metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 8| August 2008| Pages m1069-m1070

Trisodium bis­­{1-[iminio­(morpholino)meth­yl]guanidinium} bis­­[hexa­hydrogen­hexa­molybdoaluminate(III)] chloride icosa­hydrate

aKey Laboratory of Polyoxometalates Science of the Ministry of Education, College of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China
*Correspondence e-mail: liusx@nenu.edu.cn

(Received 17 June 2008; accepted 19 July 2008; online 26 July 2008)

In the title compound, Na3(C6H15N5O)2[Al(OH)6Mo6O18]2Cl·20H2O, the [Al(OH)6Mo6O18]3− polyoxo­anion has a B-type Anderson structure exhibiting approximate D3d symmetry. There are two types of sodium cations: the Na+ cations of type I have a distorted octa­hedral coordination geometry formed by six O atoms and are statistically distributed over two positions with equal occupancies, while the coordination polyhedra of the two Na+ cations of type II share one Cl anion located on an inversion center. The latter fragment, containing a Cl anion and two sodium cations, links two polyoxoanions into centrosymmetric blocks. The diprotonated 1-[imino­(morpholino)meth­yl]guanidinium cations and uncordinated water mol­ecules contribute to extensive N—H⋯O and O—H⋯O hydrogen bonding, resulting in the formation a three-dimensional supra­molecular structure.

Related literature

For related literature, see: Cao et al. (2007[Cao, R. G., Liu, S. X., Xie, L. H., Pan, Y. B., Cao, J. F., Ren, Y. H. & Xu, L. (2007). Inorg. Chem. 46, 3541-3547.]); Cheng et al. (2007[Cheng, H. Y., Liu, S. X., Xie, L. H., Ren, Y. H. & Zhang, C. D. (2007). Chem. Lett. 36, 746-747.]); Lee et al. (1991[Lee, H. Y., Park, K. M., Lee, U. & Ichida, H. (1991). Acta Cryst. C47, 1959-1961.]); Li et al. (2005[Li, D. H., Liu, S. X., Sun, C. Y., Xie, L. H., Wang, E. B., Hu, N. H. & Jia, H. Q. (2005). Inorg. Chem. Commun. 8, 433-436.]); Pope (1983[Pope, M. T. (1983). Heteropoly and Isopoly Oxometalates. New York: Springer-Verlag.]); Shivaiah et al. (2003[Shivaiah, V., Nagaraju, M. & Das, S. K. (2003). Inorg. Chem. 42, 6604-6606.]); Wang et al. (2007[Wang, F., Liu, S.-X., Wang, C.-L., Cao, R.-G. & Cao, J.-F. (2007). Acta Cryst. E63, m1708-m1709.]). For general background, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

[Scheme 1]

Experimental

Crystal data
  • Na3(C6H15N5O)2[Al(OH)6Mo6O18]2Cl·20H2O

  • Mr = 2796.54

  • Triclinic, [P \overline 1]

  • a = 10.1070 (6) Å

  • b = 11.3869 (7) Å

  • c = 17.2548 (10) Å

  • α = 81.6980 (10)°

  • β = 75.3140 (10)°

  • γ = 77.0570 (10)°

  • V = 1864.03 (19) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 2.15 mm−1

  • T = 296 (2) K

  • 0.31 × 0.25 × 0.22 mm

Data collection
  • Bruker SMART diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.528, Tmax = 0.624

  • 9902 measured reflections

  • 6882 independent reflections

  • 6108 reflections with I > 2σ(I)

  • Rint = 0.021

Refinement
  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 0.092

  • S = 1.06

  • 6882 reflections

  • 503 parameters

  • H-atom parameters constrained

  • Δρmax = 1.36 e Å−3

  • Δρmin = −1.29 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N2—H2⋯O8i 0.90 2.00 2.855 (5) 158
N3—H3⋯O7ii 0.90 1.86 2.750 (5) 173
N5—H6⋯O9iii 0.90 1.92 2.821 (5) 179
O1—H8⋯O31 0.85 1.79 2.631 (5) 170
O3—H10⋯O32 0.85 1.87 2.715 (5) 169
O4—H11⋯O27iv 0.85 1.90 2.736 (4) 170
O5—H12⋯O30v 0.85 1.94 2.769 (5) 164
O6—H13⋯O28iv 0.85 1.91 2.737 (4) 164
O26—H14⋯O19vi 0.85 2.11 2.919 (5) 159
O26—H15⋯O35vii 0.85 2.13 2.898 (5) 150
O27—H16⋯O34vii 0.85 2.12 2.918 (5) 155
O27—H17⋯O35viii 0.85 1.95 2.784 (5) 169
O28—H18⋯O17vii 0.85 2.04 2.845 (5) 158
O28—H19⋯O16vii 0.85 1.98 2.790 (5) 160
O29—H20⋯O20vi 0.85 2.08 2.853 (5) 152
O29—H21⋯O12v 0.84 1.90 2.735 (5) 168
O30—H22⋯O21vi 0.85 2.11 2.890 (5) 152
O30—H23⋯O33v 0.85 1.93 2.640 (7) 141
O31—H24⋯O32 0.86 2.09 2.889 (7) 154
O31—H25⋯O29 0.86 2.08 2.885 (6) 155
O32—H26⋯O33 0.85 2.00 2.632 (8) 130
O32—H27⋯O23ix 0.85 2.03 2.843 (6) 160
O33—H29⋯O10 0.85 1.96 2.812 (6) 176
O34—H30⋯O14ii 0.85 2.14 2.991 (5) 175
O34—H31⋯O11ix 0.85 1.94 2.756 (5) 161
O35—H32⋯O34 0.85 2.03 2.768 (5) 145
O35—H33⋯O18 0.85 2.14 2.927 (5) 155
Symmetry codes: (i) x, y+1, z; (ii) x-1, y+1, z; (iii) -x+1, -y+1, -z+1; (iv) -x+2, -y, -z+1; (v) -x+2, -y, -z; (vi) x, y-1, z; (vii) -x+1, -y, -z+1; (viii) x+1, y-1, z; (ix) x-1, y, z.

