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1.
Diethyl telludi reacts with both copper(I) and copper(II) chloride to give polymeric chloro(diethyl telluride)copper(I) which is characterised by elemental analysis and by its IR and 1H NMR spectra. X-ray analysis shows that its structure contains infinite sheets in which two Et2Te ligands are bridged between two di-μ-chlorodicopper(I) cores. The CuTe distances are 2.535(1) and 2.625(1) Å and the geometry around both copper and tellurium atoms in that of a distorted tetrahedron. The angels around copper range from 95.5(1) to 122.6(1)° and around tellurium from 95.6(1) to 130.5(1)°. The crystals are monoclinic, C2/c with a 19.761(11), b 7.114(4), c 11.76(7) Å, β 111.17(1)°, V 1542(2) Å3, ?calcd 2.45 ?obsd 2.43 g/cm3Z = 8 for 1220 unique “observed” reflections and the structure refined to an R index of 0.0243. 相似文献
2.
The crystal structures of C8H8TeMe+ BPh4? (I) and C4H8TePh+ BPh4? (II) have been determined from three-dimensional X-ray counter data.I is monoclinic, space group P21/n with a 9.175(1), b 17.402(3), c 16.998(3) Å, β 98.92(6)°, Z = 4, R = 5.1% for 1641 observed reflections.II is triclinic, space group P with a 9.635(3), b 17.721(3), c 16.858(8) Å, α 89.77(2), β 104.36(4), γ 90.16(2)°, Z = 4, R = 9.0% for 6466 observed reflections.In both I and II tellurium is three-coordinate in a pyramidal geometry, with TeC distances in the range 2.07(1)–2.14(1) Å (I) and 2.10(1)–2.17(1) Å (II). In both structures short contacts of 3.4—3.5 Å occur between tellurium and carbon atoms of the tetraphenylborate anion. 相似文献
3.
The crystal structures of the title compounds have been determined from three-dimensional X-ray counter data.C8H8Te(CH2CHCH2)Br (I) is orthorhombic, space group Pbca with a 9.642(1), b 25.586(7), c 9.680(3) Å, Z = 8. The structure has been refined to R 5.2% for 1262 observed reflections.C8H8Te(CH2COPh)Br (II) is orthorhombic, space group Pccn with a 23.593(6), b 14.337(3), c 9.180(2) Å, Z = 8. R = 5.5% for 1374 reflections.C8H8Te(CD3)I (III) is orthorhombic, space group Pbca with a 11.200(3), b 15.976(2), c 23.328(3) Å, Z = 16. R = 5.6% for 2142 reflections.In I and II, tellurium is coordinated in an approximately octahedral geometry by the organic residues and three halogen contacts, with TeC and TeBr distances in the ranges 2.14(1)–2.19(1) Å and 3.328(2)–3.368(2) Å in (I) and 2.12(1)–2.18(1) Å and 3.292(2)–3.391(2) Å in II.In III, each of the two crystallographically independent complexes has tellurium coordinated in a distorted octahedral geometry. The TeC bond lengths are 2.10(2)–2.16(2) Å. In each case two TeI distances are in the range 3.596(2)–3.688(2) Å and a third, longer interaction (3.870(2) and 4.112(2) Å) completes the coordination.In each of the structures I–III the three covalent TeC bonds are oriented cis within the octahedra and exert a trans bond-lengthening effect on the Tehalogen interactions, precluding covalent-type bonding; the structures are essentially ionic, (C8H8TeR)+ cations and halide anions forming extended arrays. 相似文献
4.
《Polyhedron》1988,7(14):1267-1271
Synthetic and structural aspects of perchlorato complexes of tellurium(IV) with different dithiocarbamates (dtc) [(R1R2NCS2) where R1 = R2 = methyl, ethyl, n-propyl, i-propyl; R1R2 = (CH2)5(piperidine), C2H4OC2H4 (morpholine)] are reported. The crystal structure of TeL3ClO4 (where L = diethyl dtc) has been determined. The crystals of the complex are monoclinic, space group P21/n, a = 11.379(3), b = 17.745(7), c = 14.016(8) Å, γ = 103.30(2)°, V = 2754.2 Å3, F(000) = 1352, DX = 1.61 mg M−3. The final R and Rw values are 0.047 and 0.058, respectively for 5224 unique reflections. Tellurium displays a distorted dodecahedral stereochemistry formed by two interposing trapezoids, one resulting from the four sulphurs of two L groups and the other from the two sulphurs of the third L and the two oxygens of the perchlorate ion. The average TeS distance 2.648(2) Å is close to that reported in other tris(dithiocarbamato)tellurium(IV) complexes. The perchlorate is weakly coordinated to tellurium(IV), with the average TeO distance being 2.994(8) Å. The unusual coordination of perchlorate (as a bidentate ligand) to tellurium(IV) dithiocarbamate is reported for the first time. 相似文献
5.
