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Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program)

International Centre for Diffraction Data. Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program). Diffractometer alignment and calibration. International Centre for Diffraction Data. Sample preparation: synthesis, analysis. Data collection. File

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Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program)

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  1. International Centre for Diffraction Data Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program)

  2. Diffractometer alignment and calibration International Centre for Diffraction Data Sample preparation: synthesis, analysis Data collection File preparation: general form reflection file NBS*AIDS83 PDF-3 Phase analysis & indexing Data reduction: profile analysis, least squares ICDD

  3. Plan for the Use of Internal Standards International Centre for Diffraction Data Alignment with a certified X-ray standard, such as, Si, SRM-1976, SRM-676 (these are the preferred standards), or silver behenate * * obtained from the ICDD Pattern of certified standard should be sent to the ICDD annually

  4. Sample preparation International Centre for Diffraction Data 1. Synthesis 2. Chemical analysis (if possible) 3. Check purity by X-ray diffraction

  5. Data collection International Centre for Diffraction Data 1. Check the alignment before each experiment (recommended) 2. Data collection - Scan Range: at least 6-90 2q - Step Interval: 0.02 2q - Dwell Time: depends on equipment, but at least 50,000 counts at Imax is recommended

  6. Data reduction Profile analysis International Centre for Diffraction Data Peak positions and intensities are taken from pattern & profile fitting

  7. Data reduction Least Squares International Centre for Diffraction Data In the refinement check: • Wavelength : 1.54060 • 2Theta zeropoint : 0.0000 ( fixed ) • Refined cell parameters : • Cell_A : 3.8441(5) • Cell_B : 3.8720(5) • Cell_C : 27.2486(23) • Cell_Volume: 405.57(6) • 2Th[obs] H K L 2Th[calc] obs-calc Int. • 6.478 0 0 2 6.482 -0.0040 32.0 • 12.976 0 0 4 12.985 -0.0093 3.0 • 19.528 0 0 6 19.531 -0.0034 4.7 • 23.175 0 1 1 23.184 -0.0089 14.3 • 24.030 1 0 2 24.035 -0.0047 15.8 • 24.980 0 1 3 24.980 0.0005 1.6 • 26.140 0 0 8 26.142 -0.0010 5.7 • 26.602 1 0 4 26.605 -0.0028 18.7 • 30.441 1 0 6 30.441 0.0001 27.6 • 32.594 0 1 7 32.592 0.0016 81.5 • 32.969 1 1 1 32.972 -0.0031 100.0 • 34.293 1 1 3 34.295 -0.0020 18.9 • 35.176 1 0 8 35.175 0.0016 46.5 • 36.827 1 1 5 36.815 0.0118 0.7 • 37.687 0 1 9 37.685 0.0020 9.6 • 39.661 0 0 12 39.660 0.0009 6.8 • 40.343 1 1 7 40.340 0.0030 18.4 Wavelength Zeropoint Systematic errors in obs-calc In the listing file you need: 2 or d observed Indices hkl 2 or d calculated Difference 2 or d Peak (preferred) intensities You will need these data for the preparation of a peak file

  8. Phase analysis International Centre for Diffraction Data The sample must be a single phase. If not single, then the admixture must be defined and indicated in the PDF-3 File and discussed with the Editor-in-Chief.

  9. File preparation General form International Centre for Diffraction Data Sample characterization - fill in for each sample Technique - fill in for your diffractometer and your sample Cell data - fill in for each sample Reference - fill in for each sample

  10. File preparation General form - Sample characterization International Centre for Diffraction Data SAMPLE CHARACTERIZATION NAME (CHEMICAL, MINERAL, Trivial) EMPIRICAL FORMULA CHEMICAL ANALYSIS. NO YES SOURCE/PREPARATION CHEMICAL ABSTRACT REGISTRY NUMBERPEARSON SYMBOL CODE COLOR: Potassium Indium Hydrogen Phosphate NAME (CHEMICAL, MINERAL, Trivial)Potassium Indium Hydrophosphate KInH2P2O8 EMPIRICAL FORMULAKIn(HPO4)2 X X Name Add mineral, trivial, etc., name(s) if exists Empirical formula Add detailed formula(s) if possible Chemical analysis For pure samples only; do if possible

