Chang, Kelvin B., \u2710

Norquist, Alexander J.

Smith, Matthew D, \u2713

Zeller, Matthias

English

Haverford College: Haverford Scholarship

Haverford CollegeHaverford ScholarshipFaculty Publications Chemistry10-2013catena-Poly [2, 2', 2''-nitrilotris (ethanaminium)[tri--oxido-tris [dioxidovanadate (V)]] monohydrate]Kelvin B. Chang '10Class of 2010, Haverford CollegeMatthew D. Smith '13Class of 2013, Haverford CollegeMatthias ZellerAlexander J. NorquistHaverford College, anorquis@haverford.eduFollow this and additional works at: http://scholarship.haverford.edu/chemistry_facpubsThis Journal Article is brought to you for free and open access by the Chemistry at Haverford Scholarship. It has been accepted for inclusion in FacultyPublications by an authorized administrator of Haverford Scholarship. For more information, please contact nmedeiro@haverford.edu.Repository Citation"catena-Poly [2, 2', 2''-nitrilotris (ethanaminium)[tri--oxido-tris [dioxidovanadate (V)]] monohydrate]" KB Chang, MD Smith, MZeller, AJ Norquist; Acta Crystallographica Section E: Structure Reports Online, 69 (11), m570-m57, 2013catena-Poly[2,20,20 0-nitrilotris(ethan-aminium) [tri-l-oxido-tris[dioxido-vanadate(V)]] monohydrate]Kelvin B. Chang,a Matthew D. Smith,a Matthias Zellerband Alexander J. Norquista*aDepartment of Chemistry, Haverford College, 370 Lancaster Avenue, Haverford, PA19041, USA, and bDepartment of Chemistry, Youngstown State University,1 University Plaza, Youngstown, OH 44555, USACorrespondence e-mail: anorquis@haverford.eduReceived 31 July 2013; accepted 20 September 2013Key indicators: single-crystal X-ray study; T = 100 K; mean (C–C) = 0.006 Å;R factor = 0.052; wR factor = 0.094; data-to-parameter ratio = 13.8.The title compound, {(C6H21N4)[V3O9]H2O}n, crystallizes as asalt with [trenH3]3+ cations [tren is tris(2-aminoethyl)amine],and one-dimensional anionic {[VVO3]}n (metavanadate)chains along the c-axis direction. Three crystallographicallydistinct VV sites and one occluded water molecule are presentfor every [trenH3]3+ cation in the unit cell. The {[VVO3]}nchains are composed of vertex-sharing [VO4] tetrahedra andhave a repeat unit of six tetrahedra. Each tetrahedron in thechain contains two terminal and two 2-bridging oxide ligands.The [trenH3]3+ cations, {[VVO3]}n anions and occluded watermolecules participate in an extensive three-dimensonalhydrogen-bonding network. The three terminal ammoniumsites of the [trenH3]3+ cations each form strong N—H  Ohydrogen bonds to terminal oxide ligands on the {[VVO3]}nchain. Each occluded water molecule also donates two O—H  O hydrogen bonds to the terminal oxide ligands.Related literatureFor properties of organically templated