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 analysis of 5‐amino‐7‐(pyrrolidin‐1‐yl)‐2,4,4‐trimethyl‐1,4‐dihydro‐1,6‐naphthyridine‐8‐carbonitrile

The title compound [CCDC 199359], C₁₆H₂₀N₅ crystallized in Monoclinic system with the space group C2/c. The unit cell parameters are: a = 16.554(6), b = 12.145(4), c = 16.221(5)Å and β = 102.67(1)°. The molecular structure is stabilized by an intramolecular C‐H…N type hydrogen bond and the molecular packing by the intermolecular C‐H…N and N‐H…N type hydrogen bonds. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of N‐(3,4‐dichlorophenyl)‐N′‐hydroxy‐2‐oxo‐2‐phenylacetamidine

The title compound (C₁₄H₁₀N₂O₂Cl₂) crystallizes in the monoclinic space group P2₁/a with a=10.042(1) Å, b=10.317(1) Å, c=13.877(2) Å, β=97.36(2)°, V=1425.8(3) ų, Z=4, D_x=1.44 g.cm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.0457). The title molecule consists of 3,4‐dichlorophenylamino and 2‐phenyl‐1,2‐ethanedione‐1‐oxime groups. The intermolecular O‐H…N and N‐H…O hydrogen bonds [O…N 2.760(6) and 3.087(5) Å] are highly effective in forming the polymeric chains. The oxime group has an E configuration. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Presence of pseudo‐peptide bond in the crystal structure of n‐(t‐butoxycarbonyl)‐ε‐n′‐benzyloxycarbony‐l‐lysyl‐l‐isoleucine (boc‐lys(obzl)‐ile)

The dipeptide Boc‐Lys(OBzl)‐Ile crystallizes in monoclinic space group P2₁ with cell parameters a = 5.003(1), b = 19.199(3), c = 15.270(2)Å, β =93.42(1)°, V = 1464.1(3)ų, Z = 2, D_cal = 1.117 Mg/m³ at T = 293 K. The structure was solved by direct methods and refined by full‐matrix least‐squares procedure to a final R = 0.096 and wR = 0.101 using 1379 reflections. The peptide unit is in trans conformation and the molecule takes up an extended conformation. In the lysine side chain, delocalization of electrons and pseudo peptide bond formation is observed at the interaction site of benzyloxycarbonyl group. Both N‐H…O and main chain C‐H…O hydrogen bonds stabilize the molecules in the unit cell in a parallel β‐sheet fashion. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,spectroscopic studies and ab‐initio structure determination from X‐ray powder diffraction of bis‐(N‐3‐acetophenylsalicylaldiminato)copper(II)

The synthesis, spectroscopic studies and crystal structure determination from X‐ray powder diffraction have been carried out for bis‐(N‐3‐acetophenylsalicylaldiminato)copper(II). The structure is triclinic, space group P1 with unit cell dimensions a = 11.817(1) Å, b = 12.087(1) Å, c = 9.210(1) Å, α = 102.62(1)°, β = 111.16(1)°, γ = 86.15(1)°, V = 1197.0(2)ų, Z = 2. The structure has been solved by Monte Carlo simulated annealing approach and refined by GSAS package. The final Rp value was 8.68%. The coordination geometry around the copper atom in the complex is intermediate between square‐planar and tetrahedral with two salicylaldimine ligands in trans arrangement. Intermolecular C–H…O hydrogen bonds between molecules related by translation generate infinite chains along [010] direction. The molecular chains are linked via additional C–H…O hydrogen bonds to form a three‐dimensional supramolecular network. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystallographic characterization of a six coordinate Cu(II) complex based on hexamethylenetetramine ligand

