Crystallographic study of a heteroleptic chloroberyllium borohydride carbodicarbene complex

2020 ◽  
Vol 75 (5) ◽  
pp. 497-501 ◽  
Author(s):  
Jacob E. Walley ◽  
Diane A. Dickie ◽  
Robert J. Gilliard
Keyword(s):  
Crystal Structure ◽  
Crystallographic Data ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Unique Data ◽  
Crystallographic Study ◽  
Group 2

AbstractInterest in beryllium, the lightest member of group 2 elements, has grown substantially within the synthetic community. Herein, we report the synthesis and crystal structure of a heteroleptic haloberyllium borohydride bis(1-isopropyl-3-methyl-benzimidazol-2-ylidene)methane ‘carbodicarbene’ (CDC) complex [(CDC)BeCl(BH4)]. Crystallographic data: Triclinic space group P1̅, a = 8.8695(14), b = 12.394(2), c = 16.844(3) Å, α = 102.395(4), β = 96.456(4), γ = 99.164(4)°, wR2 (all data) = 0.2706 for 6720 unique data and 357 refined parameters.

Facile Synthesis and Crystal Structure of [(PhSO2 N)2 WVI Cl2 (CH3CN)2] - the Oxidative Imination of W(CO)6 by N,N-Dichlorophenylsulphonamide

1985 ◽  
Vol 40 (6) ◽  
pp. 736-739 ◽  
Author(s):  
Herbert W. Roesky ◽  
Jörg Sundermeyer, ◽  
Jürgen Schimkowiak ◽  
Peter G. Jones ◽  
Mathias Noltemeyer ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Good Yield ◽  
Polymeric Complex ◽  
Facile Synthesis ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Tungsten Hexacarbonyl ◽  
Space Group

AbstractThe reaction of N,N-dichlorophenylsulphonamide with tungsten hexacarbonyl in refluxing CCl4 leads in good yield to the yellow polymeric complex [(PhSO2N)2WCl2]x, which may be converted to the octahedral nitrene complex [(PhSO2N)2WCl2(CH3CN)2] by recrystallisation from aceto­nitrile. Crystals of the acetonitrile complex are triclinic, space group P 1̅, a = 820.7(2), b = 1128.8(3), c = 1286.9(3) pm, α = 89.25(3), β = 89.54(3). γ = 72.67(2)°, Z = 2, R = 0.027 for 2527 unique observed reflections.

Synthese und Kristallstruktur des koordinativ ungesättigten Komplexes [FeRu(CO)5(μ-PBut2)2] / Synthesis and Crystal Structure of the Coordinatively Unsaturated Complex [FeRu(CO)5(μ-PBut2)2]

1995 ◽  
Vol 50 (8) ◽  
pp. 1175-1180 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Helmut Hartung ◽  
André Krug
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Metal Atoms

[{Ru(CO)3Cl2}2] reacts with the in situ prepared reagent Li2[Fe(CO)3(PBut2)2] to give the new heterobinuclear complex [FeRu(CO)5(μ-PBut2)2] (1). Crystals of 1 are isomorphous to those of the known compound [Fe2(CO)5(μ-PBut2)2] (2) and crystallize in the triclinic space group P1̄ with a = 867,5(1), b = 1181,0(2), c = 1373,1(2) pm; α = 76,64(1), β = 79,72(1) and γ = 76,48(1)°. A double bond between the two metal atoms concluded for 2 from the results of EHMO calculations is also proposed for 1 (Fe=Ru: 259,8(1) pm).