metal oxides, see:Cheetham et al. (1999). A host of amine-templated metava-nadate chains with connectivities identical to the titlecompound have been reported previously, for examples, see:Riou & Ferey (1996); Roman et al. (1991); Smith et al. (2012).Metavanadate chains with repeat units of six tetrahedra areknown to exist, see: Lin et al. (2003); Tyrselová et al. (1995).For details of the H-atom treatment in the refinement, see:Cooper et al. (2010).ExperimentalCrystal data(C6H21N4)[V3O9]H2OMr = 464.09Monoclinic, P21=ca = 9.6624 (14) Åb = 10.9179 (15) Åc = 15.768 (2) Å = 100.565 (2)V = 1635.2 (4) Å3Z = 4Mo K radiation = 1.73 mm1T = 100 K0.26  0.20  0.16 mmData collectionBruker SMART APEX CCD area-detector diffractometerAbsorption correction: multi-scan(SADABS; Bruker, 2008)Tmin = 0.623, Tmax = 0.74614279 measured reflections4719 independent reflections3195 reflections with I > 2.0(I)Rint = 0.061RefinementR[F 2 > 2(F 2)] = 0.052wR(F 2) = 0.094S = 1.002860 reflections208 parametersH-atom parameters not refinedmax = 1.44 e Å3min = 0.68 e Å3Table 1Selected bond lengths (Å).V1—O1 1.613 (3)V1—O2 1.651 (3)V1—O3 1.773 (4)V1—O4 1.793 (3)V2—V3 3.2585 (11)V2—O4 1.793 (3)V2—O5 1.654 (3)V2—O6 1.623 (4)V2—O7 1.778 (3)V3—O3i 1.769 (4)V3—O7 1.793 (3)V3—O8 1.651 (4)V3—O9 1.632 (3)Symmetry code: (i) x;yþ 32; z12.Table 2Hydrogen-bond geometry (Å, ).D—H  A D—H H  A D  A D—H  AO10—H1  O1i 0.95 2.06 2.997 (6) 170 (1)O10—H2  O9ii 0.95 1.83 2.739 (6) 160 (1)N2—H7  O8iii 0.95 1.97 2.864 (6) 155 (1)N2—H8  O1iii 0.95 2.18 2.951 (6) 138 (1)N2—H9  O5iv 0.95 1.98 2.850 (6) 152 (1)C4—H13  O9iii 0.97 2.50 3.447 (6) 167 (1)N3—H14  O5iv 0.95 2.00 2.912 (6) 162 (1)N3—H15  O2iv 0.95 1.87 2.819 (6) 176 (1)N3—H16  O6v 0.95 2.03 2.853 (6) 144 (1)N3—H16  O10v 0.95 2.23 2.925 (6) 129 (1)C6—H19  O6v 0.97 2.54 3.222 (6) 127 (1)N4—H21  O4v 0.95 2.14 3.013 (6) 152 (1)N4—H22  O2vi 0.95 1.94 2.796 (6) 150 (1)N4—H23  O5iv 0.95 1.90 2.803 (6) 157 (1)Symmetry codes: (i) x;yþ 32; z12; (ii) xþ 1; yþ12;zþ12; (iii)x þ 1;yþ 1;zþ 1; (iv) x 1; y; z; (v) xþ 1;yþ 2;zþ 1; (vi)x  1;yþ 32; z12.Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT(Bruker, 2009); data reduction: SAINT; program(s) used to solvemetal-organic compoundsm570 Chang et al. doi:10.1107/S1600536813026056 Acta Cryst. (2013). E69, m570–m571Acta Crystallographica Section EStructure ReportsOnlineISSN 1600-5368structure: SHELXS86 (Sheldrick, 2008); program(s) used to refinestructure: CRYSTALS (Betteridge et al., 2003); molecular graphics:CAMERON (Watkin et al., 1996); software used to prepare materialfor publication: CRYSTALS.The authors acknowledge support from the NSF (AwardNo. CHE-0911121), the Henry Dreyfus Teacher–ScholarAwards Program, and grants to