Synthesis, crystal structure and fluorescence spectrum of some new 1,2,3-triazol-xanthen-3-one derivatives

In this paper, a novel hybrid material, entitled histaminium bis(trioxonitrate), with the general chemical formula (C5H11N3)(NO3)2, denoted by HTN was presented. Single-crystal X-ray diffraction was used to determine the structural characteristics of this compound after it was made using a slow evaporation method at room temperature. This compound was elaborated and crystallized to the monoclinic system with space group P21/c, and the lattice parameters obtained were: a = 10.4807 (16)Å, b = 11.8747 (15)Å, c = 16.194 (2)Å, β = 95.095 (6)°, V = 2007.4 (5)Å3 and Z = 8. The title compound’s atomic structure couldbe modeled as a three-dimensional network. Organic cations and nitrate anions were connected via N–H...O and C–H...O hydrogen bonds in the HTN structure. The intermolecular interactions responsible for the formation of crystal packing were evaluated using Hirshfeld surfaces and two-dimensional fingerprint plots. The compound’s infrared spectrum, which ranged from 4000 to 400 cm−1, confirmed the presence of the principal bands attributed to the internal modes of the organic cation and nitrate anions. Additionally, spectrofluorimetry and the ultraviolet–visible spectrum was used to investigate this compound. DFT calculations were used to evaluate the composition and properties of HTN. The energy gap, chemical reactivity and crystal stability of HTN were quantified by performing HOMO-LUMO frontier orbitals analysis. Topological analysis (AIM), Reduced Density Gradient (RDG), molecular electrostatic potential surface (MEPS) and Mulliken population were processed to determine the types of non-covalent interactions, atomic charges and molecular polarity in detail.

Reliable evaluation of molecular structure of methyl 3-O-nitro-α-d-glucopyranoside and its intermediates by means of solid-state NMR spectroscopy and DFT optimization in the absence of appropriate crystallographic data

The title compound has been prepared and characterized by elemental analyses, infrared and NMR spectra, and thermal analyses. The crystal and molecular structure of tris(N′‐ethyl‐N‐piperazinly‐carbodithioato‐s,s′)cobalt(III) complex, Co(S2CNC4H8NC2H5)3·3H2O, was determined by X‐ray diffraction methods. The compound crystallizes in trigonal system, space group R‐3, with lattice parameters a=1.37700(19) nm, b=1.37700(19) nm, c=3.0090(6) nm, γ=120°, Mr=680.98, V=4.9411(14) nm3, Z=6, Dc=1.373 g/cm3, F(000)=2160, R=0.0510 and wR=0.1436. In the structure, central Co atom coordination geometry is slightly distorted octahedron with the six S atoms from the three bidentate S2CNC4H8NC2H5 ligands. The octahedron is distorted resulting from forced configuration of the four‐membered chelate ring. The six CoS bond distances are in the range of 0.22682(13)‐0.22703(14) nm. The IR and NMR spectral data are in agreement with the structural data. The thermal analytical data indicate that it decomposed completely at the temperature of 799.97 °C, leaving CoS.

A new compound (CHZ)(HTNPG)·0.5H2O was synthesized by mixing carbohydrazide(CHZ) and trinilrophloroglucinol(TNPG) and characterized by elemental analysis and Fourier transform infrared (FTIR) spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, P space group, with a=0.45578(9) nm, b=1.0142(2) nm, c=1.3041(3) nm, α=86.53(3)°, β=99.56(3)°, γ=81.94(3)°, V= 0.5958(2) nm3, Z=2, Dc=2.008 g/cm3, R1,=0.0476, and wR2=0.1139. The compound is a di-substituted salt of TNPG, which consists of a cation (CHZ)2+ and an anion (HTNPG)2+. The thermal analysis of the compound was studied by means of differential scanning calorimetry(DSC) and thermogravimetry-derivative thermogravimetry(TG-DTG). Under nitrogen atmosphere at a heating rate of 10 °C/min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140—232 °C on the DSC trace. The decomposition products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between (CHZ)2+ and (HTNPG)2- enhance the thermal stability of the title compound.