Spezielle Alkylammoniumhexachlorometallate, III [1] Synthese und Kristallstruktur von Tris(guanidinium)- hexachlororhodat(III)-monohydrat, [C(NH2)3]3 [RhCl6] · H2O / Alkylammonium Hexachlorometallates, III [1] Synthesis, and Crystal Structure of Tris(guanidinium) Hexachlororhodate(III) Monohydrate, [C(NH2)3]3[RhCl6] · H2O

1996 ◽  
Vol 51 (10) ◽  
pp. 1464-1468 ◽  
Author(s):  
Walter Frank ◽  
Guido J. Reiß
Keyword(s):  
Crystal Structure ◽  
Hydrochloric Acid ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Acid Solution ◽  
Hydrochloric Acid Solution ◽  
Guanidine Hydrochloride ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group

Tris(guanidinium) hexachlororhodate(III) monohydrate, [C(NH2)3]3[RhCl6] · H2O (1 ) has been obtained by the reaction of rhodium(III) chloride with guanidine hydrochloride in hydrochloric acid solution. 1 crystallizes in the triclinic space group P1̅ (a = 7.6013(9) Å, b = 8.6912(10) Å, c = 15.956(2) Å, α = 93.177(10)°, β = 101.691(10)°, γ = 113.995(9)°, V = 931.8(2), Z = 2). Two crystallographically independent hexachlororhodate ions, three crystallographically independent guanidinium ions and one water molecule are linked by a complex framework of hydrogen bonds.

Synthesis and Crystal Structure of (Trimethylsilyl)acetylide-Bridged Dimeric Titanocene

1998 ◽  
Vol 63 (11) ◽  
pp. 1884-1892 ◽  
Author(s):  
Róbert Gyepes ◽  
Petr Štěpnička ◽  
Ulf Thewalt ◽  
Miroslav Polášek ◽  
Jiří Čejka ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Soluble Compound

Dimeric titanocene [(μ-η5:η5-C10H8){(μ-H)(η5-C5H5)Ti}2] (1) reacts with one equivalent of (trimethylsilyl)acetylene (TMSA) to give a mixture of diamagnetic (trimethylsilyl)acetylide-bridged compounds [(μ-η5:η5-C10H8)(μ-H)(μ-η1:η2-C≡CSiMe3){(η5-C5H5)Ti}2] (2) and [(μ-η5:η5-C10H8){(μ-η1:η2-C≡CSiMe3)(η5-C5H5)Ti}2] (3), and some oligomers of TMSA. Compound 2 crystallizes from hexane in the triclinic space group P1 (No. 2; a = 9.385(4) Å, b = 14.487(6) Å, c = 18.085(6) Å, α = 110.34(2)°, β = 101.56(2)°, γ = 96.65(3)°, V = 2 212(2) Å3, Z = 2). A highly soluble compound 3 could not be isolated from a mixture with oligomers of TMSA.

Darstellung und Kristallstruktur von 2,4,6-Triferrocenyl- 1,3,5,2,4,6-triselenatriborinan/Synthesis and Crystal Structure of 2,4,6-Triferrocenyl-1,3,5,2,4,6-triselenatriborinane

1992 ◽  
Vol 47 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Hans Horn ◽  
Frank Rudolph ◽  
Reinhart Ahlrichs ◽  
Kurt Merzweiler
Keyword(s):  
Crystal Structure ◽  
Electronic Structure ◽  
Ab Initio ◽  
Model Compound ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Lattice Constants

The reaction of [(NEt3)FcBBr2] (Fc:C5H5FeC5H4) with bis(trim ethylsilyl)selenane leads to the formation of Fc3B3Se3 (1). 1 crystallizes in the triclinic space group P1̄. The lattice constants (at 210 K) are: a = 1487.8(8) pm , b = 1563.1(8) pm, c = 1588.6(9) pm, ɑ = 107.81(4)°, β = 101.06(4)°, γ = 115.85(4) . 1 contains a nearly planar B3Se3 ring with alternating B and Se atoms. The electronic structure of the model compound Ph3B3Se3 was investigated by ab initio SCF studies.