Haverford College from theHHMI Undergraduate Science Education Program. MZacknowledges support for the purchase of a diffractometerfrom the NSF Grant 0087210, the Ohio Board of RegentsGrant CAP-491, and Youngstown State University.Supplementary data and figures for this paper are available from theIUCr electronic archives (Reference: HP2060).ReferencesBetteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J.(2003). J. Appl. Cryst. 36, 1487.Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.Bruker (2009). SAINT and APEX2. Bruker AXS Inc., Madison, Wisconsin,USA.Cheetham, A. K., Ferey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38,3268–3292.Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100–1107.Lin, B. Z., Li, Z., Pei, X. K. & Liu, P. D. (2003). J. Mol. Struct. 660, 181–186.Riou, D. & Ferey, G. (1996). J. Solid State Chem. 124, 151–154.Roman, P., Aranzabe, A., Luque, A. & Gutierrez-Zorrilla, J. (1991). Mater.Res. Bull. 26, 19–27.Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.Smith, M. D., Blau, S. M., Chang, K. B., Tran, T. T., Zeller, M., Halasyamani,P. S., Schrier, J. & Norquist, A. J. (2012). J. Solid State Chem. 195, 86–93.Tyrselová, J., Kuchta, L. & Pavelcı́k, F. (1995). Acta Cryst. C51, 1752–1754.Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. ChemicalCrystallography Laboratory, Oxford, England.metal-organic compoundsActa Cryst. (2013). E69, m570–m571 Chang et al.  (C6H21N4)[V3O9]H2O m571supplementary materialssup-1Acta Cryst. (2013). E69, m570–m571    supplementary materialsActa Cryst. (2013). E69, m570–m571    [doi:10.1107/S1600536813026056]catena-Poly[2,2′,2′′-nitrilotris(ethanaminium) [tri-µ-oxido-tris-[dioxidovanadate(V)]] monohydrate]Kelvin B. Chang, Matthew D. Smith, Matthias Zeller and Alexander J. Norquist1. Comment Organically templated metal oxides have been the subject of sustained interest for many years, owing to their structural diversity and potential to exhibit technologically desirable physical properties (Cheetham et al., 1999). Amine-templated metavanadate chain compounds are no exception, with a number of different topologies for chains with identical connectivity having been reported. The synthesis and crystal structure of the title compound, [trenH3][VO3]3·H2O, is described here. The three-dimensional packing of the title compound is shown in Fig. 2. The {[VVO3]-}n chains are composed of vertex-sharing [VO4] tetrahedra and have a repeat unit of six tetrahedra. Each tetrahedron in the chain contains two terminal and two µ2-bridging oxide ligands. The V – Oterminal and V – Obridging bond lengths range from 1.613 (4) to 1.653 (3) Å and 1.770 (4) to 1.794 (4) Å, respectively. Several compounds containing amine