Structure determination by X-ray crystallography:
Saved in:
| Main Authors: | , |
|---|---|
| Format: | Book |
| Language: | English |
| Published: |
New York [u.a.]
Plenum Press
1993
|
| Edition: | 3. ed. |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Physical Description: | XXIV, 586 S. Ill., zahlr. graph. Darst. |
| ISBN: | 0306442906 |
Staff View
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| 245 | 1 | 0 | |a Structure determination by X-ray crystallography |c M. F. C. Ladd and R. A. Palmer |
| 250 | |a 3. ed. | ||
| 264 | 1 | |a New York [u.a.] |b Plenum Press |c 1993 | |
| 300 | |a XXIV, 586 S. |b Ill., zahlr. graph. Darst. | ||
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Record in the Search Index
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| adam_text | CONTENTS NOTATION XXI CHAPTER 1 CRYSTAL GEOMETRY. I 1 1.1 INTRODUCTION 1
1.2 THE CRYSTALLINE STATE 2 1.2.1 REFERENCE AXES 5 1.2.2 EQUATION OF A
PLANE 8 1.2.3 MILLER INDICES 10 1.2.4 AXIAL RATIOS 14 1.2.5 ZONES 14 1.3
STEREOGRAPHIC PROJECTION 18 1.4 EXTERNAL SYMMETRY OF CRYSTALS 26 1.4.1
TWO-DIMENSIONAL POINT GROUPS 28 1.4.2 THREE-DIMENSIONAL POINT GROUPS 31
BIBLIOGRAPHY 50 PROBLEMS 51 CHAPTER 2 CRYSTAL GEOMETRY. II 59 2.1
INTRODUCTION 59 2.2 LATTICES 59 2.2.1 TWO-DIMENSIONAL LATTICES 60 2.2.2
CHOICE OF UNIT CELL 61 2.2.3 THREE-DIMENSIONAL LATTICES 62 2.3 FAMILIES
OF PLANES AND INTERPLANAR SPACINGS 72 2.4 RECIPROCAL LATTICE 73 2.4.1
TRUTH OF THE RECIPROCAL LATTICE 78 2.5 ROTATIONAL SYMMETRIES OF LATTICES
79 2.6 SPACE GROUPS 80 2.6.1 TWO-DIMENSIONAL SPACE GROUPS 82 2.6.2 PLANE
GROUPS RELATED TO 2MM 91 2.6.3 THREE-DIMENSIONAL SPACE GROUPS 92 2.6.4
SCREW AXES 97 2.6.5 GLIDE PLANES 98 2.6.6 ANALYSIS OF THE SPACE-GROUP
SYMBOL 107 2.7 MATRIX REPRESENTATION OF SYMMETRY OPERATIONS 108 2.7.1
MATRICES IN POINT-GROUP SYMMETRY 108 2.7.2 MATRICES IN SPACE-GROUP
SYMMETRY ILL BIBLIOGRAPHY 113 PROBLEMS 113 CHAPTER 3 PRELIMINARY
EXAMINATION OF CRYSTALS BY OPTICAL AND X-RAY METHODS 117 3.1
INTRODUCTION 117 3.2 POLARIZED LIGHT 118 3.3 OPTICAL CLASSIFICATION OF
CRYSTALS 119 3.3.1 UNIAXIAL CRYSTALS 119 3.3.2 BIREFRINGENCE 122 3.3.3
BIAXIAL CRYSTALS 125 3.3.4 INTERFERENCE FIGURES 128 3.4 DIRECTION OF
SCATTERING OF X-RAYS BY CRYSTALS 129 3.4.1 LAUE EQUATIONS FOR X-RAY
SCATTERING 131 3.4.2 BRAGG S TREATMENT OF X-RAY DIFFRACTION 134 3.4.3
EQUIVALENCE OF LAUE AND BRAGG TREATMENTS OF X-RAY DIFFRACTION 137 3.5
X-RAY TECHNIQUES 139 3.5.1 LAUE METHOD 139 3.5.2 OSCILLATION METHOD 147
