μ-Nitridokomplexe von Wolfram(VI) Die Kristallstruktur von PPh4[W2NCl10]/ μ-Nitrido Complexes of Tungsten(VI) The Crystal Structure of PPh4[W2NCl10]

1985 ◽  
Vol 40 (8) ◽  
pp. 999-1004 ◽  
Author(s):  
Thomas Godemeyer ◽  
Alexander Berg ◽  
Hans-Dieter Groß ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Phosphorus Oxide ◽  
Tungsten Atom ◽  
Triclinic Space Group ◽  
X Ray ◽  
Nitrido Complexes ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

AbstractW2NCl9 was obtained as a brilliant red crystal powder from tungsten hexachloride and tris(trimethylsilyl)amine. According to its IR spectrum it has dimeric molecules [W2NCl9]2 with bridging chlorine atoms. Its reaction with tetraphenylphosphonium chloride yields PPh4[W2NCl10], and with phosphorus oxide chloride W2NCl9 ·OPCl3 is obtained; both are soluble in dichlorom ethane. The crystal structure of PPh4[W2NCl10] was determined by X-ray diffraction (2521 observed reflexions. R = 0.065). Crystal data: triclinic, space group P1̄, Z = 2, a = 1125.7, b - 1278.2, c = 1347.8 pm, α = 110.08, β = 94.55, γ = 111.55°. The structure consists of PPh4ⓛ ions which are arranged to (PPh4ⓛ)2 pairs about inversion centres, and of [W2NCl10]⃝ anions. The latter possess an almost linear W NW group (173°) with slightly different WN bond lengths of 179 and 188 pm corresponding to double bonds. Each tungsten atom has an octahedral coordination. The WCl bonds trans to the nitrido ligand are about 9 pm longer than the bonds in the cis positions.

Notizen: Tetraphenylphosphonium-octabromodiantimonat, (PPh4)2[Sb2Br8]. Synthese und Kristallstruktur / Tetraphenylphosphonium Octabromodiantimonate, (PPh4)2[Sb2Br8]. Synthesis and Crystal Structure

1985 ◽  
Vol 40 (4) ◽  
pp. 562-564 ◽  
Author(s):  
Abdulalah T. Mohammed ◽  
Ulrich Muller
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Raman Spectral Data ◽  
Raman Spectral ◽  
Ir And Raman

(PPh4)2[Sb2Br8] can be prepared from SbBr3 and PPh4Br in CH2Br2 or from Sb2S3, PPh4Br and HBr in 1,2-dichloroethane. Its crystal structure was de­termined with X-ray diffraction data (2764 observed reflexions, R = 0.039). Crystal data: triclinic, space group P1̄, a = 1024.9. b = 1127.1, c = 1282.4 pm, α = 111.80, β = 94.52, γ = 106.92°, Z = 1. The centrosymmetric [Sb2Br8]2- ions consist of two square pyramids sharing a basal edge. The cations are grouped to (PPh4+)2 pairs similarly as in (PPh4)2[As2Cl8]; although the latter compound has a comparable general crystal packing, it is not isotopic. IR and Raman spectral data are reported.

Cyclothiazeno-Vanadiumdibromid, VBr2(N3S2) / Cyclo-Thiazeno Vanadium Dibromide, VBr2(N3S2)

1985 ◽  
Vol 40 (11) ◽  
pp. 1457-1462 ◽  
Author(s):  
Jürgen Hanich ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

VBr2(N3S2) was synthesized by reaction of VCl2(N3S2) with Me3SiBr. It reacts with PPh4Br in dibromomethane solution to form (PPh4)2[VBr3(N3S2)]2. The compounds were characterized by their IR and 51V NMR spectra. The crystal structure of VBr2(N3S2) was determined by X-ray diffraction (2060 reflexions. R = 0.114). Crystal data: triclinic, space group P1̄, a = 586.4, b = 794.2, c = 744.6 pm. α - 89.25, β - 108.58, γ = 99.67°. Z = 2. The vanadium atoms form planar, six-membered rings wjith the N3S2 groups, with short VN distances (172 and 185 pm). Bromine- bridged dimers are associated via V−N links to form chains in a similar way as in some tetrahalides. The structure is similar to that of VCl2(N3S2), but the chains are rotated by 17° along their axes.

scholarly journals Crystal structure of a one-dimensional coordination polymer of gadolinium dibromoacetate with 4,4'-bipyridine

2018 ◽  
Vol 9 (3) ◽  
pp. 178-181 ◽  
Author(s):  
Leslaw Sieron ◽  
Agnieszka Czylkowska ◽  
Bartlomiej Rogalewicz
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Coordination Polymer ◽  
Stacking Interactions ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Coordinate Geometry

