X-ray structure of 14-phenyldiquino[3,4 b;4′,3′-e][1,4]thiazine<Superscript>(1)</Superscript>

The title compound 1 (C₂₄H₁₅N₃S) crystallizes in an orthorhombic unit cell, with a = 8.2355(3), b = 19.1499(8), and c = 11.3520(5) Å, Z = 2, and space group Pnma. The pentacyclic ring system is folded mainly along the S–N(2) axis and slightly along the C(3)–C(4) and C(3′)–C(4′) axes. The butterfly folding angle between the two quinoline planes is 48.96(3)^∘ and the angle between the planes of the two halves of the thiazine ring is 43.46(7)^∘. The central thiazine ring is in a boat conformation. The phenyl substituent is unexpectedly in an axial location with respect to the thiazine ring with the C–N⋅ < eqid1 > ⋅S angle of 114.0(1)^∘ and it is perpendicular to the bisecting plane of the pentacyclic ring system.     

Crystal structure of syn-1-acetyl-9′aH-8′- methoxyspiro[indole-3,2′-oxeto[3′,2′:4,5]furo[3,2-g][1] benzopyran]2,6′-dione

The crystal structure of syn-1-acetyl-9a-hydro-8-methoxyspiro[3H-indole-3,2(2aH) oxeto[3,2-g]furo[3,2-g]benzo[ b]pyran-2,6-dione 1 was determined by X-ray diffraction analysis. It possesses P2(1)/c space group symmetry, with a = 12.391(3), b = 15.035(3), c = 9.5435(19) Å, = 93.66(3), and D _calc. = 1.517 Mg/m³ for Z = 4.     

Synthesis and supramolecular interactions involved in the crystal structure of (2,4,10,12-tetrabromo-6,7,14,15-tetrahydro-6, 14-thiacycloocta[1,2-b:5,6-b’]diquinoline)2·(1,1,2,2-tetrachloroethane) inclusion compound

The tetrahalo aryl inclusion host 2,4,10,12-tetrabromo-6,7,14,15-tetrahydro-6,14-thiacycloocta[1,2-b:5,6-b’]diquinoline 3 was re-synthesized to explore its ability to trap toxic polychlorinated hydrocarbons such as 1,1,2,2-tetrachloroethane (TCE) in the form of host–guest compound. Host 3 crystallizes from a fresh sample of TCE to form an inclusion compound of the formula (3)₂·(TCE) in triclinic system, space group P-1, with a = 7.7732(16) Å, b = 10.739(2) Å, c = 14.816(3) Å, α = 97.329(4)°, β = 98.619(4)°, γ = 103.359(4)°, V = 1172.7(4) ų, and Z = 2. The X-ray crystal structure of the (3)₂·(1,1,2,2-TCE) is described and analyzed in terms of crystal engineering and supramolecular chemistry. The hosts assemble by means of different types of packing motifs. The included TCE molecules are enclosed within host molecular pens. Novel halogen···halogen intermolecular interactions as well as other non-covalent intermolecular interactions involved in the crystal structure are presented and proved to play an important role in linking these host–host, host–guest, and guest–guest building blocks.     

Crystal structure of tetrachlorobisd[μ-imidocarbonylchloridato]diboron

Boron trichloride and mercuric cyanide react slowly to form the title compound, B₂N₂C₂Cl₈, which contains a four-membered B₂N₂ ring with alternating BCl₂ and N—CCl₂. Crystals are triclinic, space group P , a = 6.1198(1), b = 7.4457(3), c = 7.9186(3) Å, = 117.064(2), = 106.923, = 93.712(2)°, Z = 1, and V = 299.07(2) ų. The compound has a crystallographic center of symmetry but the metric symmetry is close to the expected mmm.     

X-ray crystal structure of 2-hydroxy-2′-(1,4-bisoxo-6-hexanol)-1,1′-biphenyl

The X-ray crystal structure of 2-hydroxy-2-(1,4-bisoxo-6-hexanol)-1,1-biphenyl, 3, is presented. This molecule crystallizes in the monoclinic space group P2₁/n (a = 9.440(2), b = 12.679(3), c = 11.679(3) Å = 94.60(2)° V = 1382.5(5) ų; Z = 4). One of the unique features of the X-ray structure of 3 is the intramolecular hydrogen bonding. The hydrogens of the phenolic and hydroxy groups occupies bridging positions via hydrogen bonding to an ether oxygen (O₁) and a phenolic oxygen (O₄), respectively. This hydrogen bonding does not affect the interplanar angle between phenyl rings (49.34°), which is in the range expected for ortho-disubstituted biphenyl compounds. The hydrogen bonding of this type explains why it is difficult to alkylate both phenoxy groups of 2,2-biphenol with tetrahydropyranyl protected 2-(2-chloroethoxy)ethanol.     

