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Vol 45, No 12 (2019)

Article

Formation of New Unusual Cadmium Polymer with Bridging Thiocyanate Ions

Kokunov Y.V., Kovalev V.V., Kiskin M.A., Razgonyaeva G.A., Eremenko I.L.

Abstract

The reaction of cadmium thiocyanate with 2-(methylamino)pyridine (2-Map) in an ethyl alcohol solution gave a new unusual coordination polymer [Cd2(NCS)4(2-Map)3]. The structure of the polymer was determined (CIF file CCDC no. 1917586). The crystals are triclinic, space group P\(\bar {1}\). The polymer elementary unit is composed of binuclear [Cd2 (NCS)4(2-Map)3] moiety in which the Cd atoms are connected by μ-NCS bridges. The Cd(1) environment is completed to an octahedron (CdS2N4) via coordination of two pyridine nitrogen atoms of the 2-Map molecules in the apical positions. The Cd(2) coordination environment (CdS2N3) is a trigonal bipyramid supplemented by the pyridine nitrogen atom of the 2-Map molecule. The uncoordinated nitrogen atoms of the NH group are involved in the intrachain H-bonds with the NCS-group nitrogen atoms. The luminescence spectrum of the synthesized compounds was recorded.

Russian Journal of Coordination Chemistry. 2019;45(12):831-835
pages 831-835 views

Solvothermal Synthesis of the Metal-Organic Framework MOF-5 in Autoclaves Prepared by 3D Printing

Denisov G.L., Primakov P.V., Korlyukov A.A., Novikov V.V., Nelyubina Y.V.

Abstract

The known metal-organic framework {Zn4O(BDC)3} (MOF-5 (I), where BDC is terephthalate anion) is synthesized by the solvothermal method in autoclaves prepared by 3D printing from polypropylene. The synthesized polymer is isolated in the individual state and characterized by elemental analysis and powder X-ray diffraction analysis. The crystal structures of MOF-5 and another coordination polymer based on zinc(II) terephthalate {Zn4O(BDC)3} · (ZnO)0.125 (SUMOF-2 (II)) obtained as a by-product of the solvothermal synthesis are confirmed by X-ray diffraction analysis (СIF files ССDС nos. 1920366 (I) and 1926136 (II)).

Russian Journal of Coordination Chemistry. 2019;45(12):836-842
pages 836-842 views

Dianilineglyoxime Salt and Its Binuclear Zn(II) and Mn(II) Complexes with 1,3-Benzenedicarboxylic Acid: Synthesis and Structures

Ureche D., Bulhac I., Rija A., Coropceanu E., Bourosh P.

Abstract

Single crystals of dianilineglyoxime (DAnH2) in the form of hydrate salts [DAnH3](ClO4) ∙ H2O (I) and [DAnH3](ClO4) ∙ 1.25H2O (II) are obtained. Three binuclear zinc(II) and manganese(II) compounds with dianilineglyoxime and 1,3-benzenedicarboxylic acid (1,3-Н2Bdc) are synthesized: [Zn2(DAnH2)2(1,3-Bdc)2(DMF)4] ∙ 2DMF ∙ MeOH · 1.5H2O (III), [Mn2(DAnH2)2(1,3-Bdc)2(DMF)4] ∙ 2DMF (IV), and {[Mn2(DAnH2)2(1,3-Bdc)2(DMF)2(CH3OH)2][Mn2(DAnH2)2(1,3-Bdc)2(DMF)4] ∙ 2CH3OH} (V). The compositions and structures of compounds IV are confirmed by IR spectroscopy and X-ray diffraction analysis (CIF files CCDC nos. 1906360 (I), 1906362 (II), 1906361 (III), 1906363 (IV), and 1906364 (V)). The X-ray diffraction data show that DAnH2 coordinates to the metal ions via the bidentate chelate mode, whereas (1,3-Вdc)2– coordinates to the metal ions via the bidentate bridging mode to form binuclear structures. As the most part of α-dioximes, one neutral DAnH2 coordinates to each metal atom by two nitrogen atoms, whereas two (1,3-Вdc)2– anions coordinate to the metal atom by one oxygen atom each. The coordination polyhedra of the metals in compounds IIIV are built up by the oxygen atoms of DMF and CH3OH.

