103 Une suspension de [(pcym )RuCl 2 ] 2 (140 mg, 0,23 mmol) et de NH 4 PF 6 (78,2 mg, 0,48 mmol) dans 5 mL de pyridine, est laissée sous agitation pendant 3 jours, durant lesquels un précipité blanc de NH 4 Cl apparaît. La solution est filtrée, puis le solvant est évaporé sous vide. L'huile obtenue est alors être triturée dans l'éther pour conduire à un solide orangé ,
RMN 13 C{ 1 H} (101 MHz, CD 2 Cl 2 ): C Ph non visibles, pp.37081-1382874531203 ,
Des cristaux adaptés à une étude par diffraction des rayons X ont été obtenus par évaporation lente d'une ,
s, CH p-cym ), 33,04 (s, H 2 C 9BBN (s, H 3 C, (s, H 2 CB) MHz, CD 2 Cl 2 ) ? = 86,3. Analyse élémentaire pour C 33 H 44 RuCl 4 PB (en accord avec une molécule de CH 2 Cl 2 par molécule de [(pcym )RuCl 2 ((Ph) 2 PCH 2 CH 2 B(9-BBN))] à l'état cristallin): % calculé, p.321240544858049904282410 ,
10 (d, 3 J H,H = 6 Hz, RMN 13 C{ 1 H} (75 MHz, CD 2 Cl, pp.542650888-155 ,
s, CH p-cym, pp.733404465350619632-93 ,
(s, C p-cym ) (s, HC iPr, (s, H 2 C 9BBN ) CCN), H 2 CB et CN acétonitrile non visibles. RMN 11 B{ 1 H} (75 MHz, CD 2 Cl 2 ): ? = 87, pp.5338988158473015021278009258-3 ,
La solution est agitée pendant une heure, puis évaporée à sec et le solide obtenu est lavé au pentane. 20 est obtenu sous la forme d'un solide rouge, p.80 ,
RMN 13 C{ 1 H} (75 MHz, CD 2 Cl 2 ): ? = 133, p.40 ,
(s, CH p-cym ) (s, H 3 C iPr(p-cym)RuCl(PEtPh 2 )(CH 3 CN))][BF 4 ] (21) A un mélange de 20 (311 mg, 0,60 mmol) et de tétrafluoroborate d'argent (122 mg, 0,63 mmol) protégé de la lumière est ajoutée une solution d'acétonitrile (91 mg, puis filtré et évaporé à sec. Le solide obtenu est lavé au pentane. 21 est obtenu sous la forme d'un solide jaune, pp.4114457143559702070322-2 ,
09 (d, 3 J H,H = 7 Hz, 3H, H 3 C iPr ), 0.89 (td, 3 J H,H = 8 Hz, pp.22-39 ,
21 (s, C p-cym ), 100.95 (s, C p-cym ), 90.84 (s, CH p-cym ), 90.51 (s, CH p-cym ), 89.72 (s, CH p-cym ), pp.131-363086807125 ,
12 (s, CH pcym, pp.07445435387942-3 ,
Analyse élémentaire pour C 24 H 28 RuClP: % calculé:C, 59.55 ,
I>2sigma(I)] R1 = 0.0685, wR2 = 0.1647 R indices (all data) ,
I>2sigma(I)] R1 = 0.0663, wR2 = 0.1613 R indices (all data) ,
I>2sigma(I)] R1 = 0.0766, wR2 = 0.1300 R indices (all data) ,
I>2sigma(I)] R1 = 0.0316, wR2 = 0.0545 R indices (all data) ,
Zur Addition von Alkyldichlorboranen an Bis(??5-cyclopentadienyl)dihydridowolfram, Chemische Berichte, vol.79, issue.9, p.1613, 1994. ,
DOI : 10.1002/cber.19941270910
Coordination of metal carbonyl anions to triphenylaluminum, -gallium, and -indium and the crystal structure of tetraethylammonium triphenyl((.eta.5-cyclopentadienyl)dicarbonyliron)aluminate(Fe-Al), Inorganic Chemistry, vol.18, issue.4, p.1097, 1979. ,
DOI : 10.1021/ic50194a040
with Main Group Metal Alkyls and Aryls:?? Synthesis and Structure of Three Novel Ir???Al and Ir???Mg Heterobimetallics, Journal of the American Chemical Society, vol.120, issue.1, p.223, 1998. ,
DOI : 10.1021/ja973230v
Scorpionates : the coordination chemistry of polypyrazolylborate ligands, 1999. ,
DOI : 10.1142/p148
Platinum(0) Complex, Organometallics, vol.23, issue.24, p.5656, 2004. ,
DOI : 10.1021/om040114+
) (mt = Methimazolyl, R = mt, H), Organometallics, vol.24, issue.6, p.1062, 2005. ,
DOI : 10.1021/om040128f
The transition-metal-hydrogen bond, Chemical Reviews, vol.85, issue.1, p.41, 1985. ,
DOI : 10.1021/cr00065a002
Basicities of Transition Metal Complexes from Studies of Their Heats of Protonation: A Guide to Complex Reactivity, Accounts of Chemical Research, vol.28, issue.2, p.51, 1995. ,
DOI : 10.1021/ar00050a001
An Unambiguous Electron-Counting Notation for Metallaboratranes, Organometallics, vol.25, issue.20, p.4741, 2006. ,
DOI : 10.1021/om0602512
