Crystal and molecular structure of 3-methoxy-6-nor-6,7-secooestra-1,3,5(10),9(11), 14-penten-17-one-8β-ethyl carboxylate

C₂₀H₂₂O₄,M _r =326.39, triclinic,P¯1,a=10.365(2),b=11.383(2),c=8.461(1) Å, =103.60(1),=104.44(1), =105.23(1)°,Z=2, (CuK)=1.54178 Å;R=0.0633 for 1940 reflections. The results of the X-ray analysis have shown that the ethyl carboxylate substituent is oriented. The geometry of the main skeleton of the molecule has not revealed any significant differences in the present compound and in the case of the epimeric molecule.     

Synthesis and structure of tris(N-methylaminoethanoldithiocarbamato)arsenic(III)

The title compound was synthesized by the interaction of arsenic(III)chloride with freshly prepared N-methylaminoethanoldithiocarbamic acid in methanol. The compound crystallized in the triclinic system, space groupP with two molecules per unit cell, the dimensions area=6.509(10)Å,b=14.077(3)Å,c=14.195(3)Å, =64.16(2)^o, =84.67(2)^o and =84.00(2)^o. The molecule is monomeric with three short (mean 2.320(3)Å) and three long (mean 2.927(2)Å) As-S bonds. Asymmetry in the As-S bonds is due to the presence of stereochemically active lone pair on arsenic and the coordination polyhedron deviates from the usual D₃ symmetry to C₃ symmetry. Disorder exists in one of the dithiocarbamate ligands probably due to the O...O interaction arising from the water molecule. The anisobidenticity of the As-S bond distances is as a consequence of stereochemical requirement of the ligand and the lone pair of electrons on arsenic.     

Synthesis and structure of 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2, 2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, a chiral ligand building block

A triphenyl analog of taddol, 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2,2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, has been synthesized and structurally characterized. This molecule could act as a chiral ligand building block in the creation of tuned taddol analogs. Structural analysis of the title compound reveals that the hydroxyl group is involved in an intramolecular hydrogen bond and does not take part in any intermolecular interaction. Crystal packing is influenced by C–H O hydrogen bonding and phenyl phenyl interactions. Crystal data: Triclinic, P1 (No. 1), a = 5.9343(4) Å, b = 8.2367(17) Å, c = 10.987(2) Å, = 88.290(6), = 75.442(4), = 80.655(6), V = 512.86(15) ų, Z = 1, D _calc = 1.258 mg/m³. Final residual values were R ₁ = 0.0407 for 3022 observed data (I > 2s(I) ) and wR ₂ = 0.0941 for all 3524 unique data.     

Crystal and molecular structure of 3-(4-chlorobenzoylimino)-5,6-dihydro-3H-imidazo[2,1-c]-1,2,4-dithiazole

Crystal structure of the title compound belonging to the group of-acylimino derivatives of sulfur(II) compounds has been determined by X-ray structure analysis. The crystals are monoclinic, P2₁/c,a=11.210(2),b=8.197(1),c=13.659(2) Å,=102.36(2)°,V=1226.0(3) ų,Z=4,D _x =1.61 g cm^–3, (MoK)=0.71069 Å,=6.3 cm^–1. The structure has been refined to a finalR value of 0.035 for 1401 observed reflexions.The molecule is nearly planar with symmetrym. The title compound contains a very short intramolecular C=OS contact of 2.328(3) Å, suggesting a bond-non-bond resonance interaction.     

C−Cl...π(Ar)...Cl−C,Cl...Cl and other interactions in the structures of two 6-substituted-2,4-bis(trichloromethyl)-1,3-benzdioxin's: (I) 6-carboxymethyl; (II) 6-propionyl,an antimethanogenesis food additive

C₁₂H₃Cl₆O₄, (I),M _r=428.91, triclinic, ,a=9.197(1),b=9.336(2),c=9.830(1) Å, =79.29(1), =83.33(1), =85.38(1)°,V=822.16,Z=2,D _x=1.73 Mg m^–3,F(000)=428, (MoK)=0.71069 Å, =10.62 cm^–1, room temperature, finalR=0.033 for 2573 unique counter reflections withF _o>4(F _o). C₁₃H₁₀Cl₆O₃, (II),M _r=426.94, triclinic, ,a=9.374(2),b=9.503(1),c=9.888(4) Å, =79.26(2), =82.10(3), =84.43(1)°,V=854.88,Z=2,D _c=1.66 Mg m^–3,F(000)=428, =0.71069 Å, =10.17 cm^–1, room temperature, finalR=0.030 for 2609 unique counter reflections withF _o>4(F _o). Compounds I and II are isostructural. Centrosymmetric dimers are formed by hydrogen bonds from the two methine hydrogen atoms to the carbonyl oxygen atom. The dimers are linked by Cl...(Ar)...Cl, Cl...O and Cl...Cl interactions to form a three-dimensional pattern. The geometry associated with these interactions is discussed in terms of the electrophile: nucleophile model.     