The title compound, Cu(H₂O)₆]Cl₂.2{(CH₂)₆N₄}.4H₂O ( 1 ), has been prepared under mild hydrothermal conditions. Each Cu^II atom, located on a centre of symmetry, is coordinated by six water molecules in distorted octahedral coordination geometry. The hexamethylenetetramine molecule does not coordinate to the Cu atom but links with the Cu complex via three O—H…N hydrogen bonds. The remaining N atom of the hexamethylenetetramine is hydrogen‐bonded to the solvent water molecule. In the crystal structure, intermolecular O—H…O, O—H…N and O—H…Cl hydrogen bonds link the components into a three‐dimensional network. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,thermal analysis and IR spectroscopy investigations of N,N‐dimethyl‐1,3‐propanediammonium monohydrogenmonophosphate trihydrate

A new organic monohydrogenmonophosphate (C₅H₁₆N₂)HPO₄.3H₂O (abbreviate as MPAP) is prepared by reacting H3PO4 with N, N‐dimethyl‐1,3‐propanediamine. This compound crystallizes in the orthorhombic crystal system, space group Pca2₁. Unit cell parameters are a % 8.1445(1) Å, b % 11.7734(2) Å, c % 12.9021(2) Å, with, Z % 4 and ρ_m % 1.31 g cm⁻³. The structure was solved, using the direct methods and refined against F² to a reliability R factor of 0.0257. Three types of hydrogen bonds participate to the structural cohesion: O(P)—H…O, O(W)—H…O and N—H…O. The first one connects HPO₄ groups in infinite chains. This organization of the phosphoric groups creates voids in which are located the water molecules which are themselves connected by the second type of hydrogen bonds to the adjacent phosphoric groups that lead to a typical layer organization of a polyanion [HPO₄.(H₂O)₃ ]²ⁿ⁻_n. The third hydrogen bond type is responsible for the cohesion between the two‐dimensional polyanions. Thus, a framework in a threedimensional way is then created. The thermal decomposition of MPAP shows a large endothermic effect corresponding to the elimination of the water molecules and a set of endotherms which are probably due to the evolution of ammonia from the structure and the decomposition. The title compound was also characterized by IR spectroscopy, the interpretation of the spectra is based on theoretical analyses and literature data. (© 2003 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)     

Crystallization and structural studies of n‐benzyloxycarbonyl‐L‐tyrosine‐L‐glycine‐ethyl ester (Z‐Tyr‐Gly‐OEt)

It is axiomatic that efficient crystal production reflects upon the quality of structure. An empirical relation for mass proportions of two solvents in crystallization of Z‐Tyr‐Gly‐OEt shows a linear relationship. The dipeptide crystallizes in orthorhombic space group P2₁2₁2_1, with cell parameters a = 5.0680(1) Å, b = 13.8650(1) Å and c = 28.2630(1) Å, Z = 4, D_calc= 1.339Mg/m³, μ=0.820mm^‐1, F₀₀₀=848, CuKα = 1.5418 Å. The structure was solved by direct methods and final R1 and wR2 are 0.444 and 0.1276, respectively. The structure analysis reveals the trans conformation of the peptide unit with ω = ‐178.2(5)°, implying only a slight deviation from planarity. The torsion angles at glycine [ϕ, ψ = ‐84.4(7)°, 179.9(5)°] are characteristic of left‐handed poly glycine II helices. A number of N‐H…O, O‐H…O and C‐H…O hydrogen bondings play a role in stabilizing the molecules within unit cell. (© 2004 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,spectroscopic characterization and crystal structure of 5-bromo-1-(2-cyano-pyridin-4-yl)-1H-indazole-3-carboxylic acid diethylamide

