RIETICA PERICLASE **** MULTI-RIETVELD ANALYSIS PROGRAM LH-RIET 7.200 periclase NUMBER OF PHASES = 1 NUMBER OF HISTOGRAMS = 1 NUMBER OF PARAMETER LIMITS = 0 NUMBER OF BOND RESTRAINTS = 0

*** HISTOGRAM 1 *** FOR X-RAY DATA NEWTON-RAPHSON ALGORITHM BACKGROUND TO BE REFINED (MAX 6 PARAMETERS) - POLYNOMIAL BACKGROUND THE PSEDUO-VOIGT PROFILE FUNCTION WAS SELECTED - USING THE HOWARD, SUM OF 5 PEAKS, ASYMMETRY WAVELENGTHS = 1.54051 1.54433 ALPHA2:ALPHA1 RATIO = 0.5000 BASE OF PEAK = 2.0*HW* 7.00 MONOCHROMATOR CORRECTION = 1.0000 ABSORPTION CORRECTION FOR CYLINDER SAMPLE USING ALGORITHM OF SABINE(1996)/DWIGGINS(1972) WITH mu = 0.0000 NO ILLUMINATION CORRECTION PREFERRED ORIENTATION USING MARCH MODEL - NO SUMMING OF EQUIVALENTS HISTOGRAM WEIGHTING = 1.0000 NO OTHER GEOMETRY CORRECTIONS APPLIED OUTPUT STRUCTURE FACTORS OUTPUT CORRELATION MATRIX GENERATE NEW INPUT FILE NUMBER OF CYCLES = 1 RELAXATION FACTORS: FOR COORDINATES, ISOTROPIC B, SITE OCCUPANCY = 0.90 FOR ANISOTROPIC TEMPERATURE FACTORS = 0.90 FOR SCALE, ZERO, B OVERALL, UNIT CELL, PREFERRED ORIENTATION BACKGROUND = 0.90 FOR PEAK WIDTH, ASYMMETRY, SHAPE PARAMETERS = 0.90 EPS-VALUE = 0.100

NUMBER OF PARAMETERS VARIED = 9

GLOBAL PARAMETERS AND CODEWORDS: ZEROPOINT( 1) = 0.00 0.00 HISTOGRAM READ IN AS CPI FORMAT HISTOGRAM 1 FROM 10.000000 TO 80.000000 IN STEPS OF 0.020000 DEGREES

BACKGROUND PARAMETERS AND CODEWORDS( 1) 9561.240234 -496.369995 9.460290 -0.059532 0.000000************ 11.000000 21.000000 31.000000 41.000000 0.000000 51.000000

****** PHASE 1 ******* periclase #1000053

PHASE IS CALCULATED USING STRUCTURAL INPUT NUMBER OF FORMULA PER UNIT CELL = 4 NUMBER OF ATOMS = 2 PREFERRED ORIENTATION VECTOR( 1) = 0.0000 0.0000 1.0000 THE SPACE GROUP IS F M 3 M

***INITIAL PARAMETERS*** ATOM NTYP X Y Z B N B11 B22 B33 B12 B13 B23 MG MG 0.00000 0.00000 0.00000 0.60000 0.02083 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 O O 0.00005 0.00005 0.00005 0.60000 0.16667 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000

***** PHASE INFORMATION ***** OVERALL SCALE FACTOR =0.100000E-01 OVERALL TEMP. FACTOR = 0.00000 DIRECT CELL PARAMETERS = 4.2219 4.2219 4.2219 90.0000 90.0000 90.0000

*** HISTOGRAM 1 *** HISTOGRAM SCALE FACTOR = 1.00000 0.00 PREFERRED ORIENTATION PARAMETER = 1.0000 ABSORPTION R = 0.0000 ASYMMETRY PARAMETERS = 0.020000 0.000000 GAUSSIAN HALF-WIDTH PARAMETERS = 0.0950 -0.0050 0.0200 ANISOTROPIC PARAMETER = 0.000000 PSEUDO-VOIGT PEAK SHAPE = 1.9408 + 0.00000 * TWOTH + 0.000000 * TWOTHSQ EXTINCTION PARAMETER = 0.000000 The Laue symmetry is: M3M

***CODING OF VARIABLES*** ATOM X Y Z B N B11 B22 B33 B12 B13 B23 MG 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 O 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00

***** PHASE INFORMATION CODEWORDS ***** OVERALL SCALE FACTOR = 0.00 OVERALL TEMP. FACTOR = 0.00 CELL CONSTANTS = 71.00 71.00 71.00 0.00 0.00 0.00

