Документ взят из кэша поисковой машины. Адрес оригинального документа : http://www.chem.msu.ru/rus/teaching/tafejenko-fetisov-STADIVARI-Pilatus-2012.pdf Дата изменения: Mon Oct 28 17:01:16 2013 Дата индексирования: Thu Feb 27 23:55:28 2014 Кодировка:

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STADIVARI Pilatus

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2012

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CAD-4 Stadivari : RUN, FRAME, a X-Area (1) (2) .hkl. 1) 2) 3) RUN 4) 5) 6-7) RUN 8) 9) 10) 11) , .hkl 12) 13) 14)

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STADIVARI Pilatus .
" StadiVari Pilatus 100K" , SHELX - . (X-Area), . Software manual X-Area, 2011, Stoe & Cie GmbH, Stoe, . . , . `'. Ia . Ib ( ) . , ( 42, 60, 80, 100, 120, 170 ) . 2


" StadiVari Pilatus 100K" . . pocket terminal . , , . , ( ), . , , . - , , . . - , .

CAD-4 Stadivari
, , , CAD-4, . 1 - CAD-4 , , .dat, .hkl, .cry Stadivari ­ , .x . 2 - , CAD-4- SEARCH, 15-20 . , . Stadivari- , , . , RUN () FRAM (), , . -RUN - ( ). FRAME ­ , . , / . 0.5 3o , . (1-150c), . RUN LIST ( DATCIN), . Stadivari CAD-4 . , , 3


. (150 ), . . , , . . . . , . 3 . CAD-4 DATCIN Stadivari ­ , , RUN Optimaizer. CAD-4 .dat, , .hkl . Stadivari . X-Area (Find Peaks). . ( ) (postrefine). .hkl SHELX - . Integrate/integrate integrate/integrate(big mask). , . . . ( ), 20% . , , , , . . , ( I/(I); 2 , , . , . +/0.5%. , . , , . 2 ­ . ­ , . . . W=A+B*tg, W/cos(2) + /*tg; ( 1,2 ) -. A,B . A,B (SIMULATION) (Optimisation) EMS ­ effective mosaic 4


spread, . 0.005-0.02. `' , () . , ). . CAD4, . . , s Faceit . , , X-Shape . , ( , [redundancy]) . , . , .

Ia a X-Area
, ,

X-Area/
X-Area (I) (II); (I)- ( X-Area) File Edit Instrument Display Peak/Cell Integrate Extras Help (2)- , (1)­ Instrument/ Measure/Mo (2) -File Runlist Extras Help X-Area , (I), (II) ( EXTRAS ). , . , (), (2). , , , , , (1). (2) , (1) .x . 5


.hkl.
1) - . - . (Viewing position I) Faceit : (2)- Instrument/Extras/ Viewing position I Faceit/Start ( ) 2)- .x : (1) File/New 3)- 2-5 , , : (2) RunList/Edit/+/Exit/Start 4) ( ) : (1) Peak/Cell--/FindPeak 5) . : (1) Peak/cell, Recipe/Index/Refine, Index, Direction, Cell, Refine - Exit 6)- (max , , , ) Run Optimizer. : (1) Instrument/Run Optimizer; ­ Optimize. - Save Funlist. 7) Funlist .x . : (2) RunList/Edit/reset delete all files/load funlist/exit 8) - . Start 9)- . 4) 10)- . : (1) Peak/cell, Recipe/Index/Refine, Index, Direction, Cell, Refine ­ Exit Cell, Refine 11)- ( ). : (1) Integrate/Integrate/OK/Simulation/Exit/Integration 6


.hkl 12)- (postrefine). : (1) Peak/cell, Recipe/Index/Refine, Postrefine, Cell, Refine; .sum 13)- ­ , , , . : (2) - Instrument/Extras/ Viewing position I Faceit/StartVideo/ . (1) Extras/Xred32/ -- ( , , Z) Abs.Correction/Process - .hkc F2 `' , , Rint . : (1) Extras/Xred32/OK/Extras/ Select X-Shape Reflection .eqv : (1) Extras/X-Shape : automatic, `' : Shape\ : automatic\Exit (1) Extras/X-RED32 /Abs.Correction/Process .hkc 14) . Decay Correction (1) : EXTRAS/DECAY 14) x- . : (1) EXTRAS/SCALE DATASETS

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Ib

, , , X-Area. . , , ( ) (I). File Edit Instrument Display Peak/Cell Integrate Extras Help (I)

File ­ , . Edit ­ , , , . Instrument ­ ., . Display ­ . Peak/Cell ­ , 8


Integrate , , hkl Shelx Extras- , X-RED32, X-SHAPE - (1) Instrument, Measure, \OK

c (2) File Runlist Extras Help (II) Extras, Synchronize axes

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( ) Move to Viewing Position 1. . , Start Faceit StartVideo. . . 1) . 10


X-Y. - (- ); ( ), , (Z). - ( , , ). - . . ( ) . .

