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1.
The crystal and molecular structure of hexaphenylditin selenide (C6H5)3SnSeSn(G6H5)3 was determined by X-ray diffraction data and was refined to R 0.055. The compound is monoclinic, space group P21, with a 9.950(4), b 18.650(7), c 18.066(6) Å, β 106.81(4)°, Z 4. The two molecules in the asymmetric unit differ slightly in their conformations, both having approximate C2 symmetry. Bond lengths and angles are: SnSe 2.526 (2.521(3) ? 2.538(3)) Å; SnC 2.138 (2.107(16)?2.168(19)) Å; SnSeSn 103.4(1)°, 105.2(1)°. There are only slight angular distortions at the SnSeC3 tetrahedra (SeSnC angles: 104.3(5)?114.8(4)°). The bond data indicate essentially single bonds around the Sn atoms. 相似文献
2.
Kim Henrick Mary McPartlin Glen B. Deacon Roderic J. Phillips 《Journal of organometallic chemistry》1980,204(3):287-294
An X-ray crystallographic study has shown that the complex (C6H5)2TlO2CC6F5(OPPh3) has a dimeric structure with unsymmetrical pentafluorobenzoate bridging (TlO 2.531 and 2.789 Å) but an exact crystallographic centre of symmetry. The pentafluorobenzoate groups are also unsymmetrically chelated to thallium (TlO 2.389 and 2.531 Å.), which overall has irregular six coordination. 相似文献
3.
A.A. Pasynskii I.L. Eremenko Yu.V. Rakitin V.M. Novotortsev V.T. Kalinnikov G.G. Aleksandrov Yu.T. Struchkov 《Journal of organometallic chemistry》1979,165(1):57-64
The binuclear complex (C5H5)2Cr2(S)(SCMe3)2 was prepared by refluxing a solution of chromocene and t-butylmercaptane in heptane. The structure of the product was determined by single crystal X-ray diffraction. The chronium atoms are linked by a sulphide bridge (SCr 2.24 Å;, <CrSCr 74.1° and two SCMe3 bridges (CrS 2.38 Å;, <CrSCr 68.3–69.3°). The two cyclopentadienyl ligands (CC 1.41 Å;, CrC 2.23 Å;) are in apical positions, their ring planes being parallel to each other. The complex is an antiferromagnet (?2J cm?1) despite the small CrSCr angles and short chromiumchromium distance (2.689 Å;) indicative of strong CrCr bonding. 相似文献
4.
A.G. Osborne A.J. Blake R.E. Hollands R.F. Bryan S. Lockhart 《Journal of organometallic chemistry》1985,287(1):39-47
A series of [3]ferrocenophanes of general formula Fe(C5H4X)2YCl2 and the spiro compounds [Fe(C5H4X)2]2Ge (X = S, Se; Y = Ge, Sn) have been prepared by the reaction of ferrocene 1,1′-dithiol and ferrocene 1,1′-diselenol with tetrahalides of germanium and tin. Spectroscopic properties of the compounds are reported. In solution, the compounds are fluxional by a bridge reversal process. The crystal structure of 1,3-diselena-2,2-dichlorogermyl-[3]ferrocenophane at 163 K. has been determined by X-ray diffraction methods. At that temperature, crystals have space group P21/n with a 6.222(3), b 16.156(13), c 12.968(4) Å, β 97.53(1)° and Z = 4. Least-squares refinement gave R = 0.033 for 2834 unique significant reflections whose intensities were measured by counter diffractometry. The two SeGe bond lengths are 2.323 and 2.325(1) Å, with GeCl 2.148 and 2.161(1) Å. The SeGeSe bond angle is 118.2(1)°, ClGeCl 104.7(1)°, and SeGeCl angles range from 106.2 to 109.8(1)°. The SeC bond lengths are 1.901 and 1.904(5) Å, with CSeGe angles of 95.8 and 96.5(2)°. The cyclopentadienyl rings are in an eclipsed conformation with a mean twist angle of 2.7°, and are inclined to one another at 6.1°. The Se atoms are displaced from the ring planes by 0.17 and 0.20 Å yielding a non-bonded intramolecular Se…Se contact of 3.99 Å. 相似文献
5.