*** HISTROGRAM 1 CODEWORDS *** PREFERRED ORIENTATION PARAMETER = 0.00 ABSORPTION R/Po PARAMETER = 0.00 ASYMMETRY PARAMETERS = 91.00 0.00 GAUSSIAN COMPONENT = 61.00 0.00 0.00 ANISOTROPIC = 0.00 LORENZTIAN COMPONENTS = 81.00 0.00 0.00 EXTINCTION = 0.00

FORMFACTORS FOR HISTOGRAM FOR MG DFP= 0.171900 DFPP= 0.177100 COEFFICIENTS= 5.420400 2.827500 2.173500 79.261101 1.226900 0.380800 2.307300 7.193700 0.858400 FOR O DFP= 0.049200 DFPP= 0.032200 COEFFICIENTS= 3.048500 13.277100 2.286800 5.701100 1.546300 0.323900 0.867000 32.908901 0.250800 LAUE SYMMETRY M3M WILL BE USED TO GENERATE INDICES ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++

CYCLE NUMBER= 1

PHASE 1: periclase #1000053 NEW PARAMETERS, SHIFTS, AND STANDARD DEVIATIONS=

ATOM X DX SX Y DY SY Z DZ SZ B DB SB N DN SN MG 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.6000 0.0000 0.0000 0.0208 0.0000 0.0000 O 0.00005 0.00000 0.00000 0.00005 0.00000 0.00000 0.00005 0.00000 0.00000 0.6000 0.0000 0.0000 0.1667 0.0000 0.0000 ATOM B11 DB11 SB11 B22 DB22 SB22 B33 DB33 SB33 B12 DB12 SB12 B13 DB13 SB13 B23 DB23 SB23 MG 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 O 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000

+----------------------------------------------------+| Phase: 1 |+----------------------------------------------------+ PHASE SCALE FACTOR = 0.100000E-01 0.000000 0.000000 OVERALL TEMP. FACTOR = 0.000000 0.000000 0.000000 CELL PARAMETERS = 4.222899 0.000999 0.001331 4.222899 0.000999 0.001331 4.222899 0.000999 0.001331 90.000008 0.000008 0.000000 90.000008 0.000008 0.000000 90.000008 0.000008 0.000000 RECIPROCAL CELL = 0.237 0.237 0.237 90.000 90.000 90.000 CELL VOLUME = 75.306458 0.041110 SCALE * VOLUME = 0.753065 0.000411 MOLECULAR WEIGHT = 609.235 DENSITY = 13.428 ABSOLUTE PHASE VALUES: INC = NEUTRONS ON SAMPLE/CM^2 ( in cm^-2) MASS = MASS OF PHASE IN BEAM (in g) ls/R = RATIO OF DETECTOR HEIGHT TO SAMPLE-DETECTOR Then: INC*MASS*ls/R = 261752.

+----------------------------------------------------+| Histogram: 1 |+----------------------------------------------------+ SCALE FACTOR = 1.0000 0.00000 0.00000 ZEROPOINT = 0.00000 0.00000 0.00000

BACKGROUND PARAMETER B 0 = 9742.17 180.932 1480.16 BACKGROUND PARAMETER B 1 = -506.925 -10.5548 72.7733 BACKGROUND PARAMETER B 2 = 9.70110 0.240807 1.38914 BACKGROUND PARAMETER B 3 = -0.613680E-01 -0.183596E-02 0.892300E-02 BACKGROUND PARAMETER B 5 = -59228.7 -1028.27 9818.07 PREFERRED ORIENTATION = 1.00000 0.00000 0.00000 ABSORPTION R = 0.00000 0.00000 0.00000 ASYMMETRY PARAMETERS = 0.04888 0.02888 0.02881 0.00000 0.00000 0.00000 HALFWIDTH PARAMETERS U = 0.278500 0.183500 0.018791 V = -0.005000 0.000000 0.000000 W = 0.020000 0.000000 0.000000 ANISOTROPIC GAUSSIAN BROADENING = 0.000000 0.000000 0.000000 PEAK SHAPE PARAMETER Gam0 = 1.716885 -0.223915 0.046657 PEAK SHAPE PARAMETER Gam1 = 0.000000 0.000000 0.000000 PEAK SHAPE PARAMETER Gam2 = 0.000000 0.000000 0.000000 EXTINCTION PARAMETER = 0.000000 0.000000 0.000000

+------------------------------------------------------------------------+| Hist | Rp | Rwp | Rexp |Durbin Unwght| Durbin Wght | N-P |+------------------------------------------------------------------------+| 1 |1212.68 |3591.14 | 10.29 | 0.008 | 0.009 | 3491 |+------------------------------------------------------------------------+| SUMYDIF | SUMYOBS | SUMYCALC | SUMWYOBSSQ | GOF | CONDITION |+------------------------------------------------------------------------+| 0.3999E+07| 0.3297E+06| 0.3221E+07| 0.3297E+06| 0.1218E+06| 0.9946E+18 |+------------------------------------------------------------------------+

