CN106478674A - 一种基于铜(ii)的双核金属有机配合物及其制备方法 - Google Patents
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- 239000002184 metal Substances 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 40
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 150000001875 compounds Chemical class 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000010949 copper Substances 0.000 claims abstract description 14
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical class OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000003252 repetitive effect Effects 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 239000003446 ligand Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- JNMUQURIAOKWTB-UHFFFAOYSA-N 3-methyl-4-(3-methylpyridin-4-yl)pyridine Chemical group CC1=CN=CC=C1C1=CC=NC=C1C JNMUQURIAOKWTB-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 230000005303 antiferromagnetism Effects 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 230000005291 magnetic effect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- YQBPLVKHEZNFMQ-UHFFFAOYSA-N 2-methyl-4-pyridin-4-ylpyridine Chemical group C1=NC(C)=CC(C=2C=CN=CC=2)=C1 YQBPLVKHEZNFMQ-UHFFFAOYSA-N 0.000 description 1
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical group C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 description 1
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- -1 Cu2+ Cation Chemical class 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009432 framing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000013612 plasmid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
- C07F1/08—Copper compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
- C07F1/005—Compounds containing elements of Groups 1 or 11 of the Periodic Table without C-Metal linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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Abstract
本发明涉及一种基于铜(II)的双核金属有机配合物,该金属有机配合物是重复单元为Cu(fdc)(dmbpy)(H2O)的铜金属有机配合物,所述的化学式Cu(fdc)(dmbpy)(H2O)中的fdc为呋喃‑2,5‑二羧酸,dmbpy为3,3’‑二甲基‑4,4’‑联吡啶;本发明所述的铜(II)金属有机配合物具有良好的反铁磁性。
Description
技术领域
本发明涉及金属有机配合物,具体涉及一种基于铜(II)的双核金属有机配合物及其制备方法。
背景技术
近年来,设计和合成具有高维有序空间结构和优良理化性能的分子基功能材料已经引起了人们极大的兴趣。金属配合物分子基磁体是目前研究得最广泛和深入的一类,其自旋载体为顺磁性金属离子。由这些高自旋的配合物进行适当的分子组装可以形成多核、一维、二维及三维分子基磁体。
金属有机配合物是一种新型功能材料,由金属离子与有机配体在一定条件下通过自组装合成。由于其具有独特的骨架结构及孔径可控等特点,在气体吸附、光电材料、磁性材料[1]、载药、催化等方面具有极其广阔的应用空间,吸引了许多国内外专家学者的关注。
呋喃-2,5-二羧酸是一种具有多种连接和协调模式的配体,对于构建金属有机配合物的结构非常重要[2]。此外,越来越多的金属有机配合物已被证实是由羧酸配体和含N辅助配体构成[3]。其中,4,4'-联吡啶及其衍生物是用来构造新颖结构的辅助配位体的理想选择,既可以进行双齿配位形成不同的构造,也可以进行单齿配位作为终端配体,从而形成各种各样的一维链状,二维层状和三维网状结构[4-5]。但是,迄今为止,基于呋喃-2,5-二羧酸和联吡啶构造新的过渡金属有机配合物还少有研究,Sen等人报道了1D+1D→2D网络结构的金属有机配合物[6],Li等人获得一种三维金属有机配合物[7]。但涉及利用呋喃-2,5-二羧酸和3,3’-二甲基-4,4’-联吡啶合成的过渡金属有机配合物还未见报导。
参考文献:
[1]C.L.Chang,X.Y.Qi,J.W.Zhang,Y.M.Qiu,X.J.Li,X.Wang,Y.Bai,J.L.Sun,H.W.Liu,Chem.Commun.51,3566(2015).
[2]F.Bu,Q.Lin,Q.Zhai,L.Wang,T.Wu,S.T.Zheng,X.Bu,P.Feng,Angew.Chem.Int.Ed.51,8538(2012).
[3]F.P.Huang,J.L.Tian,G.J.Chen,D.D.Li,W.Gu,X.Liu,S.P.Yan,D.Z.Liao,P.Cheng,CrystEngComm 12,1269(2010).
[4]K.Biradha,M.Sarkar,L.Rajput,Chem.Commun.4169(2006).
[5]H.Guo,J.Lei,L.Qin,Y.Liang,J.Yan,W.Lin,W.Ding,H.Sakiyama,J.Liu,D.Ma,J.Inorg.Organomet.Polym.26,413(2016).
[6]R.Sen,D.Mal,P.Brandao,R.A.S.Ferreira,Z.Lin,Cryst.Growth Des.13,5272(2013).
[7]Y.F.Li,Y.Gao,X.L.Qin,Y.Xu,W.Y.Gao,L.Zhang,Inorg.Chem.Commun.25,86(2012).
