Synthese und Kristallstrukturen der 1,3,4-λ5σ4-Diazaphosphole / Syntheses and Crystal Structures of the 1,3,4-λ5σ4-Diazaphospholes

1993 ◽  
Vol 48 (6) ◽  
pp. 730-736 ◽  
Author(s):  
Gudrun Stieglitz ◽  
Bernhard Neumüller ◽  
Kurt Dehnicke
Keyword(s):  
Nitrogen Atom ◽  
Oxygen Atom ◽  
Crystal Structures ◽  
Structure Determination ◽  
Lithium Atom ◽  
Ion Pair ◽  
Space Group ◽  
X Ray ◽  
Lithium Complex ◽  
Moisture Sensitive

has been prepared by the reaction of Li(DME)[P(t-Bu)2] with benzonitrile in 1,2-dimethoxyethan solution. The compound forms violet, moisture sensitive crystals, which were characterized by an X-ray structure determination [Space group P21/n, Z = 4, 3282 observed unique reflections, R = 0.082. Lattice dimensions at -40°C: a = 851.0(5), b = 1238.0(3), c = 3029.2(4) pm, β = 90.53(4)°]. The compound forms an ion pair, in which the lithium atom is coordinated by two oxygen atoms of a chelating DME molecule, by an oxygen atom of a nonchelating DME molecule, and by the nitrogen atom of the planar diazaphosphole ring in 1-position. The phenyl groups are nearly coplanar with the diazaphosphole ring. is the product of the reaction of the lithium complex with methanol. It forms colourless crystals [Space group Ρ21/n, Ζ = 4, 2015 observed unique reflections, R = 0.068. Lattice dimensions at -80°C: a = 1458.3(2), b = 824.8(1), c = 1716.9(2) pm, β = 105.37(9)°]. The molecules have planar 5 H-diazaphosphole rings.

Synthese und Kristallstrukturen von Diazadien-Komplexen der Erdalkalimetalle / Syntheses and Crystal Structures of Diazadiene Complexes of the Alkaline Earth Metals

1995 ◽  
Vol 50 (1) ◽  
pp. 71-75 ◽  
Author(s):  
Volker Lorenz ◽  
Bernhard Neumüller ◽  
Karl-Heinz Thiele
Keyword(s):  
Crystal Lattice ◽  
Crystal Structures ◽  
Structure Determination ◽  
Alkaline Earth ◽  
Alkaline Earth Metals ◽  
The Other ◽  
Calcium Atom ◽  
Space Group ◽  
X Ray ◽  
Moisture Sensitive

(DME)2] 1 (R = C6H4-4-CH3; DME = dimethoxyethane) was prepared by reaction of calcium with NR=CPh-CPh=NR in DME solution. The compound forms orange, moisture sensitive crystals, which were characterized by an X-ray structure determination [space group orthorhombic, P212121, Z = 4, 4634 observed unique reflections, R = 0.046; lattice dimensions at –70 °C: a = 1340.2(3), b = 1528.1(3), c = 1609.1(3) pm]. The calcium atom is coordinated by the four oxygen atoms of two chelating DME molecules and two nitrogen atoms of the diazadiene ligand, bonded in its enediamide form.[Ba2(DME)3(NPh–CPh=CPh–NPh)2 · DME] 3 was obtained from barium metal and NPh=CPh-CPh=NPh in DME solution as red crystals [space group monoclinic, P2l/c, Z = 4, 4000 observed unique reflections, R = 0.166; lattice dimensions at -70 °C: a = 1704.5(3), b = 1786.1(4), c = 2177.4(4) pm, β = 105.98(3)°]. The two barium atoms are bridged by two differently bonded diazadiene ligands (μ2-Ν,Ν′;μ-Ν, σ-Ν′). Additionally, one of the barium atoms is coordinated to two DME molecules and the other one to only one of the ether molecules. A further DME molecule is a constituent of the crystal lattice.

Zur Struktur und Dotierung von Selenosilikaten: die Kristallstruktur von Er2SeSiO4 und Er3,75Ca0,25Se2,75Cl0,25Si2O7 Structure and Doping of Seleno Silicates: the Crystal Structures of Er2SeSiO4 and Er3,75Ca0,25Se2,75Cl0,25Si2O7

1994 ◽  
Vol 49 (6) ◽  
pp. 733-740 ◽  
Author(s):  
Klaus Stöwe
Keyword(s):  
Crystal Structures ◽  
Structure Analysis ◽  
Rare Earths ◽  
Structure Determination ◽  
Lattice Parameters ◽  
Energy Dispersive ◽  
Space Group ◽  
X Ray ◽  
By Products

