Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XXX. Synthesis and X-Ray Structure of [Ru(dppm-P)(dppm-P,P')(η-C5H5)][PF6]0.5[PO2F2]0.5

1988 ◽  
Vol 41 (4) ◽  
pp. 597 ◽  
Author(s):  
MI Bruce ◽  
MP Cifuentes ◽  
KR Grundy ◽  
MJ Liddell ◽  
MR Snow ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Phenyl Group ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
One Pot ◽  
Full Matrix ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

An improved, one-pot synthesis is reported for the [Ru (dppm -P)(dppm -P, P′)(η-C5H5)]+ cation as its BF4- salt. The crystal structure of [Ru ( dppm - P)( dppm -P,P′)(η-C5H5)]+, obtained as the mixed PF6-/PO2F2- salt, has also been determined. There are few differences in dimensions between the mono- and bi-dentate dppm ligands; chelation sharply reduces the P-CH2-P angle, and one phenyl group on each phosphorus is bent away from the metal. Crystals are monoclinic, space group C2/c with unit cell dimensions a 21.743(3), b 23.594(3), c 21.352(3)Ǻ, β 110.17(1) and Z 8. The structure was refined by a full-matrix least-squares procedure to final R 0.078 and Rw 0.087 for 4490 reflections with I > 2.5σ(I).

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

Die Kristallstruktur von PPh4[MoOCl4(OCHNMe2)] / The Crystal Structure of PPh4[MoOCl4(OCHNMe2)]

1986 ◽  
Vol 41 (4) ◽  
pp. 523-526 ◽  
Author(s):  
Dieter Fenske ◽  
Kay Jansen ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Carbon Tetrachloride ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Dimethyl Formamide ◽  
Structural Investigations ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Ray Methods

Green crystals of the title compound are formed in the reaction of (PPh4)2 [Mo2(O2C -Ph)4Cl2] ·2 CH2Cl2 with dimethyl formamide/carbon tetrachloride in the presence of water. According to the structural investigations by X-ray methods PPh4[MoCl4(O CHNMe2)] crystallizes orthorhombically in the space group C2221 with four formula units per unit cell (3132 observed, independent reflexions, R - 0.068). The cell dimensions are a = 792.1 pm, b = 1656.8 pm, c = 2211.3 pm. The structure consists of PPh4⊕ cations and anions [MoOCl4(OCHNMe2)]⊖, in which the coordination sphere of the molybdenum atom is of distorted octahedral geometry. The ligands are four equatorial chlorine atoms, one terminal O atom (Mo = O 165 pm) and the O atom of the dimethyl formamide molecule (MoO 232 pm). The IR spectrum is reported

X-Ray structure of tris(acetonitrile)tricarbonylrhenium(I) tetrafluoroborate

1977 ◽  
Vol 55 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Lillian Y. Y. Chan ◽  
E. E. Isaacs ◽  
W. A. G. Graham
Keyword(s):  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
The Mean ◽  
Unit Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data

Reaction of [n-Bu4N]2[Re4(CO)16] with AgBF4 in acetonitrile affords the compound [(CH3CN)3Re(CO)3][BF4]. The latter crystallizes in monoclinic space group P21/c with unit cell dimensions a = 11.021(5) Å, b = 11.136(5) Å, c = 12.980(6) Å, β = 96.906(25)°, and four molecules per unit cell. Data were collected by counter methods and the structure was refined using least-squares procedures to give R = 0.041. The rhenium cation is approximately octahedrally coordinated by six facially arranged ligands. The mean rhenium–nitrogen distance is 2.13 Å, and the mean rhenium–nitrogen–carbon angle in the coordinated acetonitrile is 174.7°.

