Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

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.

Oxidationsreaktionen an ΧnB6Η6-n2-, Χ = Cl, Br, I; n = 1-6 und Kristallstrukturen von [(n-C4H9)4N]B6I6 und [(n-C4H9)4N]2B6I6 / Oxidation Reactions on XnB6H6-n2-, X = Cl, Br, I; n = 1-6, and Crystal Structures of [(n-C4H9)4N]B6I6 and [(n-C4H9)4N],B6I6

1990 ◽  
Vol 45 (2) ◽  
pp. 184-190 ◽  
Author(s):  
A. Heinrich ◽  
H.-L. Keller ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Magnetic Measurements ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Oxidation Reactions ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Deep Blue

By cyclic voltammetry investigations in acetonitrile solution it has been shown, that the halogenohydrohexaborates X„B6H6-n2-, X = Cl, Br, I; n = 1-6, undergo a one-electron oxidation to form the corresponding radical anions. The reactions are completely reversible only for the perhalogenated ions B6X62- and for trans-Br4Β6Η22-. The oxidation by Ce(IV) in CH3CN yields deep blue B6I6, orange B6Br6- and yellow green B6Cl6-, characterized by their UV-VIS, IR/Raman spectra and by magnetic measurements. The crystal structures of the paramagnetic, air-stable, blue-black [(n-C4H9)4N]B6I6 (I) and the diamagnetic, colourless [(n-C4H9)4N]2B6I6 (II) were determined from single crystal X-ray diffraction analyses. I is monoclinic, space group P21/c, with a = 14.398(7), b = 14.638(3), c = 16.511(6) Å, β = 109.24(1)° (at —50°C), containing two crystallographically independent centrosymmetric B6 entities, which are strongly distorted with B— B bond lengths between 1.63 and 1.91 and I— I between 2.02 and 2.22 A. II is monoclinic, space group P21, with a = 11.246(3), b = 15.576(4), c = 14.900(4) Å, β = 92.10(1)° (at 23 °C) and contains nearly regular octahedral anions with bond lengths B—B 1.64-1.68 and B—I 2.17-2.21 A.

The Crystal and Molecular Structures of Bis(diethyldithiocarbamato)platinum(II) and Bis[di(2-hydroxyethyl)dithiocarbamato]platinum(II)

1992 ◽  
Vol 45 (2) ◽  
pp. 429 ◽  
Author(s):  
AT Baker ◽  
MT Emett
Keyword(s):  
Single Crystal ◽  
Bond Length ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures

The structures of [Pt(S2CN(C2H5)2)2] (1) and [Pt(S2CN(C2H4OH)2)2] (2) have been determined by single-crystal X-ray diffractometry. Compound (1) crystallizes in the tetragonal space group P42/n, a 16.4692(10),c 6.2160(6) � (Z = 4); R was 0.029 for 1012 observed reflections. Compound (2) is monoclinic, space group Pc, a 6-0663(11), b 1.1784(15), c 12.5740(21) � ,β92.569(8)� (Z = 2); R was 0.019 for 1573 observed reflections. The presence of electron-withdrawing groups in the ligands of (2) appears to have little effect on the Pt-S distances but causes an increase in the C-N bond length, with the C-N bond lengths being significantly different at the 2 σ level.

On racemic and L-malates: a comparison of their crystal structures

2004 ◽  
Vol 219 (2) ◽  
Author(s):  
Michel Fleck ◽  
Ekkehart Tillmanns ◽  
Ladislav Bohatý ◽  
Peter Held
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray

AbstractThe crystal structures of eight different L-malates have been determined and refined from single-crystal X-ray diffraction data. The compounds are the monoclinic (space groupIn addition, for all the compounds, powder diffraction data were collected, analysed and submitted to the powder diffraction file (PDF).

Isoselenocyanatoborate -Kristallstrukturen von (n-Bu4N)[BH(NCSe)3] und (Ph4P)[B3H7(NCSe)] / Isoselenocyanatoborates -Crystal Structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]

1998 ◽  
Vol 53 (3) ◽  
pp. 271-274 ◽  
Author(s):  
B. Steuer ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Elemental Selenium ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Average Bond

Abstract The treatment of [B6H6]2- with an excess of (SCN)2 in dichloromethane in the presence of solid KOH gives the hexaisoselenocyanatodiborate anion [B2(NCSe)6]2- as an intermediate (δ(11B) = -10.3 ppm), from which [BH(NCSe)3]- and elemental selenium are formed. The X-ray structure determinations on single crystals of (n-Bu4N)2[BH(NCSe)3] (1) (triclinic, space group Pi with a = 8.512(2), b = 10.885(3), c = 14.895(4) Å, α = 79.52(2), β = 74.86(2), γ = 86.768(2)°, Z = 2) and (Ph4P)[B3H7(NCSe)] (2) (monoclinic, space group C2, a = 7.686(5), b = 10.366(3), c = 17.533(3) A, β = 108.89°, Z = 4) show that the selenocyanate groups are coordinated exclusively via the N atoms with average bond lengths of B-N = 1.52, C-N = 1.15, C-Se = 1.75 A and angles N-C-Se = 179°, B-N-C = 168.7 - 176.8°. The N-B-N angles of 1 range from 107.5 to 109.5°.

