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[Co2(L)1.5(OH)(H2O)2]•2H2O (1). A mixture of H2L (0.188 g, 0.5 mmol), Co(NO3)2•6H2O (0.146 g, 0.5 mmol), NaOH (20 ml, 0.05 mol/L), and H2O (10 mL) was stirred for 30 min. The pH value of the mixture was adjusted to 7.0, then transferred and sealed in a 25 mL Teflon-lined stainless-steel container, which was heated at 160 °C for 72 h. After slowly cooled to room temperature at a rate of 3.25 °C/h, the purple single crystals of 1 were collected. Yield: 65% based on Co(NO3)2•6H2O. Elemental anal. Calcd for C33H27Co2O14 (%): C, 51.78; H, 3.56. Found: C, 51.80; H, 3. 59. IR (KBr, cm-1): 1675 (s), 1607 (m), 1483 (w), 1412 (m), 1347 (s), 1251 (s), 1070 (w), 923 (m), 791 (s), 699 (w). [CoL(bpp)] (2). The same synthetic procedure as that for 1 was used except that bpp (0.099 g, 0.5 mmol) was added, giving purple crystals of 2 in a 55% yield. Elemental anal. Calcd for C35H26CoN2O6 (%):C, 66.77; H, 4.17; N, 4.45. Found: C, 66.73; H, 4.20; N, 4.49. IR (KBr, cm-1): 1663 (m), 1617 (s), 1405 (s), 1338 (s), 1147 (w), 917 (m), 788 (s), 711 (w), 667 (w), 518 (m).
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Crystal data for 1: Triclinic, Pī, a = 12.188(2) Å, b = 12.348(2) Å, c = 12.715(2) Å, α = 98.354(4)° β = 113.399(2)° γ = 110.390(4)° V = 1554.1(4) Å3, Z = 2, R(int) = 0.0320, R1 = 0.0449, wR2 = 0.1019, GOF = 1.019. Crystal data for 2, Monoclinic, P21/c, a = 10.1966(8) Å, b = 19.5357(16) Å, c = 14.7368(12) Å, β = 98.262(1)° V = 2905.1(4) Å3, Z = 4, R(int) = 0.0277, R1 = 0.0308, wR2 = 0.0717, GOF = 1.027. Single-crystal X-ray diffraction data for complexes 1 and 2 were recorded on a Bruker Apex CCD diffractometer with graphite-monochromated Mo-Kα radiation (λ = 0.71073 Å) at 293 K. Empirical absorption corrections were applied using multiscan technique. All the structures were solved by Direct Method of SHELXS-97 and refined by full-matrix least-squares techniques on F2 using the SHELXL-97 program within WINGX. The hydrogen atoms of organic ligand and coordinated water are located by geometrically. The hydrogen atoms of water molecules (O5W) were fixed in ideal position for complex 1. Crystal date and structure refinement parameters for 1 and 2 are summarized in Table S1.Selected bond distances and angles for complexes 1 and 2 are listed in Table S2.
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