《Journal of organometallic chemistry》1987,323(2):247-259
The reaction of trans-MeOIr(CO)(PPh3)2 with TCNE (tetracyanoethylene) gives rise to the stable adduct MeOIr(CO)(PPh3)2(TCNE), the structure of which has been determined via a single-crystal X-ray diffraction study. This complex crystallizes in the centrosymmetric orthorhombic space group Pbca (D152h; No. 61) with a 17.806(4), b 20.769(4), c 20.589(6) Å, V 7614(3) Å3 and Z = 8. Diffraction data (Mo-Kα, 2θ = 5–45°) were collected on a Syntex P21 automated four-circle diffractometer and the structure was solved and refined to RF 6.2% for 3502 data with |F0| > 3σ(|F0|) (RF 4.3% for those 2775 data with |F0| > 6 σ(|F0|)). The central iridium atom has a distorted trigonal bipyramidal coordination geometry in which the methoxy group (Ir-OMe 2.057(8) Å) and carbonyl ligand (Ir-CO 1.897(14) Å) occupy axial sites with ∠MeOIrCO 174.7(4)°. The two triphenylphosphine ligands occupy equatorial sites (IrP(1) 2.399(3), IrP(2) 2.390(3) Å, ∠P(1)IrP(2) 110.32(11)° and the TCNE ligand is linked in an η2 “face-on” fashion with the olefinic bond parallel to the equatorial coordination plane (IrC(4) 2.176(10), IrC(7) 2.160(12) Å) and lengthened substantially from its value in the free olefin (C(4)C(7) 1.539(17) Å). 相似文献
6.
The structure of (Ph3SiN)2C has been determined by single crystal X-ray diffraction. The structure was solved by direct methods and refined to R = 0.071 for 593 independent diffractometer data. The crystals are rhombohedral, R with a = b = c 18.201(20) Å, α = β = γ = 48.82(2)°, and Z = 4. The three crystallographically independent molecules each have linear SiNCNSi chains lying along the crystallographic threefold axes; in two of the molecules the central carbon atom lies on a centre of symmetry. Principal mean bond lengths and angles are: Si, 1.696(25); SiC, 1.846(20); NC, 1.164(30); CC, 1.387(14) Å; CSi, 108.2(6); and CSiC, 110.8(6)°. 相似文献
7.
C5H5Co(PMe3)CS2 (IV) is formed in practically quantitative yield in the reaction of C5H5Co(PMe3)2 (I) or the heterobinuclear complex C5H5(PMe3)Co(CO)2Mn(CO)C5H4Me (III) with CS2. The crystal structure shows that the carbon disulfide bonds as a dihapto ligand through the carbon and one sulfur atom (S(2)) (CoC = 1.89, CoS(2) = 2.24 Å, S(2)CS(1) = 141.2°). The two CS bond lengths in IV (CS(2) = 1.68, CS(1) =1.60 Å) are greater than in free CS2 (1.554Å) which is in agreement with the strong π-acceptor character of h2-CS2 as shown in the spectroscopic data. IV reacts with Cr(CO)5THF and C5H5Mn(CO)2THF to give the complexes C5H5(PMe3)Co(SCS)Cr(CO)5 (V) and C5H5(PMe3)Co(SCS)Mn(CO)2C5H5 (VI) respectively, in which the sulfur atom S(1) that is not bound to cobalt coordinates to the 16-electron fragments Cr(CO)5 and Mn(CO)2C5H5. The spectroscopic data of IV, V and VI are discussed. 相似文献
8.
The molecular structure of the title compounds have been investigated by gas-phase electron diffraction. Both molecules exist as about equal amounts of the two gauche conformers. There is no evidence for the presence of a syn conformer, but small amounts of this form cannot be excluded. Some of the important distance (ra) and angle (∠α) parameters for 1,1-dichloro-2-bromomethyl-cyclopropane are: r(CH) = 1.095(19) Å, r(C1C2) = 1.476(11) Å, r(C2C3) = 1.517(31) Å, r(CCH2Br) = 1.543(32) Å, r(CCl) = 1.752(6) Å, r(CBr) = 1.950(13) Å, ∠CCBr = 110.5(1.9)°, ∠ClCCl = 111.9(6)°, ∠CCC = 117.5(1.3)°, σ1 (CC torsion angle between CBr and the three-membered ring for gauche-1) = 116.2(5.6)°, σ2 = −132.7(7.6). For 1,1-dichloro-2-cyanomethyl-cyclopropane the parameter values are: r(CH) = 1.101(16) Å, r(C1C2) = 1.498(9) Å, r(C2C3) = 1.544(21) Å, r(C2C4) = 1.497(33) Å, r(CCN) = 1.466(26) Å, r(CN) = 1.165(8) Å, r(CCl) = 1.754(5) Å, ∠CCCN = 113.7(2.0)°, ∠CCC = 122.8(1.6)°, ClCCl = 112.5(4)°, σ1 = 113(13)°, σ2 = −124(10)°. 相似文献
9.
