scholarly journals Hydrogen bonded homodimetallic compounds of the formula [M(H2O)5M(dipic)2]·2H2O, M = CoII or NiII and dipic = dipicolinate anion

2017 ◽  
Vol 10 (2) ◽  
pp. 132-138 ◽  
Author(s):  
Petra Masárová ◽  
Jan Moncol

AbstractTwo homodimetallic dipicolinate compounds of the formulae [Co(H2O)5Co(dipic)2]·2H2O (1) and [Ni(H2O)5Ni(dipic)2]·2H2O (2) have been synthesized and their crystal structures have been determined by single-crystal X-ray diffraction analysis. The prepared isostructural compounds consist of cationic {MO5O’}2+and anionic {MN2O4}2-moieties, where CoII/CoIIor NiII/NiIImetal centers are connected together by bridging μ-carboxylate oxygen atoms from dipicolinate anions. H-bond interactions involving aqua ligands, dipicolinate oxygens and lattice solvent molecules stabilize the dimeric units by linking them into 3-D polymeric networks.

2009 ◽  
Vol 63 (3) ◽  
Author(s):  
Ján Halgaš ◽  
Viera Kolenová ◽  
Zuzana Števíková ◽  
Lucia Perašínová ◽  
Jozef Kožíšek

AbstractAlthough thienopyridines attract attention because of their biological activities, they have not been used as ligands in coordination compounds. Thieno[2,3-b]pyridine was prepared by known procedures; by reduction of 2-nitrothiophene, and reaction of the resulting 2-thienyl ammonium salt with malondialdehyde tetramethylacetal in the presence of zinc chloride. The same procedure was used for the preparation of a new derivative, 2-methylthieno[2,3-b]pyridine, starting from 2-methyl-5-nitrothiophene. The thienopyridines were used in the synthesis of coordination compounds. Chlorides, isothiocyanates, acetates, and chloroacetates of copper(II), nickel(II), or cobalt(II) were used as starting salts. The prepared complexes were characterized by elemental analysis and FT IR. Structures of the four complexes were determined by single-crystal X-ray diffraction analysis.


1984 ◽  
Vol 37 (5) ◽  
pp. 921 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White

The crystal structures of the title compounds, [Ni(OH2)4(en)] [SO4].2H2O, (1), and [Ni(OH2)4(bpy)]- [SO4].2H2O, (2), have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by full matrix least-squares methods to residuals of 0.028,0.031 for 1852, 4323 independent 'observed' reflections respectively. Crystals of (1) are monoclinic, C2/c, a 9.459(4), b 12.192(7), c 12.294(3) �, β 119.84(4)�, Z 4. In the cation, Ni-N is 2.061(2) �; Ni-O (trans to O, N respectively) are 2.106(2), 2.063(2) �. Instead of being enlarged above 90� as predicted from repulsion theory, the angle between the pair of oxygen atoms trans to nitrogen is diminished, being 87 14(7)�. Crystals of (2) are triclinic, P1, a 11.476(5), b 9.351(5), c 7.793(4) �, α 77.63(4), β 83.52(3), γ87.40(4)�, Z 2. In the cation, Ni-N are both 2.063(2) �. Ni-O (trans to N, O respectively) are 2.060(2), 2.O42(2); 2.O80(2), 2�. The short Ni-O distance [2.042(2)�] is associated with the coordination of a trigonal water molecule.


Crystals ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 364 ◽  
Author(s):  
Mariia V. Kniazeva ◽  
Alexander S. Ovsyannikov ◽  
Daut R. Islamov ◽  
Aida I. Samigullina ◽  
Aidar T. Gubaidullin ◽  
...  

A combination of tetrasulfonylcalix[4]arene (3-4H) together with a calix[4]arene dicarboxylate derivative 2-4H led, in the presence of MII(NO3)2 (M = Co, Ni, Zn), to the formation of three novel isostructural metallomacrocycles of formula [M3(DMF)2(μ3-H2O)-(2-2H)-3]. The structure of the prepared coordination compounds was studied in the solid state using single crystal/powder X-ray diffraction studies. The X-ray diffraction on single crystal revealed that the structure of the obtained supramolecular complexes is composed of a trinuclear metallic cluster [M3]+6 held between one di-deprotonated molecule of (2-2H)2− offering two carboxylate groups for binding metal cations and one tetra-deprotonated compound 34−, where four oxygen atoms, belonging to four deprotonated phenolic moieties and three oxygen atoms coming from three SO2 groups, are coordinated with the cluster core. Thus, an example of an easily reproducible molecular recognition pattern involving two different types of calix[4]arene based ligands, displaying different coordination moieties, and trinuclear metallic clusters, is reported here. In addition, it has been shown that the cone moieties of the calixarene also encapsulate solvent molecules.


