# This is a template file for RIETAN-2000 for angle-dispersive X-ray and neutron # diffraction. # Many comments are sprinkled in this file for beginners. Power users may # delete part of them to shorten it. Addition of memorandums is also fine. # Comments can be input in the following manner: # (1) # comment # (2) Comment { # (3) } comment # (4) Variable name = value: comment # (5) Variable name = value! comment # Form (1) may in input from the middle of a line. Lines with a top character # of '#' or forms (2) and (5) are regarded as comment lines as a whole. # Form (2), which is usually used in combination with form (3), is optional; # that is, it is a mere comment line without any effect during refinement. # Form (3) is used to indicate the end of a series of input lines. Variable # names in Forms (4) and (5) should appear only once in one file. The first # character of an integer variable should be I, J, K, L, M, or N whereas that # of a real variable capital letters other than these characters. # Title (CHARACTER*80) Fluorapatite, Ca5F(PO4)3 NBEAM = 0! Neutron powder diffraction. NBEAM = 1: Conventional X-ray powder diffraction with characteristic X rays. NBEAM = 2! Synchrotron X-ray powder diffraction. NMODE = 0: Rietveld analysis of powder diffraction data. NMODE = 1! Calculation of powder diffraction intensities (plus simulation). NMODE = 2! Total-pattern fitting where structure factors are fixed at Fc(MEM)'s. NMODE = 3! The same as NMODE = 2 but refine |Fc|'s for relaxed reflections. NMODE = 4! Conventional Le Bail analysis. NMODE = 5! Le Bail analysis using a partial structure. NMODE = 6! Individual profile fitting. NPRINT = 0! Minimal output. NPRINT = 1! Standard output. NPRINT = 2! Detailed output. NPRINT = 0 If NBEAM = 0 then XLMDN = 1.5401: Neutron wavelength/Angstrom. RADIUS = 0.5: Radius/cm of the cylindrical cell. ABSORP = 1.0! Positive --> Density/g.cm-3 of the sample.* ABSORP = 0.0: Zero --> Neglect absorption. ABSORP = -1.0! Negative --> -(Linear absorption coefficient)*(radius). # * Calculated from the inner diameter, height, and mass of the sample. else if NBEAM = 1 then NTARG = 1! Ag K_alpha radiation. NTARG = 2! Mo K_alpha radiation. NTARG = 3! Cu K_beta radiation. NTARG = 4: Cu K_alpha radiation. NTARG = 5! Co K_alpha radiation. NTARG = 6! Fe K_alpha radiation. NTARG = 7! Cr K_alpha radiation. R12 = 0.497: Intensity(K-alpha2)/Intensity(K-alpha1). R12 = 0.0 for Cu K_beta radiation. CTHM1 = 0.7998: (cos(2*alpha))**n for the monochromator.* # * alpha: Bragg angle of the monochromator. CTHM1 = 1.0 if no monochromator is installed. NSURFR = 0: Do not correct for surface roughness. NSURFR = 1! Correct for surface roughness by combining NSURFR = 2 and 3. NSURFR = 2! Correct for surface roughness with Sparks et al.'s model. NSURFR = 3! Correct for surface roughness with Suortti's model. NSURFR = 4! Correct for surface roughness with Pitschke et al.'s model. NTRAN = 0: Bragg-Brentano geometry (conventional divergence slit). NTRAN = 1! Bragg-Brentano geometry (automatic divergence slit*). NTRAN = 2! Transmission geometry (e.g., Guinier diffractometer). NTRAN = 3! Debye-Scherrer geometry. # * This slit gives variable divergence angles and a fixed irradiation width. else if NBEAM = 2 then XLMDX = 1.5401: X-Ray wavelength/Angstrom. PCOR2 = 0.05: I0(perpendicular)/I0(parallel). I0: incident intensity. # Refer to D.E. Cox, "Synchrotron Radiation Crystallography," ed by # P. Coppens, Academic Press, London (1992), p. 233. CTHM2 = 1.0: cos(2*alpha)**2 for the crystal monochromator (see above). XMUR2 = 0.0: (Linear absorption coefficient)*(radius). end if If NBEAM = 1 and NTRAN = 1 then DSANG = 0.5: Angle/degree of the divergence slit at the minimum 2-theta. RGON = 185.0: Goniometer radius/mm. SWIDTH = 20.0: Irradiation width/mm for the sample. else if NBEAM = 1 and NTRAN = 2 then PCOR1 = 0.5: Fraction of the perfect crystal contribution. SABS = 1.0: (Linear absorption coefficient)*(effective thickness). else if NBEAM = 1 and NTRAN = 3 then XMUR1 = 0.0: (Linear absorption coefficient)*(radius). end if If NBEAM = 0 then # Real neutral chemical species, amounts of substances, plus '/'. Names of # 'real chemical species' are recorded in the database file asfdc. The # amounts of substances are used to calculate absorption factors. When # magnetic scattering is observed, attach '*' to magnetic atoms if any, # e.g., 'Fe*' and 'Mn*'. 