Diammonium bis­[(2-amino­acetato-κ2N,O)(2,2′-bipyridine-κ2N,N′)(N,N-dimethyl­formamide-κO)copper(II)] hexa­cosa­oxidoocta­molybdate(VI)

Liu, H.; Zhang, Y.; Yu, D.

doi:10.1107/S1600536808000020

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Pages m305-m306

doi:10.1107/S1600536808000020

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Diammonium bis[(2-aminoacetato-κ²N,O)(2,2′-bipyridine-κ²N,N′)(N,N-dimethylformamide-κO)copper(II)] hexacosaoxidooctamolybdate(VI)

Haiyan Liu,^a ^* Yunjie Zhang ^a and Decheng Yu ^a

^aCollege of Chemistry and Pharmacy, Jiamusi University, Jiamusi 154007, People's Republic of China
^*Correspondence e-mail: hyliu2007@yahoo.cn

(Received 6 December 2007; accepted 1 January 2008; online 9 January 2008)

The title compound, (NH₄)₂[Cu(C₂H₄NO₂)(C₁₀H₈N₂)(C₃H₇NO)]₂[Mo₈O₂₆], contains a centrosymmetric β-type octamolybdate anion, two copper(II) complex cations and two ammonium ions. The Cu^II atom is coordinated in a square-pyramidal geometry by a 2,2′-bipyridine and a 2-aminoacetate ligands in the basal plane and by an O atom of N,N-dimethylformamide in the apical position. The anions and cations are linked by N—H⋯O hydrogen bonds into a three-dimensional network.

Related literature

For related literature, see: Allis et al. (2004 ); Brown & Altermatt (1985 ).

Experimental

Crystal data

(NH₄)₂[Cu(C₂H₄NO₂)(C₁₀H₈N₂)(C₃H₇NO)]₂[Mo₈O₂₆]
M_r = 1953.38
Triclinic, $[P \overline 1]$
a = 10.222 (2) Å
b = 10.849 (2) Å
c = 13.020 (3) Å
α = 81.82 (3)°
β = 69.91 (2)°
γ = 81.61 (3)°
V = 1334.9 (5) Å³
Z = 1
Mo Kα radiation
μ = 2.69 mm⁻¹
T = 291 (2) K
0.28 × 0.20 × 0.14 mm

Data collection

Bruker SMART APEXII diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.530, T_max = 0.690
10864 measured reflections
4889 independent reflections
3591 reflections with I > 2σ(I)
R_int = 0.070

Refinement

R[F² > 2σ(F²)] = 0.046
wR(F²) = 0.110
S = 0.99
4889 reflections
370 parameters
H-atom parameters constrained
Δρ_max = 0.86 e Å⁻³
Δρ_min = −0.83 e Å⁻³

Table 1
Selected bond lengths (Å)

Cu—O14	1.925 (4)
Cu—O16	2.604 (4)
Cu—N1	1.985 (6)
Cu—N2	1.989 (6)
Cu—N3	1.990 (6)
Mo1—O1	1.705 (5)
Mo1—O6	1.720 (4)
Mo1—O11	1.896 (4)
Mo1—O10	1.995 (5)
Mo1—O12	2.306 (4)
Mo1—O7ⁱ	2.356 (5)
Mo2—O8	1.699 (4)
Mo2—O2	1.722 (5)
Mo2—O9	1.897 (4)
Mo2—O7ⁱ	1.998 (5)
Mo2—O10	2.340 (4)
Mo2—O12ⁱ	2.346 (4)
Mo3—O4	1.696 (5)
Mo3—O5	1.756 (5)
Mo3—O10	1.960 (4)
Mo3—O7	1.967 (4)
Mo3—O12	2.143 (4)
Mo3—O12ⁱ	2.380 (4)
Mo4—O13	1.693 (4)
Mo4—O3	1.716 (5)
Mo4—O9ⁱ	1.921 (4)
Mo4—O11	1.945 (4)
Mo4—O5ⁱ	2.257 (5)
Mo4—O12	2.491 (4)
Symmetry code: (i) -x+1, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O3ⁱⁱ	0.90	2.32	3.093 (7)	144
N1—H1B⋯O6	0.90	2.01	2.863 (6)	158
N5—HN1⋯O1	0.90	2.10	2.888 (7)	146
N5—HN2⋯O4	0.95	2.13	3.028 (8)	158
N5—HN3⋯O15ⁱⁱⁱ	0.95	1.94	2.761 (8)	143
N5—HN4⋯O14ⁱⁱⁱ	0.98	2.26	3.132 (7)	148
Symmetry codes: (ii) -x+1, -y+2, -z+1; (iii) x, y, z-1.

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997 ); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXTL (Bruker, 1997.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000020/hy2114sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808000020/hy2114Isup2.hkl

checkCIF report

Comment top

Polymolybdates (POMs) modified by transition metal complexes have been extensively explored (Allis et al., 2004). To further explore new POMs belonging to this family, the title compound is reported here.

The title compound consists of a [Mo₈O₂₆]^4- anion, two [Cu(bpy)(gly)(dmf)]⁺ cations and two ammonium ions (bpy = 2,2'-bipyridine, gly = 2-aminoacetate, dmf = N,N-dimethylfomamide) (Fig. 1). The [Mo₈O₂₆]^4- anion in the β-type lies on an inversion center, made up of eight edge-sharing MoO₆ octahedra. The Cu^II atom in the [Cu(bpy)(gly)(dmf)]⁺ cation displays a distorted square-pyramidal geometry with two N atoms from the 2,2'-bipyridine ligand and an O atom and an N atom from the 2-aminoacetate ligand in the basal plane and an O atom of N,N-dimethylfomamide in the apical position. The Mo—O, Cu—N and Cu—O distances are given in Table 1. A calculation of bond valence sum (Brown & Altermatt, 1985) indicates the oxidation states of 5.71–5.84 for the Mo atoms and 2.17 for the Cu atom, in agreement with the expected values. These anions and cations connect to each other by N—H···O hydrogen bonds (Table 2), forming a three-dimensional supramolecular network, as shown in Fig. 2.

Related literature top

For related literature, see: Allis et al. (2004); Brown & Altermatt (1985).

