CN104788363A - 一种三氮烯-钴(iii)单核配合物及其制备方法 - Google Patents
一种三氮烯-钴(iii)单核配合物及其制备方法 Download PDFInfo
- Publication number
- CN104788363A CN104788363A CN201510124059.6A CN201510124059A CN104788363A CN 104788363 A CN104788363 A CN 104788363A CN 201510124059 A CN201510124059 A CN 201510124059A CN 104788363 A CN104788363 A CN 104788363A
- Authority
- CN
- China
- Prior art keywords
- triazene
- cobalt
- pyridine
- iii
- coordination compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims description 7
- 238000010668 complexation reaction Methods 0.000 title 1
- 239000013078 crystal Substances 0.000 claims abstract description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 30
- AYNNSCRYTDRFCP-UHFFFAOYSA-N triazene Chemical group NN=N AYNNSCRYTDRFCP-UHFFFAOYSA-N 0.000 claims description 22
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012954 diazonium Substances 0.000 claims description 8
- 150000001989 diazonium salts Chemical class 0.000 claims description 8
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000006193 diazotization reaction Methods 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- VAMXMNNIEUEQDV-UHFFFAOYSA-N methyl anthranilate Chemical class COC(=O)C1=CC=CC=C1N VAMXMNNIEUEQDV-UHFFFAOYSA-N 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 4
- 235000010288 sodium nitrite Nutrition 0.000 claims description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 3
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical class [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 230000005595 deprotonation Effects 0.000 claims description 2
- 238000010537 deprotonation reaction Methods 0.000 claims description 2
- 125000000623 heterocyclic group Chemical group 0.000 claims description 2
- 125000006850 spacer group Chemical group 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 239000003446 ligand Substances 0.000 abstract description 4
- XTZNUMUGTYZOIP-UHFFFAOYSA-N 3-(aminodiazenyl)pyridin-2-amine Chemical compound NN=NC1=CC=CN=C1N XTZNUMUGTYZOIP-UHFFFAOYSA-N 0.000 abstract 1
- 210000002858 crystal cell Anatomy 0.000 abstract 1
- -1 Triazenes compound Chemical class 0.000 description 3
- 150000004654 triazenes Chemical group 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- HWYNRVXFYFQSID-UHFFFAOYSA-M benzo[a]phenoxazin-9-ylidene(dimethyl)azanium;chloride Chemical compound [Cl-].C1=CC=C2C(N=C3C=CC(C=C3O3)=[N+](C)C)=C3C=CC2=C1 HWYNRVXFYFQSID-UHFFFAOYSA-M 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/76—Nitrogen atoms to which a second hetero atom is attached
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