'O' 12.0 'P' 3.0 'Ca' 5.0 'F' 1.0 / # Input LCMFF (= 0) and CMFF(I) (I = 1-7) for magnetic atoms attached with # '*'. LCMFF and CMFF corresponds to l and seven coefficients in Eqs. # (4.4.5.2) and (4.4.5.3) in "International Tables," Vol. C (1999), p. 456. # The total number of these lines equals the number of magnetic atoms. # The following line is input for Fe2+ (l = 0): # 0 0.0263 34.960 0.3668 15.943 0.6188 5.594 -0.0119 # '}' is unnecessary because the number of atoms attached with '*." has # already been known. else if NBEAM >= 1 then # Real chemical species plus '/'. # Refer to the data base file asfdc for chemical species to be input here. 'O-' 'P' 'Ca2+' 'F-' / end if If NBEAM = 0 then # Skip else if NBEAM = 2 or NTARG = 3 then # Read pairs of anomalous dispersion corrections, Delta-f' and Delta-f''. # Input statements in RIETAN: READ(5,*) (DELTF1(J), DELTF2(J), J=1, NREAL). # NREAL: Number of real chemical species. # Neither '/' nor '}' is required bacause the number of input data (2*NREAL) # has been already known. end if # When a site is occupied by two or more chemical species as in solid # solutions, supposing an 'virtual' chemical species where these chemical # species are mixed with each other in definite amount-of-substance # fractions (total = 1) serves to decrease the total number of sites. # Of course, such virtual species can be used only when their occupancies # are fixed. Input one virtual species plus '/' per line and '}' (plus comment) # in the last line in the following way: # Virtual chemical species # 'M1' 'Ba' 0.633 'Nd' 0.367 / # Metal on the rock-salt layer # 'M2' 'Nd' 0.675 'Ce' 0.325 / # Eight-coordinated atom in the fluorite block # } End of virtual chemical species. # 'M1' and 'M2' are names of virtual chemical species, 'Ba', 'Nd,' and 'Ce' are # names of real chemical species input above, and numbers are amount-of- # substance fractions of constituent elements. For the above species, Refer to # F. Izumi et al., Physica C 160 (1989) 235. # When no virtual species are used, all the lines must be commented out. Data concerning crystalline phases contained in the sample { # Phase No. 1 PHNAME1 = 'Fluorapatite': Phase name (CHARACTER*25). VNS1 = 'A-176': (Vol.No. of Int.Tables: A or I)-(Space group No)-(Setting No). LSPSYM1 = 0: Information on the space group is read from the data base. LSPSYM1 = 1! In addition to LSPSYM = 0, reflection conditions are specified. LSPSYM1 = 2! A non-standard axes-setting method is adopted. # Additional input data are required when SSPSYM1 > 0 but not described here # because of its rare use. If NBEAM >= 1 then LPAIR1 = 0: No Bijvoet pairs (hkl & -h-k-l) are generated. LPAIR1 = 1! Bijvoet pairs (hkl & -h-k-l) are generated. # Set at 0 in a centrosymmetric space group. Note that in 24 centrosymmetric # space groups, e.g., origin choice 1 for Pnnn (No. 48), descriptions with # points of higher symmetry as origin are also provided. Setting this value # at 0 for a noncentrosymmetric space group increases the calculation speed # with lowering accuracy of structure factors. end if INDIV1 = 0! The overall isotropic atomic displacement parameter is input. INDIV1 = 1: Atomic displacement parameters are assinged to all the sites. # Neither B's nor beta_ij's are input if INDIV1 = 0. Input zero for the # overal isotropic atomic displacement parameter, Q, when INDIV1 = 1. # Correction of perferred orientation NPROR1 = 0! Preferred orientation is not corrected for. NPROR1 = 1! Sasa-Uda function for plate crystals. NPROR1 = 2! Sasa-Uda function for needle-like crystals. NPROR1 = 3: March-Dollase function.