scholarly journals S4N4 und seine Derivate: Isolierung und Struktur von Pd2(S3N)2(S3N2) / S4N4 and its Derivatives: Isolation and Structure of Pd2(S3N)2(S3N2)

1982 ◽  
Vol 37 (3) ◽  
pp. 276-280 ◽  
Author(s):  
Ulf Thewalt

Abstract The reaction of S4N4 with PdCl2 in methanol yields among other products the dinuclear complex Pd2 (S3N)2(S3N2) (D): dark red needles, space group R"3̄ with a = 32.759(15), c = 6.516(4) Å and Z = 18. The structure of D was determined by an X-ray analysis. Each palladium atom is part of an almost planar PdS3N metallocycle. The SNSNS group acts as a bridge whereby each of its terminal S atoms is bonded to both Pd atoms. The Pd atoms possess a square planar coordination by four S atoms. The coordination planes form an angle of 114.9°. The Pd-Pd distance of 2.921(2) Å is rather short.

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.


1986 ◽  
Vol 41 (4) ◽  
pp. 409-412 ◽  
Author(s):  
Joachim Pickardt ◽  
Norbert Rautenberg

By reaction of PdCl2(C6H5CN) 2 with 1,3,5,7-tetram ethyl-2,4,6,8,9,10-hexathiaadam antane, (CH3)4C4S6, (“TMTA”), the complex PdCl2-TMTA could be obtained. X-ray structure analyses were performed for the free ligand TMTA as well as for the adduct. Both com pounds crystallize monoclinically, space group P21/n, lattice parameters for TMTA are a= 845.9(5), b= 1225.8(7), c= 1314.8(8) pm, ß= 93.28(5)°; for PdCl2-TMTA a= 1262.3(3), b= 1376.3(4), c= 939.1(3) pm, and ß= 92.86(5)°. In the palladium complex TMTA acts as a bidentate chelating ligand. The coordination about the Pd atom is approximately square planar, but the bond angle S -Pd -S is only 76.2°


1993 ◽  
Vol 71 (7) ◽  
pp. 1086-1093 ◽  
Author(s):  
Liqin Chen ◽  
Laurence K. Thompson ◽  
John N. Bridson

The preparation and properties of the thioether–pyridazine macrocycle (L4; C16H20S6N4) containing two pyridazine subunits, and its Cu(II), Cu(II)Cu(I), and Cu(I) complexes are described. The ligand is characterized by 1H nuclear magnetic resonance and mass spectrometry, and the complexes by infrared, eleetronic spectra, and magnetism, and in some cases by X-ray crystallography. The complex [Cu2(L4)Cl4]x, (1) crystallized in the triclinic system, space group [Formula: see text] with a = 8.6204(8) Å, b = 9.850(1) Å, c = 8.348(1) Å, α = 111.46(1)°, β = 102.50(1)°, γ = 71.818(9)°, V = 622.6(1) Å3, and Z = 1 (R = 0.043, Rw = 0.042 for 1312 reflections). Two monodentate pyridazine rings in the same ligand bind to one trans square-planar copper centre (CuN2Cl2) with two sulfurs from each ligand binding to another trans square-planar copper centre (CuS2Cl2) to form a polynuclear chain. The complex [Cu(L4)Cl2] (3) crystallized in the triclinic system, space group [Formula: see text] with a = 11.001(1) Å, b = 12.888(2) Å, c = 8.704(1) Å, α = 102.89(1)°, β = 103.36(1)°,γ = 75.84(1)°, V = 1145.8(3) Å3 and Z = 2 (R = 0.056, Rw = 0.044 for 2059 reflections). A trans square-planar structure (CuN2Cl2) exists for 3 with monodentate pyridazines. [Cu(L4)(NO3)2] (4) crystallized in the orthorhombic system, space group P212121, with a = 15.148(2) Å, b = 15.562(3) Å, c = 11.064(1) Å, V = 2608.2(7) Å3 and Z = 4 (R = 0.039, Rw = 0.034 for 1864 reflections). Two monodentate pyridazine rings and two bidentate nitrates bind to a pseudo-octahedral copper(II) centre.


