Synthesis and structural characterization of an ether-bridged cobalta-bis(dicarbollide): a model for Venus flytrap cluster reagents

1995 ◽  
Vol 73 (7) ◽  
pp. 1044-1049 ◽  
Author(s):  
David E. Harwell ◽  
Juliet Nabakka ◽  
Carolyn B. Knobler ◽  
M. Frederick Hawthorne
Keyword(s):  
Structural Characterization ◽  
Heavy Atom ◽  
Cobalt Complex ◽  
Monoclinic Space Group ◽  
Model Compounds ◽  
Ether Linkage ◽  
X Ray ◽  
New Class ◽  
Venus Flytrap

The synthesis of bis-(1-carboranylmethyl) ether was first published in 1963; however, its subsequent complexation with a transition metal was never reported. We now report the complexation of cobalt and the corresponding X-ray structure for the triphenylmethylphosphonium salt of the cobalta-bis(carboranylmethyl) ether. The cobalt complex crystallized in the monoclinic space group C2/c with a = 21.729(6) Å, b = 9.845(2) Å, c = 35.565(9) Å, β = 105.363(9)°, V = 7336 Å3, and Z = 8. Data were collected using CuKα radiation, to a maximum 2θ = 115°, giving 4123 unique reflections, and the structure was solved by heavy atom methods. The final discrepancy index was R = 0.093, Rw = 0.100 for 1919 independent reflections with I > 3σ(I). This metala-bis(carboranylalkyl) ether is the first in a new class of Venus flytrap compounds (VFC), containing an ether linkage, to be synthesized as model compounds for the development of reagents suitable for use in the radioimmunodetection and radioimmunotherapy of cancer. Keywords: cobalt, radioimmunodetection, radioimmunotherapy, Venus flytrap.

A new class of dinuclear compounds: The synthesis and x-ray structural characterization of tris(μ-diphenyl-formamidinato) diiron

1994 ◽  
Vol 219 (1-2) ◽  
pp. 7-10 ◽  
Author(s):  
F. Albert Cotton ◽  
Lee M. Daniels ◽  
Larry R. Falvello ◽  
Carlos A. Murillo
Keyword(s):  
Structural Characterization ◽  
X Ray ◽  
New Class ◽  
Dinuclear Compounds

Synthesis and structural characterization of BaV4O9

2007 ◽  
Vol 63 (2) ◽  
pp. 270-276 ◽  
Author(s):  
Thomas Reeswinkel ◽  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth
Keyword(s):  
Crystal Structure ◽  
Thermal Expansion ◽  
Structural Characterization ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
Temperature Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermal Expansion Tensor

The new spin ½ V4+ barium oxovanadate BaV4O9 was synthesized and studied by means of single-crystal X-ray diffraction. Its room-temperature structure is monoclinic, space group P2/c. We discuss the temperature evolution of the crystal structure and thermal expansion tensor of the material between 293 and 100 K.

Structural Characterization of Cationic 16-Electron Pentamethylcyclopentadienyl Ruthenium(II) Complexes Containing the Binuclear [Cp*Ru(μ-Cl)3RuCp*]– Anion

2008 ◽  
Vol 63 (10) ◽  
pp. 1155-1159 ◽  
Author(s):  
Thomas Glöge ◽  
Dejan Petrovic ◽  
Cristian G. Hrib ◽  
Peter G. Jones ◽  
Matthias Tamm
Keyword(s):  
Crystal Structures ◽  
Structural Characterization ◽  
Complex Salt ◽  
Monoclinic Space Group ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Diimine Ligand ◽  
Half Sandwich

AbstractThe reaction of the diimine ligand 1,2-bis(1,3-diisopropyl-4,5-dimethylimidazolin-2-imino)ethane (BLiPr) with tetrameric [Cp*RuCl]4 in a 1 : 0.75 ratio afforded the complex salt [1][2] containing the 16-electron half-sandwich cation [Cp*Ru(BLiPr)]+ (1) and the dinuclear anion [Cp*Ru(μ- Cl)3RuCp*]− (2). The X-ray crystal structures of [1][2]·31/2THF (monoclinic, space group P21/n, Z = 4) and of [1][2]·THF (monoclinic, space group C2/m, Z = 4) are reported, allowing the structural characterization of the unprecedented anion 2, in which two [(η5-C5Me5)Ru(II)] moieties are bridged by three μ2-chlorine atoms.

