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The compounds Co(OC2OPor).CH2Cl2 (1), Co(OC2OPor)(NO)out.0.46CHCl3 (2), Co(OC3OPor).CHCl3 (3), and Co(OC3OPor)(MeIm).3C7H8 (4) (OC2OPor = 5,10,15,20-(benzene-1,2,4,5- tetrakis(2-phenyloxy)ethoxy)-2',2",2"',2"-tetraylporphyrinato dianion; OC3OPor = 5,10,15,20-(benzene-1,2,4,5-tetrakis(2- phenyloxy)propoxy)-2',2",2"',2"-tetraylporphyrinato dianion; MeIm = 1-methylimidazole), have been synthesized, and their structures have been determined by single-crystal X-ray diffraction methods at T = -120 degrees C: 1, a = 8.824(1) A, b = 16.674(1) A, c = 16.836(1) A, alpha = 104.453(1) degrees, beta = 92.752(1) degrees, gamma = 90.983(1) degrees, P1, Z = 2; 2, a = 9.019(1) A, b = 16.588(2) A, c = 16.909(2) A, alpha = 103.923(2) degrees, beta = 92.082(2) degrees, gamma = 93.583(2) degrees, P1, Z = 2; 3, a = 13.484(3) A, b = 14.404(3) A, c = 14.570(3) A, alpha = 105.508(3) degrees, beta = 100.678(3) degrees, gamma = 93.509(4) degrees, P1, Z = 2; 4, a = 16.490(1) A, b = 22.324(2) A, c = 17.257(1) A, b = 92.437(1) degrees, P2(1)/n, Z = 4. These compounds are the first structurally characterized Co-bound members of the OCnOPor ligand system. The NO ligand in 2 and the MeIm ligand in 4 bind asymmetrically and lead to several metrical changes in these porphyrins, e.g., variations in average porphyrin deviations and Co atom displacements relative to the porphyrinato N atoms and the mean porphyrin planes. 相似文献
5.
The polyoxo rare-earth core
(Ln = Y, Gd, and Yb) has been synthesized from the appropriate rare-earth chloride hydrate and K2Se and Se in dmf (dimethylformamide). The cluster core is ligated with a variety of polyselenido chains in addition to a number of dmf molecules. The structure of the Gd8(dmf)13(4-O)(3-OH)12(Se3)(Se4)2(Se5)2 cluster, 1, was determined by X-ray diffraction methods. It is similar to an Eu cluster previously characterized. Two new clusters, Yb8(dmf)11(4-O)(3-OH)12(Se4)2(Se5)2Cl2·dmf, 2, and Y8(dmf)12(4-O)(3-OH)12(Se4)4Cl2·6 dmf, 3, have also been synthesized and characterized. Clusters 2 and 3 have the same octanuclear core of rare-earth atoms as the Gd cluster but contain two chloro ligands in two isomeric conformations in place of the Se
3
2-
ring in the Gd cluster. The geometry of the Ln
8 core is described as a triangulated dodecahedron with 3-OH groups capping the 12 faces. A 4-O atom centers the cluster with close contacts to four Ln atoms in an approximate tetrahedral arrangement. Pertinent crystallographic data are: Compound 1, monoclinic,
, a= 14.410(3) Å, b = 24.439(5) Å, c = 28.927(6) Å, = 101.05(3)°, V = 9998(3) Å3, T = 106(2) K, Z = 4; Compound 2, orthorhombic,
, a = 17.049(9) Å, b = 24.68(1) Å, c = 45.03(2)Å, V = 18,945(16) Å3, T = 153(2) K, Z = 8; Compound 3, monoclinic, C
2h
5
-P21/c, a =18.728(l) Å, b = 29.263( 1) Å, c = 20.548(1) Å, = 90.144(1)°, V = 11,261(1) Å3, T = 153(2) K, Z = 4. 相似文献
6.
Ismail Ijjaali James A. Ibers 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(9):i124-i125
From a single‐crystal study, Nd2Te3 is found to be isostructural with Gd2Te3, crystallizing in the U2S3 structure type. Each of the two non‐equivalent Nd atoms is surrounded by seven Te atoms, with the polyhedra best described as a seven‐octahedron and a monocapped trigonal prism. All atoms lie on mirror planes. 相似文献
7.
The compound [PPh(4)](2)[NEt(4)][CuTe(7)] has been synthesized from the reaction of CuCl with a polytelluride solution in dimethylformamide at room temperature. The compound crystallizes with two formula units in the triclinic space group P(-)1 in a cell with dimensions a = 8.9507(18) A, b = 14.714(3) A, and c = 23.277(5) A and alpha= 86.32(3) degrees, beta= 80.17(3) degrees, and gamma= 75.63(3) degrees (T = -120 degrees C). Ab initio calculations indicate that the nonclassical [CuTe(7)](3)(-) anion is the result of joining Te(3)(2-) and [CuTe(4)](1-) fragments through donor-acceptor interactions. 相似文献
8.