  11. File preparation General form - Sample characterization (cont.) International Centre for Diffraction Data SAMPLE CHARACTERIZATION NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrogen Phosphate NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrophosphate EMPIRICAL FORMULA KInH2P2O8 EMPIRICAL FORMULA KIn(HPO4)2 CHEMICAL ANALYSIS. NO X YES SOURCE/PREPARATION CHEMICAL ABSTRACT REGISTRY NUMBER PEARSON SYMBOL CODE COLOR: Provided by A.A.Filaretov, Moscow State University, Russia / Synthesized by hydrothermal synthesis from indium oxide, phosphorous acid, potassium dihydrophosphate, hydrofluoric acid and water (ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours. mP56.00 00000-00-0 White Source/preparation Sample provided by Name, Organization; Description of synthesis procedure Chemical Abstract registry number Find (if exists) in Chemical Abstracts Formula Index m - symmetry, P - centering, 56.00 - number of atoms in unit cell Pearson symbol code Color Define color of the sample

  12. File preparation General form - Technique: diffractometer International Centre for Diffraction Data TECHNIQUE RADIATION TYPE, SOURCEX-rays, Cu lVALUE USED1.5406 Å,Ka1 l DISCRIM.(Filters Mono, Etc.)Primary beam, curved Ge Mono. l DETECTOR(Film, Scint, Position Sensitive, etc.)mini PSD INSTRUMENT DESCRIPTION(Type, Slit, etc.)130 mm, Transmission modeDIV= 0.3REC= Slit type: ___fixed ___variable INSTRUMENTAL PROFILE BREADTH.11(Si) °256.121TEMPERATURE (oC)20 SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2FROM 9.00 °2TO110.00 °2, SPECIMEN MOTIONSample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309 Radiation type, source Radiation (X-rays, neutrons), Anode material for tubes  value used Wavelength, Line type for tubes Description of filters, monochromators, mirrors (primary/secondary beam, flat/curved, material)  discriminator Counter type (scintillation, mini/large PSD, film, image plate, etc.) detector

  13. File preparation General form - Technique: diffractometer (cont.) International Centre for Diffraction Data TECHNIQUE RADIATION TYPE, SOURCEX-rays, Cu lVALUE USED1.5406 Å,Ka1 l DISCRIM.(Filters Mono, Etc.)Primary beam, curved Ge Mono. l DETECTOR(Film, Scint, Position Sensitive, etc.)mini PSD INSTRUMENT DESCRIPTION(Type, Slit, etc.)130 mm, Transmission modeDIV= 0.3REC= INSTRUMENTAL PROFILE BREADTH.11(Si) °256.121TEMPERATURE (oC)20 SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2FROM 9.00 °2TO110.00 °2, SPECIMEN MOTIONSample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309 Instrument description Diffractometer or camera type, its radius, types of slits Instrument profile FWHM of intensive line at medium angles, sample, 2 Temperature Temperature of data collection: room if not high or low Specimen form Usually powder or plate Range of 2 For particular sample! Range of data collection

  14. File preparation General form - Technique: diffractometer (cont.) International Centre for Diffraction Data TECHNIQUE RADIATION TYPE, SOURCEX-rays, Cu lVALUE USED1.5406 Å,Ka1 l DISCRIM.(Filters Mono, Etc.)Primary beam, curved Ge Mono. l DETECTOR(Film, Scint, Position Sensitive, etc.)mini PSD INSTRUMENT DESCRIPTION(Type, Slit, etc.)130 mm, Transmission modeDIV= 0.3REC= INSTRUMENTAL PROFILE BREADTH.11(Si) °256.121TEMPERATURE (oC)20 SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2FROM 9.00 °2TO110.00 °2, SPECIMEN MOTIONSample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309 Specimen motion Usually Sample spinner if not texture study Internal/external 2 calibration (underline), material used Lattice parameter(s) Lattice parameter of material used for 2 calibration

  15. File preparation General form - Technique: sample characteristics International Centre for Diffraction Data 2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan dataPEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)0.2 INTENSITY STD USEDa-Al2O3 °2's OF INTENSITY STD25.58 <0 1 2> INTENSITY RATIO I/Ic1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796 RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2AT27.835 °2 2REPRODUCIBILITY FOR THIS MATERIAL:0.003 °2AT27.835 °2 X X Intensity measurement technique Depends on registration device; for diffractometer usually step scan data Intensity presentation - integrated/peak (the last preferred) Intensity Minimum intensity threshold In relative intensity units; actually, depends on peak/background ratio

