Crystal Structure of Hexamethylcyclotriphosphazene-Iodine (1:1 Adduct)

1974 ◽  
Vol 52 (12) ◽  
pp. 2197-2200 ◽  
Author(s):  
Peter L. Markila ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Title Compound ◽  
Chair Conformation ◽  
The Other ◽  
Iodine Molecule ◽  
Full Matrix ◽  
Space Group

Crystals of the title compound, N3P3Me6•I2, are triclinic, a = 10.707(13), b = 8.873(5), c = 8.871(6) Å, α = 96.65(6), β = 103.91(12), γ = 97.81(12)°, Z = 2, space group [Formula: see text] The structure was determined with MoKα diffractometer data by Patterson and Fourier syntheses, and was refined by full-matrix least-squares methods to R = 0.053 for 1934 observed reflexions. One atom of the iodine molecule is weakly bonded to nitrogen, N—I = 2.417(7), I—I = 2.823(1) Å, N—I—I = 177.8(2)°. The six-membered phosphazene ring is slightly non-planar, with a chair conformation. The two P—N bonds involving the nitrogen atom bonded to iodine are longer, mean 1.64 Å, than the other four P—N bonds, mean 1.598 Å Other mean dimensions are: P—C = 1.789 Å, N—P—N = 114.7, P—N—P = 124.0, C—P—C = 104°.

Crystal Structure of Bis[hexakis(dimethylamino)cyclotriphosphonitrilium] Tetrachlorocobaltate(II)

1974 ◽  
Vol 52 (5) ◽  
pp. 734-737 ◽  
Author(s):  
Alistair L. Macdonald ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Electron Density ◽  
Title Compound ◽  
Full Matrix ◽  
Space Group ◽  
Density Methods ◽  
Protonated Nitrogen Atom ◽  
Hydrogen Bonded

Crystals of the title compound, [N3P3(NMe2)6H]2CoCl4, are orthorhombic, a = 34.623, b = 13.964, c = 10.486 Å, Z = 4, space group P212121. The structure was determined by Patterson and electron-density methods and refined by full-matrix least-squares procedures to R = 0.088 for 2178 observed reflexions. Both rings are slightly non-planar, with three distinct pairs of NP bonds: commencing at the protonated nitrogen atom, 1.68, 1.56, and 1.58 Å. The CoCl42− ion is tetrahedral and is hydrogen bonded to both rings, N—H … Cl = 3.32, 3.36 Å.

Die Kristallstruktur des Lithium-Benzamidinats {Li3[C6H5 - C(NSiMe3)2]3 · NC - C6H5} / The Crystal Structure of the Lithium Phenylamidinate {Li3[C6H5 - C(NSiMe3)2]3 · NC - C6H5}

1994 ◽  
Vol 49 (10) ◽  
pp. 1444-1447 ◽  
Author(s):  
Helmut Goesmann ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Single Crystals ◽  
Title Compound ◽  
The Other ◽  
Space Group ◽  
Structure Solution

AbstractSingle crystals of the title compound have been prepared by the reaction of benzonitrile with LiN-(SiMe3)2 in hexane and subsequent evaporation of the solvent. Space group P21/n, Z = 4, structure solution with 7945 observed unique reflections. R = 0.052. Lattice dimensions at -70 °C: a = 1485.2(9); b = 2486.9(11); c = 1568.9(8) pm; β = 91.06(4)°. The compound forms a trimeric ion ensemble in which two of the lithium cations are coordinated by three nitrogen atoms of two phenylamidinate an ions, the other one by four nitrogen atoms of two chelating phenylaminidate anions and in addition by the nitrogen atom of a benzonitrile molecule.

Crystal structure of Tris(N,N-diethyldithiocarbamato)thallium(III)

1978 ◽  
Vol 31 (9) ◽  
pp. 1927 ◽  
Author(s):  
DL Kepert ◽  
CL Raston ◽  
NK Roberts ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The crystal structure of the title compound, [Tl(S2CNEt2)3], has been determined by single-crystal X-ray diffraction methods at 295 K and refined by full-matrix least squares to a residual of 0.050 for 2517 'observed' reflections. Crystals are monoclinic, with space group A2/a, a 14.789(7), b 10.428(4), c 18.207(9) Ǻ, β 118.11(4)°, Z 4, and are isostructural with those of the previously determined gallium and indium analogues, the molecule having 2 symmetry with <Tl-S> 2.666 Ǻ. As in the dimethyl/thallium analogue, the departure of the TlS6 core symmetry from 3 is large and is examined in terms of electron-pair repulsion theory.

