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1.
Refinement of the X-ray crystal structures of Pr[M(CN)6] · 5H2O (M = Cr, Fe, Co) enables their space group to be reassigned to P63/mmc. Spectral characteristics are reported for M = Cr and the distinction between the pentahydrate and tetrahydrate series is clearly made from assignments of the infrared spectra. 相似文献
2.
Andrey Zadesenets Evgeny Filatov Pavel Plyusnin Iraida BaidinaVasiliy Dalezky Yuri Shubin Sergey Korenev Artyom Bogomyakov 《Polyhedron》2011,30(7):1305-1312
All the steps of the proposed technique, from the synthesis of single-source precursors to the preparation of CoPd and CoPt nanoalloys, are described. The double complex salts (DCS) [M(NH3)4][Co(C2O4)2(H2O)2]·2H2O (M = Pd, Pt), which were synthesized by mixing solutions containing [M(NH3)4]2+ cations and [Co(C2O4)2(H2O)2]2− anions, have been used as precursors. The salts obtained were characterized by IR spectroscopy, thermal analysis, XRD and single crystal X-ray diffraction. The prepared compounds crystallize in the monoclinic (space group I2/m, M = Pd) and orthorhombic (space group I222, M = Pt) crystal systems. Thermal decomposition of the salts in helium or hydrogen atmosphere at 200-600 °C results in the formation of nanoalloys powders (random solid solution Co0.50Pd0.50 and chemically ordered CoPt). The size of the bimetallic particles varied from 5 to 20 nm. Order-disorder structural transformations in Co0.50Pt0.50 nanoalloys were studied. The magnetic properties of both chemically disordered Co0.50Pd0.50 and ordered CoPt clusters have also been measured. 相似文献
3.
The organic-inorganic hybrid materials vanadium oxide [VIVO2(phen)2]·6H2O (1) and [(2,2′-bipy)2VVO2](H2BO3)·3H2O (2) have been conventional and hydrothermal synthesized and characterized by single crystal X-ray diffraction, elemental analyses, respectively. Although the method and the ligand had been used in the syntheses of the compounds (1) and (2) are different, they almost possess similar structure. They all exhibit the distorted octahedral [VO2N4] unit with organonitrogen donors of the phen and 2,2′-bipy ligands, respectively, which coordinated directly to the vanadium oxide framework. And they are both non-mixed-valence complexes. But the compound (1) is isolated, and the compound (2) consists of a cation of [(2,2′-bipy)2VVO2]+ and an anion of (H2BO3)−. So the valence of vanadium of (1) and (2) are tetravalence and pentavalence, respectively. Meanwhile it is noteworthy that π-π stacking interaction between adjacent phen and 2,2′-bipy groups in compounds 1 and 2 also play a significant role in stabilization of the structure. Thus, the structure of [VIVO2(phen)2]·6H2O and [(2,2′-bipy)2VVO2](H2BO3)·3H2O are both further extended into interesting three-dimensional supramolecular. Crystal data: (1) Triclinic, a=8.481(4), b=12.097(5), and α=66.32(2), β=82.97(3), and γ=82.59(4)°, Z=2, R1=0.0685, wR2=0.1522. (2) Triclinic, a=6.643(13), b=11.794(2), and α=101.39(3), β=101.59(3), and γ=97.15(3)°, Z=2, R1=0.0736, wR2=0.1998. 相似文献
4.
5.
