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Volumn 120, Issue 7, 1998, Pages 1447-1455

Experimental electron density studies for investigating the metal π- Ligand bond: The case of bis(1,5-cyclooctadiene)nickel

Author keywords

[No Author keywords available]

Indexed keywords

BIS(1,5 CYCLOOCTADIENE)NICKEL; METAL; NICKEL; UNCLASSIFIED DRUG;

EID: 0032564853     PISSN: 00027863     EISSN: None     Source Type: Journal    
DOI: 10.1021/ja972558l     Document Type: Article
Times cited : (107)

References (75)
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    • See, for instance: (a) Rees, B.; Coppens, P. Acta Crystallogr. 1973, B29, 2516-2527. (b) Rees, B.; Mitschler, A. J. Am. Chem. Soc. 1976, 98, 7918-7924. (c) Nielsen, F. S.; Lee, P.; Coppens, P. Acta Crystallogr. 1986, 359-364.
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    • See, for instance: (a) Rees, B.; Coppens, P. Acta Crystallogr. 1973, B29, 2516-2527. (b) Rees, B.; Mitschler, A. J. Am. Chem. Soc. 1976, 98, 7918-7924. (c) Nielsen, F. S.; Lee, P.; Coppens, P. Acta Crystallogr. 1986, 359-364.
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    • note
    • 6 delocalized π-systems coordinated to a transition metal atoms. Moreover, a QTAM analysis has not been performed in these works.
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    • The test has been performed on 2-[(4-butyl-2-methyl-6-oxo-5-{4-[2-(1H-tetrazol-5yl)phenyl]benzyl}-1H-pyrimidin- 1-yl)methyl]-3-thiophenecarboxylate (LR-B/081), a pharmacological compound. See: (a) Destro, R.; Soave, R. Acta Crystallogr. 1995, C51, 1383-1385 for its room temperature geometry; a complete report of this test is in press [(b) Macchi, P.; Proserpio, D. M.; Sironi, A.; Soave, R.; Destro, R. J. Appl. Crystallogr.] and a short description is here added as Supporting Information. We thank Prof. R. Destro, Dr. P. Roversi, and Dr. R. Soave for kindly supplying a few low-temperature data sets for this (and other) tests.
    • (1995) Acta Crystallogr. , vol.C51 , pp. 1383-1385
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    • The test has been performed on 2-[(4-butyl-2-methyl-6-oxo-5-{4-[2-(1H-tetrazol-5yl)phenyl]benzyl}-1H-pyrimidin- 1-yl)methyl]-3-thiophenecarboxylate (LR-B/081), a pharmacological compound. See: (a) Destro, R.; Soave, R. Acta Crystallogr. 1995, C51, 1383-1385 for its room temperature geometry; a complete report of this test is in press [(b) Macchi, P.; Proserpio, D. M.; Sironi, A.; Soave, R.; Destro, R. J. Appl. Crystallogr.] and a short description is here added as Supporting Information. We thank Prof. R. Destro, Dr. P. Roversi, and Dr. R. Soave for kindly supplying a few low-temperature data sets for this (and other) tests.
    • J. Appl. Crystallogr.
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    • note
    • 2 this ratio is considerably high, S = 0.83.
  • 26
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    • note
    • The greatest difference in accuracy and overall costs between a conventional detector and a CCD area-detector collection is reached when dealing with large cell volumes, nevertheless the best absolute accuracy is still available when dealing with small volumes.
  • 27
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    • The contamination of λ/2 has been demonstrated to be negligible for both crystal structure determination (Kirschbaum, K.; Martin, A.; Pinkerton, A. A. J. Appl. Crystallogr. 1997, 30, 514-516) and accurate charge density studies (ref 7b), thus a high voltage setting is not incorrect.
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    • note
    • This strategy provided 77% of data in 2θ < 96°(99% in 2θ < 66°).
  • 33
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    • note
    • Whenever a mean value is reported in the text or in the tables, the value in parentheses is the standard deviation of the average.
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    • Wilson, A J. C., Ed.; Kluwer Academic Publishers: Dordrecht
    • We applied the statistical test reported in: Prince, E.; Spiegelman, C. H. In International Tables for Crystallography Wilson, A J. C., Ed.; Kluwer Academic Publishers: Dordrecht, 1995; Vol. C, pp 618-624. (This has been already employed for comparing different refinements in electron density determinations; see ref 2d. We use it to verify that the expansion of the set of parameters by including a higher multipole gave significant improvement to the fit.
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    • note
    • In references 4f and 4g the authors demonstrated the important contribution of expanded 4s orbitals and that taking into account contracted 3d orbitals only produces a significant loss in model flexibility.
  • 44
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    • note
    • We have used a coordinate system defined by the three (orthogonal) 2-fold axes in the symmetrized molecule.
  • 54
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    • note
    • 2|) and their eigenvectors are perpendicular to the bond path.
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    • note
    • Of course, the atomic electronic structure is not considered in this context.
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    • note
    • 2 no ambiguity arises (vide infra).
  • 65
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    • note
    • -5.
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    • note
    • i less than its esd).
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    • note
    • 3 cycle.
  • 71
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    • -3]. Moreover, some longer contacts may exhibit other cp's, while we have considered only H-H contacts smaller than 2.8 Å(further work is in progress to have a complete picture of the intermolecular interactions but the major focus here is on intramolecular bonding features).
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    • note
    • i ≈ 0°. However in refs 38 and 39 bond path angles are not reported, thus a comparison is not possible.


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.