CIF常见错误及应对策略

1、checkClF/PLATON reportNo syntax errors found.C|F dictionary| Intepreting this reportDatablock: 4-926Bond precisi on:C-C = 0.0104 AWavele ngth=0.71073c=15.512 (2) gamma=90Cell:a=8.1996(12)b=24.564CalculatedReportedVolume3107.9(8)3107.9(8)Space groupP 21/cP2(1)/cHall group-P 2ybc?Moiety formulaC25 H36

2、 B Ir N6 O4, C H2C25 H36 B Ir N6 O4, C H2Cl2Cl2Sum formulaC26 H38 B Cl2 Ir N6 O4C26 H38 B Cl2 Ir N6 O4Mr772.55772.53Dx,g cm-31.6511.651Z44Mu (mm-1)4.5094.509F0001536.01536.0F000'1532.02h,k,lmax11,34,2111,34,21Nref90728739Tmi n,Tmax0.258,0.6970.280,0.700Tmi n'0.258alpha=90beta=95.884(3)Correc

3、tion method= ' MULTI-SCANTheta(max)= 30.010Data complete ness= Ratio = 0.963R(reflectio ns)= 0.0536( 6904)wR2(reflectio ns)= 0.1269( 8739)S = 1.043Npar= 369The following ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level.Click on the hyperlinks for more detai

4、ls of the test.Alert level B|PLAT366_ALERT_2_BShort? C(sp?)-C(sp?) Bond C53- C54.1.29 Ang.Author Response: C53-C54 is a eta2-bonded olefin ligand with C(sp2)=C(sp2) disposition.Alert level CABSTM02_ALERT_3_c The ratio of expected to reported Tmax/Tmin(RR) is > 1.10Tmin and Tmax reported: 0.2800.7

5、00Tmin and Tmax expected: 0.2500.697RR =1.114Please check that your absorption correction is appropriate.Author Resp on se: The absorpti on correctti on (SADABS, multi-sca n) was found to be appropriate, PLATON n ecessarily overestimates absorpti on effects.PLATU29_ALERT_3_C_diffrn_measuredraction_t

6、heta_full Low0.96Author Response: Due to broad reflections, some of them had to be removed because of in acceptable disagreeme nt with equivale nts.|PLAT220_ALERI_2_C Large Non-Solvent C Ueq(max)/Ueq(min) .2.55 RatioAuthor Response: Remote terminations of a Ir complex with higher mobility.|PLAT222_A

7、LER_3_C Large Non-Solvent H Ueq(max)/Ueq(min) .3.18 RatioAuthor Response: Remote terminations of a Ir complex with higher mobility.|PLAT232_ALERT_2_CHrshfeld Test Diff (M-X) Ir - C51.7.22 suAuthor Resp on se: Moderate data quality in con text with desolvati on and Ir as heavy atom.PLAT342_ALERT_3_C

8、Low Bond Precision on C-C bonds (x 1000) Ang .10Author Resp on se: Moderate data quality in con text with desolvati on and Ir as heavy atom.|PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .51.00 A*3Author Resp on se: The structure contains con ti nu ous cha nn els exte nding at x,0

9、.5,0 and x,0,0.5 along the a-axis. These cha nn els are loosely filled with comparatively well ordered CH2Cl2. The rema ining voids betwee n the CH2Cl2 molecules (51 %AA3A per cavity, four equivale nt cavities per unit cell) might be suitable to take up further solve nt (crystals from CH2Cl2 / penta

10、n e), but none was see n in differe nee Fourier syn theses and squeez ing with program PLATON did not give sig nifica nt improveme nt or cha nge.pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)30 ALERT level A 1 ALERT level B8 ALERT level C 0 ALERT level GIn general: serious problem Potenti

11、ally serious problem Check and explain General alerts; check0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data4 ALERT type 2 Indicator that the structure model may be wrong or deficient4 ALERT type 3 Indicator that the structure quality may be low1 ALERT type 4 Improvement, m

12、ethodology, query or suggestion0 ALERT type 5 Informative message, checkDatablock: 6-897S = 0.996Npar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3S = 0.996Npar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3Bond precisi on:C-C = 0.0086 AWavele ngth=0.71073S = 0.996Np

