The crystal and molecular structures of isoperezone, aminoperezone, and isoaminoperezone: a comparative study of their crystal packing

The crystal structures of isoperezone (1), aminoperezone (2), and isoaminoperezone (3) have been determined by single-crystal X-ray diffraction. Compound (1) yields orange crystals, orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 6.271(6), b = 30.373(7), c = 7.257(1) Å, and Z = 4; compound (2) yields purple crystals, orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 6.498(3), b = 7.500(1) c = 29.200(6) Å, and Z = 4; compound (3) yields purple crystals, monoclinic space group P2₁ with unit cell dimensions a = 7.354(1), b = 7.511(1), c = 13.283(1) Å, = 102,07(1)°, and Z = 2. The side chains in (1)–(3) are oriented out of the plane of the quinone ring at an angle of 124, 144, and 97°, respectively. The molecules in the crystal are held together by hydrogen-bonding networks and van der Waals interactions.     

Crystal and molecular structure of 3β-hydroxy-5β-estr-8(14)-en-17-one

The title compound crystallizes in the orthorhombic space group P2₁2₁2₁ with 4 formula units C₁₈H₂₆O₂ in the unit cell. The lattice constants are a = 10.356(2) Å, b = 19.743(3) Å, and c = 7.487(1) Å. The structure was solved by direct methods of phases determination and refined by least-squares calculations to the conventional R = 0.054. The configuration and conformation of the molecule were determined and compared with those of Δ-8,14-anhydrodigitoxigenin.     

Tautomeric properties and crystal structure of N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline

The title compound has been synthesised by the reaction of 2-hydroxy-1-naphthaldehyde with 2,5-dichloroaniline. The compound was characterized by elemental analysis, IR and UV-Visible techniques. The UV-Visible spectra of the Schiff base with OH group in ortho position to the imino group was studied in polar and nonpolar solvents in acidic and basic media. The structure of compound has been examined cyrstallographically. It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 6.059(1), b = 12.105(2) c = 20.006(2) Å, V = 1467.4(3) ų, D_x = 1.431 g.cm^-3 and Z = 4. The crystal structure was solved by direct methods and refined by full-matrix least squares. Molecule of the title compound N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline is nearly planar. The molecule contains a strong intramolecular N…H-O hydrogen bond between the imine and hydroxyl group [O1 and N1 = 2.540(4) Å]. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

A novel oxazine from the condensation of chloroanthraquinone and t-butyl L-prolinate

A new, fused-ring oxazine was synthesized in a one-pot condensation of L-proline t-butyl ester and 1-chloroanthraquinone. The compound crystallized in space group P2₁2₁2₁ with cell parameters a = 10.1820(10) Å, b = 15.213(2) Å, c = 18.649(2) Å, and Z = 4. The absolute structure of the compound was obtained by the Flack parameter.     

Crystal structure of 3,3-diphenylnaphtho [1, 2-c] furan-1 (3H)-one

The crystal structure of 3, 3-diphenylnaphtho[1, 2-c]furan-1(3H)-one 2 was determined by X-ray diffraction analysis. It possesses P2₁2₁2₁ (#19) space group symmetry, with a = 11.922(2), b = 17.142(4), c = 8.429(2) Å, and D _calc = 1.297 mg/m³ for Z = 4.     

Structural Properties of S-alkylated Dithiolene Chelates (I). Crystal and Molecular Structures of Bis(S-ethyl-ethene-1,2- dithiolato)palladium (II) and Bis(S-ethyl-ethene-1,2-dithiolato) platinum (II)

Bis(S-ethyl-ethene-1,2-dithiolato)palladium(II), Pd(S₂C₄H₇)₂, is monoclinic, P 2₁/n, with a = 7.598(1) Å, b = 10.445(2) Å, c = 8.031(1) Å, β = 95.3(1)° and Z = 2. The structure was determined by 893 independent reflections and refined by the block-diagonal leastsquares method to R = 0.12. The chelate molecule is nearly planar and the palladiumsulfur distances are 2.278(6) Å and 2.403(6) Å. Bis(S-ethyl-ethene-1,2-dithiolato)platinum(II), Pt(S₂C₄H₇)₂, is monoclinic, P 2₁/a, with a 13.114(2) Å, b = 12.873(2) Å, c = 7.446(2) Å, β = 96.1(1)° and Z = 4. The structure was solved from 2040 independent reflections. The compound is not isomorphic with the isomeric palladium complex. In the unit cell there exist two symmetry independent molecules. The platinum-sulfur distance is 2.280 (6) Å.     