Some new quaternary compounds of the type BaLnMQ3 (Ln = rare earth or Sc; M = Cu, Ag; Q = S, Se) have been synthesized by the reaction of the constituent binary chalcogenides and elements at 1000°C. The crystal structures of two of these compounds have been determined by single-crystal X-ray diffraction techniques and are isostructural. Crystal data: BaErCuS3—space group D172h —Cmcm, M= 464.32, Z = 4 , a = 3.987(1), b = 13.377(3), c = 10.101(2) Å (T = 115 K), V = 538.7(4) Å3, Rw (F2) = 0.095 for 848 observations and 24 variables, R(F) = 0.037 for 840 observations having F20 > 2σ (F20); BaYAgSe—space group D172h —Cmcm, M = 571.0, Z = 4, a = 4.239(1), b = 14.030(2), c = 10.636(2) Å (T = 115 K), V = 632.6(2) Å3, Rw (F2) = 0.057 for 645 observations and 24 variables, R(F) = 0.023 for 595 observations having F20 > 2σ(F20). These two compounds adopt the layered KZrCuS3 structure type. The layers, which are separated by Ba2+ ions, consist of edge-sharing octahedral chains and corner-sharing tetrahedral chains. The other compounds synthesized crystallize either with this same structure or with that of β-BaLaCuSe3, a slightly distorted variation, which is isostructural with Eu2CuS3. The diffuse reflective UV-visible spectra of several of these compounds have been measured. From magnetic susceptibility measurements, both BaNdCuS3 and BaGdCuS3 show Curie-Weiss behavior, whereas BaCeCuS3 and BaCeCuSe3 show in addition temperature-independent paramagnetism. 相似文献
9.
The new compounds K(2)TiCu(2)S(4), Rb(2)TiCu(2)S(4), Rb(2)TiAg(2)S(4), Cs(2)TiAg(2)S(4), and Cs(2)TiCu(2)Se(4) have been synthesized by the reactions of A(2)Q(3) (A = K, Rb, Cs; Q = S, Se) with Ti, M (M = Cu or Ag), and Q at 823 K. The compounds Rb(2)TiCu(2)S(4), Cs(2)TiAg(2)S(4), and Cs(2)TiCu(2)Se(4) are isostructural. They crystallize with two formula units in space group P4(2)/mcm of the tetragonal system in cells of dimensions a = 5.6046(4) A, c = 13.154(1) A for Rb(2)TiCu(2)S(4), a =6.024(1) A, c = 13.566(4) A for Cs(2)TiAg(2)S(4), and a =5.852(2) A, c =14.234(5) A for Cs(2)TiCu(2)Se(4) at 153 K. Their structure is closely related to that of Cs(2)ZrAg(2)Te(4) and comprises [TiM(2)Q(4)(2)(-)] layers, which are separated by alkali metal atoms. The [TiM(2)Q(4)(2)(-)] layer is anti-fluorite-like with both Ti and M atoms tetrahedrally coordinated to Q atoms. Tetrahedral coordination of Ti(4+) is rare in the solid state. On the basis of unit cell and space group determinations, the compounds K(2)TiCu(2)S(4) and Rb(2)TiAg(2)S(4) are isostructural with the above compounds. The band gaps of K(2)TiCu(2)S(4), Rb(2)TiCu(2)S(4), Rb(2)TiAg(2)S(4), and Cs(2)TiAg(2)S(4) are 2.04, 2.19, 2.33, and 2.44 eV, respectively, as derived from optical measurements. From band-structure calculations, the optical absorption for an A(2)TiM(2)Q(4) compound is assigned to a transition from an M d and Q p valence band (HOMO) to a Ti 3d conduction band. 相似文献
10.
Douglas C. Miller Martin R. Johnson John J. Becker James A. Ibers 《Journal of heterocyclic chemistry》1993,30(6):1485-1490
The new 22-π, aromatic “pentaplanar” macrocycle, ozaphyrin ( 6 ), has been synthesized by a McMurry coupling of 5,5′-diformyl-4,4′-dipropyl-2,2′-bipyrrole ( 1 ) with 2,5-bis(5-formyl-4-propyl-2-pyrrolyl)furan ( 5 ). This synthetic pathway to ozaphyrin and its characterization by 1H nmr spectroscopy, uv-visible spectroscopy, cyclic voltammetry, and X-ray crystallography are described. The structure consists of layers of planar, staggered macrocycles stacked perpendicular to the α-axis. Ozaphyrin crystallizes with four formula units in the monoclinic space group C52h-P21/n in a cell of dimensions a = 10.481(7) Å, b = 17.353(17) Å, c = 18.726(12) Å, and β = 102.84(5)° (108 K). The structure has been refined on F2 (5171 unique reflections, 411 variables) to Rw(Fo2) = 0.165. The conventional agreement index R(F) is 0.074 for the 3289 reflections have Fo2>2o(Fo2). 相似文献