13、ar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3S = 0.996Npar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3Cell:a=13.7032(12)b=13.9350(12)alpha=90beta=90CalculatedVolume2894.3Space groupP 21 21 21Hall groupP 2ac 2abMoiety formulaC23 H32 B Cl Ir N7 O4Sum formulaC23 H

14、32 B Cl Ir N7 O4Mr709.04Dx,g cm-31.627Z4Mu (mm-1)4.745F0001400.0F000'1395.42h,k,lmax19,19,21Nref4696(8475)Tmi n,Tmax0.418,0.566Tmi n'0.063Correcti on method='MULTI-SCANc=15.1568(14) gamma=90Reported2894.3 P2(1)2(1)2( ?C23 H32 B Cl Ir N7 O4C23 H32 B Cl Ir N7 O4 709.02 1.62744.7451400.019,

15、19,21 8304 0.330,0.570Theta(max)= 30.040Data complete ness= 1.77(0.98)S = 0.996Npar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3S = 0.996Npar= 345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3R(reflectio ns)= 0.0381( 6683) wR2(reflectio ns)= 0.0680( 8304)S = 0.996Npar=

16、345pLAl/20_ALERl_4_C Npmber of Unusual/Non-Standard Label(s)3S = 0.996Npar= 345The following ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-levelClick on the hyperlinks for more details of the test.Alert level A|PLAI222_aleri_3_a L?rge Non-Solvent H Ueq(max)/Ueq(mi

17、n) .6.11 RatioAuthor Respo nse: One term inal COOMe group (C54, 058, 059, C510) is somewhat mobile despite low temperature measurement at 173K. This is probably in con text with a solve nt content of the crystal largely lost prior to X-ray data collecti on (see below).Alert level BPLAI220_ALERI_2_B

18、Lqrge Non-Solvent C Ueq(max)/Ueq(min) .4.21 RatioAuthor Respo nse: One term inal COOMe group (C54, 058, 059, C510) is somewhat mobile despite low temperature measurement at 173K. This is probably in con text with a solve nt content of the crystal largely lost prior to X-ray data collecti on (see bel

19、ow).Alert level C|PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang .9Author Respo nse: One term inal COOMe group (C54, O58, O59, C510) is somewhat mobile despite low temperature measurement at 173K. This is probably in con text with a solve nt content of the crystal largely lost prior

20、to X-ray data collecti on (see below).|PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .58.00 A*3Author Resp on se: The structure was appare ntly a solvate, crystallized from dichlorometha ne / pentane, and has largely lost the solve nt prior to X-ray measureme nt duri ng tran sport

21、. 4 separate symmetry equivale nt solve nt cavities of 58.00 A*3 each exist in the unit cell. Application of procedure SQUEEZE (program PLATON) did not bring about a sig nifica nt improval of refinement results and therefore was not retained for the final refinement. The compo und is therefore con s

22、idered as a DESOLVATE with no solve nt content given in chemical formula and quantities derived thereof.PLAT720_ALERT_4_C N»mber of Unusual/Non-Standard Label(s)4Alert level GREFLT03_ALERT_4_G P|lease check that the estimate of the number of Friedel pairs is correct. If it is not, please give t

23、he correct count in the _publ_section_exptl_refinement section of the submitted CIF.From the CIF: _diffrn_reflns_theta_max 30.04From the CIF: _reflns_number_total8304Count of symmetry unique reflns 4696 Completeness (_total/calc) 176.83% TEST3: Check Friedels for noncentro structure Estimate of Frie

24、del pairs measured 3608 Fraction of Friedel pairs measured 0.768 Are heavy atom types Z>Si present yesAuthor Response: The estimate ic correct. Note that the compound was a racemate which crystallized in a chiral space group. Absolute configuration is therefore not of importa nee.1ALERT level A=I

25、n general: serious problem1ALERT level B=Potentially serious problem3ALERT level C=Check and explain1ALERT level G=General alerts; check0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data2 ALERT type 2 Indicator that the structure model may be wrong or deficient2 ALERT type 3 Indicator that the structure quality may be low2 ALERT type 4 Improvement, methodology, query or suggestion0 ALERT type 5 Informative message, checkPublication of your