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note
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To prepare crystals of 1, Zn(CH3COO)2 32H2O (0.878 g, 4.0 mmol), thiourea (0.038 g, 0.5 mmol), and Acridine Yellow G (0.274 g, 1.0 mmol) were dissolved in H2O (15 mL) in a Teflon-lined stainless steel autoclave (23 mL). Thiophenol (0.770 g, 7.0 mmol) was added to the clear solution, and the mixture was stirred efficiently for 15 min, leading to the formation of an orange-red sticky suspension. The sealed vessel was then heated at 165Ćfor 7 days. After cooling to room temperature, pink block crystals of 1 (suitable for X-ray analysis) were obtained (weight, 0.815 g; yield, 67% based on the Zn source). Anal. Calcd for C105H93N3OS16Zn8 (2449.13): C, 51.49; H, 3.83; N, 1.72; O, 0.65. Found: C, 51.91; H, 4.08; N, 2.86; O, 0.72 (Chemical & MicroAnalytical Services Pty. Ltd., Belmont, Victoria, Australia). Notes: There are discrepancies between the experimental elemental analyses and the theoretical values. This is not unusual for this class of Zn-S cluster compounds.7, 13 ε 267: 7.73-104 M-1 cm-1, ε 467: 3.60-104 M-1 cm-1. FTIR data (cm-1): 3461 (m, ν (NH2)), 3048 (m, ν (dCH)), 1626 (vs, ν (NH2)), 157(vs, δ (CdC)), 1564 (s, ν (NH2)), 1476 (vs, δ (CdC)), 1436 (vs, δ (CdC)), 1389 (m, ν (CH3)), 1085 (s, ν (C-S)), 1069 (m, ν (C-S)), 1023 (vs, ν (C-S)), 734 (vs, δ (dCH)), 685 (vs, δ (dCH)). 1HNMR(400 MHz, (CD3)2SO, 25Ć): δ 2.23 (s, 2CH3, 6H), 6.79 (s, 1CH, 1H), 6.82 (t, J=6.8 Hz, 15CH, 15H), 6.95 (m, 15C(CH)2, 30H), 7.27 (m, 15C(CH)2, 30H), 7.37 (t, J = 8.0 Hz, 2CH, 2H), 7.51 (t, J = 4.0 Hz, 2CH, 2H).
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33
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77249135135
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Crystal data for 1: C105H93N3OS16Zn8, M = 2449.13, monoclinic, C2/c, a=27.752
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Crystal data for 1: C105H93N3OS16Zn8, M = 2449.13, monoclinic, C2/c, a=27.752
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34
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77249114303
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note
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A °, b=25.752, A °, c=33.771, A °, β =103.656(5)-, V=23453(13)A ° 3, Z=8, T=130, K, Dc=1.334 g cm-3, F(000)=9240, μ (Mo KR) = 1.934 mm-1, GOF = 1.012. A total of 67 119 reflections measured, 26 441 unique (Rint = 0.2729), that were used in all calculations. R1=0.1640, wR2=0.3800 [I> 2σ (I)], CCDC 731860. The surface-SC6H5 ligands have severe disorder, and this is responsible for the elevated agreement values (R values) found for this structure.
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