TABLE 3.

Summary of diffraction data and structure refinement statistics

	Caspase-3
	Compound I	Compound II	Compound III	Compound IV
Statistics of diffraction data
Wavelength (Å)	1.0000	1.0000	1.0000	1.0000
Resolution range (Å)a	50.0–2.50 (2.59–2.50)	50.0–2.80 (2.90–2.80)	50.0–2.60 (2.69–2.60)	50.0–2.40 (2.49–2.40)
Space group	P212121	P212121	P212121	P212121
Cell parameters
a (Å)	65.1	65.7	65.4	65.2
b (Å)	96.9	96.5	96.7	96.3
c (Å)	180.4	180.5	180.4	180.2
Observed reflections	180,300	137,332	156,710	196,328
Unique reflections	36,312	27,196	35,800	41,447
Average redundancy	5.0 (4.7)	5.0 (4.7)	4.4 (3.0)	4.7 (2.9)
Average I/σ(I)	13.9 (2.0)	15.0 (1.9)	13.2 (1.3)	17.1 (1.8)
Completeness (%)	90.1 (70.8)	94.3 (94.7)	99.2 (94.1)	91.5 (90.8)
Rmerge (%)b	11.4 (43.5)	12.8 (53.0)	12.1 (48.2)	9.1 (39.6)
Statistics of refinement
Number of reflections	36,280	27,133	35,739	41,413
Working set	34,487	25,767	33,954	39,360
Free R set	1,793	1,366	1,785	2,053
R factor (%)c	20.8	21.1	21.4	20.9
Free R factor (%)	26.8	29.1	27.4	25.3
Number of residues	930	933	930	936
Number of water molecules	181	74	124	241
Average B factor of all atoms (Å2)	59.9	72.4	61.7	56.3
Caspase-3	60.0	72.6	61.9	56.4
Inhibitor	48.8	63.0	50.6	48.5
Water molecule	55.4	53.8	50.7	53.7
r.m.s. deviationd bond lengths (Å)	0.010	0.012	0.010	0.009
r.m.s. deviation bond angles (°)	1.2	1.4	1.2	1.2
Ramachandran plot (%)
Ramachandran favored	96.3	95.3	96.5	97.2
Ramachandran allowed	99.7	99.6	99.6	99.8
Ramachandran outliers	0.3	0.4	0.4	0.2

^aNumbers in parentheses refer to the highest resolution shell

^bR_merge = Σ_hklΣ_i|I_i(hkl)_i – 〈I(hkl)〉|/Σ_hklΣ_iI_i(hkl)

^cR_factor = Σ_hkl||F_o| – |F_c||/Σ_hkl|F_o|

^dr.m.s. deviation, root mean square deviation