All experimental manipulations were performed under purified dry nitrogen using standard Schlenk and vacuum line techniques. Solvents were dried and freshly distilled under an atmosphere of nitrogen prior to use [26 ]. The chemicals Mo(CO)6, W(CO)6, Cr(CO)6, chlorodiphenylphosphine, and p-aminoacetophenone were purchased from Aldrich and used as received. N-(4-acetylphenyl)-N-(diphenylphosphino)amine ligand (1 ) was previously prepared [19 ]. Infra-red spectra were recorded with a PerkinElmer System 2000 FT-IR spectrometer between 4000 and 400 cm−1 using KBr disks. Microanalyses were performed on a Flash 2000 elemental analyzer. Infra-red spectra were recorded on a Shimadzu FTIR-8400S spectrometer between 4000-400 cm−1 using KBr disks. The NMR spectra were recorded at 25 °C on a Bruker-Avance-DRX-400 MHz NMR spectrometer operating at 400.17 (1H), 100.63 (13C), and 161.98 (31P) using tetramethylsilane for 1H and 85% H3PO4 for 31P NMR as external standards. Melting points were carried out on a Gallenkamp apparatus with open capillaries.
Cr co 6
Manufactured by Merck Group
Sourced in United States
Cr(CO)6 is a chemical compound consisting of chromium and carbon monoxide. It is a crystalline solid that is used as a precursor in various chemical processes.
Automatically generated - may contain errors
Lab products found in correlation
Mo co 6, by Merck Group (2 mentions)
System 2000 ftir spectrometer, by PerkinElmer (1 mentions)
Ftir 8400s spectrometer, by Shimadzu (1 mentions)
Avance drx 400 mhz nmr spectrometer, by Bruker (1 mentions)
W co 6, by Merck Group (1 mentions)
N n dimethylformamide (dmf), by Merck Group (1 mentions)
Chloranil, by Merck Group (1 mentions)
Pyrrole, by Merck Group (1 mentions)
K2cr2o7, by Merck Group (1 mentions)
4 protocols using cr co 6
1
Synthesis and Characterization of Phosphino-Amine Complexes
2
Synthesis of K8SnSb4 under Inert Conditions
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All manipulations and reactions were performed under a nitrogen atmosphere using standard Schlenk or glovebox techniques. En (Aldrich, 99%) and DMF (Aldrich, 99.8%) were freshly distilled by CaH2 prior to use, and stored in N2 prior to use. Tol (Aldrich, 99.8%) was distilled from sodium/benzophenone under nitrogen and stored under nitrogen. [2.2.2]-crypt (4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo (8.8.8) hexacosane, purchased from Sigma-Aldrich, 98%) was dried in a vacuum for one day prior to use. K8SnSb4 was prepared by heating a stoichiometric mixture of the elements (K: 625.6 mg, Sn: 237.4 mg, Sb: 974.4 mg; K: +99%, Sn: 99.999%, Sb: 99.9%, all from Strem) at a rate of 70 °C per hour to 700 °C and keeping it for 36 h in sealed niobium containers closed in evacuated quartz ampules according to the previous procedures26 (link). The K8SnSb4 solid was obtained with a high yield (~92%, 1.7 g) and stored under a dry nitrogen atmosphere in a glove box. Cr(CO)6 and Mo(CO)6 were purchased from Aldrich while Ag4Mes4 and Cu(PPh3) Cl were synthesized according to the literature with a yield of 55 and 60%, respectively58 (link),59 (link).
3
Synthesis of Chromium Corrole and Porphyrin Complexes
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Pyrrole, chloranil, Cr(CO)6, and
TBAP (tetrabutylammonium perchlorate) were purchased from Sigma-Aldrich
(USA). p-Cyanobenzaldehyde was purchased from Merck
(India). Hexane and dichloromethane were obtained via distillation from KOH and CaH2, respectively. The rest
of the starting chemicals were of reagent grade. Oxo-[5,10,15-tris(p-cyanophenyl)corrolato]chromium(V),1 , was
synthesized by following a literature-reported method.39 (link) (Saloph)MnV(N) was prepared by following
a literature-reported method.41 (link) 5,10,15-Tris(4-cyanophenyl)corrole
was prepared according to a literature-reported protocol.24 (link) The chloro(porphyrinato)chromium(III) complex,4 , was also prepared by following a literature-reported method.38f
TBAP (tetrabutylammonium perchlorate) were purchased from Sigma-Aldrich
(USA). p-Cyanobenzaldehyde was purchased from Merck
(India). Hexane and dichloromethane were obtained via distillation from KOH and CaH2, respectively. The rest
of the starting chemicals were of reagent grade. Oxo-[5,10,15-tris(p-cyanophenyl)corrolato]chromium(V),
synthesized by following a literature-reported method.39 (link) (Saloph)MnV(N) was prepared by following
a literature-reported method.41 (link) 5,10,15-Tris(4-cyanophenyl)corrole
was prepared according to a literature-reported protocol.24 (link) The chloro(porphyrinato)chromium(III) complex,
4
Chromium Complexes Synthesis and Purification
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Tetrahydrofuran (THF), benzene,
dichloromethane, acetonitrile, n-pentane, and diethyl
ether were dried via the method of Grubbs, using a custom-built solvent
purification system. Where required, compounds were maintained under
inert N2 atmospheres using Mbraun gloveboxes or standard
Schlenk techniques. K2Cr2O7, Cr(CO)6, Cr(η6-C6H6)2, and Cr(η6-C6H6)(CO)3 were purchased from Sigma–Aldrich and used without
further purification. Cp2Cr (Cp = cyclopentadienyl) was
purchased from Strem and used without further purification. The following
model compounds were prepared following literature procedures: Np4Cr (Np = neopentyl),18 Cr(OtBu)4,19 (tpfc)CrO
(tpfc = tris(pentafluorophenyl)corrole),20 (link) Cr(14-TMC)(O2)(Cl) (14-TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane),21 (link) [Cr(bpy3)](PF6)3 (bpy = 2,2′-bipyridine),22 [Cr(NH3)6](NO3)3,23 and (NH4)2[CrNCl4].24 (link)
dichloromethane, acetonitrile, n-pentane, and diethyl
ether were dried via the method of Grubbs, using a custom-built solvent
purification system. Where required, compounds were maintained under
inert N2 atmospheres using Mbraun gloveboxes or standard
Schlenk techniques. K2Cr2O7, Cr(CO)6, Cr(η6-C6H6)2, and Cr(η6-C6H6)(CO)3 were purchased from Sigma–Aldrich and used without
further purification. Cp2Cr (Cp = cyclopentadienyl) was
purchased from Strem and used without further purification. The following
model compounds were prepared following literature procedures: Np4Cr (Np = neopentyl),18 Cr(OtBu)4,19 (tpfc)CrO
(tpfc = tris(pentafluorophenyl)corrole),20 (link) Cr(14-TMC)(O2)(Cl) (14-TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane),21 (link) [Cr(bpy3)](PF6)3 (bpy = 2,2′-bipyridine),22 [Cr(NH3)6](NO3)3,23 and (NH4)2[CrNCl4].24 (link)
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