ABSTRACT: The title compound, C(13)H(20)O(3)S(5), is bis-ected by a crystallographic twofold rotation axis, which relates the two halves of the mol-ecule to one another: one S, one C and one O atom lie on the axis. The thione S atom lies in the plane of the five-membered rings with an r.m.s. deviation of 0.0042?(5)?Å. Parts of the 17-membered macrocycle were refined using a two-part disorder model [occupancies of 0.553?(14) and 0.447?(14)]. There are no noteworthy inter-molecular inter-actions.
Project description:In the title compound, [Ni(C40H28N4S4)]·0.5C6H6, the Ni(II) atom is in a square-planar geometry defined by four pyrrole N atoms. There is considerable buckling in the porphyrin ring with the dihedral angles between the N4 donor set and the pyrrole rings being in the range 16.24?(5)-22.47?(5)°. Each of the six-membered chelate rings is twisted about an Ni-N bond and the dihedral angles between diagonally opposite chelate rings are 21.36?(4) and 23.87?(4)°; each pair of rings is oriented in opposite directions. The methyl-thienyl rings are twisted out of the plane of the central N4 core with dihedral angles in the range 75.98?(2)-88.70?(5)°. All four methyl-thienyl groups are disordered over two sets of sites, as is commonly found with such groups, with occupancies of 0.553?(8):0.447?(8), 0.579?(7):0.421?(7), 0.796?(6):0.204?(6) and 0.956?(7):0.044?(7). The benzene solvent mol-ecule was found to be present in half-occupancy.
Project description:In the crystal structure of the title compound, C(25)H(30)N(2)O(4), the steric size of the tert-butyl group causes the 3,5-dimethyl-phenyl ring to adopt a transoid geometry with respect to the N-C(O) bond. The six-membered heterocyclic ring is disordered over two sites, with occupancies of 0.553?(4) and 0.447?(4). Intra-molecular C-H?O inter-actions are present. In the crystal, mol-ecules are linked by inter-molecular N-H?O and C-H?O hydrogen bonds.
Project description:In the title mol-ecule, C(11)H(16)O(2)S(5), the two S atoms from the macrocycle are situated on opposite sides of the mean plane of the five-membered ring, deviating from it by 1.288?(3) and 1.728?(3)?Å. In the crystal, weak inter-molecular C-H?S and C-H?O hydrogen bonds link the mol-ecules into layers parallel to (100). The crystal studied was a racemic twin.
Project description:The title compound, [Cu4(C2O4)2(N3)4(C5H9N3)2]·0.9H2O, contains a tetranuclear Cu(II)-based molecule composed of two oxalate-bridged Cu(II) dimers linked through end-on azide ions and related by an inversion center. The tetranuclear unit contains two crystallographically independent Cu(II) ions. One Cu(II) ion coordinates to two N atoms of a histamine mol-ecule, two O atoms of a bridging oxalate ligand, and an N atom of an end-on bridging azide ligand, leading to an elongated square-pyramidal coordination geometry in which the azide ion occupies the axial position. The other Cu(II) ion, which has a square-planar coordination geometry, is coordinated by two O atoms of a bridging oxalate ligand and two N atoms of two different azide ligands, one which is bridging. In the crystal, a two-dimensional network parallel to (010) is formed by N-H?N and N-H?O hydrogen bonds. A partially occupied solvent water mol-ecule refined to an occupancy of 0.447?(5). Two of the azide ligands were refined as disordered over two sets of sites with refined occupancies in the ratios 0.517?(8):0.483?(8) and 0.553?(5):0.447?(5).
Project description:The asymmetric unit of the title compound, (C7H10N)2[HgBr4], consists of one cation and one half-anion, bis-ected by a twofold rotation axis passing through the metal atom. The anion exhibits a distorted tetra-hedral arrangement about the Hg(II) atom. In the crystal, the cations and anions are linked by N-H?Br hydrogen-bonding inter-actions along . Cation-cation ?-? stacking and Br?Br inter-molecular inter-actions are absent.
