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1.
V. V. Sharutin I. V. Egorova O. K. Sharutina E. A. Boyarkina 《Russian Journal of Coordination Chemistry》2008,34(6):461-465
The complexes [Ph3PMe] 2 + [BiI5]2? (I) and [Ph3PMe] 2 + [BiI5 · C 5H5N]2? · C 5H5N (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-CPh 1.779(2), P-CMe 1.793(1) Å. The Bi atom in the anion of complex I has an ideal trigonal-bipyramidal coordination polyhedron (Bi-Ieq 3.0031(4), Bi-Ieq 3.0485(5) Å). The crystal of complex II consists of the anions [BiI5 · C 5H5N]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-CPh 1.785(3)–1.792(3), P-CMe 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
2.
3.
《Journal of organometallic chemistry》1986,315(1):105-112
Neutral hydrido complexes [ML]ClH(PPh3)3 ([ML] = Ru(CO), Os(CO) and Ir(Cl)] react with thionitrosodimethylamine, Me2NNS, to give [ML]ClH-(SNNMe2)(PPh3)2 with H trans to Me2NNS, while the hydrido cations cis,trans-[[ML]H(SNNMe2)2(PPh3)2]+ are obtained from Me2NNS and [Ru(NCMe)2(CO)-(PPh3)2]+, [OsH(OH2)(CO)(PPh3)3]+ and [IrClH(NCMe)2(PPh3)2]+, respectively. The coordinatively unsaturated aryl complexes [ML′]Cl(p-tolyl)(PPh3)2 ([ML′]Ru(CO), Os(CO) and Os(CS)) coordinate one molecule of Me2NNS to give [ML′]Cl(p-tolyl)(SNNMe2)(PPh3)2, the chloride ligands of which are labile. Spectroscopic data suggest that in all these complexes the Me2NNS ligand adopts a η1(S) coordination mode. 相似文献
4.
LI Zao-YingDepartment of Chemistry Wuhan University Wuhan Hubei ChinaCHE Chi-Ming Department of Chemistry The Hong Kong University Hong Kong 《中国化学》1997,(1)
Oxo(tert-butylimido) or bis(tert-butylimido)osmium(VI) porphyrins Os(Por)(O)(NBut) and Os(Por)(NBut)2, [Por=meso-tetrakis(p-tolyl)porphyrinato (TTP) and meso-tetrakis(4-chlorophe-nyl)porphyrinato (4-Cl-TPP)] were synthesized by air oxidation of bis(tert-butylamme)osmium(II) porphyrins [Os(Por)(H2NBut)2 (Por=TPP, 4-Cl-TPP], depending on whether tert-butylamine is present. The bis(tert-butylamine)ruthenium(II) porphyrins [Ru(Por)(H2NBut)2, Por=TTP, 4-Cl-TPP] can undergo bromine oxidation to give oxo(tert-butylimido)ruthenium(VI) complexes in quantitative yields. All these new complexes were characterized by 1H NMR, UV-Visible and IR spectroscopy. The X-ray crystal structures of Os(TTP)(O)(NBut).EtOH and Os(4-Cl-TPP)(NBut)2 have been determined. Crystal data: for Os(TTP)(O)(NBut).EtOH: monoclinic, space group P21/c, a=1.3546(6) nm, b=2.3180(3) nm, c=1.6817(3) nm, B=90.84(2), V=527.97(1) nm3, Z=4. The Os=O and Os=NBut distances in Os(TTP)(O)(NBut).EtOH are 0.1772(7) nm and 0.1759(9) nm, respectively. The av 相似文献
5.
《Journal of organometallic chemistry》1986,310(2):161-167
The disilazane (Ph2SiNC6F5)2 crystallises from benzene solution with four molecules of solvent in the orthorhombic space group Pnna with a 18.182(6), b 21.480(8) and c 13.631(5) Å, Z = 4. The structure was solved by direct methods and refined by least-squares to R 0.069 for 937 observed reflections. The Si2N2 ring is planar with NSiN and SiNSi angles of 85.2 and 95.5° respectively; the mean SiN distance is 1.755 Å. The C6F5 groups are twisted by ca. 16° from the Si2N2 plane and the benzene molecules are arranged face-on above and below each of the C6F5 groups. There are, in addition, short intermolecular contacts between four fluorines of each C6F5 group and hydrogen atoms from both solvate benzene and the phenyl groups of a symmetry related silazane. Attempts to refine the related (Me2SiNC6F5)2 structure were not successful, probably due to disorder. 相似文献
6.
