4RSZ

The X-ray structure of the Primary Adduct formed in the Reaction between Cisplatin and Cytochrome c

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	ENRAF-NONIUS FR571
Temperature [K]	100
Detector technology	CCD
Collection date	2014-07-21
Detector	RIGAKU SATURN 944
Wavelength(s)	1.5418
Spacegroup name	P 3
Unit cell lengths	120.344, 120.344, 36.673
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	104.220 - 2.190
R-factor	0.23403
Rwork	0.231
R-free	0.28211
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PDB code 1HRC
RMSD bond length	0.015
RMSD bond angle	1.845
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall
Low resolution limit [Å]	104.220
High resolution limit [Å]	2.190
Rmerge	0.109
Number of reflections	30538
Completeness [%]	99.8
Redundancy	10.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	300	A new crystal form of horse heart cytochrome c that co-crystallized with nitrate and sulphate ions has been obtained. Crystallization was prepared by using the hanging-drop vapour diffusion method in Linbro plates and a reservoir contained 3.5 M ammonium sulphate, 0.6 M sodium nitrate. The droplets consisted of 1 microliter protein (30 mg/mL in water) and 1 microliter of reservoir. They were equilibrated against a 500 microliters reservoir solution at 20 C. These conditions produced well shaped red crystals after 1 month. These crystals have been soaked for 24 h in a solution consisting of 0.005 M cisplatin in 2.0 M ammonium sulphate and 0.4 M sodium nitrate. To prepare this solution, Cisplatin was first dissolved in 5 mM sodium acetate buffer at pH 5.0. , VAPOR DIFFUSION, HANGING DROP, temperature 300K