DICVOL91.WP1

Documentation & Examples

for

DICVOL91

Automatic Powder Indexing

Successive Dichotomy

D. Louër

Robin Shirley

18 September 95

Based on DICVOL91.DOC

(27 March 1993)

C THIS PROGRAM NEEDS AT LEAST 522 kB OF FREE MEMORY TO RUN. CHECK

C THIS BY RUNNING THE DOS COMMAND CHKDSK.

C **********************************************************************

C --------------------------------------------------------------

C | TO EXECUTE THE PROGRAM, TYPE : |

C | |

C | DICVOL91 "DATA FILE NAME" "OUTPUT FILE NAME" |

C --------------------------------------------------------------

C A FILE EXAMPLE.DAT IS SUPPLIED FOR TESTING THE PROGRAM.

C ======================================================================

C ==========================================================================

C DDDDDDD IIII CCCCCC VV VV OOOOOO LL 999999 11

C DD DD II CC CC VV VV OO OO LL 99 99 1111

C DD DD II CC VV VV OO OO LL 99 99 111 11

C DD DD II CC VV VV OO OO LL 9999999 11

C DD DD II CC VV VV OO OO LL 99 11

C DD DD II CC CC VVVV OO OO LL LL 99 99 11

C DDDDDDD IIII CCCCCC VV OOOOOO LLLLLLLL 999999 1111

C ==========================================================================

C ======================================================================

C DICVOL91-VERSION PC : 30/06/1992

C (VERSION WITH SCREEN AND FILE OUTPUT - 19/03/93)

C TRIAL AND ERROR METHOD FOR THE AUTOMATIC INDEXING OF POWDER DIFFRACTION

C PATTERNS - VARIATION OF PARAMETERS BY SUCCESSIVE DICHOTOMY.

C THIS VERSION INCLUDES PARTITION OF VOLUME SPACE.

C THE FOLLOWING CRYSTALLINE SYSTEMS CAN BE EXAMINED :

C CUBIC, TETRAGONAL,HEXAGONAL, ORTHORHOMBIC, MONOCLINIC

C AND TRICLINIC.

C PRECURSOR PROGRAMS : P1 AND P2 (REF. 1), DICVOL (REF. 2)

C DICVOL91 HAS BEEN WRITTEN BY D. LOUER AND A. BOULTIF (REFS. 3)

C FOR FURTHER INFORMATION CONTACT

C D. LOUER

C LABORATOIRE DE CRISTALLOCHIMIE

C UNIVERSITE DE RENNES I

C CAMPUS DE BEAULIEU

C 35042 RENNES CEDEX -FRANCE-

C TEL. (33) 99-28-62-48

C FAX (33) 99-38-34-87

C E-MAIL [email protected]

C ---------------------------------------------------------------

C | G E N E R A L I N S T R U C T I O N S |

C ---------------------------------------------------------------

C DICVOL PROPOSES SOLUTIONS; THE USER DISPOSES OF THEM.

C THE AUTHORS DISCLAIM RESPONSABILITY FOR ALL USE OF THIS

C PROGRAM, WHETHER GOOD, BAD OR INDIFFERENT.

C DATA CARDS

C ----------

C CARD 1 TITLE FORMAT(16A4)

C CARD 2 N,ITYPE,JC,JT,JH,JO,JM,JTR FREE FORMAT

C N NUMBER OF LINES USED.

C ITYPE SPACING DATA TYPE.

C =1 THETA BRAGG IN DEGREES.

C =2 2-THETA ANGLE IN DEGREES.

C =3 D-SPACING IN ANGSTROMS.

C =4 Q SPECIFIED IN Q-UNITS AS E+04/D**2.

C JC =0 CUBIC SYSTEM IS NOT TESTED.

C =1 CUBIC SYSTEM IS TESTED.

C JT =0 TETRAGONAL SYSTEM IS NOT TESTED.

C =1 TETRAGONAL SYSTEM IS TESTED.

C JH =0 HEXAGONAL SYSTEM IS NOT TESTED.

C =1 HEXAGONAL SYSTEM IS TESTED.

C JO =0 ORTHORHOMBIC SYSTEM IS NOT TESTED.

C =1 ORTHORHOMBIC SYSTEM IS TESTED.

C JM =0 MONOCLINIC SYSTEM IS NOT TESTED.

C =1 MONOCLINIC SYSTEM IS TESTED.

C JTR =0 TRICLINIC SYSTEM IS NOT TESTED.

C =1 TRICLINIC SYSTEM IS TESTED.