Experimental top

(NH₄)₆(Mo₇O₂₄).4H₂O (1.50 g, 1.2 mmol), Cu(CH₃COO)₂.2H₂O (0.20 g, 1.0 mmol), 2-aminoacetic acid (0.075 g, 1.0 mmol) and bpy (0.16 g, 1.0 mmol) were dissolved in 0.5 M HCl solution (15 ml) with stirring. Then the suspension was added to a dmf solution (10 ml), which was refluxed at 333 K for 3 h. After cooling to room temperature, the mixture was filtrated and transferred into a 50 ml beaker. Blue block crystals of the title compound suitable for X-ray diffraction were obtained after several days.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL (Bruker, 1997; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Bruker, 1997.

Figures top

	Fig. 1. The structures of the anion and cation of the title compound (the ammonium ion has been omitted). Displacement ellipsoides are drawn at the 30% probability level. [Symmetry code: (i) 1 - x, 1 - y, 1 - z.]
	Fig. 2. Crystal packing of the title compound. The ammonium ions are drawn as ball. Dotted lines denote hydrogen bonds.

Diammonium bis[(2-aminoacetato-κ²N,O)(2,2'-bipyridine-κ²N,N')(N,N- dimethylformamide-κO)copper(II)] hexacosaoxidooctamolybdate(VI) top

Crystal data top

(NH₄)₂[Cu(C₂H₄NO₂)(C₁₀H₈N₂)(C₃H₇NO)]₂[Mo₈O₂₆]	Z = 1
M_r = 1953.38	F(000) = 946
Triclinic, P1	D_x = 2.430 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.222 (2) Å	Cell parameters from 3544 reflections
b = 10.849 (2) Å	θ = 1.6–26.3°
c = 13.020 (3) Å	µ = 2.70 mm⁻¹
α = 81.82 (3)°	T = 291 K
β = 69.91 (2)°	Block, blue
γ = 81.61 (3)°	0.28 × 0.20 × 0.14 mm
V = 1334.9 (5) Å³

Data collection top

Bruker SMART APEXII diffractometer	4889 independent reflections
Radiation source: fine-focus sealed tube	3591 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.071
ϕ and ω scans	θ_max = 25.6°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
T_min = 0.530, T_max = 0.690	k = −13→13
10864 measured reflections	l = −15→14

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.110	H-atom parameters constrained
S = 0.99	w = 1/[σ²(F_o²) + (0.0226P)²] where P = (F_o² + 2F_c²)/3
4889 reflections	(Δ/σ)_max < 0.001
370 parameters	Δρ_max = 0.86 e Å⁻³
0 restraints	Δρ_min = −0.83 e Å⁻³

Crystal data top

(NH₄)₂[Cu(C₂H₄NO₂)(C₁₀H₈N₂)(C₃H₇NO)]₂[Mo₈O₂₆]	γ = 81.61 (3)°
M_r = 1953.38	V = 1334.9 (5) Å³
Triclinic, P1	Z = 1
a = 10.222 (2) Å	Mo Kα radiation
b = 10.849 (2) Å	µ = 2.70 mm⁻¹
c = 13.020 (3) Å	T = 291 K
α = 81.82 (3)°	0.28 × 0.20 × 0.14 mm
β = 69.91 (2)°