R. Brec G. Ouvrard M. Evain P. Grenouilleau J. Rouxel 《Journal of solid state chemistry》1983,47(2):174-184
PV2S10 was obtained by heating the elements in stoichiometric proportions at 490°C in evacuated Pyrex tubes. The crystal symmetry is monoclinic, space group , with the unit cell parameters a = 12.734(8)Å, b = 7.349(7)Å, c = 23.662(4)Å, β = 95°22(1), V = 2205(4)Å3, and Z = 8. The structure was solved from 2269 independant reflexions, and anisotropic least squares refinement gave R = 0.036 with 236 variables. The structure can be described as made of [V2S12] units forming endless chains themselves linked, two by two, by [PS4] tetrahedra. In these units each vanadium is surrounded by eight sulfur atoms (mean dVS = 2.459Å) arranged in a distorted bicapped triangular prism. Two of these prisms shared a rectangular face to form [V2S12] groups, in which intercationic distances implied vanadium-vanadium bonds (mean dVV = 2.852(2)Å). Between the infinite double chains, only SS weak van der Waals' bonds exist. More than two thirds of the sulfur atoms are present as [SS]?II pairs, (mean dSS = 2.015Å); the rest are S?II anions. 相似文献
6.
The crystal and molecular structure of 3,4-quinoxalino-1-tellura(II)cyclopentane has been determined by X-ray diffraction at room temperature. The crystals are tetragonal, space group I41/a with a = b = 25.315(8), c = 6.010(1) Å and V = 3851.38 Å3. The density of 1.96 g cm?3 calculated on the basis of 16 molecules per unit cell is in agreement with the flotation value of 1.91 g cm?3. The structure has been refined to a conventional R value of 0.0408 using 744 independent observed reflections obtained from four-circle diffractometer measurements. The structure consists of discrete molecules TeC = 2.134 Å (av.), CN = 1.343 Å (av.) and angle CTeC = 80.7° (e.s.d. 0.5) but the intermolecular TeTe bonds (3.791 and 3.998 Å) are less than the sum of the Van der Waals' radii thus indicating the presence of secondary bonding. These short intermolecular contacts in the crystal structure are consistent with the anomalous physical properties observed. 相似文献
7.
The structure of Rh2(CH3CO2)4(DMF)2 {DMF = HCON(CH3)2} has been determined by single crystal X-ray methods. The compound crystallizes with eight formula units in a cell of dimensions: a = 29.438(7) Å, b = 7.978(2) Å, c = 20.279(5) Å, β = 113.20(4)°, V = 4377.5 Å3, space group C2/c. The structure has been refined by full-matrix least-squares method to a final R = 0.030 for the 4156 observed data. Two Rh(II) atoms are linked by four acetate groups forming a dimeric unit, where the RhRh distance is 2.383(1) Å. The coordination sphere about each Rh atom is completed by a DMF molecule; the average RhO(DMF) distance is 2.296(3) Å. 相似文献
8.
Ta4P4S29 was prepared from the elements heated together in stoichiometric proportions in an evacuated Pyrex tube for 10 days at 500°C. The crystal symmetry is tetragonal, space group P43212, with the cell parameters: a = b = 15.5711(7) Å, c = 13.6516(8) Å, V = 3309.9(5) Å3, and Z = 4. The structure calculations were conducted from 2335 reflections and 146 variables, leading to R = 0.033. The structure basic framework, corresponding to the chemical composition [TaPS6], is made of biprismatic bicapped [Ta2S12] units (average dTaS = 2.539 Å), including sulfur pairs (average dSS = 2.039 Å), bonded to each other through [PS4] tetrahedral groups (average dPS = 2.044 Å) sharing sulfurs. This framework leaves large tunnels running along the c axis of the cell and in which (S10)∞ sulfur chains are found to be inserted (average dSS = 2.052 Å and SSS = 105.75°). Diamagnetic and semiconducting Ta4P4S29 can be formulated: TaV4PV4(S?II)16(S?II2)4(S05). 相似文献
9.