3.5.3 EWALD S CONSTRUCTION 152 3.5.4 WEISSENBERG METHOD 162 3.5.5
PRECESSION METHOD 166 3.6 RECOGNITION OF CRYSTAL SYSTEM 168 3.7
SINGLE-CRYSTAL X-RAY DIFFRACTOMETRY 172 3.7.1 INSTRUMENT GEOMETRY 172
3.7.2 ROTATION OF THE CRYSTAL INTO A DIFFRACTING POSITION . . 173 3.7.3
TRANSFORMATION FROM MILLER INDICES TO GEOMETRY . . 174 3.7.4 DATA
COLLECTION 175 3.8 TWINNING 176 BIBLIOGRAPHY 178 PROBLEMS 179 CHAPTER 4
SCATTERING OF X-RAYS BY CRYSTALS 183 4.1 INTRODUCTION 183 4.2 PATH
DIFFERENCE 184 4.3 MATHEMATICAL REPRESENTATION OF A WAVE: AMPLITUDE AND
PHASE 186 4.4 COMBINATION OF TWO WAVES 189 4.5 ARGAND DIAGRAM 191 4.6
COMBINATION OF TV WAVES 192 4.7 COMBINED SCATTERING OF X-RAYS FROM THE
CONTENTS OF THE UNIT CELL 194 4.7.1 PHASE DIFFERENCE 194 4.7.2
SCATTERING BY ATOMS 194 4.8 STRUCTURE FACTOR 196 4.9 INTENSITY
EXPRESSIONS 198 4.10 PHASE PROBLEM IN STRUCTURE ANALYSIS 198 4.11
APPLICATIONS OF THE STRUCTURE FACTOR EQUATION 199 4.11.1 FRIEDEL S LAW
199 4.11.2 STRUCTURE FACTOR FOR A CENTROSYMMETRIC CRYSTAL . . 201 4.11.3
LIMITING CONDITIONS AND SYSTEMATIC ABSENCES . . . 203 4.11.4
DETERMINATION OF UNIT-CELL TYPE 205 4.11.5 STRUCTURE FACTORS AND
SYMMETRY ELEMENTS 206 4.11.6 LIMITING CONDITIONS FROM SCREW-AXIS
SYMMETRY . . 209 4.11.7 CENTROSYMMETRIC ZONES 211 4.11.8 LIMITING
CONDITIONS FROM GLIDE-PLANE SYMMETRY . . 212 4.12 PRELIMINARY STRUCTURE
ANALYSIS 218 4.12.1 PRACTICAL DETERMINATION OF SPACE GROUPS 218
BIBLIOGRAPHY 222 PROBLEMS 223 CHAPTER 5 FOURIER TRANSFORM THEORY 225 5.1
IMAGE FORMATION AND FOCUSING 225 5.2 HOLES AND ATOMS 227 5.3 GENERALIZED
FOURIER TRANSFORM * * * 229 5.3.1 FOURIER TRANSFORM FOR A MOLECULE 231
5.3.2 FOURIER TRANSFORM OF A UNIT CELL 231 5.4 PRACTICE WITH TRANSFORMS
232 5.4.1 OPTICAL DIFFRACTOMETER 232 5.4.2 SINGLE HOLE 233 5.4.3 TWO
HOLES 233 5.4.4 MORE HOLES 235 5.4.5 CHANGE OF ORIGIN 235 5.4.6
SYSTEMATIC ABSENCES 235 5.4.7 PATTERNS 237 5.5 RECONSTRUCTION OF THE
IMAGE 237 5.6 REPRESENTATION OF FOURIER TRANSFORMS 239 5.7 PRACTICAL
EXAMPLE 239 5.8 CONVOLUTION 243 5.9 STRUCTURE SOLUTION METHODS IN BRIEF
244 5.9.1 USE OF HEAVY ATOMS 244 5.9.2 GENERAL PHASE-FREE TRANSFORM 246
5.9.3 SIGN RELATIONSHIPS 247 PROBLEMS 250 CHAPTER 6 TECHNIQUES IN X-RAY
STRUCTURE DETERMINATION 253 6.1 INTRODUCTION 253 6.2 ANALYSIS OF THE
UNIT-CELL CONTENTS 253 6.2.1 PAPAVERINE HYDROCHLORIDE, C 20) H 21 NO 4 *
HCL . . . . 254 6.2.2 NAPHTHALENE, C 10 H 8 254 6.2.3 MOLECULAR SYMMETRY
