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 structure of 6-phenyldiquino[3,2-b;5,6-b′] [1,4]thiazine

The title compound (C₂₄H₁₅N₃S) is monoclinic, with a = 10.816(1), b = 8.193(1), c = 10.892(1), = 104.20(1)° and space group P2₁. The molecule is folded with the central ring in a boat conformation. It can also be considered as folded around the C—C axis between the thiazine and pyridine rings. The butterfly folding angle between the two quinoline planes is 20.5(1)° and between the planes of the two halves of the thiazine ring is 30.6(1)°. The phenyl substituent is in an equatorial location with respect to the thiazine ring with the C—N···S angle of 163.0(2)°. The phenyl plane nearly bisects the pentacyclic ring system and is nearly perpendicular to the C(2), C(3), C(12), C(13) plane.     

Self-Assembly of C-Methyl Calix[4]resorcinarene with 5,5′-Bipyrimidine

Abstract The X-ray crystal structure of the complex formed between 5,5′-bipyrimidine and C-methylresorcinarene is described. The structure (C₄₁H₄₅N₅O₁₂) is triclinic with a = 12.8610(10), b = 13.0560(10), c = 13.6068(11)?, α = 104.0730(10), β = 104.9260(10), γ = 111.6430(10)° and space group P-1. The structure reveals that the resorcinarene adopts a boat conformation and forms a three-dimensional network through hydrogen bonding to two water molecules and one dipyrimidine ligand. A single nitromethane molecule is included in the superstructure. Graphical Abstract Self-Assembly of C-Methyl Calix[4]resorcinarene with 5,5’-Bipyrimidine Charles L. Barnes(1) and Eric Bosch(2)* The X-ray crystal structure of the complex formed between 5,5′-bipyrimidine and C-methylresorcinarene is reported.      

Structure of p-tert-butylcalix[5]arene·ethyl acetate. A polymeric array of neighbor-included calixarenes

p-tert-Butylcalix[5]arene crystallizes from ethyl acetate in the monoclinic space groupC2/c witha=34.793(9),b=13.637(3),c=25.577(7), =114.28(2)°, andD _c =1.08 g cm^–3 forZ=8 (C₅₉H₇₈O₇). Refinement based on 2789 observed reflections led toR=0.071. The complex crystallizes with one molecule of ethyl acetate per calixarene molecule, with the solvent residing between calixarene units instead of within the cavity. The calixarene units neighbor-include to form a polymeric array: a t-butyl group of one calixarene is housed in the cavity of an adjacent calixarene. The packing arrangement of the calixarene molecules bears a remarkable resemblance to a zeolitic array.     

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.     

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,design and characterization of supramolecular self-assembly of calix[4]resorcinare substituted LCs”

A new class of supramolecular calix[4 (a) Kuang, G.C., Jia, X.R., Teng, M.J., Chen, E.Q., Li, W.S., Ji, Y., Chem Mater. 2012, 24,71–80; (b) Macros, M., Omenat, A., Serrano, J.L., and Ezcurra, A., Adv. Mater. 1992, 4, 285–287.[Crossref], [Web of Science ®] , [Google Scholar], [Google Scholar]]resorcinarene substituted alkoxy side chain (-OC₅H₁₁, -OC₈H₁₇, -OC₁₀H₂₁) has been synthesized and well characterized. These supramolecular compounds were investigated by polarizing optical microscope (POM), differential scanning calorimetry (DSC), thermogravimmetric analysis (TGA) and high-temperature X-ray diffraction studies (XRD). The present synthesized supramolecular derivatives are promising to stabilize the hexagonal columnar phase over a broad thermal range. All the synthesized derivatives showed hexagonal columnar phase at lower temperature and showed enantiotropical nature. Compound 2a with small alkyl spacer on eight side showed higher thermal stability as compare to higher alkyl spacer substituted compounds 2b and compound 2c. These research results suggest that calix[4 (a) Kuang, G.C., Jia, X.R., Teng, M.J., Chen, E.Q., Li, W.S., Ji, Y., Chem Mater. 2012, 24,71–80; (b) Macros, M., Omenat, A., Serrano, J.L., and Ezcurra, A., Adv. Mater. 1992, 4, 285–287.[Crossref], [Web of Science ®] , [Google Scholar], [Google Scholar]]resorcinarene was a good platform to construct bowl-shaped derivatives to exhibits the columnar liquid crystal phase and the observed liquid crystalline properties were greatly effected by the substituted alkoxy side chain on eight side of calix[4 (a) Kuang, G.C., Jia, X.R., Teng, M.J., Chen, E.Q., Li, W.S., Ji, Y., Chem Mater. 2012, 24,71–80; (b) Macros, M., Omenat, A., Serrano, J.L., and Ezcurra, A., Adv. Mater. 1992, 4, 285–287.[Crossref], [Web of Science ®] , [Google Scholar], [Google Scholar]]resorcinarene skeletone. All the synthesized compounds were characterized by FT-IR, ¹H NMR and ¹³C NMR spectroscopy.     

