Electronic Supplementary Material (ESI) for CrystEngComm This journal is The Royal Society of Chemistry 2012
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1 Halogen Dipole Moment Effect of Phenolic Ring on Formation of Stair Like Polymers or Polymers with Tetranuclear Cubic Cage Units; New Precursors for Preparation of TlCl and Tl 2 O 3 Nanostructures Kamran Akhbari, Ali Morsali* Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box , Tehran, Islamic Republic of Iran Tel. and Fax: address: Morsali_a@modares.ac.ir (A. Morsali) 1
2 Table S1. Bond lengths /Å of secondary Tl Tl, Tl C, Tl H, Tl F, Tl Cl and Tl I interactions in compounds 1-9. [Tl 4(μ 3-2,4-dcp) 4] (1) [Tl 4(μ 3-3,4-dcp) 4] (2) [Tl(μ 3-2,5-dcp)] (3) Tl1-Tl Tl1-C Tl1-C Tl1-Tl Tl1-Tl Tl1-C Tl2-Tl Tl1-Tl [Tl(μ 3-2,4,6-tcp)] (4) Tl1-Tl Tl1-O [Tl 4 (μ 3-2,4-bcp) 4 ] (5) Tl1-Tl Tl1-Tl Tl1-Tl Tl1-H Tl1-Tl Tl1-Tl Tl1-Cl Tl1-Tl Tl1-Cl Tl1-Cl [Tl 4 (μ 3-4-cp) 4 ] (7) Tl1-Cl Tl1-Cl Tl1-C Tl1-Cl Tl1-C [Tl 4 (μ 3-4-ip) 4 ] (8) Tl1-Tl Tl1-C [Tl 4 (μ 3-2,4-cfp) 4 ] (6) Tl1-Tl Tl2-C Tl1-C Tl1-Cl Tl4-C Tl1-C Tl4-C Tl1-C [Tl(μ 3-4-fp)] (9) Tl4-C Tl1-C Tl1-C Tl4-C Tl1-C Tl1-C Tl4-C Tl1-C Tl1-C Tl4-C Tl4-C Tl1-C Tl1-Tl Tl4-C Tl1-C Tl1-Tl Tl1-Tl Tl1-C Tl2-Tl Tl1-Tl Tl3-Tl Tl2-Tl Tl2-I Tl4-H Tl3-I Tl2-Cl Tl3-I Tl2-F Tl4-I
3 a) b) c) 3
4 d) e) f) Figure S1. View of the two types of primary structural units; a-e) distorted tetranuclear cubic cage unit in compounds 1, 5, 6, 7 and 8 and f) dimeric unit in compound 4 (Tl = purple, O = red, C = gray, F = orange, Cl = green, Br = yellow, I = dark purple and H = white). 4
5 Figure S2. A fragment of three-dimensional supramolecular network in [Tl 4 (μ 3-2,4- dcp) 4 ] (1) constructed from Cl Cl interactions (Tl = purple, O = red, C = gray, Cl = green and H = white). 5
6 a) b) c) Figure S3. a) A fragment of one-dimensional supramolecular polymer of [Tl 4 (μ 3-3,4- dcp) 4 ] (2) along the crystallographic a axis, constructed from short Tl C contacts, b) the role of Cl Cl interactions in formation of two-dimensional supramolecular polymer of 2 along the crystallographic c axis and c) side view of two-dimensional supramolecular polymer of 2 constructed from secondary Tl C and Cl Cl interactions along the crystallographic a axis (Tl = purple, O = red, C = gray, Cl = green and H = white). 6
7 Figure S4. A fragment of three-dimensional supramolecular network in [Tl 4 (μ 3-2,4- bcp) 4 ] (5) constructed from Cl Br interactions (Tl = purple, O = red, C = gray, Cl = green, Br = yellow and H = white). 7
8 a) b) c) 8
9 d) e) f) Figure S5. a) A fragment of one-dimensional supramolecular polymer in [Tl 4 (μ 3-2,4- cfp) 4 ] (6) constructed from inter-cage Tl Tl interaction, b) representation of secondary η 6 -Tl C and η 2 -Tl C interactions in 6, c) the role of agostic interaction in formation of one-dimensional supramolecular polymer in 6, d) a fragment of two-dimensional supramolecular polymer in 6, constructed from agostic Tl H and inter-cage thallophillic interactions, e) The role of Tl2 Cl3 short contact in connection of two tetranuclear cubic cage units to each other, f) A fragment of one-dimensional supramolecular polymer in 6 constructed from short Tl2 F1 contact along the crystallographic c axis (Tl = purple, O = red, C = gray, F = orange, Cl = green and H = white). 9
10 Figure S6. Represents the role of short Tl I contacts in formation of three-dimensional supramolecular network in 8 (Tl = purple, O = red, C = gray, I = dark purple and H = white). 1
11 a) b) c) Figure S7. Representation of secondary intra-chain a) Tl Tl, b) Tl C and c) Tl H interactions in [Tl(μ 3-2,5-dcp)] (3) (Tl = purple, O = red, C = gray, Cl = green and H = white). 11
12 a) b) Figure S8. a) Intra-chain thallophillic interactions between the Tl(I) and three other thallium atoms in [Tl(μ 3-2,4,6-tcp)] (4) and b) the role of three inter-chain Tl Cl and one inter-chain Cl Cl interactions in connection of one-dimensional coordination polymers in 4, resulting in a two-dimensional supramolecular network (Tl = purple, O = red, C = gray, Cl = green and H = white). 12
13 a) 12 1 b) TG DTA 6 5 Weight of loss(%) Weight of loss(%) Temperature( C) c) 6 TG DTA Temperature( C) t( C) t( C) 13
14 12 1 d) TG DTA 35 3 Weight of loss(%) t( C) Temperature( C) e) 12 1 TG DTA 6 5 Weight of loss(%) t( C) Temperature( C) f) 12 TG 7 1 DTA 6 Weight of loss(%) Temperature( C) t( C) 14
15 12 g) TG 6 1 DTA 5 Weight of loss(%) Temperature( C) t( C) Figure S9. Thermal behavior of compounds a) 1, b) 3, c) 5, d) 6, e) 7, f) 8 and g) 9. 15
16 Figure S1. IR spectra of the residues obtained after calcination process of compounds 3 at 6 C (a) and 9 at 4 C (b) which attributed to TlCl and Tl 2 O 3, respectively. 16
17 a) b) Figure S11. XRD pattern of the residue obtained after calcination process of compounds 3 (a) and 9 (b) at 6 and 4 C, respectively. 17
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