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The crystal structures of the title compounds Sb(C9H6NO)2(S2COC2H5) (1) and Sb(S2COC2H5)3 (2) have been determined by three dimensional X-ray diffraction techniques and refined by a least squares method; final R 0.049 for 2911 reflections [I ? 3σ(I)] for (1) and R 0.047, Rw 0.046 for 846 reflections [I ? 2σ(I)] for (2). Crystals of (1) are triclinic, space group P1, a = 10.825(2), b = 11.131(2), c = 8.911(1) Å, α = 109.45(1), β = 95.92(1) and γ = 93.02(1)° with Z = 2. Crystals of (2) are rhombohedral, space group R, arhomb = 10.138(3) Å and α = 103.43(2)°. The environment of the Sb atom in (1) is based on a pentagonal bipyramidal geometry consisting of the six donor atoms of the three chelating ligands and a stereochemically active lone-pair of electrons which occupies the remaining axial position. The xanthate ligand chelates the Sb atom almost symmetrically with two long SbS bonds of 3.059(2) and 3.171(2) Å. In contrast the xanthate ligands in (2) chelate the Sb atom with asymmetric SbS bonds of 2.511(2) and 3.002(3) Å. 相似文献
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The crystal structures of the title compounds, M(S2COiC3H7)3, M = As(III), (1); Sb(III), (2); and Bi(III), (3) have been determined by three dimensional X-ray diffraction techniques and refined by a least square method. Crystals of (1) and (2) are isomorphous and both crystallize in the rhombohedral space group R, with unit cell parameters for (1) ahex = 11.559(2), chex = 28.131(3) Å and for (2) ahex = 11.696(2) and chex = 28.135(2) Å, Z = 6. The central metal atom in both (1) and (2) is coordinated by three asymmetrically chelating xanthate ligands [AsS 2.305(2) and 2.978(2) Å and SbS 2.508(1) and 3.006(1) Å] which form a distorted octahedral environment consistent with the presence of a stereochemically active lone pair of electrons. Crystals of (3) are orthorhombic, space group Pnma, Z = 4 with dimensions a = 11.003(3), b = 20.833(4) and c = 9.428(2) Å. The environment of the bismuth atom in (3) is seven coordinate and is comprised of six sulphur atoms, derived from three asymmetrically coordinating xanthate ligands, and a bridging sulphur atom from a neighbouring molecule which results in the formation a polymeric array. For (1) final R and RW 0.050 and 0.047 respectively for 936 reflections [I ? 3σ(I); (2) R 0.040, Rw 0.040 for 1455 reflections I ? 2σ(I)]; and (3) R 0.052, Rw 0.039 for 1796 reflections [I ? 2σ(I). 相似文献
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《Inorganica chimica acta》1988,147(2):189-197
Complexes of the M(en)3Ag2(CN)4 (M = Ni, Zn, Cd) and M(en)2Ag2(CN)4 (M = Ni, Cu, Zn, Cd) type were prepared and identified by elemental analysis, infrared spectroscopy, measurement of magnetic susceptibility, and X-ray powder diffractometry. The crystal structures of Ni(en)3Ag2(CN)4 (I) and Zn(en)2Ag2(CN)4 (II) were determined by the method of monocrystal structure analysis. Complex I crystallizes in the space group C2/c, a = 1.2639(5), b = 1.3739(4), c = 1.2494(4) nm, β = 113.25(4)°, Dm = 1.86(1), Dc = 1.86 gcm−3 Z = 4, R = 0.0429. The crystal structure of I consists of complex cations [Ni(en)3]2+ and complex anions [Ag(CN)2]−. Complex II crystallizes in the space group I2/m, a = 0.9150(3), b = 1.3308(4), c = 0.6442(2) nm, β = 95.80(3)°, Dm = 2.14(1), Dc = 2.15 gcm−3, Z = 2, R = 0.0334. Its crystal structure consists of infinite, positively charged chains of the [-NCAgCNZn- (en)2]nn+ type and isolated [Ag(CN)2]− anions. The atoms of Ag are positioned parallely to the z axis and the AgAg distance is equal to 0.3221(2) nm. 相似文献
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《Inorganica chimica acta》1988,145(1):91-98
The reaction between [(R-DAB)Rh(PR3)2]+ and molecular hydrogen produces cationic cis-dihydride complexes of Rh(III), of general formula [RhH2(R-DAB)(PR3)2]X. They are stable in air, 1:1 conductors and have been characterized by 1H NMR, 31P NMR, IR and elemental analysis. The tertiary phosphines employed were: PPh3, P(p-C6H4F)3, PMePh2, PEt3, and the R-DAB ligands (RN:CR′CR′:NR)1, Ph-DAB, c-Hex-DAB, NH2-DAB(CH3,CH3), t-but-DAB.The structure of [RhH2(c-Hex-DAB){P(p-C6H4F)3}2]ClO4 has been determined by an X-ray diffraction study. Crystals are orthorhombic, space group Pbnm. Unit cell parameters are: a = 13.032(1), b = 18.166(2), c = 21.449(2) Å, Z = 4, R = 0.081, Rw = 0.082 for 2906 reflections, with I> 3σ(I) the rhodium atom is octahedrally coordinated with the two hydride-hydrogens and c-Hex-DAB in the equatorial plane; the two phosphine ligands are in an axial position bent towards the hydrogens making an angle of 164.9(4)°. 相似文献
