Supporting Information
Wiley-VCH 2010
69451 Weinheim, Germany
The Structures of d-PdCl2 and g-PdCl2 : Phases with Negative Thermal
Expansion in One Direction**
Jrgen Evers,* Wolfgang Beck, Michael Gbel, Stefanie Jakob, Peter Mayer, Gilbert Oehlinger,
Marianne Rotter, and Thomas M. Klaptke
ange_201000680_sm_miscellaneous_information.pdf
1
Tabelle S1.
Abstände (Å) und Winkel (°) für die monokline Hochtemperatur-Phase dPdCl2.
T(K)
793
gleicher Strang:
Pd(1)-Cl(1) 4x
Pd(2)-Cl(2) 4x
2.35(2)
2.35(2)
Cl(1)-Cl(1) 2x
Cl(2)-Cl(2) 2x
3.29(1)
3.29(1)
Cl(1)-Cl(1) 1x
Cl(2)-Cl(2) 1x
3.36(3)
3.36(3)
Pd(1)-Pd(1) 2x
Pd(2)-Pd(2) 2x
3.29(1)
3.29(1)
Cl(1)Pd(1)Cl(1)
Cl(2)Pd(2)Cl(2)
89(1), 91(1)
89(1), 91(1)
Cl(1)-Cl(2) 2x
Cl(2)-Cl(1) 2x
3.71(3)
3.71(3)
Cl(1)-Cl(2) 2x
Cl(2)-Cl(1) 2x
3.78(3)
3.78(3)
Nachbarstrang:
Cl(1)-Cl(1) 1x
3.79(3)
Pd(1)-Cl(1) 4x
3.89(3)
Tabelle S2.
Abstände (Å) und Winkel (°) für die monokline Tieftemperatur-Phase ?PdCl2.
T(K)
300
Quadrate:
Pd-Cl
2.30(1) 2x, 2.32(1) 2x
Cl-Cl
3.21(1) 2x, 3.32(1) 2x
ClPdCl
88.0(1) 2x, 92.1(1) 2x
Verknüpfung Quadrate:
PdClPd
108.3(1)
Pd-Cl
3.55(2) 2x, 3.60(2) 2x
Cl-Cl
3.57(2),
3.62(2) 2x
Cl-Cl
3.63(2),
3.86(2) 2x
2
Pd-Pd
(a)
3.74(2) 4x, 3.86(2) 2x
3
(b)
(c)
Abbildung S1.
Rietveld-Plots mit dem Progamm FullProf
[18]
der Guinier-Diffraktogramme von (a) a-
PdCl2 bei 480°C, (b) d-PdCl2 bei 520°C und (c) ?-PdCl2 bei 300 K. Für (a) und für (b)
wurde monochromatische MoKa1-Strahlung (?=0.7093 Å) verwendet, für (c) monochromatische CuKa1-Strahlung (?=1.54056 Å). Gezeigt sind die Messpunkte als rote
4
Quadrate, das berechnete Diffraktogramm als schwarze, die Differenz als blaue Linie.
Die berechneten Winkel-Lagen der Reflexe sind als grüne Striche dargestellt. Die
Richtigkeitskoeffizienten betragen für (a) R=0.0662 und Rp=0.0865, für (b) R=0.0695
und Rp=0.0879, für (c) R=0.
FullProf-out-Files für drei Guinier-Diffraktogramme:
1) a-PdCl2 bei 480oC
2) d-PdCl2 bei 520oC
3) ?-PdCl2 bei 300 K
*********************************
1) a-PdCl2 bei 480oC
**********************************************************
** PROGRAM FullProf.2k (Version 1.9c - May2001-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: 14/10/2009 Time: 22:20:33.442
=> PCR file code: ALFA_P6C480
=> DAT file code: ALFA_P6C480
-> Relative contribution: 1.0000
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
++++++++++++++++++++++++++++++++++++
=> CYCLE No.:
1
--------------------------------------------------------------------------------------=> Phase 1 Name: PdCl2 OEH 480grad C
--------------------------------------------------------------------------------------=> New parameters, shifts, and standard deviations
Atom
PD
x
dx
sx
y
dy
sy
z
dz
sz
B
dB
sB
occ.
docc. socc.
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.50000 0.00000 0.00000 6.77672-0.00087 0.24587
0.50000 0.00000 0.00000
5
CL
0.15656-0.00036 0.00356 0.13056 0.00009 0.00109 0.00000 0.00000 0.00000 9.30719 0.04739 0.61433
1.00000 0.00000 0.00000
=> Distance constraints:
(PD - CL ):
Dobs
Dcalc diff/sigma
2.32000 2.32438
-0.43781
=> Slack Constraints(dist):
Sum{W(Dobs-Dcal)**2}/ 1 =
1.07
SM=Chi2*Sum{W(Dobs-Dcal)**2} =
S2=
SM/S2 =
0.00146
6.02
Sum{w(yobs-ycal)**2} = 0.412E+04
Rms=Sqrt{Sum[Dobs-Dcal]**2/ 1}=
0.0044
==> PROFILE PARAMETERS FOR PATTERN# 1
=> Overall scale factor:
0.000094563 0.000000706 0.000002782
=> Eta(p-Voigt) or m(Pearson VII): 0.555141 -0.000529 0.031277
=> Overall tem. factor: 0.000000 0.000000 0.000000
=> Halfwidth parameters:
0.250000 0.000000 0.000000
0.402006 -0.001185 0.064480
0.048774 0.000166 0.006155
=> Cell parameters:
3.985459 0.000010 0.001353
11.595340 -0.000223 0.006786
3.300237 0.000039 0.001522
90.000000 0.000000 0.000000
90.000000 0.000000 0.000000
90.000000 0.000000 0.000000
=> Preferred orientation:
-0.177063 -0.004963 0.021931
0.000000 0.000000 0.000000
=> Asymmetry parameters:
0.065485 0.000075 0.003074
0.024640 0.000000 0.000000
0.009100 0.000000 0.000000
0.000270 0.000000 0.000000
=> X and Y parameters:
-0.023532 0.000000 0.000000
0.000000 0.000000 0.000000
=> Strain parameters:
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
6
=> Size parameters (G,L):
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
==> GLOBAL PARAMETERS FOR PATTERN# 1
=> Zero-point: 0.0000 0.0000 0.0000
=> Cos( theta)-shift parameter : 0.0000 0.0000 0.0000
=> Sin(2theta)-shift parameter : 0.0000 0.0000 0.0000
==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS FOR PATTERN: 1
=> R-Factors: 8.08
=> Expected :
10.5
Chi2: 5.60
DW-Stat.: 0.4520 Patt#: 1
4.42
=> Deviance :0.404E+04
=> GoF-index: 2.3
1.8071
Dev*: 5.481
Sqrt(Residual/N)
=> N-P+C: 736
=> SumYdif
0.3048E+05
SumYobs
SumYcal
0.3773E+06
SumwYobsSQ Residual
0.3778E+06
0.3773E+06
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 28.1
4123.
25.2
10.6
Condition
0.5176E+12
5.602
=> (Values obtained using Ynet, but true sigma(y))
=> SumYnet, Sum(w Ynet**2):
0.1086E+06
0.6497E+05
=> N-sigma of the GoF: 88.284
==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS FOR PATTERN: 1
=> R-Factors: 8.08
=> Expected :
10.5
Chi2: 5.60
DW-Stat.: 0.4520 Patt#:
4.42
=> Deviance :0.404E+04
=> GoF-index: 2.3
1.8071
Dev*: 5.481
Sqrt(Residual/N)
=> N-P+C: 736
=> SumYdif
0.3048E+05
SumYobs
0.3773E+06
SumYcal
SumwYobsSQ Residual
0.3778E+06
0.3773E+06
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 28.1
=> (Values obtained using Ynet, but true sigma(y))
25.2
4123.