Russian Journal of Coordination Chemistry. 2019;45(12):843-855
pages 843-855 views

Cyclometalated Iridium(III) Complexes with a Norbornene-Substituted Picolinate Ligand and Electroluminescent Polymers Based on them

Begantsova Y.E., Bochkarev L.N., Baranov E.V., Ilichev V.A.

Abstract

New cyclometalated iridium(III) complexes, NBEpicIr(Ppy)2 (I) and NBEpicIr(Dfppy)2 (II), were synthesized (NBEpicH = 3-(((1S,4S)-bicyclo[2.2.1]hept-5-ene-2-carbonyl)oxy)picolinic acid, PpyH = 2-phenylpyridine, DfppyH = 2-(2,4-difluorophenyl)pyridine). Complex I was characterized by X‑ray diffraction analysis (CIF file CCDC no. 1878882). Ring opening metathesis polymerization involving compounds I and II and carbazole norbornene monomers gave new iridium-containing copolymers. The photophysical properties of complexes I and II and copolymers based on them were studied.

Russian Journal of Coordination Chemistry. 2019;45(12):856-866
pages 856-866 views

Cu(II), Ni(II), and Co(II) Complexes of Tetradentate Azomethine Ligands: Chemical and Electrochemical Syntheses, Crystal Structures, and Magnetic Properties

Lifintseva T.V., Burlov A.S., Vlasenko V.G., Koshchienko Y.V., Garnovskii D.A., Mashchenko S.A., Levchenkov S.I., Lazarenko V.A., Khrustalev V.N., Trigub A.L.

Abstract

Complexes CuL1 ⋅ MeOH (Ia), NiL1 ⋅ MeOH (Ib), CоL1 ⋅ MeOH (Ic), CuL2 (IIa), NiL2 (IIb), and CоL2 (IIc) of the tetradentate azomethine compounds, namely, 4-methyl-N-[2-[(E)-2-[2-[2-[(E)-[2-(p-toluenesulfamino)phenyl]methyleneamino]ethoxy]ethyliminomethyl]phenyl]benzenesulfamide (H2L1) and 4-methyl-N-[2-[(E)-3-[4-[3-[(E)-[2-(p-toluenesulfamino)phenyl]methyleneamino]propoxy]butoxy]-propyliminomethyl]phenyl]benzenesulfamide (H2L2), which are the condensation products of 2-(N-tosylamino)benzaldehyde with 3,4-dioxa-1,8-octanediamine and 4,9-dioxa-1,12-dodecanediamine, are synthesized using the chemical and electrochemical methods. The structures, compositions, and properties of the synthesized metal complexes are studied by the methods of elemental analysis, IR spectroscopy, X-ray absorption spectroscopy, magnetochemistry, and X-ray diffraction analysis (СIF files CCDC nos. 1910746 (Ia), 1910747 (Ib), and 1910748 (Ic)). In the molecules of compounds IaIc, the L1 macrocyclic ligand coordinates the metal atom by four nitrogen atoms via the tetradentate chelate mode to form the polyhedron as a distorted tetrahedron.

Russian Journal of Coordination Chemistry. 2019;45(12):867-875
pages 867-875 views

Molecular and Inner Complex Compounds of Dioxomolybdenum(VI) with Disubstituted Salicydenealcoholimines: Crystal Structure of 1 : 1 Dioxo(3,5-Dibromosalicylidenemonoethanoliminato)molybdenum(VI) Solvate with Methanol [MoO2(L1) · MeOH] (L1 = C9H7Br2NO2)

Sergienko V.S., Abramenko V.L., Gorbunova Y.E., Churakov A.V.

