The preparation of 1,2,3,5-dithiadiazolium chlorides from the reaction of nitrile sulphides with thiazyl chloride

1994 ◽  
Vol 72 (4) ◽  
pp. 1143-1153 ◽  
Author(s):  
John N. Bridson ◽  
Steven B. Copp ◽  
Melbourne J. Schriver ◽  
Shuguang Zhu ◽  
Michael J. Zaworotko
Keyword(s):  
Crystal Structure ◽  
Cycloaddition Reaction ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Alkyl Derivatives ◽  
First Time

Adamantyl-1,3,4-oxathiazol-2-one has been prepared for the first time and from it 1-adamantyl nitrile sulphide has been generated. Characterisation data are presented, including the X-Ray crystal structure of the oxathiazolone. (Crystal data for C12H15NO2S: monoclinic, space group P21/c, a = 11.334(2) Å,b = 7.344(1) Å, c = 14.373(2) Å,β = 107.74(1)°, V = 1139.5(3) Å3, Z = 4, R = 0.042). The planar heterocyclic ring is similar to structures observed in the gas phase for other oxathiazolone derivatives. The nitrile sulphide was reacted with dimethyl-acetylene dicarboxylate in situ to give an isothiazole derivative. The X-Ray crystal structure of 3-adamantyl-4,5-bis(methoxycarbonyl)-isothiazole has been obtained. (Crystal data for C17H21NO4S: monoclinic, space group P21/n, a = 7.305(4) Å, b = 7.339(4) Å, c = 31.552(4) Å, β = 92.75(3)°, V = 1690(1) Å3, Z = 4, R = 0.079). A general cycloaddition reaction was discovered between the nitrile sulphides and thiazyl chloride to give 1,2,3,5-dithiadiazolium chlorides. The structure of the new 4-adamantyl-1,2,3,5-dithiadiazolium chloride was confirmed by reduction to the 4-adamantyl-1,2,3,5-dithiadiazolyl for which the X-Ray crystal structure has been determined. (Crystal data for C11H15N2S2: monoclinic, space group C2, a = 10.284(4) Å, b = 8.651(2) Å, c = 13.669(2) Å, β = 112.83(1)°, V = 1120.9(4) Å3, Z = 4, R = 0.042). The radical adopts a twisted dimer structure in the solid state which is similar to the structures observed for other alkyl derivatives.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse polymerer 1:1-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen / Crystal Growth in Gels and X-Ray Characterization of Polymeric 1:1-Complexes of CuBr2 and CuCl2 with Pyrazine

1989 ◽  
Vol 44 (5) ◽  
pp. 553-556 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Growth ◽  
Chloro Complex ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Linear Chains

Single crystals of Cu(pz)Br2 and Cu(pz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a = 1239.2(3) pm, b = 685.9(2) pm, c = 390.7(3) pm, β = 96,23(5)°. Crystal data for the chloro-complex: monoclinic, space group C2/m with a = 1197.1(3) pm, b = 684.9(3) pm, c = 370.1(3) pm, β = 95.96(5)°. Crystal structure analyses reveal that CuHal2 molecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atoms.

Substitutionsreaktionen an der N-Chlornitrenogruppe des [WCl4(NCl)]2. Die Kristallstrukturen von [CH3CN—WCl4(NSMe)] und [WNCl3 · NC—CH3]4 / Substitution Reactions at the N-Chloronitreno Group of [WCl4(NCl)]2. The Crystal Structures of [CH3CN—WCl4(NSMe)] and [WNCl3 · NC—CH3]4

1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Crystal Data ◽  
Substitution Reactions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).

Schwermetall-π-Komplexe II [1] Arenkomplexe des Quecksilbers(I)

1987 ◽  
Vol 42 (7) ◽  
pp. 828-834 ◽  
Author(s):  
W. Frank ◽  
B. Dincher
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Aluminium Trichloride

Abstract The crystalline compounds [(CH3C6H5)2Hg,][AlCl4]2 (1), [(1,2-(CH3)2C6H4)2Hg2][AlCl4]2(2), [(1,3,5-(CH3)3C6H3)2Hg2][AlCl4]2 (3), [1,2,4,5-(CH3)4C6H2Hg2][AlCl4]2 (4) and [((CH3)6C6)2Hg2][AlCl4]2-CH3C6H5 (5) have been prepared from mercury(I)chloride, aluminium trichloride and the corresponding arenes and characterized by elem ental analysis. The crystal structure of 5 has been determ ined from single crystal X-ray diffraction data and refined to R - 0.093 for 3269 unique reflections. Crystal data: monoclinic, space group P21/c, a = 2116(1), b = 1095.1(7), c = 1880(1) pm, β - 104,9(1)°, Z = 4. Each atom of a central Hg2 unit (Hg -Hg distance 251.5 pm) is asymmetrically complexed by hexamethylbenzene, the Hg - Carene distances being in the range from 241 to 340 pm. Two distorted AlCl4 tetrahedra complete a “molecular” [arene2Hg2][AlCl4]2 unit. The shortest Hg-Cl distances are 310 and 312 pm, respectively.

