Briarane diterpenoids from the formosan gorgonian Coral Junceella fragilis

A new trihydroxy briarane-related diterpenoid, junceellolide I (1), along with a known metabolite, (1R,2R,5Z,7R,8S,9R,10R,12R,14R,17S)-2,14-diacetoxy-8,17-epoxy-9,12-dihydroxybriara-5,11(20)-dien-19-one (2), have been isolated from the gorgonian coral Junceella fragilis, collected off the southern Taiwan coast. The structure, including the relative configuration of the new compound 1, was elucidated by the combination of spectral data, particularly in high-resolution 1H- and 13C-NMR spectroscopy utilizing COSY, HMBC, HMQC, and NOESY experiments.     

Megastigmane glucosides from Equisetum debile and E. diffusum

A new megastigmane diglucoside, (3S,5R,6S,7E,9S)-megastigman-7-ene-5,6-epoxy-3,9-diol 3,9-O-beta-D-diglucopyranoside (3), was isolated from the aerial portion of Equisetum debile along with macarangioside D (debiloside A), sammangaoside A, (6R,9S)-3-oxo-alpha-ionol 9-O-beta-D-glucopyranoside, debiloside B, kaempferol 3-O-sophoroside, kaempferol 3,7-O-beta-D-diglucopyranoside, kaempferol 3-O-sophoroside-7-O-beta-D-glucopyranoside, phenylethyl O-beta-D-glucopyranoside, (Z)-3-hexenyl O-beta-D-glucopyranoside, (7S,8R)-dehydrodiconiferyl 4-O-beta-D-glucopyranoside, and L-tryptophan. The absolute configuration at C-6 of the original structure of debilo-side A was revised to 6R-configuration, and was identical with macarangioside D (1). From the aerial portion of E. diffusum, four compounds, sammangaoside A, kaempferol 3-O-sophoroside and L-tryptophan and (3S,5R,6S,7E,9S)-megastigman-7-ene-5,6-epoxy-3,9-diol 3-O-beta-D-glucopyranoside were identified. The spectroscopic data of (3S,5R,6S,7E,9S)-megastigman-7-ene-5,6-epoxy-3,9-diol 3-O-beta-D-glucopyranoside (13) were found to be identical with corchoionoside A (9R-isomeric compound). The structure of corchoionoside A was also discussed. Structure determinations were based on physical data and spectroscopic evidence.     

Synthesis and magnetic and transport properties of Sr6V9S22O2: "AM2S5" phases revisited

The compound Sr6V9S22O2 was prepared from SrS, sulfur, vanadium metal, and V2O5 at 950 degrees C in an evacuated quartz tube. The compound is rhombohedral, R3, with a = 8.7538(6) A, c = 34.934(3) A, and Z = 3, and shows strong preferred orientation in its XRD profiles (00l) due to the layered nature of the structure. The compound contains charged CdI2 type VS2 layers of formula [V7S14]4- separated by [Sr6(VOS3)2(S2)]4+ layers. The latter has VOS3(3-) tetrahedra and S2(2-) disulfide units linked by Sr2+ ions. Magnetic susceptibility and four-probe resistivity studies show essentially temperature-independent paramagnetism above 80 K and small gap semiconductor behavior, respectively. The compound has a positive Hall coefficient at room temperature. The relationship among Sr6V9S22O2, "SrV2S5" (J. Solid State Chem. 1996, 126, 189), and other AM2S5 phases is discussed.     

Constructing conformationally constrained macrobicyclic musks

To investigate the structure-odor correlation of musks, (12R)-12-methyl-13-tridecanolide (1), a macrocyclic musk, and 13-tridecanolide, its non-musky demethyl analogue, were conformationally constrained by introduction of methylene bridges between C-3 and C-8 or C-9. These [7.5.1]- and [8.4.1]-macrobicycles were synthesized starting from bicyclo[5.3.1]undec-8-en-9-one (3) and bicyclo[4.3.1]dec-7-en-8-one (8), respectively, by a sequence consisting of catalytic hydrogenation, alpha-alkylation with a TBS-protected (tert-butyldimethylsilyl) hydroxy halide, acid-catalyzed cyclization, oxidative cleavage of the formed enol ether double bond, and subsequent reduction of the carbonyl group via its tosylhydrazone. The compound (1R,6R,9R)-(+)-6-methyl-4-oxa-bicyclo[7.5.1]pentadecan-3-one (22) was found to possess the most pronounced musk odor, and this was rationalized by a superposition analysis with the polycyclic aromatic musk odorant (4S,7R)-Galaxolide (2). In its (1S,6R,9S)-(+)-stereoisomer 23 as well as in (1S,6R, 10R)-(+)-6-methyl-4-oxabicyclo[8.4.1]-pentadecan-3-one (18) the (6R)-methyl group seems to hinder the interaction with the musk receptor, while the demethyl compounds 7 and 12 showed only very faint odors.     

