Synthesis, crystal structures and magnetic and electrochemiluminescence properties of three manganese(II) complexes

2020 ◽  
Vol 76 (3) ◽  
pp. 236-243 ◽  
Author(s):  
Yating Chen ◽  
Shaonan Zhang ◽  
Yu Xiao ◽  
Shuhua Zhang

Three novel complexes, namely, penta-μ-acetato-bis(μ2-2-{[2-(6-chloropyridin-2-yl)hydrazinylidene]methyl}-6-methoxyphenolato)-μ-formato-tetramanganese(II), [Mn4(C13H11ClN3O2)2(C2H3O2)5.168(CHO2)0.832], 1, hexa-μ2-acetato-bis(μ2-2-{[2-(6-bromopyridin-2-yl)hydrazinylidene]methyl}-6-methoxyphenolato)tetramanganese(II), [Mn4(C13H11BrN3O2)2(C2H3O2)6], 2, and catena-poly[[μ2-acetato-acetatoaqua(μ2-2-{[2-(6-chloropyridin-2-yl)hydrazinylidene]methyl}-6-methoxyphenolato)dimanganese(II)]-μ2-acetato], [Mn2(C13H11ClN3O2)(C2H3O2)3(H2O)] n , 3, have been synthesized using solvothermal methods. Complexes 1–3 were characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. Complexes 1 and 2 are tetranuclear manganese clusters, while complex 3 has a one-dimensional network based on tetranuclear Mn4(L 1)2(CH3COO)6(H2O)2 building units (L 1 is 2-{[2-(6-chloropyridin-2-yl)hydrazinylidene]methyl}-6-methoxyphenolate). Magnetic studies reveal that complexes 1–3 display dominant antiferromagnetic interactions between MnII ions through μ2-O bridges. In addition, 1–3 also display favourable electrochemiluminescence (ECL) properties.

Author(s):  
Sergei V. Voitekhovich ◽  
Berthold Kersting ◽  
Oleg A. Ivashkevich

The dinuclear nickel(II) complex [Ni2LmClO4] + , where Lm represents a 24-membered macrocyclic hexaaza-dithiophenolate ligand, reacts with 5-(4-pyridyl)tetrazole (PyrCN4H) to give the dinuclear complex [Ni2Lm(PyrCN4)]+ . The new complex was both isolated as perchlorate or tetraphenylborate salts and characterised by elemental analysis and IR spectroscopy. The structure of [Ni2Lm(PyrCN4)]BPh4 ⋅ MeCN was determined by single crystal X-ray diffraction, showing that tetrazolate units are in a N2,N3-bridging mode to generate dioctahedral N3Ni(µ-S)2(µ-N4CPyr)NiN3 core.


2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.


2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.


2020 ◽  
Vol 76 (7) ◽  
pp. 690-694
Author(s):  
Qianjun Deng ◽  
Jiming Wang ◽  
Guangzhao Li ◽  
Shuhua Zhang

A new ionic pentanuclear FeIII cluster, namely, triethylazanium tetrakis(μ2-5-amino-1,2,3,4-tetrazolido)tetrakis(μ3-4-chloro-2-{[(1H-tetrazol-1-id-5-yl)imino]methyl}phenolato)di-μ3-oxido-pentairon(III) acetonitrile monosolvate monohydrate, (C6H16N)[Fe5(C8H4ClN5O)4(CH2N5)4O2]·CH3CN·H2O, was synthesized using microvial synthesis methods and characterized by elemental analysis, FT–IR spectroscopy, single-crystal X-ray diffraction and thermogravimetric analysis. Magnetic studies reveal that the complex displays dominant antiferromagnetic intracluster interactions between the FeIII ions through the μ3-oxide bridges.


2005 ◽  
Vol 58 (2) ◽  
pp. 115 ◽  
Author(s):  
Chun-Long Chen ◽  
Qian Zhang ◽  
Ji-Jun Jiang ◽  
Qin Wang ◽  
Cheng-Yong Su

The reaction of AgCF3CO2 with nitrilotriacetate (NTA) yields the three-dimensional silver(i) coordination polymer {Ag3[N(CH2COO)3]}n 1 which was characterized by means of elemental analysis and IR spectroscopy as well as X-ray diffraction. The single crystal structure shows that the NTA3– anions act as unusual heptadentate 13-coordination agents and the silver(i) atoms exhibit various coordination numbers in the range 3–6.


Author(s):  
Shao-Dong Li ◽  
Feng Su ◽  
Cheng-Yong Zhou ◽  
Qi-Long Hu ◽  
Ya-Qi Li ◽  
...  

