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Crystal Growth and Design

Volumn 7, Issue 9, 2007, Pages 1672-1675

Polymeric capsules and honeycomb aggregates formed by p-sulfonatocalix[6] arene with phenanthrolinium compounds

(4) Liu, Yu a Li, Qiang a Guo, Dong Sheng a Chen, Kun a

a NANKAI UNIVERSITY (China)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 34748911324 PISSN: 15287483 EISSN: None Source Type: Journal
DOI: 10.1021/cg0704854 Document Type: Conference Paper

Times cited : (22)

References (27)

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22
- 34748914123
- Crystal complexes of [C6AS6-+2H, Phen, 4·21H2O (1) and [C6AS 6, PPQ2+]3·31.5H2O (2) were prepared by the method of slow evaporation of solution, a) Preparation of complex 1: To an aqueous solution of C6AS (0.05 mmol, 20 mL) was added 6 equiv of Phen. Under stirring, 2 M HCl was dropped to adjust the pH to 1-2. After filtration, the filtrate was set aside to evaporate for 3 weeks. The colorless crystal that formed was then collected along with its mother liquor for the X-ray crystallographic analysis. 1H NMR (D 2O, δ, 8.99 (d, J, 4.8 Hz, 8H, Phen, 8.67 (d, J, 8.4 Hz, 8H, Phen, 7.93 (m, 16H, Phen, 7.23 (s, 12H, C6AS, 3.55 s, 12H, C6AS
- +), 7.23 (s, 12H, C6AS), 3.55 (s, 12H, C6AS).

23
- 34748874570
- 2+). The corresponding PXRD data of complexes 1 and 2 are shown in the Supporting Information.
- 2+). The corresponding PXRD data of complexes 1 and 2 are shown in the Supporting Information.

24
- 34748876469
- The X-ray intensity data for 1 and 2 were collected on a Rigaku MM-007 rotating anode diffractometer equipped with a Saturn CCD Area Detector System using monochromated Mo-Kα radiation at T, 113(2) K. Data collection and reduction were performed by program of Crystalclear. The structures were solved by using the direct method and refined employing full-matrix least squares on F2 (CrystalStructure, SHELXTL-97, a) Crystal data for 1: C90H108N 8O45S6, M, 2214.20, triclinic, space group P1̄, a, 11.862(2) Å, b, 18.883(3) Å, c, 22.445(4) Å, α, 96.668(3)°, β, 94.163(3)°, γ, 95.226(2)°, V, 4954.9(14) Å3, Z, 2, Dc, 1.484 g cm -3, λ(Mo-Kα, 0.71070 Å, T, 113(2) K, F000, 2320, μ, 0.239 mm-1
- 2 = 1.072. To satisfy charge balance, C6AS in 1 should possess two protonated sulfonate groups, which are acceptable given the pH of the reaction solution. The oxygen atoms of the sulfonate group (S5) are disordered over two positions. In addition, there are two very similar host-guest complex units in complex 1, so there are likewise two kinds of polymeric capsules. We give only the data of one, and the other is negligibly discussed in this text.

25
- 34748832151
- Crystal data for 2: C87H 185N6O55.50S6, M, 2395.77, triclinic, space group P1̄, a, 18.256(3) Å, b, 18.995(3) Å, c, 20.708(4) Å, α, 104.437(3)°, β, 107.218(6)°, γ, 109.746(8)°, V, 5948.7(17) Å3, Z, 2, Dc, 1.338 g cm-3, λ(Mo-Kα, 0.71070 Å, T, 113(2) K, F(000, 2578, μ, 0.209 mm-1, approximate crystal dimensions 0.34 × 0.26 × 0.20 mm3, θ range, 1.24-25.00°, reflections collected/unique, 43 950/20 542 (R int, 0.0717, final R indices [I > 2σ(I, R1, 0.1415, wR2, 0.3945, R indices (ail data) R1, 0.1677, wR2, 0.4195, goodness of fit on F
- 2 = 1.381. The oxygen atoms of some sulfonate groups (S2 and S6) are disordered over two positions. Unfortunately, it was not possible to locate all hydrogen atoms from the Fourier difference map for this to be clarified. In addition, the R factor of crystal 2 is so high because the quality of crystal is not good enough and there are too many disordered water molecules.

26
- 33645460602
- (a) Makha, M.; Sobolev, A. N.; Raston, C. L. Chem. Commun. 2006, 5, 511-513.
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- Makha, M.¹ Sobolev, A.N.² Raston, C.L.³

27
- 33744801951
- (b) Nichols, P. J.; Makha, M.; Raston, C. L. Cryst. Growth Des. 2006, 6, 1161-1167.
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- Nichols, P.J.¹ Makha, M.² Raston, C.L.³

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.