PLAT010_ALERT_1_A No Suitable (Embedded) Reflection Data Supplied Please Do !

(http://journals.iucr.org/services/cif/checking/PLAT010.html)

警告原因：CIF文件中無hkl信息。

解決策略：將hkl信息填入CIF文件即可。若使用2014及以上版本XL精修，則程序會自動將hkl信息寫入CIF文件。

PLAT011 Type_1 Test for any ATOMS found in CIF

No atom coordinates were detected in the CIF prior to the U(i,j) loop.

CIF中U(I,j)循環(huán)之前未檢測到任何原子坐標(biāo)。

(http://journals.iucr.org/services/cif/checking/PLAT011.html)

警告原因：CIF文件中沒有任何原子的信息。

解決策略：一般不會出現(xiàn)，除非是只擬合晶胞參數(shù)。如果誤操作刪除了原子信息，只需要重新精修生成CIF文件即可。

PLAT012 Type_1 Check for valid _shelx_res_checksum

The supplied CIF contains a '_shelx_res_file' record but not a valid associated '_shelx_res_checksum' record. A valid pair of embedded .res and .hkl files allows the automatic creation of a .fcf file with SHELXL20xy to be used for a detailed analysis of the refinement result. A file is valid when the calculated and reported checksums are identical. Only characters with an ASCII value higher than 32 contribute to the checksum. An embedded .res file might be broken, either due to tranfer errors or to deliberate or accidental post-refinement editing of its content.

所提供的CIF包含“_shelx_res_file”記錄，但缺失有效的相關(guān)的“_shelx_res_checksum”記錄。一對有效的嵌入式res和hkl文件允許使用SHELXL20xy自動創(chuàng)建fcf文件以用于對精修結(jié)果進(jìn)行細(xì)節(jié)分析。當(dāng)計算和報告的校驗和相同時，文件有校。只有ASCII值大于32的字符才構(gòu)成校驗和。嵌入的res文件可能由于傳輸錯誤或故意或意外地對其內(nèi)容進(jìn)行精修后編輯而損壞。

(http://journals.iucr.org/services/cif/checking/PLAT012.html)

例：PLAT012_ALERT_1_A No _shelx_res_checksum found in CIF...........Please Check

警告原因：CIF文件中包含“_shelx_res_file”記錄，即res文件的內(nèi)容，但是缺少“_shelx_res_checksum”這一信息。

解決策略：一般不會出現(xiàn)，如果誤操作刪除了checksum信息，只需要重新精修生成CIF文件即可。

PLAT013 Type_1 Check for _shelx_hkl_checksum

The supplied CIF contains a '_shelx_hkl_file' record but not a valid associated '_shelx_hkl_checksum' record. A valid pair of embedded .res and .hkl files allows the automatic creation of a .fcf file with SHELXL20xy to be used for a detailed analysis of the refinement result. A file is valid when the calculated and reported checksums are identical. Only characters with an ASCII value higher than 32 contribute to the checksum. An embedded .res file might be broken, either due to tranfer errors or to deliberate or accidental post-refinement editing of its content.

所提供的CIF包含“_shelx_hkl_file”記錄，但缺失有效的相關(guān)的“_shelx_hkl_checksum”記錄。一對有效的嵌入式res和hkl文件允許使用SHELXL20xy自動創(chuàng)建fcf文件以用于對精修結(jié)果進(jìn)行細(xì)節(jié)分析。當(dāng)計算和報告的校驗和相同時，文件有校。只有ASCII值大于32的字符才構(gòu)成校驗和。嵌入的res文件可能由于傳輸錯誤或故意或意外地對其內(nèi)容進(jìn)行精修后編輯而損壞。

(http://journals.iucr.org/services/cif/checking/PLAT013.html)

