyelectrolytes were prepared via in-situ thiol-ene click polymerization. This method provides a novel way for preparing high quality humidity sensors. Method The polyelectrolytes were prepared by thiol-ene click polymerization (Fig. 1). Mercaptopropyl polyhedral oligomeric silsesquioxane (50.0 mg), 1,4-divinylbenzene (30.0 mg), sodium p-styrene sulfonate hydrate (5.6 mg), and benzoin dimethyl ether (4.0 mg) were dissolved in mixed solvents of methanol (0.75 mL) and THF (0.5 mL). Then, the obtained mixture was drop-cast onto the ceramic plate interdigitated carbon electrodes. The substrates covered with precursor solution were irradiated under UV light (365 nm, 0.12 J/cm2) for 30 min. The cross-linked humidity sensors were then rinsed with the mixed solvents of methanol and THF to remove unreacted monomers and the catalyst. The thickness of the sensing film is ∼30 μm. Results and Conclusions The impedance results of PMDS and PPDS sensors in a batch were tested at different relative humidities (RHs) (Fig. 2a). There is only tiny response for these two sensors in the humidity range of 11-54% RH. At high humidity range, PPDS sensors show an incredibly small variation, while PMDS sensors show an impedance change of nearly 2 orders of magnitude. PMDS sensor’s response/recovery time between 33 and 95% RH is 0.29/0.47 s (Fig. 2b), and that of PPDS sensor is 0.75/0.48 s (Fig. 2c). In addition, the PMDS sensor shows good long-term response/recovery time stability and impedance stability. The PMDS sensor could distinguish the variation of breath rate and depth among a normal breath, a fast breath, a slow breath, a deep breath, a random breath, and a paused breath (Fig. 3). It is worthy to note that almost every cycle behaves inhaled and exhaled platforms. The signal equilibrium value is very important and beneficial to recognize the single inspiration and expiration.The polyelectrolytes were in situ cross-linked on the substrates with interdigitated electrodes successfully by thiol-ene click polymerization. The obtained optimum sensor shows high response and recovery speeds to humidity change and good stability. Different respiration patterns can be distinguished, and the breath rate/depth of detection subjects can also be determined by the sensor., which is meaningful in future diagnostic breath analysis. References Q.Trung, N.-E.Lee, Flexible and Stretchable Physical Sensor Integrated Platforms for Wearable Human-Activity Monitoring and Personal Healthcare. Adv. Mater. 28 (2016) 4338-4372. doi: 10.1002/adma.201504244.Kano, K.Kim, M.Fujii, Fast-Response and Flexible Nanocrystal-Based Humidity Sensor for Monitoring Human Respiration and Water Evaporation on Skin. ACS Sens. 2 (2017) 828−833. doi: 10.1021/acssensors.7b00199. Figure 1

Stepwise Fragmentation of Asymmetric Triangular Shape Ln3 Cluster and Magnetocaloric Effect of Gd3 Analogue

N-Methylbenzimidazole-2-methanol (L) and Ln(NO3)3·6H2O are dissolved in a mixed solvent of methanol and acetonitrile and then reacted at 80 °C to obtain [Ln3(L)5(NO3)4] (Ln3, Ln = Gd, Tb). In Ln3, three L− are located in the same plane as the three Ln3+ ions, and the other two L− are located above and below the plane, respectively. Two of the four NO3− ions are respectively coordinated with two Ln3+, and the other two are coordinated with one Ln3+ ion, which results in the asymmetry of the above-described triangular shape Ln3. When the Ln3 single crystal was tested by Electrospray Ionization Mass Spectrometry, the main frame [Ln3L5(NO3)3]+ was found to be stable, only one NO3−ion was lost. As the energy of the ion source increases, we observe the gradual fragmentation of the triangular shape Ln3, and propose that the fragmentation mechanism is: Ln3L5 → Ln3L4 → Ln2L4 → Ln2L3 → Ln2L2 → LnL. This provides the basis for the assembly of triangular shaped Ln3 clusters. For the first time, the magnetocaloric effect (MCE) of triangular Gd3 clusters was studied and it exhibited a large MCE of 10.65 J kg−1 K−1 at 7 K for ΔH = 5 T.

