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信源：https://journals.iucr.org/c/services/cif/reqdata.html | | 在线CIF帮助页面提供了投稿的CIF中所需的所有数据项的列表。作者需要在投稿之前使用checkCIF服务验证每个CIF和相关的结构因子，网址为http://journals.iucr.org/services/cif/checking/checkfull.html（参见《作者指南》第2.1节和第2.3节）。 |
| All validation alerts returned by checkCIF should be considered carefully and corrected as far as possible. Often the minor alerts point to easily fixed oversights, errors or omissions in the CIF or refinement strategy. In order to resolve some of the more serious items it may be necessary to carry out additional measurements or structure refinements. However, the nature of the study might justify the reported deviations from the checkCIF criteria and in such cases these should be commented upon in the paper. If level A alerts remain and are believed to be justified or unavoidable deviations, the validation response form (VRF) supplied by checkCIF should be completed and included in the submitted CIF, preferably with the addition of appropriate explanatory text in the published experimental section of the CIF. A completed VRF will look something like: | 应仔细考虑checkCIF返回的所有验证警报，并尽可能进行更正。通常，次要警报指向CIF或改进策略中易于修复的疏忽、错误或遗漏。为了解决一些更严重的项目，可能有必要进行额外的测量或结构精修。然而，研究的性质可能会证明报告的偏离checkCIF标准的合理性，在这种情况下，应在论文中对其进行评论。如果A级警报仍然存在，并且被认为是合理的或不可避免的偏差，则应填写checkCIF提供的验证响应表（VRF），并将其包含在提交的CIF中，最好在CIF的已发布实验部分添加适当的解释性文本。一个完整的VRF如下： |
#start Validation Reply Form _vrf_CHEMW03_6 ; PROBLEM:The ratio of given/expected molecular weight as calculated from the _atom_site*data lies outside... RESPONSE:SQUEEZE used to remove disordered diethyl ether solvent molecule, but thereported formula includes the solvent. See _refine_special_details. ; #end Validation Reply Form | At the time of submission, if the CIF is incomplete, has a syntax problem or generates validation A alerts and there is no corresponding validation response form (VRF) in the CIF, the submission process will not proceed to the next step until these matters are rectified. | 在提交时，如果CIF不完整、存在语法问题或生成验证A级警报，并且CIF中没有相应的验证响应表（VRF），则在这些问题得到纠正之前，投稿过程不会进入下一步。 |
| A commented list of some of the more important data requirements are summarized below and a more complete description of the data-validation checks applied to submitted CIFs is available from the online CIF help page. | 下面总结了一些更重要的数据要求的评论列表，在线CIF帮助页面上提供了适用于提交的CIF的数据验证检查的更完整描述。 |
| _chemical_formula_moiety _chemical_formula_sum | | | The chemical formula must be consistent with the atomic content specified by the _atom_site_ information, and match the _chemical_formula_weight. If atoms are missing from the atomic model (e.g. unlocated H atoms or solvent molecules suppressed by the 'SQUEEZE' or similar approach), the moiety and sum formulae should state the assumed overall formula. | 化学式必须与_atom_site_信息指定的原子含量一致，并与_chemical_formula_weight匹配。如果原子模型中缺少原子（例如未定位的氢原子或被“挤压”或类似方法抑制的溶剂分子），则部分和总和化学式应说明假定的总体化学式。 |
| _symmetry_space_group_name_H-M | | | The space group must encompass the highest symmetry permitted by the diffraction intensities and be consistent with the _cell_length_ and _cell_angle_ values. | 空间群必须包含衍射强度允许的最高对称性，并与_cell_length_和_cell_angle_值一致。 |
| _cell_formula_units_Z | | | The number of formula units in the unit cell must comply with that expected from the chemical formula, the space group and the _atom_site_ data. | 晶胞中的化学式单元数必须符合化学式、空间群和_atom_site_数据的预期值。 |
| _exptl_crystal_colour | | The crystal colour should comply with the codes listed in the online CIF help page. | |