  16. File preparation General form - Technique: sample characteristics International Centre for Diffraction Data 2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan dataPEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)0.2 INTENSITY STD USEDa-Al2O3 °2's OF INTENSITY STD25.58 <0 1 2> INTENSITY RATIO I/Ic1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796 RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2AT27.835 °2 2REPRODUCIBILITY FOR THIS MATERIAL:0.003 °2AT27.835 °2 Material used for reference intensity ratio (RIR) determination (SRM676 or other phase with known RIR) Intensity standard used 2 and indices of a reflection for a standard used for RIR; use any intensive nonoverlapping reflection 2 of intensity Defined RIR with standard deviation multiplied by conversion factor. Use integral intensities Intensity ratio Conversion factor I/I100 of the standard;if not the most intensive reflection was used (overlapping with corundum)

  17. File preparation General form - Technique: sample characteristics International Centre for Diffraction Data 2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan dataPEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)0.2 INTENSITY STD USEDa-Al2O3 °2's OF INTENSITY STD25.58 <0 1 2> INTENSITY RATIO I/Ic1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796 RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2AT27.835 °2 2REPRODUCIBILITY FOR THIS MATERIAL:0.003 °2AT27.835 °2 Resolution FWHM of intensive well-resolved a1 line between 30 and 60 2 angle 27.837 27.836 27.832 Aver. 27.835(3) 2 reproducibility Standard deviation of a 2 determination

  18. File preparation General form - Cell data International Centre for Diffraction Data CELL DATA METHOD OF CELL DETN. Cell parameters and structure are known from Ref.[1] CELL REFINEMENT METHODleast-squares a= ( ) Å; b= ( ) Å; c= ( ) Å a= ( ) ; b= ( ) ; g= ( )  Z= ; Dm = ( )g cm -3 Dx =g cm -3 V=Å3 ; FORMULA Wt= CRYSTAL SYS.; SPACE GROUP ;CRYSTAL DATA INDEX No FIGURE OF MERIT TYPE Fn =[1/delta(2av)]*No/Npos VALUE F30 = 9.6233 3 8.2591 3 9.4577 3 115.715 3 4 3.392 677.25 345.88 Monoclinic P21/c [14] Method of cell determination Present the method of cell determination; from reference is the most common Cell refinement method Usually least-squares Cell parameters Input cell parameters with standard deviations Crystallographic data Input: Z, measured density (if measured) (Dm), Calculated Density (Dx), cell volume, molecular weight, symmetry, space group with its number

  19. File preparation General form - Cell data (cont.) International Centre for Diffraction Data CELL DATA METHOD OF CELL DETN. Cell parameters and structure are known from Ref.[1] CELL REFINEMENT METHODleast-squares a=9.6233 (3) Å; b= 8.2591 (3) Å; c=9.4577 (3) Å a= ( ) ; b= 115.715 (3) ; g= ( )  Z=4 ; Dm = ( )g cm -3 Dx =3.392g cm -3 V=677.25Å3 ; FORMULA Wt=345.88 CRYSTAL SYS.Monoclinic; SPACE GROUP P21/c [14];CRYSTAL DATA INDEX No FIGURE OF MERIT TYPE Fn =[1/delta(2av)]*No/Npos VALUE F30 = 147.1 (0.0055, 37) Figure of merit Put the figure of merit with average deviation and number of observed lines in brackets Attention! Calculated density, cell volume, molecular weight and figure of merit you can obtain by the program processing your data (NBS*AIDS83 file).

  20. File preparation General form - Reference International Centre for Diffraction Data REFERENCES 1. Filaretov A.A.,. private communication, 2001 Reference for cell parameters Papers from journals, proceedings, private communications, etc.

