Search

A single-crystal structure determination of the cubic phase of CsNO 3 based on data collected at 439 K up to sinθ max /λ = 0.995000 Å -1 , i.e. to an unprecedentedly high-θ value, is reported. The structure has been refined in Pm3m (Z = 1). Analysis of the difference electron-density maps revealed that the most appropriate model is the twelve-orientation model with the Cs, N, O1 and O2 atoms situated on the Wyckoff positions 1a, 6f, 6f and 24l, respectively, rather than the eight-orientation aragonite model with the Cs, N and O atoms situated on the Wyckoff positions 1a, 8g and 24m, respectively. Both models, however, show close similarities if the large anisotropic displacement parameters of the O atoms in the eight-orientation aragonite model are taken into account. The reason for this is shown to lie in the smeared electron density around the positions of the disordered [NO 3 ] - anion.

The mixed-amide phosphinates, rac-phenyl (N-methylcyclohexylamido)(p-tolylamido)phosphinate, C20H27N2O2P, (I), and rac-phenyl (allylamido)(p-tolylamido)phosphinate, C16H19N2O2P, (II), were synthesized from the racemic phosphorus-chlorine compound (R,S)-(Cl)P(O)(OC6H5)(NHC6H4-p-CH3). Furthermore, the phosphorus-chlorine compound ClP(O)(OC6H5)(NH-cyclo-C6H11) was synthesized for the first time and used for the synthesis of rac-phenyl (benzylamido)(cyclohexylamido)phosphinate, C19H25N2O2P, (III). The strategies for the synthesis of racemic mixed-amide phosphinates are discussed. The P atom in each compound is in a distorted tetrahedral (N(1))P(=O)(O)(N(2)) environment. In (I) and (II), the p-tolylamido substituent makes a longer P-N bond than those involving the N-methylcyclohexylamido and allylamido substituents. In (III), the differences between the P-N bond lengths involving the cyclohexylamido and benzylamido substituents are not significant. In all three structures, the phosphoryl O atom takes part with the N-H unit in hydrogen-bonding interactions, viz. an N-H···O=P hydrogen bond for (I) and (N-H)(N-H)···O=P hydrogen bonds for (II) and (III), building linear arrangements along [001] for (I) and along [010] for (III), and a ladder arrangement along [100] for (II).

The asymmetric unit in the title compound, C24H26N2O3, comprises two independent mol-ecules (A and B). In molecule A, the central 2-hydroxyphenyl ring is inclined to the mean plane of the major component of the imidazolidine ring by 84.52 (14)°, and by 68.08 (9) and 47.48 (9)° to the outer phenol rings. The later are inclined to one another by 66.76 (9)° and by 78.12 (14) and 80.20 (14)° to the imidazoline ring mean plane. In molecule B, the central 2-hydroxyphenyl ring is inclined to the mean plane of the imidazolidine ring by 73.64 (10)°, and by 75.60 (8) and 38.32 (9)° to the outer phenol rings. The later are inclined to one another by 69.47 (9)° and by 82.60 (10) and 64.26 (10)° to the imidazolidine ring mean plane. In each of the independent mol-ecules, two intra-molecular O-H⋯N hydrogen bond form S(6) ring motifs. In disordered mol-ecule A, the O-H groups of the 2-hy-droxy-benzyl groups are also involved in intra-molecular O-H⋯O hydrogen bonds, with the O atom of the hy-droxy-phenyl group acting as the acceptor. In the crystal, A molecules are linked by pairs of O-H⋯O hydrogen bonds forming inversion dimers. These dimers are linked to the B molecules via O-H⋯O hydrogen bonds forming double-layered slabs lying parallel to the bc plane.

Crystals of the title salt, C(21)H(20)OP(+)·NO(3) (-), are composed of acetonyltriphenyl-phospho-nium cations and nitrate anions that mainly inter-act through electrostatic forces. The P atom in the cation has a slightly distorted tetra-hedral environment, with C-P-C angles ranging from 104.79 (7) to 112.59 (6)°. The sum of O-N-O angles of the nitrate anion is 359.99°, reflecting its trigonal-planar character. C-H⋯O hydrogen bonds help to consolidate the crystal packing.

The title compound, C10H10N4, shows chemical but not crystallographic C2 symmetry. The two cyano-methyl groups are located in an anti position with respect to the aromatic ring. In the crystal, mol-ecules form parallel ladder-like tapes linked through two N-H⋯N hydrogen bonds. Further weak intra-molecular N-H⋯N hydrogen bonding is responsible for the elongation of one of the Caromatic-N bonds.

In the title compound, C(17)H(18)F(2)N(2)O(2), the imidazolidine ring system exists in a twist conformation. The mean plane through this ring system forms dihedral angles of 80.8 (8)° and 66.2 (13)°, with the benzene rings. The dihedral angle between the benzene rings is 52.0 (14)°. Two intra-molecular O-H⋯N hydrogen bonds each generate S(6) ring motifs. In the crystal, weak C-H⋯O hydrogen bonds form dimers, which are connected by further C-H⋯O inter-actions.