3.2.2. Synthesis of [Zn4Cl2(ClQ)6(H2O)2]·4DMF (**2**)

HClQ (263 mg, 1.46 mmol) was dissolved in a mixture of DMF (7.5 mL) and ethanol (15 mL). KOH (29 mg, 1 mmol KOH in 1 mL water) was added afterwards, and the formed solution was cooled down to approximately −10 ◦C. Additionally, zinc chloride solution, (136 mg, 1 mmol ZnCl<sup>2</sup> in 10 mL of ethanol) cooled down to approximately −10 ◦C, was added and the reaction mixture was mixed for couple of minutes. After keeping the solution in the fridge for around four months, yellow crystals of **2** were formed, filtered off and dried in air.

[Zn4Cl2(ClQ)6(H2O)2]·4DMF (**2**): Anal. Calc. for C66H62Cl8N10O12Zn<sup>4</sup> (1732.42 g·mol−<sup>1</sup> ): C, 45.76; H, 3.61; N, 8.08%. Found: C, 45.91; H, 3.13; N, 7.88%. Yield: 88.53 mg (21%). <sup>1</sup>H NMR (DMSO-d6): *δ* = 8.74 (1H, br s, H-2), 8.54 (1H, dd, *J* 8.4, 1.5 Hz, H-4), 7.95 (1H, s, HDMF-1), 7.75 (1H, dd, *J* 8.4, 4.4 Hz, H-3), 7.50 (1H, d, *J* 8.4 Hz, H-6), 6.74 (1H, d, *J* 8.4 Hz, H-7), 2.89 (3H, s, HDMF-4), 2.73 (3H, s, HDMF-3) ppm. <sup>13</sup>C NMR (DMSO-d6): *δ* = 162.3 (C-8, CDMF-1), 145.7 (C-2), 140.2 (C-8a), 135.0 (C-4), 130.0 (C-6), 126.6 (C-4a), 122.8 (C-3), 111.7 (C-7), 109.0 (C-5), 35.8 (CDMF-4), 30.8 (CDMF-3) ppm. IR (ATR, cm−<sup>1</sup> ): 3075(vw), 2923(w), 2847(w), 1672(m), 1649(m), 1598(m), 1573(m), 1495(m), 1457(m), 1398(w), 1378(m), 1364(m), 1320(m), 1257(w) 1241(w), 1200(w), 1155(w), 1129(w), 1100(w), 1087(m), 1044(m), 956(m), 885(w), 862(w), 834(w), 820(m), 784(m), 739(m), 666(m), 656(w), 636(m), 613(m), 541(m), 501(m), 451(m), 429(m).
