CIF常见错误及应对策略

checkCIF/PLATON reportNo syntax errors found. CIF dictionary Interpreting this report Datablock: 4-926Bond precision:C-C = 0.0104 A Wavelength=0.71073 Cell:a=8.1996(12)b=24.564(4)c=15.512(2) alpha=90beta=95.884(3)gamma=90Calculated ReportedVolume3107.9(8)3107.9(8)Space group P 21/c P2(1)/cHall group-P 2ybc ?Moiety formula C25 H36 B Ir N6 O4, C H2Cl2C25 H36 B Ir N6 O4, C H2Cl2Sum formula C26 H38 B Cl2 Ir N6 O4C26 H38 B Cl2 Ir N6 O4Mr772.55772.53Dx,g cm-3 1.651 1.651Z44Mu (mm-1) 4.509 4.509F0001536.01536.0F000’1532.02h,k,lmax11,34,2111,34,21Nref9072 8739Tmin,Tmax0.258,0.6970.280,0.700Tmin’0.258Correction method= ’MULTI-SCAN’Data completeness= Ratio = 0.963Theta(max)= 30.010R(reflections)= 0.0536( 6904)wR2(reflections)= 0.1269( 8739)S = 1.043Npar= 369The following ALERTS were generated. Each ALERT has the formattest-name_ALERT_alert-type_alert-level.Click on the hyperlinks for more details of the test.Alert level BPLAT366_ALERT_2_B Short? 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: 0.280 0.700Tmin and Tmax expected: 0.250 0.697RR = 1.114Please check that your absorption correction is appropriate.Author Response: The absorption correcttion (SADABS, multi-scan) wasfound to be appropriate, PLATON necessarily overestimates absorptioneffects.PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96Author Response: Due to broad reflections, some of them had to be removedbecause of inacceptable disagreement with equivalents.PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.55 Ratio Author Response: Remote terminations of a Ir complex with higher mobility.PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.18 Ratio Author Response: Remote terminations of a Ir complex with higher mobility.PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ir - C51 .. 7.22 su Author Response: Moderate data quality in context with desolvation andIr as heavy atom.PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang (10)Author Response: Moderate data quality in context with desolvation andIr as heavy atom.PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 51.00 A**3 Author Response: The structure contains continuous channels extending atx,0.5,0 and x,0,0.5 along the a-axis. These channels are loosely filled withcomparatively well ordered CH2Cl2. The remaining voids between theCH2Cl2 molecules (51 \%A^3^ per cavity, four equivalent cavities per unitcell) might be suitable to take up further solvent (crystals from CH2Cl2 /pentane), but none was seen in difference Fourier syntheses and squeezingwith program PLATON did not give significant improvement or change.PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) (3)0 ALERT level A = In general: serious problem1 ALERT level B = Potentially serious problem8 ALERT level C = Check and explain0 ALERT level G = 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, methodology, query or suggestion0 ALERT type 5 Informative message, checkDatablock: 6-897Bond precision:C-C = 0.0086 A Wavelength=0.71073Cell:a=13.7032(12)b=13.9350(12)c=15.1568(14)alpha=90beta=90gamma=90Calculated ReportedVolume2894.3(4)2894.3(4)Space group P 21 21 21 P2(1)2(1)2(Hall group P 2ac 2ab ?Moiety formula C23 H32 B Cl Ir N7 O4C23 H32 B Cl Ir N7 O4Sum formula C23 H32 B Cl Ir N7 O4C23 H32 B Cl Ir N7 O4Mr709.04709.02Dx,g cm-3 1.627 1.627Z44Mu (mm-1) 4.745 4.745F0001400.01400.0F000’1395.42h,k,lmax19,19,2119,19,21Nref4696( 8475)8304Tmin,Tmax0.418,0.5660.330,0.570Tmin’0.063Correction method= ’MULTI-SCAN’Data completeness= 1.77(0.98)Theta(max)= 30.040R(reflections)= 0.0381( 6683)wR2(reflections)= 0.0680( 8304)S = 0.996Npar= 345The following ALERTS were generated. Each ALERT has the formattest-name_ALERT_alert-type_alert-level.Click on the hyperlinks for more details of the test.Alert level APLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.11 Ratio Author Response: One terminal COOMe group (C54, O58, O59, C510) issomewhat mobile despite low temperature measurement at 173K. This isprobably in context with a solvent content of the crystal largely lost prior toX-ray data collection (see below).Alert level BPLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.21 Ratio Author Response: One terminal COOMe group (C54, O58, O59, C510) issomewhat mobile despite low temperature measurement at 173K. This isprobably in context with a solvent content of the crystal largely lost prior toX-ray data collection (see below).Alert level CPLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang (9)Author Response: One terminal COOMe group (C54, O58, O59, C510) issomewhat mobile despite low temperature measurement at 173K. This isprobably in context with a solvent content of the crystal largely lost prior toX-ray data collection (see below).PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 58.00 A**3 Author Response: The structure was apparently a solvate, crystallized fromdichloromethane / pentane, and has largely lost the solvent prior to X-raymeasurement during transport. 4 separate symmetry equivalent solventcavities of 58.00 A**3 each exist in the unit cell. Application of procedureSQUEEZE (program PLATON) did not bring about a significant improval ofrefinement results and therefore was not retained for the final refinement. Thecompound is therefore considered as a DESOLVATE with no solvent contentgiven in chemical formula and quantities derived thereof.PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) (4)Alert level GREFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the 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_total 8304Count of symmetry unique reflns 4696Completeness (_total/calc) 176.83%TEST3: Check Friedels for noncentro structureEstimate of Friedel pairs measured 3608Fraction of Friedel pairs measured 0.768Are heavy atom types Z>Si present yesAuthor Response: The estimate ic correct. Note that the compound was aracemate which crystallized in a chiral space group. Absolute configurationis therefore not of importance.1 ALERT level A = In general: serious problem1 ALERT level B = Potentially serious problem3 ALERT level C = Check and explain1 ALERT 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 type3 Indicator that the structure quality may be low2 ALERT type 4 Improvement, methodology, query or suggestion0 ALERT type 5 Informative message, checkPublication of your CIF in IUCr journalsA basic structural check has been run on your CIF. These basic checks will be run on all CIFs submitted for publication in IUCr journals (Acta Crystallographica, Journal of Applied Crystallography, Journal of Synchrotron Radiation); however, if you intend to submit to Acta Crystallographica Section C or E, you should make sure that full publication checks are run on the final version of your CIF prior to submission.Publication of your CIF in other journalsPlease refer to the Notes for Authors of the relevant journal for any special instructions relating to CIF submission.PLATON version of 09/07/2006; check.def file version of 27/06/2006。