异金属螺旋链化合物{[W_6Ag_6S_(24)][La(DMSO)_8]_2}_n的合成及结构表征

合成了异金属含硫化合物{[W6Ag6S24][La(Me2SO)8]2}n,并用X射线单晶衍射法测定了其结构.结果表明,该化合物属三斜晶系,P-墿空间群;晶胞参数为:a=1.577 5(3),b=1.818 7(4),c=1.952 3(4)nm,α=92.210(2)°,β=106.567(3)°,γ=92.494(2)°,Z=2,Dc=2.510 g/cm3,μ=9.081 mm-1,F(000)=3 792,R1=0.040 9,wR2=0.086 9.化合物中的阴离子[(W6Ag6S24)6-]n具有异金属螺旋链结构,所有W原子和Ag原子均与S原子形成四面体配位构型.     

Conformationally constrained dipeptide surrogates with aromatic side-chains: synthesis of 4-aryl indolizidin-9-one amino acids by conjugate addition to a common alpha,omega-diaminoazelate enone intermediate

Four methyl 9-oxo-8-(N-(Boc)-amino)-4-phenyl-1-azabicyclo[4.3.0]nonane carboxylates (11, 4-Ph-I(9)aa-OMe) were synthesized from (2S,8S,5E)-di-tert-butyl-4-oxo-5-ene-2,8-bis[N-(PhF)amino]azelate [(5E)-7, PhF = 9-(9-phenylfluorenyl)] via a seven-step process featuring a conjugate addition/reductive amination/lactam cyclization sequence. Various nucleophiles were used in the conjugate addition reactions on enone (5E)-7 as a general route for making alpha,omega-diaminoazelates possessing different substituents in good yield albeit low diastereoselectivity except in the case of aryl Grignard reagents (9/1 to 15/1 drs). 6-Phenylazelates (6S)-8d and (6R)-8d were separated by chromatography and diastereoselective precipitation and independently transformed into 4-Ph-I(9)aa-OMe. From (6S)-8d, (2S,4R,6R,8S)-4-Ph-I(9)aa-OMe 11 was prepared selectively in 51% yield. Reductive amination of (6R)-8d provided the desired pipecolates 9 along with desamino compound 10, which was minimized by performing the hydrogenation in the presence of ammonium acetate. Subsequent ester exchange, lactam cyclization, and amine protection provided three products (2R,4S,6S,8R)-, (2R,4S,6S,8S)-, and (2S,4S,6R,8S)-4-Ph-I(9)aa-OMe 11 in 10, 6, and 6% yields, respectively, from (6R)-8d. Ester hydrolysis of (2S,4R,6R,8S)-11 furnished 4-phenyl indolizidin-9-one N-(Boc)amino acid 3 as a novel constrained Ala-Phe dipeptide surrogate for studying conformation-activity relationships of biologically active peptides.     

手性3,5-二甲基-2-芳基-2-吗啉醇盐酸盐的合成及其晶体结构

以(S)-2-氨基丙醇为手性源与α-溴-3-氯苯丙酮反应, (R)-2-氨基丙醇为手性源与6-甲氧基-2-(2-溴丙酰基)萘反应, 分别合成了手性纯化合物(2R,3R,5S)-3,5-二甲基-2-(3-氯苯基)-2-吗啉醇盐酸盐(4a)和(2S,3S,5R)-3,5-二甲基-2-(6-甲氧基-2-萘基)-2-吗啉醇盐酸盐(4b), 利用X射线单晶衍射仪测定了两化合物的晶体结构和两化合物的空间结构, 并初步分析两化合物空间结构, 化合物4a晶体属正交晶系, 空间群为P2₁2₁2, 晶胞参数为: a＝0.8718(2) nm, b＝0.7883(2) nm, c＝2.0247(6) nm, Z＝4, V＝1.3915(7) nm³, D_c＝1.328 g/cm³, F(000)＝584, R₁＝0.0399, wR₂＝0.0797, S＝1.042. 化合物4b晶体属正交晶系, 空间群为P2₁2₁2₁, 晶胞参数为: a＝0.71035 (9) nm, b＝0.77703(10) nm, c＝2.9820(4) nm, Z＝4, V＝1.6318(4) nm³, D_c＝1.318 g/cm³, F(000)＝688, R₁＝0.0520, wR₂＝0.1108, S＝0.994.     

