The Crystal and Molecular-Structure of 4,7,13-Trioxa-1,10-diazacyclopentadecanepotassium(I) Thiocyanate

1988 ◽  
Vol 41 (9) ◽  
pp. 1363 ◽  
Author(s):  
A Abouhamdan ◽  
SF Lincoln ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Compound K ◽  
Unit Cell Parameters ◽  
Full Matrix ◽  
Cell Parameters

The crystal structure of the title compound [K(-NHCH2CH2OCH2CH2OCH2CH2NHCH2CH2OCH2CH2-)(NCS)] has been determined. Potassium(I) is 1.41 Ǻ above the plane of the three oxygens of the 4,7,13-trioxa-1,10-diazacyclopentadecane ligand, and is seven-coordinated. Potassium(I) is 2.871(7), 2.798(7) and 2.772(7)Ǻ from the three oxygens, and 2.905(8) and 2.945(8)Ǻ from the two nitrogens of 4,7,13-trioxa-1,10-diazacyclopentadecane, 2.861(7)Ǻ from an oxygen of a second such ligand, and 2.809(8)Ǻ from the thiocyanate nitrogen. Crystals are monoclinic, space group P21/n with unit cell parameters a 8.015(4), b 14.755(4), c 13.744(4)Ǻ, β 95.37(3)°, and Z 4. The structure was solved by direct methods and refined by a full-matrix least-squares procedure to final R 0.089, Rw 0.099 for 981 reflections with I ≥ 2.5σ(I).

The Crystal Structure of S-Methyl 1-[Dicyclohexyl(thiophosphoryl)]-dithioformate: (c-C6H11)2P(S)C(S)Sme

1988 ◽  
Vol 41 (3) ◽  
pp. 405 ◽  
Author(s):  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Mirror Plane ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Interatomic Distances ◽  
Full Matrix ◽  
Cell Parameters ◽  
Compound C

The crystal structure of the title compound, (c-C6H11)2P(S)C(S)SMe , has been determined and shows that the P(S)C(S)SC chromophore is situated on a crystallographic mirror plane with the cyclohexyl groups related to each other across this plane. Significant interatomic distances are: P=S 1.951(1), P-C 1.860(4), C=S 1.632(4) and C-S 1.700(4)Ǻ. A resonance scheme involving the delocalization of π-electrons over the CS2 moiety has been invoked to account for the observed C-S bond distances in the molecule. Crystals are orthorhombic, space group Pnma with unit cell parameters a 10.196(2), b 10.612(1) and c 15.370(3)Ǻ, and Z 4. The structure was solved by direct methods and refined by a full-matrix least-squares procedure to final R 0.045, Rw 0.047 for 1191 reflections with I ≥ 3.0σ(I).

Crystal and Molecular Structure of 2-Deacylusnic Acid

1974 ◽  
Vol 52 (5) ◽  
pp. 723-733 ◽  
Author(s):  
Alistair L. Macdonald ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structural Feature ◽  
Absolute Configuration ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Anomalous Scattering ◽  
Full Matrix

Crystals of the title compound are monoclinic a = 9.801(2) b = 9.120(1) c = 8.026(2) Å, β = 107.45(1)°, Z = 2, space group P21. The structure was determined by direct methods, and refined by electron-density and full-matrix least-squares procedures to R = 0.0325 for 1363 observed reflections. An attempt to determine the absolute configuration by use of the anomalous scattering of oxygen and carbon atoms has been made. The most important structural feature is delocalization in the cyclohexadiene ring. There are two intramolecular O—H … O hydrogen bonds, O … O distances 2.532(3) and 2.712(2) Å. The crystal structure consists of molecules linked by intermolecular O—H … O hydrogen bonds, O … O = 2.625(2)Å, to form continuous spirals about the 21 axes.

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.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

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.

Structural studies of organoboron compounds. XXII. Preparation and crystal and molecular structure of tetramethylammonium-2,4,6,6-tetraphenyl-1,3,5-trioxa-2,4- dibora-6-boratacyclohexane

1985 ◽  
Vol 63 (12) ◽  
pp. 3516-3520 ◽  
Author(s):  
W. Kliegel ◽  
H.-W. Motzkus ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Physical Properties ◽  
Crystal And Molecular Structure ◽  
Structural Parameters ◽  
Direct Methods ◽  
Maximum Deviation ◽  
Structural Studies ◽  
Full Matrix ◽  
The Mean

