The 1:1photoadduct reaction of indole and 9,10-phenanthraquinone(PQ),10-hydroxy-10-(3-indolyl)-9-phenanthrenone(HIPN).forms a 1:1 inclusion complex with tetrahydrofuran (THF)·C_(22)H_(15)NO_2·C_4H_8O,M_r=397...The 1:1photoadduct reaction of indole and 9,10-phenanthraquinone(PQ),10-hydroxy-10-(3-indolyl)-9-phenanthrenone(HIPN).forms a 1:1 inclusion complex with tetrahydrofuran (THF)·C_(22)H_(15)NO_2·C_4H_8O,M_r=397.45,space group Pbn2_1,a=11.041(2),b=13.147(3),c=13.958(1),V= 2026(1),Z=4,D_x=1.30g/cm￣3,μ=0.79 cm￣(-1), F(000)=840,R=0.060,Rω=0.067.There are three main planes in the HIPN molecule,the dihedral angles between them are 16.47°,89.21° and 89.83°,respectively.The THF molecule is included through H-bond with the-OH group of HIPN,adopting a unique planar conformation.展开更多
Two inclusion complexes of β-cyclodextrin-7-hydroxycoumarin （1） and ,β-cyclodextrin-4-hydroxycoumarin （2） were prepared and their crystal structures were investigated by single crystal X-ray crystallography unde...Two inclusion complexes of β-cyclodextrin-7-hydroxycoumarin （1） and ,β-cyclodextrin-4-hydroxycoumarin （2） were prepared and their crystal structures were investigated by single crystal X-ray crystallography under cryogenic condition. Both structures consist of stacks of face-to-face cyclodextrin dimers arranged in brickwork-like pattern along the crystallographic a-axis. For complex 1, each of the two dimeric β-cyclodextrins includes one 7-hydroxycoumarin molecule that penetrates deeply into the cyclodextrin dimer and locates its lactonering at the center of the dimer cavity. For complex 2, each cyelodextrin dimer accommodates three 4-hydroxycoumarin molecules. One of them is sandwiched between two units of the cyclodextrin dimer, the other two are shallowly included in the cavities of the dimeric cyclodextrins respectively and protrude their lactone rings from the primary end of the cyclodextrin. The substituent effects of guest molecules on inclusion geometry of various coumarin molecules in fl-cyclodextrin were examined.展开更多
The X-ray crystal structure of the inclusion complex of p-tert-butylcalix [4] crown-6 with actonitrile is reported. C54H70O10·3CH3CN, Mr=1002. 3 ,monoclinic, space group C2/c with cell dimensions of a=23.587(7),b...The X-ray crystal structure of the inclusion complex of p-tert-butylcalix [4] crown-6 with actonitrile is reported. C54H70O10·3CH3CN, Mr=1002. 3 ,monoclinic, space group C2/c with cell dimensions of a=23.587(7),b=21.153(6),c=15.608(8) A,β=116.99(3)°,V=6939.2 A3,Z=4, F(000)=2160,Dc=0.959 g/cm3,μ=1.114 cm-1; R=0.088 for 2066 reflections with I>3σ(I).The calixarene subunit exists in a distorted cone conformation. One of the three acetonitrile molecules is located in the intracavity of the calixarene subunit and the other two in the intermolecular channels.展开更多
The inclusion complex of β-cyclodextrin （β-CD） with 4-chlorobenzoic acid was synthesized and its crystal structure was determined by single crystal X-ray diffraction under cryogenic condition. The complex contains...The inclusion complex of β-cyclodextrin （β-CD） with 4-chlorobenzoic acid was synthesized and its crystal structure was determined by single crystal X-ray diffraction under cryogenic condition. The complex contains two β-CDs, two 4-chlorobenzoic acids and twenty-nine water molecules in the asymmetric unit, and can be formulated as 2（C42H70O35）·2（CTH5O2Cl）·29（H2O）. In the crystal lattice, two β-CDs form a face-to-face dimer jointed together through hydrogen bonding between the secondary hydroxyl groups of β--CDs. Two 4-chlorobenzoic acid molecules which contact by C-Cl…π interactions are included in the β-CD dimer cavity. The β-CD dimers are arranged in brickwork-like pattern along the crystallographic a-axis. The effect of guest molecule length on the inclusion geometry was discussed by comparative study of some fl-CD complexes containing similar guests.展开更多
The inclusion complex of β-cyclodextrin with m-nitrophenoxyacetic acid was studied by single crystal X-ray diffraction,2D NMR spectroscopy and semi-empirical methods AMI.The crystallographic study shows that two β-c...The inclusion complex of β-cyclodextrin with m-nitrophenoxyacetic acid was studied by single crystal X-ray diffraction,2D NMR spectroscopy and semi-empirical methods AMI.The crystallographic study shows that two β-cyclodextrins are held together by hydrogen bonds to form head-to-head dimers.The disordered guest molecule adjusts itself to attain the most stable accommodation into the cavity in which the nitro group is located at the dimer interface while the carboxyl group is buried in the primary hydroxyl groups of β-cyclodextrin.The guest inside the cavity is disordered over two sites and exhibits mobility.Moreover,2D NMR spectroscopy and theoretical study show the same inclusion behavior.In comparison to the inclusion complex of β-cyclodextrin with p-nitrophenoxyacetic acid,the host-guest stoichiometries are different,i.e.,2：1 for m-nitrophenoxyacetic acid and 1：1 for p-nitrophenoxyacetic acid,while the inclusion orientation and the packing pattern of the host are similar in both complexes.展开更多