Data collection top

Bruker SMART APEXII diffractometer	4889 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3591 reflections with I > 2σ(I)
T_min = 0.530, T_max = 0.690	R_int = 0.071
10864 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.046	0 restraints
wR(F²) = 0.110	H-atom parameters constrained
S = 0.99	Δρ_max = 0.86 e Å⁻³
4889 reflections	Δρ_min = −0.83 e Å⁻³
370 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cu	0.56754 (7)	0.78752 (8)	0.79555 (7)	0.0191 (2)
Mo1	0.39065 (5)	0.75790 (5)	0.50257 (5)	0.01630 (15)
Mo2	0.36042 (5)	0.54294 (5)	0.72689 (5)	0.01687 (15)
Mo3	0.34518 (5)	0.48004 (5)	0.47185 (5)	0.01409 (15)
Mo4	0.69102 (5)	0.74002 (5)	0.30214 (5)	0.01864 (16)
O1	0.3028 (4)	0.8061 (4)	0.4114 (4)	0.0242 (11)
O2	0.4582 (4)	0.4794 (4)	0.8097 (4)	0.0244 (11)
O3	0.5990 (4)	0.7957 (4)	0.2141 (4)	0.0258 (11)
O4	0.2585 (4)	0.5422 (4)	0.3833 (4)	0.0227 (11)
O5	0.2406 (4)	0.3680 (4)	0.5603 (4)	0.0211 (11)
O6	0.3191 (4)	0.8577 (4)	0.6038 (4)	0.0235 (11)
O7	0.4909 (4)	0.3616 (4)	0.3840 (4)	0.0172 (10)
O8	0.2517 (5)	0.6614 (4)	0.7940 (4)	0.0256 (11)
O9	0.2357 (4)	0.4195 (4)	0.7536 (4)	0.0223 (11)
O10	0.2874 (4)	0.6092 (4)	0.5743 (4)	0.0167 (10)
O11	0.5653 (4)	0.8223 (4)	0.4285 (4)	0.0192 (10)
O12	0.5191 (4)	0.5901 (4)	0.4106 (3)	0.0150 (9)
O13	0.8335 (4)	0.8205 (5)	0.2580 (4)	0.0282 (12)
O14	0.4272 (4)	0.7617 (4)	0.9377 (4)	0.0223 (11)
O15	0.2086 (4)	0.8280 (4)	1.0374 (4)	0.0247 (11)
O16	0.6474 (5)	0.9741 (5)	0.8567 (5)	0.0330 (13)
N1	0.4294 (5)	0.9213 (5)	0.7618 (4)	0.0186 (12)
H1A	0.4624	0.9962	0.7515	0.022*
H1B	0.4162	0.9084	0.6994	0.022*
N2	0.7255 (5)	0.8036 (5)	0.6548 (5)	0.0195 (13)
N3	0.7002 (5)	0.6481 (5)	0.8305 (5)	0.0176 (12)
N4	0.8488 (6)	0.8849 (6)	0.8898 (5)	0.0257 (14)
N5	0.3354 (5)	0.7456 (6)	0.1944 (5)	0.0272 (14)
HN1	0.3438	0.7903	0.2442	0.033*
HN2	0.3330	0.6704	0.2418	0.033*
HN3	0.2584	0.7693	0.1687	0.033*
HN4	0.3996	0.7429	0.1189	0.033*
C1	0.6771 (7)	0.5713 (7)	0.9239 (6)	0.0281 (18)
H1	0.5909	0.5821	0.9791	0.034*
C2	0.7758 (6)	0.4768 (6)	0.9418 (5)	0.0214 (15)
H2	0.7570	0.4254	1.0076	0.026*
C3	0.9044 (7)	0.4610 (7)	0.8582 (6)	0.0305 (17)
H3	0.9719	0.3967	0.8667	0.037*
C4	0.9304 (7)	0.5408 (7)	0.7636 (6)	0.0269 (17)
H4	1.0174	0.5328	0.7089	0.032*
C5	0.9663 (7)	0.7332 (7)	0.5632 (6)	0.0243 (16)
H5	1.0468	0.6802	0.5620	0.029*
C6	0.9666 (7)	0.8216 (8)	0.4778 (7)	0.037 (2)
H6	1.0483	0.8279	0.4179	0.044*
C7	0.8487 (7)	0.9025 (6)	0.4776 (6)	0.0242 (15)
H7	0.8492	0.9621	0.4186	0.029*
C8	0.7291 (6)	0.8904 (6)	0.5697 (6)	0.0202 (15)
H8	0.6489	0.9446	0.5724	0.024*
C9	0.8275 (6)	0.6337 (6)	0.7489 (6)	0.0200 (15)
C10	0.8423 (6)	0.7234 (6)	0.6532 (5)	0.0177 (14)
C11	0.2938 (6)	0.9214 (7)	0.8538 (6)	0.0216 (15)
H11A	0.2230	0.8961	0.8293	0.026*
H11B	0.2635	1.0053	0.8761	0.026*
C12	0.3090 (6)	0.8328 (6)	0.9503 (6)	0.0213 (16)
C13	0.7109 (7)	0.9109 (7)	0.9152 (7)	0.0316 (19)
H14	0.6564	0.8782	0.9842	0.038*
C14	0.9409 (7)	0.9421 (8)	0.7868 (7)	0.039 (2)
H14A	1.0368	0.9144	0.7803	0.058*
H14B	0.9257	1.0316	0.7863	0.058*
H14C	0.9208	0.9179	0.7261	0.058*
C15	0.9148 (8)	0.8121 (9)	0.9643 (7)	0.043 (2)
H15A	1.0146	0.8049	0.9296	0.065*
H15B	0.8833	0.7302	0.9825	0.065*
H15C	0.8902	0.8530	1.0301	0.065*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu	0.0149 (4)	0.0195 (5)	0.0211 (5)	0.0014 (3)	−0.0060 (3)	0.0001 (4)
Mo1	0.0182 (3)	0.0128 (3)	0.0184 (3)	0.0010 (2)	−0.0078 (2)	−0.0011 (2)
Mo2	0.0177 (3)	0.0176 (3)	0.0147 (3)	0.0002 (2)	−0.0052 (2)	−0.0019 (2)
Mo3	0.0135 (3)	0.0140 (3)	0.0155 (3)	−0.0008 (2)	−0.0062 (2)	−0.0008 (2)
Mo4	0.0185 (3)	0.0172 (3)	0.0199 (3)	−0.0037 (2)	−0.0073 (2)	0.0036 (3)
O1	0.027 (2)	0.023 (3)	0.024 (3)	0.004 (2)	−0.012 (2)	−0.002 (2)
O2	0.027 (2)	0.026 (3)	0.018 (3)	0.001 (2)	−0.006 (2)	−0.003 (2)
O3	0.027 (3)	0.020 (3)	0.029 (3)	−0.002 (2)	−0.012 (2)	0.009 (2)
O4	0.019 (2)	0.029 (3)	0.023 (3)	0.004 (2)	−0.011 (2)	−0.007 (2)
O5	0.017 (2)	0.021 (3)	0.027 (3)	−0.0034 (19)	−0.009 (2)	−0.001 (2)
O6	0.030 (3)	0.019 (3)	0.024 (3)	0.002 (2)	−0.012 (2)	−0.005 (2)
O7	0.021 (2)	0.013 (2)	0.020 (2)	0.0024 (18)	−0.0121 (19)	0.001 (2)
O8	0.031 (3)	0.021 (3)	0.025 (3)	0.003 (2)	−0.012 (2)	−0.005 (2)
O9	0.017 (2)	0.025 (3)	0.023 (3)	0.0033 (19)	−0.007 (2)	−0.002 (2)
O10	0.017 (2)	0.018 (2)	0.016 (2)	0.0007 (18)	−0.0081 (19)	−0.001 (2)
O11	0.022 (2)	0.016 (2)	0.021 (3)	−0.0067 (18)	−0.008 (2)	0.002 (2)
O12	0.014 (2)	0.015 (2)	0.016 (2)	−0.0009 (17)	−0.0053 (19)	0.0000 (19)
O13	0.026 (3)	0.026 (3)	0.034 (3)	−0.012 (2)	−0.012 (2)	0.008 (2)
O14	0.015 (2)	0.029 (3)	0.016 (3)	−0.0027 (19)	−0.0006 (19)	0.006 (2)
O15	0.021 (2)	0.028 (3)	0.023 (3)	−0.002 (2)	−0.006 (2)	−0.002 (2)
O16	0.036 (3)	0.031 (3)	0.042 (3)	−0.012 (2)	−0.023 (3)	0.000 (3)
N1	0.022 (3)	0.019 (3)	0.015 (3)	−0.002 (2)	−0.006 (2)	−0.002 (3)
N2	0.019 (3)	0.015 (3)	0.027 (3)	0.001 (2)	−0.010 (3)	−0.006 (3)
N3	0.020 (3)	0.013 (3)	0.021 (3)	−0.001 (2)	−0.011 (2)	0.003 (3)
N4	0.027 (3)	0.026 (3)	0.024 (3)	−0.010 (3)	−0.007 (3)	0.001 (3)
N5	0.029 (3)	0.034 (4)	0.019 (3)	0.002 (3)	−0.012 (3)	0.004 (3)
C1	0.022 (3)	0.026 (4)	0.034 (4)	0.004 (3)	−0.006 (3)	−0.006 (4)
C2	0.026 (3)	0.020 (4)	0.014 (3)	−0.005 (3)	−0.005 (3)	0.010 (3)
C3	0.029 (4)	0.032 (5)	0.027 (4)	0.006 (3)	−0.013 (3)	0.005 (4)
C4	0.018 (3)	0.026 (4)	0.029 (4)	−0.001 (3)	−0.001 (3)	0.006 (3)
C5	0.020 (3)	0.027 (4)	0.020 (4)	0.003 (3)	−0.005 (3)	0.006 (3)
C6	0.020 (4)	0.042 (5)	0.042 (5)	−0.001 (3)	−0.006 (4)	0.000 (4)
C7	0.027 (4)	0.020 (4)	0.023 (4)	−0.009 (3)	−0.008 (3)	0.012 (3)
C8	0.018 (3)	0.015 (3)	0.027 (4)	0.000 (3)	−0.009 (3)	0.001 (3)
C9	0.020 (3)	0.018 (4)	0.023 (4)	0.000 (3)	−0.008 (3)	−0.005 (3)
C10	0.020 (3)	0.018 (4)	0.015 (3)	−0.003 (3)	−0.007 (3)	0.001 (3)
C11	0.021 (3)	0.022 (4)	0.022 (4)	0.003 (3)	−0.009 (3)	−0.005 (3)
C12	0.022 (3)	0.022 (4)	0.024 (4)	0.000 (3)	−0.011 (3)	−0.008 (3)
C13	0.029 (4)	0.031 (5)	0.040 (5)	−0.008 (3)	−0.013 (4)	−0.011 (4)
C14	0.033 (4)	0.046 (5)	0.031 (4)	−0.021 (4)	0.002 (4)	0.004 (4)
C15	0.031 (4)	0.054 (6)	0.038 (5)	0.010 (4)	−0.009 (4)	−0.001 (5)