10.6
Condition
0.5176E+12
5.602
7
=> SumYnet, Sum(w Ynet**2):
=> N-sigma of the GoF:
0.1086E+06
0.6497E+05
88.284
=> Global user-weigthed Chi2 (Bragg contrib.):5.60
=> ---------> Pattern# 1
=> Phase: 1
=>
Bragg R-factor: 14.5
=>
RF-factor
: 26.8
-------------------------------------------------------------------------------------------------------------Pattern# 1 Phase No: 1 Phase name: PdCl2 480 grad C
--------------------------------------------------------------------------------------------------------------
No. Code
H K L Mult
Hw
ETA/M
2theta/TOF
Icalc
Iobs
Sigma StrFactor^2
d-hkl
1 1
0 2 0
2 0.272500 0.390089
7.014
1168.1
1144.9
25.461
5945.0625 5.797781
2 1
1 1 0
4 0.298243 0.301030
10.799
1025.8
1042.4
20.530
8048.8286 3.769038
3 1
1 2 0
4 0.308790 0.263389
12.398
143.7
68.6
36.052
1343.6814 3.284316
4 1
0 1 1
4 0.311611 0.253221
12.830
115.6
123.8
9.920
1314.2922 3.174145
5 1
0 4 0
2 0.319541 0.224415
14.054
25.3
15.6
6.850
6 1
1 3 0
4 0.323607 0.209525
14.687
154.3
103.1
34.510
7 1
1 0 1
4 0.332238 0.177674
16.041
66.8
60.5
6.045
8 1
0 3 1
4 0.333545 0.172821
16.247
423.1
450.2
29.377
9 1
1 1 1
8 0.334667 0.168650
16.424
42.4
37.6
4.558
409.5770 2.482904
10 1
1 4 0
4 0.340835 0.145633
17.402
0.7
0.8
0.133
12.3932 2.344331
11 1
1 2 1
8 0.341610 0.142730
17.526
274.2
278.8
12 1
1 3 1
8 0.352232 0.102720
19.226
17.1
36.7
42.420
196.4031 2.123772
13 1
1 5 0
4 0.359399 0.075510
20.382
55.7
73.0
23.078
1280.6307 2.004454
14 1
2 0 0
2 0.360148 0.072656
20.503
16.8
17.3
1.307
1142.0841 1.992725
15 1
2 1 0
4 0.362023 0.065505
20.807
7.7
4.8
16 1
0 6 0
2 0.364126 0.057474
21.149
44.9
40.5
4.508
17 1
1 4 1
8 0.365600 0.051838
21.388
204.7
174.8
25.774
2808.5649 1.911202
18 1
0 5 1
4 0.366564 0.048151
21.545
107.3
91.6
13.578
2815.6040 1.897464
19 1
2 2 0
4 0.367484 0.044626
21.694
50.7
39.2
9.253
20 1
2 3 0
4 0.376099 0.011525
23.101
3.6
0.0
3.046
124.5147 1.771189
21 1
1 6 0
4 0.378752 0.001298
23.536
7.4
4.5
3.286
228.0344 1.738931
22 1
1 5 1
8 0.380937 -0.007140
23.894
8.9
5.9
2.682
149.3451 1.713207
23 1
2 1 1
8 0.383169 -0.015766
24.261
65.8
29.2
16.707
1469.5284 1.687701
24 1
0 0 2
2 0.386582 -0.028980
24.822
23.7
26.6
3.690
2393.3611 1.650099
25 1
2 4 0
4 0.387323 -0.031850
24.944
37.7
37.0
2.747
1479.0272 1.642158
26 1
2 2 1
8 0.387855 -0.033912
25.032
9.9
9.9
1.443
27 1
0 2 2
4 0.392662 -0.052570
25.825
17.8
56.2
121.809
8.113
2.169
518.7910 2.898891
1916.3289 2.774642
1371.2366 2.541860
6625.3833 2.509806
2775.3076 2.327957
247.8576 1.963935
2124.9897 1.932594
1648.4058 1.884519
221.1895 1.636500
850.7755 1.587072
8
28 1
2 3 1
8 0.395357 -0.063048
26.270
26.4
46.0
34.261
618.4449 1.560632
29 1
1 6 1
8 0.397692 -0.072133
26.656
35.0
44.8
12.734
721.7906 1.538430
30 1
1 7 0
4 0.398634 -0.075804
26.812
30.0
38.0
10.133
1198.3824 1.529643
31 1
1 1 2
8 0.400606 -0.083486
27.139
37.1
66.1
52.021
1055.2695 1.511582
32 1
2 5 0
4 0.400626 -0.083561
27.142
2.2
4.0
3.170
33 1
0 7 1
4 0.404115 -0.097169
27.720
5.6
23.1
73.019
240.0339 1.480475
34 1
1 2 2
8 0.404810 -0.099882
27.835
3.8
15.5
47.380
108.1873 1.474465
35 1
2 4 1
8 0.405307 -0.101819
27.918
0.1
0.4
1.083
2.4504 1.470203
36 1
0 8 0
2 0.407766 -0.111422
28.326
15.4
39.2
60.752
1341.1566 1.449445
37 1
0 4 2
4 0.409637 -0.118729
28.636
3.2
7.9
38 1
1 3 2
8 0.411600 -0.126400
28.962
12.5
38.1
77.991
39 1
1 7 1
8 0.415508 -0.141684
29.612
0.8
2.3
4.243
20.7906 1.387815
40 1
2 6 0
4 0.415573 -0.141938
29.623
9.1
25.1
44.639
480.6716 1.387321
41 1
2 5 1
8 0.417319 -0.148773
29.913
14.0
24.6
19.085
398.2865 1.374153
42 1
1 8 0
4 0.418940 -0.155118
30.183
0.1
0.0
0.229
5.1056 1.362158
43 1
1 4 2
8 0.420703 -0.162019
30.476
0.0
0.0
0.221
1.2282 1.349357
44 1
3 1 0
4 0.424899 -0.178455
31.174
2.6
0.0
4.600
198.5184 1.319849
45 1
3 2 0
4 0.428597 -0.192946
31.790
0.0
0.0
0.168
2.4069 1.294924
46 1
2 6 1
8 0.431051 -0.202564
32.199
1.7
0.6
1.407
54.1891 1.278914
47 1
1 5 2
8 0.431824 -0.205592
32.328
7.3
7.7
2.311
250.1895 1.273957
48 1
2 7 0
4 0.431840 -0.205657
32.330
0.2
0.3
0.074
14.7933 1.273852
49 1
2 0 2
4 0.432299 -0.207454
32.407
2.6
3.1
0.850
229.2171 1.270930
50 1
2 1 2
8 0.433496 -0.212148
32.606
0.7
0.8
0.195
27.8281 1.263364
51 1
1 8 1
8 0.434175 -0.214807
32.719
6.0
7.0
1.523
187.3613 1.259120
52 1
3 3 0
4 0.434621 -0.216555
32.793
7.2
8.1
1.556
555.2823 1.256346
53 1
0 6 2
4 0.434853 -0.217467
32.832
5.4
6.0
1.082
368.9865 1.254903
54 1
2 2 2
8 0.437050 -0.226079
33.198
7.2
3.9
2.432
299.9004 1.241452
55 1
3 0 1
4 0.438560 -0.231998
33.450
6.0
0.0
1.469
568.2088 1.232380
56 1
1 9 0
4 0.439649 -0.236264
33.631
5.3
0.0
1.977
335.0659 1.225929
57 1
3 1 1
8 0.439725 -0.236563
33.644
0.0
0.0
0.008
0.8858 1.225479
58 1
3 4 0
4 0.442788 -0.248569
34.154
0.0
0.0
0.000
0.0280 1.207705
59 1
2 3 2
8 0.442853 -0.248822
34.165
0.4
0.0
0.175
15.0219 1.207337
60 1
3 2 1
8 0.443184 -0.250120
34.220
5.2
0.0
2.277
233.5528 1.205449
No. Code
H K L Mult
Hw
ETA/M
2theta/TOF
Icalc
100.8858 1.511406
11.861
Iobs
170.9498 1.434051
366.2618 1.418249
Sigma StrFactor^2
d-hkl
61 1
0 9 1
4 0.444114 -0.253766
34.375
2.3
0.3
0.847
157.1400 1.200177
62 1
1 6 2
8 0.444685 -0.256003
34.470
0.7
0.2
0.290
27.8543 1.196969
63 1
2 7 1
8 0.446226 -0.262040
34.726
8.0
6.4
3.269
295.0856 1.188395
64 1
3 3 1
8 0.448840 -0.272280
35.162
0.0
0.0
0.012
0.4796 1.174143
65 1
2 8 0
4 0.449208 -0.273722
35.223
2.1
2.5
1.374
149.1664 1.172165
66 1
2 4 2
8 0.450746 -0.279745
35.479
6.2
1.3
2.601
268.7573 1.163978
67 1
0 10 0
2 0.451586 -0.283035
35.619
1.0
0.1
0.399
145.1944 1.159556
68 1
3 5 0
4 0.452894 -0.288156
35.836
2.4
0.0
1.066
285.1856 1.152744
9
=> Phase: 1
=> Bragg R-factor: 14.5
=> Rf-factor= 25.0
Vol: 152.513( 0.125) Fract(%): 100.00( 1.05)
ATZ: 354.610
Brindley: 1.0000
2) d-PdCl2 bei 520oC
**********************************************************
** PROGRAM FullProf.2k (Version 1.9c - May2001-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: 08/12/2009 Time: 15:05:59.449
=> PCR file code: DELTA_P6C620
=> DAT file code: DELTA_P6C620
-> Relative contribution: 1.0000
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+++++++++++++++++++++++++++++++++++
……….