Melita Tramšek 《Journal of fluorine chemistry》2005,126(7):1088-1094
New compounds of the type M2(H2F3)(HF2)2(AF6) with M = Ca, A = As and M = Sr, A = As, P) were isolated. Ca2(H2F3)(HF2)2(AsF6) was prepared from Ca(AsF6)2 with repeated additions of neutral anhydrous hydrogen fluoride (aHF). It crystallizes in a space group P4322 with a = 714.67(10) pm, c = 1754.8(3) pm, V = 0.8963(2) nm3 and Z = 4. Sr2(H2F3)(HF2)2(AsF6) was prepared at room temperature by dissolving SrF2 in aHF acidified with AsF5 in mole ratio SrF2:AsF5 = 2:1. It crystallizes in a space group P4322 with a = 746.00(12) pm, c = 1805.1(5) pm, V = 1.0046(4) nm3 and Z = 4. Sr2(H2F3)(HF2)2(PF6) was prepared from Sr(XeF2)n(PF6)2 in neutral aHF. It crystallizes in a space group P4122 with a = 737.0(3) pm, c = 1793.7(14) pm, V = 0.9744(9) nm3 and Z = 4. The compounds M2(H2F3)(HF2)2(AF6) gradually lose HF at room temperature in a dynamic vacuum or during being powdered for recording IR spectra or X-ray powder ray diffraction patterns. All compounds are isotypical with coordination of nine fluorine atoms around a metal center forming a distorted Archimedian antiprism with one face capped. This is the first example of the compounds in which H2F3− and HF2− anions simultaneously bridge metal centers forming close packed three-dimensional network of polymeric compounds with low solubility in aHF. The HF2− anions are asymmetric with usual F?F distances of 227.3-228.5 pm. Vibrational frequency (ν1) of HF2− is close to that in NaHF2. The anion H2F3− exhibits unusually small F?F?F angle of 95.1°-97.6° most probably as a consequence of close packed structure. 相似文献
6.
Yan-Jun Zhu Wen-Hua Zhang Yong Zhang Seik-Weng Ng 《Journal of organometallic chemistry》2005,690(14):3479-3487
Reactions of Ln2O3 and trans-4-pyridylacrylic acid (4-Hpya) in EtOH/H2O or MeOH/H2O produced two new lanthanide/4-pya complexes [Ln(4-pya)3(H2O)2]2 (1: Ln = Eu; 2: Ln = La) in low yields. However, reactions of LnCl3 · 6H2O with 4-Hpya/aqueous ammonia in EtOH/H2O or MeOH/H2O gave rise to 1 or 2 in higher yields. Both compounds were structurally characterized by elemental analysis, IR spectroscopy and X-ray analysis. Compounds 1 · 2EtOH · 2H2O and 2 · 2MeOH · 2H2O were confirmed to possess one-dimensional polymeric chain structures. In the structure of 1, each Eu(III) adopts a monocapped square-antiprism coordination geometry and each dimer [Eu(4-pya)3(H2O)2]2 within the chain is interconnected by two pairs of different bridging 4-pya ligands. On the other hand, each La(III) of 2 takes a bicapped square-antiprism coordination geometry and each dimer [La(4-pya)3(H2O)2]2 within the chain is linked by two pairs of tridentate bridging 4-pya ligands. The luminescent properties of 1 and 2 in the solid state were investigated. 相似文献
7.
Michael Veith Hinka Hreleva-Carparrotti Volker Huch 《Journal of organometallic chemistry》2007,692(13):2784-2788
When the polycyclic alumosiloxane [Ph2SiO]8[AlO(OH)]4 is allowed to react with either cyclopentadienyl sodium in tetrahydrofuran or with dimethyl zinc in diethyl ether the organic ligands on the metal elements are eliminated as cyclopentadiene or methane and the metals are bonded to oxygen atoms in the alumosiloxane forming [Ph2SiO]8[AlO2(Na)]4 · 5(THF) or [Ph2SiO]8[AlO(OH)]2[AlO2]2[Zn(OH)]2 · 2(OEt2), respectively. X-ray structure determinations reveal that in the sodium derivative the original polycycle rests almost unchanged while in the zinc derivative the inner skeleton is rearranged. 相似文献
8.
Long-Fei Jin 《Journal of organometallic chemistry》2006,691(13):2909-2914
A novel macrocyclic hexanuclear manganese(III) 18-metallacrown-6 compound, [Mn6(H2O)6 (anshz)6] · 10DMF, has been prepared using a trianionic pentadentate ligand N-acetyl-5-nitrosalicylhydrazide (anshz3−) and characterized by X-ray diffraction (DMF = N,N-dimethylformamide). The crystal structure contains a neutral 18-membered metallacrown ring consisting of six Mn(III) and six anshz3− ligands. The 18-membered metallacrown ring is formed by the succession of six structural moieties of the type [Mn(III)NN]. Due to the meridional coordination of the ligand to the Mn3+ ion, the ligand enforces the stereochemistry of the Mn3+ ions as a propeller configuration with alternating Δ/Λ forms. The disc-shaped hexanuclear ring shows at its largest diameter about 7.14 Å at entrance, about 9.76 Å at the center of the cavity, respectively. Antibacterial screening data showed that the manganese metallacrown has strong antimicrobial activity against Bacillus subtilis. 相似文献
9.
