1V3X

Factor Xa in complex with the inhibitor 1-[6-methyl-4,5,6,7-tetrahydrothiazolo(5,4-c)pyridin-2-yl] carbonyl-2-carbamoyl-4-(6-chloronaphth-2-ylsulphonyl)piperazine

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	vapor diffusion, macro-seeding, Soaking	5	293	PEG6000, sodium acetate, Malate imidazole, Calcium chloride, pH 5.00, vapor diffusion, macro-seeding, Soaking, temperature 293K

Crystal Properties
Matthews coefficient	Solvent content
2.49	50.54

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 56.05	α = 90
b = 71.927	β = 90
c = 78.799	γ = 90

Symmetry
Space Group	P 21 21 21

Diffraction

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	100	IMAGE PLATE	RIGAKU		1998-12-03	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	ROTATING ANODE	RIGAKU	1.5418

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Merge I (Observed)	R Sym I (Observed)	Net I Over Average Sigma (I)	Redundancy	Number Reflections (All)	Number Reflections (Observed)	Observed Criterion Sigma (F)	Observed Criterion Sigma (I)	B (Isotropic) From Wilson Plot
1	2.2	53.124	96	0.044	0.044	13.6	3.1	15999	15999			35.621

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	R-Sym I (Observed)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
	2.2	2.27	90.4		0.259	0.259	2.9	2.6	1332

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Starting model	Resolution (High)	Resolution (Low)	Number Reflections (All)	Number Reflections (Observed)	Number Reflections (R-Free)	Percent Reflections (Observed)	R-Factor (All)	R-Factor (Observed)	R-Work	R-Free	R-Free Selection Details	Mean Isotropic B
X-RAY DIFFRACTION	RIGID BODY REFINEMENT	THROUGHOUT	1FAX	2.2	25	15207	15207	751	100	0.19374	0.19374	0.1917	0.23302	RANDOM	35.912

Temperature Factor Modeling
Anisotropic B[1][1]	Anisotropic B[1][2]	Anisotropic B[1][3]	Anisotropic B[2][2]	Anisotropic B[2][3]	Anisotropic B[3][3]
1.55			-2.16		0.61

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_1_deg	6.971
r_scangle_it	3.331
r_mcangle_it	2.604
r_scbond_it	2.339
r_angle_refined_deg	1.798
r_mcbond_it	1.582
r_nbd_refined	0.214
r_symmetry_hbond_refined	0.186
r_xyhbond_nbd_refined	0.172
r_symmetry_vdw_refined	0.163

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_1_deg	6.971
r_scangle_it	3.331
r_mcangle_it	2.604
r_scbond_it	2.339
r_angle_refined_deg	1.798
r_mcbond_it	1.582
r_nbd_refined	0.214
r_symmetry_hbond_refined	0.186
r_xyhbond_nbd_refined	0.172
r_symmetry_vdw_refined	0.163
r_chiral_restr	0.117
r_metal_ion_refined	0.115
r_bond_refined_d	0.019
r_gen_planes_refined	0.007

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	2146
Nucleic Acid Atoms
Solvent Atoms	161
Heterogen Atoms	37

Software

Software
Software Name	Purpose
MOSFLM	data reduction
SCALA	data scaling
REFMAC	refinement
CCP4	data scaling

RCSB PDB Core Operations are funded by the National Science Foundation (DBI-1832184), the US Department of Energy (DE-SC0019749), and the National Cancer Institute, National Institute of Allergy and Infectious Diseases, and National Institute of General Medical Sciences of the National Institutes of Health under grant R01GM133198.