Bis[2-(pyrimidin-2-ylamino)pyrimidin­ium] hexa­molybdate

Yeh, C.-W.; Lin, C.-H.; Chen, J.-D.

doi:10.1107/S1600536807062897

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 1| January 2008| Page m41

https://doi.org/10.1107/S1600536807062897

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Bis[2-(pyrimidin-2-ylamino)pyrimidinium] hexamolybdate

Chun-Wei Yeh,^a Chia-Her Lin ^a ^* and Jhy-Der Chen ^a

^aDepartment of Chemistry, Chung-Yuan Christian University, Chung-Li 320, Taiwan
^*Correspondence e-mail: jdchen@cycu.edu.tw

(Received 24 October 2007; accepted 24 November 2007; online 6 December 2007)

The title compound, (C₈H₈N₅)₂[Mo₆O₁₉], was prepared by reaction of Mo(CO)₆ and dipyrimidylamine in refluxing toluene. The hexanuclear polyoxomolybdate anions lie on centres of inversion. Each 2-(pyrimidin-2-ylamino)pyrimidinium cation forms an intramolecular N—H⋯N hydrogen bond and the cations are linked through self-complementary pairs of N—H⋯N hydrogen bonds into dimers across centres of inversion. The cations and anions are interlinked through C—H⋯O contacts.

Related literature

For related literature, see: Shivaiah (2006 ); Bridgeman & Cavigliasso (2002 ); Shi et al. (2006 ); Wang et al. (2004 ); Guo et al. (2004 ); Burkholder & Zubieta (2004 ); Hagrman et al. (1999 ).

Experimental

Crystal data

(C₈H₈N₅)₂[Mo₆O₁₉]
M_r = 1228.03
Monoclinic, P 2₁ /n
a = 10.4338 (19) Å
b = 13.7437 (19) Å
c = 11.0792 (17) Å
β = 105.471 (13)°
V = 1531.2 (4) Å³
Z = 2
Mo Kα radiation
μ = 2.48 mm⁻¹
T = 295 (2) K
0.40 × 0.20 × 0.05 mm

Data collection

Bruker P4 diffractometer
Absorption correction: ψ scan (North et al., 1968 ) T_min = 0.578, T_max = 0.883
3399 measured reflections
2660 independent reflections
1833 reflections with I > 2σ(I)
R_int = 0.082
3 standard reflections every 97 reflections intensity decay: none

Refinement

R[F² > 2σ(F²)] = 0.057
wR(F²) = 0.146
S = 1.02
2660 reflections
232 parameters
H-atom parameters constrained
Δρ_max = 0.91 e Å⁻³
Δρ_min = −1.78 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H3N⋯N4	0.86	1.95	2.605 (12)	132
N1—H1N⋯N5ⁱ	0.86	2.07	2.924 (13)	180
C2—H2⋯O8ⁱⁱ	0.93	2.65	3.444 (14)	144
C4—H4⋯O2ⁱⁱⁱ	0.93	2.69	3.391 (14)	133
C6—H6⋯O6^iv	0.93	2.38	3.250 (15)	157
C7—H7⋯O1^v	0.93	2.51	3.196 (14)	131
Symmetry codes: (i) -x+1, -y+2, -z+1; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: XSCANS (Siemens, 1996 ); cell refinement: XSCANS; data reduction: XSCANS program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536807062897/bi2259sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807062897/bi2259Isup2.hkl

checkCIF report

Comment top

Polyoxomolybdates are an important class of metal-oxygen cluster compounds (Shivaiah, 2006; Bridgeman & Cavigliasso, 2002) which show interesting chemical and physical properties (Shi, et al., 2006; Wang, et al., 2004; Guo, et al., 2004; Burkholder & Zubieta, 2004; Hagrman, et al., 1999). Since the anions contain many oxygen atoms which are good hydrogen-bond acceptors, cocrystallization with organic cations should result in interesting supramolecular chemistry. In the title complex (Fig. 1), the protonated dipyrimidylamine molecules (Hdipm) are linked into dimers by N—H···N hydrogen bonds. The cations and anions are interlinked through C—H···O contacts (Fig. 2).