Project description:In the title compound, [PtCl(C(27)H(35)N(3))]Cl·C(7)H(8), the Pt(II) atom is coordinated in a pseudo-square-planar fashion by the N atoms of a 4,4',4''-tri-tert-butyl-2,2':6',2''-terpyridine (tbtrpy) ligand and a Cl atom. The Pt-N distance of the N atom on the central pyridine is 1.941?(4)?Å, while the peripheral N atoms have Pt-N distances of 2.015?(4) and 2.013?(4)?Å. The Pt-Cl bond distance is 2.3070?(10)?Å. The cations pack as dimers in a head-to-tail orientation with an inter-molecular Pt?Pt distance of 3.2774?(3)?Å and Pt?N distances of 3.599?(4), 3.791?(4) and 4.115?(4)?Å. The solvent mol-ecule is disordered and occupies two positions with a ratio of 0.553?(6):0.447?(6).
Project description:The reaction of bis-(anthracene)cobaltate(-I) with excess cyclo-hepta-triene, C7H8, resulted in a new 18-electron cobaltate containing two different seven-membered ring ligands, based on single-crystal X-ray diffraction. The asymmetric unit of this structure contains two independent cation-anion pairs of the title complex, [K(18-crown-6)][Co(?(3)-C7H7)(?(5)-C7H9)], where 18-crown-6 stands for 1,4,7,10,13,16-hexa-oxa-cyclo-octa-decane (C12H24O6), in general positions and well separated. Each (18-crown-6)potassium cation is in contact with the ?(3)-coordinating ligand of one cobaltate complex. Each ?(3)-coordinating ligand behaves as an allylic anion whose exo-diene moiety is bent away from the allylic plane, and thus is not involved directly in the bonding. The metal-coordinating portions of the anionic ?(5) ligands are planar and one of these ligands is modeled as disordered over two positions, with occupancy ratio 0.699?(5):0.301?(5), such that one orientation is rotated by one carbon atom with respect to the other. The diffraction intensities were integrated according to non-merohedral twin law [-1 0 0/0 -1 0/0.064 0 1], a 180° rotation about reciprocal lattice axis , and the masses of the twin domains refined to equal amounts. As both ligands are formally coordinated as anions, the cobalt atom is best considered to be Co(I). This compound is of inter-est as the first to possess cyclo-hepta-trienyl and cyclo-hepta-dienyl ligands in an anionic metal complex.
Project description:The whole mol-ecule of the title compound, C20H19NO4S2, is generated by twofold rotational symmetry. The N atom is located on the twofold rotation axis and has a trigonal-planar geometry. It is bonded by two S atoms of two symmetry-related 4-methyl-phenyl-sulfonyl groups and by the C atom of the phenyl ring, which is bis-ected by the twofold rotation axis. The benzene and phenyl rings are oriented at a dihedral angle of 51.48?(5)° while the pendant benzene rings are inclined to one another by 87.76?(9)°. In the crystal, weak C-H?O hydrogen bonds link the mol-ecules, forming a three-dimensional network.
Project description:In the title salt, [Ag(C27H36N2)2]Cl·C4H8O, the Ag(I) atom is coordinated by two 1,3-bis-(2,6-di-methyl-phen-yl)imidazol-2-yl-idene ligands. The imidazole rings are inclined to one another by 46.69?(13)° and the benzene rings in each ligand are almost normal to the imdazole ring to which they are attached, with dihedral angles varying from 82.39?(13) to 88.27?(12)°. There are C-H?? inter-actions present in the cation, involving the two ligands, and the solvent mol-ecule is linked to the cation via a C-H?O hydrogen bond. In the crystal, mol-ecules are linked by trifurcated C-H?(Cl,Cl,Cl) hydrogen bonds, forming slabs parallel to (101). One isopropyl group is disordered over two sets of sites with an occupancy ratio of 0.447?(17):0.553?(17) and the THF mol-ecule is disordered over two positions with an occupancy ratio of 0.589?(6):0.411?(6).
Project description:The mol-ecule of the title binuclear copper(II) complex, [Cu(2)(C(14)H(8)O(4))(2)(C(12)H(12)N(2))(2)(H(2)O)(2)], is bis-ected by a crystallographic twofold axis. Each Cu(II) atom is coordinated in a distorted octa-hedral geometry by three O atoms from two biphen-yl-2,2'-dicarboxyl-ate anions, one aqua O atom and two N atoms of a 4,4'-dimethyl-2,2'-bipyridine ligand. Intramolecular O-H?O hydrogen bonds between the coordinated water molecules and the carboxylate O atoms are also present.