templated metavanadate chains have been previously reported, see: Riou et al. (1996), Roman et al. (1991), Smith et al. (2012), Lin et al. (2003) and Tyrselová et al. (1995). However, the chain topology of the inorganic anion in the title compound is novel. The [trenH3]3+ cations, {[VVO3]-}n anions and occluded water molecules participate in an extensive three-dimensonal hydrogen-bonding network. The three terminal ammonium sites of the [trenH3]3+ cations each form strong N–H···O hydrogen bonds to terminal oxide atoms on the {[VVO3]-}n chain, with N···O distances ranging from 2.796 (5) to 3.013 (5) Å. Each occluded water molecule also donates two O–H···O hydrogen bonds to the terminal oxide atoms, with O···O distances ranging from 2.738 (4) to 2.996 (5) Å.2. Experimental All chemicals (reagent grade) were commercially available and were used as received. Deionized water was used in this synthesis. The title compound was prepared under mild hydrothermal conditions in a 23 mL Teflon-lined stainless-steel autoclave. V2O5 (0.1449 g, 0.7967 mmol), Na2TeO3 (0.0889 g, 0.4012 mmol), tren (0.0620 g, 0.4240 mmol), ethanol (4 ml, 0.069 mol), and H2O (4 ml, 0.22 mol) were mixed to give a reaction mixture with a molar composition ratio of 2:1:1:170:550. The role of Na2TeO3 in this reaction is not understood. Reactions were placed in a 110 °C oven for 5 d. The reactions were then cooled to room temperature at a rate of 6 °C h-1 to promote the growth of large single crystals. Reaction vessels were opened in air, and the title compound was recovered as clear colorless needles in the presence of an unidentified tan powder via vacuum filtration.3. Refinement While the H atoms were all located in a difference map, they were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularize their geometry (C—H in the range 0.93–0.98, N—H to 0.95, and O—H = 0.95 Å) and Uiso(H) (in the range 1.2–1.5 times Ueq of the parent atom), after which the positions were refined with riding constraints (Cooper et al., 2010).supplementary materialssup-2Acta Cryst. (2013). E69, m570–m571    Computing details Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: CRYSTALS (Betteridge et al., 2003).Figure 1The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. supplementary materialssup-3Acta Cryst. (2013). E69, m570–m571    Figure 2A packing diagram of the title compound, viewed down the c axis. Orange tetrahedra represent [VO4], while red, blue and white spheres represent oxygen, nitrogen, carbon and hydrogen atoms, respectively. catena-Poly[2,2′,2′′-nitrilotris(ethanaminium) [tri-µ-oxido-tris[dioxidovanadate(V)]] monohydrate] Crystal data (C6H21N4)[V3O9]·H2OMr = 464.09Monoclinic, P21/cHall symbol: -P 2ybca = 9.6624 (14) Åb = 10.9179 (15) Åc = 15.768 (2) Åβ = 100.565 (2)°V = 1635.2 (4) Å3Z = 4F(000) = 944Dx = 1.885 Mg m−3Mo Kα radiation, λ = 0.71073 ÅCell parameters from 2067 reflectionsθ = 2.6–29.5°µ = 1.73 mm−1T = 100 KBlock, colorless0.26 × 0.20 × 0.16 mmData collection Bruker SMART APEX CCD area-detector diffractometerRadiation source: fine focus sealed tubeGraphite monochromatorω scansAbsorption correction: multi-scan (SADABS; Bruker, 2008)Tmin = 0.623, Tmax = 0.74614279 measured reflections4719 independent reflections3195 reflections with I > 2.0σ(I)Rint = 0.061θmax = 30.1°, θmin = 2.1°h = −13→13k = −15→15l = −20→22Refinement Refinement on F2Least-squares matrix: fullR[F2 > 2σ(F2)] = 0.052wR(F2) = 0.094S = 1.002860 reflections208 parameters0 restraintssupplementary materialssup-4Acta Cryst. (2013). E69, m570–m571    Primary atom site location: structure-invariant direct methodsHydrogen site location: inferred from neighbouring sitesH-atom parameters not refinedMethod = Modified Sheldrick w = 1/[σ2(F2) + (0.03P)2 + 7.47P] , where P = (max(Fo2,0) + 2Fc2)/3(Δ/σ)max = 0.0004Δρmax = 1.44 e Å−3Δρmin = −0.68 e Å−3Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) x y z Uiso*/UeqV1 0.92597 (7) 0.75226 (7) 0.71937 (5) 0.0135V2 0.87185 (7) 0.80317 (7) 0.49412 (4) 0.0120V3 0.75379 (8) 0.58481 (7) 0.35925 (5) 0.0152O1 0.8914 (4) 0.6089 (3) 0.7288 (2) 0.0320O2 1.0944 (3) 0.7734 (3) 0.7595 (2) 0.0217O3 0.8219 (5) 0.8480 (4) 0.7734 (2) 0.0498O4 0.8935 (3) 0.8036 (3) 0.6095 (2) 0.0244O5 1.0270 (3) 0.7839 (3) 0.4659 (2) 0.0220O6 0.8112 (4) 0.9374 (3) 0.4625 (2) 0.0379O7 0.7512 (4) 0.6883 (4) 0.4472 (2) 0.0354O8 0.8542 (4) 0.4695 (4) 0.4011 (3) 0.0429O9 0.5943 (3) 0.5335 (3) 0.3264 (2) 0.0233O10 0.6272 (4) 0.9517 (3) 0.2942 (2) 0.0326N1 0.3633 (3) 0.7571 (3) 0.4750 (2) 0.0124N2 0.1483 (4) 0.5617 (3) 0.4189 (2) 0.0186N3 0.2327 (4) 0.8310 (4) 0.6220 (2) 0.0199N4 0.1714 (4) 0.9305 (3) 0.3650 (2) 0.0173C1 0.3965 (4) 0.6257 (4) 0.4704 (3) 0.0144C2 0.2953 (4) 0.5559 (4) 0.4031 (3) 0.0161C3 0.4414 (4) 0.8077 (4) 0.5560 (3) 0.0180C4 0.3751 (4) 0.7766 (4) 0.6334 (3) 0.0178C5 0.4008 (5) 0.8229 (4) 0.4007 (3) 0.0195C6 0.3272 (4) 0.9449 (4) 0.3853 (3) 0.0186H1 0.7169 0.9334 0.2807 0.0389*H2 0.5660 0.9794 0.2437 0.0389*H3 0.4912 0.6178 0.4588 0.0191*H4 0.3936 0.5894 0.5259 0.0187*H5 0.2977 0.5904 0.3470 0.0191*H6 0.3247 0.4713 0.4050 0.0189*H7 0.1445 0.5268 0.4736 0.0240*H8 0.0880 0.5172 0.3752 0.0240*H9 0.1185 0.6447 0.4180 0.0240*H10 0.5379 0.7765 0.5656 0.0209*H11 0.4435 0.8963 0.5511 0.0211*H12 0.4324 0.8092 0.6858 0.0219*H13 0.3682 0.6886 0.6390 0.0222*H14 0.1764 0.7994 0.5709 0.0245*H15 0.1904 0.8116 0.6701 0.0245*H16 0.2399 0.9174 0.6173 0.0245*H17 0.3702 0.7723 0.3497 0.0240*supplementary