Solution thermodynamics of trans‑Cinnamic acid in (methanol + water) and (ethanol + water) mixtures at different temperatures

The gravimetric method was utilized here for obtaining the solubility of trans‑Cinnamic (t‑CA) under atmospheric pressure (p = 101.1 kPa) in water, methanol, ethanol and aqueous binary mixed solvents from T = (288.15 15 to 328.15) K. The solubility of t‑CA was strongly affected by both the mass ratio of the solvents and experimental temperature. The mole division solubility of t‑CA was observed to be most in pure ethanol at 328.15 K and least in unadulterated water at 288.15 K. The experimental values were regressed by the Jouyban−Acree, van't Hoff−Jouyban−Acree, Apelblat−Jouyban−Acree and Ma models. The biggest estimation of root-mean-square deviation was 1.94 × 10−3 and 4.11 × 10−3 and the relative normal deviation was 4.06 × 10−2 and 5.58 × 10−2 for the binary (ethanol + water) and (methanol + water) mixtures, respectively. Moreover, the disintegration enthalpy and disintegration entropy of t-CA in the comparing blended solvents were anticipated. The results may supply a basic theoretical guidance for industry.

Growth and characterization of organic 4-chlorobenzaldehyde-N- methyl 4-stilbazolium tosylate crystal: A promising material for nonlinear optical device applications

The organic crystal 4-chlorobenzaldehyde-N-methyl 4-stilbazolium tosylate (CMST) was grown from acetonitrile and methanol mixed solvent using slow cooling method for the first time. The optimum growth conditions based on different solution concentrations were investigated. The crystal atomic packing and bond length alternation (BLA) of CMST were identified through single crystal X-ray diffraction analysis, the calculated BLA value 0.1475 Å is close to optimum value for nonlinear optical (NLO) response. The composition and different functional groups of CMST compound were determined by 1H NMR and FT-IR studies. Moreover, the thermal stability and melting point were obtained through TG/DTG and DSC analyses. Important optical parameters such as optical transmittance, cut-off wavelength, absorption coefficient, band gap energy and refractive index were ascertained through UV–vis-NIR study, the low cut-off wavelength and wide optical transmittance of CMST crystal are favorable to optical device fabrication. The dielectric constant has been investigated. Green emission occurred at 521 nm was found through photoluminescence excitation study. These encouraging results suggest that the CMST crystal is a promising candidate for nonlinear optical device applications.

Solubility Determination and Modeling for 4-Nitrobenzonitrile in Binary Solvent Mixtures of Ethyl Acetate Plus (Methanol, Ethanol, n-Propanol, and Isopropanol)

The solubility of 4-nitrobenzonitrile in mixed solvents of (ethanol + ethyl acetate), (methanol + ethyl acetate), (isopropanol + ethyl acetate), and (n-propanol + ethyl acetate) over temperatures ranging from 278.15 to 318.15 K was obtained experimentally. From analysis results in the present study, we found that the equilibrium 4-nitrobenzonitrile solubility in the ethyl acetate (1) + (ethanol, methanol, isopropanol, and n-propanol) (2) mixed solvents increased with the temperature and the ethyl acetate composition increasing. The largest 4-nitrobenzonitrile solubility was in neat ethyl acetate at T = 318.15 K (1.346 × 10–3 in methanol, 1.082 × 10–2 in n-propanol, 1.159 × 10–2 in ethanol, 0.8765 × 10–3 in isopropanol, and 14.22 × 10–2 in ethyl acetate). The lowest 4-nitrobenzonitrile solubility was observed in neat isopropanol (0.1624 × 10–2 at T = 278.15 K). The solubility dependence on both ethyl acetate composition and temperature was mathematically described by the Apelblat–Jouyban–Acree, van’t Hoff–...

