Crystal structure of bis(5-bromo-1,10-phenanthroline-?2 N,N')bis-[di-hydro-bis-(pyrazol-1-yl)borato-?2 N 2,N 2']iron(II) toluene disolvate.
ABSTRACT: The structure determination of the title compound was undertaken as part of a project on the modification and synthesis of new spin-crossover (SCO) compounds based on octa-hedral FeII bis-(pyrazol-yl)borate complexes. In the course of these investigations, the compound [Fe(C6H8BN4)2(C12H7BrN2)] was synthesized, for which magnetic measurements revealed an incomplete spin-crossover behaviour. Crystallization of this compound from toluene led to the formation of crystals of the toluene disolvate, [Fe(C6H8N4B)2(C12H7N2Br)]·2C7H8. Its asymmetric unit comprises two discrete metal complex mol-ecules and two toluene solvent mol-ecules. One of the latter is severely disordered and its contribution to the diffracted intensities was removed using the SQUEEZE routine [Spek (2015 ?). Acta Cryst. C71, 9-18]. In each complex mol-ecule, the FeII cation is coordinated by the two N atoms of a 5-bromo-1,10-phenanthroline ligand and by two pairs of N atoms of chelating di-hydro-bis(pyrazol-1-yl)borate ligands in the form of a slightly distorted octa-hedron. The discrete complexes are arranged in columns along the a-axis direction with the toluene solvate mol-ecules located between the columns. The 5-bromo-1,10-phenanthroline ligands of neighbouring columns are approximately parallel and are slightly shifted relative to each other, indicating ?-? inter-actions.
Project description:The asymmetric unit of the title compound, [Zn(C6H8N4B)2(C12H8N2)], comprises one half of a ZnII cation (site symmetry 2), one di-hydro-bis-(pyrazol-1-yl)borate ligand in a general position, and one half of a phenanthroline ligand, the other half being completed by twofold rotation symmetry. The ZnII cation is coordinated in form of a slightly distorted octa-hedron by the N atoms of a phenanthroline ligand and by two pairs of N atoms of symmetry-related di-hydro-bis-(pyrazol-1-yl)borate ligands. The discrete complexes are arranged into columns that elongate in the c-axis direction with a parallel alignment of the phenanthroline ligands, indicating weak π-π inter-actions.
Project description:The asymmetric unit of the title compound, [Fe(C13H18BN6)2], contains two half independent complex mol-ecules. In each complex, the FeII atom is located on an inversion center and is surrounded by two scorpionate ligand butyl-tris-(1H-pyrazol-1-yl)borate mol-ecules that coordinate to the iron(II) ion through the N atoms of the pyrazole groups. The two independent complex mol-ecules differ essentially in the conformation of the butyl substituents. In the crystal, the complex mol-ecules are linked by a series of C-H⋯π inter-actions, which generate a supra-molecular three-dimensional structure. At 120 K, the average Fe-N bond distance is 1.969 Å, indicating the low-spin state of the iron(II) atom, which does not change upon heating, as demonstrated by high-temperature magnetic susceptibility measurements.
Project description:In the title compound, [Cu(2)(C(10)H(12)O(4))(C(12)H(8)N(2))(2)(H(2)O)(2)](BF(4))(2)·H(2)O, the two Cu atoms are each chelated by the acetyl-acetonate unit of the 3,4-diacetyl-hexa-2,4-diene-2,5-diolate (tae) ligand. The Cu atoms are square-pyramidally penta-coordinated, with one bidentate 1,10-phenanthroline (phen) and the tae ligand basal and one water mol-ecule apical. The pyridyl rings of the phen ligands participate in ?-? [centroid-centroid distance = 3.894?(3)?Å] and C-H ? ? inter-actions, generating layers which are inter-connected through O-H?O and O-H?F hydrogen bonds between the water mol-ecules and the tetra-fluorido-borate anions. The F atoms of both tetra-fluorido-borate anions are each disordered over two positions of equal occupancy.
Project description:In the title complex, [Pd(N(3))(2)(C(12)H(8)N(2))], the Pd(II) ion is four-coordinated in a slightly distorted square-planar environment by two N atoms of the chelating 1,10-phenanthroline (phen) ligand and two N atoms from two azide anions. The azido ligands are slightly bent with bond angles of 174.8?(4) and 174.5?(5)°. The complex mol-ecules are stacked in columns along the a axis and are connected by inter-molecular C-H?N hydrogen bonds, forming a three-dimensional network. In the columns, numerous inter-molecular ?-? inter-actions between the six-membered rings are present, the shortest ring centroid-centroid distance being 3.607?(2)?Å.