An inclusion complex (1) has been prepared by β-cyclodextrin with α-aminopyridine. The result of X-ray crystallographic analyses showed that the α-aminopyridine molecules in the β-cyclodextrin cavities possess two...An inclusion complex (1) has been prepared by β-cyclodextrin with α-aminopyridine. The result of X-ray crystallographic analyses showed that the α-aminopyridine molecules in the β-cyclodextrin cavities possess two opposite orientations, i.e. the amine group of α-aminopyridine pointing to the primary side (1a, occupancy: 41.2%) or the secondary side (1b, occupancy: 58.8%) of β-cyclodextrin, forming two scalelike supramolecular aggregations. The studies of 2D NMR and circular dichroism spectra indicated that the α-aminopyridine molecule is deeply embedded in the β-cyclodextrin cavity to form host-guest inclusion complex, showing a circular dichroism spectrum induced by the chiral cavity of cyclodextrin. The results obtained are helpful for understanding the molecular recognition and aggregation mechanism between the host and guest.展开更多
The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compoun...The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compound upon one molecule of CH 3CN or one molecule of CH 3NO 2, forms an intramolecular inclusion complex, respectively, by CH 3-π interactions. The complex of L with tetrabutyl ammonium bromide(TBAB), L·TBAB, was obtained. The results of DTA-TG and XRD analysis of L·TBAB can also be considered as an intramolecular inclusion complex.展开更多
Unprecedented synthesis of chiral (aza)crown ethers of calix[4]arene derivatives bearing a carboxyl amide bridge was described. The synthesis proceeds through condensation of the corresponding dinitriles with opticall...Unprecedented synthesis of chiral (aza)crown ethers of calix[4]arene derivatives bearing a carboxyl amide bridge was described. The synthesis proceeds through condensation of the corresponding dinitriles with optically active 1,2-aminoalcohols, and is catalyzed by the ZnCl<SUB>2</SUB> Lewis acid at elevated temperature in a very efficient one-pot process. The cavity of calix[4](aza)crowns can encapsulate methanol molecules by O-H⋯п interaction, which has been confirmed by X-ray crystal structures and ESI-MS.展开更多
文摘The 1:1photoadduct reaction of indole and 9,10-phenanthraquinone(PQ),10-hydroxy-10-(3-indolyl)-9-phenanthrenone(HIPN).forms a 1:1 inclusion complex with tetrahydrofuran (THF)·C_(22)H_(15)NO_2·C_4H_8O,M_r=397.45,space group Pbn2_1,a=11.041(2),b=13.147(3),c=13.958(1),V= 2026(1),Z=4,D_x=1.30g/cm￣3,μ=0.79 cm￣(-1), F(000)=840,R=0.060,Rω=0.067.There are three main planes in the HIPN molecule,the dihedral angles between them are 16.47°,89.21° and 89.83°,respectively.The THF molecule is included through H-bond with the-OH group of HIPN,adopting a unique planar conformation.
基金Project supported by the Natural Science Foundation of Hainan Province （No. 808145）.
文摘Two inclusion complexes of β-cyclodextrin-7-hydroxycoumarin （1） and ,β-cyclodextrin-4-hydroxycoumarin （2） were prepared and their crystal structures were investigated by single crystal X-ray crystallography under cryogenic condition. Both structures consist of stacks of face-to-face cyclodextrin dimers arranged in brickwork-like pattern along the crystallographic a-axis. For complex 1, each of the two dimeric β-cyclodextrins includes one 7-hydroxycoumarin molecule that penetrates deeply into the cyclodextrin dimer and locates its lactonering at the center of the dimer cavity. For complex 2, each cyelodextrin dimer accommodates three 4-hydroxycoumarin molecules. One of them is sandwiched between two units of the cyclodextrin dimer, the other two are shallowly included in the cavities of the dimeric cyclodextrins respectively and protrude their lactone rings from the primary end of the cyclodextrin. The substituent effects of guest molecules on inclusion geometry of various coumarin molecules in fl-cyclodextrin were examined.