例：PLAT013_ALERT_1_A No _shelx_hkl_checksum found in CIF...........Please Check

警告原因：CIF文件中包含“_shelx_hkl_file”記錄，即hkl文件的內(nèi)容，但是缺少“_shelx_hkl_checksum”這一信息。

解決策略：一般不會出現(xiàn)，如果誤操作刪除了checksum信息，只需要重新精修生成CIF文件即可。

PLAT014 Type_1 Check for _shelxl_fab_checksum

The supplied CIF contains a '_shelx_fab_file' record but not a valid associated '_shelx_fab_checksum' record. A valid pair of embedded .res and .hkl files allows the automatic creation of a .fcf file with SHELXL20xy to be used for a detailed analysis of the refinement result. A file is valid when the calculated and reported checksums are identical. Only characters with an ASCII value higher than 32 contribute to the checksum. An embedded .res file might be broken, either due to tranfer errors or to deliberate or accidental post-refinement editing of its content.

所提供的CIF包含“_shelx_fab_file”記錄，但缺失有效的相關(guān)的“_shelx_fab_checksum”記錄。一對有效的嵌入式res和hkl文件允許使用SHELXL20xy自動創(chuàng)建fcf文件以用于對精修結(jié)果進(jìn)行細(xì)節(jié)分析。當(dāng)計算和報告的校驗和相同時，文件有校。只有ASCII值大于32的字符才構(gòu)成校驗和。嵌入的res文件可能由于傳輸錯誤或故意或意外地對其內(nèi)容進(jìn)行精修后編輯而損壞。

(http://journals.iucr.org/services/cif/checking/PLAT014.html)

警告原因：CIF文件中包含“_shelx_fab_file”記錄，即fab文件的內(nèi)容，但是缺少“_shelx_fab_checksum”這一信息。

解決策略：一般不會出現(xiàn)，如果誤操作刪除了checksum信息，只需要從新精修生成CIF文件即可。

PLAT015 Type_5 Check for refinement reflections details (SHELXL20xy)

No embedded reflection record was found in the CIF file that was created with SHELXL20xy (or XL). SHELXL20xy automatically includes the '.hkl' file that was used in the refinement (along with the final '.res' file) as an embedded comment with the dataname '_shelx_hkl_file'. Do not change this dataname in _iucr_refine_reflections_details. Such a record is useful for archival and follow-up calculations.

在使用SHELXL20xy(或XL)生成的CIF文件中找不到嵌入的衍射點記錄。SHELXL20xy自動以數(shù)據(jù)名“_shelx_hkl_file”將用于精修的hkl文件(以及最終的res文件)以嵌入式注釋包含在CIF中。切勿更改_iucr_refine_reflections_details中的該數(shù)據(jù)名。這樣的記錄對于存檔和后續(xù)計算非常有用。

(http://journals.iucr.org/services/cif/checking/PLAT015.html)

警告原因：CIF文件中未包含hkl和res文件信息，這些對審稿和后續(xù)修正是十分有用的，建議將hkl和res文件包含進(jìn)CIF文件中。

解決策略：使用ShelXL2014及以上版本進(jìn)行精修，程序會自動把hkl文件和ins文件加入到cif文件中。(如果使用OLEX2的話，在Report里HKL/RES中選擇Leave as is即可)。

PLAT016 Type_5 Check for refinement FAB file (SHELXL20xy)

No embedded .fab record was found in the CIF file that was created with SHELXL20xy (or XL). SHELXL20xy automatically includes the '.fab' file that was used in the refinement (along with the final '.res' & '.hkl' files) as an embedded comment with the dataname '_shelx_fab_file'. Do not change this dataname. Such a record is useful for archival and follow-up calculations.

