A new phosphorothioic triamide structure: P(S)[NHCH2C6H5]3.

The structure of N,N',N''-tribenzylphosphorothioic triamide, C21H24N3PS, (I), and analysis of the bond-angle sums at the N atoms for this compound, and for 74 structures with a P(S)[N]3 skeleton and the N atom in a three-coordinate geometry found in the Cambridge Structural Database [CSD; Groom & Allen (2014). Angew. Chem. Int. Ed. 53, 662-671], are reported. For (I), the bond-angle sum at one of the N atoms [359 (1)°] shows a nearly planar configuration, while the other two show a nonplanar geometry with bond-angle sums of 342 (1) and 347 (1)°. The location of the atoms attached to the nonplanar N atoms suggests an anti orientation of the corresponding lone electron pairs (LEPs) on these N atoms with respect to the P=S group. For 74 structures with a P(S)[N]3 skeleton and with the N atom in a three-coordinate geometry, the bond-angle sums at the N atoms were found to be in the range 293-360°. Among 307 such three-coordinate N atoms, 39% (120 N atoms) have bond-angle sums in the range 359-360°, in accordance with sp(2) hybridization, and 45% (138 N atoms) have bond-angle sums in the range 352-359°, with hybridization close to sp(2). For the orientation of the LEP with respect to the P=S group, the anti orientation was found to be a general rule for N atoms, with the corresponding bond-angle sums deviating by more than 8° from the planar value of 360°. In the title structure, the S atom takes part in intermolecular (N-H···)(N-H···)S hydrogen bonds, connecting the molecules into extended chains parallel to the b axis. The co-operation of one N atom in an N-H···S hydrogen bond as an H-atom donor, and in an N-H···N hydrogen bond as an acceptor, is a novel feature of the crystal structure.

Hexa-kis-{[1-(dimethyl-amino)-propyl-idene]oxidanium} bis-(dodeca-molybdo-phosphate) N,N-dimethyl-propionamide penta-solvate.

In the asymmetric unit of the title salt, (C(5)H(12)NO)(6)[PMo(12)O(40)](2)·5C(5)H(11)NO, there are two independent α-Keggin-type [PMo(12)O(40)](3-) polyoxidoanions, which show characteristic features with respect to bond lengths and angles. One of the [CH(3)CH(2)C(=OH)N(CH(3))(2)](+) cations is hydrogen bonded to the neighboring polyoxidoanion through a C=O-H⋯O(bridge) hydrogen bond. The organic mol-ecules and the remaining organic cations form [(C(5)H(11)NO)(2)H](+) mol-ecule-cation pairs, two of which lie about inversion centers, through O-H⋯O hydrogen bonds.

N,N'-Bis(4-methyl-phen-yl)-N''-(2,2,2-trichloro-acet-yl)phospho-ric triamide.

The P atom in the title compound, C(16)H(17)Cl(3)N(3)O(2)P, is bonded in a distorted tetra-hedral geometry with the phosphoryl and carbonyl groups anti with respect to one another. In the crystal, mol-ecules are linked through (N-H)(2)⋯O(=P) and N-H⋯O(=C) hydrogen bonds into chains along [001]. The phosphoryl O atom acts as a double hydrogen-bond acceptor.

N,N-Dibenzyl-O,O'-dimethyl thio-phosphate.

The P atom in the title compound, C(16)H(20)NO(2)PS, is bonded in a distorted tetra-hedral P(S)(O)(2)N environment with the bond angles at the P atom in the range 99.37 (7) to 115.68 (5)°. The angles at the amido N atom (with bond-angle sum of 357.8°) confirm its sp(2) character. The C-O-P bond angles are 119.78 (11) and 119.39 (12)°.

N,N,N',N'-Tetra-benzyl-N''-(2,6-difluoro-benzo-yl)phospho-ric triamide.

In the C(O)NHP(O) fragment of the title compound, C(35)H(32)F(2)N(3)O(2)P, the P-N bond is longer and the O-P-N angle is contracted compared with the other two P-N bonds and O-P-N angles. The P atom adopts a distorted tetra-hedral environment and the phosphoryl and carbonyl groups are anti with respect to each other. The two tertiary N atoms of the dibenzyl-amido groups show sp(2) character with a slight deviation from planarity. In the crystal, pairs of N-H⋯O(P) hydrogen bonds form inversion dimers.

N,N'-Dicyclo-pentyl-N'',N''-dimethyl-phospho-ric triamide.

The P atom in the title mol-ecule, C(12)H(26)N(3)OP, has a distorted tetra-hedral configuration: its bond angles lie in the range 101.1 (2)-119.1 (2)°. The P-N bonds to the two cyclo-pentyl-amido moieties are significantly different [1.619 (4) and 1.643 (4) Å], with the shorter bond related to an anti orientation of the lone electron pair of the corresponding N atom relative to the P=O bond. The O atom of the P=O group acts as a double hydrogen-bond acceptor and is involved in two different inter-molecular N-H⋯O(P) hydrogen bonds, building R(2) (2)(8) rings that are further linked into chains along [001].

p-Tolyl bis-(cyclo-hexyl-amido)-phosphinate.