Structural characterization of 2,6-bis(N-methylenepiperidino)-4-nitrophenol (MPN) and 2,6-bis-(N-methylenemorpholino)-4-nitrophenol (MMN)3

MPN: C₁₈H₂₇N₃O₃,M _r=333.43, monoclinic,P2₁/n. a=6.207(2),b=21.893(6),c=13.693(3) Å; =96.12(2)^o,V=1850.1(8) ų.,Z=4,D _cal=1.20 mg/m³,F(000)=720, (CuK)=1.5418 Å, andT=298K.R=0.042 andwR=0.049 for 1675 observed reflections. MMN: C₁₆H₂₃N₃O₅,M _r=337.38, triclinic,P,a=9.642(1) Å,b=10.123(5) Å,c=9.341(2) Å, =93.00(3)^o, =90.96(1)^o, =110.46(1)^o, V=852.5(5) ų,D _cal=1.31 mg m^–3.F(000)=360,Z=2, (CuK)=1.5418 Å,R=0.054 andwR=0.074 for 2804 observed reflections. The piperidine and morpholino rings assumechair conformation and orient each other at an angle of 44.8(1)^o (MPN) and 47.1(1)^o (MMN), respectively.Contribution No. 827 from DCB.     

Crystal structures of 4-amino-1,2,4-triazolidine-3,5-dione (urazine) (C2H4N4O2) and dichlorobis (4-amino-1,2,4-triazolidine-3,5-dione-N,O) copper (II) (C4H8Cl2CuN8O4)

Crystal structure analyses of urazine and of its adduct with CuCl₂ show that this ligand can exchange interactions of stacking that cannot be defined as simple - interactions. The copper atoms are octahedrally coordinated by two oxygen atoms and two aminic nitrogen from chelating uraxines and two chlorine atoms. The crystals of urazine are monoclinicP2₁ c:a=6.741(1),b=5.815(1),c=11.141(2) Å,/gb=92.13(1)°,V _c=436.4(1) ų,Z=4,R=0.0402 for 714 independent observed reflections; the crystals of [CuCl₂(urazine)₂] are triclinicP¯1:a=5.236(1),b=6.662(1),c=8.411(1) Å,=93.00(1),=104.87(1), =105.69(1)°,V _c=270.66(8) ų,Z=1,R=0.0380 for 875 independent observed reflections.     

Crystal structure of 8-(3,4-dimethylphenoxy)-16H dinaphtho[2,1-d:1′,2′-g] dioxaphosphocin 8-oxide

The title compound, C₂₉H₂₃O₄P crystallizes in the triclinic space group witha=9.636(1),b=10.327(1),c=13.406(1) Å, =102.22(1), =100.59(1), =109.84(1)^o.V=1178.1(2) ų,Z=2,D _cal=1.32 M gm^–3, (CuK)=6.16 cm^–1, (CuK)=1.5418 Å andT=295K. The structure was solved by direct methods and refined by full-matrix least-squares method to a finalR=0.052 andwR=0.063 for 2708 reflections withl3(l). The napthalene ring A lies perpendicular to the best plane of the phenyl ring [91.6(1)^o] and the ring B orients at an angle of 55.7(1)^o with this plane and is inclined at an angle of 77.8(1)^o with ring A. The heterocyclic phosphorous eight-membered ring assumes a distorted boat conformation.DCB Contribution No. 822.     

The crystal structure of a cyclodecabis[1,2,3]selenadiazole

4,5,6,10,11,12-hexahydrocyclodeca[1,2-d6,7-d]bis[1,2,3]selenadiazole, C₁₀H₁₂N₄Se₂, crystallizes in triclinic space group P witha=5.4625(3),b=7.2091(4),c=8.3122(6) , =65.313(5), =77.476(5), =77.442(5)°,V=287.35(4) ³,Z=1. The structure was refined toR=0.031 andR _w=0.030 for 2018 observed reflections. The molecule lies on an inversion center. The cyclodecadiene ring adopts an elongated chair conformation. The near-zero torsion angle of the elongated chair lies at the ring-fusion bonds, with a magnitude of 2.9(3)°. The five atoms of the selenadiazole ring exhibit maximum deviation 0.005(2) from planarity, with the adjacent carbon atoms lying respectively 0.020(2) and 0.059(2) to the same side of this plane. The torsion angles about the bonds comprising the sides of the elongated chair vary in magnitude from 61.0(2)° to 55.7(2)°. The cyclodecadiene C=C bond lengths are 1.368(2) . The selenium-carbon bond length is 1.850(2) . The Se–N distance is quite long, 1.888(2) .     

