The hydrothermal reaction of 1,4-bis（imidazol-1-yl）butane （bimb） and 1,4-bis（2- methylimidazol-1＇-yl）butane （bmib） with CdBr2·4H2O gave rise to two coordination polymers, [Cd（bimb）2Br2]n （1） and [Cd...The hydrothermal reaction of 1,4-bis（imidazol-1-yl）butane （bimb） and 1,4-bis（2- methylimidazol-1＇-yl）butane （bmib） with CdBr2·4H2O gave rise to two coordination polymers, [Cd（bimb）2Br2]n （1） and [Cd（bmib）Br2]n （2）, respectively. Single-crystal X-ray diffraction analysis reveals that 1 and 2 crystallize in the monoclinic space group P21/n and the orthorhombic space group Pccn, respectively. In 1, bimb adopts an anti-anti-anti conformation and bridges adjacent Cd（Ⅱ） to form a two-dimensional （2D） network containing rhombohedral rings. The 2D layers are arranged in an offset ABCABC sequence to fill large void in the rhombohedral rings. In 2, bmib also exhibits an anti-anti-anti conformation, but it links neighboring Cd（Ⅱ） into a one-dimensional （1 D） chain. Br in 1 and 2 serves as a monodentate ligand to balance charge.展开更多
A short synthesis starting from 4-imidazolylmethanol(2)was developed for the phosphonoisostere of histidine,-amino-β-(4-imidazolyl)- ethylphosphosphonic acid,His(P)(1).The synthesis features Wittig-Horner reaction of...A short synthesis starting from 4-imidazolylmethanol(2)was developed for the phosphonoisostere of histidine,-amino-β-(4-imidazolyl)- ethylphosphosphonic acid,His(P)(1).The synthesis features Wittig-Horner reaction of aldehyde(4)with diphosphonate(5)followed by selective detritylation with 50% formic acid.展开更多
A new coordination complex, [Ag(IIMB)N 3], was prepared by self-assembly of asymmetric ligand 1-(1-imidazolyl)-4-(imidazol-1-ylmethyl)benzene(IIMB) with [Ag(NH 3) 2]N 3. The crystal structural analysis indicates that ...A new coordination complex, [Ag(IIMB)N 3], was prepared by self-assembly of asymmetric ligand 1-(1-imidazolyl)-4-(imidazol-1-ylmethyl)benzene(IIMB) with [Ag(NH 3) 2]N 3. The crystal structural analysis indicates that the structure of the complex contains fifty-two-membered macrometallacyclic rings, and the complex crystallizes in monoclinic system, space group of P2 1/c with a=0.739 8(1) nm, {b=}1.045 1(1) nm, c=1.812 4(2)nm, β=91.65(1)°, V=1.400 7(3) nm3, Z=4, D c=1.774 g/cm3, {F(000)=}744, R=0.050 5, wR=0.084 0. It is notable that the azide ion bridges two silver(Ⅰ) atoms in end-on fashion.展开更多
3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Th...3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.展开更多
Three new different dimensional coordination polymers, namely, [Zn（BA-）2（4,4？-bib）-1.5]n（1）, [Zn（4-Br BA-）2（1,4-bmb）]n（2） and [Mn（4-Br BA）2（4,4？-bib）]n（3） have been assembled through the mixed-liga...Three new different dimensional coordination polymers, namely, [Zn（BA-）2（4,4？-bib）-1.5]n（1）, [Zn（4-Br BA-）2（1,4-bmb）]n（2） and [Mn（4-Br BA）2（4,4？-bib）]n（3） have been assembled through the mixed-ligand synthetic strategy（4-HBr BA = 4-bromobenzoic acid, HBA = benzoic acid, 1,4-bmb = 1,4-bis（1 H-imidazol-4-yl）benzene, 4,4？-bib = 4,4？-bis（imidazolyl）biphenyl）. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses（EA）, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. Single-crystal X-ray diffraction analysis reveals that the crystals of complexes 1~3 are all in triclinic systems, space group P1. Complexes 1 and 2 are 0D binuclear structures, and 3 is a 1 D chain. Moreover, the solid state fluorescence properties of 1 and 2 have been investigated.展开更多
基金Supported by NSFC (21001025)NSF of Fujian Province (2010J05017)SRF for ROCS, SEM
文摘The hydrothermal reaction of 1,4-bis（imidazol-1-yl）butane （bimb） and 1,4-bis（2- methylimidazol-1＇-yl）butane （bmib） with CdBr2·4H2O gave rise to two coordination polymers, [Cd（bimb）2Br2]n （1） and [Cd（bmib）Br2]n （2）, respectively. Single-crystal X-ray diffraction analysis reveals that 1 and 2 crystallize in the monoclinic space group P21/n and the orthorhombic space group Pccn, respectively. In 1, bimb adopts an anti-anti-anti conformation and bridges adjacent Cd（Ⅱ） to form a two-dimensional （2D） network containing rhombohedral rings. The 2D layers are arranged in an offset ABCABC sequence to fill large void in the rhombohedral rings. In 2, bmib also exhibits an anti-anti-anti conformation, but it links neighboring Cd（Ⅱ） into a one-dimensional （1 D） chain. Br in 1 and 2 serves as a monodentate ligand to balance charge.
文摘A short synthesis starting from 4-imidazolylmethanol(2)was developed for the phosphonoisostere of histidine,-amino-β-(4-imidazolyl)- ethylphosphosphonic acid,His(P)(1).The synthesis features Wittig-Horner reaction of aldehyde(4)with diphosphonate(5)followed by selective detritylation with 50% formic acid.
文摘A new coordination complex, [Ag(IIMB)N 3], was prepared by self-assembly of asymmetric ligand 1-(1-imidazolyl)-4-(imidazol-1-ylmethyl)benzene(IIMB) with [Ag(NH 3) 2]N 3. The crystal structural analysis indicates that the structure of the complex contains fifty-two-membered macrometallacyclic rings, and the complex crystallizes in monoclinic system, space group of P2 1/c with a=0.739 8(1) nm, {b=}1.045 1(1) nm, c=1.812 4(2)nm, β=91.65(1)°, V=1.400 7(3) nm3, Z=4, D c=1.774 g/cm3, {F(000)=}744, R=0.050 5, wR=0.084 0. It is notable that the azide ion bridges two silver(Ⅰ) atoms in end-on fashion.
文摘3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.
基金Supported by the National Natural Science Foundation of China(No.21451001)the Key Discipline,Innovation Team,and Key Lab.of Qilu Normal University
文摘Three new different dimensional coordination polymers, namely, [Zn（BA-）2（4,4？-bib）-1.5]n（1）, [Zn（4-Br BA-）2（1,4-bmb）]n（2） and [Mn（4-Br BA）2（4,4？-bib）]n（3） have been assembled through the mixed-ligand synthetic strategy（4-HBr BA = 4-bromobenzoic acid, HBA = benzoic acid, 1,4-bmb = 1,4-bis（1 H-imidazol-4-yl）benzene, 4,4？-bib = 4,4？-bis（imidazolyl）biphenyl）. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses（EA）, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. Single-crystal X-ray diffraction analysis reveals that the crystals of complexes 1~3 are all in triclinic systems, space group P1. Complexes 1 and 2 are 0D binuclear structures, and 3 is a 1 D chain. Moreover, the solid state fluorescence properties of 1 and 2 have been investigated.
