Nitridomolybdenum Complexes of Tris(3,5-dimethylpyrazol-1-yl)Hydroborate and the X-Ray Crystal-Structure of {HB(3,5-Me2C3N2H)3)MoN(N3)2

1990 ◽  
Vol 43 (8) ◽  
pp. 1347 ◽  
Author(s):  
CG Young ◽  
F Janos ◽  
MA Bruck ◽  
PA Wexler ◽  
JH Enemark
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Least Squares ◽  
Elemental Analysis ◽  
Bond Distance ◽  
Octahedral Complex ◽  
Fourier Methods ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The reaction of (NEt4)2[MoNCl5] and K{HB(Me2pz)3}[HB(Me2pz)3- = tris (3,5- dimethylpyrazol-1-yl) hydroborate anion] produces both purple, diamagnetic {HB(Me2pz)3}MoNCl2 (1) and yellow, paramagnetic Net4 [{HB(Me2pz)3}MoNCl2] (2) (e.s.r.: {g} 1.961, {a}(95Mo) 57×10-4 cm-1), which have been separately isolated under different conditions. In contrast, the reaction of [ MoN (N3)4]- with Na{HB(Me2pz)3} results in the exclusive formation of red {HB(Me2pz)3} MoN (N3)2 (3). Crystals of (3) are monoclinic and belong to space group P21/n with a 16.440(2), b 8.787(2), c 16.754(2) Ǻ,β 112.47(1)°, V 2236.4 Ǻ3, and Z 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 3208 reflections, to a conventional R value of 0.032 ( Rw 0.047). In the distorted octahedral complex the molybdenum(VI) atom is coordinated by a facial HB(Me2pz)3- ligand , a terminal nitrido ligand with a Mo-N bond distance of 1.646(4)Ǻ, and two azide ligands. All complexes have been characterized by elemental analysis, infrared, 1H n.m.r. or e.s.r. spectroscopy, and mass spectrometry. Improved syntheses for the starting materials (NEt4)2 [MoNCl5] and (NEt4)2 [MoNCl4] are also reported.

Tp*WIVO(S2CNEt2): the Missing Member of the Series

2004 ◽  
Vol 57 (3) ◽  
pp. 269 ◽  
Author(s):  
Aston A. Eagle ◽  
Charles G. Young ◽  
Edward R. T. Tiekink
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cyclic Voltammetry ◽  
1H Nmr Spectroscopy ◽  
Octahedral Complex ◽  
Synthesis And Characterization ◽  
Oxygen Atom Transfer ◽  
X Ray ◽  
Distorted Octahedral

The missing member of the series Tp*ME(S2CNEt2) (M = Mo, W; E = O, S), namely Tp*WO(S2CNEt2), has been synthesized by oxygen-atom transfer from pyridine N-oxide to Tp*W(S2CNEt2)(CO)2. The air-stable, blue-purple complex was characterized by microanalysis, mass spectrometry (m/z 645 (100%), [M]+), cyclic voltammetry, and IR and 1H NMR spectroscopy. Solutions of the complex are dichroic and solvatochromic. The X-ray crystal structure of the complex revealed a six-coordinate, distorted octahedral complex with axial oxo (W = O 1.680(5) Å), ‘equatorial’ dithiocarbamate (W—S 2.3962(17) and 2.4102(17) Å), and facial tridentate Tp* ligands. The synthesis and characterization of Tp*WCl3 are also reported.

Structural studies of Technetium Complexes. VIII. The Crystal Structure of Tetraphenylarsonium Tetrabromonitridotechnetate(VI)

1985 ◽  
Vol 38 (1) ◽  
pp. 215 ◽  
Author(s):  
J Baldas ◽  
J Bonnyman ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Bond Distance ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Angles ◽  
R Value

The crystal structure of [AsPh4] [TcNBr4] has been determined by single- crystal X-ray diffraction methods at 20�1°C. Crystals are tetragonal, space group P4/n, with a 12.875(2), c 7.992(1)Ǻ, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.039 for 1263 independent reflections. The compound is isostructural with the series [AsPh4] [MNBr4] (M = Mo, Ru , Re or Os) and [AsPh4] [MNCl4](M = Mo, Tc , Ru, Re or Os), and with [AsPh4] [OsNI4] and [AsPh4]- [MOCl4](M = Mo or Re). The [TcNBr4]- anion in [AsPh4] [TcNBr4] possesses C4v symmetry with Br- Tc -Br bond angles of 87.08(1) and 153.91(4)°, and N= Tc -Br bond angles of 103.04(2)°. The Tc≡N bond distance is 1.596(6)Ǻ, and the Tc - Br distances are 2.4816(5)Ǻ.