The crystal structure of 9-(4-methoxyphenyl)-3,3-dimethyl-10-(4-methylphenyl)-1,2,3,4,5,6,7,8,9,10- decahydroacridin-1,8-dione is determined by X-ray diffraction at 153(2) K. The title compound 1, C22H21N5O6, is triclinic, space group P-1, a = 9.6382(15) A, b = 11.5847(15) A, c = 12.4722(11) A, α = 66.075(9)°, β = 70.176(9)°, γ = 85.800(13)°, Z = 2, V = 1194.1(3) A3. It is interesting that the central pyridine ring of the acridine moiety is slightly distorted and adopts a boat conformation. The outer six-membered ring with two methyl groups adopts half-chair conformation, while another outer partially saturated six-membered ring adopts distorted boat form. In addition, the un-classical hydrogen bonds of C–H···O link the molecules forming polymers in the crystals. The crystal structure of 9-(4-methoxyphenyl)-3,3-dimethyl-10-(4-methylphenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacridin-1,8-dione is determined by X-ray diffraction. The title compound 1, C22H21N5O6, is triclinic, space group P-1, a = 9.6382 (15) A, b = 11.5847(15) A, c = 12.4722(11) A, α = 66.075(9) o, β = 70.176 (9) o, γ = 85.800 (13) o, Z = 2, V = 1194.1(3) A3. It is interesting that the central pyridine ring of the acridine moiety is slightly distorted and adopts a boat conformation. The outer six-membered ring with two methyl groups adopts half-chair conformation, while another outer partially saturated six-membered ring adopts distorted boat form. In addition, the un-classical hydrogen bonds of C–H···O link the molecules forming polymers in the crystals.

The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C18H21NO3, M r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) A, β = 92.056(2)°, V = 1,632.4(3) A3, Z = 4, D c = 1.218 g cm−3, λ = 0.71073 A, μ(Mo Kα) = 0.083 mm−1, F(000) = 640. The final refinement gave R = 0.0497, wR(F 2) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity. The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C18H21NO3, M r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) A, β = 92.056(2)°, V = 1,632.4(3) A3, Z = 4, D c = 1.218 g cm−3, λ = 0.71073 A, μ(Mo Kα) = 0.083 mm−1, F(000) = 640. The final refinement gave R = 0.0497, wR(F 2) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.

The title compound has been prepared and characterized by P1PHNMR, FT-IR, fluorescence spectrum and thermal analysis. The crystal and molecular structures of dimethyl-(4-(7-acetoxyl-2H -chromen-2-one))-methyl-(2-acrylate)-ethyl-ammonium bromide were determined by X-ray diffraction methods. The compound crystallizes in Monoclinic system, space group C2/c, with lattice parameters a = 22.799(5), b =12.122(2), c =14.580(3) Å, β = 90.76(3)°, Mr = 440.29, V = 4029.1(14) ÅP3P, Z = 8, Dc= 1.452 g/cmP3P, F(000) = 1808, R = 0.0679 and wR = 0.1450. In the structure, The four N-C bond distances are in the range of 1.473(6) ~ 1.531(6) Å. The P1PHNMR and FT-IR data are in agreement with the structural data. The title compound also shows good fluorescent behaviors. The fluorescent intensity changed little at pH ranging from 7.5 to 9.5. The pH value of the circulation cooling water is in this range so that the title compound can be used in tracer detection.

