Kristall- und Molekülstruktur von Bis(pyridin)bis(trifluoromethyl)zink

Crystal and Molecular Structure of Bis(pyridine)bis(trifluoromethyl)zinc Bis(pyridin)bis(trifluoromethyl)zinc 1 has been isolated and characterized by means of single-crystal X-ray diffraction techniques. The title compound represents the first structure determination of a fully fluorinated alkylzinc compound (monoclinic, space group P2₁/c, Z = 4, a = 8.856(3), b = 18.158(3), c = 8.979(3) Å, β = 98.14(2)°, R = 0.054, R_w = 0.035). The zinc atom is in a distorted tetrahedral environment. The molecular structure of [ClZn(CCl₂CF₃) η₂O]₂ 2 was solved, but is not included in a structural comparison due to crystallographic disorder.     

Kristall- und Molekülstruktur von Tris(1,1-diethyl-3-benzoyl-thioureato)ruthenium(III)

Crystal and Molecular Structure of Tris(1,1-diethyl-3-benzoyl-thioureato)ruthenium(III) The crystal and molecular structure of tris(1,1-diethyl-3-benzoyl-thioureato)-ruthenium(III) has been determined by an X-ray structure analysis. The compound crystallizes in the trigonal space group P3 with a = 16.556, c = 8.476 Å and Z = 2. The structure was solved by Patterson methods and refined to a final R value R = 0.074 for 801 observed reflections. The molecule has the symmetry C₃. The coordination polyhedron is an octahedron with facial arrangement of the ligator atoms. The Ru? S and Ru? O distances are 2.293 Å and 2.047 Å, respectively.     

Kristall- und Molekülstruktur von Bis(1,1-diethyl-3-thiobenzoyl-thioureato)nickel(II)

Crystal and Molecular Structure of Bis(1,1-diethyl-3-thiobenzoyl-thioureato)nickel(II). Bis(1, 1-diethyl-3-thiobenzoyl-thioureato)nickel(II) forms two modifications, whose structures have been determined by X-ray structure analysis. The monoclinic modification crystallizes in the space group P2₁/n with a = 13.709, b = 8.571, c = 12.803 Å, β = 68.10° and Z = 2. The triclinic modification crystallizes in the space group I1 with a = 14.406, b = 7.761, c = 11.734 Å, α = 86.10, β = 97.39, γ = 90.18° and Z = 2. The molecular structures of both modifications are nearly identical (packing polymorphism). The coordination is exactly planar, the ligands are arranged in trans position. The average Ni? S bond length is 2.153 Å in the monoclinic form and 2.163 Å in the triclinic form. The chelate rings deviate from planarity.     

Kristall- und Molekülstruktur von Bis(N,N-diethyl-2-benzoylthioacetamidato)kupfer(II)

Crystal and Molecular Structure of Bis(N, N-diethyl-2-benzoylthioacetamidato)copper(II) Bis(N, N-diethyl-2-benzoyl-thioacetamidato)copper(II) has been investigated by X-ray structure analysis. It crystallizes in the triclinic space group P1 with a = 10.709, b = 12.150, c = 15.651 Å, α = 90.13, β = 103.73, γ = 98.30° and with 3 formula units per unit cell. The structure was solved by heavy atom technique. The final R value was 0.04 for 4151 symmetry independent reflections. The crystal contains two symmetry independent molecules. One of them shows a nearly planar cis-arrangement of the ligator atoms but the other has an exactly planar trans-arrangement. The chelate rings show a distorted planarity in both molecules. The results of the structure determination confirm the conclusions from the EPR crystal spectrum.     