………
=> CYCLE No.: 10
--------------------------------------------------------------------------------------=> Phase 1 Name: PdCl2-1 Geheizt Januar 2008
--------------------------------------------------------------------------------------=> New parameters, shifts, and standard deviations
Atom
PD1
x
dx
sx
y
dy
sy
z
dz
sz
B
dB
sB
occ.
docc. socc.
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.50000 0.00000 0.00000 7.68454-0.00264 0.26776
0.25000 0.00000 0.00000
PD2
0.50000 0.00000 0.00000 0.50000 0.00000 0.00000 0.00000 0.00000 0.00000 7.68454-0.00264 0.26776
0.25000 0.00000 0.00000
CL1 -0.15696-0.00019 0.00762 0.12584-0.00003 0.00135 0.00000 0.00000 0.00000 9.45247-0.00080 0.69494
0.50000 0.00000 0.00000
CL2
0.55762-0.00005 0.00573 0.64371 0.00000 0.00012 0.50000 0.00000 0.00000 9.45247-0.00080 0.69494
0.50000 0.00000 0.00000
=> Distance constraints:
Dobs
Dcalc diff/sigma
10
(PD1 - CL1 ):
2.35000 2.35061
-0.60797
(PD2 - CL2 ):
2.35000 2.35093
-0.92912
=> Slack Constraints(dist):
Sum{W(Dobs-Dcal)**2}/ 2 =
2.34
SM=Chi2*Sum{W(Dobs-Dcal)**2} =
S2=
SM/S2 =
0.00639
17.8
Sum{w(yobs-ycal)**2} = 0.278E+04
Rms=Sqrt{Sum[Dobs-Dcal]**2/ 2}=
0.0008
==> PROFILE PARAMETERS FOR PATTERN# 1
=> Overall scale factor:
0.000363670 -0.000000098 0.000008886
=> Eta(p-Voigt) or m(Pearson VII): 0.370770 -0.000070 0.034025
=> Overall tem. factor: 0.000000 0.000000 0.000000
=> Halfwidth parameters:
0.250000 0.000000 0.000000
0.200323 0.000037 0.048667
0.060409 -0.000002 0.005025
=> Cell parameters:
4.011713 0.000000 0.001378
11.781547 0.000000 0.006880
3.287779 -0.000002 0.001337
90.000000 0.000000 0.000000
90.000000 0.000000 0.000000
97.026306 -0.000122 0.033589
=> Preferred orientation:
-0.325253 0.000260 0.020540
0.000000 0.000000 0.000000
=> Asymmetry parameters:
0.056417 -0.000002 0.003119
0.017730 0.000000 0.000000
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
=> X and Y parameters:
-0.023532 0.000000 0.000000
0.000000 0.000000 0.000000
=> Strain parameters:
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
=> Size parameters (G,L):
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
11
==> GLOBAL PARAMETERS FOR PATTERN# 1
=> Zero-point: 0.0000 0.0000 0.0000
=> Cos( theta)-shift parameter : 0.0000 0.0000 0.0000
=> Sin(2theta)-shift parameter : 0.0000 0.0000 0.0000
==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS FOR PATTERN: 1
=> R-Factors: 6.88
=> Expected :
8.78
Chi2: 3.80
DW-Stat.: 0.6243 Patt#: 1
4.50
=> Deviance :0.279E+04
=> GoF-index: 1.9
1.8154
Dev*: 3.805
Sqrt(Residual/N)
=> N-P+C: 733
=> SumYdif
0.2486E+05
SumYobs
SumYcal
0.3613E+06
SumwYobsSQ Residual
0.3605E+06
0.3613E+06
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 28.1
2783.
23.6
12.1
Condition
0.5937E+11
3.796
=> (Values obtained using Ynet, but true sigma(y))
=> SumYnet, Sum(w Ynet**2):
0.8838E+05
0.4989E+05
=> N-sigma of the GoF: 53.531
==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS FOR PATTERN: 1
=> R-Factors: 6.88
=> Expected :
8.78
Chi2: 3.80
DW-Stat.: 0.6243 Patt#:
4.50
=> Deviance :0.279E+04
=> GoF-index: 1.9
1.8154
Dev*: 3.805
Sqrt(Residual/N)
=> N-P+C: 733
=> SumYdif
0.2486E+05
SumYobs
SumYcal
0.3613E+06
SumwYobsSQ Residual
0.3605E+06
0.3613E+06
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 28.1
2783.
