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1.
Eugene R. Corey Joyce Y. Corey Milton D. Glick 《Journal of organometallic chemistry》1975,101(2):177-186
The structure of 5-p-N-N-dimethylaminophenyl-10,11-dihydro-5H-dibenzo-[b,f]silepin has been determined from three-dimensional X-ray data collected by counter methods. The compound crystallizes in the monoclinic space group P21/ca 14.121(4), b 14.379(3), c 9.126(2) Å and β = 99.57(2)°. The observed and calculated densities (Z 4) are 1.19 and 1.20 g cm?3, respectively. Anisotropic refinement of nonhydrogen atoms with hydrogen atoms at fixed calculated positions gave a conventional R-factor of 4.6% for 2023 reflections with F > 3σ(F20). The central seven-membered ring of the tricyclic system exhibits a folded boat conformation; the dihedral angle between the benzo groups is 137.2°. The benzo groups are twisted approximately 21° relative to one another and skewed such that the two carbons bonded to silicon are 0.33 Å closer to one another than the two benzo ring carbons one atom removed from the silicon. The nitrogen atom is displaced 0.04 Å from the plane of the adjacent carbon atoms. 相似文献
2.
Eugene R. Corey William F. Paton Joyce Y. Corey Milton D. Glick 《Journal of organometallic chemistry》1979,179(3):241-252
The solid state structure of the hydrofumarate salt of 5,5-dimethyl-10-(4-methylpiperazinyl)-1O,11-dihydro-5H-dibenzo[b,f]silepin (II), a silicon analog of perathiepin (I) in which divalent sulfur is replaced by the (CH3)2Si moiety, has been determined by X-ray diffraction methods. The compound, C25H32N2O4Si, crystallizes in the orthorhombic space group, Pbc21 with a 9.304(2), b 23.010(7), c 11.599(3) Å; the structure was refined by full-matrix least-squares techniques to a conventional R of 0.039 for 1858 counter reflections. The structure consists of a network of hydrogen-bonded hydrofumarate anions and the protonated heterocyclic unit. The tricyclic framework of the cation adopts a folded boat conformation with a dihedral angle between benzo group planes of 151.2°. In contrast to related systems, the piperazinyl substituent which has the expected chair conformation occupies a pseudoaxial site on the ethano bridge. Structural parameters of the tricyclic framework of the title compound and related compounds are compared. 相似文献
3.
A.B. Zolotoy O.A. Dyachenko L.O. Atovmyan I.P. Yakovlev V.O. Reichsfeld 《Journal of organometallic chemistry》1980,190(3):267-276
The structure of 5-ethyl-5,10-dihydro-10,10-diphenylphenazasiline has been determined from three-dimensional X-ray data collected by counter methods. The compound in the monoclinic space group P21/b with a 10.782(5), b 22.642(9), c 8.830(4) Å and γ 74°41′(2). The observed and calculated densities (Z = 4) are 1.22 and 1.21 g cm-3, respectively. Anisotropic(Si, N, C)-isotropic block-diagonal least squares refinement gave a conventional R factor of 3.9% for 1871 reflections with I>2σ(I). The central six-membered ring of the tricyclic system adopts a boat conformation; the dihedral angle between the benzo-group planes is 157.3°. The CSiC angle in the heterocycle is 101.1(1)°; the mean SiC bond length is 1.850(2) Å (in the cycle) and 1.862(2) Å (with Ph group). The nitrogen atom is displaced 0.05 Å from the plane of the adjacent carbon atoms; the sum of the angle about N is 359.7°. 相似文献
4.
Single crystals of BaTiF5 and CaTiF5 were obtained by the Czochralski and Bridgman techniques, respectively. The crystal structures were determined by X-ray diffraction; BaTiF5: Å, c = 7.670(3)Å; CaTiF5: Å, b = 6.614Å, c = 7.696(3)Å, β = 115.16(3)°. Both structures are characterized by the presence of either branched or straight chains of TiF6 octahedra. BaTiF5 contains the unusual dimeric unit (Ti2F10)4?. Magnetic susceptibility measurements were performed on both compounds in the temperature range 4.2 to 300 K, however, no evidence for magnetic interactions between the Ti3+ moments were observed. 相似文献
5.
6.
Gerhard Cordier Christoph Schwidetzky Herbert Schäfer 《Journal of solid state chemistry》1984,54(1):84-88
The new compound BaSb2S4 crystallizes in the monoclinic system (space group: , No. 14) with a = 8.985(2) Å, b = 8.203(3) Å, c = 20.602(5) Å, β = 101.36(3)°. SbS3 ψ tetrahedra and ψ-trigonal SbS4 bipyramids are connected by common corners and edgers to infinite strings. These are arraged cross-wise in sheets perpendicular to the c axis. 相似文献
7.