90 - . . , 180 - . - (< >, <<>>, -90, +90, -180, +180) , Stop Video, File Exit. , . . . . 2) , - (1) File, New. c ( - ), .x . . 11


. Ok. 3) RUN LIST (II) Runlist, Edit

Reset and Delete all runs + . . , . , . . 0 180 . . -30, -30, -60, -60 . 3 , . + ( -). run list OK. START.

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. ( ).

Measurement ( ) , , . Current frame Frame browser . 4) ( ) : (1) Peak/Cell--/FindPeak

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Start. . Omitt Graphics. Exit. 5) . : (1) Peak/cell, Recipe/Index/Refine,

Index . ( +X,+Y,+Z ­X,-Y,-Z) . , , , . 14


Direction . . .

OK Cell

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Refine ( Crystal system) 6)- (max , , , ) Run Optimaizer. : (1) Instrument/Run Optimazer; ­ Optimize. - Save Funlist. (I) INSTRUMENT Run Optimaizer. .

RUN Optimizer : Max 2, , , , (REDUNDANCY), , completeness. OPTIMAIZE. , , , . (, 16


.) , RUN LIST save fun. .x , funlist 7) funlist .x . : (2) RunList/Edit/reset delete all files/load funlist/exit Funlist .x (II) Run list , Edit. (reset and delete all files) Load fun list. Run List . . 8) Measurement ((II) Start. . , . , (RESUME) . START . , , . , , Faceit; View position 1. ) - . : (1) Peak/Cell--/FindPeak - : (1) Peak/cell, Recipe/Index/Refine. Postrefine, Cell, Refine. 11) ( ). : (1) Integrate/Integrate/OK/Simulation/Exit/Integration .hkl , , A,B,EMS ­ , ­ EMS (effective mosaic spread) (I) Integrate/ Integrate

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. ( Mo Cu), (Apply beamstop mask), OK.

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Simulation A, B, EMS. Optimisation, , 20% () . , . Exit, / Integrate - - ( . - - , - - overflowed ( ). - .hkl (( h k l F2 (F2) B (6 ), B batch number, )) SHELX (HKLF 5). 12)- (Postrefine). 19


: (1) Peak/cell, Recipe/Index/Refine, Postrefine, Cell, Refine; .sum 13) . X-Area . , , , . : (2) - Instrument/Extras/ Viewing position I Faceit/StartVideo/ . (1) Extras/Xred32/ --

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( , , Z) : OK/ Abs.Correction/Process - .hkc F2 , `' , , Rint . : (1) Extras/Xred32/OK/Extras

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: Select X-Shape Reflection

.eqv : (1) Extras/X-Shape

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: automatic, `' : Shape\ : automatic\Exit (1) Extras/X-RED32 /Abs.Correction/Process .hkc 14) , (Decay Correction) DECAY (1) : EXTRAS/DECAY DECAY . a) DECAY . b) DECAY . . , a), b) ; a) b) . . , x , , . . DECAY , N . , . . , . INTEGRATE .DEC, DECAY . ASCII .DEC X-AREA DECAY. DECAY, DECAY . , . ReferenceFrames, MeanIntensities. SETUP : DECAY/SETUP . . , Reference Frame, Load frames. , , N(strongest) , Nstrongest . , N=200, 200 . .dec . SETUP DECAY, WEGHTS, . SETUP ­ POLYnomial Spline DECAY Apply correction .hkl. DECAY , .hkl Reset Correction. 23


Exluding time span, . DECAY Software manual X-Area, 2011, Stoe & Cie GmbH, 14, 101-108 14a) (SCALE DATASETS) . , , . X-Area 4- . : (1) EXTRAS/SCALE DATASETS , _1.x _2.x. *.hkl. , x- , SCALE x-. , N , N-1 - x-. : - ( ) .(EXTRAS\XRED32) - (EXTRAS/DECAY Correction) - SCALE (SCALE/OPTIONs) hkl .

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