Cyclocondensation reactions of heterocyclic carbonyl compounds XII. The double course of cyclization of 3‐(2‐aminobenzyl)‐1,2‐dihydro‐quinoxaline‐2‐one

The cyclocondensation reaction of compound 1 in boiling hydrochloric acid had an unexpected course. Instead of supposed 5,11‐dihydro‐quinoxalino[2,3‐b]quinoline 6a , 2‐(indol‐2‐yl)‐benzimidazole 4 was isolated as the major product.     

Microbial transformation of diosgenin by Syncephalastrum racemosum (Cohn) Schroeter

<正>Microbial transformation of diosgenin(1) by Syncephalastrum racemosum yielded five new polar metabolites,which wereidentified as(25R)-spirost-5-en-3β,7α,9α-triol-12-one(2),(25R)-spirost-5-en-3β,9α,12α-triol-7-one(3),(25R)-spirost-5-en-3β,9α-diol-7,12-dione(4),(25R)-spirost-4-en-9α,12β,14α-triol-3-one(5),and(25S)-spirost-4-en-9α,14α,25β-triol-3-one(6).Compounds 1-6 exhibited moderate cytotoxicity against K562 cells and among them compounds 2,3,and 6 were more potentthan the parent compound 1.     

Synthesis and Self‐Assembled Helical Supramolecular Polymer of Ethyl 7,8‐dihydro‐3‐hydroxy‐9‐methyl‐7‐(4′‐nitrophenyl)‐6H‐dibenzo[c]‐ pyran‐6‐one‐8‐carboxylate

A structurally novel compound was isolated as the main product of tandem Pechmann–dehydration between diethyl 4‐hydroxy‐4‐methyl‐2‐(4′‐nitrophenyl)‐6‐oxocyclohexane‐1,3‐dicarboxylate ( 1 ) and resorcinol in the presence of trifluoroacetic acid. The structure of the product was determined as a racemate of (7R,8R)‐ and (7S,8S)‐ethyl 7,8‐dihydro‐3‐hydroxy‐9‐methyl‐7‐(4′‐nitrophenyl)‐6H‐dibenzo[c]‐pyran‐6‐one‐8‐carboxylate ( 3a ) enantiomers by single crystal X‐ray diffraction analysis. The X‐ray crystal structure revealed that 3a possesses an extended and more stable conjugated aromatic system as a consequence of the stereoselectivity of intramolecular dehydration behavior of Pechmann condensation product 2 . In the crystal superstructure, the (7R,8R)‐ and (7S,8S)‐isomers of 3a respectively self‐assembled into left‐ and right‐handed supramolecular helical chains with a channel size of 3.70 Å × 10.20 Å in virtue of intermolecular hydrogen bonding together with dramatic twisting between carboxylate group at C8 and tricyclic ring framework of 3a , which are then arranged alternatively along the b‐axis direction with a pitch length of 7.894 Å.     

Bullvalene trisepoxide and its stereospecific rearrangement to 2,8,12-trioxahexacyclo[8.3.0.0(3,9)0(4,6)0(5,13)0(7,11)]tridecane: two new C3-symmetrical oligocycles with propeller chirality

