(E)‐2‐[2‐(1‐Naphthyl)­vinyl]‐3‐tosyl‐2,3‐di­hydro‐1,3‐benzo­thia­zole

The title compound, C₂₆H₂₁NO₂S₂, which consists of a benzo­thia­zole skeleton with α‐naphthyl­vinyl and tosyl groups at positions 2 and 3, respectively, was prepared by palladium–copper‐catalyzed heteroannulation. The E configuration of the mol­ecule about the vinyl C=C bond is established by the benzothiazole–naphthyl C—C—C—C torsion angle of 177.5 (4)°. The five‐membered heterocyclic ring adopts an envelope conformation with the Csp³ atom 0.380 (6) Å from the C₂NS plane. The two S—C [1.751 (4) and 1.838 (4) Å] and two N—C [1.426 (5) and 1.482 (5) Å] bond lengths in the thia­zole ring differ significantly.     

7,7‐Di­chloro‐1,6‐di­methyl‐2‐oxa‐5‐thia­bi­cyclo­[4.1.0]­heptane 5,5‐dioxide and 6‐chloro‐2,3‐di­hydro‐7‐methyl‐5‐methyl­ene‐2H,3H,5H‐1,4‐dithiepine 1,1,4,4‐tetraoxide

The structures of a 2‐oxa‐5‐thia­bi­cyclo­[4.1.0]­heptane derivative, C₇H₁₀Cl₂O₃S, (I), and a 2H,3H,5H‐1,4‐dithiepine derivative, C₇H₉ClO₄S₂, (II), are reported. The six‐membered ring in (I) has an envelope conformation and the seven‐membered ring in (II) adopts a chair conformation. There are no untoward intermolecular interactions in (I), but two Cl atoms make a short intermolecular contact across an inversion centre in (II), with a Cl?Cl distance of 3.2784 (9) Å, some 0.22 Å less than the sum of the van der Waals radii.     

4‐[1‐(Phenylsulfonyl)indol‐3‐yl]‐3a,4,5,9b‐tetrahydro‐3H‐cyclopenta[c]quinoline

In the title compound, C₂₆H₂₂N₂O₂S, the tetra­hydro­pyridine ring has a conformation intermediate between half‐chair and sofa. The tetrahydroquinoline mean plane makes a dihedral angle of 73.3 (1)° with the cyclopentene ring, which adopts an envelope conformation, and an angle of 45.45 (4)° with the indole best plane. The dihedral angle between the benzene and pyrrole rings is 2.6 (1)°. The orientations of the phenyl ring on the sulfonyl group and of the indole are governed by weak C—H?O interactions. The packing of the mol­ecule in the solid state is stabilized by C—H?O and C—H?N hydrogen bonds.     

Bis­[2‐(di­phenyl­phosphinoyl)­benzene] di­sulfide

The title compound, [2‐Ph₂P(O)C₆H₄S]₂ or C₃₆H₂₈O₂P₂S₂, obtained by electrochemical oxidation of 2‐(di­phenyl­phosphino)­benzene­thiol, has twofold crystallographic symmetry. Principal dimensions include S—S 2.0212 (15) Å, S—C 1.786 (3) Å and C—S—S—C 81.34 (14)°.     

Two isomers of 2,4‐di­benzyl‐8‐azabicyclo­[3.2.1]­octan‐3‐ol

The crystal structures of the title compounds, 2α,4α‐di­benzyl‐3α‐tropanol (2α,4α‐di­benzyl‐8‐methyl‐8‐aza­bi­cyclo­[3.2.1]­octan‐3α‐ol), C₂₂H₂₇NO, (I), and 2α,4α‐di­benzyl‐3β‐tropanol (2α,4α‐di­benzyl‐8‐methyl‐8‐aza­bi­cyclo­[3.2.1]­octan‐3β‐ol), C₂₂H₂₇NO, (II), show that both compounds have a piperidine ring in a chair conformation and a pyrrolidine ring in an envelope conformation. Isomer (I) is asymmetric, the benzyl groups having different orientations, whereas isomer (II) is mirror symmetric, and the N and O atoms, the C atom attached to the hydroxy group, and the methyl C atom attached to the N atom lie on the mirror plane. In the crystal structures of both (I) and (II), the mol­ecules are linked together by intermolecular O—H⋯N hydrogen bonds to form chains that run parallel to the a direction in (I) and parallel to b in (II).     

Benzyl 5‐{2‐[2‐(diethoxy­phosphinoyl)­acetyl]‐3‐oxo‐7‐thia‐2,4‐di­aza­bi­cyclo­[3.3.0]­oct‐6‐yl}pentanoate,a novel biotin derivative

The title compound, C₂₃H₃₃N₂O₇PS, has its phospho­no­acetate carbonyl group rotated slightly out of the plane of the ureido ring, with a C—N—C—O torsion angle of ?6.9 (4)°. The sulfur‐containing ring has an envelope conformation, while the ureido ring is nearly planar.     

