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.

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

scholarly journals Synthesis and Characterization of Nickel(II) Complexes of Nitrogen based Ligands of Type N,N,N′,N′-tetrakis(2-Pyridylmethyl)alkanediamine

2021 ◽  
Vol 33 (9) ◽  
pp. 2157-2161
Author(s):  
F.M. Nareetsile ◽  
R. Gontse ◽  
O.A. Oyetunji ◽  
V.C. Obuseng
Keyword(s):  
Crystal Structure Data ◽  
Octahedral Geometry ◽  
Methanol Solution ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Ethanol Medium ◽  
Hexadentate Ligand

Hexadentate ligand of the type N,N,N′,N′-tetrakis(2-pyridylmethyl)alkanediamine (where alkane is butane (L1), hexane (L2) and octane (L3) reacted with Ni(ClO4)2·6H2O (stoichiometry 1:1) in alcoholic solutions yielding mononuclear complexes of the type [Ni(L)](ClO4)2·xH2O. The ligand L1 reacted with Ni(ClO4)2·6H2O in ethanol medium to give a violet powder of [Ni(L1)](ClO4)2·3H2O. The other mononuclear nickel(II) complexes using L2 and L3 were synthesized in methanol solution to give violet powders of [Ni(L2)](ClO4)2·2H2O and [Ni(L3)](ClO4)2·2H2O, respectively. All the three complexes were characterized by IR and elemental analysis. The X-ray crystallographic results for the purple crystals of [Ni(L1)](ClO4)2·3H2O shows the octahedral geometry on the Ni(II) ions together with the tetrahedral perchlorate anions separated from the [Ni(L1)]2+ cation. The crystal structure data show monoclinic space group P 21/c; a = 17.1748(10), b = 9.8273(6), c = 17.8146(10) Å; α = 90º, β = 95.0200(10)º, γ = 90º; V = 2995.2(3) Å3 , Z = 4.

In-depth understanding of π-electron systems: New vistas in fullerene endohedrals

2010 ◽  
Vol 82 (4) ◽  
pp. 757-767 ◽  
Author(s):  
Michio Yamada ◽  
Takahiro Tsuchiya ◽  
Takeshi Akasaka ◽  
Shigeru Nagase
Keyword(s):  
Electronic Properties ◽  
Theoretical Calculations ◽  
Crystallographic Analysis ◽  
Synthesis And Characterization ◽  
Electron Systems ◽  
X Ray ◽  
Endohedral Metallofullerenes ◽  
Metal Atoms ◽  
Nmr Study

The synthesis and characterization of various endohedral metallofullerenes and their derivatives are described. The encapsulated metal atoms’ positions and movements were determined using NMR study, X-ray crystallographic analysis, and theoretical calculations. The results of electrochemical investigations clarified the relation between the electronic properties and the π-electron systems of the fullerene endohedrals.

Synthesis and Characterization of the Nickel(II) Complex of a Macrocyclic Schiff Base Ligand with a Single Pendant Coordinating Hydroxyl Arm

2003 ◽  
Vol 56 (12) ◽  
pp. 1255 ◽  
Author(s):  
Ali Akbar Khandar ◽  
Seyed Abolfazl Hosseini-Yazdi
Keyword(s):  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Macrocyclic Schiff Base ◽  
Template Reaction ◽  
Pentadentate Ligand

The synthesis and characterization of a nickel(II) complex of the ligand 8,9,18,19-tetrahydro-7H,17H-dibenzo[f,o][1,5,9,13]dioxadiazacyclohexadecin-18-ol (L) is described. Complex [NiL(NO3)]NO3 was prepared by facile template reaction of the appropriate dialdehyde 2-(3-(2-formylphenoxy)-2-hydroxypropoxy)benzaldehyde (1) and 1,3-diaminopropane in the presence of nickel nitrate. X-Ray crystallography indicated that the compound was a six-coordinate complex that contained a pentadentate ligand and an NO3− anion trans to the alcoholic donor. The blue complex contains nickel(II) in a distorted octahedral environment of N2O4 donors, and crystallizes in the monoclinic space group C2/c with a 26.921(10), b 9.075(2), c 21.193(7) Å, β 122.12(2)°, and Z 8. From spectro-scopic and conductivity studies of the complex it has been found that six-coordinate [NiL(NO3)]+ cations and NO3− anions are formed in solution.

Synthesis and characterization of 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7

1993 ◽  
Vol 71 (7) ◽  
pp. 1057-1063 ◽  
Author(s):  
Donna L. Draper ◽  
Richard J. Barton ◽  
Beverly E. Robertson ◽  
Barbara R. Nelson ◽  
John A. Weil
Keyword(s):  
Nitro Group ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Phenyl Rings ◽  
Common Plane ◽  
Twist Boat

The reaction of 2,2-diphenyl-1-(2,4,6-trinitrophenyl)hydrazine with the enolate of acetone, followed by acidification, yields the title compound 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7. The identity of the latter was confirmed by a combination of mass spectrometry, FTIR, elemental analysis, and 1H NMR. Crystals were grown from dichloromethane –95% ethanol and the structure was determined by X-ray diffraction. Crystals are monoclinic, P21/c, a = 9.254(3), b = 13.531(3), c = 17.39(5) Å, β = 106.18(2)° at 225 K. R = 0.073, Rω = 0.038 for reflections with I > 2σ(I). The Zachariasen extinction factor, g, refined to 18(3) × 10−4. The cyclohexadiene ring is puckered with a primarily twist-boat conformation. Atoms C(1) to C(3), C(6), the nitro group on C(2), and the hydrazine moiety (N(8)—N(7)—H(7) attached to C(1)) all lie close to a common plane. The planes of the two phenyl rings, the acetonyl substituent, and the C(6) nitro group are each roughly perpendicular to this plane. The C(5) acetonyl and C(6) nitro groups are trans to each other.

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