Synthese und Kristallstruktur von Bis(m-aminobenzonitril)- diquecksilber(I)-dinitrat/Synthesis and Crystal Structure of Bis(m-aminobenzonitrile)dimercury(I)-dinitrate

1992 ◽  
Vol 47 (4) ◽  
pp. 460-464 ◽  
Author(s):  
Klaus Brodersen ◽  
Jürgen Hofmann
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Amino Nitrogen ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

The structure of bis(m-aminobenzonitrile)dimercury(I) dinitrate, [Hg2(m -NH2C6H4CN)2](NO3)2 has been determined by single crystal X-ray diffraction techniques and refined to an Rw-value of 0.022. The crystals are triclinic, space group P1 with a = 5.4878(1) Å, b = 8.4085(1) Å, c = 9.6062(1) Å, α = 92.599(3)°, β = 94.763(3)°, γ = 89.614(3)° and Z = 1.The Hg22+-ion [Hg-Hg 2.524(1) Å] is approximately axially coordinated to amino nitrogen atoms [Hg - N 2.209(4) Å, Hg - Hg - N 169.5(3)°]. Additional amino hydrogen bonds to oxygen are building chains along the b-axis containing units of L - Hg - Hg - L groups.

Synthesis and Crystal Structure of a Novel Neutral Polymeric Lead(II)-thiosemicarbazonato Complex

1998 ◽  
Vol 53 (1) ◽  
pp. 81-86 ◽  
Author(s):  
Alfonso Castiñeiras ◽  
Ricardo Domínguez ◽  
Leandro Bresolin ◽  
Adaílton Joao Bortoluzzi ◽  
Robert Alan Burrow ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Acetate Group ◽  
Lead Atom ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Polymeric Structure ◽  
Space Group

The reaction between lead(II) acetate and 2-acetylpyridine 4N-methylthiosemicarbazone (H4ML) produced a complex of the formula [Pb(4ML)(OOCMe)] with an unusual polymeric structure in which the lead atom is hepta-coordinate, the deprotonated thiosemicarbazone is a tetradentate bridge, and the acetate group both chelates and bridges. The complex crystallizes in the triclinic space group P1̄ with a = 8.860(2), b = 9.394(2), c = 9.783(3) A, α = 108.93(4), β = 98.67(3), γ = 107.87(5)°, V = 704.1(3) Å3 , Z = 2.

Synthese und Kristallstruktur von Tribrommethyltriphenylphosphonium-bromid und Bis(tribrommethyltriphenylphosphonium)-tribroniid-bromid / Synthesis and Crystal Structure of Tribromomethyltriphenylphosphonium Bromide and Bis(tribromomethyltriphenylphosphonium) Tribromide Bromide

1995 ◽  
Vol 50 (2) ◽  
pp. 223-228 ◽  
Author(s):  
H. Vogt ◽  
C. Frauendorf ◽  
A. Fischer ◽  
P. G. Jones
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Red Light ◽  
Monoclinic Space Group ◽  
Reaction Conditions ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group

Tribromotriphenylphosphonium bromide 1 has been prepared by the reaction of triphenylphosphine with tetrabromomethane in dichloromethane. Colourless crystals were obtained by recrystallization from the same solvent. The light-sensitive crystals change colour to yellow. The crystals are triclinic, space group P1̄ , Z = 4, a = 1008.6(5), b = 1357.8(6), c = 1560.7(7) pm, α = 106.61(4), β = 91.80(4), γ = 93.88(4)°. In the solid state there are discrete monomeric (C6H5)3PCBr3+ cations and Br- anions. The cation has a slightly irregular tetrahedral geometry around the P atom. The crystals contain one molecule CH2C12 per four molecules (C6H5)3PCBr4.Bis(tribromomethyltriphenylphosphonium) tribromide bromide 2 can be obtained as a byproduct of the reaction of (C6H5)3P with CBr4 by variation of the reaction conditions. Red light-stable crystals are obtained by recrystallization from CH2C12. The crystals are monoclinic, space group C2/c, Z = 8, a = 2231.5(7), b = 1532.7(7), c = 1556.9(6) pm, β = 129.69(2)°. In the solid state bis(tribromomethyltriphenylphosphonium) tribromide bromide exists as discrete monomeric (C6H5)3PCBr3+ cations and Br- and Br3- anions. The Br anion and the central Br of Br3- anion lie on crystallographic twofold axes. The cation has also a slightly irregular tetrahedral geometry around the P atom, with a long P-CBr3 bond.