Data collection: SMART (Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1997[Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

N-Amidino-4-morpholincarboxamidine (ABOB) is an effective antiviral agent to influenza, chickenpox, and measles. It is expected that the supramolecular interaction between ABOB and polyoxometalates (POMs) (Pope, 1983) may exhibit synergistic pharmaceutical activity. In our previous work, we have isolated a few compounds based on various polyoxoanions (Cheng et al., 2007; Li et al., 2005; Wang et al., 2007). When investigating the reaction of B-type Anderson polyoxoanion [Al(OH)6Mo6O18]3- and ABOB, a compound formulated as Na3(H2ABOB)2[Al(OH)6Mo6O18]2Cl.20H2O (I) was obtained.

The asymmetric unit of (I) is composed of a [Al(OH)6Mo6O18]3- polyoxoanion, a protonated ABOB, one and a half Na+ cation, half of a Cl- ion, and ten water molecules (Fig. 1). The [Al(OH)6Mo6O18]3- polyoxoanion has a B-type Anderson structure in which six {MoO6} octahedra arrange hexagonally around the central {Al(OH)6} octahedron with approximate D3d symmetry; bond lengths and angles are within the normal ranges (Cao et al., 2007; Lee et al., 1991; Shivaiah et al., 2003). There are two types - I and II, respectively - of sodium cations: the Na+ cations of type I have a distorted octahedral coordination geometry formed by six O atoms and are statistically distributed between two positions with equal occupancies, while coordination polyhedrons of two Na+ cations of type II share one Cl anion located on an inversion center. The latter atomic fragment containig a Cl anion and two sodium cations link two polyoxoanions into centrosymmetric blocks. The diprotonated ABOB which acquires two protons from its two imine groups (N2, N4) were adopted to compensate for charge balance. Hydrogen-bonding interactions among the dimer, diprotonated ABOB, water molecules, and Cl- ion result in a three-dimensional supramolecular structure (Fig. 2).

Bond valence sum calculations (Brown & Altermatt, 1985) indicated oxidation states of 5.94–6.01 for the Mo atoms and 2.85 for the Al atom in good agreement with the expected values of 6 and 3, respectively. Furthermore, bond valence sum calculations showed that the oxidation states of the O1–O6 atoms are in the range 1.14–1.22 and the O7–O24 atoms are in the range 1.70–1.91, which agrees with the results of X-ray single-crystal diffraction determination that there are six oxygen atoms protonated.

Related literature top

For related literature, see: Cao et al. (2007); Cheng et al. (2007); Lee et al. (1991); Li et al. (2005); Pope (1983); Shivaiah et al. (2003); Wang et al. (2007). For general background, see: Brown & Altermatt (1985).

Experimental top

To a 30 ml aqueous solution of AlCl3.6H2O (0.36 g, 1.5 mmol), the 10 ml aqueous solution of Na2MoO4.2H2O (0.90 g, 3.7 mmol) and 5 ml of glacial acetic acid were added, respectively, followed by addition of 10 ml ABOB (0.10 g, 0.6 mmol). The pH of the mixture was adjusted with dilute HCl to about 2.6 and it was stirred for half an hour. The filtrate was kept for one week under ambient condition and then block crystals of (I) were collected in about 71% yield based on Mo.