Epoxidation of bullvalene (1) with a neutralized solution of Oxone gave racemic trisepoxide rac-6 in 93 % isolated yield. Its structure was examined by X-ray crystallography. The two enantiomers of 6 were separated by preparative HPLC and exhibited specific rotations of [alpha](25)(D)= +160, [alpha](25)(365)= +567 (c=0.946, CHCl(3)) for the firstly eluted and [alpha](25)(D)= -157, [alpha](25)(365)= -554 (c=0.986, CHCl3) for the secondly eluted enantiomer of 6. The geometry of (+)-6 and the absolute configuration of (-)-6 were determined by X-ray crystal structure analysis and anomalous diffraction, respectively. According to this, (-)-6 possesses (3R,5S,7S,9R,11R,13S)- and (+)-6 has (3S,5R,7R,9S,11S,13R)-configuration. Upon treatment with BF(3)Et(2)O at -78 degrees C, trisepoxide rac-6 rearranges with retention of the skeletal three-membered carbocycle to give the cage trisether rac-8, as proved by X-ray crystal structure analysis, in virtually quantitative yield. Enantiomers of rac-8 were separated by preparative HPLC and exhibited specific rotations of [alpha](25)(D)= +49, [alpha](25)(365)= +170 (c=1.01, CHCl3) (firstly eluting) and [alpha](25)(D)= -46, [alpha](25)(365)= -160 (c=1.02, CHCl(3)) (secondly eluting enantiomer). The absolute configuration of (-)-8 was determined by anomalous diffraction to be (1R,3R,7R,9R,11R,13R). DFT computations at the TD-B3 LYP/6-31+G(d,p)//B3 LYP/6-31+G(d) level of theory for (3R,5S,7S,9R,11R,13S)-6 and (1R,3R,7R,9R,11R,13R)-8 predicted specific rotations of -206.7 and -83.4, respectively. Acid-catalyzed isomerization of the enantiomerically pure (+)-6 proceeded without racemization to give exclusively (-)-8, and (-)-6 provided only (+)-8. Thus, this isomerization occurs with ring opening of the three C--O bonds in the epoxide moieties in the alpha-position relative to the three-membered carbocycle rather than in the beta-position.     

Biotransformation of clovane derivatives. Whole cell fungi mediated domino synthesis of rumphellclovane A

Here we describe the biotransformation of clovane derivatives by filamentary fungi Pestalotiopsis palustris and Penicillium minioluteum, and the application of the latter to the synthesis and determination of the absolute configuration of rumphellclovane A (2). Methoxyclovanol (1), a growth inhibitor of the phytopathogen Botrytis cinerea, is metabolised by P. palustris to yield rumphellclovane A (2), a natural compound recently isolated from the gorgonian coral Rumphella antipathies, two new compounds, (1R,2S,5S,8R,9S,10R)-2-methoxyclovane-9,10-diol (5) and (1S,2S,5S,7R,8R,9R)-2-methoxyclovane-7,9-diol (6), hydroxylated in positions not easily accessed by classic synthetic chemistry, and clovanodiols 3 and 4. P. minioluteum is able to selectively transform methoxyclovanol (1) into clovanodiols 3 and 4 and, in turn, lactone 8, the putative intermediate in the above mentioned synthesis of rumphellclovane A (2), into compound 2 via a domino process. The ability of P. minioluteum to carry out the cleavage of ethers on clovane derivatives is also evaluated.     

A dihydro‐β‐agarofuran sesquiterpene from Maytenus boaria

The natural compound (1S ,4S ,5S ,6R ,7R ,8R ,9R ,10S )‐6‐acetoxy‐4,9,10‐trihydroxy‐2,2,5a,9‐tetramethyloctahydro‐2H‐3,9a‐methanobenzo[b ]oxepin‐5‐yl furan‐3‐carboxylate, C₂₂H₃₀O₉, (I), is a β‐agarofuran sesquiterpene isolated from the seeds of Maytenus boaria as part of a study of the secondary metabolites from Chilean flora. The compound presents a central structure formed by a decalin system esterified with acetate at site 1 and furan‐3‐carboxylate at site 9. The chirality of the skeleton can be described as 1S ,4S ,5S ,6R ,7R ,8R ,9R ,10S , which is consistent with that suggested by NMR studies. Unlike previously reported structures of sesquiterpenes containing a pure dihydro‐β‐agarofuran skeleton, (I) exhibits a three‐dimensional hydrogen‐bonded network.     

