Four new coordination polymers,{[Cd(mbtx)(4OHphCOO)]NO_(3)}n(1),{[Zn(mbtx)(1,4-bdc)_(0.5)(H_(2)O)_(2)]·(1,4-bdc)_(0.5)·4H_(2)O}n(2),{[Cd2(mbtx)(5NO_(2)-bdc)_(2)(H_(2)O)_(3)]·4.5H_(2)O}n(3),and{[Zn(H_(2)...Four new coordination polymers,{[Cd(mbtx)(4OHphCOO)]NO_(3)}n(1),{[Zn(mbtx)(1,4-bdc)_(0.5)(H_(2)O)_(2)]·(1,4-bdc)_(0.5)·4H_(2)O}n(2),{[Cd2(mbtx)(5NO_(2)-bdc)_(2)(H_(2)O)_(3)]·4.5H_(2)O}n(3),and{[Zn(H_(2)O)6][Zn_(2)(mbtx)_(2)(btc)_(2)(H_(2)O)_(4)]·2H_(2)O}n(4)(mbtx=1,3-bis(4H-1,2,4-triazole)benzene,4OHphCOO-=p-hydroxybenzoate,1,4-bdc2-=1,4-benzenedicarboxylate,5NO_(2)-bdc2-=5-nitro-isophthalate,btc3-=1,3,5-benzenetricarboxylate),were synthesized under room temperature condition and characterized by single-crystal X-ray diffraction,elemental analyses,and powder X-ray diffraction.Single-crystal X-ray structural analysis shows that complexes 1 and 3 are 2D networks.In 1,the adjacent 2D networks are linked to a 3D network byπ-πstacking interaction.2 and 4 exhibit 1D chains,and the 1D chains are connected into a 3D network byπ-πstacking interaction and intermolecular hydrogen bond.Luminescence and thermogravimetric analysis of the four complexes were discussed.CCDC:2416406,1;2416407,2;2416408,3;2416409,4.展开更多
Two-dimensional energetic materials(2DEMs),characterized by their exceptional interlayer sliding properties,are recognized as exemplar of low-sensitivity energetic materials.However,the diversity of available 2DEMs is...Two-dimensional energetic materials(2DEMs),characterized by their exceptional interlayer sliding properties,are recognized as exemplar of low-sensitivity energetic materials.However,the diversity of available 2DEMs is severely constrained by the absence of efficient methods for rapidly predicting crystal packing modes from molecular structures,impeding the high-throughput rational design of such materials.In this study,we employed quantified indicators,such as hydrogen bond dimension and maximum planar separation,to quickly screen 172DEM and 16 non-2DEM crystal structures from a crystal database.They were subsequently compared and analyzed,focusing on hydrogen bond donor-acceptor combinations,skeleton features,and intermolecular interactions.Our findings suggest that theπ-πpacking interaction energy is a key determinant in the formation of layered packing modes by planar energetic molecules,with its magnitude primarily influenced by the strongest dimericπ-πinteraction(π-π2max).Consequently,we have delineated a critical threshold forπ-π2max to discern layered packing modes and formulated a theoretical model for predictingπ-π2max,grounded in molecular electrostatic potential and dipole moment analysis.The predictive efficacy of this model was substantiated through external validation on a test set comprising 31 planar energetic molecular crystals,achieving an accuracy of 84%and a recall of 75%.Furthermore,the proposed model shows superior classification predictive performance compared to typical machine learning methods,such as random forest,on the external validation samples.This contribution introduces a novel methodology for the identification of crystal packing modes in 2DEMs,potentially accelerating the design and synthesis of high-energy,low-sensitivity 2DEMs.展开更多
采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometr...采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。展开更多
The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carri...The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.展开更多
文摘Four new coordination polymers,{[Cd(mbtx)(4OHphCOO)]NO_(3)}n(1),{[Zn(mbtx)(1,4-bdc)_(0.5)(H_(2)O)_(2)]·(1,4-bdc)_(0.5)·4H_(2)O}n(2),{[Cd2(mbtx)(5NO_(2)-bdc)_(2)(H_(2)O)_(3)]·4.5H_(2)O}n(3),and{[Zn(H_(2)O)6][Zn_(2)(mbtx)_(2)(btc)_(2)(H_(2)O)_(4)]·2H_(2)O}n(4)(mbtx=1,3-bis(4H-1,2,4-triazole)benzene,4OHphCOO-=p-hydroxybenzoate,1,4-bdc2-=1,4-benzenedicarboxylate,5NO_(2)-bdc2-=5-nitro-isophthalate,btc3-=1,3,5-benzenetricarboxylate),were synthesized under room temperature condition and characterized by single-crystal X-ray diffraction,elemental analyses,and powder X-ray diffraction.Single-crystal X-ray structural analysis shows that complexes 1 and 3 are 2D networks.In 1,the adjacent 2D networks are linked to a 3D network byπ-πstacking interaction.2 and 4 exhibit 1D chains,and the 1D chains are connected into a 3D network byπ-πstacking interaction and intermolecular hydrogen bond.Luminescence and thermogravimetric analysis of the four complexes were discussed.CCDC:2416406,1;2416407,2;2416408,3;2416409,4.
基金support from National Natural Science Foundation of China(Grant Nos.22275145,22305189and 21875184)Natural Science Foundation of Shaanxi Province(Grant Nos.2022JC-10 and 2024JC-YBQN-0112).
文摘Two-dimensional energetic materials(2DEMs),characterized by their exceptional interlayer sliding properties,are recognized as exemplar of low-sensitivity energetic materials.However,the diversity of available 2DEMs is severely constrained by the absence of efficient methods for rapidly predicting crystal packing modes from molecular structures,impeding the high-throughput rational design of such materials.In this study,we employed quantified indicators,such as hydrogen bond dimension and maximum planar separation,to quickly screen 172DEM and 16 non-2DEM crystal structures from a crystal database.They were subsequently compared and analyzed,focusing on hydrogen bond donor-acceptor combinations,skeleton features,and intermolecular interactions.Our findings suggest that theπ-πpacking interaction energy is a key determinant in the formation of layered packing modes by planar energetic molecules,with its magnitude primarily influenced by the strongest dimericπ-πinteraction(π-π2max).Consequently,we have delineated a critical threshold forπ-π2max to discern layered packing modes and formulated a theoretical model for predictingπ-π2max,grounded in molecular electrostatic potential and dipole moment analysis.The predictive efficacy of this model was substantiated through external validation on a test set comprising 31 planar energetic molecular crystals,achieving an accuracy of 84%and a recall of 75%.Furthermore,the proposed model shows superior classification predictive performance compared to typical machine learning methods,such as random forest,on the external validation samples.This contribution introduces a novel methodology for the identification of crystal packing modes in 2DEMs,potentially accelerating the design and synthesis of high-energy,low-sensitivity 2DEMs.
文摘采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。
文摘The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.
