Refinement of X-ray and/or Neutron Data

(powder and/or single-crystal)

SHORT REFERENCE GUIDE OF THE PROGRAMFFFFFF PPPPPP F l l P P f F l l P P f FFFF l l PPPPPP f F u u l l P r r r ooo fff F u u l l P r o o f F uuuuu lll lll P r ooo f*************************************** * Program : FullProf * *************************************** (Version 3.5d Oct98-LLB-JRC) Juan Rodriguez-Carvajal Laboratoire Leon Brillouin (CEA-CNRS) Tel: (33) 1 6908 3343, Fax: (33) 1 6908 8261 Disclaimer:

The most recent version of FullProf is either in "pub/divers/fullp" or in "pub/divers/fullp" of the anonymous ftp-area of the LLB unix-cluster. Users interested in create their own subroutines to link with FULLP-library are asked to read the fileFullProf is a program for Rietveld analysis (structure profile refinement) of neutron (CW, TOF, nuclear and magnetic scattering) or X-ray powder diffraction data collected as a function of the scattering variable T (2theta or TOF). The program can be also used as a Profile Matching tool, without the knowlegde of the structure."fpreadme" in the above mentioned disk-area. To access this area from Internet, one has to type in the local host the following commands: LocalPrompt> ftp charybde.saclay.cea.frAnswer with the word:anonymous, to the Login request and password. Within the ftp prompt, do: From a UNIX host: ftp>cd pub/divers/fullp-> Go to FullProf area ftp>get fpreadme-> Obtain the document ftp>bye-> Return to host From some VMS-VAX hosts: ftp>set def "pub/divers/fullp" -> Go to FullProf area ftp>get "fpreadme" -> Obtain the document ftp>ex -> Return to host ----------------------------------------------------1.1: Purpose, authors, references and documentation----------------------------------------------------

Single Crystal refinements can also be performed alone or in combination with powder data.

FullProf has been developed starting from the program of Wiles & Young, J. Applied Cryst.14,149(1981), (DBW3.2S, Versions 8711 and 8804). The modifications of the code are mainly related with the re-organization of the central routines performing the calculation of profile functions, derivatives, structure factors, and the introduction of many other things. The total source is more than 1 Megabyte (more than 28.000 fortran lines). The format of the main control input file (e.g. a control file created for use with DBW-8711 can be used by FullProf with minor modifications). The input file is accepted as "interpreted free format".

The source is written in standard FORTRAN 77 language, and is organized as to be easily adapted to different computers. The actual version can be run on VAX, Alpha and Unix computers, MacIntoshes and on PCs (Lahey Computer Systems Inc. FORTRAN-compiler, minimum 386/4Mb with co-processor required). The migration towards genuine Fortran 90 is in progress.

---------------------------1.2: Features of FullProf:--------------------------- - Choice of line shape (Gaussian, Lorentzian, modified Lorentzians, pseudo-Voigt, Pearson-VII or Thompson-Cox-Hastings) for each phase. - Neutron (constant wavelength and TOF) and X-ray (laboratory and synchrotron sources) - One or two wavelengths (Ka1 + Ka2) - Background refinement - Multi-phase (up to 8 phases) - Preferred orientation : two functions available - Absorption correction for a cylinder - Choice between three weighting schemes: standard least squares, maximum likelihood and unit wheights. - Choice between automatic generation of hkl and/or symmetry operators and file given by user. - Magnetic structure refinement (crystallographic and spherical representation of the magnetic moments). Two methods: describing the magnetic structure in the magnetic unit cell of making use of the propagation vectors using the crystallographic cell. This second method is necessary for incommesurate magnetic structures. - Automatic generation of reflections for an incommensurate structure with up to 24 propagation vectors. Refinement of propagation vectors in reciprocal lattice units. - h,k,l dependence FWHM for strain and size effects - h,k,l dependence