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

Wang, F.; Cao, R.-G.; Pan, Y.-B.; Liu, S.-X.

doi:10.1107/S1600536808022745

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

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

doi:10.1107/S1600536808022745

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

Feng Wang,^a Rui-Ge Cao,^a Yi-Bing Pan ^a and Shu-Xia Liu ^a ^*

^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 D_3d 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 ); 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

Crystal data

Na₃(C₆H₁₅N₅O)₂[Al(OH)₆Mo₆O₁₈]₂Cl·20H₂O
M_r = 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 ) T_min = 0.528, T_max = 0.624
9902 measured reflections
6882 independent reflections
6108 reflections with I > 2σ(I)
R_int = 0.021

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.092
S = 1.06
6882 reflections
503 parameters
H-atom parameters constrained
Δρ_max = 1.36 e Å⁻³
Δρ_min = −1.29 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	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⋯O27^iv	0.85	1.90	2.736 (4)	170
O5—H12⋯O30^v	0.85	1.94	2.769 (5)	164
O6—H13⋯O28^iv	0.85	1.91	2.737 (4)	164
O26—H14⋯O19^vi	0.85	2.11	2.919 (5)	159
O26—H15⋯O35^vii	0.85	2.13	2.898 (5)	150
O27—H16⋯O34^vii	0.85	2.12	2.918 (5)	155
O27—H17⋯O35^viii	0.85	1.95	2.784 (5)	169
O28—H18⋯O17^vii	0.85	2.04	2.845 (5)	158
O28—H19⋯O16^vii	0.85	1.98	2.790 (5)	160
O29—H20⋯O20^vi	0.85	2.08	2.853 (5)	152
O29—H21⋯O12^v	0.84	1.90	2.735 (5)	168
O30—H22⋯O21^vi	0.85	2.11	2.890 (5)	152
O30—H23⋯O33^v	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⋯O23^ix	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⋯O11^ix	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); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808022745/cv2425sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808022745/cv2425Isup2.hkl

checkCIF report

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 D₃_d 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.

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

	Fig. 1. Asymmetric unit of (I), showing 30% probability displacement ellipsoids. Solvent waters have been omitted.
	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·20H₂O	Z = 1
M_r = 2796.54	F(000) = 1364
Triclinic, P1	D_x = 2.491 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.1070 (6) Å	Cell parameters from 6444 reflections
b = 11.3869 (7) Å	θ = 1.8–25.6°
c = 17.2548 (10) Å	µ = 2.15 mm⁻¹
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 tube	6108 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
Detector resolution: 0 pixels mm^-1	θ_max = 25.6°, θ_min = 1.8°
ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 1997)	k = −12→13
T_min = 0.528, T_max = 0.624	l = −20→20
9902 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.034	H-atom parameters constrained
wR(F²) = 0.092	w = 1/[σ²(F_o²) + (0.0443P)² + 4.9534P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
6882 reflections	Δρ_max = 1.36 e Å⁻³
503 parameters	Δρ_min = −1.29 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0137 (3)

