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Crystal Structure of 5-Hydroxy-4, 6, 9, 10-Tetramethyl-1-Oxo-6

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Crystal Structure of 5-Hydroxy-4, 6, 9, 10-Tetramethyl-1-Oxo-6 Z. Kristallogr. NCS 2017; 232(2): 173–176 Open Access Guirong Wang and Fengwu Zhao* Crystal structure of 5-hydroxy-4,6,9,10-tetra- methyl-1-oxo-6-vinyldecahydro-3a,9-propano- cyclopenta[8]annulen-8-yl 2-((2-methyl-1-(3- methylbenzamido)propan-2-yl)thio)acetate, C34H49NO5S DOI 10.1515/ncrs-2016-0175 Table 1: Data collection and handling. Received May 30, 2016; accepted November 2, 2016; available online December 17, 2016 Crystal: Colourless block Size: 0.35 × 0.33 × 0.31 mm Abstract Wavelength: Mo Kα radiation (0.71073 Å) µ: 1.4 cm−1 C34H49NO5S, monoclinic, P21 (no. 4), a = 14.4605(4) Å, Diractometer, scan mode: SuperNova, ω-scans b = 9.9703(4) Å, c = 22.7599(7) Å, β = 94.799(3) Å; V = θ > 3 2 2 max, completeness: 52°, 99% 3269.90 Å , Z = 4, Rgt(F) = 0.0638, wRref(F ) = 0.1482, N(hkl)measured, N(hkl)unique, Rint: 13678, 9926, 0.039 T = 293 K. Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 5866 N(param) : 755 CCDC no.: 1482589 rened Programs: CrysAlisPRO [7], SHELX [8], OLEX2 A part of the title crystal structure is shown in the gure. [9] Tables 1 and 2 contain details on crystal structure and mea- surement conditions and a list of the atoms including atomic Source of material coordinates and displacement parameters. 3-Methylbenzoic acid (0.45 g, 3.3 mmol) was added drop- wise to a solution of 14-O-[(1-amino-2-methylpropane-2- *Corresponding author: Fengwu Zhao, Lanzhou Vocational Techni- yl)thioacetyl]mutilin (1.39 g, 3.0 mmol) and triethylamine cal College, No. 37, LiushaGonglu, Anning District, Lanzhou 730070, Gansu Province, P. R. China, e-mail: [email protected] (0.81 g, 8.0 mmol) in dichloromethane (60 mL) and was Guirong Wang: Gansu Agricultural University, No.1 Yingmen Village, stirred at room temperature for 4.5 h. Then the reaction Anning District, Lanzhou 730070, Gansu Province, P. R. China mixture was washed with saturated aqueous NH4Cl and © 2016 Guirong Wang et al., published by De Gruyter. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License. 174 Ë Wang and Zhao: C34H49NO5S Table 2: Fractional atomic coordinates and isotropic or equivalent Table 2 (continued) isotropic displacement parameters (Å2). Atom x y z Uiso*/Ueq Atom x y z Uiso*/Ueq C20 0.2904(4) 0.6786(7) 0.5173(3) 0.072(2) S1 0.49527(10) 0.2562(2) 0.26776(6) 0.0552(4) H20A 0.2392 0.7402 0.5162 0.108* O1 0.3369(4) 0.0282(6) 0.6105(2) 0.106(2) H20B 0.3396 0.7168 0.4969 0.108* O2 0.1137(3) 0.5768(5) 0.53492(18) 