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ISSN: 2056-9890

Tetra­imidazolium hexa-μ4-oxido-dodeca-μ2-oxido-dodeca­oxidohexa­arsenate(III)hexa­molybdenum(VI)cuprate(II)

aCollege of Chemistry and Chemical Engineering, Harbin Normal University, Harbin, People's Republic of China, and bDepartment of Safety and Environmental Engineering, Jixi University, Jixi, People's Republic of China
*Correspondence e-mail: su_zhan_hua@yahoo.com

(Received 3 September 2010; accepted 18 September 2010; online 30 September 2010)

The title compound, (C3H5N2)4[As6CuMo6O30], is made up of a centrosymmetric anionic cluster and four imidazolium cations. In the cluster, the central CuII atom is six-coordinated and lies on an inversion center. Adjacent clusters are linked via N—H⋯O hydrogen bonds between the imidazole cations and polyoxidoanions into a three-dimensional supra­molecular architecture.

Related literature

For general background to polyoxidometalates, see: Müller et al. (1998[Müller, A., Peters, F., Pope, M. T. & Gatteschi, D. (1998). Chem. Rev. 98, 239-271.]). For general background to molybdoarsenates, see: Fidalgo et al. (2002[Fidalgo, E. G., Neels, A., Stoeckli-Evans, H. & Süss-Fink, G. (2002). Polyhedron, 21, 1921-1928.]); Sun et al. (2007[Sun, C.-Y., Li, Y.-G., Wang, E.-B., Xiao, D.-R., An, H.-Y. & Xu, L. (2007). Inorg. Chem. 46, 1563-1574.]).

[Scheme 1]

Experimental

Crystal data
  • (C3H5N2)4[As6CuMo6O30]

  • Mr = 1845.07

  • Monoclinic, P 21 /c

  • a = 10.5696 (7) Å

  • b = 19.2842 (12) Å

  • c = 10.4678 (7) Å

  • β = 106.747 (1)°

  • V = 2043.1 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 7.22 mm−1

  • T = 298 K

  • 0.28 × 0.25 × 0.20 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.237, Tmax = 0.326

  • 12666 measured reflections

  • 4906 independent reflections

  • 4057 reflections with I > 2σ(I)

  • Rint = 0.029

Refinement
  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 0.073

  • S = 1.03

  • 4906 reflections

  • 286 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 0.56 e Å−3

  • Δρmin = −1.94 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N1—H1A⋯O4i 0.86 1.81 2.664 (5) 173
N2—H2A⋯O3 0.86 1.99 2.748 (5) 146
N2—H2A⋯O9ii 0.86 2.42 3.020 (5) 127
N3—H3A⋯O7ii 0.86 2.09 2.867 (6) 150
N4—H4A⋯O2iii 0.86 2.00 2.834 (6) 165
Symmetry codes: (i) [x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (ii) x-1, y, z; (iii) x, y, z+1.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Polyoxometalates have unusual structural chemistry and properties that make them attractive for applications in materials science, electrochemical, catalysis and photochemical (Müller et al., 1998). Molybdenum arsenates are an important part in this field. So far the reports on molybdenum arsenates have been mainly concentrated on several discrete molybdenum arsenate clusters (Fidalgo et al., 2002; Sun et al., 2007). Therefore, further research is necessary to enrich and develop this branch. We try to obtain new materials based on inorganic molybdenum arsenate with novel structures. Here, the synthesis and crystal structure of the title compound is reported.

The structure of the title compound is shown in Fig. 1. The asymmetric unit consists of two protonated imidazole cations and a half cluster anion. The anion is centrosymmetric with the CuII atom lying on an inversion center. The cluster is derived from the A-type Anderson anion, in which a central CuO6 octahedron is coordinated with six MoO6 octahedra hexagonally arranged by sharing their edges in a plane. Two cyclic As3O3 trimers are capped on the opposite faces of the Anderson-type anion plane. The four free protonated imidazole molecules act as charge compensating cations. The adjacent clusters are linked via N—H···O hydrogen bonds between the imidazole cations and polyoxoanions into a three-dimensional supramolecular architecture (Table 1).