Crystal data top

Na₃(C₆H₁₅N₅O)₂[Al(OH)₆Mo₆O₁₈]₂Cl·20H₂O	γ = 77.057 (1)°
M_r = 2796.54	V = 1864.03 (19) Å³
Triclinic, P1	Z = 1
a = 10.1070 (6) Å	Mo Kα radiation
b = 11.3869 (7) Å	µ = 2.15 mm⁻¹
c = 17.2548 (10) Å	T = 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)
T_min = 0.528, T_max = 0.624	R_int = 0.021
9902 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.092	H-atom parameters constrained
S = 1.06	Δρ_max = 1.36 e Å⁻³
6882 reflections	Δρ_min = −1.29 e Å⁻³
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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Al1	0.90661 (12)	0.18649 (10)	0.25816 (7)	0.0126 (3)
Mo1	0.96744 (4)	−0.11386 (3)	0.27426 (2)	0.01484 (11)
Mo2	0.66462 (4)	0.04088 (3)	0.37024 (2)	0.01508 (11)
Mo3	0.60225 (4)	0.34140 (3)	0.34933 (2)	0.01652 (11)
Mo4	0.84344 (4)	0.48692 (3)	0.23681 (2)	0.01781 (11)
Mo5	1.14688 (4)	0.33344 (3)	0.14622 (2)	0.01812 (11)
Mo6	1.20687 (4)	0.03452 (3)	0.16141 (2)	0.01669 (11)
Na1	0.8711 (2)	−0.19733 (17)	0.50224 (11)	0.0280 (4)
Na2	1.0528 (4)	−0.1445 (4)	0.0459 (2)	0.0327 (9)	0.50
Cl1	1.0000	0.0000	0.5000	0.0242 (3)
C1	0.4802 (7)	0.6826 (7)	0.0390 (4)	0.0534 (17)
H1A	0.4184	0.7562	0.0244	0.064*
H1B	0.5480	0.6580	−0.0096	0.064*
C2	0.5541 (6)	0.7090 (7)	0.0956 (3)	0.0472 (16)
H2A	0.5920	0.7812	0.0744	0.057*
H2B	0.6315	0.6425	0.1002	0.057*
C3	0.2954 (7)	0.6335 (6)	0.1381 (4)	0.0460 (15)
H3A	0.2348	0.5752	0.1573	0.055*
H3B	0.2391	0.7097	0.1222	0.055*
C4	0.3559 (6)	0.6502 (6)	0.2029 (3)	0.0402 (14)
H4A	0.3980	0.5716	0.2250	0.048*
H4B	0.2822	0.6871	0.2453	0.048*
C5	0.4993 (5)	0.7834 (4)	0.2270 (3)	0.0223 (9)
C6	0.4182 (5)	0.8042 (4)	0.3722 (3)	0.0197 (9)
N1	0.4633 (4)	0.7272 (4)	0.1760 (2)	0.0274 (9)
N2	0.6204 (4)	0.8142 (4)	0.2137 (2)	0.0284 (9)
H1	0.6948	0.7823	0.1765	0.034*
H2	0.6464	0.8679	0.2374	0.034*
N3	0.3989 (4)	0.8116 (3)	0.2962 (2)	0.0214 (8)
H3	0.3159	0.8429	0.2840	0.026*
N4	0.5371 (4)	0.7469 (4)	0.3894 (2)	0.0287 (9)
H4	0.6087	0.7685	0.3512	0.034*
H5	0.5516	0.7488	0.4385	0.034*
N5	0.3136 (4)	0.8525 (4)	0.4272 (2)	0.0285 (9)
H6	0.3317	0.8378	0.4765	0.034*
H7	0.2377	0.9106	0.4244	0.034*
O1	0.9705 (3)	0.0596 (3)	0.19008 (17)	0.0151 (6)
H8	0.9421	0.0643	0.1472	0.018*
O2	0.8941 (3)	0.0588 (2)	0.34240 (17)	0.0137 (6)
H9	0.9311	0.0607	0.3812	0.016*
O3	0.7143 (3)	0.1875 (2)	0.26901 (17)	0.0144 (6)
H10	0.6828	0.1832	0.2285	0.017*
O4	0.8404 (3)	0.3137 (3)	0.32567 (17)	0.0151 (6)
H11	0.8805	0.3146	0.3633	0.018*
O5	0.9193 (3)	0.3124 (3)	0.17301 (17)	0.0156 (6)
H12	0.8869	0.3112	0.1323	0.019*
O6	1.0986 (3)	0.1831 (3)	0.24666 (17)	0.0146 (6)
H13	1.1312	0.1796	0.2880	0.018*
O7	1.1509 (3)	−0.0732 (3)	0.25770 (18)	0.0186 (6)
O8	0.7693 (3)	−0.0652 (3)	0.28711 (18)	0.0181 (6)
O9	0.6296 (3)	0.1915 (3)	0.41825 (17)	0.0193 (6)
O10	0.6638 (3)	0.4432 (3)	0.25302 (19)	0.0210 (6)
O11	1.0414 (3)	0.4388 (3)	0.22920 (19)	0.0211 (7)
O12	1.1770 (3)	0.1847 (3)	0.09572 (18)	0.0211 (7)
O13	0.9982 (3)	−0.2022 (3)	0.1980 (2)	0.0272 (7)
O14	0.9798 (3)	−0.2103 (3)	0.35929 (19)	0.0252 (7)
O15	0.6820 (3)	−0.0552 (3)	0.45441 (19)	0.0254 (7)
O16	0.5052 (3)	0.0407 (3)	0.3533 (2)	0.0260 (7)
O17	0.4406 (3)	0.3449 (3)	0.3343 (2)	0.0291 (8)
O18	0.5761 (4)	0.4378 (3)	0.4208 (2)	0.0309 (8)
O19	0.8044 (4)	0.5837 (3)	0.3101 (2)	0.0292 (8)
O20	0.8410 (4)	0.5760 (3)	0.1485 (2)	0.0333 (8)
O21	1.1373 (4)	0.4294 (3)	0.0617 (2)	0.0332 (8)
O22	1.3079 (4)	0.3260 (3)	0.1628 (2)	0.0328 (8)
O23	1.3700 (3)	0.0303 (3)	0.1751 (2)	0.0293 (8)
O24	1.2263 (4)	−0.0587 (3)	0.08914 (19)	0.0282 (7)
O25	0.4015 (4)	0.5917 (4)	0.0695 (2)	0.0443 (10)
O26	0.7727 (4)	−0.3471 (3)	0.4712 (2)	0.0412 (9)
H14	0.7606	−0.3567	0.4257	0.049*
H15	0.7767	−0.4063	0.5072	0.049*
O27	1.0513 (4)	−0.3434 (3)	0.5500 (2)	0.0320 (8)
H16	1.0269	−0.4106	0.5687	0.038*
H17	1.1231	−0.3797	0.5185	0.038*
O28	0.7555 (3)	−0.1911 (3)	0.6411 (2)	0.0287 (7)
H18	0.7086	−0.2468	0.6578	0.034*
H19	0.6784	−0.1420	0.6539	0.034*
O29	0.8521 (5)	−0.1943 (4)	0.0585 (2)	0.0469 (10)
H20	0.8663	−0.2705	0.0695	0.056*
H21	0.8414	−0.2015	0.0126	0.056*
O30	1.1468 (5)	−0.3344 (4)	−0.0247 (3)	0.0468 (10)
H22	1.1144	−0.3929	0.0046	0.056*
H23	1.2350	−0.3517	−0.0313	0.056*
O31	0.8656 (6)	0.0541 (4)	0.0661 (3)	0.0680 (16)
H24	0.7963	0.1050	0.0906	0.082*
H25	0.8343	−0.0111	0.0688	0.082*
O32	0.5896 (5)	0.1589 (5)	0.1528 (3)	0.0566 (12)
H26	0.5532	0.2243	0.1292	0.068*
H27	0.5356	0.1083	0.1671	0.068*
O33	0.5983 (6)	0.3897 (5)	0.1147 (3)	0.0774 (16)
H28	0.5206	0.4255	0.1042	0.093*
H29	0.6148	0.4084	0.1568	0.093*