255 6.2.4 SPECIAL POSITIONS 256 6.2.5 NICKEL TUNGSTATE, NIWO 4 257 6.3
FOURIER SERIES 260 6.3.1 COMPUTATION OF PSI (X) FOR A SQUARE WAVE 261
6.3.2 EXPONENTIAL FORM OF FOURIER EXPRESSIONS 264 6.4 REPRESENTATION OF
CRYSTAL STRUCTURES BY FOURIER SERIES . . . 265 6.4.1 ELECTRON DENSITY
AND STRUCTURE FACTORS 267 6.4.2 ELECTRON DENSITY EQUATIONS 270 6.4.3
INTERPRETATION OF ELECTRON DENSITY DISTRIBUTIONS . . . 273 6.5 METHODS
OF SOLVING THE PHASE PROBLEM 277 6.5.1 NUMBER OF REFLECTIONS IN THE DATA
SET 277 6.5.2 THE PATTERSON FUNCTION 278 6.5.3 EXAMPLES OF THE USE OF
THE PATTERSON FUNCTION IN SOLVING THE PHASE PROBLEM 288 6.5.4 ABSOLUTE
SCALE OF F 0 AND OVERALL TEMPERATURE FACTOR 305 6.5.5 HEAVY-ATOM
METHOD AND PARTIAL FOURIER SYNTHESIS 308 6.5.6 DIFFERENCE-FOURIER
SYNTHESIS 314 6.5.7 LIMITATIONS OF THE HEAVY-ATOM METHOD 315 6.5.8
ISOMORPHOUS REPLACEMENT 317 6.5.9 FURTHER DETAILS OF THE ISOMORPHOUS
REPLACEMENT PHASING PROCEDURE 327 6.6 ANOMALOUS SCATTERING 335 6.6.1
HAMILTON S R RATIO 336 6.6.2 EFFECT OF ANOMALOUS SCATTERING ON SYMMETRY
OF THE DIFFRACTION PATTERNS 338 6.6.3 FORM OF THE STRUCTURE FACTOR FOR A
STRUCTURE COMPOSED OF HEAVY-ATOM ANOMALOUS SCATTERERS . . 341 6.6.4
PHASING BY USE OF ANOMALOUS SCATTERING 344 6.6.5 RESOLUTION OF THE PHASE
PROBLEM FOR PROTEINS USING ANOMALOUS SCATTERING MEASUREMENTS (SIRAS*
METHOD) 344 6.6.6 PROTEIN PHASING USING THE MULTIPLE-WAVELENGTH
ANOMALOUS DISPERSION TECHNIQUE (MAD) WITH SYNCHROTRON RADIATION (SR) 345
6.7 NEUTRON DIFFRACTION 348 6.7.1 COMPLEMENTARY NATURE OF NEUTRON
DIFFRACTION . . . 350 6.7.2 REFINEMENT OF HYDROGEN ATOM POSITIONS 352
BIBLIOGRAPHY 352 PROBLEMS 353 CHAPTER 7 DIRECT METHODS AND REFINEMENT
367 7.1 INTRODUCTION 367 7.2 DIRECT METHODS OF PHASE DETERMINATION 367
7.2.1 NORMALIZED STRUCTURE FACTORS 367 7.2.2 STRUCTURE INVARIANTS AND
ORIGIN-FIXING REFLECTIONS . . 370 7.2.3 SIGN
DETERMINATION*CENTROSYMMETRIC CRYSTALS . . . 372 7.2.4 AMPLITUDE
SYMMETRY AND PHASE SYMMETRY 377 7.2.5 SIGMA 2 LISTING 377 7.2.6
SYMBOLIC-ADDITION PROCEDURE 378 7.2.7 CALCULATION OF E MAPS 381 7.2.8
PHASE DETERMINATION*NONCENTROSYMMETRIC CRYSTALS 382 7.2.9 PHASE
DETERMINATION IN SPACE GROUP P2 1 388 7.2.10 ADVANTAGES AND
DISADVANTAGES OF SYMBOLIC ADDITION 392 7.2.11 MULTISOLUTION PHILOSOPHY
AND BRIEF DESCRIPTION OF THE PROGRAM MULTAN 394 7.2.12 FIGURES OF MERIT
400 7.2.13 EXAMPLE OF THE USE OF MULTAN 402 7.2.14 SOME EXPERIENCES 404
7.3 PATTERSON SEARCH METHODS 406 7.3.1 ORIENTATION SEARCH 407 7.3.2