Related literature top

For related literature, see: Shivaiah (2006); Bridgeman & Cavigliasso (2002); Shi et al. (2006); Wang et al. (2004); Guo et al. (2004); Burkholder & Zubieta (2004); Hagrman et al. (1999).

Experimental top

Mo(CO)₆ (0.52 g, 2.00 mmol) was added to a solution of dipyrimidylamine (dipm) (0.34 g, 2.00 mmol) in 20 ml toluene. The mixture was refluxed for 18 h to yield an orange solution. The solvent was reduced and n-hexanes added to induce precipitation. The precipitate was filtered and washed by ether (3 × 10 ml) and then dried under reduced pressure to give an orange powder. The green plate crystals were obtained by slow diffusion of ether into a CH₂Cl₂ solution of the orange powder. The crystals were filtered and washed by ether (3 × 10 ml) and then dried under reduced pressure. Overall crystal yield: 0.207 g (8.43%, based on Mo). Elemental analysis calculated: C, 15.16%; H, 1.31%; N, 11.41%; found: C, 15.02%; H, 1.34%; N, 11.03%.

Structure description top

For related literature, see: Shivaiah (2006); Bridgeman & Cavigliasso (2002); Shi et al. (2006); Wang et al. (2004); Guo et al. (2004); Burkholder & Zubieta (2004); Hagrman et al. (1999).

Computing details top

Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS (Siemens, 1996); data reduction: XSCANS (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1997.

Figures top

	Fig. 1. The molecular structure of the title compound showing displacement ellipsoids at the 30% probability level for non-H atoms.
	Fig. 2. Partial packing diagram showing N—H···N hydrogen bonding between Hdipm molecules and C—H···O contacts to the polyoxometalate.

Bis[2-(pyrimidin-2-ylamino)pyrimidinium] hexamolybdate top

Crystal data top

(C₈H₈N₅)₂[Mo₆O₁₉]	F(000) = 1172
M_r = 1228.03	D_x = 2.664 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 31 reflections
a = 10.4338 (19) Å	θ = 4.8–12.5°
b = 13.7437 (19) Å	µ = 2.48 mm⁻¹
c = 11.0792 (17) Å	T = 295 K
β = 105.471 (13)°	Plate, green
V = 1531.2 (4) Å³	0.40 × 0.20 × 0.05 mm
Z = 2

Data collection top

Bruker P4 diffractometer	1833 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.082
Graphite monochromator	θ_max = 25.0°, θ_min = 2.4°
ω scans	h = −1→12
Absorption correction: ψ scan (North et al., 1968)	k = −1→16
T_min = 0.578, T_max = 0.883	l = −13→12
3399 measured reflections	3 standard reflections every 97 reflections
2660 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.057	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.146	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0858P)²] where P = (F_o² + 2F_c²)/3
2660 reflections	(Δ/σ)_max < 0.001
232 parameters	Δρ_max = 0.91 e Å⁻³
0 restraints	Δρ_min = −1.78 e Å⁻³

Crystal data top

(C₈H₈N₅)₂[Mo₆O₁₉]	V = 1531.2 (4) Å³
M_r = 1228.03	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 10.4338 (19) Å	µ = 2.48 mm⁻¹
b = 13.7437 (19) Å	T = 295 K
c = 11.0792 (17) Å	0.40 × 0.20 × 0.05 mm
β = 105.471 (13)°