《Journal of Coordination Chemistry》2012,65(18):3229-3239
Co(II), Cu(II), Zn(II), and Fe(III) complexes of phenylthiourea have been synthesized and characterized by elemental analyses, molar conductivity, magnetic susceptibility, FT-IR, and electronic spectroscopy. The spectroscopic data of the complexes are consistent with four-coordinate geometry for the metal(II) complexes and six-coordinate octahedral for the Fe(III) complex. Single crystal X-ray analysis of the Zn(II) complex revealed distorted tetrahedral geometry around the metal ion with two molecules of phenylthiourea and two acetate ions. The in vitro antibacterial activity of the complexes was studied against six bacterial strains using disc diffusion and broth microdilution methods. The complexes showed selective antibacterial activity against Staphylococcus aureus and Bacillus pumilus when compared to standard antibiotic ampicillin. The minimum inhibitory concentrations of the sensitive compounds are between 0.625 and 5.0 mg mL?1. 相似文献
7.
Batista Alzir A. Wonrath Karen Queiroz Salete L. Porcu Ornella M. Castellano Eduardo E. Barberato Claudio 《Transition Metal Chemistry》2001,26(3):365-368
The compound [RuCl2(CO)(DMA)(PPh3)2] [DMA = dimethylacetamide] was obtained from [RuCl3(PPh3)2-(DMA)] · DMA and CO in DMA. Orange crystals of [RuCl2(CO)(DMA)(PPh3)2] · 1/2CH2Cl2 were isolated by slow evaporation of a CH2Cl2/DMA solution and its structure was determined by single crystal X-ray diffraction. The analogous compounds containing DMF and DMSO were obtained from the precursor ttt-[RuCl2(CO)2(PPh3)2]. Characterization of the other complexes is based on i.r. and n.m.r. spectroscopy, including 31P{1H} data. 相似文献
8.
《Journal of Coordination Chemistry》2012,65(4):550-562
Three new cyano-bridged complexes 1 [Ni(tn)2Ni(CN)4] (tn?=?1,3-diaminopropane), 2 [CuII(dipn)NiII(CN)4], and 3 [Cu(dipn)]6[Co(CN)6]4?·?4H2O (dipn?=?dipropylenetriamine) have been assembled by the templates [Ni(CN)4]2? and [Co(CN)6]3?. 1 consists of a one-dimensional linear chain–Ni(tn)2–NC–Ni(CN)2–CN–Ni(tn)2? in which the Ni(II) centers are linked by two CN groups. One 1-D zigzag chain of 2 is formed with–Ni(2)–C–N–Cu(1)–N–C–linkages. A 2D structure of 3 is formed by an alternate array of [Co(CN)6]3? and [Co][Cu6] units. For 1, there is an overall weak antiferromagnetic interaction between Ni(II) ions through the–NC–Ni–CN–bridges of the diamagnetic [Ni(CN)4]2? anions. 2 exhibits a weak antiferromagnetic exchange interaction between copper(II) ions mediated by [Ni(CN)4]2? diamagnetic bridges. Complex 3 exhibits a weak ferromagnetic interaction between nearest CuII and CuII atoms through–NC–Co–CN–bridges. 相似文献
9.
A. V. Tikhomirova E. V. Peresypkina A. V. Virovets T. G. Cherkasova 《Russian Journal of Inorganic Chemistry》2013,58(5):534-542
The X-ray diffraction study of the crystalline products of the reaction between potassium tetraiodomercurate(II), ?-caprolactam, and lanthanum(III) nitrate at a ratio of 3: 16: 2 in an aqueous solution has shown the presence of the following three new crystalline compounds: [LaCpl8]2[HgI4]3 (I), [LaCpl8][HgI4]I3 (II), and [LaCpl7(H2O)]2[HgI4]2[Hg2I6] (III), where Cpl is ?-caprolactam ?-C6H11NO. Compounds I and II crystallize in tetragonal crystal system, space groups P42/n and $I\bar 4$ , respectively. For compound I, a = 18.59320(10) Å, c = 19.5782(3) Å, V = 6738.32(12) Å3, Z = 2, and ρcalc = 2.067 g/cm3. For compound II, a = 13.2245(10) Å, c = 20.0310(3) Å, V = 3503.17(6) Å3, Z = 2, ρcalc = 2.022 g/cm3. The crystals of compound III are monoclinic (space group P 2 1/n, a = 20.1202(6) Å, b = 14.0569(4) Å, c = 46.3228(12) Å, β = 93.4770(10)°, V = 13077.3(6) Å3, Z = 4, ρcalc = 2.274 g/cm3). [La(Cpl)8]2[Hg2I6]3 (IV), a new double ionic complex salt, has also been synthesized and studied by X-ray diffraction. The crystals of compound IV are triclinic (space group $P\bar 1$ , a = 12.5021(3) Å, b = 14.6436(3) Å, c = 21.4695(4) Å, α = 84.2300(10)°, β = 87.2230(10)°, γ = 74.9970(10)°, V = 3776.30(14) Å3, Z = 1, ρcalc = 2.452 g/cm3). All complexes have a dicrete ionic structure, and the nearest surrounding of a La atom is distorted square-prismatic or trigonal-dodecahedral. The crystal packing of cations is distorted face-centered cubic (I and II) or body-centered cubic (III and IV) with anions located in its cavities. 相似文献
10.