Syntheses, crystal structures, and characterization of two Mn(II) coordination polymers with bis(4-(1H-imidazol-1-yl)phenyl)methanone ligands

2016 ◽  
Vol 71 (8) ◽  
pp. 869-874 ◽  
Author(s):  
Gao-Feng Wang ◽  
Xiao Zhang ◽  
Shu-Wen Sun ◽  
Hong Sun ◽  
Xia Yang ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractTwo Mn(II) complexes, {[Mn(BIPMO)2Cl2] · 2(H2O)}n (1) and {[Mn(BIPMO)2(SCN)2] · 2(CH3OH)}n (2) (BIPMO = bis(4-(1H-imidazol-1-yl)phenyl)methanone) with V-shaped BIPMO ligands, were synthesized and characterized by IR spectroscopy and elemental analyses along with their single-crystal X-ray diffraction analyses. The Mn(II) ions in 1 and 2 are both six-coordinated to four nitrogen atoms of four BIPMO ligands and two anions (Cl− for 1, and SCN− for 2) to form a distorted octahedral geometry.

Cationic iron(III) complex with a hexadentate N2,N'2',O2-aminopyridylphenolate ligand

1999 ◽  
Vol 77 (12) ◽  
pp. 2033-2038 ◽  
Author(s):  
Ika A Setyawati ◽  
Steven J Rettig ◽  
Chris Orvig
Keyword(s):  
Heavy Atom ◽  
Crystallographic Analysis ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Cyclic Voltammogram ◽  
X Ray ◽  
R Factor ◽  
Distorted Octahedral ◽  
Elemental Analyses

Iron(III) complexation with potentially hexadentate H2bbpen (N,N'-bis(2-hydroxybenzyl)-N,N'-bis(2-methylpyridyl)ethylenediamine) was studied. The resulting monocationic complex, [Fe(bbpen)]+ as its NO3- and PF6- salts, was characterized by infrared spectroscopy, mass spectrometry, elemental analyses, cyclic voltammetry, and X-ray crystallographic analysis. Crystals of [Fe(bbpen)]NO3·CH3OH are monoclinic, space group P21/c, a = 10.2640(13), b = 14.7526(10), c = 18.3172(5) Å, β = 97.904(1)°, and Z = 4. The structure was solved by heavy-atom Patterson methods and refined to an R factor of 0.039 for 3526 reflections with I > 3σ(I). The structure of the [Fe(bbpen)]+ cation showed that the ligand is bound in a hexadentate fashion to the central Fe(III) ion, resulting in a distorted octahedral geometry. Magnetic susceptibility measurements indicated the presence of a high-spin Fe(III) ion, and the UV-vis spectrum of [Fe(bbpen)]NO3 exhibits absorption maxima, λmax, at 575 nm (ε = 5400 M-1 cm-1), 323 (8900), and 275 (13 500). The cyclic voltammogram of [Fe(bbpen)]NO3 showed a quasi-reversible, one-electron process corresponding to [FeIII(bbpen)]+ + e- <_> [FeII(bbpen)] at -0.47 V vs. SCE.Key words: cationic, iron(III), phenolate, pyridyl, hexadentate.

Synthesis and structural characterization of Mn(II) and Cu(II) complexes with bis(4-(1H-imidazol-1-yl)phenyl)methanone ligands

2017 ◽  
Vol 72 (1) ◽  
pp. 83-87 ◽  
Author(s):  
Gao-Feng Wang ◽  
Xiao Zhang ◽  
Zhao-Rong Liu ◽  
Yu-Chun Wang ◽  
Hong-Shi Jiang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Octahedral Geometry ◽  
Helical Chain ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractTwo complexes, {Mn(hfac)2(BIPMO)}n (1), {Cu(hfac)2(BIPMO)}n (2) [hfac=1,1,1,5,5,5-hexafluoro-pentane-2,4-dionato(–), BIPMO=bis(4-(1H-imidazol-1-yl)phenyl)methanone], with the V-shaped ligands were synthesized and characterized by infrared spectroscopy, elemental analyses, along with single-crystal X-ray diffraction analyses. The X-ray diffraction studies have shown that the metal ions in 1 and 2 are both six-coordinated to two nitrogen atoms of two BIPMO ligands and four oxygen atoms of two hfac ligands to form a distorted octahedral geometry. Each BIPMO ligand acts as a bridging ligand to link two adjacent metal(II) atoms to form a helical chain in the crystal structure.

