Synthesis,characterization and crystal structures of two alkaline-earth metal complexes of olsalazine

Two one-dimensional linear coordination polymers, [Mg(L)?·?4(H₂O)] (H₂L?=?olsalazine) and 2 [Ca(L)?·?4(H₂O)] were obtained from self-assembly of CaCl₂ or MgSO₄ with olsalazine and their structures determined by single crystal X-ray diffraction. Both complexes are one-dimensional polymers, for complex 1 with crystal data: P2(1)/c, a?=?9.5224(18), b?=?11.309(2), c?=?16.211(3)?Å, β?=?106.648(3)°, V?=?1672.6(6)?ų, Z?=?4, R ₁?=?0.0695, wR ₂?=?0.2183, for complex 2 with crystal data: P4(3)2(1)2, a?=?10.4006(2), b?=?10.4006(2), c?=?32.0746(10)?Å, V?=?3469.59(14)?ų, Z?=?8, R ₁?=?0.0332, wR ₂?=?0.1015. In the complexes, Mg and Ca adopt totally different coordination modes. Alkaline-earth Mg is six-coordinate octahedronal geometry, however, in 2, the local coordination geometry around calcium atom can be best described as a slightly distorted pentagonal bipyramid crystallizing in a homo-chiral space group. Olsalazine in both compounds also adopts dissimilar coordination modes.     

Bis(2-Amino-5-bromopyrimidinium) Tetrahalometallates: Crystal structures of (2-amino-5-bromopyrimidinium)2 MCl4 (M = Co,Zn)

The reactions of metal(II) chlorides and bromides with 2-amino-5-bromopyrimidine (2-abpm) in neutral and acidic solution were investigated. The reaction with ZnCl₂, ZnBr₂, CoCl₂, CoBr₂ and MnCl₂ in acidic nitromethane solution gave complexes of the formula (2-abpmH)₂MX₄ (1, M?=?Zn, X?=?Cl; 2, M?=?Zn, X?=?Br; 3, M?=?Co, X?=?Cl; 4, M?=?Co, X?=?Br; 5, M?=?Mn, X?=?Cl). Crystals of 1 and 3 suitable for single crystal X-ray diffraction were obtained. Crystal data: For (1): triclinic, P-1, a?=?6.2485(13), b?=?9.0520(14), c?=?15.334(4)?Å, α?=?94.81(2), β?=?95.224(17), γ?=?98.027(17)°, V?=?851.1(3)?ų, Z?=?2, R?=?0.0596 for [|I|?≥?2σ(I)]. For (3): triclinic, P-1, a?=?6.2438(13), b?=?9.0597(15), c?=?15.318(3)?Å, α?=?94.749(18), β?=?95.343(15), γ?=?98.021(17)°, V?=?850.2(3)?ų, Z?=?2, R?=?0.0452 for [|I|?≥?2σ(I) ]. Variable temperature magnetic susceptibility data indicates weak antiferromagnetic interactions in the cobalt and manganese complexes.     

Syntheses,crystal structures and fluorescent properties of four one-dimensional lanthanide coordination polymers with 3-cyanobenzoato

The hydrothermal reactions of Nd(ClO₄)₃·6H₂O, Gd(ClO₄)₃·6H₂O, Dy(ClO₄)₃·6H₂O, Er(ClO₄)₃·6H₂O with 1,3-dicyanobenzene, give rise to four one-dimensional rare earth-based coordination polymers: [M(3-CNC₆H₄COO)₃(H₂O)₂] _n (where M?=?Nd (1), Gd (2), Dy (3), Er (4), 3-CNC₆H₄COO?=?3-cyanobenzoato), respectively. Their solid-state structures have been characterized by X-ray single-crystal diffraction studies. The results show that 1,3-dicyanobenzene hydrolyzed to give 3-cyanobenzoato under hydrothermal condition, and the four complexes are isomorphous. Crystal data for 1: triclinic, space group P-1, a?=?9.4063(19), b?=?11.485(2), c?=?12.616(3)?Å, α?=?66.38(3), β?=?74.01(3), γ?=?86.96(3)°, V?=?1197.9(4)?ų, Z?=?1, D _c?=?1.704?Mg?m^?3; for 2: triclinic, space group P-1, a?=?9.3712(19), b?=?11.446(2), c?=?12.627(3)?Å, α?=?65.86(3), β?=?73.89(3), γ?=?86.84(3)°, V?=?1184.8(4)?ų, Z?=?1, D _c?=?1.759?Mg?m^?3; for 3: triclinic, space group P-1, a?=?9.3425(19), b?=?11.432(2), c?=?12.703(3)?Å, α?=?65.28(3), β?=?73.80(3), γ?=?86.86(3)°, V?=?1180.6(4)?ų, Z?=?1, D _c?=?1.780?Mg?m^?3; for 4: triclinic, space group P-1, a?=?9.3425(19), b?=?11.432(2), c?=?12.703(3)?Å, α?=?65.28(3), β?=?73.80(3), γ?=?86.86(3)°, V?=?1180.6(4)?ų, Z?=?1, D _c?=?1.7794?Mg?m^?3. The fluorescence emission spectra of compounds 1 to 4 are also reported.     

Solid state structures of the chiral heterobimetallic complexes [Cu(dach)2][Pt(CN)4] · 2H2O, [Ni(dach)3][Pt(CN)4] · 2DMF · H2O,and [Pd(dach)2][Pt(CN)4] · H2O (dach = 1 R , 2 R -diaminocyclohexane)

The chiral dinuclear heterometallic complexes [Cu(dach)₂][Pt(CN)₄]?·?2H₂O (1), [Ni(dach)₃][Pt(CN)₄]?·?2DMF?·?H₂O (2), and [Pd(dach)₄][Pt(CN)₄]?·?H₂O (3) (dach?=?1R,2R-cyclohexanediamine) have been prepared and characterized by X-ray diffraction analysis. Crystal data: 1, monoclinic, P2₁, a?=?8.108(3), b?=?15.552(6), c?=?9.914(4)?Å, β?=?110.931(6)°, V?=?1167.6(8)?ų, Z?=?2, R ₁?=?0.0420, wR ₂?=?0.1122; 2, monoclinic, P2₁, a?=?13.264(11), b?=?9.285(7), c?=?16.211(13)?Å, β?=?111.640(9)°, V?=?1856(3)?ų, Z?=?2, R ₁?=?0.0276, wR ₂?=?0.0698; 3, monoclinic, P2₁, a?=?6.887(2), b?=?12.809(4), c?=?12.975(4)?Å, β?=?94.865(4)°, V?=?1140.6(6)?ų, Z?=?2, R ₁?=?0.057, wR ₂?=?0.156. In complex 1, the Pt and Cu atoms are linked by a CN bridge that presents a very bent C=N–Cu angle [136.8(8)°].