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1.
Marzena Sokalska Ma?gorzata Prussakowska Marcin Hoffmann B?a?ej Gierczyk Rafa? Frański 《Journal of the American Society for Mass Spectrometry》2010,21(10):1789-1794
The following ions [UO2(NO3)3]−, [UO2(ClO4)3]−, [UO2(CH3COO)3]− were generated from respective salts (UO2(NO3)2, UO2(ClO4)3, UO2(CH3COO)2) by laser desorption/ionization (LDI). Collision induced dissociation of the ions has led, among others, to the
formation of UO4
− ion (m/z 302). The undertaken quantum mechanical calculations showed this ion is most likely to possess square planar geometry as
suggested by MP2 results or strongly deformed geometry in between tetrahedral and square planar as indicated by DFT results.
Interestingly, geometrical parameters and analysis of electron density suggest it is an UVI compound, in which oxygen atoms bear unpaired electron and negative charge. 相似文献
2.
A. A. Rybinskaya P. E. Plyusnin E. A. Bykova S. A. Gromilov Yu. V. Shubin S. V. Korenev 《Journal of Structural Chemistry》2012,53(3):527-533
Two new double complex salts [Pd(NH3)4]3[Rh(NO2)6]2 (I) and [Pd(NH3)4]3[Rh(NO2)6]2·H2O (II) are synthesized and characterized. The techniques to produce one-phase residues of the salts are developed. The crystallographic data for I: a = 18.915(2) ?, V = 6767.4 ?3, F-43c space group, Z = 8, d x = 2.548 g/cm3; II: a = 21.160(6) ?, b = 8.085(7) ?, c = 21.363(4) ?, β = 91.71(4)°, V = 3661.1(6) ?3, P21/c space group, d x = 2.357 g/cm3. Thermal properties of the obtained compounds in the hydrogen and helium atmosphere are studied. It is shown that the final product of their decomposition both in the inert and reducing atmosphere is a powder consisting of bimetallic nanosized particles (nanoalloy) of Pd0.59Rh0.41 (Fm-3m space group, a = 3.856(2) ?, crystallite size of 8–11 nm). 相似文献
3.
Nanthawat Wannarit Viwat Hahnvajanawong Chaveng Pakawatchai Sujittra Youngme 《Transition Metal Chemistry》2012,37(1):79-84
Two multiple-layer heterometallic MnII–AgI coordination polymers, {MnII(ampyz)(H2O)[Ag2I(CN)3][AgI(CN)2]·ampyz}
n
(1) and {[MnII(benzim)2[AgI(CN)2]2][(benzim)AgI(CN)]·H2O}
n
(2) where ampyz = 2-aminopyrazine and benzim = benzimidazole, have been prepared and structurally characterized. Compound 1 reveals a multiple-layer two-dimensional network with strong hexanuclear argentophilic interactions leading to an infinite
three-dimensional framework. Compound 2 has an unprecedented double-layer two-dimensional squared grid-type network with (4,4) topology through AgI···AgI and π–π interactions between two adjacent squared layers. These double-layer networks of 2 are linked to others by π–π interactions, leading to a three-dimensional framework. 相似文献
4.
A. A. Rybinskaya E. A. Shusharina P. E. Plyusnin Yu. V. Shubin S. V. Korenev S. A. Gromilov 《Journal of Structural Chemistry》2011,52(4):816-819
A single crystal of [Pd(NH3)4]3[Ir(NO2)6]2·H2O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?3, P21/c space group, Z = 4, d
x = 2.714 g/cm3. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex
cations and crystallization water molecules are located between the mentioned layers. 相似文献
5.
