Unusual reaction of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol with triphenylborane: crystal structures and optical properties
The molecular and crystal structure of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol (C18H19N3O2S, Et2N-Bz) and its unexpected reaction product with triphenylborane, 2,2-diphenyl-1,3-dioxa-2-borata-1,2-dihydronaphthalene [systematic name: N,N-diethyl-2,2-diphenyl-2H-1,3 λ 3,2 λ 4-benzodioxaborinin-7-amine, C23H24BNO2, (I)] are described. For Et2N-Bz, the hydroxyl group is involved in an intramolecular hydrogen bond with the imino nitrogen atom and the C=N bond displays an E configuration. The crystal packing is characterized by layers of inversion dimers parallel to the (10\overline{1}) plane and chain...
Source: Acta Crystallographica Section E - October 3, 2023 Category: Chemistry Authors: Le Thi Hong, H. Le Phuong, T. Van Pham, T. Minh Thi Nguyen, H. Van Meervelt, L. Tags: crystal structure benzothiazole boranils fluorescence aggregation-induced emission research communications Source Type: research
Crystal structure of bis(3-carboxy-1-methylpyridinium) octabromide
The crystal structure of the title salt, bis(3-carboxy-1-methylpyridinium) octabromide, 2C7H8NO2+ · Br82 − , consists of 3-carboxy-1-methylpyridinium (N-methylnicotinic acid) cations, which are stacked between relatively rare [Br8]2 – anions. The polybromide [Br8]2 – anion has point group symmetry \overline{1} and can be described as being composed of two [Br3] − anions connected with a Br2 molecule in a Z-shaped manner. Contacts between neighboring octabromide anions ensure the creation of pseudo-polymeric chains propagating along [111]. The organic cations are located between anionic chains and are connected to ...
Source: Acta Crystallographica Section E - October 3, 2023 Category: Chemistry Authors: Sirenko, V.Y. Naumova, D.D. Golenya, I.A. Shova, S. Gural'skiy, I.A. Tags: crystal structure octabromide anion polyhalogen ions N-methylnicotinic acid research communications Source Type: research
Synthesis, crystal structure and reactivity of bis( μ -2-methylpyridine N-oxide- κ 2O:O)bis[dibromido(2-methylpyridine N-oxide- κ O)cobalt(II)] butanol monosolvate
Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2]2(2-methylpyridine N-oxide)4 · n-butanol or [Co2Br4(C6H7NO)4] · C4H10O. The asymmetric unit of the title compound consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions and one n-butanol molecule that is disordered around a center of inversion. The CoII cations are fivefold coordinated by two bromide anions and one terminal as well as two bridging 2-methylpyridine N-oxide and linked by two symmetry-related μ -1,1(O,O) 2-methylpyridine N-oxide...
Source: Acta Crystallographica Section E - October 3, 2023 Category: Chemistry Authors: N ä ther, C. Jess, I. Tags: crystal structure synthesis thermoanalytical investigations cobalt thiocyanate 2-methylpyridine N-oxide research communications Source Type: research
Synthesis, crystal structure, stereochemical and Hirshfeld surface analysis of trans-diaquabis(1-phenylpropane-1,2-diamine- κ 2N,N ′ )nickel(II) dichloride dihydrate
In the hydrated complex salt, [Ni(C9H14N2)2(H2O)2]Cl2 · 2H2O, the asymmetric unit comprises of half of the complex cation along with one chloride anion and one non-coordinating water molecule. The central nickel(II) atom is located on an inversion center and is coordinated in a trans octahedral fashion by four N atoms from two bidentate 1,2-diamino-1-phenylpropane ligands in the equatorial plane, and by two oxygen atoms from two water molecules occupying the axial sites. The five-membered chelate ring is in a slightly twisted envelope conformation. The crystal packing features O — H...Cl, N — H...O and N — H...Cl hy...
Source: Acta Crystallographica Section E - September 29, 2023 Category: Chemistry Authors: Akila, S. Vidhyasagar, T. Thiruvalluvar, A.A. Rajeswari, K. Tags: synthesis X-ray crystal structure NiII complex ethylenediamine metal complex vicinal diamine derivative DFT Hirshfeld surface analysis distorted octahedral complex trans-Ni complex. research communications Source Type: research
Crystal structure of bis{3-(3,4-dimethoxyphenyl)-5-[6-(pyrazol-1-yl)pyridin-2-yl]-1,2,4-triazol-3-ato}iron(II) – methanol – chloroform (1/2/2)
The unit cell of the title compound, [Fe(C18H15N6O2)2] · 2CH3OH · 2CHCl3, consists of a charge-neutral complex molecule, two methanol and two chloroform molecules. In the complex, the two tridentate 2-(5-(3,4-dimethoxyphenyl)-1,2,4-triazol-3-yl)-6-(pyrazol-1-yl)pyridine ligands coordinate to the central FeII ion through the N atoms of the pyrazole, pyridine and triazole groups, forming a pseudo-octahedral coordination sphere. Neighbouring tapered molecules are linked through weak C — H(pz)... π (ph) interactions into one-dimensional chains, which are joined into two-dimensional layers through weak C — H...N/C/O inte...
Source: Acta Crystallographica Section E - September 29, 2023 Category: Chemistry Authors: Znovjyak, K. Fritsky, I.O. Sliva, T.Y. Amirkhanov, V.M. Malinkin, S.O. Shova, S. Seredyuk, M. Tags: crystal structure iron(II) complexes neutral complexes research communications Source Type: research
Co-crystal sustained by π -type halogen-bonding interactions between 1,4-diiodoperchlorobenzene and naphthalene
The formation and crystal structure of a co-crystal based upon 1,4-diiodoperchlorobenzene (C6I2Cl4) as the halogen-bond donor along with naphthalene (nap) as the acceptor is reported. The co-crystal [systematic name: 1,2,4,5-tetrachloro-3,6-diiodobenzene – naphthalene, (C6I2Cl4) · (nap)] generates a chevron-like structure that is held together primarily by π -type halogen bonds (i.e. C — I... π contacts) between the components. In addition, C6I2Cl4 also interacts with the acceptor via C — Cl... π contacts that help stabilize the co-crystal. Within the solid, both aromatic components are found to engage in offset ...
Source: Acta Crystallographica Section E - September 29, 2023 Category: Chemistry Authors: Bosch, E. Reinheimer, E.W. Unruh, D.K. Groeneman, R.H. Tags: halogen bonding co-crystal Type I chlorine-chlorine contacts Type II iodine-chlorine contacts research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of cyclo-tetrabromido-1 κ 2Br,3 κ 2Br-tetrakis( μ 2-2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiolato- κ 3N,S:S)tetramercury(II)
The macrometallacyclic title compound, [Hg4Br4(C8H11N2S)4] or [((HgL2)(HgBr2))2] (1) where HL = 2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiol, was prepared and structurally characterized. The Hg2+ complex crystallizes in the P21/c space group. The centrosymmetric Hg4S4 metallacycle is constructed from metal ions with alternating distorted tetrahedral Br2S2 and distorted seesaw N2S2 primary coordination environments with pendant pyridyl groups. The backfolded extended chair metallacycle conformation suggests interactions between each of the bis-chelated mercury atoms and Br atoms lying above and below the central Hg2S4 plan...
Source: Acta Crystallographica Section E - September 29, 2023 Category: Chemistry Authors: Thomas, I.D. Kocher, K.R. Viehweg, J.A. Pike, R.D. Bebout, D.C. Tags: crystal structure Hirshfeld surface analysis metallacycle chelating N,S-ligands Hg2 complex research communications Source Type: research
Crystal structures of five compounds in the aluminium – ruthenium – silicon system
Single crystals of five compounds with approximate compositions ∼ Ru16(Al0.78Si0.22)47, (I), ∼ Ru9(Al0.70Si0.30)32, (II), ∼ Ru10(Al0.67Si0.33)41, (III), ∼ Ru(Al0.57Si0.43)5, (IV), and ∼ Ru2(Al0.46Si0.54)9, (V), were obtained from polycrystalline lumps mainly composed of the target compounds, and their crystal structures were determined by means of single-crystal X-ray diffraction. The crystal structure of (I) can be related to that of a cubic rational crystalline approximant to an icosahedral quasicrystal through crystallographic shear and then unit-cell twinning. The crystal structure of (II) is isotypic with th...
Source: Acta Crystallographica Section E - September 29, 2023 Category: Chemistry Authors: Kitahara, K. Takakura, H. Iwasaki, Y. Kimura, K. Tags: crystal structure aluminium – ruthenium silicon system single-crystal X-ray diffraction isotypism structural similarity crystallographic shear unit-cell twinning quasicrystal approximant research communications Source Type: research
Growth and characterization of a new inorganic metal – halide crystal structure, InPb2Cl5
A new solid-state inorganic compound, indium dilead pentachloride, InPb2Cl5, was synthesized by melting InCl and PbCl2 in a vacuum-sealed quartz ampoule. The ampoule was heated to 793 K and then slowly cooled to room temperature to induce crystallization of InPb2Cl5. InPb2Cl5 crystallizes in the monoclinic crystal system adopting a space group of type P21/c, which is isostructural with other metal halides such as RbPb2Cl5, KPb2Cl5 and TlPb2Cl5. The bulk InPb2Cl5 exhibits a metallic black/grey colour, allowing it to be separated from white/yellow PbCl2 crystals. Due to the incongruent nature of the compound, the pure bu...
Source: Acta Crystallographica Section E - September 26, 2023 Category: Chemistry Authors: Lewis, M.P. Kandel, R. Schatte, G. Wang, P.L. Tags: crystal structure inorganic InPb2Cl5 solid-state research communications Source Type: research
Racemic cis-bis[bis(pyrimidin-2-yl)amine- κ N]bis(dicyanamido- κ N1)iron(II) dihydrate: synthesis, crystal structure and Hirshfeld surface analysis
The title compound, [Fe(C2N3)2(C8H7N5)2] · 2H2O, has been synthesized solvothermally and characterized by single-crystal X-ray diffraction. The octahedral iron coordination polyhedron contains two di(pyrimidin-2-yl)amine ligands coordinated in a bidentate fashion, and two monodentate dicyanimido ligands, each coordinated via a terminal N atom, with the latter in a cis orientation. The ligand configuration about the iron atom is chiral, although the compound crystallizes as a racemic mixture: the Fe — N distances (> 2.07 Å ) are characteristic of high-spin iron(II). In the crystal, an extensive series of N — H...N...
Source: Acta Crystallographica Section E - September 26, 2023 Category: Chemistry Authors: Saadallah, Y. Setifi, Z. Jelsch, C. Setifi, F. Al-Douh, M.H. Satour, A. Glidewell, C. Tags: solvothermal synthesis iron complex dicyanamido ligands hydrogen bonding Hirshfeld surface analysis crystal structure research communications Source Type: research
Synthesis and crystal structure of bis(tert-butyl isocyanide- κ C)[5,10,15,20-tetrakis(4-chlorophenyl)porphyrinato- κ 4N]iron(II)
In the title compound, [FeII(C44H24Cl4N4)(C5H9N)2] or [FeII(TClPP)(t-BuNC)2] [where TClPP and t-BuNC are 5,10,15,20-tetrakis(4- chlorophenyl)porphyrinate and tert-butyl isocyanide ligands, respectively], the metal ion lies on an inversion center and is octahedrally coordinated by the N atoms of the porphyrin ring in the equatorial plane and by carbon atoms of the trans t-BuNC ligands in the axial sites. The Fe — N bond length of 2.0074 (14) Å suggests a low-spin complex (S = 0). The crystal packing of the title compound is sustained by C — H...Cl, C — H...N and C__H...Cg (Cg = the centroid of a pyrrole ring ...
Source: Acta Crystallographica Section E - September 26, 2023 Category: Chemistry Authors: Nasri, S. Tags: crystal structure Hirshfeld surface analysis iron(II) porphyrin complex tert butyl isocyanide research communications Source Type: research
Synthesis, crystal structure, and Hirshfeld surface analysis of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine
A key step towards utilizing polynuclear metal-based systems in magnetic device applications involves the careful design of ligands. This strategic planning aims to produce metal assemblies that exhibit some kind of `switch' mechanism. Towards this end, a ligand that incorporates a redox-active functional group (ferrocene) is reported. This communication presents the multi-step synthesis, characterization (1H and 13C NMR), and structural analysis (single-crystal X-ray diffraction and Hirshfeld surface analysis) of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine, [Fe(C5H5)(C13H11N4)]. Supramolecular features, including π ...
Source: Acta Crystallographica Section E - September 19, 2023 Category: Chemistry Authors: Joekar, D. Hiscock, L.K. Dawe, L.N. Tags: crystal structure aminopyrazole ferrocene Hirshfeld surface analysis research communications Source Type: research
Synthesis and crystal structure of silicon pernitride SiN2 at 140 GPa
Silicon pernitride, SiN2, was synthesized from the elements at 140 GPa in a laser-heated diamond anvil cell. Its crystal structure was solved and refined by means of synchrotron-based single-crystal X-ray diffraction data. The title compound crystallizes in the pyrite structure type (space group Pa\overline{3}, No. 205). The Si atom occupies a site with multiplicity 4 (Wyckoff letter b, site symmetry .\overline{3}.), while the N atom is located on a site with multiplicity 8 (Wyckoff letter c, site symmetry .3.). The crystal structure of SiN2 is comprised of slightly distorted [SiN6] octahedra interconnected with each o...
Source: Acta Crystallographica Section E - September 19, 2023 Category: Chemistry Authors: Jurzick, P.L. Krach, G. Br ü ning, L. Schnick, W. Bykov, M. Tags: nitrides pernitrides silicon nitrides high pressure crystal structure research communications Source Type: research
Crystal structure of a 1:1 co-crystal of quabodepistat (OPC-167832) with 2,5-dihydroxybenzoic acid using microcrystal electron diffraction
Quabodepistat [(5-{[(3R,4R)-1-(4-chloro-2,6-difluorophenyl)-3,4-dihydroxypiperidin-4-yl]methoxy}-8-fluoro-3,4-dihydroquinolin-2(1H)-one); C21H20ClF3N2O4] and 2,5-dihydroxybenzoic acid (2,5DHBA; C7H6O4) were successfully co-crystallized. Given the small size of the crystals (1 × 0.2 × 0.2 µ m) the structure was solved via microcrystal electron diffraction (MicroED). The C — O and C=O bond-length ratio of the carboxylic group in 2,5DHBA is 1.08 (1.34 Å /1.24 Å ), suggesting that 2,5DHBA remains protonated. Therefore, the material is a co-crystal rather than a salt. The amide group of quabodepistat particip...
Source: Acta Crystallographica Section E - September 19, 2023 Category: Chemistry Authors: Sakamoto, N. Gato, K. Tags: crystal structure co-crystal quabodepistat 2,5-dihydroxybenzoic acid microcrystal electron diffraction research communications Source Type: research
2,6-Dibromo-3,4,5-trimethoxybenzoic acid
The title compound, 2,6-dibromo-3,4,5-trimethoxybenzoic acid (DBrTMBA), C10H10Br2O5, was obtained by bromination and transhalogenation of 2-iodo-3,4,5-trimethoxybenzoic acid with KBrO3. Like the previously reported 2,6-diiodo-3,4,5-trimethoxybenzoic acid (DITMBA), the structure of the title compound features a catemeric arrangement of DBrTMBA molecules along an endless chain of carboxylic H – carbonyl interactions. A short carbonyl – phenyl contact hints at a possible lone pair(O) – π -hole interaction further stabilizing the chain-like structure over a dimeric arrangement of the carboxylic acid. (Source: Acta Cryst...
Source: Acta Crystallographica Section E - September 14, 2023 Category: Chemistry Authors: Meurer, F. Dimova, T. Bodensteiner, M. Kolev, I. Tags: crystal structure Hirshfeld atom refinement (HAR) NoSpherA2 substituted trimethoxybenzoic acid research communications Source Type: research
