Finding a soft spot for vanadium: a P-bound OCP ligand

2019 ◽  
Vol 55 (42) ◽  
pp. 5966-5969 ◽  
Author(s):  
Lauren N. Grant ◽  
J. Krzystek ◽  
Balazs Pinter ◽  
Joshua Telser ◽  
Hansjörg Grützmacher ◽  
...  
Keyword(s):  
Transition Metal ◽  
Single Crystal ◽  
Computational Studies ◽  
Squid Magnetometry ◽  
X Ray Diffraction ◽  
Detailed Characterization ◽  
X Ray ◽  
Soft Spot

The first example of a P-bound phosphaethynolato ligand, [OCP]−, to an early 3d transition metal is presented, along with detailed characterization by single crystal X-ray diffraction, SQuID magnetometry, HFEPR spectroscopy, and computational studies.

Dinuclear oxofluorometallates as a new structural type of d 0 transition metal oxofluoride compound

2012 ◽  
Vol 68 (6) ◽  
pp. 602-609 ◽  
Author(s):  
Anatoly A. Udovenko ◽  
Natalia M. Laptash
Keyword(s):  
Transition Metal ◽  
Single Crystal ◽  
Structural Type ◽  
The Other ◽  
Orthorhombic Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Unit Cell ◽  
Fluoride Ions ◽  
X Ray ◽  
Irradiation Process

Five isomorphous d 0 transition metal oxofluoride compounds A 3[M 2O x F11 − x ]·(AF)0.333 (A = K, Rb, NH4; M = Nb, Mo, W; x = 2, 4) have been synthesized from acid fluoride solutions, and their crystal structures have been determined by single-crystal X-ray diffraction. The basic structural building units are dinuclear M 2 X 11 (dimers) formed from NbOF5 or Mo(W)O2F4 octahedra connected by the fluorine bridging atom. In the Nb2O2F9 dimer, the O atoms occupy apical corners. In the M 2O4F7 (M = Mo, W) dimers two O atoms are also apically placed, whereas the other two O atoms are statistically disordered in equatorial planes. The arrangement of dimers is so that the hexagonal tunnels containing `free' fluoride ions are formed. During the irradiation process the orthorhombic structure of K3Nb2O2F9·(KF)0.333 transforms into a pseudo-trigonal one with a = 23.15 Å, which is the [101] diagonal of the orthorhombic unit cell. The other four trigonal crystals are merohedral twins.

Transition metal coordination complexes of chrysazin

CrystEngComm ◽  
2016 ◽  
Vol 18 (27) ◽  
pp. 5121-5129 ◽  
Author(s):  
Patrick J. Beldon ◽  
Sebastian Henke ◽  
Bartomeu Monserrat ◽  
Satoshi Tominaka ◽  
Norbert Stock ◽  
...  
Keyword(s):  
Transition Metal ◽  
Transition Metals ◽  
Single Crystal ◽  
Coordination Compounds ◽  
Coordination Complexes ◽  
Metal Coordination ◽  
X Ray Diffraction ◽  
X Ray

Eleven novel coordination compounds, composed of chrysazin (1,8-dihydroxyanthraquinone) and different first-row transition metals (Fe, Co, Ni, Cu), were synthesised and the structures determined by single-crystal X-ray diffraction.

Reactions of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

Two Zr−based heterometal−organic frameworks for efficient CO2 reduction under visible light

CrystEngComm ◽  
2021 ◽  
Author(s):  
Ying Wang ◽  
Yao-mei Fu ◽  
Si-qi You ◽  
xuexin Li ◽  
Xinlong Wang ◽  
...  
Keyword(s):  
Transition Metal ◽  
Visible Light ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Co2 Reduction ◽  
X Ray Diffraction ◽  
Transition Metal Cations ◽  
One Pot ◽  
X Ray ◽  
Secondary Building Units

Two new zirconium−based heterometal−organic frameworks, Zr3CP3−Mn (1) and Zr3CP3−Ni (2) constructed from [Cp3Zr3(μ3−O)(μ2−OH)3(IN)3] secondary building units and transition metal cations, were successfully synthesized through one−pot method. Single-crystal X-ray diffraction analysis...

scholarly journals Order in disorder: solution and solid-state studies of [MIII2MII5] wheels (MIII = Cr, Al; MII = Ni, Zn)

2018 ◽  
Vol 47 (34) ◽  
pp. 11834-11842 ◽  
Author(s):  
Hector W. L. Fraser ◽  
Gary S. Nichol ◽  
Dušan Uhrín ◽  
Ulla Gro Nielsen ◽  
Marco Evangelisti ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Squid Magnetometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy ◽  
Esi Mass Spectrometry

Heterometallic species with Anderson-like structures are characterised by single-crystal X-ray diffraction, solution- and solid-state NMR spectroscopy, ESI mass spectrometry and SQUID magnetometry.

