scholarly journals Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate)

2021 ◽  
Vol 77 (10) ◽  
Author(s):  
Sergey Shapovalov ◽  
Olga Tikhonova ◽  
Ivan Skabitsky
Keyword(s):  
Transition Metal Complexes ◽  
Diethyl Ether ◽  
Solvent Molecule ◽  
Palladium Complexes ◽  
Acta Cryst ◽  
Bond Lengths ◽  
Free Model ◽  
The Given ◽  
Ether Molecule

The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate, [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O or [Pd(IMe)4][Re4(CO)16]·2C4H10O, (1), and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium, [Pd4Re2(C18H15P)4(CO)10] or Pd4Re2(PPh3)4(μ-CO)8(CO)2, (2), from the reaction of Pd(PPh3)4 with 1,3-dimethylimidazolium-2-carboxylate and Re2(CO)10 in a toluene–acetonitrile mixture. In complex 1 the Re—Re bond lengths [2.9767 (3)–3.0133 (2) Å] are close to double the covalent Re radii (1.51 Å). The palladium–rhenium carbonyl cluster 2 has not been structurally characterized previously; the Pd—Re bond lengths [2.7582 (2)–2.7796 (2) Å] are about 0.1 Å shorter than the sum of the covalent Pd and Re radii (1.39 + 1.51 = 2.90 Å). One carbene ligand and a diethyl ether molecule are disordered over two positions with occupancy ratios of 0.5:0.5 and 0.625 (15):0.375 (15) in 1. An unidentified solvent is present in compound 2. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s). The SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18] in PLATON was used to remove the contribution of the electron density in the solvent region from the intensity data and the solvent-free model was employed for the final refinement. The cavity with a volume of ca 311 Å3 contains approximately 98 electrons.

scholarly journals Crystal structure of (diethyl ether-κO)[5,10,15,20-tetrakis(2-isothiocyanatophenyl)porphyrinato-κ4 N]zinc diethyl ether solvate

2018 ◽  
Vol 74 (11) ◽  
pp. 1609-1612 ◽  
Author(s):  
Lisa Leben ◽  
Eike Schaub ◽  
Christian Näther ◽  
Rainer Herges
Keyword(s):  
Crystal Structure ◽  
Diethyl Ether ◽  
Metal Cation ◽  
Title Compound ◽  
Rotation Axis ◽  
Solvent Molecule ◽  
Apical Position ◽  
Picket Fence ◽  
Ether Molecule ◽  
Porphyrin Moiety

The crystal structure of the title compound, [Zn(C48H24N8S4)(C4H10O)]·C4H10O, consists of discrete porphyrin complexes that are located on a twofold rotation axis. The ZnII cation is fivefold coordinated by four N atoms of the porphyrin moiety and one O atom of a diethyl ether molecule in a slightly distorted square-pyramidal environment with the diethyl ether molecule in the apical position. The porphyrin backbone is nearly planar with the metal cation slightly shifted out of the plane towards the coordinating diethyl ether molecule. All four isothiocyanato groups of the phenyl substituents at the meso-positions face the same side of the porphyrin, as is characteristic for picket fence porphyrins. In the crystal structure, the discrete porphyrin complexes are arranged in such a way that cavities are formed in which additional diethyl ether solvate molecules are located around a twofold rotation axis. The O atom of the solvent molecule is not positioned exactly on the twofold rotation axis, thus making the whole molecule equally disordered over two symmetry-related positions.

scholarly journals Crystal structure of bis[cis-diaquabis(phenanthroline)cobalt(II)] bis(citrato)germanate(IV) dinitrate

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Olha Buchko ◽  
Viktoriya Dyakonenko ◽  
Elena Martsinko ◽  
Elena Chebanenko
Keyword(s):  
Crystal Structure ◽  
Solvent Molecule ◽  
Crystal Data ◽  
Chemical Formula ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Water Oxygen ◽  
Solvent Molecules ◽  
The Given ◽  
Oxygen Atoms