I. V. Korol’kov S. A. Martynova K. V. Yusenko S. V. Korenev 《Russian Journal of Inorganic Chemistry》2010,55(9):1347-1351
Double complex salts [Ru(NH3)5Cl][OsCl6] and [Ru(NH3)5Cl]2[OsCl6]Cl2 were prepared and characterized. An X-ray diffraction study showed that [Ru(NH3)5Cl][OsCl6] is isostructural to the previously synthesized [Rh(NH3)5Cl][OsCl6]. The structure of [Ru(NH3)5Cl]2[OsCl6]Cl2 was solved by X-ray diffraction (a = 11.1849(8) ?, b = 7.9528(6) ?, c = 13.4122(9) ?; β = 99.765(2)°; V= 1175.75 ?3; space group C2/m; Z = 2). Thermolysis of the compounds under hydrogen and helium was studied. According to X-ray diffraction, nanosized metallic
powders of the corresponding alloys are formed as the final products of thermolysis. The compositions of the obtained solid
solutions are consistent with the phase diagram of the Ru-Os system. 相似文献
6.
K. V. Yusenko I. A. Baidina E. A. Shusharina S. A. Gromilov 《Journal of Structural Chemistry》2008,49(1):170-174
The [Ru(NH3)5Cl]2[Re6S8(CN)6]·3H2O salt was obtained; its crystal structure was analyzed: a = 10.7713(9) Å, b = 13.9602(11) Å, c = 14.7956(11) Å, α = 91.961(3)°, β = 109.985(3)°, γ = 110.030(3)°, V = 1935.3(3) Å3, space group P1ˉ, Z = 2, d
calc = 3.441 g/cm3. In the cluster anion, the Re-Re distances lie in the range from 2.594 Å to 2.612 Å. For two crystallographically independent
complex cations, Ru-Nav is 2.105 Å, and Ru-Clav 2.329 Å. A pseudohexagonal motif of the structure was found.
Original Russian Text Copyright ? 2008 by K. V. Yusenko, I. A. Baidina, E. A. Shusharina, and S. A. Gromilov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 1, pp. 178–181, January–February, 2008. 相似文献
7.
Crystal structure of a tetrahedral cluster complex [Zn2(NH3)6(μ-OH)][Zn(NH3)4]0.5[Re4Te4(CN)12]·5H2O
A cluster complex of the composition [Zn2(NH3)6(μ-OH)][Zn(NH3)4]0.5[Re4Te4(CN)12]·5H2O is obtained by the interaction of an aqueous solution of K4[Re4Te4(CN)12]·5H2O with an aqueous ammonia solution of ZnCl2. The compound crystallizes in the C2/m (12) monoclinic space group with unit cell parameters a = 23.233(2) ?, b = 14.5906(16) ?, c = 14.3825(15) ?, β = 125.169(1)°, V = 3985.5(7) ?3, Z = 4, d
x = 3.290 g/cm3. The structure is built from cluster [Re4Te4(CN)12]4− anions and complex [Zn2(NH3)6(μ-OH)]3+ and [Zn(NH3)4]2+ cations; the latter is disordered over two positions. 相似文献
8.
V. A. Nadolinny N. A. Nebogatikova P. E. Plyusnin S. V. Korenev 《Journal of Structural Chemistry》2009,50(5):915-918
In order to determine the features of the structure of double complex salts (DCSs) of [Cr(NH3)5Cl]×[MCl4]·nH2O, where M = Pd, Pt, n = 0, 1, the DCS solid solutions of palladium and platinum with isostructural DCSs containing the chloropentaammine rhodium
cation, [Cr(NH3)5Cl]
x
[Rh(NH3)5Cl]1−x
[MCl4]·nH2O, where x = 0.01–0.2, are synthesized and studied by the EPR method. DCSs with the isostructural chloropentaammine rhodium cation are
used as a diluter for magneto concentrated systems. It is shown that DCS of platinum and anhydrous DCS of palladium have the
identical environment of chromium ions. The EPR spectra of chromium ions for these compounds are described by the following
spin Hamiltonian parameters: S = 3/2, g
xx
= 1.987, g
yy
= 1.987, g
zz
= 1.985, D = 1660 Gs, E = 235 Gs. For the palladium complex containing crystalline water, the EPR spectra of chromium ions are described by the parameters:
S = 3/2, g
xx
= 1.984, g
yy
= 1.984, g
zz
= 1.984, D = 1060 Gs, E = 350 Gs. A decrease in the crystal field parameters for the aqueous palladium complex is caused by a redistribution of the
electron density to the oxygen atom in the second sphere of the chromium ion environment. 相似文献
9.
