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Presentation of Data in the Experimental Section Physical and Spectroscopic Data (Example)
M. p. 41 °C.
– B.p. 120 °C/0.018 mbar.
– UV/Vis (CH2Cl2): l max(lg e max ) = 321 nm (3.86).
–
Crystallographic Data The following essential crystallographic information must be given in the text (Experimental Section) or in tabular form: Crystal shape and size, empirical formula, relative molecular mass, crystal system, space group with number as listed in the International Tables, unit cell dimensions ( a, b, c, in Å or pm, a , b , g in degrees) with estimated standard deviations in units of the last significant figure in parentheses, number of molecules (formula units) in unit cell, calculated and/or measured density, linear absorption coefficient, total of electrons in unit cell, temperature of data collection. Type of diffractometer and radiation used, monochromator, data collection mode (scan type and width), q range and reciprocal lattice segments measured, number of reflections measured, number of symmetry-independent reflections, cut-off criterion if applied, method of absorption and/or decay correction. Method of structure solution and refinement, number of positional and atomic displacement parameters refined, restraints and constraints if applied, final R and Rw values (in decimal numbers) for the data set used in the final refinement (for non-centrosymmetric crystal structures also the Flack parameter x has to be refined), information on the weighting scheme used in the refinement, residual electron density. Programs used (with references). Complete tables with positional parameters, displacement parameters, bond angles and interatomic distances will be printed only if these data are indispensable for the discussion of the structure. Deposition of Crystal Structure Data Crystal structure data of compounds not containing C–H bonds must be deposited by the authors at Fachinformationszentrum (FIZ) Karlsruhe. E-mail to: crysdata@fiz-karlsruhe.de. Further information: http://www.fiz-informationsdienste.de/en/DB/icsd/depot.html. The following standard footnote should appear in the manuscript:
Further details of the crystal structure investigation may be obtained from Fachinformationszentrum Karlsruhe, 76344 Eggenstein-Leopoldshafen, Germany (fax: +49-7247-808-666; e-mail: crysdata@fiz-karlsruhe.de, http://www.fiz-informationsdienste.de/en/DB/icsd/depot_anforderung.html) on quoting the deposition number CSD-######. Crystal structure data of compounds containing C–H bonds must be deposited by the authors at the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK, and the respective CCDC number must be provided at the time of manuscript submission. E-mail to: deposit@ccdc.cam.ac.uk. Further information: http://www.ccdc.cam.ac.uk. The following standard footnote should appear in the manuscript:
CCDC ###### 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. Crystal structure data of metals and alloys have to be deposited at The Metals Database (CRYSTMET®). See http://www.tothcanada.com/ for details. |
= –15.4 (c =
0.15, CHCl3).
– IR (film): n = 1738 (C=O), 1439, 1325, 1260, 1201, 1167, 1081 cm–1.
– 1H NMR (500.14 MHz, CDCl3):
d = 1.06, 1.07, 1.15, 1.17
(4 × d, 12 H, CHMe), 2.00 (d, J = 4.1 Hz, 1 H, 4-H),
2.50 (dd, J = 4.1, 3.4 Hz, 1 H, 3a-H), 3.68 (s, 3 H, OMe), 3.69 (s, 3 H, OMe),
4.01 (d, 2J = 10.3 Hz, 3-H1),
4.21 (dd, 2J = 10.3 Hz,
3J = 3.4 Hz, 3-H2).
– 13C NMR (125.76 MHz, CDCl3):
d = 12.04 (SiCH),
13.18 (SiCH), 16.64, 16.89, 17.37, 17.51 (all CHMe), 25.80 (C-4), 27.78 (C-4a), 30.73 (C-3a),
51.95 (OMe), 52.00 (OMe), 67.07 (CH2), 170.33 (C=O), 170.84 (C=O).
– 29Si{1H} NMR:
d = 28.18.
– MS (EI, 70 eV): m/z (%) = 453 (100) [M–Cl]+.
HRMS ((+)-ESI): m/z = 365.03250
(calcd. 365.03258 for C16H24O8SNa, [M+Na]+) –
C14H24O5Si (300.4): calcd. C 55.97, H 8.05; found C 55.82, H 8.01.