| _exptl_crystal_size_max | | | Authors are encouraged to use crystals no larger than the incident X-ray beam diameter, particularly when heavy or strongly absorbing elements are present in the material. For best results, the crystal should be uniformly bathed in the X-ray beam. The size of the beam at the crystal is normally determined by inter alia the nature of the X-ray source and the beam optics. Note that with fine-focus sealed X-ray tubes, the use of a collimator larger than the filament diameter does not automatically increase the size of the uniform part of the incident beam. | 鼓励作者使用不大于入射X射线束直径的晶体，特别是当材料中存在重或强吸收元素时。为了获得最佳结果，晶体应该均匀地沐浴在X射线束中。晶体处光束的大小通常由X射线源和光束光学器件的性质等决定。请注意，对于精细聚焦密封X射线管，使用大于灯丝直径的准直器不会自动增加入射光束均匀部分的尺寸。 |
| _exptl_absorpt_correction_type | | Permitted absorption-type codes are listed in the online CIF help page. A type code must be accompanied by a reference to the method or the software used; this should be given in the field _exptl_absorpt_process_details. The need for absorption corrections, and the appropriate type of correction, is dependent on the value, _exptl_absorpt_coefficient_mu, and the crystal size values, _exptl_crystal_size_min, _mid and _max. If x is the medial size _mid, the product x provides an indication of the type of correction needed. **ytical or numerical corrections may be beneficial if x exceeds 1.0 and are strongly recommended if x is above 3.0. However, corrections based on **yses of equivalent and redundant reflections (multi-scan methods) are acceptable. Corrections are usually unnecessary if x is below 0.1. Refined absorption methods are discouraged except in special circumstances. The experimentally determined transmission-factor limits _exptl_absorpt_correction_T_min and _max should be consistent with those expected for the crystal shape and size, and. Whenever a multi-scan type absorption correction is being employed (e.g. by using SADABS), authors are also encouraged to measure a multiplicity of observations (measurement of symmetry equivalents or the same reflection at different crystal orientations) of at least 4. The algorithms used in such programs work best and produce the highest quality data only when the multiplicity of observations or coverage of the full sphere of reflections is high. | 在线CIF帮助页面中列出了允许的吸收类型代码。类型代码必须附有对所用方法或软件的参考文献；这应该在字段_exptl_absorpt_process_details中给出。吸收校正的需要和适当的校正类型取决于值_exptl_absorpt_coefficient_mu和晶体尺寸值_exptl_crystal_size_min、_mid和_max。如果x是中间尺寸_mid，则乘积x提供所需校正类型的指示。如果x超过1.0，分析或数值校正可能是有益的，如果x超过3.0，强烈建议进行分析或数值校正。然而，基于等效和冗余衍射点分析的校正（多扫描方法）是可以接受的。如果x小于0.1，通常不需要进行校正。除特殊情况外，不鼓励采用精修吸收法。实验确定的透射因子极限_exptl_absorpt_correction_T_min和_max应与晶体形状和尺寸的预期值一致。每当采用多扫描型吸收校正时（例如，通过使用SADABS），作者也被鼓励测量至少4的多次观测（对称当量的测量或不同晶体取向下的相同衍射点）。这种程序中使用的算法工作得最好，只有当观测的多重性或整个衍射点范围的覆盖率高时才能产生最高质量的数据。 |
| _diffrn_reflns_number _diffrn_reflns_av_R_equivalents _diffrn_reflns_limit_h_min _diffrn_reflns_limit_h_max _diffrn_reflns_limit_k_min _diffrn_reflns_limit_k_max _diffrn_reflns_limit_l_min _diffrn_reflns_limit_l_max | | | These items should refer to the complete set of measured data before any merging of symmetry-equivalent reflections, and not only to the unique set of data. | 这些项目应参考对称等效衍射点合并之前的完整测量数据集，而不仅仅是唯一的数据集。 |
| _reflns_number_total | | | The number of symmetry-independent reflections excludes the systematically extinct intensities. Authors are encouraged to use all symmetry-independent reflections in the refinement of the structure parameters. | 对称独立衍射点的数量排除了系统消失的强度。鼓励作者在结构参数的精修中使用所有对称独立衍射点。 |
| _reflns_threshold_expression | | | This threshold, which is based on multiples of I, F2 or F, serves to identify the significantly intense reflections, the number of which is given by _reflns_number_gt. These reflections are used in the calculation of _refine_ls_R_factor_gt. The multiplier in the threshold expression should be as small as possible, typically 2 or less. | 该阈值基于I、F2或F的倍数，用于识别显著强烈的衍射点，衍射点的数量由_reflns_number_gt给定。这些衍射点用于计算_refine_ls_R_factor_gt。阈值表达式中的倍数应尽可能小，通常为2或更小。 |