Geometric parameters (Å, º) top

Cu—O14	1.925 (4)	N2—C10	1.367 (8)
Cu—O16	2.604 (4)	N3—C1	1.343 (10)
Cu—N1	1.985 (6)	N3—C9	1.373 (8)
Cu—N2	1.989 (6)	N4—C13	1.329 (8)
Cu—N3	1.990 (6)	N4—C15	1.447 (10)
Mo1—O1	1.705 (5)	N4—C14	1.462 (9)
Mo1—O6	1.720 (4)	N5—HN1	0.8954
Mo1—O11	1.896 (4)	N5—HN2	0.9477
Mo1—O10	1.995 (5)	N5—HN3	0.9466
Mo1—O12	2.306 (4)	N5—HN4	0.9785
Mo1—O7ⁱ	2.356 (5)	C1—C2	1.384 (10)
Mo1—Mo3	3.2161 (10)	C1—H1	0.9300
Mo2—O8	1.699 (4)	C2—C3	1.395 (9)
Mo2—O2	1.722 (5)	C2—H2	0.9300
Mo2—O9	1.897 (4)	C3—C4	1.370 (11)
Mo2—O7ⁱ	1.998 (5)	C3—H3	0.9300
Mo2—O10	2.340 (4)	C4—C9	1.390 (9)
Mo2—O12ⁱ	2.346 (4)	C4—H4	0.9300
Mo3—O4	1.696 (5)	C5—C6	1.361 (12)
Mo3—O5	1.756 (5)	C5—C10	1.405 (9)
Mo3—O10	1.960 (4)	C5—H5	0.9300
Mo3—O7	1.967 (4)	C6—C7	1.383 (10)
Mo3—O12	2.143 (4)	C6—H6	0.9300
Mo3—O12ⁱ	2.380 (4)	C7—C8	1.395 (9)
Mo4—O13	1.693 (4)	C7—H7	0.9300
Mo4—O3	1.716 (5)	C8—H8	0.9300
Mo4—O9ⁱ	1.921 (4)	C9—C10	1.446 (10)
Mo4—O11	1.945 (4)	C11—C12	1.508 (10)
Mo4—O5ⁱ	2.257 (5)	C11—H11A	0.9700
Mo4—O12	2.491 (4)	C11—H11B	0.9700
O14—C12	1.307 (7)	C13—H14	0.9300
O15—C12	1.242 (8)	C14—H14A	0.9600
O16—C13	1.239 (10)	C14—H14B	0.9600
N1—C11	1.488 (8)	C14—H14C	0.9600
N1—H1A	0.9000	C15—H15A	0.9600
N1—H1B	0.9000	C15—H15B	0.9600
N2—C8	1.342 (9)	C15—H15C	0.9600

