scholarly journals Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K

2015 ◽  
Vol 71 (10) ◽  
pp. 1203-1206
Author(s):  
Elena A. Buvaylo ◽  
Olga Yu. Vassilyeva ◽  
Brian W. Skelton
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Room Temperature ◽  
Complex Molecule ◽  
Water Molecules ◽  
Temperature Structure ◽  
Hydroxymethyl Group ◽  
Oh Groups ◽  
Small Contraction ◽  
Lower Temperature

The crystal structure of the tetranuclear title compound, [Cu4(C12H15NO5)4(H2O)4], has been previously reported by Back, Oliveira, Canabarro & Iglesias [Z. Anorg. Allg. Chem.(2015),641, 941–947], based on room-temperature data. In the previously published structure, no standard uncertainties are recorded for the deprotonated hydroxymethyl group and water molecule O atoms coordinating to the metal atom indicating that they were not refined; furthermore, the H atoms of some OH groups and water molecules have not been positioned accurately. Since the current structure was determined at a lower temperature, all atoms, including the H atoms of these hydroxy groups and the water molecule, have been determined more accurately resulting in improved standard uncertainties in the bond lengths and angles. Diffraction data were collected at 200 K, rather than the more usual 100 K, due to apparent disordering at lower temperatures. In addition, it is now possible to report intra- and intermolecular O—H...O interactions. In the title complex molecule, which has crystallographic -4 symmetry, the CuIIions are coordinated by the tridentate Schiff base ligands and water molecules, forming a tetranuclear Cu4O4cubane-like core. The CuIIion adopts a CuNO5elongated octahedral environment. The coordination environment of CuIIat 200 K displays a small contraction of the Cu—N/O bonds, compared with the room-temperature structure. In the crystal lattice, the neutral clusters are linked by intermolecular O—H...O hydrogen bonds into a one-dimensional hydrogen-bonding network propagating along thebaxis.

scholarly journals Crystal structure of aqua(1H-pyrazole-κN2)(pyridine-2,6-dicarboxylato-κ3O2,N,O6)copper(II) dihydrate

2017 ◽  
Vol 73 (12) ◽  
pp. 1875-1877
Author(s):  
Daeyoung Kim ◽  
Sung Kwon Kang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Layer Structure ◽  
Complex Molecule ◽  
Water Ligand ◽  
Water Molecules ◽  
Apical Position ◽  
Pyramidal Geometry ◽  
Square Pyramidal Geometry

In the title compound, [Cu(C7H3NO4)(C3H4N2)(H2O)]·2H2O, the CuIIatom is coordinated by three O atoms and two N atoms, provided by a tridentate pyridine-2,6-dicarboxylate (pdc), one pyrazole and one water ligand, forming a slightly distorted square-pyramidal geometry [range of O—Cu—O and O—Cu—N bond angles = 79.55 (8)–166.22 (10)°]. The water molecule is positioned at the apical position. In the crystal, the complex molecule and the two crystallographically independent non-coordinating water molecules are linked into a supramolecular layer structure parallel to theabplaneviaO—H...O and N—H...O hydrogen bonds.

scholarly journals Crystal structure of bis(2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)manganese(IV) 0.39-hydrate

2015 ◽  
Vol 71 (11) ◽  
pp. 1307-1310 ◽  
Author(s):  
Elena A. Buvaylo ◽  
Olga Yu. Vassilyeva ◽  
Brian W. Skelton
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Title Compound ◽  
Room Temperature ◽  
Cell Parameter ◽  
Temperature Data ◽  
Temperature Structure ◽  
Coordination Environment ◽  
Manganese Ion ◽  
Central Manganese

The title compound, [Mn(C12H15NO5)2]·0.39H2O, is a 0.39 hydrate of the isostructural complex bis(2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)manganese(IV) that has previously been reported by Back, Oliveira, Canabarro & Iglesias [Z. Anorg. Allg. Chem.(2015),641, 941–947], based on room-temperature data. The current structure that was determined at 100 K reveals a lengthening of theccell parameter compared with the published one due to the incorporation of the partial occupancy water molecule. The title compound crystallizes in the tetragonal chiral space groupP41212; the neutral [MnIV(C12H15NO5)2] molecule is situated on a crystallographicC2axis. The overall geometry about the central manganese ion is octahedral with an N2O4core; each ligand acts as a meridional ONO donor. The coordination environment of MnIVat 100 K displays a difference in one of the two Mn–O bond lengths, compared with the room-temperature structure. In the crystal, the neutral molecules are stacked in a helical fashion along thec-axis direction.

