Structures of organo-transition metal complexes determined by diffraction methods. Reports appearing during 1977.

Bruce, Michael I.

doi:10.1016/s0022-328x(00)91916-8

Cited by 3 publications

(1 citation statement)

References 969 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…These are consistent with the space groups Cmcm, Cmc2x, and Amal. The crystal was oriented, and lattice parameters were accurately determined by 25 automatically centered reflections (Table II).…”

Section: Introductionmentioning

confidence: 99%

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Raymond¹

1982

Inorg. Chem.

View full text Add to dashboard Cite

2653correction was applied (see Table I). Atomic scattering factors of Doyle and Turnerg were used, and anomalous scattering corrections'O were applied.Three-dimensional Patterson maps indicated the positions of the Mo atoms. Subsequent least-squares refinements and difference Fourier maps revealed all of the nonhydrogen atoms. Most of the hydrogen atom peaks were not resolved in the Fourier maps, and none were included in the least-squares refinements. All of the atoms with the exception of the carbon atoms in isomer A were assigned anisotropic thermal parameters in the final refinements. Because of the poor resolution of the ethyl groups in the A isomer, restraints were imposed on the geometry of the triethylphosphine groups by a procedure suggested by Waser," and described in a previous paper.12For the A isomer, the C-C and P-C bond distances were restrained to 1.54 and 1.82 A, respectively. The full-matrix least-squares program minimizes the function E w ( A F )~/ X W F~. After the last cycle of refinement, the largest shift of the parameter was 0.03 and 0.01 of its esd for the A and B isomer, respectively. R factors and other statistical results of the least-squares refinement are given in Table I. Contract No. W-7405-Eng-48. J.D.A. thanks the Equal Opportunity Program at UCB for a fellowship. Registry No. C~-MO~C~~(O~CCM~,)~(PE~,)~. 8 1276-73-5; C2h-MO~C~~(O~CCM~,)~(PE~,),, 8 1339-50-6; M o~C I~( P E~~)~, 59780-36-8; M o~( O~C C M~, )~, 55946-68-4; Me,SiCI, 75-77-4. Supplementary Material Available: Listings of thermal parameters and observed Structure factors (26 Pages). Ordering information is given on any current masthead page. (9) Doyle, P. A.; Turner, P. S. Acta Crystallogr., Sect. A 1968, A 2 4 390. (IO) Cromer, D. T.; Liberman, D.The title compounds have keen prepared by the reaction between U(C5MeS)2C12 and pyrazole (C3H4N2), or sodium pyrazolate (NaC3H3N2), in THF. The new compounds are characterized by their infrared, 'H NMR visible-near-IR, and mass spectra and by singlecrystal X-ray diffraction (monochromatic Mo Ka radiation). The molecular structure of U(C5Me5)2C12(C3H4N2) consists of discrete mononuclear units at positions of mm (C,) symmetry. The U4+ ion is coordinated by two a5-pentamethylcyclopentadienide rings, two chloride ions, and one nitrogen atom from the neutral pyrazole ring, for a total coordination number of 9. Red-brown crystals from toluene conform to space group Cmcm with a = 13.697 (4) A, b = 11.496 (2) A, c = 15.555 (2) A, and four molecules per unit cell. For the 924 independent reflections with F2 > 3 u ( p ) , the final weighted and unweighted R factors are 3.48 and 2.4556, respectively. The average U-C bond distance is 2.74 (2) A, the U-N bond distance is 2.607 (8) A, and the U-C1 distance is 2.696 (2) A. This compound exhibits Curie-Weiss behavior with C = 1.46,8 = 43.3 K, and pa (from the slope of 1/x vs. fl = 3.24 pB. The molecular structure of U(C5MeS)2C1(C3H3N2) consists of discrete U4+ ions coordinated by two 7,-pentamethylcyclopentadienide rings, one chloride ion...

show abstract

Section: Introductionmentioning

confidence: 99%

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Raymond¹

1982

Inorg. Chem.

View full text Add to dashboard Cite

show abstract

Stereochemie der Metall—Metall‐Bindung Die Strukturen der Verbindungen (CO)₄Cr[μ‐PMe₂]₂Ni(CO)₂ und (CO)₃Fe[μ‐PMe₂, μ‐I]Fe(CO)₃ mit je zwei verschiedenen Komplexhälften

Fischer

Vahrenkamp

1981

Zeitschrift anorg allge chemie

View full text Add to dashboard Cite

Die Kristallstrukturen der Titelkomplexe, deren einer zwei verschiedene Carbonylmetall‐Einheiten, deren anderer zwei verschiedene Brückenliganden besitzt, wurden bestimmt. Die Stereochemie des CrNi‐Komplexes entspricht der Erwartung, seine Metall—Metall‐Bindung ist jedoch kürzer als der Durchschnittswert aus den entsprechenden Cr2‐ bzw. Ni2‐Verbindungen. Bei dem Fe2‐Komplex ist die Gesamt‐Molekülgeometrie ebenfalls normal, doch der Metall—Metall‐Abstand ist deutlich kürzer als erwartet. Die Verkürzung der Metall—Metall‐Bindungen steht bei beiden Komplexen in Zusammenhang mit der Minimisierung der intramolekularen sterischen Hinderung. Stereochemistry of the Metal—Metal Bond. Structures of the Compounds (CO)4Cr[μ‐PMe2]2Ni(CO)2 and (CO)3Fe[μ‐PMe2, μ‐I]Fe(CO)3. Each with Two Different Complex Halves The crystal structures of the title complexes, one of which has two different carbonylmetal units and the other has two different bridging ligands, were determined. The stereochemistry of the CrNi complex is as expected, its metal—metal bond however is shorter than the average value of the corresponding Cr2 and Ni2 compounds. For the Fe2 complex the overall molecular geometry is also normal, but the metal—metal distance is considerably shorter than expected. The shortening of the metal—metal bonds is in both complexes correlated with the minimization of intramolecular steric strain.

show abstract

Platinum

Hartley¹

1982

Comprehensive Organometallic Chemistry

View full text Add to dashboard Cite

Structures of organo-transition metal complexes determined by diffraction methods. Reports appearing during 1977.

Cited by 3 publications

References 969 publications

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Stereochemie der Metall—Metall‐Bindung Die Strukturen der Verbindungen (CO)₄Cr[μ‐PMe₂]₂Ni(CO)₂ und (CO)₃Fe[μ‐PMe₂, μ‐I]Fe(CO)₃ mit je zwei verschiedenen Komplexhälften

Platinum

Contact Info

Product

Resources

About

Structures of organo-transition metal complexes determined by diffraction methods. Reports appearing during 1977.

Cited by 3 publications

References 969 publications

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Organouranium complexes of pyrazole and pyrazolate. Synthesis and x-ray structures of U(C5Me5)2Cl2(C3H4N2), U(C5Me5)2Cl(C3H3N2), and U(C5Me5)(C3H3N2)2

Stereochemie der Metall—Metall‐Bindung Die Strukturen der Verbindungen (CO)4Cr[μ‐PMe2]2Ni(CO)2 und (CO)3Fe[μ‐PMe2, μ‐I]Fe(CO)3 mit je zwei verschiedenen Komplexhälften

Platinum

Contact Info

Product

Resources

About

Stereochemie der Metall—Metall‐Bindung Die Strukturen der Verbindungen (CO)₄Cr[μ‐PMe₂]₂Ni(CO)₂ und (CO)₃Fe[μ‐PMe₂, μ‐I]Fe(CO)₃ mit je zwei verschiedenen Komplexhälften