* # * Note that the preferred orientation effect disappears in March-Dollase # function when r = 1. IHP1 = 1: € IKP1 = 0: --> Preferred-orientation vector, hp, kp, lp. ILP1 = 0: / # The preferred-orientation vector should be set in such a way that it is # a reciprocal-lattice vector, hpa* + kpb* + lpc*, perpendicular to a cleavage # plane for a plate crystal and parallel with an extention direction for a # needle-like crystal. They are dummies when NPROR1 = 0. LSUM1 = 0! No summation when calculating the March-Dollase function. LSUM1 = 1: Summation when calculating the March-Dollase function.* # * Required when the symmetry is cubic, or the preferred-orientation vector # does not lie along the unique axis. Dummy unless NPROR1 = 3. IHA1 = 0: € IKA1 = 0: --> Anisotropic-broadening axis, ha, ka, la. ILA1 = 1: / # They are dummies when parameters related to anisotropic profile # broadening are set at null. # If two or more phases are included in the sample, repeat their date below. # Note that the same label should not be input repeatedly. # Place '}" (+ comment) after the input of information on all the phases. } End of information about phases. # Selection of the profile function. NPRFN = 0! Pseudo-Voigt function of Thompson et al.* NPRFN = 1! Split pseudo-Voigt function of Toraya.** NPRFN = 2! Modified split pseudo-Voigt function*** for relaxed reflections. NPRFN = 3! Split Pearson VII function of Toraya.** # * P. Thompson et al., J. Appl. Crystallogr. 20 (1987) 79. # ** H. Taraya, J. Appl. Crystallogr., 23 (1990) 485. # *** FWHM(Lorentz) <> FWHM(Gauss). The split pseudo-Voigt function is # applied for the other reflections. Refer to the following paper: # F. Izumi and T. Ikeda, Mater. Sci. Forum, 321-324 (2000) 198. NPRFN = 1 If NPRFN = 0 then NASYM = 0! Made asymmetric according to the procudure of Finger et al.* NASYM = 1! Made asymmetric according to the procudure of Howard.** # * L. W. Finger et al., J. Appl. Crystallogr. 27 (1994) 892. # ** C. J. Howard, J. Appl. Crystallogr. 15 (1982) 615. NASYM = 0 end if If NPRFN >= 1 then # Selection of the peak-shift function. # t0 - t3: Peak-shift parameters; x: 2-theta. NSHIFT = 0! t0. NSHIFT = 1! t0 + t1*cos(x) + t2*sin(x) + t3*tan(theta). NSHIFT = 2! t0 + t1*x + t2*x^2 + t3*x^3. NSHIFT = 3! t0 + t1*tan(theta) + t2*(tan(theta))^2 + t3*(tan(theta))^3. NSHIFT = 4: Legendre polynomials where 2-theta is normalized as -1 to 1. NSHIFT = 5! Legendre polynomials where tan(theta) is normalized as -1 to 1. end if # Labels (CHARACTER*25), parameters, A(I), to calculate diffraction intensities, # and refinement identifiers, ID(I). ID(I)'s are input without inserting any # spaces between them only when NMODE = 0 (no problem even if they are input # when NMODE = 1). # In what follows, PPP and SPP denote a primary profile parameter and a # secondary profile parameter, respectively. For example, when calculating # the FWHM, H, with the equation H = [U(tan(theta)**2 + Vtan(theta) + W]^0.5, # H is a PPP, the FWHM parameters U, V, and W are SPPs. In conventional # Rietveld analysis, SPP's which are common to the whole 2-theta range are # refined whereas PPPs are locally refined for relaxed reflections. # ID(I) = 0: Fix parameter A(I) at the value input by the user. # ID(I) = 1: Refine parameter A(I). # ID(I) = 2: Impose a constraint to parameter A(I). # ID(I) = 3: Fix a PPP at the value calculated from SPP's. # If A(I) is set at zero by the user, A(I) is calculated from the SPP's in each # cycle. In this case, if A(I) should actually be fixed at zero, input a value # which is