A.A. Pasynskii I.L. Eremenko G.Sh. Gasanov O.G. Ellert V.M. Novotortsev Yu.V. Rakitin T.Kh. Kurbanov V.T. Kalinnikov Yu.T. Struchkov V.E. Shklover 《Polyhedron》1984,3(7):775-780
Reactions of (RC5H4)2Cr2(SCMe3)2S(I, R = H; II, R = Me) with (PPh3)2PdCl2 in benzene at 20°C gives trinuclear complexes (RC5H4)2Cr2Cl2(μ3-S)(μ-SCMe3)2Pd(PPh3)(III, R = H; IV, R = Me). The structure of IV as a monobenzene solvate is established by an X-ray analysis (black-green triclinic crystals space group P with a = 11.403(4), b = 14.933(5), c = 14.131(5) Å, α = 99.13(3), β = 112.72(3), γ = 95.65(3)°, V = 2201.6 Å, Z = 2; IV·C6H6). The structure was solved by direct methods and refined in an anisotropic approximation to R = 0.046, Rw = 0.058 for 7643 reflections with I ? 2σ(I). In the molecule of IV metal atoms are separated by non-bonding distances (Cr … Cr 4.079(I), Cr … Pd 3.230(I) and 3.380(I) Å) but linked by the bridging tridentate sulphur atom (CrS 2.339(2) and 2.329(2), PdS 2.327(2) Å), and two SCMe3 groups between Pd and Cr (CrS 2.396(2) and 2.403(2), PdS 2.350(2) and 2.381(2) Å, Cr?Pd 85.14(6) and 89.92(6)°). The Cl atoms are transferred from Pd to Cr atoms (CrCl 2.308(2) Å) and being terminally coordinated are in trans-positions to each other (as well as η-CH3C5H4 rings) with respect to the Cr2Pd plane. Cr atoms in III and IV exhibit ferromagnetic exchange interactions over the Cr?Cr system (+2J = 28 and 11 cm?1, respectively). 相似文献
10.
β-TeVO4 crystallizes in the monoclinic system with the space group and the parameters: a = 4.379 Å, b = 13.502 Å, c = 5.446 Å, and β = 91.72°. Vanadium occupies the center of a square pyramid of oxygens, an extra oxygen is at VO = 2.77 Å. These distorted octahedra share corners forming puckered sheets parallel to (010). The sheets are held together by [Te2O6]4? groups in which tellurium is one-side coordinated by four oxygen atoms. 相似文献
11.
Michael Laing Magriet J. Nolte Eric Singleton Erwin van der Stok 《Journal of organometallic chemistry》1978,146(1):77-86
The crystal structure of [(C8H12)6H3Me)(OC6H4Me)2} {P(OCH2)3CMe}] has been determined. a 18.32, b 18.98, c 9.35 Å, U 3251 Å3, Pn21a, Z = 4, R = 0.048, 2541 observed data.The coordination about the iridium atom is distorted trigonal bipyramidal; the two phosphorus atoms are equatorial, the σ-bonded carbon is axial, and the bidentate cyclooctadiene is bonded axialequatorial. The IrC(axial) bonds are longer than the IrC(equatorial) bonds: 2.22, 2.26; 2.17, 2.19 Å. The IrC(σ) bond length is 2.19 Å, not significantly different from the formally π-bonded C to Ir distances. The IrP lengths of 2.201 and 2.240 Å and the PIrP angle of 108.7° are normal. The longer IrP bond is in the five-membered chelate ring. The inertness to substitution is discussed. 相似文献
12.
Crystal and molecular structure of tricyclopentadienyltetrahydrofuranuranium(III), (η5-C5H5)3U·OC4H8
H.J. Wasserman A.J. Zozulin D.C. Moody R.R. Ryan K.V. Salazar 《Journal of organometallic chemistry》1983,254(3):305-311
Tricyclopentadienyltetrahydrofuranuranium(III), (η5-C5H5)3U·OC4H8, crystallizes in the centrosymmetric monoclinic space group P21/n with a 8.248(3), b 24.322(17), c 8.357(4) Å, β 101.29(5)°, V 1644.0 Å3 and ρ(calc) 2.04 g cm?1 for Z = 4 and mol.wt. 595.0. Diffraction data (Mo-Kα, 2θ(max) 45°) were collected on an Enraf-Nonius CAD4 diffractometer and the structure was refined to Rw(F) 4.7% for those 1530 reflections having I > 2σ(I). The molecule consists of a distorted tetrahedral arrangement of THF and (η5-C5H5) ligands with CpUCp angles in the range 110.4–122.4° and CpUO angles between 90.2 and 106.0°. Individual uranium-carbon distances range from 2.76(2) to 2.82(2) Å and average 2.79[1] Å. The uranium-oxygen distance of 2.551(10) Å suggests a 10-coordinate U3+ radius of 1.20 Å in this class of compounds. 相似文献
13.