1989 ◽  
Vol 44 (9) ◽  
pp. 999-1002 ◽  
Author(s):  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
Alfred Zinn ◽  
Kurt Dehnicke

Ph—C(NSiMe3)2AuCl2 has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)-benzamidine with AuCl3 in CH2Cl2 suspension, forming orange-red crystals, which were characterized by an X-ray structure determination.Space group P21/n, Z = 4, 2358 observed independent reflexions, R = 0.028. Lattice dimensions (20°C): a = 695.9(3); b = 1576.1(3); c = 1830.9(3) pm; β = 94.27(3)°. The compound forms monomeric molecules, in which the gold atom is in a square planar arrangement of the two nitrogen atoms of the benzamidinato chelate (Au—N 201.6(7); 203.3(6) pm) and by two chlorine atoms (Au—Cl 227.9(3); 228.5(2) pm).


2001 ◽  
Vol 56 (8) ◽  
pp. 759-764 ◽  
Author(s):  
Soheila Chitsaz ◽  
Effat Iravani ◽  
Jochen Pauls ◽  
Bernhard Neumüller

[(THF)2LiCl2VCl2(THF)2] (1) and [Li(THF)4][OMoCl4(THF)] (2) can be prepared by the reactions of VCI3 with LiCl in THF and of Li(H)PtBu with OM0 CI4 in THF, respectively. 1 and 2 were characterized by IR spectroscopy, MS spectrometry (2) and X-ray crystallography. 1 can be obtained in two modifications depending on the temperature of crystallization. At -30 °C a triclinic form, 1a, was isolated from THF solution with one unique molecule per asymmetric unit. However, at 20 °C, 1b crystallized in the monoclinic space group P2/c. It possesses four independent molecules per asymmetric unit. According to the structure analyses 1 consists of a dinuclear complex with a planar LiCl2V four-membered ring while 2 consists of seperate ions [Li(THF)4]+ and [OMoCl4(THF)]-


2021 ◽  
Vol 8 ◽  
pp. 43-47
Author(s):  
Kh.I. Gasanov ◽  
S.I. Nurullayeva ◽  
Z.H. Babayev

New complex compounds of palladium (II) with biologically active ligand 2 - ethyl - 6 methyl - 3 - hydroxy-pyridine - mexidol in acidic medium (pH = 5,3) of the following composition have been synthesized – . In this case, the ligand is protonated and as a single-charged cation occupies an external coordination sphere. The structure of the complex is proved by X-ray structure analysis. It is shown that the structure is constructed of an isolated complex anion – and cation . The square planar coordination of the palladium atom is formed from three chlorine atoms and the formed tetraacidoanion ligand forms a hydrogen bond. The average length of Pd-Cl bond is 2, 3030 , there are no deviations from 900 valence angles of Cl-Pd-Cl. The palladium atom is not shifted from the plane coordination polyhedron (square) and therefore trance angles of Cl-Pd-Cl are 1800. Two different lengths -2,289 and 2,713 of hydrogen bonds are related to the geometric location of the ligand functional group. The obtained 2 – ethyl – 6 – methyl – 3 -hydroxypyridinetrachloro - palladium - mexidazole was tested for radioprotective properties. Toxicity of the preparation is LD50 - 240 mg/kg of animal weight. Toxicological studies of mexidazole in mice, rats and dogs did not reveal cardiotoxic, immunotoxic, embryonic, nephrotoxic, hematoxic and other types of side effects. Mexidazole is removed from the body with urine 5-8 hours after intravenous injection. The carried out biological test showed that the compound, along with radioprotective properties, has some antitumor activity.


1984 ◽  
Vol 39 (12) ◽  
pp. 1633-1641 ◽  
Author(s):  
Bernt Krebs ◽  
Andreas Schäffer ◽  
Siegfried Pohl

The novel anion SeBr42- was prepared by dissociation of SeOBr2 with formation of SeBr2 and subsequent reaction with bromide in acetonitrile solution; it was isolated as the crystalline tetraphenylphosphonium salt. The X-ray structure analysis of [P(C6H 5)4]2SeBr4 (space group P 1̄ , a = 14.190(3), b = 15.125(3), c = 10.383(2) Å , α = 92.69(2), β = 100.89(2), γ = 92.04(2)° Å , V = 2182.2 Å3) shows the structure to contain monomeric SeBr42- anions with a square planar coordination of Se(II). The mean Se -Br bond length in the anion is 2.598 Å .[P(C6H5)4]2Se2Br6 was obtained from the reaction of SeBr4 (which is in equilibrium with SeBr2, Se2Br2, and Br2, in solution) and bromide in acetonitrile. It crystallizes in the space group P 1̄, with a = 1 0 . 9 3 3 ( 4 ) , = 11.154(4), c = 10.344(4) Å , α = 79.26(3), β = 72.63(3), y = 81.35(3)°, γ = 1176.7 Å3 (at -120 °C), and contains a novel type of centrosymmetric Se2Br62- ions with square planar Se-coordination. The mean terminal and bridging Se -Br bond lengths are 2.442 and 2.799 Å , resp. Vibrational spectra are reported and discussed.