nearly zero, e.g., 10^(-15). # Relations between ID(I)'s, NPRFN, and partial profile relaxation: # (1) Partial profile relaxation cannot be used when NPRFN = 0. # (2) ID(I)'s are 1-3 when NPRFN = 1, 3 under partial profile relaxation. # (3) ID(I)'s are 1 or 2 when NPRFN = 2 under partial profile relaxation. Label, A(I), and ID(I) now starts here { # (1) Parameters common to all the phases. # Peak-shift parameters. # NPRFN = 0: Z, Ds, Ts & dummy1 (Ds = Ts = 0 in neutron diffraction). # NPRFN > 0: t0, t1, t2 & t3. If NPRFN = 0 then SHIFT0 0.14849 -1.14695E-1 1.28877E-2 0.0 1110 else SHIFTN 7.11671E-2 2.42176E-2 3.77026E-3 0.0 1000 end if # Surface-roughness parameters. ROUGH 0.0 0.0 0.0 0.0 0000 # Background parameters, b_j (j = 0-11). BKGD 114.755 -1.26653E2 139.198 -1.01964E2 68.0988 -3.93928E1 23.3125 -7.44573 -2.02245 3.58392 0.0 0.0 111111111100 # PPP's of relaxed reflections (input as requied. May be lacking). # Format of each label: PPPn_h.k.l (n: phase number, hkl: diffraction index). # PPP's refined in relaxed reflections: # NPRFN = 1 (split pseudo-Voigt function): W, A, eta_L, eta_H. # NPRFN = 2 (modified split pseudo-Voigt function): W1, W2, A, eta_L, eta_H. # NPRFN = 3 (split Pearson VII function): W, A, mL, mH. # PPP1_1.0.0 0.123836 6.79726E-2 0.936762 0.228537 0.186868 11111 # PPP1_-1.0.0 0.123836 6.79726E-2 0.936762 0.228537 0.186868 22222 # (2) Parameters relevant to the first phase. # Scale factor, s. SCALE 3.56387E-5 1 # Profile parameters. If NPRFN = 0 and NASYM = 1 then # TCH's pseudo-Voigt function made asymmetric by Howard's method. # FWHM parameters of the Gauss function, U, V, W, and P. GAUSS01 1.49395E-4 7.401285E-5 2.558033E-4 0.0 0110 # FWHM parameters of the Lorentz function, X, Xe, Y, and Ye. LORENTZ01 3.157068E-2 2.282011E-3 2.879626E-2 -1.928188E-3 1111 # Asymmetry parameter, As, plus five dummies. ASYM 2.800001E-2 0.0 0.0 0.0 0.0 0.0 100000 else if NPRFN = 0 and NASYM = 0 then # TCH's pseudo-Voigt function made asymmetric by Finger et al.'s method. # FWHM parameters of the Gauss function, U, V, W, and P. GAUSS00 1.49395E-4 1.41366E-4 2.07988E-4 0.0 0110 # FWHM parameters of the Lorentz function, X, Xe, Y, and Ye. LORENTZ00 3.3918E-2 1.85408E-3 2.48941E-2 -1.11746E-3 1010 # Asymmetry parameters, rs and rd, plus four dummies. ASYM00 2.82968E-2 9.34981E-3 0.0 0.0 0.0 0.0 110000 else if NPRFN = 1 or NPRFN = 2 then # Non-relaxed reflections: split pseudo-Voigt function # Relaxed reflections: Modified split pseudo-Voigt function. # FWHM parameters, U, V, and W, plus a dummy. FWHM12 5.77641E-3 -1.67383E-3 5.66877E-3 0.0 1110 # Asymmetry parameters, a0, a1, and a2 plus a dummy. ASYM12 1.03944 0.141961 -4.10434E-2 0.0 1110 # Decay parameters, eta_L0, eta_L1, eta_H0, and eta_H1. ETA12 0.611844 0.140346 0.504656 0.175874 1111 # Asymmetric-broadening parameters, Ue and Pe. ANISOBR12 0.0 0.0 00 else if NPRFN = 3 then # Split Pearson VII function # FWHM parameters, U, V, W, plus a dummy. FWHM3 5.874843E-3 -2.614835E-3 5.290567E-3 0.0 1110 # Asymmetry parameters, a0, a1, and a2, plus a dummy. ASYM3 0.976399 0.184397 -4.801547E-2 0.0 1110 # Decay parameters, eta_L0, eta_L1, eta_H0, and eta_H1. M3 0.712220 0.219749 0.630807 0.125848 1111 # Asymmetric-broadening parameter, Ue and Pe. ANISOBR3 0.0 0.0 00 end if # Preferred-orientation parameter, r, dummy9 (March-Dollase function); # p1, p2 (Sasa-Uda function). PREF 0.998331 0.0 10 # Lattice parameters, a, b, c, alpha, beta, & gamma. # Overall isotropic atomic displacement parameter, Q. CELLQ 9.36884 9.36884 6.88371 90.0 90.0 120.0 0.0 1010000 # Lable/(chemical species name), occupancy (g) , fractional coordinates # (x,y,z), istropic atomic displacement parameter (B), ID(I)'s. # One label is given to each site. 