Synthesis and Comprehensive Characterization of Hydrated Alkaline Earth Metal Salts of 5‐Amino‐1H‐tetrazole

Hydrated alkaline earth metal salts of 5‐amino‐1H‐tetrazole ( B ) were synthesized by reaction of B with a suitable metal hydroxide in water. All compounds were fully characterized by analytical (elemental analysis and mass spectrometry) and spectroscopic (IR, Raman, ¹H and ¹³C NMR) methods. Additionally, the crystal structures of the magnesium [ 1· 4H₂O: triclinic, P$\bar {1}$ , a = 5.940(1) Å, b = 7.326(1) Å,c = 7.383(1) Å, α = 106.10(1)°, β = 106.51(1)°, γ = 111.85(1)°, V = 258.0(1) ų], calcium [ 2· 6H₂O: monoclinic, P2₁/m, a = 6.904(1) Å,b = 6.828(1) Å, c = 10.952(2) Å, β = 94.50(2)°, V = 514.6(1) ų], and strontium [ 3· 6H₂O: orthorhombic, Cmcm, a = 6.987(1) Å, b = 28.394(2) Å, c = 7.007(1) Å, V = 1390.3(2) ų] were determined by low temperature X‐ray diffraction. Additionally, the (gas phase) structure of the 5‐amino‐1H‐tetrazole anion ([ B ]^–) was also studied by natural bond orbital (NBO) analysis [B3LYP/6‐31+G(d,p)]. Lastly, standard tests were used to determine the sensitivity towards impact, friction, and electrostatic discharge of the compounds and the thermal stability was assessed by differential scanning calorimetry (DSC) analysis.     

Preparation,X-ray crystal structure and 13C- and 1H-NMR study of 1-methyl-2-(N-methyl-N-phenylglycyl)-3-(N-methylanilino)indole

Reaction of N-methylaniline with 40% glyoxal yields 1-methyl-2-(N-methyl-N-phenylglycyl)-3-(N-methylanilino)indole ( 1a ) as the main product together with 1-methyl-3-(N-methylanilino)indole ( 1b ). The reaction appears to be general for aromatic secondary amines since N-ethylaniline and N-phenylbenzylamine yield the corresponding indoles. The structure of 1a has been verified by single crystal X-ray diffraction. Compound 1a (C₂₅H₂₅N₃O) crystallized in the triclinic space group Pl? with cell dimensions a = 10.085(3)Å, b = 10.371(3)Å, c = 11.908(5)Å, α = 74.2(3)°, β = 74.7(3)° and γ = 60.7(2)° with Z = 2. The complete ¹H and ¹³C nmr assignment of indoles 1a and 1b was achieved from two-dimensional HETCOR and COSY spectra with the aid of homonuclear and heteronuclear double resonance experiments.     

Syntheses,Characterizations, and Crystal Structures of Two New Organically Templated Borates

Two new organically templated borates, [H₂DAB][B₇O₉(OH)₅]·2H₂O ( 1 ) and [H₂DAB][B₇O₁₀(OH)₃] ( 2 ), have been synthesized under mild conditions in the presence of DAB acting as structure‐directing agent (DAB = 1,4‐diaminobutane). The structures were determined by single crystal X‐ray diffraction and further characterized by FTIR, elemental analysis, and thermogravimetric analysis. Both 1 and 2 crystallize in the same triclinic system, space group (No. 2); 1: a = 8.238(4) Å, b = 8.348 (5) Å, c = 14.574(8) Å, a = 101.050(3)°, β = 92.313(7)°, γ = 112.694(5)°, V = 900.3(8) ų, Z = 2; 2: a = 8.8769(3) Å, b = 9.3204(2) Å, c = 10.2204(5) Å, α = 74.474(2)°, β = 85.292(5)°, γ = 72.730(2)°, V = 778.01(5) ų, Z = 2. The structure of 1 consists of [B₇O₉(OH)₅]^2? groups, which represents the first example of organically templated heptaborate. The structure exhibits interesting hydrogen‐bonded network formed by borate polyanion [B₁₄O₂₀(OH)₆]^4?, which can be regarded as being constructed from the dehydration of the FBBs in 1 . The diprotonated organic amines are filled in the free space of the hydrogen‐bonded network and interact with the inorganic framework by extensive hydrogen bonds.     

