Improved Synthetic Route to Unsymmetrically Substituted Phosphinimino-phosphonium Salts. Crystal Structure of Tri-n-butyl- [tris(diethylamino)phosphinimino]phosphonium Chloride

2001 ◽  
Vol 56 (12) ◽  
pp. 1319-1321 ◽  
Author(s):  
R. Bartsch ◽  
M. Freytag ◽  
S. Goller ◽  
R G. Jones ◽  
R. Schmutzler

Abstract The title compound was prepared from tri-n-butyl-chlorophosphonium chloride and N-tri-methylsilyl-tris(diethylamino)-phosphinimine. A low temperature X-ray crystal structure de­termination revealed PN bond lengths of 156.1(2) and 158.0(2) pm, with a PNP angle of 149.36(17)°.

1998 ◽  
Vol 53 (5-6) ◽  
pp. 634-636 ◽  
Author(s):  
Martina Näveke ◽  
Armand Blaschette ◽  
Peter G. Jones

Abstract The crystal structure of the known title compound was determined by low-temperature X-ray diffraction (orthorhombic, space group Pbcn, Z = 4). The molecule displays an unusually short O-N bond, a relatively long C-O bond and a moderately pyramidal O-NS2 skeleton (O-N 133.1, C-O 148.5 pm, sum of bond angles at N: 347.4°).


2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides


1978 ◽  
Vol 33 (6) ◽  
pp. 610-613 ◽  
Author(s):  
Siegfried Pohl

Abstract The crystal structure of the title compound was determined from single crystal X-ray data. The compound crystallises in the orthorhombic space group Pnma. In contrast to the solution where fluctuating P-Te bonds have been established by NMR analyses the crystals contain isolated molecules with fixed P-Te bonds (bond length: 235.4 pm). The four-membered phosphorus nitrogen ring exhibits significant deviations from planarity. The P-N bond lengths were found to be 168.3 and 175.0 pm, respectively


1976 ◽  
Vol 31 (9) ◽  
pp. 1295-1296 ◽  
Author(s):  
T. Stanley Cameron ◽  
M. Gerard Magee ◽  
Samuel Mclean

The title compound was synthesised and its structure determined by X-ray crystallography. The structure contains a hydrogen bond between the OH group of the alcohol and the phosphoryl oxygen atom. The P–N bond lengths are significantly different and the differences can be attributed to varying ρπ—dπ interactions along the bonds.


1975 ◽  
Vol 30 (11-12) ◽  
pp. 973-974 ◽  
Author(s):  
T. Stanley Cameron ◽  
Kh. Mannan ◽  
Malcolm Biddlestone ◽  
Robert A. Shaw

The title compound was synthesized and its structure determined by X-ray crystallography. The NPPh3 substituent adopts a type I conformation with its nitrogen and phosphorus atoms coplanar with the ring. The compound, the first asymmetric 1,3,5-triazine to be crystallographically investigated, shows significant variations in ring bond lengths and angles; these are discussed.


1989 ◽  
Vol 44 (7) ◽  
pp. 857-859 ◽  
Author(s):  
Dieter Fenske ◽  
Christina Ergezinger ◽  
Kurt Dehnicke

The title compound has been prepared as a byproduct of the reaction of Se2Cl2 with Ν,Ν,N′-Tris(trimethylsilyl)benzamidine in CH2Cl2 solution. [SeCl2(HNC2N2Ph2)]2 was characterized by an X-ray structure determination. Space group P21/n, Z = 2, 2979 observed independent reflexions, R = 0.032. Lattice dimensions (-65 °C): a = 1050.1(4), b = 1018.9(4), c = 1402.1(6) pm; β = 99.78(3)°. The compound forms centrosymmetric dimeric molecules with SeCl2Se bridges (bond lengths 241.6(1) and 339.3(1) pm), the selenium atoms being members of nearly planar [xxx] selenatriazine rings with Se—N bond lengths of 182.2(2) and 181.5(2) pm.


1968 ◽  
Vol 46 (4) ◽  
pp. 605-612 ◽  
Author(s):  
B. E. Robertson ◽  
C. Calvo

The crystal structure of β-CU2P2O7 has been determined by X-ray methods. The crystals are monoclinic with a = 6.827(8) Å, b = 8.118(10) Å, c = 4.576(6) Å, β = 108.85(10)°, Z = 2, and space group C2/m. This structure is analogous to that of the mineral thortveitite and the high temperature forms of the pyrophosphates of Zn, Mg, and Mn. The cations are octahedrally coordinated to oxygen atoms with equatorial Cu—O bonds of 2.00 Å and 1.94 Å while the axial bond lengths are 2.58 Å. The anion has inner P—O bonds of 1.542 Å and average terminal bonds of 1.509 Å. In addition to the usual refinement with anisotropic thermal parameters, the structure has been refined in terms of a disordered structure generated from the low temperature α form of CU2P2O7. This disordered model agrees as well with the data (R = 0.12) as the structure based on the thortveitite structure with large anisotropic motion assigned to the atoms.


1989 ◽  
Vol 44 (9) ◽  
pp. 1003-1006 ◽  
Author(s):  
Kurt Merzweiler ◽  
Dieter Fenske ◽  
Eva Hartmann ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with tantalum pentachloride in CH2Cl2 suspension, forming amber-coloured, moisturesensitive crystals, which were characterized by an X-ray structure determination. Space group P 21/n, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (-65°C): a = 1165.2(6), b = 1335.4(6), c = 1629.0(7) pm, β = 93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCl2Ta with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in trans-position to the imido group, which can be formulatedas [xxx] (bond lengths Ta=Ν = 183.5(8), C=N = 134(1) pm, bond angle TaNC = 162.7(7)°).


1978 ◽  
Vol 33 (7) ◽  
pp. 728-730 ◽  
Author(s):  
T. Stanley Cameron ◽  
Ruth E. Cordes ◽  
Florence A. Jackman

The title compound was synthesised in an attempt to prepare phosphenyl-tri-ortho-toluidine, X-ray crystallographic studies show that it contains a P-O-P bridge with extensively hydrogen bonding between groups. The P-N bond lengths are different and this can be attributed to some combination of hydrogen bonding and varying p II-d ZII interactions along the bond.


1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.


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