scholarly journals Monoclinic polymorph of chlorido(dimethyl sulfoxide-κO)triphenyltin(IV)

2018 ◽  
Vol 74 (2) ◽  
pp. 163-166 ◽  
Author(s):  
Serigne Fallou Pouye ◽  
Ibrahima Cissé ◽  
Libasse Diop ◽  
Francisco Javier Ríos-Merino ◽  
Sylvain Bernès
Keyword(s):  
Dimethyl Sulfoxide ◽  
Dmso Molecule ◽  
Relative Orientation ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Phenyl Rings ◽  
Orthorhombic Cell ◽  
Long Time ◽  
Monoclinic Cell

The crystal structure of the title tin complex, [Sn(C6H5)3Cl(C2H6OS)], (I), has been reported with one molecule in the asymmetric unit in an orthorhombic cell [Kumar et al. (2009). Acta Cryst. E65, m1602–m1603]. While using SnPh3Cl as a starting material for a reaction for which the products were recrystallized over a very long time (six months) from dimethyl sulfoxide (DMSO), a new polymorph was obtained for (I), with two independent molecules in the asymmetric unit of a monoclinic cell. The coordination geometry of the Sn centres remains unchanged, with the Cl− ion and the DMSO molecule in the apical positions and the phenyl C atoms in the equatorial positions of a trigonal bipyramid. The main difference between the polymorphs is the relative orientation of the phenyl rings in the equatorial plane, reflecting a degree of free rotation of these groups about their Sn—C bonds. In the crystal, molecules are linked into [010] chains mediated by weak C—H...O interactions.

scholarly journals Crystal structure of μ-oxalato-κ2O1:O2-bis[(dimethyl sulfoxide-κO)triphenyltin(IV)]

2017 ◽  
Vol 73 (7) ◽  
pp. 1033-1036
Author(s):  
Serigne Fallou Pouye ◽  
Ibrahima Cisse ◽  
Libasse Diop ◽  
Alessandro Dolmella ◽  
Sylvain Bernès
Keyword(s):  
Dimethyl Sulfoxide ◽  
Reaction Medium ◽  
Dmso Molecule ◽  
Title Complex ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
Disordered System ◽  
Group Type ◽  
Trigonal Bipyramidal ◽  
Phenyl Rings

In the previously reported [C2O4(SnPh3)2] complex [Diopet al.(2003).Appl. Organomet. Chem.17, 881–882.], the SnIVatoms are able to formally complete their coordination by addition of dimethyl sulfoxide (DMSO) molecules provided by the reaction medium, affording the title complex, [Sn2(C6H5)6(C2O4)(C2H6OS)2]. The SnIVatoms are then pentacoordinated, with a commontranstrigonal–bipyramidal arrangement. The asymmetric unit contains one half-molecule, which is completed by inversion symmetry in space group typeC2/c. The inversion centre is placed at the mid-point of the central bis-monodentate oxalate dianion, C2O42−, which bridges the [(SnPh3)(DMSO)] moieties. The molecule crystallizes as a disordered system, with two phenyl rings disordered by rotation about their Sn—C bonds, while the DMSO molecule is split over two positions due to a tetrahedral inversion at the S atom. All disordered parts were refined with occupancies fixed of 0.5.

scholarly journals Bis(μ2-4-nitrophenolato)bis(4-nitrophenolato)di-μ3-oxido-octaphenyltetratin chloroform sesquisolvate [+ solvate]: a tetranuclear stannoxane

IUCrData ◽  
2019 ◽  
Vol 4 (8) ◽  
Author(s):  
Patrick Butler
Keyword(s):  
Hydrogen Bonds ◽  
Electron Density ◽  
Three Dimensional ◽  
The Other ◽  
Dimensional Structure ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Complex Molecules ◽  
Three Dimensional Structure

The title tetranuclear stannoxane, [Sn4(C6H5)8(C6H4NO3)4O2]·1.5CHCl3·solvent, crystallized with two independent complex molecules, A and B, in the asymmetric unit together with 1.5 molecules of chloroform. There is also a region of disordered electron density, which was corrected for using the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18]. The oxo-tin core of each complex is in a planar `ladder' arrangement and each Sn atom is fivefold SnO3C2 coordinated, with one tin centre having an almost perfect square-pyramidal coordination geometry, while the other three Sn centres have distorted shapes. In the crystal, the complex molecules are arranged in layers, composed of A or B complexes, lying parallel to the bc plane. The complex molecules are linked by a number of C—H...O hydrogen bonds within the layers and between the layers, forming a supramolecular three-dimensional structure.