在使用SHELXL20xy(或XL)生成的CIF文件中找不到嵌入的fab記錄。SHELXL20xy自動以數(shù)據(jù)名“_shelx_fab_file”將用于精修的fab文件(以及最終的res和hkl文件)以嵌入式注釋包含在CIF中。切勿更改該數(shù)據(jù)名。這樣的記錄對于存檔和后續(xù)計算非常有用。

(http://journals.iucr.org/services/cif/checking/PLAT016.html)

警告原因：CIF文件中未包含fab文件信息，這對審稿和后續(xù)修正是十分有用的，建議將fab文件包含進(jìn)cif文件中。(fab文件在SQUEEZE里使用較多)

解決策略：使用ShelXL2014進(jìn)行精修，程序會自動把hkl文件和ins文件加入到cif文件中。(如果使用OLEX2的話，在Report里HKL/RES中選擇Leave as is即可)。

PLAT017 Type_1 Check the Consistency of Scattering Type

Check for the correct scattering type assignment to this atom.

檢查原子的散射類型是否正確。

(http://journals.iucr.org/services/cif/checking/PLAT017.html)

警告原因：原子的散射類型有誤。

解決策略：一般不會出現(xiàn)，注意區(qū)分是中子衍射還是X射線衍射即可。

PLAT018 Type_1 Check _diffrn_measured_fraction_theta_max and full identical

The reported value of _diffrn_measured_fraction_theta_full is not equal to the reported value of _diffrn_measured_fraction_theta_max with _diffrn_reflns_theta_max and _diffrn_reflns_theta_full reported as equal.

CIF中“_diffrn_reflns_theta_max”和“_diffrn_reflns_theta_full”相等，但是“_diffrn_measured_fraction_theta_max”和“_diffrn_measured_fraction_theta_full”不相等。

(http://journals.iucr.org/services/cif/checking/PLAT018.html)

例：PLAT018_ALERT_1_C _diffrn_measured_fraction_theta_max .NE. *_full ! Check

警告原因：CIF中“_diffrn_reflns_theta_max”和“_diffrn_reflns_theta_full”相等，但是“_diffrn_measured_fraction_theta_max”和“_diffrn_measured_fraction_theta_full”不相等。

解決策略：一般不會出現(xiàn)，多數(shù)是手動填寫CIF時填寫錯誤所致。改成正確的數(shù)值即可。

PLAT019 Type_1 Check _diffrn_measured_fraction_theta_max/full consistency

The reported value of _diffrn_measured_fraction_theta_full is less than the reported value of _diffrn_measured_fraction_theta_max. Their ratio is reported when less than 1.0. When theta_full is less than theta_max such a value indicates that there are relatively more reflections missing at lower resolution. This ALERT can easily be addressed by updating the reported '*_full' values with the corresponding '*_max' values in the CIF.

_diffrn_measured_fraction_theta_full報告值比_diffrn_measured_fraction_theta_max報告值小。它們的比值小于1.0時將其報告出來。當(dāng)theta_full小于theta_max這樣一種情況出現(xiàn)時，表明在低分辨率處缺少相對較多的衍射點。通過使用CIF中相應(yīng)的“*_max”值來更新報告的“*_full”值，可以輕松解決此警告。

(http://journals.iucr.org/services/cif/checking/PLAT019.html)

警告原因：一般來說“_diffrn_measured_fraction_theta_full”要大于等于“_diffrn_measured_fraction_theta_max”。當(dāng)“_diffrn_measured_fraction_theta_full”小于“_diffrn_measured_fraction_theta_max”表明低角度衍射點有較大量的丟失。使用omit或者shel命令刪(壞)點過多。

解決策略：不用或者減少刪(壞)點數(shù)量。重新還原數(shù)據(jù)或者重新收集數(shù)據(jù)。

補充知識：

Cif項：_diffrn_reflns_theta_max

官方解釋：Maximum theta angle in degrees for the measured intensities. Thefraction of unique reflections measured out to this angle is given by _diffrn_measured_fraction_theta_max.

中文解釋：所有衍射數(shù)據(jù)的最大θ角即為_diffrn_reflns_theta_max。通過_diffrn_reflns_theta_max算出的數(shù)據(jù)完整度即為_diffrn_measured_fraction_theta_max。

Cif項：_diffrn_reflns_theta_full

官方解釋：The theta angle (in degrees) at which the measured reflection countis close to complete. The fraction of unique reflections measured out to thisangle is given by _diffrn_measured_fraction_theta_full.