Synthesis and Characterization of a New Organically Templated Aluminophosphite with a Chainlike Structure

A new aluminophosphite (H₄bape)_0.5[Al(OH)(HPO₃)₂] has been synthesized under hydrothermal conditions and its structure was determined by single‐crystal X‐ray diffraction (bape = N,N′‐bis(2‐aminopropyl)ethylenediamine). This compound crystallizes in the triclinic system with the space group (No. 2), a = 6.919(2) Å, b = 8.704(2) Å, c = 9.786(2) Å, α = 77.74(3)°, β = 72.43(3)°, γ = 72.52(3)°, V = 531.08(2) ų, Z = 2. The structure consists of distorted octahedral AlO₆ and pseudo pyramidal HPO₃, which are connected by vertex oxygen atoms to form a chainlike framework with a Al/P ratio of 1/2. The presence of 1D infinite Al‐O‐Al linkage in the framework is noteworthy. The organic templates are fully protonated and interact with the aluminophosphite chains through extensive hydrogen bonds to form a 3D supramolecular network.     

Three Copper(II) Coordination Polymers Constructed by Both Rigid and Flexible Ligands

Three new Copper(II) polymers coordinated by both rigid and flexible ligands, [Cu(bpy)(C₅H₆O₄)]_n ( 1 ), [Cu(bpy)(C₆H₈O₄)]_n ( 2 ), and [Cu₂(bpy)₂(C₆H₈O₄)₂]_n ( 3 ) (bpy = 4,4′‐bipyridine), have been hydrothermally synthesized and structurally characterized. Complex 1 features a box‐like bilayer motif of (4, 4) net. It crystallizes in triclinic space group with cell parameters: a = 8.1395(6) Å, b = 9.43 12(8) Å, c = 10.5473(8) Å, α = 112.1830(1)°, β = 92.423(2)°, γ = 104.752(2)°, V = 716.31(1) ų, Z = 2. Complex 2 crystallizes in triclinic space group with a = 8.8652(4) Å, b = 8.9429(4) Å, c = 10.6390(4) Å, α = 89.520(2)°, β = 69.123(2)°, γ = 75.2440(1)°, V = 758.92(6) ų, Z = 2. Complex 3 crystallizes in monoclinic space group Cc with a = 11.1521(1) Å, b = 15.3961(1) Å, c = 17.7419(1) Å, β = 105.715(3)°, V = 2932.4(5) ų, Z = 4. Complexes 2 and 3 are isomeric with different coordination modes of adipato ligand. Both of them possess the two‐fold interpenetrated 3‐D pcu topological net.     

Synthese und Kristallstruktur des Lewis‐Säure/Base‐Addukts AlCl3·C3N3Cl3

Synthesis and Crystal Structure of the Lewis Acid‐Base Adduct AlCl₃·C₃N₃Cl₃ The reaction between cyanuric chloride (C₃N₃Cl₃) and the strong Lewis acid AlCl₃ yielded colorless crystals of the adduct AlCl₃·C₃N₃Cl₃. The crystal structure was determined by single crystal X‐ray diffraction at room temperature and was solved in the space group with Z = 4, a = 7.3802(7) Å, b = 9.688(1) Å, c = 16.272(2) Å, α = 72.80(1)°, β = 89.97(1)°, γ = 87.23(1)°, and V = 1110.0(2) ų. In the crystal structure, AlCl₃ is closely associated to the triazine ring with Al–N distances of 2.042(3) Å and 2.067(4) Å, respectively. The AlCl₃·C₃N₃Cl₃ units are connected with each other via intermolecular N···Cl donor–acceptor interactions, forming tape‐like arrangements in the ac‐plane, with tapes running parallel to the a‐axis.     

Synthesis and Characterization of the Rubidium Thiophosphate Rb6(PS5)(P2S10) and the Rubidium Silver Thiophosphates Rb2AgPS4, RbAg5(PS4)2 and Rb3Ag9(PS4)4