CORRELATION MATRIX= 1 2 3 4 5 6 7 8 9 1 100 -98 97 -93 -98 5 0 0 0 2 -98 100 -98 97 96 -5 0 1 0 3 97 -98 100 -98 -92 6 0 -1 0 4 -93 97 -98 100 89 -5 0 2 0 5 -98 96 -92 89 100 -4 0 1 0 6 5 -5 6 -5 -4 100 -19 -79 -21 7 0 0 0 0 0 -19 100 11 95 8 0 1 -1 2 1 -79 11 100 13 9 0 0 0 0 0 -21 95 13 100 AVERAGE INTENSITY DIFFERENCE FOR PATTERN, GIVEN FOR BLOCKS OF 20 OBSERVATIONS. 1 299.9 2 210.1 3 135.1 4 72.8 5 19.2 6 -25.4 7 -60.6 8 -90.5 9 -99.9 10 -99.9 11 -99.9 12 -99.9 13 -99.9 14 -99.9 15 -99.9 16 -99.9 17 -99.9 18 -99.9 19 -99.9 20 -99.9 21 -96.2 22 -81.0 23 -64.2 24 -48.1 25 -31.9 26 -14.0 27 3.8 28 23.0 29 40.3 30 60.6 31 78.3 32 97.3 33 115.6 34 133.8 35 151.3 36 169.9 37 187.3 38 202.9 39 221.5 40 237.6 41 253.6 42 266.8 43 283.4 44 299.5 45 310.9 46 326.2 47 337.5 48 349.2 49 359.6 50 371.8 51 382.0 52 392.0 53 399.9 54 408.9 55 417.3 56 424.7 57 430.6 58 437.5 59 442.2 60 445.8 61 452.5 62 456.5 63 461.3 64 465.1 65 -99.9 66 -99.9 67 -99.9 68 -99.9 69 -99.9 70 -99.9 71 133.7 72 459.6 73 459.6 74 454.2 75 450.6 76 455.1 77 452.3 78 456.9 79 376.9 80 -99.9 81 -99.9 82 -99.9 83 -99.9 84 -99.9 85 -99.9 86 198.9 87 388.2 88 371.0 89 359.1 90 347.8 91 332.5 92 323.4 93 312.1 94 300.5 95 291.4 96 280.7 97 268.6 98 258.8 99 248.8 100 237.4 101 225.3 102 216.1 103 205.0 104 193.9 105 184.6 106 173.9 107 163.6 108 151.0 109 142.2 110 132.4 111 123.3 112 116.2 113 106.4 114 96.4 115 86.8 116 79.8 117 70.5 118 63.6 119 58.5 120 48.7 121 42.0 122 39.2 123 33.9 124 27.2 125 28.6 126 27.3 127 -99.9 128 -99.9 129 -99.9 130 -99.9 131 -99.9 132 -99.9 133 -99.9 134 -99.9 135 -99.9 136 7.2 137 5.2 138 6.1 139 7.1 140 11.2 141 15.0 142 18.5 143 26.5 144 31.7 145 40.9 146 51.1 147 58.2 148 68.8 149 81.8 150 94.7 151 108.6 152 124.7 153 140.7 154 156.3 155 176.0 156 196.2 157 143.5 158 -59.0 159 -99.9 160 -99.9 161 -99.9 162 -99.9 163 -99.9 164 -99.9 165 -39.3 166 215.7 167 418.2 168 442.6 169 410.1 170 205.5 171 -99.9 172 -99.9 173 95.3 174 540.6 175 703.6 176 682.2 NO. CODE H K L HW SHAPE POSN ICALC COBS DIFF ESD

1 1 1 1 1 0.170 1.941 36.842 1508716. 8554.-1500161.9 83.1 2 2 1 1 1 0.170 1.941 36.937 750111. 4540. -745571.6 62.7 3 1 0 0 2 0.181 1.941 42.801 666704. 97953. -568750.6 310.2 4 2 0 0 2 0.181 1.941 42.912 331413. 44619. -286793.8 145.8 5 1 0 2 2 0.227 1.941 62.132 304059. 68158. -235900.7 226.5 6 2 0 2 2 0.227 1.941 62.303 151108. 33045. -118063.1 114.2 7 1 1 1 3 0.267 1.941 74.471 289181. 14526. -274655.7 380.0 8 2 1 1 3 0.267 1.941 74.687 143823. 7491. -136332.5 252.1 9 1 2 2 2 0.281 1.941 78.396 79094. 37069. -42025.1 687.1 10 2 2 2 2 0.282 1.941 78.628 39357. 20671. -18686.4 468.6 DERIVED BRAGG R-FACTOR= 1166.56