S. A. Adonin A. V. Virovets M. N. Sokolov V. P. Fedin 《Russian Journal of Coordination Chemistry》2010,36(10):734-738
New cluster complexes [W3S4(Acac)3(PPh3)3]PF6 · 0.5CHCl3 (Acac = CH3C(O)CHC(O)CH3) (I) and [W3S4(Hfac)3(PPh3)2Br] · 2CHCl3 (Hfac = CF3C(O)CHC(O)CF3) (II) were synthesized. Their molecular and crystal structures were determined by X-ray diffraction. The cis-cis type of coordination of acetylacetonate and hexafluoroacetylacetonate ligands in I and II, respectively, was established, and the PPh3 ligands were found in the trans-positions with respect to the “capping” sulfide ligand (μ3-S). 相似文献
10.
I. V. Kalinina D. G. Samsonenko Z. A. Starikova A. A. Korlyukov J. Lipkowski V. P. Fedin M. Yu. Antipin 《Journal of Structural Chemistry》2005,46(1):137-146
[Ni(dien)2]3[W4S4(CN)12]·20H2O and [Cu(dien)(Hdien)]2[W4S4(CN)12]·8H2O were obtained by evaporating water-ammonia solutions containing K6[W4S4(CN)12]·2H2O·2CH3OH, diethylene triamine, and NiCl2·6H2O or CuCl2·6H2O. The crystals of the complex compounds were obtained within 3 days. The complex compounds were characterized by IR spectroscopy
and by XRD and elemental analysis. XRD data for the complex [Ni(dien)2]3[W4S4(CN)12]·20H2O are: triclinic system,
, a = 14.671(2) Å, b = 16.448(3) Å, c = 19.814(3) Å, α = 67.841(3)°, β = 68.996(3)°, γ = 67.527(3)°, V = 3961.6(11) Å3, Z = 2; for the complex [Cu(dien)(Hdien)]2[W4S4(CN)12]·8H2O: monoclinic system, C2/c, a = 37.4290(1) Å, b = 17.7370(1) Å, c = 25.7370(2) Å, β = 105.3840(2)°, V = 16474.02(16) Å3, Z = 12.
Original Russian Text Copyright ? 2005 by I. V. Kalinina, D. G. Samsonenko, Z. A. Starikova, A. A. Korlyukov, J. Lipkowski,
V. P. Fedin, and M. Yu. Antipin
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 1, pp. 139–148, January–February, 2005. 相似文献
11.
Charles E. Ellul 《Journal of organometallic chemistry》2010,695(1):6-2376
The reduction of trans-[Pd(NHC)2Cl2] (NHC = IMes, 1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene; IiPr2 = 1,3-bis-isopropylimidazol-2-ylidene) with potassium graphite under an atmosphere of CO affords the palladium NHC carbonyl clusters [Pd3(μ-CO)3(NHC)3] (NHC = IMes, 1; IiPr2, 3). Treatment of 1 with SO2 at room temperature yields the bridging SO2 complex [Pd3(μ-SO2)3(IMes)3] (4) in quantitative yield. Complexes 1, 3 and 4 have been structurally characterised by X-ray crystallography. 相似文献
12.
The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354. 相似文献
13.