of shift and asymmetry for special kind of defects - Profile Matching. The full profile can be fitted without prior knowledge of the structure (needs only good starting cell and profile parameters) - Quantitative analysis without need of structure factor calculations. - Chemical(distances) and magnetic (magnetic moments) slack constraints - Resolution function (for pseudo-Voigt peak shape) may be supplied in a file - Structural or magnetic model could be supplied by an external subroutine for special purposes (rigid body, TLS, polymers, form factor refinements, small angle scattering of amphifilic crystals, description of incommensurate structures in real direct space, etc.) - Single crystal data or integrated intensities can be used as observations (alone or in combination with a powder profile) - Neutron (or X-rays) powder patterns can be mixed with integrated intensities of X-rays (or neutron) from single crystal or powder data. --------------------------------------------------1.3: Running the program, input and output files.-------------------------------------------------- To run the program the user has to invoke the name of the executable file and press the ENTER/INTRO key. Of course the executable file must be in a directory included in the PATH or an alias should exist. For for doing sequential refinements there is a number of command files that can be used. The command files (scripts) depend on the operating system. A facility is included in FullProf for versions higher that 3.2 that allows sequential of cyclic refinements. Examples: 1: Prompt> FULLPROF 2: Prompt> FullProf , ... -----------Input files: ----------- To run the program, you need at least one input file, CODFIL is the code of the control file given by the user.CODFIL.PCR: Input control file It must be in the current directory to run the program. This file contains the title and crystallographic data and must be prepared by user with a file editor. There are two different formats for this file: the first one is free format and closely related to that of the Young & Wiles's program. The second is based on keywords and commands. (this last format is not available at present) Warning : this file is normally up-dated every time you run the program (see parameter NXT on line 3). In the first stages of a refinement, it is wise to save a copy of this file with a different name. The following files are optional.FILE.DAT: Intensity data file (unit 4) : format depends on instrument. If you do not specify the name FILE, the program takes FILE=CODFIL. Not necessary for pattern calculation modes.FILE.BAC: Background file (unit 12). The format of this file is the following (as that ofFILE.DATfor INSTRM=0): first line : 2theta(initial) step 2theta(final) following lines: list of intensities in free format.CODFILn.HKL: Set of files with the reflections corresponding to phase "n" (n is the ordinal number of a phase). These files are optional and depend on the value of the parameter IRF(n) (see below) If sequential refinements have to be done, this file is calledHKLn.HKLMYRESOL.INSTRU: File describing the instrumental resolution function. Any name can be used and its content depend on the value of the paramenter IRESO (see below).GLOBAL.SHP: File providing a numerical table for calculating the or peak shape and its derivative. The peak shape shouldCODFIL.SHP: be given in a normalized form P(x) where the variable x is chosen to give a FWHM=1 and the area is equal to 1 => Integ{x1,x2}[P(x).dx]=1. That allows the use of the conventional U,V,W parameters for defining the FWHM as a function of angle. The format of this file is the following: Line1: Any comment Line2: Np8, nupr, (anpr(j),j=1,nupr) Np8 = Number of points nupr= Number of different profiles anpr(j)= Angle to which profile "j" is best adapted The rest of the lines are columns with X, P(X,1), PP(X,1),P(X,2), PP(X,2),...P(X,nupr), PP(X,nupr) in free format. PP(X,j) is the derivative of P(X,j) with respect to X. The profile of a reflection situated between anpr(j) and anpr(j+1) is linearly interpolated between the profiles P(X,j) and P(X,j+1)CODFIL.COR: File with corrections for integrated intensities of profile intensities depending on the value of the variable ICORR. See below.Output files: Except for*.OUTand*.SUM, their creation depends on the value of a flag which is quoted in parenthesis. The ordinal number on the flag list is given in brackets.CODFIL.OUT: This is the main output file (unit 7) which contains all control variables and structure parameters.CODFIL.PRF: Observed and calculated profile (unit 1) : to be fed into PLOTPOW, PLOTR, ...