C CARD 3 AMAX,BMAX,CMAX,VOLMIN,VOLMAX,BEMIN,BEMAX FREE FORMAT

C AMAX MAXIMUM VALUE OF UNIT CELL DIMENSION A IN ANGSTROMS.

C (IF AMAX= 0.0 DEFAULT= 20. ANGSTROMS)

C BMAX MAXIMUM VALUE OF UNIT CELL DIMENSION B IN ANGSTROMS.

C (IF BMAX= 0.0 DEFAULT= 20. ANGSTROMS)

C CMAX MAXIMUM VALUE OF UNIT CELL DIMENSION C IN ANGSTROMS.

C (IF CMAX= 0.0 DEFAULT= 20. ANGSTROMS)

C VOLMIN MINIMUM VOLUME FOR TRIAL UNIT CELLS IN ANGSTROMS**3.

C VOLMAX MAXIMUM VOLUME FOR TRIAL UNIT CELLS IN ANGSTROMS**3.

C (IF VOLMAX= 0.0 DEFAULT= 1500. ANGSTROMS**3)

C BEMIN MINIMUM ANGLE FOR UNIT CELL IN DEGREES

C (IF BEMIN= 0.0 DEFAULT= 90. DEGREES).

C BEMAX MAXIMUM ANGLE FOR UNIT CELL IN DEGREES

C (IF BEMAX= 0.0 DEFAULT= 125. DEGREES).

C CARD 4 WAVE,POIMOL,DENS,DELDEN FREE FORMAT

C WAVE WAVELENGTH IN ANGSTROMS (DEFAULT=0.0 IF CU K ALPHA1).

C POIMOL MOLECULAR WEIGHT OF ONE FORMULA UNIT IN A.M.U.

C (DEFAULT =0.0 IF FORMULA WEIGHT NOT KNOWN).

C DENS MEASURED DENSITY IN G.CM(-3)

C (DEFAULT =0.0 IF DENSITY NOT KNOWN).

C DELDEN ABSOLUTE ERROR IN MEASURED DENSITY.

C CARD 5 EPS,FOM FREE FORMAT

C EPS =0.0 THE ABSOLUTE ERROR ON EACH OBSERVED LINE

C IS TAKEN TO .03 DEG. 2THETA, WHATEVER THE

C SPACING DATA TYPE (ITYPE IN CARD 2).

C =1.0 THE ABSOLUTE ERROR ON EACH OBSERVED LINE IS

C INPUT INDIVIDUALLY IN THE FOLLOWING CARDS,

C TOGETHER WITH THE OBSERVED 'D(I)', ACCORDING

C WITH THE SPACING DATA UNIT.

C EPS NE 0.0 AND 1.0

C THE ABSOLUTE ERROR IS TAKEN AS A CONSTANT

C (=EPS),IN DEG. 2THETA, WHATEVER THE SPACING

C DATA TYPE (ITYPE IN CARD 2).

C FOM LOWER FIGURE OF MERIT M(N) REQUIRED FOR PRINTED

C SOLUTION(S) (DEFAULT=0.0 IF LOWER M(N)=5.0).

C CARD 6 TO 6+N D(I),EPSIL(I) FREE FORMAT

C (ONE FOR EACH OBSERVED LINE, UP TO N)

C D(I) VALUE DESCRIBING THE OBSERVED POSITION

C OF THIS LINE ACCORDING TO 'ITYPE'.

C EPSIL ABSOLUTE ERROR IN 'D(I)', ACCORDING TO 'ITYPE',

C ONLY IF EPS=1.0 (CARD 5).

C NOTE:

C IF ITYPE=1,2,4 THE VALUES OF 'D(I)' AND 'EPSIL(I)' MUST

C BE LISTED IN INCREASING ORDER.

C IF ITYPE=3 THEY MUST BE IN DECREASING ORDER.

C REFERENCES:

C 1.- LOUER, D. AND LOUER, M., METHODE D'ESSAIS ET ERREURS POUR

C L'INDEXATION AUTOMATIQUE DES DIAGRAMMES DE POUDRE,

C J. APPL. CRYST. 5, 271-275 (1972).

C 2.- LOUER, D. AND VARGAS, R., INDEXATION AUTOMATIQUE DES

C DIAGRAMMES DE POUDRE PAR DICHOTOMIES SUCCESSIVES,

C J. APPL. CRYST. 15, 542-545, (1982).

C 3.- BOULTIF, A. AND LOUER, D., INDEXING OF POWDER DIFFRACTION

C PATTERNS FOR LOW SYMMETRY LATTICES BY THE SUCCESSIVE

C DICHOTOMY METHOD, J. APPL. CRYST. 24, 987-993 (1991).

C 4.- DE WOLFF, P.M., A SIMPLIFIED CRITERION FOR THE RELIABILITY

C OF A POWDER PATTERN INDEXING, J. APPL. CRYST. 5, 108-113 (1968).

C 5.- SMITH, G. S. AND SNYDER, R. L., F(N): A CRITERION FOR RATING

C POWDER DIFFRACTION PATTERNS AND EVALUATING THE RELIABILITY

C OF POWDER-PATTERN INDEXING, J. APPL. CRYST. 12, 60-65 (1979).

C 6.- MIGHELL, A.D., HUBBARD, C.R. AND STALIK, J.K., NBS*AIDS80:

C A FORTRAN PROGRAM FOR CRYSTALLOGRAPHIC DATA EVALUATION.

C NAT. BUR. STAND. (U.S.) TECH. NOTE 1141 (1981). (NBS*AIDS83

C IS AN EXPANDED VERSION OF NBS*AIDS80).

C 7.- LOUER, D., AUTOMATIC INDEXING: PROCEDURES AND APPLICATIONS, IN

C 'ACCURACY IN POWDER DIFFRACTION II', NIST, SPEC. PUBL. No. 846,

C GAITHERSBURG, MD, USA, pp. 92-104, 1992.

C *****************************************************

C * *

C * THE USE OF DICVOL91 (VERSION 1.0) *

C * *

C *****************************************************

C USE AS INPUT DATA THE FIRST 20 LINES (ALTHOUGH THIS NUMBER

C CAN BE DIFFERENT). AVOID SPURIOUS LINES OR TOO INACCURATE DATA.

C ALL SYMMETRIES CAN BE EXAMINED IN ONE RUN. HOWEVER, IT IS

C RECOMMENDED TO USE A TWO- OR THREE-STAGE PROCEDURE :

C 1- SEARCH IN HIGH SYMMETRIES DOWN TO ORTHORHOMBIC.

C CARD 2 : N,ITYPE,1,1,1,1,0,0

C 2- SEARCH IN MONOCLINIC SYMMETRY.

C CARD 2 : N,ITYPE,0,0,0,0,1,0

C 3- IF NECESSARY, SEARCH IN TRICLINIC SYMMETRY.

C CARD 2 : N,ITYPE,0,0,0,0,0,1

C NOTE THAT FOR SOLUTIONS WITH TRICLINIC SYMMETRY THE USE OF A

C REDUCTION CELL PROGRAM IS USUALLY USEFULL TO OBTAIN THE

C CONVENTIONAL UNIT CELL (E.G. CDF-SRCH/JCPDS).

C NOTE - CASE OF TRIGONAL SYMMETRY WITH RHOMBOEDRAL LATTICE:

C THE PATTERN IS INDEXED WITH AN HEXAGONAL LATTICE, HAVING

C A UNIT CELL VOLUME THREE TIMES GREATER. OWING TO THE

C STRATEGY BASED ON THE PATITION OF VOLUME SPACE (SHELLS OF

C 400 A**3) YOU CAN MISS THE SOLUTION IF, BY ACCIDENT, A

C SMALLER (PSEUDO) SOLUTION IS FOUND IN AN OTHER SYMMETRY.

C IF YOU SUSPECT SUCH A CASE, RUN DICVOL91 WITH THE HEXAGONAL

C CASE ONLY (JC=0, JT=0, JH=1, JO=0, JM=0, JTR=0).

C RECOMMENDATIONS

C ---------------

C 1- PLEASE SPEND TIME TO ENSURE THE QUALITY OF YOUR OBSERVED DATA.

C WITH ACCURATE DATA THE SUCCESS RATE OF DICVOL91 IS VERY HIGH

C (SEE REF. 3).

C WITH BAD DATA THE CHANCE TO OBTAIN THE CORRECT SOLUTION IS VERY

C SMALL AND THE CALCULATION CAN BE TIME-CONSUMMING.

C WITH MODERN X-RAY POWDER DIFFRACTOMETERS (THE USE OF MONOCHROMATIC

C RADIATION IS STRONGLY RECOMMENDED) ABSOLUTE ERRORS ON PEAK

C POSITIONS LOWER THAN 0.03 DEGREES 2-THETA CAN BE ROUTINELY OBTAINED.

