Crystal Structure of 2‐methyl cinnamanilide and 2‐methoxy cinnamanilide

The crystal structures of two cinnamanilide derivatives 2‐methyl cinnamanilide (C₁₆ H₁₅ N O – compound I) and 2‐methoxy cinnamanilide (C₁₆ H₁₅ N O₂ – compound II) are reported. In both crystal structures, the cinnamamide group is almost planar. The inter‐planar angle between the two phenyl rings are 71.6(1)° for compound I and 7.5(1)° for compound II. The N‐H…O and C‐H…O type of hydrogen bond interactions between the amide group and the carbonyl group stabilizes the molecular packing as chains in the crystal lattice.     

Crystal structure of 4'‐O‐methylalpinumisoflavone at 90K

4′‐O‐Methylalpinumisoflavone crystals which hitherto had been difficult to crystallize for X‐ray diffraction analyses have been obtained from a demethylated product of O, O‐dimethylalpinumisoflavone. The structural and conformational features of the crystal measured at 90 K are reported and compared with previously reported work of O,O‐dimethylalpinumisoflavone and 5‐O‐methyl‐4′‐O‐(3‐methyl‐but‐2‐en‐1‐yl) alpinumisoflavone. Each of these compounds is characterized by a six membered ring that is further fused to a benzopyrone isoflavone moiety resulting in a tricyclic ring system. This six membered ring shows a half‐chair conformation in all the molecules studied, with the ring in the title compound showing the least Cremer‐Pople puckering amplitude Q and shorter inter and intramolecular contacts. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structures of 2‐ chloro cinnamoyl phenolate (I) and 3‐chloro cinnamanilide (II)

The title compounds (I) and (II) crystallize in the monoclinic space group P2₁/c and orthorhombic space group Pbca respectively. The inter‐planar angle between the two phenyl rings are 55° in I and 24.5(1)° in II. The molecular packing of the compounds I and II are stabilized by C‐H…O and C‐H…π, and N‐H…O, C‐H…O and C‐H…π interactions, respectively. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 3‐hydroxy methyl 4,6‐dimethoxy‐9‐phenylsulfonyl‐carbazole

The crystal structure of 3‐Hydroxy methyl 4,6‐dimethoxy‐9‐phenylsulfonyl‐carbazole. (C₂₁H₁₉NO₅S) has been determined [CCDC 194425]. The compound crystallizes from methanol in the monoclinic system, space group I2/c, with unit cell parameters: a = 20.498(2), b = 9.258(2), c = 21.866(3)Å, β = 116.450(10)°, Z = 8, V = 3715.2(10)ų. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.050 with 3508 unique reflections. The planar carbazole ring fragment is inclined at an angle of 79.9(1)° to the phenylsulfonyl group. The sum of the angle about N is 351.6(2)°. The atoms linked to the central hexavalent S atom are arranged in a tetrahedral configuration with the larger deviations in the O‐SO angles [O1‐S‐O2 = 119.7(2)°] and the O1‐S‐N and O2‐S‐N angles [106.1(2) and 106.9(1)°, respectively].     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure investigation of pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide

Pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide (I), is a higher homologue of 1‐oxopyridinium‐2‐thioacetic acid (II) [1]. It crystallizes in monoclinic space group P2₁ with a = 9.2168(2) Å, b = 4.1423(2) Å, c = 11.3904(4) Å, β = 98.65(2)°, V = 429.93(3) ų and Z = 2. The least‐squares refinement gave residual index R = 0.024 for 1070 observed reflections. The introduction of an additional methylene group in (II) causes a flip in the carboxylic acid group of (I) that facilitates the molecules to align infinite antiparallel chains through strong C–H···O interactions. The molecules are interlinked by O–H···O hydrogen bonding across the chains and forming an infinite screw chain along y‐direction. The molecular packing is stabilized by O–H···O and C–H···O hydrogen bonding and π‐π electron interactions. This is an important facet of the crystal packing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural studies of crystalline oligosaccharides VI: Crystal structure and conformation of benzyl‐4,6‐O‐benzylidene‐3‐O‐benzoyl‐β‐D‐galactoside

