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xi2004 老师：
DMF的问题解决啦。但是新的问题出现啦。由于选定了Cc空间群，platon建议C2/c。而且每轮精修后，都有一句提示：Possible racemic twinning or wrong absolute structure - try TWIN refinement。 看看了相关文章，加了句命令
TWIN -1 0 0 0 -1 0 0 0 -1 2
提示倒是消失了，但是不知道该命令加的对不对？
check cif 后有几个A alert：
Alert level A
SHFSU01_ALERT_2_A The absolute value of parameter shift to su ratio > 0.20
Absolute value of the parameter shift to su ratio given 0.803
Additional refinement cycles may be required.
PLAT057_ALERT_3_A Correction for Absorption Required RT(exp) ... 1.32
PLAT080_ALERT_2_A Maximum Shift/Error ............................ 0.80
PLAT211_ALERT_2_A ADP of Atom C16 is NPD ..................... ?
PLAT213_ALERT_2_A Atom N6 has ADP max/min Ratio ..... 6.50 oblat
PLAT213_ALERT_2_A Atom C2 has ADP max/min Ratio ..... 6.50 oblat
PLAT213_ALERT_2_A Atom C7 has ADP max/min Ratio ..... 6.30 prola
PLAT213_ALERT_2_A Atom C14 has ADP max/min Ratio ..... 11.30 oblat
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Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 97 PerFi
PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Space-group. C2/c
PLAT213_ALERT_2_B Atom C6 has ADP max/min Ratio ..... 5.00 oblat
PLAT213_ALERT_2_B Atom C11 has ADP max/min Ratio ..... 4.40 prola
PLAT213_ALERT_2_B Atom C12 has ADP max/min Ratio ..... 5.00 prola
感觉就是应该没有精修到收敛。 可是计算前后的权重已经一样的啊？ 如下是我最后一轮的XL，请老师指点：
Read instructions and data
Data: 6728 unique, 0 suppressed R(int) = 0.0509 R(sigma) = 0.0480
Systematic absence violations: 0 Bad equivalents: 0
wR2 = 0.0684 before cycle 1 for 6728 data and 336 / 336 parameters
GooF = S = 1.016; Restrained GooF = 1.016 for 2 restraints
Mean shift/esd = 0.249 Maximum = 1.228 for U33 C4 at 14:00:39
Max. shift = 0.021 A for H30A Max. dU = 0.002 for C14
wR2 = 0.0685 before cycle 2 for 6728 data and 336 / 336 parameters
GooF = S = 1.017; Restrained GooF = 1.017 for 2 restraints
Mean shift/esd = 0.327 Maximum = 1.554 for U33 C3 at 14:00:40
Max. shift = 0.024 A for H30A Max. dU =-0.003 for C14
wR2 = 0.0685 before cycle 3 for 6728 data and 336 / 336 parameters
GooF = S = 1.017; Restrained GooF = 1.016 for 2 restraints
Mean shift/esd = 0.298 Maximum = 1.465 for U33 C4 at 14:00:42
Max. shift = 0.023 A for H30A Max. dU = 0.003 for C14
wR2 = 0.0685 before cycle 4 for 6728 data and 336 / 336 parameters
GooF = S = 1.017; Restrained GooF = 1.016 for 2 restraints
Mean shift/esd = 0.216 Maximum = 0.898 for U33 C3 at 14:00:44
Max. shift = 0.019 A for H30A Max. dU =-0.002 for C14
wR2 = 0.0685 before cycle 5 for 6728 data and 2 / 336 parameters
GooF = S = 1.016; Restrained GooF = 1.016 for 2 restraints
R1 = 0.0305 for 5462 Fo > 4sig(Fo) and 0.0442 for all 6728 data
wR2 = 0.0685, GooF = S = 1.016, Restrained GooF = 1.016 for all data
R1 = 0.0358 for 3586 unique reflections after merging for Fourier
Highest peak 0.79 at 0.0843 0.5437 0.1594 [ 0.90 A from CD1 ]
Deepest hole -0.87 at 0.3062 0.9624 0.0540 [ 0.85 A from CD2 ] |
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