  21. File preparation Reflection file - file content International Centre for Diffraction Data File (ASCII) should contain: K In ( H P O4 )2 14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001 ..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001 ..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002 Formula (elements with indices separated by blanks) 2 observed (three decimal digits) Peak (preferred) intensities (integer if >1%, one digit if less) d observed (3-5 decimal digits; depends on d value) Indices hkl (all sets in column with difference) Difference 2

  22. File preparation Reflection file - printed form International Centre for Diffraction Data Powder data K In ( H P O4 )2 ESSENTIAL DESIRED 2exp I/I0 dexp hkl 2 (degrees) (degrees) 14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001 ..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001 ..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002 Powder data K In ( H P O4 )2 ESSENTIAL DESIRED 2exp I/I0 dexp hkl 2 (degrees) (degrees) 14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001 ..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001 ..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002 Printedform to be sent to the ICDD Recommended! Write the program for conversion of your listing file to reflection file and print the data in the proper form

  23. File preparation Main file –NBS*AIDS83-Data input International Centre for Diffraction Data Use PDFENTRY.EXE to create the file!!! Creation of FILE for input to PDFEAPC Processing R esearch [R] Cell Analysis Generation of d-Spacings Powder Pattern Analysis D atabase Submission File Your Selection > D a t a b a s e R u n Enter name of file to be written for PDFEAPC run: (include PATH ) ID number: (6 CHARACTERS) Crystal System: (select by letter code) A> northic M> onoclinic O> rthorhombic T> etragonal H> exagonal R> hombohedral C> ubic Your Selection: Dialog box of the program Selection: kind of work Preparation of the file for Database D File Give Filename KInHPO4.dat ID number Input ID number of the sample: Grant letters+No. APS107 Symmetry Input symmetry M

  24. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Unique axis For monoclinic symmetry only a / b / c unique? : Enter cell Parameters and Standard deviations as cell(std) a(): b(): c(): beta(): Editorial CODE for Cell : blank Cell by author, normal Temperature and Pressure. T Cell data at high or low temperature. P Cell data at high pressure (maybe high or low T). Your Selection : Radiation ( X -ray / N eutron / E lectron / G amma ): b Cell parameters Input cell parameters with standard deviations in brackets 9.6233(3) 8.2591(3) 9.4577(3) 115.715(3) Editorial Code Blank if not at high or low temperatures or high pressure Radiation Give radiation type, usually X-ray X

  25. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Cell Source: S ingle crystal. P owder diffraction. R ietveld or profile fit analysis. Your Selection: Structure Code: N no structure information given. L limited qualitative structure. T total quantitative structure. Your Selection: Space Group Symbol: Enter NUMBER for Space Group: Z: Measured Density, Dm: Calculated Density, Dx: 3.392 File Codes (up to 4-character string) I norganic; O rganic; M inerals; A lloys Enter Your Selections: I Cell source Powder for Grant-inAid if not special task P Structure code Total Space group, calculated density... T P21/c Space group Input space group symbol; nonstandard is possible 14 Sp. Gr. number Sp. Gr. number in International Tables

  26. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Cell Source: S ingle crystal. P owder diffraction. R ietveld or profile fit analysis. Your Selection: P Structure Code: N no structure information given. L limited qualitative structure. T total quantitative structure. Your Selection: T Space Group Symbol: P21/c Enter NUMBER for Space Group: 14 Z: Measured Density, Dm: Calculated Density, Dx: File Codes (up to 4-character string) I norganic; O rganic; M inerals; A lloys Enter Your Selections: Z Number of formula units Measured density Input measured density if measured or blank Calculated density Calculated by NBS*AIDS83 4 File code Type of compound 3.392 I

  27. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Subfile indicator Ceramic, Explosive, Pharmaceutical, etc. Enter Sub-File Indicators ? Y / [N] Enter C A S Registry Number : Y / [N] Name of compound: (TERMINATE with BLANK LINE) USE UPPER/lower CASE BEGIN EACH WORD with Capital LETTER Editorial code for name: P owder diffraction file index name. M ineral name. C ommon or trivial name. Your Selection: CAS Number Blank for new compound; otherwise follow prompts Potassium Indium Hydrogen Phosphate Nomenclature name should be the first; for inorganic compounds each word with Capital letter; + blank line; for organic compounds use Merck nomenclature when available Compound Name P Code for name The first name should be Powder one

  28. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data More names Yes if several names exist More names? ( Y / [N] ): Name of compound: (TERMINATE with BLANK LINE) USE UPPER/lower CASE BEGIN EACH WORD with Capital LETTER, if inorganic Editorial code for name: P owder diffraction file index name. M ineral name. C ommon or trivial name. Your Selection: More names? ( Y / [N] ): Y Compound Name Common, trivial, mineral name(s) if exist(s) + blank line; Potassium Indium Hydrogen Phosphate Code for name Should be Common (trivial) or Mineral C Items above can be repeated several times! Otherwise No

  29. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Chemical formula Input elements with indices in alphabetic order (cations, anions) separated by blanks followed by blank line Chemical Formula: (TERMINATE WITH BLANK LINE) More formulas? ( Y / [N] ): Chemical Formula: (TERMINATE WITH BLANK LINE) More formulas? ( Y / [N] ): H2 In K P2 O8 More formulas Give at least one more formula if possible Y K In ( H P O4 )2 Chemical formula Give detailed formula consider brackets as elements Two items above can be repeated several times! Otherwise No

  30. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Empirical formula Left blank Empirical formula: (GENERALLY LEFT BLANK) Literature reference? ( [Y] / N ): First reference: Literature Reference source identified by CODEN: (6 CHARACTERS -- 00GRNT is GRANT-in-AID) ENTER XXXXXX if CODEN is not known. Year: Enter Authors: (using UPPER/lower CASE) (TERMINATE entry with a BLANK LINE) More references? ( Y / [N] ): Literature reference Yes - default Reference is identified by coden (6 characters) List is in PDF-4 and PDF-2 products Literature reference 00GRNT 2001 Mironov, A.V., Antipov, E.V., Moscow State Univ., Russia Year Year of current Grant-in-Aid Author(s) Author(s), initials, and place of work More references Additional references for physical properties

  31. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Structure type information: Enter Comments. No checking of entry performed. Place appropriate CODE in columns 1-2 followed by text of line. AD,AT,AN,AX,CL,CR,DB,FF,FN,HK,LN,MP,OO,OP,PD,PM,PR,SC,SM,ST,TH,TM,UC ( TERMINATE entry with a BLANK line ) 1 2 3 4 5 6 7 @@....+…..0.….+.….0.….+.....0…..+.….0…..+…..0…..+…..0…..+.….0. PR PR PR UC TM CL SM Additional information Each line is coded with 2 characters in the first two positions The following items are recommended to fill out: Synthesized by hydrothermal synthesis from indium oxide, phospho- rous acid, potassium dihydrophosphate, hydrofluoric acid and water (ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours PR - Synthesis of a sample 0PCOMC 2001 Filaretov, A.A. Pattern was taken at room temperature. White SM - Comments: provided by… application; property(ies) (e.g.ferroelectric); etc. Sample was provided by Filaretov, A.A., Moscow State Univ., Russia Literature reference for unit cell parameters; (coden, volume, page, year, authors) TM - Temperature of data collection CL - Color of a sample

  32. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Powder pattern information Enter Powder Pattern information Wavelength in Angstroms: [1.54056] Enter one of the following letter codes: F <beta filter> M <monochromator> S <solid state> Your selection: Alphanumeric description for filter or monochormator Enter code for input data type 1 = theta 2 = 2-theta D = d-spacing S = sin**2 theta Q = d2 Your selection: Wavelength (A) Wavelength of data collection 1.5406 Filtering Choose the code from menu M GE(PB) Monochromator type Material(position) PB - primary beam DB - diffracted beam Input data type Format of Reflection position 2

  33. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Instrument Code for spacing measurements: D = diffractometer. G = Guinier . S = Debye-Scherrer. F = Gandolfi. X = Other. C = Calculated spacings. Your selection Mnemonic for compound used as spacing standard Code for Standard. I = internal E = external Your selection: Device type Choose the code from menu Standard Standard used for calibration D Si Standard type Internal or External I

  34. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Code for intensity measurements: D = diffractometer. F = film, densiometer reading. V = visual estimation from film. X = other. C = calculated intensities. Your selection Type of intensity: I = integrated P = peak height Your selection: Intensity measurement Choose the code from menu D Intensity type Integrated Or Peak P

  35. File preparation Main file -NBS*AIDS83-Data input (cont.) International Centre for Diffraction Data Reference intensity ratio Input RIR; see General Form Reference intensity ratio (with decimal point) ESD of r i r (include decimal point) 2-theta resolution: Spacings are to be entered as 2-theta Spacings are floating point; I, h, k, and l are integer Enter lines as SPACING,I,h,k,l **** Separate items with commas - NO spaces allowed **** Terminate by entering a blank line. Line 1: Your Initials please: (3 CHARACTERS) 1.37 0.03 ESD of reference intensity ratio Input standard deviation of RIR 0.11 2 resolution in determining possible resolutions of calculated 2 Input resolution; see General Form Input the data according to instructions Reflection data 2,I,h,k,l Attention! Another way of reflection data input - write the program to attach peak file. Warning! NBS*AIDS83 and Peak files have different formats. APS Grant number Initials

  36. File preparation Main file -NBS*AIDS83-Format International Centre for Diffraction Data 1 1 0 2 0 2 0 1 60 0 0 0 0 0 9.6233 8.2591 9.4577 115.715 X P T P APS107M1 .0003 .0003 .0003 .003 APS107M2 P21/c 14A 4 3.392 APS107M3 I 00000-00-0 APS107M5 Potassium Indium Hydrogen Phosphate P APS107M6 H2 In K P2 O8 1 APS107M7 K In ( H P O4 )2 2 APS107M7 00GRNT 2001 Mironov,A.V., Antipov,E.V., Moscow State C1 APS107M9 University, Russia 2 APS107M9 Synthesized by hydrothermal synthesis from indium oxide, phospho- PRC1 APS107MB rous acid, potassium dihydrophosphate, hydrofluoric acid and water PRC2 APS107MB (ratio ofK:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours. PR 3 APS107MB 0PCOMC 2001 Filaretov,A.A., UC 4 APS107MB Pattern was taken at room temperuture. TM 5 APS107MB White CL 6 APS107MB Sample was provided by Filaretov A.A., Moscow State Univ., Russia SM 7 APS107MB Data collected in transmission mode 8 APS107MB CuKa 1.5406 M GE(PB) 2 9.0 D Si E APS107MF D P 1.37 0.03 0.11 S APS107MG 14.803 57 1 1 0 14.927 61 0 1 1 20.475 16 2 0 0 1 APS107MI 20.563 1L 1 1 1 20.836 8 0 0 2 21.412 7 -2 1 1 2 APS107MI 21.672 11 -1 1 2 21.993 74 -2 0 2 23.156 1L 2 1 0 3 APS107MI 23.479 19 0 1 2 23.850 11 1 2 0 24.189 14 -1 2 1 4 APS107MI ..... 71.372 1L 2 2 5 71.702 3 6 1 1M 71.702 3 -2 1 7M 61 APS107MI 72.392 3 -7 2 3 72.855 1 1 1 6 73.005 1 4 4 2 62 APS107MI 73.418 1 2 4 4 73.732 4 -3 2 7 74.503 1L -4 2 7 63 APS107MI 74.745 2 4 0 4 74.836 1L -2 2 7 75.100 1L -3 6 1 64 APS107MI 75.205 1 -6 4 2 75.808 1L 4 1 4 75.929 1L 1 2 6 65 APS107MI 76.036 1 5 4 1 76.223 2 -7 2 1 76.321 1 -7 2 5 66 APS107MI 76.531 1L -2 5 5 76.598 1L 1 5 4 67 APS107MI APS APS107MK NBS*AIDS83 is thepreferred format! Append reflection file to main file with your program. Watch format! Warning! Change starting angle of data collection. The program set to 4.0

  37. File preparation Main file -NBS*AIDS83-Checking data International Centre for Diffraction Data C:\NBSAIDS> 25 July, 1990 * P D F E A P C * P owder D iffraction F ile E ditorial A ids for the P ersonal C omputer Personal Computer version of the program: NBS*AIDS. A FORTRAN program for Crystallographic Data Evaluation. by: A D Mighell, C R Hubbard, and J K Stalick National Bureau of Standards, Technical Note 1141 (1981) Implemented under a Grant in Aid from: JCPDS - International Centre for Diffraction Data 12 Campus Boulevard, Newtown Square, Pennsylvania 19073 by: Roy Garvey Department of Chemistry North Dakota State University Fargo, North Dakota 58105-5516 USA Press <ENTER> key to CONTINUE. Enter Name of input DATAfile >- EA.BAT Check your data with EA.BAT See results in PDFEAPC.OUT (protocol file) and P1FORM.OUT KInHPO4

