Crystal and Molecular Structure of Benzylidenimine Disulfide

1974 ◽  
Vol 52 (17) ◽  
pp. 2985-2989
Author(s):  
James C. Barrick ◽  
Crispin Calvo ◽  
Fredric P. Olsen
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Molecular Geometry ◽  
Intensity Measure ◽  
Full Matrix ◽  
Sulfur Bond ◽  
Automatic Diffractometer ◽  
Nitrogen Bond

The crystal and molecular structure of benzylidenimine disulfide has been determined. Crystals are monoclinic with space group P21/c, Z = 4, a = 12.93(2), b = 5.554(9), c = 20.46(3) Å, and β = 112.5(2)°. A full matrix least squares refinement on 2304 unique reflections of positive intensity measure collected on a [Formula: see text] Automatic diffractometer produced a conventional R of 0.029. The molecular geometry is very similar to that in the corresponding tetra- and trisulfides with a fairly short sulfur–sulfur bond length of 2.033(2) Å and a fairly long sulphur–nitrogen bond length of 1.690(3) Å.

Crystal and Molecular Structure of Benzylidenimine Tetrasulfide, (C6H5CHN)2S4

1973 ◽  
Vol 51 (22) ◽  
pp. 3691-3696 ◽  
Author(s):  
James C. Barrick ◽  
Crispin Calvo ◽  
Fredric P. Olsen
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Least Squares ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Aromatic Rings ◽  
Intensity Measure ◽  
Full Matrix ◽  
Space Group

The structure of the title compound has been determined. Crystals are monoclinic with space group P21/a, Z = 4, a = 13.83(1), b = 19.66(2), c = 5.983(5) Å, β = 101.4(1)°, dcalcd = 1.404, dobs = 1.40(1). A full-matrix least-squares refinement on 1085 unique reflections of positive intensity measure produced a conventional R of 0.066. The spiral arrangement of the S4 chains (nearly generating a 31 axis) is such that the two aromatic rings are eclipsed. Alternation in bond length along the sulfur chain was observed, the long inner bond being 2.083(4) Å and the shorter outer bonds averaging 2.026(3) Å in length. No intermolecular non-bonding interactions involving sulfur were found.

The crystal and molecular structure of (4-diethylaminophenyl)diazenyltriphenylphosphonium tetrafluoroborate

1978 ◽  
Vol 56 (7) ◽  
pp. 891-895 ◽  
Author(s):  
Frederick W. B. Einstein ◽  
Derek Sutton ◽  
Peter L. Vogel
Keyword(s):  
Molecular Structure ◽  
Electronic Structure ◽  
Least Squares ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
Bond Lengths ◽  
A Cell ◽  
Automatic Diffractometer

The title compound crystallizes in the space group P21/c with four formula units in a cell of dimensions a = 10.146(6) Å, b = 10.593(4) Å, c = 26.31(1) Å, β = 103.14(3)°. Using 1496 observed reflections (I = 2.3σ(I)) in the range 0° < 2θ < 40° measured on a Picker FACS-1 automatic diffractometer with Mo-Kα radiation, the structure was solved (symbolic addition) and refined (full-matrix least-squares procedure) to R = 0.062 (Rw = 0.058), with all hydrogen atoms included and all non-hydrogen atoms having anisotropic thermal parameters. The dimensions within the cation are consistent with a delocalized electronic structure which is intermediate between valence formulations involving benzenoid or quinonoid structures for the (4-diethylaminophenyl)diazenyl residue. Some important bond lengths are N3—C22 1.336(7) Å, N2—C19 1.356(7) Å, N1—N2 1.308(6) Å, and P—N1 1.648(5) Å.

scholarly journals Crystal and molecular structure of 2,2,4,6,6-pentamethyl-5-benzoyl-4-(N-methylbenzamido)-1,3-diaza-2,4,6(Pv)-triphosphorin

1977 ◽  
Vol 55 (13) ◽  
pp. 2534-2539 ◽  
Author(s):  
Richard T. Oakley ◽  
Norman L. Paddock ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Full Matrix ◽  
Bond Lengths ◽  
Benzoyl Group ◽  
Electron Withdrawal ◽  
Related Compounds ◽  
Twist Boat