O34	0.1012 (4)	0.5252 (3)	0.3550 (2)	0.0393 (9)
H31	0.1008	0.4880	0.3158	0.047*
H30	0.0624	0.5995	0.3560	0.047*
O35	0.2881 (4)	0.5691 (4)	0.4350 (2)	0.0400 (9)
H32	0.2634	0.5508	0.3954	0.048*
H33	0.3707	0.5461	0.4418	0.048*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Al1	0.0114 (6)	0.0125 (6)	0.0131 (6)	0.0000 (5)	−0.0035 (5)	−0.0004 (5)
Mo1	0.01445 (19)	0.01288 (19)	0.01581 (19)	−0.00011 (14)	−0.00296 (14)	−0.00181 (14)
Mo2	0.01243 (19)	0.01500 (19)	0.01653 (19)	−0.00142 (14)	−0.00272 (14)	−0.00036 (14)
Mo3	0.0136 (2)	0.01542 (19)	0.0182 (2)	0.00193 (14)	−0.00290 (14)	−0.00296 (14)
Mo4	0.0185 (2)	0.01218 (19)	0.0213 (2)	0.00010 (14)	−0.00548 (15)	0.00012 (14)
Mo5	0.0164 (2)	0.0168 (2)	0.0192 (2)	−0.00425 (14)	−0.00140 (15)	0.00134 (15)
Mo6	0.0132 (2)	0.01648 (19)	0.0180 (2)	0.00022 (14)	−0.00215 (14)	−0.00154 (14)
Na1	0.0300 (10)	0.0288 (10)	0.0256 (10)	−0.0043 (8)	−0.0102 (8)	0.0007 (8)
Na2	0.034 (2)	0.040 (2)	0.026 (2)	−0.0118 (18)	−0.0036 (17)	−0.0084 (17)
Cl1	0.0264 (8)	0.0258 (8)	0.0232 (8)	−0.0042 (6)	−0.0117 (6)	−0.0015 (6)
C1	0.053 (4)	0.076 (5)	0.033 (3)	−0.020 (3)	0.001 (3)	−0.018 (3)
C2	0.034 (3)	0.086 (5)	0.026 (3)	−0.025 (3)	0.010 (2)	−0.025 (3)
C3	0.043 (3)	0.047 (4)	0.053 (4)	−0.018 (3)	−0.006 (3)	−0.014 (3)
C4	0.034 (3)	0.053 (4)	0.036 (3)	−0.022 (3)	0.005 (2)	−0.016 (3)
C5	0.021 (2)	0.026 (2)	0.019 (2)	0.0008 (18)	−0.0077 (18)	−0.0025 (18)
C6	0.025 (2)	0.015 (2)	0.020 (2)	−0.0021 (17)	−0.0081 (18)	−0.0012 (17)
N1	0.025 (2)	0.041 (2)	0.019 (2)	−0.0114 (18)	−0.0028 (16)	−0.0093 (18)
N2	0.022 (2)	0.038 (2)	0.027 (2)	−0.0077 (18)	−0.0031 (17)	−0.0125 (18)
N3	0.0178 (19)	0.029 (2)	0.0152 (18)	0.0043 (15)	−0.0063 (15)	−0.0052 (15)
N4	0.027 (2)	0.035 (2)	0.025 (2)	−0.0001 (18)	−0.0141 (17)	0.0013 (18)
N5	0.030 (2)	0.031 (2)	0.022 (2)	0.0012 (18)	−0.0032 (17)	−0.0094 (17)
O1	0.0162 (15)	0.0164 (14)	0.0132 (14)	−0.0020 (11)	−0.0045 (11)	−0.0027 (11)
O2	0.0129 (14)	0.0144 (14)	0.0142 (14)	−0.0005 (11)	−0.0067 (11)	0.0007 (11)
O3	0.0119 (14)	0.0165 (14)	0.0155 (14)	−0.0002 (11)	−0.0064 (11)	−0.0018 (11)
O4	0.0145 (15)	0.0146 (14)	0.0179 (14)	−0.0011 (11)	−0.0074 (11)	−0.0033 (11)
O5	0.0167 (15)	0.0171 (14)	0.0133 (14)	−0.0006 (11)	−0.0080 (11)	0.0017 (11)
O6	0.0115 (14)	0.0164 (14)	0.0166 (14)	−0.0014 (11)	−0.0051 (11)	−0.0025 (11)
O7	0.0129 (15)	0.0193 (15)	0.0225 (16)	−0.0011 (12)	−0.0055 (12)	0.0011 (12)
O8	0.0141 (15)	0.0182 (15)	0.0235 (16)	−0.0022 (12)	−0.0059 (12)	−0.0057 (12)
O9	0.0199 (16)	0.0187 (15)	0.0158 (15)	0.0000 (12)	−0.0006 (12)	−0.0029 (12)
O10	0.0157 (15)	0.0183 (15)	0.0269 (17)	0.0015 (12)	−0.0079 (13)	0.0026 (13)
O11	0.0159 (15)	0.0197 (15)	0.0281 (17)	−0.0025 (12)	−0.0059 (13)	−0.0041 (13)
O12	0.0244 (17)	0.0192 (15)	0.0160 (15)	−0.0022 (13)	−0.0007 (12)	0.0000 (12)
O13	0.0271 (18)	0.0250 (17)	0.0298 (18)	0.0005 (14)	−0.0063 (14)	−0.0129 (14)
O14	0.0274 (18)	0.0184 (16)	0.0260 (17)	−0.0006 (13)	−0.0060 (14)	0.0038 (13)
O15	0.0261 (18)	0.0222 (16)	0.0238 (17)	−0.0019 (13)	−0.0040 (14)	0.0043 (13)
O16	0.0163 (16)	0.0260 (17)	0.0361 (19)	−0.0034 (13)	−0.0073 (14)	−0.0027 (14)
O17	0.0187 (17)	0.0305 (18)	0.0363 (19)	−0.0011 (14)	−0.0097 (14)	0.0026 (15)
O18	0.033 (2)	0.0261 (18)	0.0303 (19)	0.0022 (15)	−0.0020 (15)	−0.0124 (15)
O19	0.0308 (19)	0.0184 (16)	0.039 (2)	−0.0014 (14)	−0.0072 (16)	−0.0097 (14)
O20	0.034 (2)	0.0271 (18)	0.035 (2)	−0.0041 (15)	−0.0101 (16)	0.0115 (15)
O21	0.041 (2)	0.0246 (18)	0.0289 (18)	−0.0069 (15)	−0.0048 (16)	0.0087 (15)
O22	0.0211 (18)	0.0329 (19)	0.046 (2)	−0.0099 (15)	−0.0063 (16)	−0.0031 (17)
O23	0.0155 (16)	0.0285 (18)	0.043 (2)	−0.0030 (13)	−0.0106 (15)	0.0038 (15)
O24	0.035 (2)	0.0224 (17)	0.0234 (17)	−0.0013 (14)	−0.0014 (14)	−0.0051 (14)
O25	0.049 (3)	0.049 (2)	0.037 (2)	−0.015 (2)	0.0010 (18)	−0.0233 (19)
O26	0.056 (3)	0.035 (2)	0.037 (2)	−0.0177 (19)	−0.0168 (19)	0.0055 (17)
O27	0.0309 (19)	0.0327 (19)	0.0318 (19)	0.0024 (15)	−0.0117 (15)	−0.0068 (15)
O28	0.0192 (17)	0.038 (2)	0.0297 (18)	−0.0064 (14)	−0.0061 (14)	−0.0035 (15)
O29	0.061 (3)	0.047 (2)	0.031 (2)	0.003 (2)	−0.0201 (19)	−0.0056 (18)
O30	0.057 (3)	0.035 (2)	0.053 (3)	−0.0123 (19)	−0.025 (2)	0.0108 (19)
O31	0.107 (4)	0.041 (2)	0.076 (3)	0.010 (3)	−0.070 (3)	−0.020 (2)
O32	0.049 (3)	0.078 (3)	0.050 (3)	−0.016 (2)	−0.024 (2)	0.002 (2)
O33	0.068 (4)	0.094 (4)	0.075 (4)	−0.002 (3)	−0.029 (3)	−0.021 (3)
O34	0.038 (2)	0.036 (2)	0.048 (2)	−0.0004 (17)	−0.0182 (18)	−0.0154 (18)
O35	0.029 (2)	0.044 (2)	0.048 (2)	0.0031 (17)	−0.0107 (17)	−0.0188 (19)