Gerry Rother Ronald Stief Ursula Bentrup Werner Massa 《Journal of fluorine chemistry》2011,132(10):740-746
Using biprotonated dabco (1,4-diazabicyclo[2.2.2]octane) or pipz (piperazine) as counter cations, mixed-ligand fluoromanganates(III) with dimeric anions could be prepared from hydrofluoric acid solutions. The crystal structures were determined by X-ray diffraction on single crystals: dabcoH2[Mn2F8(H2O)2]·2H2O (1), space group P21, Z = 2, a = 6.944(1), b = 14.689(3), c = 7.307(1) Å, β = 93.75(3)°, R1 = 0.0240; pipzH2[Mn2F8(H2O)2]·2H2O (2), space group , Z = 2, a = 6.977(1), b = 8.760(2), c = 12.584(3) Å, α = 83.79(3), β = 74.25(3), γ = 71.20(3)°, R1 = 0.0451; (dabcoH2)2[Mn2F8(H2PO4)2] (3), space group P21/n, Z = 4, a = 9.3447(4), b = 12.5208(4), c = 9.7591(6) Å, β = 94.392(8)°, R1 = 0.0280. All three compounds show dimeric anions formed by [MnF5O] octahedra (O from oxo ligands) sharing a common edge, with strongly asymmetric double fluorine bridges. In contrast to analogous dimeric anions of Al or Fe(III), the oxo ligands (H2O (1,2) or phosphate (3)) are in equatorial trans-positions within the bridging plane. The strong pseudo-Jahn-Teller effect of octahedral Mn(III) complexes is documented in a huge elongation of an octahedral axis, namely that including the long bridging Mn-F bond and the Mn-O bond. In spite of different charge of the anion in the fluoride phosphate, the octahedral geometry is almost the same as in the aqua-fluoro compounds. The strong distortion is reflected also in the ligand field spectra. 相似文献
10.
Lorena M. CallejoNoelia De la Pinta Gotzon MadariagaLuis Lezama M. Luz FidalgoRoberto Cortés 《Polyhedron》2011,30(6):923-928
Here we report the synthesis and characterization by X-ray diffraction, FTIR, UV-Vis and EPR spectroscopies, and the magnetic measurements of two new compounds: [Mn(NCS)2(bpe)2(H2O)2] (1) and [Fe(NCS)2(bpe)2(H2O)2] (2) (bpe = 1,2-bis(4-pyridyl)ethylene). Single-crystal structure analyses reveals discrete octahedral metal units that are assembled into 2D sheets through O-Hw?N(bpe) and O-Hw?S(thiocyanate) hydrogen bonds. The intermetallic M?M distances are 6.90 and 6.87 Å for 1 and 2, respectively. Supramolecular architectures are obtained by connections through H-bonds. Slight interactions are observed for compound 2. 相似文献
11.
Gašper Tav?ar 《Journal of fluorine chemistry》2006,127(10):1368-1373
[Cu(XeF2)6](SbF6)2 crystallizes in the rhombohedral symmetry with a = 1003.6(2) pm, c = 2246.5(12) pm at 200 K and Z = 3, space group (No. 148). [Zn(XeF2)6](SbF6)2 is isostructural to [Cu(XeF2)6](SbF6)2 with a = 1007(2) pm and c = 2243(6) pm. The structures are characterized by isolated homoleptic [M(XeF2)6]2+ (M = Cu, Zn) cations and of [SbF6]− octahedra.Reactions of M(SbF6)2 (M = Cu, Zn) with XeF2 in anhydrous hydrogen fluoride (aHF) and reactions of MF2 with Xe2F3SbF6 in aHF always yield a mixture of [M(XeF2)6](SbF6)2, Xe2F3SbF6 and MF2. 相似文献
12.