发明内容
本发明的目的是提供一种基于铜(II)的双核金属有机配合物,该铜(II)金属有机配合物具有很好的反铁磁性。
本发明解决上述问题的技术方案是:
一种基于铜(II)的双核金属有机配合物,该金属有机配合物是重复单元为Cu(fdc)(dmbpy)(H2O)的铜(II)金属有机配合物,所述的重复单元的化学式Cu(fdc)(dmbpy)(H2O)中的fdc为呋喃-2,5-二羧酸,dmbpy为3,3’-二甲基-4,4’-联吡啶;所述的铜(II)金属有机配合物具有一维阶梯链状结构,其空间群为Pī,晶胞参数分别为 α=66.666(2)°,β=74.466(2)°,γ=67.940(2)°,红外光谱数据(KBr)为:3416(vs),2975(w),1609(vs),1571(vs),1360(s),1221(m),1070(m),1022(w),973(w),788(s),730(w),638(m),497(m)cm-1。
上述铜(II)金属有机配合物在常温下为蓝色晶体,其重复结构单元含有一个Cu2+阳离子,一个fdc2-阴离子,一个dmbpy配体和一个配位水分子。每个Cu2+为六配位结构,分别与来自2个fdc配体中的3个羧基氧原子以桥连和螯合的方式配位、与2个dmbpy配体中的2个N原子桥连配位,以及一个水分子配位,连接成畸变八面体构型。其中,Cu2+作为六连接节点,fdc配体作为三连接节点,dmbpy配体作为二连接节点,形成一维阶梯链状结构。
本发明所述的铜(II)金属有机配合物是将呋喃-2,5-二羧酸与Cu(NO3)2·3H2O和dmbpy反应得到。
本发明所述的基于铜(II)的双核金属有机配合物的制备方法,包括以下步骤:
(1)将H2fdc溶解分散在水中,用NaOH溶液将pH调至7.0~8.0,得到配体溶液;
(2)在配体溶液中加入等摩尔量的Cu(NO3)2·3H2O和dmbpy,;然后将混合溶液加入到23mL聚四氟乙烯反应釜中,自生压力下保持130℃反应72小时;
(3)将步骤2得到的产物过滤,收集晶体,并用无水乙醇洗涤后干燥,得到所述的基于铜(II)的双核金属有机配合物。
本发明所述的基于铜(II)的双核金属表现出良好的反铁磁性质。
本发明所述的基于铜(II)的双核金属的其制备方法具有以下优点:反应条件温和,纯度高,无毒无害,做到了绿色化学,无需惰性气体保护;原料来源广泛,容易获得。
附图说明
图1为fdc和dmbpy配体的连接节点图。
图2为Cu2+的六连接节点图。
图3为本发明所述基于铜(II)的双核金属有机配合物的一维阶梯链状结构图。
图4为本发明所述基于铜(II)的双核金属有机配合物的变温磁化率。
具体实施方式
实施例1
1、基于铜(II)的双核金属有机配合物的制备
制备方法包括以下步骤:
(1)将0.25mmol(0.039mg)的呋喃-2,5-二羧酸溶解分散在水中,并且使用NaOH(0.016g,0.4mmol)溶液调节pH值7.0-8.0,得到配体溶液;
(2)在配体溶液中加入等摩尔量的Cu(NO3)2·3H2O(0.060g;0.25mmol)和3,3’-二甲基-4,4’-联吡啶(0.046g;0.25mmol);
(3)将混合溶液加入到23mL聚四氟乙烯反应釜中,在自生压力下保持130℃反应72小时,然后以5℃/h的速率降至室温;
(4)将步骤3中的混合物过滤,收集晶体,并用无水乙醇洗涤后干燥,获得蓝色晶体(经测试产率:48%)。
2、基于铜(II)的双核金属有机配合物的鉴定
通过下述元素分析、IR光谱和X-射线单晶衍射分析鉴定,上述步骤1所得到的蓝色晶体为本发明所述的基于铜(II)的双核金属有机配合物,其重复单元的分子式为Cu(fdc)(dmbpy)(H2O)。
(1)元素分析C18H16CuN2O6:理论值:C,51.4;H,3.8;N,6.7;实验值:C,52.0;H,4.1;N,5.4。
(2)红外光谱(KBrpellet,cm-1):3416(vs),2975(w),1609(vs),1571(vs),1360(s),1221(m),1070(m),1022(w),973(w),788(s),730(w),638(m),497(m)。
(3)X-射线单晶衍射:晶体学参数和部分键长如表1和表2所示。X-射线单晶衍射结果表明,基于铜(II)的双核金属有机配合物中的重复单元为不对称单元,每个不对称单元中含有一个Cu2+阳离子,一个fdc2-阴离子,一个dmbpy配体和一个配位水分子。每个Cu2+为六配位结构,分别与来自2个fdc配体中的3个羧基氧原子、2个dmbpy配体中的2个N原子和一个水分子配位,构成畸变八面体构型。其中fdc配体作为三连接节点(图1a),dmbpy配体作为二连接节点(图1b)。如图2所示,每个Cu2+与2个fdc配体中的氧原子以螯合(O1和O3)和桥连(O4ii)方式配位,与dmbpy配体以桥连方式配位(N1和N2i),水分子作为终端配体连接(O1W)。每2个Cu2+与2个fdc配体形成双核结构单元,2个dmbpy配体将相邻的双核结构单元连接成一维阶梯链状结构(图3)。
表1.Cu(fdc)(dmbpy)(H2O)的晶体学参数
R=∑(‖Fo|-|Fc‖)/∑|Fo|.wR=[∑w(Fo 2–Fc 2)2/∑w(Fo)2]1/2.