Crystals of 2,2,4,6,6-pentamethyl-5-benzoyl-4-(N-methylbenzamido)-1,3-diaza-2,4,6(Pv)-tri-phosphorin are triclinic, a = 13.375(1), b = 11.313(1), c = 7.925(1) Å, α = 107.72(1), β = 98.23(1), γ = 87.00(1)°, Z = 2, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.067 and Rw of 0.089 for 3954 reflections with. I ≥ 3σ(I) The P3N2C ring is nearly planar and has a conformation corresponding to a flattened version of the chair – twist boat. Bond lengths in the azaphosphorin ring, P—N, 1.579–1.614(2), and P—C, 1.752(3) and 1.777(3) Å, indicate conjugation with the C-benzoyl group. The exocyclic P—N bond length, 1.742(3) Å, is longer than those in related compounds as a result of competitive electron withdrawal from the N-benzoyl group. Other bond lengths (corrected for libration) are: mean P—Me, 1.796(4); C=O, 1.242(3) and 1.247(4); C—N, 1.472(3) and 1.369(4); mean C—C(phenyl), 1.391(10); other C(sp2)—C(sp2); 1.417–1.518(4) Å.

Crystal and molecular structure of 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[3,4-methoxy]phenyl-l,4-dihydropyridine hemihydrate and 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[furan]1,4-dihydropyridine

1999 ◽  
Vol 214 (12) ◽  
Author(s):  
M. Bidya Sagar ◽  
K. Ravikumar ◽  
Y. S. Sadanandam
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal Structures ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Asymmetric Unit ◽  
Full Matrix

AbstractThe crystal structures of two dihydropyridines were solved by direct methods and refined by full-matrix least-squares procedure. 2,6-Dimethyl-3,5-di[N-methyl]-carbamoyl-4-[3,4-methoxy]phenyl-1,4-dihydropyridine hemihydrate, CBoth compounds crystallize with two molecules in the asymmetric unit. In compound

Crystal and molecular structure of [dimethyl(3,5-dimethyl-1-pyrazolyl)(ethanol-amino)gallato (N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum

1981 ◽  
Vol 59 (11) ◽  
pp. 1665-1670 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Amino Nitrogen ◽  
Full Matrix ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Unusual Type

Crystals of [dimethyl(3,5-dimethyl-l-pyrazolyl)(ethanolamino)gallato(N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum are monoclinic, a = 10.511(1), b = 8.335(1), c = 24.138(3) Å, β = 102.22(1)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was reflned by full-matrix least-squares procedures to R = 0.028 and Rw = 0.046 for 3708 reflections with I ≥ 3σ(I). The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.929(5) Å). The Mo atom is in a distorted octahedral environment with the η3-C7H7 ligand occupying one coordination site, trans to the amino nitrogen, as a π-donating ligand. Important bond distances (corrected for libration) are: Mo—O, 2.245(2), Mo—N(amino), 2.249(3), Mo—N(pyrazolyl), 2.270(3), Mo—C(O), 1.950(4) and 1.947(4), Mo—C(C7H7), 2.176(4), 2.364(4), and 2.380(4), Ga—O, 1.919(3), Ga—N, 1.984(3), and Ga—C, 1.982(5) and 1.983(5) Å. An unusual type of disorder is present in which a second image of the molecule, approximately mirrored by the plane y = 1/4, is in evidence at low occupancy.

The crystal and molecular structure of anti-1,2,4,5-tetraphenyl-3,6-dicarbomethoxytricyclo[3.1.0.02,4]hexane

1978 ◽  
Vol 56 (10) ◽  
pp. 1364-1367 ◽  
Author(s):  
M. J. Bennett ◽  
J. T. Purdham
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Experimental Error ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Bond Lengths ◽  
Highly Strained ◽  
Least Squares Techniques

1,2,4,5-Tetraphenyl-3,6-dicarbornethoxytricyclo[3.1.0.02,4]hexane crystallizes in the monoclinic space group P21/c with a = 10.044(4), b = 9.500(2), c = 14.172(4) Å, β = 104.38(2)°, and Z = 2. Using 1032 unique reflections with I > 3σ(I), the structural data were refined by full matrix least-squares techniques to R = 0.038. The molecule was found to be in the anti-configuration. All bond lengths within the highly strained central tricyclic framework were equal within experimental error and average 1.531 Å.