The asymmetric unit of the title compound, [Co(C12H8N2)2(H2O)2]2[Ge(C6H5O7)2](NO3)2, features two complex [(C12H8N2)2(H2O)2Co]2+ cations, two NO3 − anions as well as one centrosymmetric [(C6H5O7)2Ge]2− anion. Two HCit ligands (Cit = citrate, C6H4O7) each coordinate via three different oxygen atoms (hydroxylate, α-carboxylate, β-carboxylate) to the Ge atom, forming a slightly distorted octahedron. The coordination polyhedron of the Co atom is also octahedral, formed by coordination of four nitrogen atoms from two phenanthroline molecules and two water oxygen atoms. In the crystal, the cations and anions are linked by hydrogen bonds and form layers parallel to the bc plane. The structure exhibits disorder of the NO3 − anion [disorder ratio 0.688 (9) to 0.312 (9)]. There are also highly disordered solvent molecules (presumably water and/or ethanol) in the crystal structure; explicit refinement of these molecules was not possible, and the content of the voids was instead taken into account using reverse Fourier transform methods [SQUEEZE procedure in PLATON; Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Bis(μ-2-hydroxymethyl-2-methylpropane-1,3-diolato)bis[dichloridotitanium(IV)] diethyl ether disolvate

2013 ◽  
Vol 69 (12) ◽  
pp. m676-m677
Author(s):  
Alastair J. Nielson ◽  
Chaohong Shen ◽  
Joyce M. Waters
Keyword(s):  
Bond Length ◽  
Diethyl Ether ◽  
Solvent Molecule ◽  
Octahedral Geometry ◽  
Title Complex ◽  
Distorted Octahedral Geometry ◽  
Tripodal Ligand ◽  
Oh Groups ◽  
Bond Lengths ◽  
Distorted Octahedral

The title complex, [Ti2Cl4{CH3C(CH2O)2(CH2OH)}2], lies across a centre of symmetry with a diethyl ether solvent molecule hydrogen bonded to the –CH2OH groups on either side of it. The TiIVatom is coordinated in a distorted octahedral geometry by a tripodal ligand and two terminal chloride atoms. There are three coordination modes for the tripodal ligand distinguishable on the basis of their very different Ti—O bond lengths. For the terminal alkoxo ligand, the Ti—O distance is 1.760 (1) Å, the asymmetric bridge system has Ti—O bond lengths of 1.911 (1) and 2.048 (1) Å. The Ti—O bond length for the alcohol O atom is the longest at 2.148 (1) Å.

scholarly journals Crystal structure of (20S)-21-[4-(2-hydroxypropan-2-yl)-1H-1,2,3-triazol-4-yl]-20-(4-methylpentyl)-5-pregnen-3β-ol with an unknown solvate

2018 ◽  
Vol 74 (4) ◽  
pp. 465-468
Author(s):  
Hugo Santalla ◽  
Saray Argibay
Keyword(s):  
Crystal Structure ◽  
Solvent Molecule ◽  
Hydroxyl Group ◽  
Crystal Data ◽  
Chemical Formula ◽  
Isopropyl Group ◽  
Terminal Position ◽  
Acta Cryst ◽  
The Given ◽  
Tertiary Hydroxyl

In the title cholesterol analogue, [systematic name: (3S,8S,9S,10R,13S,14S,17R)-17-{(S)-1-[4-(2-hydroxypropan-2-yl)-1H-1,2,3-triazol-1-yl]-6-methylheptan-2-yl}-10,13-dimethyl-2,3,4,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-3-ol] C32H53N3O2, a new chain, including an intermediate triazole and a tertiary hydroxyl group in the terminal position, has been added at position 20 inducing a change in its stereochemistry. In the crystal, molecules are linked by O—H...O and O—H...N hydrogen bonds, forming layers lying parallel to (-201) and enclosing R 4 4(36) ring motifs. The isopropyl group is disordered about two positions with a refined occupancy ratio of 0.763 (5):0.237 (5). A region of disordered electron density was corrected for using the SQUEEZE routine in PLATON (Spek (2015). Acta Cryst. C71, 9–18). The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Tetracarbonyl[N-(diphenylphosphanyl-κP)-N,N′-diisopropyl-P-phenylphosphorus diamide-κP]molybdenum(0) with an unknown solvent

IUCrData ◽  
2018 ◽  
Vol 3 (6) ◽  
Author(s):  
Martha Höhne ◽  
Marc Gongoll ◽  
Anke Spannenberg ◽  
Bernd H. Müller ◽  
Normen Peulecke ◽  
...  
Keyword(s):  
Solvent Molecule ◽  
Coordination Geometry ◽  
Crystal Data ◽  
Chemical Formula ◽  
Acta Cryst ◽  
Carbonyl Ligands ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Solvent Molecules ◽  
The Given