Rafael Usón Antonio Laguna María U. De La Orden R.V. Parish Laila S. Moore 《Journal of organometallic chemistry》1985,282(1):145-148
Addition of a bidentate ligand (LL = 1,10-phenanthroline, o-phenylenebis(dimethylarsine)) to solutions of Au(C6F5)X2(tht) (X = Cl, Br; tht = tetrahydrothiophene) leads to potentially five-coordinate gold(III) derivatives. 197Au Mössbauer spectroscopy points, however, to four-coordinate square-planar complexes with a weak penta-coordination in the phen-containing derivatives. The complexes react with AgClO4 to give four-coordinate cationic complexes of the types [Au(C5F5)X(LL)]ClO4 or [Au(C6F5)(PPh3)(LL)](ClO4)2. 相似文献
10.
R. M. Bellabarba M. Nieuwenhuyzen G. C. Saunders 《Journal of Structural Chemistry》2013,54(2):471-473
The salt (η5-pentamethylcyclopentadienyl){bis(pentafluorophenyl)thiomethylphenylphosphine-κ2 S,P)chloroiridium(III) tetrafluoroborate, [(η5-C5Me5)IrCl{κ2 S,P-(C6F5)2PC6H4SMe-2}]BF4, crystallizes as a conglomerate in the orthorhombic crystal system in space group P212121 with unit cell parameters a = 9.9621(9) Å, b = 16.7793(15) Å, c = 18.5040(16) Å, V = 3093.1(5) Å3, Z = 4, d calc = 2.014 g·cm?3. The structure of the S Ir, S S stereoisomer reveals three-legged piano stool geometry about Ir, with Cp*-Ir, Ir-P, Ir-S and Ir-Cl distances of 1.847(5) Å, 2.2791(14) Å, 2.3451(13) Å, and 2.3840(12) Å respectively. 相似文献
11.
Four organometallic palladium(IV) complexes: Cl2(C6F5)2Pd(LL) (LL being a bidentate nitrogen-donor ligand) have been prepared by the oxidative addition of chlorine to the corresponding bis(pentafluorophenyl)palladium(II) complexes, (C6F5)2Pd(LL). Some of their properties are described. 相似文献
12.
B. V. Bukvetskii T. V. Sedakova A. G. Mirochnik 《Russian Journal of Coordination Chemistry》2010,36(9):651-656
The crystal structure of (C2H5)4N)2TeCl6 was determined by X-ray diffraction (a = 14.130(2) Å, b = 14.547(2)Å, c = 13.296(2)Å, β= 90.356(3)°; space group C2/c, Z = 4, ρ(calcd) = 1.387 g/cm3). The crystal structure is composed of the [TeCl6]2? anions and tetraethylammonium cations ((C2H5)4N)+. The electronic and geometric aspects that determine the spectral luminescence and thermochromic properties of the complex are discussed. 相似文献
13.
14.
B. Cetinkaya P.B. Hitchcock M.F. Lappert S. Torroni J.L. Atwood W.E. Hunter M.J. Zaworotko 《Journal of organometallic chemistry》1980,188(3):C31-C35
The 2,6-di-t-butyl-4-methylphenoxo ligand (ArO?) is ambidentate, giving rise to the O-bonded 15-electron d1 [Ti(η-C5H5)2OAr] and the η5 -[C(2)-C(6)]-bonded 18-electron d8 complex [Rh(ArO-η5)(PPh3)2], obtained from [{Ti(η-C5H5)2Cl}2]-LiO Ar and [Rh{N(SiMe3)2}(PPh3)2]-ArOH, respectively; the average TiC(η) distance is 2.362(10) Å, TiO 1.892(2) Å, and O:C(of Ar) 1.352(3) Å, and TiOC 142.3(2)°; in the RhI complex, C(2)C(6) are coplanar (with CC(av.) 1.38(2) Å). C(1)O 1.28 Å, and Rh to C(2) C(6) bond lengthsare in the range 2.19–2.65 Å. 相似文献
15.