Reaction of N,N′-dihydroxy-.N,N′-dimethylmethanediamine with phenylboronic acid and the crystal and molecular structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine

1989 ◽  
Vol 67 (11) ◽  
pp. 1959-1963 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Exact Formula ◽  
Full Matrix ◽  
Space Group ◽  
Hydrogen Bonded

The reaction of N,N′-dihydroxy-N,N′-dimethylmethanediamine with phenylboronic acid leads to the product 1,7-dimethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5-boratabicyclo[3.3.0]octane rather than the expected product 1,5-dimethyl-3-phenyl-1,5-diaza-2,4-dioxa-3-boracyclohexane. The structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine has been determined and is discussed in terms of its reaction with PhB(OH)2. Crystals of N,N′-dihydroxy-N,N′-dimethylmethanediamine are tetragonal, a = 8.5346(3), c = 8.4178(7) Å, Z = 4, space group P421c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.036 and Rw of 0.038 for 333 reflections with I ≥ 3σ(I). The structure consists of hydrogen-bonded dimers having exact [Formula: see text] symmetry. Keywords: N,N′-dihydroxy-N,N′-dimethylmethanediamine, crystal structure.

Crystal and molecular structure of 3-ethyl-4-hydroxy-1,2,3(4H)-benzotriazine and 6-chloro-4-hydroxy-3-methyl-4-phenyl-1,2,3-benzotriazine

1985 ◽  
Vol 63 (3) ◽  
pp. 581-585 ◽  
Author(s):  
Kwong Khee Lai ◽  
Carl H. Schwalbe ◽  
Keith Vaughan ◽  
Ronald J. Lafrance ◽  
Clive D. Whiston
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Tetrahedral Geometry ◽  
Orthorhombic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor

The crystal structures of the title compounds have been determined from X-ray data collected on a four-circle diffractometer and refined by the full-matrix least-squares method. The former compound crystallizes in the orthorhombic system, space group Pbcn, with a = 14.346(8), b = 7.239(1), c = 17.276(2) Å, and has been refined to a conventional R factor of 0.043 for 890 observed reflections. Corresponding results for the latter compound are monoclinic, P21/n, a = 12.222(4), b = 7.482(2), c = 14.170(8) Å, β = 94.06(4)°, R = 0.060 for 2128 observed data. The triazine rings of both compounds exhibit short N(1)—N(2) bonds and tetrahedral geometry at C(4); however, the ring is puckered in the first compound but flat in the second. Molecules in both crystals are linked by [Formula: see text] hydrogen bonds.

Crystal and molecular structure of difluoroboron N-methylacethydroxamate (2,2-difluoro-4,5-dimethyl-1,3-dioxa-4-azonia-2-boranatacyclopent-4-ene)

1977 ◽  
Vol 55 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
D. Nanninga
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of difluoroboron N-methylacethydroxamate are monoclinic, a = 5.097(1), b = 10.653(2), c = 11.520(2) Å, β = 103.57(2)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.056 and Rw of 0.077 for 988 reflections with I ≥ 3σ(I). The structure features a planar five-membered BO2CN ring. Bond lengths (corrected for libration) are: B—F, 1.374(3) and 1.381(3), O—B, 1.496(3) and 1.497(3), O—N, 1.349(2), O—C, 1.346(2), C—N, 1.298(3) and 1.458(3), and C—C, 1.468(3) Å.

Crystal and Molecular Structure of 2,5-Bis(2′-hydroxyethylamino)-1,4-benzoquinone

1975 ◽  
Vol 53 (5) ◽  
pp. 777-783 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Compound C ◽  
Related Compounds ◽  
Centrosymmetric Molecule

Crystals of 2,5-bis(2′-hydroxyethylamino)-1,4-benzoquinone are monoclinic, a = 5.020(1), b = 19.238(3), c = 5.214(1) Å, β = 96.15(3)°, Z = 2, space group P21/n. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.045 for 646 reflections with I ≥ 3σ(I). The benzoquinone ring in the centrosymmetric molecule is slightly, but significantly, nonplanar. Bond distances in the compound (C—C, 1.247 (2) and 1.410 (3), C—N, 1.332 (3) and 1.457 (3), C—C, 1.384–1.514 (3), N—H, 0.89 (3), O—H, 1.07 (5), and C—H, 0.95–1.09 (3) Å) are similar to those in related compounds. The structure features an extensive network of N—H … O (N … O = 2.639 (3) and 3.033 (2) Å) and O—H … O(O … O = 2.757 (3) Å ) hydrogen bonds.

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