Monsaccharides are the building blocks of polysaccharides and hence are the simplest sugar molecules to study the conformation and molecular structures of sugars. Benzyl‐4,6‐O‐benzylidene‐3‐O‐benzoyl‐β‐D‐galactoside is a key intermediate in the synthesis of polysaccharides. Crystal structural investigation of the title compound was undertaken to establish their chemical structure as well as to study their solid state conformation. Crystals of the title compound, obtained from water/methanol, are orthorhombic, space group P2₁2₁2₁, with cell dimensions a=11.290 (4), b=9.941 (1), c= 21.442(2)Å, V= 2406ų, Z=4, D_obs= 1.42 gm/cm³, D_calc=1.423 g/cm³, 2886 reflections were collected on a CAD‐4 diffractometer. The structure was solved by direct methods and refined to a final reliability index of 4.7%. The galactoside sugar has the chair conformation with C2' and C5' deviating from the mean plane of the other atoms of the sugar. The 4,6‐O‐benzylidene ring also has a chair conformation with the benzoyl group proximal to O6'. The crystal structure is stabilized by O‐H…O hydrogen bonds involving O2' as donor and three C‐H…O hydrogen bond interactions. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 3‐phenyl‐4‐(p‐chlorobenzylamino)‐4,5‐dihydro‐1‐H‐1,2,4‐triazol‐5‐on

The structure of the title compound, C₁₅H₁₃N₄OCl was determined by single crystal X‐ray diffraction technique. The structure consists of a p‐chlorobenzylamino moiety and triazol and phenyl rings. The title compound crystallizes in the monoclinic space group P2₁/c with a = 14.368(3), b = 6.255(3), c = 17.631(3) Å, β = 113.24(3)°, Z = 4, V = 1455.8(8) ų and D_x = 1.372 gcm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.0477). The dihedral angle between the triazole moiety and the phenyl ring is 28.8(3)°. The molecular packing is stabilized by N‐H…N and N‐H…O types of inter molecular hydrogen bonds. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 11,12‐dibromo‐ 7,8—benzo‐1,5‐di(p—tolylsulphonyl)‐1,5‐diazacyclononan

The crystal structure of the title compound, C₂₅H₂₆Br₂N₂O₄S₂ was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/c, with a=20.7142(2) Å b=11.7910(2) Å, c= 10.6735(3) Å, β=98.549(2)°, V=2577.94(9) ų, Z=4. The structure was solved by direct methods and refined by least‐squares methods to a final R=0.046 for 1866 observed reflections with I>2sigma(I). The title compound, displays disordered geometry around the C1 atom located almost on twofold axis. The nine‐membered heterocylic ring is close to the half‐chair conformation. The dihedral angle between phenyl rings is 34.2(1)°.     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Crystal Structure of Spiro[2‐benzoyl‐cyclohexyl‐4,5‐diphenylpyrrolidine‐3,3'‐chroman‐4‐one]

3‐Phenyl‐chroman‐4‐one is the basic unit of isoflavonoids which are found in the plants of the sub‐family papilionoidae of Leguminosae. They are known to possess antifungal and antibacterial properties. Crystal data of the title compound : Monoclinic, space group P2₁/c, a = 14.021(3), b = 18.682(4), c = 11.362(2) Å, β = 95.75(3)°, R = 0.066. The two phenyl rings directly attached to the pyrrolidine ring are nearly perpendicular to it. The dihydropyrone moiety adopts a half‐chair conformation while the cyclohexane ring attached to the pyrrolidine ring adopts a chair conformation. The best plane passing through the chroman‐4‐one moiety makes a dihedral angle of 82.2(3)° with the pyrrolidine ring. The molecule is stabilized by one intra‐ and two intermolecular C‐H...O hydrogen bonds.     

Structure Analysis of Methyl‐3,4‐dihydro‐3‐(p‐methylphenyl)‐4‐oxo‐2‐quinazolinyl thiopropionate

The crystal structure of methyl‐3, 4‐dihydro‐3‐(p‐methylphenyl)‐4‐oxo‐2‐quinazolinyl thiopropionate (C₁₉H₁₈N₂O₃S) has been determined by X‐ray diffraction methods. The compound crystallizes in the triclinic space group P with unit cell parameters: a = 9.094(2), b = 9.428(3), c = 10.612(3) Å, α = 94.55(3), β = 95.44(2), γ = 106.75(3)° and Z = 2. The structure has been refined to an R‐value of 0.054 for 2533 observed reflections [F_o > 4σ(F_o)]. The quinazoline moiety and the methyl substituted phenyl ring is almost planar. The dihedral angle between these two moieties is 84.96(8)° . The crystal structure is stabilized by an intermolecular C‐H … O interaction.     

