Six new transition metal complexes, [Zn（HBTC）（PYTPY）]n·n PYTPY（1）, [Cu（HBTC）（PYTPY）]n·n PYTPY（2）, [Co（HBTC）（PYTPY）]n·n DMF（3）, [Mn（HBTC）（PYTPY）]n·n DMF（4）, [Cd（HBTC）（PYTP...Six new transition metal complexes, [Zn（HBTC）（PYTPY）]n·n PYTPY（1）, [Cu（HBTC）（PYTPY）]n·n PYTPY（2）, [Co（HBTC）（PYTPY）]n·n DMF（3）, [Mn（HBTC）（PYTPY）]n·n DMF（4）, [Cd（HBTC）（PYTPY）（H2O）]n·2nH2O（5）, and [Co（HBTC）（PYTPY）（H2O）2]（6）,（H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4＇-（4-pyridyl）-2,2＇：6＇,2＇＇-terpyridine, DMF = N,N？-dimethylformamide）, have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional（3D） supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.展开更多
One novel nickel coordination polymer, {[Ni（OTP）（bib）1.5（H2O）]·2H2O}n（1, H2 OTP = 2-hydroxy-5-（3＇,5＇-terephthalic acid） pyridine, bib = 1,4-bis（1-imdazoly）benzene）, has been synthesized and characte...One novel nickel coordination polymer, {[Ni（OTP）（bib）1.5（H2O）]·2H2O}n（1, H2 OTP = 2-hydroxy-5-（3＇,5＇-terephthalic acid） pyridine, bib = 1,4-bis（1-imdazoly）benzene）, has been synthesized and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a = 12.2860（5）, b = 13.8246（6）, c = 19.0140（8） A, β = 104.3870（1）°, V = 3128.2（2） A3, Z = 4, C32H28N7 Ni O8, Mr = 697.32, Dc = 1.481 g/cm^3, F（000） = 1444 and μ（Mo Kα） = 0.684 mm-1. The final R = 0.0704 and w R = 0.1764 for 5485 observed reflections with I 2σ（I） and R = 0.1087 and wR = 0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {4^4·6^6}-nov net based on the 1D [Ni（OTP）]n chain and the 2D [Ni2（bib）3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.展开更多
A new spectrofluorimetric method for determination of trace terbium based on its reaction with 2.6-his-(1'-phenyl-3'-methyl-5'- pyridinediacyl (H_2PMBPP) and N- cetylpyridium bromide (CPB). at an apparent ...A new spectrofluorimetric method for determination of trace terbium based on its reaction with 2.6-his-(1'-phenyl-3'-methyl-5'- pyridinediacyl (H_2PMBPP) and N- cetylpyridium bromide (CPB). at an apparent pH=5.0 provided by a hexamethylenetetramine (5% w/w)-hydrochloric acid buffer,is propesed. The calibration graph is linear in the ran ge from展开更多
Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental anal...Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental analy. sis.The molar conductance,IR,~4H-NMR,electronic spectra and thermogravimetric analysis of the chelates have been measured and discussed.展开更多
The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 7...The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 726(3), c=16. 602(3) A ; β= 100. 375(13)°; V=2651. 4(10) A3, Z=4, Dc= 1. 387 g/cm3, μ(MoKa) =0. 319 mm-1, F(000) =1160, R=0. 0428, wR(F2) =0. 0910 for 2438 observed reflections (I>2(I)). X-ray analysis reveals that interatomic distances for C(5)-C(6), C(13)-C(14) and C(21)-C(22) are 1. 331(4), 1. 351(4), 1. 344(4)A respectively, which show that they are normal C=C double bonds. All S-C bondlengths are similar to typical S-C single bonds (1. 75 - 1. 78 A ). The five-membered ring A (C(5) -C(6) -S(2)-C(13) -S(1) ) (Fig. 1) and six-membered ringB (C(14) -C(15) -C(20) -C(21)-C(22)-S(3) ) (Fig. 1) adopt the flat twist conformation. Furthermore, the morpholine ring adopts chair conformtion.展开更多
基金Supported by the National Natural Science Foundation of China(No.21576112)Natural Science Foundation of Jilin Province(20150623024TC-19,20170520147JH)the Science and Technology Development Plan of Siping City(2015049)
文摘Six new transition metal complexes, [Zn（HBTC）（PYTPY）]n·n PYTPY（1）, [Cu（HBTC）（PYTPY）]n·n PYTPY（2）, [Co（HBTC）（PYTPY）]n·n DMF（3）, [Mn（HBTC）（PYTPY）]n·n DMF（4）, [Cd（HBTC）（PYTPY）（H2O）]n·2nH2O（5）, and [Co（HBTC）（PYTPY）（H2O）2]（6）,（H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4＇-（4-pyridyl）-2,2＇：6＇,2＇＇-terpyridine, DMF = N,N？-dimethylformamide）, have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional（3D） supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.
基金supported by the Natural Science Foundation of Shandong Province(ZR2011BL020,ZR2012CM019)National Natural Science Foundation of China(21451001)Key Discipline and Innovation Team of Qilu Normal University
文摘One novel nickel coordination polymer, {[Ni（OTP）（bib）1.5（H2O）]·2H2O}n（1, H2 OTP = 2-hydroxy-5-（3＇,5＇-terephthalic acid） pyridine, bib = 1,4-bis（1-imdazoly）benzene）, has been synthesized and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a = 12.2860（5）, b = 13.8246（6）, c = 19.0140（8） A, β = 104.3870（1）°, V = 3128.2（2） A3, Z = 4, C32H28N7 Ni O8, Mr = 697.32, Dc = 1.481 g/cm^3, F（000） = 1444 and μ（Mo Kα） = 0.684 mm-1. The final R = 0.0704 and w R = 0.1764 for 5485 observed reflections with I 2σ（I） and R = 0.1087 and wR = 0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {4^4·6^6}-nov net based on the 1D [Ni（OTP）]n chain and the 2D [Ni2（bib）3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.
基金The authors are gratelbl for financial supports IYom the National Natural Science roundation of Chinathe Educational Commiss
文摘A new spectrofluorimetric method for determination of trace terbium based on its reaction with 2.6-his-(1'-phenyl-3'-methyl-5'- pyridinediacyl (H_2PMBPP) and N- cetylpyridium bromide (CPB). at an apparent pH=5.0 provided by a hexamethylenetetramine (5% w/w)-hydrochloric acid buffer,is propesed. The calibration graph is linear in the ran ge from
文摘Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental analy. sis.The molar conductance,IR,~4H-NMR,electronic spectra and thermogravimetric analysis of the chelates have been measured and discussed.
文摘The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 726(3), c=16. 602(3) A ; β= 100. 375(13)°; V=2651. 4(10) A3, Z=4, Dc= 1. 387 g/cm3, μ(MoKa) =0. 319 mm-1, F(000) =1160, R=0. 0428, wR(F2) =0. 0910 for 2438 observed reflections (I>2(I)). X-ray analysis reveals that interatomic distances for C(5)-C(6), C(13)-C(14) and C(21)-C(22) are 1. 331(4), 1. 351(4), 1. 344(4)A respectively, which show that they are normal C=C double bonds. All S-C bondlengths are similar to typical S-C single bonds (1. 75 - 1. 78 A ). The five-membered ring A (C(5) -C(6) -S(2)-C(13) -S(1) ) (Fig. 1) and six-membered ringB (C(14) -C(15) -C(20) -C(21)-C(22)-S(3) ) (Fig. 1) adopt the flat twist conformation. Furthermore, the morpholine ring adopts chair conformtion.