Data collection top

Bruker P4 diffractometer	1833 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.082
T_min = 0.578, T_max = 0.883	3 standard reflections every 97 reflections
3399 measured reflections	intensity decay: none
2660 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.057	0 restraints
wR(F²) = 0.146	H-atom parameters constrained
S = 1.02	Δρ_max = 0.91 e Å⁻³
2660 reflections	Δρ_min = −1.78 e Å⁻³
232 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
Mo1	0.06601 (9)	0.95848 (7)	0.32376 (8)	0.0380 (3)
Mo2	−0.15184 (9)	0.87281 (7)	0.46013 (9)	0.0418 (3)
Mo3	0.16049 (9)	0.89727 (7)	0.61876 (9)	0.0434 (3)
N1	0.4384 (8)	0.9695 (6)	0.3239 (8)	0.040 (2)
H1N	0.4607	1.0166	0.3764	0.048*
N2	0.4053 (10)	1.0908 (7)	0.1792 (9)	0.052 (2)
N3	0.3659 (9)	0.9281 (7)	0.1128 (8)	0.043 (2)
H3N	0.3676	0.8676	0.1331	0.052*
N4	0.4025 (9)	0.8036 (6)	0.2961 (9)	0.046 (2)
N5	0.4845 (8)	0.8709 (6)	0.4968 (9)	0.040 (2)
O1	0.1142 (7)	0.9318 (7)	0.1952 (7)	0.065 (2)
O2	−0.2622 (8)	0.7811 (6)	0.4336 (9)	0.072 (3)
O3	0.2743 (9)	0.8222 (7)	0.7019 (9)	0.076 (3)
O4	0.0000	1.0000	0.5000	0.0286 (19)
O5	−0.0732 (7)	0.8658 (5)	0.3211 (7)	0.052 (2)
O6	0.1775 (7)	1.0683 (5)	0.3902 (7)	0.0414 (17)
O7	0.1797 (7)	0.8825 (5)	0.4514 (7)	0.0446 (18)
O8	0.0033 (7)	0.8138 (5)	0.5623 (8)	0.056 (2)
O9	−0.0736 (7)	1.0520 (6)	0.2626 (6)	0.052 (2)
O10	−0.2525 (6)	0.9816 (6)	0.3719 (6)	0.0465 (19)
C1	0.4034 (10)	0.9955 (8)	0.1993 (9)	0.041 (3)
C2	0.3673 (12)	1.1171 (10)	0.0578 (12)	0.060 (3)
H2	0.3699	1.1827	0.0376	0.072*
C3	0.3249 (13)	1.0509 (11)	−0.0372 (12)	0.064 (4)
H3	0.2968	1.0711	−0.1202	0.077*
C4	0.3252 (12)	0.9553 (10)	−0.0069 (11)	0.055 (3)
H4	0.2971	0.9089	−0.0694	0.066*
C5	0.4425 (9)	0.8789 (7)	0.3750 (10)	0.037 (2)
C6	0.4060 (12)	0.7135 (9)	0.3495 (12)	0.054 (3)
H6	0.3774	0.6596	0.2987	0.064*
C7	0.4491 (11)	0.7019 (8)	0.4714 (11)	0.048 (3)
H7	0.4537	0.6402	0.5068	0.057*
C8	0.4876 (10)	0.7831 (8)	0.5462 (10)	0.046 (3)
H8	0.5161	0.7758	0.6327	0.055*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0374 (5)	0.0496 (6)	0.0324 (5)	−0.0021 (4)	0.0188 (4)	−0.0061 (4)
Mo2	0.0393 (5)	0.0414 (5)	0.0508 (6)	−0.0114 (4)	0.0228 (4)	−0.0095 (4)
Mo3	0.0400 (5)	0.0502 (6)	0.0424 (6)	0.0122 (4)	0.0151 (4)	0.0098 (5)
N1	0.043 (5)	0.041 (5)	0.035 (5)	−0.002 (4)	0.009 (4)	−0.005 (4)
N2	0.059 (6)	0.049 (6)	0.048 (6)	−0.006 (5)	0.016 (5)	0.000 (5)
N3	0.053 (5)	0.046 (5)	0.034 (5)	0.004 (4)	0.016 (4)	−0.005 (4)
N4	0.047 (5)	0.042 (5)	0.051 (6)	0.003 (4)	0.018 (4)	−0.007 (5)
N5	0.036 (5)	0.045 (5)	0.038 (5)	0.004 (4)	0.009 (4)	0.001 (4)
O1	0.046 (4)	0.120 (7)	0.036 (4)	−0.014 (5)	0.023 (4)	−0.025 (5)
O2	0.069 (6)	0.067 (6)	0.100 (7)	−0.029 (5)	0.054 (5)	−0.034 (5)
O3	0.067 (6)	0.088 (7)	0.075 (6)	0.035 (5)	0.026 (5)	0.038 (5)
O4	0.024 (4)	0.037 (5)	0.029 (5)	−0.002 (4)	0.014 (4)	−0.009 (4)
O5	0.047 (4)	0.055 (5)	0.061 (5)	−0.024 (4)	0.029 (4)	−0.029 (4)
O6	0.040 (4)	0.042 (4)	0.049 (4)	0.004 (3)	0.025 (3)	0.003 (3)
O7	0.042 (4)	0.042 (4)	0.058 (5)	0.012 (3)	0.028 (4)	0.003 (4)
O8	0.062 (5)	0.032 (4)	0.085 (6)	0.012 (4)	0.037 (5)	0.014 (4)
O9	0.042 (4)	0.083 (6)	0.034 (4)	0.013 (4)	0.017 (3)	0.016 (4)
O10	0.028 (3)	0.077 (5)	0.035 (4)	−0.003 (4)	0.009 (3)	−0.002 (4)
C1	0.046 (6)	0.047 (7)	0.034 (6)	−0.002 (5)	0.018 (5)	0.004 (5)
C2	0.063 (8)	0.066 (8)	0.053 (8)	0.001 (7)	0.021 (7)	0.007 (7)
C3	0.067 (8)	0.085 (10)	0.039 (7)	−0.007 (7)	0.011 (6)	0.010 (7)
C4	0.055 (7)	0.066 (8)	0.046 (8)	0.004 (6)	0.017 (6)	−0.005 (6)
C5	0.025 (5)	0.047 (6)	0.038 (6)	−0.001 (4)	0.008 (4)	−0.012 (5)
C6	0.061 (7)	0.044 (7)	0.060 (9)	0.002 (6)	0.023 (6)	−0.012 (6)
C7	0.058 (7)	0.035 (6)	0.048 (8)	0.000 (5)	0.011 (6)	−0.002 (5)
C8	0.051 (7)	0.052 (7)	0.041 (7)	0.007 (5)	0.023 (5)	0.008 (6)