Synthesis and structural characterization of a Ni(II) coordination polymer with a tripodal 4-imidazolyl-functional ligand

2019 ◽  
Vol 74 (11-12) ◽  
pp. 857-860
Author(s):  
Hai-Wei Kuai ◽  
Xiao-Hong Zhu ◽  
Ding-Yun Jiang ◽  
Xiao-Chun Cheng ◽  
Deng-Hao Li
Keyword(s):  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Network Structure ◽  
Structural Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray

Abstract1,3,5-Tri(1H-imidazol-4-yl)benzene (H3L) reacts with Ni(ClO4)2 · 6H2O under hydrothermal conditions at T = 100°C to yield a new complex: [Ni(H2L)2] · 5.5H2O (1). The product is characterized by single crystal and powder X-ray diffraction, infrared spectroscopy, and elemental and thermogravimetric analyses. Complex 1 crystallizes in the monoclinic space group C2/c and exhibits a binodal (3,6)-connected 2D kgd network structure with (43)2(46.66.83) topology.

Synthesis and structure of 3,5-dimethylpyrazolyl iron and cobalt dinitrosyl dimers

1979 ◽  
Vol 57 (23) ◽  
pp. 3119-3125 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Cobalt Complex ◽  
Cobalt Complexes ◽  
Iron Complex ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
Coordination Geometry ◽  
X Ray ◽  
Metal Atoms

The synthesis and characterization of two 3,5-dimethylpyrazolyl metal dinitrosyl dimers [(N2C5H7)M(NO)2]2 (where M = Fe or Co) are described and their X-ray crystal structures detailed. Both complexes crystallize in the monoclinic space group C2/c, a = 23.848(2), 23.722(4), b = 10.7775(7), 10.6888(6), c = 14.764(1), 14.712(2) Å, β = 117.366(6), 117.094(7)°, Z = 8 (for the iron and cobalt complexes respectively). The structure of the iron complex was solved by Patterson and Fourier syntheses. The cobalt complex is isomorphous with the iron analog. Both structures were refined by full-matrix least-squares procedures to R = 0.028 and 0.035 for 4251 and 3376 reflections with I ≥ 3σ(I) respectively. Both complexes adopt a boat conformation for the central M—(N—N)2—M ring and display significantly non-linear M—N—O groups. The coordination geometry about the metal atoms is distorted tetrahedral. Important molecular dimensions (distances corrected for libration) are: mean Fe—N(pyrazolyl), 2.009(5), mean Fe—NO, 1.696(2) Å, Fe—N—O, 158.5(3)–168.2(2)°, mean Co—N(pyrazolyl), 1.992(7), Co—NO, 1.646(3)–1.680(3) Å, and Co—N—O, 161.6(3)–173.5(3)°. The iron complex is paramagnetic with formally "17-electron" iron atoms. Both structures are compared with similar four-coordinate metal dinitrosyl compounds.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LII. Synthesis and Structural Characterization of Mononuclear Chloro- and Bromo-pyridinebis-(triphenylphosphine)silver(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 907 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Silver Atom ◽  
Lewis Base ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Weak Coordination

The mononuclear adducts chloro - and bromo-pyridinebis (triphenylphosphine)silver have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The two complexes are isomorphous, monoclinic, space group P21 or P21/m, a ≈ 9.8, b ≈ 20.0, c ≈ 9.1 � , β ≈ 97.5�, Z 2; in space group P21/m, they were refined to residuals of 0.038, 0.036 for 2392, 2157 'observed' reflections respectively. No comparable iodide adduct has been isolated. In both structures the silver atom is four-coordinate; Ag-Cl,Br are 2.511(2), 2.629(1) �; Ag-P, 2.472(1), 2.476(1) �, and Ag-N, 2.585(5), 2.570(5) � respectively, the Ag-N distance being longer than Ag-P, indicating very weak coordination of the pyridine.