Single crystals of the title compounds have been grown by the Czochralski technique. Pb4P2O9 crystallizes in the space group with the parameters a = 9.4812 Å, b = 7.1303 Å, c = 14.390 Å, β = 104.51° and Pb8P2O13 in with a = 10.641 Å, b = 10.206Å c = 14.342 Å, β = 98.34°. 相似文献
8.
Patrice de Meester Shirley S. C. Chu Misa V. Jovanovic Edward R. Biehl 《Journal of heterocyclic chemistry》1985,22(5):1237-1241
The crystal structure of 3′-methoxy-5-phenyl-5,10-dihydrophenarsazine, C19H16AsNO has been determined by the single crystal x-ray diffraction method. The crystals are monoclinic with a = 15.305(6), b = 5.809(2), c = 17.595(6)Å, β = 92.92(2)°, V = 1562.3(1.0Å3, space group P2,/n, Z = 4 and dcalc = 1.485g cm−3. An automatic diffractometer with graphite monochromatized MoKα radiation was used to obtain 1480 observed reflection with I > 3σ(I) at 2θ < 50°. Final R = 0.040 and wR = 0.032. The tricyclic ring is folded with the central ring in a flattened boat conformation. The folding angle between the least-squares planes of the two benzo rings is 164.6(2)°. The 3′-methoxyphenyl group is in a boat-axial conformation with respect to the central ring. 相似文献
9.
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
10.
Ce6Mo10O39 crystallizes in the triclinic system with unit-cell dimensions (from single-crystal data) a = 10.148(5), Å, b = 18.764(6), Å, c = 9.566(5), Å, α = 103.12(7)°, β = 78.07(7)°, γ = 107.69(7)°, and space group . The structure was solved using direct methods with 3113 countermeasured reflections (MoKα radiation), and refined using Fourier and least-squares techniques to a conventional R of 0.039 (ωR = 0.047). Ce6Mo10O39 has a structure that consists of isolated MoO4 tetrahedra together with one corner-shared pair of tetrahedra, linked to irregular eight-coordinate Ce(III) polyhedra. The average MoO distance of 1.77 Å, and average CeO distance of 2.52 Å are in good agreement with previously reported values. 相似文献
11.
Jeffrey L. Petersen 《Journal of organometallic chemistry》1979,166(2):179-192
The hydrolysis of (η5-C5H5)2Zr(SC6H5)2 was shown previously by IR spectroscopy to produce an oxo-bridged complex. The molecular structure of this material has been determined by X-ray diffraction methods and consists of two (η2-C5H5)2Zr(SC6H5) units linked by an oxo bridge. The ZrOZr bond is nonlinear at 165.8(2)° with a Zr?Zr interatomic separation of 3.902(1)Å. The two independent SZrO bond angles of 98.7(1) and 103.3(1)° are consistent with a d° electronic structure for each zirconium atom. The relatively short ZrO distances of 1.968(3) and 1.964(3) Å support the presence of partial double-bond character arising from the donation of electron density from filled pπ-orbitals on the oxygen atom to unfilled d-orbitals on the electron deficient d0 metal atoms. This bonding feature requires based upon orbital symmetry arguments that the (ML)2O molecular core in [(η5-C5H5)2ML]2O complexes must be nonplanar with a dihedral angle between the two LMO planes less than 90°. For [(η5-C5H5)2Zr(SC6H5)]2O, dihedral angle of 61.7° was observed. The compound crystallizes in an orthorhombic space group, Pbca, with refined lattices parameters a 16.458(4), b 20.281(5), and c 17.016(4) Å. Full-matrix least-squares refinement of 2613 diffractometry data I > σ(I) led to a final discrepancy index R(F02) = 0.044. 相似文献
12.
Régnault von der Mühll Françoise Daut Jean Ravez 《Journal of solid state chemistry》1973,8(3):206-212
The crystal structure of SrFeF5 has been determined by single crystal X-ray diffraction methods.The unit cell is monoclinic (space group ) with a = 7.062 ± 0.001 Å, b = 7.289 ± 0.001 Å, c = 14.704 ± 0.001 Å, β = 95.40 ± 0.01° and Z = 8.The lattice is built up of spiral chains of octahedra parallel to the Oy axis. These chains are formed by (FeF6)3? octahedra sharing corners of the same edge. The strontium atoms bridge three neighbouring chains. The SrTiF5, SrVF5, SrCoF5, and BaInF5 phases are isostructural with SrFeF5. 相似文献
13.