1983 ◽  
Vol 38 (12) ◽  
pp. 1615-1621 ◽  
Author(s):  
Annegret Lipka

2,2′-Bipyridinium pentachloroantimonate (III) and the metastable modification of 4,4′-bipyridinium pentachloroantimonate(III) were synthezised and investigated by single crystal X-ray diffraction analysis. The structures consist of 2,2′-bipyridinium and 4,4′-bipyridinium cations, respectively, and of pentachloroantimonate anions. With regard to bonding and short intermolecular contacts the coordination of the Sb atoms is distorted octahedral in both structures. Bond lengths of equivalent Sb-Cl bonds differ strongly within the structure of the 2,2′-bipyridinium salt (239.9 pm to 312.1 pm) and are not distinguishable from short intermolecular contacts (305.4 pm and 321.8 pm). In the structure of the 4,4′-bipyridinium salt, bond distances vary only from 240.9 pm to 267.8 pm and are clearly below intermolecular contacts at 318.2 pm. In spite of the different distances the total bond order for each Sb atom is 3. In the structure of the 2,2′-bipyridinium salt the anions build tetramers, whereas in the structure of the 4,4′-bipyridinium salt the anions form chains


2003 ◽  
Vol 2003 (7) ◽  
pp. 445-447
Author(s):  
Qing-Xiang Liu ◽  
Hai-Bin Song ◽  
Feng-Bo Xu ◽  
Qing-Shan Li ◽  
Xian-Shun Zeng ◽  
...  

The 9-methylanthracene photodimer (6) and lepidopterene (7) were prepared by a photo-dimerisation reaction of 1-(9-anthracenylmethyl)-3-ethylimidazolium iodide (1) or α, α'-di[1-(9-anthracenylmethyl) imidazolium]- p-xylene dibromide (2). Compound 6 is derived from the head-tail [4+4] cycloaddition of two molecular 9-methylanthracenes, and the butterfly-shaped compound 7 is formed via the 9-methyleneanthracene radical in a two steps precess. The single crystal structure of 6 was determined by X-ray diffraction analysis. The changes of luminescent intensities of compounds 1, 2 and 7 are reported.


1994 ◽  
Vol 49 (9) ◽  
pp. 1267-1271 ◽  
Author(s):  
A. Franken ◽  
W. Preetz

By reaction of [B6H6]2- with N-(chloromethyl)phthalimide in dichloromethane the intermediate phthalimidomethylhexahydro-closo-hexaborate(1-), [B6H6(CH2(NC8O2H4)]-, is formed which with an excess of hydrazine reacts to give am inomethylhexahydro-closo-hexaborate(1-). The crystal structures of Cs[Bf,H6(CH2NH2)] and K[B6H6(CH2NH2)] have been determined by single crystal X -ray diffraction analysis. They are monoclinic, space group C2/m with a = 11.123(6), b = 6.8441(11), c = 12.810(7) Å, β = 124.032(5)° for Cs[B6H6(CH2NH2)] and with a = 10.767(2), b = 6.6255(6), c = 12.2648(14) Å, β = 123.880(10")° for K [B6H6(CH2NH2)]. The 11B NMR spectrum is consistent with a monohetero substituted octahedral B6 cage with local C4v symmetry. In the 13C NMR spectrum of Cs[B6H6(CH2NH2)] a quartet at 32.7 ppm with 1J(C,B) 65 Hz is observed. The IR and Ram an spectra exhibit characteristic CH, NH, BH and B6 vibrations


2019 ◽  
Vol 75 (7) ◽  
pp. 1041-1045
Author(s):  
Lotfi Rghioui ◽  
Lahcen El Ammari ◽  
Abderrazzak Assani ◽  
Mohamed Saadi

The crystal structures of dirubidium potassium dysprosium bis(vanadate), Rb2KDy(VO4)2, and caesium potassium gadolinium bis(vanadate), Cs1.52K1.48Gd(VO4)2, were solved from single-crystal X-ray diffraction data. Both compounds, synthesized by the reactive flux method, crystallize in the space group P\overline{3}m1 with the glaserite structure type. VO4 tetrahedra are linked to DyO6 or GdO6 octahedra by common vertices to form sheets stacking along the c axis. The large twelve-coordinate Cs+ or Rb+ cations are sandwiched between these layers in tunnels along the a and b axes, while the K+ cations, surrounded by ten oxygen atoms, are localized in cavities.


2017 ◽  
Vol 23 (4) ◽  
Author(s):  
Ren-Yin Yang ◽  
Jing Sun ◽  
Ju Xie ◽  
Chao-Guo Yan

AbstractTriethylamine-promoted domino cyclodimerization reaction of 3-phenacylideneoxindolines with amino ester hydrochlorides in acetonitrile afforded substituted dispiro[indoline-3,1′-cyclopentane-3′,3″-indolines] in good yields. The relative configuration of the major diastereoisomers was determined by the X-ray diffraction analysis of three single crystal structures.


Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(


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