(IUCr) Crystallography Journals Online checkcif report

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Acta Cryst. (2003). E59, o1584-o1585 [ doi:10.1107/S160053680302097X ]

4-Ammonio-1-hydroxy-2,2,6,6-tetramethylpiperidin-1-ium dichloride monohydrate

T. Q. Hu, B. O. Patrick, D. A. Osmond and B. R. James

Online 30 September 2003

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.002 Å
R factor = 0.033
wR factor = 0.081
Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.93

Author Response: This problem of incomplete coverage is a common one for us, as our diffractometer has a large chi-circle and unreliable collision protection software, so achieving orientations that would allow us to collect all of the high-angle data is impossible. However, from the output below hopefully you can see that we have complete coverage out to 0.90 angstroms, near-complete data out to 0.86 angstroms, and that the only data missing is out beyond 0.86 angstroms.

 Redundancy vs Resolution
 

  Resolution      Calc  Percent of reflections measured N times, N =  %Comp %Comp
     range      unique    0     1     2     3     4   5-8  9-12   >12 shell cumul
 

   9.18 - 1.63     453  3.8   5.1   9.7  10.6   7.7  29.8  28.9   4.4  96.2  96.2
   1.63 - 1.30     420  0.7   2.1   5.0   9.0   5.7  28.1  45.0   4.3  99.3  97.7
   1.30 - 1.13     400  0.2   0.7   3.5   9.0   3.8  33.0  46.5   3.2  99.8  98.4
   1.13 - 1.03     397  0.0   0.3   2.8   5.5   6.5  32.2  49.9   2.8 100.0  98.7
   1.03 - 0.96     400  0.0   0.7   3.5   6.5   5.2  33.8  46.0   4.3 100.0  99.0
   0.96 - 0.90     386  0.0   2.6   2.6   6.5   6.0  36.0  42.0   4.4 100.0  99.1
   0.90 - 0.86     406  4.4   1.5   3.2   6.4   6.2  30.8  44.1   3.4  95.6  98.6
   0.86 - 0.82     381  8.9   6.6   9.2   8.7   5.8  28.6  30.2   2.1  91.1  97.7
   0.82 - 0.79     402 26.9   4.5   7.7  12.4   5.0  30.1  12.4   1.0  73.1  95.0
   0.79 - 0.76     380 41.8   8.4   3.4  12.1  11.1  20.8   2.4   0.0  58.2  91.6
 

   9.18 - 0.76    4025  8.4   3.2   5.1   8.7   6.3  30.3  34.9   3.0  91.6  91.6


PLAT707_ALERT_1_A D...A   Calc    3.833(6), Rep    3.531(5), Dev..      50.33 Sigma 
              C7   -CL2B    1.555   1.555                                       
PLAT726_ALERT_1_A H...A   Calc     3.05434, Rep     2.70000, Dev..       0.35 Ang.  
              H(7A)-CL2B    1.555   1.555                                       
PLAT728_ALERT_1_A D-H..A  Calc      137.32, Rep      142.00, Dev.        4.68 Deg.  
              C7   -H(7A)-CL2B    1.555   1.555   1.555                         

Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H14    ..  H15      =       2.09 Ang.  

Alert level C
CELLV02_ALERT_1_C  The supplied cell volume s.u. differs from that
            calculated from the cell parameter s.u.'s by > 2
            Calculated cell volume su =       2.44
            Cell volume su given      =       5.00
REFLT03_ALERT_3_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           27.87
           From the CIF: _diffrn_reflns_theta_full           0.00
           From the CIF: _reflns_number_total               3286
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         3552
           Completeness (_total/calc)             92.51%
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT213_ALERT_2_C Atom Cl2     has ADP max/min Ratio .............       3.10 prolat
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.38 Ratio 
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.39 Ratio 
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.44       
PLAT301_ALERT_3_C Main Residue  Disorder .........................       6.00 Perc. 
PLAT353_ALERT_3_C Long    N-H Bond (0.87A)   N2     -   H14      =       1.01 Ang.  

Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
           From the CIF: _diffrn_reflns_theta_max           27.87
           From the CIF: _reflns_number_total               3286
           From the CIF: _diffrn_reflns_limit_ max hkl   16.   10.   29.
           From the CIF: _diffrn_reflns_limit_ min hkl  -14.  -11.  -29.
           TEST1: Expected hkl limits for theta max
           Calculated maximum hkl   17.   12.   32.
           Calculated minimum hkl  -17.  -12.  -32.

   4 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion