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[求助]
遇到一个奇怪的审稿人，对晶体提出一堆问题，求高手指点迷津，谢谢！在线等 已有1人参与
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Firstly, in every CIF the embedded RES file (_shelx_res_file) does not match the _shelx_res_checksum entry - which means that the RES is not the one generated by SHELXL but was edited later. This practice is not acceptable and checksum was introduced specifically to prevent it. For three structures, 1, 2 and 3, the same problem appears with the embedded HKL file, which (I suspect) was replaced by an altogether different one (see below). Please leave the embedded RES and HKL (as well as FAB, where applicable) as they are generated automatically - they are there for good reason. For structures 1, 2 and 3，In each case, the solvent-masking procedure (PLATON SQUEEZE) was applied to the contents of large solvent-accessible voids. In such cases, its is mandatory to submit the original (before SQUEEZE and before merging Laue equivalents) HKL file for checking purposes. The old (1999) version of SQUEEZE generated a peculiar file containing both the merged (!) original structure factors and the corrections in a single line (HKP format). Note that important information is lost in the process of merging equivalent (important, e.g. if symmetry is in doubt). Today, SQUEEZE generates the FAB file (with corrections) and the original HKL under an amended name (_sq). Some intermediate versions were generating both options simultaneously, labelled with _sq_s and _sq_d extensions in the filename. Here we have some strange confusion: all three CIF files contain a FAB file (new version!) but also an old-style HKL (HKP) file. What is worse, when I extracted from the latter the initial HKL - I found that this one had been already processed by SQUEEZE (so, it was applied twice!). Thus, in fact the starting HKL is not available and I cannot make the final assessment. A propos, in all three cases the embedded SQUEEZE output gives a clear alarm signal: negative number of masked electrons, e.g. for 2  ,loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.129 -0.110 0.137 289 -12 ' ' 2 0.870 0.110 0.863 289 -12 ' ' 3 0.871 0.390 0.363 289 -12 ' ' 4 1.130 0.610 0.637 289 -12 ' ' I am surprised that the authors did not take notice of this. It is also clear that the present CIFs could not be generated by SHELXL - the authors for some reason removed the HKL-format files and replaced (manually) with HKP-format. Why? To repeat: I need the original and unmerged HKL. |
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wuhuzxc: 金币+50 2018-01-22 09:50:16
感谢参与，应助指数 +1
wuhuzxc: 金币+50 2018-01-22 09:50:16
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没什么奇怪的，基本的意思是你的hkl和res不相符，用新版的shelx精修就好了，另外就是hkp文件 发自小木虫Android客户端 |
2楼2018-01-21 23:20:47
zhaopch_2015
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5楼2018-01-22 10:54:05
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