Structural studies of some 1-polymethyleneimino-2,4-dinitrobenzenesand related compounds; crystal structure of 1-(cis-2′,6′-dimethylpiperidin-1′-yl)-2,4-dinitrobenzene

2000 ◽  
Vol 53 (8) ◽  
pp. 715 ◽  
Author(s):  
Maureen F. Mackay ◽  
Douglas J. Gale ◽  
John F. K. Wilshire
Keyword(s):  
Crystal Structure ◽  
Phenyl Ring ◽  
Ring Opening ◽  
Boat Conformation ◽  
Structural Studies ◽  
X Ray ◽  
X Ray Crystallography ◽  
The Mean ◽  
Related Compounds ◽  
Solid State Conformation

The ultraviolet and 1H n.m.r. spectra of some 1-polymethyleneimino-2,4-dinitrobenzenes and related compounds are discussed. The effect of trifluoroacetic acid on these spectra was also investigated; with 1-azetidinyl-2,4-dinitrobenzene, acid-catalysed ring opening was observed. The solid-state conformation of 1-(cis-2′,6′-dimethylpiperidin-1′-yl)-2,4-dinitrobenzene has been defined by single-crystal X-ray crystallography. Triclinic crystals belong to the space group P–1 with a 8.165(1), b 7.865(1), c 11.148(1) Å, α 95.23(1), β 106.00(1), γ 92.63(1)˚ and Z 2. The structure was refined to a final R of 0.048 for the 2222 observed data. In the crystal, the phenyl ring adopts a slight boat conformation, while the amino and o-nitro groups are significantly twisted from the mean plane of the ring.

scholarly journals Crystal structure of (3S*,4R*)-4-fluoro-3-(4-methoxyphenyl)-1-oxo-2-phenyl-1,2,3,4-tetrahydroisoquinoline-4-carboxylic acid

2017 ◽  
Vol 73 (6) ◽  
pp. 867-870
Author(s):  
Anna Lehmann ◽  
Lisa Lechner ◽  
Krzysztof Radacki ◽  
Holger Braunschweig ◽  
Ulrike Holzgrabe
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Carboxylic Acid ◽  
Phenyl Ring ◽  
Ring System ◽  
Piperidine Ring ◽  
Boat Conformation ◽  
Bond Forming ◽  
Compound C ◽  
The Mean

The title compound, C23H18FNO4, crystallized as a racemate. It exhibits acisconformation with respect to the F atom and the methine H atom. The piperidine ring has a screw-boat conformation. The methoxyphenyl ring and the phenyl ring are inclined to the mean plane of the isoquinoline ring system by 89.85 (4) and 46.62 (5)°, respectively, and by 78.15 (5)° to one another. In the crystal, molecules are linked by an O—H...O hydrogen bond forming chains propagating along thea-axis direction. The chains are linked by C—H...F hydrogen bonds, forming layers lying parallel to theabplane.

scholarly journals Synthesis, Characterization, and Bioactivity of Schiff Bases and TheirCd2+,Zn2+,Cu2+, andNi2+Complexes Derived from Chloroacetophenone Isomers with S-Benzyldithiocarbazate and the X-Ray Crystal Structure of S-Benzyl-β-N-(4-chlorophenyl)methylenedithiocarbazate

2013 ◽  
Vol 2013 ◽  
pp. 1-13 ◽  
Author(s):  
Mohammed Khaled bin Break ◽  
M. Ibrahim M. Tahir ◽  
Karen A. Crouse ◽  
Teng-Jin Khoo
Keyword(s):  
Crystal Structure ◽  
Phenyl Ring ◽  
Crystallographic Analysis ◽  
Gram Negative Bacteria ◽  
Schiff Base Ligands ◽  
Gram Negative ◽  
X Ray ◽  
X Ray Crystallography ◽  
Gram Positive Bacteria ◽  
Antimicrobial Assay

Two bidentate Schiff base ligands having nitrogen sulphur donor sequence were derived from the condensation of S-benzyldithiocarbazate (SBDTC) with 2-chloroacetophenone and 4-chloroacetophenone to give S-benzyl-β-N-(2-chlorophenyl)methylenedithiocarbazate (NS2) and S-benzyl-β-N-(4-chlorophenyl)methylenedithiocarbazate (NS4) isomers. Each of the ligands was then chelated with Cd2+, Zn2+, Cu2+, and Ni2+. The compounds were characterized via IR spectroscopy and melting point while the structure of NS4 was revealed via X-ray crystallography. Finally, the compounds were screened for antimicrobial activity to investigate the effect that is brought by the introduction of the chlorine atom to the benzene ring. X-ray crystallographic analysis showed that the structure of NS4 is planar with a phenyl ring that is nearly perpendicular to the rest of the molecules. The qualitative antimicrobial assay results showed that NS4 and its complexes lacked antifungal activity while Gram-positive bacteria were generally inhibited more strongly than Gram-negative bacteria. Furthermore, NS4 metal complexes were inhibited more strongly than the ligand while the opposite was seen with NS2 ligand and its complexes due to the partial solubility in dimethyl sulfoxide (DMSO). It was concluded that generally NS2 derivatives have higher bioactivity than that of NS4 derivatives and that the Cd complexes of both ligands have pronounced activity specifically onK. rhizophila.

