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将适量邻菲啰啉、丁二酸和CuCl_2·2H_2O(摩尔比=1:1:1)溶于水和甲醇的混合溶剂[V(水):V(甲醇)=1:1]后,滴加NaOH溶液至pH=4.8.滤去沉淀物后,滤液于室温下缓慢蒸发得蓝色细长[Cu(phen)(H_2O)(C_4H_4O_4)]·2H_2O晶体.晶体属三斜晶系,P1(No.2)空间群.晶胞参数a=0.7462(1)nm,b=0.9959(1)nm,c=1.2266(1)nm,α=75.02(1)°,β=82.38(1)°,γ=74.76(1)°,V=0.8475(2)nm~3,Z=2,D_c=1.622g/cm~3,F(000)=426,3882个独立衍射点中,2789个可观测点满足F_0~2≥2σ(F_0~2),R=0.0450,wR~2=0.0951.配合物内每个Cu与邻菲啰啉螯合配体中的2个N原子、来自不同羧酸根的2个羧基O和1个水分子O原子配位,形成扭曲的四方锥体,其中一羧基O位于锥顶[d(Ci—N)=0.2006(3)0 .2032(3)nm;赤道d(Cu—0)=0.1972(2),0.1973(2)nm;轴向d(Cu—O)=0.2210(2)nm].双齿桥联丁二酸根连接Cu原子形成平行于[100]方向的多聚超分子链_∞~1[Cu(phen)_2(H_2O)(C_4H_4O_4)_(2/2)].紧邻链分子上的邻菲啰啉配体互相穿插产生芳环堆积作用,并形成沿[100]方向无限延伸的超分子双链_∞~1[Cu(phen)_2(H_2O)·(C_4H_4O_4)_(2/2)]_2.芳环堆积间距交替为0.366nm和0.380nm.未配位的H_2O分子位于超分子双链之间.
The appropriate amount of phenanthroline, succinic acid and CuCl 2 · 2H 2 O (molar ratio = 1: 1: 1) was dissolved in a mixed solvent of water and methanol [V (water): V (methanol) = 1: 1] Add NaOH solution to pH = 4.8. After the precipitate was filtered off, the filtrate was slowly evaporated at room temperature to give a blue elongated [Cu (phen) (H_2O) (C_4H_4O_4)] 2H_2O crystal. The crystals are triclinic and P1 (1) nm, α = 75.02 (1) ° and β = 82.38 (1) °, respectively, and the lattice parameter of a unit cell was 0.7462 (1) nm and b = 0.9959 γ = 74.76 (1) °, V = 0.8475 (2) nm ~ 3, Z = 2, D_c = 1.622g / cm ~ 3, F (000) = 426,3882 independent diffraction points, 2789 observable points F_0 ~ 2≥2σ (F_0 ~ 2), R = 0.0450, wR ~ 2 = 0.0951. Two N atoms in chelate ligand of each Cu with phenanthroline in the complex, two A carboxyl group O and a water molecule O atoms coordinate to form a twisted tetragonal pyramid, wherein a carboxyl O is located at the top of the cone [d (Ci-N) = 0.2006 (3) 0 .2032 (3) nm; Cu-0) = 0.1972 (2), 0.1973 (2) nm; d (Cu-O) = 0.2210 (2) nm] Polypeptide Supramolecular Chain _∞ ~ 1 [Cu (phen) _2 (H_2O) (C_4H_4O_4) _ (2/2)]. The adjacent phenanthroline ligands interpenetrating each other Aromatic rings and the formation of supramolecular double chain [Cu (phen) _2 (H_2O) (C_4H_4O_4) _ (2/2)] _2 infinitely extending along [100] 0.366 nm and 0.380 nm. Uncoordinated H 2 O molecules are located between supramolecular double strands.