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铁杆木虫 (正式写手)

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注册: 2005-11-22
性别: GG
专业: 无机材料化学

[交流] 【请教】单晶衍射数据的优劣已有4人参与

单晶衍射数据精修后，得到了主结构，但是Rint太大，无法减小。其中，所测样品为一薄片状晶体。请问网友是不是收集的数据很差？是否需要重新收集数据？另外请教一下，判断衍射数据优劣的标准通常是什么？

谢谢了！

部分精修结果如下：
R1 =  0.1514 for 2339 Fo > 4sig(Fo)  and  0.2071 for all 3749 data
wR2 =  0.3621,  GooF = S = 1.162,  Restrained GooF = 1.162  for all data
R1 =  0.2010 for 3749 unique reflections after merging for Fourier

部分lst文件数据如下：
h k l    Fo^2    Sigma    Why rejected
0  11 0    13.83    1.47    observed but should be systematically absent
0  21 2    29.02    6.87    observed but should be systematically absent
3 1 0    23.44    3.59    observed but should be systematically absent
7 8 0    71.90    7.59    observed but should be systematically absent
7 9 0    116.37    7.04    observed but should be systematically absent
7  10 0    162.77    6.58    observed but should be systematically absent
7  11 0    191.17    5.70    observed but should be systematically absent
7  12 0    234.08    5.69    observed but should be systematically absent

8967  Reflections read, of which 727  rejected
  -9 =< h =<  5, -24 =< k =< 30, -24 =< l =< 23, Max. 2-theta = 57.59
   8  Systematic absence violations

Inconsistent equivalents etc.
h k l    Fo^2 Sigma(Fo^2)  N  Esd of mean(Fo^2)
2 1 0    344.97    2.39 2    16.32
4 4 0    1048.74    4.48 2    44.30
0 6 0    58.87    1.01 2    6.14
2 9 0    1743.35    8.70 2    69.16
2  18 0    461.06    3.85 2    20.57
2 0 1    802.81    4.34 2    78.93
3 0 1    2784.41    24.51 2 135.89
2 1 1    362.03    1.48 4    7.51
3 1 1    58.22    0.99 6    19.03
3 2 1    770.52    2.19 5    18.21
1 4 1    919.64    2.98 3    19.82
5 5 1    91.75    1.76 6    24.34
1 6 1    3303.71    12.93 6    85.97
6 7 1    123.92    2.41 6    30.50
1 8 1    967.55    2.33 5    12.82
6 8 1    185.68    2.44 6    50.21
7  10 1    163.01    3.99 4    59.29
7  11 1    192.18    3.89 4    59.39
3  12 1    1079.26    3.98 4    24.34
0  15 1    185.58    3.46 2    24.30
1  15 1    697.80    1.82 6    12.23
2 0 2    268.58    1.25 4    6.91
1 1 2    65.23    1.50 2    32.67
2 2 2    577.00    1.85 4    9.60
4 4 2    1182.15    4.11 3    30.87
3 7 2    316.46    1.76 5    9.14
2 8 2    565.08    2.33 4    14.94
2 9 2    1249.88    3.79 3    21.53
0  10 2    1558.01    8.58 2    61.85
0  14 2    756.50    3.48 3    17.74
3 0 3    1124.11    4.01 3    88.00
1 1 3    167.07    1.87 2    87.94
2 1 3    89.02    1.10 5    21.40
1 2 3    273.60    2.37 2    16.26
3 4 3    203.40    1.71 5    9.75
3 5 3    112.54    1.33 4    7.02
0 7 3    376.48    2.34 3    11.78
1 7 3    157.61    1.09 7    5.76
1 8 3    1154.44    2.62 6    14.32
3 8 3    427.71    2.24 4    15.39
2  10 3    234.55    3.23 2    29.17
3  12 3    857.52    4.30 3    25.26
8  13 3    205.22    6.46 2 108.50
1  15 3    205.27    1.67 4    9.08
1  20 3    708.61    4.18 4    45.73
4 1 4    78.35    1.42 6    14.46
1 3 4    319.44    1.98 3    10.96
2 3 4    235.85    1.55 4    7.86
0 6 4    295.31    1.49 4    8.46
4 6 4    299.39    3.14 3    15.85
** etc. **
   296  Inconsistent equivalents
3749  Unique reflections, of which    0  suppressed
R(int) = 0.1068    R(sigma) = 0.1192    Friedel opposites merged
Maximum memory for data reduction =  1814 / 37504

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