(IUCr) Crystallography Journals Online checkcif report

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Acta Cryst. (2006). E62, m492-m495 [ doi:10.1107/S1600536806004636 ]

-Oxo-bis[(diethyl 6,17-dimethyldibenzo[a,h]-5,9,14,18-tetraaza[14]annulene-7,16-dicarboxylato)iron(III)] sesquihydrate

E.-G. Jäger, J. Knaudt and W. Imhof

Online 15 February 2006

Key indicators

Single-crystal X-ray study
T = 213 K
Mean (C-C) = 0.006 Å
Disorder in main residue
R factor = 0.047
wR factor = 0.131
Data-to-parameter ratio = 13.2

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level A
PLAT220_ALERT_2_A Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       7.72 Ratio

Author Response: All atoms are correctly assigned, the composition of the compound is clear from other analytical data. The reason for this problem are disordered methyl groups which nevertheless could not be resolved.

PLAT222_ALERT_3_A Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       5.17 Ratio

PLAT242_ALERT_2_A Check Low       Ueq as Compared to Neighbors for        C17

Author Response: The methyl group C18 is disordered. Unfortunately this disorder could not be resolved.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O10

Author Response: This is indeed one of the solvate water molecules. H-atoms could not be resolved from Difference Fourier Analysis.

PLAT430_ALERT_2_A Short Inter D...A Contact  O11X   ..  O11X    ..       2.45 Ang.

Author Response: This is caused by the highly disordered water molecule O11 which is only weakly bound and in addition to being disordered thus shows an site occupation factor below 1.

PLAT432_ALERT_2_A Short Inter X...Y Contact  C32X   ..  C32X    ..       2.75 Ang.

Author Response: This effect again is due to disorder of the ethyl group which unfortunately could not be resolved.


Alert level B
PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............      24.98 Deg.

Author Response: Since the criterion for MoKa is 25.24 deg and the data parameter ratio for I looks alright, I hope this is not a real problem.

PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          4

Author Response: Again this is due to the disorder of some of the ethyl substituents which could not be resolved.

PLAT430_ALERT_2_B Short Inter D...A Contact  O10    ..  O11     ..       2.65 Ang.

Author Response: This is caused by the highly disordered water molecule O11 which is only weakly bound and in addition to being disordered thus shows an site occupation factor below 1.


Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio 
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.01 Ratio

PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O4     
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for       C17X

Author Response: The methyl group C18 is disordered. Unfortunately this disorder could not be resolved.

PLAT301_ALERT_3_C Main Residue  Disorder .........................       5.00 Perc. 
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      17.00 Perc. 
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....       <O11     
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....      <O11X     
PLAT430_ALERT_2_C Short Inter D...A Contact  O1     ..  O10     ..       2.89 Ang.

Author Response: This is caused by the highly disordered water molecule O11 which is only weakly bound and in addition to being disordered thus shows an site occupation factor below 1.

PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .      31.00 A   3  
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.12 Ratio 
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      27.30 Deg.  
              C6X  -C5   -C6      1.555   1.555   1.555                         
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.23 Deg.  
              N2   -C8   -FE1     1.555   1.555   1.555                         
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.47 Deg.  
              N3   -C13  -FE1     1.555   1.555   1.555                         
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      30.40 Deg.  
              C17  -O4   -C17X    1.555   1.555   1.555                         
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.38 Deg.  
              N6   -C34  -FE2     1.555   1.555   1.555                         
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.09 Deg.  
              N7   -C39  -FE2     1.555   1.555   1.555                         
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2       
              O                                                                 

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C52 H52 Fe2 N8 O10.5
            Atom count from _chemical_formula_moiety:C52 H55 Fe2 N8 O10.5

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

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