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Di-μ-azido-bis[azido(2-aminopyridine)aquo]dicopper(II), [Cu(2-ampy)(N3)2(H2O)]2, was synthesized and characterized by X-ray crystallography. The crystals are triclinic, space group P, with a = 7.142(1), b = 7.812(1), c = 9.727(1) Å, a = 96.52(1), β = 95.52(1), γ = 113.47(1)°, and Z = 1. The structure was refined to RF = 0.030 for 1960 observed MoKα diffractometer data. The dimeric molecule, which possesses a crystallographic inversion center, contains both terminal and μ(1)-bridging azido groups. Each copper(II) atom is further coordinated by a 2-aminopyridine ligand (via its ring N atom) and a water molecule to give a distorted square pyramid, with the metal atom raised by 0.17 Å above the N4 basal plane [CuN (ring) = 2.001(2), CuN (azide) = 1.962(3)–2.018(2) Å] towards the apical aquo ligand [CuO = 2.371(2) Å]. Each water molecule forms an intramolecular O?HN (amine) acceptor hydrogen bond, and is linked by two OH?N (terminal azide) intermolecular donor hydrogen bonds to adjacent dimeric complexes to yield a layer structure parallel to (001). Infrared and electronic spectral data are presented and discussed. 相似文献
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K.K. Sarker S. Saha Halder T.K. Mondal P.K. Nanda C. Sinha 《Inorganica chimica acta》2010,363(12):2955-623
Reaction of Cu(ClO4)2·6H2O, SRaaiNR′ (1-alkyl-2-[(o-thioalkyl)phenylazo]imidazole) and NH4SCN (1:1:2 mol ratio) affords distorted square pyramidal, [CuII(SRaaiNR′)(SCN)2] (3) compound while identical reaction with [Cu(MeCN)4](ClO4) yields -SCN- bridged coordination polymer, [CuI(SRaaiNR′)(SCN)]n (4). These two redox states [CuII and CuI] are interconvertible; reduction of [CuII(SRaaiNR′)(SCN)2] by ascorbic acid yields [CuI(SRaaiNR′)(SCN)]n while the oxidation of [CuI(SRaaiNR′)(SCN)]n by H2O2 in presence of excess NH4SCN affords [CuII(SRaaiNR′)(SCN)2]. They are structurally confirmed by single crystal X-ray diffraction study. Cyclic voltammogram of the complexes show Cu(II)/Cu(I) redox couple at ∼0.4 V and azo reductions at negative to SCE. UV light irradiation in MeCN solution of [CuI(SRaaiNR′)(SCN)]n (4) show trans-to-cis isomerisation of coordinated azoimidazole. The reverse transformation, cis-to-trans, is very slow with visible light irradiation while the process is thermally accessible. Quantum yields (?t→c) of trans-to-cis isomerisation are calculated and free ligands show higher ? than their Cu(I) complexes. The activation energy (Ea) of cis-to-trans isomerisation is calculated by controlled temperature experiment. Copper(II) complexes, 3, do not show photochromism. DFT and TDDFT calculation of representative complexes have been used to determine the composition and energy of molecular levels and results have been used to explain the solution spectra, photochromism and redox properties of the complexes. 相似文献
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H. Noel 《Inorganica chimica acta》1985,109(3):205-207
The crystal structure of UTe5 (a = 17.915(5), b = 10.407(3), c = 4.220(2) Å, Pnma, Pn21a, Z =4) was refined from 822 intensities with I>3σ(I) to a conventional R factor of 0.060. The uranium coordination polyhedron is a three capped tellurium trigonal prism, and all the Te atoms are involved in TeTe bonds. The structure is built up with infinite chains of prisms stacked in the direction. The chains are linked into (b, c) layers by a single Te atom which exhibits some positional disorder. 相似文献
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《Inorganica chimica acta》1988,144(2):193-199
Addition of 1,2-W2Cl2(NMe2)4(W≡W) to a toluene slurry of LiCH(SiMe3)2(2 equiv) results in the formation of 1,2-W2[CH(SiMe3)2]2(NMe2)4(W≡W) (I) in 79% isolated yield. Compound I has been characterized by 1H and 13C NMR, IR, elemental analysis and single-crystal X-ray diffraction. The molecule exists exclusively in the gauche conformation in solution and in the solid state with WW = 2.320(1) Å. Compound I is very sterically encumbered as evidenced by: (1) large WWC angles, 110°, at the disyl ligand; (2) skewing of the NC2 planes of the NMe2 ligands off the WW vector; (3) anomalously large barriers to WNM2 bond rotation in solution; (4) the inertness of I towards CO2 and alcohols. However, compound I reacts with acetic anhydride to form 1,2-W2[CH(SiMe3)2]2(O2CMe)4(W≡W) (II) in 31% isolated yield. Compound II has been characterized by 1H and 13C NMR, IR, and elemental analysis. The mechanistic implications of these studies with regard to alcoholysis and CO2 insertion reactions of other 1,2-W2R2(NMe2)4 compounds are discussed. Crystal data for 1,2-W2[CH(SiMe3)2]2(NMe2)4 at −140°C: space group P21/n, a = 12.555(3), b = 18.699(5), c = 15.214(4) Å, β = 95.24(1)° and Z = 4. 相似文献