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C7H21NO7P2, triclinic, PI (No. 2), a = 11.404(2) A, b = 10.426(2) A, c = 6.199(2) A, a = 92.1(1)°,/? = 95.9(1)°, γ = 110.5( 1)°, V = 684.9 Α*, Ζ = 2, RP(F) = 0.061, wRidfF) = 0.160, T= 291 K. C12H44N2O18P4, triclinic, P\ (No. 2), a = 10.052(2) A, b = 9.336(2) A, c = 8.289(2) A, a = 98.4(1),/? = 104.9(1)°, γ = 106.6(1)°, V= 699.9 A 3 ,Z= 1, Rp(F) = 0.084, wRreffF) = 0.209, T= 291 K. Source of material The syntheses of the acids C5H14O7P2 and C8H22O14P4 have already been reported [1,2]. Crystallizations were done by slow evaporation from methanolic solutions at room temperature: 0.1 g of C5H14O7P2 or C8H22O14P4 were dissolved in 25 ml of methanol:water ( 1:1 ). By slow evaporation, only oily products were obtained. If a separate solution of dimethylamine is set in the vicinity of the crystallization pot, the dimethylamonium salts (C7H21NO7P2, C12H36N2O14P4 · 4H2O) shortly crystallize as large prisms. Experimental details All H atoms were initially calculated at idealized positions and refined with C-Η and O-H distances restraints. An isotropic displacement parameter was set for each hydrogen in HB PA and BHTP, riding 1.2 times of the value for the bonded atom. Discussion The hydroxy-bisphosphonic acid HBPA and the bishydroxytetraphosphonic acid BHTP are very efficient compounds for complexing metallic ions and for their transport properties in biological media [3-5]. The wide application of HBPA and BHTP ranges from their use in bone scintigraphy [6] to the extraction of trans actinides in nuclear industry [7]. In addition, several amino substituted hydroxy-bis phosphonic acids are under evaluation in medicinal treatment of bone deseases as they strongly interact and regulate the transport of calcium [3,8], Most of these biological active bis-acids have an extended alkyl-amino chain linked to the central carbon. In this respect, the crystal structures of these uncomplexed amino phosphonic acids are zwitterionic species like amino-acids. HBPA and BHTP without amino function at C(l) show superacid properties [9,10]. These compounds as free acids have poor crystalline properties although a number of structures have been reported [10-13]. In this communication, it is given evidence that they can trap and stabilize cationic species derived from volatile alcaline compounds like dimethylamine to give particularly stable crystals. A possible catalytic intermolecular dehydration of methanol, the solvent used in crystallizations, cannot be ruled out because of the superacid properties of the title compounds. This will lead to a dimethyloxonium cation [14] with a similar density signature than dimethylamonium. To confirm the nature of the central atom of the cation (N or O) and for accurate hydrogen bon network location, a neutron study on HBPA has been undertaken. This study will be published elsewhere [15]. 