23.6
=> (Values obtained using Ynet, but true sigma(y))
=> SumYnet, Sum(w Ynet**2):
=> N-sigma of the GoF:
53.531
0.8838E+05
0.4989E+05
12.1
Condition
0.5937E+11
3.796
12
=> Global user-weigthed Chi2 (Bragg contrib.):3.80
=> ---------> Pattern# 1
=> Phase: 1
=>
Bragg R-factor: 16.3
=>
RF-factor
: 28.5
-------------------------------------------------------------------------------------------------------------Pattern# 1 Phase No: 1 Phase name: PdCl2-1 Geheizt Januar 2008
--------------------------------------------------------------------------------------------------------------
No. Code
H K L Mult
Hw
ETA/M
2theta/TOF
Icalc
Iobs
1043.2
Sigma StrFactor^2
1 1
0 2 0
2 0.271120 0.207096
6.955
1040.8
2 1
1 0 0
2 0.283411 0.130261
10.221
4.1
3 1
-1 1 0
2 0.284042 0.126357
10.386
366.5
4 1
0 3 0
2 0.284250 0.125070
10.441
1.9
5 1
1 1 0
2 0.287129 0.107318
11.195
483.6
427.3
6 1
-1 2 0
2 0.288851 0.096738
11.645
23.6
5.4
7 1
0 0 1
2 0.291695 0.079327
12.385
0.0
0.0
8 1
0 1 1
4 0.293555 0.067978
12.867
83.2
84.6
4.562
320.1743 3.165049
9 1
1 2 0
2 0.294305 0.063413
13.061
35.8
12.7
8.648
212.7785 3.118238
10 1
-1 3 0
2 0.296790 0.048327
13.702
30.0
9.0
7.102
190.4161 2.972994
11 1
0 4 0
2 0.297700 0.042815
13.937
25.7
13.2
7.068
134.2816 2.923266
12 1
0 2 1
4 0.298794 0.036198
14.218
1.2
0.0
1.635
4.6291 2.865737
13 1
1 3 0
2 0.303827 0.005912
15.505
55.4
77.0
30.331
425.1183 2.629135
14 1
1 0 1
4 0.306101 -0.007699
16.083
28.4
35.2
8.437
205.6395 2.535177
15 1
-1 1 1
4 0.306522 -0.010211
16.190
11.4
12.7
1.395
79.1455 2.518568
16 1
0 3 1
4 0.306661 -0.011045
16.225
356.0
390.4
38.166
1623.5674 2.513107
17 1
-1 4 0
2 0.306813 -0.011948
16.264
1.8
1.9
0.174
14.6943 2.507215
18 1
1 1 1
4 0.308633 -0.022793
16.725
4.6
4.8
1.105
29.9894 2.438593
19 1
-1 2 1
4 0.309846 -0.030009
17.031
150.0
20 1
0 5 0
2 0.311488 -0.039748
17.445
1.7
10.1
50.181
13.9702 2.338613
21 1
1 2 1
4 0.313842 -0.053673
18.037
74.0
92.3
23.458
484.6303 2.262491
22 1
1 4 0
2 0.314905 -0.059942
18.303
0.1
0.2
0.538
0.5251 2.229832
23 1
-1 3 1
4 0.315731 -0.064808
18.510
0.6
8.8
131.082
3.7324 2.205137
24 1
0 4 1
4 0.316433 -0.068936
18.685
0.1
1.8
30.566
0.5572 2.184614
25 1
-1 5 0
2 0.318236 -0.079525
19.135
37.2
46.9
13.456
411.5732 2.133706
26 1
1 3 1
4 0.321278 -0.097324
19.892
7.5
44.5
219.680
54.1661 2.053342
27 1
-2 1 0
2 0.323296 -0.109087
20.392
5.4
7.7
3.338
28 1
-1 4 1
4 0.323708 -0.111485
20.494
115.7
115.8
29 1
2 0 0
2 0.323829 -0.112188
20.523
22.1
20.7
1.515
505.4344 1.990792
30 1
-2 2 0
2 0.325190 -0.120094
20.859
13.8
10.8
2.527
300.0277 1.959078
3.4
329.7
1.6
182.3
12.473
d-hkl
0.658
33.907
0.222
50.283
1352.4030 5.846532
22.9436 3.981585
1923.4381 3.918155
5.4803 3.897688
2470.0010 3.635805
5.365
123.5977 3.495888
0.000
0.0000 3.287782
39.738
4.143
964.3449 2.395006
130.9194 2.003522
867.8495 1.993664
13
31 1
0 6 0
2 0.325639 -0.122700
20.970
46.2
38.0
32 1
2 1 0
2 0.326752 -0.129147
21.244
0.3
0.2
33 1
1 5 0
2 0.327084 -0.131069
21.326
16.0
13.9
2.034
216.7592 1.916710
34 1
0 5 1
4 0.327592 -0.134005
21.451
79.9
82.1
4.999
572.2682 1.905691
35 1
-2 3 0
2 0.329382 -0.144344
21.890
0.0
0.0
0.001
0.0456 1.867895
36 1
1 4 1
4 0.330484 -0.150692
22.160
71.8
40.9
18.229
602.8572 1.845435
37 1
-1 6 0
2 0.330674 -0.151784
22.206
0.5
0.3
0.120
6.9403 1.841628
38 1
2 2 0
2 0.331875 -0.158692
22.500
15.7
13.4
39 1
-1 5 1
4 0.333342 -0.167109
22.857
1.5
4.3
9.885
13.3671 1.789826
40 1
-2 4 0
2 0.335626 -0.180177
23.413
9.0
7.6
4.909
196.2210 1.747944
41 1
-2 1 1
4 0.337750 -0.192286
23.927
14.5
16.5
42 1
2 0 1
4 0.338219 -0.194953
24.041
1.5
1.1
0.467
24.4925 1.702935
43 1
2 3 0
2 0.338926 -0.198971
24.211
2.9
0.4
1.073
64.7131 1.691101
44 1
-2 2 1
4 0.339418 -0.201771
24.330
2.3
0.0
0.808
34.5634 1.682957
45 1
0 6 1
4 0.339816 -0.204025
24.426
0.7
0.0
0.228
6.6874 1.676456
46 1
1 6 0
2 0.340118 -0.205743
24.499
2.8
0.5
0.819
49.8016 1.671535
47 1
0 7 0
2 0.340186 -0.206128
24.515
0.1
0.0
0.022
1.2249 1.670438
48 1
2 1 1
4 0.340801 -0.209614
24.664
12.6
7.1
3.773
189.2948 1.660560
49 1
1 5 1
4 0.341096 -0.211284
24.735
2.2
1.3
0.625
22.0442 1.655869
50 1
0 0 2
2 0.341857 -0.215593
24.918
13.5
5.6
3.848
521.5826 1.643891
51 1
0 1 2
4 0.342894 -0.221453
25.167
0.0
0.0
0.001
0.1087 1.627882
52 1
-2 3 1
4 0.343143 -0.222859
25.226
20.6
17.4
53 1
-2 5 0
2 0.343634 -0.225630
25.344
1.9
1.6
54 1
-1 7 0
2 0.343923 -0.227259
25.413
24.5
19.7
55 1
-1 6 1
4 0.344299 -0.229379
25.504
8.8
6.7
1.839
92.7088 1.606733
56 1
2 2 1
4 0.345377 -0.235452
25.762
2.9
2.1
0.833
42.0565 1.590905
57 1
0 2 2
4 0.345958 -0.238718
25.900
10.1
9.6
2.729
164.3819 1.582525
58 1
2 4 0
2 0.347617 -0.248030
26.296
7.1
26.8
75.404
176.8767 1.559119
59 1
-2 4 1
4 0.348764 -0.254455
26.569
1.5
19.5
233.994
22.5266 1.543382
60 1
1 0 2
4 0.350557 -0.264476
26.995
0.1
0.3
0.904
No. Code
H K L Mult
Hw
ETA/M
2theta/TOF
Icalc
7.440
0.051
5.9506 1.923996
3.763
4.045
3.357
0.296
333.1857 1.817903
246.8963 1.710882
304.0077 1.624088
44.8389 1.616664
4.421
Iobs
557.8991 1.948844
467.2559 1.612334
1.6027 1.519476
Sigma StrFactor^2
d-hkl
61 1
-1 1 2
4 0.350832 -0.266013
27.060
10.2
29.8
57.686
214.8586 1.515877
62 1
0 3 2
4 0.350924 -0.266524
27.082
0.0
0.1
0.107
0.3862 1.514684
63 1
2 3 1
4 0.351765 -0.271212
27.281
10.1
15.0
7.433
153.9279 1.503831
64 1
1 1 2
4 0.352231 -0.273804
27.391
13.3
16.4
3.979
264.5457 1.497898
65 1
1 6 1
4 0.352855 -0.277278
27.539
11.6
12.0
1.152
140.1282 1.490021
66 1
0 7 1
4 0.352917 -0.277623
27.554
3.8
3.9
0.366
43.2331 1.489244
67 1
-1 2 2
4 0.353047 -0.278343
27.584
0.5
0.5
0.046
9.1533 1.487625
68 1
-2 6 0
2 0.353137 -0.278845
27.606
8.1
8.2
0.811
217.3684 1.486497
69 1
1 7 0
2 0.353884 -0.282994
27.782
8.8
9.8
1.715
199.6950 1.477248
70 1
0 8 0