| _diffrn_reflns_theta_max | | | The θmax of measured reflections should be such that sinθmax/λ exceeds 0.6 Å-1 (i.e. θmax > 25° for Mo K; θmax > 67° for Cu K). It is expected that all possible unique reflections out to at least the specified minimum limits are measured. This provides the minimum number of reflections recommended for an average structural study. If intensities are consistently weak at the recommended θmax, low-temperature measurements may be needed unless a study at a specific temperature (or pressure) is being reported. | 测量衍射点的θ最大值应使sinθmax/λ超过0.6 Å-1（即，Mo K的θmax > 25°；Cu K的θmax > 67°）。预计至少在规定的最小限度内测量所有可能的唯一衍射点。这提供了平均结构研究建议的最小衍射点数量。如果强度在建议的θ最大值下持续较弱，则可能需要进行低温测量，除非报告在特定温度（或压力）下进行研究。 |
| _diffrn_measured_fraction_theta_max | | | This is the fraction of unique (symmetry-independent) reflections measured out to _diffrn_reflns_theta_max. Ideally, this should be as close to 1.0 as possible. | 这是测量到_diffrn_reflns_theta_max的唯一（与对称无关）衍射点的占比。理想情况下，这应该尽可能接近1.0。 |
| _diffrn_reflns_theta_full | | | When _diffrn_measured_fraction_theta_max is less than 1.0 because of some missing high-angle reflections, full is the diffractometer angle at which the measured reflection count is close to complete. The fraction of unique reflections measured out to this angle is given by _diffrn_measured_fraction_theta_full. | 当_diffrn_measured_fraction_theta_max由于某些高角度衍射点缺失而小于1.0时，full是测量衍射点计数接近完成的衍射仪角度。测量到此角度的唯一衍射点的占比由_diffrn_measured_fraction_theta_full给出。 |
| _diffrn_reflns_av_R_equivalents | | | Sufficient symmetry-equivalent reflections must be measured to provide a good estimate of the intensity reproducibility. This is particularly important when absorption corrections are applied (this value is calculated after the corrections are applied to the intensities). See also _exptl_absorpt_correction_type. | 必须测量足够的对称等效衍射点，以提供强度再现性的良好估计。当应用吸收校正时，这一点尤其重要（该值是在对强度应用校正后计算的）。另请参阅_exptl_absorpt_correction_type。 |
| _refine_ls_R_factor_gt | | | Note that this value is not intended as a reliable gauge of structure precision which is better determined from the standard uncertainties of the parameters (these depend on the number and reliability of the measured structure factors used in the refinement process). | 请注意，该值不是结构精度的可靠指标，结构精度可以更好地由参数的标准不确定度确定（这些不确定度取决于精修过程中使用的测量结构因子的数量和可靠性）。 |
| _refine_ls_number_reflns | | | The number of reflections used in the refinement should be as large as possible, and should, if possible, be greater than the number of refined parameters _refine_ls_number_parameters by at least a factor of 10 if the structure is centrosymmetric, or by a factor of 8 if it is not. Omission of outlier reflections should be avoided unless there is good reason and, in such cases, details of the omitted reflections and the reasons for doing so should be included in the _publ_section_exptl_refinement section. | 精修中使用的衍射点数量应尽可能多，如果可能，如果结构是中心对称的，则应至少比精修参数_refine_ls_number_parameters的数量大10倍，如果不是，则应大8倍。除非有充分的理由，否则应避免遗漏异常值衍射点。在这种情况下，应在_publ_section_exptl_refinement部分中包含遗漏衍射点的详细信息及其原因。 |
| _refine_ls_number_parameters | | | This is the number of coordinate, atomic displacement, scale, occupancy, restraint, extinction and other parameters refined independently in the least-squares process. It is possible, and sometimes desirable, to reduce this number by the appropriate application of geometric constraints. | 这是在最小二乘过程中独立精修的坐标、原子位移、尺度、占有率、限制、消光等参数的数量。通过适当应用几何约束来减少这个数字是可能的，有时也是可取的。 |
