The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more...The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more precise lattice parameters using the interaction points for the pseudo-Kossel pattern obtained from laser-induced X-ray diffraction(XRD).This method has been validated by the analysis of an XRD experiment conducted on iron single crystals.Furthermore,the method was used to calculate the compression ratio and rotated angle of an LiF sample under high pressure loading.This technique provides a robust tool for in-situ characterization of structural changes in single crystals under extreme conditions.It has significant implications for studying the equation of state and phase transitions.展开更多
The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compou...The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compounds were characterized by elemental analysis, IR, 1H NMR and X-ray structural determination.展开更多
Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This pa...Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This paper describes the preparation of type I crystal and its single crystal diffraction data, the comparison of the powder diffraction data for both type I and II crystals as well as their stability and solubility in methanol.展开更多
Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with c...Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with copper（Ⅱ） perchlorate hexahydrate in methanol, acetonitrile and water mixture as solvent. Slow evaporation of the filtered reaction mixture in air produced blue color block crystals suitable for single crystal X-ray diffraction study of the title complex. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell parameters, α = 8.1269（1） ,A, b = 21.8348（2）A, c = 9.1522（1） A, a = γ= 90° , β = 99.7611 （4）°. The structure of the compound was characterized by IR Spectroscopy, elemental analysis and single crystal X-ray diffraction analysis.展开更多
New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been s...New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been synthesized by reaction of cobalt(III) salt and the ligand, in amounts equal to metal-ligand molar ratio of 1:2. Both the Schiff base and the complex of Co(III) were characterized by IR, UV-Vis, 1H NMR- and 13C NMR-spectroscopy techniques. Single crystal X-ray diffraction investigation, at low temperature T = 120 K, shows that the cobalt complex is triclinic P-1, a = 10.426(5) ?, b = 11.3234(2) ?, c = 15.729(5) ?, α(°) = 70.102(4), β(°) = 86.049(4), γ(°) = 82.497(4), Z = 2, and its structure consists of isolated [Co(III)(C13H13N2O3)2]+ complex cations with distorted octahedral geometry, ClO-4 counter anions, acetone solvent and water molecules. The crystal cohesion is stabilized by hydrogen bonds between ligands and water molecules, and ionic interactions between complex cations and counter anions.展开更多
Fast,precise structure determination of unknown compounds has been the foundation but with a persistent challenge in the field of chemical research.Among various chemical characterization techniques,single-crystal X-r...Fast,precise structure determination of unknown compounds has been the foundation but with a persistent challenge in the field of chemical research.Among various chemical characterization techniques,single-crystal X-ray diffraction(SCXRD)stands out as the most straightforward and accurate method in modern structural chemistry.By precisely determining the three-dimensional arrangement of atoms within a crystal,it provides direct atomic-level evidence for understanding the relationship between material structure and properties[1].展开更多
Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- a...Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- and 2D-NMR and X-ray single crystal diffraction. Compounds 1-3 showed antibacterial activity against Mycobacterium smegmatis.展开更多
The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine...The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4, 6-dichloro-2-methyl-5-{1-[1-(2- oxo-tetrahydro-imidazolyl)]-acetyene}-aminopyrimidine as by-product. No 4, 6-dichloro-2- methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi- cation-addition-elimination mechanism.展开更多
An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-o...An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.展开更多
Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twi...Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twigs and leaves of Tabernaemontana divaricata.Their structures were established on the basis of spectroscopic data interpretation,single crystal X-ray diffraction analysis and circular dichroism spectrum.展开更多
A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crysta...A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.展开更多
A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined...A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.展开更多
A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-sti...A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.展开更多