C FOR INDEXING PURPOSES, ERRORS SHOULD NOT EXCEED 0.03 DEG. 2-THETA

C [IN EXCEPTIONAL CASES, A FEW LINES WITH GREATER ERROR CAN BE

C INTRODUCED IN INPUT DATA. IN THIS CASE, USE THE PARAMETER EPS= 1.

C (CARD 5), AND ENTER INDIVIDUAL ERRORS ON EACH LINE(CARD 6 TO 6+N)].

C WITH HIGH RESOLUTION POWDER DIFFRACTION DATA (CONVENTIONAL OR,

C PARTICULARLY, SYNCHROTRON X-RAY SOURCES) THE ABSOLUTE ERROR IS

C USUALLY LESS THAN 0.02 (OR EVEN 0.01) DEG. 2-THETA; CONSEQUENTLY,

C EPS=0.02 (OR EVEN EPS=0.01) IS THEN RECOMMENDED; THE CONVERGENCE

C OF THE DICHOTOMY PROCEDURE WILL BE IMPROVED. HOWEVER, BE SURE THAT

C THIS CONDITION IS TRUE FOR ALL THE LINES USED AS INPUT DATA.

C 2- IF DICVOL91 HAS FOUND A SOLUTION FROM THE FIRST 20 (OR N) LINES,

C THIS SOLUTION MUST INDEXED THE COMPLETE POWDER DIFFRACTION

C PATTERN FOR THIS PURPOSE, THE PROGRAM NBS*AIDS83 (REF. 6) CAN BE

C USED.

C ---------- ------------------ ----------

C | |=========>| CUBIC |=========>| |

C | | ------------------ | |

C | | V | |

C | | ---------- | |

C | | | CUDHKL | | |

C | | ---------- | A |

C | | | F |

C | | | I |

C | | ------------------ | N |

C | |=========>| TETRAGONAL |=========>| E |

C | P | ------------------ | M |

C | R | V | E |

C | O | ---------- | N |

C | G | | TEDHKL | | T |

C | R | ---------- | |

C | A | | |

C | M | | D |

C | M | | E |

C | E | ------------------ | S |

C | |=========>| HEXAGONAL |=========>| |

C | | ------------------ | |

C | P | V | P |

C | R | ---------- | A |

C | I | | TEDHKL | | R |

C | N | ---------- | A |

C | C | | M |

C | I | | E |

C | P | | T |

C | A | ------------------ | R |

C | L |=========>| ORTHORHOMBIC |=========>| E |

C | | ------------------ | S |

C | | V | |

C | | ---------- | |

C | | | ORDHKL | | |

C | | ---------- | |

C | | | |

C | | ------------------ | R |

C | |=========>| MONOCLINIC |=========>| E |

C | | ------------------ | S |

C | | V | |

C | | ---------- | |

C | | | MODHKL | | |

C | | ---------- | |

C | | | |

C | | ------------------ | |

C | |=========>| TRICLINIC |=========>| |

C | | ------------------ ----------

C | | V V

C | | ---------- ----------

C ---------- ---------- ----------

Example Run 1

TEST1.IN

*** Cd3(OH)5(NO3) J. Solid State Chem. 84, 58, 1990. ***

20 2 1 1 1 1 0 0

0. 0. 0. 0. 0. 0. 0.

0. 0. 0. 0.

0. 0.

8.025

11.925

16.070

18.340

19.432

23.970

24.190

25.794

27.286

27.530

27.869

28.716

30.119

30.733

31.265

32.447

32.680

33.686

36.745

36.967

TEST1.OUT

--------------------------------------------------------------------

| *** Cd3(OH)5(NO3) J. Solid State Chem. 84, 58, 1990. *** |

--------------------------------------------------------------------

INPUT DATA

**********

EXPERIMENTAL EXPERIMENTAL

2-THETA ERROR

8.025 .030

11.925 .030

16.070 .030

18.340 .030

19.432 .030

23.970 .030

24.190 .030

25.794 .030

27.286 .030

27.530 .030

27.869 .030

28.716 .030

30.119 .030

30.733 .030

31.265 .030

32.447 .030

32.680 .030

33.686 .030

36.745 .030

36.967 .030

******************************************

------- PARAMETER LIMITS -------- -------- VOLUME LIMITS ---------

| | | |

| A MAXIMUM = 20.00 A | | |

| | | VOLUME MINIMUM = .00 A**3 |

| B MAXIMUM = 20.00 A | | |

| | | VOLUME MAXIMUM = 1500.00 A**3 |

| C MAXIMUM = 20.00 A | | |

| | | |

----------------------------------- ----------------------------------

WAVELENGTH = 1.540598

LOWER FIGURE OF MERIT REQUIRED FOR PRINTED SOLUTION(S) : M( 20) = 5.0

************************************************************

** **

** ATTENTION : VOS DONNEES SONT-ELLES IRREPROCHABLES ? **

** WARNING : ARE YOUR DATA IRREPROACHABLE ? **

** **

************************************************************

SEARCH OF CUBIC SOLUTION(S)