New Dinuclear Mn(II) Phenanthroline Adipato Complex: Synthesis and Structural and Thermal Characterization of Mn2(phen)2(H2O)2(C6H8O4)2

2003 ◽  
Vol 58 (4) ◽  
pp. 266-270 ◽  
Author(s):  
Yue-Qing Zheng ◽  
Ming-Fang Zheng
Keyword(s):  
Thermal Characterization ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Stacking Interactions ◽  
Phen Ligand ◽  
Complex Molecules ◽  
X Ray ◽  
Distorted Octahedral ◽  
Argon Stream

Reaction of freshly precipitated Mn(OH)2−2x(CO3)x · yH2O, adipic acid and phenanthroline in CH3OH/H2O afforded a new dinuclear Mn(II) complex, Mn2(phen)2(H2O)2(C6H8O4)2 1, aside the known [Mn(phen)2(H2O)(C6H8O4)]·7H2O 2. Single crystal X-ray analyses showed that complex 1 consists of the centrosymmetric dinuclear molecules resulting from two [Mn(phen)(H2O)]2+ moities bridged by two twisted tridentate adipato ligands. The Mn atoms are each in severely distorted octahedral geometry defined by two N atoms of one phen ligand, three carboxyl O atoms of two adipato ligands and one H2O molecule with d(Mn-N) = 2.246 and 2.296 Å and d(Mn-O) = 2.066 - 2.339 Å . The complex molecules are assembled via π-π stacking interactions into 2D layers, which are held together by both strong O-H ··· O and weak C- H ··· O hydrogen bonds. The thermal behavior of 1 and 2 upon heating in argon stream is discussed.

The Crystal Structure of a Thiathiophthen Nitrogen Isostere, 3,5-Epidithio-2,5-diphenyl-2,4-pentadienylidene-3-aminoquinoline

1971 ◽  
Vol 49 (2) ◽  
pp. 167-172 ◽  
Author(s):  
F. Leung ◽  
S. C. Nyburg
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
Triclinic System ◽  
R Factor ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structure of a thiathiophthen nitrogen isostere (7) has been solved by X-ray analysis. The crystal belongs to the triclinic system with unit cell dimensions: a = 11.275(11), b = 9.558(10), c = 10.797(10) Å, α = 92.50(10), β = 116.98(10), γ = 92.61(10)°. There are two molecules per unit cell, space group [Formula: see text]. The data were collected by diffractometer with CuKα radiation. The structure was solved by symbolic addition procedures, and fully refined anisotropically using full-matrix least squares to an R factor of 6.3%.The S—S and S—N bond lengths were found to be 2.364 and 1.887 Å, respectively. This reveals the partial bonding character between S … S … N atoms.

The External Shape of Human γ GI Immunoglobulin from Crystal Sections

1971 ◽  
Vol 29 ◽  
pp. 428-429
Author(s):  
L. W. Labaw
Keyword(s):  
Molecular Weight ◽  
Sodium Phosphate ◽  
Osmium Tetroxide ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Large Molecular Weight ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Crystallographic Axes

Crystals of a human γGl immunoglobulin have the external morphology of diamond shaped prisms. X-ray studies have shown them to be monoclinic, space group C2, with 2 molecules per unit cell. The unit cell dimensions are a = 194.1, b = 91.7, c = 51.6Å, 8 = 102°. The relatively large molecular weight of 151,000 and these unit cell dimensions made this a promising crystal to study in the EM.Crystals similar to those used in the x-ray studies were fixed at 5°C for three weeks in a solution of mother liquor containing 5 x 10-5M sodium phosphate, pH 7.0, and 0.03% glutaraldehyde. They were postfixed with 1% osmium tetroxide for 15 min. and embedded in Maraglas the usual way. Sections were cut perpendicular to the three crystallographic axes. Such a section cut with its plane perpendicular to the z direction is shown in Fig. 1.This projection of the crystal in the z direction shows periodicities in at least four different directions but these are only seen clearly by sighting obliquely along the micrograph.

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