Synthesis,crystal and molecular structure of 1,3-dimethyl-10-benzyl-2,4,9-trioxo-1,3,6,7,8,10-hexahydro-1,3-diazepino-[2,1-f]-purine

The crystal and molecular structure of the title compound, obtained as a result of intramolecular cyclization of 4-(8-benzylaminotheophylline-7-yl)-butanoic acid, has been determined by X-ray diffraction. Two rings, (comprising the theophylline skeleton) are planar, but the 7-membered 1,3-diazepinon ring is undulated, with a twisted chair conformation.     

Crystal and molecular structure of 5-carbamyl-5H-dibenzo[b,f] azepine

The structure of the title compound has been determined by direct methods from diffractometer data, and refined by full-matrix least squares. Crystals are monoclinicP2₁/n,a=7.534(1),b=11.150(2),c=13.917(3) Å,=92.94(4)°,Z=4,D _x=1.34 (3) g cm^–3,R=0.084 for 1259 observed reflections. The azepine ring has a boat conformation. The fused benzene rings are planar. Molecules are packed as hydrogen-bonded dimers through the carboxamide groups. The atomic charge distribution over the fused ring system is approximately symmetrical.     

Synthesis and crystal structure of 4,5-dibromo[2.1.1]triblattene

Reaction of 4-bromopentacyclo[7.3.0.0^2,7.0^3,11.0^6,10]dodec-11-ene (1) with Br₂—CCl₄ afforded 4,4,5-tribromopentacyclo[7.3.0.0^2,7.0^3,11.0^6,10]dodecane (2) in 89–94% yield. Subsequent treatment of 2 with KOt-Bu-t-BuOH resulted in competitive elimination of the elements of HBr and of Br₂ with concomitant formation of 4,5-dibromopentacyclo[7.3.0.0^2,7.0^3,11.0^6,10]dodec-11-ene (3, 76%) and 1 (17%), respectively. The structure of 3 was established unequivocally via application of X-ray crystallographic methods. Crystal data for 3: monoclinic, C2/c, a = 9.895(1), b = 9.0963(7), c = 12.471(1) Å, = 106.875(8)°, z = 4.     

Synthesis and crystal structure of 7,7-dimethyl-2,4-diphenyl-5-oxo-1,4,5,6,7,8-hexahydroquinolin

The 7,7-dimethyl-2,4-diphenyl-5-oxo-1,4,5,6,7,8-hexahydroquinolin was synthesized and the compound was identified by IR, ¹H NMR, elemental analysis and X-ray crystallography. It crystallized in the triclinic space group , with a = 7.129(2) Å, b = 10.514(3) Å, c = 13.040(3) Å, =76.58(2)°, =88.97(2)°, =79.24(2)°, and D _calc = 1.172 g cm^–3 for Z = 2. X-ray analysis revealed that the atoms C(2), C(3), C(4), C(10), C(9), and N form a six-membered ring that adopts a boat conformation, and another six-membered ring (C(10)–C(9)–C(8)–C(7)–C(6)–C(5)) adopts a half-chair conformation. In addition, there is an intermolecular hydrogen bond (N–H0O) in the product molecule.     

Synthesis and crystal structure of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.02,6.04,10.08,12]pentadecane

Crystals of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.0^2,6.0^4,10 .0^8,12]pentadecane, a new hexaazaisowurtzitane derivative, were obtained from a condensation reaction of 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0^5,9.0^3,11] dodecane with aqueous formaldehyde and subsequent crystallization of the product from aqueous acetone. X-ray diffraction analysis at room temperature indicates that the compound crystallizes in monoclinic system, space group P2₁/n with a = 9.4564(15), b = 14.184(2), c = 13.334(2) ?, β = 107.671(4)°, V = 1704.1(5) ?³, Z = 4, D _calc = 1.475 g/cm³, F(000) = 800, μ(MoK) = 0.112 mm⁻¹, and final R ₁ = 0.0505, wR ₂ = 0.1215 for observed reflections 2641 (I > 2σ(I)). The ether link (C–O–C) forms two heptacyclic rings with the N, C atoms in the cage respectively. The results of elemental analysis, IR and NMR spectroscopy are included.     

