10QS

N-Alkyl & N-Aryl Aminopyrazole Spirocarbamates: A Two-Pronged Lead Optimization Strategy to Identify Orally Bioavailable Plasma Kallikrein Inhibitors Compound 13 ((3'R)-1'-{5-amino-1-[(2S)-1,1,1-trifluorobutan-2-yl]-1H-pyrazole-4-carbonyl}-6-chloro-5-fluorospiro[[3,1]benzoxazine-4,3'-piperidin]-2(1H)-one)

This is a non-PDB format compatible entry.

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	CLSI BEAMLINE 08B1-1
Synchrotron site	CLSI
Beamline	08B1-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2020-02-01
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.981920
Spacegroup name	P 21 21 2
Unit cell lengths	65.212, 74.503, 47.221
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	49.070 - 1.733
R-factor	0.2152
Rwork	0.213
R-free	0.25920
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	0.990
Data reduction software	autoPROC (1.1.7)
Data scaling software	autoPROC (1.1.7)
Phasing software	MOLREP (11.6.02)
Refinement software	BUSTER (2.11.7)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	49.070	1.937
High resolution limit [Å]	1.733	1.733
Number of reflections	15798	791
<I/σ(I)>	14.3
Completeness [%]	93.6
Redundancy	6.9
CC(1/2)	0.999	0.586

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	298	0.1 M MES, pH 6.5, 24% PEG8000, 5% glycerol