0.0594(12) H20C 0.3123 0.6613 0.5576 0.108* H2 0.1223 0.6037 0.5690 0.089* C21 0.4201(4) 0.3255(6) 0.3679(3) 0.0475(16) O3 0.4257(2) 0.3043(4) 0.42586(16) 0.0464(11) C22 0.5128(3) 0.2954(8) 0.3445(2) 0.0581(19) O4 0.3510(2) 0.3602(5) 0.33942(17) 0.0654(14) H22A 0.5420 0.2203 0.3658 0.070* O5 0.8192(3) 0.1258(6) 0.34510(19) 0.0781(16) H22B 0.5534 0.3727 0.3502 0.070* N1 0.7371(3) 0.0472(6) 0.2635(2) 0.0567(15) C23 0.6141(4) 0.2230(6) 0.2483(2) 0.0462(15) H1 0.7390 0.0053 0.2306 0.068* C24 0.6027(4) 0.2023(8) 0.1816(3) 0.080(2) C1 0.3410(3) 0.3181(6) 0.4578(2) 0.0387(14) H24A 0.5617 0.1281 0.1725 0.120* H1A 0.2862 0.3128 0.4295 0.046* H24B 0.6621 0.1838 0.1675 0.120* C2 0.3433(3) 0.1945(6) 0.4992(2) 0.0418(15) H24C 0.5772 0.2819 0.1630 0.120* C3 0.2767(3) 0.2158(6) 0.5483(2) 0.0476(16) C25 0.6782(4) 0.3400(7) 0.2633(3) 0.071(2) H3 0.2942 0.3015 0.5671 0.057* H25A 0.6507 0.4208 0.2468 0.107* C4 0.1711(4) 0.2250(7) 0.5290(3) 0.0563(18) H25B 0.7366 0.3248 0.2472 0.107* C5 0.1408(3) 0.3533(6) 0.4950(3) 0.0494(16) H25C 0.6879 0.3490 0.3054 0.107* H5 0.1647 0.3456 0.4561 0.059* C26 0.6478(4) 0.0948(7) 0.2798(3) 0.0540(17) C6 0.1843(4) 0.4814(6) 0.5236(3) 0.0468(16) H26A 0.6521 0.1106 0.3220 0.065* H6 0.2154 0.4555 0.5618 0.056* H26B 0.6019 0.0249 0.2712 0.065* C7 0.2584(4) 0.5467(6) 0.4874(3) 0.0452(15) C27 0.8172(4) 0.0658(7) 0.2974(3) 0.0553(17) C8 0.3459(4) 0.4578(6) 0.4861(3) 0.0473(16) C28 0.9049(4) 0.0086(7) 0.2754(3) 0.0535(17) H8A 0.3912 0.5090 0.4663 0.057* C29 0.9108(4) −0.0249(7) 0.2177(3) 0.0589(19) H8B 0.3711 0.4462 0.5266 0.057* H29 0.8586 −0.0169 0.1911 0.071* C9 0.3115(4) 0.0660(7) 0.4656(3) 0.0558(17) C30 0.9939(4) −0.0712(7) 0.1978(3) 0.0588(18) H9 0.3175 −0.0066 0.4947 0.067* C31 1.0687(4) −0.0828(8) 0.2383(3) 0.067(2) C10 0.2079(4) 0.0720(7) 0.4442(3) 0.074(2) H31 1.1248 −0.1138 0.2263 0.080* H10A 0.1982 0.1431 0.4153 0.089* C32 1.0629(5) −0.0500(9) 0.2958(4) 0.080(2) H10B 0.1900 −0.0119 0.4250 0.089* H32 1.1151 −0.0598 0.3222 0.096* C11 0.1461(4) 0.0968(8) 0.4940(4) 0.078(2) C33 0.9821(4) −0.0026(8) 0.3161(3) 0.068(2) H11A 0.1508 0.0208 0.5207 0.093* H33 0.9791 0.0211 0.3554 0.082* H11B 0.0821 0.1029 0.4776 0.093* C34 1.0008(5) −0.1042(9) 0.1339(3) 0.088(3) C12 0.2786(5) 0.1127(9) 0.5972(3) 0.080(2) H34A 0.9907 −0.0244 0.1106 0.132* C13 0.1905(5) 0.1248(10) 0.6280(4) 0.121(4) H34B 0.9546 −0.1699 0.1215 0.132* H13A 0.2034 0.1621 0.6671 0.145* H34C 1.0613 −0.1395 0.1287 0.132* H13B 0.1615 0.0377 0.6313 0.145* S2 0.45272(10) 0.2528(2) 0.76987(7) 0.0571(5) C14 0.1281(4) 0.2181(9) 0.5895(3) 0.089(3) O6 0.1262(3) 0.6114(5) 1.06007(18) 0.0636(13) H14A 0.1265 0.3065 0.6072 0.106* H6A 0.1326 0.6306 1.0952 0.095* H14B 0.0654 0.1831 