Structural determination plays a pivotal role in chemical research by providing detailed insights into molecular architecture and functionality.Single-crystal X-ray diffraction(SCXRD)is widely regarded as the premier ...Structural determination plays a pivotal role in chemical research by providing detailed insights into molecular architecture and functionality.Single-crystal X-ray diffraction(SCXRD)is widely regarded as the premier technique for achieving precise three-dimensional structural elucidation[1].The persistent challenge of determining atomic-level structures for non-crystalline or conformationally flexible molecules has driven transformative innovations in crystallographic methodologies[2-5].展开更多
Copper/silver-containing chalcogenides have recently attracted significant interest for their promising thermoelectric applications.In this article,we report the syntheses of five new layered quaternary Cu/Ag-containi...Copper/silver-containing chalcogenides have recently attracted significant interest for their promising thermoelectric applications.In this article,we report the syntheses of five new layered quaternary Cu/Ag-containing chalcogenides:SrScCuSe_(3),SrScCuTe_(3),BaScCuSe_(3),BaScCuTe_(3),and BaScAgTe_(3).The single-crystal X-ray diffraction studies show that all the Cu-containing compounds are isostructural and crystallize in the orthorhombic crystal system in the Cmcm space group.Interestingly,the crystal structure of isoelectronic BaScAgTe_(3)does not adopt the same structure type as observed for AkScCuQ_(3)(Ak=Sr/Ba;Q=Se/Te).展开更多
The four main stable isotopes of the[^(A)Dy(tta)_(3)(L)]·C_(6)H_(14)(^(A)Dy with A=161-164)Single-Molecule Magnet(SMM)(tta^(−)=2-thenoyltrifluoroacetylacetonate and L=2-{[2-methylpyridiyl]-4,5-[4,5-bis(propylthio...The four main stable isotopes of the[^(A)Dy(tta)_(3)(L)]·C_(6)H_(14)(^(A)Dy with A=161-164)Single-Molecule Magnet(SMM)(tta^(−)=2-thenoyltrifluoroacetylacetonate and L=2-{[2-methylpyridiyl]-4,5-[4,5-bis(propylthio)-tetrathiafulvalenyl]-1H-benzimidazol-2-yl}pyridine)have been magnetically investigated and structurally characterized by single crystal X-ray diffraction.The two nuclear spin-free ^(162/164)Dy behave the same from a dynamic magnetic point of view and with slower magnetic relaxation than the two pure magnetically active isotopically substituted ^(161/163)Dy.In addition,this paper demonstrates that ^(161)Dy and ^(163)Dy relax differently even if they both carry I=5/2 nuclear spin.After the release of the dipolar interactions through magnetic dilution,([^(161)Dy_(0.05)Y_(0.95)(tta)_(3)(L)]·C_(6)H_(14))(^(161)Dy@Y)relaxes four times slower than ^(163)Dy@Y due to different hyperfine coupling constants.展开更多
A series of three mono-dimensional polymers[Dy(hfac)_(3)((S/R)-L^(2))]n((S/R)-2),[Dy(hfac)_(3)((S/R)-L^(3))]n((S/R)-3)and[Dy(hfac)_(3)((S/R)-L4)]n((S/R)-4)involving different binaphthyl-2,2′-diyl phosphate ligands((S...A series of three mono-dimensional polymers[Dy(hfac)_(3)((S/R)-L^(2))]n((S/R)-2),[Dy(hfac)_(3)((S/R)-L^(3))]n((S/R)-3)and[Dy(hfac)_(3)((S/R)-L4)]n((S/R)-4)involving different binaphthyl-2,2′-diyl phosphate ligands((S/R)-L^(2–4))were designed from our pioneer reported system of formula[Dy(hfac)_(3)((S/R)-L^(1))]n((S/R)-1).The single-crystal X-ray diffraction structures revealed that the final compounds are in their enantiopure form with the ligands bearing the same chirality in the free and coordinated mode.All the polymers can be described as assemblies of mononuclear single-molecule magnets(SMM)in both zero and applied magnetic field.The fitting of the thermal dependence of the relaxation times shows that magnetic relaxation takes place through a combination of thermally activated mechanism(Raman)and quantum tunneling of the magnetization(QTM in zero applied magnetic field).The effect of the nature of the antenna and the number of chiral centres of the BINOL-derived bisphosphate ligands on both chiroptical and magnetic properties were studied.Photophysical and magnetic properties were rationalized by TD-DFT and ab initio calculations.Finally magneto-structural correlations between Dy(III)luminescence,calculations and magnetism were performed.展开更多
Three new chalcohalide nonlinear optical crystals,[ASr_(4)Cl][Ge_(3)S_(10)](A=Na,K)and[KBa_(4)Cl][Ge_(3)S_(10)],have been successfully designed and synthesized by combining the covalent[Ge_(3)S_(9)]clusters and ionic[...Three new chalcohalide nonlinear optical crystals,[ASr_(4)Cl][Ge_(3)S_(10)](A=Na,K)and[KBa_(4)Cl][Ge_(3)S_(10)],have been successfully designed and synthesized by combining the covalent[Ge_(3)S_(9)]clusters and ionic[AB_(4)Cl]frameworks.Their crystal structures were determined by single crystal X-ray diffraction,which showed that all three compounds crystallized in the noncentrosymmetric and polar space group of P6_(3).展开更多