scholarly journals Synthesis and Conformational Analysis of Sterically Congested (4R)-(−)-1-(2,4,6-Trimethylbenzenesulfonyl)-3-n-butyryl-4-tert-butyl-2-imidazolidinone: X-Ray Crystallography and Semiempirical Calculations

2014 ◽  
Vol 2014 ◽  
pp. 1-15 ◽  
Author(s):  
Ibrahim A. Al-Swaidan ◽  
Adel S. El-Azab ◽  
Amer M. Alanazi ◽  
Alaa A.-M. Abdel-Aziz
Keyword(s):  
Crystal Structure ◽  
Conformational Analysis ◽  
Phenyl Ring ◽  
Crystal Packing ◽  
Molecular Mechanic ◽  
Structural Data ◽  
Am1 Method ◽  
Geometrical Parameters ◽  
X Ray ◽  
X Ray Crystallography

The crystal structure of (4R)-(−)-1-(2,4,6-trimethylbenzenesulfonyl)-3-n-butyryl-4-tert-butyl-2-imidazolidinone(3)was determined by single-crystal X-ray diffraction. Compound3crystallizes in triclinic system in space groupP1 (≠1). The crystal data area=10.62165 Å,b=16.5321 Å,c=8.95729 Å,∝=91.1936∘,β=93.8496∘,γ=88.0974∘,V=1568.22 Å3,Z=3,Dcalc=1.253 g/cm3,μCuKα=15.98 cm−1,F000=636.00,T=20.0°C, andR=0.037. The crystal structure confirmed the occurrence of three molecules of3A,3B, and3Cin which then-butyryl moiety adopted thes-transoidconformation. Crystal structure also revealed that the conformation of 2,4,6-trimethylbenzenesulfonyl groups was inanti-position relative totert-butyl group. The crystal packing showed that three molecules of compound3are stacked as a result of intermolecularπ-πinteractions between the phenyl ring of one molecule and the phenyl ring of the other molecule by approaching each other to an interplanar separation of 5.034 Å. Interestingly, these stacked molecules are also connected by intermolecularCH-πinteraction. The conformational analysis of thes-transoid  3A,3B, and3Cwas separately performed by molecular mechanic MM+ force field. Additionally, computational investigation using semiempirical AM1 and PM3 methods was performed to find a correlation between experimental and calculated geometrical parameters. The data obtained suggest that the structural data furnished by the AM1 method is in better agreement with those experimentally determined for the above compound. It has been found that the lowest energetic conformer computed gives approximate correspondence with experimental solid state data.

Kinetic benzylidenation. Part I. The selective formation of five-membered ring benzylidene acetals from aldose diethyl dithioacetals

1986 ◽  
Vol 64 (12) ◽  
pp. 2388-2396 ◽  
Author(s):  
T. Bruce Grindley ◽  
Srihari Kusuma ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Phenyl Ring ◽  
Dimethyl Acetal ◽  
Membered Ring ◽  
Sugar Chain ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Intermolecular Reaction ◽  
Selective Formation

Reaction of D-arabinose diethyl dithioacetal with one equivalent of benzaldehyde dimethyl acetal in the presence of p-toluenesulfonic acid at −40 °C gave a mixture of the two epimers of 5-O-methoxyphenylmethyl-D-arabinose diethyl dithioacetal initially. After 14 h at −20 °C, the major products were R- and S-4,5-O-benzylidene-D-arabinose diethyl dithioacetal. The structure of the S isomer was determined by X-ray crystallography. The crystal was orthorhombic, with space group P212121, cell dimensions a = 5.179(4), b = 12.469(3), c = 27.150(4) Å, and Z = 4. The crystal structure was solved using the SHELX (76) system and refined to R = 0.060 for 714 reflections. The sugar chain was in a zigzag conformation, the 4,5-O-benzylidene ring in a 0−5Tc conformation, and the plane of the phenyl ring was nearly perpendicular to the plane of the five-membered ring (88° angle). There were two short OH—S hydrogen bonds, one intramolecular and one intermolecular. Reaction of the diethyl dithioacetals of D-glucose, D-galactose, D-mannose, and D-ribose at −20 °C as above also gave mixtures of the terminal five-membered ring O-benzylidene diastereomers.