scholarly journals Diosgenin hemihydrate

2012 ◽  
Vol 68 (8) ◽  
pp. o2357-o2357 ◽  
Author(s):  
María-Guadalupe Hernández Linares ◽  
Sylvain Bernès ◽  
Marcos Flores-Alamo ◽  
Gabriel Guerrero-Luna ◽  
Anselmo A. Martínez-Gallegos
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Dimethyl Sulfoxide ◽  
Starting Material ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
X Ray ◽  
Hydroxy Groups ◽  
Hydrogen Bonded

Diosgenin [or (22R,25R)-spirost-5-en-3β-ol] is the starting material of the Marker degradation, a cheap semi-synthesis of progesterone, which has been designated as an International Historic Chemical Landmark. Thus far, a single X-ray structure for diosgenin is known, namely its dimethyl sulfoxide solvate [Zhanget al.(2005).Acta Cryst.E61, o2324–o2325]. We have now determined the structure of the hemihydrate, C27H42O3·0.5H2O. The asymmetric unit contains two diosgenin molecules, with quite similar conformations, and one water molecule. Hydroxy groups in steroids and water molecules form O—H...O hydrogen-bondedR54(10) ring motifs. Fused edge-sharingR(10) rings form a backbone oriented along [100], which aggregates the diosgenin molecules in the crystal structure.

scholarly journals Dichlorido[1,1-(diphenylphosphino)hydrazide]palladium(II) dichloromethane monosolvate

IUCrData ◽  
2018 ◽  
Vol 4 (1) ◽  
Author(s):  
Martha Höhne ◽  
Bhaskar R. Aluri ◽  
Anke Spannenberg ◽  
Bernd H. Müller ◽  
Normen Peulecke ◽  
...  
Keyword(s):  
Diffraction Data ◽  
Title Compound ◽  
Complex Molecule ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Square Planar ◽  
Solvent Molecules

In the title compound, [PdCl2(C24H22N2P2)]·CH2Cl2, the palladium(II) atom is surrounded by a chelating P—N—P ligand Ph2P—N(NH2)—PPh2 containing a hydrazine entity and two chlorido ligands in a distorted square-planar coordination geometry. Beside the complex molecule, the asymmetric unit contains a co-crystallized dichloromethane molecule. The contributions of further disordered solvent molecules were removed from the diffraction data using the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] procedure.

scholarly journals Ethyl 6-amino-5-cyano-4-phenyl-2,4-dihydropyrano[2,3-c]pyrazole-3-carboxylate dimethyl sulfoxide monosolvate

2014 ◽  
Vol 70 (7) ◽  
pp. o795-o796 ◽  
Author(s):  
Naresh Sharma ◽  
Goutam Brahmachari ◽  
Bubun Banerjee ◽  
Rajni Kant ◽  
Vivek K. Gupta
Keyword(s):  
Dimethyl Sulfoxide ◽  
The Other ◽  
Dihedral Angles ◽  
Boat Conformation ◽  
Asymmetric Unit ◽  
Pyran Ring ◽  
Compound C ◽  
Phenyl Rings ◽  
The Mean ◽  
Solvent Molecules

In the asymmetric unit of the title compound, C16H14N4O3·C2H6OS, there are two independent main molecules (AandB) and two dimethyl sulfoxide solvent molecules. In moleculeA, the pyran ring is in a flattened sofa conformation, with thesp3-hydridized C atom forming the flap. In moleculeB, the pyran ring is in a flattened boat conformation, with thesp3-hydridized C atom and the O atom deviating by 0.073 (3) and 0.055 (3) Å, respectively, from the plane of the other four atoms. The mean planes the pyrazole and phenyl rings form dihedral angles of 84.4 (2) and 84.9 (2)°, respectively, for moleculesAandB. In the crystal, N—H...O and N—H...N hydrogen bonds link the components of the structure into chains along [010]. In both solvent molecules, the S atoms are disordered over two sites, with occupancy ratios of 0.679 (4):0.321 (4) and 0.546 (6):0.454 (6).