scholarly journals Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2′-bipyridine-κ2 N,N′)(oxalato-κ2 O 1,O 2)nickel(II)

2014 ◽  
Vol 70 (5) ◽  
pp. 477-481 ◽  
Author(s):  
Nela Farkašová ◽  
Juraj Černák ◽  
Milagros Tomás ◽  
Larry R. Falvello
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Room Temperature ◽  
Complex Molecule ◽  
Ethanol Solution ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Extended System ◽  
Complex Molecules ◽  
Solvent Water

The reaction of NiCl2, K2C2O4·H2O and 2,2′-bipyridine (bpy) in water–ethanol solution at 281 K yields light-purple needles of the new pentahydrate of bis(2,2′-bipyridine)oxalatonickel(II), [Ni(C2O4)(C10H8N2)2]·5H2O or [Ni(ox)(bpy)2]·5H2O, while at room temperature, deep-pink prisms of the previously reported tetrahydrate [Ni(ox)(bpy)2]·4H2O [Román, Luque, Guzmán-Miralles & Beitia (1995), Polyhedron, 14, 2863–2869] were gathered. The asymmetric unit in the crystal structure of the new pentahydrate incorporates the discrete molecular complex [Ni(ox)(bpy)2] and five solvent water molecules. Within the complex molecule, all three ligands are bonded as chelates. The complex molecules are involved in an extended system of hydrogen bonds with the solvent water molecules. Additionally, π–π interactions also contribute to the stabilization of the extended structure. The dehydration of the pentahydrate starts at 323 K and proceeds in at least two steps as determined by thermal analysis.

scholarly journals Crystal structure of the new hybrid material bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate

2015 ◽  
Vol 71 (11) ◽  
pp. 1384-1387
Author(s):  
Marwen Chouri ◽  
Habib Boughzala
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Molar Ratio ◽  
Water Molecules ◽  
Site Symmetry ◽  
Two Dimensional ◽  
Slow Evaporation ◽  
Solution Ph

The title compound bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate, (C6H14N2)2[Bi2Cl10]·2H2O, was obtained by slow evaporation at room temperature of a hydrochloric aqueous solution (pH = 1) containing bismuth(III) nitrate and 1,4-diazabicyclo[2.2.2]octane (DABCO) in a 1:2 molar ratio. The structure displays a two-dimensional arrangement parallel to (100) of isolated [Bi2Cl10]4−bioctahedra (site symmetry -1) separated by layers of organic 1,4-diazoniabicyclo[2.2.2]octane dications [(DABCOH2)2+] and water molecules. O—H...Cl, N—H...O and N—H...Cl hydrogen bonds lead to additional cohesion of the structure.

scholarly journals Crystal structure of 2,6-bis(3-hydroxy-3-methylbut-1-yn-1-yl)pyridine monohydrate

2020 ◽  
Vol 76 (11) ◽  
pp. 1737-1740
Author(s):  
Take-aki Koizumi ◽  
Toshikazu Takata
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Pyridine Ring ◽  
Pyridine Molecule ◽  
Pyridine Derivative ◽  
Oh Groups

In the title pyridine derivative, C15H17NO2·H2O, the two OH groups are oriented in directions opposite to each other with respect to the plane of the pyridine ring. In the crystal, hydrogen bonds between the pyridine molecule and the water molecule, viz. Ohydroxy—H...Owater, Ohydroxy—H...Ohydroxy, Owater—H...Ohydroxy and Owater—H···Npyridine, result in the formation of a ribbon-like structure running along [011].

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.

Crystal Structure of Calcium Picrate Pentahydrate: A New Eight-Coordinate Stereochemistry for [M(bidentate)2(unidentate)4]

1979 ◽  
Vol 32 (2) ◽  
pp. 301 ◽  
Author(s):  
V Diakiw ◽  
TW Hambley ◽  
DL Kepert ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Title Compound ◽  
Lattice Site ◽  
The Other ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triangular Face ◽  
X Ray

The crystal structure of the title compound, Ca(C6H2N307)2,5H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.049 for 1513 'observed' reflections. Crystals are orthorhombic, Pmab, a 24.169(6), b l0.292(7), c 8.554(2) �, Z 4. The stereochemistry about the calcium has not been observed previously for the system [M(bidentate)2- (unidentate)4]; in the present structure, the calcium is coordinated by a pair of bidentate picrate ligands and the four water molecules in an array in which three of the water molecules occupy a triangular face of a square antiprism, the overall array having m symmetry. The remaining water molecule occupies a lattice site with no close interaction with the other species.

