Browse
Submit Data
Databases
API
Help

Dataset Information

0 Views

0 Connections

0 Citations

0 Reanalyses

0 Downloads

Omics score: 0

Nitro-sonium complexation by the tetra-phospho-nate cavitand 5,11,17,23-tetra-methyl-6,10:12,16:18,22:24,4-tetra-kis-(phenyl-phospho-nato-?²O,O)resorcin(4)arene.

ABSTRACT: The crystal structure of a new supra-molecular complex between the tetra-phos-pho-nate cavitand 5,11,17,23-tetra-methyl-6,10:12,16:18,22:24,4-tetra-kis(phenyl-phospho-nato-?²O,O')resorcin(4)arene and the nitrosyl cation NO⁺, as the BF₄^- salt, is reported. The complex, of general formula [(C₅₆H₄₄P₄O₁₂)(NO)]BF₄·CH₂Cl₂ or NO@Tiiii[H, CH₃, C₆H₅] BF₄·CH₂Cl₂, crystallizes in the space group P-1. The nitrosyl cation is disordered over two equivalent positions, with occupancies of 0.503?(2) and 0.497?(2), and inter-acts with two adjacent P=O groups at the upper rim of the cavitand through dipole-charge inter-actions. In the lattice, the cavitands are connected through a series of C-H?? inter-actions involving the methyl and methyl-enic H atoms and the aromatic rings of the macrocycle. The structure is further stabilized by the presence of C-H?F inter-actions between the hydrogen atoms of the cavitands and the F atoms of the tetra-fluorido-borate anion. As a result of the disorder, the lattice di-chloro-methane mol-ecules could not be modelled in terms of atomic sites, and were treated using the PLATON SQUEEZE procedure [Spek (2015 ?). Acta Cryst. C71, 9-18]. The complexation process has also been studied in solution through NMR titrations.

SUBMITTER: Pinalli R

PROVIDER: S-EPMC5730227 | biostudies-literature | 2017 Dec

REPOSITORIES: biostudies-literature

ACCESS DATA

Json Xml

Similar Datasets

7,11,15,28-Tetra-bromo-1,21,23,25-tetra-phenethyl-resorcin[4]arene cavitand-acetone-chloro-form (1/1.31/0.69)?at 173?K.

Project description:The crystal structure of the title compound, C(64)H(52)Br(4)O(8)·1.31C(3)H(6)O·0.69CHCl(3), is described. The structure has been reported previously [Bryant, Blanda, Vincenti & Cram (1991). J. Am. Chem. Soc.113, 2167-2172]; however, the lower data acquisition temperature results in an improved refinement model. In addition, the presence of residual acetone and (disordered) chloro-form within the mol-ecular structure of the title compound represents a new clathrate of the title compound. One half of the resorcin[4]arene cavitand mol-ecule appears in the asymmetric unit; the complete resorcin[4]arene cavitand structure was generated across a mirror plane.

| S-EPMC2968614 | biostudies-literature

7,11,15,28-Tetra-kis[(2-formyl-phen-oxy)methyl]-1,21,23,25-tetra-methyl-resorcin[4]arene cavitand ethyl acetate clathrate at 173 K.

Project description:The title compound, C(68)H(56)O(16), was synthesized as a novel synthetic inter-mediate towards deeper and more elaborate resorcin[4]arene cavitands. The structure is the first reported example of a resorcin[4]arene cavitand bearing aromatic aldehyde functional groups at the extra-annular rim of the mol-ecule. The 2-formyl-phen-oxy residues are found to assume two different orientations above the mol-ecular cavity. One half of the resorcin[4]arene cavitand mol-ecule appears in the asymmetric unit; the complete resorcin[4]arene cavitand structure was generated across a mirror plane. In addition, a highly disordered ethyl acetate solvent mol-ecule is present within the mol-ecular cavity.

| S-EPMC2968874 | biostudies-literature

Crystal structure of a host-guest complex between mephedrone hydro-chloride and a tetra-phospho-nate cavitand.

Project description:A new supra-molecular complex (I) between the tetra-phospho-nate cavitand Tiiii[C3H7,CH3,C6H5] [systematic name: 2,8,14,20-tetra-propyl-5,11,17,23-tetra-methyl-6,10:12,16:18,22:24,4-tetra-kis-(phenyl-phospho-nato-O,O')resorcin[4]arene] and mephedrone hydro-choride {C11H16NO+·Cl-; systematic name: meth-yl[1-(4-methyl-phen-yl)-1-oxopropan-2-yl]aza-nium chloride} has been obtained and characterized both in solution and in the solid state. The complex of general formula (C11H16NO)@Tiiii[C3H7,CH3,C6H5]Cl·CH3OH or C11H16NO+·Cl-·C68H68O12P4·CH3OH, crystallizes in the monoclinic space group P21/c with one lattice methanol mol-ecule per cavitand, disordered over two positions with occupancy factors of 0.665?(6) and 0.335?(6). The mephedrone guest inter-acts with the P=O groups at the upper rim of the cavitand through two charge-assisted N-H?O hydrogen bonds, while the methyl group directly bound to the amino moiety is stabilized inside the ? basic cavity via cation?? inter-actions. The chloride counter-anion is located between the alkyl legs of the cavitand, forming C-H?Cl inter-actions with the aromatic and methyl-enic H atoms of the lower rim. The chloride anion is also responsible for the formation of a supra-molecular chain along the b-axis direction through C-H?Cl inter-actions involving the phenyl substituent of one phospho-nate group. C-H?O and C-H?? inter-actions between the guest and adjacent cavitands contribute to the formation of the crystal structure.

| S-EPMC6362660 | biostudies-literature

5,11,17,23-Tetra-tert-butyl-25,26,27,28-tetra-propyn-yloxy-2,8,14,20-tetra-thia-calix[4]arene.