Studies on tellurium-carbon bonded compounds. II. The crystal structure of [Heptane-3,5-dionato(2 - )]tellurium(II) ('1,1′-Dimethylacetylacetone tellurium(II)')

1977 ◽  
Vol 30 (3) ◽  
pp. 487 ◽  
Author(s):  
JC Dewan ◽  
J Silver
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chair Conformation ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
Heavy Atom Method

The structure of the title compound has been determined by the heavy- atom method from 973 reflections, measured with a diffractometer, and refined by full-matrix least-squares methods to R 0.030. Crystals are monoclinic, space group P21, a = 8.69(1), b = 4.86(1), c = 10.14(2) Ǻ, β = 98.7(1)�, Z = 2. In the discrete molecules of the complex a tellurium(II) atom is bonded to one bivalent heptane-3,5-dione ligand through the α-carbon atoms [Te-C 2.184(6), 2.206(7) Ǻ; C-Te-C 89.7(3)�], forming a heterocyclic ring of chair conformation with the methyl substituents both in equatorial positions. The molecules are arranged in a zig-zag polymeric manner about the 21 axes at x = 0 and z = 0. All hydrogen atoms have been located.

Structural studies of organoboron compounds. XXXVI. 2,2-Dimethyl-3,3-diphenyl-1,4-dioxa-2-azonia-3-boratacyclohexane

1989 ◽  
Vol 67 (12) ◽  
pp. 2218-2221 ◽  
Author(s):  
Klaus Drückler ◽  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Boron Compound ◽  
Structural Studies ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group

The synthesis of O-(2-hydroxyethyl)-N,N-dimethylhydroxylamine and its reaction with oxybis(diphenylborane) to yield the title compound are reported. Crystals of 2,2-dimethyl-3,3-diphenyl-1,4-dioxa-2-azonia-3-boratacyclohexane are orthorhombic, a = 7.0332(6), b = 9.2269(6), c = 22.967(2) Å, Z = 4, space group P212121. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.051 and Rw = 0.047 for 1247 reflections with 1 ≥ 2σ(I). The molecule exhibits the longest N—B and the shortest O—B distances (1.723(6) and 1.468(5) Å, respectively, corrected for libration) yet reported for a six-membered N,O-chelate of diphenylboron. Keywords: crystal structure, boron compound, organoboron compound.

Structural studies of organoboron compounds. XXXIX.1 1,4-Bis(2,2-diethoxyethyl)-6,8-diphenyl-5,7,9-trioxa-4-aza-1-azonia-8- bora-6-boratabicyclo[4.3.0]nonane

1990 ◽  
Vol 68 (10) ◽  
pp. 1791-1796 ◽  
Author(s):  
Henning Amt ◽  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Reaction of N,N′-1,2-ethanediylidenebis(2,2-diethoxyethanamine)- N,N′-dioxide and phenylboronic acid yields the title compound. Crystals of 1,4-bis(2,2-diethoxyethyl)-6,8-diphenyl-5,7,9-trioxa-4-aza-1-azonia-8-bora-6-boratabicyclo[4.3.0]-nonane are triclinic, a = 12.625(2), b = 13.962(2), c = 9.273(1) Å, α = 104.81(1), β = 98.61(1), γ = 106.52(1)°, Z = 2, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.058 and Rw = 0.081 for 3677 reflections with I ≥ 3σ(I). The molecule has a bicyclo[4.3.0]nonane structure containing one transannular N—B bond. Important bond lengths are sp3-bomn, N—B = 1.759(3), O—B = 1.435(3) and 1.454(3), C—B = 1.579(4); sp2-boron, O—B = 1.335(3) and 1.404(3), C—B = 1.557(4) Å. The (sp3)B—C(phenyl) bond is the shortest yet reported for this type of compound.Keywords: crystal structure, boron compound, organoboron compound.