(if IPL2 different from zero) In the case of ICRYG=1 (Integrated intensity mode) a list of sin(theta)/lambda, Gobs, Gcalc is output after two lines of comments.CODFIL.RPA: Summary of refined parameters (unit 2) : short version ofCODFIL.SUM(if JCIL=1) If the file exist the new data are APPENDED at the end.CODFIL.SYM: List of symmetry operators (unit 3) (if IPL1=JSY=1) (The last two files are necessary to run DISTAN or BONDSTR)CODFIL.SUM: Parameter list after last cycle (unit 8) : the summary of the last parameters, their standard deviations and reliability factors. An analysis of the goodness of the refinement is included at the end.CODFIL.FOU: If JFOU=1 H,K,L, Structure Factors in Cambridge format (unit 9) : to be fed into FOURTK (FOURPL) to produce Fourier maps. It corresponds to the file usually called HKLFF.DAT but you must prepare the second file CRYST.cry If JFOU=2 (List of 'observed' structure factors in SHELXS format) H,K,L, Fo, sigma(Fo) (3I4,2F8.2) JFOU=-1 or -2, as above but they are calculated in another way. The Fcalc in JFOU>0 may depend on the peak shape and the integration interval, because they are obtained by integration of the calculated profile in the same way as the 'Fobs' are obtained from 'Iobs'. If JFOU is negative, Fcalc are really the structure factors of the conventional cell in absolute units. JFOU=3 Format suitable for the program FOURIER (3I4,2F10.4,f8.5,f10.4) H,K,L,Freal,Fimag,sintheta/lambda,fobs JFOU=4 Format (3I4,2F10.4,i8) H,K,L,Fobs,Fcalc,nint(10000.* Phrd) For JFOU= 3,4: Phrd is the phase in radians and the observed and calculated structure factors of the conventional cell are in absolute unitsCODFILn.SHX:If JFOU=2,-2, template of SHELXS*.INfile.CODFILn.INP:If JFOU=3,-3, template of FOURIER*.INPfile.CODFILn.HKL:Files that can be input or output files. Depending on the value of IRF(n)CODFIL.INT:Single integrated intensity file when the program is used for refining with ICRYG=1,2 (see below).CODFIL.HKL: (if JLKH<>0, unit 10). Complete list of reflections of each phase. JLKH=1 --> If JOBTYP less than 2 reflection code, h, k,l, multiplicity, dspacing,twotheta, FWHM, Iobs, Icalc, Iobs-Icalc. --> If JOBTYP >1 h, k, l, multiplicity, Icalc, twotheta, dspacing JLKH=2 --> Output for SIRPOW92 h,k,l,mul,sint/l,2t,Fwhm,F2,sF2 JLKH=-2 --> Output for EXPO h,k,l,Fwhm,F2 JLKH=3,-3 --> Output of real and imaginary part of structure factors (only for crystal structures) h, k, l, mul, Freal, Fimag, 2theta, Intensity If JLKH<0 the structure factors are given for the conventional cell. Otherwise the structure factor corresponds to the non-centrosymmetric part of the primitive cell. (the obtained file can be used as aCODFILn.HKLfiles for new runs) JLKH=4 --> Output of: h, k, l, F2, sigmaF2. Where F2 is the "observed" structure factor squared. The file could be used as input for a "pseudo-single" crystal integrated intensity file using ICRYG=1 and IRF=4 JLKH=5 --> Output of: h, k, l, mult, Fcalc, T, D-spacing, Q. Where Fcalc is the module of the calculated structure factor. This file can be used as input for JBT=-3 and IRF=2 in order to perform quantitative analysis without re-calcultating the structure factors for each cycle. The Fcalc are in absolute units for the conventionnel call.CODFIL.SAV: (if JCIL=2) List of reflections between two selected angles h, k, l, multiplicity, Iobs, twotheta, dspacing For build-in sequential refinements (version 3.2 and higher) the user must prepare the data files using names of the formCODnnn.dat. COD stands for the code of these