********************************************************** ** PROGRAM FullProf.2k (Version 2.30 - Mar2003-LLB JRC) ** ********************************************************** M U L T I -- P A T T E R N Rietveld, Profile Matching & Integrated Intensity Refinement of X-ray and/or Neutron Data Date: 14/01/2004 Time: 11:43:53.360 => PCR file code: corrected => DAT file code: mgznzf2hs -> Relative contribution: 1.0000 => Title: ==> CONDITIONS OF THIS RUN FOR PATTERN No.: 1 => Global Refinement of X-ray powder diffraction data => Global Refinement of X-ray powder diffraction data Flat plate with PSD => The 7th default profile function was selected => Data supplied in free format for pattern: 1 => Analysis of refinement at the end => Wavelengths: 1.54056 1.54056 => Cos(Monochromator angle)= 90.0000 => Absorption correction (AC), muR-eff = 0.0000 => Base of peaks: 2.0*HW* 20.50 ==> Angular range, step and number of points: 2Thmin: 10.1460 2Thmax: 80.1384 Step: 0.0146 No. of points: 4795 =>-------> Pattern# 1 => Crystal Structure Refinement for phase: 1 => Scor: 2.0551 ==> RESULTS OF REFINEMENT: => No. of fitted parameters: 12 ------------------------------------------------------------------------------ => Phase No. 1 MgZnFe2O3 F d 3 m ------------------------------------------------------------------------------ => No. of reflections for pattern#: 1: 18 ==> ATOM PARAMETERS: Name x sx y sy z sz B sB occ. socc. Mult Fe 0.12500( 0) 0.12500( 0) 0.12500( 0) 0.000( 0) 0.018( 0) 8 Mg 0.12500( 0) 0.12500( 0) 0.12500( 0) 0.000( 0) 0.003( 0) 8 O 0.25725( 22) 0.25725( 22) 0.25725( 22) 0.000( 0) 0.167( 0) 32 Fe 0.50000( 0) 0.50000( 0) 0.50000( 0) 0.000( 0) 0.066( 0) 16 Mg 0.50000( 0) 0.50000( 0) 0.50000( 0) 0.000( 0) 0.018( 0) 16 Zn 0.12500( 0) 0.12500( 0) 0.12500( 0) 0.000( 0) 0.021( 0) 8 ==> PROFILE PARAMETERS FOR PATTERN# 1 => Cell parameters : 8.41259 0.00004 8.41259 0.00004 8.41259 0.00004 90.00000 0.00000 90.00000 0.00000 90.00000 0.00000 => overall scale factor : 0.000010146 0.000000044 => Eta(p-v) or m(p-vii) : 0.00000 0.00000 => Overall tem. factor : -6.19353 0.03025 => Halfwidth parameters : -0.05958 0.00000 0.05848 0.00000 -0.00246 0.00000 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 => X and y parameters : 0.08865 0.00000 0.00427 0.00000 => Strain parameters : 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 => Size parameters (G,L): -0.00245 0.00000 0.00000 0.00000 => Add. shape parameters: 0.00000 0.00000 0.00000 0.00000 ==> GLOBAL PARAMETERS FOR PATTERN# 1 => Zero-point: 0.1345 0.0004 => Background Polynomial Parameters ==> 25801.8 6.67194 4436.96 41.6337 -2452.45 108.353 3504.87 404.238 -2706.56 320.359 -4857.10 900.639 => Cos( theta)-shift parameter : 0.0000 0.0000 => Sin(2theta)-shift parameter : 0.0000 0.0000 ==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS FOR PATTERN: 1 => Cycle: 1 => MaxCycle: 50 => N-P+C: 4313 => R-factors (not corrected for background) for Pattern: 1 => Rp:0.575 Rwp:0.795 Rexp: 0.62 Chi2: 1.62 M.L. refinement => Conventional Rietveld R-factors for Pattern: 1 => Rp: 40.8 Rwp: 11.0 Rexp: 8.65 Chi2: 1.62 => Deviance: 0.706E+04 Dev* : 1.637 => DW-Stat.: 1.3093 DW-exp: 1.9111 => N-sigma of the GoF: 29.005 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS FOR PATTERN: 1 => N-P+C: 3422 => R-factors (not corrected for background) for Pattern: 1 => Rp:0.583 Rwp:0.818 Rexp: 0.62 Chi2: 1.76 M.L. refinement => Conventional Rietveld R-factors for Pattern: 1 => Rp: 33.5 Rwp: 10.2 Rexp: 7.71 Chi2: 1.76 => Deviance: 0.608E+04 Dev* : 1.778 => DW-Stat.: 1.5213 