Solid state conformational parameters in dibenzo[b,f]heteroepin drugs: Crystal structures of 3-methoxy-10-methyl-11-phenyldibenzo[b,f]thiepine and 3-allyloxy-10-ethyl-11-phenyldibenzo[b,f]oxepine

The structures of 3-methoxy-10-methyl-11-phenyldibenzo[b, f]thiepine (I) [C₂₂H₁₈OS, tetragonal,I4₁/a, witha=33.81(1),c=6.065(5)Å,Z=16] and 3-allyloxy-10-ethyl-11-phenyldibenzo[b,f]oxepine (II) [C₂₅H₂₂O₂, mono-clinic,P2₁/c,a=12.115(7),b=16.316(9),c=10.136(7)Å,=105.05(9)°,Z=4] have been determined by the symbolic addition procedure and refined by least-squares method to anR of 0.090 for 784 diffractometer-measured reflections (I) and to anR of 0.083 for 442 reflections (II). The dihedral angle between the phenyl-ring mean planes is 111.3° in (I) and 121.1° in (II), the middle seven-membered ring has the boat conformation, and the tricyclic moiety has twist and skew values of 6° and 0.42 Å in (I) and 0.3° and 0.79 Å in (II). The overall conformational characteristic for the tricyclic (6, 7, 6)-dibenzo[b,f]heteroepin derivatives have been reviewed to gain a better understanding of what requirements may be important for interaction of drugs of this class at the receptor site.     

Synthesis and crystal structure of charge-transfer salt (BEDT-TTF) [Pt(mnt)2]

The synthesis and crystal structure of the title organic charge-transfer salt (BEDT-TTF)[Pt(mnt)₂] (BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene; mnt = cis-3,4-dimercapto-2-butenedinitrile) is described. The salt crystallizes in the P1 space group with a = 6.728(2) Å, b = 7.371(2) Å, c = 13.596(4) Å, = 97.904(5)°, = 90.114(5)°, and =108.147(5)°. The stoichiometry between BEDT-TTF and [Pt(mnt)₂] is 1:1. The bond length of the central C=C bond in a BEDT-TTF ion is 1.398 (16) Å, indicating an oxidation state of +1 in BEDT-TTF ion. The structure consists of layers of BEDT-TTF and Pt(mnt)₂ along the c axis. Within each layer, both BEDT-TTF and Pt(mnt)₂ ions form segregated stacks. The stacking is not in a face-to-face manner, but instead, is through a side-by-side arrangement along the a axis, with closest SS contacts of 3.461(3) Å between neighboring BEDT-TTF ions. The structure is consistent with the semiconducting behavior found in the solid.     

The crystal structure of a cyclodecabis[1,2,3]selenadiazole

4,5,6,10,11,12-hexahydrocyclodeca[1,2-d6,7-d]bis[1,2,3]selenadiazole, C₁₀H₁₂N₄Se₂, crystallizes in triclinic space group P witha=5.4625(3),b=7.2091(4),c=8.3122(6) , =65.313(5), =77.476(5), =77.442(5)°,V=287.35(4) ³,Z=1. The structure was refined toR=0.031 andR _w=0.030 for 2018 observed reflections. The molecule lies on an inversion center. The cyclodecadiene ring adopts an elongated chair conformation. The near-zero torsion angle of the elongated chair lies at the ring-fusion bonds, with a magnitude of 2.9(3)°. The five atoms of the selenadiazole ring exhibit maximum deviation 0.005(2) from planarity, with the adjacent carbon atoms lying respectively 0.020(2) and 0.059(2) to the same side of this plane. The torsion angles about the bonds comprising the sides of the elongated chair vary in magnitude from 61.0(2)° to 55.7(2)°. The cyclodecadiene C=C bond lengths are 1.368(2) . The selenium-carbon bond length is 1.850(2) . The Se–N distance is quite long, 1.888(2) .     