Crystal and molecular structure of [H3O·18-crown-6]2-[ReCl6] isolated from a liquid clathrate medium

The crystal and molecular structure of [H₃O·18-crown-6]₂[ReCl₆]1 is reported. Crystal data for1: trigonal, space group R ,a=13.857(2) Å,c=10.154(2) Å,D _c =2.85 g/cm³,Z=3,R _f =0.073,R _w =0.064. The oxonium ion is observed to be crystallographically disordered lying 0.37 Å on both sides of the plane defined by the crown ether oxygen atoms. The anion resides on a crystallographic position forming a slightly distorted octahedron.     

Hydrothermal crystallization and X-ray structure determination of a new decavanadate with mixed cations [Mn(H2O)6]2[N(CH3)4]2[V10O28]·2H2O

A new decavanadate with mixed cations, [Mn(H₂O)₆]₂[N(CH₃)₄]₂[V₁₀O₂₈]·2H₂O (1), was crystallized from a hydrothermal reaction between MnCO₃ and V₂O₅ in the presence of N(CH₃)₄Br at 100°C. The structure of 1, as determined by x-ray single crystal analysis, consists of cations and anions of hexa-aqua manganese [Mn(H₂O)₆]²⁺, tetramethyl ammonium [N(CH₃)₄]⁺ and decavanadate [V₁₀O₂₈]^6–. The extended H-bonding between the [Mn(H₂O)₆]²⁺ and [V₁₀O₂₈]^6– ions gives rise to a pseudo- two-dimensional network in the crystal lattice x-ray crystallographic data for 1: monoclinic P2₁/n, a = 9.1499(5), b = 12.8725(7), c = 18.625(1) Å, = 92.252(1)°, V = 2192.0(2) ų, MZ = 2, and D _calcd = 2.22 g cm^–3.     

Crystal structure of 9,12-ethano-12a-methoxycarbonyl-5, 8a,9,12,12a,12b-hexahydro-6H-[1,2]dioxino[4′,5′:4,5] isoxazolo[3,2-a]isoquinoline, C17H19NO5

The title compound crystallizes in the space group P2₁/n, with a = 18.423(3), b = 9.628(3), c = 19.243(2) Å, = 116.208(8)°, with two independent molecules in the asymmetric unit, which are not enantiomers. The chiral centers C8a, C9, C12, C12a, C12b are either S,R,S,R,R or R,S,R,S,S, respectively, because of the centric space group.     

Synthesis,Structure, and Electrochemical Properties of New Sterically Hindered o-Benzoquinone—6,9-Di-tert-Butyl-1,2,3a,4-Tetrahydrobenzo[b]oxazolo[3,2-d][1,4]oxazine-7,8-Dione

Crystallography Reports - A new representative of sterically hindered 3,6-di-tert-butyl-o-benzoquinones bearing an annulated tetrahydrooxazolo[3,2-d][1,4]oxazine...     

Crystal structure of a synthetic anabolic agent: stanazolol ethanol solvate, 17β-hydroxy-17α methylandrostano[3,2-c]pyrazole ethanoate

The crystal and molecular structure of 17-hydroxy-17 methylandrostano[3,2-c]pyrazole ethanoate (stanazolol ethanol solvate), C₂H₃₀N₂OC₂H₅OH, has been determined by direct methods and refined by full-matrix least squares to a final R of 0.0577 for 4021 observed reflections and 245 parameters using Cu K radiation, = 1.54178 Å. The compound crystallizes in space group P2₁2₁2₁ with Z = 4 molecules per unit cell. In the steroid skeleton the ring A adopts a half-chair conformation, being considerably strained, as a consequence of the fused planar pyrazole ring E. Rings B and C however are chairs and ring D has a 13,14 half-chair conformation. All rings of the steroid skeleton are trans-connected. The OH group of the solvated ethanol molecule is hydrogen bonded to the -oriented carbonyl substituent O(20) of ring D. The molecules are further held together in the crystal structure by head–tail hydrogen bonding between N(1)H in the pyrazole ring and O(20), which consequently is an acceptor for the two H-bonds. Overall the molecule lacks any significant curvature with no interplanar dihedral angle greater than 7°. Possible binding modes of stanazolol with the human androgen receptor are discussed.     

