(IUCr) Crystallography Journals Online checkcif report

[Contents scheme]

Acta Cryst. (2010). E66, o833 [ doi:10.1107/S1600536810008263 ]

Tetraphenylphosphonium octahydrotriborate

M. A. Beckett, P. N. Horton, M. B. Hursthouse and C. Pszolla

Online 13 March 2010

Key indicators

Single-crystal X-ray study
T = 120 K
Mean (C-C) = 0.008 Å
Disorder in solvent or counterion
R factor = 0.070
wR factor = 0.191
Data-to-parameter ratio = 10.3

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.78

Author Response: The data was collected based on a strategy for a body-centred tetragonal crystal system. It was only much later that the need to integrate and solve in triclinic crystal system by which time the crystals had gone (See experimental for additional information).

PLAT113_ALERT_2_A ADDSYM Suggests Possible Pseudo/New Space-group.        I-4

Author Response: Although the tetraphenylphosphonium cations do show the suggested additional symmetry, the octahydrotriborate anions do not. However, because of the relative contributions of the two ions, for which the cation dominates, a large percentage for the extra symmetry exists. Attempts to refine in I-4 occurred, but resulted in horrible modelling of disordered anions over symmetry sites and a more than doubling of the final R-factors.


Alert level B
PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem...         -4     
PLAT910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) .....         12      
PLAT911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L=  0.600       1633      
PLAT915_ALERT_3_B Low Friedel Pair Coverage ......................      31.64 Perc.
PLAT722_ALERT_1_B Angle   Calc       27.00, Rep      24(10) Dev...       3.00 Deg. 
              B42  -B41  -H15G    1.555   1.555   1.555                        
PLAT722_ALERT_1_B Angle   Calc       92.00, Rep       94.60 Dev...       2.60 Deg. 
              H41A -B41  -H15G    1.555   1.555   1.555                        
PLAT722_ALERT_1_B Angle   Calc      133.00, Rep      130.20 Dev...       2.80 Deg. 
              H41B -B41  -H15G    1.555   1.555   1.555                        
PLAT722_ALERT_1_B Angle   Calc       49.00, Rep      46(10) Dev...       3.00 Deg. 
              H45A -B41  -H15G    1.555   1.555   1.555                        

Alert level C
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          3      
PLAT245_ALERT_2_C U(iso) H45A    Smaller than U(eq) B42     by ...       0.01 AngSq
PLAT340_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..          8      
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          5      
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         B43     
PLAT732_ALERT_1_C Angle   Calc       42(3), Rep    41.2(13) ......       2.31 su-Ra
              B12  -B13  -H15B    1.555   1.555   1.555                        
PLAT732_ALERT_1_C Angle   Calc      100(3), Rep    99.6(14) ......       2.14 su-Ra
              B11  -B13  -H15B    1.555   1.555   1.555                        
PLAT732_ALERT_1_C Angle   Calc      101(3), Rep   101.0(14) ......       2.14 su-Ra
              B23  -B21  -H25A    1.555   1.555   1.555                        
PLAT732_ALERT_1_C Angle   Calc       42(3), Rep    41.7(13) ......       2.31 su-Ra
              B22  -B21  -H25A    1.555   1.555   1.555                        
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         10      
              B3 H8                                                            
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         11      
              B3 H8                                                            
PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600       1093      

Alert level G
REFLT03_ALERT_4_G  WARNING: Large fraction of Friedel related reflns may
                     be needed to determine absolute structure
           From the CIF: _diffrn_reflns_theta_max           27.48
           From the CIF: _reflns_number_total              13369
           Count of symmetry unique reflns        12230
           Completeness (_total/calc)            109.31%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1139
           Fraction of Friedel pairs measured     0.093
           Are heavy atom types Z>Si present        yes
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         48      
PLAT302_ALERT_4_G Note: Anion/Solvent Disorder ...................      17.00 Perc.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.70 Deg. 
              B2   -B1   -H5A     1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.20 Deg. 
              B1   -B2   -H5A     1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.50 Deg. 
              B3   -B2   -H5B     1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.70 Deg. 
              B2   -B3   -H5B     1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.80 Deg. 
              B12  -B11  -H15A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      40.90 Deg. 
              B11  -B12  -H15A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      40.70 Deg. 
              B13  -B12  -H15B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.20 Deg. 
              B12  -B13  -H15B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.70 Deg. 
              B22  -B21  -H25A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.70 Deg. 
              B21  -B22  -H25A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.70 Deg. 
              B23  -B22  -H25B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.90 Deg. 
              B22  -B23  -H25B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      44.60 Deg. 
              B32  -B31  -H35A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      43.80 Deg. 
              B31  -B32  -H35A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.20 Deg. 
              B33  -B32  -H35B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      43.00 Deg. 
              B32  -B33  -H35B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.80 Deg. 
              B42  -B41  -H45A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      24.00 Deg. 
              B42  -B41  -H15G    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.40 Deg. 
              B41  -B42  -H45A    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      43.20 Deg. 
              B43  -B42  -H45B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......       3.00 Deg. 
              B41  -B42  -H15G    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.00 Deg. 
              H45A -B42  -H15G    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.90 Deg. 
              B42  -B43  -H45B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      22.00 Deg. 
              B143 -B141 -H45B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      41.10 Deg. 
              B142 -B141 -H15G    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      40.30 Deg. 
              B141 -B142 -H15G    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      43.70 Deg. 
              B143 -B142 -H15H    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      36.00 Deg. 
              B141 -B143 -H45B    1.555   1.555   1.555                        
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      42.70 Deg. 
              B142 -B143 -H15H    1.555   1.555   1.555                        

   2 ALERT level A = In general: serious problem
   8 ALERT level B = Potentially serious problem
  13 ALERT level C = Check and explain
  32 ALERT level G = General alerts; check

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