Anhydrous Li2SeO4 crystallizes in the trigonal space group with a = 13.931(2), c = 9.304(3) Å, V = 1563.7 Å3, Z = 18, Dc = 2.988 g cm?3. The unit cell transforms to the rhombohedral coordinate system as a = 8.620 Å, α = 107.81(2)°, V = 521.2 Å3, Z = 6. The structure contains selenate anions bridged by Li in the phenacite structural type. Data collection was performed at low temperature for precise placement of the Li cations which are tetrahedrally surrounded by oxygen atoms. Some problems with secondary extinction were apparent and a correction was made. The structure refined to an R value of 0.034. 相似文献
14.
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
15.
Berhan Teclé Kaniz F. Siddiqui Christopher Ceccarelli John P. Oliver 《Journal of organometallic chemistry》1983,255(1):11-15
The structure of di-trans-β-styrylmercury has been determined by single crystal X-ray methods from counter data. The compound crystallizes in the orthorhombic space group Pbcn with unit cell dimensions a 15.413(6), b 11.161(9), c 7.668(5) Å, V 1319(1) Å3, Dcalc 2.049 g/cm3, and Z = 4. The crystal was solved by conventional heavy atom techniques. The crystal consists of individual molecular units with the mercury atom located on a two fold axis of symmetry. The CHgC fragment is nearly linear with an angle of 178°. The β-styryl groups are oriented so that a dihedral angle of 66.8° is formed between the planes defined by HgC(1)C(2) and HgC(1)′C(2)′ fragments. The HgC bond distance is 2.07(4) Å. 相似文献
16.
Two new aroylhydrazones 3-bromo-N′-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (1) and 4-hydroxy-3-methoxy-N′-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (2), derived from 5-methoxysalicylaldehyde, are prepared and determined by means of infrared and 1H NMR spectroscopy and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group P21/n with a = 5.9406(7) Å, b = 31.833(3) Å, c = 7.6460(8) Å, β = 94.522(4)°, V = 1441.4(3) Å3, Z = 4. Compound 2 crystallizes in the monoclinic space group P21/c with a = 14.3471(9) Å, b = 11.3893(7) Å, c = 9.6853(6) Å, β = 94.063(2)°, V = 1578.6(2) Å3, Z = 4. Both molecules have very similar bond lengths and angles. The crystal structures of both compounds are stabilized by N-H...O and O-H...O hydrogen bonds as well as π...π interactions. 相似文献
17.
Cu4(PO4)2O crystallizes in the space group with a = 7.5393(8) Å, b = 8.1021(9) Å, c = 6.2764(8) Å, α = 113.65(1)°, β = 98.42(1)° and γ = 74.19(1)°. The structure was refined by full-matrix least-squares techniques using automatic diffractometer data to R = 0.046 (Rw = 0.056). Four unique copper atoms are in six, five-, and four-coordinated polyhedra which are linked together to form a three-dimensional network. The structure is best described in terms of a cubic close-packed array of oxygen atoms with one-tenth of the possible anion sites vacant. 相似文献
18.
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
19.
Isao Kawada Mitsuko Nakano-Onoda Motohiko Ishii Masanobu Saeki Mitsuoki Nakahira 《Journal of solid state chemistry》1975,15(3):246-252
Crystal structures of the ordered phases of V3S4 and V5S8 were refined with single crystal data. Both are monoclinic. Chemical compositions, space groups and lattice constants are as follows: VS1.47, (No. 12), a = 5.831(1), b = 3.267(1), c = 11.317(2)Å, β = 91.78(1)° and VS1.64, (No. 12), a = 11.396(11), b = 6.645(7), c = 11.293(4), Å, β = 91.45(6)°. In both structures, short metal-metal bonds were found between the layers as well as within them. In comparison with the structure of Fe7S8, the stability of NiAs-type structure was discussed based on the detailed metal-sulfur distances. 相似文献
20.
LLi2Mo4o13 crystallizes in the triclinic system with unit-cell dimensions a = 8.578 Å, b = 11.450 Å, c = 8.225 Å, α = 109.24°, β = 96.04°, γ = 95.95° and space group . The calculated and measured densities are 4.02 g/cm3 and 4.1 g/cm3 respectively. The structure was solved using three-dimensional Patterson and Fourier techniques. Of the 2468 unique reflections collected by counter methods, 1813 with I ? 3σ(I) were used in the least-squares refinement of the model to a conventional R of 0.031 (ωR = 0.038). LLi2Mo4O13 is a derivative of the V6O13 structure with oxygen ions arranged in a face-centred cubic type array with octahedrally coordinated molybdenum and lithium ions ordered into layers. 相似文献