Refinement top

All H atoms (except H24 and H25) were placed in idealized positions and refined as riding model approximation with C–H = 0.97 Å, Uiso(H) = 1.2 Ueq(C), O–H = 0.85 Å, N–H = 0.90 Å and Uiso(H) = 1.2 Ueq(O,N). Atoms H24 and H25 (attached to O31) were geometrically positioned and not refined. Na2 atom was treated as disordered over two positions with equal occupancies equal to 0.5.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Asymmetric unit of (I), showing 30% probability displacement ellipsoids. Solvent waters have been omitted.
[Figure 2] Fig. 2. The crystal packing of (I) along b axis with hydrogen bonds drawn as dashed lines. Solvent waters have been omitted.
Trisodium bis{1-[iminio(morpholino)methyl]guanidinium} bis[hexahydrogenhexamolybdoaluminate(III)] chloride icosahydrate top
Crystal data top
Na3(C6H15N5O)2[Al(OH)6Mo6O18]2Cl·20H2OZ = 1
Mr = 2796.54F(000) = 1364
Triclinic, P1Dx = 2.491 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.1070 (6) ÅCell parameters from 6444 reflections
b = 11.3869 (7) Åθ = 1.8–25.6°
c = 17.2548 (10) ŵ = 2.15 mm1
α = 81.698 (1)°T = 296 K
β = 75.314 (1)°Block, colourless
γ = 77.057 (1)°0.31 × 0.25 × 0.22 mm
V = 1864.03 (19) Å3
Data collection top
Bruker SMART
diffractometer
6882 independent reflections
Radiation source: fine-focus sealed tube6108 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 0 pixels mm-1θmax = 25.6°, θmin = 1.8°
ω scansh = 1212
Absorption correction: multi-scan
(SADABS; Bruker, 1997)
k = 1213
Tmin = 0.528, Tmax = 0.624l = 2020
9902 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.092 w = 1/[σ2(Fo2) + (0.0443P)2 + 4.9534P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
6882 reflectionsΔρmax = 1.36 e Å3
503 parametersΔρmin = 1.29 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0137 (3)
Crystal data top
Na3(C6H15N5O)2[Al(OH)6Mo6O18]2Cl·20H2Oγ = 77.057 (1)°
Mr = 2796.54V = 1864.03 (19) Å3
Triclinic, P1Z = 1
a = 10.1070 (6) ÅMo Kα radiation
b = 11.3869 (7) ŵ = 2.15 mm1
c = 17.2548 (10) ÅT = 296 K
α = 81.698 (1)°0.31 × 0.25 × 0.22 mm
β = 75.314 (1)°
Data collection top
Bruker SMART
diffractometer
6882 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1997)
6108 reflections with I > 2σ(I)
Tmin = 0.528, Tmax = 0.624Rint = 0.021
9902 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.092H-atom parameters constrained
S = 1.06Δρmax = 1.36 e Å3
6882 reflectionsΔρmin = 1.29 e Å3
503 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Al10.90661 (12)0.18649 (10)0.25816 (7)0.0126 (3)
Mo10.96744 (4)0.11386 (3)0.27426 (2)0.01484 (11)
Mo20.66462 (4)0.04088 (3)0.37024 (2)0.01508 (11)
Mo30.60225 (4)0.34140 (3)0.34933 (2)0.01652 (11)
Mo40.84344 (4)0.48692 (3)0.23681 (2)0.01781 (11)
Mo51.14688 (4)0.33344 (3)0.14622 (2)0.01812 (11)
Mo61.20687 (4)0.03452 (3)0.16141 (2)0.01669 (11)
Na10.8711 (2)0.19733 (17)0.50224 (11)0.0280 (4)
Na21.0528 (4)0.1445 (4)0.0459 (2)0.0327 (9)0.50
Cl11.00000.00000.50000.0242 (3)
C10.4802 (7)0.6826 (7)0.0390 (4)0.0534 (17)
H1A0.41840.75620.02440.064*
H1B0.54800.65800.00960.064*
C20.5541 (6)0.7090 (7)0.0956 (3)0.0472 (16)
H2A0.59200.78120.07440.057*
H2B0.63150.64250.10020.057*
C30.2954 (7)0.6335 (6)0.1381 (4)0.0460 (15)
H3A0.23480.57520.15730.055*
H3B0.23910.70970.12220.055*
C40.3559 (6)0.6502 (6)0.2029 (3)0.0402 (14)
H4A0.39800.57160.22500.048*
H4B0.28220.68710.24530.048*
C50.4993 (5)0.7834 (4)0.2270 (3)0.0223 (9)
C60.4182 (5)0.8042 (4)0.3722 (3)0.0197 (9)
N10.4633 (4)0.7272 (4)0.1760 (2)0.0274 (9)
N20.6204 (4)0.8142 (4)0.2137 (2)0.0284 (9)
H10.69480.78230.17650.034*
H20.64640.86790.23740.034*
N30.3989 (4)0.8116 (3)0.2962 (2)0.0214 (8)
H30.31590.84290.28400.026*