The atom-level manipulation of atomically precise metal nanoclusters(NCs)has attracted considerable attention due to its potential for facilitating the elucidation of structure-property relationships.Herein,we report ...The atom-level manipulation of atomically precise metal nanoclusters(NCs)has attracted considerable attention due to its potential for facilitating the elucidation of structure-property relationships.Herein,we report two atomically precise gold NCs,[Au_(9)(DPPF)_(4)]Cl_(3)(DPPF=bis(diphenylphosphino)ferrocene)(Au_(9))and[Au_(8)(DPPF)_(4)]Cl_(2)(Au_(8)),identified by single-crystal X-ray diffraction(SCXRD)and electrospray ionization mass spectrometry(ESI-MS).SCXRD analysis revealed that the two gold NCs contain a similar Au_(8)unit enclosed by a tetrahedral framework consisting of four DPPF ligands,and the only difference is the addition of a gold atom on the kernel surface of the Au_(9)NC,which can be resected to form the Au_(8)NC.This represents the achievement of precise atomic“tailoring”of the surface of a kernel of a gold NC without altering the other parts of the structure.Notably,the two NCs allow for the identification of free valence electrons(6e).A further investigation into their electronic structures and electrocatalytic CO_(2)reduction reaction activity was performed to explore the functionality of such minimal kernel tailoring at the atomic level.This study not only enriches the family of diphosphine-protected small-sized gold NCs but also realizes the atomic-level tailoring of specific sites on a nanoparticle.展开更多
Here we report the synthesis and structural characterization of four[7]rotaxanes formed by coordinating hybrid inorganic-organic[2]rotaxanes to a central{Ni_(12)}core.X-ray single crystal diffraction demonstrate that[...Here we report the synthesis and structural characterization of four[7]rotaxanes formed by coordinating hybrid inorganic-organic[2]rotaxanes to a central{Ni_(12)}core.X-ray single crystal diffraction demonstrate that[7]rotaxanes are formed,with a range of conformations in the crystal.Small angle X-ray scattering supported by molecular dynamic simulations demonstrates that the large molecules are stable in solution and also show that the conformers present in solution are not those found in the crystal.Pulsed EPR spectroscopy show that phase memory times for the{Cr_(7)Ni}rings,which have been proposed as qubits,are reduced but not dramatically by the presence of the{Ni_(12)}cage.展开更多
基金National Natural Science Foundation of China(12102410)Fund of National Key Laboratory of Shock Wave and Detonation Physics(JCKYS2022212005)。
文摘The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more precise lattice parameters using the interaction points for the pseudo-Kossel pattern obtained from laser-induced X-ray diffraction(XRD).This method has been validated by the analysis of an XRD experiment conducted on iron single crystals.Furthermore,the method was used to calculate the compression ratio and rotated angle of an LiF sample under high pressure loading.This technique provides a robust tool for in-situ characterization of structural changes in single crystals under extreme conditions.It has significant implications for studying the equation of state and phase transitions.
基金We are grateful to the National Natural Science Foundation of China(project 20072034)the Foundation for Young Teacher in Zhenzhou University for the financial support.
文摘The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compounds were characterized by elemental analysis, IR, 1H NMR and X-ray structural determination.
文摘Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This paper describes the preparation of type I crystal and its single crystal diffraction data, the comparison of the powder diffraction data for both type I and II crystals as well as their stability and solubility in methanol.
文摘Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with copper（Ⅱ） perchlorate hexahydrate in methanol, acetonitrile and water mixture as solvent. Slow evaporation of the filtered reaction mixture in air produced blue color block crystals suitable for single crystal X-ray diffraction study of the title complex. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell parameters, α = 8.1269（1） ,A, b = 21.8348（2）A, c = 9.1522（1） A, a = γ= 90° , β = 99.7611 （4）°. The structure of the compound was characterized by IR Spectroscopy, elemental analysis and single crystal X-ray diffraction analysis.
文摘New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been synthesized by reaction of cobalt(III) salt and the ligand, in amounts equal to metal-ligand molar ratio of 1:2. Both the Schiff base and the complex of Co(III) were characterized by IR, UV-Vis, 1H NMR- and 13C NMR-spectroscopy techniques. Single crystal X-ray diffraction investigation, at low temperature T = 120 K, shows that the cobalt complex is triclinic P-1, a = 10.426(5) ?, b = 11.3234(2) ?, c = 15.729(5) ?, α(°) = 70.102(4), β(°) = 86.049(4), γ(°) = 82.497(4), Z = 2, and its structure consists of isolated [Co(III)(C13H13N2O3)2]+ complex cations with distorted octahedral geometry, ClO-4 counter anions, acetone solvent and water molecules. The crystal cohesion is stabilized by hydrogen bonds between ligands and water molecules, and ionic interactions between complex cations and counter anions.
基金the National Natural Science Foundation of China(Nos.22471014 and 22271013)the Beijing Natural Science Foundation(No.2232024)for financial support.