1995 ◽  
Vol 50 (6) ◽  
pp. 879-883 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of Ag0.5Cu3V0,5Mo2,5O12 have been prepared by crystallization from melts and investigated by X -ray methods. They crystallize with triclinic symmetry, space group Ci1 -P 1̄ , a = 6.797(6), b = 8.575(6), c = 9.897(7) Å, α = 103.47(6), β = 103.69(6), γ = 101.48(6)° and Z = 4. The crystal structure is characterized by chains of edge-sharing CuO6 octahedra and CuO5 pyramids. Special features of this com pound are the square planar surrounding of Ag+ by O2− and a statistical distribution of molybdenum and vanadium at one point position.


1992 ◽  
Vol 47 (11) ◽  
pp. 1505-1512 ◽  
Author(s):  
Thorsten Gebauer ◽  
Gerlinde Frenzen ◽  
Kurt Dehnicke

The crystal structures of the title compounds were solved by X-ray methods.[Pd(CH3CN)4](BF4)2: Space group Pbca, Z = 4,812 observed unique reflections, R = 0.057, wR = 0.033. Lattice dimensions at -80 °C: α = 1027.5(5), b = 1242.8(6), c = 1280.3(6) pm. The compound consists of planar [Pd(CH3CN)4]2+ ions with Pd-N bond lengths of 195.6 pm and BF4- anions.[PdCl(μ2-PPh2(HPPh2)]2 • CH2Cl2 crystallizes in two polymorphic forms in the same space group type but with different cell parameters, which depends on the conditions of the synthesis. α-form: Space group P21/c, Z = 4, 4680 observed unique reflections, R = 0.041, wR = 0.033. Lattice dimensions at -80 °C: a = 937.2(2), b = 1750.3(6), c = 1593.9(5) pm, β = 106.32(2)°. β-form: Space group Ρ21/n, Ζ = 4, 2519 observed unique reflections, R = 0.105, wR = 0.067. Lattice dimensions at -80 °C: a = 1118.0(4), b = 1222.4(3), c = 1849.9(4) pm, β = 90.72(2)°. Both polymorphs contain centrosymmetric molecules [PdCl μ2- PPh2)(HPPh2)]2 with Pd-P bond lengths of 226.6 pm for the bridging PPh2 groups and Pd-P bond lengths of 232.2 pm for the terminal HPPh2 ligands.[PdCl(HPPh2){H(OPPh2)2}]: Space group Pbca, Z = 8,3673 observed unique reflections, R = 0.038, wR = 0.032. Lattice dimensions at -80 °C: a = 1736.6(3), b = 1874.4(4), c = 1983.1(4) pm. The palladium atom has planar coordination consisting of the chlorine atom, the phosphorus atom of the HPPh2 ligand (Pd-P bond length 235.5 pm), and by the two phosphorus atoms of the H(OPPh2)2 chelate (Pd-P bond lengths 225.9 and 231.0 pm).


1996 ◽  
Vol 61 (9) ◽  
pp. 1335-1341 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová

The crystal structure of [(η4-C8H12)PdBr2] has been determined by a single crystal X-ray diffraction with R = 3.82% for 2 147 independent diffractions. The compound crystallizes with the symmetry of orthorhombic space group P212121 (No. 19) within the following parameters: a = 7.0785(5) Å, b = 11.1896(9) Å, c = 12.514(1) Å, V = 991.2(1) Å3, Z = 4. The square planar arrangement of ligands around Pd(II) is distorted due to the steric requirements of 1,5-cyclooctadiene in a twisted boat conformation. Formula units are joined by the weak C2-H2...Br1(1 + x, y, z) hydrogen bonds.


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