The metal thiophosphates Rb₂AgPS₄ ( 2 ), RbAg₅(PS₄)₂ ( 3 ), and Rb₃Ag₉(PS₄)₄ ( 4 ) were synthesized by stoichiometric reactions, whereas Rb₆(PS₅)(P₂S₁₀) ( 1 ) was prepared with excess amount of sulfur. The compounds crystallize as follows: 1 monoclinic, P2₁/c (no. 14), a = 17.0123(7) Å, b = 6.9102(2) Å, c = 23.179(1) Å, β = 94.399(4)°; 2 triclinic, P$\bar{1}$ (no. 2), a = 6.600(1) Å, b = 6.856(1) Å, c = 10.943(3) Å, α = 95.150(2)°, β = 107.338(2)°, γ = 111.383(2)°; 3 orthorhombic, Pbca (no. 61), a = 12.607(1) Å, b = 12.612(1) Å, c = 17.759(2) Å; 4 orthorhombic, Pbcm (no. 57), a = 6.3481(2) Å, b = 12.5782(4) Å, c = 35.975(1) Å. The crystal structures contain discrete units, chains, and 3D polyanionic frameworks composed of PS₄ tetrahedral units arranged and connected in different manner. Compounds 1 – 3 melt congruently, whereas incongruent melting behavior was observed for compound 4 . 1 – 4 are semiconductors with bandgaps between 2.3 and 2.6 eV and thermally stable up to 450 °C in an inert atmosphere.     

Synthesis and Crystal Structure of the Zinc Borate Zn3B4O9

The new zinc borate Zn₃B₄O₉ was synthesized at high-pressure/high-temperature conditions of 10 GPa and 1173 K in a Walker-type multianvil pressure device. It crystallizes in the space group P (no. 2) with a=5.5028(2) Å, b=6.7150(3) Å, c=7.8887(3) Å, α=83.99(1)°, β=73.38(1)°, γ=74.75(1)°, V=269.35(2) ų, and two formula units (Z=2) per unit cell. The structure was confirmed via single-crystal X-ray diffraction. Zn₃B₄O₉ can be synthesized phase pure, which is shown with a Rietveld refinement. IR-spectroscopic data of a powder sample were collected.     

Synthesis,crystal structure and magnetic properties of a new 1-D oxamidate-bridged Cu(II)-Mn(II) polymer

A new coordination polymer, {[Cu(aeop)Mn(H₂O)₃]₂}_n (H₄aeop = N′-(2-aminoterephthalic acid)-N′′-(1,3-propanediamine)oxamidate), has been synthesized and characterized structurally and magnetically. This complex features a 1-D ladder-like chain structure constructed from neutral tetranuclear units through the syn-anti carboxylate bridges. This crystal forms in the triclinic system, space group P 1, with a = 9.653(1) Å, b = 9.686(1) Å, c = 10.903(1) Å, α = 80.984(1)°, β = 69.776(1)°, γ = 80.729(1)° and z = 2. The relationship between its magnetic properties and structure has also been investigated.     

A Highly Stable 3D Porous Lanthanum Metal‐organic Framework Constructed From A New Flexible Bis(benzoic acid) Ligand Produced in Situ

By employing diethyl 1,3‐propylidenebis(4‐oxybenzoate) as a precursor, the new three‐dimensional metal‐organic framework [La₂L₂(HL)₂]_n [L = 1,3‐propylidenebis(4‐oxybenzoate)] was prepared and characterized by single‐crystal X‐ray diffraction analysis, elemental analysis, infrared spectroscopy, and thermogravimetric analysis. The compound crystallizes in the triclinic space group P , with cell parameters: a = 8.299 (2) Å, b = 14.127 (3) Å, c = 14.520 (3) Å, α = 112.43 (3) °, β = 103.10 (3) °, γ = 95.28 (3)°, V = 1502.2 (5) Å³, and Z = 1. Under hydrothermal reaction conditions, two ester groups of the ligand hydrolyzed into carboxylate groups. The carboxylate groups coordinated in situ to metal ions to form the 3D coordination polymer. It exhibits a 10.4 × 10.6 Å rhombic channel along the [011] direction. On the basis of the results of TG analysis, the structure is thermally stable up to ≈? 400 °C.     

Synthesis of two novel cobalt complexes and their crystal structures

Two new cobalt complexes were successfully synthesized from the reaction of binaphthyl Schiff base 2 with Co(OAc)₂ in the presence of sodium methoxide at 80 °C for 24 h and Co(acac)₃ in toluene under reflux. Their unique crystal structures are unambiguously disclosed by X‐ray analysis. Complex 3 is triclinic, space group P1 , unit cell dimensions a = 10.742(2) Å, b = 11.153(2) Å, c = 12.715 Å, α = 79.865(3) °, β = 76.053 °, γ = 72.532(4) °, volume 1401.3(5) ų, Z = 2. Complex 4 is triclinic, space group P1 , unit cell dimensions a = 10.801(2) Å, b = 12.554(3) Å, c = 15.219(3) Å, α = 105.672(4) °, β = 103.048 °, γ = 104.594(4) °, volume 1824.8(7) ų, Z = 2, calculated density 1.428 Mg m⁻³. Copyright © 2003 John Wiley & Sons, Ltd.     