2 0.355169 -0.290120
28.085
11.9
12.2
71 1
1 2 2
4 0.355792 -0.293575
28.232
0.9
0.8
2.188
0.197
263.9078 1.461633
16.7281 1.454187
14
72 1
-2 5 1
4 0.356082 -0.295175
28.300
7.5
6.4
2.103
118.6943 1.450762
73 1
-1 7 1
4 0.356347 -0.296646
28.362
0.0
0.0
0.000
0.0049 1.447631
74 1
-1 3 2
4 0.357120 -0.300918
28.544
2.1
3.0
1.856
39.5425 1.438613
75 1
0 4 2
4 0.357618 -0.303669
28.660
1.9
5.8
12.377
31.7047 1.432868
76 1
2 5 0
2 0.357701 -0.304126
28.680
0.2
0.8
1.993
6.5025 1.431918
77 1
-1 8 0
2 0.357882 -0.305122
28.722
0.0
0.1
0.525
0.8149 1.429851
78 1
2 4 1
4 0.359760 -0.315471
29.162
0.2
2.5
24.272
3.9111 1.408745
79 1
1 3 2
4 0.361125 -0.322968
29.481
3.5
17.9
75.106
65.8241 1.393854
80 1
-1 4 2
4 0.362925 -0.332836
29.900
0.1
0.6
5.349
1.3215 1.374741
81 1
-2 7 0
2 0.363917 -0.338260
30.130
0.0
0.0
0.244
1.1168 1.364465
82 1
-2 6 1
4 0.364896 -0.343608
30.358
0.3
0.0
1.678
4.9067 1.354488
83 1
1 7 1
4 0.365594 -0.347414
30.519
0.4
1.1
2.302
6.4654 1.347479
84 1
0 5 2
4 0.365856 -0.348841
30.580
0.1
0.2
0.393
1.3174 1.344871
85 1
-3 1 0
2 0.366634 -0.353079
30.760
1.5
2.9
3.852
91.0166 1.337185
86 1
0 8 1
4 0.366796 -0.353961
30.798
0.1
0.1
0.145
0.8775 1.335597
87 1
-3 2 0
2 0.367385 -0.357165
30.934
0.1
0.1
0.165
4.3702 1.329861
88 1
3 0 0
2 0.367661 -0.358664
30.998
0.2
0.1
0.375
10.5251 1.327195
89 1
1 4 2
4 0.368079 -0.360933
31.094
0.0
0.0
0.004
0.0512 1.323181
90 1
1 8 0
2 0.368325 -0.362270
31.151
0.0
0.0
0.020
0.5115 1.320827
91 1
2 6 0
2 0.368985 -0.365849
31.303
2.4
0.0
0.992
78.6858 1.314568
92 1
2 5 1
4 0.369172 -0.366860
31.346
4.0
0.4
1.386
72.1827 1.312811
93 1
-1 8 1
4 0.369342 -0.367780
31.385
2.2
0.5
0.736
33.2975 1.311218
94 1
-3 3 0
2 0.369895 -0.370777
31.512
1.8
1.3
0.704
94.2242 1.306052
95 1
-1 5 2
4 0.370308 -0.373012
31.607
3.1
3.9
1.923
61.9730 1.302226
96 1
3 1 0
2 0.370440 -0.373723
31.637
0.8
1.2
0.831
41.8013 1.301014
97 1
0 9 0
2 0.370634 -0.374773
31.682
0.1
0.3
0.275
3.8678 1.299229
98 1
-1 9 0
2 0.372510 -0.384905
32.113
2.0
7.0
18.093
61.2943 1.282259
99 1
-2 1 2
4 0.373804 -0.391871
32.409
0.4
0.7
0.537
13.7726 1.270856
100 1
-3 4 0
2 0.374099 -0.393458
32.476
0.2
0.3
0.171
12.0619 1.268287
101 1
2 0 2
4 0.374180 -0.393891
32.495
2.3
2.7
1.492
73.3108 1.267588
102 1
3 2 0
2 0.374899 -0.397758
32.659
0.1
0.1
0.038
4.8557 1.261384
103 1
-2 7 1
4 0.375032 -0.398471
32.689
1.7
2.0
0.707
31.7465 1.260246
104 1
-2 2 2
4 0.375145 -0.399075
32.715
1.6
2.0
0.758
47.2760 1.259284
105 1
0 6 2
4 0.375465 -0.400795
32.788
4.1
5.8
2.743
79.8509 1.256554
106 1
-2 8 0
2 0.375813 -0.402660
32.867
2.1
3.2
1.843
74.3763 1.253607
107 1
2 1 2
4 0.376263 -0.405071
32.970
0.0
0.0
0.031
0.6442 1.249818
108 1
1 5 2
4 0.376502 -0.406353
33.024
1.7
3.2
3.193
36.1042 1.247814
109 1
-3 1 1
4 0.377607 -0.412265
33.275
0.3
0.7
1.061
10.2564 1.238657
110 1
-2 3 2
4 0.378171 -0.415277
33.403
0.0
0.0
0.000
0.0050 1.234044
111 1
-3 2 1
4 0.378320 -0.416075
33.437
1.2
1.9
1.537
38.6828 1.232829
112 1
3 0 1
4 0.378582 -0.417474
33.497
2.0
2.7
1.537
65.3526 1.230704
113 1
-1 6 2
4 0.379119 -0.420336
33.618
0.0
0.0
0.018
0.7748 1.226379
114 1
1 8 1
4 0.379213 -0.420839
33.640
1.8
1.6
0.899
31.7866 1.225621
115 1
2 6 1
4 0.379841 -0.424183
33.782
0.5
0.4
0.267
10.4628 1.220615
15
116 1
-3 5 0
2 0.379904 -0.424519
33.796
0.9
0.8
0.469
45.4706 1.220115
117 1
2 2 2
4 0.380007 -0.425069
33.819
1.8
1.6
0.968
51.2202 1.219297
118 1
-3 3 1
4 0.380706 -0.428789
33.978
0.0
0.0
0.023
1.0715 1.213789
119 1
3 3 0
2 0.380943 -0.430049
34.031
0.9
0.4
0.670
47.7775 1.211935
120 1
3 1 1
4 0.381224 -0.431546
34.095
0.0
0.0
0.002
0.0614 1.209742
No. Code
H K L Mult
Hw
ETA/M
2theta/TOF
Icalc
Iobs
Sigma StrFactor^2
d-hkl
121 1
2 7 0
2 0.381333 -0.432126
34.119
0.2
0.0
0.141
7.0325 1.208894
122 1
0 9 1
4 0.381409 -0.432528
34.136
2.1
0.0
1.695
37.5423 1.208307
123 1
-2 4 2
4 0.382817 -0.440001
34.454
1.2
0.0
1.271
32.5677 1.197503
124 1
-1 9 1
4 0.383198 -0.442019
34.540
0.0
0.0
0.016
0.2714 1.194619
125 1
1 9 0
2 0.383433 -0.443261
34.593
1.4
0.0
1.581
50.5171 1.192852
126 1
-3 4 1
4 0.384715 -0.450044
34.881
1.3
0.9
1.270
36.8478 1.183297
127 1
2 3 2
4 0.385335 -0.453318
35.020
0.3
0.2
0.267
7.6552 1.178743
128 1
3 2 1
4 0.385480 -0.454083
35.052
1.9
0.8
1.844
54.1642 1.177684
129 1
1 6 2
4 0.386255 -0.458172
35.226
0.3
0.0
0.507
5.9363 1.172058
130 1
0 7 2
4 0.386307 -0.458448
35.238
0.0
0.0
0.014
0.1461 1.171679
131 1
-2 8 1
4 0.386353 -0.458691
35.248
0.2
0.0
0.422
4.0830 1.171348
132 1
0 10 0
2 0.386637 -0.460186
35.312
0.6
0.2
1.901
21.8962 1.169307
133 1
-3 6 0
2 0.387198 -0.463141
35.437
0.0
0.0
0.051
0.5471 1.165296
134 1
-1 10 0
2 0.387807 -0.466345
35.573
0.0
0.0
0.005
0.0354 1.160979
135 1
3 4 0
2 0.388459 -0.469770
35.719
0.0
0.0
0.092
1.8358 1.156401
136 1
-2 9 0
2 0.388719 -0.471135
35.777
0.1
0.0
0.144
3.5106 1.154588
137 1
-2 5 2
4 0.388997 -0.472591
35.839
0.1
0.0
0.188
5.4603 1.152660
138 1
-1 7 2
4 0.389224 -0.473782
35.890
1.8
0.0
1.708
69.3150 1.151087
=> Phase: 1
=> Bragg R-factor: 16.3
=> Rf-factor= 26.4
Vol: 154.227( 0.122) Fract(%): 100.00( 3.46)
ATZ: 354.610
Brindley: 1.0000
3) ?-PdCl2 bei 300 K
**********************************************************
** PROGRAM FullProf.2k (Version 3.20 - Feb2005-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: 09/03/2010 Time: 10:17:30.046
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+++++++++++++++++++++++++++
=> CYCLE No.: 10
--------------------------------------------------------------------------------------=> Phase 1 Name: PdCl2 STREM Gunier CuKa1
--------------------------------------------------------------------------------------=> New parameters, shifts, and standard deviations
16
Atom
x
dx
sx
y
dy
sy
z
dz
sz
B
dB
sB
occ. docc. socc.