Cratoxylum formosum ssp. pruniflorum is a valuable species distributed in Yunnan and Guangxi Provinces of China. Thirteen compounds have been isolated from the bark of C. formosum ssp. pruniflorum. Their structures were identified on the basis of spectroscopic analysis and chemical evidence: epifriedelinol (2), vismiaquinone B (3), 3,8-dihydroxy-1,2,4trimethoxyxanthone (5), methyl-2,6-dihydroxy-3,4-dimethylbenzoate (6), 1,7-dihydroxy-4-methoxyxanthone (7), 11-hydroxy5-methoxy-2,2,9-trimethyl-2H-naphtho[1,2-b]pyran-7,12-dione (8), physcion (9), 1,8-dihydroxy-2-methoxyxanthone (10), vismione B (11), neriifolone C (12), and 1,7-dihydroxyxanthone (13). Compounds 1 and 4 were identified by direct comparison with authentic samples as -sitosterol and friedelin, respectively. Among them, compounds 1, 2–6, 10, 11, and 13 were isolated from C. formosum ssp. pruniflorum for the first time. The air-dried and powdered bark of Cratoxylum formosum ssp. pruniflorum (7.0 kg) were extracted with 95% aqueous ethanol and filtered at room temperature. The filtrate was concentrated and extracted with petroleum ether, then extracted by ethyl acetate. The petroleum ether extract (100 g) was subjected to silica gel column chromatography eluted with a petroleum ether–EtOAc (90:10 40:60) gradient system to furnish six fractions, G1–G6. All fractions were collected and combined by monitoring with TLC. Fraction G2 (21 g) was further chromatographed over RP-18 (MeOH–H2O 70:30 100:0) to provide subfractions G2a–G2c. Subfraction G2a was further chromatographed over silica gel using acetone–petroleum ether (10%) to give compounds 1 (7 mg) and 2 (20 mg). Then, in the same way, G2b and G2c were further separated to give compounds 3 (15 mg), 4 (17 mg), 5 (12 mg), 6 (10 mg), and 7 (10 mg). Subfraction G4 was treated in the same way to give compound 11 (11 mg). The ethyl acetate (250 g) extract was subjected to silica gel column chromatography eluted with a methanol–chloroform (100:1 5:1) gradient system to furnish five fractions, F1–F5. All fractions were collected and combined by monitoring with TLC. Fraction F3 was further chromatographed over RP-18 (MeOH–H2O 60:40 100:0) to provide subfractions F3a–F3b. The F3a part was further purified by Sephadex LH-20 (MeOH) to obtain compounds 6 (7 mg), 7 (13 mg), and 12 (15 mg). Then, in the same way, F3b was further separated to give compounds 8 (14 mg), 9 (13 mg), 10 (17 mg), and 13 (13 mg). Epifriedelinol (2), colorless amorphous powder, C30H52O. ESI-MS m/z 429 [M + H]+. The MS and NMR spectral data were consistent with those reported 1 . Vismiaquinone B (3), yellow amorphous powder, C21H20O6. ESI-MS m/z 369 [M + H] +. The MS and NMR spectral data were consistent with those reported 2 . 3,8-Dihydroxy-1,2,4-trimethoxyxanthone (5), yellow amorphous powder, C16H14O7. ESI-MS m/z 319 [M + H]+. The MS and NMR spectral data were consistent with those reported 3 . Methyl 2,6-dihydroxy-3,4-dimethylbenzoate (6), colorless amorphous powder, C10H12O4. ESI-MS m/z 197 [M + H] +. The MS and NMR spectral data were consistent with those reported 4 . 7-Dihydroxy-4-methoxyxanthone (7), yellow amorphous powder, C14H10O5. ESI-MS m/z 259 [M + H]+. The MS and NMR spectral data were consistent with those reported 5 . 11-Hydroxy-5-methoxy-2,2,9-trimethyl-2H-naphtho[1,2-b]pyran-7,12-dione (8), yellow amorphous powder, C21H18O5. ESI-MS m/z 351 [M + H] +. The MS and NMR spectral data were consistent with those reported 6 . Physcion (9), yellow amorphous powder, C16H12O5. ESI-MS m/z 285 [M + H]+. The MS and NMR spectral data were consistent with those reported 7 .

Room-temperature switchable materials showing multiple responses toward external stimuli are highly desired. Herein, we report bidirectional spin-state switch and fluorescence modulation of an Fe(I...

