Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

1983 ◽  
Vol 38 (3) ◽  
pp. 347-349 ◽  
Author(s):  
Herbert W. Roesky ◽  
Pierre Schäfer ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms ◽  
C Nmr

Abstract The six membered ring of composition (CH3)2NCN3S2Cl2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1H, 13C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P21/c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C2N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

scholarly journals New Spiro-Tin Compounds: Reaction of N,N′-Dialkyl Sulfur Diimides with Cyclic Bis(amino)stannylenes - Unexpected Formation of a N-N Bond

1995 ◽  
Vol 50 (12) ◽  
pp. 1811-1817 ◽  
Author(s):  
Max Herberhold ◽  
Christian Köhler ◽  
Wolfgang Milius ◽  
Bernd Wrackmeyer
Keyword(s):  
Molecular Structure ◽  
Magnetic Resonance ◽  
Single Crystal ◽  
Structure Analysis ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Unexpected Formation ◽  
Tin Compounds ◽  
X Ray ◽  
Tert Butyl

N,N′-Dialkyl sulfur diimides (1), R(NSN)R [R = Me (a), Et (b), nPr (c), nBu (d)] react with cyclic bis(amino)stannylenes such as 1,3-di-tert-butyl-4,4-dimethyl-1,3,4,2λ2-diazasilastannetedine (2) or 1,3-di-tert-butyl-4,4,5,5-tetramethyl-1,3,4,5,2λ2-diazadisilastannolidine (3) in a 2:1 ratio to give the new spiro-tin(IV) compounds 5a-d, 6b and 6c, built from the respective cyclic bis(amino)stannylene and a seven-membered ring in which the two sulfur diimide groups are coupled via a N-N bond and across the tin atom. A 1:1 adduct 4 is proposed as an intermediate which is the final product 4e in the case of R = tBu (1e). The products were characterized by multinuclear magnetic resonance (1H, 13C, 15N, 29Si, 119Sn NMR), and in the case of 5c the molecular structure was determined by single crystal X-ray structure analysis [monoclinic, space group C2/c ; a = 1504.1(3), b = 1393.3(3), c = 1688.6(3) pm; β = 115.71(3)°].

Crystal and molecular structure of Z- and E-1,2-dichloro-1,2-bis(2-chlorophenyl)ethylene. An X-ray and NMR study

1995 ◽  
Vol 73 (9) ◽  
pp. 1520-1525
Author(s):  
Luciano Antolini ◽  
Ugo Folli ◽  
Dario Iarossi ◽  
Adele Mucci ◽  
Silvia Sbardellati ◽  
...  
Keyword(s):  
Chemical Shifts ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Study ◽  
Phenyl Rings ◽  
A Cell ◽  
C Nmr

The crystal structures of the title compounds were determined by single crystal X-ray diffraction techniques. The molecule of the Z isomer, which crystallizes in the monoclinic space group C2/c with Z = 4 in a cell of dimensions a = 14.891 (2), b = 10.780(2), c = 8.769(1) Å, β = 97.47(2)°, V = 1395.7(7) Å3 has crystallographic twofold symmetry. The E form crystallizes in the orthorhombic space group Pbca with a = 11.730(1), b = 6.932(1), c = 16.841(1) Å, V = 1369.4(2) Å3 and Z = 4. Its molecules have crystallographically dictated [Formula: see text] symmetry. In both isomers the phenyl rings are roughly perpendicular to the average ethylene plane. The atoms characterizing this plane show significant deviations from planarity in the Z isomer. Marked bond-angle distortions at the ethene carbons of both structures are observed. The 1H and 13C NMR spectra of the compounds were measured and, particularly in the case of the 1H chemical shifts, fall into two quite separate spectral regions. At low temperature, two conformational isomers, those with different relative orientation of the C—Cl bonds of the phenyl rings, are observed in the spectrum of each compound. Keywords: chlorostilbenes, overcrowded molecules. X-ray structure, conformations, NMR spectroscopy.

scholarly journals Preparation and Crystal Structure of Zinc Bis[orotate(1–)] Octahydrate

1993 ◽  
Vol 48 (7) ◽  
pp. 961-964 ◽  
Author(s):  
Otto Kumberger ◽  
Jürgen Riede ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Medical Treatment ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Structure Analysis ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

A discrete zinc bis[orotate(1—)] complex of the composition Zn(OrH)2·8 H2O has been isolated and characterized by a single-crystal X-ray structure analysis. The crystals are monoclinic, space group P21/c (No. 14), Z = 2, a = 10.884(2), b = 12.896(1), c = 6.954(1) Å, β = 98.27(1)°. The crystal lattice features hexaquo complexes of zinc, the Zn(H2O)62+ cations being associated with two hydrated OrH- ions only through hydrogen bonds. The results are relevant for applications of zinc orotates in medical treatment.