2-氨基吡啶基三氮烯为配体，合成出了未见报道的三氮烯-钴(III)单核配合物Co(C13H11N4O2)3，并通过X-ray单晶衍射对配合物晶体结构进行了表征，配合物属三斜晶系，P1空间群，晶胞参数：a=15.929(2)?，b=15.929(2)?，c=63.589(13)?，α=90°，β=90°，γ=120°；分子式：C39H33N12CoO6，Mr=823.26，V=1397.3(4)?3，Z=2，Dc=1.320Mgm-3，F(000)=577，I＞2σ(I)的数据：最终偏离因子R1=0.0697，wR2=0.1593；全部数据：R1=0.0756，wR2=0.1566。
Description
技术领域
本发明属三氮烯金属配合物制备领域，尤其涉及一种三氮烯-钴(III)单核配合物及其制备方法。
背景技术
三氮烯是指含有重氮化氨基基团(-N=N-N<)的化合物，三氮烯类化合物因其含有重氮化氨基基团(-N=N-N<)，具有较好的热力学稳定性及可修饰性，进而容易与金属离子形成三氮烯-金属配合物，因此，三氮烯类化合物在药物学、全合成、聚合物技术、构建异环体系等领域具有广阔的应用前景。自Meldola首次合成出三氮烯类配体并将其应用于三氮烯过渡金属配合物后，大量的过渡金属三氮烯配合物已经被人们研究。由于三氮烯与金属潜在的多种配位模式，所以对其的研究逐渐增多，它可以作为单齿配体；螯合配体或者是两个金属中心之间的桥联配体与金属配位。目前为止包括 K,
Ca, Mg, Al, Cu, Pt, Pd, Ag, Co, Ru, Os 等大量三氮烯类金属配合物都已经成功合成。本发明以2-氨基吡啶基三氮烯为配体，合成出了未见报道的三氮烯-钴(III)单核配合物Co(C13H11N4O2)3，并通过X-ray单晶衍射对配合物晶体结构进行了表征。
发明内容
本发明的目的是为了提供了一种新的三氮烯-钴(III)单核配合物及其制备方法，为今后研究三氮烯-钴(III)单核配合物的性质及应用打下基础。
本发明的目的可以通过以下技术方案来实现：
一种新的三氮烯-钴(III)单核配合物的制备方法，其特征在于，包括以下步骤：
(1) 将2.997 g邻氨基苯甲酸甲酯(19.3
mmol)溶解于55 mL(1 mol/L)的盐酸中，在0-5℃搅拌下，缓慢滴加0.2 g/mL的亚硝酸钠水溶液10 mL，滴加完毕后，使重氮化完全，得到澄清的重氮盐溶液；
(2) 与2-氨基吡啶偶联
将1.816 g 2-氨基吡啶(19.3
mmol)溶于10 mL的乙醇溶液中，在0-5℃搅拌下缓慢加入上述重氮盐溶液中，搅拌45 min之后用饱和醋酸钠调节混合液的pH值为7左右，再反应6 h，静置，抽滤，干燥后的粗产品用乙酸乙酯和正己烷按照9：1 的比例-4℃下重结晶1天后，得到2.62g黄色柱状单晶（C13H12N4O2），即，1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯；元素分析实测值(%，理论值)：C 60.91(60.94)，H
4.66(4.68)，N 21.85(21.87)，产率：53.03%；
(3) 金属与2-氨基吡啶三氮烯单核配合物[Co(C13H11N4O2)3]的合成
称取0.0768g(0.3mmol)的1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯，将其溶解于含有5mLCH3CN和5mL乙酸乙酯的混合溶液中，加入3滴三乙胺，在搅拌条件下，加入0.0238g
(0.1mmol) CoCl2·6H2O，在常温下磁力搅拌20min，过滤，得到黄色的澄清溶液，将所得黄色的澄清液静置5天，得到棕色块状晶体，即为三氮烯-钴(III)单核配合物[Co(C13H11N4O2)3]，产量：0.036g，产率：43.7% (以金属Co计算)，元素分析实测值（%，理论值）：C56.88(56.86)，H4.02(4.03)，N20.38(20.40)。
其中，2-氨基吡啶基三氮烯的合成原理为：在低温条件下，用盐酸和亚硝酸钠溶液将邻氨基苯甲酸甲酯重氮化完全，得到澄清重氮盐溶液，然后，在 0-5℃直接将上述重氮盐溶液与2-氨基吡啶的乙醇溶液偶合，之后再调节 pH值，最后合成目标产物1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯。
金属配合物[Co(C13H11N4O2)3]
(尺寸约为0.4 x 0.3 x 0.25 mm)的单晶数据是在113 K下测定，用Bruker Smart
1000 CCD 单晶衍射仪，采用经石墨单色器单色化的MO-Ka射线，辐射波长λ = 0.71073 Å，全部吸收强度数据经SADABS校正。晶体结构通过直接法解出，计算方法采用SHELXTL-97程序，用差值Fourier合成确定所有非氢原子的坐标，所有非氢原子的坐标及各向异性参数采用Shelxl 97程序以小二乘法对F2进行结构精修，分子结构由ORTEP-3作出。
表1配合物[Co(C13H11N4O2)3]晶体数据和结构精修参数
Crystall
data
complex
1
Empirical formula
Co(C13H11N4O2)3
Formula weight
823.62
λ(Å)
0.71073
Crystal system
triclinic
Space
group
P1
Unit cell dimension (Å,°)
a
15.929(2)
b
15.929(2)
c 63.589(13)
α 90
β 90
γ
120
V (Å3)
1397.3(4)
Z 2
Dc(Mgm-3)
1.320
F(000)
577
θ range for data collection
1.51
to 27.01
Reflections collected/unique
7860
/ 3221
Data/restraints/parameters
1203
/ 0 / 83
Goodness-of-fit on F2
1.063
Final R indices [I>2σ(I)]
R 1=
0.0697
wR 2=
0.1593