Crystal and molecular structure of (exo)-2-methoxycarbonyl-5-ethoxycarbonyl-4,5,6,11b-tetrahydroisoxazolidino-[2,3-a]-β-carboline,C18H20N2O5

The structure of the title compound, C₁₈H₂₀N₂O₅, was determined by X-rays atT=290 K.M _r =344.366, monoclinic, space groupP2₁/c,a=13.7850(8),b=8.8951(7),c=15.1603(11) Å, =111.410(6)°,V _c =1730.7 ų,Z=4,D _x =1.322 Mgm^–3. Cu K radiation (graphite crystal monochromator, =1.54178 Å),(Cu K)=7.69 cm^–1. Final conventionalR-factor=0.057,R _w =0.076 for 2160 observed reflections and 271 variables. The structure was solved usingMultan.     

Crystal structure of tylophorine methiodide monohydrate,C25H30NO 4 + I−·H2O

The crystal structure of tylophorine (Chemical name 2,3,6,7 tetramethoxy phenanthro [9,10:6, 7] indolizidine. Contribution No. 0871.) methiodide monohydrate has been determined. C₂₅H₃₀NO ₄ ⁺ I^–·H₂0, triclinic, P,a=8.831(1)Å, b=10.842(2),c=13.902(2), =105.0(1)^o, =104.7(1), =97.3(1),V=1210.22ų, Z=2,D _x =1.428 g./cm^–3, (CuK)=1.54184Å, (CUK)=107.2 cm^–1, F(000)=544,T=295^oK,R=0.038,Rw=0.046, for 2331 observed reflections withI2(I). Apart from van der Waals forces, the structure is stabilized by two hydrogen bonds of the type Ow(H) ... O and Ow(H) ... I^– involving the water molecule as the donor and atom O4 of the methoxy group and I^– as acceptors.     

Crystal structure of a nucleoside analog: 2′,3′-dideoxy-3′-fluoro-5-bromocytidine

The title compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=5.084(1),b=14.322(3),c=16.065(2)Å,Z=4. The structure was solved by the heavy atom method and refined by full-matrix least-squares calculations to a finalR value of 0.033 for 1106 unique observed reflections. The N-glycosidic torsion anglex has a value of –153.7(4)°, in the anti-range. The sugar pucker is²T₃ withP=175(1)° and=30(1)°. The C4-C5 conformation is + sc with =46.7(7)°. The structure is stabilized by N-HN, N-HO and O-HO hydrogen bonds and C-HO close contacts.     

Crystal and molecular structure of OC(CoC5H5)3(CF3CCCF3)

The structure of the title compound has been confirmed by an X-ray diffraction analysis, and refined by full-matrix least squares. The crystals are mono-clinic:a=9.171(3),b=25.176(15)c=9.192(3) Å,=117.08(3)°,Z=4,D _x =1.976g cm^–3,=2.66mm^¯1, space groupP2₁/n (No. 14). The finalR value is 5.7%. Interatomic distances and bond angles are compared with those reported in related molecules.The preferred name of this compound according to the IUPAC rules is ₃-[11–2-bis(trifluoromethyl)vinylene]- ₃-carbonyl-tris (-cyclopentadienyl)-triangulo-tricobalt.     

Crystal and molecular structure of 1-methyl-2,3,5,6-tetraphenylpiperidin-4-ol,C30H29NO

The structure of the the title compound, C₃₀H₂₉NO, was determined by X-rays.M _r =419.57, triclinic, space groupP1,a=5.8922(12),b=8.5855(11),c=12.2216(20) Å,=78.145(12)°,=79.181(15)°, =76.108(14)°,V _c =581.1(1) ų,Z=1,D _x =1.199 Mg m^–3. CuK radiation (graphite crystal monochromator, =1.54184 Å),(CuK)=5.17 cm^–1,T=290K. Final conventionalR-factor=0.039,R _w =0.042 for 2795 observed reflections and 377 variables. The structure was solved usingMultan andDirdif. With a view to determining the conformational preference of the piperidine ring when it is highly sustituted with a bulky group like the phenyl group, the present X-ray investigation was undertaken.     

[Cd<Subscript>5</Subscript>(OH)(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][CH<Subscript>3</Subscript>CO<Subscript>2</Subscript>]<Subscript>9</Subscript>, a cadmium hydroxy-acetate compound with a layered network

[Cd₅(OH)(H₂O)₃][CH₃CO₂]₉ crystallizes in the triclinic system, with the space group P , a = 10.897(3) Å, b = 11.035(5) Å, c = 16.061(12) Å, = 96.83(7), = 95.31(8), = 118.22(6) and z = 2. Its structure has been determined using 9497 unique single crystal data. The final refinements let the agreement factors R₁ and wR₂(F²) converge to reach the respective values of 0.0548 and 0.0986. R₁ = 0.0338 for the 7264 unique data with I > 2(I). [Cd₅(OH)(H₂O)₃][CH₃CO₂]₉ is a cadmium hydroxide acetate compound with a bi-dimensional structure in which hydrogen bonds insure cohesion between layers stacked along the [1 10] direction. The inorganic network is built up of layers constituted of CdO₆ octahedra and CdO₇ pentagonal bi-pyramids sharing edge or corner.     

Crystal structures of five policyclic compounds related to the natural product forskolin

(3(Z),4,6a,9a,9b)-(±)-3a,4,6a,7,8,9,9a,9b-octahydro-4,7,7, 9b-tetramethyl-3a-[3-(methoxymethyloxy)-3-methyl-1-butenyl]-5H-naphto[1,8-de]-1,3-dioxin-6-one (I), C₂₂H₃₆O₅,M _r=378.51, monoclinic,P2₁/n,a=6.330(1),b=14.576(2),c=22.837(2)Å,=93.04(1)°,V=2104.1(2)ų,Z=4,D _c=1.19 Mg/m³, (MoK)=0.71069Å,=0.8 cm^–1,F(000)=832,T=298 K,R=0.054 for 1971 observed reflections; (7a,10a,10b,12)-(±)-7a,9, 10,10a,10b,11,12,12a-octahydro-2,2,10,10,10b,12a-hexamethyl-2H,8H-1-benzopyrano[4a,5,6,-de][1,3,2]-benzodioxin-11-one (II), C₂₀H₂₉O₄,M _r=334.5, triclinic,P-1,a=10.595(2),b=12.152(1),c=8.073(1)Å,=106.53(1),=105.65(1), =66.29(1)°,V=897.9(2)ų,Z=2,D _c=1.24 Mg/m³, (MoK)=0.71069Å,=0.8 cm^–1,F(000)=362,T=298 K,R=0.046 for 2848 observed reflections; (7a,10a,10b,12, 12a)-(±)-7a,9,10,10a,10b,11,12,12a-octahydro-2,2,10,10,10b,12a-hexamethyl-2H,8H-1-benzopyrano[4a,5,6-de][1,3,2]-benzodioxin-11, 12-diol (III), C₂₀H₃₂O₅ (two molecules in the asymmetric unit),M _r=352.2, triclinic,P-1,a=12.948(3),b=13.615(3),c=12.197(4)Å,=101.16(2),=111.88(2), =69.48(2)°,V=1863.8(9)ų,Z=2,D _C=1.26 Mg/m³,(MoK)=0.71069 Å,=0.8 cm^–1,F(000)=768,T=298 K,R=0.060 for 4570 observed reflections; 4-acetoxy-4-[[(4a,5,8a)-(±)-hexahydro-4a,6,6-trimethyl-4H-1,3-benzodioxin-4-one]-5-yl]butan-2-one (IV), C₁₇H₂₆O₆,M _r=326.4, monoclinic,P2₁/c,a=10.495(2),b=12.050(2),c=14.216(2)Å,=108.51(1)°,V=1704.8(5)ų,Z=4,D _c=1.27 Mg/m³,(MoK)=0.71069 Å,=0.9 cm^–1,F(000)=704,T=298 K,R=0.049 for2455 observed reflections; (3a,4,5,6,6a,9a,9b)-(±)-4,5-epoxy-decahydro-3, 3a-dihydroxy-2-ethoxy-4,7,7,9b-tetramethyl-naphto-[1,8-bc]-pyran-6-ol-acetate (V), C₂₀H₃₂O₇,M _r=383.5, monoclinic,C2/c,a=10.353(2),b=17.975(3),c=21.188(3)Å,=91.29(1)°,V=3942(1)ų,Z=8,D _c=1.29 Mg/m³,(MoK)=0.71069 Å,=0.8 cm^–1,F(000)=1664,T=298 K,R=0.051 for 2120 observed reflections. We report here the complete structures of four decalin derivatives (compoundsI, II, III, V) and one related compound (compoundIV) synthetized in order to find an efficient synthetic approach for the natural productforskolin.     