'Chemical species' include virtual ones # (should not enclosed by ' '). On the calculation of anisotropic atomic # displacement parameters, input beta_11, beta_22, beta_33, beta_12, # beta_13 and beta_23. If a dummy '+' is input just before the value of B, # RIETAN will determine the corresponding beta_ij. Of course, six ID(I)'s # must be input in this case. O1/O- 1.0 0.324184 0.485358 0.25 0.737457 01101 O2/O- 1.0 0.591783 0.469823 0.25 0.739035 01101 O3/O- 1.0 0.339149 0.257271 6.98004E-2 0.83381 01111 P/P 1.0 0.39731 0.367878 0.25 0.554302 01101 Ca1/Ca2+ 1.0 0.333333 0.666667 1.33E-3 0.647714 00011 Ca2/Ca2+ 1.0 0.241793 -7.9608E-3 0.25 0.531388 01101 F/F- 1.0 0.0 0.0 0.25 1.42319 00001 } End of lines for label/species, A(I), and ID(I) # If two or more phases are included in the sample, repeat the input of # parameters (scale factor or later) after structure parameters in the # previous phase. Do not enter labels that have already been input. If NMODE <> 1 then # Input linear constraints for parameters with ID(I) = 2. A parameter with # ID(I) = 2 is place at the left side, and equations to calculate it from other # parameters with ID = 1. "Linear" means that the equation is linear with # respect to parameters contained in the right side. Linear constraints can # be imposed on PPPs, SPPs, and structure parameters. In the case of SPPs, # the linear constraints are used to set SPPs for two or more phases equal # to each other. Refer to the user's manual for the method of describing # linear constraints. # For example, linear constraints imposed among anisotropic atomic displacement # parameters, beta_ij, are described in the following ways: # A(X,B22)=A(X,B11) #5 # A(X,B22)=A(X,B11); A(X,B23)=A(X,B13) #6 # A(X,B22)=A(X,B11); A(X,B23)=-A(X,B13) #7 # A(X,B22)=A(X,B11) #8 # A(X,B33)=A(X,B22) #9 # A(X,B33)=A(X,B22); A(X,B13)=A(X,B12) #10 # A(X,B33)=A(X,B22); A(X,B13)=-A(X,B12) #11 # A(X,B33)=A(X,B22) #12 # A(X,B12)=0.5*A(X,B22) #13 # A(X,B12)=0.5*A(X,B22) #14 # A(X,B12)=0.5*A(X,B22); A(X,B23)=2.0*A(X,B13) #15 # A(X,B22)=A(X,B11); A(X,B12)=0.5*A(X,B11) #16 # A(X,B22)=A(X,B11); A(X,B33)=A(X,B11) #17 # A(X,B22)=A(X,B11); A(X,B33)=A(X,B11); A(X,B13)=A(X,B12); A(X,B23)=A(X,B12) #18 # where 'X' is a label (site name). Please replace it with another label. # Comments ('#'+integer) at the tails of these lines denote reference numbers in # W. J. A. M. Peterson and J. H. Palm, Acta Crystallogr. 20 (1966) 147. # Place '}" + comment after the input of all the linear constraints. # When no constraints are given, comment out them, including '}.' #} End of linear constraints. end if NCUT = 0! The profile range for relaxed reflections is determined by RIETAN. NCUT = 1! The profile range for relaxed reflections is input by the user. NCUT = 0 # NCUT = 0 when NPRFN = 0. If NCUT = 1 then # 2-theta ranges for the profiles of relaxed reflections in the same order # as PPn_h.k.l+PPP. The total number of 2-theta pairs is equal to that of # the PPn_h.k.l+PPP+ID lines. in the same order. No '}' is necessary # because the number of the relaxed reflections has been already known. 5.10 9.40 11.00 14.10 18.20 21.80 19.40 24.10 21.60 23.40 end if If NMODE <> 1 then NEXC = 0: Parameters are refined using all the data points. NEXC = 1! Parameters are refined by excluding part of the data points. end if If NMODE <> 1 and NEXC = 1 then 2-theta range not to be used for the refinement { 0.0 14.99 130.01 180.0 } End of excluded 2-theta ranges. end if If NMODE <> 1 then NRANGE = 0: Refine background parameters. NRANGE = 1! Fix backgrounds at (interpolated) values at specified 2-theta's. NRANGE = 2! Fix backgrounds of all the points at values in *.bkg. NRANGE = 3! Background = (background in *.bkg) * (Legendre polynomials). end if # When NRANGE > 0, 2-theta and background pairs are read in from *.bkg. # (1) NRANGE = 1 # If a background is zero, it is set at a smoothed value at that data point. # Backgrounds at other data points are fixed at interpolated values. Such a # manner is useful for the analysis of diffraction patterns where the number of # reflections are relatively small and the background curve is complex, for # example, having humps. # List-directed READ statement in RIETAN-2000: READ(4,*) (X(J),Y(J), J=1,100). # That is, we can input up to 100 diffraction points. To show the end of data # points, place '/' after the last data point. # (2) NRANGE = 2 # Input 2-theta and background pairs whose total number should be equal to # that of observed diffraction intensities in *.int. # List-directed READ statement in RIETAN-2000: # READ(8,*,END=9) (DEG(J),BG(J), J=1,NP) # (3) NRANGE = 3 # This composite background function is particularly useful for the Debye- # Scherrer geometry where samples are charged in capillaries, which makes the # shape of the background complex. If NMODE <> 1 then NPAT = 0! Output no file to plot Rietveld-refinement patterns. NPAT = 1! Not implemented. NPAT = 2! Ouput a RietPlot file to plot Rietveld-refinement patterns. NPAT = 3! Not implemented. NPAT = 4! Output a gnuplot text file to plot Rietveld-refinement patterns. NPAT = 5: Output an Igor text file to plot Rietveld-refinement patterns. # NPAT = 4 (every OS) or 5 (Mac OS and Windows) is recommended. end if If NMODE <> 1 and NPAT = 5 then IWIDTH = 800: Width of the graph. IHEIGHT = 400: Height of the graph. IYMIN = -2500: Minimum value for the y axis (default for zero). IYMAX = 20000: Maximum value for the y axis (default for zero). LBG = 0: Do not plot the background. LBG = 1! Plot the background. # Kind of a residual curve LDEL = 0: Plot Delta_y = (observed intensity - calculated intensity). LDEL = 1! Plot Delta_y/(standard deviation). LDEL = 2! Plot [Delta_y/(observed intenstiy)]/(standard deviation).* # * Refer to Eq. (1.13) in R. A. Young, "The Rietveld Method," p. 24. IOFFSETD = -1500: Offset for the residual curve. IPSIZE = 3: Length of tick marks to show peak positions. IFSIZE = 12: Size of numerial values attached to the x and y axes. ILSIZE = 14: Size of labels for axes. INDREF = 0: Do not output waves XREF or YREF. INDREF = 1! The profile of each reflection is output to waves XREF and YREF. IOFFSET1 = -300: Offset for tick marks (peak positions) for the first phase. # If other phases are contained, input offsets in the above way. / # Place '/' if the number of phases whose offsets are input is less than 8. # You may also edit Igor procedures at the tail of *.itx with an editor. end if If NMODE = 1 then DEG1 = 10.0: Minimum 2-theta in the calculated (simulated) pattern. DEG2 = 60.0: Maximum 2-theta in the calculated (simulated) pattern. USTP = 0.01: Step width/degree. NPAT = 0! Only the reflection list is output. NPAT = 1! Not implemented. NPAT = 2! Output a RietPlot file to plot a simulated pattern. NPAT = 3! Not implemented. NPAT = 4! Output a gnuplot text file to plot a simulated pattern. NPAT = 5: Output an Igor text file to plot a simulated pattern. # NPAT = 4 (every OS) or 5 (Mac OS and Windows) is recommended. end if If NMODE = 1 and NPAT = 5 then IWIDTH = 800: Width of the graph. IHEIGHT = 400: Height of the graph. LBG = 0: Plot no bakcground (fixed). IPIZE = 3: Length of tick marks (peak positions). IFSIZE = 12: Size of numerial values attached to the x and y axes. ILSIZE = 14: Size of labels for axes. end if # PC: A constant to determine a 2-theta range for calculating profiles. # PC < 1 ==> A region where the profile function exceeds peak intensity X PC. # If NPRFN = 0, PC < 1. # PC > 1 ==> A region within peak position +/- FWHM*PC. If NPRFN = 0 then PC = 0.002 else if NPRFN = 1 then PC = 7.00 else if NPRFN >= 2 then PC = 7.00 end if # Skip the remaining part if NMODE = 1 If NMODE = 1 then Go to *Quit end if ############################################################################## # All the data have been input in the case of NMODE = 1. Bye! # ############################################################################## If NMODE = 4 then # Initial values of multiplicity X |Fc|**2 for the 1st phase are NSFF = 0! estimated according to the Wilson statistics. NSFF = 1! read in from *.ffi. NSFF = 2! all set at 100.0. NSFF = 0 end if If NMODE = 4 and NSFF <> 1 then INCMULT = 0! The integrated intensity is regarded as |F|**2. INCMULT = 1! The integrated intensity is regarded as multiplicity X |F|**2. INCMULT = 0 CHGPC = 1.0: Cut-off is at first set at CHGPC*PC.