Crystal Engineering towards Design of Macrocyclic Coordination Compounds: Crystal Structure of Rubidium Tetrachloro-and Tetracyanoaurate(III) Complexes with 18-Crown-6

1998 ◽  
Vol 53 (7) ◽  
pp. 683-688 ◽  
Author(s):  
Julia A. Manskaya ◽  
Konstantin V. Domasevitch ◽  
Vera V. Ponomareva ◽  
Joachim Sieler ◽  
Volodimir N. Kokozay
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Crystal Engineering ◽  
Coordination Compounds ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Rubidium Atom ◽  
X Ray ◽  
X Ray Crystallography ◽  
The Mean

Abstract The new macrocyclic complexes of composition Rb(18-crown-6)AuX4 (X = Cl (1) and CN (2)) have been prepared and characterized by X-ray crystallography (1: monoclinic, space group P21/n, with a = 8.747(1), b = 8.366(1), c = 15.404(1) Å; β = 104.37(1)°, V = 1092.0(3) Å3 , Z = 2; final R1 =0.025 for 2030 independent reflections used; 2: monoclinic, space group P21/c, with a = 14.765(3), 6 = 17.134(3), c = 8.855(2) Å; β = 90.20(1)°, V = 2240.2(8) Å3, Z = 4; final R1 = 0.080 for 2034 independent reflections used). Both structures consist of Rb(18-crown-6)+ cations (A) and complex aurate(III) anions AuX4- (B). Complex 1 has a linear polymeric array -A-B-A-B-(Rb-Cl 3.604(3), 3.654(3) Å) with the rubidium ions disordered 0.276(2) Å above and below the crown ether plane (Rb-O 2.819(5)-2.884(5) Å, av. 2.846(5) Å). The positioning of the rubidium atom away from the center of the 18-crown-6 is effected by the packing of the Rb(18-crown-6)+ and AuCl4- moieties, and by the resemblance in the charge and symmetry of the cationic and anionic parts of the structure. Complex 2 has a zig-zag polymeric array -A-B-A-B-(Rb-N 2.92(2), 2.94(1) Å) with orthogonal disposition of Rb(18-crown-6)+ and Au(CN)4- planes. The rubidium atom is situated 0.90(2) Å above the mean plane of the macrocyclic oxygen atoms (Rb-O 2.93(5)-3.15(4) Å) and adopts a typical “sunrise coordination”.

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

scholarly journals Crystal structure of pimecrolimus Form B, C43H68ClNO11

2021 ◽  
Vol 36 (1) ◽  
pp. 35-42
Author(s):  
Shivang Bhaskar ◽  
Joseph T. Golab ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Density Functional ◽  
Van Der Waals Interactions ◽  
Powder Diffraction File ◽  
X Ray ◽  
Weak Intermolecular Interactions ◽  
Significant Difference ◽  
Atomic Coordinates ◽  
Solid State Conformation

The crystal structure of pimecrolimus Form B has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Pimecrolimus crystallizes in the space group P21 (#4) with a = 15.28864(7), b = 13.31111(4), c = 10.95529(5) Å, β = 96.1542(3)°, V = 2216.649(9) Å3, and Z = 2. Although there are an intramolecular six-ring hydrogen bond and some larger chain and ring patterns, the crystal structure is dominated by van der Waals interactions. There is a significant difference between the conformation of the Rietveld-refined and the DFT-optimized structures in one portion of the macrocyclic ring. Although weak, intermolecular interactions are apparently important in determining the solid-state conformation. The powder pattern is included in the Powder Diffraction File™ (PDF®) as entry 00-066-1619. This study provides the atomic coordinates to be added to the PDF entry.

Synthesis, Characterisation and Structural Studies of [Zn(phen)3][Fe(CN)5(NO)]·2H2O·0.25MeOH and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)]·0.5H2O

2003 ◽  
Vol 58 (9) ◽  
pp. 916-921 ◽  
Author(s):  
Amitabha Datta ◽  
Samiran Mitra ◽  
Georgina Rosair
Keyword(s):  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Structural Studies ◽  
Crystal Lattices ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Solvent Molecules

Two new bimetallic complexes [Zn(phen)3][Fe(CN)5(NO)] · 2 H2O · 0.25 MeOH, (1) and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)] · 0.5 H2O, (2), have been isolated (where phen = 1,10-phenanthroline and bipy = bipyridyl) and characterised by X-ray crystallography [as the 2 H2O · 0.25 CH3OH solvate for (1) and hemihydrate for (2)] infrared spectroscopy and thermogravimetric analysis. Substitution of phenanthroline for bipyridyl resulted in a cyano-bridged bimetallic species rather than two discrete mononuclear metal complexes. The bond angles of Fe-N-O were shown to be practically linear for both 1 [179.2(7)°] and 2 [178.3(3)°], and the Zn atoms have distorted octahedral geometry. The solvent molecules in both crystal lattices take part in forming hydrogen-bonded networks.

Verfeinerung der Kristallstruktur von Tripalladium-di-tetrathiophospliat Pd3(PS4)2 Refinement of the Crystal Structure of Tripalladium-di-tetrathiophosphate Pda3(PS4)2

1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Type Structure ◽  
Tetrahedral Symmetry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Planar Environment

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.

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