files and can be formed by whatever number of characters (compatible with the actual operating system). nnn stands for a sequence of integers. AllCODnnn.datfiles must be in the same directory and the numbers nnn should be in between a minimun number (first) and a maximun number (last) that are asked by program. Holes are allowed between first and last. The fileCODFIL.PCRcan have a different code (CODFILcould be different of COD) and it will be used for refining the whole set ofCODnnn.datfiles. The final results are contained in theCODFIL.RPAfile. For VaX-users using a command file to execute FullProf in cyclic mode: For sequential refinements,*.DATfiles will normally be prepared by SEPFIL. In this caseCODFILmust have three letters (e.g.XXX) as code followed by a number. The*.PCRfile must be namedXXXIN.PCRXXXCYC.RES: In the case of sequential refinements, all the above files would rapidly yield a quota exceeded error message. Thus only condensed results are saved in filesXXXCYC.RES(similar toCODFIL.RPA) andXXXSUM.RES(similar toCODFIL.SUM).XXXHKL.RES: List of reflections of a selected zone of the diffraction patern (useful with Profile Matching mode) The final version of the fileXXX**.PCR(where ** corresponds to the last data set is also saved.## 2.- DETAILED DESCRIPTION OF INPUT FILES

This file is free format. That doesn't mean free format in FORTRAN (,*)-sense A routine interprets the items given by the user that must obey the order given below. A space is needed between each item (except when the second is a negative number). When the program is run, messages of error reading a line of this file are normally due to a previous error. For example, the number of atoms you really wrote does not correspond to the number you put in the line following the name of the phase. Empty lines as well as lines starting with the symbol "!" in the first column are considered as comments and are ignored by the program. If the user starts his(her)- - -CODFIL.PCRCODFIL.PCRfile with the left-ajusted capital "COMM", the newCODFIL.PCRfile has comments with mnemonics for each variable. If the user introduce his(her) own comments, they are not saved in the new version of the file. The unexperienced user can create a template by answering "starting" (without quotes) to the prompt asking for the name of the file. Note that a star after a line number (or a variable) indicates that the line's (or variable) existence depends on the value of a control variable. ============================================================================LINE 1 :TITLE (any 70 characters to be used to label the printout) If the first four character of TITLE correspond to the word TITL the file is given in "command mode" (not available yet). If the first four characters of TITLE correspond to COMM, comments lines (starting with ! in the first column) are automatically addet to the new CODFIL.PCR (or CODFIL.NEW). The comment lines give a keyword for each variable in order to be easily recognized by the user. This comment line has been included below to ============================================================================LINE 2 :JOBTYP, NPROF, NPHASE, NBCKGD, NEXCRG, NSCAT, NORI, IDUM, IWGT, ILOR, IASG, IRESO, ISTEP, NRELL, ICRYG, IXUNIT, ICORR (15 integers) (It is understood that they are separated by a space) --------------Comment line : !Job Npr Nph Nba Nex Nsc Nor Dum Iwg Ilo Ias Res Ste Nre Cry Uni Cor ---------------------------- JOBTYP = 0 X-ray case (Job) 1 Neutron case (constant wavelength, nuclear and magnetic) 2 pattern calculation (X-ray) 3 pattern calculation (Neutron, constant wavelength) -1 Neutron case (T.O.F., nuclear and magnetic) -3 pattern calculation (Neutron, T.O.F.) If abs(JOBTYP)>1 and IDUM=1 (see below) a calculated pattern is created with the nameCODFIL.SIMin format corresponding to INSTRM=0. This pattern corresponds to an "ideal observed" pattern and can be use for simulation purposes in order to investigate the effect of systematic errors on the structural parameters and on the reliability factors. NPROF = Default value for selection of a peak shape. Particular (Npr) values can be given for each phase (see line 11-2) 0 Gaussian 1 Cauchy 2 Modified 1 Lorentzian 3 Modified 2 Lorentzian 4 Tripled pseudo-Voigt 5 pseudo-Voigt 6 Pearson VII 7 Thompson-Cox-Hastings pseudo-Voigt 8 Numerical profile given inCODFIL.SHPor inGLOBAL.SHP9 T.O.F. Convolution pseudo-Voigt x Double Exponential 10 Not yet used 11 Split pseudo-Voigt function 12 Pseudo-Voigt function convoluted with axial divergence asymmetry function (Finger, Cox & Jephcoat, J. Appl. Cryst. 