A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic,...A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.展开更多
The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH...The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH2CO2H)2]x·H2O (ZPPMIDA) by the reaction of zirconium oxychloride with phosphonic acid and H2O3PCH2N(CH2CO2H)2 in the designed x range of 0 < x < 2, which had been monitored by using the phosphorus integration value ratio of HPO42- and [O3PCH2N(CH2CO2H)2]2- group in the 31P MAS NMR spectra. After intercala- tion of n-butyl amine, the 31P chemical shift of HPO42- group at - 8.0￣- 10.0 ppm moved to 6.0 ppm with a change of 14.0￣16.0 ppm and that of [O3PCH2N(CH2CO2H)2]2- group at - 29.1 ppm changed only 0.5 ppm. Due to the pil- lared effect of [O3PCH2N(CH2CO2H)2]2- groups on the interlayer spacing, intercalated amines such as n-butylamine, n-hexyl amine and n-octyl amine easily reacted with HPO42- group in ZPPMIDA (x=0.66) rather than that in α- ZrP, and carboxylic group (-CO2H) in ZPPMIDA (x=0.66).展开更多
The title compound Mn 3(BTC) 2(DMF) 4 (BTC=1,3,5-benzenetricarboxylic acid,DMF=dimethyl formamide) was synthesized under the mild conditions and its crystal structure was determined by single crystal X-ray diffraction...The title compound Mn 3(BTC) 2(DMF) 4 (BTC=1,3,5-benzenetricarboxylic acid,DMF=dimethyl formamide) was synthesized under the mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system and belongs to space group P2 1/c with a =1.787 6(4) nm, b =1.179 7(2) nm, c =1.884 8(4) nm, β =116.35(3)°, V = 3.561 9(12) nm 3, Z =4, D c=7.413 Mg/m 3, M r=871.43, μ =5.081 mm -1 , F (000)=8 082, R = 0.045 6 , wR =0.106 3. Its structure reveals that each asymmetric unit of the title polymer contains three Mn(Ⅱ) ions,six BTC and four DMF ligands. The coordination of BTC ligands with Mn(Ⅱ) ions forms a 3D infinite framework having helical chains composed with 2 1 axes and about 0.6 nm× 0.8 nm channels along the [100] direction.展开更多
The title compound [Zn3（BTC）2（H2O）3]n（BTC=1,3,5-benzenetricarboxylic acid） was synthesized under mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystal...The title compound [Zn3（BTC）2（H2O）3]n（BTC=1,3,5-benzenetricarboxylic acid） was synthesized under mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the cubic system and belongs to space group Fm-3m with a=2.662 6（3） nm ,V=18.877（4） nm 3,Z=16,Dc=1.51 g/cm 3,Mr=664.4,μ=0.198 mm -1 , F（000）=852 ,R=0.062 5,wR=0.129 4. Its structure reveals that the title polymer is composed of dimeric zinc tetracarboxylate units,with a short Zn-Zn internuclear separation of 0.295 0（4） nm. The coordination of BTC ligands with Zn ions forms a 3D infinite framework with about 1.117 4 nm×1.327 4 nm pores along the [001],[100] and [010] direction. [WT5HZ]展开更多
The title compound Mn 3(BTC) 2(bpy)(EG)(DMF)·(DMF)·1/3(C 2H 5OH)(BTC=1,3,5-benzenetricarboxylic acid, bpy=4,4′-bipyridine, EG=ethylene glycol, DMF=dimethylformamide) was synthesized under mild conditions an...The title compound Mn 3(BTC) 2(bpy)(EG)(DMF)·(DMF)·1/3(C 2H 5OH)(BTC=1,3,5-benzenetricarboxylic acid, bpy=4,4′-bipyridine, EG=ethylene glycol, DMF=dimethylformamide) was synthesized under mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system and belongs to space group P2 1/n with a= 1.637 2(3) nm, b=1.481 4(3) nm, c=1.838 4(4) nm, β=113.70(3)°, V=4.082 5(14) nm 3, Z=4, D c=1.508 Mg/m 3, M r=958.85, μ=1.001 mm -1, F(000)=1 920. R 1=0.098 5, wR 2= 0.218 3. Its structure reveals that Mn(Ⅱ) centers and the carboxylate groups of BTC construct 1D O—C—O—Mn chains. Then, adjacent chains are interlinked by benzene rings of BTC to form a novel 3D architecture. It contains eight-membered rings channels that are about 0.8 nm×0.8 nm viewed along the (101) direction. In addition, it is believed that the bpy acts as both an organic ligand and a structure-directing agent in the synthesis of the title compound.展开更多
A 3-D inorganic-organic hybrid framework microporous material [Co 3(BDC) 3(EG) 4]·2DMF was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The...A 3-D inorganic-organic hybrid framework microporous material [Co 3(BDC) 3(EG) 4]·2DMF was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by a direct method and refined by full-matrix least-square method. The crystal is the triclinic system and belongs to space group P-1 with a=9.978(2) nm, b=11.223(2) nm, c=11.283(2) nm, α=102.26(3)°, β=113.52(3)°, γ=92.73(3)°, V=6.329(2) nm 3, Z=1, D c=1.565 Mg/m 3, M r=1 063.59, μ=1.183 mm -1, F(000)=541, GOF=1.024, R=0.044 2, wR=0.124 9.展开更多
文摘A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.