Geometric parameters (Å, º) top

Al1—O4	1.887 (3)	Na2—H25	2.3601
Al1—O1	1.890 (3)	Cl1—Na1ⁱⁱ	2.8298 (19)
Al1—O6	1.892 (3)	C1—O25	1.408 (7)
Al1—O5	1.900 (3)	C1—C2	1.468 (8)
Al1—O3	1.902 (3)	C1—H1A	0.9700
Al1—O2	1.903 (3)	C1—H1B	0.9700
Mo1—O13	1.696 (3)	C2—N1	1.471 (6)
Mo1—O14	1.715 (3)	C2—H2A	0.9700
Mo1—O8	1.918 (3)	C2—H2B	0.9700
Mo1—O7	1.953 (3)	C3—O25	1.439 (7)
Mo1—O1	2.277 (3)	C3—C4	1.455 (8)
Mo1—O2	2.317 (3)	C3—H3A	0.9700
Mo2—O15	1.709 (3)	C3—H3B	0.9700
Mo2—O16	1.709 (3)	C4—N1	1.488 (6)
Mo2—O9	1.934 (3)	C4—H4A	0.9700
Mo2—O8	1.948 (3)	C4—H4B	0.9700
Mo2—O3	2.276 (3)	C5—N2	1.304 (6)
Mo2—O2	2.296 (3)	C5—N1	1.321 (6)
Mo3—O18	1.700 (3)	C5—N3	1.383 (6)
Mo3—O17	1.709 (3)	C6—N5	1.304 (6)
Mo3—O10	1.932 (3)	C6—N4	1.316 (6)
Mo3—O9	1.943 (3)	C6—N3	1.361 (5)
Mo3—O4	2.293 (3)	N2—H1	0.9000
Mo3—O3	2.300 (3)	N2—H2	0.8998
Mo4—O20	1.706 (3)	N3—H3	0.8999
Mo4—O19	1.710 (3)	N4—H4	0.9000
Mo4—O11	1.928 (3)	N4—H5	0.9000
Mo4—O10	1.931 (3)	N5—H6	0.8999
Mo4—O5	2.296 (3)	N5—H7	0.8999
Mo4—O4	2.318 (3)	O1—H8	0.8500
Mo5—O21	1.701 (3)	O2—H9	0.8500
Mo5—O22	1.704 (3)	O3—H10	0.8501
Mo5—O11	1.943 (3)	O4—H11	0.8499
Mo5—O12	1.945 (3)	O5—H12	0.8500
Mo5—O5	2.288 (3)	O6—H13	0.8499
Mo5—O6	2.293 (3)	O26—H14	0.8499
Mo6—O24	1.698 (3)	O26—H15	0.8501
Mo6—O23	1.713 (3)	O27—H16	0.8500
Mo6—O12	1.919 (3)	O27—H17	0.8500
Mo6—O7	1.957 (3)	O28—H18	0.8500
Mo6—O1	2.274 (3)	O28—H19	0.8500
Mo6—O6	2.301 (3)	O29—H20	0.8486
Na1—O26	2.340 (4)	O29—H21	0.8441
Na1—O28	2.388 (4)	O30—H22	0.8500
Na1—O27	2.402 (4)	O30—H23	0.8501
Na1—O14	2.444 (4)	O31—Na2ⁱ	2.116 (7)
Na1—O15	2.446 (4)	O31—H24	0.8624
Na1—Cl1	2.8298 (19)	O31—H25	0.8617
Na2—O31ⁱ	2.116 (7)	O32—H26	0.8501
Na2—O29	2.177 (6)	O32—H27	0.8500
Na2—O24	2.496 (5)	O33—H28	0.8500
Na2—O30	2.513 (6)	O33—H29	0.8500
Na2—O13	2.559 (5)	O34—H31	0.8499
Na2—O31	2.607 (6)	O34—H30	0.8500
Na2—Na2ⁱ	3.502 (9)	O35—H32	0.8500
Na2—H20	2.5362	O35—H33	0.8500
Na2—H21	2.5822