The Crystal Structure of [2,6-Bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)-pyridine]dithiocyanatonickel(II), a Complex of a Potentially Pentadentate N3S2 Ligand, and a Comparison with Complexes of an N3O2 Ligand

1979 ◽  
Vol 32 (6) ◽  
pp. 1199 ◽  
Author(s):  
W Choong ◽  
NC Stephenson ◽  
MA Ali ◽  
MA Malik ◽  
DJ Phillips
Keyword(s):  
Crystal Structure ◽  
Data Structure ◽  
Pyridine Ring ◽  
Structure Refinement ◽  
Three Dimensional ◽  
Octahedral Structure ◽  
Potential Donor ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The crystal structure of Ni(dapsm)(NCS)2 [dapsm is 2,6-bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)pyridinel has been determined from three-dimensional single-crystal diffractometer X-ray data. Structure refinement was carried out by least-squares methods to a final R value of 0.059. The ligand dapsm is a potential N3S2 pentadentate, but it coordinates as a tetradentate, giving a planar N3S donor grouping. Rotation occurs about an N-N bond in dapsm, moving a potential donor sulfur atom away from the nickel(II) ion. The pyridine ring of the ligand, and the N3S donor grouping, are approximately coplanar. Two thiocyanate groups are coordinated to the nickel, giving a distorted octahedral structure. The structure and electronic spectrum of Ni(dapsm)- (NCS)2 are compared with those for seven-coordinate complexes with the related N3O2 ligand, 2,6-diacetylpyridine bissemicarbazone.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

Crystal Structure of Tetraethylammonium Bromopentacarbonyltungstate(0)

1995 ◽  
Vol 48 (5) ◽  
pp. 1045 ◽  
Author(s):  
T Whyte ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
R Value

The crystal structure of tetraethylammonium bromopentacarbonyltungstate (0), [NEt4] [W(CO)5Br], has been determined by single-crystal X-ray diffraction methods at 22�1°C. Crystals are tetragonal, space group P4/n, with a 9.206(2), c 10.484(2) Ǻ, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.034 for 820 independent reflections. The [W(CO)5Br]- anion possesses exact C4v symmetry, with bond lengths W-Br 2.736(1), W-COtrans 1.93(1) and W-COcis 2.034(6) Ǻ.

Synthesis, Characterization and X-Ray Crystal Structure of {H2B(Me2C3N2H)2}MoIVO(S2PPrI2)

1994 ◽  
Vol 47 (3) ◽  
pp. 471 ◽  
Author(s):  
LJ Laughlin ◽  
JM Gulbis ◽  
ERT Tiekink ◽  
CG Young
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometric ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
R Value

Reaction of MoO (S2PPri2)2 and K{H2B(Me2C3N2H)2} in refluxing toluene produces green, diamagnetic, air-stable {H2B(Me2C3N2H)2}MoIVO(S2Ppri2)(1), which has been characterized by analytical, mass spectrometric, infrared and n.m.r. spectroscopic, and X-ray crystallographic techniques. Crystals of (1) are triclinic and belong to space group Pī , with a 10.289(1), b 13.601(2), c 8.737(1) Ǻ, α 94.31(1), β 107.71(1), γ 79.56(1)°, V 1145.2 Ǻ3 and Z 2. The structure was solved by Patterson and Fourier methods and refined by using 3631 reflections to a final R value of 0.024 ( Rw 0.041). The five-coordinate square pyramidal complex is composed of apical terminal oxo [Mo-O(1) 1.658(2)Ǻ] and bidentate H2B(Me2C3N2H)2- and S2PPri2- ligands coordinated to molybdenum. Ferrocenium oxidation of (1) produces the mononuclear molybdenum(V) complex [{H2B(Me2C3N2H)2}MoVO(S2Ppri2)]+ ( e.p.r .: g 1.964, a(95,97Mo) 41.7×10-4cm-1, a(31P) 30.1×10-4 cm-1).