Benzothiarsolium cations: evidence for pπ-bonding between arsenic and sulfur in the first structurally characterized arsenium system

1992 ◽  
Vol 70 (3) ◽  
pp. 703-709 ◽  
Author(s):  
Neil Burford ◽  
Trenton M. Parks ◽  
Bruce W. Royan ◽  
John F. Richardson ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Keywords Arsenic

Tetrachloroaluminate salts of the benzothiazarsolium and toluodithiarsolium heteronaphthalenic cations have been prepared from the corresponding chloroarsoles by a routine halide ion abstraction procedure. Characterization data are presented, including the X-ray crystal structure of the thiaza derivative. (Crystal data for C6H5AlAsCl4NS: monoclinic, space group P21/c, a = 6.4259(5) Å, b = 23.654(3) Å, c = 8.5859(7) Å, β = 98.203(6)°, V = 1291.7(2) Å3, Z = 4, R = 0.054.) A planar bicyclic cationic unit is observed, typical of other heteronaphthalenic systems. The crystal structure of 2-chlorobenzo-1,3,2-thiazarsole has been obtained for direct comparison, and also has a close to planar heterobicyclic moiety. (Crystal data for C6H5AsClNS: monoclinic, space group P21/c, a = 8.370(3) Å, b = 10.829(3) Å, c = 8.756(2) Å, β = 95.99(2)°, V = 789.2(3) Å3, Z = 4, R = 0.025.) The planarity and short heterocyclic bond lengths observed in the two compounds imply a significant degree of pπ bonding, which is unique between sulfur and arsenic. In addition, the cation is a rare example of a structurally characterized cationic dicoordinate arsenic, or arsenium, system. Keywords: arsenic, arsolium, arsenium, pπ-bonding, sulfur, heteronaphthalenic.

Preparation and X-ray crystal structures of the arsenic pentafluoride adducts of benzo-2,1,3-thiadiazole and benzo-1,2,3-thiadiazole

1986 ◽  
Vol 64 (5) ◽  
pp. 849-853 ◽  
Author(s):  
Allen Apblett ◽  
Tristram Chivers ◽  
John F. Richardson
Keyword(s):  
Nitrogen Atom ◽  
Crystal Structures ◽  
Benzene Ring ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

The reaction of arsenic pentafluoride with benzo-2,1,3-thiadiazole, 1, or benzo-1,2,3-thiadiazole, 2, in liquid SO2 gave 1:1 adducts that were characterized spectroscopically (infrared and 13C nmr) and by X-ray crystallography. Crystal data: for 1•AsF5, monoclinic, space group P21/n, a = 6.932(1), b = 9.113(1), c = 15.136(2) Å, β = 98.035(7)°, V = 946.8(2) Å3, Z = 4; for 2•AsF5, monoclinic, space group P21/a, a = 7.573(2), b = 13.101(2), c = 9.514(3) Å, β = 90.95(2)°, V = 943.9(4) Å3, Z = 4. The coordination of AsF5 to one of the nitrogen atoms in 1 introduces asymmetry in the heterocyclic ring, with the longer bond lengths being associated with the coordinated nitrogen atom, d(S—N) = 1.633(5) and 1.577(6) Å, d(C—N) = 1.364(7) and 1.339(8) Å. The quinonoid character of the benzene ring is still apparent in the adduct. In 2•AsF5, the AsF5 molecule is coordinated to the nitrogen atom that is bonded to carbon.

Die Kristallstruktur von Ytterbiumdisulfid: YbS2 / The Crystal Structure of Ytterbiumdisulfide: YbS2

1974 ◽  
Vol 29 (1-2) ◽  
pp. 16-19 ◽  
Author(s):  
Christoph L. Teske
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Structural Element ◽  
Thermal Synthesis ◽  
Space Group ◽  
X Ray ◽  
First Time ◽  
Atomic Parameters

X-ray investigations are described using a single crystal of YbS2 for the first time which formed during a ammono thermal synthesis. It crystallizes in the monoclinic space group C2h6-C2/c with a = 9,326, b = 4,754, c = 9,025 and β = 118,39°. The atomic parameters and a detailed description of the crystal structure are given. Especially the sulfur-sulfurbridges (dS-S = 2,11 A) represent a characteristic structural element in the a lattice of the genuine disulfide.

Metallorganische Verbindungen für MOCVD-Prozesse: Kristallstruktur des dimeren Addukts [Et3AsXAsCl3]2 / Crystal Structure of the Dimeric Triethylarsine-Arsenictrichloride Adduct, Dimer [Et3AsxAsCl3: Synthesis, Molecular and Crystal Structure

1989 ◽  
Vol 44 (5) ◽  
pp. 560-564 ◽  
Author(s):  
Gerhard Baum ◽  
Arnd Greiling ◽  
Werner Massa ◽  
Benjamin C. Hui ◽  
Jörg Lorberth
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Quantitative Yield ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Arsenic Atom ◽  
Space Group ◽  
X Ray

Reaction of Et3As with AsCl3 in n-pentane yields dimeric [Et3AsxAsCl3]2 in quantitative yield; sublimation in vacuo affords white crystals.X-Ray diffraction data were collected at 133 K (3149 independent observed reflections; R = 0.029. Rw = 0.026). Crystal data: monoclinic space group P21/c, a = 761.9(8). b = 1118.8(4). c = 1406.0(14) pm; β = 100.90(4)°. Ζ = 2 dimers.The dimer contains a planar As2Cl6-unit with terminal and bridging As-Cl bonds; each arsenic atom is bonded to a Et3As molecule via an arsenic-arsenic bond. The dimer thus has pseudo four- and six-coordinate arsenic atoms.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

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