The title compound 5-bromo-1-(2-cyano-pyridin-4-yl)-1H-indazole-3-carboxylic acid diethylamide, C₁₈H₁₆BrN₅O, is prepared from 5-bromoindazole-3-carboxylic acid methylester. N ¹-arylation is carried out with 4-chloro-2-cyanopyridine and the resulting product is converted to diethylamide by reacting with thionyl chloride and diethylamine. The structure is identified from its FT-IR, ¹H NMR, ¹³C NMR spectroscopy, elemental analysis data and unambiguously confirmed by single crystal X-ray diffraction studies. There are two symmetry independent molecules in the asymmetric unit with no significant differences in bond lengths and angles. The title compound crystallizes in the triclinic system, space group \(P\bar 1\) , with a = 11.2330(2); b = 11.6130(2); c = 15.4710(3) Å, α = 92.515(1)°; β = 109.956(1)°; γ = 107.199(1)°; V = 1788.45(6)ų and z = 4. An intramolecular C-H…N hydrogen bond forms an S(6) ring motif in one of the unique molecules. In the crystal, two molecules are linked about a center of inversion by C-H…O hydrogen bonded dimers generating an R ₂ ² (16) ring motif. The crystal packing is stabilized by C-H…N, C-H…O hydrogen bonds and π…π stacking interactions.     

Synthesis and X‐ray structure of two conformational isomers of [Zn(medpt)(SCN)2], medpt = bis (3 – aminopropyl)methylamine

Two conformational isomers of [Zn (medpt)(NCS)₂], medpt=bis(3‐aminopropyl) methylamine, (1) and (2) have been synthesised and the crystal structures are determined using single crystal X‐ray diffraction. The structures of the complexes have been solved by Patterson method and refined by full‐matrix least‐ squares techniques to R1 = 0.0524 for (1) and R1 = 0.0506 for (2), respectively. The geometry around the Zn(II) centre in both isomers is distorted trigonal bipyramidal. The two pendent thiocyanate moieties in (1), with Zn–N–C angles 167.9(4)–173.9(4)º, coordinate the mental centre almost linearly while the corresponding coordinations in (2) are significantly bent [Zn–N–C angles 150.8(3)–153.1(2)°]. Intermolecular N–H…S hydrogen bonds stabilise the crystal packing in the complexes forming infinite chains parallel to the [100] direction. The combinations of molecular chains generate three/two dimensional supramolecular framework in complexes (1) and (2). (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,Crystal and Molecular Structure of 2‐Pyridylethanolbis(saccharinato)mercury(II)

2‐Pyridylethanolbis(saccharinato)mercury(II), [Hg(sac)2(pyet)], where sac and pyet are the saccharinate anion and the 2‐pyridylethanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 10.4518(6), b = 11.3796(6) (5), c = 19.9945(12) Å, a = 102.758(3)° b = 98.146(3)°, g = 104.751(3)°, Z = 4, V = 2193.0(2) ų. The unit cell contains two crystallographically independent [Hg(sac)2(pyet)] units in which the mercury(II) ion is tetrahedrally coordinated by two nitrogen atoms of two sac ligands, and one nitrogen and one oxygen atoms of one neutral pyet ligands. The pyet acts as a bidentate N‐ and O‐donor ligand forming a six‐membered chelate ring, while sac behaves as a monodentate N‐donor ligand. The average bite angle of the pyet ligand is 75.8(5)°. The Hg‐N_sac bond distances are in the range 2.0874(18) and 2.1931(18) Å, whereas the Hg‐N_pyet and Hg‐O_pyet bond distances are 2.2452(19)‐2.3202(19) and 2.6036(17)‐2.5902(16) Å, respectively. The crystal exhibits two strong hydrogen bonds between the hydroxyl O atom of pyet and sulfonyl O atoms of sac and the C‐H…O type weak hydrogen bonds between H atoms of the aromatic rings of the pyet and the sulfonyl O atoms of the sac ligands. Furthermore, packing of the molecules in the solid‐state results in aromatic π‐π interactions associated with the aromatic rings of sac‐sac and py‐py.     