Synthesis and crystal structure of 5-allyl-5<Emphasis Type="Italic">H</Emphasis>dibenzo[b,f]azepine

The crystals 5H-dibenzo[b,f]azepine 2 and 5-allyl-5H-dibenzo[b,f]azepine 3 were synthesized and characterized by X-ray crystallography. The compound 3 is a novel synthon for the construction of unusual isoxazoli(ne)dine rings bearing at the 5th position of dibenzo[b,f]azepine moiety. The compound 2 (C₁₄H₁₁N) crystallizes in the orthorhombic space group P2₁2₁2₁ with the parameters a = 6.036(1) Å, b = 8.250(7) Å, c = 20.528(4) Å, Z = 4 and the final R factor is R1 = 0.0544. The compound 3 (C₁₇H₁₅N) crystallizes in the Hexagonal space group P6₁ with the parameters a = 11.043(9) Å, c = 18.575 Å, Z = 6 and the final R factor is R1 = 0.0373.     

Crystal and molecular structure of 2-bromobenzo[b]indeno[1,2-e]pyran

2-bromobenzo[b]indeno[1,2-e]pyran crystallizes in the monoclinic system: space groupP2₁/c,a = 7·508,b = 5·959,c= 26·172 Å, = 92·55 °. The structure has been determined by the heavy-atom method and refined by full-matrix least squares toR = 0·072 for 1027 observed reflections.The molecule is non-planar; the maximum deviations from the best plane occur at both ends of the length of the molecule, which results in distortion of the central portion from the expected geometry. The closest approach of two molecules, those related by a 2₁ axis, is 3·5 Å.     

Synthesis and structure of 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2, 2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, a chiral ligand building block

A triphenyl analog of taddol, 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2,2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, has been synthesized and structurally characterized. This molecule could act as a chiral ligand building block in the creation of tuned taddol analogs. Structural analysis of the title compound reveals that the hydroxyl group is involved in an intramolecular hydrogen bond and does not take part in any intermolecular interaction. Crystal packing is influenced by C–H O hydrogen bonding and phenyl phenyl interactions. Crystal data: Triclinic, P1 (No. 1), a = 5.9343(4) Å, b = 8.2367(17) Å, c = 10.987(2) Å, = 88.290(6), = 75.442(4), = 80.655(6), V = 512.86(15) ų, Z = 1, D _calc = 1.258 mg/m³. Final residual values were R ₁ = 0.0407 for 3022 observed data (I > 2s(I) ) and wR ₂ = 0.0941 for all 3524 unique data.     

Configuration,conformation and crystal structure of rabdosianin b

Rabdosianin B, 7,20‐epoxy‐7β‐hydroxy‐1α,6β,11α,15β‐tetraacetoxy‐ent‐kaur‐16‐ene, C₂₈H₃₈O₁₀, was the first isolated from Isodon henryi. It consists of three six‐membered rings A, B, C and one five‐membered ring D. The fused‐ring system A, B and C are in chair, boat and chair conformations, respectively, and ring D is in an envelope conformation, on the basis of NMR and X‐ray diffraction analysis. The crystal of rabdosianin B is in orthorhombic crystal system with space group P2₁2₁2₁, lattice constants: a = 9.969(1) Å, b = 15.400(3) Å, and c = 17.624(3) Å, Z = 4. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of 2-propyl-5-phenyl-1, 4-dioxo-1,2,3,4,5,6,7,8-octahydro-[1,4,2]diazaphosphorino [1,2-a][1,3,2]benzodiazaphosphorine 3-oxide

The synthesis and structure characterization of 2-propyl-5-phenyl-1,4-dioxo-1,2,3,4,5, 6,7,8-octahydro-[1,4,2]diazaphosphorino[1,2-a][1,3,2]benzodiazaphosphorine 3-oxide are described. The title compound has been designed to incorporate proximate carbonyl and phosphoryl groups in a heterocycle fused to benzophosphadiamide heterocycle. Crystal data: C₁₉H₂₀N₃O₃P, Monoclinic, space group P2(1)/c, with a = 9.7585(9) Å, b = 21.4319(19) Å, c = 17.7900(16) Å, β = 100.823(2)°, Z = 8, V = 3654.5(6) ų. The crystal structure shows that the proximate carbonyl and phosphoryl groups are not coplanar, and the [1,4,2]diazaphosphorino moiety prefers the boat conformation.     