文摘The X-ray crystal structure of the inclusion complex of p-tert-butylcalix [4] crown-6 with actonitrile is reported. C54H70O10·3CH3CN, Mr=1002. 3 ,monoclinic, space group C2/c with cell dimensions of a=23.587(7),b=21.153(6),c=15.608(8) A,β=116.99(3)°,V=6939.2 A3,Z=4, F(000)=2160,Dc=0.959 g/cm3,μ=1.114 cm-1; R=0.088 for 2066 reflections with I>3σ(I).The calixarene subunit exists in a distorted cone conformation. One of the three acetonitrile molecules is located in the intracavity of the calixarene subunit and the other two in the intermolecular channels.
基金the financial support from the Natural Science Foundation of Hainan Province(no.808145)Doctoral Foundation of Hainan Normal University(no.103303)
文摘The inclusion complex of β-cyclodextrin （β-CD） with 4-chlorobenzoic acid was synthesized and its crystal structure was determined by single crystal X-ray diffraction under cryogenic condition. The complex contains two β-CDs, two 4-chlorobenzoic acids and twenty-nine water molecules in the asymmetric unit, and can be formulated as 2（C42H70O35）·2（CTH5O2Cl）·29（H2O）. In the crystal lattice, two β-CDs form a face-to-face dimer jointed together through hydrogen bonding between the secondary hydroxyl groups of β--CDs. Two 4-chlorobenzoic acid molecules which contact by C-Cl…π interactions are included in the β-CD dimer cavity. The β-CD dimers are arranged in brickwork-like pattern along the crystallographic a-axis. The effect of guest molecule length on the inclusion geometry was discussed by comparative study of some fl-CD complexes containing similar guests.
文摘The inclusion complex of β-cyclodextrin with m-nitrophenoxyacetic acid was studied by single crystal X-ray diffraction,2D NMR spectroscopy and semi-empirical methods AMI.The crystallographic study shows that two β-cyclodextrins are held together by hydrogen bonds to form head-to-head dimers.The disordered guest molecule adjusts itself to attain the most stable accommodation into the cavity in which the nitro group is located at the dimer interface while the carboxyl group is buried in the primary hydroxyl groups of β-cyclodextrin.The guest inside the cavity is disordered over two sites and exhibits mobility.Moreover,2D NMR spectroscopy and theoretical study show the same inclusion behavior.In comparison to the inclusion complex of β-cyclodextrin with p-nitrophenoxyacetic acid,the host-guest stoichiometries are different,i.e.,2：1 for m-nitrophenoxyacetic acid and 1：1 for p-nitrophenoxyacetic acid,while the inclusion orientation and the packing pattern of the host are similar in both complexes.
基金supported by the National Natural Science Foundation of China (Grant Nos. 20272028 and 90306009).
文摘An inclusion complex (1) has been prepared by β-cyclodextrin with α-aminopyridine. The result of X-ray crystallographic analyses showed that the α-aminopyridine molecules in the β-cyclodextrin cavities possess two opposite orientations, i.e. the amine group of α-aminopyridine pointing to the primary side (1a, occupancy: 41.2%) or the secondary side (1b, occupancy: 58.8%) of β-cyclodextrin, forming two scalelike supramolecular aggregations. The studies of 2D NMR and circular dichroism spectra indicated that the α-aminopyridine molecule is deeply embedded in the β-cyclodextrin cavity to form host-guest inclusion complex, showing a circular dichroism spectrum induced by the chiral cavity of cyclodextrin. The results obtained are helpful for understanding the molecular recognition and aggregation mechanism between the host and guest.
文摘The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compound upon one molecule of CH 3CN or one molecule of CH 3NO 2, forms an intramolecular inclusion complex, respectively, by CH 3-π interactions. The complex of L with tetrabutyl ammonium bromide(TBAB), L·TBAB, was obtained. The results of DTA-TG and XRD analysis of L·TBAB can also be considered as an intramolecular inclusion complex.
基金Supported by the National Basic Research Program of China (Grant No. 2007CB925103)the National Natural Science Foundation of China (Grant No. 20602017)NCET-07-0425
文摘Unprecedented synthesis of chiral (aza)crown ethers of calix[4]arene derivatives bearing a carboxyl amide bridge was described. The synthesis proceeds through condensation of the corresponding dinitriles with optically active 1,2-aminoalcohols, and is catalyzed by the ZnCl<SUB>2</SUB> Lewis acid at elevated temperature in a very efficient one-pot process. The cavity of calix[4](aza)crowns can encapsulate methanol molecules by O-H⋯п interaction, which has been confirmed by X-ray crystal structures and ESI-MS.