Well-shaped brown and pink isometric crystals were obtained as by-products of the synthesis of erbium selenides from the elements in evacuated and sealed silica ampoules with graphite inlets. They could be identified as erbium seleno mono- and disilicates by energy dispersive X-ray fluorescence and X-ray structure determination. The monosilicate Er2SeSiO4 crystallizes isotypically to Nd2SeSiO4 in the space group Pbcm with the lattice parameters a = 600.2(2), b = 688.0(2), c = 1075.2(2) pm and represents the second known seleno inosilicate of the rare earths. From X-ray structure analysis an isotypic relation between the disilicate Er3,75Ca0,25Se2,75Cl0,25Si2O7 and the compound Sm4S3Si2O7 was found, the former crystallizing in the space group I41/amd with the lattice parameters a - 1177.7(2) and c = 1376.5(2) pm. The doping o f the sorosilicate with the elements Ca and Cl originated from contam inations in the graphit inlets used in the procedure

Über die Reaktion von C(NMe2)4 mit zweikernigen Übergangsmetallcarbonylen; Kristallstrukturen von [C(NMe2)3][Mn(CO)5] und [C(NMe2)3][Co(CO)4] / On the Reaction of C(NMe2)4 with Binuclear Transition Metal Carbonyls: Crystal Structures of [C(NMe2)3][Mn(CO)5] and [C(NMe2)3][Co(CO)4]

1991 ◽  
Vol 46 (3) ◽  
pp. 297-302 ◽  
Author(s):  
Wolfgang Petz ◽  
Frank Weller
Keyword(s):  
Transition Metal ◽  
Crystal Structures ◽  
Structure Determination ◽  
Metal Carbonyls ◽  
Space Group ◽  
X Ray ◽  
Transition Metal Carbonyls ◽  
C Nmr

The reactions of C(NMe2)4 (1) with Mn2(CO)10 or Co2(CO)8 in THF yield[C(NMe2)3][Co(CO)4] (3) and [C(NMe2)3][Mn(CO)5] (4), respectively. The compounds Co(CO)4NMe2 (5) and Mn(CO)5NMe2 (6) could not be found. With CH2Cl2 4 is quantitatively converted into [C(NMe2)3][Mn(CO)4Cl2] (7) as shown by IR and 13C NMR investigations. 3 and 4 were characterized by an X-ray structure determination. 3: Space group Pnma, Z = 4, a = 7.435(2), b = 10.79(2), c = 20.299(5)Å. 4: Space group C2/c, Z = 4, a = 11.378(2), b = 10.165(1), c = 14.533(1) Å; β = 103.37(1)°. The compounds form independent ions with no bonding interactions between cation and anion; the central CN3 unit of the [C(NMe2)3]+ cation in 3 and 4 is disordered.

Notizen: Synthese und Kristallstruktur von [OsCl4(CH3CN)2] · 1/2 CH3CN / Synthesis and Crystal Structure of [OsCl4(CH3CN)2] · 1/2CH3CN

1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Room Temperature ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Slow Reaction ◽  
Moisture Sensitive

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.

Die Kristallstruktur von [YbCl2(THF)5]+[WOCl4(THF)]- / Crystal Structure of [YbCl2(THF)5]+[WOCl4(THF)]-

1999 ◽  
Vol 54 (12) ◽  
pp. 1609-1610 ◽  
Author(s):  
M. Karl ◽  
G. Seybert ◽  
W. Massa ◽  
K. Dehnicke
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Ytterbium Atom ◽  
Moisture Sensitive ◽  
Tungsten Hexachloride

Blue moisture sensitive single crystals of [YbCl2(THF)5]+[WOCl4(THF)]- were obtained as a by-product from the reaction of the ytterbium trisamide Yb[N(SiMe3)2]3 with tungsten hexachloride in THF solution. The crystals were suitable for an X-ray crystal structure determination. Space group P2/c, Z = 2, lattice dimensions at -80 °C: a = 1192.5(1), b = 1117.1(1), c = 1349.9(1) pm, ß = 104.115(7)°, R = 0.0424. The structure consists of cations [YbCl2(THF)5]+ in which the ytterbium atom is coordinated in a pentagonalbipyramidal way by the chlorine atoms in the axial positions and by the oxygen atoms of the THF molecules in equatorial positions. Counterions are the well-known [WOCl4(THF)]- ions.

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.

Notizen: Notiz zur Kristallstruktur von APb2Cl5-Verbindungen / Notice about Crystal Structures of APb2Cl5-Compounds

1976 ◽  
Vol 31 (6) ◽  
pp. 885 ◽  
Author(s):  
H.-L. Keller.
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Single crystals of TlPb2Cl5 and NH4Pb2Cl5 were prepared. X-ray diffraction data confirm the space group C2h5—P21/c (No. 14). Crystal structure determination shows a new typ, belonging to the PbCl2-structure.

