Journal of Chemical Crystallography最新文献

Recrystallization of [Zn(malt)₂(H₂O)_1.5] (malt = maltolato(-1), C₆H₅O₃) from a concentrated aqueous solution acidified with HCl to pH 3.0 yielded colorless crystals of [Zn(Hmalt)₂Cl₂] (Hmalt = neutral maltol, C₆H₆O₃). The Zn(II) site exhibits distorted tetrahedral coordination through bonding to two chloride ligands and to two neutral maltol ligands, each bonding through the ketonic oxygen. [Zn(Hmalt)₂Cl₂] is a unique example of a neutral monodentate coordination by the maltol ligand.

Graphical Abstract

A view of the tetrahedral [Zn(Hmalt)₂Cl₂] (Hmalt = neutral maltol, C₆H₆O₃).

A novel Co(II) complex [Co₄(HL)₂Phen₂(H₂O)₁₀]·20(H₂O) (HL = 5-(Bis-carboxymethyl-amino)-isophthalic acid; Phen = 1,10-Phenanthroline) was synthesized by hydrothermal methods, and its crystal structure was determined by single-crystal X-ray diffraction. The title complex crystallized in the monoclinic space group C2/c as an isolated tetranuclear structure. The strong π···π stacking, hydrogen bonding and van de Waals attractions produce 3D supramolecular structure. A series of properties of the title complex were tested by solid-state photoluminescence, CIE analysis and solid-state diffuse reflectance. The results show that the title complex is blue light emitter, CIE (0.2172, 0.5581) and has an energy bandwidth of 2.33 eV.

Graphical Abstract

A novel monoclinic space group C2/c complex of [Co₄(L)₂Phen₂(H₂O)₁₀]·20(H₂O) (HL = 5-(Bis-carboxymethyl-amino)-isophthalic acid; Phen = 1,10-Phenanthroline) was synthesized by hydrothermal methods, and a series of properties of the complex were tested by solid-state photoluminescence, CIE analysis and solid-state diffuse reflectance, which results show that the title complex is blue light emitter, CIE (0.2172, 0.5581) and has an energy bandwidth of 2.33 eV.

One quaternary selenidoantimonate of [Mn(en)₃]CdSb₂Se₅ (1) (en = ethylenediamine) was prepared under 1,2-propanediamine condition by mild solvothermal method. Single-crystal X-ray diffraction analysis reveals that compound 1 crystallizes in the monoclinic space group C2/c. Its structure consists of infinite 1D [CdSb₂Se₅]_n²ⁿ⁻ anionic chains and [Mn(en)₃]²⁺ cations. Meanwhile, “Z” shaped eight-membered [Cd₂Sb₂Se₄] and six-membered [CdSb₂Se₃] rings are alternately found. As estimated from UV–Vis absorption spectrum, the band gap of 1 is 2.58 eV. Compound 1 also showed rapid response and excellent reproducibility based on photoelectric test. In addition, the magnetic and other properties of 1 were studied.

Graphical Abstract

The manuscript describes the synthesis, crystal structure, single-crystal X-ray diffraction, elemental analysis, photoelectric response, thermogravimetric analysis, magnetic properties, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy of [Mn(en)₃]CdSb₂Se₅. The photoelectric response of compound 1 was explored, and a highly repetitive and stable photocurrent curve was found, indicating that 1 is a typical p-type semiconductor. In addition, the magnetism of compound 1 was also studied, which showed that 1 had antiferromagnetic behavior.

The crystal structures of C₂₃H₃₀O₆·C₂H₅OH and C₂₃H₃₀O₆·C₃H₇OH were determined by X-ray diffraction analysis at temperatures 100 K (space group P2₁, Z = 2): a = 9.6973(4), b = 7.4950(3), c = 16.1828(7) Å, β = 93.559(4)°, R = 0.0698 (C₂₃H₃₀O₆·C₂H₅OH); a = 9.8941(3), b = 7.3833(2), c = 16.5816(5) Å, β = 90.110(3)°, R = 0.0318 (C₂₃H₃₀O₆·C₃H₇OH). The method molecular Voronoi–Dirichlet polyhedra were also used to analyze non-bonded interactions in the structures of solvate crystals. The analysis showed that the studied solvates are isostructural. There is a slight increase in the fraction of intermolecular H/H contacts for isopropanol solvate.