* # * Restored when lattice or profile parameters are refined. end if If NMODE = 4 and NSFF = 1 then NCONST = 0! |Fc|'s are varied during least-squares fitting. NCONST = 1! |Fc|'s remain constant during least-squares fitting.* # * |Fo|'s are calculated from final refined parameters. NCONST = 0 end if If NMODE <> 1 then # Nonlinear least-squares methods NLESQ = 0! Marquardt method (recommended in most cases). NLESQ = 1! Gauss-Newton method. NLESQ = 2! Conjugate-direction method (stable but very slow). NLESQ = 0 NESD = 0: Standard deviations are estimated by the conventional method. NESD = 1! Standard deviations are estimated by Scott's method.* # * Much larger standard deviations will result in comparison with NESD = 0. end if If NLESQ <= 1 then NAUTO = 0! Refine all the variable parameters simultaneously. NAUTO = 1! Refine incrementally (specify variable parameters in each cycle). NAUTO = 2! Refine incrementally (automatic; recommended in most cases). NAUTO = 3! In addition to NAUTO = 2, check convergence to the global min. NAUTO = 2 # Set NAUTO at 2 usually and at zero near the convergence. NCYCL = 10: Maximum number of cycles. CONV = 0.0001: Small positive number used for convergence judgement. NCONV = 6: Number of cycles used for convergence judgement. NC = 0: No nonlinear restraints are imposed on geometric parameters. NC = 1! Nonlinear restraints are imposed on geometric parameters. TK = 650.0: Penalty parameter. FINC = 2.0: Factor by which TK is multiplied when TK is increased. end if If NLESQ <= 1 and NAUTO = 1 then # Specify parameters to be refined in each cycle plus '/'. # In addition to absolute parameter numbers, "label,number/symbol" may be # used (Refer to user's manual). Parameters refined in each cycle { BKGD,1 BKGD,2 BKGD,3 BKGD,4 BKGD,5 BKGD,6 BKGD,7 BKGD,8 BKGD,9 BKGD,10 SCALE,1 / CELLQ,1 CELLQ,3 / # Place '}' (+ comment) after the last cycle. } End of inputs for numbers of refinable parameters. end if If NLESQ <=1 and NAUTO = 3 then # Input data for the conjugate-direction method (used to check the # convergence at a local minimum). MITER = 4: Maximum number of iterations. STEP = 0.02: Coefficient to calculate the initial step interval. ACC = 1.0E-6: Small positive number used for convergence judgement. end if If NLESQ = 2 then MITER = 4: Maximum number of iterations. STEP = 0.02: Coefficient to calculate the initial step interval. ACC = 1.0E-6: Small positive number used for convergence judgement. NC = 0: No nonlinear restraints are imposed on geometric parameters. NC = 1! Nonlinear restraints are imposed on geometric parameters. TK = 650.0: Penalty parameter. end if If NC = 1 then # To specify nonlinear restraints, an input file for ORFFE, Filename.xyz, # must be created by inputting non-zero NDA (described below). Then, ORFFE # is executed to output Filename.ffe, which is referred to learn serial # numbers for various interatomic distances and bond angles to enter them # in addition to their expected values and allowed deviations below. # If Filename.ffe has already been created, it is not created at all. # Therefore, note that Filename.ffe must be wasted to make it again. Ser. No. Exp. value Allowed dev. { 122 1.47 0.01 123 1.54 0.01 178 108.0 3.0 # Place '}' (+ comment) after the last restraint. } End of nonlinear restraints. end if NUPDT = 0! Variable parameters (ID = 1, 2) in the input file remain unchanged. NUPDT = 1! Variable parameters (ID = 1, 2) are updated in the packing mode. NUPDT = 0 # In the case of NUPDT = 1, parameters are updated by inserting two spaces # between data. NFR = 0! No file is output for Fourier/D synthesis. NFR = 1! Filename.hkl for Fourier/D synthesis is output for the first phase. NFR = 2! Filename.hkl for Fourier/D synthesis is output for the second phase. NFR = 0 NMEM = 0! No file is output for MEM analysis. NMEM = 1! Filename.fos for MEM analysis is output for the first phase. NMEM = 2! Filename.fos for MEM analysis is output for the second phase. NMEM = 0 NDA = 0! No file is output which store ORFFE data. NDA = 1! Filename.xyz for ORFFE is output for the first phase. NDA = 2! Filename.xyz for ORFFE is output for the second phase. NDA = 1 If NFR > 0 then NPIXAF = 32: Number of pixels along the a axis. NPIXBF = 32: Number of pixels along the b axis. NPIXCF = 128: Number of pixels along the c axis. TSCAT = 232.01: Total number of electrons (X-ray) or sum of b_c (N). # b_c: coherent scattering length (International Tables, Vol. C, p. 384). end if If NMEM > 0 then # Title (CHARACTER*70) written in *.fos. TITLE = 'Fluorapatite' LANOM = 0: Calculate esd's from I's without contributions of a.d. LANOM = 1! Calculate esd's from I's with contributions of a.d. # esd: estimated standard deviation, I: integrated intensity, # a.d.: anomalous dispersion NPIXA = 32: Number of pixels along the a axis. NPIXB = 32: Number of pixels along the b axis. NPIXC = 128: Number of pixels along the c axis. LGR = 0: All the reflections are output independently. LGR = 1! Reflections overlapped heavily are output by being grouped. LFOFC = 0: Using calculated F'o' based on Rietveld refinement. LFOFC = 1! Using Fcal (dependent on the model) in Rietveld refinement. EPSD = 0.001: Maximum difference in d/Angstrom in grouped reflections. TSCAT1 = 232.01: Total number of electrons (X-ray diffraction) or # sum of positive b_c (neutron diffraction). TSCAT2 = 0.0: Zero (X-ray diffraction) or # sum of negative b_c (Neutron diffraction). end if If NDA > 0 then # Input ORFFE instructions as required and place '}' (+ comment) at the tail. # Refer to the user's manual for ORFFE instructions used frequently. ORFFE # instructions must be input with a fixed column format; note not to set input # data at erroneous positions. If NDA > 0, Filename.xyz is output. This file # is used as an input file for ORFFE to calculate interatomic distances and bond # angles. ORFFE instructions in Filename.xyz can be modified and/or added by # the user. ORFFE instructions start { # Note that the formats of ORFFE instructions differ from original ones! # 1 2 3 4 5 6 7 8 #2345678901234567890123456789012345678901234567890123456789012345678901234567890 # Instruction 201, FORMAT(2I5,15X,I5). Output a list of interatomic distances # for all the sites. The second number is the number of sites. The third # integer is 10 X (maximum distance in Angstroms). # Interatomic distances less than 3.1 angstroms are listed 201 7 31 # Instruction 2, FORMAT(7I5). Calculate a bond angle. Three sets of A and # 1000*C + S (refer to the output of ORFFE) follow after instruction 2. # O3-P-O1 2 3 0 4 0 1 0 # O3-P-O2 2 3 0 4 0 2 0 } End of ORFFE instructions. # ORFFE instructions can be modified and added by editing *.xyz directly. end if # Cite the following reference whenever you report scientific results obtained # with RIETAN-2000: # F. Izumi and T. Ikeda, Mater. Sci. Forum, 321-324 (2000) 198. # Giving credit to RIETAN-2000 is fine in the case of abstracts, reports, etc. # If you like RIETAN-2000, please send me a postcard of your home town. # Is that too much to ask? # Fujio IZUMI # Advanced Materials Laboratory # National Institute for Materials Science # 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan *Quit