  38. File preparation Main file -NBS*AIDS83-PDFEAPC.OUT International Centre for Diffraction Data JCPDS - ICDD ** Edit Aids PC-90 ** Revision pc 90/07/12 DATA BANK Evaluation Run FILE = JCPDS PDF P1 FORMAT PAGE to be PRINTED PARAMETERS as INPUT: IJOB = 1 INCODN = 1 IBK = 0 IWHO = 2 IOUT = 2 IINPUT = 2 IFRMT = 1 ITHMX = 60 ICOL = 0 IXCD = 0 IXPD = 0 IPHKL = 0 IDOLSQ = 0 .............................................................................. *** MONOCLINIC *** *** :2/ 3/12 11:58:02 ** WARNING ==> **** Line # 201 is more than MAXOBS = 200 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 Watch warnings! This warning is not significant

  39. File preparation Main file -NBS*AIDS83-PDFEAPC.OUT International Centre for Diffraction Data *** MONOCLINIC *** *** :2/ 3/12 12:32:17 ** WARNING ==> CALCULATED and AUTHORS calc DENSITIES DIFFER by > 1.0% 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 4 2.392 677.25 SG-I 3 P21/c 14A 4 3.12A 3.392 345.88 677.25 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6 ... ***SUMMARY** ID# = APS107 *** 1 WARNINGS*** 0 ERRORS*** " S " QUALITY assigned Watch warnings at the very end of PDFEAPC.out Calculated and authors calc. density differ significantly

  40. File preparation Main file -NBS*AIDS83-PDFEAPC.OUT International Centre for Diffraction Data *** MONOCLINIC *** *** :2/ 3/12 12:32:17 ** WARNING ==> CALCULATED and AUTHORS calc DENSITIES DIFFER by > 1.0% ** WARNING ==> CALCULATED and APPROXIMATE DENSITIES DIFFER by 84 % 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 2 1.392 677.25 SG-I 3 P21/c 14A 2 3.12A 1.696 345.88 677.25 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6 H2 In K P2 O8 1 CHEM 7 ... ***SUMMARY** ID# = APS107 *** 2 WARNINGS*** 0 ERRORS*** " S " QUALITY assigned Watch warnings and errors at the very end of PDFEAPC.out Calculated and authors calc. density differ significantly Calculated and approximated density differ significantly Check crystallographic information - composition or Z

  41. File preparation Main file -NBS*AIDS83-PDFEAPC.OUT International Centre for Diffraction Data Watch warnings and errors at the very end of PDFEAPC.out 2 CONDITIONS for NON-EXTINCTION requested H0L L = 2n 0K0 K = 2n **ERROR** REFLECTION 0 0 3/ANGLE= 20.836/D= 4.2598 ABSENT in P21/c ** ERROR >==> delta 2-? EXCEEDS .50°. LINE MARKED as UNINDEXED ** badHKL 1 ** ** BAD HKL = -2 1 2 2-? = 21.412 delta 2-? = 3.105 SET to UNINDEXED ** ** badHKL 3 ** <AUTHOR > <PROGRAM> OBS CALC DIFF FINL N D calc D obs INT H K L H K L 2Theta 2Theta 2Theta WT 1 8.6702 1 0 0 10.194 2 5.9801 5.9796 57 1 1 0 -1 1 0 14.803 14.802 -.001 1.0 ………... ABSOLUTE MAXIMUM DELTA 2-Theta = .018 AVERAGE( ABS(DELTA 2-Theta) ) = .003 1 INCLUDED UNINDEXED LINES *** PATTERN QUALITY MARK LOWERED from "S" to "I" ***SUMMARY** ID# = APS107 *** 1 WARNINGS*** 1 ERRORS*** " I " QUALITY assigned Indices of reflection are inconsistent with the Space Group Check indexing or purity of a phase 2 exceeds 0.05; reflection is marked as unindexed, quality mark is reduced to “I” Check indexing or purity of a phase

  42. File preparation Main file -NBS*AIDS83-PDFEAPC.OUT International Centre for Diffraction Data 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 4 3.392 677.25 SG-I 3 P21/c 14A 4 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6 H2 In K P2 O8 1 CHEM 7 K In ( H P O4 )2 2 CHEM 7 H2 In K O8 P2 EMPR 8 00GRNT JCPDS Grant-in-Aid Report 00GRNT 2001 Mironov,A.V., Antipov,E.V., Moscow State C1 REFR 9 University, Russia 2 REFR 9 TYPE A ……………... M(20) = 63.5 (DLIMIT = 3.0531, # POSSIBLE = 25) X(20) = 0 F(30) = (DELTA 2-Theta = .0055, # POSSIBLE = 37) Information you need! Calculated density 3.12A 3.392 345.88 677.25 Approximated density Cell Volume mP 56.00 Molecular weight Pearson alloy designation 147.1 Figure of merit

  43. File preparation PDF-3 File International Centre for Diffraction Data PDF-3 files can be accepted in either modified JCAMP or CIF file formats. The following examples are for JCAMP.