O14—Cu—N1	85.8 (2)	Mo3—O12—Mo1	92.51 (14)
O14—Cu—N2	174.4 (2)	Mo3—O12—Mo2ⁱ	91.87 (13)
N1—Cu—N2	99.6 (2)	Mo1—O12—Mo2ⁱ	163.2 (2)
O14—Cu—N3	93.0 (2)	Mo3—O12—Mo3ⁱ	104.57 (19)
N1—Cu—N3	177.5 (2)	Mo1—O12—Mo3ⁱ	97.46 (14)
N2—Cu—N3	81.7 (2)	Mo2ⁱ—O12—Mo3ⁱ	97.08 (14)
O1—Mo1—O6	104.5 (2)	Mo3—O12—Mo4	164.8 (2)
O1—Mo1—O11	101.9 (2)	Mo1—O12—Mo4	86.10 (14)
O6—Mo1—O11	100.25 (19)	Mo2ⁱ—O12—Mo4	85.44 (13)
O1—Mo1—O10	96.6 (2)	Mo3ⁱ—O12—Mo4	90.65 (12)
O6—Mo1—O10	100.2 (2)	C12—O14—Cu	114.8 (5)
O11—Mo1—O10	147.87 (18)	C11—N1—Cu	110.1 (4)
O1—Mo1—O12	94.64 (17)	C11—N1—H1A	109.6
O6—Mo1—O12	160.6 (2)	Cu—N1—H1A	109.6
O11—Mo1—O12	78.82 (16)	C11—N1—H1B	109.6
O10—Mo1—O12	73.67 (15)	Cu—N1—H1B	109.6
O1—Mo1—O7ⁱ	164.75 (17)	H1A—N1—H1B	108.2
O6—Mo1—O7ⁱ	87.88 (19)	C8—N2—C10	119.9 (6)
O11—Mo1—O7ⁱ	84.26 (18)	C8—N2—Cu	125.9 (4)
O10—Mo1—O7ⁱ	72.04 (16)	C10—N2—Cu	113.9 (5)
O12—Mo1—O7ⁱ	72.68 (15)	C1—N3—C9	119.0 (6)
O1—Mo1—Mo3	85.12 (15)	C1—N3—Cu	126.7 (4)
O6—Mo1—Mo3	135.43 (17)	C9—N3—Cu	114.4 (5)
O11—Mo1—Mo3	120.55 (12)	C13—N4—C15	123.2 (7)
O10—Mo1—Mo3	35.24 (11)	C13—N4—C14	119.4 (7)
O12—Mo1—Mo3	41.75 (10)	C15—N4—C14	117.1 (6)
O7ⁱ—Mo1—Mo3	79.76 (10)	HN1—N5—HN2	92.1
O8—Mo2—O2	105.0 (2)	HN1—N5—HN3	117.9
O8—Mo2—O9	101.5 (2)	HN2—N5—HN3	117.0
O2—Mo2—O9	101.2 (2)	HN1—N5—HN4	125.0
O8—Mo2—O7ⁱ	100.7 (2)	HN2—N5—HN4	116.8
O2—Mo2—O7ⁱ	96.4 (2)	HN3—N5—HN4	90.7
O9—Mo2—O7ⁱ	146.90 (17)	N3—C1—C2	122.9 (7)
O8—Mo2—O10	89.67 (19)	N3—C1—H1	118.5
O2—Mo2—O10	163.20 (16)	C2—C1—H1	118.5
O9—Mo2—O10	83.47 (18)	C1—C2—C3	118.1 (7)
O7ⁱ—Mo2—O10	72.36 (16)	C1—C2—H2	121.0
O8—Mo2—O12ⁱ	161.3 (2)	C3—C2—H2	121.0
O2—Mo2—O12ⁱ	93.45 (17)	C4—C3—C2	119.5 (7)
O9—Mo2—O12ⁱ	77.44 (15)	C4—C3—H3	120.2
O7ⁱ—Mo2—O12ⁱ	73.72 (15)	C2—C3—H3	120.2
O10—Mo2—O12ⁱ	71.65 (15)	C3—C4—C9	120.4 (7)
O4—Mo3—O5	104.9 (2)	C3—C4—H4	119.8
O4—Mo3—O10	100.12 (19)	C9—C4—H4	119.8
O5—Mo3—O10	96.24 (19)	C6—C5—C10	118.9 (7)
O4—Mo3—O7	102.04 (19)	C6—C5—H5	120.5
O5—Mo3—O7	96.87 (19)	C10—C5—H5	120.5
O10—Mo3—O7	150.32 (16)	C5—C6—C7	121.9 (7)
O4—Mo3—O12	98.9 (2)	C5—C6—H6	119.1
O5—Mo3—O12	156.13 (19)	C7—C6—H6	119.1
O10—Mo3—O12	78.15 (16)	C6—C7—C8	117.0 (7)
O7—Mo3—O12	79.11 (16)	C6—C7—H7	121.5
O4—Mo3—O12ⁱ	174.24 (19)	C8—C7—H7	121.5
O5—Mo3—O12ⁱ	80.71 (18)	N2—C8—C7	122.5 (6)
O10—Mo3—O12ⁱ	77.72 (16)	N2—C8—H8	118.8
O7—Mo3—O12ⁱ	78.29 (15)	C7—C8—H8	118.8
O12—Mo3—O12ⁱ	75.43 (19)	N3—C9—C4	120.1 (7)
O4—Mo3—Mo1	89.45 (15)	N3—C9—C10	114.3 (6)
O5—Mo3—Mo1	132.20 (13)	C4—C9—C10	125.5 (6)
O10—Mo3—Mo1	35.97 (13)	N2—C10—C5	119.9 (7)
O7—Mo3—Mo1	124.84 (12)	N2—C10—C9	115.5 (6)
O12—Mo3—Mo1	45.74 (10)	C5—C10—C9	124.6 (6)
O12ⁱ—Mo3—Mo1	85.72 (10)	N1—C11—C12	110.5 (5)
O13—Mo4—O3	105.1 (2)	N1—C11—H11A	109.6
O13—Mo4—O9ⁱ	103.1 (2)	C12—C11—H11A	109.6
O3—Mo4—O9ⁱ	97.9 (2)	N1—C11—H11B	109.6
O13—Mo4—O11	104.12 (19)	C12—C11—H11B	109.6
O3—Mo4—O11	97.0 (2)	H11A—C11—H11B	108.1
O9ⁱ—Mo4—O11	144.2 (2)	O15—C12—O14	122.6 (7)
O13—Mo4—O5ⁱ	91.8 (2)	O15—C12—C11	119.1 (6)
O3—Mo4—O5ⁱ	163.15 (19)	O14—C12—C11	118.2 (6)
O9ⁱ—Mo4—O5ⁱ	77.85 (18)	O16—C13—N4	126.8 (8)
O11—Mo4—O5ⁱ	78.55 (18)	O16—C13—H14	116.6
O13—Mo4—O12	161.5 (2)	N4—C13—H14	116.6
O3—Mo4—O12	93.44 (18)	N4—C14—H14A	109.5
O9ⁱ—Mo4—O12	73.45 (16)	N4—C14—H14B	109.5
O11—Mo4—O12	73.35 (15)	H14A—C14—H14B	109.5
O5ⁱ—Mo4—O12	69.71 (15)	N4—C14—H14C	109.5
Mo3—O5—Mo4ⁱ	118.9 (2)	H14A—C14—H14C	109.5
Mo3—O7—Mo2ⁱ	109.0 (2)	H14B—C14—H14C	109.5
Mo3—O7—Mo1ⁱ	108.78 (19)	N4—C15—H15A	109.5
Mo2ⁱ—O7—Mo1ⁱ	103.33 (16)	N4—C15—H15B	109.5
Mo2—O9—Mo4ⁱ	118.6 (2)	H15A—C15—H15B	109.5
Mo3—O10—Mo1	108.8 (2)	N4—C15—H15C	109.5
Mo3—O10—Mo2	110.6 (2)	H15A—C15—H15C	109.5
Mo1—O10—Mo2	104.01 (16)	H15B—C15—H15C	109.5
Mo1—O11—Mo4	117.12 (19)