***************************

VOLUME DOMAIN BEING SCANNED :

===========================

LOWER BOUND = .00 A**3 HIGHER BOUND = 1500.00 A**3

CUBIC SYSTEM

------------

ITERATION NUMBER AT EACH DICHOTOMY LEVEL : 0 0 0 0 0 0 0

NO SOLUTION

END OF SEARCH FOR CUBIC SOLUTION(S)

***********************************

SEARCH OF TETRAGONAL AND/OR HEXAGONAL AND/OR ORTHORHOMBIC SOLUTION(S)

*********************************************************************

VOLUME DOMAIN BEING SCANNED :

===========================

LOWER BOUND = .00 A**3 HIGHER BOUND = 400.00 A**3

TETRAGONAL SYSTEM

-----------------

ITERATION NUMBER AT EACH DICHOTOMY LEVEL : 0 0 0 0 0 0 0

NO SOLUTION

HEXAGONAL SYSTEM

----------------

ITERATION NUMBER AT EACH DICHOTOMY LEVEL : 0 0 0 0 0 0 0

NO SOLUTION

ORTHORHOMBIC SYSTEM

-------------------

O R T H O R H O M B I C S Y S T E M

DIRECT PARAMETERS : A= 11.02817 B= 10.02693 C= 3.42061 VOLUME= 378.25

STANDARD DEVIATIONS : .00107 .00117 .00040

H K L DOBS DCAL DOBS-DCAL QOBS QCAL 2TH.OBS 2TH.CAL DIF.2TH.

1 0 0 11.00834 11.02817 -.01983 .00825 .00822 8.025 8.011 .014

1 1 0 7.41545 7.41888 -.00343 .01819 .01817 11.925 11.919 .006

2 0 0 5.51087 5.51409 -.00321 .03293 .03289 16.070 16.061 .009

2 1 0 4.83357 4.83168 .00190 .04280 .04284 18.340 18.347 -.007

1 2 0 4.56434 4.56399 .00035 .04800 .04801 19.432 19.434 -.002

2 2 0 3.70950 3.70944 .00006 .07267 .07267 23.970 23.970 .000

3 0 0 3.67626 3.67606 .00020 .07399 .07400 24.190 24.191 -.001

3 1 0 3.45117 3.45142 -.00024 .08396 .08395 25.794 25.792 .002

1 0 1 3.26576 3.26706 -.00131 .09376 .09369 27.286 27.275 .011

0 1 1 3.23736 3.23741 -.00005 .09542 .09541 27.530 27.530 .000

1 3 0 3.19875 3.19864 .00011 .09773 .09774 27.869 27.870 -.001

1 1 1 3.10630 3.10633 -.00003 .10364 .10363 28.716 28.716 .000

3 2 0 2.96472 2.96453 .00019 .11377 .11379 30.119 30.121 -.002

2 0 1 2.90687 2.90674 .00013 .11834 .11836 30.733 30.734 -.001

2 3 0 2.85861 2.85823 .00038 .12237 .12241 31.265 31.269 -.004

4 0 0 2.75712 2.75704 .00008 .13155 .13156 32.447 32.448 -.001

1 2 1 2.73800 2.73717 .00082 .13339 .13347 32.680 32.690 -.010

4 1 0 2.65849 2.65838 .00011 .14149 .14150 33.686 33.687 -.001

1 4 0 2.44389 2.44438 -.00049 .16743 .16736 36.745 36.737 .008

3 1 1 2.42972 2.42956 .00017 .16939 .16941 36.967 36.970 -.003

* NUMBER OF LINES

.- INPUT DATA = 20

.- CALCULATED = 30

* MEAN ABSOLUTE DISCREPANCIES

<Q> = .2416E-04

<DELTA(2-THETA)> = .4255E-02

MAX. ERROR ACCEPTED (DEG. 2-THETA) = .4500E-01

* FIGURES OF MERIT

1.- M( 20) = 116.8 (REF. 4)

2.- F( 20) = 156.7( .0043, 30) (REF. 5)

---------

ITERATION NUMBER AT EACH DICHOTOMY LEVEL : 2 4 1 1 1 1 1

END OF SEARCH FOR TETRAGONAL AND/OR HEXAGONAL AND/OR ORTHORHOMBIC SOLUTION(S)

*****************************************************************************

--- CALCULATION TIME FOR SEARCH DOWN TO ORTHORHOMBIC SYMMETRY : .610 SEC.

