Recent advances in the CRANK software suite for experimental phasing.

For its first release in 2004, CRANK was shown to effectively detect and phase anomalous scatterers from single-wavelength anomalous diffraction data. Since then, CRANK has been significantly improved and many more structures can be built automatically with single- or multiple-wavelength anomalous diffraction or single isomorphous replacement with anomalous scattering data. Here, the new algorithms that have been developed that have led to these substantial improvements are discussed and CRANK's performance on over 100 real data sets is shown. The latest version of CRANK is freely available for download at http://www.bfsc.leidenuniv.nl/software/crank/ and from CCP4 (http://www.ccp4.ac.uk/).

CRANK: new methods for automated macromolecular crystal structure solution.

CRANK is a novel suite for automated macromolecular structure solution and uses recently developed programs for substructure detection, refinement, and phasing. CRANK utilizes methods for substructure detection and phasing and combines them with existing crystallographic programs for density modification and automated model building in a convenient and easy-to-use CCP4i graphical interface. The data model used conforms to the XML eXtensible Markup Language specification and works as a common language to communicate data between many different applications inside and outside of the suite. The application of CRANK on various test cases has yielded promising results: with minimal user input, CRANK can produce better quality solutions over currently available programs.

Synthesis, Characterization, and Single-Crystal EPR Studies of Three Dinuclear Copper(II) Complexes and One Mixed-Valence Tetranuclear Copper(I)-Copper(II) Cluster with an Asymmetric Imidazole-Containing Tripodal Ligand with Copper(II)-Copper(II) Distances between 3.35 and 3.63 Å

The synthesis and characterization of three dinuclear copper(II) complexes and one mixed-valence tetranuclear cluster with the asymmetric imidazole-containing ligand bis(1,1'-imidazole-2-yl)(4-imidazole-4(5)-yl)-2-azabutane (biib) are described. X-ray crystallographic parameters for the copper complexes are as follows. [Cu(2)(biib)(2)(BF(4))(2)](BF(4))(2)(H(2)O)(4): triclinic, space group P&onemacr;, a = 10.178(1) Å, b = 9.4881(9) Å, c = 11.037(1) Å, alpha = 95.130(10) degrees, beta = 112.20(1) degrees, gamma = 92.142(9) degrees, and Z = 1. [Cu(2)(biib)(2)(NO(3))(2)](NO(3))(2)(H(2)O)(4): monoclinic, space group &Pmacr;2(1)/n, a = 9.207(6) Å, b = 17.0516(6) Å, c = 12.6107(7) Å, beta = 109.82(1) degrees, and Z = 2. [Cu(2)(biib)(2)(CuBr(3))(2)]: monoclinic, space group P2(1)/c, a = 11.583(2) Å, b = 11.864(2) Å, c = 16.070(2) Å, beta = 112.459(12) degrees, and Z = 2. The two Cu(II) ions in all four complexes are coordinated in a square-pyramidal geometry by three imidazole nitrogens and one amine nitrogen donor in the equatorial plane, and each copper ion is weakly coordinated at the axial position by respectively a tetrafluoroborate, a perchlorate, a nitrate, or a tribromocuprate(I) anion. By comparison of the structural data of the four complexes a relationship has been established between the donor strength of the anion and some structural features, like the Cu(II)-Cu(II) distance, of the dinuclear Cu(II)-Cu(II) unit in the four complexes. Single-crystal EPR spectra of [Cu(2)(biib)(2)(BF(4))(2)](BF(4))(2)(H(2)O)(4) were recorded at room temperature at X-band frequencies. The triplet spectra have been fit with nonparallel g and D tensors, whose principle values are as follows: g(xx)() = 2.022(8), g(yy)() = 2.060(7), g(zz)() = 2.211(8), D(x)()(')(x)()(') = -0.0182(9) cm(-)(1), D(y)()(')(y)()(') = -0.081(6) cm(-)(1), D(z)()(')(z)()(') = 0.0264(7) cm(-)(1). The compounds were further characterized and studied by ligand field and by frozen-solution and polycrystalline powder EPR spectroscopy. EPR spectra recorded at 77 K of frozen solutions of the perchlorate complex show that upon dilution in methanol the dinuclear complex reacts to form a mononuclear species.