Related literature top

For general background to polyoxometalates, see: Müller et al. (1998). For general background to molybdenum arsenates, see: Fidalgo et al. (2002); Sun et al. (2007).

Experimental top

A mixture of hexaammonium heptamolybdate tetrahydrate (1.11 g, 0.89 mmol), sodium arsenite (0.41 g, 3.03 mmol), cupric chloride (0.20 g, 1.17 mmol), imidazole (0.27 g, 4.01 mmol) and water (20 ml) was placed in a 30 ml Teflon-lined Parr bomb. The bomb was heated to 413 K for 5 d. Blue block shaped crystals were isolated from the cooled solution in a 72% yield based on Mo. Analysis, calculated for C12H20As6CuMo6N8O30: C 7.81, H 1.09, N 6.07%; found: C 7.83, H 1.13, N 6.04%.

Refinement top

H atoms were positioned geometrically and refined using a riding model, with C—H = 0.93 and N—H = 0.86 Å, and with Uiso(H) = 1.2Ueq(C, N).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted. [Symmetry code: (i) 2-x, -y, -z.]
Tetraimidazolium hexa-µ4-oxido-dodeca-µ2-oxido- dodecaoxidohexaarsenate(III)hexamolybdenum(VI)cuprate(II) top
Crystal data top
(C3H5N2)4[As6CuMo6O30]F(000) = 1734
Mr = 1845.07Dx = 2.999 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4555 reflections
a = 10.5696 (7) Åθ = 2.3–28.1°
b = 19.2842 (12) ŵ = 7.22 mm1
c = 10.4678 (7) ÅT = 298 K
β = 106.747 (1)°Block, blue
V = 2043.1 (2) Å30.28 × 0.25 × 0.20 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer
4906 independent reflections
Radiation source: fine-focus sealed tube4057 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
ϕ and ω scansθmax = 28.3°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1314
Tmin = 0.237, Tmax = 0.326k = 2519
12666 measured reflectionsl = 1313
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0338P)2 + 2.1525P]
where P = (Fo2 + 2Fc2)/3
4906 reflections(Δ/σ)max = 0.001
286 parametersΔρmax = 0.56 e Å3
1 restraintΔρmin = 1.94 e Å3
Crystal data top
(C3H5N2)4[As6CuMo6O30]V = 2043.1 (2) Å3
Mr = 1845.07Z = 2
Monoclinic, P21/cMo Kα radiation
a = 10.5696 (7) ŵ = 7.22 mm1
b = 19.2842 (12) ÅT = 298 K
c = 10.4678 (7) Å0.28 × 0.25 × 0.20 mm
β = 106.747 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
4906 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
4057 reflections with I > 2σ(I)
Tmin = 0.237, Tmax = 0.326Rint = 0.029
12666 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0301 restraint
wR(F2) = 0.073H-atom parameters constrained
S = 1.03Δρmax = 0.56 e Å3
