The extensivey used, very powerful and most readily available method for characterising compounds which can be obtained as SINGLE Crystals (= with almost perfect periodicity of the molecules/ions/atoms). It gives extensive information about compounds in solid state.

My Experiences are described below:
Operation of Enraf-Nonius CAD4 Diffractometer;
Structure Solution and Refinement using MULTAN-82, SHELX-76, SHELXS-86 & SHELXL-93 Programs;
Experienced from ~220 crystal structures during 1989-1999; AND
Operation of Nonius KappaCCD Single Crystal X-ray Diffractometer (660 datasets during 2000-2011)

NEW! Edited a NEW, Free Access Online book (Dec-2011): "Current Trends in X-ray Crystallography" NEW!
Written a MANUAL for Single crystal X-ray Crystallography:
Written a FORTRAN program for the data processing.

Use of PCs (DOS and Windows), VAX, MicroVax, DEC-1090, IBM RISC-6000 and some UNIX systems.

Writing programs in FORTRAN. (Little C and Turbo Basics)

Published Two Papers in Crystallography Journals:

"Superstructural Variety from an Alkylated Triazine: Formation of One-Dimensional Hydrogen-Bonded Arrays or Cyclic Rosettes", M.L. Highfill, A. Chandrasekaran, D.E. Lynch, D.G. Hamilton, Crystal Growth & Design, 2002, 2, 15-20.

"Crystal Structure of the Protonated Salt of an (Amino)spirocyclic Cyclotriphosphazene", A.Chandrasekaran, Acta Cryst. Sect. C, 1994, C50, 1692-1694.
Including SHELXS, SHELXL and ORTEX programs (Totally complete for crystallography!).
Some Useful References are:
Some useful WWW connections for crystallography
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Created by Dr. A. Chandrasekaran
Department of Chemistry, University of Massachusetts, AMHERST, MA 01003, USA.

Suggestions Welcome!