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1.
The reaction of equimolar amounts of triphenylamyl- and triphenylpropylphosphonium iodides and triethanolammonium iodide with antimony iodide in dimethyl sulfoxide, dioxane, or acetone gave complexes [Ph 3AmP] 2 + [Sb 2I 8 · 2DMSO] 2?, [Ph 3PrP] 2 + [Sb 2I 8 · C 4H 8O 2] 2?, and [(HOCH 2CH 2) 3NH] 4 + [Sb 4I 16] 4?, the structure of which was established by X-ray diffraction analysis. The cations of all complexes have slightly distorted tetrahedral structure, and the antimony atoms in the anions are hexacoordinated. The crystals of the complexes have intra- and intermolecular contacts, which form the structure. 相似文献
2.
The reaction of pentaphenylantimony with mercury iodide affords the ionic complex [Ph 4Sb] 2 + [Hg 2I 6] 2?·Ph 2Hg ( I). The [Ph 4Sb] 2 + [Hg 2I 6] 2? ( II) and [Ph 4Sb] 2 + [Cd 2I 6] 2? ( III) complexes are synthesized from tetraphenylantimony iodide and mercury and cadmium iodides. The [Ph 4Sb] 2 + [Hg 4I 10] 2? complex ( IV) is prepared from tetraphenylantimony 2,4-dimethylbenzenesulfonate and mercury iodide. According to the X-ray diffraction data, the Sb atom in the [Ph 4Sb] + cations of complex I has virtually ideal tetrahedral coordination (the CSbC angles are 108.09°–109.64°). In the central square fragment Hg 2I 2 of the [Hg 2I 6] 2? anion, the Hg-I br bond lengths are 2.825 and 3.075 Å, and the terminal iodine atoms are more strongly bonded to the mercury atoms (Hg-I term 2.691 and 2.700 Å). The [Cd 2I 6] 2? anion in complex III has a similar structure (the Cd-I bridg and Cd-I term distances are 2.865, 2.872 and 2.723, 2.748 Å, respectively). The anions in complex IV are joined by I…Hg (3.651 Å) and I…I (4.058 Å) interactions into an infinite dimeric network. 相似文献
3.
Complexes [(4-MeC 6H 4) 4Sb] 2 + [Hg 2I 6] 2? ( I), [(4-MeC 6H 4) 4Sb] 2 + [HgI 4] 2? ( II), [(4-MeC 6H 4) 4Sb] 3 + [Sb 3I 12] 2? ( III), were synthesized by reactions of tetra- p-tolylantimony iodide with mercury iodide and antimony iodide, respectively. Tetra- p-tolylantimony perrhenate [(4-MeC 6H 4) 4Sb] +[ReO 4] ? ( IV) was prepared from tetra- p-tolylantimony chloride and sodium perrhenate in acetone. Crystal structures of complexes I, II, and IV were determined by X-ray crystallography. Mercury and rhenium atoms have tetrahedral coordinations in these complexes. The Hg-I and Re-O distances in the structures of I, II, and IV vary within 2.7719(13)–2.7908(12)Å, 2.7028(3)–2.9163(3) Å, and 1.693(3)–1.744(3) Å, respectively. Antimony atoms in two crystallographically independent trinuclear centrosymmetric [Sb 3I 12] 2? anions of complex III have an octahedral environment. Each terminal SbI 3 fragment (Sb-I t, 2.8265(9)–2.8333(10)Å) is bound to the central atom through tree bridging iodine atoms (Sb(2)-I br, 3.2275(9)–3.3620(10)Å). The distances between the central Sb atom and bridging iodine atoms are much shorter (Sb(1)-I br, 3.0153(6)–3.0316(6) Å; Sb(3)-I br, 2.9926(6)–3.0074(6) Å). 相似文献
4.
Complexes [Ph 3MeP] 2 + [BiI 3.5Br 1.5(C 5H 5N)] 2? · C 5H 5N( I), [Ph 4Bi] 4 + [Bi 4I 16] 4? · 2Me 2C=O ( II), and [Ph 3( iso-Am)P] 4 + [Bi 8I 28] 4? · 2Me 2C=O ( III) were synthesized by reactions of bismuth iodide with triphenylmethylphosphonium bromide, triphenylbismuthonium sulfosalicylate, and triphenylisoamylphosphonium iodide, respectively. The crystal structures of complexes I–III were determined by X-ray crystallography. The complexes contain, in addition to cations and solvent molecules, mono-, tetra-, and octanuclear anions, in which bismuth atoms are in octahedral coordination. 相似文献
5.