Synthesis and characterization of [MII(bqb)] (M = Co, Ni, Cu), [N(n-Bu)4][CoIII(bqb)(CN)2], and [N(n-Bu)4][CoIII(bqb)(N3)2] containing deprotonated N,N'-bis(2-quinolinecarboxamide)-1,2-benzene (bqb) – X-ray crystal structures of [NiII(bqb)] and [N(n-Bu)4][CoIII(bqb)(N3)2]

2006 ◽  
Vol 84 (7) ◽  
pp. 971-978 ◽  
Author(s):  
Soria Meghdadi ◽  
Mehdi Amirnasr ◽  
Vratislav Langer ◽  
Alison Zamanpoor
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Elemental Analyses

Cobalt(II), nickel(II), copper(II), and two cobalt(III) complexes of a new dianionic ligand, bqb, [H2bqb = N,N'-bis(2-quinolinecarboxamide)-1,2-benzene] have been synthesized and characterized by elemental analyses, IR, and 1H NMR spectroscopy. The crystal and molecular structures of the [Ni(bqb)] (2) and [N(n-Bu)4][CoIII(bqb)(N3)2] (5) complexes were determined by X-ray crystallography. Complex 2 crystallizes in the monoclinic space group C2/c with a distorted square-planar structure including two short Ni–N (1.848 Å) and two long Ni–N (1.958 Å) bonds. The structure consists of sheets formed in the plane parallel to the b axis and diagonal to vectors a and c by intermolecular hydrogen bonds. Complex 5 crystallizes in the monoclinic space group C2 with a distorted octahedral structure. The [N(n-Bu)4]+ ion is disordered at the C3A and C4A atoms of one Bu. The IR and 1H NMR spectra of the complexes are also discussed.Key words: N4-dianionic amido ligand (bqb), (bqb) complexes of Co(II), Ni(II), Cu(II), and Co(III), azide, cyanide, X-ray crystal structures.

Stereospecific reactions of aryltellurium(IV) trichlorides with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol: the X-ray crystal structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride

1995 ◽  
Vol 73 (2) ◽  
pp. 255-263 ◽  
Author(s):  
Bozena Borecka ◽  
T. Stanley Cameron ◽  
M. Azad Malik ◽  
Barry C. Smith
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lone Pair ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Compound C ◽  
Stereospecific Reactions

Aryltellurium(IV) trichlorides react with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol to give aryl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides and aryl(cis-1-hydroxymethyl-trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides. The structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride has been determined by single crystal X-ray analysis. The compound C15H20Cl2O3Te, Mr = 446.8, crystallizes in the monoclinic space group P21/c with a = 9.626(2) Å, b = 15.768(5) Å, c = 11.176(3) Å, β = 92.08(1)°, V = 1695.2(5) Å3 and D(calc) = 1.751 for Z = 4. Tellurium is bonded axially to two chlorines and equatorially to aryl carbon and carbon from the cyclohexyl portion of oxabicyclo[3.2.1]oct-4-yl in a pseudo-trigonal-bipyramidal arrangement having an equatorial lone pair of electrons. Bond lengths are Te—Cl(1) = 2.492(3) Å, Te—Cl(2) = 2.539(3) Å, Te—C(4) = 2.175(10) Å, and Te—C(9) = 2.090(10) Å. Keywords: organotellurium(IV), 3-cyclohexene-1-methanol, 3-cyclohexene-1, 1-dimethanol.

scholarly journals Ni(II) complexes with thioether-functionalized silylamide ligands. Synthesis and crystal structures of [Ni{Me2Si(N-C6H4-2-S-t-Bu)2}], [Ni{Ph2Si(N-C6H4-2-SMe)2}] and [Ni{Ph2Si(N-C6H4-2-SPh)2}]

2019 ◽  
Vol 74 (2) ◽  
pp. 233-240 ◽  
Author(s):  
Ralf Albrecht ◽  
Phil Liebing ◽  
Uwe Morgenstern ◽  
Christoph Wagner ◽  
Kurt Merzweiler
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Nickel Complexes ◽  
Subsequent Reaction ◽  
X Ray ◽  
Bond Lengths ◽  
Tetradentate Ligands ◽  
Square Planar ◽  
Structure Determinations

AbstractThioether-functionalized aminosilanes R2Si(NH-C6H4-2-SR′)2 with R=Me, Ph and R′=t-Bu, Me, Ph were synthesized from the corresponding dichlorosilanes R2SiCl2 and lithiated aniline derivatives LiNH-C6H4-2-SR′. Treatment of the functionalized aminosilanes R2Si(NH-C6H4-2-SR′)2 with two eq. of n-BuLi and subsequent reaction with nickel(II) halides NiX2 (X=Cl, Br) or [Ni(acac)2(TMEDA)] led to the formation of the Ni(II) complexes [Ni{R2Si(N-C6H4-2-SR′)2}]. The X-ray single-crystal structure determinations of the nickel complexes revealed that the thioether-functionalized silylamides R2Si(NC6H4-2-SR′)22− act as tetradentate ligands. The nickel atoms exhibit a distorted square-planar coordination with Ni–N and Ni–S bond lengths in the range of 186.4(3)–186.9(2) pm and 217.5(1)–221.5(1) pm, respectively.