Synthese und Kristallstruktur von Te42+(WCl6-)2 / Synthesis and Crystal Structure of Te42+(WCl6-)2

1990 ◽  
Vol 45 (4) ◽  
pp. 413-416 ◽  
Author(s):  
Johannes Beck
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Moist Air ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Lattice Constants ◽  
Temperature Range

WCl6 reacts with two equivalents of tellurium in a sealed evacuated ampoule in the temperature range from 170 to 190 °C to give Te42+(WCl6-)2. Under the same conditions with one equivalent of tellurium WCl5 yields Te42+(WCl6-)2 and WCl4. Te4(WCl6), formes black crystals, which are sensitive to moist air. It decomposes at temperatures above 300° C to Te and WCl6. The crystal structure determination (lattice constants a = 638.9(1), b = 753.2(2), c = 1102.0(5) pm, α = 101.19(2)°, β = 102.85(2)°, γ = 90.21(1)°, Z = 1, triclinic space group P 1̄, 3572 unique reflections for 82 parameters, final R = 0.026) shows the nearly ideal square Te42+ cation with Te–Te distances of 268.8 and 268.7 pm and markedly distorted WCl6– octaedra with W–Cl bond length from 227.5 to 237.3 pm. The structure involves interionic Te–Cl contacts as short as 319 pm.

Kristallstruktur von β-VCl2(N3S2). Synthese und Kristallstruktur von [VCl(N3S2)(Pyridin)2]2·2 CH2Cl2, einem Cyclothiazenokomplex mit Vanadium(IV)/Crystal Structure of β-VCl2(N3S2). Synthesis and Crystal Structure of [VCl(N3S2)(pyridine)2]2·2 CH2Cl2, a Cyclothiazeno Complex with Vanadium (IV)

1986 ◽  
Vol 41 (11) ◽  
pp. 1420-1425 ◽  
Author(s):  
Ruth Christophersen ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Polymer Chains ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
The Difference

Abstract β-VCl2(N3S2) was obtained by sublimation. It represents a new modification compared to the known α-VCl2(N3S2) which can be obtained from solution. Its crystal structure was determined by X-ray diffraction (864 observed reflexions, R = 0.034). Crystal data: triclinic, space group P1̄, Z = 2, a = 570.0, b = 779.9, c = 735.3 pm , α = 90.85°, β = 108.26°, y = 98.77°. Both modifications consist of polymer chains in which the vanadium atoms are linked alternatively by chloro and nitrogen bridges. The packing of the chains is rather similar, the only difference being that in β-VCl2(N3S2) the chains are rotated by 11° as compared to the orientation in α-VCl2(N3S2). The difference of the two modifications also shows up in the slightly different IR spectra. By reduction of VCl2(N3S2), dissolved in CH2Cl2/pyridine, with H2S, zinc or PPh3, the cyclothiazeno complex [VCl(N3S2)(pyridine)2]2·2 CH2Cl2 was obtained. It crystallizes in the monoclinic space group P 21/c, Z = 4, a = 1010.4, b = 917.3, c = 1967.8 pm, β = 103.03° (structure determination with 649 observed reflexions. R = 0.081). In this vanadium(IV) compound the metal atoms are part of planar VN3S2 rings as found in the VCl2(N3S2) modifications. The two vanadium atoms of the centrosymmetrical dimer are linked via one nitrogen atom of each of the VN3S2 rings; the resulting V2N2 ring is coplanar with the two VN3S2 rings.

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