Crystal Structure of 1-Cyanotetracyclo[3.3.1.13,7.03,7]decane

1973 ◽  
Vol 51 (1) ◽  
pp. 87-91 ◽  
Author(s):  
Cyril S. Gibbons ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Scintillation Counter ◽  
Bond Distance ◽  
Direct Methods ◽  
Full Matrix ◽  
Bond Lengths ◽  
Central Bond ◽  
Least Squares Techniques ◽  
Counter Data

Crystals of 1-cyanotetracyclo[3.3.13,7.03,7]decane, C11H13N, are monoclinic, a = 6.442(2), b = 11.739(2), c = 11.965(4) Å, β = 98.14(9)°, Z = 4, space group P21/c. The structure was determined with CuKα scintillation counter data by direct methods, and refined by full-matrix least-squares techniques to R 0.048 for 690 observed reflexions. C(3) and C(7) have all four bonds directed to one side of the atoms, and the central bond distance is 1.643 Å. Other bond lengths and angles are normal.

The crystal structure of p-diethylaminobenzenediazonium hexafluorophosphate

1985 ◽  
Vol 63 (2) ◽  
pp. 332-335 ◽  
Author(s):  
Richard G. Ball ◽  
Richard MacLeod Elofson
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Triple Bond ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
The Mean ◽  
Least Squares Techniques ◽  
Diazo Group

p-Diethylaminobenzenediazonium hexafluorophosphate, C10H14N3+•PF6−, crystallized in space group [Formula: see text] with a = 12.105(4), b = 12.340(5), c = 10.439(4) Å, α = 96.53(3), β = 104.11(3), γ = 64.44(3)°, and Z = 4. The structure was solved using direct methods and refined with full-matrix least-squares techniques on F, to a final R of 0.054 for 1917 reflections with F2 > 3σ(F2). The mean bond lengths for the diazo group are: N—N 1.096(6); C—N 1.357(7) Å. The geometry of the molecule is discussed in terms of the possible resonance forms and it is shown to be consistent with a form in which the N—N triple bond is essentially intact and the aminobenzene moiety has "quinoidal" character.

Structural studies of organoboron compounds. XLIII. 4-[(1-Hydroxycyclohexyl)methyl]-2,2,5-triphenyl-1,3-dioxa-4-azonia-2-borata-4-cyclopentene

1991 ◽  
Vol 69 (3) ◽  
pp. 545-549 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Ute Schumacher ◽  
Mahmood Tajerbashi ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Key Words ◽  
Hydroxamic Acid ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths ◽  
Acid Chelate

The reaction of N′-hydroxy-N-[(1-hydroxycyclohexyl)methyl]benzamide and diphenylborinic anhydride gives 4-[(1-hydroxycyclohexyl)methyl]-2,2,5-triphenyl-1,3-dioxa-4-azonia-2-borata-4-cyclopentene in nearly quantitative yield. Crystals of the product are monoclinic, a = 9.9117(6), b = 13.308(1), c = 17.339(2) Ǻ, β = 99.420(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 = 0.040 and Rw = 0.047 for 2423 reflections with I > 3σ(I). The molecule has a normal five-membered hydroxamic acid chelate structure, the BONCO ring having a B-envelope conformation. Bond lengths (corrected for libration) (N)O—B = 1.535(3), (C)O—B = 1.569(3), C—B = 1.603(3) and 1.601(3) Ǻ are normal for this type of complex. Key words: organoboron compound, boron compound, crystal structure.

Crystal structures of optically active naphthidine (4,4′-diamino-1,1′-binaphthyl) and 1,1′-binaphthyl

1983 ◽  
Vol 61 (1) ◽  
pp. 69-71 ◽  
Author(s):  
Richard A. Pauptit ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Direct Methods ◽  
Optically Active ◽  
Dihedral Angles ◽  
Full Matrix ◽  
Bond Lengths ◽  
Least Squares Techniques

Crystals of optically active naphthidine and of binaphthyl are tetragonal, P41212 (or P43212), a = 7.945(1), 7.164(2), c = 24.264(5), 27.70(1) Å, respectively, Z = 4. The structures were solved by direct methods and refined by full-matrix least-squares techniques to respective R = 0.068 and 0.030 for 548 and 562 reflexions. The dihedral angles between the planes of the naphthalene residues are 87 and 102°, respectively. Bond lengths and angles are normal.