[Ni(H2O)6][Cu3Cl8(H2O)2] · (15-crown-5)2 · 2H2O can be conveniently prepared by the interaction of NiCl2 · 6H2O, CuCl2 · 2H2O and 15-crown-5 in water. The X-ray crystal structure reveals an ionic complex involved in a hydrogen-bonded two dimensional network with the [Ni(H2O)6]2+ and [Cu3Cl8(H2O)2]2− ions sandwiched between the 15-crown-5 macrocycles. The magnetic susceptibility data (4–300 K) and magnetisation isotherms (2–5.5 K; 0–5 T) are best interpreted in terms of intra-trimer ferromagnetic coupling within the [Cu3Cl8(H2O)2]2− moieties, with J ∼ 6 cm−1, and antiferromagnetic coupling between the trimers, the latter mediated by H-bonding pathways. Comparisons are made to other reported quaternary ammonium salts of [Cu3Cl8]2− and [Cu3Cl12]6−, most of which display structures that involve close stacking of such Cu(II) trimers, rather than being of the present isolated, albeit H-bonded, types. 相似文献
13.
Qianling Guo Wenxiang Zhu Shujing Dong Shulan Ma Xi Yan 《Journal of Molecular Structure》2003,650(1-3):159-164
The title calixarene, dimanganese thiacalix[4]arene tetrasulfonate, was prepared and its crystal structure was determined. [Mn(H2O)6]2[thiacalix[4]arene tetrasulfonate]·0.5H2O crystallizes in the monoclinic system, P2(1)/m space group, with a=13.014 (6), b=14.146 (9), c=13.184 (7) Å, β=113.307 (10)°, V=2229 (2) Å3 and Dc=1.710 gcm−3, Z=2. The title calixarene exists in the solid state as bilayer structure. The hydrophobic organic layer consists of thiacalix[4]arene tetrasulfonate in an up-down fashion, whereas, the hydrophilic inorganic layer consists of hexaaquamanganese (II) which is linked to the former through a second-sphere coordination. 相似文献
14.
A. Leineweber 《Journal of solid state chemistry》2003,176(1):198-202
A re-interpretation and re-evaluation of single-crystal X-ray diffraction data of a previously reported ‘(NH4)2(NH3)[Ni(NH3)2Cl4]’ (J. Solid State Chem. 162 (2001) 254) give a new formula (NH4)2−2z[Ni(NH3)2]z[Ni(NH3)2Cl4] with z=0.152. This new formula results from defects in an idealized ‘(NH4)2[Ni(NH3)2Cl4]’ basic structure, where two adjacent NH4+ cations are replaced by one Ni(NH3)22+ unit. Cl− anions from the basic structure complete the coordination sphere of the new Ni2+ to [Ni(NH3)2Cl4]2−. 相似文献
15.
16.
C.J. Antony M. Junaid Bushiri Hema Tresa Varghese C. Yohannan Panicker Michel Fleck 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2009,73(5):942-945
Raman and FTIR spectra of guanidinium zinc sulphate [C(NH2)3]2Zn(SO4)2 are recorded and the spectral bands assignment is carried out in terms of the fundamental modes of vibration of the guanidinium cations and sulphate anions. The analysis of the spectrum reveals distorted SO42− tetrahedra with distinct S–O bonds. The distortion of the sulphate tetrahedra is attributed to Zn–O–S–O–Zn bridging in the structure as well as hydrogen bonding. The CN3 group is planar which is expressed in the twofold symmetry along the C–N (1) vector. Spectral studies also reveal the presence of hydrogen bonds in the sample. The vibrational frequencies of [C(NH2)3]2 and HC(NH2)3 are computed using Gaussian 03 with HF/6-31G* as basis set. 相似文献
17.
