Single crystals of Rb4Cu4OCl (I), Rb2Cu3O(SeO3)4Cl2 (II), and RbCu3(OH)(SeO3)Cl4(H2O)2 (III) have been prepared by chemical transport reactions method from ÑuO – SeO2 – RbCl – CuCl2 mixture. The unit cell parameters were determined by the least squares method. Compound I has a monoclinic symmetry [s.g. Ñ2/ñ, a = 14.907(10) Å, b = 15.094(10) Å, c = 9.079(6) Å, β = 104.090(13)î, V = 1981(2) Å3, Z = 8]. The crystal structure have been solved by the direct methods from X-ray diffraction data and refined by the least-squares techniques to R1 = 0.0448 (wR2 = 0.0984) for 1745 reflections with |Fo| ≥ 4σF. Compound II has a triclinic symmetry [s.g. P1 ̅, a = 7.856(7) Å, b = 8.162(8) Å, c = 8.940(8) Å, α = 110.356(14)î, β = 109.905(14)î, γ = 100.567(14)î, V = 474.7(8) Å3, Z = 1]. The crystal structure have been solved by the direct methods from X-ray diffraction data and refined by the least-squares techniques to R1 = 0.0448 (wR2 = 0.0984) for 1612 reflections with |Fo| ≥ 4σF. Compound I has a monoclinic symmetry [s.g. P21/ñ, a = 10.972(9) Å, b = 8.879(7) Å, c = 15.430(13) Å, β = 110.347(14)î, V = 1409(2) Å3, Z = 2]. The crystal structure have been solved by the direct methods from X-ray diffraction data and refined by the least-squares techniques to R1 = 0.0328 (wR2 = 0.0440) for 1680 reflections with |Fo| ≥ 4σF.
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