Crystal structure of zerumbone [(E,E,E)-2,6,9,9-Tetramethylcycloundeca-2,6,10-trien-1-one]

1981 ◽  
Vol 34 (10) ◽  
pp. 2243 ◽  
Author(s):  
SR Hall ◽  
S Nimgirawath ◽  
CL Raston ◽  
A Sittatrakul ◽  
S Thadaniti ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Zingiber Zerumbet ◽  
Space Group ◽  
X Ray ◽  
Considerable Distortion

The crystal structure of zerumbone, C15H22O, extracted from the rhizomes of Zingiber zerumbet Smith, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.051 for 925 'observed' reflections. Crystals are monoclinic, space group P21/c, a 9.036(3), b 9.712(5), c 15.643(6) �, β 97.19(3)�, Z = 4. Although the molecule has no chiral centre, the presence of the three trans double bonds confers considerable distortion and rigidity on the eleven-membered ring and renders the whole molecule chiral and potentially resolvable.

Synthese Und Kristallstrukturen Von Chlorometallaten [M = V(III), Mo(V)]

2001 ◽  
Vol 56 (8) ◽  
pp. 759-764 ◽  
Author(s):  
Soheila Chitsaz ◽  
Effat Iravani ◽  
Jochen Pauls ◽  
Bernhard Neumüller
Keyword(s):  
Ir Spectroscopy ◽  
Membered Ring ◽  
Dinuclear Complex ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Independent Molecules ◽  
Triclinic Form

[(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)]-

Silaheterocyclen: Molekülstruktur eines 3-Oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptans / Silaheterocycles: Molecular Structure of a 3-Oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptane

1989 ◽  
Vol 44 (7) ◽  
pp. 796-799 ◽  
Author(s):  
Gabriele Reber ◽  
Jürgen Riede ◽  
Nils Wiberg ◽  
Gerhard Wagner ◽  
Gerhard Müller
Keyword(s):  
Molecular Structure ◽  
Dihedral Angle ◽  
Structure Analysis ◽  
Membered Ring ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

According to an X-ray structure analysis 1,5-bis(di-tert-butylmethylsilyl)-2,2,4,4,6,6,7,7-octamethyl-3-oxa-2,4,6,7-tetrasilabicyclo[3.1.1]heptane (1) is a rigid bicyclic molecule consisting of a 1,3-disilacyclobutane ring whose 2,4 positions are bridged by a Me2Si—O—SiMe2 fragment. The four-membered ring is non-planar with a dihedral angle of 33.8° along the C—C axis. The intraring valence angles at carbon are significantly smaller than those at silicon leading to a transannular Si ··· Si distance of only 2.558(1) Å (triclinic, space group P 1̄ with a = 9.125(2), b = 12.668(2), c = 15.499(3) Å, α = 101.25(1), β = 87.87(1), γ = 96.88(1)°, V = 1744.4 Å3 R (wR) = 0.044 (0.051) for 316 refined parameters and 5156 observables).

Binuclear Fulvalene and Bis(cyclopentadienyl)methane Halfsandwich Complexes of Manganese and Rhenium Containing Tetrahydrothiophene Ligands. X-Ray Structure Analysis of {(CO)2Mn[C5H4-C5H4]Mn(CO)2}(μ-SC4H8)

1993 ◽  
Vol 48 (2) ◽  
pp. 161-170 ◽  
Author(s):  
Max Herberhold ◽  
Martin Biersack ◽  
Thomas E. Bitterwolf ◽  
Arnold L. Rheingold
Keyword(s):  
Molecular Structure ◽  
Ir Spectra ◽  
Structure Analysis ◽  
Nmr Spectra ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Tetrahydrofuran Solution ◽  
C Nmr