Project description:The title compound, [Cu(3)(C(5)HN(2)O(4))(2)(C(12)H(8)N(2))(2)(H(2)O)(4)]·2H(2)O, is a trinuclear copper(II) complex in which two centrosymmetrically related pyrazole-3,5-dicarboxyl-ate(3-) and 1,10-phenanthroline ligands bind three Cu(II) atoms, with one Cu(II) atom located on a center of symmetry. In each complex, there are four coordinated water mol-ecules and two solvent water mol-ecules, which participate in extensive hydrogen-bond patterns. These inter-actions, as well as ?-? inter-actions between neighbouring 1,10-phenanthroline ligands [shortest atom-to-atom distance = 3.363?(3)?Å], extend the crystal structure into a three-dimensional supra-molecular network.
Project description:The title compound, [Mg(NCS)(2)(C(12)H(8)N(2))(2)], has been synthesized from the hydro-thermal reaction of MgCl(2), KSCN, 1,10-phenanthroline and H(2)O. Its structure is isotypic with the Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) analogues. The Mg(II) cation has a slightly distorted octa-hedral geometry containing four N atoms from two 1,10-phenanthroline mol-ecules and two N atoms from two thio-cyanate anions. The asymmetric unit contains one-half mol-ecule, and the complete complex has 2 symmetry.
Project description:In the title compound, [Mg(C(12)H(8)N(2))(2)(H(2)O)(2)][Cr(2)O(7)]·2C(12)H(8)N(2), the cation and anion are situated on a twofold rotation axis. The Mg(II) ion is coordinated by four N atoms from two 1,10-phenanthroline ligands and two O atoms from coordinated water mol-ecules in a distorted octa-hedral geometry. Inter-molecular O-H?N and O-H?O hydrogen bonds and ?-? inter-actions between the aromatic rings [shortest centroid-centroid separation = 3.527?(2)?Å] link the cations, anions and 1,10-phenanthroline solvent mol-ecules into a hydrogen-bonded cluster.
Project description:The title compound, [Co(C(12)H(8)N(2))(H(2)O)(4)](2)[Co(H(2)O)(6)](C(11)H(7)O(8))(2)·4H(2)O, was obtanied by the reaction of cobalt acetate with 3,5-bis-(carb-oxy-meth-oxy)benzoic acid and 1,10-phenanthroline. The asymmetric unit contains one tetra-aqua-(1,10-phenanthroline)cobalt(II) cation, one half of a hexa-aqua-cobalt(II) cation that is completed by inversion symmetry, one 3,5-bis-(carboxyl-atometh-oxy)benzoate trianion and two lattice water mol-ecules. The two Co(II) atoms each show a slightly distorted octa-hedral coordination (CoO(6) and CoO(4)N(2)). The cations, anions and lattice water mol-ecules are linked by an intricate network of O-H?O hydrogen bonds into a three-dimensional structure.
Project description:The crystal structure of the title compound, [Cu(SO4)(C12H8N2)2]·C2H5OH, arises from the assembly of the neutral complex [Cu(SO4)(C12H8N2)2] and an ethanol solvent mol-ecule. The Cu(II) ion is five-coordinate, surrounded by two pairs of N atoms from two independent N,N'-chelating 1,10-phenanthroline ligands, and one O atom of monodentate sulfate ligand, in a distorted trigonal-bipyramidal fashion. Spatial orientation of the ligands and the assembly in the solid state are stabilized by the C-H?O hydrogen-bonding inter-actions, established between the O atoms (from the sulfate ligand and the ethanol mol-ecule) and the neighbouring 1,10-phenanthroline mol-ecules. There is also an offset face-to-face ?-? stacking between the 1,10-phenanthroline ligands. The ethanol solvent mol-ecule is disordered over two orientations in the ratio 0.663?(10):0.337?(10). The crystal examined was subject to racemic twinning and the refined twin fraction was 0.346?(19).
Project description:The title complex, [Pr(C(7)H(5)O(3))(2)(NO(3))(C(12)H(8)N(2))]·2C(12)H(8)N(2), has a polymeric chain structure, with two uncoordinated 1,10-phenanthroline mol-ecules in the lattice. The Pr(III) centre has a monocapped square-anti-prismatic coordination geometry, comprised of two N atoms from one chelating 1,10-phenanthroline ligand, four carboxyl-ate O atoms from four 4-hy-droxy-benzoate anions and three O atoms from two nitrate anions. The 4-hy-droxy-benzoate and nitrate anions function as ?(2)-bridging ligands and link the Pr(III) ions into a one-dimensional chain structure along the c axis. Inter-molecular O-H?N hydrogen bonds are observed between the 4-hy-droxy-benzoate anions and the uncoordinated 1,10-phenanthroline mol-ecules.