013-精修A,B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-5-36-2

PLAT413_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：Wq1-5

PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. N1 .. 2.66 Ang.

dfix 2.80 0.01 o2 n1

PLAT230_ALERT_2_B Hirshfeld Test Diff for O2 -- C10 .. 7.15 su PLAT431_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.

---OK dfix 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.

---OK

dfix 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：p16-9

PLAT230_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, e75

PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cu1 -- Cl1 .. 13.26 su

delu 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范例：e75

必需成倍数关系)

PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.12 Ratio

PLAT029_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--00

PLAT057_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：wq1-2

PLAT148_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：f15-4

ZERR 6.00 0.0143 0.0143 0.0222 0.000 0.000 0.000

ZERR 6.00 0.0143 0.0143 0.0182 0.000 0.000 0.000

PLAT148_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 0.000

PLAT242_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：f9-34

PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C11

范例：p4-2

PLAT035_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：p16-9

PLAT053_ALERT_1_A Minimum Crystal Dimension Missing (or Error) ... ? PLAT0_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：e11

PLAT060_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：e11

PLAT761_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：e11

DIFF003_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'

----P1-4

PLAT420_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.

RINTA01_ALERT_3_B The value of Rint is greater than 0.15 Rint given 0.152

PLAT020_ALERT_3_B The value of Rint is greater than 0.10 ......... 0.15

PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 19

PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 1.00 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为例) Weights Suggested GooF = S R1 R2 R(int) R(sigma) 0.061200, 0.311600 1.006 0.09 0.1726 0.0408 0.0655 0.071200, 0.311600 0.985 0.0550 0.1844 0.0408 0.0655 0.081200, 0.311600 0.966 0.0550 0.1957 0.0408 0.0655 0.061200, 0.411600 0.985 0.09 0.1739 0.0408 0.0655