《Journal of organometallic chemistry》1991,417(3):C59-C62
Reaction of [(η6-p-cymene)RuCl(L*)] with AgClO4 in Me2CO gives a perchlorate complex which on subsequent treatment with PPh3, γ-picoline or Cl− yields adducts showing that there can be retention as well as inversion of configuration at the metal centre. The (R)Ru,(SC absolute configurations of the chiral centres in the triphenylphosphine adduct have been established by an X-ray diffraction study [HL*, (S-α-methylbenzylsalicylaldimine]. The CD spectral study reveals that there is an inversion of configuration during formation of the PPh3 adduct. 相似文献
11.
《Journal of organometallic chemistry》1986,304(3):C24-C26
Treatment of cis-[M(C6F5)2(THF)2] (M = Pd, Pt; THF = tetrahydrofuran) with PhCCPh has given the novel bis-acetylene-palladium(II) and -platinum(II) complexes cis-[M(C6F5)2(PhCCPh)2]; these are stable even though there seems to be no significant π-back bonding according to the X-ray structure of the platinum complex. 相似文献
12.
13.
The cluster [Cu4(S5)2(C5H5N)4]·S8 with cage structure has been obtained by reaction of copper powder with sulfur and K2S
x
in pyridine, and its structure was determined by X-ray crystallography. The crystal data for the title compound: triclinic, P
(No. 2),Z = 2,a = 11.818(4) Å,b = 13.155(3) Å,c = 14.177(4) Å, = 93.79(2)°, = 96.68(2)°, = 115.76(2)°,V = 1954.52(1) Å3. The structure was refined toR = 0.038R
w
= 0.053) for 6444 data withI > 3.0(I).Dedicated to Professor Jiaxi Lu on the occasion of his 80th birthday. 相似文献
14.
《Journal of organometallic chemistry》1988,356(1):C29-C31
The dimer [Ru(η6-C16H16)Cl2]2 reacts with ligands L (L PMe2Ph, PPh3, C5H5N) to give both neutral monomeric [Ru(η6-C16H16)Cl2L] and cationic monomeric [Ru(η6-C16H16)ClL2]+ products. One example, [Ru(η6-C16H16)Cl(C5H5N)2]-[PF6], has been characterised by X-ray crystallography. Reaction with the bidentate ligand 2,2′-bipyridyl gives the mononuclear cation [Ru(η6-C16H16)Cl(bipy)]+, isolated as its [BPh4]− salt, whereas reaction with OMe− or OEt− gives dinuclear products [Ru(η6-C16H16)2(OR)3]+. 相似文献
15.
《Journal of organometallic chemistry》1990,381(2):C47-C51
[Fe(η-C5Me5)(CO)2(OH2)]+ BF4- (2a) reacts with alkenes and alkynes to give the new complexes [Fe(η-C5Me5)(CO)2(alkene)]+ BF4- and [Fe(η-C5Me5)(CO)2(alkyne)]+ BF4-. The crystal structure of the ruthenium analogue [Ru(η-C5Me5)(CO)2(OH2)]+ CF3SO3- (2b) is described. 相似文献
16.
《Polyhedron》1999,18(26):3553-3558
[CrX3(thf)3] (X=Cl or Br) reacts with L (L=L1–L3 or Ph2[14]aneP2S2) (L1=Ph2P(CH2)2S(CH2)2S(CH2)2PPh2, L2=Ph2P(CH2)2S(CH2)3S(CH2)2PPh2, L3=Ph2P(CH2)2S(o-C6H4)S(CH2)2PPh2, Ph2[14]aneP2S2=4,8-diphenyl-1,11-dithia-4,8-diphosphacyclotetradecane) and TlPF6 in MeNO2 solution to yield the distorted octahedral complexes [CrX2(L)]PF6 as green coloured solids in high yield. UV/visible spectroscopy suggests that these are cis-dihalo species and they have also been characterised by IR spectroscopy, electrospray mass spectrometry and microanalyses. The Co(III) analogues [CoX2(L)]+ are readily prepared in a two-stage reaction, involving treatment of CoX2·6H2O with L (L=L1–L3) and NH4PF6 in EtOH solution to give a green/brown solid, followed by halogen oxidation of this product in CH2Cl2 solution using X2/CCl4, to give the final products as brown coloured solids. A mixture of PF6− and [CoX4]2− anions are present in the final Co(III) compounds in varying ratios. Crystal structures of [CoCl2(L2)]2[CoCl4]·4H2O and [CoCl2(L3)]PF6·CH2Cl2 confirm tetradentate P2S2 coordination of L in each case, with mutually cis halogens completing the distorted octahedral geometry. In both cases the complex cation adopts the cis-α form in the solid state and this is also consistent with the solution 31P{1H} NMR spectroscopic data. 59Co NMR spectroscopy reveals a very broad single resonance at ≈3200 ppm for these species. 相似文献
17.