TRANSLATION SEARCH. 409 7.3.3 EXAMPLE OF A STRUCTURE SOLUTION BY VECTOR
VERIFICATION 409 7.3.4 INTEGRATED PATTERSON AND DIRECT METHODS 414 7.4
LEAST-SQUARES REFINEMENT 415 7.4.1 UNIT-CELL DIMENSIONS 416 7.4.2 ATOMIC
PARAMETERS 416 7.4.3 STRATEGY IN LEAST-SQUARES REFINEMENT 422 7.5
MOLECULAR GEOMETRY 425 7.5.1 BOND LENGTHS AND ANGLES 425 7.5.2 TORSION
ANGLES 427 7.5.3 CONFORMATIONAL ANALYSIS 428 7.5.4 MEAN PLANES 431 7.6
PRECISION 431 7.7 CORRECTNESS OF A STRUCTURE ANALYSIS 433 7.8
LIMITATIONS OF X-RAY STRUCTURE ANALYSIS 436 7.9 DISORDER IN SINGLE
CRYSTALS 437 BIBLIOGRAPHY 443 PROBLEMS 445 CHAPTER 8 EXAMPLES OF CRYSTAL
STRUCTURE DETERMINATION 447 8.1 INTRODUCTION 447 8.2 CRYSTAL STRUCTURE
OF 2-BROMOBENZO[6]INDENO[L,2-E]PYRAN (BBIP) 448 8.2.1 PRELIMINARY
PHYSICAL AND X-RAY MEASUREMENTS . . . 448 8.2.2 INTENSITY MEASUREMENT
AND CORRECTION 456 8.2.3 STRUCTURE ANALYSIS IN THE XZ PROJECTION 459
8.2.4 THREE-DIMENSIONAL STRUCTURE DETERMINATION . . . . 460 8.2.5
REFINEMENT 467 8.2.6 MOLECULAR GEOMETRY 467 8.3 CRYSTAL STRUCTURE OF
POTASSIUM 2-HYDROXY- 3,4-DIOXOCYCLOBUT-L-ENE-L-OLATE MONOHYDRATE (KHSQ)
. . . 469 8.3.1 PRELIMINARY X-RAY AND PHYSICAL MEASUREMENTS . . . 470
8.3.2 INTENSITY MEASUREMENT AND CORRECTION 471 8.3.3 SIGMA 2 LISTING 473
8.3.4 SPECIFYING THE ORIGIN 473 8.3.5 SIGN DETERMINATION 474 8.3.6 THE E
MAP 477 8.3.7 COMPLETION AND REFINEMENT OF THE STRUCTURE . . . . 479 8.4
CONCLUDING REMARKS 483 BIBLIOGRAPHY 483 PROBLEMS 483 APPENDIX 487 AL
STEREOVIEWS AND CRYSTAL MODELS 487 AL.L STEREOVIEWS 487 A1.2 MODEL OF A
TETRAGONAL CRYSTAL 488 A2 CRYSTALLOGRAPHIC POINT-GROUP STUDY AND
RECOGNITION SCHEME 490 A3 SCHOENFLIES SYMMETRY NOTATION 492 A3.1
ALTERNATING AXIS OF SYMMETRY 492 A3.2 NOTATION 493 A4 GENERATION AND
PROPERTIES OF X-RAYS 494 A4.1 X-RAYS AND WHITE RADIATION 494 A4.2
CHARACTERISTIC X-RAYS 494 A4.3 ABSORPTION OF X-RAYS 496 A4.4 FILTERED
RADIATION 497 A5 CRYSTAL PERFECTION AND INTENSITY MEASUREMENT 498 A5.1
CRYSTAL PERFECTION 498 A5.2 INTENSITY OF REFLECTED BEAM 500 A5.3
INTENSITY MEASUREMENTS ON PHOTOGRAPHS 502 A5.4 DATA PROCESSING 503
A5.4.1 INTRODUCTION 503 A5.4.2 STANDARD DEVIATION OF INTENSITY 506
A5.4.3 ABSORPTION CORRECTIONS 507 A5.4.4 SCALING 508 A5.4.5 MERGING
EQUIVALENT REFLECTIONS 509 A6 TRANSFORMATIONS 509 A7 COMMENTS ON SOME
ORTHORHOMBIC AND MONOCLINIC SPACE GROUPS 511 A7.1 ORTHORHOMBIC SPACE
GROUPS 511 A7.2 MONOCLINIC SPACE GROUPS 514 A8 VECTOR ALGEBRAIC
RELATIONSHIPS IN RECIPROCAL SPACE . . . . 514 A8.1 INTRODUCTION 514 A8.2