R indices(all
data)
R 1=
0.0756
wR 2=
0.1566
_____________________________________________________________________
表2 配合物[Co(C13H11N4O2)3]的部分键长和键角
_____________________________________________________________________
Bond distances
Co(2)-N(2)
1.906(3)
Co(2)-N(2)#3
1.906(3)
Co(2)-N(2)#4
1.906(3)
Co(2)-N(4)#4 1.924(3)
Co(2)-N(4)#3
1.924(3)
N(2)-N(1)
1.266(5)
N(2)-N(3) 1.337(5)
N(4)-C(11)
1.351(5)
N(4)-C(15)
1.362(6)
O(2)-C(7)
1.338(6)
O(2)-C(8)
1.461(6) N(1)-C(1)
1.436(5)
N(3)-C(15)#4
1.359(6)
C(1)-C(2)
1.390(6)
C(1)-C(6)
1.390(7)
C(14)-C(13) 1.368(7)
Bond angles
N(2)-Co(2)-N(2)#3
92.85(13)
N(2)-Co(2)-N(2)#4
92.85(13)
N(2)#3-Co(2)-N(2)#4 92.85(13)
N(2)-Co(2)-N(4)
90.95(14)
N(2)#3-Co(2)-N(4) 81.45(14)
N(2)#4-Co(2)-N(4)
173.31(14)
N(2)-Co(2)-N(4)#4 81.45(14)
N(2)#3-Co(2)-N(4)#4
173.31(14)
N (2)#4-Co(2)-N(4)#4
90.95(14)
N(4)-Co(2)-N(4)#4
95.07(14)
N(2)-Co(2)-N(4)#3
173.31(15)
N(2)#3-Co(2)-N(4)#3
90.95(14)
N(2)#4-Co(2)-N(4)#3
81.45(14)
N(4)-Co(2)-N(4)#3
95.07(14)
N(4)#4-Co(2)-N(4)#3 95.07(14)
N(1)-N(2)-N(3)
121.1(3)
N(1)-N(2)-Co(2)
121.1(3)
N(3)-N(2)-Co(2)
117.7(3)
C(11)-N(4)-C(15)
120.2(4)
C(11)-N(4)-Co(2)
129.1(3)
N(2)-N(1)-C(1)
117.0(3) N(2)-N(3)-C(15)#4
110.1(3)
_____________________________________________________________________
配合物[Co(C13H11N4O2)3]属于三斜晶系，P1空间群，单晶 X-射线衍射分析结果表明配合物中包含一个单核钴的[Co(C13H11N4O2)3]的结构，该结构由三个去质子化的1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯配体与一个钴配位连接组成，Co与三氮烯上的N及来自吡啶结构中杂环上的 N进行配位，是典型的六配位对称结构，其ORTEP图及原子编号见说明书附图图2。
钴原子配位数为六，分别与配体吡啶环上三个氮原子和三氮烯上三个氮原子相连，其中Co(2)-N(2)、Co(2)-N(2)#3和Co(2)-N(2)#4的键长为1.906(3)Å，Co(2)-N(4)#4和Co(2)-N(4)#3的键长为1.924(3)Å，Co(2)-N(2)#4的键长为1.906(3)Å，N(2)-N(1)的键长为1.351(5)Å，N(2)-N(3)的键长为1.337(5)Å；N(2)-Co(2)-N(2)#3、N(2)-Co(2)-N(2)#4和N(2)#3-Co(2)-N(2)#4的键角为92.85(13)o，N(2)-Co(2)-N(4)、N
(2)#4-Co(2)-N(4)#4、N(2)#3-Co(2)-N(4)#3、N(4)#4-Co(2)-N(4)#3的键角为90.95(14)o，N(2)#3-Co(2)-N(4)、N(2)-Co(2)-N(4)#4、N(2)#4-Co(2)-N(4)#3的键角为81.45(14)o，N(2)#3-Co(2)-N(4)#4、N(2)-Co(2)-N(4)#3、N(2)#3-Co(2)-N(4)#4的键角为173.31(14)o。
附图说明
图1为本发明1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯的合成步骤；
图2为采用ORTEP作出的配合物[Co(C13H11N4O2)3]的晶体结构图。
具体实施方式
实施例1
(1) 将2.997 g邻氨基苯甲酸甲酯(19.3
mmol)溶解于55 mL(1 mol/L)的盐酸中，在0-5℃搅拌下，缓慢滴加0.2 g/mL的亚硝酸钠水溶液10 mL，滴加完毕后，使重氮化完全，得到澄清的重氮盐溶液；
(2) 与2-氨基吡啶偶联
将1.816 g 2-氨基吡啶(19.3
mmol)溶于10 mL的乙醇溶液中，在0-5℃搅拌下缓慢加入上述重氮盐溶液中，搅拌45 min之后用饱和醋酸钠调节混合液的pH值为7左右，再反应6 h，静置，抽滤，干燥后的粗产品用乙酸乙酯和正己烷按照9：1 的比例-4℃下重结晶1天后，得到2.62g黄色柱状单晶（C13H12N4O2），即，1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯；元素分析实测值(%，理论值)：C 60.91(60.94)，H
4.66(4.68)，N 21.85(21.87)，产率：53.03%；
(3) 金属与2-氨基吡啶三氮烯单核配合物[Co(C13H11N4O2)3]的合成