Preparation and X-ray structure of [(methyl quinaldate)2H]+ [AuBr4]−

The crystal structure of the title complex (R _F =0.051 for 2384 observed MoK data) consists of a packing of tetrabromoaurate(III) anions and [(methyl quinaldate)₂H]⁺ cations in which the two planar heterocyclic ring moieties are interlinked by a proton to form a NHN hydrogen bond of length 2.88(1) Å; the dihedral angle of the planes is 79.5°. The infrared spectrum of the compound is also discussed.     

Crystal structure of cesium sodium hexathiocyanatobismuthate Cs2Na[Bi(SCN)6] and characterization of Cs2Na[Bi(SCN)6−x Cl x ] and Cs2Na[Bi2(SCN)9−x Cl x ] complexes by X-ray powder diffraction

Cs₂Na[Bi(SCN)₆] crystallizes in the trigonal space group with one formal molecule per unit cell.M=846.25,a=7.189(1),c=10.580(2) ,V=473.5(1) ,D _x =2.967 g cm^–3, (MoK)=13.70 mm^–1,F(000)=378. FinalR=0.029 for 917 absorption-corrected reflections. The structure consists of infinite[Bi(SCN)₆Na] ^2– anionic chains along thec axis with slightly distorted octahedral Bi–6S and Na–6N coordination and Cs⁺ ions surrounded by three anionic chains with irregular coordination by six N and three S atoms. X-ray powder diffractograms of three complexes, Cs₂Na[Bi(SCN)_6–x Cl _x ] withx=2, 3 and 4, indicate that the mixed complexes are not isostructural and can be indexed in different orthorombic unit cells witha=14.617(8),b=12.32(1),c=10.769(6) forx=2;a=15.37(1),b=10.81(1),c=10.287(6) forx=3 anda=14.662(7),b=14.366(7),c=7.932(4) forx=4. The two dinuclear complexes Cs₂Na[Bi₂(SCN)_9–x Cl _x ] withx=2 and 3, despite the large similarity of their diffractograms, are not isostructural and can be indexed in different orthorombic unit cells witha=14.79(1),b=13.72(1),c=10.591(5) forx=2 anda=18.423(8),b=15.657(7),c=7.410(7) forx=3.     

X-ray crystal structure ofcis-H(Ph3Si)Pt[Ph2P(CH2)4PPh2] ·0.5 C6H6

The title compound, cis-hydrido(triphenylsilyl)-1,4-butanediyl-bis-(diphenylphosphine)platinum(II) (I), crystallizes in the monoclinic space groupP2 ₁/n (No. 14) witha=9.472(4),b=16.924(5),c=25.799(4) Å, β=91.29(3)° andZ=4. The structure was solved using the direct methods and refined by the full-matrix least-squares procedure to yield residuals ofR=0.024 andR _w =0.025 based on 4160 unique reflections. The square-planar geometry about the Pt atom is angularly distorted with P(1)?Pt?P(2) and Si?Pt?P(2) angles of 103.5(1) and 102.1(1)°, respectively. The Pt?P(1) bond is longer than the Pt?P(2) bond due to thetrans influence of the SiPh₃ group. Distortion due to steric bulk of the ligands is accommodated by the opening of the tetrahedral angles at the silicon and phosphorous atoms.     

Phosphinimine complexes of technetium(VII): X-ray crystal structure of [Ph3P=NH+2][TcO−4]1

An X-ray diffraction study and the solution chemistry is reported for the very stable ion pair [Ph₃P=NH⁺₂][TcO^–₄]. This compound crystallizes in the orthorhombic system, in space group P2₁2₁2₁, with cell dimensions of a = 11.1454(6), b = 11.449(2), and c = 14.570(2)Å, and refining to R = 0.023 and R_W = 0.031. Strong hydrogen bonds are formed between the iminium protons and the pertechnetate oxygens (1.89(6) and 2.23(6) Å) in the solid state, and similar hydrogen bonding apparently occurs in aqueous solution to stabilize the phosphiniminium cation to hydrolysis.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]-imino]ethanolato]N,O,O′]di-copper(II) dihydrate