Synthesis, crystal structure, and vibrational spectra of the complex maleic acid•2H2O•18-crown-6

1990 ◽  
Vol 68 (12) ◽  
pp. 2183-2189 ◽  
Author(s):  
Pierre Audet ◽  
Rodrigue Savoie ◽  
Michel Simard
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Maleic Acid ◽  
Water Molecules ◽  
Infrared And Raman Spectra ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
O 18 ◽  
Stoichiometric Complex

A stoichiometric complex of formula maleic acid•2H2O•18-crown-6 has been obtained from maleic acid and the macrocyclic polyether 18-crown-6. Crystals of this complex have been shown by X-ray diffraction crystallography to belong to the Cc space group of the monoclinic system. The acid molecules in the adduct are linked to each other through a water molecule, giving infinite [-acid-H2O-]n chains. They are also linked to the crown ether via water molecules. The infrared and Raman spectra of the complex are presented and compared to those of crystalline maleic acid. Keywords: maleic acid/18-crown-6, structure, X-ray, spectra.

Crystal Structures of Piperazinium Tetrabromocadmate(II)-Monohydrate [C4H12N2]CdBr4 · H2O, PiperaziniumTetraiodocadmate(II) [C4H12N2]CdI4, and Bis(trimethylsulphonium) Tetrabromocadmate(II) [(CH3)3S]2CdBr4

2002 ◽  
Vol 57 (5) ◽  
pp. 503-508 ◽  
Author(s):  
Hideta Ishihara ◽  
Keizo Horiuchi ◽  
Thorsten M. Gesing ◽  
Shi-qi Dou ◽  
J.-Christian Buhl ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Room Temperature ◽  
Water Molecules ◽  
Temperature Phase

Piperazinium tetrabromocadmate(II)-monohydrate, [C4H12N2]CdBr4 · H2O (1) crystallizes with isolated [CdBr4]2- anions, piperazinium cations, and water molecules (monoclinic, P21/c, Z = 4, a = 698.7(1), b = 1348.6(3), and c = 1432.4(3) pm, β = 92.97(3)˚ at 293 K). The crystal structure of 1 is almost the same as that reported in Inorg. Chim. Acta 187, 141 (1991). The crystal of piperazinium tetraiodocadmate(II), [C4H14N2]CdI4 (2) consists of isolated [CdI4]2- anions and piperazinium cations (orthorhombic,P212121, Z=4, a = 903.2(5), b = 1226.3(6), and c = 1307.9(7) pm at 293 K). The room temperature phase of bis(trimethylsulphonium) tetrabromocadmate( II), [(CH3)3S]2CdBr4 (3) has isolated [CdBr4]2- anions and trimethylsulphonium cations (orthorhombic, P212121, Z = 4, a = 911.3(1), b = 1329.2(2), and c = 1454.7(2) pm at 293 K).

Komplexe mit substituierten 2,5-Dihydroxy-p-benzochinonen: EA[C6(NO2)2O4] · H2O (EA = Ca, Sr)/ Complexes with Substituted 2,5-D ihydroxy-p-benzoquinones: EA [C6(NO2)2O4] · 4H2O(EA = Ca, Sr)

1987 ◽  
Vol 42 (8) ◽  
pp. 972-976 ◽  
Author(s):  
Christian Robl
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Single Crystals ◽  
Coordination Sphere ◽  
Trigonal Prism ◽  
Water Molecules ◽  
Additional Water ◽  
Oxygen Atoms

AbstractSingle crystals of EA[Q(NO2)2O4] · 4H2O (EA = Ca. Sr) were grown in aqueous silicagel. Ca2+ has CN 8. It is surrounded by 4 oxygen atoms of two bis-chelating [C6(NO2)2O4]2- ions and 4 water molecules, which form a distorted, bi-capped trigonal prism. Sr2+ is coordinated similarly, with an additional water molecule joining the coordination sphere to yield CN 8+1. Corrugated chains extending along [010] and consisting of EA2+ and nitranilate ions are the main feature of the crystal structure. Adjacent chains are interlinked by hydrogen bonds.

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