文摘Fast,precise structure determination of unknown compounds has been the foundation but with a persistent challenge in the field of chemical research.Among various chemical characterization techniques,single-crystal X-ray diffraction(SCXRD)stands out as the most straightforward and accurate method in modern structural chemistry.By precisely determining the three-dimensional arrangement of atoms within a crystal,it provides direct atomic-level evidence for understanding the relationship between material structure and properties[1].
基金supported by the 973 Program(Nos.2010CB833802 and 2012CB721005)the National Science Fund for Distinguished Young Scholars(No.30325044)the Natural Science Foundation of China(No.81373304)
文摘Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- and 2D-NMR and X-ray single crystal diffraction. Compounds 1-3 showed antibacterial activity against Mycobacterium smegmatis.
文摘The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4, 6-dichloro-2-methyl-5-{1-[1-(2- oxo-tetrahydro-imidazolyl)]-acetyene}-aminopyrimidine as by-product. No 4, 6-dichloro-2- methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi- cation-addition-elimination mechanism.
文摘An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.
基金This work was financially supported by the“Large-scale Compound Library”project of National Development and Reform Commission of China.
文摘Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twigs and leaves of Tabernaemontana divaricata.Their structures were established on the basis of spectroscopic data interpretation,single crystal X-ray diffraction analysis and circular dichroism spectrum.
文摘A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.
文摘A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.
文摘A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.
文摘Structural determination plays a pivotal role in chemical research by providing detailed insights into molecular architecture and functionality.Single-crystal X-ray diffraction(SCXRD)is widely regarded as the premier technique for achieving precise three-dimensional structural elucidation[1].The persistent challenge of determining atomic-level structures for non-crystalline or conformationally flexible molecules has driven transformative innovations in crystallographic methodologies[2-5].
基金financial support under the early career research(ECR)award(Grant number:ECR/2017/000822)IIT Hyderabad for seed grant and research facilities.MI and SJ thank DST India and MOE,IIT Hyderabad for the research fellowships.The authors also gratefully acknowledge DST-FIST(SR/FST/ETI-421/2016)for the SEM-EDS facilityDST-FIST(SR/FST/PSI-215/2016)for com-putational resources used in this work.The authors thank Gopabandhu Panigrahi(Dept.of Chemistry,IIT Hyderabad)for helping in the preparation of samples for SEM and EDS studies.
文摘Copper/silver-containing chalcogenides have recently attracted significant interest for their promising thermoelectric applications.In this article,we report the syntheses of five new layered quaternary Cu/Ag-containing chalcogenides:SrScCuSe_(3),SrScCuTe_(3),BaScCuSe_(3),BaScCuTe_(3),and BaScAgTe_(3).The single-crystal X-ray diffraction studies show that all the Cu-containing compounds are isostructural and crystallize in the orthorhombic crystal system in the Cmcm space group.Interestingly,the crystal structure of isoelectronic BaScAgTe_(3)does not adopt the same structure type as observed for AkScCuQ_(3)(Ak=Sr/Ba;Q=Se/Te).
基金supported by the CNRS,Universitéde Rennes and the European Research Council through the ERC-CoG 725184 MULTIPROSMM(project no.725184).
文摘The four main stable isotopes of the[^(A)Dy(tta)_(3)(L)]·C_(6)H_(14)(^(A)Dy with A=161-164)Single-Molecule Magnet(SMM)(tta^(−)=2-thenoyltrifluoroacetylacetonate and L=2-{[2-methylpyridiyl]-4,5-[4,5-bis(propylthio)-tetrathiafulvalenyl]-1H-benzimidazol-2-yl}pyridine)have been magnetically investigated and structurally characterized by single crystal X-ray diffraction.The two nuclear spin-free ^(162/164)Dy behave the same from a dynamic magnetic point of view and with slower magnetic relaxation than the two pure magnetically active isotopically substituted ^(161/163)Dy.In addition,this paper demonstrates that ^(161)Dy and ^(163)Dy relax differently even if they both carry I=5/2 nuclear spin.After the release of the dipolar interactions through magnetic dilution,([^(161)Dy_(0.05)Y_(0.95)(tta)_(3)(L)]·C_(6)H_(14))(^(161)Dy@Y)relaxes four times slower than ^(163)Dy@Y due to different hyperfine coupling constants.
基金supported by the CNRS,Universitéde Rennes 1 and the European Commission through the ERC-CoG 725184 MULTIPROSMM(project no.725184)the French GENCI/IDRIS-CINES centre for high-performance computing resources.
