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2015

Number: 4

19411.
IONIC MOBILITY AND PHASE TRANSITION IN HEPTAFLUORODIANTIMONATE(III) Cs0.4Rb0.6Sb2F7

V. Ya. Kavun1, M. M. Polyantsev1, L. A. Zemnukhova1,2
1Institute of Chemistry, Far Eastern Branch, Russian Academy of Sciences, Vladivostok, Russia
2Far Eastern Federal University, Vladivostok, Russia
Keywords: гептафтородиантимонаты(III) цезия, рубидия, ионная подвижность, фазовый переход, ионная проводимость, спектры ЯМР 19F, ДСК, cesium-rubidium heptafluorodiantimonates(III), ionic mobility, phase transition, ionic conductivity, 19F NMR spectra, DSC

Abstract >>
The ionic mobility and conductivity in the crystalline phase of Cs0.4Rb0.6Sb2F7 (I) is studied using 19F NMR, DSC, and impedance spectroscopy methods. The analysis of the 19F NMR spectra makes it possible to follow the character of ion motions in the fluoride sublattice in the temperature range of 150−470 K, and to determine the types and temperature ranges of these motions. It is found that diffusion of fluorine ions becomes the dominant type of ion motions in the modification formed as a result of the reversible phase transition ( T = 415 K, the DSC data) in compound I. According to the preliminary results of electrophysical studies, the ionic conductivity in this compound is ~10-3 S/cm at temperatures above 450 K.



Number: 4

19412.
CRYSTAL STRUCTURE OF Cs2[Mo10S10O10(OH)10(H2O)4](C4H2S(PO2H)2)·21H2O

D. S. Ogienko1, A. I. Smolentsev1,2, S. N. Konchenko1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: полиядерные комплексы, молибден, сера, фосфор, гетероциклические соединения, супрамолекулярные соединения, кристаллическая структура, polynuclear complexes, molybdenum, sulfur, phosphorus, heterocyclic compounds, supramolecular compounds, crystal structure

Abstract >>
We have determined the crystal structure of a supramolecular compound Cs2[Mo10S10O10(OH)10(H2O)4](C4H2S(PO2H)2)×21H2O comprising quasi-one-dimensional chains consisting of alternating cyclical [Mo10S10O10(OH)10(H2O)4] clusters and C4H2S(PO2H2)2 acid residuals of thiophene-2,5-diphosphonic acid hydrogen bonded with each other.



Number: 4

19413.
CRYSTAL STRUCTURE OF THE SEVEN-ELECTRON MOLYBDENUM CLUSTER [MO3S4(DPPE)3CL3]·3.5C4H8O2·0.5ET2O

P. A. Petrov1,2, G. A. Sosnin2, D. Yu. Naumov1, S. N. Konchenko1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: кластерные комплексы, молибден, сера, рентгеноструктурный анализ, cluster complexes, molybdenum, sulfur, single crystal X-ray diffraction study

Abstract >>
The seven-electron neutral cluster complex [Mo3S4(dppe)3Cl3] (dppe = Ph2PCH2CH2PPh2) is obtained by the reduction of the [Mo3S4(dppe)3Cl3]Cl cluster with gallium metal. The molecular and crystal structure of [Mo3S4(dppe)3Cl3]×3.5C4H8O2×0.5Et2O solvate is determined by single crystal XRD. The crystallographic data are as follows: monoclinic crystal symmetry, space group C2/c, a = 41.1775(16) Å, b = 17.7178(7) Å, c = 28.9609(9) Å, β = 110.363(1)°, V = 19808.7(13) Å3, Z = 8, dcalc = 1.384 g/cm3.



Number: 4

19414.
CRYSTAL STRUCTURE OF [PbCo(NO2)3(μ−OH)2]2

S. P. Khranenko1, N. V. Kuratieva1,2, A. V. Zadesenets1,2, S. A. Gromilov1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: свинец, кобальт, рентгеноструктурный анализ, кристаллохимия, твердый раствор, сплав, lead, cobalt, single crystal X-ray diffraction study, crystal chemistry, solid solution, alloy

Abstract >>
The structure of [PbCo(NO2)3(μ-OH)2]2 is determined by single crystal X-ray diffraction. The geometric characteristics are analyzed and the packing motif is determined.



Number: 4

19415.
NEW TRINUCLEAR μ3−VINYLIDENE CLUSTER CpReFePt(μ3−C=CHPh)(CO)5[P(OPri)3]2

V. V. Verpekin1, O. S. Chudin1, D. A. Piryazev2,3, A. I. Rubaylo1,4,5, S. A. Gromilov2,3, O. V. Semeikin6
1Institute of Chemistry and Chemical Technology, Siberian Branch, Russian Academy of Sciences, Krasnoyarsk, Russia
2Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
3Novosibirsk National Research State University, Novosibirsk, Russia
4Krasnoyarsk Scientific Center, Siberian Branch, Russian Academy of Sciences, Krasnoyarsk, Russia
5Siberian Federal University, Krasnoyarsk, Russia
6Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, Russia
Keywords: рений, железо, платина, винилиденовые комплексы, гетерометаллические комплексы, кластеры, рентгеноструктурный анали, rhenium, iron, platinum, vinylidene complexes, heterometallic complexes, clusters, single crystal X-ray diffraction study

Abstract >>
The X-ray diffraction study of a new heterometallic cluster CpReFePt(μ3-C=CHPh)(CO)5[P(OPri)3]2 is performed. The crystallographic characteristics are as follows: a = 11.0275(4) Å, b = 33.0367(12) Å, c = 12.2691(5) Å, β = 98.3660(10)°, V = 4422.2(3) Å3, space group P21/n , Z = 4, dcalc = 1.744 g/cm3. The cluster contains the phenylvinylidene ligand coordinated with a trimetallic core in the form of a Re-Fe-Pt chain (the Re-Fe and Fe-Pt bond lengths are 2.794(7) Å and 2.628(1) Å respectively; the Re∙∙∙Pt distance is 3.354(1) Å).