O4—Al1—O1	179.20 (13)	O29—Na2—H20	18.8
O4—Al1—O6	96.29 (13)	O24—Na2—H20	153.3
O1—Al1—O6	84.45 (13)	O30—Na2—H20	69.5
O4—Al1—O5	84.77 (13)	O13—Na2—H20	75.6
O1—Al1—O5	94.99 (13)	O31—Na2—H20	91.6
O6—Al1—O5	84.48 (13)	Na2ⁱ—Na2—H20	111.3
O4—Al1—O3	84.60 (13)	O31ⁱ—Na2—H21	99.6
O1—Al1—O3	94.66 (13)	O29—Na2—H21	18.0
O6—Al1—O3	179.09 (13)	O24—Na2—H21	169.8
O5—Al1—O3	95.81 (13)	O30—Na2—H21	74.0
O4—Al1—O2	96.00 (13)	O13—Na2—H21	99.1
O1—Al1—O2	84.23 (13)	O31—Na2—H21	77.7
O6—Al1—O2	95.63 (13)	Na2ⁱ—Na2—H21	86.7
O5—Al1—O2	179.20 (13)	H20—Na2—H21	27.3
O3—Al1—O2	84.06 (13)	O31ⁱ—Na2—H25	95.2
O13—Mo1—O14	106.44 (16)	O29—Na2—H25	54.5
O13—Mo1—O8	97.66 (14)	O24—Na2—H25	109.9
O14—Mo1—O8	101.93 (14)	O30—Na2—H25	133.5
O13—Mo1—O7	100.20 (15)	O13—Na2—H25	86.1
O14—Mo1—O7	95.41 (14)	O31—Na2—H25	19.2
O8—Mo1—O7	150.41 (12)	Na2ⁱ—Na2—H25	49.6
O13—Mo1—O1	93.31 (14)	H20—Na2—H25	72.4
O14—Mo1—O1	158.53 (13)	H21—Na2—H25	60.0
O8—Mo1—O1	83.25 (12)	Na1—Cl1—Na1ⁱⁱ	180.00 (4)
O7—Mo1—O1	72.38 (11)	O25—C1—C2	114.0 (5)
O13—Mo1—O2	158.48 (14)	O25—C1—H1A	108.8
O14—Mo1—O2	94.31 (13)	C2—C1—H1A	108.8
O8—Mo1—O2	71.94 (11)	O25—C1—H1B	108.8
O7—Mo1—O2	83.10 (11)	C2—C1—H1B	108.8
O1—Mo1—O2	67.22 (10)	H1A—C1—H1B	107.7
O15—Mo2—O16	107.36 (16)	C1—C2—N1	112.6 (5)
O15—Mo2—O9	97.76 (14)	C1—C2—H2A	109.1
O16—Mo2—O9	101.84 (14)	N1—C2—H2A	109.1
O15—Mo2—O8	100.08 (14)	C1—C2—H2B	109.1
O16—Mo2—O8	94.96 (14)	N1—C2—H2B	109.1
O9—Mo2—O8	150.56 (12)	H2A—C2—H2B	107.8
O15—Mo2—O3	157.71 (14)	O25—C3—C4	111.5 (5)
O16—Mo2—O3	94.40 (13)	O25—C3—H3A	109.3
O9—Mo2—O3	72.44 (11)	C4—C3—H3A	109.3
O8—Mo2—O3	82.39 (12)	O25—C3—H3B	109.3
O15—Mo2—O2	91.79 (13)	C4—C3—H3B	109.3
O16—Mo2—O2	158.68 (13)	H3A—C3—H3B	108.0
O9—Mo2—O2	84.31 (12)	C3—C4—N1	112.9 (5)
O8—Mo2—O2	71.95 (11)	C3—C4—H4A	109.0
O3—Mo2—O2	67.73 (10)	N1—C4—H4A	109.0
O18—Mo3—O17	105.49 (17)	C3—C4—H4B	109.0
O18—Mo3—O10	100.65 (15)	N1—C4—H4B	109.0
O17—Mo3—O10	96.30 (15)	H4A—C4—H4B	107.8
O18—Mo3—O9	97.33 (15)	N2—C5—N1	123.4 (4)
O17—Mo3—O9	101.13 (15)	N2—C5—N3	120.5 (4)
O10—Mo3—O9	150.56 (12)	N1—C5—N3	116.0 (4)
O18—Mo3—O4	93.17 (14)	N5—C6—N4	121.7 (4)
O17—Mo3—O4	159.96 (14)	N5—C6—N3	117.6 (4)
O10—Mo3—O4	72.67 (11)	N4—C6—N3	120.7 (4)
O9—Mo3—O4	83.28 (12)	C5—N1—C2	120.3 (4)
O18—Mo3—O3	158.31 (14)	C5—N1—C4	122.1 (4)
O17—Mo3—O3	95.15 (14)	C2—N1—C4	115.3 (4)
O10—Mo3—O3	83.29 (12)	C5—N2—H1	122.8
O9—Mo3—O3	71.74 (11)	C5—N2—H2	129.3
O4—Mo3—O3	67.44 (10)	H1—N2—H2	107.9
O20—Mo4—O19	106.06 (17)	C6—N3—C5	127.3 (4)
O20—Mo4—O11	100.82 (16)	C6—N3—H3	122.6
O19—Mo4—O11	98.43 (15)	C5—N3—H3	109.9
O20—Mo4—O10	97.79 (15)	C6—N4—H4	109.8
O19—Mo4—O10	99.41 (15)	C6—N4—H5	119.8
O11—Mo4—O10	149.46 (13)	H4—N4—H5	109.9
O20—Mo4—O5	92.72 (14)	C6—N5—H6	112.3
O19—Mo4—O5	160.56 (14)	C6—N5—H7	132.5
O11—Mo4—O5	72.58 (11)	H6—N5—H7	113.4
O10—Mo4—O5	82.59 (12)	Al1—O1—Mo6	104.56 (13)
O20—Mo4—O4	158.16 (14)	Al1—O1—Mo1	105.23 (13)
O19—Mo4—O4	94.86 (14)	Mo6—O1—Mo1	93.54 (11)
O11—Mo4—O4	81.85 (12)	Al1—O1—H8	120.5