A Dramatic Effect of Lewis-Acid Catalysts on Nickel-Catalyzed Carbocyanation of Alkynes, Journal of the American Chemical Society, vol.129, issue.9, p.2428, 2007. ,
DOI : 10.1021/ja067364x
Co-operative effect of Lewis acids with transition metals for organic synthesis, Chemical Society Reviews, vol.41, issue.9, p.1395, 2007. ,
DOI : 10.1039/b608694m
???Lebende Polymere??? bei Ziegler-Katalysatoren extremer Produktivit??t, Angewandte Chemie, vol.15, issue.5, p.396, 1980. ,
DOI : 10.1002/ange.19800920517
Cocatalysts for Metal-Catalyzed Olefin Polymerization:?? Activators, Activation Processes, and Structure???Activity Relationships, Chemical Reviews, vol.100, issue.4, p.1391, 2000. ,
DOI : 10.1021/cr980462j
Theoretical studies of the structure and function of MAO (methylaluminoxane), Progress in Polymer Science, vol.29, issue.2, p.107, 2004. ,
DOI : 10.1016/j.progpolymsci.2003.10.003
Cation-like homogeneous olefin polymerization catalysts based upon zirconocene alkyls and tris(pentafluorophenyl)borane, Journal of the American Chemical Society, vol.113, issue.9, p.3623, 1991. ,
DOI : 10.1021/ja00009a076
Pd(R)(CN), Organometallics, vol.18, issue.3, p.297, 1999. ,
DOI : 10.1021/om980897x
Lewis Acid Acceleration of C???N Bond-Forming Reductive Elimination from Heteroarylpalladium Complexes and Catalytic Amidation of Heteroaryl Bromides, Journal of the American Chemical Society, vol.129, issue.25, p.7734, 2007. ,
DOI : 10.1021/ja0722473
), Organometallics, vol.19, issue.8, p.1599, 2000. ,
DOI : 10.1021/om9909744
Functional trimethylphosphine derivatives. 21. (Phosphinomethyl)aluminum compounds: phosphinomethyl-bridged dimers and x-ray structures of [Me2AlCH2PMe2]2 and [ClAl(CH2PMe2)2]2, Organometallics, vol.4, issue.2, p.231, 1985. ,
DOI : 10.1021/om00121a004
1,1,4,4-Tetramethyl-1,4-diazonia-2,5-diboratacyclohexane. Crystal structure and a new preparation, Inorganic Chemistry, vol.14, issue.2, p.330, 1975. ,
DOI : 10.1021/ic50144a025
Synthesis, structural characterization and reactivity of the amino borane 1-(NPh2)-2-[B(C6F5)2]C6H4, Journal of Organometallic Chemistry, vol.680, issue.1-2, p.218, 2003. ,
DOI : 10.1016/S0022-328X(03)00384-X
)boron, Organometallics, vol.17, issue.1, p.123, 1998. ,
DOI : 10.1021/om9708236
Synthesis and structure of potential Lewis acid???Lewis base bifunctional catalysts: 1-N,N-dimethylamino-8-borononaphthalene derivatives, Journal of Organometallic Chemistry, vol.680, issue.1-2, p.257, 2003. ,
DOI : 10.1016/S0022-328X(03)00399-1
Preparation and Some Reactions of (Acylamino)diorganoboranes, Chemische Berichte, vol.122, issue.3, p.565, 1993. ,
DOI : 10.1002/cber.19931260303
Nuclear Magnetic Resonance Spectroscopy of Boron Compounds, 1978. ,
DOI : 10.1007/978-3-642-66757-2
The synthesis and separation of the isomeric compounds dimeric dimethyl(2-pyridyl)borane and dimethylboronium bis(2-pyridyl)dimethylborate, Inorganic Chemistry, vol.32, issue.26, p.6115, 1993. ,
DOI : 10.1021/ic00078a034
Bis(enamino-Cp) Group 4 metal complex chemistry: developing a Mannich-type carbon???carbon coupling reaction at the bent metallocene famework, Journal of Organometallic Chemistry, vol.690, issue.1, p.14, 2005. ,
DOI : 10.1016/j.jorganchem.2004.08.021
= 0???3):?? Poor Performance of the B3LYP Approach for Dative B???N Bonds, The Journal of Physical Chemistry A, vol.108, issue.13, p.2550, 2004. ,
DOI : 10.1021/jp031242z
Study of the Dative Bond in 2-Aminoethoxydiphenyl Borate at Various Levels of Theory:?? Another Poor Performance of the B3LYP Method for B???N Dative Bonds, The Journal of Physical Chemistry A, vol.109, issue.51, p.12014, 2005. ,
DOI : 10.1021/jp054479z
Organic Synthesis, The Role of Boron and Silicon, p.9, 1991. ,