The complexes [Ph 3PMe] 2 + [BiI 5] 2? (I) and [Ph 3PMe] 2 + [BiI 5 · C 5H 5N] 2? · C 5H 5N (II) were synthesized by the reaction of bismuth triiodide with triphenylmethylphosphonium iodide, and their structures were determined by X-ray diffraction analysis. The P atom in cation I has slightly distorted tetragonal coordination polyhedron (the CPC angles 109.42(4)° and 109.52(4)°, the bond lengths P-C Ph 1.779(2), P-C Me 1.793(1) Å. The Bi atom in the anion of complex I has an ideal trigonal-bipyramidal coordination polyhedron (Bi-I eq 3.0031(4), Bi-I eq 3.0485(5) Å). The crystal of complex II consists of the anions [BiI 5 · C 5H 5N] 2?, solvated pyridine molecules, and two types of crystallographically independent tetrahedral triphenylmethylphosphonium cations (the angles CPC 106.9(1)°–111.7(1)°, the distances P-C Ph 1.785(3)–1.792(3), P-C Me 1.793(3), 1.786(3) Å). The Bi atoms in the anion of complex II have a distorted octahedral coordination polyhedron (Bi-I 3.0878(4)–3.1240(3), Bi-N(1) 2.628(3) Å). 相似文献
6.
The reactions of tetraphenylbismuthonium and -stibonium salts Ph 4EX (E = Bi, Sb; X = I, OSO 2 (C 6H 3(CH 3) 2-2,5), OSO 2C 6H 3(OH-4)(COOH-3)) with bismuth triiodide in acetone afford complexes [Ph 4Bi] +[PhBi(C 5H 5N)I 3] -, [(Ph 4BiO) 2S(O){2,5-(CH 3) 2C 6H 3S(O)} [Ph 2Bi 2I 6] 2–, [Ph 4Sb [Bi 4I 16] 4-·2(CH 3) 2C=O, and [Ph 4Sb] 3+ + [Bi 5I 18] 3-, whose structural units, according to the X-ray diffraction data, are tetraphenylbismuthonium (-stibonium) cations and mono-, di-, tetra-, and pentanuclear anions, respectively. 相似文献
7.
Synthesis and characterisation of [tris(1,3-dithiole-2-thione-4,5-dithiolato)-stannate]2−, [Q]2[Sn(dmit)3], [tris(1,3-dithiole-2-one-4,5-dithiolato)stannate]2−, [Q]2[Sn(dmio)3] and [tris(1,3-dithiole-2-thione-4,5-selenolato)stannate]2−, [Q]2[Sn(dsit)3], complexes: Analysis of the structural variations of the [Sn(dmit)3]2− and [Sn(dmio)3]2− dianions
[Tris(1,3-dithiole-2-thione-4,5-dithiolato)stannate] 2−, [Q] 2[Sn(C 3S 5) 3], [tris(1,3-dithiole-2-one-4,5-dithiolato)stannate] 2−, [Q] 2[Sn(C 3S 4O) 3], and [tris(1,3-dithiole-2-thione-4,5-diselenolato)stannate] 2− [Q] 2[Sn(C 3S 3Se 2) 3], complexes, have been synthesised and characterised. Crystal structure determinations of [Q] 2[Sn(C 3S 5) 3] (Q=1,4-dimethylpyridinium, monoclinic and orthorhombic forms; NMe 4, NEt 4, and PPh 4) and [NEt 4] 2[Sn(C 3S 4O) 3] revealed variations in the overall dianion structures. The geometry about tin in each case is essentially octahedral with the chelate bite angles in the range 80.7(5)–87.45(4)°: the range of Sn–S distances is 2.5207(18)–2.571(17) Å. A statistical analysis, carried out on the crystal structure data for the six complexes, indicated that the most critical factors in controlling the overall shape of the dianion were the distances of the Sn atom from the dithiolate ligand planes [Sn–OOP]. Interanionic S⋯S interactions, within the sum of the van der Waals’ radii for two S atoms, are affected by the size of the cation, Q; the secondary connectivity is 3-dimensional for the smallest cations, Q=1,4-dimethylpyridinium and NMe 4, in chains for the somewhat larger cation, NEt 4 and is absent for the still larger, PPh 4 cation. 相似文献
8.
The [NpO 2(DPPMO 2) 2Cl][NpO 2Cl 4] complex (where DPPMO 2 = bis(diphenylphosphino)methanedioxide) contains the linear neptunyl group, {NpO 2} 2+, with two bidentate P=O donor ligands. Coordinating anion Cl ? fills the fifth equatorial coordination site yielding a complex of general formula [NpO 2(DPPMO 2) 2X] 2[Y] ( 1) (where X = Cl ? and Y = [NpO 2Cl 4] 2?. Reaction between our newly prepared neptunium starting material [NpO 2Cl 2(thf)] n and phosphinimine ligand produced crystals of [Ph 3PNH 2] 2[NpO 2Cl 4] ( 2). Compounds 1 and 2 have been structurally characterised. 相似文献
9.