The crystal of [Ni(dien)2]2[Mn(NCS)6]·H2O was synthesized and the structure of its single crystal was determined by X-ray diffraction. The crystal is monoclinic system, space group P21/c with a=16.544(3),b=15.137(2), c=17.334(3)?, β=99.90(1)°, V=4276.3(12)?3, Z=4, Dc=1.479g·cm-3, Mr=951.55, F(000)=1998, μ=1.489mm-1, R=0.0399, Rw=0.0958. IR was also determined. 相似文献
14.
15.
Oxo/hydoxo zirconium(IV) complex of the general formula [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 has been isolated, when Zr(OiPr)4 reacted with a 2-fold excess of 3,3-dimethylbutyric acid. Single crystal X-ray diffraction data, collected at 103 and 153 K, showed that the studied compound crystallizes in hexagonal system (P63/m (no. 176)). Structure consists of dimers composed of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9] sub-units, linked by six μ2-OH bridges. Infrared spectroscopic studies proved the presence of hydroxo groups in the structure of studied clusters and formation of different types of oxo/hydroxo bridges. The application of variable temperature infrared spectroscopy and differential scanning calorimetry revealed that the structure of this complex undergoes the phase transitions at 143–183 and 203–293 K. Comparison of spectral and crystallographic data suggests that these phase transitions might be related to changes in the strength of Zr–O bonds of μ2-OH bridges linking complex sub-units, and change in symmetry of the crystal lattice (from hexagonal to trigonal). Analysis of thermogravimetric data showed that decomposition of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 proceeds with complete conversion to ZrO2 (monoclinic form) between 603 and 803 K. 相似文献
16.
A. I. Gubanov N. V. Kuratieva E. Yu. Filatov S. V. Korenev 《Journal of Structural Chemistry》2012,53(3):503-508
The structures of two salts [Co(NH3)6][Rh(NO2)6] (I) and [Co(NH3)6][(NO2)3Rh(μ-NO2)1+x (μ-OH)2−x Rh(NO2)3]·(2−x)(H2O), x = 0.17 (II) are solved. Single crystals of the salts are obtained by the counter diffusion method through the gel of aqueous solutions of [Co(NH3)6]Cl3 and Na3[Rh(NO2)6]. The structure of [Co(NH3)6][Rh(NO2)6] is consistent with the diffraction data for a polycrystalline sample of poorly soluble fine salt formed in the exchange reaction between aqueous solutions of [Co(NH3)6]Cl3 and Na3[Rh(NO2)6]. The structure of [Co(NH3)6][(NO2)3Rh(μ-NO2)1+x (μ-OH)2−x Rh(NO2)3]·(2−x)(H2O), x = 0.17 exhibits the stabilizing effect of a large cation in the formation of novel, unknown previously coordination ions: [(NO2)3Rh(μ-NO2)(μ-OH)2Rh(NO2)3]3− and [(NO2)3Rh(μ-NO2)2(μ-OH)Rh(NO2)3]3−. 相似文献
17.
A. V. Ermolaev A. I. Smolentsev Yu. V. Mironov 《Journal of Structural Chemistry》2011,52(6):1124-1126
Counter-diffusion of the aqueous solution of Cs2.75K1.25[Re6Se8(CN)4(OH)2] and a water-ammonia solution of NiCl2 afforded crystals of a rhenium cluster complex trans-{[Ni(NH3)5]2[Re6Se8(CN)4(OH)2]}·6H2O. The structure of the complex is determined by single crystal X-ray diffraction. In the structure, nickel atoms have an
octahedral coordination environment involving nitrogen atoms of five NH3 ligands and one CN ligand of the cluster anion. The anion has two bridging CN ligands in the trans-positions 相似文献
18.
X. Chen P. Yang S. -L. Ma S. Ren M. -Y. Tang Y. Yang Z. -J. Guo L. -Z. Liu 《Journal of Structural Chemistry》2009,50(3):495-499
Two novel cyano-bridged complexes, {[Cu(men)2][Ni(CN)4]
n
(1) (men = N,N′-dimethyl-ethylenediamine) and [Mn(bpy)2]4[Mo(CN)8]2·0.5MeOH·0.75H2O (2) (bpy = 2,2′-bipyridine) have been synthesized and structurally characterized by IR spectroscopy and X-ray crystallography.