Details of the preparation and physical properties of (Me4N)+ (Ph4B3O3)− are given. Crystals of tetramethylammonium 2,4,6,6-tetraphenyl-1,3,5-trioxa-2,4-dibora-6-boratacyclohexane are orthorhombic, a = 18.130(2), b = 11.9745(7), c = 12.5187(5) Å, Z = 4, space group Pna21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.056 and Rw = 0.064 for 1460 reflections with I ≥ 2σ(I). The crystal structure consists of discrete tetramethylammonium cations and tetraphenylboroxinate anions, the first such anion to be structurally characterized. The six-membered B3O3 ring is significantly non-planar, having a flattened O(1)-envelope conformation (maximum deviation from the mean plane = 0.074(4) Å for O(1)). The boroxine ring in the anion shows significant deviations from the D3h symmetry observed for neutral boroxines. Important mean structural parameters: B(sp3)—O = 1.494(2), B(sp2)—O[B(sp3)] = 1.320(9), B(sp2)—O[B(sp2)] = 1.389(3) Å, O—B(sp3)—O = 110.5(5), O—B(sp2)—O = 121.7(6), B(sp2)—O—B(sp2) = 118.9(5), and B(sp3)—O—B(sp2) = 122.9(1)°.

The Crystal and Molecular Structure of Butorphanol Hydrogen Tartrate

1994 ◽  
Vol 59 (6) ◽  
pp. 1361-1367 ◽  
Author(s):  
Alexandr Jegorov ◽  
Roman Sobotík ◽  
Svetlana Pakhomova ◽  
Jan Ondráček ◽  
Jiří Novotný ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Triclinic Space Group ◽  
Space Group

The structure of butorphanol hydrogen tartrate {(9R,13S,14S)-(-)-17-(cyclobutylmethyl)morphinan-3,14-diol (2S,3S)-(-)-hydrogen tartrate} (C21H29NO2 .C4H6O6) was solved by direct methods and refined anisotropically to the R value of 0.029 for 2 069 observed reflections. The title morphine analogue crystallizes in the triclinic space group P1 with lattice parameters a = 7.620(1), b = 9.140(1), c = 9.591(1) Å, α = 105.48(1), β = 112.91(1), γ = 84.29(1)°, Z = 1. The butorphanol B ring possesses the 3E envelope conformation with small 3H2 distortion, C and D rings have a regular chair conformation. The intramolecular N17-H17...O2 hydrogen bond is observed in crystal structure of the title compound. The butorphanol and hydrogen tartrate molecules are joined together by means of O2-H(O2)...O7, O1-H(O1)...O7' and O3-H(O3)...O8" hydrogen bonds to form networks.

Crystal and molecular structure of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]octane

1976 ◽  
Vol 54 (20) ◽  
pp. 3142-3151 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
H. Becker
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Boron Atom ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
The Other ◽  
Full Matrix ◽  
Atom Bond ◽  
Tetrahedral Boron

Crystals of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]-octane are monoclinic, a = 22.323(1), b = 9.555(1), c = 16.0027(6) Å, β = 109.055(4)°, Z = 8, space group C2/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.048 and Rw of 0.066 for 2629 reflections with I ≥ 3σ(I). The central part of the molecule consists of two fused five-membered rings. One of them is a familiar BOCCN ring while the other is a novel and nearly planar BOBON ring containing one tetrahedral boron atom and one trigonal planar boron atom. Bond lengths are: O—B, 1.337(2)–1.467(2), N—B, 1.692(2), O—N, 1.440(2), O—C, 1.426(2), N—C, 1.513(2), B—C, 1.557(2) and 1.599(2), C(sp3)—C(sp3), 1.520(2)–1.530(2), C—C(ar), 1.372(4)–1.407(2), N—H, 0.89(2), mean C(ar)—H, 0.97(1), and mean C(sp3)—H, 1.01(1) Å. The crystal structure consists of discrete molecules each linked to two others by N—H … O hydrogen bonds (N … O = 2.853(2) Å).

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.

Oxide meets silicide – synthesis and single-crystal structure of Ca21SrSi24O2

2017 ◽  
Vol 72 (4) ◽  
pp. 313-316
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Calcium Ions ◽  
Title Compound ◽  
Silicon Powder ◽  
Thin Plates ◽  
Monoclinic Space Group ◽  
Strontium Chloride ◽  
Unit Cell Parameters ◽  
Cell Parameters ◽  
Calcium Metal

AbstractA few black, rectangular thin plates of Ca21SrSi24O2 were obtained by serendipity in a solid-state reaction of calcium metal, strontium chloride and silicon powder at 1200 K for 2 days designed to produce ‘Ca2SrCl2[Si3]’. The title compound forms next to some CaSi and some remaining educts. Ca21SrSi24O2 crystallizes in the monoclinic space group C2/m (no. 12) with unit cell parameters of a=1895.2(2), b=450.63(5) and c=1397.33(18) pm and β=112.008(7)° (Z=1). The title compound shows planar, eight-membered, kinked Si8 chains with Si–Si distances between 241.4 and 245.0 pm indicating bonding interactions and kinked ‘rope ladders’ connecting the chains with interatomic Si–Si distances in the range 268.1–274.7 pm. Embedded in between these silicon substructures are columns of oxygen centered, apex sharing [(Ca1−x Srx)6/2O] octahedra and calcium ions.

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