Crystal structure of 751-1751-1751-1751-2751-2751-2

The title compound crystallizes in the centrosymmetric triclinic space group (No. 2) witha=10.818(1)Å,b=10.876(1)Å,c=11.072(2)Å, =98.74(1)°, =98.83(1)°, =96.61(1)°,V=125906(3)ų andZ=2. Interatomic distances include Fe–P=2.243(2)Å, Fe–CO=1.771(6)–1.781(5)Å, Fe–C(C₅H₅)=2.074(6)–2.103(5)Å and P–F=1.511(6)–1.571(4)Å.     

Anticancer agent development. 5. X-ray structure and1H nmr spectral analysis of (1α,2α,5α,6α)-2,6-bis(3,4-methylenedioxyphenyl)-3,7-dioxabicyclo[3.3.0]octane-4,8-dione

The title compound, C₂₀H₁₄O₈, Mr=382.3, crystallized from chloroform in the centric space group P¯1 witha=6.516(4),b=6.798(3),c=9.545(7) Å,=85.31(5),=73.87(5), =79.59(4)°,V=399.2 ų, and D_calc=1.59 g cm^–3 forZ=1. Least-squares refinement of 1035 observed [F_o5(F_o)] reflections led to the final agreement index ofR=0.074. The molecule resides on a crystallographic center of inversion and is disordered into two different conformations. This manifests itself as a 50/50 disorder at O(4), C(2), and C(3). The observed structure reveals acis relationship between the bridgehead hydrogen atoms and the aryl rings. The 90 MHz¹H nmr spectrum of the title compound exhibits an AAXX spin system with a H(1)C(2) to H(1)C(3) and H(1)C(2) to H(1)C(3) coupling constant of 2.8 Hz. Computer spectral simulation and Karplus equation analysis are utilized to illustrate a relaxation of the torsion angles between H(1)C(2) and H(1)C(3), and H(1)C(2) and H(1)C(3) is solution.     

X-ray and NMR studies on the rotational isomerism about the C(5)-C(6) bond of 6-substituted methyl 2,3,4,-tri-O-acetyl-6-X-α-D-glucopyranoside derivatives

The rotamers about the C(5)–C(6) bond of a series of 2,3,4-tri-O-acetyl-6-X--D-glucopyranozide derivatives resulting by substitution at C(6) or O(6) have been studies with¹H-NMR spectroscopy (400 MHz) and X-ray structure analysis. The methyl 2,3,4-tri-O-acetyl-6-O-triphenylmethyl--D-glucopyranoside and the N-(I-O-methyl-2,3,4-tri-O-acetyl--D-glucopyranose-6-yl)-pyridinium nitrate crystallize in the P2₁ space group with =14.940(1),b=11.232(1),c=9.0773(7), and =94.480(7) anda=7.670(1),b=15.384(3),c=9.624(1) and =104.90(1), respectively; the methyl 2,3,4-tri-O-acetyl-6-O-nitro--D-glucopyranoside and methyl 2,3,4-tri-O-acetyl-6-O-deoxy-6-iodo--D-glucopyrano-side crystallize in the P2₁2₁2₁ space group witha=5.630(1),b=14.360(1) andc=22.388(3), anda=5.556(1),b=14.303(6) andc=21.963(6), respectively.     

Synthesis and structural characterization of 2,6-bis-(N-methylenemorpholino)-4-methylphenol (MMP) and 2,6-bis-(N-methylenemorpholino)-4-bromophenol (MBrP)

MMP: C₁₇H₂₆N₂O₃,M _r =306.40, monoclinic, space groupP2₁/c,a=10.927(2),b=10.777(2),c=14.197(2) , =94.04(2)°,V=1667.7(5) ³,D _cal=1.22 Mgm^–3,Z=4,F(000)=664, =5.93 cm^–1,T=293K. FinalR=0.049 andwR=0.063 for 2724 observed reflections. MBrP; C₁₆H₂₃N₂O₃Br,M _r =371.27, monoclinic, space groupP2₁/c,a=10.955(1),b=10.785(1),c=14.213(1) , =94.54(2)°,V=1674.0(4) ³,D _cal=1.48 Mgm^–3,Z=4,F(000)=768, =32.35 cm^–1,T=293K. FinalR=0.055 andwR=0.069 for 2886 observed reflections. MMP and MBrP are isostructural and in both the molecules the morpholino rings assume a chair conformation.DCB Contribution No. 824.