The crystal and molecular structure of three homologue 1,4-dialkanoyloxy-biphenyls (SYM-n)

The three homologue compounds with the general formula C_nH_2n+1 COO C₆H₄ C₆H₄ OOC C_nH_2n+1 (SYM-n) crystallize in the following space groups: SYM-1: triclinic, P1 , a = 7.400(6), b = 9.227(3), c = 10.579(3) Å, α = 85.97(3), β = 89.09(3), γ = 71.47(3)°; SYM-2; monoclinic, P2₁/c, a = 11.712(7), b = 5.648(1), c = 12.408(6), Å, β = 103.84(3)°; SYM-5: triclinic, P1, a = 5.505(4), b = 8.342(8), c = 24.79(2) Å, α = 86.67(3), β = 85.45(6), γ = 71.74(7)°. The structures have been solved by direct methods and refined to R = 0.075, 0.061 and 0.053, respectively. The packing arrangements show a layer-like structure. The layers are almost separated for SYM-1 as well as for SYM-2 and interdigitated for the structure of SYM-5.     

Synthesis and crystal structure of 1-acetyl-3-bromo-3-phenylazetidine and 1-phenyl-2-(N-acetyl-N-formyl)-aminoethanone

1-Acetyl-3-bromo-3-phenylazetidine (1), C₁₁H₁₂BrNO, has been synthesized and characterized by spectroscopic methods and single crystal X-ray analysis. It crystallizes in the space group P2 ₁/c with a = 8.633(1), b = 7.461(1), c = 17.204(1) Å, = 98.403(7)°, V = 1096.2(2) ų, Z = 4, D _calc = 1.540 g cm^–3. The azetidine ring is nearly planar since the four atoms are within ±0.039(5) Å of the mean square plane calculated for the heterocycle. The attempt to obtain a highly strained 2-azetine derivative from the above compound gave, surprisingly, 1-phenyl-2-(N-acetyl-N-formyl)-aminoethanone (2), C₁₁H₁₁NO₃. This compound has been also characterized by spectroscopic methods and single crystal X-ray analysis. It crystallizes in the space group P2₁2₁2₁, with a = 5.4719(3), b = 8.3205(6), c = 23.298(3) Å, V = 1060.7(2) ų, Z = 4, D _calc = 1.286 g cm^–3. The aminoethanone residue is in a near planar conformation where the torsion angles are 7(2)° for N–C–C–=O and –173(2)° for N–C–C–C(Ph).     

The crystal and molecular structure of a dioxan photoadduct of 3-dehydro-gibberellin A1 methyl ester

The three-dimensional structure of a dioxan photoadduct of 3-dehydro-gibberellin A₁ methyl ester has been established as (2′S)-3-[dioxanyl-(2′)]-3-epi-gibberellin A₁ methyl ester (1) by X-ray analysis. The compound crystallizes in the orthorhombic space group P2₁2₁2₁ with four molecules in the unit cell of dimensions a = 9.751, b = 22.189, c = = 10.064 Å. The final R-value is 0.103 for 1151 reflections.     

Synthesis and Crystal Structure of Copper II and Silver I Complex with 1,4-diazabicyclo[2.2.2]octane[Cu(CBC)2(Dabco)(H2O)] n (1) and [Ag2(HBC)2(Dabco)] n (2)

Two 1D polymeric complex, [Cu(CBC)₂(Dabco)(H₂O)] _n (1) and [Ag₂(HBC)₂(Dabco)] _n (2) have been synthesized and characterized by X-ray single crystal analysis, where CBCH is p-chlorobenzoic acid, HBCH 2 is 2-hydroxybenzoic acid and Dabco is 1,4-diazabicyclo[2.2.2]octane. Complex 1 has been obtained in high yield by hydrothermal synthesis from CuO and CBCH and Dabco, and complex 2 has been obtain by evaporation of the solvent from silver salicylate and Dabco, 1 crystallizes in the orthorhombic space group Pmn2 ₁ with a = 24.3310(5) ?, b = 6.9050(6) ?, c = 5.9980(5) ?, Z = 2, V = 1007.70(4) ?³ and Dx = 1.657 g cm⁻³, 2 crystallizes in the monoclinic space group P2 ₁ /m with a = 10.292(3) ?, b = 6.913(2) ?, c = 14.417(4) ?, β = 95.660(5), Z = 2, V = 1020.8(5) ?³ and Dx = 1.959 g cm⁻³. The final R value is 0.0302 for 1323 measured reflections for 1 and the final R value is 0.0684 for 1545 measured reflections for 2. The atomic arrangement is built by infinite one-dimensional polymeric chain in both complexes. These chains are cross-linked by hydrogen bonds involving the coordinated water molecules to form a two-dimensional framework in complex 1.     