The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·2H₂O crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C₂₆H₂₄Cl₂Cu₂N₂O₄ molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu₂Cl₂ (C₁₃H₁₂NO₂)₂]·1/2H₂O is given.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]imino]-ethanolato]N,O,O′]di-copper(II) hemihydrate

The structure of the title compound [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·1/2 H₂O has been determined from single crystal X-ray diffraction data by direct methods. Full-matrix least-squares refinement of the structural parameters led to conventionalR factor of 0.037 for 4367 intensities above 3(I). The compound forms a dinuclear complex with distorted tetragonal-pyramidal geometry at each copper center. The unsymmetrical dimers are formed by weak axial coordination to one copper center by chloride ligands which are in the base plane of the adjacent copper atom. The apical Cu1-C12 and Cu2-C11 distances are 2.788(1) and 3.130(1) Å, respectively. The Cu1-Cu2 separation is 3.4995(3) Å in the dimers. A disorder of one five-membered chelate ring has been observed. Two alternative positionsa andb of the C26 atom were found and refined with constrained bond lengths. The geometry of the ligand and hydrogen bonds is discussed.     

Air-stable liquid clathrates. 1. Crystal structure of [NBu4][Br3] and reactivity of the [NBu4][Br3]·5 C6H6 liquid clathrate

[NBu₄][Br₃] interacts with C₆H₆ to form an air-stable liquid clathrate. The tribromide anion reacts with phenol to give para-bromophenol in>95% yield. The HBr which is generated in the reaction combines with the Br^– anion to form [Br-H-Br]^–. The latter forms the basis for a new liquid clathrate, [NBu₄][Br-H-Br]·n C₆H₆. The parent salt, [NBu₄][Br₃], crystallizes in the monoclinic space group C2/c witha=12.983(5),b=10.380(7),c=16.222(6) Å,=93.93(3)°, andD _c =1.47 g cm^–3 forZ=4. The final R value is 0.068 based on 787 observed reflections.     

Synthesis,characterization, and crystal structure of 1,3,7,9-tetramethylpyrido-[2,3-d∶6,5-d′]-dipyrimidine-2,4,6,8-tetrone

A new and easy method for the preparation of 1,3,7,9-tetramethylpyrido-[2,3-d6,5-d]-dipyrimidine-2,4,6,8-tetrone is described. The structure of this compound has been solved by means of X-ray diffraction methods. The chemical characterization by spectral (mass, ultraviolet, infrared, and proton nuclear magnetic resonance) and thermal (thermogravimetry and differential scanning calorimetry) method is also reported. The compound is monoclinic, space groupP2₁/c,a=12.720(5),b=13.688(7),c=8.079(2) Å, =107.06(4)°,Z=4. The structure consists of discrete tricyclic molecules, stacking playing an important role in crystal packing.     

The Chair–Envelope Conformation of Two Derivatives of Triethylammonium 3-Oxo-8,9-Dinitro-Bicyclo [3.3.1] Non-7-En-6-Nitronate [I] and [II]

Abstract  

The title compounds C₁₉H₁₈N₃O₉ ⁻·C₆H₁₆N⁺ (I) [triethylammonium 2-benzyl-2-ethoxycarbonyl-3-oxo-8,9-dinitro-bicyclo [3.3.1] non-7-en-6-nitronate] and C₁₉H₁₇N₄O₁₁ ⁻·C₆H₁₆N⁺ (II) [triethylammonium 2(4-nitrophenylmethyl)-2-ethoxycarbonyl-3-oxo-8,9-dinitro-bicyclo [3.3.1] non-7-en-6-nitronate] crystallize in monoclinic crystal system with P2 ₁ /c space group. In compounds I and II, the bicyclo [3.3.1] nonane has chair–envelope conformation. The crystal structure of compound (I) is stabilized by N–H⋯O, N–H⋯N hydrogen bonds. In both the crystal structures weak C–H⋯O hydrogen bond is observed. Both compounds adopt chair–envelope conformation. An examination of puckering parameters, torsion angles and model (Dreiding) of the title compounds clearly indicates that the ring A has slightly distorted chair conformation and ring B has slightly distorted envelope conformation.