两个基于2,2'-联吡啶-5,5'-二羧酸配体构筑的碱土金属配合物的合成、晶体结构及其光致发光性质-区泳聪.pdf
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1、第32卷第4期2016年4月无 机 化 学 学 报CHINESE JOURNAL OF INORGANIC CHEMISTRYV0132 No4738744两个基于22 7联吡啶55 7二羧酸配体构筑的碱土金属配合物的合成、晶体结构及其光致发光性质区泳聪 钟均星 宋萦怡 朱岚岚 吴建中(广州市能源转化与储能材料重点实验室,华南师范大学化学与环境学院,广州 510006)摘要:从2,2 7一联吡啶一5,5一二羧酸配体出发,利用溶剂热的方法,合成了两种新颖的碱土金属配位聚合物【Ca(bpdc)(DMF):(H20h。(1)和Mg(bpdc)(H:0),。(2),并且对其进行r元素分析、红外光谱、热
2、重分析和光致发光性质表征。单晶结构分析表明,配合物1和2都是一维链结构并且通过分子间的氢键和7r一丌堆积作用连接成三维的超分子结构。有趣的是,固态荧光光谱显示两种结构的荧光出现了明显的不同,联系结构分析推断可能是有机配体的不同配位构象导致的。关键词:碱土金属配合物;溶剂热合成;构象;光致发光中图分类号:061423+1;061422 文献标识码:A 文章编号:10014861(2016)04073807DoI:10118621CJIC2016092Two 1D Chain Structures Derived from AlkalineEarth Metal Complexesand 2,2-
3、Bipyridine-5,5-dicarboxylate Ligand:Syntheses,Crystal Structures and Luminescent Properties0U Yong-Cong。ZHONG JunXing SONG YingYi ZHU LanLan WU Jian-Zhong(Guangzhou Key Laboratory ofMaterials for Eriergy Conversion and Storage,School of Chemistry and Environment,South China Normal University,Guangzh
4、ou 5 10006,China)Abstract:Two alkaline-earth metal coordination complexes,Ca(bpdc)(DMF)2(H20)d。(1)andMg(bpdc)(H20)3。(2)(H2bpdc=2,2一Bipyridine一5,5 7dicarboxylic acid),have been obtained via solvothermal conditions and characterizedby elemental analysis,IR spectra,thermogravimetric analysis and photol
5、uminescent measurementSingle crystalXrav diffractions reveal that complexes 1 and 2 are 1 D chain structures which are further connected into 3Dsupramolecular structures by hydrogen bonding interactions and 77订stacking interactionsItS noted that thesolidstate fluorescent emissions of 1 and 2 are dif
6、ferent in related to the different conformation modes of thebpdcligandCCDC:1444695,1;1444696,2Keywords:alkaline-earth metal complexes;solvothermal syntheses;conformation;photoluminescenceMetal coordination polymers(MCPs)have beenwidely researched in recent years not only due to theirnovel and intrig
7、uing topological structures,but alsobecause of various potential applications in manyaspects,for example,as porous,magnetic,luminescentand catalytic materials【141Among themtransition metaland lanthanide metal complexes have been extensivelystudied,but there are relatively less reported for thealkali
8、ne-earth metal complexes【5As the characteristicsof alkalineearth are intriguing for their electronic收稿日期:2015-1230。收修改稿日期:201603Ol。国家自然科学基金(No21401058)和广东普通高校青年创新人才项目(No2014KQNCX058)资 。+通信联系人。E-mail:ouyongcongmscnueducn;会员登记号:S06N6724M1506。万方数据第4期区泳聪等:两个基于2,2 7一联吡啶一5,5 7一二羧酸配体构筑的碱土金属配合物的合成、晶体结构及其光致发
9、光性质 739structures,wide emission peaks and large Stokes shift,the syntheses of alkaline-earth complexes would bepregnant2,2 7一Bipyridine-5,5一dicarboxylic acid fH2bpdc),as a muhifunctional bridging ligand,has been used toconstruct various MCPs9According to our previousstudiesll6。mthe different coordin
10、ation modes might lcadto the different propertiesIts interesting that H2bpdccan be fixed in the structure in two modes:the Natoms are in transor cis-positionTo our best knowledge,the researches on the different photoluminescentproperties based on the different conformation ofH2bpdc are rareI呲1 81Her
11、ein,two novel coordinationcomplexes,Ca(bpdc)(DMF)2(H20)2。(1)andMg(bpdc)(H20)32),are constructed via solvothermal conditionsand characterized by elemental analysis,IR spectra,thermogravimetric analysis and photoluminescentmeasurementTo be noticed that the solidstate fluorescent emissions of 1 and 2 a
12、re difierent in relatedto the different conformation modes of the bpdc2一ligand1 Experiment11 Materials and physical measurementsThe chemicals and solvents were commerciallyavailable and used without further purificationC,H,and N microanalyses were carried out with ElementarVarioEL CHN elemental anal