Geometric parameters (Å, º) top

Mo1—O1	1.673 (7)	N3—C1	1.315 (13)
Mo1—O7	1.897 (7)	N3—C4	1.333 (14)
Mo1—O9	1.926 (7)	N3—H3N	0.860
Mo1—O5	1.926 (7)	N4—C5	1.347 (13)
Mo1—O6	1.927 (7)	N4—C6	1.369 (15)
Mo1—O4	2.3087 (9)	N5—C5	1.308 (13)
Mo2—O2	1.680 (8)	N5—C8	1.321 (13)
Mo2—O8	1.892 (8)	O4—Mo1ⁱ	2.3087 (9)
Mo2—O6ⁱ	1.927 (7)	O4—Mo3ⁱ	2.3137 (9)
Mo2—O5	1.931 (8)	O4—Mo2ⁱ	2.3210 (9)
Mo2—O10	1.935 (7)	O6—Mo2ⁱ	1.927 (7)
Mo2—O4	2.3210 (9)	O9—Mo3ⁱ	1.916 (7)
Mo3—O3	1.655 (8)	O10—Mo3ⁱ	1.911 (8)
Mo3—O10ⁱ	1.911 (8)	C2—C3	1.372 (18)
Mo3—O9ⁱ	1.916 (7)	C2—H2	0.930
Mo3—O7	1.928 (8)	C3—C4	1.356 (19)
Mo3—O8	1.963 (8)	C3—H3	0.930
Mo3—O4	2.3137 (9)	C4—H4	0.930
N1—C5	1.364 (13)	C6—C7	1.314 (16)
N1—C1	1.378 (13)	C6—H6	0.930
N1—H1N	0.860	C7—C8	1.384 (15)
N2—C1	1.329 (14)	C7—H7	0.930
N2—C2	1.347 (15)	C8—H8	0.930