4906 reflectionsΔρmin = 1.94 e Å3
286 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.73132 (3)0.054936 (18)0.07751 (3)0.01939 (9)
Mo21.01930 (3)0.143475 (18)0.18894 (3)0.02087 (9)
Mo31.29116 (3)0.084229 (18)0.11868 (4)0.02065 (9)
Cu11.00000.00000.00000.02300 (16)
As11.03800 (5)0.16004 (2)0.13845 (4)0.02655 (11)
As20.75566 (4)0.08081 (2)0.24782 (4)0.02711 (11)
As30.98689 (4)0.02215 (2)0.32318 (4)0.02600 (11)
O10.7044 (3)0.04164 (14)0.0461 (3)0.0222 (6)
O20.5905 (3)0.09037 (16)0.0244 (3)0.0324 (7)
O30.7135 (3)0.05775 (16)0.2348 (3)0.0301 (7)
O40.8381 (3)0.13750 (14)0.0796 (3)0.0222 (6)
O50.9982 (3)0.14957 (17)0.3446 (3)0.0335 (7)
O61.0471 (3)0.22633 (16)0.1453 (3)0.0347 (7)
O71.1939 (3)0.10410 (15)0.2460 (3)0.0240 (6)
O81.3348 (3)0.16566 (16)0.0847 (3)0.0355 (8)
O91.4277 (3)0.05057 (17)0.2328 (3)0.0330 (7)
O101.0708 (3)0.10168 (14)0.0027 (3)0.0194 (6)
O110.8615 (3)0.15371 (15)0.1931 (3)0.0311 (7)
O120.8071 (3)0.02681 (14)0.1035 (3)0.0190 (6)
O130.9515 (3)0.02733 (14)0.1712 (3)0.0193 (6)
O140.9234 (3)0.10364 (16)0.2570 (3)0.0294 (7)
O151.1601 (3)0.03719 (17)0.3501 (3)0.0306 (7)
C10.7300 (6)0.1970 (3)0.4181 (6)0.0547 (16)
H10.81000.19110.39890.066*
C20.5755 (5)0.2391 (3)0.4939 (5)0.0402 (12)
H20.53010.26790.53690.048*
C30.5305 (6)0.1807 (3)0.4292 (6)0.0481 (14)
H30.44770.16100.41810.058*
C40.2581 (6)0.1681 (3)0.5787 (6)0.0498 (14)
H40.20560.20320.52970.060*
C50.3261 (7)0.1725 (4)0.7012 (7)0.072 (2)
H50.33260.21090.75650.087*
C60.3535 (7)0.0703 (4)0.6296 (9)0.072 (2)
H60.38150.02490.62540.086*
N10.6994 (4)0.2487 (2)0.4856 (5)0.0422 (11)
H1A0.75010.28310.51900.051*
N20.6282 (5)0.1554 (2)0.3826 (5)0.0511 (13)
H2A0.62400.11790.33690.061*
N30.2742 (4)0.1053 (3)0.5320 (5)0.0493 (12)
H3A0.23880.09060.45210.059*
N40.3864 (5)0.1108 (5)0.7346 (6)0.091 (3)
H4A0.43780.09980.81180.109*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01533 (17)0.02100 (17)0.02186 (18)0.00083 (13)0.00538 (13)0.00261 (13)
Mo20.01802 (18)0.02131 (18)0.02259 (18)0.00029 (14)0.00474 (14)0.00575 (13)
Mo30.01496 (17)0.02128 (18)0.02509 (19)0.00293 (13)0.00477 (14)0.00520 (13)
Cu10.0210 (4)0.0247 (4)0.0227 (4)0.0005 (3)0.0052 (3)0.0014 (3)
As10.0304 (3)0.0220 (2)0.0268 (2)0.00166 (18)0.00755 (19)0.00428 (17)
As20.0213 (2)0.0327 (2)0.0245 (2)0.00458 (18)0.00205 (18)0.00643 (18)
As30.0291 (2)0.0318 (2)0.0175 (2)0.00211 (19)0.00728 (18)0.00140 (17)
O10.0210 (15)0.0219 (14)0.0254 (15)0.0049 (12)0.0095 (12)0.0016 (11)