Project description:THE TITLE COMPOUND [SYSTEMATIC NAME: 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetra-propyn-yloxy-2,8,14,20-tetra-thia-calix[4]arene], C(52)H(56)O(4)S(4), is an alkyl-ated product bearing four propyne groups at the lower rim of a 5,11,17,23-tetra-tert-butyl-tetrathia-calix[4]arene. The mol-ecule is located on a crystallographic twofold rotation axis, running through two S atoms and perpendicular to the long axis of the mol-ecule. The four propyne groups, located in an alternate fashion above and below the mean plane of the four S atoms, are almost parallel to the calixarene long axis. The dihedral angle between the two crystallographically independent benzene rings is 86.77?(14)°. Two tert-butyl groups are disordered over two positions with site occupancies of 0.59?(2) and 0.41?(2).

| S-EPMC2972022 | biostudies-literature

25,26,27,28-Tetra-butoxy-5,11,17,23-tetra-tert-butyl-calix[4]arene chloro-form tetra-solvate dihydrate.

Project description:The title compound, C(60)H(88)O(4)·4CHCl(3)·2H(2)O, is the alkyl-ated product of 5,11,17,23-tetra-tert-butyl-calix[4]arene. It adopts a distorted cone conformation which leads to an open cavity. All the phenolic rings are tilted so that their tert-butyl groups are pitched away from the calix cavity. Two opposite aromatic rings are close to being perpendicular to one another [dihedral angle 85.0?(2)°], while the other pair of opposite rings is almost parallel [dihedral angle 8.1?(2)°], and adjacent phenolic rings are almost perpendicular [dihedral angles 82.4?(1) or 87.9?(1)°]. In the crystal, the water molecule and calixarene interact by way of O-H?O hydrogen bonds.

| S-EPMC2969488 | biostudies-literature

2-(4-Bromo-benz-yl)-5,11,17,23-tetra-tert-butyl-25,26,27,28-tetra-methoxy-calix[4]arene.

Project description:In the title compound, C(55)H(69)BrO(4), the calixarene mol-ecule displays a 'partial cone' conformation bearing the lateral substituent in a sterically favorable equatorial arrangement between two syn-orientated arene units. The crystal packing is stabilized by weak C-H?? contacts, involving one tert-butyl group, and ?-stacking inter-actions of the lateral bromo-benzene units [centroid-centroid distance = 3.706?(1)?Å].

| S-EPMC2969344 | biostudies-literature

5,11,17,23-Tetra-kis(chloro-meth-yl)-25,26,27,28-tetra-propoxycalix[4]arene.

Project description:The title calix[4]arene, C(44)H(52)Cl(4)O(4), displays the 1,3-alternate conformation with crystallographically imposed twofold symmetry. Four phenolic rings of the calixarene backbone are tilted into the calix cavity, making dihedral angles of 77.42?(2) and 77.71?(2)° with the plane of the four bridging methyl-ene C atoms. Pairs of opposite aromatic rings make dihedral angles of 25.16?(3) and 24.58?(4)° with each other. In the crystal, the calixarene mol-ecules pack with the formation of infinite columns along the b axis. The crystal packing shows a network of C-H?Cl contacts, which can be considered as non-classical hydrogen bonds.

| S-EPMC3052014 | biostudies-other

7,11,15,28-Tetra-methyl-1,21,23,25-tetra-kis(2-phenyl-ethyl)resorcin[4]arene ethyl acetate clathrate.

Project description:The title compound, C(68)H(64)O(8)·C(4)H(8)O(2), is a new resorcin-[4]arene cavitand synthetic precursor, obtained by alkyl-ation of a previously reported resorcin[4]arene. The additional alkyl bridges significantly rigidify the structure and enforce a 'bowl' shape on the mol-ecular cavity. In the crystal structure, the mol-ecule lies on a crystallographic mirror plane, and a single ethyl acetate mol-ecule (also lying on the mirror plane) is present within the compound cavity, illustrating the host capabilities of the mol-ecule.

| S-EPMC2915052 | biostudies-literature

4,10,16,22-Tetra-kis(2-chloro-acet-oxy)-6,12,18,24-tetra-meth-oxy-2,8,14,20-tetra-pentyl-resorcin[4]arene.

Project description:The title compound, C(60)H(76)Cl(4)O(12), has a macrocyclic structure and both the upper and lower rim have disordered atoms. There are no hydrogen bonds or ?-? stacking inter-actions in the crystal.

| S-EPMC3247323 | biostudies-literature

Poly[tetra-butyl-tetra-kis-(μ(2)-hydrogen phenyl-phospho-nato)ditin(IV)].

Project description:In the title compound, [Sn(2)(C(4)H(9))(4)(C(6)H(6)PO(3))(4)](n), the basic unit is a dimer containing two symmetry-related Sn(IV) atoms bridged by two hydrogenphenylphosphonate anions. This fragment is located about an inversion center, and each Sn(IV) atom is linked to two other hydrogenphenylphosphonate anions, giving a layered structure parallel to (010). The coordination geometry for the Sn(IV) atoms is close to octa-hedral. The layers are connected via O-H⋯O hydrogen bonds, generating a three-dimensional network. One butyl group is disordered over two sets of sites, with occupancies of 0.49 (2) and 0.51 (2).

| S-EPMC3515099 | biostudies-literature