RECIPROCAL LATTICE 514 A8.2.1 INTERPLANAR SPACINGS 516 A8.2.2 VOLUME OF
A PARALLELEPIPEDON 518 A8.2.3 RECIPROCITY OF UNIT-CELL VOLUMES 519
A8.2.4 ANGLE BETWEEN BRAVAIS LATTICE PLANES . . . 520 A8.2.5 RECIPROCITY
OF F AND I UNIT CELLS 521 A8.3 X-RAY DIFFRACTION AND THE RECIPROCAL
LATTICE . . . . 522 A8.3.1 BRAGG S EQUATION . . 523 A8.4 CRYSTAL SETTING
525 A8.4.1 SETTING TECHNIQUE 525 A9 INTENSITY STATISTICS 527 A9.1
WEIGHTED RECIPROCAL LATTICE 527 A9.1.1 LAUE SYMMETRY 527 A9.1.2
SYSTEMATIC ABSENCES 528 A9.1.3 ACCIDENTAL ABSENCES 528 A9.1.4 ENHANCED
AVERAGES 528 A9.1.5 SPECIAL DISTRIBUTIONS 530 A10 ENANTIOMORPH SELECTION
533 ALL ANALYTICAL GEOMETRY OF DIRECTION COSINES 534 ALL.L DIRECTION
COSINES OF A LINE 534 ALL.2 ANGLE BETWEEN TWO LINES 535 A12 THE
STEREOGRAPHIC PROJECTION OF A CIRCLE IS A CIRCLE . . . . 536 A13 SETTING
A CRYSTAL FOR PRECESSION PHOTOGRAPHY 538 A13.1 SETTING A CRYSTAL AXIS
PARALLEL TO THE X-RAY BEAM 538 A13.2 SETTING A RECIPROCAL LATTICE ROW
HORIZONTALLY . . . 540 A13.3 SCREEN SETTING 540 A14 SYNCHROTRON
RADIATION 541 SOLUTIONS 545 INDEX 573
|
| any_adam_object | 1 |
| author | Ladd, Marcus F. Palmer, Rex A. |
| author_facet | Ladd, Marcus F. Palmer, Rex A. |
| author_role | aut aut |
| author_sort | Ladd, Marcus F. |
| author_variant | m f l mf mfl r a p ra rap |
| building | Verbundindex |
| bvnumber | BV008313563 |
| classification_rvk | UQ 5600 VG 9900 |
| classification_tum | PHY 605f GEO 425f PHY 606f |
| ctrlnum | (OCoLC)611071556 (DE-599)BVBBV008313563 |
| discipline | Chemie / Pharmazie Geowissenschaften Physik |
| edition | 3. ed. |
| format | Book |
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| id | DE-604.BV008313563 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T17:18:08Z |
| institution | BVB |
| isbn | 0306442906 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-005492392 |
| oclc_num | 611071556 |
| open_access_boolean | |
| owner | DE-355 DE-BY-UBR DE-19 DE-BY-UBM DE-188 |
| owner_facet | DE-355 DE-BY-UBR DE-19 DE-BY-UBM DE-188 |
| physical | XXIV, 586 S. Ill., zahlr. graph. Darst. |
| publishDate | 1993 |
| publishDateSearch | 1993 |
| publishDateSort | 1993 |
| publisher | Plenum Press |
| record_format | marc |