The Crystal Structure of Dimedone

1975 ◽  
Vol 53 (7) ◽  
pp. 1046-1050 ◽  
Author(s):  
Ishwar Singh ◽  
Crispin Calvo
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Symmetry ◽  
Enolic Form ◽  
Full Matrix ◽  
Space Group ◽  
Least Squares Techniques

Dimedone, C8H12O2, crystallizes with monoclinic symmetry, a = 10.079(7), b = 6.835(3), c = 12.438(4) Å, β = 110.24(5)°, space group P21/n and Z = 4. The structure of this compound was solved by direct methods and refined by full-matrix least-squares techniques using 1205 unique reflections to a final R of 0.047. In the solid state it exists in the enolic form and these molecules pack in the crystal in systems of infinite chains linked together by hydrogen bonds in the y direction. These results are virtually the same as recently reported by Semmingsen.

Structural studies of organoboron compounds. XLII. 4,6-Bis(1-cyano-1-methylethyl)-2-mesityl-1,3-dioxa-4,6-diaza-2-boracyclohexane

1991 ◽  
Vol 69 (2) ◽  
pp. 234-238 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Gottfried Lubkowitz ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Least Squares ◽  
Key Words ◽  
Good Yield ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths

The condensation of N,N′-bis(1-cyano-1-methylethyl)-N,N′-dihydroxymethanediamine and mesitylboronic acid gives 4,6-bis(1-cyano-1-methylethyl)-2-mesityl-1,3-dioxa-4,6-diaza-2-boracyclohexane in good yield. Crystals of the latter compound are orthorhombic, a = 15.825(1), b = 17.958(1), c = 14.014(1) Ǻ, Z = 8, space group Pbca. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.037 and Rw = 0.051 for 2844 reflections with 1 ≥ 3σ(I). The molecule has a six-membered cycloboronate structure featuring the first structurally characterized BONCNO ring. The ring was found to have a C-envelope conformation in the solid state. Bond lengths include: O—B(sp2) = 1.356(2) and 1.370(2), and C(aryl)—B = 1.560(2) Ǻ. Key words: organoboron compound, boron compound, crystal structure.

Crystal and molecular structure of L-prolinatodiphenylboron

1977 ◽  
Vol 55 (6) ◽  
pp. 958-965 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Conformational Disorder ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of L-prolinatodiphenylboron are monoclinic, a = 5.9427(5), b = 14.4633(7), c = 8.9654(4) Å, β = 98.423(8)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.037 and Rw of 0.053 for 1477 reflections with I ≥ 3σ(I). The proline ring exhibits conformational disorder. The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.893(3) Å) along the short a axis. Intramolecular N—B coordination occurs to form a system of two fused five-membered rings. Bond lengths (corrected for libration) are: N—B, 1.630(3), O—B, 1.529(3), O—C, 1.219(3) and 1.300(3), N—C, 1.506(3) and 1.507(3), C(sp3)–C(sp3), 1.525(4), C(sp2)—C(sp3), 1.517(3), and mean C—C(phenyl), 1.394 Å.

Crystal structure of 17,18,19-trisnorstemodan-3,13-dione

1984 ◽  
Vol 62 (9) ◽  
pp. 1828-1830 ◽  
Author(s):  
Stephen V. Evans ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Direct Methods ◽  
Membered Ring ◽  
Full Matrix ◽  
Bond Lengths ◽  
Compound C ◽  
Tetracyclic System ◽  
Atom Bond

Crystals of the title compound, C17H24O2, are monoclinic, P21/c, a = 10.395(2), b = 10.980(1), c = 13.181(3) Å, β = 113.55(1)°, Z = 4. The structure was solved by direct methods and refined by full-matrix least-squares to R = 0.051 for 1622 reflections with I ≥ 3σ(I). The molecule contains a tetracyclic system of three six-membered rings and one five-membered ring; the structure exhibits disorder of one C atom. Bond lengths and angles are normal.

