Synthesis and crystal structure of N-benzylmethy- lammonium pentachlorothallate (III), [C6H5CH2NH2CH3]2TlCl5

N-Benzylmethylammonium pentachlorothallate (III) salt crystallizes in the monoclinic system P2₁/c with the following unit cell dimensions: a = 10.9540 (8), b = 12.559(1), c = 18.099(2)Å, = 112.1(3)° and Z = 4. The examination of the structure shows an alternate stacking of inorganic layers of pentachlorothallate (III) anions and organic layers of [C₆H₅CH₂NH₂CH₃]⁺ cations parallel to the c axis. The cohesion forces of the packing of N-benzylmethylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N—HsCl) and van der Waals contacts.     

Synthesis and crystal structure of 7,9-dideacetyl-1-deoxybaccatinVI

7,9-dideacetyl-1-deoxybaccatinVI was synthesized from 1-deoxybaccatinVI and its crystal structure was determined by X-ray crystallographic techniques. The compound (C₃₃H₄₂O₁₁·2CH₄O) crystallizes into monoclinic space group P2₁ with unit cell parameters: a=8.654(17) ?, b=16.470(5) ?, c=12.671(3) ?, β=97.63(2)°, and Z=2. The X-ray results demonstrated that the reaction of 7,9,10-Trideacetyl-1-deoxy-baccatinVI with Ac₂O in tetrahydrofuran, using CeCl₃ as catalyst, yielded monoacetylated product 7,9-dideacetyl-1-deoxy baccatinVI. In the structure, the six-membered A ring exhibits boat conformation, the eight-membered B ring adopts boat-chair conformation, and the six-membered C ring exhibits sofa conformation.     

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.     

Synthesis and structure ofexo-11-cyano-endo-11-(trimethylsilyloxy)pentacyclo[5.4.0.02,6.03,10.05,9]undecan-8-one

The crystal structure of an asymmetric pentacyclo[5.4.0.0^2,6.0^3,10.0^5,9]undecan-8,11-dione derivative is reported, in which Me₃SiCN has been added across one of the keto groups. The cage structure demonstrates the expected effects of this addition.     

Synthesis and Crystal Structure of Compound 1,5-bis(4-methoxyphenyl)-3a-(2-phenyl-2H-1,2,3-triazol-4-yl)-4,5-dihydro-3aH-benzo[b][1,2,4]oxadiazolo[4,5-d][1,4]thiazepine

Abstract The crystal structure of title compound has been determined. The compound crystallizes in the triclinic system with space group P-1, lattice parameters; a = 9.2938 (5) ?, b = 11.9992 (7) ?, c = 25.5918 (13) ?, α = 91.343 (2)°, β = 95.8360 (10)°, γ = 101.005 (2)°, V = 2784.3 (3) ?³, Z = 4, X-Ray analysis reveals that the molecular backbone consists of tricyclic system with the central seven-membered ring in twisted chair-like conformation. Graphical abstract The crystal structure of 1,5-bis(4-methoxyphenyl)-3a-(2-phenyl-2H-1,2,3-triazol-4-yl)-4,5-dihydro-3aH-benzo[b][1,2,4]oxadiazolo[4,5-d][1,4]thiazepine was first determined by single-crystal X-ray diffraction which reveals that the molecular backbone consists of a tricyclic system with the central seven-membered ring in twisted chair-like conformation .     

The crystal structure of hexabenzoylhexaazaisowurtzitane

The crystal and molecular structure of an interesting cage compound is described. Crystal data: C₄₈H₃₆N₆O₆·(CH₃)₂CO; monoclinic; space group: P2 ₁ /n; a = 14.948(3) Å, b = 15.079(3) Å, c = 19.539(4)Å, = 93.93(3)°, V = 4394(2)ų; and Z = 4.     