27, 892, 1994) NPHASE = number of phases ( max:8) (if NPHASE <0 the number of phases is (Nph) abs(NPHASE) and the asymmetry correction is applied following the approximation of C.J.Howard, J.Appl.Cryst.15 615-620 (1982) with the Simpson formula for five points) NBCKGD =0 Refine background with polynomial function (Nba) 1 Read background from file CODFIL.BAC. The format of this file is explained above. Some coefficients are read below. 2,3,.,N linear interpolation between the N given points If NBCKGD<0 but IABS(NBCKGD)>4 the interpolation is performed using cubic splines -1 refine background with Debye-like + polynomial function. -2 Background treated iteratively by using a Fourier filtering technique. An extra parameter is read below. The starting backgroung is read from fileFILE.BACas for NBCKGD=1. -3 Read 6 additional polynomial background coefficients NEXCRG = number of excluded regions (Nex) NSCAT = number of scattering sets (zero in most cases) (Nsc) If NSCAT>0, the program performs an internal fit if a table is given in order to get coefficients for the exponential expansion (see below). If NSCAT<0, a linear interpolation is made. NORI = 0 preferred orientation function No 1 (Nor) 1 preferred orientation function No 2 (March) IDUM =1 If equal to 1 and some of the phases are treated (Dum) with Profile Matching modes, the criterium of convergence when shifts are lower than a fraction of standard deviations is not applied. =2 If equal to 2, the program is stopped in case of local divergence: chi2(icycle+1) > chi2(icycle) =3 If equal to 3 the reflections near excluded regions (excl+/-wdth*2theta) are not taken into account to calculate the Bragg R-factor. These reflections are omitted in the output files with hkl's. If JOBTYP greater than 1 and IDUM is different than zero a fileCODFIL.SIMis generated IWGT =0 standard least squares refinement (Iwg) 1 maximum likelihood refinement 2 unit weights ILOR =0 Standard Debye-Scherrer geometry, or Bragg-Brentano if (Ilo) the iluminated area does not exceed the sample surface. If Bragg-Brentano geometry is used but the above condition is not fulfilled, the intensity data must be corrected for the geometric effect before attempting any refinement. (A partial correction can be done by using the parameter SENT0 in line 5) =1 Flat plate PSD geometry =2 Transmission geometry. Flat plate with the scattering vector within the plate (Stoe geometry for X-rays) =3 Polarization correction is applied even if the format of the DATFIL.DAT file does not correspond to one of the synchrotron explicitely given formats (see below). This must be used for synchrotron data given in a X,Y,Sigma format (INSTRM=10). IASG =1 Subroutine ASSIGN is called at each cycle, then reflections (Ias) are re-ordered. =0 Subroutine ASSIGN is called only at the first cycle (If JBT=2 for one phase, IASG must be =1) IRESO=0 Resolution function of the instrument is not given (Res) If IRESO is not zero, the next line contains the name of the file where the instrumental resolution function is given. The profile is assumed to be a Voigt function (NPROF=7). 