Synthesis and reactivity of a mononuclear parent amido nickel complex. Structures of Ni[C6H3-2,6-(CH2P iPr2)2] (NH2) and Ni[C 6H3-2,6-(CH2PiPr2) 2](OMe)

Organometallics

Volumn 23, Issue 24, 2004, Pages 5653-5655

  Cámpora, Juan ^a   Palma, Pilar ^a   Del Río, Diego ^a   Conejo, M Mar ^a   Alvarez, Eleuterio ^a  

^a INSTITUTO DE INVESTIGACIONES QUÍMICAS   (Spain)

Author keywords

[No Author keywords available]

Indexed keywords

AMMONIA; CATALYSIS; CRYSTAL STRUCTURE; CRYSTALLINE MATERIALS; CRYSTALLOGRAPHY; DERIVATIVES; METHANOL; SOLUTIONS; SYNTHESIS (CHEMICAL); TRANSITION METALS;

AMIDO NICKEL COMPOUNDS; MONONUCLEAR HYDROXIDES; STRUCTURAL CHARACTERIZATION;

NICKEL COMPOUNDS;

EID: 10044228414     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om049312r     Document Type: Article

References (31)

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18. 2 ligands.
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20. 2) (1) was obtained as an orange crystalline solid after cooling to -30°C. Yield: 70%.
21. 9, Z = 8. The final r factor was 0.0422 for 10 027 independent reflections with I > 2a(7) (wR2 = 0.0922). GOF = 1.040.
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24. 2) was optimized using the B3LYP functional and the 6-311+G** basis set for all atoms: Ni-N = 1.883 Å, Ni-N-H(1) = 118.4°, Ni-N-H(2) = 119.2°, H(1)-N-H(2) = 105.5°.
25. 2. The reaction mixture was sonicated for 3 h and centrifuged and the solvent removed under reduced pressure. The solid residue was extracted with hexane and the resulting suspension centrifuged again. The orange solution of complex 1 was treated with 50 μL (1.2 mmol) of MeOH, the solvent removed under vacuum, and the solid residue dissolved in hexane. Complex 3 was isolated as a dark orange crystalline solid after adding some hexamethyldisiloxane and cooling to -30°C, Yield: 60%.
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28. 3, Z = 8. The final r factor was 0.0520 for 10 386 independent reflections with I > 2σ(I) (wR2 = 0.0898). GOF = 1.026.
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30. To a solution of 150 mg (0.36 mmol) of complex 1 in 8 mL of benzene was added 74 μL (0.73 mmol) of PhCHO. The mixture was stirred overnight at room temperature and then taken to dryness and the residue extracted with hexane (10 mL). After filtration, concentration, and cooling to -30°C several crops of orange crystals of complex 4 were isolated, some of them with a small amount of the hydroxide derivative 2.
31. 3 to a mixture of PhCHO and 2 causes the slow conversion of the latter in 4.