O1—Mo1—O7	104.1 (4)	C1—N3—H3N	120.6
O1—Mo1—O9	102.6 (4)	C4—N3—H3N	120.6
O7—Mo1—O9	153.3 (3)	C5—N4—C6	116.5 (10)
O1—Mo1—O5	103.8 (4)	C5—N5—C8	117.9 (9)
O7—Mo1—O5	88.1 (3)	Mo1ⁱ—O4—Mo1	180.0
O9—Mo1—O5	86.5 (4)	Mo1ⁱ—O4—Mo3	90.22 (4)
O1—Mo1—O6	102.0 (4)	Mo1—O4—Mo3	89.78 (4)
O7—Mo1—O6	87.3 (3)	Mo1ⁱ—O4—Mo3ⁱ	89.78 (4)
O9—Mo1—O6	86.2 (3)	Mo1—O4—Mo3ⁱ	90.22 (4)
O5—Mo1—O6	154.1 (3)	Mo3—O4—Mo3ⁱ	180.0
O1—Mo1—O4	178.3 (4)	Mo1ⁱ—O4—Mo2	90.27 (3)
O7—Mo1—O4	76.9 (2)	Mo1—O4—Mo2	89.73 (3)
O9—Mo1—O4	76.4 (2)	Mo3—O4—Mo2	90.14 (4)
O5—Mo1—O4	77.4 (2)	Mo3ⁱ—O4—Mo2	89.86 (4)
O6—Mo1—O4	76.7 (2)	Mo1ⁱ—O4—Mo2ⁱ	89.73 (3)
O2—Mo2—O8	102.7 (4)	Mo1—O4—Mo2ⁱ	90.27 (3)
O2—Mo2—O6ⁱ	102.7 (4)	Mo3—O4—Mo2ⁱ	89.86 (4)
O8—Mo2—O6ⁱ	87.6 (3)	Mo3ⁱ—O4—Mo2ⁱ	90.14 (4)
O2—Mo2—O5	103.9 (3)	Mo2—O4—Mo2ⁱ	180.0
O8—Mo2—O5	88.8 (4)	Mo1—O5—Mo2	115.7 (3)
O6ⁱ—Mo2—O5	153.3 (3)	Mo2ⁱ—O6—Mo1	116.7 (3)
O2—Mo2—O10	103.7 (4)	Mo1—O7—Mo3	117.0 (3)
O8—Mo2—O10	153.6 (3)	Mo2—O8—Mo3	116.7 (3)
O6ⁱ—Mo2—O10	85.9 (3)	Mo3ⁱ—O9—Mo1	116.9 (3)
O5—Mo2—O10	85.6 (3)	Mo3ⁱ—O10—Mo2	116.6 (3)
O2—Mo2—O4	179.1 (3)	N3—C1—N2	125.9 (10)
O8—Mo2—O4	77.2 (2)	N3—C1—N1	119.6 (10)
O6ⁱ—Mo2—O4	76.4 (2)	N2—C1—N1	114.3 (10)
O5—Mo2—O4	77.0 (2)	N2—C2—C3	122.4 (13)
O10—Mo2—O4	76.4 (2)	N2—C2—H2	118.8
O3—Mo3—O10ⁱ	103.7 (4)	C3—C2—H2	118.8
O3—Mo3—O9ⁱ	104.2 (4)	C4—C3—C2	118.3 (12)
O10ⁱ—Mo3—O9ⁱ	88.2 (3)	C4—C3—H3	120.9
O3—Mo3—O7	103.1 (4)	C2—C3—H3	120.9
O10ⁱ—Mo3—O7	88.0 (3)	N3—C4—C3	119.8 (12)
O9ⁱ—Mo3—O7	152.6 (3)	N3—C4—H4	120.1
O3—Mo3—O8	103.1 (4)	C3—C4—H4	120.1
O10ⁱ—Mo3—O8	153.1 (3)	N5—C5—N4	124.5 (10)
O9ⁱ—Mo3—O8	85.6 (3)	N5—C5—N1	118.0 (9)
O7—Mo3—O8	85.7 (3)	N4—C5—N1	117.5 (9)
O3—Mo3—O4	179.0 (4)	C7—C6—N4	121.1 (11)
O10ⁱ—Mo3—O4	77.1 (2)	C7—C6—H6	119.5
O9ⁱ—Mo3—O4	76.4 (2)	N4—C6—H6	119.5
O7—Mo3—O4	76.2 (2)	C6—C7—C8	118.8 (11)
O8—Mo3—O4	76.0 (2)	C6—C7—H7	120.6
C5—N1—C1	128.6 (9)	C8—C7—H7	120.6
C5—N1—H1N	115.7	N5—C8—C7	121.2 (10)
C1—N1—H1N	115.7	N5—C8—H8	119.4
C1—N2—C2	114.8 (10)	C7—C8—H8	119.4
C1—N3—C4	118.7 (10)