文摘A series of three mono-dimensional polymers[Dy(hfac)_(3)((S/R)-L^(2))]n((S/R)-2),[Dy(hfac)_(3)((S/R)-L^(3))]n((S/R)-3)and[Dy(hfac)_(3)((S/R)-L4)]n((S/R)-4)involving different binaphthyl-2,2′-diyl phosphate ligands((S/R)-L^(2–4))were designed from our pioneer reported system of formula[Dy(hfac)_(3)((S/R)-L^(1))]n((S/R)-1).The single-crystal X-ray diffraction structures revealed that the final compounds are in their enantiopure form with the ligands bearing the same chirality in the free and coordinated mode.All the polymers can be described as assemblies of mononuclear single-molecule magnets(SMM)in both zero and applied magnetic field.The fitting of the thermal dependence of the relaxation times shows that magnetic relaxation takes place through a combination of thermally activated mechanism(Raman)and quantum tunneling of the magnetization(QTM in zero applied magnetic field).The effect of the nature of the antenna and the number of chiral centres of the BINOL-derived bisphosphate ligands on both chiroptical and magnetic properties were studied.Photophysical and magnetic properties were rationalized by TD-DFT and ab initio calculations.Finally magneto-structural correlations between Dy(III)luminescence,calculations and magnetism were performed.
基金supported by the National Natural Science Foundation of China(Grant No.52172006,22071179,51972230,51890864 and 51890865)the Natural Science Foundation of Tianjin(Grant No.20JCJQJC00060 and 21JCJQJC00090).
文摘Three new chalcohalide nonlinear optical crystals,[ASr_(4)Cl][Ge_(3)S_(10)](A=Na,K)and[KBa_(4)Cl][Ge_(3)S_(10)],have been successfully designed and synthesized by combining the covalent[Ge_(3)S_(9)]clusters and ionic[AB_(4)Cl]frameworks.Their crystal structures were determined by single crystal X-ray diffraction,which showed that all three compounds crystallized in the noncentrosymmetric and polar space group of P6_(3).
基金supported by the National Natural Science Foundation of China(22371108,21971246,22209002)the Taishan Scholar Foundation of Shandong Province(tsqn202211242)the Natural Science Foundation of Shandong Province(ZR2024MB125,ZR2024MB007,ZR2024QB238,and ZR2020QB031).
文摘The atom-level manipulation of atomically precise metal nanoclusters(NCs)has attracted considerable attention due to its potential for facilitating the elucidation of structure-property relationships.Herein,we report two atomically precise gold NCs,[Au_(9)(DPPF)_(4)]Cl_(3)(DPPF=bis(diphenylphosphino)ferrocene)(Au_(9))and[Au_(8)(DPPF)_(4)]Cl_(2)(Au_(8)),identified by single-crystal X-ray diffraction(SCXRD)and electrospray ionization mass spectrometry(ESI-MS).SCXRD analysis revealed that the two gold NCs contain a similar Au_(8)unit enclosed by a tetrahedral framework consisting of four DPPF ligands,and the only difference is the addition of a gold atom on the kernel surface of the Au_(9)NC,which can be resected to form the Au_(8)NC.This represents the achievement of precise atomic“tailoring”of the surface of a kernel of a gold NC without altering the other parts of the structure.Notably,the two NCs allow for the identification of free valence electrons(6e).A further investigation into their electronic structures and electrocatalytic CO_(2)reduction reaction activity was performed to explore the functionality of such minimal kernel tailoring at the atomic level.This study not only enriches the family of diphosphine-protected small-sized gold NCs but also realizes the atomic-level tailoring of specific sites on a nanoparticle.
基金supported by the EPSRC(EP/R043701/1)including an Established Career Fellowship(EP/R011079/1)to REPWREPW also thanks the European Research Council for an Advanced Grant(ERC-2017-ADG-786734)+2 种基金We also thank the EPSRC for an X-ray diffractometer(EP/K039547/1)the National Research Facility for EPR(EP/W014521/1 and EP/V035231/1)We thank the University of Manchester for a President's Scholarship(to TSB).
文摘Here we report the synthesis and structural characterization of four[7]rotaxanes formed by coordinating hybrid inorganic-organic[2]rotaxanes to a central{Ni_(12)}core.X-ray single crystal diffraction demonstrate that[7]rotaxanes are formed,with a range of conformations in the crystal.Small angle X-ray scattering supported by molecular dynamic simulations demonstrates that the large molecules are stable in solution and also show that the conformers present in solution are not those found in the crystal.Pulsed EPR spectroscopy show that phase memory times for the{Cr_(7)Ni}rings,which have been proposed as qubits,are reduced but not dramatically by the presence of the{Ni_(12)}cage.