Crystal Structure of 1,3,5,7-Tetrasulfur-2,4,6,8-tetramethylimide, S4(NCH3)4

1973 ◽  
Vol 51 (15) ◽  
pp. 2504-2506 ◽  
Author(s):  
Alistair L. Macdonald ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Membered Ring ◽  
Molecular Symmetry ◽  
Fourier Methods ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of S4(NCH3)4 are orthorhombic, a = 25.483(6), b = 15.842(3), c = 5.642(2) Å, Z = 8, space group Fdd2, required molecular symmetry C2.•The structure was determined with CuKα diffractometer data by Patterson and Fourier methods, and refined by full-matrix least-squares methods to R = 0.067 for 473 observed reflexions. The eight-membered ring has a crown conformation, with approximate C4v symmetry, and the bonds at each nitrogen atom are slightly but significantly non-planar. Mean bond lengths are S—N = 1.677(4), C—N = 1.479(7) Å.

Structural studies of organoboron compounds. XXXVII. 8,8-Pentamethylene-6-phenyl-6,9-epoxy-5,7-dioxa-8-azonia-6-borata-6,7,8,9-tetrahydro-5H-benzocycloheptene

1990 ◽  
Vol 68 (1) ◽  
pp. 64-68 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Hans-Walter Motzkus ◽  
Klaus Drückler ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Structural Studies ◽  
Boron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Condensation of equimolar amounts of salicylaldehyde, N-hydroxypiperidine, and phenylboronic acid yields the title compound. Crystals of 8,8-pentamethylene-6-phenyl-6,9-epoxy-5,7-dioxa-8-azonia-6-borata-6,7,8,9-tetrahydro-5H-benzocycloheptene are monoclinic, a = 12.773(1), b = 11.9600(7), c = 10.6411(6) Å, β = 103.786(7)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.039 and Rw = 0.047 for 2420 reflections with I ≥ 3σ(I). The compound has a bridged heterocyclic B,N-betaine structure with a PhB(OR)3 anionic centre. Bond lengths (corrected for libration) include: B—O(aryl C) = 1.481(2), B—O(alkyl C) = 1.488(2), B—O(N) = 1.539(2), and B—C = 1.591(2) Å. Keywords: organoboron, boron compounds, crystal structure.

The preparation and crystal structure of pentaiodinium hexafluoroantimonate(V) containing I153+

1979 ◽  
Vol 57 (9) ◽  
pp. 968-973 ◽  
Author(s):  
Jack Passmore ◽  
Peter Taylor ◽  
Tom Whidden ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Multiple Solution ◽  
The Other ◽  
Full Matrix ◽  
Space Group ◽  
Bond Angles

Crystalline pentaiodinium hexafluoroantimonate was prepared by the reaction of I2 and SbF5 in AsF3. The crystals were triclinic, a = 8.295(4) Å, b = 15.61(1) Å, c = 8.390(4) Å, α = 81.49(4)°, β = 110.02(4)°, γ = 85.06(4)°, Z = 3, space group [Formula: see text]. The structure was solved by multiple-solution direct methods and Fourier syntheses and refined by full-matrix and blocked-matrix least-squares procedures to a final R of 0.062 and Rw of 0.090 for 2229 reflections with I ≥ 3σ(I). The two crystallographically independent planar, bent I5+ chains (one centrosymmetric, the other essentially centrosymmetric), each have two collinear central bonds of 2.899(2) Å (× 2); 2.896(2), and 2.920(2) Å, bond angles 180° and 178.7(6)°, respectively, and two shorter terminal bonds of 2.680(3) Å (× 2); 2.666(3) and 2.698(2) Å, with bond angles between central and terminal bonds of 94.53(6)° (× 2); 93.86(7) and 93.17(7)°, respectively. Three I5+ units are joined by a weak (3.416(3) Å) interaction to form what may be regarded as an I153+ unit. The SbF6− anions are approximately octahedral.

X-Ray structure analysis of methyl 2,3,4,5-Tetra-O-acetyl-α-D-galactoseptanoside

1980 ◽  
Vol 33 (5) ◽  
pp. 979 ◽  
Author(s):  
W Choong ◽  
JF McConnell ◽  
NC Stephenson ◽  
JD Stevens
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Structure Analysis ◽  
Title Compound ◽  
Chair Conformation ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal structure of the title compound was determined by X-ray diffraction and the use of the multi-solution programs MULTAN 74. Crystals are monoclinic, space group C2 with Z = 4 in a unit cell of dimensions: a 21.140(6), b 9.394(3), c 9.765(3) Ǻ, β 108.73(5)°. The structure was refined by full-matrix least-squares methods to a final R of 0.036 for 1858 diffractometer reflections. The seven-membered ring approximates to a twist-chair conformation very similar to that found for the gluco analogue.

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