PD1
0.00000 0.00000 0.00000 0.50000 0.00000 0.00000 0.00000 0.00000 0.00000 0.65234 0.00135 0.02768 0.34700
0.00000 0.00000
PD2
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.65234 0.00135 0.02768 0.15362
0.00000 0.00000
CL1
0.25498 0.00006 0.00035 0.25731 0.00012 0.00065 0.81406 0.00000 0.00069 1.34288 0.00411 0.04797 1.02915
0.00000 0.00000
==> PROFILE PARAMETERS FOR PATTERN# 1
=> Overall scale factor:
0.023515712
0.000005232
0.000153167
=> Eta(p-Voigt) or m(Pearson VII): 0.701643 -0.000451 0.007475
=> Overall tem. factor: 0.000000 0.000000 0.000000
=> Halfwidth parameters:
0.250000 0.000000 0.000000
0.075820 0.000141 0.004380
0.024864 0.000005 0.000841
=> Cell parameters:
5.549611 0.000001 0.000292
3.860778 -0.000007 0.000151
6.410491 -0.000018 0.000299
90.000000 0.000000 0.000000
107.150993 -0.000038 0.002487
90.000000 0.000000 0.000000
=> Preferred orientation:
-0.007832 -0.000006 0.002592
0.000000 0.000000 0.000000
=> Asymmetry parameters:
-0.006133 -0.000262 0.002436
0.041230 0.000000 0.000000
0.205250 0.000000 0.000000
0.000820 0.000000 0.000000
=> X and Y parameters:
-0.000049 0.000000 0.000000
0.000000 0.000000 0.000000
=> Strain parameters:
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
=> Size parameters (G,L):
0.000000 0.000000 0.000000
0.000000 0.000000 0.000000
==> GLOBAL PARAMETERS FOR PATTERN# 1
=> Zero-point:
0.0820 -0.0001 0.0016
=> Cos( theta)-shift parameter : 0.0000 0.0000 0.0000
=> Sin(2theta)-shift parameter : 0.0000 0.0000 0.0000
==> RELIABILITY FACTORS WITH ALL NON-EXCLUDED POINTS FOR PATTERN: 1
17
=> R-Factors: 5.84
=> Expected :
8.18
Chi2: 22.7
1.72
1.9546
=> Deviance :0.422E+06
=> GoF-index: 4.8
DW-Stat.: 0.0137 Patt#: 1
Dev*: 24.54
Sqrt(Residual/N)
=> N-P+C: 17185
=> SumYdif
SumYobs
SumYcal
SumwYobsSQ Residual
Condition
0.3413E+07 0.5840E+08 0.5785E+08 0.5840E+08 0.3907E+06 0.2162E+10
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 27.7
24.6
5.16
22.73
=> (Values obtained using Ynet, but true sigma(y))
=> SumYnet, Sum(w Ynet**2):
0.1232E+08 0.6446E+07
=> N-sigma of the GoF: 2014.724
==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS FOR PATTERN: 1
=> R-Factors: 5.84
=> Expected :
8.18
Chi2: 22.7
1.72
1.9546
=> Deviance :0.422E+06
=> GoF-index: 4.8
DW-Stat.: 0.0137 Patt#:
Dev*: 24.54
Sqrt(Residual/N)
=> N-P+C: 17185
=> SumYdif
SumYobs
SumYcal
SumwYobsSQ Residual
Condition
0.3413E+07 0.5840E+08 0.5785E+08 0.5840E+08 0.3907E+06 0.2162E+10
=> Conventional Rietveld Rp,Rwp,Re and Chi2: 27.7
24.6
5.16
22.73
=> (Values obtained using Ynet, but true sigma(y))
=> SumYnet, Sum(w Ynet**2):
=> N-sigma of the GoF:
0.1232E+08 0.6446E+07
2014.724
=> Global user-weigthed Chi2 (Bragg contrib.): 22.7
=> ---------> Pattern# 1
=> Phase: 1
=> Bragg R-factor: 12.5
=> RF-factor
: 12.8
-------------------------------------------------------------------------------------------------------------Pattern# 1 Phase No: 1 Phase name: PdCl2 STREM Gunier CuKa1
--------------------------------------------------------------------------------------------------------------
No. Code
1 1
H K L Mult
1 0 0
Hw
ETA/M 2theta/TOF
2 0.203367 0.700824
Icalc
Iobs
Sigma StrFactor^2 d-hkl
16.704 13609.5 13232.3 363.352
CORR
7186.1846 5.302823
2 1
0 1 1
4 0.240725 0.700306
27.282
1413.4
3150.3 3850.030
3 1
1 1 0
4 0.245654 0.700242
28.575
3737.2
3792.5
4 1
-1 0 2
2 0.247394 0.700220
29.028
1004.7
1157.5 175.151
1653.1755 3.073583
0.980874
5 1
0 0 2
2 0.247801 0.700215
29.133
1012.0
1239.1 276.513
1677.9337 3.062719
0.980874
56.508
1003.8369 3.266154
0.980874
2927.0911 3.121183
0.997528
0.996906
18
6 1
-1 1 1
4 0.250235 0.700184
29.760
902.3
1028.0 142.603
7 1
2 0 0
2 0.266234 0.699987
33.778
275.5
214.6
8 1
1 1 1
4 0.268817 0.699956
34.410
808.0
577.7 163.864
9 1
-1 1 2
4 0.281134 0.699812
37.366
814.8
872.1
61.105
10 1
0 1 2
4 0.281490 0.699808
37.450
821.8
897.2
81.847
1147.8405 2.399416
0.993679
11 1
-2 0 2
2 0.282687 0.699794
37.732
3916.1
4101.9 193.595 11263.0537 2.382126
12 1
1 0 2
2 0.283751 0.699781
37.982
3856.4
3924.7
13 1
-2 1 1
4 0.293601 0.699670
40.266
422.7
288.8
14 1
2 1 0
4 0.298017 0.699620
41.272
4.3
15 1
-2 1 2
4 0.313250 0.699454
44.662
394.5
482.1 106.394
808.7592 2.027289
0.991923
16 1
1 1 2
4 0.314249 0.699443
44.880
380.8
500.8 157.030
788.9228 2.017951
0.991878
0.0
770.2098 2.999540
47.357
0.996377
625.0684 2.651411
0.980874
940.3376 2.604136
0.994617
1132.4675 2.404629
0.993703
69.357 11250.4707 2.367016
91.089
690.9999 2.237893
0.514
7.4841 2.185634
0.980874
0.980874
0.992925
0.992678
17 1
0 2 0
2 0.324247 0.699338
47.035
134.4
185.7
70.599
611.8162 1.930392
1.000000
18 1
2 1 1
4 0.325967 0.699320
47.401
251.0
91.7
57.968
586.2550 1.916347
0.991386
19 1
-1 1 3
4 0.332795 0.699250
48.838
257.6
859.4 1996.574
20 1
0 2 1
4 0.335801 0.699219
49.464
4.2
21 1
1 2 0
4 0.339637 0.699180
50.256
1559.8
1571.7
22 1
0 1 3
4 0.340942 0.699167
50.524
190.1
186.2
23 1
-1 2 1
4 0.343284 0.699143
51.003
0.6
24 1
-3 0 2
2 0.345560 0.699121
51.467
1339.7
