(IUCr) Crystallography Journals Online checkcif report

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Acta Cryst. (2004). E60, m637-m640 [ doi:10.1107/S1600536804008979 ]

Tetrakis(2,2'-bipyridine)tetra-₃-hydroxo-di--trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core

H. Zhao, J. Bacsa and K. R. Dunbar

Online 24 April 2004

Key indicators

Single-crystal X-ray study
T = 110 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R factor = 0.058
wR factor = 0.139
Data-to-parameter ratio = 16.2

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact  I1B    ..  C34     ..       3.14 Ang.

Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.


PLAT702_ALERT_1_A Angle   Calc    55.70(2), Rep    55.79(2), Dev..       4.50 Sigma 
              CO3  -CO4  -CO2     1.555   1.555   1.555                         

Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.88 Ratio

Author Response: Please see _publ_section_exptl_refinement. This is likely to be due to partial disorder. The anisotropic displacement parameters for some of the carbon atoms have a component perpendicular to the rings that is much larger than those nearly parallel to the rings. Following the advice given in the SHELX frequently-asked-questions; these atoms were not split. However, this approach results in larger ellipsoids for these atoms (and the physical validity of these ellipsoids representing harmonic motion may be doubtful).

PLAT432_ALERT_2_B Short Inter X...Y Contact  C24    ..  C3SB    ..       2.92 Ang.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.


PLAT432_ALERT_2_B Short Inter X...Y Contact  C33    ..  C4SB    ..       3.04 Ang.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.


PLAT432_ALERT_2_B Short Inter X...Y Contact  C34    ..  C3SB    ..       3.03 Ang.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97

Author Response: The completeness drops from 99% to 97% between 25 and 27 degrees.

PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms .....         12       
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          6

Author Response: see _publ_section_exptl_refinement.

PLAT213_ALERT_2_C Atom C23     has ADP max/min Ratio .............       3.40 prolat
PLAT213_ALERT_2_C Atom F43F    has ADP max/min Ratio .............       3.40 prolat
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.39 Ratio 
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C23     
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C33     
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C34     
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        C42     
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....       C44B     
PLAT301_ALERT_3_C Main Residue  Disorder .........................       5.00 Perc. 
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      44.00 Perc. 
PLAT432_ALERT_2_C Short Inter X...Y Contact  C4SA   ..  C34     ..       3.16 Ang.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.


PLAT432_ALERT_2_C Short Inter X...Y Contact  C34    ..  C4SB    ..       3.17 Ang.

 PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 (25%) of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.

 PROBLEM: Short Inter X...Y Contact  C33..C4SB = 3.04 Ang.
 RESPONSE:

 These non-bonded interatomic contacts are between the minor component
 of a disordered acetonitrile solvent molecule and carbon atom with
 a prolate thermal ellipsoid. The intermolecular contacts between the major
 components make chemical sense.


PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         26       
PLAT735_ALERT_1_C D-H     Calc   0.967(19), Rep    0.967(9) ......       2.11 su-Rat
              O2   -H2O     1.555   1.555                                       

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

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  14 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
   2 ALERT type 4 Improvement, methodology, query or suggestion

Tetrakis(2,2'-bipyridine)tetra-3-hydroxo-di--trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core

H. Zhao, J. Bacsa and K. R. Dunbar

Key indicators

checkCIF/PLATON results

Tetrakis(2,2'-bipyridine)tetra-₃-hydroxo-di--trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core