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.

The crystal and molecular structure of lead(II)bromide-bis-dimethylsulphoxide, PbBr2•2[(CH3)2SO]

1977 ◽  
Vol 55 (5) ◽  
pp. 849-855 ◽  
Author(s):  
Anthony D. Baranyi ◽  
Mario Onyszchuk ◽  
Yvon Le Page ◽  
Gabrielle Donnay
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Title Compound ◽  
Lone Electron Pair ◽  
Electron Pair ◽  
Crystal And Molecular Structure ◽  
Crystal Packing ◽  
The Other ◽  
Full Matrix ◽  
A Cell

The title compound has two PbBr2•2[(CH3)2SO] units, Z = 2, in a cell with a = 11.093(2), b = 12.382(3), c = 4.540(1) Å, belonging to space group Pmmn. The structure was solved by Patterson functions and was refined by full-matrix least-squares calculations to a final R of 0.054 for 348 observed diffractometer intensities. Passing through the unit cell are two antiparallel, infinite polar chains, each with symmetry mm2, extending along z and interacting with each other by weak van der Waals forces. Lead(II) is six-coordinate with a close, covalent hemisphere consisting of two bromine atoms [Pb—BrIBrII 2.93(1) Å], and two oxygen atoms [Pb—O,O′ 2.50(3) Å] which subtend an angle of 157.9(9)° at lead, located at the intersection of the O—Pb—O′ and BrI—Pb—BrII perpendicular mirror planes. The other hemisphere consists of bridging bromine atoms from the neighboring PbBr2•2dmso unit [Pb—BrIII,BrIV 3.24(1) Å], resulting in a rectangle of bromine atoms around lead [BrI—Pb—BrII 90.5(1)°, BrIII—Pb—BrIV 80.2(1)°]. The distortion of the octahedral coordination sphere around lead is discussed in terms of (a) a repulsive effect of the Pb(II) valence lone electron-pair, (b) weak Br—S bonding, and (c) crystal packing forces.

Contributions to the Chemistry of Boron, LXXV The Crystal and Molecular Structure of a Tetraazadiborine: 3,6-Bis(dimethylamino)-1,2,4,5-tetramethyl-1,2,4,5,3,6-tetraazadiborine

1976 ◽  
Vol 31 (3) ◽  
pp. 289-293 ◽  
Author(s):  
J. C. Huffman ◽  
H. Fusstetter ◽  
H. Nöth
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Membered Ring ◽  
Unit Cell ◽  
Hydrogen Atoms ◽  
Monoclinic System ◽  
Full Matrix ◽  
Bond Lengths

The title compound crystallizes in the monoclinic system with dimensions of the unit cell a = 14.09(2), b = 8.60(1), c = 11.34(1) Å and β = 101.7°. The space group was determined to be A 2/a with four molecules in the unit cell. The structure was solved by direct methods, and all hydrogen atoms were located. Full matrix refinement led to R = 0.059. The B2N4 six membered ring is nonplanar as expected for an 8π electron heterocycle. The molecule possesses C2 symmetry but the ring itself is near the D2 symmetry as derived from earlier CNDO/S-calculations. The BN bond lengths are 1.43 A, the NN distances 1.43 Å and the average CN distances 1.44 A. The boron atoms and four of the six nitrogen atoms are trigonal-planarly coordinated while the remaining two N-atoms (N1,N2) deviate little, but significantly, from sp2 hybridisation. The structure of the molecule can be interpreted as the best compromise between ΒΝ-π-bonding, nonbonding repulsion between adjacent CH3 groups, and the interaction between neighbouring ‘free pairs of electrons’ of the ring N-N-units.