Crystal and molecular structure of Octacarbonylbis(diphenylarsino)-methanedimanganese(0)

1983 ◽  
Vol 36 (4) ◽  
pp. 683 ◽  
Author(s):  
BF Hoskins ◽  
RJ Steen
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Parent Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
X Ray

The crystal structure of the complex Mn2(CO)8(dam) (dam = Ph2AsCH2AsPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are triclinic, space group P1, with a 11.191(1), b 16.498(5), c 9.455(1) �, a 93.64(2), β 109.08(2), γ 89.36(2)� and contain two discrete, binuclear molecules of Mn2(CO)8(dam) per unit cell. The structure, solved by direct and Fourier methods, was refined by a least-squares procedure to R and Rw of 0.065 and 0.082 respectively for 1907 independent, statistically significant reflections collected by counter methods. The feature of particular interest in this compound is the accommodation of the bridging bidentate dam ligand [As.. .As separation 3.242(2) �] across a shorter Mn�-Mn� bond [2.962(3) �] which constrains the molecule so that a much less staggered configuration of the two manganese coordination octahedra is observed relative to the parent compound Mn2(CO)10, the rotation of the two equatorial planes in the former being 30�.

scholarly journals Molecular design and synthesis of new dithiocarbazate complexes; crystal structure, bioactivities and nano studies

RSC Advances ◽  
2018 ◽  
Vol 8 (73) ◽  
pp. 41795-41809 ◽  
Author(s):  
Zahra Yekke-ghasemi ◽  
Reza Takjoo ◽  
Mohammad Ramezani ◽  
Joel T. Mague
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Metal Complexes ◽  
Elemental Analysis ◽  
Molecular Design ◽  
X Ray ◽  
Design And Synthesis

New metal complexes are synthesized and characterized by elemental analysis, mass spectrometry, spectroscopic, TGA and X-ray techniques. The compounds were evaluated in anin vitrocytotoxicity. Interaction of the samples with HSA was investigated.

scholarly journals Molekül- und Kristallstruktur von C7H7Mo(CO)2-SnCl3 / The Crystal Structure of C7H7Mo(CO)2-SnCl3

1975 ◽  
Vol 30 (1-2) ◽  
pp. 22-25 ◽  
Author(s):  
M. L. Ziegler ◽  
H.-E. Sasse ◽  
B. Nuber
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Three Dimensional ◽  
Unit Cell ◽  
Fourier Methods ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Group D

The structure of the title compound has been determined from three dimensional X-ray data by Patterson and Fourier methods. The crystals are orthorombic, with unit cell dimensions a = 1181,50 pm, b = 943,68 pm, c = 1181,50 pm, space group D2h16 and Z = 4. Least squares refinement, by use of 1540 independent reflections measured on a diffractometer has reached R = 5,9%.There are discrete C7H7Mo(CO)2 SnCl3 molecules, the molybdenum-tin bond has been dicussed together with the corresponding bonds in other C7H7Mo(CO)2 SnR3 compounds.

Al2Sb2I12: Vierkern-Einheiten in einem 1:1-Addukt aus AlI3 und SbI3 / Al2Sb2I12: Tetrameric Units in a 1:1 Adduct of AlI3 and SbI3

1983 ◽  
Vol 38 (12) ◽  
pp. 1539-1542 ◽  
Author(s):  
Siegfried Pohl
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Electron Pair ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Layer Structures ◽  
R Value ◽  
Stereochemical Activity ◽  
Bonding Electron

Al2Sb2I12 (1) was prepared by heating stoichiometric amounts of AlI3 and SbI3 in CS2. The crystal structure of 1 was determined from single crystal X-ray data. The compound crystallizes in the monoclinic space group C2/m with a = 1644.0(3), b = 1318.3(2), c = 728.9(1) pm, β = 119.33(1)°, and Z = 2. The structure was refined by least squares methods to a final unweighted R value of 0.064 for 676 nonequivalent reflections.The structure is built up of Al2Sb2I12 units in which two Sb-I octahedra share four common edges with two Al-I tetrahedra. As a consequence of the stereochemical activity of the non-bonding electron pair of antimony these cations are displaced from the centers of the iodine octahedra so that three different Sb-I bonds with distances of 270.8, 312.3, and 358.9 pm are observed in 1. The structure of Al2Sb2I12 can also be derived from the layer structures of the BiI3 type

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