称取0.0768g(0.3mmol)的1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯，将其溶解于含有5mLCH3CN和5mL乙酸乙酯的混合溶液中，加入3滴三乙胺，在搅拌条件下，加入0.0238g
(0.1mmol) CoCl2·6H2O，在常温下磁力搅拌20min，过滤，得到黄色的澄清溶液，将所得黄色的澄清液静置5天，得到棕色块状晶体，即为三氮烯-钴(III)单核配合物[Co(C13H11N4O2)3]，产量：0.036g，产率：43.7% (以金属Co计算)，元素分析实测值（%，理论值）：C56.88(56.86)，H4.02(4.03)，N20.38(20.40)。
Claims (2)
1.一种三氮烯-钴(III)单核配合物，其特征在于：分子式为：C39H33N12CoO6，其中，配合物中包含一个单核镍的[Co(C13H11N4O2)3]的结构，该结构由三个去质子化的1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯配体与一个钴配位连接组成，Co与三氮烯上的N及来自吡啶结构中杂环上的 N进行配位，钴原子配位数为六，分别与配体吡啶环上三个氮原子和三氮烯上三个氮原子相连，配合物[Co(C13H11N4O2)3]属于三斜晶系，P1空间群，晶胞参数为：a = 15.929(2)Å，b = 15.929(2) Å，c =
63.589(13)Å，α= 90o，β = 90o，γ = 120o，V = 1397.3(4) Å3，Z =
2，Dc = 1.320 Mgm-3，F(000) = 577，I >2σ(I)的数据：最终偏离因子R 1= 0.0697，wR 2 = 0.1593；全部数据：R 1 = 0.0756，wR 2 = 0.1566。
2.一种如权利要求1中所述三氮烯-镍(II)单核配合物制备方法，其特征在于，包括以下步骤：
(1) 将2.997 g邻氨基苯甲酸甲酯(19.3 mmol)溶解于55 ml(1 mol/L)的盐酸中，在0-5℃搅拌下，缓慢滴加0.2
g/mL的亚硝酸钠水溶液10 ml，滴加完毕后，使重氮化完全，得到澄清的重氮盐溶液；
(2) 与2-氨基吡啶偶联
将1.816 g 2-氨基吡啶(19.3 mmol)溶于10 ml的乙醇溶液中，在0-5℃搅拌下缓慢加入上述重氮盐溶液中，搅拌45 min之后用饱和醋酸钠调节混合液的pH值为7左右，再反应6 h，静置，抽滤，干燥后的粗产品用乙酸乙酯和正己烷按照9：1 的比例-4℃下重结晶1天后，得到2.62g黄色柱状单晶（C13H11N4O2），即，1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯；元素分析实测值(%，理论值)：C 60.91(60.94)，H 4.66(4.68)，N 21.85(21.87)，产率：53.03%；
(3) 金属与2-氨基吡啶三氮烯单核配合物[Co(C13H11N4O2)3]的合成
称取0.0768g(0.3mmol)的1-[(2-羧甲基)苯]-3-[2-(吡啶)]三氮烯，将其溶解于含有5mlCH3CN和5ml乙酸乙酯的混合溶液中，加入3滴三乙胺，在搅拌条件下，加入0.0238g
(0.1mmol) CoCl2·6H2O，在常温下磁力搅拌20min，过滤，得到黄色的澄清溶液，将所得黄色的澄清液静置5天，得到棕色块状晶体，即为三氮烯-钴(III)单核配合物[Co(C13H11N4O2)3]，产量：0.036g，产率：43.7% (以金属Co计算)，元素分析实测值（%，理论值）：C56.88(56.86)，H4.02(4.03)，N20.38(20.40)。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510124059.6A CN104788363B (zh) | 2015-03-22 | 2015-03-22 | 一种三氮烯‑钴(iii)单核配合物及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510124059.6A CN104788363B (zh) | 2015-03-22 | 2015-03-22 | 一种三氮烯‑钴(iii)单核配合物及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104788363A true CN104788363A (zh) | 2015-07-22 |
| CN104788363B CN104788363B (zh) | 2017-10-03 |
Family
ID=53553605
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510124059.6A Active CN104788363B (zh) | 2015-03-22 | 2015-03-22 | 一种三氮烯‑钴(iii)单核配合物及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104788363B (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226913A (zh) * | 2017-06-28 | 2017-10-03 | 江汉大学 | 一种以四核钴为节点的框架配位材料及其制备方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB884582A (en) * | 1957-11-12 | 1961-12-13 | Geigy Ag J R | Process for the dyeing and printing of fibrous materials and films |
| CN1127756A (zh) * | 1994-07-01 | 1996-07-31 | 瓦克化学有限公司 | 作为氢化硅烷化催化剂的三氮烯氧化物——过渡金属配合物 |
| CN1669361A (zh) * | 2001-08-29 | 2005-09-14 | 普林斯顿大学理事会 | 具有含金属配合物的载流子阻挡层的有机发光元件 |