1. (l-Hydroxy-l-phosphono-pentyl)-phosphonic acid dimethyl ammonium salt, C7H21NO7P2 * Correspondence author (e-mail: prange@lure.u-psud.fr) Unauthenticated Download Date | 9/20/19 9:13 PM C 7 H 2 1 N O 7 P 2 and C 1 2 H 3 6 N 2 O 1 4 P 4 · 4H 2 0 155 Table 1. Data collection and handling. Table 2. Atomic coordinates and displacement parameters (in A2). Crystal: Wavelength: ftDiffractometer. scan mode: 20mux: MM/jmeaiured. N(hkl)unique: Criterion for/0bs. N(hkl)g): N(param)Kürxií· Programs: colourless, irregular, size 0.2 χ 0.2 χ 0.3 mm Cu Ka radiation (1.54180 Λ) 31.26 cm"1 Philips p w i 100. ene 128.04° 1790, 1790 /o b s > 2 σί/obsA 1776 163 SHELXS-86 [I6J, SHELXL-97 [17], Xtal-GX (18) Atom Site χ ζ fiso H(120) 21 0.324(4) -0.139(3) 0.082(7) 0.030 H(230) 21 0.490(4) 0.487(3) -0.209(7) 0.029 H(IO) 21 0.425(3) 0.030(4) -0.277(7) 0.024 H(21) 2/ 0.2832 0.2936 0.0032 0.025 H(22) 21 0.2846 0.2838 -0.2487 0.025 H(31) 21 0.1407 0.0507 -0.2570 0.037 H(32) 21 0.1292 0.0800 -0.0118 0.037 H(41) 21 0.0573 0.2214 -0.3511 0.045 H(42) 2/ -0.0390 0.1019 -0.2438 0.045 H(51) 2/ 0.1022 0.3076 0.0595 0.077 H(52) 21 -0.0451 0.2392 0.0191 0.077 H(53) 2/ 0.0251 0.3596 -0.1184 0.077 H(1N1) 2i 0.6549 0.3360 0.3705 0.034 H(2N1) 2i 0.6845 0.3101 0.5947 0.034 H(IS1) 2 i 0.7432 0.1731 0.3719 0.060 H(1S2) 21 0.8621 0.2756 0.5171 0.060 H(1S3) 2i 0.8309 0.3044 0.2755 0.060 H(2S1) 2 i 0.7348 0.5366 0.5724 0.066 H(2S2) 2¡ 0.8249 0.5315 0.4002 0.066 H(2S3) 2 i 0.8566 0.5035 0.6421 0.066 Table 3. Atomic coordinates and displacement parameters (in Â2). Atom Site χ y ζ í/ll U22 Un t/12 t/13 Í/23 P(l) 2 i 0.38297(8) 0.0808(1) 0.1529(1) 0.0287(5) 0.0162(7) 0.0107(5) 0.0147(4) -0.0002(4) 0.0059(4) P(2) 2 i 0.53859(8) 0.3216(1) -0.0715(1) 0.0285(5) 0.0121(7) 0.0159(5) 0.0124(4) -0.0006(4) 0.0057(5) 0(12) 2 i 0.2869(2) -0.0661(3) 0.0891(4) 0.029(1) 0.014(2) 0.033(2) 0.011(1) 0.001(1) 0.009(1) O( l l ) li 0.5106(2) 0.0840(3) 0.2379(4) 0.032(1) 0.020(2) 0.019(1) 0.017(1) -0.004(1) 0.004(1) 0(13) 2 i 0.3230(3) 0.1495(3) 0.3151(4) 0.047(2) 0.036(2) 0.015(1) 0.030(2) 0.004(1) 0.006(1) 0(21) 2 i 0.6384(2) 0.2673(3) -0.1274(4) 0.031(1) 0.018(2) 0.031(1) 0.017(1) 0.006(1) 0.010(1) 0 ( 2 2 ) 2 i 0.5616(2) 0.3980(3) 0.1491(4) 0.042(2) 0.018(2) 0.019(1) 0.020(1) -0.007(1) -0.000(1) 0(23) li 0.5233(3) 0.4147(3) -0.2589(4) 0.043(2) 0.019(2) 0.019(1) 0.021(1) 0.004(1) 0.012(1) O(l) li 0.3740(2) 0.0915(3) -0.2838(4) 0.038(1) 0.018(2) 0.009(1) 0.020(1) -0.005(1) -0.002(1) C( l ) li 0.3851(3) 0.1787(4) -0.0912(5) 0.031(2) 0.012(2) 0.011(2) 0.016(2) -0.000(1) 0.001(2) C(2) li 0.2759(3) 0.2313(4) -0.1215(6) 0.030(2) 0.018(2) 0.019(2) 0.014(2) -0.001(1) 0.006(2) C(3) li 0.1444(4) 0.1219(5) -0.1484(7) 0.030(2) 0.026(3) 0.039(2) 0.013(2) -0.001(2) 0.011(2) C(4) li 0.0409(4) 0.1779(5) -0.2161(8) 0.029(2) 0.040(3) 0.046(3) 0.016(2) -0.002(2) 0.013(2) C(5) 2 i 0.0298(5) 0.2804(7) -0.049(1) 0.051(3) 0.083(5) 0.072(4) 0.043(3) 0.005(3) 0.000(4) N(l) 2 i 0.7185(3) 0.3460(4) 0.4759(5) 0.030(2) 0.033(2) 0.021(2) 0.011(2) -0.003(1) 0.006(2) C(1S) 2 i 0.7954(4) 0.2680(6) 0.4038(9) 0.037(2) 0.062(4) 0.050(3) 0.023(3) -0.008(2) -0.011(3) C(2S) li 0.7898(5) 0.4918(5) 0.527(1) 0.060(3) 0.033(3) 0.061(3) 0.003(3) 0.008(3) 0.010(3) 2 . ( 1 ,8-Dihydroxy-1 ^ ^ t r i s p h o s p h o n o o c t y l ) p h o s p h o n i c a c i d b i s d i m e t h y l a m m o n i u m s a l t t e t r a h y d r a t e , C12H36N2O14P4 · 4 H 2 0 » " M Table 4. Data collection and handling. Crystal: colourless, irregular, size 0.15 χ 0.30 χ 0.60 mm Wavelength: Cu Ka radiation (1.54180 Â) μ· 32.07 cm"1 Diffractometer, scan mode: Philips PWI 100, ΘΓ2Θ 123.92° N(hkl)measured, N(hkl)unique: 1538,1538 Criterion for An». N(hkl)g¡: / o b s > 2 0 ^ , 1 5 2 0 N(param)refined: 182 Programs: SHELXS-86 [16], SHELXL-97 [17], Xtal-GX [18] Unauthenticated Download Date | 9/20/19 9:13 PM 156 C7H21NO7P2 and C12H36N2O14P4 · 4 H 2 0 Table 5. Atomic coordinates and displacement parameters (in Â). Atom Site χ y ζ fiso H(12) li 0.2980 0.3702 0.2125 0.032 H(21) li 0.1214 0.4979 0.7642 0.043 H(22) li -0.0936 0.3604 0.5749 0.037 H(l) li 0.0664 0.0737 0.3438 0.027 H(21C) li 0.3932 0.2914 0.6527 0.038 H(22C) li 0.2733 0.1443 0.6587 0.038 H(1C3) li 0.2737 0.0153 0.3953 0.038 H(2C3) li 0.3903 0.1630 0.3848 0.038 H(1C4) li 0.5610 0.1420 0.6143 0.044 H(2C4) li 0.4450 0.0006 0.6362 0.044 H(1NS) li 0.8657 0.3642 0.1982 0.036 Table S. Continued Atom Site X y ζ fiso H(2NS) li 0.9138 0.2315 0.1992 0.036 H(1S1) li 0.6301 0.2048 0.0495 0.068 H(2S1) li 0.6877 0.1782 0.2333 0.068 H(3S1) li 0.6859 0.0661 0.0717 0.068 H(1S2) li 0.8058 0.3187 -0.0911 0.060 H(2S2) li 0.8602 0.1772 -0.0886 0.060 H(3S2) li 0.9719 0.3445 -0.0062 0.060 H(1E) li 0.63(1) 0.598(3) 0.98(2) 0.142 H(2E) li 0.69(1) 0.48(1) 1.05(1) 0.142 H(3E) li 0.14(2) -0.006(6) -0.01(2) 0.157 H(4E) li 0.12(2) 0.14(1) 0.10(1) 0.157 Table 6. Atomic coordinates and displacement parameters (in Â). Atom Site X y ζ Un Í/22 Í/33 f i 2 l / | 3 1/23 P C O li 0.2683(2) 0.4427(2) 0.4270(3) 0.021(1) 0.022(1) 0.030(2) 0.0108(9) 0.013(1) 0.010(1) P(2) li 0.0752(2) 0.2905(2) 0.6310(3) 0.018(1) 0.019(1) 0.014(2) 0.0064(8) 0.004(1) 0.003(1) 0(I3) li 0.3722(6) 0.5623(6) 0.5957(8) 0.032(3) 0.026(3) 0.037(5) 0.003(3) 0.013(4) -0.006(3) CK12) li 0.3531(5) 0.4056(6) 0.3116(7) 0.022(3) 0.038(3) 0.021(4) 0.010(2) 0.006(3) 0.011(3) CKll) li 0.1473(5) 0.4981(5) 0.3460(7) 0.033(3) 0.028(3) 0.040(5) 0.016(2) 0.015(3) 0.013(3) 0(21) li 0.1579(6) 0.4307(5) 0.7783(7) 0.035(3) 0.024(3) 0.030(5) 0.014(2) 0.015(3) 0.001(3) CX23) li 0.0379(5) 0.1421(5) 0.6954(7) 0.034(3) 0.021(3) 0.033(5) 0.003(2) 0.011(3) 0.014(3) CX22) li -0.0639(6) 0.3052(6) 0.5173(7) 0.037(3) 0.035(3) 0.025(5) 0.022(3) 0.012(4) -0.002(3) CHI) li 0.0886(6) 0.1624(5) 0.3324(8) 0.028(3) 0.017(2) 0.017(5) 0.006(2) 0.002(3) 0.001(3) C(l) li 0.1873(8) 0.2638(8) 0.491(1) 0.028(5) 0.021(4) 0.011(7) 0.011(4) 0.007(6) -0.001(5) C(2) li 0.3087(9) 0.2037(9) 0.582(1) 0.031(5) 0.042(4) 0.032(7) 0.024(4) 0.010(5) 0.017(5) C(3) li 0.3575(9) 0.1048(9) 0.463(1) 0.035(5) 0.027(4) 0.035(7) 0.016(4) 0.009(5) 0.004(4) C(4) li 0.476(1) 0.052(1) 0.552(1) 0.040(5) 0.042(4) 0.035(8) 0.026(4) 0.010(6) 0.006(5) N(1S) 2i 0.8490(7) 0.2688(7) 0.1385(9) 0.034(4) 0.021(3) 0.017(6) 0.000(3) -0.006(4) -0.004(3) C(1S) li 0.700(1) 0.171(1) 0.122(2) 0.050(6) 0.044(5) 0.060(9) -0.002(5) 0.019(7) -0.002(6) C(2S) li 0.874(1) 0.278(1) -0.026(1) 0.076(7) 0.043(5) 0.036(8) 0.022(5) 0.025(7) 0.007(5) CK1E) li 0.6139(9) 0.488(1) 0.967(1) 0.075(6) 0.18(1) 0.046(7) 0.060(7) 0.014(5) 0.055(7) CK2E) li 0.147(1) 0.103(1) 0.003(1) 0.141(9) 0.18(1) 0.026(6) 0.114(9) 0.022(6) 0.022(7)

zeitschrift für kristallographie. new crystal structures/zeitschrift für kristallographie. new crystal structures

Crystal structure of (1-hydroxy-l-phosphono-pentyl)-phosphonic acid dimethyl ammonium salt, C 7 H 21 NO 7 P 2 , and of (1,8-dihydroxy-1,8,8-trisphosphono- octyl)-phosphonic acid bis-dimethylammonium salt tetrahydrate, C 12 H 36 N 2 O 14 P 4  · 4H 2 O, evidence for trapped alcaline species by bisphosphonic and tetraphosphonic acids in the crystalline state