10MV

N-Alkyl & N-Aryl Aminopyrazole Spirocarbamates: A Two-Pronged Lead Optimization Strategy to Identify Orally Bioavailable Plasma Kallikrein Inhibitors complex with Compound 15 ((3'R)-1'-(5-amino-1-phenyl-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	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	PIXEL
Collection date	2019-03-07
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.000000
Spacegroup name	P 21 21 2
Unit cell lengths	65.474, 77.959, 47.465
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.470 - 1.660
Rwork	0.206
R-free	0.22630
Structure solution method	MOLECULAR REPLACEMENT
Data reduction software	autoPROC (1.1.7)
Data scaling software	STARANISO (1.1.7)
Phasing software	PHASER (2.11.7)
Refinement software	autoBUSTER (2.11.7)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.137	1.833
High resolution limit [Å]	1.653	1.653
Number of reflections	20401	1018
<I/σ(I)>	12.6	1.6
Completeness [%]	93.9
Redundancy	6.5
CC(1/2)	0.999	0.672

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