The synthesis of a new class of two-dimensional triazole compounds is described, including the crystal structure of [Co(NCS)2(btr)2]H2O [btr stands for 4,4′-bis-1,2,4-triazole (C4H4N6)]. Crystals are monoclinic, space group C2/c, a = 11.159(1) Å, b = 13.047(4) Å, c = 12.993(3) Å, β = 91.81(2)°, Z = 4. The structure has been solved by Fourier and direct methods and refined by full-matrix least squares to R = 0.0229, Rw = 0.0283. The structure consists of layers of six-coordinated cobalt atoms, each having two trans-oriented N-bonded thiocyanate groups [CoNCS 2.098(2) Å] and linked together in the equatorial plane by single bridges of btr to a two-dimensional network. The btr ligand coordinates through its N(1) and N(1′) atoms [CoN 2.128(1) and 2.142(1) Å]. The intralayer CoCo distance is 9.207(2) Å, and the inter-layer CoCo distance is 8.584(1) Å. The magnetic susceptibilities of the compound and of the isostructural nickel and iron compounds are discussed. The iron compound exhibits a high-spin-low-spin crossover at liquid-nitrogen temperatures, as shown by magnetic susceptibility. 相似文献
14.
The crystal structure of the title compound has been determined by conventional X-ray diffraction techniques. The red diamond-shaped crystals are monoclinic, space group P21/n, a 8.914(4), b 16.090(12), c 14.991(5) Å, β 95.97(2)°, V 2138.44 Å3, Z = 4. Refinement by full-matrix least-squares methods employed anisotropic thermal parameters for all non-hydrogen atoms and isotropic temperature factors for hydrogen atoms, and returned final residuals of R = 0.028 and Rw = 0.028.The complex is monomeric, with a square planar coordination geometry comprising the S and P atoms of the bidentate (o-methylthiophenyl)diphenylphosphine ligand and the two iodine atoms. The PdI distance trans to P is 2.658(1) Å whereas that trans to S is 2.602(1) Å. The difference of 56 standard deviations illustrates the greater structural trans influence of phosphine over thioether donors. The PdP and PdS distances of 2.250(2) and 2.288(2) Å, respectively, are normal. Two phenyl hydrogen atoms approach the Pd atom in the axial regions above and below the square plane at distances of 2.98 and 2.99 Å. 相似文献
15.
S.Candeloro de Sanctis N.V. Pavel L. Toniolo 《Journal of organometallic chemistry》1976,108(3):409-421
For the class of compounds mentioned in the title it is difficult to the stucture unambiguously on the molecular and crystal structure of CH3-p)]2 by single crystal X-ray analysis. The crystal data are: M == 743 a.m.u. Space group P21/c. a = 8.510(2), b = 40.652(9), c = 9.762(2) Å, β = 103.61(2)° Dc = 1.50 g/cm3. R = 0.041, R = 0.060, based on 3978 independent reflections. The two π-allylpalladium residues are bridged azenido groups, gaining an approximate square planar coordination around each heavy atom. The two allyl units are stereochemically equivalent, with the central carbon atoms pointing outwars. The rigid triazenido groups force the two palladium atoms into close contact (2.86 Å). The aromatic rings are somewhat rotated with respect to the bonded NNN planes, but some π-conjugation over the whole ligand is still retained. 相似文献
16.
《Journal of organometallic chemistry》1987,334(3):295-305
Dimethylbis(2-pyridinethiolato-N-oxide)tin(IV), Me2Sn(2-SPyO)2, crystallizes in space group P21/c with a 9.877(3), b 11.980(4), c 13.577(3) Å, β 109.1(2)° and Z = 4. The structure was refined to RF = 0.036 for 2263 Mo-Kα observed reflections. The coordination geometry at tin is a skew-trapezoidal bipyramid, with the oxygen [SnO 2.356(3), 2.410(4) Å] and sulfur [SnS 2.536(1), 2.566(1) Å] atoms of the chelating groups occupying the trapezoidal plane and the methyl groups [SnC 2.106(6), 2.128(7) Å] occupying the apical positions. The methyl-tin-methyl skeleton is bent [CSnC 138.9(2)°]. The SSnS angle is 77.8(1)°, but the OSnO angle is opened to 136.7(1)° to accommodate the intruding methyl groups. The carbontincarbon angles predicted from quadrupole splitting (119mSn Mössbauer) and one-bond 119Sn13C coupling constant (solution 13C NMR) data agree closely with the experimental value. 相似文献
17.
