[HTML version][PDF version][Article Abstract][CIF][3d view][Structure Factors][Supplementary Material][Issue contents]  [Buy article online]

[Contents scheme]

Acta Cryst. (2007). E63, m2480-m2481  [ doi:10.1107/S1600536807042857 ]

[mu]-Sulfato-1[kappa]O:2[kappa]O-[mu]-oxo-bis[tris(2-pyridylmethyl)amine-[kappa]4N,N',N'',N''']diiron(III) diperchlorate acetonitrile/water (0.75/0.25) solvate

C. M. Smith and R. E. Norman

Key indicators

checkCIF/PLATON results

No syntax errors found




Alert level A
PLAT223_ALERT_4_A Large Solvent/Anion  H     Ueq(max)/Ueq(min) ...       5.11 Ratio
Author Response: There is a solvent cavity. In the original stages of solution and refinement, this was modelled with a single acetonitrile molecule in the asymmetric unit with full occupancy. The thermal parameters continued to grow and there was a persistent peak of electron density near the nitrile carbon atom. This feature was assigned to an oxygen atom of a water molecule, and apparent hydrogen atom positions were found. The populations of the acetonitrile and water were fixed at 0.75 and 0.25 respectively which produced a model with relatively reasonable thermal parameters. I was asked to reconsider the occupancies and place the hydrogen atoms of the water molecule in chemically more reasonable positions. When the occupancies were refined, they all increased as did the thermal parameters. In particular N1 increased from a B~iso~ of 8.8506 to 10.092. R and wR did not improve significantly. The occupancies were returned to their original values, and the hydrogen atoms placed in chemically more reasonable positions. This resulted in an increase of the O6 U~eq~ from 0.111(6) to 0.119(6) which generated this alert. 

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         C1     
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      18.00 Perc.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          2     
            FE1 -O1  -FE2 -N21  -144.70  0.40   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         25     
            FE2 -O1  -FE1 -N14  -163.80  0.80   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         57     
            O1  -FE1 -N14 -C116  -18.80  0.90   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         58     
            O1  -FE1 -N14 -C126 -141.20  0.80   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         59     
            O1  -FE1 -N14 -C136  100.20  0.80   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         60     
            O1  -FE2 -N21 -C211  127.20  0.40   1.555   1.555   1.555   1.555  
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         61     
            O1  -FE2 -N21 -C215  -40.20  0.60   1.555   1.555   1.555   1.555  


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

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

Copyright © International Union of Crystallography
IUCr Webmaster