| _refine_ls_number_restraints | | | This gives the number of applied restraints. Concise details of what these restraints were, including any target values applied and the effective standard deviation of the restraint, should be included in the _publ_section_exptl_refinement section of the CIF. | 这给出了应用限制的数量。这些限制的简明细节，包括所应用限制的任何目标值和有效标准偏差，应包含在CIF的_publ_section_exptl_refinement部分。 |
| _refine_ls_hydrogen_treatment | | The codes which identify the treatment of H-atom parameters are listed in the online CIF help page. When special procedures for locating and refining H atoms have been employed, details about the treatment of H-atom sites should be placed in _publ_section_exptl_refinement. Authors should note the advice on H-atom treatment given in the SHELXL97 manual, §4.6: `For most purposes it is preferable to calculate the hydrogen positions according to well-established geometrical criteria and then adopt a refinement procedure which ensures that a sensible geometry is retained'. Authors should note that H-atom sites which have been fixed or constrained by geometry (e.g. riding) will not have s.u. values associated with them. | 在线CIF帮助页面中列出了识别氢原子参数处理的代码。如果采用了定位和精修氢原子的特殊程序，有关氢原子位点处理的详细信息应放在_publ_section_exptl_refinement中。作者应注意SHELXL97手册第4.6节中给出的关于氢原子处理的建议：“对于大多数目的，最好根据公认的几何标准计算氢位置，然后采用精修程序，确保保留合理的几何结构”。作者应该注意到，已经被几何结构（例如骑行）固定或约束的氢原子位点将不具有与其相关的标准不确定度值。 |
| _refine_ls_weighting_scheme | | | Weighting schemes for refinements should be based on the standard uncertainties in the measured reflection data. | 精修的权重方案应基于测量衍射点数据中的标准不确定度。 |
| _refine_ls_shift/su_max | | | This is the largest ratio of the parameter shift to standard uncertainty after the final round of refinement and is typically within ±0.01 if sufficient least-squares refinement cycles have been employed. A value above ±0.05 is considered unusual and values beyond ±0.1 are a sign of incomplete refinement, unaccounted-for disorder or high correlation between parameters that should be constrained. Authors should explain the reasons for a high value in _publ_section_exptl_refinement. | 这是最后一轮精修后参数偏移与标准不确定度的最**值，如果使用了足够的最小二乘精修循环，通常在±0.01以内。超过±0.05的值被认为是不寻常的，超过±0.1的值是不完整精修、未解释的无序或应约束的参数之间的高度相关性的迹象。作者应在_publ_section_exptl_refinement中解释值高的原因。 |
| _refine_diff_density_min _refine_diff_density_max | | | These values are expected to be small, especially for light-atom structures. If their magnitudes are such that a validation alert is generated, the label and the distance of the closest atom site should be reported in _publ_section_exptl_refinement. | 这些值预期会很小，特别是对于轻原子结构。如果它们的大小足以产生验证警报，则应在_publ_section_exptl_refinement中报告最近原子位点的标签和距离。 |
| _geom_ | | | All geometry values must originate from the submitted _atom_site_fract_ values. Only geometry values of significance to the structure will be published. These must be identified with a _geom_..._flag value of yes in the submitted CIF. Note that dimensions involving H-atom sites which have been fixed or constrained by geometry will not have s.u. values associated with them. Details of all bond lengths and angles involving H atoms must be included in the CIF, even if they have been constrained. | 所有几何参数值都必须源自投稿的_atom_site_fract_值。只有对结构具有重要意义的几何参数值才会发表。这些必须用投稿的CIF中_geom_..._flag值为“yes”来标识。请注意，涉及氢原子位点的尺寸（已被几何结构固定或约束）将不具有与之相关的标准确定值。涉及氢原子的所有键长和角度的细节必须包括在CIF中，即使它们受到了约束。 |
| _atom_site_ | | | | | | Atomic coordinates for molecular and the unique part of extended species should be supplied as connected sets. Whenever structure geometry permits, it is good practice to choose the set of connected coordinates which specify the asymmetric unit to have their centre of gravity within the primary unit cell. In systems with hydrogen-bonded networks, it is helpful to choose the asymmetric unit so that the minimum number of symmetry operators is required to specify the hydrogen-bond network. Among other things, these concepts help simplify the labelling of packing diagrams. | 分子的原子坐标和扩展物种的唯一部分应作为连通集提供。只要结构几何形状允许，最好选择一组连接坐标，指定不对称单元，使其重心位于主晶胞内。在具有氢键网络的系统中，选择不对称单元是有帮助的，这样就需要最小数量的对称算符来指定氢键网络。除其他外，这些概念有助于简化堆积图的标记。 |