Russian Chemical Bulletin - The complexes [Et2H2N]+2[ZrCl6]2– (1), [Me3NCH2Ph]+2[ZrCl6]2–?MeCN (2), [Ph3PC6H4(CHPh2-4)]+2[ZrCl6]2–?2 MeCN (3), and... 相似文献
10.
The electrophoretic behavior of twenty anions has been studied on silica gel-G, titanium (IV) tungstate and silica gel-G- titanium (IV) tungstate admixture layers using 0.1 M solutions of oxalic acid, citric acid, tartaric acid, succinic acid and acetic acid as background electrolyte. The mechanism of migration is explained in terms of adsorption and the solubility of various sodium or potassium salts of the anions in water. Titanium (IV) tungstate behaves only as an adsorbent and not as an ion exchanger. Being a cation exchanger, there is no exchange phenomenon occurring with anions. The migration of halides increase linearly with an increase in the bare ion radii of these ions. Differential migration of the anions on silica gel-G layers led to binary, ternary and quaternary separations of similar anions such as F− – Cl− – Br− – I−, I− – IO3− – IO4−, BrO3− – IO3− and Fe(CN)63− – Fe(CN)64−. The two cyanoferrate ions are separated from industrial waste water and from fixer and bleach solutions. The migration of anions has also been found to be in accordance with their lyotropic numbers. 相似文献
11.
Zusammenfassung Die Absorptions- und Reflexionsspektren der Oktocyanokomplexe des Mo(IV) und W(IV) sowie die Absorptionsspektren der Oktocyanotomplexe des Mo(V) und W(V) werden mitgeteilt. Die Spektren werden unter Zugrundelegung der durch Raman- und IR-spektroskopische Untersuchungen geforderten D
4d-Symmetrie dieser Verbindungen interpretiert. Die beobachteten Banden niedriger Intensität (log <3) werden Übergängen in einem Termsystem zugeordnet, das für die Konfigurationen d
2 und d
1 und die Symmetrie D
4d berechnet worden ist. Banden hoher Intensität (log >3) werden auf Übergänge in antibindende Zustände zurückgeführt, an denen höhere p-Zustände des Zentralions sowie Ligandenzustände beteiligt sind. Die erhaltenen Werte des Feldparameters stimmen mit ligandenfeldtheoretischen Erwartungen überein.
Absorption and reflection spectra of the octacyanides ofMo(IV) andW(IV) and the absorption spectra of the octacyanides ofMo(V) andW(V) are presented. The spectra are interpreted in terms of theD
4d symmetry of the compounds supported by investigations of Raman and infrared spectra. Bands of low intensity (log<3) correspond to transitions between levels obtained in the case of the configurationsd
2 andd
1 respectively, in a field ofD
4d symmetry. Bands of high intensity (log>3) are attributed to transitions into antibonding levels in which p-orbitals of the central ion and ligand orbitals participate. The values of the field parameter obtained are in accord with ligand field theory.
Résumé Les spectres d'absorption et de réflexion des complexes octocyanurés duMo(IV) et duW(IV) ainsi que les spectres d'absorption des mêmes complexes deMo(V) et de W(V) sont présentés. Les spectres sont interprétés en supposant la symétrieD
4d des molécules indiquée par des analyses des spectres Raman et infrarouges. Les bandes de faible intensité (log<3) sont attribuées à des transitions dans un système de niveaux, calculé pour les configurationsd
2 etd
1, respectivement, en symétrieD
4d. Des bandes de forte intensité (log>3) sont attribuées à des transitions vers des niveaux antiliants auxquels participent des fonctions élevéesp de l'ion central et des fonctions des groupes liés. Les valeurs obtenues pour le paramètre de champ sont en accord avec les prévisions de la théorie. 相似文献
12.
Russian Journal of Coordination Chemistry - The reaction of bis(tetraphenylantimony) succinate with iodine in benzene affords [(μ4-succinato) hexadecaphenyltetraantimony] triiodide solvate... 相似文献
13.
<正> Compound (Ph3PCH2Ph)[Ni (OSNC5H3)2] . DMF was obtained from the reaction.of NiCl2,Na2(OSNC5H3)and Ph3PCH2PhCl. Mr = 735. 53,monoclinic,P21/ c,a=9. 857(6),b=17. 594(9),c=21. 369(10) A,β=102. 85(4)°,V=3613. 1A3,Z = 4,Dc=1. 35g/cm3,λ(Mo-Ka) = 0.71073A.μ=7. 3cm-1,F(000) = 1532,The nickel (Ⅲ) ion is coordinated by two 2-mercapto-3-pyridinolate ligands to give an approximate square-plannar configuration with cis-geometry. 相似文献
14.