The title complex, [Mo(C24H30N2P2)(CO)4], contains a molybdenum centre bearing a P,P′-cis-chelating Ph2PN( i Pr)P(Ph)NH( i Pr) and four carbonyl ligands in a distorted octahedral coordination geometry. This results in a nearly planar four-membered metallacycle. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds to form layers parallel to the ac plane. For the final refinement, the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Crystal structure of an unknown solvate of bis(tetra-n-butylammonium) [N,N′-(4-trifluoromethyl-1,2-phenylene)bis(oxamato)-κ4O,N,N′,O′]nickelate(II)

2015 ◽  
Vol 71 (6) ◽  
pp. 578-581
Author(s):  
François Eya'ane Meva ◽  
Dieter Schaarschmidt ◽  
Tobias Rüffer
Keyword(s):  
Rotation Axis ◽  
Point Group ◽  
Solvent Molecule ◽  
Three Dimensional ◽  
Group Symmetry ◽  
Acta Cryst ◽  
Coordination Environment ◽  
Dimensional Network ◽  
Square Planar ◽  
The Given

In the title compound, [N(C4H9)4]2[Ni(C11H3F3N2O6)] or [N(n-Bu)4]2[Ni(topbo)] [n-Bu =n-butyl and topbo = 4-trifluoromethyl-1,2-phenylenebis(oxamate)], the Ni2+cation is coordinated by two deprotonated amido N atoms and two carboxylate O atoms, setting up a slightly distorted square-planar coordination environment. The [Ni(topbo]2−anion lies on a twofold rotation axis. Due to an incompatibility with the point-group symmetry of the complete molecule, orientational disorder of the CF3group is observed. The tetrahedral ammonium cations and the anion are linked by weak intermolecular C—H...O and C—H...F hydrogen-bonding interactions into a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s). The given chemical formula and other crystal data do not take into account the unknown solvent molecule.

scholarly journals Crystal structure of ethyl 3-amino-6-methyl-2-[(4-methylphenyl)carbamoyl]-4-[(E)-2-phenylethenyl]thieno[2,3-b]pyridine-5-carboxylate monohydrate

2016 ◽  
Vol 72 (3) ◽  
pp. 297-299 ◽  
Author(s):  
Joel T. Mague ◽  
Mehmet Akkurt ◽  
Shaaban K. Mohamed ◽  
Etify A. Bakhite ◽  
Mustafa R. Albayati
Keyword(s):  
Hydrogen Bonds ◽  
Dihedral Angle ◽  
Phenyl Ring ◽  
Pyridine Ring ◽  
Solvent Molecule ◽  
Crystal Data ◽  
Chemical Formula ◽  
Acta Cryst ◽  
Title Molecule ◽  
The Given

In the title molecule, C27H25N3O3S·H2O, the dihedral angle between the planes of the thienyl ring and the pendantp-tolyl group is 39.25 (6)°, while that between the pyridine ring and the pendant phenyl ring is 44.37 (6)°. In addition, there is a slight twist in the bicyclic core, with a dihedral angle of 2.39 (4)° between the thienyl and pyridine rings. The conformation of the carbamoyl moiety is partially determined by an intramolecular N—H...O hydrogen bond. In the crystal, complementary N—H...O hydrogen bonds form dimers which are then associated into chains parallel to thecaxis through O—H...N hydrogen bonds involving the water molecule of crystallization. Electron density associated with an additional solvent molecule of partial occupancy and disordered about a twofold axis was removed with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst.C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Construction of a supramolecule comprising [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) and (5,10,15,20-tetraphenylporphyrinato)zinc(II)

IUCrData ◽  
2018 ◽  
Vol 3 (12) ◽  
Author(s):  
Masatomo Makino ◽  
Kazuhiko Matsubayashi ◽  
Yukiko Kodama-Oda ◽  
Naoto Imawaka ◽  
Nobuhiro Mizuno ◽  
...  
Keyword(s):  
Self Assembly ◽  
Solvent Molecule ◽  
Phenyl Group ◽  
Van Der Waals Interactions ◽  
Crystal Data ◽  
Chemical Formula ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Solvent Molecules ◽  
The Given

