2-(4-Bromo-phen-yl)-N-(3,4-di-fluoro-phen-yl)acetamide.

In the title compound, C14H10BrF2NO, the dihedral angle between the mean planes of the 4-bromo-phenyl and 3,4-di-fluoro-phenyl rings is 66.4 (1)°. These two planes are twisted by 40.0 (5) and 86.3 (2)°, respectively, from that of the acetamide group. In the crystal, N-H⋯O hydrogen bonds and weak C-H⋯O and C-H⋯F inter-actions form infinite chains along [100].

2-(4-Chloro-phen-yl)-N-(3,4-di-fluoro-phen-yl)acetamide.

In the title compound, C14H10ClF2NO, the dihedral angle between the mean planes of the 4-chloro-phenyl and 3,4-di-fluoro-phenyl rings is 65.2 (1)°. These two planes are twisted by 83.5 (5) and 38.9 (9)°, respectively, from that of the acetamide group. In the crystal, N-H⋯O hydrogen bonds form infinite chains along [100]. Weak C-H⋯O and C-H⋯F inter-actions are also observed and stack mol-ecules along the b axis.

(2E)-1-(4-Chloro-phen-yl)-3-(4-nitro-phen-yl)prop-2-en-1-one.

In the title compound, C15H10ClNO3, a substituted chalcone, the dihedral angle between the benzene rings is 5.1 (7)°. The nitro group makes a dihedral angle of 12.5 (3)° with the benzene ring to which it is attached. In the crystal, weak C-H⋯O inter-actions link the mol-ecules into a one-dimensional array along [010]. The crystal studied was an inversion twin, with a refined ratio for the twin components of 0.6060 (9):0.3939 (1).

Sequential [3 + 2] and [4 + 2] cycloadditions for stereoselective synthesis of a novel polyheterocyclic scaffold.

A strategy of combining [3 + 2] cycloaddition and intramolecular Diels-Alder reaction is developed for the synthesis of a novel polycyclic scaffold with skeletal and substitutional diversities. Intermediates generated from stereoselective [3 + 2] cycloaddition of azomethine ylides and maleimides were derivatized for intramolecular Diels-Alder reaction of furan to form highly condensed heterocyclic products as racemic single diastereomers.

Bosentan monohydrate.

In the title compound, C27H29N5O6S·H2O {systematic name: 4-tert-butyl-N-[6-(2-hy-droxy-eth-oxy)-5-(2-meth-oxy-phen-oxy)-2-(pyrimidin-2-yl)pyrimidin-4-yl]benzene-1-sulfonamide monohydrate], the dihedral angle between the mean planes of the pyrimidine rings is 27.0 (1)°. The dihedral angle between the mean planes of the benzene rings is 47.7 (8)°, forming a U-shaped channel around the chain of twisted pyrimidine rings. The crystal packing is stabilized by O-H⋯O, O-H⋯N and N-H⋯O hydrogen bonds with a single water mol-ecule, and weak O-H⋯N inter-molecular inter-actions between the hy-droxy group and one of the pyrimidine rings producing an two-dimensional supra-molecular array in the bc plane. The title compound studied was a merohedral twin with the major component being approximately 57%.

Diphenyl-methyl benzoate.

In the title mol-ecule, C20H16O2, the dihedral angle between the phenyl rings of the diphenyl-methyl group is 68.3 (2)°. The benzoate group is essentially planar, with a maximum deviation of 0.017 (2) Šfor the carbonyl O atom, and the two phenyl rings are twisted by 27.5 (4) and 85.6 (9)° from this plane. In the crystal, weak C-H⋯O hydrogen bonds link mol-ecules along [100].

Ethyl 6-(6-meth-oxy-naphthalen-2-yl)-4-(naphthalen-2-yl)-2-oxocyclo-hex-3-ene-1-carboxyl-ate.

The title compound, C30H26O4, contains an oxo-cyclo-hexane ring in a distorted half-chair configuration, with disorder of two C atoms in a 0.859 (4):0.141 (4) ratio. The dihedral angle between the mean planes of the two napthalene ring systems is 58.6 (8)°.

(E)-N'-(4-Fluoro-benzyl-idene)-2-(3-methyl-phen-yl)acetohydrazide.