G. Eulenberger 《Journal of solid state chemistry》1984,55(3):306-313
The new compound Tl6[Ge2Te6] was prepared by thermal synthesis from the elements. The material is triclinic, space group , with a = 9.471(2), b = 9.714(2), c = 10.389(2) Å, α = 89.39(1), β = 97.27(1), γ = 100.79(1)°, and Z = 2. The crystal structure was determined from single-crystal intensity data measured by means of an automated four-circle diffractometer and refined to an R value of 0.053 for 1831 observed reflections. Tl6[Ge2Te6] is characterized by Ge2Te6 units with GeGe bonds which are linked into a three-dimensional structure by Tl atoms coordinated to essentially six Te atoms. The most important mean distances are Å, Å, and Å. The lone 6s electron pairs of the thallium(I) atoms exhibit significant stereochemical activity. Tl6[Ge2Te6] represents a new structure type. 相似文献
18.
Dimethylaluminium- and dimethylgallium-N,N′-dimethylacetamidine (I and II) are doubly associated forming a puckered eight-membered ring. They crystallize isostructurally in the monoclinic space group P21/c with two dimers per unit cell. The lattice constants of I are a 8.187, b 7.266, c 14.778 Å, β 103.58° and those of II a 8.163, b 7.277, c 14.835 Å, β 103.46°. The MN and the NC bond lengths within the rings are nearly equal, their mean values are for I: AlN 1.925 Å, CN 1.330 Å and for II: GaN 1.979 Å, CN 1.335 Å. This is also true for the exocyclic bond lengths with average values AlC 1.975 Å, NC 1.474 Å, CC 1.509 Å (for I) and GaC 1.998 Å, NC 1.484 Å and CC 1.507 Å (for II). The metal atoms are tetrahedrally coordinated, and the distortion is only slight. The final R-values are 0.034 and 0.056, respectively. 相似文献
19.
Melvyn Rowen Churchill Clifford Bueno David A. Young 《Journal of organometallic chemistry》1981,213(1):139-150
The species FeRu3(CO)13(μ-PPH2)2, synthesized from Ru3(CO)12 and Fe(CO)4(Ph2PPPh2),has been characterized both spectroscopically and via a single-crystal X-ray structural analysis. This complex crystallizes in the centrosymmetric triclinic space group P [No. 2, Ci1] with a 10.066(3), b 12.899(3), c 17.003(4) Å, α 111.89(2), β 91.02(2), γ 102.00(2)°, V 1992.7(9) Å3, Z 2, ?(obsd) 1.79(2) g cm-3 and ?(calcd) 1.82 cm-3. Diffraction data were collected with a Syntex P21 automated four-circle diffractometer and the structure was refined to RF 6.0% and RWF 3.6% for all 5213 reflections (RF 3.8%, RWF 3.6% for those 4140 reflections with |Fo|> 3σ(|Fo|).The metal atoms define a planar triangulated rhombus, with atoms Ru(1) and Ru(2) at the bridgehead, and Fe(1) and Ru(3) at the acute apices. Fe(1) is linked to four terminal carbonyl ligands and is associated with the heteronuclear bonds Fe(1)Ru(1) 2.861(1) Å and Fe(1)Ru(2) 2.868(1) Å. The ruthenium atoms are each bonded to three terminal carbonyl groups. The retheniumruthenium distances are Ru(1)Ru(2) 3.098(1), Ru(1)Ru(3) 3.147(1), and Ru(2)Ru(3) 3.171(1) Å. The structure is completed by Ph2P bridges across the Ru(1)Ru(3) and Ru(2)(ru(3) vectors (<Ru(1)P(1)Ru(3) 84.89(5)° and <Ru(2)P(2)Ru(3) 85.56(6)°). 相似文献
20.
Kunio Miki Masahiro Yama Yasushi Kai Nobutami Kasai 《Journal of organometallic chemistry》1982,239(2):417-428
The molecular structure of a three-coordinate palladium(II)-styrene complex, [Pd(η5-C5H5)(PEt3)(styrene)]BF4 has been determined by means of X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c, with four formula units in a cell of dimensions: a 10.229(3), b 11.262(3), c 18.760(5) Å and β 103.77(2)°. The structure was solved by the heavy atom method, and refined by the least-squares procedure to R = 0.050 for 3635 observed reflections. The palladium atom is surrounded by the cyclopentadienyl group, the triethylphosphine ligand and the olefinic bond of styrene in the cationic complex. In the palladiumstyrene bonding, the olefinic bond is inclined by 77.3° to the coordination plane defined by the Pd and P atoms and the center of the cyclopentadienyl ring (PdC(1) 2.176(6), PdC(2) 2.234(5) and C(1)C(2) 1.369(8) Å). 相似文献