Crystal and Molecular Structure of B,B- Diphenylboroxazolidine (2-Aminoethyl Diphenylborinate),

1973 ◽  
Vol 51 (8) ◽  
pp. 1288-1294 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Electron Density ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Full Matrix ◽  
Bond Lengths

Crystals of the title compound are monoclinic, a = 13.840(1), b = 8.9169(5), c = 10.170(1) Å, β = 98.85(1)°, Z = 4, space group P21/n. The structure was determined by direct methods, and refined by electron-density and full-matrix least-squares procedures to R 0.041 for 1458 observed reflections. The five-membered boroxazolidine ring is in the half-chair conformation. Bond angles in the ring range from 99.7° for OBN to 110.1° for BOC. Bond lengths are as follows: mean B—C, 1.611(2), B—N, 1.653(3), B—O, 1.484(3), C—N, 1.485(3), C—O, 1.413(3), mean C—C (aromatic), 1.383(11), and C—C, 1.505(4) Å. The structure consists of discrete molecules linked by O…H—N hydrogen bonds (2.874(2) Å) to form continuous spirals about the 21 axes.

Crystal and molecular structure of (salicylaldehydato)diphenylboron

1976 ◽  
Vol 54 (7) ◽  
pp. 1168-1175 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Thermal Motion ◽  
Hydrogen Atoms ◽  
Weighted Mean ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of (salicylaldehydato)diphenylboron are orthorhombic, a = 11.6548(5), b = 16.2983(5), c = 8.0806(2) Å, Z = 4, space group Pna21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.051 for 1386 reflections with I ≥ 3σ(I). The BO2C3 ring has a distorted 'sofa' conformation. Bond lengths in the molecule (those not involving hydrogen atoms have been corrected for thermal motion) are: C—O, 1.263(4) and 1.334(4), B—O, 1.500(4) and 1.574(4), C—B, 1.603(5) and 1.610(5), C—C(salicylaldehyde), 1.368–1.423(5–8), C—C(phenyl), 1.352–1.413(5–11), and weighted mean C(sp2)—H, 0.96 Å.

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.

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 [dimethyl(1-pyrazolyl)(2-pyridyl-methoxy)gallato-N2,O,N3](η3-allyl)dicarbonylinolybdenum(II)

1988 ◽  
Vol 66 (3) ◽  
pp. 355-358 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
Pyridyl Nitrogen ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of [dimethyl(1-pyrazolyl)(2-pyridylmethoxy)gallato-N2,O,N3](η3-allyl)dicarbonylmolybdenum(II) are triclinic, a = 9.632(2), b = 9.798(2), c = 10.255(2) Å, α = 80.16(1), β = 87.38(1), γ = 81.75(1)°, Z = 2, space group [Formula: see text]. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.037 for 3000 reflections with I ≥ 3σ(I). The molecule has pseudo-octahedral coordination geometry with the tridentate [Me2Ga(N2C3H3)(OCH2(C5H4N))]− ligand facially coordinated and the η3-allyl ligand occupying one coordination site trans to the pyridyl nitrogen atom. Important bond lengths are Mo—O = 2.219(2), Mo—N(py) = 2.212(3), Mo—N(pz) = 2.232(2), Mo—C(allyl) = 2.290(4), 2.189(4), 2.341(4), Mo—CO (trans to O) = 1.928(4), and Mo—CO (trans to N) = 1.952(4) Å.

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 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 diphenylboron N-methylacethydroxamate (4,5-dimethyl-2,2-diphenyl-1,3-dioxa-4-azonia-2-boratacyclopent-4-ene)

1978 ◽  
Vol 56 (12) ◽  
pp. 1676-1680 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
D. Nanninga
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Heterocyclic Ring ◽  
Mirror Plane ◽  
Full Matrix ◽  
Space Group ◽  
Carbon And Nitrogen ◽  
Bond Lengths

Crystals of diphenylboron N-methylacethydroxamate are orthorhombic, a = 12.5478(8), b = 7.8735(3), c = 13.6809(5) Å, Z = 4, space group Pnam. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.037 and Rw = 0.054 for 1265 reflections with I ≥ 3σ(I). The molecule features a five-membered BO2CN ring which lies in the crystallographic mirror plane. The carbon and nitrogen atoms of the heterocyclic ring are positionally disordered. Mean bond lengths (corrected for libration) are: O—B, 1.550(2), B—C, 1.609(2), O—C/N, 1.340(3), C—N, 1.300(2), C/N—CH, 1.470(2), and C—C(phenyl), 1.394(8) Å.

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