| CN1738838A (zh) * | 2003-01-14 | 2006-02-22 | 英诺文尼欧洲有限公司 | 聚合催化剂 |
-
2015
- 2015-03-22 CN CN201510124059.6A patent/CN104788363B/zh active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB884582A (en) * | 1957-11-12 | 1961-12-13 | Geigy Ag J R | Process for the dyeing and printing of fibrous materials and films |
| CN1127756A (zh) * | 1994-07-01 | 1996-07-31 | 瓦克化学有限公司 | 作为氢化硅烷化催化剂的三氮烯氧化物——过渡金属配合物 |
| CN1669361A (zh) * | 2001-08-29 | 2005-09-14 | 普林斯顿大学理事会 | 具有含金属配合物的载流子阻挡层的有机发光元件 |
| CN1738838A (zh) * | 2003-01-14 | 2006-02-22 | 英诺文尼欧洲有限公司 | 聚合催化剂 |
Non-Patent Citations (7)
| Title |
|---|
| WAN-YUAN JIAN，等: "Isolation and Properties of a Chain of Cyano-Bridged Complex {LCuII(m-CN)}n With Triazenido Ligand and a Cyano-Bridged Mixed-Valence Complex {CuIICuI(m-CN)3}n", 《SYNTHESIS AND REACTIVITY IN INORGANIC, METAL-ORGANIC,AND NANO-METAL CHEMISTRY》 * |
| 余钢: "三氮烯配合物的设计合成、性质表征及其电化学催化制氢性能的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 周能，等: "1-(6-硝基-2-苯并噻唑)-3-(5-溴-8-喹啉)-三氮烯与Co(Ⅱ)的高灵敏显色反应及其应用", 《分析试验室》 * |
| 唐计光: "过渡金属、稀土与C4H9N11O含能配合物的合成、表征和性能研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 李玮: "三氮烯过渡金属多核配合物的合成、结构与磁性研究", 《中国博士学位论文全文数据库工程科技I辑》 * |
| 杨明华，等: "1-(6-硝基-2-苯并噻唑)-3-(4-硝基苯)-三氮烯与钴的显色反应", 《浙江师范大学学报(自然科学版)》 * |
| 章汝平，等: "1-(5-硝基-3-苯并异噻唑)-3-[4-(苯基偶氮)苯基]-三氮烯的合成及与钴(Ⅱ)的显色反应", 《冶金分析》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226913A (zh) * | 2017-06-28 | 2017-10-03 | 江汉大学 | 一种以四核钴为节点的框架配位材料及其制备方法 |
| CN107226913B (zh) * | 2017-06-28 | 2021-03-09 | 江汉大学 | 一种以四核钴为节点的框架配位材料及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104788363B (zh) | 2017-10-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102516270B (zh) | 具有二维层状结构的金属银配位聚合物及其制备与应用 | |
| CN104230996A (zh) | 四苯乙烯锰配合物及其制备方法及镉离子荧光探针的应用 | |
| Nepveu et al. | New polynuclear manganese (II) complexes with orotic acid and some of its derivatives: crystal structures, spectroscopic and magnetic studies | |
| Kuriakose et al. | Synthesis, spectroscopic studies and crystal structures of two new vanadium complexes of 2-benzoylpyridine containing hydrazone ligands | |
| CN101914108A (zh) | 4-氨基-3,5-双(2-吡啶基)-1,2,4-三唑-银(i)配合物及其制备方法 | |
| CN107098392A (zh) | 一种基于三价锰离子的砷钨酸夹心型多金属氧酸盐化合物及其制备方法与应用 | |
| CN104788363A (zh) | 一种三氮烯-钴(iii)单核配合物及其制备方法 | |
| Grewe et al. | Crystal and molecular structure of bis (N-benzoylglycinato) triaquozinc (II) dihydrate | |
| CN106397345B (zh) | 一种3-羧基-1，2，4-三氮唑类钴配合物及其原位合成方法 | |
| Hökelek et al. | Diaquabis [4-(dimethylamino) benzoato]-κ2O, O′; κO-(isonicotinamide-κN1) cobalt (II) | |
| CN104292247A (zh) | 一种具有混合配体的含镉二维聚合物及其制备方法 | |
| CN108148096B (zh) | 一种六核钌nnn配合物及其制备和应用 | |