O10—Mo4—O4	72.12 (11)	Mo6—O1—H8	110.4
O5—Mo4—O4	67.18 (10)	Mo1—O1—H8	118.5
O21—Mo5—O22	106.29 (18)	Al1—O2—Mo2	103.71 (12)
O21—Mo5—O11	100.95 (15)	Al1—O2—Mo1	103.31 (12)
O22—Mo5—O11	97.37 (15)	Mo2—O2—Mo1	92.32 (10)
O21—Mo5—O12	96.44 (15)	Al1—O2—H9	117.7
O22—Mo5—O12	100.96 (15)	Mo2—O2—H9	119.0
O11—Mo5—O12	150.02 (13)	Mo1—O2—H9	116.9
O21—Mo5—O5	94.55 (15)	Al1—O3—Mo2	104.49 (12)
O22—Mo5—O5	158.37 (14)	Al1—O3—Mo3	103.59 (12)
O11—Mo5—O5	72.51 (11)	Mo2—O3—Mo3	93.06 (10)
O12—Mo5—O5	81.98 (12)	Al1—O3—H10	121.1
O21—Mo5—O6	159.79 (14)	Mo2—O3—H10	112.8
O22—Mo5—O6	92.62 (14)	Mo3—O3—H10	117.6
O11—Mo5—O6	83.22 (12)	Al1—O4—Mo3	104.35 (13)
O12—Mo5—O6	72.48 (11)	Al1—O4—Mo4	103.82 (13)
O5—Mo5—O6	67.61 (10)	Mo3—O4—Mo4	91.65 (10)
O24—Mo6—O23	107.00 (17)	Al1—O4—H11	119.0
O24—Mo6—O12	97.20 (14)	Mo3—O4—H11	121.2
O23—Mo6—O12	101.23 (15)	Mo4—O4—H11	112.5
O24—Mo6—O7	99.93 (14)	Al1—O5—Mo5	103.92 (12)
O23—Mo6—O7	95.46 (15)	Al1—O5—Mo4	104.23 (13)
O12—Mo6—O7	151.39 (12)	Mo5—O5—Mo4	91.93 (10)
O24—Mo6—O1	92.32 (14)	Al1—O5—H12	120.6
O23—Mo6—O1	158.90 (14)	Mo5—O5—H12	116.0
O12—Mo6—O1	84.23 (12)	Mo4—O5—H12	115.8
O7—Mo6—O1	72.38 (11)	Al1—O6—Mo5	103.97 (13)
O24—Mo6—O6	157.89 (14)	Al1—O6—Mo6	103.45 (12)
O23—Mo6—O6	94.42 (14)	Mo5—O6—Mo6	91.97 (10)
O12—Mo6—O6	72.74 (11)	Al1—O6—H13	120.2
O7—Mo6—O6	83.02 (11)	Mo5—O6—H13	117.2
O1—Mo6—O6	67.51 (10)	Mo6—O6—H13	115.6
O26—Na1—O28	98.76 (15)	Mo1—O7—Mo6	116.00 (15)
O26—Na1—O27	92.75 (15)	Mo1—O8—Mo2	118.76 (15)
O28—Na1—O27	85.13 (13)	Mo2—O9—Mo3	117.88 (15)
O26—Na1—O14	78.03 (14)	Mo4—O10—Mo3	117.74 (15)
O28—Na1—O14	176.70 (14)	Mo4—O11—Mo5	116.73 (15)
O27—Na1—O14	95.76 (13)	Mo6—O12—Mo5	117.58 (15)
O26—Na1—O15	85.00 (14)	Mo1—O13—Na2	129.4 (2)
O28—Na1—O15	94.41 (13)	Mo1—O14—Na1	133.86 (17)
O27—Na1—O15	177.61 (15)	Mo2—O15—Na1	136.74 (18)
O14—Na1—O15	84.57 (12)	Mo6—O24—Na2	131.4 (2)
O26—Na1—Cl1	166.36 (12)	C1—O25—C3	107.9 (4)
O28—Na1—Cl1	93.76 (10)	Na1—O26—H14	127.7
O27—Na1—Cl1	93.69 (11)	Na1—O26—H15	109.1
O14—Na1—Cl1	89.35 (10)	H14—O26—H15	120.0
O15—Na1—Cl1	88.69 (10)	Na1—O27—H16	113.0
O31ⁱ—Na2—O29	116.0 (2)	Na1—O27—H17	122.8
O31ⁱ—Na2—O24	82.05 (19)	H16—O27—H17	90.5
O29—Na2—O24	155.2 (2)	Na1—O28—H18	112.3
O31ⁱ—Na2—O30	85.3 (2)	Na1—O28—H19	118.8
O29—Na2—O30	83.64 (19)	H18—O28—H19	86.1
O24—Na2—O30	116.1 (2)	Na2—O29—H20	105.3
O31ⁱ—Na2—O13	159.2 (2)	Na2—O29—H21	109.3
O29—Na2—O13	81.59 (18)	H20—O29—H21	91.0
O24—Na2—O13	77.99 (15)	Na2—O30—H22	109.5
O30—Na2—O13	108.83 (19)	Na2—O30—H23	109.4
O31ⁱ—Na2—O31	84.8 (3)	H22—O30—H23	107.5
O29—Na2—O31	73.6 (2)	Na2ⁱ—O31—Na2	95.2 (3)
O24—Na2—O31	92.50 (18)	Na2ⁱ—O31—H24	106.6
O30—Na2—O31	148.0 (2)	Na2—O31—H24	158.0
O13—Na2—O31	90.10 (18)	Na2ⁱ—O31—H25	121.3
O31ⁱ—Na2—Na2ⁱ	47.84 (16)	Na2—O31—H25	64.0
O29—Na2—Na2ⁱ	93.1 (2)	H24—O31—H25	105.3
O24—Na2—Na2ⁱ	87.08 (17)	H26—O32—H27	112.7
O30—Na2—Na2ⁱ	125.6 (2)	H28—O33—H29	115.7
O13—Na2—Na2ⁱ	124.5 (2)	H31—O34—H30	118.8
O31—Na2—Na2ⁱ	36.99 (15)	H32—O35—H33	122.5
O31ⁱ—Na2—H20	124.6

