Single-Crystal X-ray Diffraction
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021Using X-ray Diffraction to ProvideAnswers, Theory and Practice.Dr. Richard J. StaplesSpecial Topics 913 Section 002Department of Chemistry, MSUTest, Midterm and FinalHomework Assignments, count as the third test.Solve one Structure to publication quality or perform experiment approvedby instructor, can not get credit if not completed.Textbook and RequirementsRequired Text Single Crystal Diffraction:”Crystal Structure Determination” W.Massa ISBN: 3-540-65970-6ORRequired Text Powder Diffraction:”Fundamentals of Powder Diffraction andStructural Characterization” Vitalij Pecharsky and Peter Y. Zavalij, 2nd editionISBN: 978-0-387-09578-3ORRequired Text Macromolecular Crystallography:”Crystallography MadeCrystal Clear” 2nd edition, A guide for users of Macromolecular Models, G.Rhodes ISBN: 0-12-587072-8Recommend: “Chemical Applications of Group Theory” F. A. Cotton, 3rdedition.Recommend: “International Tables for Crystallography, Brief Teaching Editionof Volume A.” Kluwer Academic Publishers.Text Books Dealing with X-ray Diffraction andStructure AnalysisSanders, Donald E. Introduction to Crystallography, Dover Publications, Inc.,New York, 1993.Ladd, M.F.; Palmer, R.A. Structure Determination by X-ray Crystallography, 3rded.; Plenum: New York, 1994.Stout, G.H.; Jensen, L.H. X-ray Structure Determination, A Practical Guide, 2nded.; Wiley & Sons, New York, 1989.Giacovazzo, C. Fundamentals of Crystallography, IUCr, Oxford SciencePublications, 1994.Gluster and Trueblood ”Crystals Structure Analysis; A Primer”, 2nd, edition. Richard J. Staples, Michigan State University, Department of Chemistry, 2021
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021January 20. L1. IntroINTRO, syllabus, grading .LAB requirementDistribute Practical OptionsJanuary 22, L2. History, SafetyHistory of Single Crystal DiffractionSafety Concerns in X-ray Diffraction Experiments.-Register to get a badge-Exposure-Regulations-Safety DevicesDistribute Homework 1January 27, L3. Growing Crystals. Mounting, EvaluationKey factors in obtaining good crystals.Read: “Crystal Growing”, Peter G. Jones, Chemistry inBritain, 17 (1981) 222-225.“Some thoughts about the single crystal growth of smallmolecules” B. Spingler, S. Schnidrig, T. Todorova and F.Wild Cryst. Eng. Comm., 2012, 14, 751-757.January 29, L4. Symmetry4.1Group Theory4.2Crystallographic Symmetry and Space GroupsDistribute Homework 2TURN IN HOMEWORK 1 Richard J. Staples, Michigan State University, Department of Chemistry, 2021
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021February 3, L5 4.3Symmetry and Space Groups4.4Space Groups and TablesFebruary 5, L6. Symmetry Matrix MethodDistribute Homework 3February 10, L7. DiffractionInstruments, SCXRDTURN IN HOMEWORK 2February 12, L8. Data Base Searching and Uses (notcovered diffraction)(CSD)(ICSD)(PDB)REVIEW HOMEWORK 1&2Distribute Homework Prob-Database 21TURN IN HOMEWORK 3February 17, L9. Math of the SCXRDData ReductionPhase ProblemResolving the ProblemAnomalous Dispersion and Absolute ConfigurationDistribute Homework 4February 19, L10. Math of the SCXRD Part 2Anomalous Dispersion and Absolute ConfigurationStructure RefinementDisorder and twinningStructural Parameters: Analysis of ResultsDistribute Homework-Structure Solving 21 Richard J. Staples, Michigan State University, Department of Chemistry, 2021
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021February 24, L11. REVIEW and Homework AnswersTURN IN HOMEWORK 4February 26, L12. EXAM 1: FEBRUARY 11, 2020MARCH 3, NO ClasSMarch 5, L13. Small Molecule OLEX2 DEMOOrganization of FilesPrograms for Structure SolutionRefinement ParametersSpecial FactorsGraphical InterfaceFinal Publication Tables and CIFDistribute Homework-Structure Solving 21Distribute Homework-SCXRDMarch 10, L14. PWXRD Powder X-ray DiffractionDifferencesMath of PeaksSample PrepDistribute Homework -PWXRDMarch 12, L15. PWXRD Powder X-ray DiffractionData AcquisitionPrep to get a Unit Cell Richard J. Staples, Michigan State University, Department of Chemistry, 2021
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021March 17, L16. PWXRD Powder X-ray DiffractionIndexing to Solve StructureTURN IN HOMEWORK-SCXRDMarch 19, L17. PWXRD Powder X-ray DiffractionFinalizing, Limitations, other methods.March 24, L18. Macromolecular CrystallographyGrowing the crystalsProtein PropertiesMounting ChallengesDistribute Homework-MacroTURN IN HOMEWORK-PWXRDMarch 26, L19. MC: Data CollectionInstrumentsGetting all the dataQualityDemonstrationMarch 31, L20. MC: Solving Phase ProblemAnomalous dispersionHeavy AtomStructure interpretationDemonstrationApril 2, L21. MC: Structure InterpretationViewsSurfaceStructure interpretation Richard J. Staples, Michigan State University, Department of Chemistry, 2021