scholarly journals Crystal structure ofcis,fac-{N,N-bis[(pyridin-2-yl)methyl]methylamine-κ3N,N′,N′′}dichlorido(dimethyl sulfoxide-κS)ruthenium(II)

2015 ◽  
Vol 71 (9) ◽  
pp. m169-m170
Author(s):  
Kasey Trotter ◽  
Navamoney Arulsamy ◽  
Elliott Hulley
Keyword(s):  
Dimethyl Sulfoxide ◽  
Complex Molecule ◽  
Title Complex ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
The Mean ◽  
Chloride Ligands

The reaction of dichloridotetrakis(dimethyl sulfoxide)ruthenium(II) withN,N-bis[(pyridin-2-yl)methyl]methylamine affords the title complex, [RuCl2(C13H15N3)(C2H6OS)]. The asymmetric unit contains a well-ordered complex molecule. TheN,N-bis[(pyridin-2-yl)methyl]methylamine (bpma) ligand binds the cation through its two pyridyl N atoms and one aliphatic N atom in a facial manner. The coordination sphere of the low-spind6RuIIis distorted octahedral. The dimethyl sulfoxide (dmso) ligand coordinates to the cation through its S atom and iscisto the aliphatic N atom. The two chloride ligands occupy the remaining sites. The bpma ligand is folded with the dihedral angle between the mean planes passing through its two pyridine rings being 64.55 (8)°. The two N—Ru—N bite angles of the ligand at 81.70 (7) and 82.34 (8)° illustrate the distorted octahedral coordination geometry of the RuIIcation. Two neighboring molecules are weakly associated through mutual intermolecular hydrogen bonding involving the O atom and one of the methyl groups of the dmso ligand. One of the chloride ligands is also weakly hydrogen bonded to a pyridyl H atom of another molecule.

scholarly journals Triphenyltelluronium(IV) bromide acetone hemisolvate

2013 ◽  
Vol 69 (11) ◽  
pp. o1666-o1666 ◽  
Author(s):  
Sari M. Närhi ◽  
Raija Oilunkaniemi ◽  
Risto S. Laitinen
Keyword(s):  
Title Compound ◽  
Solvent Molecule ◽  
Site Occupancy ◽  
The Other ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Phenyl Rings ◽  
Coordination Spheres ◽  
Secondary Bonding

The asymmetric unit of the title compound, 2C18H15Te+·2Br−·C3H6O or Ph3TeBr·0.5Me2CO, contains two crystallographically independent triphenyltelluronium cations, two bromide anions, and one disordered [site-occupancy ratio = 0.581 (7):0.419 (7)] solvent molecule. Interionic Te...Br interactions connect the cations and anions into a tetrameric step-like structure. The primary coordination spheres of both Te atoms are TeC3trigonal pyramids: three short secondary tellurium–bromine interactions expand the coordination geometry of one of the Te atoms to an octahedron. While the other Te atom shows only two Te...Br secondary bonding interactions, it is also six-coordinated due to a Te...π interaction [3.769 (2) Å] with one of the phenyl rings of the adjacent cation.

scholarly journals Tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-nitrophenolato)tetracopper(II)

2014 ◽  
Vol 70 (2) ◽  
pp. m54-m55
Author(s):  
Eduard N. Chygorin ◽  
Yuri O. Smal ◽  
Vladimir N. Kokozay ◽  
Irina V. Omelchenko
Keyword(s):  
Hydrogen Bond ◽  
Metal Ion ◽  
Reaction System ◽  
Symmetry Element ◽  
Coordination Geometry ◽  
Chemical Formula ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Solvent Molecules ◽  
The Given

The title cluster, [Cu4(C11H12N2O6)4], was obtained from the Cu0–FeCl2·4H2O–H4L–Et3N–DMF reaction system (in air), where H4Lis 2-hydroxymethyl-2{[(2-hydroxy-3-nitrophenyl)methylidene]amino}propane-1,3-diol and DMF is dimethylformamide. The asymmetric unit consists of one Cu2+ion and one dianionic ligand; a -4 symmetry element generates the cluster, which contains a {Cu4O4} cubane-like core. The metal ion has an elongated square-based pyramidal CuNO4coordination geometry with the N atom in a basal site. An intramolecular O—H...O hydrogen bond is observed. The solvent molecules were found to be highly disordered and their contribution to the scattering was removed with the SQUEEZE procedure inPLATON[Spek (2009).Acta Cryst. D65, 148–155], which indicated a solvent cavity of volume 3131 Å3containing approximately 749 electrons. These solvent molecules are not considered in the given chemical formula.