《Journal of organometallic chemistry》1986,301(3):375-384
The complex [uRh(oq)Br(P(o-Cu6F4)Ph2)(H2O)]2 is obtained by refluxing a solution of Rh(oq)(CO)(P(o-BrC6F4)Ph2) (oq = 8-oxyquinolinate) in toluene. The structure of this compound has been determined by X-ray diffraction and refined to R = 0.061 and Rw = 0.065 factors. The cell has monoclinic symmetry, space group P21/n; a 19.513(2), b 17.049(1), c 16.898(1) Å and β 99.69(1)°. The structure consists of two independent Rh(oq)Br(P(o-C6F4)Ph2)H2O) units linked by hydrogen bonds between the coordinated water molecules and oq ligands to form a distorted boat (six atom ring of junction between the two units). In each unit the metal atom has a distorted octahedral coordination, with a four-atom metallocyclic ring (uRhPCCu) with CRhP and RhPC angles 69.3(2) and 85.3(3)°, respectively, in one unit, and 70.0(2) and 81.1(2)° in the other. The water molecule is readily displaced by a variety of phosphorus donor ligands to form the complexes uRh(oq)Br(P(o-Cu6F4)Ph2)P′, P′ = PPh3, P(p-CH3C6H4)3 and P(OCH3)3, in which the P atoms are in trans-dispositions. 相似文献
16.
Gerhard Thiele Günther Liehr Ekkehard Lindner 《Journal of organometallic chemistry》1974,70(3):427-435
The molecular structure of [(C6H5)3P]2Pd(C3H4) has been determined from three-dimensional X-ray diffraction data. The crystal belongs to the triclinic system, space group P, with two formula units in a cell of dimensions: a = 19.475(2), b = 10.204(2), c = 18.341(2) Å, α = 108.46(2), β = 85.46(1), and γ = 118.80(1)°.One of the olefinic bonds of allene is coordinated to the palladium atom: PdC(1) = 2.118(9) and PdC(2) = 2.067(8) Å. The coordinated allene is no longer linear, the C(1)C(2)C(3) angle being 148.3(8)°. The C(1)C(2) distance is 1.401(11) Å, whereas the uncoordinated bond remains unchanged [C(2)C(3) = 1.304(12) Å]. The Pd, P(1), P(2), C(1) and C(2) atoms lie almost in the same plane. 相似文献
17.
(C6F5)3Sb has been found to react with interhalogens and halo-pseudohalogens, IX(X = Cl, Br, N3 and NCO), pseudohalogen (SCN), and elemental sulphur to give oxidative addition products (I–VI). (C6F5)3SbS(VI) may also be prepared by the reaction of (C6F5)3SbCl2 with H2S. Metathetical reactions of (C6F5)3SbCl2 with appropriate metallic salts yield covalent pentacoordinate disubstituted products (V, VII–XII) of the general formula, (C6F5)3SbY2 (Y = NCS, NCO, ?ONCMe2, ?ONCMePh O and p-NO2C6H4OCO). Treatment of (C6F5)3SbCl2 with aqueous NaN3 gives the binuclear oxo-bridge compound, [(C6F5)3SbOSb(C6F5)3](N3)2·(III) and (IV) are also accessible by displacement reaction of (I) or (II) with the corresponding metallic salt. Molecular weight, conductance measurements, and IR spectra on the new organoantimony(V) derivatives have been obtained.Reductive cleavage reactions of (C6F5)3SbS with hexaaryldileads, Ar6Pb2(Ar = Phenyl, p-tolyl) produce (C6F5)3Sb and the corresponding bis(triaryllead) sulphide but treatment of (C6F5)3SbX2(X = NCO, Cl) with Ar6Pb2 gave Ar4Pb and Ar2PbX2 together with (C6F5)3Sb.(C6F5)3SbCl2 and bis(triorganotin)sulphides undergo exchange of anionic groups. 相似文献
18.