--- T O T A L CALCULATION TIME : .6100 SEC.

DICVOL91 : USEFUL REFERENCES

--------

* LOUER, D. & LOUER, M. (1972). J. APPL. CRYST. 5, 271-275.

* BOULTIF, A. & LOUER, D. (1991). J. APPL. CRYST. 24, 987-993.

Example Run 2

TEST2.IN

*** CdWO4 NBS Monograph 25 Sect.2 p.9 1963 ***

20 3 0 0 0 0 1 0

0. 0. 0. 0. 0. 0. 0.

0. 0. 0. 0.

0. 0.

5.87

5.04

3.818

3.077

3.020

2.928

2.530

2.514

2.311

2.287

2.253

2.131

2.092

1.953

1.916

1.907

1.820

1.809

1.797

1.774

TEST2.OUT

--------------------------------------------------------------------

| *** CdWO4 NBS Monograph 25 Sect.2 p.9 1963 *** |

--------------------------------------------------------------------

INPUT DATA

**********

EXPERIMENTAL EXPERIMENTAL

D VALUES ERROR

5.8700 .0116

5.0400 .0085

3.8180 .0049

3.0770 .0031

3.0200 .0030

2.9280 .0028

2.5300 .0021

2.5140 .0020

2.3110 .0017

2.2870 .0017

2.2530 .0016

2.1310 .0014

2.0920 .0014

1.9530 .0012

1.9160 .0011

1.9070 .0011

1.8200 .0010

1.8090 .0010

1.7970 .0010

1.7740 .0010

******************************************

------- PARAMETER LIMITS -------- -------- VOLUME LIMITS ---------

| | | |

| A MAXIMUM = 20.00 A | | |

| B MAXIMUM = 20.00 A | | VOLUME MINIMUM = .00 A**3 |

| C MAXIMUM = 20.00 A | | |

| BETA MINIMUM = 90.00 Deg. | | VOLUME MAXIMUM = 1500.00 A**3 |

| BETA MAXIMUM = 125.00 Deg. | | |

| | | |

----------------------------------- ----------------------------------

WAVELENGTH = 1.540598

LOWER FIGURE OF MERIT REQUIRED FOR PRINTED SOLUTION(S) : M( 20) = 5.0

************************************************************

** **

** ATTENTION : VOS DONNEES SONT-ELLES IRREPROCHABLES ? **

** WARNING : ARE YOUR DATA IRREPROACHABLE ? **

** **

************************************************************

SEARCH OF MONOCLINIC SOLUTION(S)

********************************

MONOCLINIC SYSTEM

-----------------

SEARCH OF MONOCLINIC SOLUTION(S) WITHIN THE LIMITS ON LINEAR PARAMETERS

***********************************************************************

(SLIGHT TOLERANCE ACCEPTED): A MAX= 12.263 B MAX= 12.263 C MAX= 12.263

VOLUME DOMAIN BEING SCANNED :

===========================

LOWER BOUND = .00 A**3 HIGHER BOUND = 400.00 A**3

ANGLE RANGE SCANNED : BETA MIN= 90.000 Deg. BETA MAX= 95.000 Deg.

M O N O C L I N I C S Y S T E M

DIRECT PARAMETERS : A= 5.0702 B= 5.8574 C= 5.0309 BETA= 91.495 VOLUME= 149.36

STANDARD DEVIATIONS : .0013 .0011 .0011 .022

H K L DOBS DCAL DOBS-DCAL QOBS QCAL 2TH.OBS 2TH.CAL DIF.2TH.