Symmetry code: (i) −x, −y+2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3N···N4	0.86	1.95	2.605 (12)	132
N1—H1N···N5ⁱⁱ	0.86	2.07	2.924 (13)	180
C2—H2···O8ⁱⁱⁱ	0.93	2.65	3.444 (14)	144
C4—H4···O2^iv	0.93	2.69	3.391 (14)	133
C6—H6···O6^v	0.93	2.38	3.250 (15)	157
C7—H7···O1^vi	0.93	2.51	3.196 (14)	131

Symmetry codes: (ii) −x+1, −y+2, −z+1; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x+1/2, −y+3/2, z−1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) x+1/2, −y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula	(C₈H₈N₅)₂[Mo₆O₁₉]
M_r	1228.03
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	295
a, b, c (Å)	10.4338 (19), 13.7437 (19), 11.0792 (17)
β (°)	105.471 (13)
V (Å³)	1531.2 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.48
Crystal size (mm)	0.40 × 0.20 × 0.05

Data collection
Diffractometer	Bruker P4
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.578, 0.883
No. of measured, independent and observed [I > 2σ(I)] reflections	3399, 2660, 1833
R_int	0.082
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.057, 0.146, 1.02
No. of reflections	2660
No. of parameters	232
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.91, −1.78

Computer programs: XSCANS (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL (Bruker, 1997.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3N···N4	0.86	1.95	2.605 (12)	131.5
N1—H1N···N5ⁱ	0.86	2.07	2.924 (13)	179.6
C2—H2···O8ⁱⁱ	0.93	2.65	3.444 (14)	144.0
C4—H4···O2ⁱⁱⁱ	0.93	2.69	3.391 (14)	133.3
C6—H6···O6^iv	0.93	2.38	3.250 (15)	156.5
C7—H7···O1^v	0.93	2.51	3.196 (14)	131.3

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x+1/2, −y+3/2, z−1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) x+1/2, −y+3/2, z+1/2.

Acknowledgements

We are grateful to the National Science Council of the Republic of China for support. This research was also supported by the project of the specific research fields in Chung Yuan Christian University, Taiwan, under grant CYCU-95-CR-CH.

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