3,3,4,4,5,5‐Hexafluoro‐1‐(2‐methoxyphenyl)‐2‐[5‐(4‐methoxyphenyl)‐2‐methyl‐3‐thienyl]cyclopent‐1‐ene: a photochromic compound

The photochromic title compound, C₂₄H₁₈F₆O₂S, has thienyl and aryl substituents on the C=C double bond of the shallow half‐chair‐shaped cyclopentene ring. The planes of the two substituent rings are inclined to that of the cyclopentene ring, with dihedral angles between the mean plane of the cyclopentene ring and those of the phenylene and thienyl rings of 51.2 (1) and 51.3 (1)°, respectively. The molecule adopts an antiparallel conformation, with a distance between the two photoreactive C atoms of 3.717 (2) Å.     

11‐Methyl‐12a‐phenyl‐9a,12a‐di­hydro­phenanthro­[9′,10:5,6][1,4]­dioxino­[2,3‐d]­thia­zole

In the title compound, C₂₄H₁₇NO₂S, the dioxine and thia­zoline rings are distorted from planarity towards a half‐chair and an envelope conformation, respectively. The configurations of the dioxine ring, the thiazoline ring and the attached phenyl ring are conditioned by the sp³ state of the two bridgehead C atoms. The phenanthrene system is nearly coplanar with the dioxine ring, while the attached phenyl ring is orthogonal to the thia­zoline ring.     

2‐(4‐Chloro­phenyl)‐1,3‐di­cyano‐6,7‐di­hydro‐4‐imino‐9,10‐di­methoxy­benzo­[a]­quinolizine–water (2/5)

Crystals of the title compound, C₂₃H₁₇ClN₄O₂·2.5H₂O, contain channels filled with highly disordered water mol­ecules. The best structure refinement was obtained by removing the solvent contribution from the intensity data and refining against a solvent‐free model. The central six‐membered ring of the quinolizine mol­ecule has a slightly distorted screw‐boat conformation.     

(±)‐6‐Benzyl‐3,3‐di­methyl­morpholine‐2,5‐dione and its 5‐mono­thio and 2,5‐di­thio derivatives

The morpholine ring of the title dione, C₁₃H₁₅NO₃, shows a boat conformation that is distorted towards a twist‐boat, with the boat ends being the two Csp³ atoms of the ring. The benzyl substituent is in the favoured `exo' position. In the mono­thione derivative, (±)‐6‐benzyl‐3,3‐di­methyl‐5‐thioxo­morpholin‐2‐one, C<sub>13</sub>H<sub>15</sub>NO<sub>2</sub>S, this ring has a much flatter conformation that is midway between a boat and an envelope, with the di­methyl end being almost planar. The orientation of the benzyl group is `endo'. The di­thione derivative, (±)‐6‐benzyl‐3,3‐di­methyl­morpholine‐2,5‐di­thione, C₁₃H₁₅N­OS₂, has two symmetry‐independent mol­ecules, which show different puckering of the morpholine ring. One mol­ecule has a flattened envelope conformation distorted towards a screw‐boat, while the conformation in the other mol­ecule is similar to that in the mono­thione derivative. Intermolecular hydrogen bonds link the mol­ecules in the three compounds, respectively, into centrosymmetric dimers, infinite chains, and dimers made up of one of each of the symmetry‐independent mol­ecules.     

Di­spiro­[fluorene‐9,5′‐[1,2,3,4]­tetra­thia­ne‐6′,9′′‐fluorene]

The tetra­thia­ne ring of the title compound, C₂₆H₁₆S₄, has a chair conformation and the mol­ecule has approximate C₂ symmetry. Each of the two fluorene ring systems is virtually planar, with the ring planes intersecting at an angle of 67.58 (5)°. This novel compound has been formed as a side product from the treatment of 9H‐fluorene‐9‐thione with methyl N‐[(benzyl­idene)­phenyl]­glycinate in the presence of LiBr and 1,6‐di­aza­bi­cyclo­[5.4.0]­un­decane.     

2‐[3‐Furyl­(hydroxy)­methyl]‐2,3‐di­methyl­cyclo­hexanone

In the mol­ecule of the title compound, C₁₃H₁₈O₃, there is a syn relationship between the two vicinal methyl groups. The six‐membered ring adopts a chair conformation, with one equatorial and two axial groups, and the furyl group is almost parallel to the ketone group. Intermolecular hydrogen bonds [O—H?O=C 2.814 (3) Å] form chains along [100].     

7‐Chloro‐1‐(2,6‐di­fluoro­phenyl)‐1H,3H‐thia­zolo­[3,4‐a]­benz­imidazole and 1‐(2,6‐di­fluoro­phenyl)‐6‐methyl‐1H,3H‐thia­zolo­[3,4‐a]­benz­imidazole

The title mol­ecules, C₁₅H₉ClF₂N₂S and C₁₆H₁₂F₂N₂S, respectively, display the well known butterfly‐like conformation with a flat thia­zolobenz­imidazole system. In both compounds, the mean plane through the tricyclic system is almost perpendicular to the 2,6‐di­fluoro­phenyl ring. This arrangement of the aryl group is determined by two intramolecular hydrogen bonds and by an attractive F?S interaction.     