Crystal and molecular structure of 2-diazo-5-phenyl-cyclohexan-1,3-dione

M_r = 214.24, monoclinic space group P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ (MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.034. M_r = 214.24, monokline Raumgruppe P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ(MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹.     

Preparation and crystal structure of a quadruply bonded dimolybdenum complex with trans-crotonate ligands

A quadruply bonded dimolybdenum complex with trans-crotonate ligands, Mo₂(O₂CC₃H₅)₄, was synthesized and characterized by UV–VIS, IR, and NMR spectra. The crystal structure was determined by an X-ray single crystal diffraction analysis. The title complex (C₁₆H₂₀O₈Mo₂, M _w = 532.2) crystallized in the triclinic space group P-1 with the following crystallographic parameters: a = 10.236(2) ?, b = 10.393(2) ?, c = 10.524(2) ?, α = 89.59(1)°, β = 73.34(1)°, γ = 70.78(2)°, V = 1008.1(3) ?³, Z = 2, D _c = 1.753 Mg m⁻³, μ(Mo Kα = 0.71073 ?, F(000) = 528, and final R ₁ = 0.041, wR ₂ = 0.114 for observed reflections 2889 (I > 2σ(I)). The Mo₂ ⁴⁺ unit was surrounded by four trans-crotonate ligands resulting in a paddle wheel structure with one disordered trans-crotonate ligand. Molecules are bonded together by means of interactions consisting of the donation of lone pairs of electron on carboxylate O atoms on one molecule to the Mo atom on an adjacent complex. A new pattern of intermolecular bonding is observed.     

Crystal and molecular structure of 1-diazo-2,3,4,5-tetraphenylcyclopentadiene

M_r = 396.30, monoclinic space group P 2₁/c, a = 10.145(2), b = 18.523(4), c = 12.443(2) Å, β = 110.31(2)°, V = 2193(1) ų, Z = 4, D_x = 1.201 Mg m⁻³, F(000) = 832, λ(MoKα) = 0.71069 Å, μ = 0.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039.     

Crystal and molecular structure of 14-desoxy-14ß-azido-digitoxigenin-3-acetate

The crystal and molecular structure of 14-desoxy-14ß-azido-digitoxigenin-3-acetate was determined by X-ray analysis. The compound crystallizes in the orthorhombic space group P 2₁2₁2₁ with four molecules C₂₅H₃₅N₃O₄ in the unit cell. The lattice parameters are a = 8.975, b = 13.698, and c = 18.958 Å. The structure was solved by direct methods and refined by least-squares procedures up to the discrepancy factor R = 0.041.     

Crystal structures of substituted imidazolidine derivatives

The crystal structures of isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]methyl-5-phenyl-,N-oxide] (C₁₃H₁₃N₅O₃) (I), isoxazole,3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(4-methylphenyl)-,N-oxide] (C₁₄H₁₅N₅O₃) (II) and isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(2-methoxyphenyl)-,N-oxide] (C₁₄H₁₅N₅O₄) (III) have been determined by X-ray diffraction studies. The compound I, crystallized in triclinic space group with unit cell dimensions a = 7.2405(7) ?, b = 7.9936(8) ?, c = 11.6573(11) ?, α = 97.801(2)°, β = 90.884(2)°, γ = 96.250(2)° and Z = 2. Compound II crystallized in orthorhombic space group Pna2₁ with unit cell dimensions a = 10.1778(10) ?, b = 28.228(3) ?, c = 5.1206(5) ?, and Z = 4. Compound III crystallized in monoclinic space group P2₁/n with unit cell dimensions a = 7.8439(9) ?, b = 7.8544(9) ?, c = 23.534(3) ?, β = 99.464(2)° and Z = 4. For all three compounds, the five-membered imidazolidine ring adopts an envelope conformation. The crystal structures are stabilized by both the intramolecular N–H···O and intermolecular N–H···N hydrogen bonding.     

Crystal and Molecular Structures of Modified Progestagens (IV). 17α-Azidomethyl-17β-hydroxy-estra-4,9-dien-3-one,C19H25N3O2

The crystal and molecular structure of 17α-azidomethyl-17β-hydroxy-estra-4,9-dien-3-one has been determined by X-ray structure analysis. It crystallizes in the orthorhombie space group P 2₁2₁2₁ with cell parameters a = 9.118(1), b = 9.252(1), and c = 20.444(2) Å. The structure was solved by MULTAN-82 and refined to R = 0.042 for 1408 observed reflections. Steroid ring and 17β-side chain conformations are discussed in the paper. Intermolecular hydrogen bridges between hydroxyl groups and carbonyl oxygen atoms link molecules forming chains in c-direction.     