Dimesitylborane monomer-dimer equilibrium in solution, and the solid-state structure of the dimer by single crystal neutron and X-ray diffraction, Journal of Organometallic Chemistry, vol.680, issue.1-2, p.165, 2003. ,
DOI : 10.1016/S0022-328X(03)00316-4
Derivatives of the Dimethylbis(2-pyridyl)borate(1???) Ion:?? Synthesis and Structure, Inorganic Chemistry, vol.35, issue.7, p.2140, 1996. ,
DOI : 10.1021/ic950775m
Boron-Nitrogen Compounds, Anorganishe und Allgemeine Chemie in Einzeldarstellungen VI, p.16, 1965. ,
The Potential of Palladacycles:?? More Than Just Precatalysts, Chemical Reviews, vol.105, issue.6, p.2527, 2005. ,
DOI : 10.1021/cr030681r
Organoborane Chemistry, p.91, 1975. ,
Nuclear magnetic resonance studies in coordination chemistry X. The reactions of (??-methallyl)palladium chloride containing various phosphines with 1,5-cyclooctadiene-rhodium chloride dimer, Journal of Organometallic Chemistry, vol.20, issue.1, p.219, 1969. ,
DOI : 10.1016/S0022-328X(00)80109-6
New neutral and cationic ??6-arene ruthenium complexes with phosphine and amine ligands: syntheses and molecular structures of [(??6-p-cymene)Ru(NH2CH2C6H5)Cl2], [(??6-C6Me6)Ru(PPh2Py)Cl2] and [(??6-C6Me6)Ru(PPh2Py)Cl]+, Polyhedron, vol.23, issue.18, p.3115, 2004. ,
DOI : 10.1016/j.poly.2004.09.031
Facile preparation of ??6-p-cymene ruthenium diphosphine complexes. Crystal structure of [(??6-p-cymene)Ru(dppf)Cl]PF6, Journal of Organometallic Chemistry, vol.556, issue.1-2, p.151, 1998. ,
DOI : 10.1016/S0022-328X(97)00776-6
Synthesis and structure of cyclic phosphine???boranes, Journal of Organometallic Chemistry, vol.529, issue.1-2, p.323, 1997. ,
DOI : 10.1016/S0022-328X(96)06616-8
CRC Handbook of Phosphorus-31 Nuclear Magnetic resonance Data, 1991. ,
Mechanistic Investigations on the Hydrogenation of Alkenes Using Ruthenium(II)-arene Diphosphine Complexes, Organometallics, vol.23, issue.21, p.4849, 2004. ,
DOI : 10.1021/om049665q
Asymmetric hydrosilylation of ketones catalyzed by ruthenium complexes with chiral tridentate ligands, Journal of Organometallic Chemistry, vol.547, issue.1, p.97, 1997. ,
DOI : 10.1016/S0022-328X(97)00201-5
Catalytic Asymetric Synthesis, p.111, 2000. ,
Synthesis of monohydridohexamethylbenzeneruthenium(II) complexes containing group V donor ligands. Isomerism arising from cyclometallation of a tertiary phosphine at aliphatic and aromatic carbon atoms, Journal of Organometallic Chemistry, vol.272, issue.2, p.189, 1984. ,
DOI : 10.1016/0022-328X(84)80466-0
Synthesis and properties of alkylruthenium complexes bearing primary and secondary amine ligands, Journal of Organometallic Chemistry, vol.692, issue.1-3, p.408, 2007. ,
DOI : 10.1016/j.jorganchem.2006.04.047
Comprehensive Organometallic Chemistry II, p.480, 1995. ,
Density???functional thermochemistry. III. The role of exact exchange, The Journal of Chemical Physics, vol.98, issue.7, p.5648, 1993. ,
DOI : 10.1063/1.464913
Development of the Colle-Salvetti correlation-energy formula into a functional of the electron density, Physical Review B, vol.37, issue.2, p.785, 1988. ,
DOI : 10.1103/PhysRevB.37.785
A theoretical method to determine atomic pseudopotentials for electronic structure calculations of molecules and solids, Theoretica Chimica Acta, vol.10, issue.4, p.283, 1975. ,
DOI : 10.1007/BF00963468
Self-consistent perturbation theory of diamagnetism, Molecular Physics, vol.2, issue.4, p.789, 1974. ,
DOI : 10.1021/ja00776a006
Efficient implementation of the gauge-independent atomic orbital method for NMR chemical shift calculations, Journal of the American Chemical Society, vol.112, issue.23, p.8251, 1990. ,
DOI : 10.1021/ja00179a005
Organometallics in synthesis. A manual. 2 nd ed, p.473, 2004. ,
??-Bonded 2-Phenylpyridine Palladium Complex, Bulletin of the Chemical Society of Japan, vol.41, issue.5, p.1272, 1968. ,
DOI : 10.1246/bcsj.41.1272