Graphical Abstract

The crystal structures of C₂₃H₃₀O₆·C₂H₅OH and C₂₃H₃₀O₆·C₃H₇OH were determined by X-ray diffraction analysis at temperatures 100 K and the method molecular Voronoi–Dirichlet polyhedra were also used to analyze non-bonded interactions in the structures.

Arrangement of molecules in the unit cell of solvates of cortisone acetate (a—ethanol solvate; b—isopropanol solvate).

One Ni(II)-Na(I) complex namely {[Ni^II-L-Na^I(dca)]₂}_n [H₂L = 1,2-ethanediylbis(2-iminomethylene-6-methoxy-phenol)] was synthesized under mild conditions at room temperature and characterized by elemental analysis, infrared spectroscopy, X-ray diffraction and thermogravimetric analysis. Single crystal X-ray diffraction analyses show that Ni(II) centers are in four-coordinate D_4h geometry and Na(I) centers are in a six-coordinate slightly distorted pentagonal pyramidal C_5v geometry in the complex. The basic structural components of the complex are the [Ni^II-L-Na^I] units, which are further connected by the dicyanamide through μ_1,5 mode between the Na centers to form 1D chain structures. Thermogravimetric analysis indicate that complex 1 shows good thermal stability.

Graphical Abstract

In this paper, we report the crystal and molecular structure of two compounds obtained from the reactions between the ligand 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine (TpymT) with Pd(II) and Pt(II) [M(Cl₂(CH₃CN)₂] complexes. The ligand hydrolyses into the anion N-[(pyrimidine)carbonyl]pyrimidine-2-carboxamidato (bpcam⁻), giving compounds with the formula [Pd(bpcam)Cl]·H₂O, 1, and [Pt(bpcam)Cl]·DMSO, 2. Compounds 1 and 2 crystallize in the monoclinic crystal system with C2/c and P2₁/n space groups. The compounds are square planar, with the bpcam⁻ acting as a tridentate-κ³N anionic ligand and the Cl⁻ anion in the fourth position. In both complexes, the molecules stack in columns presenting interactions between the aromatic rings, reinforced in 2 by Pt···Pt interactions. The complexes interact with the solvent molecules through H-bonds building a 3D structure. We analyzed the systems through geometric parameters and Hirshfeld surface studies. The energy frameworks indicate that the main interactions between molecules in the crystal are dispersion forces.

Graphical Abstract

The paper presents the X-ray structures of [M(bpcam)Cl]·where bdcam- is the anion N-[(pyrimidine)carbonyl]pyrimidine-2-carboxamidato and M = Pd(II) and Pt(II), as well as Hirshfeld Surface and Energy Framework studies.

Two novel taxoids were synthesized from 1-deoxybacctin VI (1) and their crystal structures were determined by X-ray crystallographic techniques. The influence of the 11,12-olefin of the tetracyclic moiety on molecular conformations were investigated. Comparison to other baccatin analogs, a larger effect on the conformation of the diterpenoid core is observed when the 11,12-olefin is reducted. Conformational analysis show that the reduction of the 11,12-olefin has a decisive influence on the conformation of the A and B ring. Compounds 3 and 5 crystallize in orthorhombic system, space group P2₁2₁2₁. In the structure of compound 3, the six-membered A ring exhibits the 1,3-diplanar boat conformation, the eight-membered B ring adopts a boat–chair conformation, and the six-membered C ring exhibits a slightly distorted half-chair conformation. However, in 11,12-dihydro-taxoids 5, the six-membered A ring exhibits a chair conformation and the conformation of the eightmembered B ring has a large distortion.

Graphical Abstract

The synthesis of novel 11,12-dihydro-taxoids from 1-deoxybacctin VI are presented, in which the crystal structure of the compound 5 was characterized.

Five years after we published the synthesis of the first diamidocarbene (DAC)-supported amino borylene 4, we now report the elusive single crystal X-ray structure. The X-ray structure of 4 was found to corroborate our previous computational studies which indicated that the borylene adopted a heterocumulenic geometry with a near linear C_(carbene) = B = N unit (175.88(18)^◦) as well as short C = B and B = N distances of 1.416(3) and 1.344(3) Å, respectively. Additionally, we further provide a qualitative and quantitative discourse on said structure with respect to the precursor compounds used to prepare 4 as well as to the known cyclic (alkyl) amino carbene (CAAC) analog 2.