| Munoz et al. | Structures of bis (di-2-pyridylamine) dinitratocopper (II) and bis (acetato) bis (di-2-pyridylamine) copper (II) monohydrate | |
| CN111747889B (zh) | 一种含多个配位点的NNO型喹啉Fe(II)配合物及其制备方法和应用 | |
| CN104761513A (zh) | 一种三氮烯-镍(ii)单核配合物及其制备方法 | |
| Cronin et al. | A new class of macrocycle capable of binding exogenous metals: synthesis, structure, magnetic and electrochemical properties of a Cu (II) trinuclear complex based upon 1, 4, 8, 11-tetraazacyclotetradecane-2, 3-dione [exo O 2] cyclam | |
| Shuai et al. | Diaquabis (1H-imidazole-4-carboxylato-κ2N3, O) zinc | |
| Tabatabaee et al. | Butane-1, 4-diammonium bis (pyridine-2, 6-dicarboxylato-κ3O2, N, O6) cadmate (II) dihydrate | |
| Phuengphai et al. | Synthesis, crystal structure and magnetic properties of an unexpected new coordination Cu (II) compound, containing two different phosphato-bridged dinuclear units;[Cu2 (phen) 2 (μ-H2PO4-O, O′) 2 (H2PO4) 2][Cu2 (phen) 2 (μ-H2PO4-O, O′)(μ-H2PO4-O)(μ-HPO4-O)] 2 (H2O) 9 (phen= 1, 10-phenanthroline) | |
| CN102603780B (zh) | 具有三维开放骨架结构的配位聚合物及其制备与应用 | |
| Hu et al. | STUDIES ON THE ANTITUMOR ANTIMONY (III) TRIAMINOCARBOXYLIC COMPLEXONATES. CRYSTAL STRUCTURES OF NH4 [Sb (Hdtpa)]· H2O AND Na [Sb (Hdtpa)]· 41/2 H2O (dtpa= DIETHYLENETRIAMINEPENTAACETIC ACID) | |
| Chen et al. | (2, 2′-Bipyridine) chlorido [diethyl (2, 2′: 6′, 2′′-terpyridin-4-yl) phosphonate] ruthenium (II) hexafluoridophosphate acetonitrile/water solvate | |
| Lee et al. | Structure of the blue copper (II) complex {[7R (S), 14R (S)]-5, 5, 7, 12, 12, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradecane} nitratocopper (II) perchlorate,[Cu (NO3)(C16H36N4)](ClO4) | |
| Hibbs et al. | The structural characterization of YbI2 (DME) 3 | |
| Yang et al. | A nanoscale slipped sandwich of Tb 10-stabilization of a benzaldehyde methyl hemiacetyl |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Cheng Faliang Inventor after: Zhang Yan Inventor after: Zhang Min Inventor after: Liu Peng Inventor after: Chen Meiqiong Inventor after: Cai Zhiquan Inventor before: Zhang Yan |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170810 Address after: 523808 Guangdong province Dongguan City Songshan Lake Science and Technology Industrial Park University Road No. 1 Applicant after: Dongguan University of technology Applicant after: City College Dongguan University of Technology Address before: 523419 Guangdong city of Dongguan province Hengkeng village Liaobu town Vanke City Golf Garden Tan Kwai Hin 13 block room 1201 Applicant before: Zhang Yan |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |