Synthesis, crystal structure and Hirshfeld surface analysis of the tetrakis complex NaNdPyr4(i-PrOH)2 · i-PrOH with a carbacylamidophosphate of the amide type
The tetrakis complex of neodymium(III), tetrakis{ μ -N-[bis(pyrrolidin-1-yl)phosphoryl]acetamidato}bis(propan-2-ol)neodymiumsodium propan-2-ol monosolvate, [NaNd(C10H16Cl3N3O2)4(C3H8O)2] · C3H8O or NaNdPyr4(i-PrOH)2 · i-PrOH, with the amide type CAPh ligand bis(N,N-tetramethylene)(trichloroacetyl)phosphoric acid triamide (HPyr), has been synthesized, crystallized and characterized by X-ray diffraction. The complex does not have the tetrakis(CAPh)lanthanide anion, which is typical for ester-type CAPh-based coordination compounds. Instead, the NdO8 polyhedron is formed by one oxygen atom of a 2-propanol molecule and seven...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: Kariaka, N.S. Dyakonenko, V.V. Znovjyak, K.O. Shishkina, S.V. Amirkhanov, V.M. Tags: crystal structure carbacylamidophosphate neodymium tetrakis-complex research communications Source Type: research
Synthesis, crystal structure and computational analysis of 2,7-bis(4-chlorophenyl)-3,3-dimethyl-1,4-diazepan-5-one
In the title compound, C19H20Cl2N2O, the seven-membered 1,4-diazepane ring adopts a chair conformation while the 4-chlorophenyl substituents adopt equatorial orientations. The chlorophenyl ring at position 7 is disordered over two positions [site occupancies 0.480 (16):0.520 (16)]. The dihedral angle between the two benzene rings is 63.0 (4) ° . The methyl groups at position 3 have an axial and an equatorial orientation. The compound exists as a dimer exhibiting intermolecular N — H...O hydrogen bonding with R22(8) graph-set motifs. The crystal structure is further stabilized by C — H...O hydrogen bonds to...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: Akila, S. Vidhyasagar, T. Winfred Jebaraj, J.P. Thiruvalluvar, A.A. Rajeswari, K. Tags: synthesis X-ray crystal structure — H...O and N H...O hydrogen bonds Cl... π (ring) interactions 1,4-diazepane derivative chair conformation DFT Hirshfeld surface analysis 3ERT protein molecular docking research communicatio Source Type: research
Synthesis and redetermination of the crystal structure of NbF5
Single crystals of NbF5, niobium(V) fluoride, have been obtained by the reaction of niobium metal in a stream of dilute elemental fluorine at 473 K and subsequent sublimation. The as-obtained bulk phase compound was shown to be pure by powder X-ray diffraction at 293 K and by IR and Raman spectroscopy. A single-crystal X-ray analysis was conducted at 100 K. In comparison to the previously reported structure model [Edwards (1964). J. Chem. Soc. pp. 3714 – 3718], the lattice parameters and fractional atom coordinates were determined to much higher precision and individual, anisotropic displacement parameters we...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: M ö bs, M. Kraus, F. Tags: crystal structure redetermination niobium(V) fluoride synthesis powder X-ray diffraction research communications Source Type: research
An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and its methyl- and n-octyl-functionalized derivatives
The molecular and crystal structure of a discrete [Ni8( μ 4-OH)6( μ -4-Rpz)12]2 − (R = H; pz = pyrazolate anion, C3H3N2 − ) cluster with an unprecedented, perfectly cubic arrangement of its eight Ni centers is reported, along with its lower-symmetry alkyl-functionalized (R = methyl and n-octyl) derivatives. Crystals of the latter two were obtained with two identical counter-ions (Bu4N+), whereas the crystal of the complex with the parent pyrazole ligand has one Me4N+ and one Bu4N+ counter-ion. The methyl derivative incorporates 1,2-dichloroethane solvent molecules in its crystal structure, whereas the other two are s...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: Al Isawi, W.A. Zeller, M. Mezei, G. Tags: crystal structure nickel pyrazolate complex octanuclear core research communications Source Type: research
Crystal structure and antimycobacterial evaluation of 2-(cyclohexylmethyl)-7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-one
The title compound, C15H15F3N2O3S, crystallizes in the monoclinic system, space group I2/a, with Z = 8. As expected, the nine-membered heterobicyclic system is virtually planar and the cyclohexyl group adopts a chair conformation. There is structural evidence for intramolecular N — S...O chalcogen bonding between the benzisothiazolinone S atom and one O atom of the nitro group, approximately aligned along the extension of the covalent N — S bond [N — S...O = 162.7 (1) ° ]. In the crystal, the molecules form centrosymmetric dimers through C — H...O weak hydrogen bonding between a C — H group of the electron-d...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: Richter, A. Goddard, R. Imming, P. Seidel, R.W. Tags: benzisothiazolinone benzothiazinone mycobacteria hydrogen bonding crystal structure research communications Source Type: research
Synthesis, crystal structure and Hirshfeld surface analysis of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine
A novel o-phenylenediamine (opda)-based cadmium complex, bis(benzene-1,2-diamine- κ 2N,N ′ )bis(benzene-1,2-diamine- κ N)cadmium(II) naphthalene-1,5-disulfonate, [Cd(C6H8N2)4](C10H6O6S2), was synthesized. The complex salt crystallizes in the monoclinic space group C2/c. The Cd atom occupies a special position and coordinates six nitrogen atoms from four o-phenylenediamine molecules, two as chelating ligands and two as monodentate ligands. The amino H atoms of opda interact with two O atoms of the naphthalene-1,5-disulfonate anions. The anions act as bridges between [Cd(opda)4]2+ cations, forming a two-dimensional netwo...
Source: Acta Crystallographica Section E - November 30, 2023 Category: Chemistry Authors: Suyunov, J. Torambetov, B. Turaev, K. Kadirova, S. Alimnazarov, B. Ashurov, J. Tags: crystal structure cadmium complex o-phenylenediamine naphthalene-1,5-disulfonate Hirshfeld surface analysis research communications Source Type: research
Crystal structure, Hirshfeld surface analysis, intermolecular interaction energies, energy frameworks and DFT calculations of 4-amino-1-(prop-2-yn-1-yl)pyrimidin-2(1H)-one
In the title molecule, C7H7N3O, the pyrimidine ring is essentially planar, with the propynyl group rotated out of this plane by 15.31 (4) ° . In the crystal, a tri-periodic network is formed by N — H...O, N — H...N and C — H...O hydrogen-bonding and slipped π – π stacking interactions, leading to narrow channels extending parallel to the c axis. Hirshfeld surface analysis of the crystal structure reveals that the most important contributions for the crystal packing are from H...H (36.2%), H...C/C...H (20.9%), H...O/O...H (17.8%) and H...N/N...H (12.2%) interactions, showing that hydrogen-bonding and van der ...
Source: Acta Crystallographica Section E - November 21, 2023 Category: Chemistry Authors: Lahyaoui, M. Haoudi, A. Kartah, B.E. Mazzah, A. H ö kelek, T. Mague, J.T. Kandri Rodi, Y. Sebbar, N.K. Tags: crystal structure amino group hydrogen bonding heterocyclic compound research communications Source Type: research
Synthesis, structure and Hirshfeld surface analysis of 1,3-bis[(1-octyl-1H-1,2,3-triazol-4-yl)methyl]-1H-benzo[d]imidazol-2(3H)-one
The title molecule, C29H44N8O, adopts a conformation resembling a two-bladed fan with the octyl chains largely in fully extended conformations. In the crystal, C — H...O hydrogen bonds form chains of molecules extending along the b-axis direction, which are linked by weak C — H...N hydrogen bonds and C — H... π interactions to generate a three-dimensional network. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H...H (68.3%), H...N/N...H (15.7%) and H...C/C...H (10.4%) interactions. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - November 21, 2023 Category: Chemistry Authors: Zouhair, M. El Ghayati, L. El Monfalouti, H. Abchihi, H. H ö kelek, T. Ahmed, M. Mague, J.T. Sebbar, N.K. Tags: crystal structure benzimidazolone triazole — H... π (ring) interaction hydrogen bond research communications Source Type: research
Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
Reaction of FeCl2 · 4H2O with KSCN and 3-cyanopyridine (pyridine-3-carbonitrile) in ethanol accidentally leads to the formation of single crystals of Fe(NCS)(Cl)(3-cyanopyridine)4 or [FeCl(NCS)(C6H4N2)4]. The asymmetric unit of this compound consists of one FeII cation, one chloride and one thiocyanate anion that are located on a fourfold rotation axis as well as of one 3-cyanopyridine coligand in a general position. The FeII cations are sixfold coordinated by one chloride anion and one terminally N-bonding thiocyanate anion in trans-positions and four 3-cyanopyridine coligands that coordinate via the pyridine N atom to t...
Source: Acta Crystallographica Section E - November 21, 2023 Category: Chemistry Authors: M ü ller-Meinhard, A. Jess, I. N ä ther, C. Tags: synthesis crystal structure mixed iron thiocyanate chloride complex powder diffraction thermal properties research communications Source Type: research
Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato- κ 2N2,S)palladium(II) ethanol monosolvate
The reaction between the (R,S)-fixolide 4-methylthiosemicarbazone and PdII chloride yielded the title compound, [Pd(C20H30N3S)2] · C2H6O {common name: trans-bis[(R,S)-fixolide 4-methylthiosemicarbazonato- κ 2N2S]palladium(II) ethanol monosolvate}. The asymmetric unit of the title compound consists of one bis-thiosemicarbazonato PdII complex and one ethanol solvent molecule. The thiosemicarbazononato ligands act as metal chelators with a trans configuration in a distorted square-planar geometry. A C — H...S intramolecular interaction, with graph-set motif S(6), is observed and the coordination sphere resembles a hydroge...
Source: Acta Crystallographica Section E - November 16, 2023 Category: Chemistry Authors: Melo, A.P.L. de Bresolin, L. Tirloni, B. Farias, R.L. de Oliveira, A.B. de Tags: palladium(II) thiosemicarbazone-complex fixolide 4-methylthiosemicarbazone Hirshfeld surface analysis anagostic interaction hydrogen-bonded macrocyclic environment hydrogen-bonded ribbons crystal structure research communications Source Type: research
Crystal structures of the isotypic complexes bis(morpholine)gold(I) chloride and bis(morpholine)gold(I) bromide
The compounds bis(morpholine- κ N)gold(I) chloride, [Au(C4H9NO)2]Cl, 1, and bis(morpholine- κ N)gold(I) bromide, [Au(C4H9NO)2]Br, 2, crystallize isotypically in space group C2/c with Z = 4. The gold atoms, which are axially positioned at the morpholine rings, lie on inversion centres (so that the N — Au — N coordination is exactly linear) and the halide anions on twofold axes. The residues are connected by a classical hydrogen bond N — H...halide and by a short gold...halide contact to form a layer structure parallel to the bc plane. The morpholine oxygen atom is not involved in classical hydrogen bonding. (Source:...
Source: Acta Crystallographica Section E - November 16, 2023 Category: Chemistry Authors: D ö ring, C. Jones, P.G. Tags: crystal structure gold morpholine secondary interactions research communications Source Type: research
Synthesis and crystal structures of two related Co and Mn complexes: a celebration of collaboration between the universities of Dakar and Southampton
This article therefore also showcases this productive partnership, in celebration of the IUCr's 75 year anniversary and the recent inclusion of AfCA as a Regional Associate of the IUCr. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - November 16, 2023 Category: Chemistry Authors: Orton, J.B. Diouf, N. Gueye, R.S. Gaye, M. Thiam, I.E. Coles, S.J. Tags: Africa – UK collaboration AfCA IUCr Virtual Collection manganese complex cobalt complex structural chemistry crystal structure research communications Source Type: research
Crystal structure reinvestigation and spectroscopic analysis of tricadmium orthophosphate
Single crystals of tricadmium orthophosphate, Cd3(PO4)2, have been synthesized successfully by the hydrothermal route, while its powder form was obtained by a solid-solid process. The corresponding crystal structure was determined using X-ray diffraction data in the monoclinic space group P21/n. The crystal structure consists of Cd2O8 or Cd2O10 dimers linked together by PO4 tetrahedra through sharing vertices or edges. Scanning electron microscopy (SEM) was used to investigate the morphology and to confirm the chemical composition of the synthesized powder. Infrared analysis corroborates the presence of isolated phosphate ...
Source: Acta Crystallographica Section E - November 14, 2023 Category: Chemistry Authors: Cherif, F.-Z. Taibi, M. Boukhari, A. Assani, A. Saadi, M. El Ammari, L. Tags: crystal structure cadmium phosphate orthophosphates infrared spectroscopy research communications Source Type: research
Crystal structure of polymeric bis(3-amino-1H-pyrazole)cadmium dibromide
The reaction of cadmium bromide tetrahydrate with 3-aminopyrazole (3-apz) in ethanolic solution leads to tautomerization of the ligand and the formation of crystals of the title compound, catena-poly[[dibromidocadmium(II)]-bis( μ -3-amino-1H-pyrazole)- κ 2N3:N2; κ 2N2:N3], [CdBr2(C3H5N3)2]n or [CdBr2(3-apz)2]n. Its asymmetric unit consists of a half of a Cd2+ cation, a bromide anion and a 3-apz molecule. The Cd2+ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN4Br2 octahedra, which are linked into chains by pairs of the bridging ligands. In the crystal, the ligand molecules and b...
Source: Acta Crystallographica Section E - November 14, 2023 Category: Chemistry Authors: Kuzevanova, I.S. Vynohradov, O.S. Pavlenko, V.A. Malinkin, S.O. Shova, S. Fritsky, I.O. Seredyuk, M. Tags: crystal structure cadmium complex coordination polymer hydrogen bonding research communications Source Type: research
Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-one
The title compound, C5H5NO2, is a hydroxylated pyridine ring that has been studied for its involvement in microbial degradation of nicotinic acid. Here we describe its synthesis as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - November 14, 2023 Category: Chemistry Authors: Phillips, S.K. Brancato, S.G. MacMillan, S.N. Snider, M.J. Roering, A.J. Hicks, K.A. Tags: crystal structure hydrogen bonding nicotinic acid derivative research communications Source Type: research