Iodomanganate(II): Darstellung und Kristallstrukturen von (Ph4P)MnI3L, MnI2 L3, [MnIL5]I3 und [MnL6](I3)2 (L = Tetrahydrofuran) / Iodomanganates(II): Synthesis and Crystal Structures of (Ph4P)MnI3L, MnI2L3, [MnIL5]I3 and [MnL6](I3)2

1988 ◽  
Vol 43 (2) ◽  
pp. 175-181 ◽  
Author(s):  
Peter Stolz ◽  
Siegfried Pohl
Keyword(s):  
Characteristic Feature ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The compounds (Ph4P)MnI3L (1), MnI2L3 (2), [MnIL5]I3 (3), and [MnL6](I3)2 (4) (L = C4 H8O, thf) were prepared in thf solution and their structures determined from single crystal X-ray diffraction data. 1 crystallizes in the monoclinic space group C2/c with a = 1743.6(1), b = 1985.8(1), c = 1806.7(1) pm, β = 98.74(1)°, Z = 8. The structure of 1 exhibits tetrahedral anions. The Mn-I distance was found to be 268.0 pm (mean). 2: monoclinic, C2/c with a = 1252.3(2), b = 1255.0(3), c = 1271.8(3) pm β = 113.88(2)°, Z = 4. The characteristic feature of the structure of 2 is the existence of neutral MnI2L3 molecules with a distorted trigonal bipyramidal geometry and the iodine atoms in equatorial positions (Mn-I: 271.1 pm). The compound crystallizes from a solution of Mnl2 in tetrahydrofuran. 3: monoclinic, C2/c with a = 1695.3(1), b = 1123.1(1), c = 1646.2(1̱) pm, β = 96.91(1)°, Z = 4. The preparation of 3 from 2 and iodine yields octahedral MnIL+5 cations (Mn-I: 278.8̄ pm) and triiodide anions. 4: monoclinic, P21/n with a = 1005.5(1). b = 1056.8(1), c =1835.6(2) pm, β = 91.16(1)°, Z = 2. 4 is prepared from 3 and iodine in thf solution, and shows octahedral MnL62+ cations and triiodide anions

Zur strukturellen Verzerrung von Fe4S4I42- -Clustern durch Iod-Iod-Kon Die Kristallstrukturen von (Ph4P)2Fe4S4I4 und (Me3NCH2Ph)2Fe4S4I4 / Structural Distortion of Fe4S4I22- Clusters through Iodine-Iodine Contacts: Crystal Structures of (Ph4P)2Fe4S4I4 and (Me3NCH2Ph)2Fe4S4I4

1988 ◽  
Vol 43 (4) ◽  
pp. 457-462 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Core Structure ◽  
Structural Distortion ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
The Core

AbstractThe structures of (Ph4P)2Fe4S4I4 (1) and (Me3NCH2Ph)2Fe4S4I4 (2) were determined from single crystal X-ray diffraction data.1 crystallizes in the tetragonal space group I41/a with a = 1088.3(1) and c = 4540.3(2) pm. Z = 4.2: Monoclinic, space group Cc. a = 1332.0(2), b = 1513.8(3), c = 1755.1(3) pm, β = 96.69(1)°, Z = 4.In 1 the anion Fe4S4I42- has imposed S4 symmetry with four short (226.2 pm) and eight long (228.1 and 228.4 pm) Fe-S distances parallel and perpendicular, respectively, to the crystallo­graphic 4̃ axis. The Fe-Fe distances were found to be 274.3 and 275.5 pm (Fe-I 254.1 p0m).In (Me3NCH2Ph)2Fe4S4I4 the [Fe4S4]2+ cluster also exhibits a slightly compressed tetragonal core structure but the core distortions are larger and less regular than in 1 (Fe-S distances from 224.6 to 232.9 pm, Fe-Fe distances from 269.6 to 275.9 pm, Fe-I distances from 249.5 to 255.7 pm).In addition there are in 2 iodine-iodine interactions between the anions with an I-I distance of 391.7 pm. These weak attractive forces seem to be the reason for the rather large and hitherto in [Fe4S4] clusters with four identical ligands unobserved distortion of the Fe4S4 core.

The Crystal and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

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