Symmetry codes: (i) −x+2, −y, −z; (ii) −x+2, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···O8ⁱⁱⁱ	0.90	2.00	2.855 (5)	158
N3—H3···O7^iv	0.90	1.86	2.750 (5)	173
N5—H6···O9^v	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···O27ⁱⁱ	0.85	1.90	2.736 (4)	170
O5—H12···O30ⁱ	0.85	1.94	2.769 (5)	164
O6—H13···O28ⁱⁱ	0.85	1.91	2.737 (4)	164
O26—H14···O19^vi	0.85	2.11	2.919 (5)	159
O26—H15···O35^vii	0.85	2.13	2.898 (5)	150
O27—H16···O34^vii	0.85	2.12	2.918 (5)	155
O27—H17···O35^viii	0.85	1.95	2.784 (5)	169
O28—H18···O17^vii	0.85	2.04	2.845 (5)	158
O28—H19···O16^vii	0.85	1.98	2.790 (5)	160
O29—H20···O20^vi	0.85	2.08	2.853 (5)	152
O29—H21···O12ⁱ	0.84	1.90	2.735 (5)	168
O30—H22···O21^vi	0.85	2.11	2.890 (5)	152
O30—H23···O33ⁱ	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···O23^ix	0.85	2.03	2.843 (6)	160
O33—H29···O10	0.85	1.96	2.812 (6)	176
O34—H30···O14^iv	0.85	2.14	2.991 (5)	175
O34—H31···O11^ix	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+2, −y, −z; (ii) −x+2, −y, −z+1; (iii) x, y+1, z; (iv) x−1, y+1, z; (v) −x+1, −y+1, −z+1; (vi) x, y−1, z; (vii) −x+1, −y, −z+1; (viii) x+1, y−1, z; (ix) x−1, y, z.