Kristall-und Molekülstruktur von Bis(1,1-diäthyl-3-benzolyl-thioureato)kupfer(II)

Crystal and Molecular Structure of Bis(1,1-diethyl-3-benzoyl-thioureato)copper(II) Bis(1,1-diethyl-3-benzoyl-thioureato)copper(II) exists in three monoclinic modifications, of which the crystallographic data have been determined. The crystal and molecular structure of one of the three modifications has been determined by X-ray structure analysis. This modification crystallizes in the space group P2₁/c with a = 8.871, b = 29.492, c = 12.281 Å, β = 124.50° and with 4 formula units per unit cell. The structure was solved by heavy atom technique and refined to a final R value of R = 0.05. The coordination polyhedron is a distorted tetrahedron. The S and O atoms are arranged in cis position. The chelate rings are not planar but distorted in characteristic manner.     

Molekülstruktur von 2,2-Bis(diisopropoxyphosphonyl)propyl-methylzinndibromid

Molecular Structure of 2,2-Bis(diisopropoxyphosphonyl)propyl Methyltin Dibromide By methylation of Me₃SnCH₂CH[P(O)(OPr?i)₂]₂ with NaH/MeI Me₃SnCH₂C(Me)[P(O)(OPr?i)₂]₂ ( 1 ) is obtained, which is converted by bromine into the dibromide MeBr₂SnCH₂C(Me)[P(O)(OPr?i)₂]₂ ( 2 ). An X-ray crystal structure analysis shows 2 to be monomeric. The tin atom is situated in the centre of a distorted octahedron, in which the functional substituent is intramolecular coordinated as tridentate ligand in a facial mode. The two organo groups are arranged in trans-position (C? Sn? C 155.1°), whereas the oxygen and bromine atoms are orientated cis to each other. The six-membered ring of the bicyclic molecular fragment of 2 which results from the coordination of the functional organo group to the tin atom shows a boat-conformation, whereas the two five-membered rings exist in twist-conformations. Multinuclear n.m.r. and i.r. data show that 2 retains its solid state structure also in nonpolar solvents.     

Chelate von Chinolin-8-ol-Derivaten. XII. Die Kristall- und Molekülstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II)

Chelates of 8-Quinolinol Derivatives. XII. Crystal and Molecular Structure of Bis(7-isopropyl-8-quinolinato)nickel(II) The crystal and molecular structure of bis(7-isopropyl-8-quinolinato)nickel(II) was determined by X-ray diffraction. The structure is monoclinic with the space group P2₁/n (Z = 2, 1403 observed independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 1328.3(5) pm, b = 632.8(2) pm, c = 1330.0(5) pm, β = 112.99(3)°). The coordination of the nickel atom is planar with the quinoline rings in trans position.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-benzamidin]silber(l)-nitrat

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-benzamidine]-silver(I) Nitrate The crystal structure of bis[N-(diethylaminothiocarbonyl)-benzamidine]silver(I) nitrate has been determined by X-ray structure analysis on a single crystal. The compound is monoclinic, space group P2₁/n with a = 12.541, b = 43.470, c = 11.096 Å, β = 106.27° and 8 formula units per unit cell. The structure was solved by application of direct methods to difference structure factors (DIRDIF) and refined for 5242 observed reflections to a final R value of R = 0.070. There are two symmetrically independent molecules of the title compound in the asymmetric unit. The central Ag ion is coordinated by the S atoms of two ligands. The nitrate ions do not coordinate. The coordination geometry is slightly bent.     

Zur Umsetzung von Bis(2-mercaptoethyl)phosphinen mit Organozinn-Verbindungen Molekülstruktur eines zinnhaltigen Sechzehnringes