In the title compound, C16H15FN2O, the dihedral angles between the benzene rings are74.7(8), 74.1 (1), 74.2 (7) and 74.3 (5)° in the four independent mol-ecules in the asymmetric unit. In the crystal, N-H-O hydrogen bonds involving the hydrazide and acetyl groups, which form R2(2)(18) ring motifs, link the mol-ecules into dimers, which form columns along [010].

Olanzapinium dipicrate.

THE ASYMMETRIC UNIT OF THE TITLE SALT [SYSTEMATIC NAME: 2-methyl-4-(4-methyl-piperazin-4-ium-1-yl)-10H-thieno[2,3-b][1,5]benzodiazepinium bis-(2,4,6-trinitro-phenolate)], C(17)H(22)N(4)S(2+)·2C(6)H(2)N(3)O(7) (-), consists of a diprotonated olanzapinium cation and two independent picrate anions. In the cation, the piperazine ring adopts a distorted chair conformation and contains a positively charged N atom with quaternary character and the N atom in the seven-membered 1,5-diazepine ring, which adopts a boat configuration, is also protonated. The dihedral angle between the benzene and thiene rings flanking the diazepine ring is 58.8 (1)°. In one of the picrate anions, a nitro group is disordered over two sets of sites in a 0.748 (5):0.252 (5) ratio, and the benzene ring has a flat envelope conformation with the O(-) C atom displaced from the mean plane of the other five C atoms [maximum deviation 0.0151 (14) Å] by 0.1449 (14) Å. In the crystal, N-H⋯O hydrogen bonds and weak inter-molecular C-H⋯S and C-H⋯O inter-actions link the components, forming a three-dimensional network.

Orphenadrinium dihydrogen citrate.

In the title salt, C(18)H(24)NO(+)·C(6)H(7)O(7) (-), the dihedral angle between the benzene rings in the cation is 74.2 (5)°. In the crystal, anion-anion O-H⋯O hydrogen bonds and weak O-H⋯O inter-actions form infinite chains along [100]. Between these chains, cation-anion N-H-O hydrogen bonds are observed, forming an alternate pattern of cation and anion layers and leading to a two-dimensional network parallel to (100).

Trimethyl-ammonium dichlorido-triphenyl-stannate(IV).

In the structure of the title monomeric coordination salt, (C(3)H(10)N)[Sn(C(6)H(5))(3)Cl(2)], the Sn(IV) atom is five coordinate, with the SnC(3)Cl(2) entity in a trans trigonal-bipyramidal arrangement and the chlorine atoms in apical positions. In the crystal, the cations and anions are connected by N-H⋯Cl hydrogen bonds.

[2-(Biphenyl-4-yl)-1,3-thia-zol-4-yl]methanol.

In the title compound, C(16)H(13)NOS, the central benzene ring makes dihedral angles of 3.25 (7) and 41.32 (8)°, respectively, with the thia-zole and phenyl rings. In the crystal, O-H⋯N hydrogen bonds link the mol-ecules into a chain along the c axis. A weak C-H⋯O inter-action further connects the chains into a layer parallel to the ac plane.

N,N'-Dibenzyl-N''-(2-chloro-2,2-difluoro-acet-yl)phospho-ric triamide.

In the title mol-ecule, C(16)H(17)ClF(2)N(3)O(2)P, the N-H unit of the C(=O)NHP(=O) fragment adopts a syn orientation with respect to the P=O group. The two F atoms and the Cl atom of the ClF(2)C group are disordered over two sets of sites with refined occupancies of 0.605 (6) and 0.395 (6). In the crystal, mol-ecules are linked via N-H⋯O=C hydrogen bonds the and the (N-H⋯)(N-H⋯)O=P group into chains along [010].

Three new [XC(O)NH]P(O)[N(CH2C6H5)2]2 phosphoric triamides (X = CClF2, 3-F-C6H4 and 3,5-F2-C6H3): a database analysis of tertiary N-atom geometry in compounds with a C(O)NHP(O)[N]2 core.