Electron propagator theory (EPT) is applied to calculating vertical ionization energies of the anions F −, Cl −, OH −,SH −, NH 2−, PH 2− and CN −. Third-order and outer valence approximation (OVA) quasiparticle calculations are compared with ΔMBPT(4) (MBPT, many-body perturbation theory) results using the same basis sets. Agreement with experiment is satisfactory for EPT calculations except for F − and OH −, while the ΔMBPT treatments fail for CN −. EPT(OVA) estimates are reliable when the discrepancy between second- and third-order results is small. Computational aspects are discussed, showing relative merits of direct and indirect methods for evaluating electron binding energies. 相似文献
16.
The reaction of AgNO 3 with [(“Bu 4N 2 i-MNT)] 3 in CH 3CN produces a new silver cluster anion [Ag 4( i-MNT) 4] 4? , 3, a species having a tetrahedral arrangement of silver atoms bridged by four i-MNT ligands which has been isolated and characterized by X-ray crystallography as [Bu 4N] 2[(PPh 3) 2] 2 [Ag 4( i-MNT) 4], 4. The reaction of two or three equivalents of Ag(PPh 3) 2NO 3 with [BzEt 3N] 6[Ag 6( i-MNT) 6] in CH 3CN produces two new clusters, [BzEt 3N] 4[Ag 8( i-MNT) 6(PPh 3) 4], 6, and [BzEt 3N] 3[Ag 4( i-MNT) 6(PPh 3) 6], 7, having the common structural feature of an octahedral Ag 6S 12 core. The octanuclear Ag 8 cluster also can be synthesized from the reaction of 4 and PPh 3 in CH 2Ck 2 and compound 5 has been structurally characterized as [Bu 4N] 2[(PPh 3) 2N] 2[Ag 8( i-MNT) 6(PPh 3) 4]. The 31P{ 1H} NMR spectrum of 6 in CD 3CN at ?43° shows two sets of two doublets. The corresponding chemical shift and coupling constant of each species is 9.32 ppm (354, 408.8 Hz) and 9.45 ppm (346.7, 401.7 Hz), respectively. Pertinent crystallographic data are as follows: Compound 4 crystallizes in the orthorhombic space group Cc2a, with a=18.668(3)A, b=36.793(4) A, c=17.836(3)A, Z=4, and V= 12250(3)A 3. Compound 5 crystallizes in the triclinic space group P1, with a=16.506(3)A, b=17.280(3)A, c=19.144(4) A, x=98.485(14)°, β= 105.44(2)°. y=94.63(2), Z= 1, and V = 5164(2)A 3. Compound 6 crystallizes in the monoclinic space group C2/m, with a= 25.341(9)A, b= 25.289(9)A, c= 15.076(7)A, β= 107.19(5)°, Z=2, and V=9230(6)A 3. Compound 7 crystallizes in the monoclinic space group C2/c, with a=25.872(6)A, b=21.288(4) A, c=35,928(5), β=100.98(1)°, Z-4, and V=19426(6)A 3. 相似文献
17.
121Sb Mössbauer spectra of the title complexes, whose isomer shifts are intermediate between the organoantimony(III) and organoantimony(V) compounds, suggest that considerable electrons are donated from hydrido ligand and Fe(CO) 4 fragments to the antimony atom. 相似文献
18.
The reaction of silver nitrate with Ph 3-SbBr 2 in an ethanol-acetone solution afforded the complex [Ph 3Sb(NO 3)] 2O·Me 2C=O ( 1). According to the data of X-ray diffraction study of crystals of 1, molecule 1 contains a nonlinear O-bridge, which links two Sb atoms. The Sb atoms have a trigonal-bipyramidal configuration. The NO 3 group and the bridging oxygen atom are in axial positions and the three Ph substituents are in equatorial positions.
Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 1, pp. 174–176, January, 1999. 相似文献
19.
The amine PhCH 2CH 2NH 2 undergoes dimetallation by [Ph 3Sb(NMe 2) 2] ( 1) under mild conditions to give the first structurally authenticated example of an organo-Sb(V) imido complex, [Ph 3Sb(μ-NCH 2CH 2Ph)] 2 ( 2). 相似文献
20.
Self-assembly of the precursor [Cu(L)] 2+ (L = 3,10-dipropyl-1,3,5,8,10,12-hexaazacyclotetradecane) with hexacyanometalate [Fe(CN) 6] 3− produces a 3-D cyano-bridged Cu(II)–Fe(III) bimetallic assembly, [CuL] 2[Fe(CN) 6]ClO 4 · H 2O (1), characterized by single-crystal X-ray diffraction studies, and magnetic measurements. The crystallographic determination
reveals that each hexacyanoferromate(III) ion connects four copper(II) ions using four co-planar CN − groups which axially coordinate to the copper ion in a trans fashion forming trans-CuL(N≡C) 2 moieties in (1). Magnetic studies reveal that (1) displays a ferromagnetic interaction between Cu(II) and Fe(III) through the CN linkage. 相似文献
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