materialssup-5Acta Cryst. (2013). E69, m570–m571    H18 0.5027 0.8342 0.4091 0.0241*H19 0.3508 0.9958 0.4366 0.0226*H20 0.3573 0.9845 0.3373 0.0229*H21 0.1284 1.0088 0.3561 0.0223*H22 0.1465 0.8828 0.3140 0.0223*H23 0.1400 0.8905 0.4115 0.0223*Atomic displacement parameters (Å2) U11 U22 U33 U12 U13 U23V1 0.0147 (3) 0.0181 (4) 0.0087 (3) 0.0034 (3) 0.0046 (3) −0.0010 (3)V2 0.0124 (3) 0.0158 (4) 0.0081 (3) 0.0005 (3) 0.0028 (3) −0.0025 (3)V3 0.0125 (3) 0.0188 (4) 0.0157 (4) −0.0053 (3) 0.0062 (3) −0.0037 (3)O1 0.032 (2) 0.025 (2) 0.036 (2) −0.0146 (15) −0.0010 (17) 0.0016 (16)O2 0.0239 (17) 0.0250 (18) 0.0149 (16) −0.0088 (13) 0.0000 (13) 0.0037 (13)O3 0.058 (3) 0.074 (3) 0.019 (2) 0.042 (2) 0.0113 (19) −0.001 (2)O4 0.0225 (16) 0.039 (2) 0.0122 (15) 0.0070 (15) 0.0038 (13) 0.0007 (15)O5 0.0161 (15) 0.034 (2) 0.0177 (16) −0.0063 (13) 0.0081 (13) −0.0052 (14)O6 0.056 (3) 0.031 (2) 0.025 (2) 0.0182 (19) 0.0041 (18) 0.0015 (16)O7 0.032 (2) 0.049 (2) 0.031 (2) −0.0281 (18) 0.0210 (17) −0.0238 (18)O8 0.028 (2) 0.032 (2) 0.071 (3) 0.0053 (17) 0.014 (2) 0.003 (2)O9 0.0206 (16) 0.0303 (19) 0.0184 (17) −0.0104 (14) 0.0023 (13) −0.0028 (14)O10 0.0283 (19) 0.047 (2) 0.0227 (19) 0.0063 (17) 0.0044 (15) 0.0061 (17)N1 0.0124 (16) 0.0120 (16) 0.0136 (17) 0.0000 (14) 0.0043 (13) 0.0019 (14)N2 0.0161 (18) 0.0198 (19) 0.0188 (19) −0.0023 (15) 0.0007 (15) −0.0005 (16)N3 0.0159 (18) 0.028 (2) 0.0158 (19) −0.0045 (16) 0.0041 (15) 0.0007 (16)N4 0.0143 (17) 0.0140 (18) 0.022 (2) 0.0004 (14) 0.0004 (15) −0.0020 (16)C1 0.0109 (19) 0.015 (2) 0.018 (2) 0.0030 (16) 0.0043 (16) 0.0040 (17)C2 0.015 (2) 0.015 (2) 0.019 (2) 0.0045 (16) 0.0043 (17) 0.0012 (17)C3 0.0107 (19) 0.019 (2) 0.024 (2) −0.0026 (17) 0.0016 (17) 0.0026 (19)C4 0.016 (2) 0.017 (2) 0.018 (2) −0.0043 (16) −0.0014 (17) −0.0005 (17)C5 0.015 (2) 0.024 (2) 0.021 (2) 0.0039 (18) 0.0090 (18) 0.0054 (19)C6 0.015 (2) 0.014 (2) 0.027 (2) 0.0009 (17) 0.0046 (18) 0.0065 (19)Geometric parameters (Å, º) V1—O1 1.613 (3) N3—H14 0.950V1—O2 1.651 (3) N3—H15 0.950V1—O3 1.773 (4) N3—H16 0.950V1—O4 1.793 (3) N4—C6 1.489 (5)V2—V3 3.2585 (11) N4—H21 0.950V2—O4 1.793 (3) N4—H22 0.950V2—O5 1.654 (3) N4—H23 0.950V2—O6 1.623 (4) C1—C2 1.510 (6)V2—O7 1.778 (3) C1—H3 0.969V3—O3i 1.769 (4) C1—H4 0.966V3—O7 1.793 (3) C2—H5 0.967V3—O8 1.651 (4) C2—H6 0.966V3—O9 1.632 (3) C3—C4 1.517 (6)O10—H1 0.950 C3—H10 0.978supplementary materialssup-6Acta Cryst. (2013). E69, m570–m571    O10—H2 0.950 C3—H11 0.970N1—C1 1.475 (5) C4—H12 0.975N1—C3 1.468 (5) C4—H13 0.968N1—C5 1.475 (5) C5—C6 1.508 (6)N2—C2 1.488 (5) C5—H17 0.976N2—H7 0.950 C5—H18 0.977N2—H8 0.950 C6—H19 0.974N2—H9 0.950 C6—H20 0.962N3—C4 1.479 (6)O1—V1—O2 107.86 (17) H15—N3—H16 109.5O1—V1—O3 112.5 (2) C6—N4—H21 109.5O2—V1—O3 109.83 (19) C6—N4—H22 109.2O1—V1—O4 112.94 (18) H21—N4—H22 109.5O2—V1—O4 108.21 (15) C6—N4—H23 109.6O3—V1—O4 105.41 (17) H21—N4—H23 109.5V3—V2—O4 128.76 (12) H22—N4—H23 109.5V3—V2—O5 87.55 (11) N1—C1—C2 114.0 (3)O4—V2—O5 109.31 (15) N1—C1—H3 108.5V3—V2—O6 113.39 (14) C2—C1—H3 109.6O4—V2—O6 106.12 (17) N1—C1—H4 108.2O5—V2—O6 109.05 (19) C2—C1—H4 107.9V3—V2—O7 24.27 (11) H3—C1—H4 108.6O4—V2—O7 111.67 (17) C1—C2—N2 112.1 (3)O5—V2—O7 110.85 (16) C1—C2—H5 109.0O6—V2—O7 109.7 (2) N2—C2—H5 108.7V2—V3—O3i 93.50 (13) C1—C2—H6 108.2V2—V3—O7 24.06 (10) N2—C2—H6 108.7O3i—V3—O7 112.99 (19) H5—C2—H6 110.2V2—V3—O8 100.80 (15) N1—C3—C4 112.9 (3)O3i—V3—O8 110.4 (2) N1—C3—H10 109.0O7—V3—O8 105.2 (2) C4—C3—H10 109.2V2—V3—O9 130.93 (12) N1—C3—H11 108.7O3i—V3—O9 111.19 (18) C4—C3—H11 107.8O7—V3—O9 108.37 (16) H10—C3—H11 109.1O8—V3—O9 108.46 (19) C3—C4—N3 109.4 (4)V1—O3—V3ii 159.3 (2) C3—C4—H12 110.0V2—O4—V1 161.2 (2) N3—C4—H12 109.1V3—O7—V2 131.66 (19) C3—C4—H13 110.0H1—O10—H2 109.5 N3—C4—H13 109.4C1—N1—C3 109.1 (3) H12—C4—H13 108.8C1—N1—C5 110.3 (3) N1—C5—C6 112.4 (3)C3—N1—C5 110.2 (3) N1—C5—H17 107.3C2—N2—H7 109.4 C6—C5—H17 107.7C2—N2—H8 109.6 N1—C5—H18 110.0H7—N2—H8 109.5 C6—C5—H18 110.1C2—N2—H9 109.5 H17—C5—H18 109.2H7—N2—H9 109.5 C5—C6—N4 111.7 (3)H8—N2—H9 109.5 C5—C6—H19 109.8supplementary materialssup-7Acta Cryst. (2013). E69, m570–m571    C4—N3—H14 109.4 N4—C6—H19 108.2C4—N3—H15 109.9 C5—C6—H20 108.8H14—N3—H15 109.5 N4—C6—H20 108.5C4—N3—H16 109.1 H19—C6—H20 109.8H14—N3—H16 109.5Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2.Hydrogen-bond geometry (Å, º) D—H···A D—H H···A D···A D—H···AO10—H1···O1i 0.95 2.06 2.997 (6) 170 (1)O10—H2···O9iii 0.95 1.83 2.739 (6) 160 (1)N2—H7···O8iv 0.95 1.97 2.864 (6) 155 (1)N2—H8···O1iv 0.95 2.18 2.951 (6) 138 (1)N2—H9···O5v 0.95 1.98 2.850 (6) 152 (1)C4—H13···O9iv 0.97 2.50 3.447 (6) 167 (1)N3—H14···O5v 0.95 2.00 2.912 (6) 162 (1)N3—H15···O2v 0.95 1.87 2.819 (6) 176 (1)N3—H16···O6vi 0.95 2.03 2.853 (6) 144 (1)N3—H16···O10vi 0.95 2.23 2.925 (6) 129 (1)C6—H19···O6vi 0.97 2.54 3.222 (6) 127 (1)N4—H21···O4vi 0.95 2.14 3.013 (6) 152 (1)N4—H22···O2vii 0.95 1.94 2.796 (6) 150 (1)N4—H23···O5v 0.95 1.90 2.803 (6) 157 (1)Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x+1, −y+2, −z+1; (vii) x−1, −y+3/2, z−1/2.

catena-Poly [2, 2\u27, 2\u27\u27-nitrilotris (ethanaminium)[tri--oxido-tris [dioxidovanadate (V)]] monohydrate]

https://scholarship.haverford.edu/cgi/viewcontent.cgi?article=1332&amp;context=chemistry_facpubs

catena-Poly [2, 2\u27, 2\u27\u27-nitrilotris (ethanaminium)[tri--oxido-tris [dioxidovanadate (V)]] monohydrate]

Abstract

Similar works

Full text

Available Versions

Haverford College: Haverford Scholarship