Edward J. Miller Arnold L. Rheingold Thomas B. Brill 《Journal of organometallic chemistry》1984,273(3):377-383
[η5-C5(CH3)5]Co(O2C6H4) crystallizes in the orthorhombic space group Pnma with a 12.942(4), b 12.902(4), c 8.543(3) Å, V 1426(1) Å3, and Z = 4. Least-squares refinement of 1688 independent observed reflections, F(obs) ? 2.5σ(Fobs), gives RF 3.79 and RwF 3.72%. The cyclopentadienyl ring contains two short (1.412(3) Å) and three longer (〈av〉 1.430(4) Å) CC bond lenghts, consistent with a slight preference for diolefin bonding. The O2C6H4 fragment is best described as a catecholate with a CO bond distance of 1.338(3), and a CoO distance of 1.837(2) Å. 相似文献
19.
Fausto Calderazzo Ishwerlal P. Mavani Dario Vitali Ivan Bernal James D. Korp Jerry L. Atwood 《Journal of organometallic chemistry》1978,160(1):207-222
Reactions of the tetrahydrofuran adduct Re2Br2(CO)6(THF)2 with some phosphorous- and nitrogen-containing donors under mild conditions are reported, which led to the formation of substituted products of tricarbonylrhenium(I). Bromide abstraction from the THF adduct by secondary amines and CS2 produced the dithiocarbamato derivatives Re(S2CNR2)(CO)3(HNR2) whose behaviour in solution with CO was also investigated. Mass spectral data for some of the substituted products have been measured. The title compound crystallizes in the space group P21/n with cell constants a = 8.661(2), b = 11.251(3), c = 11.424(3) Å and β = 110.36(2)°, U = 1043.67 Å3 and Dcalc = 2.686 g cm?3, Z = 2. The molecule consists of a planar Re2Br2 moiety, as demanded by symmetry. The two THF groups are on opposite sides of this plane and the three CO groups around each rhenium atom are arranged in a fac arrangement. The unique ReBr distances are 2.642(5) and 2.644(4)Å, while the ReO distance is 2.129(31) Å. The ReBrRe and BrReBr angles are 97.3(2) and 82.7(1)°, respectively. The Re?Re nonbonding distance is 3.967(3) Å. The THF ligands consist of a nearly planar C4 fragment (maximum deviation from planarity 0.06 Å), while the oxygen is 0.348 Å out of that plane, the angle defined by the C4 plane and the COC fragment of the THF ligand being 24.99°. Final values of the discrepancy indices are R(F) = 0.074 and Rw(F) = 0.095. 相似文献
20.
M.David Curtis John Greene William M. Butler 《Journal of organometallic chemistry》1979,164(3):371-380
The structure of the cyclo-metalladisiloxane, Me2SiOSiMe2Ir(H)(CO)(PPh3)2, has been determined by single crystal X-ray diffraction using Mo-Kα radiation. Data were collected to 20 = 45 ° giving 6060 unique reflections,of which 4582 had I ?3σ(I). The latter were used in the full-matrix refinement. Crystallographic data: space group, P; cell constants: 12.604(7),12.470(4), 15.821(6) Å, 66.93(6)°, 105.34(7)°, 112.41(8)°;V 2095(3) Å3; p(obs) 1.45 g/cm3; p(calc) 1.46g/cm3 (Z=2). The asymmetric unit consists of one iridium complex and one molecule of ethanol of salvation. The structure was solved by standard heavy atom methods and refined with all non-hydrogen atoms anisotrophic to final R factors, R1 0.034 and R2 0.042. The iridium metallocycle has approximate Cs symmetry with the mirror plane passing through the four-membered IrSiOSi ring. The average IrP, IrSi and SiO bond lengths are 2.38, 2.41, and 1.68 Å, respectively. The IrCO and CO bond lengths are 1.903(8) and 1.133(8). The H atom bonded to Ir was not located.The Ir atom is raised out of the basal, P2Si2 plane toward the carbonyl by about 0.26 Å. The most striking feature of the structure is the strain apparent in the four-membered ring. The internal angels are: 64.7 (SiIrSi), 96.8 (IrSiO), 97.8 (IrSiO), and 99.8 (SiOSi). In an unstrained molecule, the SiOSi angle is normally in the 130–150° range. It is proposed that the strain in the ring is consistent with the catalytic activity of the metallocycle. 相似文献