Reaction of Bis(2-mercaptoethyl)phosphines with Organotin Compounds. Molecular Structure of a Tin Containing Sixteen-membered Ring The reaction of bis(2-mercaptoethyl)phosphine with di-t-butyltin dimethoxide yields mixture of oligomers of the type [t-Bu₂Sn(SCH₂CH₂)₂Pr]_n (R ? Me, Ph) from which the trans-configurated dimers (n = 2) have been isolated. By the reaction with sulphur and selenium, respectively, these dimers were transformed to the corresponding thioxo and selenoxo derivatives. The sixteen-membered ring trans-[t-Bu₂Sn(SCH₂CH₂)₂P(S)Ph]₂ crystallizes in the space group P2₁/n with the unit cell dimensions a 1350.9, b 1310.2, c 1500.3 pm, β 96.36° and does not exhibit any intramolecular Sn? P interaction: The 1,5-diorgano-1-chloro-5-elementa-1-stanna(IV)-bicyclo-[3.3.0^1,5]octanes R(Cl)Sn(SCH₂CH₂)₂E ( 6 , R ? Ph, E ? PPh; 7 , R ? Ph, E ? NMe) have been prepared from the corresponding sodium dithiolates and phenyltrichlorostannane. The transannulare Sn? P and Sn? N interactions in 6 and 7 are confirmed by ³¹P and ¹¹⁹Sn NMR investigations.     

Synthese und Molekülstruktur chiraler Bis(1,3,2‐dioxaphospholane)

Synthesis and Molecular Structure of Chiral Bis(1,3,2‐dioxaphospholanes) Bisphosphites of the general type C₂O₂POC_nOPO₂C₂ containing chiral building blocks both in the five‐membered C₂O₂P rings and in the OC_nO bridge were prepared from 2‐chloro‐1,3,2‐dioxaphospholanes and chiral diols in the presence of a base. The molecular structure of compound 10 , which was obtained from 2‐chloro‐(4R,5R)‐4,5‐dimethyl‐1,3,2‐dioxaphospholane and (R)‐1,1′‐binaphthalin‐2,2′‐diol, was determined by X‐ray crystallography.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato]nickel(II)

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benz-amidinato]nickel(II) The structure of bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]-nickel(II) has been determined by X-ray structure analysis. The compound crystallizes in orthorhombic space group P2₁2₁2₁ with a = 16.36, b = 16.94, c = 12.96 Å and Z = 4. The solution of the structure was performed by heavy atom technique and gave a final R value of R = 0.055 for 1764 observed reflections. The coordination polyhedron has a tetrahedrally distorted shape. The ligator atoms are arranged in cis position. The chelate rings deviate clearly from planarity. Against the chelate rings the phenyl rings are appreciably twisted. The title compound is compared regarding its structure with the analogous copper chelate.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato]kupfer(II)

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]copper(II) The structure of bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]-copper(II) has been determined by X-ray structure analysis. The compound crystallizes in the orthorhombic space group Pbca with a = 27.792, b = 19.197, c = 12.325 Å and 8 formula units per unit cell. The structure was solved by heavy atom technique. The final R value was R = 0.06 for 1589 observed symmetry independent reflections. The coordination polyhedron is a distorted tetrahedron. In spite of the bulky phenyl groups the ligator atoms are arranged in cis position. The chelate rings deviate clearly from planarity. The phenyl rings are appreciably twisted against the chelate rings.     

Kristall- und Molekülstruktur von Tetra-n-butylammonium-N-methyl-N-thioformyldithiocarbamat

Crystal and Molecular Structure of Tetra-n-butylammonium N-Methyl-N-Thioformyl Dithiocarbamate [N(n-C₄H₉)₄][S₂C? N(CH₃)? CS? H] crystallizes in the triclinic space group P1 (Z = 2) with cell dimensions (?45°C) a = 9.185(2) Å, b = 10.263(3) Å, c = 13.301(3) Å, α = 101.73(2)°, ß = 99.59(2)°, γ 100.57(2)°. The crystal structure was solved by means of direct methods and refined to a conventional reliability index R = 0.066 (R_ω = 0.070). 5945 independent intensities being measured.     

Die Kristall- und Molekülstruktur des Hexaphenyldiplumbans

Crystal and Molecular Structure of Hexaphenyldiplumbane The crystal and molecular structure of (C₆H₅)₆Pb₂ (space group and lattice parameters see above) has been newly determined from 4541 independent reflexes by the heavy atom method; the positions of all atoms, except the H atoms have been refined to give R = 0.053. The unit cell contains two crystallographically independent molecules. (Mean values of bond lengths and angles see above).