13、yzerFTIR spectrawere recorded on Nicolet FT-IR-1 70SX speetrophoto-meter in KBr tablets in the range of 4 000400 cmX-ray powder diffraction(XPRD)intensities for poly-crystalline samples of complex 1 and 2 were measuredat 293 K on Bruker D8 Advance Diffratometer(CuKsA=01 54 056 nml by scanning over t
14、he range ofo-50。(o-50。for 2)with step of 02虬sSimulatedXPRD patterns were generated with MercuryThermogravimetric analyses were performed onPerkinElmer TGA 7Luminescent spectra for solidstate samples were recorded on Hitachi F一2500 atroom temperature with a xenon arc lamp as the lightSOUrce12 Synthes
15、is of【Ca(bpdc)(DMF)2(H20)21。(1)A mixture of H2bpdc(01 mmol,24 rag),CaCl2(01 mmol,1 20 mg)and succinic acid(01 mmol,1 20mg)in DMF(4 mL)was sonicated 5 min and thenheated in a stainless steel reactor with Teflon liner(23mE)at 1 20 c|C for 72 h and cooled to ambient temperatureat a rate of co5 qCh一to g
16、ive colorless sheet crystals(Yield based on H2bpdc:35 mg,7 16)Elementalanalysis calcdfor C18H240sN4Ca():C 4654,H 521,N 1206;Found():C 4635,II,529,N 1 19613 Synthesis of【Mg(bpdc)(H20)3。(2)A mixture of H2bpdc(01 mmol,23 rag),MgCl2(01 mmol,90 mg)and two drops triethylamine inDMF(3 mL)and H20(2 mL)was s
17、onicated 5 min andthen heated in a stainless steel reactor with Teflonliner f23 mE)at 120for 72 h and cooled to ambienttemperature at a rate of co5 cch。1 to give colorlesscolumn crystals(Yield based on H2bpdc:27 mg,894)Elemental analysis calcdfor C12H1207N2Mg():C4496,H 377,N 874;Found():C 4510,H,379
18、,N 88114 Xray crystallographyDiffraction data for compound 1 was collected onRigaku RAXIS SPIDER Image Plate diffractometerwith graphitemonochromated Mo Ka radiation fA=007 1 073 nm)at 150(2)KDiffraction data for compound 2 was recorded on Bruker smart ApexCCDarea detector diffractometer fMo Ks radi
19、ation。A=007 1 073 nml at 296(21 KThe intensities were integrated using SAINT+Corrections for Lorentz andpolarization effects were appliedAbsorption correctionswere applied by using the multiscan programSADABS【19】The structures were solved by directmethod,and all non-hydrogen atoms were refinedanisot
20、ropically by leastsquares method on F 2 usingthe SHELXTL programThe organic hydrogen atomswere generated geometrically;the aqua hydrogenatoms were located from difference maps and refinedwith isotropic temperature factorsCrystal data as wellas details of data collection and refinements for a11compou
21、nds are summarized in Table 1Table 2 andTable 3 give the data of selected bond lengths andangles and the hydrogen bond parameters for complexes1 and 2 respectivelyCCDC:1444695,1:14446962万方数据740 无机化学学报 第32卷Table 1 Crystal data and structure refmements for 1 and 2Complex 1 2Empirical formula GHl204N2C
22、 a【15 C12H1207N2MgFormula weight 23225 32055Crystal system Tficlinic MonoclinicSpace group P1 P2lcnnm 0638 65(61 1483 4(71bnm 0784 10(71 1197 6(51cnm 1170 04(101 0752 7(41“(o)80397(2) 90卢(。)80123(3) 96766(917(o) 66710(2) 90Vnm3 0527 01(8) 1328 O(101Z 2 4D。(gcm-3) 1464 1603pmm一1 O351 0174Reflections
23、collected 4 947 7 375Unique reflections 2 256 2 813S 1076 1025R,8,wRzb(,2口(J)0055 1,0 138 5 0 073 70209 9R-j棚2b(all data) 0073 6,0152 2 O124 6,0237 7“RFHFoMF3 MYIFol,6 wR:=(野一哟2Y,4rg)q“Table 2 Selected bond lengths(nm)and angles(。)for 1 and 21Ca(1)一0f1)0228 5(4) Ca(1)一O(3)0235 4(3) Ca(I)一o(1w)0234 9
24、f2)Ca(1)。O(1a)0228 5(4) Ca(1)一0(3a)0235 4(3) Ca(I)一O(1Wa)0234 9(2)O(1)。Ca(1)一O(1a) 180 O(1a)-Ca(1)一0(18692(5) O(1W)Ca(1)0(3)8984(5)O(1)。Ca(1)一O(1W) 9307(6) o(1a)一Ca(1)一O(1Wa) 9307(4) O(1W)Ca(1)0(3a) 9015(8)O(1)。CaO)一O(1Wa)8692(4) O(1a)-Ca(1)-0(3)8864(6) O(1Wa)Ca(1)一0(3) 9015f6)O(1)。Ca(1)一0(3) 9135(7
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