A new type of liquid crystal involving hydrogen bonding: single crystal X-ray structure characterization and properties of the liquid crystal

A new liquid crystal involving hydrogen bonding between 4-hexyloxybenzoic acid and 4-octyloxylphenylethynylpyridine has been investigated by DSC, polarizing optical microscopy and X-ray diffraction. The mesogen shows a nematic phase and an unknown liquid crystalline phase. The liquid crystal crystallizes with a triclinic space group P-1 with the parameters: a = 8.879(2)Å, b = 10.137(2)Å, c = 17.629(4)Å; α = 104.16(3)°, β = 95.47(3)°, γ = 101.48(3)°; V = 1490.3(6)ų; Z = 2; F(000) = 572; μ = 0.076 mm^?1; λ(MoK_α) = 0.71073 Å; final R ₁ = 0.0435. The complex is formed by strong intermolecular hydrogen bonding.     

Synthesis,crystal structure,and magnetism of a dinuclear nickel(II) complex [Ni2(MOBPT)2(N3)4] · 2H2O

A dinuclear nickel(II) complex, [Ni₂(MOBPT)₂(N₃)₄] · 2H₂O (MOBPT = 4-(p-methoxyphenyl)-3,5-bis(pyridine-2-yl)-1,2,4-triazole), has been synthesized and characterized by elemental analysis, UV, IR, ESI-MS, and single crystal X-ray crystallography. The complex crystallizes in triclinic system, space group P 1 with a = 9.877(2) Å, b = 10.396(2) Å, c = 11.975(3) Å, α = 71.638(3)°, β = 74.968(3)°, γ = 64.747(3)°, V = 1044.2(4) ų, Z = 1, R = 0.0371 for 5774 observed reflections. The crystal structure determination shows that the dinuclear Ni₂N₈ unit is almost planar with each Ni²⁺ coordinated by four nitrogens from two MOBPT ligands and two axial azides in a distorted octahedral geometry. Magnetic measurements reveal weak antiferromagnetic exchange in the complex.     

Adipato‐Bridged Mixed Ligand catena Complexes: ${_{\infty}^1}${[M(phen)(H2O)]L2/2} with M = NiII,CuII, ZnII; H2L = Adipic Acid

Three adipato bridged mixed ligand catena complexes {[M(phen)(H₂O)]‐(C₆H₈O₄)_2/2} with M = Ni^II ( 1 ), Cu^II ( 2 ), Zn^II ( 3 ) were synthesized. Structure determination based on X‐ray diffraction shows that they crystallize isostructurally in the monoclinic space group C2/c (no. 15) with cell dimensions of: 1 a = 22.451(4)Å, b = 9.041(1)Å, c = 17.440(2)Å, β = 103.41(1)°, U = 3443.4(9)ų, Z = 8; 2 a = 22.479(2)Å, b = 9.067(1)Å, c = 17.494(3)Å, β = 103.67(1)°, U = 3464.6(8)ų, Z = 8; 3 a = 22.635(3)Å, b = 9.052(1)Å, c = 17.571(3)Å, β = 103.24(1)°, U = 3504.5(9)ų, Z = 8. The crystal structure consists of 1D {[M(phen)(H₂O)]‐(C₆H₈O₄)_2/2} zigzag chains, in which the metal atoms are all octahedrally coordinated by two N atoms of one phen ligands and four O atoms of one H₂O molecule and two adipato ligands. The zigzag chains are held together by interchain π‐π stacking interactions and interchain hydrogen bonds.     

Crystal structure of a cholesterol-based dimesogen

The title compound, cholesteryl 6[4-(4-pentyloxyphenylethynyl)phenoxy]hexanoate (DMT5), a cholesterol-based dimesogen, crystallizes in the monoclinic space group P2₁ with the parameters a = 9.812(3) Å, b = 9.713(2) Å, c = 24.179(2) Å, β = 92.48(1)° V = 2302.2(9) ų, Z = 2, F₀₀₀ = 836, λ(MoK_α) = 0.71069 Å, μ = 0.067 cm 1, final R = 0.0772. The structure has intermolecular hydrogen bonds; it is stabilized by the presence of intermolecular contacts whose spacings are less than van der Waals' radii.     