The complex 1 has onedimensional zigzag chain structure in which the Ni atom is coordinated by four cyanide groups, and the Cu atom is
surrounded by four nitrogen atoms of the two men ligands in equatorial plane and two nitrogen atoms of the bridging cyanide
in axial positions; the Cu centre is in a distorted octahedral environment. Owing to weak interactions, complex 1 is self-assembled into two-dimensional network via N-H...N hydrogen bonds. In 2, the basic structural unit is centrosymmetric and contains four Mn centers connected by two octacyanomolybdates via eight
cyanide bridges. Each Mo atom is linked via four cyanide groups to four Mn, and the other four cyanide groups are terminal.
From X-ray single crystal analysis (room temperature), 1 crystallizes in monoclinic space group P21/n with a = 6.7332(7) ?, b = 13.9248(15) ?, c = 9.0869(10) ?, β = 98.4030(10)°, V = 843.05(16) ?3, Z = 2; 2 crystallizes in monoclinic space group P21/n with a = 13.886(6) ?, b = 24.116(11) ?, c = 15.263(7) ?, β = 90.175(6)°, V = 5111(4) ?3, Z = 2.
Original Russian Text Copyright ? 2009 by X. Chen, P. Yang, S.-L. Ma, S. Ren, M.-Y. Tang, Y. Yang, Z.-J. Guo, and L.-Z. Liu
The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 50, No. 3, pp. 518–521, May–June, 2009. 相似文献
19.
V. V. Sharutin V. S. Senchurin O. K. Sharutina A. P. Pakusina O. A. Fastovets 《Russian Journal of Inorganic Chemistry》2010,55(9):1415-1420
Triphenylbenzylphosphonium tetrachloroaurate (I) and triethanolammonium tetrachloroaurate hydrate (II) were prepared by reacting tetrachloroauric acid in acetone with triphenylbenzylphosphonium and triethanolammonium, respectively.
Triphenylethylphosphonium hexachlorodicuprate (III) was synthesized from triphenylethylphosphonium chloride and copper chloride in acetone. The crystal structures of complexes
I to III were determined by single-crystal X-ray diffraction. The phosphorus atoms in complex I have a nearly undistorted tetrahedral coordination (CPC, 108.3°–110.6°; P-C, 1.788–1.793 ?). The coordination of nitrogen
atoms in the cations of complex II is a distorted tetrahedron (CNC, 111.7°–112.4°). The square coordination of aurum in I and II is only slightly distorted: the ClAuCl angles are 89.6°–90.3° (I) and 89.5°–90.6° (II) and the Au-Cl distances are 2.256–2.278 ? I) and 2.280–2.285 ? (II). The phosphorus atoms in complex III are tetracoordinated (CPC, 106.34°–111.73°; P-C, 1.790–1.795 ?). The copper atoms in III have a distorted tetrahedral coordination (ClCuCl, 98.48°–144.85°; Cu-Cl, 2.1999–2.3263 ?). The central fragment Cu2Cl2 in the anion of complex III is bent relative to the Cu2 axis (the chlorine atom deviates from the Cu2Cl plane by 0.27 ?). 相似文献
20.
S. A. Gromilov Yu. V. Shubin A. I. Gubanov E. A. Maksimovskii S. V. Korenev 《Journal of Structural Chemistry》2009,50(6):1121-1125
Thermolysis of the complex salts (NH4)2[OsCl6]
x
[PtCl6]1−x
(x = 0.25−0.9) formed nanocrystalline Os
x
Pt1−x
phases. Pseudomorphism has been found: the habit of the single crystals of the starting salts is preserved during thermolysis,
and the ∼10–20 nm metal particles are agglomerated into octahedral structures sized 5–10 μm. 相似文献