Nitrosylated iron-thiolate-sulfinate complexes with {Fe(NO)}6/7 electronic cores: relevance to the transformation between the active and inactive NO-bound forms of iron-containing nitrile hydratases

The five-coordinated iron-thiolate nitrosyl complexes [(NO)Fe(S,S-C6H3R)2]- (R = H (1), m-CH3 (2)), [(NO)Fe(S,S-C6H2-3,6-Cl2)2]- (3), [(NO)Fe(S,S-C6H3R)2]2- (R = H (10), m-CH3 (11)), and [(NO)Fe(S,S-C6H2-3,6-Cl2)2]2- (12) have been isolated and structurally characterized. Sulfur oxygenation of iron-thiolate nitrosyl complexes 1-3 containing the {Fe(NO)}6 core was triggered by O2 to yield the S-bonded monosulfinate iron species [(NO)Fe(S,SO2-C6H3R)(S,S-C6H3R)]- (R = H (4), m-CH3 (5)) and [(NO)Fe(S,SO2-C6H2-3,6-Cl2)(S,S-C6H2-3,6-Cl2)]2(2-) (6), respectively. In contrast, attack of O2 on the {Fe(NO)}7 complex 10 led to the formation of complex 1 accompanied by the minor products, [Fe(S,S-C6H4)2]2(2-) and [NO3]- (yield 9%). Reduction of complexes 4-6 by [EtS]- in CH3CN-THF yielded [(NO)Fe(S,SO2-C6H3R)(S,S-C6H3R)]2- (R = H (7), m-CH3 (8)) and [(NO)Fe(S,SO2-C6H2-3,6-Cl2)(S,S-C6H2-3,6-Cl2)]2- (9) along with (EtS)2 identified by 1H NMR. Compared to complex 10, complexes 7-9 with the less electron-donating sulfinate ligand coordinated to the {Fe(NO)}7 core were oxidized by O2 to yield complexes 4-6. Obviously, the electronic perturbation of the {Fe(NO)}7 core caused by the coordinated sulfinate in complexes 7-9 may serve to regulate the reactivity of complexes 7-9 toward O2. The iron-sulfinate nitrosyl species with the {Fe(NO)}6/7 core exhibit the photolabilization of sulfur-bound [O] moiety. Complexes 1-4-7-10 (or 2-5-8-11 and 3-6-9-12) are interconvertible under sulfur oxygenation, redox processes, and photolysis, respectively.     

螺[1-溴-4-(1R,2S,5R)-l-孟氧基-5-氧杂-6-氧代双环[3.1.0]己烷-2,2'-(3'-α-膦酸二乙酯基-(S)-苯甲氧基-4'-l-(1R,2S,5R)-孟氧基丁内酯)]的晶体结构

报道了标题化合物合成和晶体结构。X-射线结构分析表明,该化合物的分子式为C39H58BrO10P,Mr = 797.74,晶体属于单斜晶系,空间群为P21,晶胞参数a = 12.858(3), b = 25.130(5), c = 14.125(3) ? = 105.15(3), V = 4405(2) ?, Z = 4, Dc = 1.203 g/cm3, ?= 1.019 mm-1, F(000) = 1688,R = 0.0726, wR = 0.1201,共收集到9691个独立衍射点,其中可观测点5638个(I≥2s(I))。每个分子中有6个环,13个手性中心,2个五员环呈信封式构象,并分别与三员环组合成[2.4]螺环和[3.1.0]桥环化合物,4个新生成的手性中心的绝对构型为C(6)(S), C(7)(S), C(3)(R), C(2)(R),新引入的磷酸酯官能团C(9)为S构型。     

Turpinionosides A-E: megastigmane glucosides from leaves of Turpinia ternata Nakai

From leaves of Turpenia ternata (Staphylaceae), one megastigmane and seven of its glucosides (1-8) were isolated. Megastigmane and two of the glucosides were found to be known compounds, namely, 3S,5R,6R,9S-tetrahydroxymegastigmane (1), corchoionoside C (2), and icariside B4 (3). The structures of compounds 4-8 (turpinionosides A-E, respectively) were elucidated by means of spectroscopic analyses, and then their absolute structures were determined by the modified Mosher's method to be (3S,5R,6S,9S)-3,6,9-trihydroxymegastigman-7-ene 3-O- and 9-O-beta-D-glucopyranosides (4, 5, respectively), (1S,3S,5R,6S,9R)-3,9,12-trihydroxymegastigmane 3-O-beta-D-glucopyranoside (6), (3S,4R,9R)-3,4,6-trihydroxymegastigman-5-ene 3-O-beta-D-glucopyranoside (7), and (2S,9R)-2,9-dihydroxymegastigman-5-en-4-one 2-O-beta-D-glucopyranoside (8).     