A new gadolinium(III) complex with 4,4’-bipyridine (4-bpy) and dibromoacetate ligand of general formula [Gd(4-bpy)(CBr2HCOO)3(H2O)]n, has been synthesized, crystallized and characterized by a single-crystal X-ray diffraction analysis. The gadolinium atom has an unsymmetrical eight-coordinate geometry, being coordinated by six oxygen atoms of dibromoacetate anions, one nitrogen atom of 4-bpy and one water molecule. The complex is a one-dimensional polymer as a result of dibromoacetate ligand bridging with the repeating monomeric units. There are π...π stacking interactions between the 4-bpy rings as well as O–H...O and O–H...N hydrogen bonds. Crystal Data for C16H13Br6GdN2O7 (Mw = 981.99 g/mol): triclinic, space group P-1 (no. 2), a = 9.7368(4) Å, b = 11.5416(4) Å, c = 11.7634(4) Å, α = 104.2750(10)°, β = 94.060(2)°, γ = 92.6900(10)°, V = 1275.08(8) Å3, Z = 2, T = 90 K, μ(CuKα) = 28.190 mm-1, Dcalc = 2.558 g/cm3, 8399 reflections measured (7.782° ≤ 2Θ ≤ 133.18°), 4006 unique (Rint = 0.0409, Rsigma = 0.0639) which were used in all calculations. The final R1 was 0.0527 (I > 2σ(I)) and wR2 was 0.1396 (all data).

Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), (PPh4)4Sb8Br28 / Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28

1996 ◽  
Vol 51 (9) ◽  
pp. 1245-1247 ◽  
Author(s):  
Wolfgang Fachbereich Biologie-Chemie, Univer ◽  
Ulrich Fachbereich Biologie-Chemie, Univer
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Closest Packing ◽  
Distorted Octahedral

The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloromethane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, α = 102.93(2), β = 100.83(2), γ = 100.42(2)°, Z = 2, triclinic, space group P1̄. (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284- ion can be taken as the association product of eight SbBr3 molecules with four Br− ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres.

Preparation and Crystal Structure of New 1,3-Diaza-λ5,λ5-diphosphetidines

1986 ◽  
Vol 41 (10) ◽  
pp. 1201-1205 ◽  
Author(s):  
Ch. Donath ◽  
M. Meisel ◽  
K .-H . Jost ◽  
K. K. Palkina ◽  
S. I. Maksimova ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Methyl Ester ◽  
Single Crystal ◽  
Fractional Crystallization ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Benzyl Amine

Abstract Reaction of py · PS2Cl (py = pyridine) with benzyl amine in the presence of NEt3 yields triethyl-ammonium 1,3-dibenzyl-2,4-dithioxo-1,3-diaza-2λ5,4λ5-diphosphetidine-2,4-dithiolate which reacts with MeI to give the corresponding methyl ester. By fractional crystallization from cyclohexane three modifications of the methyl ester were obtained (two trans-(A and A') and one cis-modification (B)). The crystal structure of these modifications have been determined by single crystal X-ray diffraction. Crystal data: A: triclinic, space group P1̄ , Z = 2, a = 7.100(3), b = 10.088(6), c = 17.785(6) Å , α = 99.18(4)°, β = 93.75(5)°, γ = 106.96(4)°, A': monoclinic, P21/c, Z = 2, a = 7.933(3), b = 13.689(3), c = 9.917(4) Å, β = 111.98(3)°; B: orthorhombic, P cab, Z = 8, a = 12.962(6), b = 16.581(6), c = 19.475(7).

Darstellung, IR-Spektrum und Kristallstruktur von [WNCI3 P0Cl3]4 2 POCI3 / Preparation, IR Spectra and Crystal Structure of [WNCl3 • P0Cl3]4 • 2 P0Cl3

1979 ◽  
Vol 34 (7) ◽  
pp. 942-948 ◽  
Author(s):  
Wilfried Musterle ◽  
Joachim Strähle ◽  
Wolfgang Liebelt ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Tungsten Nitride ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Tungsten Hexachloride ◽  
Preparative Route

