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Ni2(L)2(bpp)2(μ2-H2O, 1, A mixture of Ni(NO3)2·6H2O (0.2235 g, 0.5 mmol, H2L (0.1873 g, 0.1 mmol, bpp (0.1007 g, 0.1 mmol, and H2O (15 ml) was stirred for 30 min. The pH value of the mixture was adjusted to 6.0 with 0.05 mol/L NaOH solution. The resulting mixture was transferred to a 25 ml stainless steel bomb and heated at 160 °C for 3 day, then cooled to room temperature at a rate of 3.25 °C/h. The resulting blue block crystals of 1 were obtained (46% yield, based on Ni(NO3)2·6H2O, Elemental analysis, ) calcd for C70H54O13N4Ni2: C, 65.86; H, 4.26; N, 4.39. Found: C, 65.90; H, 4.22; N, 4.34. IR data (cm- 1, 1673 (s, 1618(m, 1487(w, 1423(s, 1345(m, 1265(w, 851(s, 786(m, 704s
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- 1): 1673 (s), 1618(m), 1487(w), 1423(s), 1345(m), 1265(w), 851(s), 786(m), 704(s).
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Crystal data for 1: monoclinic, P21/c, a, 16.865(2) Å, b, 11.0364(16) Å, c, 33.354(5) Å, β, 99.577(2)°, V, 6154.0(15) Å3, Z, 4, R(int, 0.1140, R1, 0.0601, wR2, 0.1093, GOF, 0.951. Single-crystal X-ray diffraction data for compound 1 was recorded on a Bruker Apex CCD diffractometer with graphite-monochromated Mo-K( 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. The hydrogen atoms of organic ligand and coordinated water are located by geometrically. Crystal data and structure refinement parameters for 1 are summarized in Table S1. Selected bond distances and angles for 1 are listed in Table S2
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Crystal data for 1: monoclinic, P21/c, a = 16.865(2) Å, b = 11.0364(16) Å, c = 33.354(5) Å, β = 99.577(2)°, V = 6154.0(15) Å3, Z = 4, R(int) = 0.1140, R1 = 0.0601, wR2 = 0.1093, GOF = 0.951. Single-crystal X-ray diffraction data for compound 1 was recorded on a Bruker Apex CCD diffractometer with graphite-monochromated Mo-K( 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. The hydrogen atoms of organic ligand and coordinated water are located by geometrically. Crystal data and structure refinement parameters for 1 are summarized in Table S1. Selected bond distances and angles for 1 are listed in Table S2
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Zhou X.H., Du X.D., Li G.N., Zuo J.L., and You X.Z. Cryst. Growth Des. 9 (2009) 4487-4496
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