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)     

The Molecular and Crystal Structure of p-methyl-phenyl-glyoxyacid-p-chloranilide

Using X-ray crystal structure analysis of the title compound the positions of all the atoms (including all H atoms) in the monoclinic unit cell with the parameters a = 13.90₀ Å, b = 5.13₈ Å, c = 17.95₆ Å and β = 91.05° and the space group P 2₁/n were localized. The existence of an intramolecular N—H(N)…︁ O(1)-bridge was inferred, whose H-bridge acceptor predominantly is the π-electron density of the carbonyl group. At the same time the H(N) atom participates in the intermolecular bridge N H(N)…︁ O′(1) to the symmetry-equivalent neighbouring molecule. H-bridge-like interactions of the two phenyl hydrogen atoms H(6) and H(15) to the carbonyl oxygen O(2) have also been inferred from the torsion angles.     

Solid-phase synthesis and crystal structure of 5(3-nitrophenyl)-3,7-diphenyl-4H,6H-1,2-diazepine

The title compound, 5-(3-nitrophenyl)-3,7-diphenyl-4H,6H-1,2-diazepine (C₂₃H₁₉N₃O₂), was synthesized, in 76% yield, by one-pot multicomponent solid-phase reaction of 3-nitrobenzylidene phenyl ketone, acetophenone and hydrazine, using the catalyst bismuth nitrate, co-catalyst ZnCl₂, adsorbed on neutral alumina, at 110°C. The compound was characterized by spectral methods and X-ray diffraction studies. The crystals are monoclinic, space group P2₁/c: a = 12.186(2), b = 14.769(3), c = 11.046(2) Å, β = 115.023(3)°, Z = 4; R = 0.0418 for 2576 observed reflections. The diazepine ring assumes a twist chair conformation. The dihedral angles between the mean planes through the diazepine ring and the nitrophenyl rings and two phenyl are: 89.19(5)°, 45.85(5)° and 20.80(6)°, respectively. The crystal structure is stabilized by C-H…N, C-H…O, C-H…π hydrogen bonds and π-π-stacking interactions.     

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)     

Structure and conformation of n‐ (t‐butoxycarbonyl)‐l‐valine‐l‐phenylalanine‐methyl ester (Boc‐Val‐Phe‐OMe)

The crystal structure of N‐ (t‐butoxycarbonyl) ‐ L‐valine‐L‐phenylalanine‐methyl ester (Boc‐Val‐Phe‐OMe), C₂₀H₃₀N₂O₅ was determined by X‐ray diffraction methods. The dipeptide crystallizes in orthorhombic space group P2₁2₁2₁, with cell parameters a = 5.0680(1) Å, b = 13.8650(1) Å and c = 28.2630(1) Å, V = 2143.8(5) ų, F.W. = 378.46, Z = 4, D_calc = 1.173 Mg/m³, μ = 0.687 mm^‐1, F₀₀₀ = 816, CuKα = 1.5418 Å. The structure was solved by direct methods and final R1 and wR2 are 0.0659 and 0.1654, respectively. The peptide unit is in trans conformation [ω = 177.4(9)°]. The conformation angles ϕ₁, ψ₁, ϕ₂ and ψ₂ for the peptide backbone are: ‐96.5(13)°, 101.2(13)°, ‐123.9(12)° and 34.0(15)°. The N‐H…O and C‐H…O hydrogen bondings influence the packing of the molecules in the dipeptide crystal. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,Characterization and Crystal Structure of Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate

Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate was synthesized from ethyl 6-(4-bromophenyl)-4-(4-fluorophenyl)-2-oxocyclohex-3-ene-1-carboxylate and ammonium acetate in glacial acetic acid. The synthesized compound was characterized by elemental analysis, FT-IR, thermogravimetric analysis (TGA), differential thermal analysis (DTA), UV-Visible, and single-crystal X-ray diffraction. The title compound, ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate, C₂₁H₂OFNO₂, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 17.417(2), b = 9.7287(9), c = 21.014(2) Å, and Z = 8. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0644 for 1616 observed reflections. An intramolecular N–H…O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N–H…O hydrogen bonds, forming a two-dimensional network.