12 parameters or a table determine the resolution function. Ui,Vi,Wi,Xi,Yi,Zi (i=1,2 for lambda1 and lambda2) The different types of functions are: =1 HG**2= (Ui*tan(q)+Vi)*tan(q)+Wi HL= Xi*tan(q)+Zi =2 HG**2= (Ui*tan(q)+Vi)*tan(q)+Wi HL= (Xi*(2q)+Yi)*(2q)+Zi =3 HG**2= (Ui*(2q)+Vi)*(2q)+Wi HL= (Xi*(2q)+Yi)*(2q)+Zi =4 List of values 2q, HG(2q), HL(2q) (a linear interpolation is applied for intermediate 2q) ISTEP=1,2,3,.. If ISTEP>1 the number of data points is reduced by (Ste) a factor of ISTEP. Only those points corresponding to the new step size ISTEP*STEP (see Line #3 below) are taken into account in the refinement. Useful for speed-up preliminary refinements. NRELL Number of parameters to be constrained within given (Nre) limits. At the end of the file you must give a list of NRELL lines specifying the number and the limit of each parameter. ICRYG If not equal to zero, only integrated intensity data (Cry) will be given. No profile parameters are needed. For ICRYG=2 no least-squares algorithm is applied. Instead a Montecarlo search of the starting configuration is performed. A selected number of parameters NRELL are moved within a box defined by the NRELL relations fixing the allowed values of the parameters. The best (lowest R-factor) NSOLU solutions are printed and theCODFIL.PCRfile is updated with the best solution. (See NRELL variable in this line and Line ) IXUNIT Units of the scattering variable (Uni) =0 2theta in degrees =1 T.O.F. in micro-seconds ICORR (Cor) =0 No correction is applied =1 A file with intensity corrections is read. The corrections are applied to the integrated intensities as a multiplicative constant. The file CODFIL.COR starts with a comment and follows with a list of pairs: a simple list of abcisae and correction values. TITLE ...... Scattering variable (T) Value of the correction " " ............. ................ Data are read in free format. For peaks between points provided in the CODFIL.COR file, the correction is linearly interpolated. Example: First line -> This is my correction FILE for Following lines -> 10.0 1.3 20.0 1.1 30.0 1.0 40.0 0.9 80.0 0.8 120.0 0.7 180.0 0.7 The intensity of a reflection at scattering variable 40 is assumed to be I(calc)*0.9. =2 A similar file is read but the coefficients of an empirical function and their standard deviations are read instead of directly the corrections. The format is: First line -> TITLE .... Second line -> ITYCORR, ITYFUNC, NPCORR Following lines -> Coefficient Sigma(Coefficient) (NPCORR lines) If ITYCORR = 1 corrections are applied to the integrated intensities. Standard deviations must not be given. ITYCORR = 2 corrections are applied to the observed profile. The corrected observed profile and their variance are obtained as: y(corr) = y(obs)/cor Sigma2(y(corr)) = sigma2(y(obs))/cor^2 + sigma2(cor)/y(obs)^2 NPCORR : Number of coefficients of the empirical function. ITYFUNC=1 Polynomial function: cor = Sum{i=1,npcorr}{coeff(i)* T**(i-1))} ITYFUNC=2 Exponential + Maxwellian for TOF raw data cor = Coeff(1)+ Coeff(2)*Exp(-Coeff(3)/T^2)/T^5+ + Sum{i=4,NPCORR,2}{Coeff(i)*Exp(-Coeff(i+1)*T^2)}Line 2-1*: FILERES(A16) Name of the file with the instrumental resolution function. To be given only in the case of IRESO<>0. The items in FILERES are read in free format. The first line is considered as a title For IRESO=1,2,3 the 12 parameters Ui, Vi, Wi, Xi, Yi, and Zi are read from lines 2 and 3 (see the above line for the available instrumental functions). Example: Line1: Resolution function of MyXrayDiffractometer Line2: 0.00802 -0.00936 0.01024 0.0029 0.0 0.0 ! U1,V1... Line3: 0.00774 -0.00552 0.00814 0.0000 0.0 0.0 ! U2,V2... For IRESO=4, the file FILERES starts with a line whith the title followed by a line with the number of points (NPOINS) where the instrumental Gaussian and Lorentzian FWHM are given. NPOINS lines follow containing the three items: 2thet, HG and HL. The Bragg peaks of the diffraction pattern must be between 2thet(1) and 2thet(NPOINS). For this case the same resolution function is applied to both wavelengths. The maximum number of NPOINS is 30. ============================================================================LINE 3 :IOT, IPL, IPC, MAT, NXT, LST1, LST2, LST3, IPL1, IPL2, INSTRM, JCIL, JSY, JLKH, JFOU, ISHOR, IANALY (17 integers) --------------Comment line : !Ipr Ppl Ioc Mat Pcr Ls1 Ls2 Ls3 Syo Prf Ins Rpa Sym Hkl Fou Sho Ana ---------------------------- List of output control flags : normally 0 = off / any value = on IOT = 1 obs. & calc. profile intensities -->CODFIL.OUT(0) (Ipr) 2 The filesCODFILn.SUBwith the calculated profile of each phase are generated. 