O1—Mo1—Mo3—O4	−0.51 (19)	O5—Mo3—O12—Mo2ⁱ	99.5 (4)
O6—Mo1—Mo3—O4	105.2 (3)	O10—Mo3—O12—Mo2ⁱ	178.02 (19)
O11—Mo1—Mo3—O4	−101.5 (2)	O7—Mo3—O12—Mo2ⁱ	17.22 (17)
O10—Mo1—Mo3—O4	108.2 (3)	O12ⁱ—Mo3—O12—Mo2ⁱ	97.81 (17)
O12—Mo1—Mo3—O4	−103.1 (2)	Mo1—Mo3—O12—Mo2ⁱ	−163.8 (2)
O7ⁱ—Mo1—Mo3—O4	−178.49 (17)	O4—Mo3—O12—Mo3ⁱ	178.77 (16)
O1—Mo1—Mo3—O5	−110.3 (3)	O5—Mo3—O12—Mo3ⁱ	1.7 (5)
O6—Mo1—Mo3—O5	−4.6 (3)	O10—Mo3—O12—Mo3ⁱ	80.22 (17)
O11—Mo1—Mo3—O5	148.8 (3)	O7—Mo3—O12—Mo3ⁱ	−80.58 (18)
O10—Mo1—Mo3—O5	−1.6 (3)	O12ⁱ—Mo3—O12—Mo3ⁱ	0.0
O12—Mo1—Mo3—O5	147.1 (3)	Mo1—Mo3—O12—Mo3ⁱ	98.37 (17)
O7ⁱ—Mo1—Mo3—O5	71.7 (2)	O4—Mo3—O12—Mo4	−4.0 (7)
O1—Mo1—Mo3—O10	−108.7 (3)	O5—Mo3—O12—Mo4	179.0 (5)
O6—Mo1—Mo3—O10	−3.0 (3)	O10—Mo3—O12—Mo4	−102.5 (7)
O11—Mo1—Mo3—O10	150.3 (3)	O7—Mo3—O12—Mo4	96.7 (7)
O12—Mo1—Mo3—O10	148.7 (3)	O12ⁱ—Mo3—O12—Mo4	177.3 (7)
O7ⁱ—Mo1—Mo3—O10	73.3 (2)	Mo1—Mo3—O12—Mo4	−84.4 (7)
O1—Mo1—Mo3—O7	103.8 (2)	O1—Mo1—O12—Mo3	−77.3 (2)
O6—Mo1—Mo3—O7	−150.5 (3)	O6—Mo1—O12—Mo3	92.3 (5)
O11—Mo1—Mo3—O7	2.9 (2)	O11—Mo1—O12—Mo3	−178.6 (2)
O10—Mo1—Mo3—O7	−147.5 (3)	O10—Mo1—O12—Mo3	18.19 (16)
O12—Mo1—Mo3—O7	1.2 (2)	O7ⁱ—Mo1—O12—Mo3	94.00 (18)
O7ⁱ—Mo1—Mo3—O7	−74.2 (2)	O1—Mo1—O12—Mo2ⁱ	27.7 (6)
O1—Mo1—Mo3—O12	102.6 (2)	O6—Mo1—O12—Mo2ⁱ	−162.7 (6)
O6—Mo1—Mo3—O12	−151.7 (3)	O11—Mo1—O12—Mo2ⁱ	−73.6 (6)
O11—Mo1—Mo3—O12	1.6 (2)	O10—Mo1—O12—Mo2ⁱ	123.2 (6)
O10—Mo1—Mo3—O12	−148.7 (3)	O7ⁱ—Mo1—O12—Mo2ⁱ	−161.0 (6)
O7ⁱ—Mo1—Mo3—O12	−75.4 (2)	Mo3—Mo1—O12—Mo2ⁱ	105.0 (6)
O1—Mo1—Mo3—O12ⁱ	176.35 (17)	O1—Mo1—O12—Mo3ⁱ	177.61 (19)
O6—Mo1—Mo3—O12ⁱ	−77.9 (2)	O6—Mo1—O12—Mo3ⁱ	−12.8 (6)
O11—Mo1—Mo3—O12ⁱ	75.39 (19)	O11—Mo1—O12—Mo3ⁱ	76.36 (18)
O10—Mo1—Mo3—O12ⁱ	−74.9 (2)	O10—Mo1—O12—Mo3ⁱ	−86.86 (18)
O12—Mo1—Mo3—O12ⁱ	73.8 (2)	O7ⁱ—Mo1—O12—Mo3ⁱ	−11.05 (14)
O7ⁱ—Mo1—Mo3—O12ⁱ	−1.63 (13)	Mo3—Mo1—O12—Mo3ⁱ	−105.0 (2)
O4—Mo3—O5—Mo4ⁱ	−178.66 (19)	O1—Mo1—O12—Mo4	87.46 (19)
O10—Mo3—O5—Mo4ⁱ	−76.4 (2)	O6—Mo1—O12—Mo4	−102.9 (6)
O7—Mo3—O5—Mo4ⁱ	76.9 (2)	O11—Mo1—O12—Mo4	−13.79 (16)
O12—Mo3—O5—Mo4ⁱ	−1.7 (5)	O10—Mo1—O12—Mo4	−177.01 (17)
O12ⁱ—Mo3—O5—Mo4ⁱ	0.01 (18)	O7ⁱ—Mo1—O12—Mo4	−101.20 (14)
Mo1—Mo3—O5—Mo4ⁱ	−75.5 (3)	Mo3—Mo1—O12—Mo4	164.8 (2)
O4—Mo3—O7—Mo2ⁱ	75.4 (2)	O13—Mo4—O12—Mo3	−176.3 (6)
O5—Mo3—O7—Mo2ⁱ	−177.7 (2)	O3—Mo4—O12—Mo3	2.7 (7)
O10—Mo3—O7—Mo2ⁱ	−62.1 (5)	O9ⁱ—Mo4—O12—Mo3	−94.5 (7)
O12—Mo3—O7—Mo2ⁱ	−21.57 (19)	O11—Mo4—O12—Mo3	99.0 (7)
O12ⁱ—Mo3—O7—Mo2ⁱ	−98.76 (19)	O5ⁱ—Mo4—O12—Mo3	−177.4 (7)
Mo1—Mo3—O7—Mo2ⁱ	−22.5 (3)	O13—Mo4—O12—Mo1	98.5 (5)
O4—Mo3—O7—Mo1ⁱ	−172.6 (2)	O3—Mo4—O12—Mo1	−82.48 (18)
O5—Mo3—O7—Mo1ⁱ	−65.7 (2)	O9ⁱ—Mo4—O12—Mo1	−179.72 (18)
O10—Mo3—O7—Mo1ⁱ	49.9 (5)	O11—Mo4—O12—Mo1	13.75 (16)
O12—Mo3—O7—Mo1ⁱ	90.45 (19)	O5ⁱ—Mo4—O12—Mo1	97.42 (15)
O12ⁱ—Mo3—O7—Mo1ⁱ	13.26 (16)	O13—Mo4—O12—Mo2ⁱ	−96.0 (5)
Mo1—Mo3—O7—Mo1ⁱ	89.5 (2)	O3—Mo4—O12—Mo2ⁱ	83.04 (17)
O8—Mo2—O9—Mo4ⁱ	−178.0 (3)	O9ⁱ—Mo4—O12—Mo2ⁱ	−14.19 (16)
O2—Mo2—O9—Mo4ⁱ	−70.0 (3)	O11—Mo4—O12—Mo2ⁱ	179.28 (19)