Synthesis and Structural Characterization of Copper(I) and Copper(II) Complexes with an Ambivalent Phenanthroline-Type Ligand

1997 ◽  
Vol 50 (10) ◽  
pp. 951 ◽  
Author(s):  
Jean-Paul Collin ◽  
Pablo Gaviña ◽  
Jean-Pierre Sauvage ◽  
André De Cian ◽  
Jean Fischer
Keyword(s):  
Cyclic Voltammetry ◽  
Structural Characterization ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Coordination Modes ◽  
X Ray Crystallography ◽  
Phenanthroline Ligand

The new phenanthroline ligand 2-(p-methoxyphenyl)-9-(5′-methylpyridin-2′-yl)-1,10-phenanthroline L has been synthesized and shown to form four-coordinate CuI(L)2 (1) and six-coordinate CuII(L)2 (2) complexes. Their structures have been determined by X-ray crystallography: (1) C50H38CuN6O2.BF4, triclinic, space group P -1, a12·924(3), b 14·567(4), c 12·649(3) Å , α 105·57(2), β 107·68(2), γ 104·00(2)°; (2) C50H38CuN6O2.2PF6, monoclinic, space group P 21/c, a 17·701(5), b 19·285(5), c 14·93(4) Å, β 98·20(2)°. In solution, cyclic voltammetry measurements indicate for the copper(I) and copper(II) complexes a very fast rearrangement of the pyridine substituent with the change of the oxidation state. Surprisingly, the X-ray data show two different coordination modes for the ligand around the copper(I) ion, the 1,10-phenanthroline nucleus being either mono- or bi-dentate. In solution, since the 1H n.m.r. spectra obtained even at several temperatures display only one set of signals, it is proposed that a fast equilibrium takes place between two coordination modes of the phenanthroline

Synthesis and X-Ray Structural Characterization of WO(S2)(S2CNEt2)2 and Related Complexes

1987 ◽  
Vol 40 (2) ◽  
pp. 381 ◽  
Author(s):  
JA Broomhead ◽  
JH Enemark ◽  
B Hammer ◽  
RB Ortega ◽  
W Pienkowski
Keyword(s):  
Structural Analysis ◽  
Structural Characterization ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray

The reaction of SO2 and W(CO)3(S2CNR2)2 in dichloromethane solution under dinitrogen gives the title complex along with WS(S2)(S2CNR2)2 and Syn-W2O2(�-S)2(S2CNR2)2 (R = Me, Et, Pri , C6H5CH2; NR2 = pyrrolidinyl ). X-ray structural analysis of WO(S2)(S2CNEt2)2 reveals a seven-coordinate tungsten complex with a terminal oxo group and a dihapto - disulfido ligand in a mutually triangular arrangement. Crystals are monoclinic space group P21 1 n, with a 9.379(2), b 22.276(7), c 9.408(2), β 106.86(1)�, U 188l.1(7) �33 and Z 4.2758 independent data were refined to a weighted agreement factor 0.036.

scholarly journals Synthesis and Structural Characterization of ‘Non-VSEPR’ Structures of Oxo-Tungsten Complex

2011 ◽  
Vol 8 (s1) ◽  
pp. S323-S329
Author(s):  
Shahriare Ghammamy ◽  
Hajar Sahebalzamani
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structural Characterization ◽  
Direct Methods ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cis And Trans

The crystal structure of [(CH3)4N]4[WOCl4F][WO3Cl4] was determined by single crystal x-ray diffraction technique. The crystal is monoclinic, space group C 2/m, with a= 28.23(10) Å, b= 11.60(4) Å,c= 13.48(5) Å, β=118.43(7)°, V= 3886(2)Å3, Z=4. The structure was solved by direct methods and refined by least-squares methods to a final R = 0.0512 for 3825 observed reflections with I>2σ(I). In crystal there are two crystallographic distinct anions, both with cis geometry; the O-W-F and O-W-O angles are 97.5(3)° and 103.1(3) ° respectively. All structures are cis configurations that confirm a preference for angles below 90° and 180° between cis and trans σ-donor ligands, respectively.

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