High-Pressure Study of Oxo-bridged Mixed-Valent MnIII/MnIV Dimers High-Pressure Study of Oxo-bridged Mixed-Valent MnIII/MnIV Dimers

2010 ◽  
Vol 65 (3) ◽  
pp. 221-230 ◽  
Author(s):  
Alessandro Prescimone ◽  
Javier Sanchez-Benitez ◽  
Konstantin V. Kamenev ◽  
John E. Warren ◽  
Alistair R. Lennie ◽  
...  
Keyword(s):  
High Pressure ◽  
Hydrostatic Pressure ◽  
Single Crystal ◽  
Magnetic Behaviour ◽  
Squid Magnetometry ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
High Pressure Study

A combination of high-pressure single crystal X-ray diffraction and high-pressure SQUID magnetometry has been used to study two oxo-bridged mixed-valent MnIII/MnIV dimers. [Mn2O2(bpy)4](ClO4)3·3CH3CN, (1·3CH3CN; bpy = 2,2ʹ-bipyridine) has been compressed to 2.0 GPa whilst [Mn2O2(bpy)4](PF6)3·2CH3CN·1H2O, (2·2CH3CN·1H2O) could be measured crystallographically up to 4.55 GPa. The PF6 salt of [Mn2O2(bpy)4]3+ has never been reported before while 1 has been reported as a hydrate and in a different crystallographic space group. The application of hydrostatic pressure imposes significant distortions and modifications in the structures of both complexes. In particular, in complex 1·3CH3CN the Mn-Mn separation is reduced by the contraction of some of the Mn-O bond lengths, whilst in 2·2CH3CN·1H2O the Mn-O-Mn bridging angles and the Mn-O bond lengths are substantially unchanged. Interestingly 2·2CH3CN·1H2O also shows a constant contraction in nearly all the Mn-N bonds. The magnetic behaviour of the complexes has been measured up to 0.87 GPa for 1·3CH3CN and 0.84 GPa for 2·2CH3CN·1H2O.

Crystal structure of Carbonatohydroxo(2,2':6',2'-terpyridyl)cobalt(III) tetrahydrate

1978 ◽  
Vol 31 (1) ◽  
pp. 47 ◽  
Author(s):  
ES Kucharski ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
The Other ◽  
X Ray Diffraction ◽  
Hydroxide Ion ◽  
X Ray

The crystal structure of the title compound, [Co(terpy)(CO3)(OH)],4H2O, has been determined at 295 K by single-crystal X-ray diffraction and the use of diffractometer data, and refined by least squares to a residual of 0.075 for 1354 ?observed? reflections. Crystals are triclinic, Pī, a 11.407(6), b 10.566(6), c 8.445(4) Ǻ, α 100.21(5), β 107.35(5), γ 102.18(5)°, Z2. The structure of the molecule is unusual for a 1 : 1 transition metal/terpy complex in that the other ligating atoms are non-halide and the complex six-coordinate. The remaining three coordination positions about the metal are occupied by the bidentate carbonate (Co-O 1.918(9), 1.918(8) Ǻ) and the hydroxide ion (Co-O 1.894(10) Ǻ). The Co-N distances are appreciably shorter than those observed in other terpy systems (Co-N(central) 1.848(8); Co-N(outer) 1.946(9), 1.952(9) Ǻ).

scholarly journals Darstellung neuer Monofluorphosphine und einiger ihrer Übergangsmetallkomplexe; Einkristall-Röntgenstrukturanalyse eines Platin(II)-Komplexes / Preparation of New Monofluorophosphines and Some of their Transition Metal Complexes; Single Crystal X-Ray Diffraction Study of a Platinum(II) Complex

1993 ◽  
Vol 48 (7) ◽  
pp. 875-885 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Diffraction Study ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Classical Method ◽  
X Ray Diffraction ◽  
X Ray

The reaction of lithiated precursors with PCl2F led to a number of monofluorophosphines, including the known di-tert-butylmonofluorophosphine, 1. Bis(phenylethinyl)monofluorophosphine (2) was accessible only via this route (the classical method of synthesizing 2 by chlorine/fluorine exchange is impossible, because the corresponding chlorophosphine is unknown). Bis(2-methoxyphenyl)fluorophosphine (5) was prepared via the organolithium/PCl2F route. The NMR results for 5 thus prepared were inconsistent with previous reports, implying that the previously reported synthesis of 5 is in error. From 5 a cis-dichloroplatinum(II) complex (6) was synthesized and subjected to a single crystal X-ray structure analysis, confirming the expected planar coordination. From bis(2,3-dimethoxynaphthyl)monofluorophosphine (7) a rhodium(I) (8) and an iron(0)tetracarbonyl complex (9) were prepared. An iron(0)tetracarbonyl complex (11) was synthesized from bis(9-anthryl)monofluorophosphine (10) which was found to be stable to redox disproportionation.

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