Research output: Contribution to journal › Article › peer-review
[NiEn3]MoO4 : Features of the Phase Transition and Thermal Decomposition in the Presence of Lithium Hydride. / Sukhikh, A. S.; Khranenko, S. P.; Komarov, V. Yu et al.
In: Journal of Structural Chemistry, Vol. 60, No. 5, 01.05.2019, p. 780-788.Research output: Contribution to journal › Article › peer-review
}
TY - JOUR
T1 - [NiEn3]MoO4
T2 - Features of the Phase Transition and Thermal Decomposition in the Presence of Lithium Hydride
AU - Sukhikh, A. S.
AU - Khranenko, S. P.
AU - Komarov, V. Yu
AU - Pishchur, D. P.
AU - Nikolaev, R. E.
AU - Buneeva, P. S.
AU - Plyusnin’, P. E.
AU - Gromilov, S. A.
N1 - Publisher Copyright: © 2019, Pleiades Publishing, Ltd.
PY - 2019/5/1
Y1 - 2019/5/1
N2 - The crystal structural characteristics of the [NiEn3]MoO4 complex salt (En is ethylenediamine) at 90 K are as follows: space group P3¯,a=15.9307(9)Å´,c=9.9238(6)Å´,V=2181.1(3)Å´3,Z=6,dx=1.822g/cm3, Ni-N is 2.1182(12)−2.1498(11)Å´, ∠Ni-N-N is 80.76(4)-82.27(4)°. According to the differential scanning calorimetry data in a range from 295 K to 310 K, there is a thermal anomaly with peaks at T1 = 299.6 K and T2 = 304.7 K. The crystal structural characteristics at 320 K are as follows: space group P3¯1c,a=9.2491(4)Å´,c=9.9713(4)Å´,V=738.72(7)Å´3,Z=2,dx=1.794g/cm3, Ni-N is 2.1302 (14) Å´, ∠N-Ni-N is 80.96(8)°. With increasing temperature from 90 K to 320 K a decrease in the average Mo-O distance from 1.769 Å´ to 1.725 Å´ is observed in the structure. The comparative analysis of the interionic N-H…O and C-H…O contacts is carried out. The ex situ powder X-ray diffraction study of the formation process of metal and carbide phases by the [NiEn3]MoO4 thermal decomposition in the presence of LiH in the He atmosphere is performed. At the temperature of 1323 K a Mo2C and MoNi4 phase mixture forms in the first minute. With increasing keeping time the Ni2Mo4Cx phase forms.
AB - The crystal structural characteristics of the [NiEn3]MoO4 complex salt (En is ethylenediamine) at 90 K are as follows: space group P3¯,a=15.9307(9)Å´,c=9.9238(6)Å´,V=2181.1(3)Å´3,Z=6,dx=1.822g/cm3, Ni-N is 2.1182(12)−2.1498(11)Å´, ∠Ni-N-N is 80.76(4)-82.27(4)°. According to the differential scanning calorimetry data in a range from 295 K to 310 K, there is a thermal anomaly with peaks at T1 = 299.6 K and T2 = 304.7 K. The crystal structural characteristics at 320 K are as follows: space group P3¯1c,a=9.2491(4)Å´,c=9.9713(4)Å´,V=738.72(7)Å´3,Z=2,dx=1.794g/cm3, Ni-N is 2.1302 (14) Å´, ∠N-Ni-N is 80.96(8)°. With increasing temperature from 90 K to 320 K a decrease in the average Mo-O distance from 1.769 Å´ to 1.725 Å´ is observed in the structure. The comparative analysis of the interionic N-H…O and C-H…O contacts is carried out. The ex situ powder X-ray diffraction study of the formation process of metal and carbide phases by the [NiEn3]MoO4 thermal decomposition in the presence of LiH in the He atmosphere is performed. At the temperature of 1323 K a Mo2C and MoNi4 phase mixture forms in the first minute. With increasing keeping time the Ni2Mo4Cx phase forms.
KW - complex salt
KW - crystal chemistry
KW - differential scanning calorimetry
KW - molybdate anion
KW - thermal decomposition
KW - tris(ethylenediamine)nickel
KW - X-ray diffraction analysis
KW - EXPANSION
KW - GROWTH
KW - CRYSTAL-STRUCTURES
UR - http://www.scopus.com/inward/record.url?scp=85067342178&partnerID=8YFLogxK
U2 - 10.1134/S002247661905010X
DO - 10.1134/S002247661905010X
M3 - Article
AN - SCOPUS:85067342178
VL - 60
SP - 780
EP - 788
JO - Journal of Structural Chemistry
JF - Journal of Structural Chemistry
SN - 0022-4766
IS - 5
ER -
ID: 20587448