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-二氯-(1,4,8,11-四氮杂环十四烷-κ)铬(III)双(甲酰胺-κ)(1,4,8,11-四氮杂环十四烷-κ)铬(III)双[四氯锌酸盐(II)]的晶体结构

Crystal structure of -di-chlorido-(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ )chromium(III) bis-(form-amide-κ)(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ )chromium(III) bis-[tetra-chlorido-zincate(II)].

作者信息

Moon Dohyun, Choi Jong-Ha

机构信息

Beamline Department, Pohang Accelerator Laboratory, POSTECH, Pohang 37673, Republic of Korea.

Department of Chemistry, Andong National University, Andong 36729, Republic of Korea.

出版信息

Acta Crystallogr E Crystallogr Commun. 2020 Apr 9;76(Pt 5):656-659. doi: 10.1107/S2056989020004910. eCollection 2020 May 1.

Abstract

The structure of the title compound, [CrCl(CHN)][Cr(HCONH)(CHN)][ZnCl] (CHN = 1,4,8,11-tetra-aza-cyclo-tetra-decane, cyclam; HCONH = formamide, fa), has been determined from synchrotron X-ray data. The asymmetric unit contains two independent halves of the [CrCl(cyclam)] and [Cr(fa)(cyclam)] cations, and one tetra-chlorido-zincate anion. In each complex cation, the Cr ion is coordinated by the four N atoms of the cyclam ligand in the equatorial plane and two Cl ligands or two O-bonded formamide mol-ecules in a axial arrangement, displaying a distorted octa-hedral geometry with crystallographic inversion symmetry. The Cr-N(cyclam) bond lengths are in the range 2.061 (2) to 2.074 (2) Å, while the Cr-Cl and Cr-O(fa) bond distances are 2.3194 (7) and 1.9953 (19) Å, respectively. The macrocyclic cyclam moieties adopt the centrosymmetric -III conformation with six- and five-membered chelate rings in chair and conformations The crystal structure is stabilized by inter-molecular hydrogen bonds involving the NH or CH groups of cyclam and the NH group of coordinated formamide as donors, and Cl atoms of the ZnCl anion as acceptors.

摘要

标题化合物[CrCl(CHN)][Cr(HCONH)(CHN)][ZnCl](CHN = 1,4,8,11-四氮杂环十四烷,环胺;HCONH = 甲酰胺,fa)的结构已通过同步辐射X射线数据确定。不对称单元包含[CrCl(环胺)]和[Cr(甲酰胺)(环胺)]阳离子的两个独立半部分,以及一个四氯锌酸根阴离子。在每个配合物阳离子中,Cr离子在赤道平面由环胺配体的四个N原子配位,在轴向排列有两个Cl配体或两个与O键合的甲酰胺分子,呈现出具有晶体学反演对称性的扭曲八面体几何构型。Cr-N(环胺)键长在2.061 (2)至2.074 (2) Å范围内,而Cr-Cl和Cr-O(甲酰胺)键距分别为2.3194 (7)和1.9953 (19) Å。大环环胺部分采用中心对称的-III构象,有椅式和构象的六元及五元螯合环。晶体结构通过分子间氢键得以稳定,这些氢键涉及环胺的NH或CH基团以及配位甲酰胺的NH基团作为供体,ZnCl阴离子的Cl原子作为受体。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/28e0/7199251/7c782917e61c/e-76-00656-fig1.jpg

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