Journal of Structural Chemistry p. 1790 - 1798 (2019)
Update date:2022-08-28
Topics:
Khranenko
Sukhikh
Komarov, V. Yu.
Gromilov
The crystal structure of [CuEn3]WO4 (En is ethylenediamine) is studied in the temperature range 100–390 K. Crystallographic data at 100 K are: a = 27.6903(8) ?, c = 9.9405(3) ?, space group P3?, V = 6600.8(4) ?3, Z = 18. Copper atomic coordination is a distorted square bipyramid. Four short Cu–N distances are within 2.038(5)–2.110(6) ?; two long distances are within 2.374(8)–2.514(7) ?. The lengths of N–H…O interionic contacts lie within 1.96–2.17 ?. A temperature elevation makes the Cu–N distances equal: at 298 K they are within 2.066(2)–2.256(3) ?(a = 16.0391(8) ?, c = 9.9608(6) ?, space group P3?c1, V = 2219.1(3) ?3, Z = 6), and at 390 K they are 2.151(6) ?(a = 9.2986(10) ?, c = 10.0520(14) ?, P3?1c, V = 752.7(2) ?3, Z = 2). In the range from 100 K to 390 K the average W–O distances decrease from 1.776 ? to 1.734 ?. Hirshfeld surfaces of complex cations are analyzed. It is shown that with increasing temperature the number of interionic N–H…O contacts decreases. The [CuEn3]WO4 phase is found to be unstable and on storing in air it transforms into [CuEn2](WO4)·2H2O.
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