Two new isostructural complexes, namely, poly[aqua[μ3-2-(4-carboxyphenoxy)terephthalato-κ3 O 1:O 4:O 4′](1,10-phenanthroline-κ2 N,N′)cobalt(II)], [Co(C15H8O7)(C12H8N2)(H2O)] n or [Co(μ3-Hcpota)(phen)(H2O)] n , I, and poly[aqua[μ3-2-(4-carboxyphenoxy)terephthalato-κ3 O 1:O 4:O 4′](1,10-phenanthroline-κ2 N,N′)nickel(II)], [Ni(C15H8O7)(C12H8N2)(H2O)] n or [Ni(μ3-Hcpota)(phen)(H2O)] n , II, have been synthesized by solvothermal reactions. Complexes I and II were fully characterized by IR spectroscopy, elemental analyses, thermogravimetric analyses, and powder and single-crystal X-ray diffraction. They both present two-dimensional structures based on [M 2(μ-COO)2]2+ (M = CoII or NiII) dinuclear metal units with a fes topology and a vertex symbol (4·82). Interestingly, the positions of the two dimeric metal motifs and the two partially deprotonated Hcpota2− ligands reproduce regular flying butterfly arrangements flipped upside down and sharing wings in the ab plane. Magnetic studies indicate antiferromagnetic interactions (J = −5.21 cm−1 for I and −11.53 cm−1 for II) in the dimeric units, with Co...Co and Ni...Ni distances of 4.397 (1) and 4.358 (1) Å, respectively, that are related to double syn–anti carboxylate bridges.


2019 ◽  
Vol 74 (3) ◽  
pp. 261-265 ◽  
Author(s):  
Gao-Feng Wang ◽  
Shu-Wen Sun ◽  
Wei-Bing Wang ◽  
Hong Sun ◽  
Shao-Fei Song

AbstractTwo coordination polymers, {[Co(bipmo)(tbip)]·3H2O}n (1) and {[Cd(bipmo)(tbip)]·3H2O}n (2) (bipmo=bis(4-(1H-imidazol-1-yl)phenyl)methanone, H2tbip=5-tert-butylisophthalic acid), were synthesized by solvothermal methods and structurally characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. The results from single-crystal X-ray diffraction data indicate that the solid state structures of 1 and 2 consist of metal-aromatic carboxylate layers, which are pillared by weak interactions to generate a three-dimensional network. The topological structures of 1 and 2 are uninodal nets based on 3-connected nodes with the Schläfli symbol of {63}.


CrystEngComm ◽  
2015 ◽  
Vol 17 (3) ◽  
pp. 653-664 ◽  
Author(s):  
Lei-Lei Liu ◽  
Cai-Xia Yu ◽  
Ya-Ru Li ◽  
Jing-Jing Han ◽  
Feng-Ji Ma ◽  
...  

Solvothermal reactions of Cd(OAc)2·2H2O with 2,2′-azodibenzoic acid and five positional isomeric N-donor bipyridyl benzene ligands in MeOH/H2O at 170 °C gave rise to five coordination polymers. Complexes 1–5 were characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction.


Author(s):  
Petar Stanic ◽  
Marko Rodic ◽  
Tanja Soldatovic ◽  
Aleksandar Pavic ◽  
Natasa Radakovic ◽  
...  

The 3-arylidene-2-thiohydantoin derivative, 3-[(2-hydroxybenzyl-idene)amino]-2-thioxoimidazolidin-4-one, was synthesized in a two-step condensation reaction of 2-hydroxybenzaldehyde, thiosemicarbazide and ethyl chloroacetate. The ligand was structurally characterized by NMR and IR spectroscopy, as well as elemental analysis. In the reaction of the well-known polymeric trans-[CuCl2(DMSO)2]n complex with the polydentate thiohydantoin type ligand, instead of the corresponding copper thiohydantoin complex, unexpectedly, the dinuclear cis-[{CuCl(DMSO)2}(m-Cl)]2 complex (1) was formed predominantly as the final stable product. The structure of the complex 1 was confirmed by single crystal X-ray diffraction analysis. The cis-complex is obtained through assisted isomerization of the trans-form, in which the thiohydantoin derivative has a crucial role.


2018 ◽  
Vol 74 (11) ◽  
pp. 1284-1288 ◽  
Author(s):  
Zhong Zhang ◽  
Yue-Lin Wang ◽  
Guo-Yu Yang

A novel zirconium(IV)-substituted tetramer polyoxotungstate, H6K4Na16[Zr4(β-GeW10O38)2(A-α-PW9O34)2]·37H2O, was synthesized hydrothermally and characterized by IR spectroscopy, elemental analysis, thermogravimetric analysis, powder X-ray diffraction, energy-dispersive X-ray spectroscopy and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic P2/n space group. The most remarkable feature is that the centrosymmetric Zr-based polyoxotungstate tetramer consists of dilacunary Keggin-type germanotungstate and trilacunary Keggin-type phosphotungstate units that are linked by ZrIV ions.


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