The supramolecular features in the title compound, [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) bis[(5,10,15,20-tetraphenylporphyrinato)zinc(II)] chloroform tetrasolvate, [Zn(C96H80N8O8)][Zn(C44H28N4)]2·4CHCl3 or [Zn(Pc)][Zn(TPP)]2·4CHCl3, result from a self-assembly of one molecule of [2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyaninato]zinc(II) (ZnPc) and two molecules of (5,10,15,20-tetraphenylporphyrinato)zinc(II) (ZnTPP). One half ZnPc, one ZnTPP and two chloroform molecules define the asymmetric unit, with the zinc(II) cation of ZnPc situated on an inversion centre. In the supramolecule, the central ZnPc moiety is sandwiched between two ZnTPPs moieties in a co-facial conformation with a π-conjugated system, leading to a nearly H-type aggregate with a distance of 3.4967 (5) Å between adjacent zinc sites. The ZnTPP units are slightly glided away to form a partial ecliptic arrangement. Each phenyl group of the TPP ligand is anchored above the N atom of the isoindole linker of the Pc ligand through weak C—H...N hydrogen bonds and is held into the crevice between the two dimethylphenoxy groups of phthalocyanine via van der Waals interactions. In the crystal, chloroform solvent molecules are situated between the supramolecules. There is another solvent-accessible void of 341 (2) Å3. The contribution of disordered solvent molecules situated in this void was removed from the diffraction data using SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not consider this unknown solvent molecule(s).

scholarly journals [6,6′-Bis(1,1-dimethylethyl)-4,4′-dimethyl-2,2′-methylenediphenolato-κ2O,O′]dichlorido(9H-fluoren-9-ol-κO)titanium(IV)–fluorene–diethyl ether (1/0.5/1)

2013 ◽  
Vol 69 (12) ◽  
pp. m673-m674
Author(s):  
Alastair J. Nielson ◽  
Chaohong Shen ◽  
Joyce M. Waters
Keyword(s):  
Hydroxy Group ◽  
Coordination Sphere ◽  
Diethyl Ether ◽  
Title Compound ◽  
Solvent Molecule ◽  
The Other ◽  
Chloride Ligands ◽  
Apical Site ◽  
Ether Molecule ◽  
Hydrogen Bonded

The title adduct, [TiCl2(C23H30O2)(C13H10O]·0.5C13H10·C4H10O, is a monomer with a trigonal–bypyramidal coordination sphere of the TiIVatom in which the ligand O atoms of the bidentate diphenolate anion are located in both apical and equatorial positions. Chloride ligands occupy the remaining two equatorial sites of the trigonal bypyramid with the fluoren-9-ol O atom occupying the other apical site. The hydroxy group H atom of this latter group is hydrogen bonded to an O atom of a non-coordinating diethyl ether molecule. The title compound also contains a further fluorene solvent molecule, which lies across a centre of symmetry and which is equally disordered over an inversion centre.

scholarly journals 13-Benzyl-4,11-dihydroxy-1,8-diphenyl-2,9-dithia-13-azadispiro[4.1.4.3]tetradecan-6-one

IUCrData ◽  
2021 ◽  
Vol 6 (2) ◽  
Author(s):  
G. Vinotha ◽  
T. V. Sundar ◽  
N. Sharmila
Keyword(s):  
Solvent Molecule ◽  
Chair Conformation ◽  
Piperidine Ring ◽  
Crystal Data ◽  
Chemical Formula ◽  
Acta Cryst ◽  
Compound C ◽  
Phenyl Rings ◽  
The Mean ◽  
The Given

In the title compound, C30H31NO3S2, the piperidine ring adopts a distorted chair conformation. The thiophene rings have twisted conformations about the C—C bonds. The mean plane of the piperidine ring makes a near orthogonal conformation with the toluene ring. Two of the phenyl rings in the structure are positionally disordered over two sets of sites with occupancies of 0.56 (2)/0.44 (2) and 0.672 (16)/0.328 (16). A region of disordered electron density was corrected for using the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] routine in PLATON. The given chemical formula and other crystal data do not take into account the unknown solvent molecule. In the crystal, O—H...O hydrogen bonds are observed along with intramolecular S...H, O...H, C...H and H...H contacts.

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