Insights into the elimination of HCHO from the clusters [MnCOm(COOMe)]- (Mn = Ru6C, m = 16; Mn = Rh6, m = 15) provided by electrospray mass spectrometry f

Journal of the Chemical Society, Dalton Transactions

Volumn , Issue 12, 2000, Pages 1813-1815

  Dyson, Paul J ^a   Feeder, Neil ^a   Johnson, Brian F G ^a   Scott Mclndoe, J ^a   Langridge Smith, Patrick R R ^a  

^a UNIVERSITY OF YORK   (United Kingdom)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0002247558     PISSN: 1470479X     EISSN: None     Source Type: Journal    
DOI: 10.1039/b002978p     Document Type: Article

References (25)

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14. EDESI mass spectra were collected using a Micromass Quattro LC instrument in negative-ion mode, with methanol as the mobile phase. The nebuliser tip was at 3100 V and 90 °C, and nitrogen was used as the bath gas. Samples were introduced directly to the source at 4 uL min"1 via a syringe pump. Data collection was carried out in continuum mode with the cone voltage initially set at 0 V. A scan time of 10 seconds per spectrum and a low resolution setting (peak width at half-height =:0.8 Da) was used to maximise the signal-to-noise ratio. The cone voltage was manually increased by increments of 1 V after every scan up to a maximum of 200 V. A full scan from 0-200 V therefore took approximately 35 minutes to collect.
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18. Given the reaction conditions, it is possible that the compound is actually the electron-precise cluster [H,Ru6C(CO)15]. The fact that the metal hydride signal in the 'H NMR spectrum splits into two singlets in a 2:1 ratio at low temperature indicates that [H3Ru6C(CO),5] is a more likely candidate than the unprecedented unsaturated cluster [HRu6C(CO)15].
19. ESI-FTICR mass spectra were recorded on a Bruker Bio-Apex II FTICR instrument in the negative-ion mode, with methanol as the mobile phase.
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24. -1.
25. Crystal data for CJ5HjjNO18P2Ru6 la: M= 1664.18, monoclinic, 0 = 37.43090(10), 6 = 9.2751(2), c = 33.8359(ll) A, /? = 103.9600(10)°, U= 11400.0(4) A3, T= 180(2) K, space group C2lc, Z = 8, /l(Mo-K) = 0.71070 A, /<= 1.678 mm"1, 21175 reflections collected, 9566 unique (Rmt = 0.0523) which were used in all calculations. The final ii\R(F2) was 0.0898 (all data). Single crystals of [N(PPh,)2][Ru6C(CO)16(COOMe)] were crystallised from hexane/ dichloromethane, mounted in inert oil and transferred to the cold gas stream of the diffractometer. The structure was solved using direct methods and refined by full-matrix least-squares on F2. CCDC reference number 186/1986. See http://www.rsc.org/ suppdata/dt/bO/b002978p/ for crystallographic files in .cif format.