DW-exp: 1.9010 => N-sigma of the GoF: 31.528 => Global user-weigthed Chi2 (Bragg contrib.): 2.05 => Phase: 1 => Bragg R-factor: 3.51 Vol: 595.372( 0.005) Fract(%): 100.00( 0.61) => Rf-factor= 5.45 ATZ: 1636.360 Brindley: 1.0000 ------------------------------------ - ANALYSIS OF THE REFINEMENT - ------------------------------------ => GLOBAL INDICATORS: The first and last reflections appears at: 2theta(degrees)/T.O.F(microsecs) => 18.250 81.671 s (angstroms-1) => 0.2059 0.8489 D (angstroms ) => 4.8570 1.1780 sin(theta/lamb) => 0.1029 0.4244 Q (angstroms-1) => 2.5873 10.6676 The average FWHM is: 0.1072 Fwhm(av)/step = 7.3426 => Sum(Yiobs-Yical): 1028.01 -7191.10 21668.85 -5341.87 <- Four regions Total -> 10163.88 Expected Rp (background uncorrected): 0.50 Observed-> 0.57 Expected cRp(background corrected): 35.50 Observed-> 40.79 -> Ratio Rp/Exp=cRp/cExp: 1.15 Weighted Average Bragg R-factor: 3.51 Weighted Average RF-factor: 5.45 Reduced Chi-square : 1.76 => Total number of "independent" reflections: 18 Effective number (account for resolution) of reflections: at level p=1.00 : 17.0 at level p=0.50 : 17.0 at level p=0.25 : 17.0 A reflection contributes as x/(x+nearest), where "x" is the fraction of the total area of the current phase and "nearest" is the number of adjacent reflections verifying the formula: Postn-p*FWHM <= Postn(adjacent) <= Postn+p*FWHM "nearest" is weighted by the corresponding "x(s)" => Number of global refined parameters: 7 Number of profile refined parameters: 3 Number of intensity-dependent refined parameters: 2 (Preferred orientation belongs to this class) => (Effective Number of reflections)/(Number of intensity parameters)= refni Ratio ( Optimistic view,p=0.25): 8.5 Ratio (Pessimistic view,p=1.00): 8.5 Ratio ( Eclectic view,p=0.50): 8.5 => PHASE DEPENDENT INDICATORS: => Positions and FWHM of the sharpest reflection Phase 2Theta/TOF FWHM Q DQ Delta Dd/d(%) 1 18.25 0.0640 1.2936 0.00450 0.47548 0.348 Q ,DQ(FWHM in Q-space) and Delta are given in 1/angstroms Delta is the expected step between consecutive reflections at Q Phase %Cont Nintdp Nprofp Nref Enref(Effective) R:p=1 R:p=1/2 R:p=1/4 1 100.00 2 3 18 17.00 17.00 17.00 8.50 8.50 8.50 Where: %Cont: percentage of the total integrated intensity (100x) Nintdp: Number of intensity-dependent refined parameters Nprofp: Number of profile refined parameters Nref: Number "independent" contributing reflections Enref: Effective Number of reflections for each p-value R:p=1/n: Ratio Enref(Effective)/Nintdp => ANALYSIS OF STANDARD DEVIATIONS Phase: 1 Degrees of freedom for p=1, 1/2, 1/4: 15.00 15.00 15.00 Chi2 based on integrated intensities: 0.48 0.48 0.48 Calculated with Scott'S FORMULA : 174.73 174.73 174.73 => Standard deviations concern the PRECISION of parameters and represent ACCURACY only if there is no systematic errors A better estimate of the accuracy of structural parameters is obtained multiplying sigmas by the parameter SCOR -> SCOR = 2.0551 { Berar'S FORMULA} -> SCOR = 2.7097 {Pawley'S FORMULA} -> Application of modified Scott'S FORMULA SCOR(p=1,1/2,1/4) = 0.5225 0.5225 0.5225 SCOR(expected Si) = 9.9577 9.9577 9.9577 Warning! Do not take into account Scott'S SCOR These indicators are under test.... => ANALYSIS OF CORRELATED PARAMETERS -> The parameter: 3 appears 3 times -> The parameter: 11 appears 3 times -> The parameter: 12 appears 4 times -> The number of correlated parameters is : 3 => Your refinement seems to be very good! CPU Time: 0.881 seconds 0.015 minutes => Run finished at: Date: 14/01/2004 Time: 11:43:54.290