Crystal structure determination of 2-acetylamino-4-benzoyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazolin,C13H15N3O2S

Thiosemicarbazone is receiving increasing interest because of the biological activity of some of its derivatives. Mr = 277.35, space group P2₁2₁2₁, Z = 4, a = 9.290(3), b = = 11.512(2), c = 13.286(2) Å, V = 1421 (1) ų, D_m = 1.29(1) Mg m⁻³, D_x = 1.296 Mg m⁻³, λ(MoK_α) = 0.71062 Å, μ = 0.230 mm⁻¹, F(000) = 584, T = 296 K, final R = 0.028 for 1255 reflections. All hydrogen atoms were located. The structure determed by X-ray analysis confirms the chemical results. The structure analysis of the title compound is described and its molecular and crystal structure discussed.     

Molecular iodine catenation in the anionic chains [Pd2I6(I2)]2–

In the easily accessible salt [(H₅O₂)(db24c8)]₂[Pd₂I₆(I₂)], iodine molecules are catenated in linear anionic chains [^…I₂PdI₂PdI₂^…I–I^…]^2– which are separated by bulky cations consisting of two (H₅O₂)⁺ cations sequestered in dibenzo‐24‐crown‐8 (db24c8) molecules. The new compound is obtained as black single crystals (triclinic, P1, a = 1001.8(2), b = 1185.8(2), c = 1503.7(3) pm, α = 102.97(1), β = 107.65(1), γ = 90.85(1)°, V = 1652.3(5) 10⁶·pm³, Z = 1) from a moist 1:1 dichloromethane/ethanol solution of PdCl₂, iodine and db24c8. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal- and molecular structure of 19-nor-digitoxigenin

19-nor-Digitoxigenin crystallizes in the orthorhombic space group P 2₁2₁2₁ with four formula units C₂₂H₃₂O₄ per unit cell. The lattice parameters are a = 7.082, b = 12.476, c = 21.486 Å. The crystal structure was determined by direct methods and refined by a least-squares procedure to the discrepancy factor R = 0.042. — The orientation of the lactone ring relative to the steroid skeleton was found to be the opposite of that known for digitoxigenin.     

Crystal structures of four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium

Herein four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium, 2(CH₃)₄N⁺·C₁₄H₈O₄S₂^2?·H₂O (1), (C₂H₅)₄N⁺·C₁₄H₉O₄S₂^?·0.25H₂O(2), (n-C₃H₇)₄N⁺·C₁₄H₉O₄S₂^? (3) and (n-C₄H₉)₄N⁺·C₁₄H₉O₄S₂^?(4) are prepared and characterized by X-ray single crystal diffraction. As shown in the results, compounds 1 and 3 belong to orthorhombic crystal system with different space groups of P2₁2₁2₁ and Pca2₁, and 2 and 4 are monoclinic system with similar groups of P2₁/n and P2₁/c. The crystallography data are displayed below: 1: a = 10.5903(7) Å, b = 10.6651(7) Å, c = 21.9476(13) Å, V = 2478.9(3) ų, Z = 4, R₁ = 0.0359; 2: a = 8.13340(1) Å, b = 22.0741(3)Å, c = 13.2143(2)Å, β = 101.6360(1) °, V = 2323.70(6) ų, Z = 1, R₁ = 0.0385; 3: a = 15.7857(2) Å, b = 8.24830(1) Å, c = 20.2599(2) Å, V = 2637.94(5) ų, Z = 4, R₁ = 0.0308_degree4: a = 11.7476(2) Å, b = 17.1346(1) Å, c = 16.3583(3)Å, β = 109.4560(1) °, V = 3104.74(9)ų, Z = 4, R₁ = 0.0562. Interestingly, although the carbon chains of the guest templates vary from methyl group to butyl group, the host molecules of 2,2′-dithiosalicylic acid all construct the similar 2D hydrogen-bonded host layers with or without the existence of water molecules to contain the guest templates to yield analogous sandwich-like inclusion compounds. Obviously, although the guest templates will have certain effects on the ultimate formation of these crystal structures, the host molecule of 2,2′-dithiosalicylic acid is a controlling factor to form these four inclusion compounds.