DOI: 10.1002/anie.200463000. An Electron‐Deficient Iridium(<scp>III</scp>) Dihydride Complex Capable of Intramolecular CH Activation

An Electron‐Deficient Iridium(III) Dihydride Complex Capable of Intramolecular CH Activation

10.1002/anie.200463000

Crossref journal-article

Wiley

Angewandte Chemie International Edition (311)

Bibliography

Scott, N. M., Pons, V., Stevens, E. D., Heinekey, D. M., & Nolan, S. P. (2005). An ElectronâDeficient Iridium(III) Dihydride Complex Capable of Intramolecular Cï£¿H Activation. Angewandte Chemie International Edition, 44(17), 2512â2515. Portico.

Authors 5

Natalie M. Scott (first)
Vincent Pons (additional)
Edwin D. Stevens (additional)
D. Michael Heinekey (additional)
Steven P. Nolan (additional)

References 33 Referenced 93

{'key': 'e_1_2_2_2_2', 'volume-title': 'Principles and Applications of Organotransition Metal Chemistry', 'author': 'Collman J. P.', 'year': '1987'} / Principles and Applications of Organotransition Metal Chemistry by Collman J. P. (1987)
10.1002/ange.19971091004
10.1002/anie.199710481
10.1021/ar00172a001
10.1021/cr00013a015
10.1021/om000990x
10.1021/ar00051a009
10.1126/science.270.5244.1970
10.1021/cr00019a005
10.1021/ja970240n
10.1021/ja981727e
10.1002/(SICI)1521-3757(19990601)111:11<1733::AID-ANGE1733>3.0.CO;2-Z
10.1002/(SICI)1521-3773(19990601)38:11<1629::AID-ANIE1629>3.0.CO;2-L
10.1002/9780470166376.ch1
10.1002/(SICI)1521-3757(19980817)110:16<2298::AID-ANGE2298>3.0.CO;2-Y
10.1002/(SICI)1521-3773(19980904)37:16<2180::AID-ANIE2180>3.0.CO;2-A
10.1007/b113929 / Metal Dihydrogen and σ‐Bond Complexes: Structure, Theory and Reactivity by Kubas G. J. (2001)
10.1021/om020997
10.1021/ja970763v
10.1021/ja981727e
N. M. Scott R. Dorta L. Cavallo E. D. Stevens S. P. Nolan J. Am. Chem. Soc. 2005 127 in press. (10.1021/ja043249f)
3: A 500‐mL Fischer–Porter vessel was charged with [Ir(ItBu′)2](PF6) (200 mg 0.280 mmol) and dichloromethane (20 mL) in a glovebox. The vessel was taken out of the box connected to a Schlenk line and pressurized with H2gas (2.5 atm). The solution was then stirred for 3 days. The solvent volume was reduced to 3 mL and then pentane (10 mL) was added which resulted in the immediate precipitation of a pale‐yellow solid. The supernatant solution was decanted and the solid washed with pentane (3×5 mL) and dried in vacuo (186 mg 95 % yield).1H NMR (750 MHz CD2Cl2):δ=7.18 (s 4 H CH‐imidazole) 1.55 (s 36 H (CH3)3) −29.03 ppm (s 2 H H);31P NMR (161.90 MHz CD2Cl2):δ=−138.67 ppm (sept J=710.4 Hz);19F NMR (376.28 MHz CD2Cl2):δ=−72.51 −74.39 ppm (J=710.8 Hz);13C NMR (100.56 MHz CD2Cl2):δ=168.14 (C‐carbene) 118.45 (C‐imidazole) 58.68 (C(CH3)3) 29.66 ppm (C(CH3)3). Elemental analysis (%) calcd for C22H42N4F6PIr (699.78): C 37.76 H 6.05 N 8.01; found: C 37.85 H 6.02 N 7.94.
10.1021/ja035166p
Crystal data for3: C22H42F6IrN4P Mr=699.77 orthorhombicPbcn a=9.8783(5) b=22.0515(12) c=12.4453(7) Å 2711.0(3) Å3 T=150(2) K Z=4 μ(MoKα)=0.711 mm−1 23 556 reflections collected (1779 independent) R1 [I>2σ(I)=0.0334 wR2 (all data)=0.0608. Towards the end of the refinement the Fourier difference map showed all the hydrogen atoms associated with the ItBu unit as well as two peaks in positions consistent with the presence of two hydride ligands which was in accordance with the NMR spectroscopic analysis. Therefore the position of all the hydrogen atoms and hydride ligands were refined in the final least‐squares cycles without constraints by using an isotropic temperature factor. The refined positional parameters gave an acceptable geometry and were left without correction. CCDC‐255338 (3) contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
10.1039/a801330f
Identical1H 13C 31P and19F NMR spectroscopic characterization to that already reported for [Ir(ItBu′)2(CO)2](PF6)[6]was obtained.
10.1002/ange.200390002
10.1002/anie.200390035
10.1021/ja049545

Dates

Type	When
Created	20 years, 5 months ago (March 22, 2005, 4:18 a.m.)
Deposited	1 year, 10 months ago (Oct. 11, 2023, 4:57 a.m.)
Indexed	1 month, 1 week ago (July 25, 2025, 6:11 a.m.)
Issued	20 years, 4 months ago (April 21, 2005)
Published	20 years, 4 months ago (April 21, 2005)
Published Online	20 years, 4 months ago (April 21, 2005)
Published Print	20 years, 4 months ago (April 22, 2005)

Funders 0

None

BibTeX

@article{Scott_2005, title={An Electron‐Deficient Iridium(<scp>III</scp>) Dihydride Complex Capable of Intramolecular CH Activation}, volume={44}, ISSN={1521-3773}, url={http://dx.doi.org/10.1002/anie.200463000}, DOI={10.1002/anie.200463000}, number={17}, journal={Angewandte Chemie International Edition}, publisher={Wiley}, author={Scott, Natalie M. and Pons, Vincent and Stevens, Edwin D. and Heinekey, D. Michael and Nolan, Steven P.}, year={2005}, month=apr, pages={2512–2515} }

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