[11,14,17110,54,57510-八氮杂-1,5(1,4)-二环十二烷-3,7(1,3)-二苯并环辛烷]四(硝酸)锌(II),[m,m-双(ZnII环素)](NO3)4的晶体结构

IF 0.1 Q4 CRYSTALLOGRAPHY
Yoshimi Ichimaru, Wanchun Jin, Y. Yamaguchi, K. Sugiura, Masanori Imai, H. Kurosaki, H. Fujioka, T. Koike, Yuhzo Hieda, Koichi Kato
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引用次数: 1

摘要

1,4,7,10-四氮杂环十二烷,环素,是一种大环(12元)四胺,其ZnII络合物已被用作生物探针。1 Fujioka等人报道了双核环素衍生物m,m-bis(ZnIIcyclen)的ZnII络合物,用于识别丙二酸二阴离子(CCDC744746)。2尽管丙二酸/m的大环二聚体的晶体结构,间双(ZnII环素)配合物的化学计量为1:1,但其单体的单体晶体结构尚未报道。丙二酸酯桥可能影响大环二聚体中的结构。在这里,为了阐明单体和丙二酸桥接二聚体之间的结构差异,我们描述了包含硝酸盐的m,mbis(ZnII环素)的单体晶体结构。m,m-bis(ZnII环素)的系统名称为[11,14,17110,51,54,57510-八氮杂-1,5(1,4)-二环十二烷-3,7(1,3)-二苯并那环辛]四(硝酸)锌(II),化学结构如图所示。1。该配合物是根据Fujioka等人先前报道的方法制备的。2在用水重结晶后获得适合X射线结构分析的晶体。进行初步检查,并在Rigaku XtaLAB Synergy-i衍射仪(Rigaku Co.,Tokyo,Japan)上使用93.15K下的石墨单色Cu-Kα辐射收集数据。表1中提供了晶体数据和有关数据收集的详细信息。使用SHELXT-2018/3.3的本征定相法求解初始结构。通过使用SHEXL-2018/3.4,使用F2上的全矩阵最小二乘法对所有非氢原子进行细化。使用几何计算定位所有氢原子,并且不对其进行细化。所有计算均使用Olex2晶体学软件进行。5晶体学数据存入剑桥晶体学数据中心(CCDC 2041868)。阳离子部分的ORTEP图如图所示。表2中提供了选定的结合长度和角度。标题络合物与m,m-bis(ZnIIcyclen)空腔中心沿a轴的结晶双折叠轴有关。中心ZnII原子Zn1周围的配位几何结构是一个畸变的正方形金字塔,τ6=0.009[τ=(β-α)/60,其中β=N1–Zn1–N3137.86(10)°和α=N2–Zn1-N4i 137.30(10)℃;对于理想的正方形金字塔来说,τ=0,而对于理想的三棱锥来说,τ=1]。来自环素单元的四个氮原子(N1、N2、N3和N4i)构成基面。顶端位置由硝酸根阴离子的氧原子O1占据。在四种硝酸盐中,两种与各自的ZnII配位,一种与N3–H3氢键,另一种位于m,m-bis(ZnII环素)的空腔上方。2021©日本分析化学学会
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Crystal Structure of [11,14,17,110,51,54,57,510-Octaaza-1,5(1,4)-dicyclododecana-3,7(1,3)-dibenzenacyclooctaphane]zinc(II) tetrakis(nitrate), [m,m-bis(ZnII-cyclen)](NO3)4
1,4,7,10-Tetraazacyclododecane, cyclen, is a macrocyclic (12-membered) tetraamine, and its ZnII complexes have been utilized as biological probes.1 Fujioka et al. reported a ZnII complex of the dinuclear cyclen derivative, m,m-bis(ZnIIcyclen), for recognizing the malonate dianion (CCDC744746).2 Although the crystal structure of a macrocyclic dimer for malonate/m,m-bis(ZnII-cyclen) complex of 1:1 stoichiometry has been revealed, the monomer crystal structure of its monomer is not reported. The malonate bridges may affect the structure in the macrocyclic dimer. Here, to elucidate the structural difference between the monomer and the malonate-bridged dimer, we describe the monomer crystal structure of m,mbis(ZnII-cyclen) comprising a nitrate. The systematic name of m,m-bis(ZnII-cyclen) is [11,14,17,110,51, 54,57,510-octaaza-1,5(1,4)-dicyclododecana-3,7(1,3)-dibenzenacyclooctaphane]zinc(II)tetrakis(nitrate), and the chemical structure is provided in Fig. 1. The complex was prepared according to a method previously reported by Fujioka et al.2 Crystals suitable for X-ray structure analysis were obtained upon recrystallization with water. A preliminary examination was performed, and data were collected on a Rigaku XtaLAB Synergy-i diffractometer (Rigaku Co., Tokyo, Japan) using graphite-monochromated Cu-Kα radiation at 93.15 K. Crystal data and details regarding data collection are provided in Table 1. The initial structure was solved using an intrinsic phasing method with SHELXT-2018/3.3 All non-hydrogen atoms were refined using the full-matrix least-squares method on F2 by utilizing SHEXL-2018/3.4 All hydrogen atoms were located using a geometrical calculation, and were not refined. All calculations were performed using Olex2 crystallographic software.5 Crystallographic data were deposited to the Cambridge Crystallographic Data Center (CCDC 2041868). An ORTEP drawing of the cationic part is shown in Fig. 2, and selected bond lengths and angles are provided in Table 2. The title complex is related by a crystallographic two-fold axis along the a-axis at the center of the cavity of m,m-bis(ZnIIcyclen). The coordination geometry around the central ZnII atom, Zn1, is a distorted square pyramidal with τ 6 = 0.009 [τ = (β – α)/60, where β = N1–Zn1–N3, 137.86(10)° and α = N2– Zn1–N4i, 137.30(10)°; for an ideal square pyramid, τ = 0, whereas, for an ideal trigonal pyramid, τ = 1]. Four nitrogen atoms (N1, N2, N3, and N4i) from the cyclen unit comprise the basal plane. The apical position is occupied by an oxygen atom, O1, of the nitrate anion. Of the four nitrates, two are coordinated to the respective ZnII, one is hydrogen bonded to N3–H3, and the other is located above the cavity of m,m-bis(ZnII-cyclen). 2021 © The Japan Society for Analytical Chemistry
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CiteScore
0.60
自引率
50.00%
发文量
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