In the phosphoric triamides N,N,N',N'-tetrabenzyl-N''-(2-chloro-2,2-difluoroacetyl)phosphoric triamide, C(30)H(29)ClF(2)N(3)O(2)P, (I), N,N,N',N'-tetrabenzyl-N''-(3-fluorobenzoyl)phosphoric triamide, C(35)H(33)FN(3)O(2)P, (II), and N,N,N',N'-tetrabenzyl-N''-(3,5-difluorobenzoyl)phosphoric triamide, C(35)H(32)F(2)N(3)O(2)P, (III), the tertiary N atoms of the dibenzylamido groups have sp(2) character with minimal deviation from planarity. The sums of the three bond angles about the N atoms in (I)-(III) deviate by less than 8° from the planar value of 360°. The geometries of the tertiary N atoms in all phosphoric triamides with C(O)NHP(O)[N](2) skeletons deposited in the Cambridge Structural Database [CSD; Allen (2002). Acta Cryst. B58, 380-388] have been examined and the bond-angle sums at the two tertiary N atoms (SUM1 and SUM2) and the parameter ΔSUM (= SUM1 - SUM2) considered. It was found that in compounds with a considerable ΔSUM value, the more pyramidal N atoms are usually oriented so that the corresponding lone electron pair is anti with respect to the P=O group. In (I), (II) and (III), the phosphoryl and carbonyl groups, separated by an N atom, are anti with respect to each other. In the C(O)NHP(O) fragment of (I)-(III), the P-N bond is longer and the O-P-N angle is contracted compared with the other two P-N bonds and the O-P-N angles in the molecules. These effects are also seen in analogous compounds deposited in the CSD. Compounds with [C(O)NH]P(O)[N]X (X ≠ N), such as compounds with a [C(O)NH]P(O)[N][O] skeleton, have not been considered here. Also, compounds with a [C(O)NH](2)P(O)[N] fragment have not been reported to date. In the crystal structures of all three title compounds, adjacent molecules are linked via pairs of P=O···H-N hydrogen bonds, forming dimers with C(i) symmetry.

N,N-Dicyclo-hexyl-cyclo-hexa-ne-carboxamide.

In the title compound, C(19)H(33)NO, all three cyclo-hexane rings adopt chair conformations. The crystal packing features weak C-H⋯O inter-actions, forming a supra-molecular chain along the c axis.

1-{4-[Bis(4-fluoro-phen-yl)meth-yl]piperazin-1-yl}ethanone.

In the title compound, C(19)H(20)F(2)N(2)O, the six-membered piperazine group adopts a slightly distorted chair conformation. The dihedral angle between the mean planes of the two benzene rings is 73.4 (6)°. The mean plane of the ethanone group is twisted from the mean planes of the two benzene rings by 66.7 (8) and 86.2 (6)°. In the crystal, C-H⋯O and C-H⋯F inter-actions link the molecules, forming a three-dimensional structure.

Di-µ-bromido-bis-{[N,N-dimethyl-N'-(thio-phen-2-yl-methyl-idene)ethane-1,2-diamine]-copper(I)]}.

In the crystal structure of the title compound, [Cu(2)Br(2)(C(9)H(14)N(2)S)(2)], the mol-ecule resides about a crystallographic inversion center. The coordination sphere around each copper ion has a distorted tetra-hedral geometry, with ligation by two bridging bromide ions, an amine N atom and an imine N atom. The thio-phene ring is disordered over two sites, with occupancies of 0.719 (3) and 0.281 (3). Weak C-H⋯π inter-actions feature in the crystal packing.

5-(Thio-phen-2-ylmeth-yl)-1,3,4-thia-diazol-2-amine.

In the title mol-ecule, C(7)H(7)N(3)S(2), the dihedral angle between the thio-phene and thia-diazole rings is 72.99 (5)°; the two rings are oriented so that the S atoms in each ring are on the same side. In the crystal, the three-dimensional network involves strong N-H⋯O hydrogen bonds, as well as C-H⋯π and π-π stacking inter-actions [centroid-centroid distances = 3.654 (1) and 3.495 (1) Å].

2-(2-Nitro-phen-yl)acetohydrazide.

In the title compound, C8H9N3O3, the dihedral angle between the benzene ring and the acetohydrazide C-C(=O)-N-N plane [maximum deviation = 0.0471 (13) Å] is 87.62 (8)°. The nitro group is twisted by 19.3 (2)° with respect to the benzene ring. In the crystal, N-H⋯O hydrogen bonds link the mol-ecules into a double-column structure along the b axis.

(E)-N'-(4-Meth-oxy-benzyl-idene)-2-m-tolyl-acetohydrazide.

In the title mol-ecule, C17H18N2O2, the benzene rings form a dihedral angle of 83.0 (7)°. In the crystal, N-H⋯O hydrogen bonds, in an R(2)2(8) graph-set motif, link mol-ecules into centrocymmetric dimers, and weak C-H⋯π inter-actions further link these dimers into columns in [100].