O7ⁱ—Mo2—O9—Mo4ⁱ	50.9 (5)	O5ⁱ—Mo4—O12—Mo2ⁱ	−97.06 (15)
O10—Mo2—O9—Mo4ⁱ	93.6 (3)	O13—Mo4—O12—Mo3ⁱ	1.1 (6)
O12ⁱ—Mo2—O9—Mo4ⁱ	21.0 (3)	O3—Mo4—O12—Mo3ⁱ	−179.91 (16)
O4—Mo3—O10—Mo1	−74.8 (2)	O9ⁱ—Mo4—O12—Mo3ⁱ	82.86 (17)
O5—Mo3—O10—Mo1	178.8 (2)	O11—Mo4—O12—Mo3ⁱ	−83.68 (17)
O7—Mo3—O10—Mo1	63.0 (5)	O5ⁱ—Mo4—O12—Mo3ⁱ	−0.01 (12)
O12—Mo3—O10—Mo1	22.3 (2)	N1—Cu—O14—C12	2.2 (4)
O12ⁱ—Mo3—O10—Mo1	99.8 (2)	N3—Cu—O14—C12	−175.7 (4)
O4—Mo3—O10—Mo2	171.6 (2)	O14—Cu—N1—C11	−5.8 (4)
O5—Mo3—O10—Mo2	65.2 (2)	N2—Cu—N1—C11	175.4 (4)
O7—Mo3—O10—Mo2	−50.6 (5)	N1—Cu—N2—C8	4.3 (5)
O12—Mo3—O10—Mo2	−91.3 (2)	N3—Cu—N2—C8	−177.9 (5)
O12ⁱ—Mo3—O10—Mo2	−13.88 (16)	N1—Cu—N2—C10	178.2 (4)
Mo1—Mo3—O10—Mo2	−113.7 (2)	N3—Cu—N2—C10	−3.9 (4)
O1—Mo1—O10—Mo3	71.8 (2)	O14—Cu—N3—C1	2.1 (5)
O6—Mo1—O10—Mo3	177.9 (2)	N2—Cu—N3—C1	−179.3 (5)
O11—Mo1—O10—Mo3	−53.3 (4)	O14—Cu—N3—C9	−176.9 (4)
O12—Mo1—O10—Mo3	−21.12 (18)	N2—Cu—N3—C9	1.7 (4)
O7ⁱ—Mo1—O10—Mo3	−97.8 (2)	C9—N3—C1—C2	−0.6 (9)
O1—Mo1—O10—Mo2	−170.27 (17)	Cu—N3—C1—C2	−179.6 (4)
O6—Mo1—O10—Mo2	−64.2 (2)	N3—C1—C2—C3	−0.4 (10)
O11—Mo1—O10—Mo2	64.6 (4)	C1—C2—C3—C4	2.0 (10)
O12—Mo1—O10—Mo2	96.81 (17)	C2—C3—C4—C9	−2.6 (10)
O7ⁱ—Mo1—O10—Mo2	20.18 (13)	C10—C5—C6—C7	0.5 (11)
Mo3—Mo1—O10—Mo2	117.9 (3)	C5—C6—C7—C8	0.7 (10)
O8—Mo2—O10—Mo3	−166.0 (2)	C10—N2—C8—C7	0.5 (9)
O2—Mo2—O10—Mo3	43.0 (7)	Cu—N2—C8—C7	174.1 (4)
O9—Mo2—O10—Mo3	−64.4 (2)	C6—C7—C8—N2	−1.2 (9)
O7ⁱ—Mo2—O10—Mo3	92.7 (2)	C1—N3—C9—C4	0.0 (8)
O12ⁱ—Mo2—O10—Mo3	14.51 (17)	Cu—N3—C9—C4	179.1 (4)
O8—Mo2—O10—Mo1	77.4 (2)	C1—N3—C9—C10	−178.5 (5)
O2—Mo2—O10—Mo1	−73.7 (7)	Cu—N3—C9—C10	0.6 (6)
O9—Mo2—O10—Mo1	178.95 (18)	C3—C4—C9—N3	1.6 (9)
O7ⁱ—Mo2—O10—Mo1	−23.95 (16)	C3—C4—C9—C10	179.9 (6)
O12ⁱ—Mo2—O10—Mo1	−102.15 (17)	C8—N2—C10—C5	0.8 (8)
O1—Mo1—O11—Mo4	−72.4 (3)	Cu—N2—C10—C5	−173.6 (4)
O6—Mo1—O11—Mo4	−179.8 (3)	C8—N2—C10—C9	179.7 (5)
O10—Mo1—O11—Mo4	51.4 (5)	Cu—N2—C10—C9	5.4 (6)
O12—Mo1—O11—Mo4	20.0 (2)	C6—C5—C10—N2	−1.3 (9)
O7ⁱ—Mo1—O11—Mo4	93.4 (3)	C6—C5—C10—C9	179.9 (6)
Mo3—Mo1—O11—Mo4	18.9 (3)	N3—C9—C10—N2	−4.0 (7)
O13—Mo4—O11—Mo1	−179.9 (3)	C4—C9—C10—N2	177.7 (5)
O3—Mo4—O11—Mo1	72.6 (3)	N3—C9—C10—C5	174.9 (5)
O9ⁱ—Mo4—O11—Mo1	−41.4 (4)	C4—C9—C10—C5	−3.4 (10)
O5ⁱ—Mo4—O11—Mo1	−90.9 (3)	Cu—N1—C11—C12	8.0 (6)
O12—Mo4—O11—Mo1	−18.9 (2)	Cu—O14—C12—O15	−179.6 (4)
O4—Mo3—O12—Mo1	80.40 (18)	Cu—O14—C12—C11	2.2 (7)
O5—Mo3—O12—Mo1	−96.6 (4)	N1—C11—C12—O15	174.8 (5)
O10—Mo3—O12—Mo1	−18.16 (17)	N1—C11—C12—O14	−6.9 (8)
O7—Mo3—O12—Mo1	−178.96 (19)	C15—N4—C13—O16	178.7 (7)
O12ⁱ—Mo3—O12—Mo1	−98.37 (16)	C14—N4—C13—O16	5.2 (10)
O4—Mo3—O12—Mo2ⁱ	−83.42 (18)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3ⁱⁱ	0.90	2.32	3.093 (7)	144
N1—H1B···O6	0.90	2.01	2.863 (6)	158
N5—HN1···O1	0.90	2.10	2.888 (7)	146
N5—HN2···O4	0.95	2.13	3.028 (8)	158
N5—HN3···O15ⁱⁱⁱ	0.95	1.94	2.761 (8)	143
N5—HN4···O14ⁱⁱⁱ	0.98	2.26	3.132 (7)	148