Solvothermal synthesis and crystal structure of an inorganic–organic hybrid compound [DAMS]2[CdI4] (DAMS = 4-dimethylaminostyryl-1-methyl-pyridinium)

An inorganic–organic hybrid compound [DAMS]₂[CdI₄] (DAMS = 4-dimethyl-amino- styryl-1-methylpyridinium cation) was synthesized via the solvothermal reaction of equimolar CdI₂ and DAMSI^– in a mixture of acetonitrile and H₂O (2:1 in volume ratio) at 130°C. The product was characterized by X-ray single crystal structure analysis. The crystals of the title compound are triclinic, , with a = 12.9849(19) Å, b = 13.1935(13) Å, c = 13.8792(10) Å, = 106.798(6)°, = 109.827(6)°, = 108.206(9)°, V = 1906.0(4) ų, Z = 2. The cadmium atom was bonded to 4 iodine atoms to form a distorted tetrahedron, which was surrounded by DAMS cations. There exist – stacking interaction between the 2 adjacent antiparallelly arrayed DAMS cations.     

Synthesis and Crystal Structure of the Salt [PPN+]2[Cu2I2Cl2]2−

Abstract The synthesis of the PPN (PPN=Ph₃P=N=PPh₃) salt of di-μ-iodo-dichlorocuprate (I) anion [Cu₂I₂Cl₂]²⁻ is described and the crystal and molecular structures of this compound are reported. It was found that the compound has the formula [PPN]₂[Cu₂I₂Cl₂]_0.7[Cu₂I₄]_0.3 (3). Compound 3 crystallizes in an orthorhombic crystal system, space group Pbca, with a = 19.654(3), b = 16.130(2), c = 20.108(3) ?, V = 6374.3(16) ?³ and Z = 4. The crystal contains 70% [Cu₂I₂Cl₂]²⁻ anions and 30% [Cu₂I₄]²⁻ anions. This was also confirmed by MSES spectroscopy. The anion [Cu₂I₂Cl₂]²⁻ is planar and the Cu atoms have a trigonal planar configuration. Graphical abstract Synthesis and Crystal Structure of the Salt [PPN ⁺ ] ₂ [Cu ₂ I ₂ Cl ₂ ] ²⁻ Andrey A. Yakovenko, Tatiana V. Timofeeva and Mikhail Yu. Antipin The title compound was synthesized and structurally investigated. The crystal contains 70% [Cu₂I₂Cl₂]²⁻ anions and 30% [Cu₂I₄]²⁻ anions. This was confirmed by MS ES spectroscopy.      

Synthesis and optical properties of poly[4-methacryloxy-(4′-carboxy)-azobenzene]

Abstract

In the present work, the homopolymer built from the free radical polymerization of methacrylic monomer incorporating an azobenzene side-group has been synthesized and structurally characterized. The optical properties such as refractive index, extinction coefficient, absorption coefficient and optical energy band gap of poly[4-methacryloxy-(4′-carboxy)-azobenzene] thin film prepared by high vacuum sublimation method were determined using spectroscopic ellipsometry combined with transmittance measurements.

We found that in the spectrum of extinction coefficient there are absorption bands, which are assigned as the n-π* and π-π* electronic transitions of the azo compound.     

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.     

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.     