A New Nonlinear Optical Stilbazolium Family Crystal of (E)-1-Ethyl-2-(4-nitrostyryl) Pyridin-1-ium Iodide: Synthesis, Crystal Structure, and Its Third-Order Nonlinear Optical Properties

The derivative of an organic stilbazolium single crystal, (E)-1-ethyl-2-(4-nitrostyryl) pyridin-1-ium iodide (hereafter abbreviated as NSPI), was synthesized by the Knoevenagel condensation method. Single crystal of NSPI of size 13 × 12 × 3 mm3 were obtained from a 1:1 ratio of methanol and acetonitrile mixed solvent using the slow evaporation technique. X-ray structural analysis has indicated that NSPI crystallizes in the centric triclinic system with the P1 space group. In addition, Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopic analyses were carried out to confirm the molecular structure of the grown crystal. The small energy difference of the frontier molecular orbitals indicates the possible nonlinear optical properties present in the title crystal. Thermal studies confirm that the material has a good thermal stability of about 151 °C. Etching studies provide the layered growth of the NSPI crystal with fewer dislocations. The optical transmission range and the b...

Seven copper (I) complexes of diphosphine ligands and N^N ligands: Syntheses, structural characterizations and spectroscopic properties

The reactions of diphosphine ligands and nitrogen-containing ligands with Cu(I) salts in the mixed solvents of methanol (MeOH) and dichloromethane (CH2Cl2) generated the corresponding complexes, {[Cu(dppbe)(Bphen)](ClO4)·2CH3OH}n (1), {[Cu2(dppe)(dmp)2(CN)2]·2CH3OH}n (2), {[Cu2(dppb)(dmp)2I2]·2CH3OH}n (3), [Cu(POP)(C16H6N6)]I (4), {[Cu(POP)(C16H6N6)](SCN)}n (5), [Cu(xantphos)(bpy)](ClO4) (6) and {[Cu(xantphos)(bpy)](CF3SO3)}n (7) {dppbe=1,2-bis(diphenylphosphanyl)benzene, dppe=1,2-bis(diphenylphosphino)ethane; dppb=1,4-bis(diphenylphosphino)butane, POP=bis[2-(diphenylphosphino)phenyl]ether, xantphos=4,5-bis (diphenylphosphio)-9,9-dimethylxanthene, Bphen=4,7-diphenyl-1,10-phenanthroline, dmp=2,9-dimethyl-1,10-phenanthroline, C16H6N6=[2,3-f]-pyrazino-[1,10]phenanthroline-2,3-dicarbonitrile, bpy=2,2′-bipyridine}. These complexes were all characterized by single-crystal X-ray crystallography, elemental analysis, IR, 1H NMR spectroscopy, luminescence and THz spectroscopy. Complexes 1 and 2 consist of 1D infinite zigzag chain structures which are linked by hydrogen bonds, while complexes 3, 5 and 7 have 2D topological architectures which are connected by hydrogen bonds, complex 4 has an annular structure and complex 6 is a mononuclear structure. The types of hydrogen bonds, choice of solvents and coordination modes of the ligands are of importance in defining the structural and topological features of the resulting networks. Furthermore, complexes 1–7 exhibit interesting luminescence in the solid state at room temperature. Complexes 1–3 can act as yellow luminophores, complex 4 acts as a red luminophore, complex 5 acts as an orange luminophore and complexes 6–7 act as green luminophores. Their terahertz spectra show more accurate characteristics of their structures.

Solubility of Benzoin in Six Monosolvents and in Some Binary Solvent Mixtures at Various Temperatures

The solubility of benzoin in monosolvents (acetone, ethyl acetate, methanol, ethanol, 1-propanol, and 1-butanol) and binary solvent mixtures (ethyl acetate + methanol, ethyl acetate + ethanol) was measured using UV–vis spectroscopy at temperatures ranging from 283.15 K to 323.15 K. It can be seen from the data that the solubility of benzoin increases expectedly as temperature increases in a given solvent or solvent mixture, the solubility in acetone is maximum among six monosolvents which could be well explained by the existence of strong H-bonds, rather than the “like dissolves like” rule. In binary solvent mixtures, the solubility reaches maximum when the mole fraction of methanol is 0.1 in ethyl acetate + methanol mixed solvents, while the maximum exhibits at 0.2 of mole fraction of ethanol in ethyl acetate + ethanol. The solubility parameter was interpreted as the cosolvency of benzoin solubility in binary solvent mixtures. The solubility data were correlated by modified Apelbalt equation, CNIBS/R-K e...