Crystal and molecular structure of 3-methoxy-10-methyl-11-phenyl-11-hydroxy-10,11-dihydrodibenzo [b,f] thiepine

Journal of Chemical Crystallography - The structure of the title compound (C22 H20O2S) is orthorhombic with space groupPca21,a=15.467(8),b=9.410(6),c=25.092(7) Å andZ=8. It has been solved by...     

X-ray crystal structure analysis of nitroxazepine: 10-(3-dimethylaminopropyl)-2-nitro-10,11-dihydrodibenz [b,f][l,4]oxazepin-11-one

The title compound, C₁₈H₁₉O₄N₃,M _r=341, the base (I) of the dibenzoxazepine anti-depressant drug Sintamil, crystallizes in the orthorhombic space group,Pbca withZ=8 in a cella=8.636(2),b=23.687(3),c=16.787(3)Å,V _c=3434 ų. The structure was solved by direct methods and refined toR=0.102 (R _w=0.093) with 1348 observed CuK reflections. The tricyclic framework takes up a saddle shape with the heterocyclic ring in boat conformation; the flanking planar aromatic rings make angles 148.2(3), 150.8(3)° with the central ring plane, compared with 143.5(5), 158.1(5)° in Sintamil monohydrate (II). BothI andII have extended-CNMe₂ side chains (with appreciable thermal motion); this conformation, and the distances of the -N(CH₃)₃ nitrogen to the centers of aromatic rings (6.4 and 7.8 Å inI), are consistent with inhibition of uptake mechanisms underlying the pharmacological action.     

Synthesis and crystal structure of 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine

The title compound 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine, C₁₅H₁₅N₅S, has been synthesized and characterized by x-ray diffraction: orthorhombic, space group Pbca, with a = 17.3480(9), b = 8.5022(5), c = 19.8132(11) Å. Z = 8, V = 2922.4(3) ų. The compound shows a fully delocalized pyrazolo[3,4-d]pyrimidine system with a sp² hybridization of the N(4) atom.     

Trimethylamine-N-oxide induced disproportionation of Re2(CO)10: Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]

An attempted synthesis of [Re(CO₃) (-OH)]₄,1, by reacting Re₂(CO)₁₀ with an excess of NMe₃O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)₃(ONMe₃)₃][ReO₄],2. The structure of2 was determined via X-ray crystallography: tri-clinic,P1^¯,a=9.499(5),b=9.841(2),c=13.448(2)Å,=109.92(2),=106.89(3), =93.15(4)°,D _calc=2.22 g^–3 andZ=2. Least-squares refinement based on 1606 observed (I>3(I)) reflections gave final values ofR=0.040 andR _w=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe₃O ligands.     

The crystal and molecular structure of 6,8,15,16b,16c,17-hexahydro-16b,16c-diphenyl-7H,16H-6a,7a,15a,16a-tetraazanaphtho[5,6]azulano[2,1,8-ij]naptho[f]azulene-7,16-dione

The crystal and molecular structure of a clip containing molecule is described. The structure was solved by vector search methods and refined by least squares methods toR _l=0.0768 [I>2(I)]. Crystal data: C₄₀H₃₀N₄O₂·HCCl₃, triclinic, space group ,a=9.302(2),b=12.981(2),c=15.765(2)Å, =65.91(2)°, =76.40(2)°, =80.15(1)°,V=1682.9(4)ų, Z=2.