N40.5371 (4)0.7469 (4)0.3894 (2)0.0287 (9)
H40.60870.76850.35120.034*
H50.55160.74880.43850.034*
N50.3136 (4)0.8525 (4)0.4272 (2)0.0285 (9)
H60.33170.83780.47650.034*
H70.23770.91060.42440.034*
O10.9705 (3)0.0596 (3)0.19008 (17)0.0151 (6)
H80.94210.06430.14720.018*
O20.8941 (3)0.0588 (2)0.34240 (17)0.0137 (6)
H90.93110.06070.38120.016*
O30.7143 (3)0.1875 (2)0.26901 (17)0.0144 (6)
H100.68280.18320.22850.017*
O40.8404 (3)0.3137 (3)0.32567 (17)0.0151 (6)
H110.88050.31460.36330.018*
O50.9193 (3)0.3124 (3)0.17301 (17)0.0156 (6)
H120.88690.31120.13230.019*
O61.0986 (3)0.1831 (3)0.24666 (17)0.0146 (6)
H131.13120.17960.28800.018*
O71.1509 (3)0.0732 (3)0.25770 (18)0.0186 (6)
O80.7693 (3)0.0652 (3)0.28711 (18)0.0181 (6)
O90.6296 (3)0.1915 (3)0.41825 (17)0.0193 (6)
O100.6638 (3)0.4432 (3)0.25302 (19)0.0210 (6)
O111.0414 (3)0.4388 (3)0.22920 (19)0.0211 (7)
O121.1770 (3)0.1847 (3)0.09572 (18)0.0211 (7)
O130.9982 (3)0.2022 (3)0.1980 (2)0.0272 (7)
O140.9798 (3)0.2103 (3)0.35929 (19)0.0252 (7)
O150.6820 (3)0.0552 (3)0.45441 (19)0.0254 (7)
O160.5052 (3)0.0407 (3)0.3533 (2)0.0260 (7)
O170.4406 (3)0.3449 (3)0.3343 (2)0.0291 (8)
O180.5761 (4)0.4378 (3)0.4208 (2)0.0309 (8)
O190.8044 (4)0.5837 (3)0.3101 (2)0.0292 (8)
O200.8410 (4)0.5760 (3)0.1485 (2)0.0333 (8)
O211.1373 (4)0.4294 (3)0.0617 (2)0.0332 (8)
O221.3079 (4)0.3260 (3)0.1628 (2)0.0328 (8)
O231.3700 (3)0.0303 (3)0.1751 (2)0.0293 (8)
O241.2263 (4)0.0587 (3)0.08914 (19)0.0282 (7)
O250.4015 (4)0.5917 (4)0.0695 (2)0.0443 (10)
O260.7727 (4)0.3471 (3)0.4712 (2)0.0412 (9)
H140.76060.35670.42570.049*
H150.77670.40630.50720.049*
O271.0513 (4)0.3434 (3)0.5500 (2)0.0320 (8)
H161.02690.41060.56870.038*
H171.12310.37970.51850.038*
O280.7555 (3)0.1911 (3)0.6411 (2)0.0287 (7)
H180.70860.24680.65780.034*
H190.67840.14200.65390.034*
O290.8521 (5)0.1943 (4)0.0585 (2)0.0469 (10)
H200.86630.27050.06950.056*
H210.84140.20150.01260.056*
O301.1468 (5)0.3344 (4)0.0247 (3)0.0468 (10)
H221.11440.39290.00460.056*
H231.23500.35170.03130.056*
O310.8656 (6)0.0541 (4)0.0661 (3)0.0680 (16)
H240.79630.10500.09060.082*
H250.83430.01110.06880.082*
O320.5896 (5)0.1589 (5)0.1528 (3)0.0566 (12)
H260.55320.22430.12920.068*
H270.53560.10830.16710.068*
O330.5983 (6)0.3897 (5)0.1147 (3)0.0774 (16)
H280.52060.42550.10420.093*
H290.61480.40840.15680.093*
O340.1012 (4)0.5252 (3)0.3550 (2)0.0393 (9)
H310.10080.48800.31580.047*
H300.06240.59950.35600.047*
O350.2881 (4)0.5691 (4)0.4350 (2)0.0400 (9)
H320.26340.55080.39540.048*
H330.37070.54610.44180.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.0114 (6)0.0125 (6)0.0131 (6)0.0000 (5)0.0035 (5)0.0004 (5)
Mo10.01445 (19)0.01288 (19)0.01581 (19)0.00011 (14)0.00296 (14)0.00181 (14)
Mo20.01243 (19)0.01500 (19)0.01653 (19)0.00142 (14)0.00272 (14)0.00036 (14)
Mo30.0136 (2)0.01542 (19)0.0182 (2)0.00193 (14)0.00290 (14)0.00296 (14)
Mo40.0185 (2)0.01218 (19)0.0213 (2)0.00010 (14)0.00548 (15)0.00012 (14)
Mo50.0164 (2)0.0168 (2)0.0192 (2)0.00425 (14)0.00140 (15)0.00134 (15)
Mo60.0132 (2)0.01648 (19)0.0180 (2)0.00022 (14)0.00215 (14)0.00154 (14)
Na10.0300 (10)0.0288 (10)0.0256 (10)0.0043 (8)0.0102 (8)0.0007 (8)
Na20.034 (2)0.040 (2)0.026 (2)0.0118 (18)0.0036 (17)0.0084 (17)
Cl10.0264 (8)0.0258 (8)0.0232 (8)0.0042 (6)0.0117 (6)0.0015 (6)
C10.053 (4)0.076 (5)0.033 (3)0.020 (3)0.001 (3)0.018 (3)
C20.034 (3)0.086 (5)0.026 (3)0.025 (3)0.010 (2)0.025 (3)
C30.043 (3)0.047 (4)0.053 (4)0.018 (3)0.006 (3)0.014 (3)
C40.034 (3)0.053 (4)0.036 (3)0.022 (3)0.005 (2)0.016 (3)
C50.021 (2)0.026 (2)0.019 (2)0.0008 (18)0.0077 (18)0.0025 (18)
C60.025 (2)0.015 (2)0.020 (2)0.0021 (17)0.0081 (18)0.0012 (17)
N10.025 (2)0.041 (2)0.019 (2)0.0114 (18)0.0028 (16)0.0093 (18)