表2.Cu(fdc)(dmbpy)(H2O)的部分键长键角
Cu1-O4ii | 1.959(2) | Cu1-O3 | 1.964(2) |
Cu1-N1 | 2.020(2) | Cu1-N2i | 2.043(3) |
O4ii-Cu1-O3 | 168.43(9) | O4ii-Cu1-N1 | 89.08(10) |
O3-Cu1-N1 | 90.49(10) | O4ii-Cu1-N2i | 89.09(10) |
O3-Cu1-N2i | 90.23(10) | N1-Cu1-N2i | 174.34(11) |
O4ii-Cu1-O1W | 105.42(10) | O3-Cu1-O1W | 86.15(10) |
N1-Cu1-O1W | 94.07(11) | N2i-Cu1-O1W | 91.58(11) |
对称Cudes:i=x,y,-1+z;ii=2–x,-y,-z。
实施例2:双核金属有机配合物的变温磁化率
本实施例采用实施例1得到的基于铜(II)的双核金属有机配合物的变温磁化率。具体研究方法如下所述:
(1)本发明所述的外加磁场:1kOe。
(2)变温磁化率的温度范围:300K-2K。
(3)实验结果
变温磁化率结果(如图4)显示:本发明所述的基于铜(II)的双核金属有机配合物在300K-2K范围内显示反铁磁性。
Claims (2)
1.一种基于铜(II)的双核金属有机配合物,其特征在于:所述金属有机配合物是重复单元为Cu(fdc)(dmbpy)(H2O)的铜(II)金属有机配合物,所述的重复单元的化学式Cu(fdc)(dmbpy)(H2O)中的fdc为呋喃-2,5-二羧酸,dmbpy为3,3’-二甲基-4,4’-联吡啶;所述的铜(II)金属有机配合物具有一维阶梯链状结构,其空间群为Pī,晶胞参数分别为α=66.666(2)°,β=74.466(2)°,γ=67.940(2)°,红外光谱数据(KBr)为:3416(vs),2975(w),1609(vs),1571(vs),1360(s),1221(m),1070(m),1022(w),973(w),788(s),730(w),638(m),497(m)cm-1。
2.如权利要求1所述的基于铜(II)的双核金属有机配合物的制备方法,其特征在于,所述方法包括以下步骤:
(1)将H2fdc溶解分散在水中,用NaOH溶液将pH调至7.0~8.0,得到配体溶液;
(2)在配体溶液中加入等摩尔量的Cu(NO3)2·3H2O和dmbpy,;然后将混合溶液加入到23mL聚四氟乙烯反应釜中,自生压力下保持130℃反应72小时;
(3)将步骤2得到的产物过滤,收集晶体,并用无水乙醇洗涤后干燥,得到所述的基于铜(II)的双核金属有机配合物。
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CN107794036A (zh) * | 2017-09-25 | 2018-03-13 | 桂林理工大学 | 基于噻吩‑2,5‑二羧酸和4,4′‑联吡啶构筑的金属有机框架化合物的合成及应用 |
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CN107794036A (zh) * | 2017-09-25 | 2018-03-13 | 桂林理工大学 | 基于噻吩‑2,5‑二羧酸和4,4′‑联吡啶构筑的金属有机框架化合物的合成及应用 |
CN111154113A (zh) * | 2019-12-31 | 2020-05-15 | 肇庆学院 | 一种基于双核钴(ⅱ)的金属有机配合物及其制备方法 |
CN111154112A (zh) * | 2019-12-31 | 2020-05-15 | 肇庆学院 | 一种基于6-(4-羧基苯基)烟酸的三核锌金属有机配位化合物及其制备方法 |
CN111154114A (zh) * | 2019-12-31 | 2020-05-15 | 肇庆学院 | 一种基于5-乙氧基间苯二甲酸的锌(ⅱ)金属有机配位化合物及其制备方法 |
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