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首页> 外文期刊>Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics >Synthesis and Structure of Mercurous Ion and Dinuclear Lead(ll) Complexes of the 28-Membered Selenaaza Macrocycle:Dominance of the Chelate Ring Size Effect and Conformational Requirement over Soft-Soft Interactions
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Synthesis and Structure of Mercurous Ion and Dinuclear Lead(ll) Complexes of the 28-Membered Selenaaza Macrocycle:Dominance of the Chelate Ring Size Effect and Conformational Requirement over Soft-Soft Interactions

机译：28元硒代硒氮大环汞离子和双核铅（II）配合物的合成和结构：螯合环大小效应和构象要求对软-软相互作用的支配。

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The flexible and larger ring size macrocycle 4 (C_(36)H_(46)N_6Se_2) afforded stable complex 5 [Hg_2(PF_6)_2{C_(36)H_(46)N_6Se_2}] on treatment with 1 equiv of mercuric acetate followed by addition of NH_4PF_6.The reaction of Pb(OCOCH_3)_2-4H_20 with 4 followed by treatment with NH_4PF_6 resulted in a dinuclear lead complex (6) [Pb_2(PF_6)_2(OCOCH_3)_2{C_(36)H_(46)N_6-Se_2}].The crystal structures of complexes 5 and 6 are described:C_(36)H_(46)F_(12)Hg_2N_6P_2Se_2 a = 9.5106(5) A,b = 11.5222(6) A,c = 11.8161(6) A,alpha = 115.6110(10)~°,beta = 96.5190(10)~°,gamma = 106.2910(10)~°,monoclinic,P1,Z =1;C_(44)H_(57)F_(12)N_80_4P_2Pb_2Se_2 a = 9.4668(5) k,b = 11.9937(6) A,c = 25.2319(14) A,alpha = 102.4130(10)~°,beta =97.6130(10)~°,gamma = 94.8540(10)~°,monoclinic,P1,Z= 2.The crystal structure of 5 revealed that Hg_2~(2+) is trapped inside the cavity of the macrocycle.The geometry around the mercurous ion is antiprismatic with Hg_2~(2+) coordinating to six nitrogen atoms forming four five-membered rings,and there is no interaction between the mercurous ion and the selenium donor atoms.The single crystal X-ray crystal structure of 6 indicates a distorted octahedral geometry around each lead atom in the cavity of the macrocycle due to presence of the sterochemically active lone pair on Pb(ll).The octahedral geometry around each Pb(ll) is satisfied by coordination to 3 nitrogen atoms,two oxygen atoms of the chelating acetate group,and bridging of one of the oxygen atoms of the nearby acetate.
机译：柔性且较大环尺寸的大环化合物4（C_（36）H_（46）N_6Se_2）在用1当量乙酸汞处理后提供稳定的络合物5 [Hg_2（PF_6）_2 {C_（36）H_（46）N_6Se_2}]通过添加NH_4PF_6。Pb（OCOCH_3）_2-4H_20与4的反应，然后用NH_4PF_6处理，生成双核铅配合物（6）[Pb_2（PF_6）_2（OCOCH_3）_2 {C_（36）H_（46） N_6-Se_2}]。描述了配合物5和6的晶体结构：C_（36）H_（46）F_（12）Hg_2N_6P_2Se_2 a = 9.5106（5）A，b = 11.5222（6）A，c = 11.8161（ 6）A，alpha = 115.6110（10）〜°，beta = 96.5190（10）〜°，gamma = 106.2910（10）〜°，单斜，P1，Z = 1; C_（44）H_（57）F_（12 N_80_4P_2Pb_2Se_2 a = 9.4668（5）k，b = 11.9937（6）A，c = 25.2319（14）A，alpha = 102.4130（10）〜°，beta = 97.6130（10）〜°，γ= 94.8540（10） 〜°，单斜晶系，P1，Z = 2 .5的晶体结构表明Hg_2〜（2+）被困在大环的腔体内。汞离子周围的几何形状与Hg_2〜（2+）配位为六个氮原子形成四个五元X射线晶体结构为6的单晶X射线晶体结构表明，由于存在立体化学活性，大环腔中每个铅原子周围的八面体几何形状都发生了扭曲通过与3个氮原子，两个螯合乙酸根的氧原子配位并桥接附近一个乙酸根的氧原子来满足每个Pb（ll）的八面体几何形状。

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