中文解釋：衍射數(shù)據(jù)接近完整時的θ角即為_diffrn_reflns_theta_full。通過_diffrn_reflns_theta_full算出的數(shù)據(jù)完整度即為_diffrn_measured_fraction_theta_full。按照定義，_diffrn_reflns_theta_full會小于等于_diffrn_reflns_theta_max。按照定義，當(dāng)衍射數(shù)據(jù)合格時，_diffrn_measured_fraction_theta_full會大于等于_diffrn_measured_fraction_theta_max；當(dāng)小于時，會報PLAT019的Alert。

PLAT020 Type_3 Check Rint

The value of Rint (i.e. _diffrn_reflns_av_R_equivalents) should normally be considerably less than 0.12 and in the order of magnitude of the reported R-values. Rint may be relatively meaningless when based on a very limited number of averaged data. Higher values should be accompanied by a suitable explanation in the _publ_section_exptl_refinement section. However, authors should first ensure that there are not overlooked problems associated with the data or the space-group. Elevated values for _diffrn_reflns_av_R_equivalents may be indicative of a need to recollect the data from a crystal of higher quality or that there is a problem with the data treatment. Consider the following

(a) The absorption corrections are inadequate or inappropriate.

(b) The overall quality of the data may be poor due to the crystal quality.

(c) The crystal is very weakly diffracting, so that a large proportion of essentially "unobserved" reflections are being used in the refinement. You should consider using a better crystal or a data collection at low temperature and/or, if the compound is organic, using Cu radiation.

(d) You are working in the wrong crystal system or Laue group.

(e) You have only a very small number of equivalent reflections, which may lead to artificially high values of _diffrn_reflns_av_R_equivalents

Note that if _diffrn_reflns_av_sigmaI/netI is also large, the quality of the data should be considered to be suspect.

Rint值(即diffrn_reflns_av_R_equivalents)一般來說應(yīng)小于0.12，并且應(yīng)為報告的R值相當(dāng)?shù)臄?shù)量級。當(dāng)基于非常有限數(shù)量的平均數(shù)據(jù)時，Rint可能相對沒有意義(Rint值是對衍射數(shù)據(jù)的統(tǒng)計值，當(dāng)數(shù)據(jù)冗余度低時Rint值意義不大)。當(dāng)Rint值較大時，需要在CIF中_publ_section_exptl_refinement部分進(jìn)行合理解釋。但是，作者應(yīng)首先判斷數(shù)據(jù)本身和空間群是否存在易被忽視的問題。Rint高表明需用高質(zhì)量的晶體重新收集數(shù)據(jù)或者表明數(shù)據(jù)處理有問題。當(dāng)Rint高時可從如下方面考慮：

(a)吸收校正未做或不合適。

(b)由于晶體質(zhì)量一般導(dǎo)致數(shù)據(jù)質(zhì)量差

(c)晶體本身衍射能力弱，大量“不可見”衍射點被用于精修過程。建議采用更好的晶體在低溫下收集數(shù)據(jù)，如果化合物為有機物，采用Cu靶進(jìn)行測試。

(d)晶系或者Laue群定錯。

(e)等效點少或者冗余度低可能會導(dǎo)致Rint值高。

注意當(dāng)_diffrn_reflns_av_sigmaI/netI值高時，數(shù)據(jù)質(zhì)量可能很差。

(http://journals.iucr.org/services/cif/checking/PLAT020.html)

警告原因：Rint值超出預(yù)期范圍。

解決策略：首先確認(rèn)晶系和Laue群。再嘗試用Shel 999 0.84 截斷部分高角度的點。再嘗試重新還原和校正數(shù)據(jù)。如果都不行就只能重新挑選質(zhì)量好的晶體在低溫下用Cu靶收集數(shù)據(jù)了。