Synthesis and structural conformation of N‐substituted 1,4‐dihyropyridine derivatives

N‐(Phenyl)‐3,5‐dicarbethoxy‐2,6‐dimethyl‐4‐(phenyl)‐1,4‐dihydropyridine (A) and N‐(4‐methoxy phenyl)‐‐3,5 dicarbethoxy‐2,6 dimethyl‐4‐(3‐nitro phenyl)‐1,4‐dihydropyridine (B) has been synthesized as per scheme and characterized by the X‐ray diffraction method. The compound A crystallizes in monoclinic space group P21/c with cell parameters a = 9.2770(11)Å, b = 8.6410(5)Å, c = 27.601(3)Å, β = 97.724(3)°, Z = 4. The compound B crystallizes in monoclinic space group P21/c with cell parameters a = 11.229(6), b = 12.746(7)Å, c =17.606(6)Å, β = 104.531(3)°, Z = 4. The structures exhibit both intra and intermolecular hydrogen bonds. Dihydropyridine ring of both the compounds adopt a flat boat conformation. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure and conformation of a nickel complex: {2‐Hydroxo‐3‐piperidine‐1‐yl‐methyl‐N,N′(bis‐5‐bromobenzylpropylenediimine)nickel(II)perchlorate}

The title compound, a nickel complex [C₂₃H₂₆N₃O₂Br₂Ni.(ClO₄)] (CCDC 199520) crystallizes in triclinic space group P with the cell parameters a = 10.2560(4), b = 10.8231(4), c = 12.0888(5)Å, α = 99.404(1), β = 99.780(1), γ = 92.252(1)° and V = 1301.49(9)ų. The structure was solved by Patterson method and refined by full‐matrix least‐squares procedures to a final R = 0.0497 using 6287 observed reflections. In the complex, the piperidine ring takes chair conformation and the geometry around the Ni ion is slightly distorted square planar. The dihedral angle between the planes [N‐Ni‐N and O‐Ni‐O] is 9.4(1)°. The chelate ring containing both the nitrogen atoms adopts twisted boat conformation. The molecules in the crystal are stabilized by N‐H…O and C‐H…O types of hydrogen bonds in addition to a C‐H…π interaction. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal and molecular structure of trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II)

Trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II), [Ni(sac)₂(pypr)₂], where sac and pypr are the saccharinate anion and the 2‐pyridinepropanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 8.1981(8), b = 9.9680(10), c = 10.4956(10) Å, α = 90.740(3)° β = 108.142(3)°, γ = 111.025(3)°, Z = 1, V = 1.537 ų. The structure of the nickel(II) complex consists of neutral molecules in which the nickel(II) ion sits on a center of symmetry and is octahedrally coordinated by two sac ligands, and two neutral pypr ligands. The pypr acts as a bidentate N‐ and O‐donor ligand forming a seven‐membered chelate ring, while sac behaves as a monodentate O‐donor ligand via the carbonyl O atom. The Ni‐N bond distance is 2.1016(15) Å, whereas the Ni‐O_pypr and Ni‐O_sac bond distances are 2.1280(12) and 2.0792(11) Å, respectively. The individual molecules are held together with a strong hydrogen bond between the hydroxyl O atom of pypr and N atom of sac and the C‐H…O type weak hydrogen bonds between some ring hydrogen atoms of pypr and sac, and the carbonyl and sulfonyl O atoms of sac in the neighbouring molecules. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 2,6‐bis(4‐chlorophenyl)‐3‐phenylpiperidin‐4‐one