Synthesis and crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one

The x-ray crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one has been determined. Yellow block shaped crystals of C₉H₁₀OS₄ crystallize in the space group P with cell dimensions a = 8.872(4), b = 9.330(8), c = 14.333(12) Å, = 95.23(7), = 91.09(5), = 107.60(5)°, V = 1124.8(14) ų, and Z = 4. This compound has two S---S contacts [3.574, 3.610 Å] shorter than 3.70 Å and the usual disordered ethylene moiety [C(3)—C(8)] of the six-membered ring is fixed by the cis-cyclohexylene subsitituent. This means that it may be a new precursor for conducting and strong near-IR absorbing nickel-dithiolenes. Also, it provides the first example of polymorphism of the dmit derivatives and contains two independent molecules I and II in the asymmetric unit.     

Synthesis and crystal structure of cyanohydrin trimethylsilyl ether of o-chlorobenzoylferrocene

The cyanohydrin trimethylsilyl ether of o-chlorobenzoylferrocene has been synthesized by the addition of trimethylsilyl cyanide (TMSCN) in methylene chloride in the presence of zinc iodide. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with the following crystallographic parameters: a = 9.480(3) ?, b = 22.319(6) ?, c = 9.783(3) ?, β = 101.197(4)°, μ = 0.943 mm^− 1, V=2030.5(10) ?³, Z=4, F(0 0 0) = 880, D _calc=1.386 mg/m³, T=293(2) K, 1.82° ≤ θ ≤ 26.40°, the final R factor: R ₁=0.0366, wR ₂=0.0802.     

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.     

Synthesis and crystal structure of macrocyclic nickel(II) complex bridged by chromate

A novel compound catena-(-CrO₄-O,O)[Ni(L¹)Ni(L²)] 3H₂O (1) (L¹ = 3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane and L² = 2,5,9,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized for the first time and structurally characterized. 1 crystallizes in the triclinic space group P with a = 9.623(1), b = 10.084(1), c = 12.723 (3) Å, = 66.74(2), = 75.20(1), = 72.02(1)°, V = 1066.2(3) ų, and Z = 2. The coordination environment around the Ni(II) ions is an axially elongated octahedron with the secondary amines of the isomeric ligands and two oxygen atoms of [CrO₄]^2–.     

Synthesis and crystal structure of a novel polymeric silver(I) complex

The complex of [Ag₂(μ–L)₂(μ–NO₃)₂]_n, where L?=?2–methyl–5–(2–pyridyl)–1,3,4–oxadiazole, has been synthesized and characterized by single–crystal X–ray diffraction analysis. The crystals are in triclinic system with space group P–1. Complex [Ag₂(μ–L)₂(μ–NO₃)₂]_n is a polymeric silver(I) complex bridged through the 1,3,4–oxadiazole rings and the nitrate ions, and the center Ag1(I) atoms have distorted trigonal bipyramidal geometries [AgN₃O₂].     

Synthesis and crystal structure of the copper(I) complex with 2-[(o-pyridyl)-sulfanylmethyl]-pyrimidine ligand

The reaction of a flexible monothioether ligand, 2-[(o-pyridyl)-sulfanylmethyl]-pyrimidine (L), with CuI leads to the formation of a novel complex [Cu₄I₄(L)₂] (1), which has been characterized by elemental analyses, IR spectroscopy, and single-crystal X-ray diffraction analysis: monoclinic, space group P2₁/n, with a = 10.921(5), b = 10.824(5), c = 13.128(6) Å, β = 109.333(5)° and Z = 2. Single-crystal X-ray analyses show that complex 1 is tetranuclear structure with a distorted chair-like Cu₄I₄ skeleton. Cu···Cu interactions are found to exist in this tetranuclear molecule. In the packing mode of complex 1, there exist N⋯⋯⋯I weak interactions and intermolecular π–π contacts. These weak interactions not only stabilize the structure of complex, but also further link the tetranuclear molecules into a high-dimensional supramolecular architecture.     

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.     