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

Experimental details

Crystal data
Chemical formula	(NH₄)₂[Cu(C₂H₄NO₂)(C₁₀H₈N₂)(C₃H₇NO)]₂[Mo₈O₂₆]
M_r	1953.38
Crystal system, space group	Triclinic, P1
Temperature (K)	291
a, b, c (Å)	10.222 (2), 10.849 (2), 13.020 (3)
α, β, γ (°)	81.82 (3), 69.91 (2), 81.61 (3)
V (Å³)	1334.9 (5)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.70
Crystal size (mm)	0.28 × 0.20 × 0.14

Data collection
Diffractometer	Bruker SMART APEXII diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.530, 0.690
No. of measured, independent and observed [I > 2σ(I)] reflections	10864, 4889, 3591
R_int	0.071
(sin θ/λ)_max (Å⁻¹)	0.607

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.046, 0.110, 0.99
No. of reflections	4889
No. of parameters	370
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.86, −0.83

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT (Bruker, 2004, SHELXTL (Bruker, 1997), SHELXTL (Bruker, 1997, DIAMOND (Brandenburg, 1999).

Selected bond lengths (Å) top

Cu—O14	1.925 (4)	Mo2—O10	2.340 (4)
Cu—O16	2.604 (4)	Mo2—O12ⁱ	2.346 (4)
Cu—N1	1.985 (6)	Mo3—O4	1.696 (5)
Cu—N2	1.989 (6)	Mo3—O5	1.756 (5)
Cu—N3	1.990 (6)	Mo3—O10	1.960 (4)
Mo1—O1	1.705 (5)	Mo3—O7	1.967 (4)
Mo1—O6	1.720 (4)	Mo3—O12	2.143 (4)
Mo1—O11	1.896 (4)	Mo3—O12ⁱ	2.380 (4)
Mo1—O10	1.995 (5)	Mo4—O13	1.693 (4)
Mo1—O12	2.306 (4)	Mo4—O3	1.716 (5)
Mo1—O7ⁱ	2.356 (5)	Mo4—O9ⁱ	1.921 (4)
Mo2—O8	1.699 (4)	Mo4—O11	1.945 (4)
Mo2—O2	1.722 (5)	Mo4—O5ⁱ	2.257 (5)
Mo2—O9	1.897 (4)	Mo4—O12	2.491 (4)
Mo2—O7ⁱ	1.998 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3ⁱⁱ	0.90	2.32	3.093 (7)	144
N1—H1B···O6	0.90	2.01	2.863 (6)	158
N5—HN1···O1	0.90	2.10	2.888 (7)	146
N5—HN2···O4	0.95	2.13	3.028 (8)	158
N5—HN3···O15ⁱⁱⁱ	0.95	1.94	2.761 (8)	143
N5—HN4···O14ⁱⁱⁱ	0.98	2.26	3.132 (7)	148

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

Acknowledgements

This work was supported financially by the Natural Science Foundation of Heilong Jiang Province (grant No. 20083145).

References

Allis, D. G., Rarig, R. S., Burkholder, E. & Zubieta, J. (2004). J. Mol. Struct. 688, 11–31. Web of Science CSD CrossRef CAS Google Scholar
Brandenburg, K. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247. CrossRef CAS Web of Science IUCr Journals Google Scholar
Bruker (1997). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar

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