Tentative, Changes may be due as the COVID Changes.Last updated 1-6-2021April 7, L22a. CRYO-EM, MICRO-EDorL22b. Rest Other WebinarsApril 9, L23. Finalizing ClassHomework reviewQuestionsALL Homework Due by April 9, 2020April 16 or 21. L24-26. EXAM II. April 20, 2020COVERS ALL MATERIALConcentration on last part.Additional Class PoliciesDiversity and Inclusion PolicyInclusion and diversity are core values of MSU and the College of NaturalScience. As Spartans, we are dedicated to respecting people of all backgrounds,beliefs, identity status, and political beliefs. The college is committed to creating asafe, supportive, and welcoming environment where all students, faculty, andstaff can pursue academic and professional success. All members of the MSUcommunity deserve each other’s respect, support, recognition, and protection. Itis essential that we all work together to foster an inclusive community whereSpartans of all backgrounds can study, work, and thrive.Americans with Disabilities Act AccommodationsMichigan State University is committed to providing equal opportunity forparticipation in all programs, services, and activities. Requests foraccommodations by persons with disabilities may be made by contacting theResource Center for Persons with Disabilities by phone at 517-884-RCPD orthrough the web at rcpd.msu.edu. Once your eligibility for an accommodation hasbeen determined, you will be issued a verified individual services accommodation(“VISA”) form. Please present this form at the start of the semester and/or atleast two weeks prior to the accommodation date. Requests received after thisdate will be honored whenever possible. Richard J. Staples, Michigan State University, Department of Chemistry, 2021
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History of Single Crystal Diffraction Safety Concerns in X-ray Diffraction Experiments. -Register to get a badge -Exposure -Regulations -Safety Devices Distribute Homework 1 January 27, L3. Growing Crystals. Mounting, Evaluation Key factors in obtaining good crystals. Read: “Crystal Growing”, Peter G. Jones, Chemistry in Britain, 17 (1981 .
Diffraction of Waves by Crystals crystal structure through the diffraction of photons (X-ray), nuetronsandelectrons. 18 Diffraction X-ray Neutron Electron The general princibles will be the same for each type of waves.
X-Ray Diffraction and Crystal Structure (XRD) X-ray diffraction (XRD) is one of the most important non-destructive tools to analyse all kinds of matter - ranging from fluids, to powders and crystals. From research to production and engineering, XRD is an indispensible method for
Single crystal diffraction with x-ray (and neutrons) Dinnebier Pre9. Dinnebier Pre6 X-ray hitting condensed matter Laue equation: Q hkl k f-k i . Imaging of reciprocal planes by high-energy x-ray diffraction Sc-Zn q x (Å )-1
We simulate XFEL spectra after diffraction on a bent crystal and show that an energy resolution of 3 10 6,or 0.04 eV for the X-ray energy of 12 keV, can be reached on diffraction on a 20 mm-thick diamond crystal bent to a radius of10 cm.Wealsotakeintoaccountthefree-spacepropagation of the waves diffracted by the bent crystal to the detector
A nonlinear optical crystal of LPKDP crystal was grown at room temperature by slow evaporation technique. The size of the grown crystal is 11*7*2 mm3 at a growth rate of .55m/day. The single crystal X-ray diffraction analysis has been carried out to find the lattice parameters and powder x-Ray diffraction patterns has been recorded
Plane transmission diffraction grating Mercury-lamp Spirit level Theory If a parallel beam of monochromatic light is incident normally on the face of a plane transmission diffraction grating, bright diffraction maxima are observed on the other side of the grating. These diffraction maxima satisfy the grating condition : a b sin n n , (1)
3. CHARACTERIZATION 3.1 Single crystal X-ray diffraction and fundamental parameters: The grown crystals of Cobalt Mercury Thiocyanate was subjected to single crystal X-ray diffraction studies using ENRAF NONIUS CAD-4 diffractometer to elucidate their lattice parameters. The title crystal belongs to the tetragonal system. 3, which is in good
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