The crystal structure of the title compound is described. The chemical formula of the compound is C₂₃H₁₉Cl₂NO. The compound is found to crystallize in monoclinic system with space group P2₁/c, Z = 4. The unit cell dimensions are a = 15.137(3) Å, b = 8.9171(18) Å, c = 14.779(3) Å, β = 91.461(4)° and V = 1994.2(7) ų, D_calc = 1.320 gcm^‐3. The final R factor is 4.4%. The central piperidone ring of the molecule adopts a slightly distorted chair conformation, the mean torsion angle being 52.3°; the phenyl rings are planar. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole

The crystal structure of 4‐(1‐methyl‐1‐mesitylcyclobutane‐3‐yl)‐2‐aminothiazole (C₁₇H₂₂N₂S₁) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the triclinic space group P‐1 with Z = 6. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.052 for 2298 observed reflections [I > 2σ ( I ) ]. There are three crystallographically independent molecules, I, II and III. These molecules are held together by intermolecular N‐H...N hydrogen bonds. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Crystal and Molecular Structure of bis[diaaqua(1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine ‐2,5‐dione))N ickel(II)]dihydrate

The title compound [Ni(CPDD)(H₂O)₂]₂(H ₂O )₂, {]Ni₂(C₄₄H₂₈N₈O₁₂)] (H₂O)₂ }, where CPDD = 1H‐cyclopenta(2,1‐b:3,4‐b')(dipyridine‐2,5‐dione) has been prepared and its crystal structure determined by single crystal X‐ray diffraction at room temperature. The complex crystallizes in the triclinic space group P1 w ith two molecules in the asymmetric unit. The cell dimensions are a=10.452(1),b=14.098(1) & c=16.023 Å; D=110.13(1), E=100.63(1) & J=100.85(1)°. The two independent molecules in the asymmertic unit are related by pseudo two fold symmetry. In both the molecules the coordination environment around the Ni(II) may be best described as a distorted octahedral. Due to some delocalization of charge towards one of the oxygens(O1a) from the O2a atom some degree of bond localization has been observed. The individual diones of both the molecules are almost right angles at the metal atom. A long the y‐axis inversion related molecules are forming pseudo‐dimers through hydrogen bonding.     

Crystallographic Investigations of 3β‐acetoxy‐5α‐cholestan‐6‐one‐semicarbazone ‐ A Steroid

The crystal structure of 3b‐acetoxy‐5a‐cholestan‐6‐one‐semicarbazone (C₃₀H₅₁O₃N₃) has been determined by X‐ray diffraction methods. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters a = 11.641(1), b = 16.552(1) c = 31.181(4) Å and Z = 8. The structure has been refined to an R‐value of 0.050 for 4407 observed reflections. Two molecules in the asymmetric unit have been observed. In both the crystallographically independent molecules, all the three six‐membered rings (A, B and C ) of steroid nucleus exist in chair conformation, while the five‐ membered ring D exists in 13β distorted‐envelope in molecule‐I and 13β, 14α half‐chair conformation in molecule‐II. Three intermolecular N‐H … O hydrogen bonds have been observed.     

Different complexation behavior of a proton transfer compound obtained from 1,10‐phenanthroline and pyridine‐2,6‐dicarboxylic acid with Sn(IV), Sb(III) and Tl(I)

The different complexation methods of a proton transfer compound, (phenH)₂(pydc) (phen=1,10‐phenanthroline; pydcH₂= pyridine‐2,6‐dicarboxylic acid), are discussed and formation of [Sn(pydc)(phen)(OH)₂]·3H₂O ( 1 ), {[Sb(pydc)(phen)]₂O}·2DMSO·4H₂O( 2 ) and [(Tl(pydcH)]_n ( 3 ) complexes are reported. The characterization was performed using IR spectroscopy and X‐ray diffraction. The structures of Sn(IV) and Sb(III) complexes show that both cationic and anionic fragments of the starting proton transfer compound have been involved in the complexation. Whereas the structure of Tl(I) complex demonstrates that only the anionic fragment of (phenH)₂(pydc) is contributed to the complexation. The complexes 1‐3 show a variety of structural features including mononuclear, binuclear and polymeric structures. In compounds ( 1 ), ( 2 ) and ( 3 ) a large number of hydrogen bonds are observed. These interactions play an important role in the formation and stabilization of supramolecular systems in the crystal lattices. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)