Di­propyl 3,6‐di­phenyl‐1,2‐di­hydro‐1,2,4,5‐tetrazine‐1,2‐di­carboxyl­ate

The title compound, C₂₂H₂₄N₄O₄, was prepared from propyl chloro­formate and 3,6‐di­phenyl‐1,2‐di­hydro‐s‐tetrazine. This reaction yields the title compound rather than di­propyl 3,6‐di­phenyl‐1,4‐di­hydro‐s‐tetrazine‐1,4‐di­carboxyl­ate. The 2,3‐di­aza­buta­diene group in the central six‐membered ring is not planar; the C=N double‐bond length is 1.285 (2) Å, and the average N—N single‐bond length is 1.401 (3) Å, indicating a lack of conjugation. The ring has a twist conformation, in which adjacent N atoms lie 0.3268 (17) Å from the plane of the ring. The mol­ecule has twofold crystallographic symmetry.     

(Z)‐7‐Chloro‐3‐[(3‐chloro­phenyl)­methyl­idene]‐4‐p‐tosyl‐3,4‐di­hydro‐2H‐1,4‐benzoxazine

In the title compound, C₂₂H₁₇Cl₂NO₃S, the mol­ecule is a substituted 3,4‐di­hydro‐2H‐1,4‐benzoxazine compound which has three phenyl rings which are essentially planar. The 3,4‐di­hydro‐2H‐oxazine part of the mol­ecule is fused to the benzo ring and has a half‐boat conformation; the dihedral angle between the planar part of the oxazine ring and the benzo ring is 10.2 (2)°. The (3‐chloro­phenyl)­methyl­idene substituent has a Z configuration in relation to the ring N atom of the oxazine moiety. Interestingly, the p‐toluenesulfonyl (p‐tosyl) substituent on the ring N atom protrudes away from the 3‐­chloro­phenyl substituent thus avoiding any steric interaction.     

1,2,4‐Triazolo­[2,3‐h]‐7,9‐thi­aza‐11‐crown‐4

The title compound, 4,7‐dioxa‐10‐thia‐1,12,13‐tri­aza­bi­cyclo­[9.3.0]­tetra­deca‐11,13‐diene, C₈H₁₃N₃O₂S, contains an 11‐membered ring, which appears in a chair conformation and has approximate mirror symmetry. It may be used for the complexation of metal atoms.     

13,13a‐Di­hydro‐13‐methoxy‐9‐methyl‐1‐benzo­pyrano­[4,3‐i]­dinaphtho­[2,1‐c;1′,2′‐f]‐2,8‐dioxa­bicyclo­[3.3.1]­nonane

The crystal structure of the title compound, C₃₂H₂₄O₄, contains three fused di­hydro­pyran rings (A, B and C); ring A is fused with a benzene ring while the other two rings, B and C, are fused with naphthalene rings. Ring A adopts a half‐chair conformation with an equatorial methoxy group, whereas ring B assumes a distorted half‐chair conformation, the A/B ring junction being trans. Ring C adopts a distorted half‐boat conformation and is nearly orthogonal to ring B. Ring C is inclined to the best plane of ring A at an angle of 112.1 (1)°.     

8‐Chloro‐6‐phenyl‐4H‐[1,2,4]­triazolo­[4,3‐a][1,5]­benzodiazepin‐5(6H)‐one

The title compound, C₁₆H₁₁ClN₄O, is an anticonvulsant agent. In the crystal, a particularly short C—H?N intermolecular hydrogen bond is noted [H?N 2.22 (2) Å]. The diazepine ring has a boat conformation.     

6‐Hydroxy‐2,2‐di­methyl‐3,4‐di­hydro‐2H‐benzo[b]pyran

The title compound, 2,2‐di­methyl­chroman‐6‐ol, C₁₁H₁₄O₂, has been identified as a side product from the condensation of hydro­quinone with 2‐methyl­but‐3‐en‐2‐ol. The pyran ring has a half‐chair conformation. The hydroxyl groups are involved in intermolecular hydrogen bonding which generates infinite spiral chains around the fourfold screw axes; the O?O hydrogen‐bonded distances are 2.661 (1) Å.     

6‐[3‐Hydroxy‐17‐oxoestra‐1,3,5(10)‐trien‐7β‐yl]­hexane­nitrile

In the title compound, C₂₄H₃₁NO₂, ring B adopts a conformation between the boat and twisted‐boat forms. This conformation best accommodates adverse intramolecular H⋯H interactions between the H atoms of the 7β‐substituent and the two nearest ring H atoms. The tilt angle between rings A and D is 28.6 (1)°.