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Acta Cryst. (2005). E61, m1525-m1527  [ doi:10.1107/S1600536805019562 ]

Diethanolaminium cyclo-octa-[mu]2-fluoro-hexadeca-[mu]2-trimethylacetato-[kappa]32O:O'-heptachromium(III)nickel(II) ethyl acetate 0.5-solvate

F. K. Larsen, C. A. Muryn, J. Overgaard, G. A. Timco and R. E. P. Winpenny

Online 13 July 2005


Key indicators

checkCIF/PLATON results

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Alert level A PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 48
Author Response: Due to quite substantial disorder or high thermal motion of in particular the pivalate bridges the best procedure was to treat all the methyl carbon atoms as isotropic. Including anisotropic adp's did not lower the residual significantly.
PLAT220_ALERT_2_A Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       7.62 Ratio 
Author Response: Some of the pivalate groups exhibit rotational disorder while others appear very settled in the refined positions. Therefore, comparing all pivalate groups a large difference between Ueq will show up.
PLAT221_ALERT_4_A Large Solvent/Anion  C     Ueq(max)/Ueq(min) ...      10.00 Ratio 
Author Response: The diethanolamine is disordered over three positions, two of which are minor components with occupation factors close to 20%. Furthermore, the central part of the amine interacts through hydrogen bonding with the ring molecule while the outer parts are not fixed through bonding. Thi explains the large difference in Ueq in the solvent molecules.
PLAT773_ALERT_2_A Suspect C-C Bond in CIF:      C1B    -C2B     ..       1.75 Ang.  
Author Response: There is significant disorder in the central diethanolammonium moeity, and the geometries of separate disordered parts is not perfect.

Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.48 Ratio
Alert level C CHEMW01_ALERT_1_C The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.99 <> 1.01 Calculated formula weight = 4672.3018 Formula weight given = 4603.0400 CHEMW01_ALERT_1_C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 2.104 Test value = 1.800 DIFMX02_ALERT_1_C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25 Weighted R factor given 0.255 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT084_ALERT_2_C High R2 Value .................................. 0.26 PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 2.10 e/A   3 PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 4 PLAT214_ALERT_2_C Atom C2B (Anion/Solvent) ADP max/min Ratio 4.60 prolat PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O74 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C12 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C17 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C37 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C47 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C52 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C57 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C62 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C67 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C87 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for N1 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C1C PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C98 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1B PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1C PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1E PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1F PLAT301_ALERT_3_C Main Residue Disorder ......................... 10.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O1A PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O1B PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O2A PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O2B PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C96 - C96_a ... 1.43 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. N1C .. 2.80 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. O2A .. 2.97 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O2B .. 2.94 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. N1C .. 2.96 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F6 .. N1E .. 2.95 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F7 .. N1 .. 2.81 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F8 .. N1 .. 2.87 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F8 .. O1B .. 2.95 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F8 .. N1C .. 2.97 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C172 H320 Cr16 F16 N2 O70 Atom count from the _atom_site data: C173.0079 H295 Cr16 F16 N2.002 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C172 H320 Cr16 F16 N2 O70 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 344.00 346.02 -2.02 H 640.00 590.00 50.00 Cr 32.00 32.00 0.00 F 32.00 32.00 0.00 N 4.00 4.00 0.00 O 140.00 138.00 2.00
4 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 46 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 33 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 9 ALERT type 4 Improvement, methodology, query or suggestion

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