0.5845 0.106* O7 0.3711(3) 0.0703(6) 1.1284(2) 0.0930(18) C15 0.3673(5) 0.0212(8) 0.4149(3) 0.086(2) O8 0.4093(2) 0.3295(4) 0.92966(16) 0.0473(10) H15A 0.3489 0.0731 0.3803 0.129* O9 0.3170(3) 0.3737(5) 0.84763(17) 0.0641(14) H15B 0.3558 −0.0721 0.4068 0.129* O10 0.7918(3) 0.1680(5) 0.82648(18) 0.0594(12) H15C 0.4322 0.0345 0.4257 0.129* N2 0.6988(3) 0.0562(6) 0.7589(2) 0.0567(14) C16 0.4425(3) 0.1779(7) 0.5280(3) 0.062(2) H2A 0.6962 0.0050 0.7284 0.068* H16A 0.4462 0.0975 0.5514 0.092* C35 0.3342(3) 0.3444(6) 0.9693(2) 0.0434(15) H16B 0.4582 0.2538 0.5528 0.092* H35 0.2739 0.3365 0.9465 0.052* H16C 0.4851 0.1719 0.4980 0.092* C36 0.3476(4) 0.2258(6) 1.0134(2) 0.0468(15) C17 0.0338(3) 0.3624(8) 0.4842(3) 0.075(2) C37 0.2950(3) 0.2505(7) 1.0683(2) 0.0429(14) H17A 0.0105 0.2828 0.4643 0.113* H37 0.3160 0.3380 1.0839 0.051* H17B 0.0174 0.4394 0.4603 0.113* C38 0.1878(3) 0.2576(7) 1.0606(2) 0.0452(14) H17C 0.0072 0.3705 0.5213 0.113* C39 0.1465(3) 0.3800(6) 1.0266(3) 0.0462(16) C18 0.2186(4) 0.5749(8) 0.4241(3) 0.067(2) H39 0.1587 0.3677 0.9852 0.055* H18 0.2404 0.5196 0.3954 0.080* C40 0.1940(4) 0.5126(6) 1.0473(3) 0.0488(16) C19 0.1603(6) 0.6629(10) 0.4054(4) 0.115(3) H40 0.2322 0.4940 1.0840 0.059* H19A 0.1357 0.7216 0.4318 0.138* C41 0.2584(4) 0.5752(6) 1.0029(3) 0.0476(15) H19B 0.1421 0.6688 0.3653 0.138* C42 0.3451(4) 0.4849(6) 0.9952(3) 0.0461(15) Wang and Zhao: C34H49NO5S Ë 175 Table 2 (continued) Table 2 (continued) Atom x y z Uiso*/Ueq Atom x y z Uiso*/Ueq H42A 0.3852 0.5344 0.9708 0.055* C64 0.9525(4) 0.0605(8) 0.7872(3) 0.065(2) H42B 0.3785 0.4760 1.0338 0.055* H64 0.9565 0.1290 0.8150 0.078* C43 0.4520(4) 0.2132(8) 1.0334(3) 0.073(2) C65 1.0331(5) 0.0030(9) 0.7705(3) 0.075(2) − H43A 0.4622 0.1340 1.0570 0.109* C66 1.0267(5) 0.0990(9) 0.7311(4) 0.087(3) − H43B 0.4717 0.2906 1.0561 0.109* H66 1.0806 0.1398 0.7204 0.104* C67 0.9427(5) −0.1431(9) 0.7069(3) 0.090(3) H43C 0.4868 0.2071 0.9993 0.109* H67 0.9397 −0.2121 0.6792 0.108* C44 0.3095(4) 0.0911(7) 0.9854(3) 0.0570(17) C68 0.8620(5) −0.0849(8) 0.7235(3) 0.074(2) H44 0.3241 0.0210 1.0149 0.068* H68 0.8047 −0.1160 0.7075 0.089* C45 0.2025(4) 0.0957(8) 0.9747(3) 0.070(2) C69 1.1259(4) 0.0544(12) 0.7977(4) 0.131(4) H45A 0.1851 0.1642 0.9456 0.084* H69A 1.1335 0.0296 0.8386 0.196* H45B 0.1803 0.0102 0.9589 0.084* H69B 1.1278 0.1504 0.7943 0.196* C46 0.1560(4) 0.1253(7) 1.0303(3) 0.0632(19) H69C 1.1751 0.0159 0.7774 0.196* H46A 0.1687 0.0521 1.0578 0.076* H46B 0.0895 0.1290 1.0207 0.076* C47 0.3105(5) 0.1518(8) 1.1194(3) 0.067(2) C48 0.2332(5) 0.1703(8) 1.1595(3) 0.087(3) water and dried with anhydrous Na2SO4 overnight.
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