Synthesis and crystal structure of bis(4-methylpiperidine-dithiocarbamato-S,S′)-palladium(II)

The complex bis(4-methylpiperidine-dithiocarbamato-S,S′)-palladium(II) was synthesized by the reaction of 4-methyl-1-piperidine dithiocarbamic acid with palladium(II) chloride. Its structure was determined by X-ray crystal diffraction analysis. It crystallizes in the monoclinic P2₁/c space group with the crystal cell parameters a=8.6491(8) ?, b=18.7305(16) ?, c=11.9933(10) ?, β=107.074(1)°, V=1857.3(3) ?³ and Z=4. The palladium (II) ion is bonded to four sulfur atoms, belonging to two dithiocarbamate ligands, in a distorted square planar geometry. The X-ray data suggest a pronounced electronic delocalization in the two NCS₂ moieties.     

Crystal structure of 2,3-dihydronaphto[2,3-b) [1,5] dioxepin

The X-ray single crystal structure of C₁₃H₁₂O₂ compound was determined. It crystallizes in the orthorombic space group P2₁2₁2₁ with a = 7.8847(7), b = 9.639(1), c = 13.432(2) Å, Z = 4 and V = 1020.8(3) ų. The final R converged to 0.037 for 1763 independent reflexions. The title compound forms layers parallel to (1 0 0) planes and the three dimensional cohesion of the crystal is assumed by Van der Waals interactions. The molecule consists of two six-membered rings (A and B) and a seven-membered ring (C). A and B rings are planar, whereas the C ring has a chair conformation     

Synthesis and crystal structure of a silver(I) complex with dithioether ligand

The reaction of the dithioether ligand, 2,3-bis(5-methyl-1,3,4-thiadiazole-2-thiomethyl) quinoxaline (L) with AgBF₄, leads to the formation of a novel complex {[AgL](BF₄)}_∞ 1, which has been characterized by single-crystal X-ray diffraction analysis: monoclinic, space group C2/c, with a = 20.316(7) ?, b = 12.401(4) ?, c = 18.039(6) ?, β = 108.404(6)° and V = 4312(3) ?³. The crystal structure of the complex consists of 1D {[AgL]⁺}_∞ cation chain and BF₄ ⁻ anions. In 1, the coordination geometry of Ag^I center can be best described as trigonal planar coordinated by three N from two distinct L ligands. The ligand is polydentate with one end adopting a bidentate conformation to chelate an Ag^I atom and the other end monodentate to bridge another Ag^I resulting in an infinite chain along b axis. There exist Ag⋯N weak coordination, π–π stacking and F⋯S weak interactions in the complex, and these weak interactions link the 1D complex into 3D supramolecular structure and further stabilize the crystal structure in the solid state.     

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.     

Synthesis and crystal structure of a 2D (6,3) coordination network, {[Ag(L)1.5]NO3} n [L = 1,3-bis(benzylthio)propane]

A new dithioether silver(I) complex, {[Ag(L)_1.5]NO₃} _n (1) has been prepared by the reaction of AgNO₃ with 1,3-bis(benzylthio)propane (L) in methanol/chloroform. The structure was characterized by single-crystal X-ray diffraction analysis: rhombohedral system, space group R –3c, with a =b = 15.651(7), c = 39.26(4) Å, V = 8328(1) ų, and Z = 6. The crystal structure consists of [Ag(L)_1.5]⁺ cations and NO₃ ^– anions. In 1, each silver(I) center is coordinated equivalently to three sulfur donors from three different ligands to give a trigonal-planar coordination geometry. Each L links two adjacent silver(I) centers in bis-monodentate bridging mode to form a 2D (6,3) network sheet. Furthermore, these 2D sheets are linked by the weak coordination interactions between nitrate ions and silver(I) atoms to form a 3D brick-wall framework.     

Synthesis and crystal structure of 1-(4-bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane

1-(4-Bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane, C₁₃H₁₅BrO₃, has been synthesized from 4-bromophenylacetic acid chloride via the oxetan ester (3-methyl-3-oxetanyl)methyl-2-(4-bromophenyl)acetate. The crystal structure of the title compound has been determined at low temperature (120 K), by X-ray diffraction methods. This compound crystallizes in the monoclinic space group P2₁/n (No. 14), Z = 4, with lattice parametersa = 6.019(5), b = 20.990(5), c = 9.915(2) Å, and = 101.29(1)°.