17 research outputs found
Strontium tetrafluoroborate. Erratum
Erratum to Acta Cryst. (2007), C63, i75–i76
Unknown <i>cis</i>-[(DMSO)<sub>2</sub>ClCu<sup>II</sup>(μ-Cl)<sub>2</sub>Cu<sup>II</sup>Cl(DMSO)<sub>2</sub>] isomer obtained via new [Cu<sub>4</sub>Cl<sub>8</sub>(DMSO)<sub>8</sub>(hmta)] template complex
<p>A missed <i>cis</i> isomeric form of a well-known <i>trans</i>-[CuCl<sub>2</sub>(DMSO)<sub>2</sub>]<sub>n</sub> complex has been prepared via the tetranuclear [Cu<sub>4</sub>Cl<sub>8</sub>(DMSO)<sub>8</sub>(<b>hmta</b>)] complex. Structurally, both complexes were found to be molecular i.e. [Cu<sub>4</sub>Cl<sub>8</sub>(DMSO)<sub>8</sub>(<b>hmta</b>)] consists of isolated tetracoordinated hexamethylenetetramine molecules, whereas the <i>cis</i>-complex consists of isolated [(DMSO)<sub>2</sub>ClCu<sup>II</sup>(μ-Cl)<sub>2</sub>Cu<sup>II</sup>Cl(DMSO)<sub>2</sub>] clusters. It should also be noted that the <i>cis</i>-configuration of DMSO molecules in [(DMSO)<sub>2</sub>ClCu<sup>II</sup>(μ-Cl)<sub>2</sub>Cu<sup>II</sup>Cl(DMSO)<sub>2</sub>] was directly transferred from that of [Cu<sub>4</sub>Cl<sub>8</sub>(DMSO)<sub>8</sub>(<b>hmta</b>)], while the <i>trans</i>-[CuCl<sub>2</sub>(DMSO)<sub>2</sub>]<sub>n</sub> isomer was always formed as a final stable product.</p
Low-temperature modification of Ba(BF4)2(H2O)3
The crystal structure of the low-temperature modification of Ba(BF4)2(H2O)3, barium bis(tetrafluoridoborate) trihydrate, was determined at 150 K. In contrast to the room-temperature modification, which crystallizes in the space group C2221 [a = 7.1763 (6), b = 18.052 (2), c = 7.1631 (6) Å, V = 927.93 (15) Å3 at 300 K, Z = 4; Charkin et al. (2023). J. Struct. Chem. 64, 253–261], the low-temperature phase is monoclinic, space group P21 [a = 7.0550 (4), b = 7.1706 (3), c = 9.4182 (6) Å, β = 109.295 (7)o, V = 449.68 (5) Å3, Z = 2]. The structure of the low-temperature modification of Ba(BF4)2(H2O)3 features O—H...F and O—H...O hydrogen bonding between water molecules and BF4− anions. One of the coordinating water molecules in the low-temperature modification is disordered over two sets of sites
Copper(I) bromide and chloride complexes with urotropine and triethylenediamine: synthesis, crystal structure, and Raman characterization<sup>*</sup>
<p>In the present study, the oxidative dissolution of metallic copper has been explored with the intention to prepare some new complexes with urotropine (<i>hmta</i>) and triethylenediamine (<i>dabco</i>) ligands. All the compounds synthesized were characterized by single-crystal X-ray diffraction and Raman spectroscopy<i>.</i> Reactions performed in a DMSO/CuCl<sub>2</sub>∙2H<sub>2</sub>O mixture resulted in [(μ-Cl)<sub>2</sub>Cu<sup>I</sup>(<i>hdabco</i><sup>+</sup>)Cu<sup>I</sup>(μ-Cl)(κ<i>S</i>-DMSO)]<sub>n</sub> and [Cu<sup>I</sup>Cl(<i>hmta</i>)<sub>2</sub>] complexes. Their isostructural bromide analogs [(μ-Br)<sub>2</sub>Cu<sup>I</sup>(<i>hdabco</i><sup>+</sup>)Cu<sup>I</sup>(μ-Br)(κ<i>S</i>-DMSO)]<sub>n</sub> and [Cu<sup>I</sup>Br(<i>hmta</i>)<sub>2</sub>] were prepared by the reaction of elemental copper with respective ligands in a DMSO/CBr<sub>4</sub> mixture. Early interrupted reaction of the copper wire with the DMSO/CBr<sub>4</sub>/<i>dabco</i> solution resulted in an appearance of crystals of the [Cu<sup>I</sup><sub>2</sub>Br<sub>2</sub>(CO)<sub>2</sub>(<i>dabco</i>)]<sub>n</sub> carbonyl complex on the copper surface. It arises with the participation of <i>in situ</i> formed carbon monoxide. Despite the identical stoichiometry, the crystal structure of the [Cu<sub>2</sub>Br<sub>2</sub>(CO)<sub>2</sub>(<i>dabco</i>)]<sub>n</sub> complex is markedly different from that of a known [Cu<sub>2</sub>Cl<sub>2</sub>(CO)<sub>2</sub>(<i>dabco</i>)]<sub>n</sub> analog.</p
Tetrahydrated bis(monoaqua-bis(ethylenediamine)copper(II))-diaqua-bis(ethylenediamine)copper(II) dicitrate
The crystals of the first copper(II) ethylenediamine complex containing citrate anion have been prepared and characterized. Despite the archetypical character of the copper(II) ethylenediamine complexes, some structural peculiarities were found to be interesting since they are quite rare even among the mentioned type of the complex compounds i.e. a presence of both mono and diaqua-bis(ethylenediamine)copper(II) cations together in the same crystal structure, intramolecular hydrogen bonding of the citric anion, cis,trans-configuration of the citric anion and the disordered C-C bond of the ethylenediamine molecule in the monoaquabis(ethylenediamine)copper(II) cation, which in fact is a co-existence of two energetically close dd and dk conformers. The Raman as well as FTIR spectra were recorded and discussed. Finally, the magnetic measurements have shown paramagnetic behavior of the prepared complex in a wide range of temperatures