1335.3
25 1
3 0 0
2 0.346560 0.699111
51.669
752.9
721.9
26 1
2 0 2
2 0.347170 0.699105
51.793
1304.3
1210.0
27 1
-2 1 3
4 0.355190 0.699026
53.400
207.0
28 1
1 2 1
4 0.358798 0.698991
54.114
0.6
29 1
-3 1 1
4 0.363313 0.698948
54.998
188.8
107.4
30 1
-1 2 2
4 0.369645 0.698888
56.225
2098.0
2054.1
31 1
0 2 2
4 0.369965 0.698885
56.286
2079.6
2029.1
32 1
-3 1 2
4 0.374156 0.698845
57.087
203.8
171.7
26.932
714.3837 1.612043
0.989879
33 1
3 1 0
4 0.375150 0.698836
57.276
348.5
334.7
13.167
1230.2858 1.607172
0.989855
34 1
2 1 2
4 0.375756 0.698830
57.391
202.8
212.7
10.409
718.9819 1.604221
0.989840
35 1
-1 0 4
2 0.376092 0.698827
57.455
1221.2
1318.7 104.701
36 1
1 1 3
4 0.379339 0.698797
58.068
132.2
37 1
-2 2 1
4 0.381022 0.698782
58.384
2.4
38 1
2 2 0
4 0.385139 0.698744
59.153
2237.0
39 1
-2 0 4
2 0.390608 0.698695
60.162
398.1
443.1
49.813
3150.0801 1.536792
0.980874
40 1
0 0 4
2 0.391894 0.698683
60.398
385.2
454.8
81.775
3072.7200 1.531359
0.980874
41 1
-2 2 2
4 0.399666 0.698614
61.808
242.5
312.8
90.181
999.6328 1.499770
0.996377
42 1
1 2 2
4 0.400634 0.698605
61.982
237.6
317.4 105.956
985.2477 1.495978
0.996344
43 1
-1 1 4
4 0.404764 0.698569
62.719
0.0
0.0
44 1
-3 1 3
4 0.407842 0.698543
63.265
98.0
86.7
10.185
427.2314 1.468687
0.989152
45 1
3 1 1
4 0.409858 0.698525
63.620
90.3
58.6
20.592
398.1082 1.461343
0.989114
3.9
0.7
0.318
5.522
0.990392
0.998040
610.3880 1.668228
0.990162
7062.1533 1.634718
49.170
0.030
0.980874
627.5506 1.714332
1.9461 1.693395
42.944
61.538
0.980874
0.980874
7473.1689 1.763683
46.091
2173.6
0.990840
0.998841
7570.5024 1.774094
50.568
32.880
0.999047
4291.1426 1.767607
87.130
0.569
0.999271
510.7625 1.804941
1.5842 1.789109
29.531
0.327
0.991127
4108.0264 1.813940
3.980
65.2
1.5
10.6250 1.841130
13.088
0.172
89.2
0.9
642.3242 1.863245
0.997542
7016.9478 1.633077
0.997528
8759.7168 1.602594
480.6660 1.587126
8.7651 1.579285
0.989754
0.997067
8400.5889 1.560592
0.0752 1.480142
0.980874
0.996906
0.989210
46 1
2 2 1
4 0.412147 0.698506
64.021
1.5
0.9
0.388
6.8709 1.453144
0.995968
47 1
-1 2 3
4 0.418971 0.698447
65.206
1.5
1.9
0.380
7.1267 1.429577
0.995759
48 1
-2 1 4
4 0.419491 0.698443
65.296
219.3
270.1
62.288
1019.3524 1.427833
0.988942
49 1
0 1 4
4 0.420800 0.698432
65.521
216.4
290.0
98.218
1013.0094 1.423473
0.988920
50 1
0 2 3
4 0.427219 0.698378
66.615
0.2
51 1
-3 0 4
2 0.436181 0.698305
68.116
47.2
69.4
32.616
480.8680 1.375424
0.980874
52 1
-4 0 2
2 0.436951 0.698299
68.243
80.6
110.9
41.575
824.5321 1.373164
0.980874
0.7
1.543
1.0218 1.402730
0.995521
53 1
1 0 4
2 0.438844 0.698283
68.556
46.4
62.2
21.017
479.4560 1.367659
0.980874
54 1
3 0 2
2 0.439282 0.698280
68.628
78.3
107.6
40.045
810.5381 1.366396
0.980874
55 1
-2 2 3
4 0.441909 0.698259
69.060
0.3
0.5
56 1
2 1 3
4 0.449328 0.698200
70.265
84.2
90.8
57 1
-3 2 1
4 0.450426 0.698191
70.442
0.1
0.1
58 1
4 0 0
2 0.454205 0.698161
71.047
594.2
0.525
7.385
0.014
683.3 102.046
1.3030 1.358910
0.995130
452.1836 1.338525
0.6905 1.335600
0.988480
0.994920
6564.4175 1.325706
0.980874
19
59 1
-3 2 2
4 0.461950 0.698101
72.270
177.1
167.9
8.770
995.2095 1.306240
60 1
3 2 0
4 0.463015 0.698093
72.437
407.4
387.1
19.326
2299.1768 1.303644
No. Code
H K L Mult
61 1
2 2 2
62 1
-4 1 1
63 1
-3 1 4
64 1
-4 1 2
65 1
66 1
Hw
ETA/M 2theta/TOF
4 0.463665 0.698088
Icalc
Iobs
167.7
0.994655
0.994631
Sigma StrFactor^2 d-hkl
9.048
CORR
72.539
177.2
4 0.463787 0.698087
72.558
69.6
65.7
4 0.466342 0.698068
72.955
0.4
0.3
4 0.467140 0.698062
73.079
59.0
38.7
1 2 3
4 0.467519 0.698059
73.138
1.1
0.6
0.264
6.2678 1.292877
0.994533
1 1 4
4 0.469106 0.698047
73.383
0.7
0.2
0.122
4.1944 1.289162
0.988223
67 1
3 1 2
4 0.469561 0.698043
73.453
56.8
4.1
4.156
330.9939 1.288103
68 1
0 3 1
4 0.482458 0.697947
75.412
51.1
140.9 245.873
69 1
4 1 0
4 0.485105 0.697928
75.807
2.0
1.5
70 1
1 3 0
4 0.486652 0.697917
76.037
129.9
30.7
23.540
71 1
-1 3 1
4 0.490676 0.697888
76.631
81.2
0.0
2.373
72 1
-1 2 4
4 0.495380 0.697854
77.320
68.0
0.0
1.909
429.1778 1.233050
0.993986
73 1
-4 1 3
4 0.495545 0.697853
77.344
48.9
0.0
1.396
310.7527 1.232728
0.987927
74 1
-3 2 3
4 0.498813 0.697830
77.817
0.8
0.0
0.055
5.1348 1.226404
0.993925
75 1
3 2 1
4 0.501067 0.697814
78.142
0.2
0.0
0.017
1.4296 1.222118
0.993886
76 1
-1 1 5
4 0.505250 0.697784
78.740
55.4
107.8 101.446
3.681
0.073
13.311
0.384
0.994617
396.7125 1.301775
2.4628 1.295658
0.988289
0.988257
340.5986 1.293768
0.988247
0.988217
307.9895 1.259433
12.3474 1.253846
0.999665
0.988038
793.4926 1.250626
0.999557
502.6871 1.242400
0.999456
361.9388 1.214323
77 1
1 3 1
4 0.508183 0.697764
79.157
34.9
72.2
-2 2 4
4 0.511916 0.697738
79.683
351.3
459.4 140.482
79 1
-2 1 5
4 0.513042 0.697730
79.841
44.4
53.2
80 1
0 2 4
4 0.513400 0.697728
79.891
355.4
415.8
81 1
-4 0 4
2 0.518420 0.697694
80.589
180.0
115.1
82 1
-1 3 2
4 0.520790 0.697678
80.916
54.8
24.5
13.478
368.3865 1.187072
0.998770
83 1
0 3 2
4 0.521166 0.697675
80.968
55.6
22.6
13.350
374.0085 1.186444