Rhenium(I) Tellurolate,Telluroether and Bidentate-Telluroether Complexes: Crystal Structures of Re(CO)3Br(PhTe(CH2)3TePh), PhTeRe(CO)5 Re2(μ-SePh)2(CO)8 and [(PhTeMe)Re(CO)5][BF4]

The monomeric rhenium(I) complex with bidentate telluroether ligand Re(CO)₃Br(PhTe(CH₂)₃TePh) (1) was accessible via reaction of the PhTe(CH₂)₃TePh with Re(CO)₅Br. This chelate complex crystallized in triclinic space group $ {\rm P}\bar 1 $ with a = 9.390(5) Å, b = 10.961(3) Å, c = 11.849(4) Å a = 63.30(3)°, β = 87.49(4)° γ = 69.31(4)°, V = 1009.5(7) ų Z = 2, R = 0.033, and R_w = 0.034. Reaction of Re(CO)₅Cl with NaTePh yielded the Re(I) specics PhTeRe(CO)₅ (2). This complex crystallized in triclinic space group $ {\rm P}\bar 1 $ with a = 7.085(1) Å, b = 9.203(1) Å, c = 11.341(1) Å, α = 107.24(1)°, β = 100.56(1)°, γ = 96.47(1)°, V = 683.2(2) ų, Z = 2, R = 0.027, R_w = 0.022. Reaction of PhTeRe(CO)₅ and (PhSe)₂ in THF at 65 °C yielded a product that was confirmed crystallographically to be the known species Re₂(μ-SePh)₂(CO)₈ (3), in which two phenylselenolate ligands bridge the two Re(I). Compound 3 crystallized in monoclinic space group P2₁/n with a = 7.210(2) Å, b = 18.862(6) Å, c = 9.083(3) Å, β = 107.48(3)° V = 1178.2(7) ų, Z = 2, R = 0.046, and R_w = 0.051. Methylation of PhTeRe(CO)₅ with [Me₃O][BF₄] afforded Re(I) product [(PhTeMe)Re(CO)₅][BF₄] (4). This monodentate telluroether species crystallized in monoclinic space group P2₁/n with a = 8.405(1) Å, b = 13.438(3) Å, c = 15.560(2) Å, β = 92.59(1)° V = 1755.5(5) ų, Z = 4, R = 0.035, and R_w = 0.035.     

THE CRYSTAL STRUCTURES OF TWO IMINO-1,2,4- DITHIAZOLES FORMED BY THERMAL DECOMPOSITION OF 5-(DIALKYLAMINO)-3-(SUBSTITUTED IMINO)-1,2,4-DITHIAZOLES

Abstract

The thermal decomposition products of two substituted imino-1,2,4-dithiazoles have been studied by single crystal x-ray analysis. Both products crystallize in space group P2^1/c with four molecules per unit cell. The first product, obtained from 5-(dimethylamino)-3-(methylimino)-1,2,4-dithiazole has cell dimensions of a=9.922(8) Å, b=12.052(11) Å, c=13.358(12) Å and β=104.9(1)°. The molecule is made up of two planar segments related by an extremely large twist (?154°) about a C?N double bond. The results from this study have also contributed further information in the area of nonbonded interactions between ring and thione sulfur atoms. The second product, from 5-(dimethylamino)-3(phenylimino)-1,2,4-dithiazole was shown to be an ordered 1:1 complex of the starting material and one of its isomers. The cell dimensions are a=12.420(6) Å, b=8.840(9) Å, c=22.276(22) Å and β= 112.2(1)°. The different molecules are linked by an inter molecular NH… N hydrogen bond.     

Synthesis,Crystal Structure,and Magnetic Properties of (2,2′‐dipyridylamine)(X−) Copper(II) Complexes (X−: Cyanate,Dicyanamide, Acetate,Thiocyanato)