N20.022 (2)0.038 (2)0.027 (2)0.0077 (18)0.0031 (17)0.0125 (18)
N30.0178 (19)0.029 (2)0.0152 (18)0.0043 (15)0.0063 (15)0.0052 (15)
N40.027 (2)0.035 (2)0.025 (2)0.0001 (18)0.0141 (17)0.0013 (18)
N50.030 (2)0.031 (2)0.022 (2)0.0012 (18)0.0032 (17)0.0094 (17)
O10.0162 (15)0.0164 (14)0.0132 (14)0.0020 (11)0.0045 (11)0.0027 (11)
O20.0129 (14)0.0144 (14)0.0142 (14)0.0005 (11)0.0067 (11)0.0007 (11)
O30.0119 (14)0.0165 (14)0.0155 (14)0.0002 (11)0.0064 (11)0.0018 (11)
O40.0145 (15)0.0146 (14)0.0179 (14)0.0011 (11)0.0074 (11)0.0033 (11)
O50.0167 (15)0.0171 (14)0.0133 (14)0.0006 (11)0.0080 (11)0.0017 (11)
O60.0115 (14)0.0164 (14)0.0166 (14)0.0014 (11)0.0051 (11)0.0025 (11)
O70.0129 (15)0.0193 (15)0.0225 (16)0.0011 (12)0.0055 (12)0.0011 (12)
O80.0141 (15)0.0182 (15)0.0235 (16)0.0022 (12)0.0059 (12)0.0057 (12)
O90.0199 (16)0.0187 (15)0.0158 (15)0.0000 (12)0.0006 (12)0.0029 (12)
O100.0157 (15)0.0183 (15)0.0269 (17)0.0015 (12)0.0079 (13)0.0026 (13)
O110.0159 (15)0.0197 (15)0.0281 (17)0.0025 (12)0.0059 (13)0.0041 (13)
O120.0244 (17)0.0192 (15)0.0160 (15)0.0022 (13)0.0007 (12)0.0000 (12)
O130.0271 (18)0.0250 (17)0.0298 (18)0.0005 (14)0.0063 (14)0.0129 (14)
O140.0274 (18)0.0184 (16)0.0260 (17)0.0006 (13)0.0060 (14)0.0038 (13)
O150.0261 (18)0.0222 (16)0.0238 (17)0.0019 (13)0.0040 (14)0.0043 (13)
O160.0163 (16)0.0260 (17)0.0361 (19)0.0034 (13)0.0073 (14)0.0027 (14)
O170.0187 (17)0.0305 (18)0.0363 (19)0.0011 (14)0.0097 (14)0.0026 (15)
O180.033 (2)0.0261 (18)0.0303 (19)0.0022 (15)0.0020 (15)0.0124 (15)
O190.0308 (19)0.0184 (16)0.039 (2)0.0014 (14)0.0072 (16)0.0097 (14)
O200.034 (2)0.0271 (18)0.035 (2)0.0041 (15)0.0101 (16)0.0115 (15)
O210.041 (2)0.0246 (18)0.0289 (18)0.0069 (15)0.0048 (16)0.0087 (15)
O220.0211 (18)0.0329 (19)0.046 (2)0.0099 (15)0.0063 (16)0.0031 (17)
O230.0155 (16)0.0285 (18)0.043 (2)0.0030 (13)0.0106 (15)0.0038 (15)
O240.035 (2)0.0224 (17)0.0234 (17)0.0013 (14)0.0014 (14)0.0051 (14)
O250.049 (3)0.049 (2)0.037 (2)0.015 (2)0.0010 (18)0.0233 (19)
O260.056 (3)0.035 (2)0.037 (2)0.0177 (19)0.0168 (19)0.0055 (17)
O270.0309 (19)0.0327 (19)0.0318 (19)0.0024 (15)0.0117 (15)0.0068 (15)
O280.0192 (17)0.038 (2)0.0297 (18)0.0064 (14)0.0061 (14)0.0035 (15)
O290.061 (3)0.047 (2)0.031 (2)0.003 (2)0.0201 (19)0.0056 (18)
O300.057 (3)0.035 (2)0.053 (3)0.0123 (19)0.025 (2)0.0108 (19)
O310.107 (4)0.041 (2)0.076 (3)0.010 (3)0.070 (3)0.020 (2)
O320.049 (3)0.078 (3)0.050 (3)0.016 (2)0.024 (2)0.002 (2)
O330.068 (4)0.094 (4)0.075 (4)0.002 (3)0.029 (3)0.021 (3)
O340.038 (2)0.036 (2)0.048 (2)0.0004 (17)0.0182 (18)0.0154 (18)
O350.029 (2)0.044 (2)0.048 (2)0.0031 (17)0.0107 (17)0.0188 (19)
Geometric parameters (Å, º) top
Al1—O41.887 (3)Na2—H252.3601
Al1—O11.890 (3)Cl1—Na1ii2.8298 (19)
Al1—O61.892 (3)C1—O251.408 (7)
Al1—O51.900 (3)C1—C21.468 (8)
Al1—O31.902 (3)C1—H1A0.9700
Al1—O21.903 (3)C1—H1B0.9700
Mo1—O131.696 (3)C2—N11.471 (6)
Mo1—O141.715 (3)C2—H2A0.9700
Mo1—O81.918 (3)C2—H2B0.9700
Mo1—O71.953 (3)C3—O251.439 (7)
Mo1—O12.277 (3)C3—C41.455 (8)
Mo1—O22.317 (3)C3—H3A0.9700
Mo2—O151.709 (3)C3—H3B0.9700
Mo2—O161.709 (3)C4—N11.488 (6)
Mo2—O91.934 (3)C4—H4A0.9700
Mo2—O81.948 (3)C4—H4B0.9700
Mo2—O32.276 (3)C5—N21.304 (6)
Mo2—O22.296 (3)C5—N11.321 (6)
Mo3—O181.700 (3)C5—N31.383 (6)
Mo3—O171.709 (3)C6—N51.304 (6)
Mo3—O101.932 (3)C6—N41.316 (6)
Mo3—O91.943 (3)C6—N31.361 (5)
Mo3—O42.293 (3)N2—H10.9000
Mo3—O32.300 (3)N2—H20.8998
Mo4—O201.706 (3)N3—H30.8999
Mo4—O191.710 (3)N4—H40.9000
Mo4—O111.928 (3)N4—H50.9000
Mo4—O101.931 (3)N5—H60.8999
Mo4—O52.296 (3)N5—H70.8999
Mo4—O42.318 (3)O1—H80.8500
Mo5—O211.701 (3)O2—H90.8500
Mo5—O221.704 (3)O3—H100.8501
Mo5—O111.943 (3)O4—H110.8499