Experimental details

Crystal data
Chemical formula	Na₃(C₆H₁₅N₅O)₂[Al(OH)₆Mo₆O₁₈]₂Cl·20H₂O
M_r	2796.54
Crystal system, space group	Triclinic, 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)
V (Å³)	1864.03 (19)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.15
Crystal size (mm)	0.31 × 0.25 × 0.22

Data collection
Diffractometer	Bruker SMART diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1997)
T_min, T_max	0.528, 0.624
No. of measured, independent and observed [I > 2σ(I)] reflections	9902, 6882, 6108
R_int	0.021
(sin θ/λ)_max (Å⁻¹)	0.608

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.092, 1.06
No. of reflections	6882
No. of parameters	503
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	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···A	D—H	H···A	D···A	D—H···A
N2—H2···O8ⁱ	0.90	2.00	2.855 (5)	157.5
N3—H3···O7ⁱⁱ	0.90	1.86	2.750 (5)	172.6
N5—H6···O9ⁱⁱⁱ	0.90	1.92	2.821 (5)	179.3
O1—H8···O31	0.85	1.79	2.631 (5)	169.9
O3—H10···O32	0.85	1.87	2.715 (5)	169.4
O4—H11···O27^iv	0.85	1.90	2.736 (4)	169.9
O5—H12···O30^v	0.85	1.94	2.769 (5)	163.9
O6—H13···O28^iv	0.85	1.91	2.737 (4)	163.7
O26—H14···O19^vi	0.85	2.11	2.919 (5)	159.2
O26—H15···O35^vii	0.85	2.13	2.898 (5)	150.1
O27—H16···O34^vii	0.85	2.12	2.918 (5)	155.4
O27—H17···O35^viii	0.85	1.95	2.784 (5)	168.5
O28—H18···O17^vii	0.85	2.04	2.845 (5)	158.4
O28—H19···O16^vii	0.85	1.98	2.790 (5)	160.0
O29—H20···O20^vi	0.85	2.08	2.853 (5)	151.6
O29—H21···O12^v	0.84	1.90	2.735 (5)	168.3
O30—H22···O21^vi	0.85	2.11	2.890 (5)	152.4
O30—H23···O33^v	0.85	1.93	2.640 (7)	140.5
O31—H24···O32	0.86	2.09	2.889 (7)	153.8
O31—H25···O29	0.86	2.08	2.885 (6)	154.8
O32—H26···O33	0.85	2.00	2.632 (8)	130.2
O32—H27···O23^ix	0.85	2.03	2.843 (6)	159.6
O33—H29···O10	0.85	1.96	2.812 (6)	176.3
O34—H30···O14ⁱⁱ	0.85	2.14	2.991 (5)	175.4
O34—H31···O11^ix	0.85	1.94	2.756 (5)	161.2
O35—H32···O34	0.85	2.03	2.768 (5)	145.3
O35—H33···O18	0.85	2.14	2.927 (5)	154.5

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.

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.

References

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

doi:10.1107/S1600536808022745

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

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

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

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