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Журнал структурной химии  / №1 2015

CRYSTAL STRUCTURE OF BIS[ 1-{(3,5-DIMETHYL-1H-PYRAZOL-1-YL)METHYL}-3,5-DIMETHYL- 1H-PYRAZOL-2-IUM] HEXACHLOROURANATE(IV): [H2C(3,5-Me2pz)(3,5-Me2pzH)]2[UCl6] (300,00 руб.)

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Первый авторCarretas
АвторыCui J., Cruz A., Santos I.C., Marçalo J.
Страниц4
ID359577
АннотацияThe X-ray diffraction study of a single crystal with the composition [H2C(3,5-Me2pz)(3,5Me2pzH)]2[UCl6] (1) is performed. This compound is the product of an attempted synthesis of a bis(pyrazolyl)methane complex of uranium(IV) obtained by the reaction of UCl4 with bis(3,5-dimethylpyrazol-1-yl)methane in THF. 1 crystallizes in the space group P-1 of the triclinic system: a = 9.6616(2) Å, b = 9.6946(2) Å, c = 10.7314(2) Å, D = 107.6210(10)q, E = = 115.5600(10)q, J = 99.6710(10)q, V = 810.45(3) Å3, Z = 1, dcalc = 1.765 g/cm3, P = 5.528 mm–1+, R1 = 0.0249. The structural unit consists of two separated [H2C(3,5-Me2pz)(3,5-Me2pzH)] cations and a UCl62 anion. In the solid state structure of 1 several short intermolecular N—HѱN and C—HѱCl contacts are identified suggesting the presence of hydrogen bonds.
УДК548.73:547.13:546.791
CRYSTAL STRUCTURE OF BIS[ 1-{(3,5-DIMETHYL-1H-PYRAZOL-1-YL)METHYL}-3,5-DIMETHYL- 1H-PYRAZOL-2-IUM] HEXACHLOROURANATE(IV): [H2C(3,5-Me2pz)(3,5-Me2pzH)]2[UCl6] / J.M. Carretas [и др.] // Журнал структурной химии .— 2015 .— №1 .— С. 189-192 .— URL: https://rucont.ru/efd/359577 (дата обращения: 25.09.2021)

Предпросмотр (выдержки из произведения)

In the solid state structure of 1 several short intermolecular N—H N and C—H Cl contacts are identified suggesting the presence of hydrogen bonds. <...> The anionic tris(pyrazolyl)borate (Tp) ligands have been used with success as supporting ligands in the molecular chemistry of the f-block elements, actinides in particular [ 1—7]. <...> These ligands provide an efficient protection of the metallic center and the possibility of tuning the steric and electronic properties of the complexes through the introduction of substituents in the pyrazolyl groups. <...> As a part of our research in this area we decided to study bis(3,5-dimethylpyrazol-1-yl)methane (Bpm*) complexes of uranium, and here we report the crystal structure of [H2C(3,5-Me2pz)(3,5Me2pzH)]2[UCl6] complex (1). <...> The addition of a Bpm* solution [ 11 ] (109 mg, 0.5 mmol) in THF to a UCl4 solution [ 12 ] (200 mg, 0.5 mmol) in the same solvent at room temperature resulted after stirring overnight in a green suspension. <...> After centrifugation and removal of the solvent under vacuum the solid was washed with n-hexane and dried until dryness to give a green solid. <...> Diffraction quality crystals were obtained from a THF/n-hexane solution at –5 C. Crystals of 1 suitable for the X-ray diffraction study were mounted on a loop with protective oil. <...> X-ray data were collected at 150 K on a Bruker APEX II CCD diffractometer using graphite monochromated MoKh radiation (y = 0.71069 Е) at 50 kV and 30 mA. <...> All hydrogen atoms were inserted in idealized positions and allowed to refine riding on the parent carbon atom. <...> The reaction of bis(3,5-dimethylpyrazol-1-yl)methane with UCl4 in THF was studied and led to a product which could not be fully characterized. <...> Nevertheless, green single crystals suitable for X-ray crystallographic studies were obtained from a THF/hexane solution at –5 C. Attempts to synthesize a bis(pyrazolyl)methane complex of uranium(IV) proved to be unsuccessful and resulted in [H2C(3,5-Me2pz)(3,5-Me2pzH)]2[UCl6] complex (1). <...> The [H2C(3,5-Me2pz)(3,5-Me2pzH)]2[UCl6] compound crystallises in the triclinic system, space group P-1, with the asymmetric unit comprising one independent [H2C(3,5-Me2pz) (3,5-Me2pzH)]+ cation located in a general position and a half of the [UCl6 <...>