Mo5—O121.945 (3)O5—H120.8500
Mo5—O52.288 (3)O6—H130.8499
Mo5—O62.293 (3)O26—H140.8499
Mo6—O241.698 (3)O26—H150.8501
Mo6—O231.713 (3)O27—H160.8500
Mo6—O121.919 (3)O27—H170.8500
Mo6—O71.957 (3)O28—H180.8500
Mo6—O12.274 (3)O28—H190.8500
Mo6—O62.301 (3)O29—H200.8486
Na1—O262.340 (4)O29—H210.8441
Na1—O282.388 (4)O30—H220.8500
Na1—O272.402 (4)O30—H230.8501
Na1—O142.444 (4)O31—Na2i2.116 (7)
Na1—O152.446 (4)O31—H240.8624
Na1—Cl12.8298 (19)O31—H250.8617
Na2—O31i2.116 (7)O32—H260.8501
Na2—O292.177 (6)O32—H270.8500
Na2—O242.496 (5)O33—H280.8500
Na2—O302.513 (6)O33—H290.8500
Na2—O132.559 (5)O34—H310.8499
Na2—O312.607 (6)O34—H300.8500
Na2—Na2i3.502 (9)O35—H320.8500
Na2—H202.5362O35—H330.8500
Na2—H212.5822
O4—Al1—O1179.20 (13)O29—Na2—H2018.8
O4—Al1—O696.29 (13)O24—Na2—H20153.3
O1—Al1—O684.45 (13)O30—Na2—H2069.5
O4—Al1—O584.77 (13)O13—Na2—H2075.6
O1—Al1—O594.99 (13)O31—Na2—H2091.6
O6—Al1—O584.48 (13)Na2i—Na2—H20111.3
O4—Al1—O384.60 (13)O31i—Na2—H2199.6
O1—Al1—O394.66 (13)O29—Na2—H2118.0
O6—Al1—O3179.09 (13)O24—Na2—H21169.8
O5—Al1—O395.81 (13)O30—Na2—H2174.0
O4—Al1—O296.00 (13)O13—Na2—H2199.1
O1—Al1—O284.23 (13)O31—Na2—H2177.7
O6—Al1—O295.63 (13)Na2i—Na2—H2186.7
O5—Al1—O2179.20 (13)H20—Na2—H2127.3
O3—Al1—O284.06 (13)O31i—Na2—H2595.2
O13—Mo1—O14106.44 (16)O29—Na2—H2554.5
O13—Mo1—O897.66 (14)O24—Na2—H25109.9
O14—Mo1—O8101.93 (14)O30—Na2—H25133.5
O13—Mo1—O7100.20 (15)O13—Na2—H2586.1
O14—Mo1—O795.41 (14)O31—Na2—H2519.2
O8—Mo1—O7150.41 (12)Na2i—Na2—H2549.6
O13—Mo1—O193.31 (14)H20—Na2—H2572.4
O14—Mo1—O1158.53 (13)H21—Na2—H2560.0
O8—Mo1—O183.25 (12)Na1—Cl1—Na1ii180.00 (4)
O7—Mo1—O172.38 (11)O25—C1—C2114.0 (5)
O13—Mo1—O2158.48 (14)O25—C1—H1A108.8
O14—Mo1—O294.31 (13)C2—C1—H1A108.8
O8—Mo1—O271.94 (11)O25—C1—H1B108.8
O7—Mo1—O283.10 (11)C2—C1—H1B108.8
O1—Mo1—O267.22 (10)H1A—C1—H1B107.7
O15—Mo2—O16107.36 (16)C1—C2—N1112.6 (5)
O15—Mo2—O997.76 (14)C1—C2—H2A109.1
O16—Mo2—O9101.84 (14)N1—C2—H2A109.1
O15—Mo2—O8100.08 (14)C1—C2—H2B109.1
O16—Mo2—O894.96 (14)N1—C2—H2B109.1
O9—Mo2—O8150.56 (12)H2A—C2—H2B107.8
O15—Mo2—O3157.71 (14)O25—C3—C4111.5 (5)
O16—Mo2—O394.40 (13)O25—C3—H3A109.3
O9—Mo2—O372.44 (11)C4—C3—H3A109.3
O8—Mo2—O382.39 (12)O25—C3—H3B109.3
O15—Mo2—O291.79 (13)C4—C3—H3B109.3
O16—Mo2—O2158.68 (13)H3A—C3—H3B108.0
O9—Mo2—O284.31 (12)C3—C4—N1112.9 (5)
O8—Mo2—O271.95 (11)C3—C4—H4A109.0
O3—Mo2—O267.73 (10)N1—C4—H4A109.0
O18—Mo3—O17105.49 (17)C3—C4—H4B109.0
O18—Mo3—O10100.65 (15)N1—C4—H4B109.0
O17—Mo3—O1096.30 (15)H4A—C4—H4B107.8
O18—Mo3—O997.33 (15)N2—C5—N1123.4 (4)
O17—Mo3—O9101.13 (15)N2—C5—N3120.5 (4)
O10—Mo3—O9150.56 (12)N1—C5—N3116.0 (4)
O18—Mo3—O493.17 (14)N5—C6—N4121.7 (4)
O17—Mo3—O4159.96 (14)N5—C6—N3117.6 (4)
O10—Mo3—O472.67 (11)N4—C6—N3120.7 (4)
O9—Mo3—O483.28 (12)C5—N1—C2120.3 (4)
O18—Mo3—O3158.31 (14)C5—N1—C4122.1 (4)
O17—Mo3—O395.15 (14)C2—N1—C4115.3 (4)
O10—Mo3—O383.29 (12)C5—N2—H1122.8
O9—Mo3—O371.74 (11)C5—N2—H2129.3
O4—Mo3—O367.44 (10)H1—N2—H2107.9
O20—Mo4—O19106.06 (17)C6—N3—C5127.3 (4)
O20—Mo4—O11100.82 (16)C6—N3—H3122.6
O19—Mo4—O1198.43 (15)C5—N3—H3109.9
O20—Mo4—O1097.79 (15)C6—N4—H4109.8
O19—Mo4—O1099.41 (15)C6—N4—H5119.8
O11—Mo4—O10149.46 (13)H4—N4—H5109.9
O20—Mo4—O592.72 (14)C6—N5—H6112.3
O19—Mo4—O5160.56 (14)C6—N5—H7132.5
O11—Mo4—O572.58 (11)H6—N5—H7113.4
O10—Mo4—O582.59 (12)Al1—O1—Mo6104.56 (13)
O20—Mo4—O4158.16 (14)Al1—O1—Mo1105.23 (13)
O19—Mo4—O494.86 (14)Mo6—O1—Mo193.54 (11)
O11—Mo4—O481.85 (12)Al1—O1—H8120.5
O10—Mo4—O472.12 (11)Mo6—O1—H8110.4
O5—Mo4—O467.18 (10)Mo1—O1—H8118.5
O21—Mo5—O22106.29 (18)Al1—O2—Mo2103.71 (12)
O21—Mo5—O11100.95 (15)Al1—O2—Mo1103.31 (12)
O22—Mo5—O1197.37 (15)Mo2—O2—Mo192.32 (10)
O21—Mo5—O1296.44 (15)Al1—O2—H9117.7
O22—Mo5—O12100.96 (15)Mo2—O2—H9119.0