The synthesis, structure, and magnetic properties of four 2,2′‐dipyridylamine ligand (abbreviated as Hdpa) containing copper(II) complexes. There is one binuclear compound, which is [Cu₂(μ_1,1‐NCO)₂(NCO)₂(Hdpa)₂] ( 1 ), and three mononuclear compounds, which are [Cu{N(CN)₂}₂(Hdpa)₂] ( 2 ), [Cu(CH₃CO₂)(Hdpa)₂·N(CN)₂] ( 3 ), and [Cu(NCS)(Acac)] ( 4 ). Compounds 1 and 4 crystallize in the monoclinic system, space group P2(1)/c and Z = 4, with a = 8.2465(6) Å, b = 9.3059(7) Å, c = 16.0817(12) Å, β = 91.090(1)°, and V = 1233.90(16) ų for 1 and a = 7.6766(6) Å, b = 21.888(3) Å, c = 10.4678(12) Å, β = 90.301(2)°, and V= 1758.8(4) ų for 4 . Compounds 2 and 3 crystallize in the triclinic system, space group P‐1 and Z = 1, with a = 8.1140(3) Å, b = 8.2470(3) Å, c = 9.3120(4) Å, β = 102.2370(10)°, and V = 592.63(4) ų for 2 and a = 7.4780(2) Å, b = 12.5700(3) Å, c = 13.0450(3) Å, β = 96.351(2)°, and V = 1211.17(5) ų for 3 . Complex ( 1 ), the magnetic data was fitted by the Bleaney‐Bowers equation (1). A very good fit was derived with J = 23.96, Θ = ?1.5 (g = 1.97). Complex ( 1 ) shows the ferromagnetism. Complexes ( 2 ), ( 3 ) and ( 4 ) of have the it is the typical paramagnetic behavior of unpaired electrons. Under a low temperature around 25 K, complexes ( 2 ) and ( 3 ) show weak ferromagnetic behavior. They are the cause of hydrogen bonds.     

Manifestations of noncovalent interactions in the solid state. Dimeric and polymeric self-assembly in imidazolium salts via face-to-face cation—cation π-stacking

Abstract

X-ray crystallographic investigation of the tertiary structure of simple 1-methylimidazolium (1-Meim) salts reveals that cation—cation face-to-face π—stacking with interplanar separations in the range typically seen for molecule—molecule and molecule—cation interactions are possible. Two salts are reported. 1-Meim-CF₃SO₃, 1, exists as a centrosymmetric dimer with an interplanar separation of only 3.16 Å. The two imidazolium rings are slipped to the extent that the interaction can be regarded as a manifestation of C—H…C—H dipole interactions. 1-Meim-NO₃ exists as a one-dimensional (1-D) polymer with interplanar separations of 3.65 Å. The cations are not as severely slipped as for 1 and the interactions can be regarded as the result of cation—cation and anion—anion complementary electrostatics. Semi-empirical calculations are used to rationalize the π-π stacking in both 1 and 2. Crystal data: 1-Meim-CF₃SO₃, 1, triclinic, P1, a=6.416(3) Å, b=7.617(4) Å, c=9.569(4) Å, α=85.36(4)°, β=86.08(3)°, γ=85.18(4)°, V=463.6(4) Å,³ Z=2, D_c =1.66 g cm^?3, μ=3.7 cm^?1, T=17°C, R=0.054 and R _w=0.076 for 1241 reflections; 1-Meim-NO₃, 2, monoclinic, P2₁/c, a=9.009(7) Å, b=9.988(6) Å, c=7.308(5) Å, β=94.93(6)°, V=655.2(8) Å,³ Z=4, D_c =1.47 g cm^?3, μ=1.2 cm^?1, T=17°C, R=0.060 and R _w=0.068 for 483 reflections.     

The crystal and molecular structure of phenothiazine-10-propionitrile. The effect of crystal packing on the dihedral angle of phenothiazine heterocycles

Phenothiazine-10-propionitrile, C₁₂H₈SNC₂H₄CN, crystallizes in the centrosymmetric monoclinic space group P2₁/n, with a = 5.785(1)Å, b = 15.427(3)Å, c = 14.497(4)Å, β = 92.50(1)°, Z = 4, D_meas = 1.29(1) g cm³ and D_calc = 1.28 g cm³ at 23°. Three dimensional X-ray data were collected with a manual diffractometer using MoKα (λ 0.71069Å) radiation and by multiple film Weissenberg techniques using CuKα (λ 1.5418Å) radiation. The structure was determined by Patterson and Fourier methods and refined with 519 observed reflections by full matrix least-squares methods to an R of 0.077. The dihedral angle between the two planes of the o-phenylene rings is 135.4(3)°. In the folded heterocyclic ring the C-S-C angle is 97.8(7)° and the average C? S bond is 1.76(1)Å. A comparison of this structure to that of phenothiazine-10-propionic acid shows the two chemically similar molecules have the same dihedral angles in spite of completely different solid state packing patterns.