, and J.F. Li, H. Lee and M. Ramon for important reading of your manuscript. Y. X. is supported by the MGH Tosteson Postdoctoral Fellowship. C.X. is supported by Chinese Academy of Sciences (KSCX3-YW-N-007). The Investigation is supported by the NSF, NIH, and WJC Special Project (PJ009106) RDA-Korea to J.S.Author Manuscript Author Manuscript Author Manuscript Author Manuscript
organic compoundsActa Crystallographica Section EStructure Reports OnlineISSN 1600-2,9-Dimethyl-1,10-phenanthrolin-1-ium two,four,5-tricarboxybenzoate monohydrateKai-Long ZhongExperimentalDepartment of Applied Chemistry, Nanjing College of Chemical Technologies, Nanjing 210048, People’s Republic of China Correspondence e-mail: zklong76@163 Received 11 October 2013; accepted ten NovemberCrystal dataC14H13N2+ 10H5O8 H2O Mr = 480.42 Orthorhombic, Pbca ?a = 7.1135 (8) A ?b = 19.4512 (11) A ?c = 30.800 (2) A ?V = 4261.7 (6) A3 Z=8 Mo K radiation = 0.12 mm? T = 223 K 0.35 ?0.20 ?0.15 mm?Key indicators: single-crystal X-ray study; T = 223 K; imply (C ) = 0.005 A; R factor = 0.088; wR factor = 0.272; data-to-parameter ratio = 13.eight.Data collectionRigaku Mercury CCD diffractometer Absorption correction: multi-scan (REQAB; Jacobson, 1998) Tmin = 0.468, Tmax = 1.000 19580 measured reflections 4346 independent reflections 2278 reflections with I two(I) Rint = 0.Within the preparation in the title hydrated salt, C14H13N2+ 10H5O8 H2O, a proton has been transfered towards the two,9dimethyl-1,10-phenanthrolinium cation, forming a two,four,5-tricarboxybenzoate anion. Inside the anion, the mean planes with the protonated carboxylate groups kind dihedral angles of 11.0 (5), four.4 (five) and 80.three (4) together with the benzene ring to which they’re attached. The imply plane on the deprotonated carboxylate group types a dihedral angle of ten.six (5) with the benzene ring. Inside the crystal, the anions are involved in carboxylic acid O–H?? carboxyl hydrogen bonds, producing a two-dimensional network parallel to (001) containing R4(28) four and R4(32) motifs. The 2,9-dimethyl-1,10-phenanthrolinium four cations and water molecules reside between the anion layers and are connected towards the anions by means of N–H?? water and Owater–H?? carboxyl hydrogen bonds. An intramolecular O– H?? hydrogen bond can also be observed inside the anion.RefinementR[F two two(F 2)] = 0.088 wR(F 2) = 0.272 S = 1.00 4346 reflections 316 parameters three restraints H-atom parameters constrained ? ax = 0.37 e A? ? in = ?.40 e A?Table?Hydrogen-bond geometry (A, ).D–H?? O2–H2?? three O5–H5?? 1i O8–H8?? 3ii N1–H1A?? 1W iii O1W–H1WA?? 4ii O1W–H1WB?? 7iv D–H 0.82 0.82 0.82 0.86 0.82 0.82 H?? 1.58 1.86 1.82 1.92 1.92 two.11 D?? two.395 (four) two.671 (3) two.645 (4) 2.738 (four) two.735 (four) 2.873 (4) D–H?? 171 172 178 160 171Related literatureFor associated structures, see: Adams Ramdas (1978); MrvosSermek et al.Formula of Pd-PEPPSI-IHept-Cl (1996); Sun et al.NHS-PEG8-amide-Br web (2002a,b); Zhu et al.PMID:23551549 (2002); Li et al. (2003; 2006); Oscar et al. (2008). For background to molecular recognition and supramolecular chemistry, see: Batten Robson (1998); Juan et al. (2002); Qiu et al. (2008). For hydrogen-bond graph-set notation, see: Bernstein et al. (1995).Symmetry codes: (i) ?1; y ?1; z; (ii) x ?1; ?1; ; (iii) x ?1; y; ?1; (iv) 2 2 two two 2 two x ?1; y; z.Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear; data reduction: CrystalClear; system(s) made use of to solve structure: SHELXS97 (Sheldrick, 2008); plan(s) utilized to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008), PLATON (Spek, 2009) and.