Danijela Čurman Petra Živec Ivan Leban Iztok Turel Anna Polishchuk Karel D. Klika Emiliya Karaseva Vladimir Karasev 《Polyhedron》2008
A novel europium complex of fluoroquinolone ciprofloxacin (cfqH) with formula [Eu(cfqH)(cfq)(H2O)4]Cl2 · 4.55H2O (1) was synthesized and its crystal structure determined by X-ray crystallography. The coordination number of europium is eight and in this structure two bidentate, O,O-bonded quinolone molecules and four aqua ligands are coordinated to the metal. One molecule of quinolone is anionic whereas the other is zwitterionic. Additionally, two chloride ions are also present in the structure to compensate the charge of the europium(III) whilst disordered solvent water molecules too are present. The spectral properties (IR, Raman, luminescence) of compound 1 were studied. Analysis of the Stark structure of the luminescence spectra was carried out and the scheme of the electronically excited states and photophysical processes of compound 1 was arranged. The spectral properties show that europium–ciprofloxacin complexes could be suitable for various applications based on their solution-state stability as measured by 1H and 19F NMR. 相似文献
18.
B. Sieklucka W.
asocha L. M. Proniewicz R. Podgajny H. Schenk 《Journal of Molecular Structure》2000,520(1-3):155-163
The bimetallic [Pt(NH3)4]2[W(CN)8][NO3]·2H2O is characterised by single-crystal X-ray diffraction [S.G.P21/m(11), a=8.0418(7), b=19.122(2), c=9.0812(6) Å, Z=2]. All platinum centres have the square-plane D4h geometry with average dimensions Pt(1)–N 2.042(2) and Pt(2)–N 2.037(10) Å. The octacyanotungstate anion has the square-antiprismatic D4d configuration with average dimensions W(1)–C 2.164(13), C–N 1.140(12), W(1)–N 3.303(5) Å. The structure exhibits two different mutual orientations of Pt versus W units resulting in Pt(2)–W(1), W(1)* separations of 4.77(2), 4.55(2)* and Pt(1)–W(1) of 6.331(8) Å. A centrosymmetric structure reveals groups of two distinct columns: the first is formed by intercalated NO3− between parallel [Pt(1)(NH3)4]2+ planes and the second consists of [W(CN)8]3− interlayered by, parallel to square faces of W-antiprisms, [Pt(2)(NH3)4]2+. The structure is stabilised through a three-dimensional hydrogen bond network via nitrogen atoms of cyanide ligands, hydrogen atoms of NH3 ligands, water molecules and oxygen atoms of NO3− counteranions. The vibrational pattern and the range of ν(CN) frequencies attributable to the electronic environment of W(V) and W(IV) are consistent with the ground state Pt(II)↔W(V) charge transfer. 相似文献
19.
ANi(AsF6)3 (A = O2+, NO+, NH4+) compounds could be prepared by reaction between corresponding AAsF6 salts and Ni(AsF6)2. When mixtures of AF (A = Li, Na, K, Rb, Cs) and NiF2 are dissolved in aHF acidified with an excess of AsF5 the corresponding AAsF6 and Ni(AsF6)2 were formed in situ. For A = Li and Na only mixtures of AAsF6 and Ni(AsF6)2 were obtained, while for A = K, Rb and Cs, the final products were ANi(AsF6)3 (A = K-Cs) compounds contaminated with AAsF6 (A = K-Cs) and Ni(AsF6)2.ANi(AsF6)3 (A = H3O+, O2+, NO+, NH4+ and K+) compounds are structurally related to previously known H3OCo(AsF6)3. The main features of the structure of these compounds are rings of NiF6 octahedra sharing apexes with AsF6 octahedra connected into infinite tri-dimensional network. In this arrangement cavities are formed where single charged cations are placed.In O2Ni(AsF6)3 the vibrational band belonging to O2+ vibration is found at 1866 cm−1, which is according to the literature data one of the highest known values, and it is only 10 cm−1 lower than the value for free O2+. 相似文献
20.
María del C. Hernández-Galindo 《Journal of organometallic chemistry》2007,692(23):5295-5302
Herein we report on the preparation of hydrated ammonium salts of the dithiophosphonic acids (RO)(Fc)P(S)(SH) (R = derivative of benzyl) featuring [(NH4 · H2O)2]2+ cations formed by N-H?O hydrogen bonds. Interaction of these cations with the PS2− units gives rise to unprecedented 2D networks, formed solely by hydrogen bonds. These unique networks containing two- and three centered hydrogen bonds are valuable examples of the acceptor properties of sulfur atoms. 相似文献