Tris(dimethylphenylphosphine)ruthenium(0) Complexes of n4-Coordinated Polycyclic Aromatic Hydrocarbons

2000 ◽  
Vol 53 (6) ◽  
pp. 507 ◽  
Author(s):  
Martin A. Bennett ◽  
Mark Bown ◽  
David C. R. Hockless
Keyword(s):  
Coordination Geometry ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Polycyclic Aromatic ◽  
R Value ◽  
Axial Site

From the reaction of [Ru2Cl3(PMe2Ph)6] Cl with the appropriate radical anions, yellow complexes of general formula [Ru(PMe2Ph)3(η4-arene)] [arene = naphthalene (C10H8) (1), anthracene (C14H10) (2), and triphenylene (C18H12) (3)] have been isolated in poor yield and characterized by elemental analysis, n.m.r. (1H, 13C, 31P) spectroscopy and single-crystal X-ray diffraction. Crystal data: (1), monoclinic, C2/c, a 31.096(8), b 12.012(4), c 17.078(8) Å, β 104.41(3)˚, V 6178(4) Å3, ? 8, refined to final R value of 0.032 with use of 3641 reflections [I > 3σ(I)]; (2), monoclinic, C2/c, a 55.909(4), b 14.348(5), c 17.573(5) Å, β 105.41(1)˚, V 13590(6) Å3, Z 16 (two molecules per asymmetric unit), refined to final R value of 0.049 with use of 7770 reflections [I > 3σ(I)]; (3), mono-clinic, Pn, a 9.377(3), b 12.229(3), c 15.975(3) Å, β 103.51(2)˚, V 1781.2 (7) Å3, Z 2, refined to final R value of 0.026 with use of 2830 reflections [I > 3σ(I)]. In each case, coordination of the zerovalent metal fragment Ru(PMe2Ph)3 to the diene section of one of the terminal rings causes the aromatic molecule to be folded by c. 40˚ at the outer carbon atoms of the diene. The coordination geometry about ruthenium is approximately square pyramidal, with the diene and two tertiary phosphines in the equatorial plane and the remaining tertiary phosphine in the axial site.

scholarly journals Crystal structure of a new monoclinic polymorph ofN-(4-methylphenyl)-3-nitropyridin-2-amine

2014 ◽  
Vol 70 (8) ◽  
pp. 58-61
Author(s):  
Aina Mardia Akhmad Aznan ◽  
Zanariah Abdullah ◽  
Vannajan Sanghiran Lee ◽  
Edward R. T. Tiekink
Keyword(s):  
Three Dimensional ◽  
Basis Set ◽  
Dihedral Angles ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Common Features ◽  
Compound C ◽  
B3lyp Level ◽  
The Common ◽  
Independent Molecules

The title compound, C12H11N3O2, is a second monoclinic polymorph (P21, withZ′ = 4) of the previously reported monoclinic (P21/c, withZ′ = 2) form [Akhmad Aznanet al.(2010).Acta Cryst.E66, o2400]. Four independent molecules comprise the asymmetric unit, which have the common features of asyndisposition of the pyridine N atom and the toluene ring, and an intramolecular amine–nitro N—H...O hydrogen bond. The differences between molecules relate to the dihedral angles between the rings which range from 2.92 (19) to 26.24 (19)°. The geometry-optimized structure [B3LYP level of theory and 6–311 g+(d,p) basis set] has the same features except that the entire molecule is planar. In the crystal, the three-dimensional architecture is consolidated by a combination of C—H...O, C—H...π, nitro-N—O...π and π–π interactions [inter-centroid distances = 3.649 (2)–3.916 (2) Å].

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