0.998763
84 1
2 0 4
2 0.522936 0.697663
81.211
179.4
29.0
24.297
2470.1375 1.183508
85 1
0 1 5
4 0.532793 0.697598
82.546
51.8
52.1
1.394
362.4321 1.167709
0.987583
86 1
4 1 1
4 0.533806 0.697591
82.682
49.0
54.2
5.872
343.4938 1.166138
0.987575
87 1
-2 3 1
4 0.534330 0.697588
82.752
52.7
62.9
12.205
88 1
2 3 0
4 0.539311 0.697555
83.414
0.4
0.8
1.059
2.6227 1.157757
0.998403
89 1
2 2 3
4 0.546279 0.697510
84.328
0.1
0.1
0.044
0.4945 1.147523
0.993193
90 1
-4 1 4
4 0.552928 0.697468
85.187
92.2
111.2
91 1
-2 3 2
4 0.557217 0.697442
85.735
41.5
42.4
1.065
300.8525 1.132260
0.998082
92 1
2 1 4
4 0.557753 0.697438
85.803
90.1
90.8
1.317
660.3613 1.131536
0.987391
93 1
-3 1 5
4 0.557786 0.697438
85.807
39.8
40.1
0.568
292.0261 1.131492
0.987390
94 1
1 3 2
4 0.558429 0.697434
85.889
40.6
40.6
0.476
294.5529 1.130625
0.998061
95 1
3 1 3
4 0.562829 0.697407
86.444
42.4
44.2
1.823
313.6615 1.124784
0.987355
96 1
-4 2 1
4 0.563341 0.697404
86.508
0.7
0.7
97 1
-3 2 4
4 0.566384 0.697385
86.888
668.9
98 1
-4 2 2
4 0.567337 0.697379
87.007
563.8
539.6
22.987
4172.5889 1.118946
0.992925
99 1
1 2 4
4 0.569685 0.697365
87.298
660.6
640.4
19.483
4905.9902 1.115962
0.992897
100 1
3 2 2
4 0.570230 0.697362
87.365
560.4
548.4
11.785
4165.1602 1.115276
0.992890
101 1
2 3 1
4 0.573019 0.697345
87.709
47.4
48.9
1.569
352.1851 1.111790
0.997822
102 1
-5 0 2
2 0.575839 0.697328
88.054
56.3
53.2
2.946
853.2866 1.108320
0.980874
103 1
4 0 2
2 0.579628 0.697305
88.515
56.3
45.7
8.587
857.6745 1.103739
0.980874
104 1
-1 3 3
4 0.581823 0.697292
88.780
33.2
24.8
6.247
249.2138 1.101128
0.997686
105 1
4 2 0
4 0.588984 0.697250
89.636
49.5
22.9
12.317
377.3356 1.092817
0.992678
106 1
0 3 3
4 0.592619 0.697229
90.066
52.9
49.9
3.442
402.5110 1.088718
0.997528
107 1
-4 2 3
4 0.601756 0.697177
91.131
0.1
0.2
108 1
1 1 5
4 0.601994 0.697176
91.158
34.1
41.8
10.505
70.377
41.302
22.857
0.024
22.041
0.034
9.518
227.5593 1.208978
0.987830
78 1
646.0
76.484
1002.6633 1.302068
0.999043
2322.8540 1.202315
296.1117 1.200333
0.987756
2358.5520 1.199708
2451.1831 1.191063
365.5885 1.165328
265.1108 1.078497
0.980874
0.980874
0.987426
0.992973
4943.1729 1.120168
1.0838 1.078751
0.993679
0.998498
670.1066 1.138133
4.9778 1.124114
0.993703
0.992936
0.992545
0.987107
20
109 1
-2 3 3
4 0.612271 0.697118
92.331
24.0
44.6
110 1
-1 2 5
4 0.613754 0.697110
92.498
0.5
0.9
111 1
-5 1 2
4 0.614814 0.697104
92.617
47.5
75.4
43.923
373.2206 1.065294
0.987036
112 1
-2 0 6
2 0.616424 0.697096
92.797
42.4
63.3
30.914
671.2037 1.063694
0.980874
113 1
-1 0 6
2 0.617800 0.697088
92.951
43.7
62.4
26.397
692.4671 1.062339
0.980874
114 1
4 1 2
4 0.618939 0.697082
93.078
47.5
65.9
25.200
374.8672 1.061224
0.987014
115 1
5 0 0
2 0.619615 0.697078
93.153
96.3
132.3
48.850
1530.0629 1.060565
116 1
-5 1 1
4 0.621430 0.697068
93.354
30.3
42.2
16.392
239.1643 1.058807
117 1
-2 2 5
4 0.623478 0.697057
93.580
0.1
0.1
118 1
-3 3 1
4 0.623918 0.697055
93.629
22.9
35.0
18.217
179.4042 1.056422
0.997113
119 1
-3 3 2
4 0.639979 0.696970
95.367
39.8
57.9
25.749
316.4240 1.041712
0.996923
120 1
-5 1 3
4 0.641346 0.696962
95.512
35.1
49.2
19.382
282.1512 1.040512
0.986902
No. Code
121 1
H K L Mult
3 3 0
Hw
ETA/M 2theta/TOF
4 0.641481 0.696962
95.526
Icalc
68.7
37.970
0.586
0.061
Iobs
96.1
186.3260 1.067845
4.0598 1.066352
0.6517 1.056841
0.997260
0.992427
0.992337
Sigma StrFactor^2 d-hkl
37.639
0.980874
0.987001
546.0848 1.040394
CORR
0.996906
122 1
2 3 2
4 0.642400 0.696957
95.624
40.2
56.2
21.988
319.5411 1.039593
0.996895
123 1
1 3 3
4 0.647866 0.696929
96.199
37.1
58.3
32.619
296.7766 1.034897
0.996834
124 1
0 2 5
4 0.648489 0.696926
96.264
0.1
0.2
0.094
0.8266 1.034370
0.992122
125 1
4 2 1
4 0.649786 0.696919
96.399
0.4
0.7
0.410
3.3734 1.033277
0.992111
126 1
-4 1 5
4 0.651499 0.696910
96.578
36.3
60.3
38.872
294.2411 1.031844
0.986856
127 1
-2 1 6
4 0.659269 0.696871
97.378
33.4
44.7
14.725
272.7739 1.025485
0.986821
128 1
-5 0 4
2 0.660224 0.696866
97.475
253.6
328.1
129 1
-3 0 6
2 0.660464 0.696865
97.500
207.8
266.8
130 1
-1 1 6
4 0.660787 0.696863
97.533
34.8
44.3
11.664
285.5622 1.024271
0.986815
131 1
5 1 0
4 0.662790 0.696854
97.736
64.0
78.3
16.850
526.2347 1.022680
0.986806
132 1
0 0 6
2 0.665046 0.696842
97.964
207.4
247.1
45.427
3447.0498 1.020906
0.980874
133 1
3 0 4
2 0.668398 0.696826
98.302
245.9
290.5
50.197
4121.5098 1.018305
0.980874
134 1
-4 2 4
4 0.674536 0.696796
98.913
180.3
223.4
49.566
1537.6798 1.013644
0.991923
135 1
2 2 4
4 0.680863 0.696765
99.535
153.3
190.1
36.943
1495.7455 1.008976
0.991878
136 1
-3 2 5
4 0.680906 0.696765
99.539
0.4
0.5
93.181
73.250
0.093
----------------------------------------------------BRAGG R-Factors and weight fractions for Pattern # 1
----------------------------------------------------=> Phase: 1
=> Bragg R-factor: 12.5
=> Rf-factor= 12.8
Vol: 131.242( 0.011) Fract(%): 100.00( 0.92)
ATZ:
354.610 Brindley: 1.0000
4178.7153 1.024720
3424.7009 1.024528
3.7761 1.008944
0.980874
0.980874
0.991878