Dodecanuclear manganese(III) phosphonates with cage structures

Treatments of Mn(O(2)CR)(2) (R = Me, Ph) with NBu(4)MnO(4) in CH(3)CN or CH(3)CN/CH(2)Cl(2) in the presence of acetic acid, delta(1)-cyclohexenephosphonic acid (C(6)H(9)PO(3)H(2)), and 2,2'-bipyridine or 1,10-phenanthroline result in three novel dodecamanganese(III) clusters [Mn(12)O(8)(O(2)CMe)(6)(O(3)PC(6)H(9))(7)(bipy)(3)] (1), [Mn(12)O(8)(O(2)CPh)(6)(O(3)PC(6)H(9))(7)(bipy)(3)] (2), and [Mn(12)O(8)(O(2)CPh)(6)(O(3)PC(6)H(9))(7)(phen)(3)] (3). They have a similar Mn(12) core of [Mn(III)(12)(mu(4)-O)(3)(mu(3)-O)(5)(mu-O(3)P)(3)] with a new type of topologic structure. Solid-state dc magnetic susceptibility measurements of complexes 1-3 reveal that dominant antiferromagnetic interactions are propagated between the magnetic centers. The ac magnetic measurements suggest an S = 2 ground state for compounds 1 and 3 and an S = 3 ground state for compound 2.     

Synthesis and Crystal Structure of（9S,13R,14S）-7,8-Dehydro-4-（4′-bromobenzyloxy）-3,7-dimethoxy-l7-methyl-morphinan-6-one Monohydrate

The title compound(9S,13R,14S)-7,8-dehydro-4-(4'-bromo-benzyloxy)-3,7-dime-thoxy-17-methyl-morphinan-6-one monohydrate(O-4-bromobenzylsinomenine) was synthesized by the reaction of(9S,13R,14S)-7,8-dehydro-4-hydroxy-3,7-dimethoxy-17-methyl-morphinan-6-one with 4-bromobenzyl alcohol.Its chemical structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21 with a = 8.890(2),b = 14.757(4),c = 9.205(2) ,β = 91.577(4)°,C26H30BrNO5,Mr = 516.42,μ = 1.740 mm-1,V = 1207.2(5)3,Z = 2,Dc = 1.421 mg/m3,F(000) = 536,R = 0.0785 and wR = 0.1889.     

Conformational analysis of 1,4,7-trithiacyclodecane and related compounds: Synthesis and complexation studies of mesocyclic and macrocyclic polythioethers VI

Molecular mechanics (MM2) calculations have been carried out on the ten-membered ring trithioethers, 1,4,7-trithiacyclodecane (10S3) and 1,4,7-trithiacyclodecan-9-one (keto-10S3). The lowest energy conformations according to these calculations are a [1333] and a [2233] conformation, respectively. The crystal and molecular structure of the ketone, 1,4,7-trithiacyclodecan-9-one, has been determined by a single-crystal X-ray study. The compound crystallizes in the monoclinic space group P2₁, with two molecules per unit cell of dimensions a = 7.176(1) Å, b = 5.3447(6) Å, c = 12.0914(6) Å, and β = 96.486(7)⁰, and R = 0.048. The conformation adopted by the compound in the crystalline state is a [2323] or boat-chair-boat conformation with two sulfur atoms endodentate and one sulfur atom exodentate.     

Synthesis and Crystal Structure of (9S,13R,14S)-7,8-Dehydro-4-(4'-bromobenzyloxy)-3,7-dimethoxy-17-methyl-morphinan-6-one Monohydrate

The title compound (9S,13R,14S)-7,8-dehydro-4-(4'-bromo-benzyloxy)-3,7-dime- thoxy-17-methyl-morphinan-6-one monohydrate (O-4-bromobenzylsinomenine) was synthesized by the reaction of (9S, 13R, 14S)-7,8-dehydro-4-hydroxy-3,7-dimethoxy- 17-methyl-morphinan-6-one with 4-bromobenzyl alcohol.Its chemical structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system, space group P2<,1> with a = 8.890(2), b = 14.757(4), c = 9.205(2) (A), β = 91.577(4)°, C<,26>H<,30>BrNO<,5>, M<,r> = 516.42,μ = 1.740 mm<'-1>, V = 1207.2(5) (A)<'3>, Z = 2, D<,c> = 1.421 mg/m<'3>, F(000) = 536, R = 0.0785 and wR = 0.1889.