0 1 0 5.87000 5.85739 .01261 .02902 .02915 15.081 15.114 -.033

0 0 1 5.04000 5.02917 .01083 .03937 .03954 17.583 17.621 -.038

0 1 1 3.81800 3.81568 .00232 .06860 .06868 23.279 23.294 -.014

1 1 -1 3.07700 3.07781 -.00081 .10562 .10556 28.995 28.988 .008

1 1 1 3.02000 3.01982 .00018 .10964 .10966 29.555 29.557 -.002

0 2 0 2.92800 2.92869 -.00069 .11664 .11659 30.506 30.498 .007

0 2 1 2.53000 2.53084 -.00084 .15623 .15612 35.452 35.440 .012

0 0 2 2.51400 2.51459 -.00059 .15822 .15815 35.685 35.677 .009

0 1 2 2.31100 2.31066 .00034 .18724 .18730 38.941 38.947 -.006

2 0 -1 2.28700 2.28724 -.00024 .19119 .19115 39.366 39.362 .004

1 2 1 2.25300 2.25247 .00053 .19701 .19710 39.985 39.995 -.010

2 1 -1 2.13100 2.13056 .00044 .22021 .22030 42.381 42.390 -.009

2 1 1 2.09200 2.09205 -.00005 .22849 .22848 43.211 43.210 .001

0 3 0 1.95300 1.95246 .00054 .26218 .26232 46.459 46.473 -.014

2 2 0 1.91600 1.91638 -.00038 .27240 .27229 47.411 47.401 .010

0 2 2 1.90700 1.90784 -.00084 .27498 .27474 47.648 47.626 .022

0 3 1 1.82000 1.82011 -.00011 .30190 .30186 50.079 50.076 .003

2 0 -2 1.80900 1.80873 .00027 .30558 .30567 50.404 50.413 -.008

1 2 -2 1.79700 1.79730 -.00030 .30967 .30957 50.765 50.756 .009

1 2 2 1.77400 1.77400 .00000 .31776 .31776 51.471 51.471 .000

* NUMBER OF LINES

.- INPUT DATA = 20

.- CALCULATED = 36

* MEAN ABSOLUTE DISCREPANCIES

<Q> = .8467E-04

<DELTA(2-THETA)> = .1096E-01

MAX. ERROR ACCEPTED (DEG. 2-THETA) = .4500E-01

* FIGURES OF MERIT

1.- M( 20) = 52.1 (REF. 4)

2.- F( 20) = 50.7( .0110, 36) (REF. 5)

---------

ANGLE RANGE SCANNED : BETA MIN= 95.000 Deg. BETA MAX=100.000 Deg.

ANGLE RANGE SCANNED : BETA MIN=100.000 Deg. BETA MAX=105.000 Deg.

ANGLE RANGE SCANNED : BETA MIN=105.000 Deg. BETA MAX=110.000 Deg.

ANGLE RANGE SCANNED : BETA MIN=110.000 Deg. BETA MAX=115.000 Deg.

ANGLE RANGE SCANNED : BETA MIN=115.000 Deg. BETA MAX=120.000 Deg.

ANGLE RANGE SCANNED : BETA MIN=120.000 Deg. BETA MAX=125.000 Deg.

ITERATION NUMBER AT EACH DICHOTOMY LEVEL : 237 171 49 11 5 2 1

END OF SEARCH FOR MONOCLINIC SOLUTIONS

**************************************

--- CALCULATION TIME FOR SEARCH DOWN TO MONOCLINIC SYMMETRY : 31.090 SEC.

--- T O T A L CALCULATION TIME : 31.0900 SEC.

DICVOL91 : USEFUL REFERENCES

--------

* LOUER, D. & LOUER, M. (1972). J. APPL. CRYST. 5, 271-275.

* BOULTIF, A. & LOUER, D. (1991). J. APPL. CRYST. 24, 987-993.

Example Run 3

TEST3.IN

*** BENACTYZINE HYDROCHLORIDE NBS Monog. 25 Sect. 16 p. 92 ***

20 2 0 0 0 0 0 1

0. 0. 0. 0. 0. 0. 0.

0. 0. 0. 0.

0.02 0.

5.58

10.10

11.18

11.36

11.70

12.58

13.26

14.26

15.34

16.02

16.76

17.64

17.86

18.26

19.62

19.92

20.12

20.58

20.82

21.22

TEST3.OUT

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| *** BENACTYZINE HYDROCHLORIDE NBS Monog. 25 Sect. 16 p. 92 ** |

--------------------------------------------------------------------

INPUT DATA

**********

EXPERIMENTAL EXPERIMENTAL

2-THETA ERROR

5.580 .020

10.100 .020

11.180 .020

11.360 .020

11.700 .020

12.580 .020

13.260 .020

14.260 .020

15.340 .020

16.020 .020

16.760 .020

17.640 .020

17.860 .020

18.260 .020

19.620 .020

19.920 .020

20.120 .020

20.580 .020

20.820 .020

21.220 .020

******************************************

------------ VOLUME LIMITS -----------

| |

| VOLUME MINIMUM = .00 A**3 |

| |

| VOLUME MAXIMUM = 1500.00 A**3 |

| |

----------------------------------------

WAVELENGTH = 1.540598

LOWER FIGURE OF MERIT REQUIRED FOR PRINTED SOLUTION(S) : M( 20) = 5.0

************************************************************

** **

** ATTENTION : VOS DONNEES SONT-ELLES IRREPROCHABLES ? **

** WARNING : ARE YOUR DATA IRREPROACHABLE ? **

** **

************************************************************

SEARCH OF TRICLINIC SOLUTION(S)