CdTe nanocrystals (CdTe NCs) were achieved by reaction of CdCl2 with KHTe solution and were capped with sodium mercaptoacetate. The product was detected by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive spectroscopy (EDS), fluorescence spectra, ultraviolet-visible spectra and X-ray diffraction (XRD). The CdTe NCs are of cubic structure and the average size is about 5 nm. The fluorescence quantum yield of CdTe NCs aqueous solution increased from 37% to 97% after 20 d under room light. The maximum λem of fluorescence changed from 543 nm to 510 nm and the blue shift was 33 nm. CdTe NCs aqueous solution can be steady for at least 10 months at 4 in° a refrigerator. The resonance Rayleigh scattering (RRS) of CdTe NCs in the aqueous solution was investigated. The maximum scattering peak was located at about 554 nm. The interactions of CdTe NCs with amikacin sulfate (AS) and micronomicin sulfate (MS) were investigated respectively. The effects of AS and MS on fluorescence and RRS of CdTe NCs were analyzed. It was found that AS and MS quenched the photoluminescence of CdTe NCs and enhanced RRS of CdTe NCs. Under optimum conditions, there are linear relationships between quenching intensity (F0-F), intensity of RRS (I-I0) and concentration of AS and MS. The detection limits (3б) of AS and MS are respectively 3.4 ng·mL−1 and 2.6 ng·mL−1 by the fluorescence quenching method, and 15.2 ng·mL−1 and 14.0 ng·mL−1 by the RRS method. The methods have high sensitivity, thus CdTe NCs may be used as fluorescence probes and RRS probes for the detection of aminoglycoside antibiotics.

The title compound 2,5,2′-triazido-1,1′-azo-1,3,4-triazole(2) has been synthesized by the reaction of 2,5,2′-trichloro-1,1′-azo-1,3,4-triazole(1) with sodium azide. Its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P−1 with a = 6.6604(13) A, b = 6.7035(13) A, c = 12.916 (3) A, α = 98.13(3)°, β = 95.56(3)°, γ = 106.48° V = 541.68(18) A3, Z = 2, C4HN17, Mr = 287.22, D c = 1.761 g cm−3, F(000) = 288 and μ(MoKa) = 0.140 mm−1, the final R = 0.0553 and wR = 0.1541. X-ray analysis indicates a stronger delocalization of the azo π bond along the hypothetical N4 moiety within the title compound than those in(E)-1,2-bis(2,6-diazido-9- azabicyclo[3.3.1]nonan-9-yl)diazene. The title compound 2,5,2′-triazido-1,1′-azo-1,3,4-triazole has been synthesized by the reaction of 2,5,2′-trichloro-1,1′-azo-1,3,4-triazole with sodium azide. Its crystal structure was determined by single-crystal X-ray diffraction. X-ray analysis indicates a stronger delocalization of the azo π bond along the hypothetical N4 moiety within the title compound than those in(E)-1,2-bis(2,6-diazido-9-azabicyclo[3.3.1] nonan-9-yl)diazene.

Synthesis, characterization and stereochemistry of N-acyl-r-2,c-4-bis(4-methoxyphenyl)-3-azabicyclo[3.3.1]nonanes

Phytochemical investigation on the roots of Asparagus cochinchinensis led to the isolation of one new furostanol saponin, named 26-O-β-d-glucopyranosyl-22α-hydroxyl-(25R)-Δ5(6)-furost-3β,26-diol-3-O-α-l-rhamnopyranosyl-(1 → 2)-[β-d-glucopyranosyl-(1 → 4)-α-l-rhamnopyranosyl-(1 → 4)]-β-d-glucopyranoside (1), along with three known congeners (2‒4). The structure of new saponin was elucidated via comprehensive inspection of its HRMS and NMR spectral data as well as chemical technology, whereas those of known ones were identified by comparison of their NMR and MS spectral data with those reported in literatures. All isolated saponins were evaluated for their cytotoxic effects on two human liver (MHCC97H) and lung adenocarcinoma (H1299) cancer cells in vitro. Among them, both 1 and 2 showed significant cytotoxicity against above mentioned cell lines. Further studies revealed that these two saponins could significantly inhibit their proliferation of MHCC97H and H1299 cells.Graphic

Study on the characterization and thermal conversion behavior of sequential extraction products from medium temperature coal pitch

Synthesis and application in solar cell of poly(3-octylthiophene)/titania nanotubes composite