O11—Mo5—O12150.02 (13)Mo1—O2—H9116.9
O21—Mo5—O594.55 (15)Al1—O3—Mo2104.49 (12)
O22—Mo5—O5158.37 (14)Al1—O3—Mo3103.59 (12)
O11—Mo5—O572.51 (11)Mo2—O3—Mo393.06 (10)
O12—Mo5—O581.98 (12)Al1—O3—H10121.1
O21—Mo5—O6159.79 (14)Mo2—O3—H10112.8
O22—Mo5—O692.62 (14)Mo3—O3—H10117.6
O11—Mo5—O683.22 (12)Al1—O4—Mo3104.35 (13)
O12—Mo5—O672.48 (11)Al1—O4—Mo4103.82 (13)
O5—Mo5—O667.61 (10)Mo3—O4—Mo491.65 (10)
O24—Mo6—O23107.00 (17)Al1—O4—H11119.0
O24—Mo6—O1297.20 (14)Mo3—O4—H11121.2
O23—Mo6—O12101.23 (15)Mo4—O4—H11112.5
O24—Mo6—O799.93 (14)Al1—O5—Mo5103.92 (12)
O23—Mo6—O795.46 (15)Al1—O5—Mo4104.23 (13)
O12—Mo6—O7151.39 (12)Mo5—O5—Mo491.93 (10)
O24—Mo6—O192.32 (14)Al1—O5—H12120.6
O23—Mo6—O1158.90 (14)Mo5—O5—H12116.0
O12—Mo6—O184.23 (12)Mo4—O5—H12115.8
O7—Mo6—O172.38 (11)Al1—O6—Mo5103.97 (13)
O24—Mo6—O6157.89 (14)Al1—O6—Mo6103.45 (12)
O23—Mo6—O694.42 (14)Mo5—O6—Mo691.97 (10)
O12—Mo6—O672.74 (11)Al1—O6—H13120.2
O7—Mo6—O683.02 (11)Mo5—O6—H13117.2
O1—Mo6—O667.51 (10)Mo6—O6—H13115.6
O26—Na1—O2898.76 (15)Mo1—O7—Mo6116.00 (15)
O26—Na1—O2792.75 (15)Mo1—O8—Mo2118.76 (15)
O28—Na1—O2785.13 (13)Mo2—O9—Mo3117.88 (15)
O26—Na1—O1478.03 (14)Mo4—O10—Mo3117.74 (15)
O28—Na1—O14176.70 (14)Mo4—O11—Mo5116.73 (15)
O27—Na1—O1495.76 (13)Mo6—O12—Mo5117.58 (15)
O26—Na1—O1585.00 (14)Mo1—O13—Na2129.4 (2)
O28—Na1—O1594.41 (13)Mo1—O14—Na1133.86 (17)
O27—Na1—O15177.61 (15)Mo2—O15—Na1136.74 (18)
O14—Na1—O1584.57 (12)Mo6—O24—Na2131.4 (2)
O26—Na1—Cl1166.36 (12)C1—O25—C3107.9 (4)
O28—Na1—Cl193.76 (10)Na1—O26—H14127.7
O27—Na1—Cl193.69 (11)Na1—O26—H15109.1
O14—Na1—Cl189.35 (10)H14—O26—H15120.0
O15—Na1—Cl188.69 (10)Na1—O27—H16113.0
O31i—Na2—O29116.0 (2)Na1—O27—H17122.8
O31i—Na2—O2482.05 (19)H16—O27—H1790.5
O29—Na2—O24155.2 (2)Na1—O28—H18112.3
O31i—Na2—O3085.3 (2)Na1—O28—H19118.8
O29—Na2—O3083.64 (19)H18—O28—H1986.1
O24—Na2—O30116.1 (2)Na2—O29—H20105.3
O31i—Na2—O13159.2 (2)Na2—O29—H21109.3
O29—Na2—O1381.59 (18)H20—O29—H2191.0
O24—Na2—O1377.99 (15)Na2—O30—H22109.5
O30—Na2—O13108.83 (19)Na2—O30—H23109.4
O31i—Na2—O3184.8 (3)H22—O30—H23107.5
O29—Na2—O3173.6 (2)Na2i—O31—Na295.2 (3)
O24—Na2—O3192.50 (18)Na2i—O31—H24106.6
O30—Na2—O31148.0 (2)Na2—O31—H24158.0
O13—Na2—O3190.10 (18)Na2i—O31—H25121.3
O31i—Na2—Na2i47.84 (16)Na2—O31—H2564.0
O29—Na2—Na2i93.1 (2)H24—O31—H25105.3
O24—Na2—Na2i87.08 (17)H26—O32—H27112.7
O30—Na2—Na2i125.6 (2)H28—O33—H29115.7
O13—Na2—Na2i124.5 (2)H31—O34—H30118.8
O31—Na2—Na2i36.99 (15)H32—O35—H33122.5
O31i—Na2—H20124.6
Symmetry codes: (i) x+2, y, z; (ii) x+2, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O8iii0.902.002.855 (5)158
N3—H3···O7iv0.901.862.750 (5)173
N5—H6···O9v0.901.922.821 (5)179
O1—H8···O310.851.792.631 (5)170
O3—H10···O320.851.872.715 (5)169
O4—H11···O27ii0.851.902.736 (4)170
O5—H12···O30i0.851.942.769 (5)164
O6—H13···O28ii0.851.912.737 (4)164
O26—H14···O19vi0.852.112.919 (5)159
O26—H15···O35vii0.852.132.898 (5)150
O27—H16···O34vii0.852.122.918 (5)155
O27—H17···O35viii0.851.952.784 (5)169
O28—H18···O17vii0.852.042.845 (5)158
O28—H19···O16vii0.851.982.790 (5)160
O29—H20···O20vi0.852.082.853 (5)152
O29—H21···O12i0.841.902.735 (5)168
O30—H22···O21vi0.852.112.890 (5)152
O30—H23···O33i0.851.932.640 (7)141
O31—H24···O320.862.092.889 (7)154
O31—H25···O290.862.082.885 (6)155
O32—H26···O330.852.002.632 (8)130
O32—H27···O23ix0.852.032.843 (6)160
O33—H29···O100.851.962.812 (6)176
O34—H30···O14iv0.852.142.991 (5)175
O34—H31···O11ix0.851.942.756 (5)161
O35—H32···O340.852.032.768 (5)145
O35—H33···O180.852.142.927 (5)155
Symmetry codes: (i) x+2, y, z; (ii) x+2, y, z+1; (iii) x, y+1, z; (iv) x1, y+1, z; (v) x+1, y+1, z+1; (vi) x, y1, z; (vii) x+1, y, z+1; (viii) x+1, y1, z; (ix) x1, y, z.