Abstract Tungsten nitride chloride-POCl3 solvate, [WNCl3 • POCl3]4 • 2 POCl3 is prepared by the reaction of WNCI3 with excess POCI3. With equimolar amounts of POCI3 in dichloromethane suspension the complex [WNCI3 • POCl3]4 • 2 CH2CI2 is formed, which is easily decomposed leaving pure [WNCI3 • POCl3]4. The IR spectra of these complexes were recorded and assigned. A new preparative route to WNCI3 from tungsten hexachloride and iodine azide is described. [WNCI3 • POCl3]4 • 2 POCl3 crystallizes in the triclinic space group P1̅ with two tetrameric units per unit cell. The crystal structure was solved by X-ray diffraction methods (Å = 0,087; 3085 observed reflexions). The structure consists of planar and almost square W4N4-eight-membered rings with alternating W-N bond lengths. The distorted octahedral environment of the tungsten atoms is completed by three terminal Cl-ligands and by the oxygen atom of a POCI3 molecule, which is coordinated trans to the W = N triple bond. The two additional POCI3 molecules are weakly linked to two of the four POCI3 solvate molecules, giving rise to an increase of the W-O bond lengths to these donor groups

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

scholarly journals CRYSTAL STRUCTURE OF BIS[1-(DIAMINOMETHYLENE)-THIOURON-1-IUM] SULFATE

2017 ◽  
Vol 60 (1) ◽  
pp. 45
Author(s):  
Yuliya V. Butina ◽  
Elena A. Danilova ◽  
Maxim V. Dmitriev ◽  
Aleksey V. Solomonov
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Diffraction Data ◽  
Crystalline State ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tautomeric Forms ◽  
Structural Database ◽  
Derivatives Of

For citation:Butina Yu.V., Danilova E.A., Dmitriev M.V., Solomonov А.V. Crystal structure of bis[1-(diaminomethylene)-thiouron-1-ium] sulfate. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2017. V. 60. N 1. P. 45-49. In this work crystal data of bis[1-(diaminomethylene)-thiouron-1-ium] sulfate is shown. This compound was characterized by IR spectroscopy and elemental analysis. The monocrystal of this compound was obtained and the structure was confirmed by single X-ray analysis. Moreover, the work describes potential application of synthesized compound. Comparative characteristics of thiourea and its known salts are demonstrated. It is known, that derivatives of thiourea have several tautomeric forms, which can be different in crystalline state or in solution. Therefore, changed scheme of the synthesis of 2-imino-4-thiobiuret is proposed. Elemental cell of crystal consists of two 1-(diaminomethylene)thiouron-1-ium cations and one sulfat anion. A full set of X-ray diffraction data was deposited in the Cambridge Structural Database (deposit CCDC 1421710) and it can be gotten from the site www.ccdc.cam.ac.uk/data_request/cif.

scholarly journals Über die Reaktion von Wolframhexachlorid mit Se4N2; Kristallstruktur von PPh4[WCl5(NSeCl)] / On the Reaction of Tungsten Hexachloride with Se4N2; Crystal Structure of PPh4[WCl5(NSeCl)]

1991 ◽  
Vol 46 (12) ◽  
pp. 1625-1628 ◽  
Author(s):  
Stefan Vogler ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Structure Determination ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)], which was characterized by an X-ray structure determination. Space group P21, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimensions at —80 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; β = 111.93(3) . The [WCl5(NSeCl)]- ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm.

Pyridin-Addukte von Cyclothiazeno-Vanadiumdichlorid Die Kristallstruktur von [VCl2(N3S2)(C5H5N)] / Pyridine Adducts of Cyclo-thiazeno Vanadium Dichloride The Crystal Structure of [VCl2(N3S2)(C5H5N)]

1985 ◽  
Vol 40 (12) ◽  
pp. 1631-1637 ◽  
Author(s):  
Ruth Christophersen ◽  
Paul Klingelhöfer ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Chlorine Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Independent Molecules

Abstract The pyridine complexes of cyclo-thiazeno vanadium dichloride, [VCl2(N3S2)py] and [VCl2(N3S2)(py)2] were synthesized by reactions of polymeric VCl2(N3S2) with varying amounts of pyridine in CH2Cl2. The compounds were characterized by their IR spectra as well as by their 51V NM R spectra. The crystal structure of [VCl2(N3S2)(C5H5N)] was determined by means of X-ray diffraction (1582 independent observed reflexions, R = 0.031). Crystal data: orthorhombic, space group Pnma, a = 1372, b - 2261, c - 1068 pm, Z = 12. In the lattice there are two monomeric, crystallographically independent molecules [VCl2(N3S2)(C5H5N)], which differ only slightly. The vanadium atoms have a trigonal bipyramidal coordination with the N atom of the pyridine molecule and one chlorine atom in apical positions, and with one chlorine atom and the N atoms of the cyclo-thiazeno ligand in equatorial positions. The VN bond lengths of the planar VN3S2 ring of 174 pm correspond to double bonds

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