Pandey KK 《The journal of physical chemistry. A》2011,115(30):8578-8585
Density functional theory calculations have been performed for the dimethylgallyl complexes of iron, ruthenium, and osmium [(η(5)-C(5)H(5))(L)(2)M(GaMe(2)] (M = Fe, Ru, Os; L = CO, PMe(3)) at the DFT/BP86/TZ2P/ZORA level of theory. The calculated geometry of the iron complex [(η(5)-C(5)H(5))(CO)(2)Fe(GaMe(2))] is in excellent agreement with structurally characterized complex [(η(5)-C(5)H(5))(CO)(2)Fe(Ga(t)Bu(2))]. The Pauling bond order of the optimized structures shows that the M-Ga bonds in these complexes are nearly M-Ga single bond. Upon going from M = Fe to M = Os, the calculated M-Ga bond distance increases, while on substitution of the CO ligand by PMe(3), the calculated M-Ga bond distances decrease. The π-bonding component of the total orbital contribution is significantly smaller than that of σ-bonding. Thus, in these complexes the GaX(2) ligand behaves predominantly as a σ-donor. The contributions of the electrostatic interaction terms ΔE(elstat) are significantly smaller in all gallyl complexes than the covalent bonding ΔE(orb) term. The absolute values of the ΔE(Pauli), ΔE(int), and ΔE(elstat) contributions to the M-Ga bonds increases in both sets of complexes via the order Fe < Ru < Os. The Ga-C(CO) and Ga-P bond distances are smaller than the sum of van der Waal radii and, thus, suggest the presence of weak intermolecular Ga-C(CO) and Ga-P interactions. 相似文献
18.
V. V. Sharutin A. P. Pakusina O. K. Sharutina I. V. Egorova M. A. Pushilin 《Russian Journal of Coordination Chemistry》2007,33(2):96-103
The reaction of pentaphenylantimony with mercury iodide affords the ionic complex [Ph4Sb] 2 + [Hg2I6]2?·Ph2Hg (I). The [Ph4Sb] 2 + [Hg2I6]2? (II) and [Ph4Sb] 2 + [Cd2I6]2? (III) complexes are synthesized from tetraphenylantimony iodide and mercury and cadmium iodides. The [Ph4Sb] 2 + [Hg4I10]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 [Ph4Sb]+ cations of complex I has virtually ideal tetrahedral coordination (the CSbC angles are 108.09°–109.64°). In the central square fragment Hg2I2 of the [Hg2I6]2? anion, the Hg-Ibr bond lengths are 2.825 and 3.075 Å, and the terminal iodine atoms are more strongly bonded to the mercury atoms (Hg-Iterm 2.691 and 2.700 Å). The [Cd2I6]2? anion in complex III has a similar structure (the Cd-Ibridg and Cd-Iterm 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
19.
《Journal of organometallic chemistry》2003,665(1-2):101-106
Treatment of K(P3C2tBu2) with Cu2I2 and PMe3 gave the binuclear complex [Cu(PMe3)2(μ-P3C2tBu2)2Cu(PMe3)2] via the isolated intermediate compound [Cu(PMe3)2(μ-P3C2tBu2)(μ-I)Cu(PMe3)2]. The reaction of K(P3C2tBu2) with [AuCl(PEt3)] on the otherhand gave the cation:anion complex [Au(PEt3)2][Au(η1-P3C2tBu2)2]. All complexes were fully characterised by multinuclear spectroscopy and single crystal X-ray diffraction studies. 相似文献
20.
《Journal of Coordination Chemistry》2012,65(4):618-626
Two supramolecular complexes, {{Ni(H2O)(phen)2[Au(CN)2]}[Au(CN)2]?·?1.5H2O} n (1) (phen?=?1,10-phenanthroline) and [H2teta][Au2(CN)4]?·?2H2O (2) (teta?=?5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene) have been synthesized and structurally characterized. Complex 1 was a one-dimensional infinite chain constructed by [Au(CN)2]? building blocks. In complex 2, there are one cation, one anion, and two water molecules in the asymmetric unit. The two complexes are interconnected through a combination of aurophilic attractions and hydrogen bonds and formed into 3D supramolecular structures. The aqueous solutions of 1 and 2 display interesting luminescence at room temperature. 相似文献