3 As 2 but the background is added to each profile. IPL = 1 line printer plot -->CODFIL.OUT(Ppl) 2 Generates the background-fileFILE.BAC3 Puts difference pattern in fileFILE.BACIPC = 1 list of obs. & calc. integr. int. -->CODFIL.OUT(Ioc) = 2 The reflections corresponding to the second wavelength are also writen if different from the first one. MAT = correlation matrix -->CODFIL.OUT(Mat) If MAT=2, the diagonal of LSQ matrix is printed before inversion at every cycle. NXT = 1CODFIL.PCRis re-written with updated parameters (Pcr) 2 new input file -->CODFIL.NEWLST1 = reflection list -->CODFIL.OUT(usually 0) (Ls1) LST2 = 1 corrected data list -->CODFIL.OUT(usually 0) (Ls2) 4 In some versions of FullProf a plot of the diffraction pattern is diplayed on the screen at each cycle of refinement. LST3 = merged reflection list -->CODFIL.OUT(usually 0) (Ls3) IPL1 = symmetry operators -->CODFIL.OUT(+CODFIL.SYMif JSY=1) (Syo) IPL2 = output data for plot -->CODFIL.PRF(Prf) = 1 Format suitable for PLOTPOW, BENSTRAP,PLOTR, etc.. = 2 " " " IGOR (MacIntosh software) = 3 " " " KaleidaGraph (MacIntosh software) & PLOTR (Pc software) = 4 " " " Picsure, Xvgr(Sun-Unix Software) INSTRM= 0 Data supplied in free format (Ins) Up to seven comment lines are accepted. The first three real numbers found at the beginning of a line are interpreted as Ti, step and Tf. The following lines after (Ti, step, Tf) must contain NPTS=(Tf-Ti)/step+1 values of the intensity profile. Data format from Argonne are also interpreted by this value of INSTRM. 1 D1A/D2B format (original Rietveld-Hewat format : the first line must be 2Thetai, step, 2Thetaf, i.e. the first four lines of the POWDER file must be removed. Note however that angles are given in degrees 2Theta, not in hundredths of degree ! ). 2 D1B old format (DEC-10) 3 new format for D1B & D20 (Vax DataBase) +/-4 Brookhaven synchrotron. 4: First line: 2thetamin, step, 2thetamax (free format) Rest of file: pairs of lines with 10 items like Y1 Y2 ......... Y10 -- (10F8) intensities S1 S2 ......... S10 -- " sigmas -4: Format given by DBWS program for synchrotron data. (Version DBW3.2S-8711) 5 Data from GENERAL FORMAT for TWO AXIS instrument 3 lines of text followed by two lines with the items: -> NPTS, TSample, Tregul, Ivari, Rmon1, Rmon2 -> Ti, step, Tf Set of lines containing 10 items corresponding to the Intensities in format 10F8.1, up to NPTS points (NPTS=(Tf-Ti)/step+1), followed by the corresponding sigmas in format (10f8.2) if Ivari=1. If Ivari=0 the sigmas are calculated as SQRT(Yi*Rmon1/Rmon2). 6 D1A/D2B standard format for filesMYFILE.SUMprepared by D1A(D2B)SUM or equivalent programs. The extension of the data file must be 'dat'. 7 Files from D4 or D20L 8 Data from DMC at Wurenlingen (Paul Scherrer Institut) 9 Data of fileCODFIL.UXDgenerated by the Socabim software on X-Rays diffractometer. 10 X,Y,Sigma format with header lines. In all cases the first 6 lines are considered as comments. If in the first line (left ajusted) appears the keyword XYDATA, then the following 5 lines are considered as the heading of the file. Among these 5 lines the following keywords and values have a meaning to the program: -> INTER fac_x fac_y Interpol Stepin -> TEMP tsamp fac_x internal multiplier of X-values fac_y internal multiplier of Y and Sigma-values Interpol=0 Variable step is used in the program =1 The variable step data are interpolated internally to the constant step Stepin. =2 Data are supplied directly at constant step If no sigma values are provided the program assumes that sigma(Y)=sqrt(Y). You can add comments to the data file if they start with the character ! in the first position of the line. These lines are ignored by the program. 11 Data from variable time X-ray data collection The first four lines are considered as comments The following lines are: -> 2Thetai, step, 2Thetaf Comment -> (Time, Intensity) in format 5(F6, I10) The program uses the information contained in Time to normalize the observed intensities to the average time