引用本文:
缪方明, 刘小兰, 张淑芬, 姜宗慧, 王耕霖. 2,3—二氢—5,6—二苯基吡嗪及其2∶1硝酸银配合物的合成与晶体结构[J]. 物理化学学报,
1988, 4(01): 20-26.
doi:
10.3866/PKU.WHXB19880105
Citation: Miao Fangming*, Liu Xiaolan
Zhang shufen, Jiang Zonghui, Wang Genglin, THE CRYSTAL AND MOLECULAR STRUCTURES OF 2,3-DIHYDRO-5,6-DIPHENYLPYRAZINE AND ITS COMPLEX WITH SILVER NITRATE[J]. Acta Physico-Chimica Sinica, 1988, 4(01): 20-26. doi: 10.3866/PKU.WHXB19880105
Citation: Miao Fangming*, Liu Xiaolan
Zhang shufen, Jiang Zonghui, Wang Genglin, THE CRYSTAL AND MOLECULAR STRUCTURES OF 2,3-DIHYDRO-5,6-DIPHENYLPYRAZINE AND ITS COMPLEX WITH SILVER NITRATE[J]. Acta Physico-Chimica Sinica, 1988, 4(01): 20-26. doi: 10.3866/PKU.WHXB19880105
2,3—二氢—5,6—二苯基吡嗪及其2∶1硝酸银配合物的合成与晶体结构
摘要:
合成了配体2,3-二氢-5,6-二苯基吡嗪(C_(16)H_(14)N_2)及其硝酸银配合物AgNO_3(C_(16)H_(14)N_2)_2, 并用CAD4衍射仪测定了它们的晶体结构。晶体学数据为, 配体C_(16)H_(14)N_2: 单斜晶系, 空间群P2_1/n, a=0.5685(3),b=0.7928(1), c=2.7261(8) nm, β=95.02(6)°, V=1.2287 nm, z=4,D_c=1.27gcm~(-3),μ=0.81cm~(-1),R=0.031, R_w=0.033; 配合物AgNO3(C_(16)H_(14)N_2)_2:单斜晶系, 空间群A2, a=0.5655(3), b=0.7771(2), c=3.0.502(5) nm, β=94.90(2)°, V=1.3355 nm, z=2, D_c=1.59gcm~(-3),μ=7.87cm~(-1), R=0.033, R_2=0.028。
测定结果表明, 在C_(16)H_(14)N_2分子中, 有关键长、键角均符合相应正常值。在AgNO3(C_(16)H_(14)N_2)_2晶体中NO_3~-为双齿配体; C_(16)H_(14)N_2则因吡嗪环上苯基的空间障碍而作为单齿配体出现; Ag原子处于二重轴上, 周围由四个氧和两个氮原子组成严重扭曲的配位八面体; Ag(1)—O(1)键长为2.828, Ag(1)—O(2)为2.520, Ag(1)—N(31)为0.2399 nm. Ag的配位八面体间借公用相对两个顶点氧原子而构成无限链状结构.
测定结果表明, 在C_(16)H_(14)N_2分子中, 有关键长、键角均符合相应正常值。在AgNO3(C_(16)H_(14)N_2)_2晶体中NO_3~-为双齿配体; C_(16)H_(14)N_2则因吡嗪环上苯基的空间障碍而作为单齿配体出现; Ag原子处于二重轴上, 周围由四个氧和两个氮原子组成严重扭曲的配位八面体; Ag(1)—O(1)键长为2.828, Ag(1)—O(2)为2.520, Ag(1)—N(31)为0.2399 nm. Ag的配位八面体间借公用相对两个顶点氧原子而构成无限链状结构.
English
THE CRYSTAL AND MOLECULAR STRUCTURES OF 2,3-DIHYDRO-5,6-DIPHENYLPYRAZINE AND ITS COMPLEX WITH SILVER NITRATE
Abstract:
The crystal and molecular structures of 2,3-dihydro-5,6-dipenylpyrazine (C_(16)H_(14)N_2) and its complex with silver nitrate AgNO_3(C_(16)H_(14)N_2)_2 were determined by CAD4 single crystal diffractometer, using graphite monochromated Mo-Kα radiation. The crystallographic data are: (1) C_(16)H_(14)N_2, monoclinic, P2_1/n, α=0.5685(3), b=0.7928(1), c=2.7261(8) nm, β=95.02(6)°, V=1.2287 nm, z=4. (2) AgNO_3 (C_(16)H_(14)N_2)_2, monoclinic, A_2, α=0.5655(3), b=0.7791(2), c=3.0502(5) nm, β=94.90(2)°, V=1.3355 nm, z=2.
The structure of (1) was solved by direct method and (2) by heavy atom method. The full matrix least squares refinement for (1) with isotripic thermal parameters for H atoms and anisotropic for the others was converged at R=0.031, and R_W=0.033, the refinement for (2), excluding H atoms, at R=0.033 and R_W=0.028. In the structure of C_(16)H_(14)N_2, bond lengths and angles are not unexpected, and dihedral angles between pyrazine ring plane and each plane of the two phenyls are 151.9° and 136.7° respectively. In the structure of AgNO_3 (C_(16)H_(14)N_2)_2, the Ag atom is positioned on a 2-fold axis, and coordinated by two N and four O atons to form a severely distorted octahedron, the distance Ag(1)—O(1) is 2.828, Ag(1)—O(2) 2.520, and Ag(1)—N(31) 0.2399 nm. The conformation of the C_(16)H_(14)N_2 molecule in the complex was compared with that of the free ligand.
The structure of (1) was solved by direct method and (2) by heavy atom method. The full matrix least squares refinement for (1) with isotripic thermal parameters for H atoms and anisotropic for the others was converged at R=0.031, and R_W=0.033, the refinement for (2), excluding H atoms, at R=0.033 and R_W=0.028. In the structure of C_(16)H_(14)N_2, bond lengths and angles are not unexpected, and dihedral angles between pyrazine ring plane and each plane of the two phenyls are 151.9° and 136.7° respectively. In the structure of AgNO_3 (C_(16)H_(14)N_2)_2, the Ag atom is positioned on a 2-fold axis, and coordinated by two N and four O atons to form a severely distorted octahedron, the distance Ag(1)—O(1) is 2.828, Ag(1)—O(2) 2.520, and Ag(1)—N(31) 0.2399 nm. The conformation of the C_(16)H_(14)N_2 molecule in the complex was compared with that of the free ligand.
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