Abstract

Complexes of dioxomolybdenum(VI) of the molecular (МоО2Сl2 · 2H2L) and inner complex ([MoO2L · Solv]) types are synthesized (H2L are azomethines, derivatives of disubstituted R1,R2-salicylaldehydes (R1, R2 = 3.5-Вr2; R1 = 3-МеО, R2 = 5-Вr) and monoethanolamine; Solv is a methanol, dimethylformamide, pyridine, or α-picoline molecule). The cis-octahedral structure of the complexes is concluded on the basis of the IR spectroscopic data. In the molecular compounds, the ligands are coordinated via the O atom of the carbonyl group of the H2L tautomeric form. In the inner complex compounds, the ligands are coordinated in the deprotonated benzoid form. The structure of [MoO2(L1) · МеОН] (I) (where L1 is C9H7Br2NO2) is determined by X-ray diffraction analysis (СIF file CCDC no. 1898088). In the mononuclear molecule of compound I, the Mo atom has the octahedral coordination by two oxo ligands, two oxygen atoms, the nitrogen atom of the tridentate bis(chelate) two-charge ligand (L1)2–, and the O atom of the methanol molecule. The neutral N(1) and O(1) atoms of the L1 and МеОН ligands, respectively, are arranged in the trans positions to the O(oxo) ligands. The Mo–N(1) (2.265 Å) and Мо–О(1) (2.372 Å) bonds are substantially elongated due to the structural manifestation of the trans effect of the multiply bonded oxo ligands. The intermolecular hydrogen bonds (МеОН)О–Н···О(oxo) join the molecules into supramolecular 1D chains.

Russian Journal of Coordination Chemistry. 2019;45(12):876-882
pages 876-882 views

Tris(1,5-dimethyl-1H-pyrazol-4-yl)-4,4,4-trifluorobutane-1,3-dionato)(dimethanol)terbium(III): synthesis, crystal structure, and luminescent properties

Taydakov I.V., Avetisov R.I., Datskevich N.P.

Abstract

The neutral complex [Tb(L3)(MeOH)2] was unexpectedly formed as the major product of the reaction of Tb(NO3)3 ∙ 6H2O with 1-(1,5-dimethyl-1H-pyrazol-4-yl)-4,4,4-trifluorobutane-1,3-dione (HL) and CsOH in aqueous alcohol in 1 : 4 : 4 molar ratio of the reactants. The composition of the complex was confirmed by elemental analysis and X-ray diffraction stidy (CIF file CCDC no. 1876652); luminescent properties of the complex were investigated.

Russian Journal of Coordination Chemistry. 2019;45(12):883-888
pages 883-888 views

Tin(IV) Complexes with Salen Type Schiff base: Synthesis, Spectroscopic Characterization, Crystal Structure, Antibacterial Screening and Cytotoxicity

Ali S., Ara T., Danish M., Shujah S., Slawin A.M.

Abstract

A series of six tin(IV) complexes [SnCl2(L) (I), Me2Sn(L) (II), Bu2Sn(L) (III), Ph2Sn(L) (IV), Oct2Sn(L) (V), BuSnCl(L) (VI)] derived from N,N'-bis(2-hydroxy-1-naphthylidene)-1,2-diaminobenzene [LH2] have been synthesized. The obtained compounds were characterized by elemental analysis, mass spectrometry, FT-IR and NMR (1H, 13C) spectroscopy. The crystal structures of compounds (IV) and (VI) have also been determined by single crystal X-ray analysis (CIF files CCDC nos. 856596 (IV) and 856595 (VI)). The study revealed that the complexes exist as discrete monomeric species and the tin atom is hexa-coordinated in a distorted octahedral geometry. The two phenyl groups in compound (IV) are at trans-positions. Similarly, in complex (VI) the butyl and chloro groups also adopt trans-orientation. The in vitro antibacterial screening and cytotoxicity investigations revealed that the biological activities significantly depend upon the alkyl or others groups present on tin atom. Most of the tin(IV) complexes are active against Escherichia coli and highest activity is shown by complex (IV) against Bacillus subtilis. Furthermore, complex (IV) has also demonstrated the highest cytotoxicity against brine shrimp with LD50 value 0.858 μg/mL.

Russian Journal of Coordination Chemistry. 2019;45(12):889-898
pages 889-898 views

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