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1, 3-Dichlorotetra-n-Butyldistannoxane as a Novel ATRP Initiator:
Property, Catalysis Ability and Mechanism
Zhi Xua, Shougen Yinb, Bin Leia, Yan Lub, Weixing Changa, Jing Lia*
a The
State Key Laboratory of Elemento-Organic Chemistry, Nankai University, No. 94 Weijing Road,
Nankai District, Tianjin, P. R. China, 300071.
Tel: +86-022-23503336, Fax: +86-022-23503627, E-mail: lijing@ nankai.edu.cn
b
College of Science, Tianjin University of Technology, No. 263 South Hongqi Road, Nankai District,
Tianjin, P. R. China, 300191.
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Figure 1. The GPC curves of the A-A copolymer (macro-initiator) obtained from the dilute solution and
the B-A-A-B copolymer (chain extension).
Conditions: Solvent = o-xylene, o-xylene/BMA (1:1 v/v): [BMA] 0 = 3.15 M; Entry 6 of Table 1 was used as macro-initator,
[macro-initator] = 0.001 M, Mn = 33800, PDI = 1.43; [CuCl]0 = [CuCl2] × 5 = [PMDETA]0/3 = 0.002 M; Temp = 110℃.
Figure 2. The 1H NMR of the B-A-A-B copolymer (chain extension)
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Figure 3. The GPC curves for the bulk ATRP of styrene at 110 C. Bulk: [styrene]0 =8.73 M; [CuCl] 0
= [CuCl2]0 × 5 = [PMDETA]0/3 = 0.02 M; [complex A]0 = 0.01 M.
Figure 4. The GPC curves for the bulk ATRP of styrene at 110 C. Bulk: [styrene] 0 =8.73 M; [CuCl] 0
= [CuCl2] 0 × 5 = [PMDETA] 0/3 = 0.2 M; [complex A]0 = 0.1 M.
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Figure 5. The GPC curves for the bulk ATRP of styrene at 110 C. Bulk: [styrene] 0 =8.73 M; [CuCl] 0
= [CuCl2] 0 × 5 = [PMDETA] 0/3 = 0.01 M; [complex A] 0 = 0.005 M.
Attention: the crystal structures of the complex A were obtained by the diamond software version 2.1c
according to the crystal data in the journal as follows:
Hämäläinen, R.; Turpeinen, U. J. Organomet Chem. 1987, 333, 323-327.
Figure 6. Crystal structure of the complex A (one molecular). All hydrogen atoms are removed for
clarity.
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Figure 7. Crystal structure of the complex A (one layer). All carbon and hydrogen atoms are removed
for clarity.
Figure 8. Crystal structure of the complex A (double layers). All carbon and hydrogen atoms are
removed for clarity.
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