*******************************

TRICLINIC SYSTEM

----------------

VOLUME DOMAIN BEING SCANNED :

===========================

LOWER BOUND = 686.48 A**3 HIGHER BOUND = 886.48 A**3

NO SOLUTION

VOLUME DOMAIN BEING SCANNED :

===========================

LOWER BOUND = 886.48 A**3 HIGHER BOUND = 1086.48 A**3

T R I C L I N I C S Y S T E M

DIRECT PARAMETERS AND THEIR STANDARD DEVIATIONS :

A=15.9364 B= 8.7898 C= 7.0840 ALP= 85.922 BET= 95.729 GAM= 92.477 VOL= 984.20

.0062 .0027 .0029 .046 .035 .033

H K L DOBS DCAL DOBS-DCAL QOBS QCAL 2TH.OBS 2TH.CAL DIF.2TH.

1 0 0 15.82521 15.84629 -.02108 .00399 .00398 5.580 5.573 .007

0 1 0 8.75091 8.76171 -.01081 .01306 .01303 10.100 10.088 .012

2 0 0 7.90787 7.92315 -.01528 .01599 .01593 11.180 11.158 .022

1 -1 0 7.78297 7.78862 -.00566 .01651 .01648 11.360 11.352 .008

1 1 0 7.55755 7.55221 .00534 .01751 .01753 11.700 11.708 -.008

0 0 1 7.03079 7.03267 -.00188 .02023 .02022 12.580 12.577 .003

1 0 -1 6.67172 6.67274 -.00101 .02247 .02246 13.260 13.258 .002

1 0 1 6.20603 6.20846 -.00243 .02596 .02594 14.260 14.254 .006

2 1 0 5.77144 5.77310 -.00166 .03002 .03000 15.340 15.336 .004

1 -1 -1 5.52796 5.52327 .00470 .03272 .03278 16.020 16.034 -.014

2 0 -1 5.53306 -.00510 .03266 16.005 .015

3 0 0 5.28552 5.28210 .00342 .03580 .03584 16.760 16.771 -.011

2 0 1 5.02377 5.02308 .00069 .03962 .03963 17.640 17.642 -.002

1 -1 1 4.96238 4.96125 .00113 .04061 .04063 17.860 17.864 -.004

2 -1 -1 4.85457 4.85296 .00161 .04243 .04246 18.260 18.266 -.006

2 1 -1 4.52103 4.52124 -.00021 .04892 .04892 19.620 19.619 .001

3 1 0 4.45361 4.45258 .00103 .05042 .05044 19.920 19.925 -.005

2 1 1 4.40979 4.40540 .00439 .05142 .05153 20.120 20.140 -.020

2 -1 1 4.31225 4.31160 .00065 .05378 .05379 20.580 20.583 -.003

1 -2 0 4.26308 4.26249 .00059 .05502 .05504 20.820 20.823 -.003

1 2 0 4.18361 4.18355 .00006 .05713 .05714 21.220 21.220 .000

* NUMBER OF LINES

.- INPUT DATA = 20

.- CALCULATED = 29

* MEAN ABSOLUTE DISCREPANCIES

<Q> = .2659E-04

<DELTA(2-THETA)> = .7156E-02

MAX. ERROR ACCEPTED (DEG. 2-THETA) = .3500E-01

* FIGURES OF MERIT

1.- M( 20) = 37.0 (REF. 4)

2.- F( 20) = 96.4( .0072, 29) (REF. 5)

ITERATION NUMBER AT EACH DICHOTOMY : 63 138 110 40 4 2 8 1

END OF SEARCH FOR TRICLINIC SOLUTIONS

*************************************

--- T O T A L CALCULATION TIME : 22.3600 SEC.

DICVOL91 : USEFUL REFERENCES

--------

* LOUER, D. & LOUER, M. (1972). J. APPL. CRYST. 5, 271-275.

* BOULTIF, A. & LOUER, D. (1991). J. APPL. CRYST. 24, 987-993.