  44. File preparation PDF-3 File International Centre for Diffraction Data Content of PD3 (ASCII) File &SAMPLE IDENT= &ICDD-DX=1.00 &DATE= &FILE IDENT= &SOURCE IDENT= &CROSS REFERENCE=APSREF11.REF &GRANT NO=91-05APS &PDFNO=XX-YYYY &DIV SLIT=0.30 &WAVELENGTH=1.5406 &COUNT TIME= 2600.00 &STEP SIZE=0.0100 &XUNITS=DEGREES 2-THETA &YUNITS=COUNTS &YFACTOR=1.0 &FIRSTX= 9.0000 &LASTX=110.0000 &MAXY= 17238. &NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. ......... 109.960 126. 126. 107. 124. 110. 0. 0. 0. &END= K In ( H P O4 )2 01/12/26 KInHPO4.PD3 KInHPO4.PD3 Sample Identification Any name, formula is preferred, admixture(s) if any Date of Data Collection Year/Month/Day Name of your PD3 file

  45. File preparation PDF-3 File (cont.) International Centre for Diffraction Data &SAMPLE IDENT=K In ( H P O4 )2 &ICDD-DX=1.00 &DATE=01/12/26 &FILE IDENT=KINHPO4.PD3 &SOURCE IDENT=KINHPO4.PD3 &CROSS REFERENCE= &GRANT NO= &PDFNO=XX-YYYY &DIV SLIT= &WAVELENGTH= &COUNT TIME= 2600.00 &STEP SIZE=0.0100 &XUNITS=DEGREES 2-THETA &YUNITS=COUNTS &YFACTOR=1.0 &FIRSTX= 9.0000 &LASTX=110.0000 &MAXY= 17238. &NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. ......... 109.960 126. 126. 107. 124. 110. 0. 0. 0. &END= File name of your annual reference experiment (SRM1976) APSREF11.REF 91-05APS 0.30 1.5406 Grant Number Slit size Wavelength

  46. File preparation PDF-3 File (cont.) International Centre for Diffraction Data &SAMPLE IDENT=K In ( H P O4 )2 &ICDD-DX=1.00 &DATE=01/12/26 &FILE IDENT=KINHPO4.PD3 &SOURCE IDENT=KINHPO4.PD3 &CROSS REFERENCE=APSREF11.REF &GRANT NO=91-05APS &PDFNO=XX-YYYY &DIV SLIT=0.30 &WAVELENGTH=1.5406 &COUNT TIME= &STEP SIZE= &XUNITS=DEGREES 2-THETA &YUNITS=COUNTS &YFACTOR=1.0 &FIRSTX= &LASTX= &MAXY= 17238. &NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. ......... 109.960 126. 126. 107. 124. 110. 0. 0. 0. &END= Count time Count time per step in seconds 2600.00 0.010 Step size of 2 (degree) 9.000 110.000 Starting angle 2 Last angle 2

  47. File preparation PDF-3 File (cont.) International Centre for Diffraction Data &SAMPLE IDENT=K In ( H P O4 )2 &ICDD-DX=1.00 &DATE=01/12/26 &FILE IDENT=KINHPO4.PD3 &SOURCE IDENT=KINHPO4.PD3 &CROSS REFERENCE=APSREF11.REF &GRANT NO=91-05APS &PDFNO=XX-YYYY &DIV SLIT=0.30 &WAVELENGTH=1.5406 &COUNT TIME= 2600.00 &STEP SIZE=0.010 &XUNITS=DEGREES 2-THETA &YUNITS=COUNTS &YFACTOR=1.0 &FIRSTX= 9.000 &LASTX= 110.000 &MAXY= &NPOINTS= &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. ......... 109.960 126. 126. 107. 124. 110. 0. 0. 0. &END= Maximal Intensity Number of steps Angle Intensity 17238. 10101 8 steps per line Keyword “&END”

  48. International Centre for Diffraction Data Good Luck! by Andrei Mironov, Moscow State University

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