| spelling | Ladd, Marcus F. Verfasser aut Structure determination by X-ray crystallography M. F. C. Ladd and R. A. Palmer 3. ed. New York [u.a.] Plenum Press 1993 XXIV, 586 S. Ill., zahlr. graph. Darst. txt rdacontent n rdamedia nc rdacarrier Strukturtheorie - Röntgenkristallographie Röntgenbeugung (DE-588)4178306-2 gnd rswk-swf Kristallstrukturanalyse (DE-588)4137204-9 gnd rswk-swf Kristall (DE-588)4033209-3 gnd rswk-swf Kristallstruktur (DE-588)4136176-3 gnd rswk-swf Röntgenstrukturanalyse (DE-588)4137203-7 gnd rswk-swf Röntgenstrukturanalyse (DE-588)4137203-7 s Kristall (DE-588)4033209-3 s DE-604 Kristallstrukturanalyse (DE-588)4137204-9 s 1\p DE-604 Röntgenbeugung (DE-588)4178306-2 s 2\p DE-604 Kristallstruktur (DE-588)4136176-3 s 3\p DE-604 Palmer, Rex A. Verfasser aut OEBV Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=005492392&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 2\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 3\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Ladd, Marcus F. Palmer, Rex A. Structure determination by X-ray crystallography Strukturtheorie - Röntgenkristallographie Röntgenbeugung (DE-588)4178306-2 gnd Kristallstrukturanalyse (DE-588)4137204-9 gnd Kristall (DE-588)4033209-3 gnd Kristallstruktur (DE-588)4136176-3 gnd Röntgenstrukturanalyse (DE-588)4137203-7 gnd |
| subject_GND | (DE-588)4178306-2 (DE-588)4137204-9 (DE-588)4033209-3 (DE-588)4136176-3 (DE-588)4137203-7 |
| title | Structure determination by X-ray crystallography |
| title_auth | Structure determination by X-ray crystallography |
| title_exact_search | Structure determination by X-ray crystallography |
| title_full | Structure determination by X-ray crystallography M. F. C. Ladd and R. A. Palmer |
| title_fullStr | Structure determination by X-ray crystallography M. F. C. Ladd and R. A. Palmer |
| title_full_unstemmed | Structure determination by X-ray crystallography M. F. C. Ladd and R. A. Palmer |
| title_short | Structure determination by X-ray crystallography |
| title_sort | structure determination by x ray crystallography |
| topic | Strukturtheorie - Röntgenkristallographie Röntgenbeugung (DE-588)4178306-2 gnd Kristallstrukturanalyse (DE-588)4137204-9 gnd Kristall (DE-588)4033209-3 gnd Kristallstruktur (DE-588)4136176-3 gnd Röntgenstrukturanalyse (DE-588)4137203-7 gnd |
| topic_facet | Strukturtheorie - Röntgenkristallographie Röntgenbeugung Kristallstrukturanalyse Kristall Kristallstruktur Röntgenstrukturanalyse |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=005492392&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT laddmarcusf structuredeterminationbyxraycrystallography AT palmerrexa structuredeterminationbyxraycrystallography |