Ring contraction of 4-substituted 2,6-dichlorophenols. The crystal structure of 2,2,4α,5α-Tetrachloro-1α,3α-dihydroxycyclopentane-1,4-carbolactone

1977 ◽  
Vol 30 (10) ◽  
pp. 2195 ◽  
Author(s):  
RM Christie ◽  
RW Rickards ◽  
KJ Schmalzl ◽  
D Taylor
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Major Product ◽  
X Ray Diffraction ◽  
Ring Contraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Counter Data

Alkaline chlorination of the 4-alkyl-2,6-dichlorophenols (2b) and (2c) proceeds through ring contraction and halolactonization to form the 4α- alkyl-2,2,5α-trichloro-1α,3α-dihydroxycyclopentane-1,4-carbolactones (4b) and (4c). Under similar conditions, 2,4,6-trichlorophenol affords the analogous 2,2,4α,5α-tetrachloro-1α,3α-dihydroxycyclopentane-1,4- carbolactone (4a) in low yield, in addition to the Hantzsch acid (3a) as the major product. The acid (3a) upon further treatment undergoes chloro-lactonization to give the lactone (4a). The structures of the lactones (4b) and (4c) follow from spectroscopic comparison with (4a), the structure of which has been established by X-ray diffraction (C6H4Cl4O4 orthorhombic a 13.485(1), b 12.348(1), c 11.371(1) Ǻ, space group Pccn, Z 8, solved by direct methods and refined by block-diagonal and full-matrix least squares to R 0.031, Rw 0.043 for 1313 unique counter data with I/σ(I) ≥ 3.0).

Crystal and Molecular Structure of B-Phenyl-diptychboroxazolidine,

1975 ◽  
Vol 53 (10) ◽  
pp. 1393-1401 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Thermal Motion ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of B-phenyl-dictychboroxazolidine are monoclinic, a = 8.4977(4), b = 9.0617(5), c = 7.0105(3) Å, β = 111.627(3)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.040 for 967 reflections with I ≥ 3σ(I). The bond lengths involving nonhydrogen atoms have been corrected for thermal motion. Bond lengths are: B—O, 1.460(3) and 1.474(3), B—N, 1.666(3), B—C, 1.613(3), C—O, 1.411(3) and 1.419(3), C—N, 1.485(3) and 1.486(3), C(sp3)—C(sp3), 1.514(4) and 1.524(4), C—C(ar), 1.384–1.400(4–6), mean C—H, 0.98(4), and N—H, 0.87(5) Å. The crystal structure consists of discrete molecules of B-phenyl-diptychboroxazolidine each linked to two others by N—H … O hydrogen bonds (O … N = 2.914(3) Å) to form continuous spirals along b.

Structural studies of organoboron compounds XL. 4,7-Dicyclohexyl-2,2,5,6-tetraphenyl- 1,3-dioxa-4-aza-7-azonia-2-boratacycloheptane

1990 ◽  
Vol 68 (10) ◽  
pp. 1797-1802 ◽  
Author(s):  
Henning Amt ◽  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Least Squares ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Chair Conformation ◽  
Membered Ring ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths

The synthesis of 4,7-dicyclohexyl-2,2,5,6-tetraphenyl-1,3-dioxa-4-aza-7-azonia-2-boratacycloheptane is reported. Crystals of the compound are orthorhombic, a = 10.893(1), b = 28.072(1), c = 10.596(1) Å, Z = 4, space group P212121. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.036 and Rw = 0.043 for 2480 reflections with I ≥ 3σ(I). The molecule has a seven-membered chelate structure. The seven-membered ring, which has a twisted chair conformation, is stabilized by an intramolecular [Formula: see text] hydrogen bond. Bond lengths O—B = 1.468(4) and 1.554(4), C—B = 1.621(5) and 1.626(4) Å are consistent with moderately strong binding of the diphenylboron moiety by the O,O-chelating ligand. Keywords: crystal structure, organoboron compound, boron compound.

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