Number: 4

19416.
CRYSTAL STRUCTURE OF A 3D Ag(I) COORDINATION POLYMER BASED ON FLEXIBLE BIS(BENZIMIDAZOLE) AND 5−NITROISOPHTHALIC ACID CO−LIGANDS

X. Zhang, L. Liu, L. Qin, G.H. Cui
Hebei United University, Tangshan, Hebei Province, P. R. China
Keywords: Ag(I) complex, 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane, crystal structure

Abstract >>
A new coordination polymer {[Ag4(L)3(nip)2](H2O)}n(L = 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane, H2nip = 5-nitroisophthalic acid) is hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The complex features a 3D sqc117 supramolecular framework based on unique tetranuclear Ag(I) clusters which involve the ligand-supported Ag-Ag interactions.



Number: 4

19417.
CRYSTAL STRUCTURE AND LUMINESCENT PROPERTIES OF A ONE-DIMENSIONAL Cd(II) COORDINATION POLYMER CONSTRUCTED BY 4,4'-DI-TERT-BUTYL-2,2'-BIPYRIDINE AND 5-TERT-BUTYL ISOPHTHALIC ACID

X.J. Xu, J. Wang
Yancheng Teachers University, Yancheng, Jiangsu, P.R. China
Keywords: Cd(II) complex, 4,4'-di-tert-butyl-2,2'-bipyridine, 5-tert-butyl isophthalic acid, crystal structure, luminescence

Abstract >>
A one-dimensional Cd(II) complex [Cd(Bu<sub>2</sub>bpy)(tbip)×H<sub>2</sub>O]<sub>n</sub> (1) (Bu<sub>2</sub>bpy = 4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine, H<sub>2</sub>tbip = 5-<i>tert</i>-butyl isophthalic acid) is synthesized and characterized using single crystal X-ray diffraction, IR spectroscopy, and elemental analysis. The single crystal X-ray diffraction analysis reveals that complex 1 is a one-dimensional double chain polymer based on {Cd<sub>2</sub>(OCO)<sub>2</sub>} dimeric kernels with a Cd⋯Cd separation of 4.3197(7) Å. The thermal stability and luminescent properties of the title complex are briefly investigated.



Number: 4

19418.
CRYSTAL AND MOLECULAR STRUCTURE OF [Au(C14H22N4)]ReO4

V. A. Afanasieva1, L. A. Glinskaya1, D. A. Piryazev1,2, S. A. Gromilov1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: золото, рений, тетраазамакроцикл, комплексная соль, рентгеноструктурный анализ, рентгенофазовый анализ, кристаллохимия, термолиз, gold, rhenium, tetraazamacrocycle, complex salt, single crystal X-ray diffraction study, powder X-ray diffraction, crystal chemistry, thermolysis

Abstract >>
Perrhenate of the tetraazamacrocyclic complex of gold(III) [Au(C14H22N4)]ReO4 is synthesized. The crystal structure of the compound is determined by single crystal X-ray diffraction. The crystallographic data are as follows: а = 7.733(2) Å, b = 11.368(2) Å, c = 11.685(2) Å, α = 116.23°, β = 104.26°, γ = 94.96°; V = 870.3(3) Å3, space group P(-1), Z = 2, dcalc = 2.647 g/cm3, R = 0.0245. The packing of the complex is comprised of double stacks of cations and chains of anions linked into two-dimensional layers due to weak intermolecular interactions (non-classical hydrogen bonds C-H…O, C-H…Au, C-H…p and the Au…Au contacts). The thermal decomposition of the obtained compound in the hydrogen atmosphere is studied. According to the powder X-ray diffraction data, the product of the reduction of the synthesized salt is a mixture of nanocrystalline phases of Re and Au with the coherent-scattering regions of 17 nm and 13 nm respectively.



Number: 4

19419.
IODOBISMUTHATE COMPLEX (Bu4N)3[Bi3I12]: CRYSTAL STRUCTURE OF A NEW POLYMORPH

S. A. Adonin1,2, E. V. Peresypkina1,2, M. N. Sokolov1,2, V. P. Fedin1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: висмут, иодидные комплексы, полиморфизм, кристаллическая структура, bismuth, iodide complexes, polymorphism, crystal structure

Abstract >>
The structure of a new polymorph of the trinuclear iodobismuthate complex TBA3[Bi3I12] (TBA = tetra-n-butylammonium) (1) synthesized by the reaction of BiI3+TBA-I in the presence of silver triflate is identified.



Number: 4

19420.
CRYSTAL STRUCTURE OF S,S'-DIMETHYL-N-NITROIMIDODITHIOCARBONATE

A. M. Astachov1, A. D. Vasiliev2, D. V. Antishin1, E. S. Buka1
1Siberian State Technological University, Krasnoyarsk, Russia
2Kirensky Institute of Physics, Siberian Branch, Russian Academy of Sciences, Krasnoyarsk, Russia
Keywords: нитримины, производные нитрогуанидина, рентгеноструктурный анализ, строение молекул, nitrimines, nitroguanidine derivatives, single crystal X-ray analysis, molecular structure

Abstract >>
The molecule of S,S'-dimethyl-N-nitroimidodithiocarbonate has a planar geometry (with the exception of hydrogen atoms of methyl groups), stabilized by the shortened S…O contact. The bond lengths in the >С=N-NO2 nitrimine moiety, in contrast to nitroguanidine derivatives, make it possible to consider the molecular structure of the compound within the traditional valence formula. The crystal structural feature of the compound is a low energy of its crystal lattice.




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