Experimental details

Crystal data
Chemical formulaNa3(C6H15N5O)2[Al(OH)6Mo6O18]2Cl·20H2O
Mr2796.54
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)10.1070 (6), 11.3869 (7), 17.2548 (10)
α, β, γ (°)81.698 (1), 75.314 (1), 77.057 (1)
V3)1864.03 (19)
Z1
Radiation typeMo Kα
µ (mm1)2.15
Crystal size (mm)0.31 × 0.25 × 0.22
Data collection
DiffractometerBruker SMART
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1997)
Tmin, Tmax0.528, 0.624
No. of measured, independent and
observed [I > 2σ(I)] reflections
9902, 6882, 6108
Rint0.021
(sin θ/λ)max1)0.608
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.092, 1.06
No. of reflections6882
No. of parameters503
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.36, 1.29

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O8i0.902.002.855 (5)157.5
N3—H3···O7ii0.901.862.750 (5)172.6
N5—H6···O9iii0.901.922.821 (5)179.3
O1—H8···O310.851.792.631 (5)169.9
O3—H10···O320.851.872.715 (5)169.4
O4—H11···O27iv0.851.902.736 (4)169.9
O5—H12···O30v0.851.942.769 (5)163.9
O6—H13···O28iv0.851.912.737 (4)163.7
O26—H14···O19vi0.852.112.919 (5)159.2
O26—H15···O35vii0.852.132.898 (5)150.1
O27—H16···O34vii0.852.122.918 (5)155.4
O27—H17···O35viii0.851.952.784 (5)168.5
O28—H18···O17vii0.852.042.845 (5)158.4
O28—H19···O16vii0.851.982.790 (5)160.0
O29—H20···O20vi0.852.082.853 (5)151.6
O29—H21···O12v0.841.902.735 (5)168.3
O30—H22···O21vi0.852.112.890 (5)152.4
O30—H23···O33v0.851.932.640 (7)140.5
O31—H24···O320.862.092.889 (7)153.8
O31—H25···O290.862.082.885 (6)154.8
O32—H26···O330.852.002.632 (8)130.2
O32—H27···O23ix0.852.032.843 (6)159.6
O33—H29···O100.851.962.812 (6)176.3
O34—H30···O14ii0.852.142.991 (5)175.4
O34—H31···O11ix0.851.942.756 (5)161.2
O35—H32···O340.852.032.768 (5)145.3
O35—H33···O180.852.142.927 (5)154.5
Symmetry codes: (i) x, y+1, z; (ii) x1, y+1, z; (iii) x+1, y+1, z+1; (iv) x+2, y, z+1; (v) x+2, y, z; (vi) x, y1, z; (vii) x+1, y, z+1; (viii) x+1, y1, z; (ix) x1, y, z.
 

Acknowledgements

This work was supported by the National Science Foundation of China (grant No. 20571014), the Program for New Century Excellent Talents in Universities (NCET-07–0169), and the Analysis and Testing Foundation of Northeast Normal University.

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Volume 64| Part 8| August 2008| Pages m1069-m1070
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