The P atom in the title mol-ecule, C(19)H(31)N(2)O(2)P, is in a distorted tetra-hedral configuration with the bond angles in the range 101.48 (10)-118.58 (9)°. The N-H units have a syn orientation with respect to one another. In the crystal, mol-ecules are connected via two different inter-molecular N-H⋯O(P) hydrogen bonds into chains along the a axis in which the O atom of the P=O group acts as a double acceptor.

Piperazine-1,4-diium bis-(pyridine-2,6-dicarboxyl-ato-κO,N,O)cobaltate(II) tetra-hydrate.

The asymmetric unit of the title complex, (C(4)H(12)N(2))[Co(C(7)H(3)NO(4))(2)]·4H(2)O, consists of one piperazinediium dication, one [Co(py-2,6-dc)(2)](2-) dianion (where py-2,6-dc is pyridine-2,6-dicarboxyl-ate) and four water mol-ecules. The piperazinediium cation adopts a chair conformation and the Co(II) ion is six-coordinated in an N(2)O(4) environment, having a distorted octa-hedral geometry. In the crystal, inter-molecular O-H⋯O, N-H⋯O and weak C-H⋯O hydrogen bonds link the components, forming a three-dimensional network.

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

In the title mol-ecule, C(18)H(21)ClF(2)N(3)O(2)P, the P=O and N-H groups are syn to each other. The P atom adopts a slightly distorted tetra-hedral environment and the N atoms of the tertiary amine groups are bonded in an essentially planar geometry. In the crystal, pairs of inter-molecular N-H⋯O(P) hydrogen bonds form centrosymmetric dimers.

Bis(2,6-diamino-pyridinium) hydrogen phthalate nitrate monohydrate.

The title hydrated salt, 2C(5)H(8)N(3) (+)·C(8)H(5)O(4) (-)·NO(3) (-)·H(2)O, was obtained fortuitously from the reaction between 2,6-diamino-pyridine, phthalic acid and Co(NO(3))(2)·6H(2)O at 343 K. The asymmetric unit consists of two crystallographically independent 2,6-diamino-pyridinium cations, a hydrogen phthalate anion, a nitrate ion and a water mol-ecule of crystallization which in the crystal structure are linked by inter-molecular O-H⋯O and N-H⋯O hydrogen bonds into a three-dimensional network. In the hydrogen phthalate anion, there is a very strong intra-molecular O-H⋯O hydrogen bond.

Tris(2-meth-oxy-ethanaminium) dodeca-molybdophosphate trihydrate.

The asymmetric unit of the polyoxidometalate-based organic-inorganic hybrid title compound, (C(3)H(10)NO)(3)[PMo(12)O(40)]·3H(2)O, consists of one α-Keggin-type [PMo(12)O(40)](3-) polyoxido-anion, three independent [CH(3)-O-CH(2)-CH(2)-NH(3)](+) cations and three solvent water mol-ecules. The polyoxidoanion shows characteristic features with respect to bond lengths and angles. In the crystal structure, extensive inter-molecular N-H⋯O and O-H⋯O hydrogen bonding between the organic cations, inorganic anions and solvent water mol-ecules leads to a three-dimensional supra-molecular network.

Penta-kis(l-prolinium) dodeca-tungsto-borate trihydrate.

The title polyoxometalate-based organic-inorganic hybrid compound, (C(5)H(10)NO(2))(5)[BW(12)O(40)]·3H(2)O, consists of one α-Keggin-type [BW(12)O(40)](5-) polyoxoanion, five crystallographically independent l-prolinium cations and three uncoordin-ated water mol-ecules. The polyoxoanion shows characteristic features with respect to bond lengths and angles. Several N-H⋯O and O-H⋯O hydrogen bonds between the organic cations, inorganic anions and crystal water mol-ecules lead to a three-dimensional supra-molecular structure.

Human genomic DNA analysis using a semi-automated sample preparation, amplification, and electrophoresis separation platform.

The growing importance of analyzing the human genome to detect hereditary and infectious diseases associated with specific DNA sequences has motivated us to develop automated devices to integrate sample preparation, real-time PCR, and microchannel electrophoresis (MCE). In this report, we present results from an optimized compact system capable of processing a raw sample of blood, extracting the DNA, and performing a multiplexed PCR reaction. Finally, an innovative electrophoretic separation was performed on the post-PCR products using a unique MCE system. The sample preparation system extracted and lysed white blood cells (WBC) from whole blood, producing DNA of sufficient quantity and quality for a polymerase chain reaction (PCR). Separation of multiple amplicons was achieved in a microfabricated channel 30 microm x 100 microm in cross section and 85 mm in length filled with a replaceable methyl cellulose matrix operated under denaturing conditions at 50 degrees C. By incorporating fluorescent-labeled primers in the PCR, the amplicons were identified by a two-color (multiplexed) fluorescence detection system. Two base-pair resolution of single-stranded DNA (PCR products) was achieved. We believe that this integrated system provides a unique solution for DNA analysis.