N-Chloronitrenokomplexe des Wolframs: Synthesen und Kristallstrukturen von PPh3Me[Cl5W(NCl)] und (PPh4)3{[Cl5W(NCl)]2Cl} • CCl4 • 4CH3CN / N-Chloro-Nitrene Complexes of Tungsten: Syntheses and Crystal Structures of PPh3Me[Cl5W(NCl)] and (PPh4)3{[Cl5W(NCl)]2Cl} CCl4-4CH3CN

1988 ◽  
Vol 43 (12) ◽  
pp. 1633-1638 ◽  
Author(s):  
Astrid Gorge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Nitrogen Atom ◽  
Bond Angle ◽  
Chloride Ion ◽  
Tungsten Atom ◽  
Space Group ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Structure Determinations ◽  
Moisture Sensitive

Abstrct The N-chloro-nitrene complexes PPh3Me[Cl5W(NCl)] and (PPh4)3{ [Cl5W(NCl)]2Cl} • CCl4 • 4CH3CN were prepared by the reaction of [CI4W(NCl)]2 with [PPh3Me]Ci in CH2Cl2 and with [PPh4]Cl in CH3CN. respectively, followed by precipitation with CCl4. Both compounds form red, moisture-sensitive crystals, which were characterized by IR spectroscopy as well as by X-ray structure determinations. PPh3Me[CUW(NCl)]: space group P1̄, Z = 2, a = 862.7(3), b = 1108.4(2), c = 1411.0(5) pm. a = 71.74(3)°, β = 76.78(3)°, y = 77.55(2)° (at 18 °C); 2843 unique observed reflexions, R = 0.042. The compound consists of ions PPh3Me+ and [Cl5W(NCl)]-, in which the tungsten atom has a distorted octahedral environment of five chlorine atoms and the nitrogen atom of the N-chloro-nitrene ligand with bond distances WN = 169 pm and N-Cl = 160 pm. bond angle WNCl = 175°. (PPh4)3{[Cl5W(NCl)]2Cl} • CCl4• 4CH3CN: space group P4/n, Z = 2, a = 1298.2(8). c = 2720.4(7) pm (at 17 °C); (1979 unique observed reflexions. R = 0.096). The compound contains cations PPh4+ and anions {[CI5W(NCl)]2Cl}3-, in which two [Cl5W(NCl)]- ions are bridged by a chloride ion to form the linear unit [Cl5W≡N-Cl ··· Cl -Cl-N≡WCl5]3- with Cl ··· Cl-contactsof 288 and 278 pm

Notizen: Kristallstruktur von [Cu4OCl6(CH3CN)4] · 2 CH3CN / Crystal Structure of [Cu4OCl6(CH3CN)4] · 2 CH3CN

1990 ◽  
Vol 45 (11) ◽  
pp. 1593-1596 ◽  
Author(s):  
Wolfgang Hiller ◽  
Alfred Zinn ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Copper Atom ◽  
Title Compound ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Distorted Trigonal Bipyramid

The title compound has been prepared by the reaction of CuCl, with hexakis(trimethylsilyl)-benzdiamidine, in boiling acetonitrile in the presence of traces of water, as brown crystals, which were characterized by their IR spectrum as well as by an X-ray structure determination. Space group C 2/c, Z = 4, 2668 observed unique reflexions, R = 0.036. Lattice dimensions at –65 C: a = 879.5(2), b = 2441.1(3), c = 1241.4(3) pm, β = 95.24(3)°. In the structure four copper atoms surround an oxygen atom in a slightly distorted tetrahedral fashion; the chlorine atoms bridge adjacent copper atoms, and each copper atom is thus bound to three chlorine atoms. The nitrogen atoms of the acetonitrile complete the slightly distorted trigonal bipyramid around the copper atoms.

scholarly journals Die Spektren und Kristallstrukturen der Addukte CI5Sb · [N(i-C3H7)CN(i-C3H7)] und Cl4Sn · 2 [N(i-C3H7)CN(i-C3H7)] / Spectra and Crystal Structures of the Adducts Cl5Sb · [N(i-C3H7)CN(i-C3H7)] and Cl4Sn · 2 [N(i-C3H7)CN(i-C3H7)]

1986 ◽  
Vol 41 (10) ◽  
pp. 1223-1229 ◽  
Author(s):  
H.-D. Hausen ◽  
W. Schwarz ◽  
G . Rajca ◽  
J. Weidlein
Keyword(s):  
Crystal Structures ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Unit Cell ◽  
Molar Ratio ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

Abstract Spectra and Crystal Structures of the Adducts C l5Sb • [N(/-C3H 7)C N (i-C3H 7)] and C l4Sn • 2 [N(/-C3H 7)CN(/-C3H 7)j X-Ray, Vibrational Data, Diisopropylcarbodiimide Adducts of SbCl5, SnCl4 Thecarbodiimide adducts Cl5Sb <-(—N (R) = C = N R)(1) and Cl4S n ^ (-N (R) = C = N R) 2(2)(R = /-C3H 7) have been prepared by the reaction o f R —N = C —N — R with SbCl5 in a 1:1 and with SnCl4 in a 2:1 molar ratio, respectively. The vibrational spectra (IR and Raman) of both compounds have been regarded and assigned to the skeleton modes. The X-ray structure determination shows the orthorhombic space group Pna2, with 4 formula units per unit cell for 1. Adduct 2 has a trans-configuration and crystallizes in the triclinic space group P 1 with only one molecule per unit cell.

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