Structure of N,N′-bis[3-(aminocarbonyl)propyl]sulfamide

The title compound, C₈H₁₈N₄O₄S, possesses C₂ symmetry, with the S atom lying on a twofold rotational axis in the unit cell. The sulfamide group of each molecule forms four identical hydrogen bonds with those of its four neighboring molecules, resulting in a rhombic two-dimensional hydrogen bonded network. This network assembles in the third dimension via hydrogen bonds between the primary amide groups of the substituents that extend from the 2D sulfamide sheets. The primary amide groups form a hydrogen-bonded eight-membered cyclic dimer around a two-fold rotational axis. These cyclic dimers are linked into a ribbon-like network via hydrogen bonding interaction between the trans-H and the carbonyl of the amide groups. The compound crystallizes in C2/ca with a = 8.6162(1), b = 57716(1), c = 24.8344(b) Å, = 96.298(1)°, D _calc = 1.441 g cm^–3, and Z = 4.     

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.     

Crystallographic analysis of Royline monohydrate [C25H41NO7 · H2O]

The crystal and molecular structures of the alkaloid Royline {(1α,6β,14α, 16β)-20-ethyl-4-hydroxymethyl)-1,6,14,16-tetramethoxyaconitane-7,8-diol} with a water molecule has been determined by X-ray diffraction analysis. The compound crystallizes in the space group P2₁ with the unit cell parameters a = 10.985(1) Å, b = 7.898(1) Å, c = 14.956(1) Å, β = 102.96(1)°, V = 1264.52 ų, Z = 2, λMoK _α = 0.71073 Å, and R = 0.033 for 2067 observed reflections. Rings A, B, and C adopt a chair conformation, ring D is a half-boat, ring E is a half-chair, and ring F is in an envelope conformation with C(14) at the flap. Molecules are linked together in the crystal by hydrogen bonds.     

[100]金刚石薄膜的辐照响应特性研究

采用热丝辅助化学气相沉积(HFCVD)方法生长得到25μm厚的[100]取向金刚石膜,用以制备辐射探测器.在100 V偏压下,测得暗电流为16.1 nA,55Fe X射线(5.9 keV)和241Am α粒子(5.5 MeV)辐照下的净光电流分别为15.9nA和7.0nA.光电流随时间的变化先快速增加随后由于"pumping"效应逐渐达到稳定.X射线和α粒子辐照下的平均电荷收集效率分别为45;和19;,并由Hecht理论计算得到对应的电荷收集距离为11.25μm和4.75μm.     

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.     

Molecular structure of [trans-FeCl2(imidazole)4]Cl·THF·H2O

The structure of [trans-FeCl₂(imidazole)₄]Cl has been determined as the THF/H₂O solvate. The Fe-Cl and Fe-N distances in the cation are shorter than analogous trans-FeCl₂(L)₄ compounds, concomitant with the decreased ionic radius of Fe³⁺ versus Fe²⁺. Crystal data: orthorhombic, Pnma, a = 8.456(2), b = 20.991(4), c = 13.288(3) Å, V = 2358.6(8), andZ = 4.     

Crystal and Molecular Structure Studies of 1′-Benzyl-8-(4-fluorobenzyl)-8-azaspiro[bicyclo-[3.2.1]octane-3,4′-imidazolodine]-2′,5′-dione

Abstract  

The title compound, C₂₃H₂₃FN₃O₂ has been synthesized and the structure was investigated by X-ray diffraction studies. The compound crystallizes in the triclinic crystal class in the space group P[`1]P\overline{1} with cell parameters a = 9.345(2) ?, b = 10.940(3) ?, c = 11.986(4) ?, α = 72.349(6)°, β = 68.106(18)°, γ = 66.867(5)°, Z = 2 and V = 1027.8(5) ?³. The hydantoin ring adopts a planar conformation and is affected by the π conjugation. The pyrrolidine and piperidine rings in the bicyclo octane moiety adopt envelope and chair conformations respectively. The structure exhibits both inter and intramolecular hydrogen bonds of the type N–H···O, C–H···O and C–H···N. One of the oxygen atoms attached to the hydantoin ring simultaneously accepts two hydrogen bonds to form a three centered hydrogen bonding pattern.