文摘The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH2CO2H)2]x·H2O (ZPPMIDA) by the reaction of zirconium oxychloride with phosphonic acid and H2O3PCH2N(CH2CO2H)2 in the designed x range of 0 < x < 2, which had been monitored by using the phosphorus integration value ratio of HPO42- and [O3PCH2N(CH2CO2H)2]2- group in the 31P MAS NMR spectra. After intercala- tion of n-butyl amine, the 31P chemical shift of HPO42- group at - 8.0￣- 10.0 ppm moved to 6.0 ppm with a change of 14.0￣16.0 ppm and that of [O3PCH2N(CH2CO2H)2]2- group at - 29.1 ppm changed only 0.5 ppm. Due to the pil- lared effect of [O3PCH2N(CH2CO2H)2]2- groups on the interlayer spacing, intercalated amines such as n-butylamine, n-hexyl amine and n-octyl amine easily reacted with HPO42- group in ZPPMIDA (x=0.66) rather than that in α- ZrP, and carboxylic group (-CO2H) in ZPPMIDA (x=0.66).
文摘The title compound Mn 3(BTC) 2(DMF) 4 (BTC=1,3,5-benzenetricarboxylic acid,DMF=dimethyl formamide) was synthesized under the mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system and belongs to space group P2 1/c with a =1.787 6(4) nm, b =1.179 7(2) nm, c =1.884 8(4) nm, β =116.35(3)°, V = 3.561 9(12) nm 3, Z =4, D c=7.413 Mg/m 3, M r=871.43, μ =5.081 mm -1 , F (000)=8 082, R = 0.045 6 , wR =0.106 3. Its structure reveals that each asymmetric unit of the title polymer contains three Mn(Ⅱ) ions,six BTC and four DMF ligands. The coordination of BTC ligands with Mn(Ⅱ) ions forms a 3D infinite framework having helical chains composed with 2 1 axes and about 0.6 nm× 0.8 nm channels along the [100] direction.
文摘The title compound [Zn3（BTC）2（H2O）3]n（BTC=1,3,5-benzenetricarboxylic acid） was synthesized under mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the cubic system and belongs to space group Fm-3m with a=2.662 6（3） nm ,V=18.877（4） nm 3,Z=16,Dc=1.51 g/cm 3,Mr=664.4,μ=0.198 mm -1 , F（000）=852 ,R=0.062 5,wR=0.129 4. Its structure reveals that the title polymer is composed of dimeric zinc tetracarboxylate units,with a short Zn-Zn internuclear separation of 0.295 0（4） nm. The coordination of BTC ligands with Zn ions forms a 3D infinite framework with about 1.117 4 nm×1.327 4 nm pores along the [001],[100] and [010] direction. [WT5HZ]
文摘The title compound Mn 3(BTC) 2(bpy)(EG)(DMF)·(DMF)·1/3(C 2H 5OH)(BTC=1,3,5-benzenetricarboxylic acid, bpy=4,4′-bipyridine, EG=ethylene glycol, DMF=dimethylformamide) was synthesized under mild conditions and its crystal structure was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system and belongs to space group P2 1/n with a= 1.637 2(3) nm, b=1.481 4(3) nm, c=1.838 4(4) nm, β=113.70(3)°, V=4.082 5(14) nm 3, Z=4, D c=1.508 Mg/m 3, M r=958.85, μ=1.001 mm -1, F(000)=1 920. R 1=0.098 5, wR 2= 0.218 3. Its structure reveals that Mn(Ⅱ) centers and the carboxylate groups of BTC construct 1D O—C—O—Mn chains. Then, adjacent chains are interlinked by benzene rings of BTC to form a novel 3D architecture. It contains eight-membered rings channels that are about 0.8 nm×0.8 nm viewed along the (101) direction. In addition, it is believed that the bpy acts as both an organic ligand and a structure-directing agent in the synthesis of the title compound.
文摘A 3-D inorganic-organic hybrid framework microporous material [Co 3(BDC) 3(EG) 4]·2DMF was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by a direct method and refined by full-matrix least-square method. The crystal is the triclinic system and belongs to space group P-1 with a=9.978(2) nm, b=11.223(2) nm, c=11.283(2) nm, α=102.26(3)°, β=113.52(3)°, γ=92.73(3)°, V=6.329(2) nm 3, Z=1, D c=1.565 Mg/m 3, M r=1 063.59, μ=1.183 mm -1, F(000)=541, GOF=1.024, R=0.044 2, wR=0.124 9.