AbstractThe photo-induced substitution of carbonyl ligands in the binuclear cyclopentadienyl-type complexes (CO)3M[C5H4(CH2)nC5H4]M(CO)3 (n = 0 (fulvalene), M = Mn (1) and Re (2); n = 1 (bis(cyclopentadienyl)methane), M = Mn (3) and Re (4)) has been studied in the presence of tetrahydrothiophene, SC4H8 (tht). Photodecarbonylation of 1 - 4 in tetrahydrofuran solution leads to solvent-stabilized intermediates which react with tht in the dark to give monosubstituted derivatives (CO)3M[C5H4(CH2)nC5H4]M(CO)2(tht) (1a - 4a). In the case of M = Mn, thtbridged compounds {(CO)2Mn[C5H4(CH2)nC5H4]Mn(CO)2}(μ-tht) (n = 0 (1b) and n = 1 (3b)) are also obtained which are the exclusive products of the photolysis of 1 and 3 in benzene in the presence of tht. Photodecarbonylation of 1 - 4 in neat tetrahydrothiophene produces disubstituted derivatives in the case of manganese, (tht)(CO)2Mn[C5H4(CH2)nC5H4]Mn(CO)2(tht) (n = 0 (1c) and n = 1 (3c)), whereas only the monosubstituted complexes 2a and 4a could be isolated in the case of rhenium. The molecular structure of the tht-bridged fulvalene complex 1b has been determined by an X-ray structure analysis. A special reaction of dimethyl disulfane with the photolyzed tetrahydrofuran solution of 2 leads to the bis(methylthiolato) compound (CO)3Re[C5H4- C5H4]Re(CO)(SMe)2 (5). The new complexes were characterized by their IR spectra v(CO) and their 1H and 13C NMR spectra.

Notizen: Darstellung und Kristallstruktur von [H3N(CH2)3NH3]SbCl5 / Preparation and Crystal Structure of [H3N(CH2)3NH3]SbCl5

1989 ◽  
Vol 44 (9) ◽  
pp. 1151-1154 ◽  
Author(s):  
André du Bois ◽  
Walter Abriel
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Intensity Data ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms

Using 293 K diffractometer intensity data, the structure of [H3N(CH2)3NH3]SbCl5 has been determined by single crystal X-ray technique and refined to a final Rw of 0.026. The colorless crystals are monoclinic (space group P21/c) with a = 10.1338(5), b = 11.4623(7), c = 11.3668(6) Å, β = 113.52(5)° and Ζ = 4. The structure contains ψ-octahedral SbCl52- anions. A center of symmetry connects two anions forming a (Sb2Cl10)4- unit with rather long Sb—Cl distances for the bridging Cl-atoms (2.92 and 3.68 A, respectively).

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

scholarly journals Kristallstrukturen der Tetrachloroniccolate (PPh4)2[NiCl4] und [Na-15-Krone-5]2[NiCl4] / Crystal Structures of the Tetrachloroniccolates (PPh4)2[NiCl4] and [Na- 15-Crown-5]2[NiCl4]

1990 ◽  
Vol 45 (7) ◽  
pp. 995-999 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Cl Atoms

The title compounds were obtained from NiS + PPh4Cl + HCl in dichloromethane, from NiCl2 and PPh4Cl and from NiCl2 + Na2S + 15-crown-5 in acetonitrile or CH2Cl2, respectively. Their crystal structures were determined by X-ray diffraction. (PPh4)2[NiCl4]: monoclinic, space group C 2/c, Z = 4, a = 1094.9(3), b = 1946.1(4), c = 2033.5(5) pm, β = 91.48(3)°; R = 0.07 for 2895 unique observed reflexions. [Na-15-crown-5]2[NiCl4]: triclinic, space group P1̄, Z = 2, a = 987.6(1), b = 998.0(1), c = 1779.9(2) pm, α = 104.17(1), β = 95.43(1), γ = 109.95(1)°; R = 0.090 for 4155 unique observed reflexions. In both cases, the [NiCl4]2- ions have distorted tetrahedral structures. With PPh4+ as the cation the distortion corresponds to a twisted tetrahedron which fulfils the point symmetry D2, the deviation from a flattened D2d-tetrahedron being small. In (PPh4)2[NiCl4] cations and anions alternate in layers parallel to (001). In [Na-15-crown-5]2[NiCl4] two of the Cl atoms of the anion are coordinated to sodium ions; one of the crown ether molecules shows positional disorder.

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