Analysis of macromolecules, ligands and macromolecule-ligand complexes

A method for determining the structure of a macromolecule-ligand complex, comprising:

• providing a sample of polycrystalline macromolecule unassociated with a ligand;
• providing a sample of a polycrystalline complex of a macromolecule and a ligand;
• obtaining powder diffraction data from said samples;
• and
• analyzing said diffraction data to generate a model structure of said macromolecule-ligand complex.

A method for determining the previously unknown structure of a macromolecule, comprising:

• providing a sample of a polycrystalline macromolecule;
• obtaining powder diffraction data from said sample;
• and
• analyzing said diffraction data to generate a model structure of said macromolecule.

A method for preparing a sample containing microcrystallites of a macromolecule-ligand complex suitable for analysis by X-ray powder diffraction, comprising:

• providing a quantity of substantially dehydrated macromolecules and a quantity of ligand molecules;
• adding a liquid to said dehydrated macromolecules and said ligands;
• physically agitating said liquid, said dehydrated macromolecules and said ligands in order to form said microcrystalline sample of said macromolecule-ligand complex;
• and,
• placing the microcrystalline sample of said macromolecule-ligand complex on or in an X-ray powder diffraction sample holder or container.

A method for preparing a sample containing microcrystallites of a macromolecule suitable for high resolution analysis by X-ray powder diffraction, comprising:

• providing a solution of macromolecules;
• inducing precipitation of macromolecules from the solution of macromolecules to produce a microcrystalline sample;
• and
• placing the microcrystalline sample on or in an X-ray powder diffraction sample holder or container.

A method for determining the structure of a macromolecule, comprising:

• producing a sample of a polycrystalline macromolecule, said sample produced by a method comprising:
• providing a quantity of substantially dehydrated macromolecules;
• and
• adding a liquid to said dehydrated macromolecules while physically agitating the macromolecules wherein said polycrystallites of said macromolecule are formed;
• collecting powder diffraction data from said sample of said polycrystalline macromolecule;
• and
• analyzing said diffraction data to yield the structure of said polycrystalline macromolecule.

A method for determining the structure of a macromolecule-ligand complex, comprising:

• producing a sample of a selected polycrystalline macromolecule-ligand complex, said sample produced by the steps comprising
• providing a quantity of substantially dehydrated macromolecules and a quantity of ligand molecules, and
• adding a liquid to said dehydrated macromolecules and said ligand molecules while physically agitating the mixture of said macromolecules and said ligands, wherein said polycrystallites of said macromolecule-ligand complex are formed;
• producing a sample of a selected polycrystalline macromolecule, said sample produced by the steps comprising
• providing a plurality quantity of substantially dehydrated macromolecules, and
• adding a liquid to said dehydrated macromolecules while physically agitating said macromolecules, wherein said polycrystallites of said macromolecule are formed;
• collecting powder diffraction data from said sample of said macromolecule and said sample of macromolecule-ligand complex;
• and
• analyzing said diffraction data to yield the structure of said macromolecule-ligand complex.

A method for preparing a sample containing microcrystallites of a macromolecule suitable for analysis by X-ray powder diffraction, comprising:

• (a) providing a quantity of substantially dehydrated macromolecules;
• (b) adding a liquid to said substantially dehydrated macromolecules;
• (c) physically agitating the mixture of step (b) in order to form said sample containing microcrystallites;
• and
• (d) placing said formed sample containing microcrystallites on or in an X-ray powder diffraction sample holder or container.

A method for preparing a sample containing microcrystallites of a macromolecule suitable for high resolution analysis by X-ray powder diffraction, comprising:

• (a) providing a solution of macromolecules;
• (b) inducing precipitation of macromolecules from said solution to form a microcrystalline sample;
• and
• (c) placing said formed microcrystalline sample on or in an X-ray powder diffraction sample holder or container.