| 查看: 641 | 回复: 1 | ||
[求助]
求解单晶，内详 已有1人参与
|
|
金币不多，如能帮忙，另作他谢 审稿人的意见如下： Compounds 3 and 4 were almost certainly assigned the wrong space group. The correct space group appears to be the centrosymmetric group P-1 (No. 2), not P1 (No. 1). The structure determinations are not acceptable in P1. There are poor ring geometries, strange C-C distances, abnormally non-planar six-membered rings and an obvious inversion center between the two molecules in P1. The refinement of the compound 3 dataset used 1282 restraints versus only 1173 data! Most restraints seem to have been applied to the Uij values of the displacement parameters, to prevent non-positive definite 'ellipsoids'. This is a direct consequence of the falsely low symmetry reported by the authors. For compound 4, the refinement did not reach convergence. The maximum refined parameter shift/error value is very large, 2.72. This is another effect of refining in a space group with incorrectly low symmetry. The authors clearly encountered some difficulty in solution and refinement, but these details are not fully reported in the MS. Data should be re-refined in the centrosymmetric space group P-1 (No. 2) and resubmitted. Alternatively, the authors should provide good reasons for adopting P1 over P-1. It would also be preferable to collect low-temperature data for 3 and 4, as was done for compound 2. Compounds 3 and 4 can be easily transformed from P1 to P-1 with the ADDSYM-SHELX function in PLATON. The metal and Si atomic positions transform to: Compound 3: Mo1 0.46691 0.20722 0.65915 Si1 1.00290 0.93210 0.75930 Si2 0.73890 0.33280 0.07460 Compound 4: W1 0.46735 -0.29233 0.65856 Si1 0.73650 -0.16862 0.07409 Si2 1.01150 0.43295 0.76276 from which the rest of the structure can be built up. Additional disorder of TIPS groups may be observed but they are already disordered and a centrosymmetric description is preferred, as shown by the refinement instabilities evident in the CIFs. |
回复此楼» 本帖附件资源列表
-
欢迎监督和反馈：小木虫仅提供交流平台，不对该内容负责。
本内容由用户自主发布，如果其内容涉及到知识产权问题，其责任在于用户本人，如对版权有异议，请联系邮箱：xiaomuchong@tal.com - 附件 1 : compound_3.zip
- 附件 2 : compound_4.zip
2015-05-10 13:26:34, 2.92 M
2015-05-10 13:32:03, 2.27 M
» 猜你喜欢
Chemdraw免费软件
已经有0人回复
-
单晶结构解析，各类疑难晶体数据处理和答疑
已经有38人回复
-
无机化学论文润色/翻译怎么收费?
已经有228人回复
-
这个水相反应有没有催化剂促进发生
已经有4人回复
-
Mn Me3TACN
已经有5人回复
-
求助最新的CCDC数据库升级包
已经有0人回复
-
高中化学教师求助：配合物一水硫酸四氨合铜的紫外可见吸收光谱数据
已经有2人回复
-
ACS omega，返修返回去目前为in peer review，求助进度问题
已经有4人回复
-
南开大学化学学院招收电催化方向2027级博士生、博士后
已经有27人回复
» 本主题相关价值贴推荐，对您同样有帮助:
- 急求推荐个合适的期刊（内详）
已经有9人回复
- 什么样的配体适合用挥发溶剂的方法培养单晶呢？求解！
已经有21人回复
2楼2015-05-11 11:04:44
20