013-精修A,B类错误的技巧.doc

013晶体解析心得精修AB类错误的技巧PLAT412_ALERT_2_C Short Intra XH3 . XHn H9 . H13C . 1.87 Ang.对策：在Ins文件中添加Dfix 2.45 0.01 h9 h13c 指令，XL XL.(尝试调整比1.87大的数)范例：wq-5-36-2PLAT413_ALERT_2_B Short Inter XH3 . XHn H2D . H2D . 2.06 Ang.对策：在Ins文件中添加Dfix 2.52 0.01 h2d h2d 指令，XL XL.(尝试调整比2.06大的数)范例：Wq1-5PLAT430_ALERT_2_B Short Inter D.A Contact O2 . N1 . 2.66 Ang.dfix 2.80 0.01 o2 n1PLAT230_ALERT_2_B Hirshfeld Test Diff for O2 - C10 . 7.15 suPLAT431_ALERT_2_C Short Inter HL.A Contact Cl1 . N3 . 3.11 Ang.dfix 2.90 0.01 o2 n1无B类错误,但是PLAT431_ALERT_2_C Short Inter HL.A Contact Cl1 . N3 . 3.11 Ang.-OKdfix 3.00 0.01 o2 n1无B类错误,但是PLAT431_ALERT_2_C Short Inter HL.A Contact Cl1 . N3 . 3.11 Ang.-OKdfix 3.10 0.01 o2 n1无B类错误,但是PLAT430_ALERT_2_C Short Inter D.A Contact O2 . N1 . 2.90 Ang.-OK范例：p16-9PLAT230_ALERT_2_B Hirshfeld Test Diff for O9 - C29 . 7.97 su对策：在Ins文件中添加Delu 0.02 0.01 o9 c29指令，XL XL. (0.02 0.01必需成倍数关系) 范例：f10, f15-2, e75PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cu1 - Cl1 . 13.26 sudelu 0.01 0.005 cu1 cl1 PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) . 4.07 Ratio对策：在Ins文件中添加simu 0.005 0.01 3.8 $c 指令，XL XL(0.005 0.01必需成倍数关系)范例：e75PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) . 4.12 RatioPLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low . 0.94对策：在Ins文件中添加omit -3.00 50.02 指令，XL XL. 范例：f15-2， e11, ye-12-00PLAT057_ALERT_3_B Correction for Absorption Required RT(exp) . 1.22对策：在Ins文件中添加size 0.21 0.19 0.18 指令，XL XL. (调整a,b,c紧凑些, 亦即三者之间的差值小一些)范例：wq1-2PLAT148_ALERT_3_B su on the c - Axis is Too Large (x 1000) . 20 Ang.对策：尝试调小ins文件中c - Axis的数据, XL XL.范例：f15-4ZERR 6.00 0.0143 0.0143 0.0222 0.000 0.000 0.000ZERR 6.00 0.0143 0.0143 0.0182 0.000 0.000 0.000PLAT148_ALERT_3_B su on the c - Axis is Too Large (x 1000) . 18 Ang.ZERR 6.00 0.0143 0.0143 0.0152 0.000 0.000 0.000PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu2 对策：在Ins文件中添加simu 0.01 0.02 3.8 cu2 o9 o10 o11 o12 n3 指令，XL XL. (尝试0.01 0.02或0.02 0.04) 包含cu2的周围的原子范例：f9-34PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C11 范例：p4-2PLAT035_ALERT_1_A No _chemical_absolute_configuration info given . ? 对策：在Cif文件中添加 _chemical_absolute_configuration s _refine_ls_structure_factor_coef Fsqd_refine_ls_matrix_type full _refine_ls_weighting_scheme calc_refine_ls_structure_factor_coef Fsqd_chemical_absolute_configuration s_refine_ls_matrix_type full _refine_ls_weighting_scheme calc范例：p16-9PLAT053_ALERT_1_A Minimum Crystal Dimension Missing (or Error) . ?PLAT054_ALERT_1_A Medium Crystal Dimension Missing (or Error) . ?PLAT055_ALERT_1_A Maximum Crystal Dimension Missing (or Error) . ?对策：在Ins文件中添加size a b c指令，XL XL（a,b,c的值见Pcf文件）范例：e11PLAT060_ALERT_4_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .3.49 对策：在Ins文件中添加size a b c指令，调整a b c 的相应比例，XL XL. 范例：e11PLAT761_ALERT_1_A CIF Contains no X-H Bonds . . . ?PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles . ?对策：在Ins文件中添加bond $h指令，XL XL. 范例：e11DIFF003_ALERT_1_A _diffrn_measurement_device_type is missing Diffractometer make and type. Replaces _diffrn_measurement_type.DIFF005_ALERT_1_A _diffrn_measurement_method is missing Mode of intensity measurement and scan.DIFF019_ALERT_1_A _diffrn_standards_number is missing Number of standards used in measurement.DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity.对策：用Pcf文件中的内容,代替Cif文件中的的？_diffrn_radiation_source fine-focus sealed tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ?_diffrn_radiation_source fine-focus sealed tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD area detector_diffrn_measurement_method phi and omega scans? -P1-4PLAT420_ALERT_2_B D-H Without Acceptor O3 - H3B . ? 以下错误均为晶体本身所引起，不可修复PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low . 31 Perc.PLAT022_ALERT_3_B Ratio Unique / Expected Reflections too Low . 0.89 RINTA01_ALERT_3_B The value of Rint is greater than 0.15 Rint given 0.152PLAT020_ALERT_3_B The value of Rint is greater than 0.10 . 0.15PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang . 19 PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 189.00 A*3调整GooF（S）值Refine时，适当改变Weights Suggested的值，Weights值越大，GooF值越小。（整个过程对R1 、R2的值略有影响）(以e-11为