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Inorganic Chemistry
Volumn 46, Issue 22, 2007, Pages 9027-9029
A pillared discrete bilayer formed from guanidinium and ferrocenedisulfonate ions: Synthesis, crystal structure, and initial electrochemical properties
Author keywords

[No Author keywords available]
Indexed keywords

FERROCENE; FERROUS ION; GUANIDINE; ION; SULFONIC ACID DERIVATIVE;
EID: 35848951639     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic7011974     Document Type: Article
Times cited : (9)
References (24)
  • 13
    • 35848938803 scopus 로고    scopus 로고
    • Preparation of salt 1. Ferrocenedisulfonic acid (0.346 g; 1 mmol) was dissolved in DMF (10 ml, Guanidinium chloride (0.191g; 2 mmol) was added, and the solution stirred at room temperature for 10 min. After filtration, diethyl ether was allowed to diffuse into the solution providing yellow needlelike X-ray quality single crystals in 1 week. Yield, 0.376 g (81 , Anal. Calcd, ) for C12H20FeN6O6S 2, C 31.04, H 4.34, N 18.10, O 20.68, S 13.81. Found C 30.98, H 4.39, N 18.20, O 20.74, S 13.84, Chemical & MicroAnalytical Services Pty. Ltd, Belmont, VIC, Australia, 1H NMR (500 MHz, CD3) 2SO, 25 °C, δ 4.1 (s, C5H4, 4H, 4.3 (s, C5H4, 4H, 6.95 (s, C(NH2)3, 12H, Figure S1, FTIR data (νmax/cm-1, 3328(s, 3183(s, 2818(w, 1674(s, 1581(m, 1176(s, 1058(s, 1043(s, 1013(s, 891w, 824
    • 2-.
  • 15
    • 35848970866 scopus 로고    scopus 로고
    • Crystal data for 1: C12H20FeN 6O6S2, M, 464.31, triclinic, space group P1, a, 7.156(5) Å, b, 7.268(5) Å, c, 11.408(7) Å, α, 99.314-(14)°, β, 98.722(15)°, γ, 119.088(12, V, 493.1(5) Å3, Z, 1, D c, 1.564 g cm-3, λ, 0.71073 Å. Data on a crystal of dimensions 0.22 × 0.08 × 0.05 mm3 were collected at 293 K. GOF, 1.007. Total of 2132 reflections (1297 unique) with Rint, 0.0916, R1, 0.0889 (I > 2σ(I, wR2, 0.2660 (all data, CCDC 620270. The structure of 1 was solved using direct methods (SHELXL V5.1)7 from single-crystal data on a Bruker SMART/CCD area detector diffractometer fitted with Mo Kα radiation (λ, 0.71073 Å) and a graphite monochromator. Structure refinements
    • 7 All non-hydrogen atoms except the carbon atoms on ferrocene rings were refined with anisotropic thermal displacement parameters.
  • 21
    • 35848949649 scopus 로고    scopus 로고
    • Voltametric experiments were performed with an Autolab (Eco Chemie, Utrecht, Netherlands) computer-controlled electrochemical workstation. Media were CH3CN and CH3CN/H2O mixtures with 0.05 M Bu4N+BF4- or [C(NH2) 3]C1 as supporting electrolyte (see caption of Figure 3 for details, A standard three-electrode arrangement was used with a glassy carbon disk (d, 3 mm) as working electrode, a Pt wire as auxiliary electrode and a Ag/Ag, reference electrode (silver wire in MeCN (Bu4NBF 4 (0.1 M) AgNO3 0.01 M, Scan rate: 100 mV s -1, sample interval: 0.45 mV, sensitivity: 1 × 10-4 A V-1. All quoted potentials are referenced to the Fc+/Fc couple
    • +/Fc couple.
  • 24
    • 35848954611 scopus 로고    scopus 로고
    • The oxidative wave shape of Figure 3d is consistent with the symmetric shape expected for a surface-confined process. Deviation from that shape at high potentials is consistent with the background contribution from the diffusion-controlled oxidation of 1 in this saturated solution (Figure 3b).
    • The oxidative wave shape of Figure 3d is consistent with the symmetric shape expected for a surface-confined process. Deviation from that shape at high potentials is consistent with the background contribution from the diffusion-controlled oxidation of 1 in this saturated solution (Figure 3b).

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