| Values of _atom_site_occupancy should be 1.0 except for disordered or non-stoichiometric atom sites. Atom sites constrained to model disorder must be indicated by _atom_site_disorder_group. The overall packing in the structure will be checked for significant vacant regions (i.e. voids) indicating omitted solvent molecules. Deliberately omitted solvent molecules should be documented in the Comment or _publ_section_exptl_refinement sections. Note that s.u. values should not be appended to parameters which are fixed by symmetry, geometry or other constraints. | _atom_site_occupancy的值应为1.0，无序或非化学计量的原子位点除外。受模型无序约束的原子位点必须由_atom_site_disorder_group表示。将检查结构中的整体填充是否存在指示省略溶剂分子的显著空位区域（即孔隙）。故意省略的溶剂分子应记录或注释在_publ_section_exptl_refinement部分。请注意，标准不确定度值不应附加到由对称、几何或其他约束固定的参数中。 |
| _atom_site_aniso_U_ | | | Checks will be made for non-positive-definite anisotropic atomic displacement parameters. The ratio of maximum to minimum eigenvalues should not, except in special circumstances (e.g. disorder), exceed 5. | 将对非正定各向异性原子位移参数进行检查。最大值与最小值的比值不应超过5，除非在特殊情况下（如无序）。 |
| _refine_ls_abs_structure_details | | This item should describe the method applied, with a literature citation if necessary, and the number of Friedel pairs used in the determination of the absolute structure parameter. Absolute structure is relevant in any non-centrosymmetric space group. Authors should be aware of the difference between absolute structure and absolute configuration. To improve the precision of the absolute structure parameter, the use of a large fraction of the complete set of Friedel pairs in the data set is strongly recommended. When the precision of the absolute structure parameter renders the **ysis inconclusive, it is not necessary to merge Friedel-pair reflections, but if authors do merge Friedel-pair reflections before final refinement, they should mention that fact in the _publ_section_exptl_refinement section and not report a value for the Flack parameter in the CIF. Useful articles on this topic by Flack & Bernardinelli [Acta Cryst. (1999), A55, 908-915; J. Appl. Cryst. (2000), 33, 1143-1148] and Flack, Sadki, Thompson & Watkin [Acta Cryst. (2011), A67, 21-34] discuss the use, meaning and significance of the Flack parameter and its s.u. value. For pertinent comments on the determination of absolute structure, authors are also referred to the articles by Jones [Acta Cryst. (1986), A42, 57], Hooft et al. [J. Appl. Cryst. (2008), 41, 96-103; J. Appl. Cryst. (2010), 43, 665-668] and Parsons & Flack [Acta Cryst. (2004), A60, s61]. | 该项目应描述所应用的方法，如有必要，还应引用文献，以及在确定绝对结构参数时使用的Friedel衍射对的数量。绝对结构在任何非中心对称空间群中都是相关的。作者应该意识到绝对结构和绝对构型之间的区别。为了提高绝对结构参数的精度，强烈建议在数据集中使用大量的Friedel衍射对全集。当绝对结构参数的精度导致分析不确定时，没有必要合并Friedel衍射对衍射点，但如果作者在最终精修之前确实合并了Friedel衍射对衍射点，他们应该在_publ_section_exptl_refinement部分提到这一事实，并且不在CIF中报告Flack参数值。Flack & Bernardinelli [Acta Cryst. (1999), A55, 908-915; J. Appl. Cryst. (2000), 33, 1143-1148]和Flack, Sadki, Thompson & Watkin [Acta Cryst. (2011), A67, 21-34]关于这一主题的有用文章讨论了Flack参数及其标准不确定度值的使用、意义和重要性。关于绝对结构测定的相关评论，作者也可参考Jones [Acta Cryst. (1986), A42, 57], Hooft et al. [J. Appl. Cryst. (2008), 41, 96-103; J. Appl. Cryst. (2010), 43, 665-668]和Parsons & Flack [Acta Cryst. (2004), A60, s61]等文章。 |
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发表于 2025-3-16 07:32:54