O20.0228 (16)0.0330 (18)0.0384 (18)0.0045 (13)0.0038 (14)0.0019 (14)
O30.0300 (17)0.0327 (17)0.0309 (17)0.0025 (14)0.0142 (14)0.0056 (13)
O40.0188 (14)0.0185 (14)0.0270 (15)0.0012 (11)0.0029 (12)0.0012 (11)
O50.0263 (17)0.046 (2)0.0284 (17)0.0003 (14)0.0087 (14)0.0085 (14)
O60.0355 (18)0.0233 (16)0.045 (2)0.0010 (14)0.0103 (15)0.0075 (14)
O70.0185 (14)0.0308 (16)0.0209 (14)0.0014 (12)0.0028 (11)0.0075 (12)
O80.0338 (18)0.0262 (16)0.050 (2)0.0092 (14)0.0182 (16)0.0082 (15)
O90.0175 (15)0.0403 (19)0.0362 (18)0.0017 (14)0.0005 (13)0.0076 (14)
O100.0177 (14)0.0203 (14)0.0196 (14)0.0009 (11)0.0046 (11)0.0005 (11)
O110.0302 (17)0.0274 (16)0.0338 (18)0.0048 (13)0.0063 (14)0.0065 (13)
O120.0150 (13)0.0215 (14)0.0190 (14)0.0002 (11)0.0028 (11)0.0025 (11)
O130.0185 (14)0.0213 (14)0.0178 (13)0.0018 (11)0.0049 (11)0.0000 (11)
O140.0324 (17)0.0286 (16)0.0296 (17)0.0015 (13)0.0126 (14)0.0037 (13)
O150.0294 (17)0.0382 (18)0.0213 (15)0.0017 (14)0.0028 (13)0.0038 (13)
C10.052 (4)0.047 (3)0.076 (4)0.002 (3)0.036 (3)0.008 (3)
C20.038 (3)0.036 (3)0.050 (3)0.000 (2)0.017 (2)0.010 (2)
C30.048 (3)0.048 (3)0.053 (3)0.021 (3)0.021 (3)0.017 (3)
C40.052 (4)0.044 (3)0.048 (3)0.011 (3)0.005 (3)0.010 (3)
C50.073 (5)0.084 (5)0.059 (4)0.036 (4)0.018 (4)0.023 (4)
C60.062 (5)0.054 (4)0.112 (7)0.019 (3)0.045 (5)0.049 (4)
N10.037 (2)0.028 (2)0.061 (3)0.0103 (18)0.014 (2)0.0152 (19)
N20.074 (4)0.032 (2)0.057 (3)0.012 (2)0.034 (3)0.019 (2)
N30.038 (3)0.055 (3)0.048 (3)0.009 (2)0.000 (2)0.004 (2)
N40.034 (3)0.190 (8)0.041 (3)0.001 (4)0.000 (3)0.060 (4)
Geometric parameters (Å, º) top
Mo1—O21.704 (3)As2—O111.785 (3)
Mo1—O31.711 (3)As2—O121.786 (3)
Mo1—O11.898 (3)As2—O15i1.788 (3)
Mo1—O41.948 (3)As3—O141.770 (3)
Mo1—O132.312 (3)As3—O151.793 (3)
Mo1—O122.324 (3)As3—O131.800 (3)
Mo2—O61.710 (3)C1—N21.308 (7)
Mo2—O51.711 (3)C1—N11.316 (7)
Mo2—O71.925 (3)C1—H10.9300
Mo2—O41.931 (3)C2—C31.329 (7)
Mo2—O102.315 (3)C2—N11.351 (6)
Mo2—O132.343 (3)C2—H20.9300
Mo3—O81.703 (3)C3—N21.354 (7)
Mo3—O91.714 (3)C3—H30.9300
Mo3—O1i1.923 (3)C4—C51.280 (9)
Mo3—O71.941 (3)C4—N31.334 (7)
Mo3—O102.320 (3)C4—H40.9300
Mo3—O12i2.365 (3)C5—N41.349 (10)
Cu1—O132.069 (3)C5—H50.9300
Cu1—O13i2.069 (3)C6—N31.308 (8)
Cu1—O122.080 (3)C6—N41.310 (10)
Cu1—O12i2.080 (3)C6—H60.9300
Cu1—O10i2.096 (3)N1—H1A0.8600
Cu1—O102.096 (3)N2—H2A0.8600
As1—O14i1.783 (3)N3—H3A0.8600
As1—O111.791 (3)N4—H4A0.8600
As1—O101.810 (3)
O2—Mo1—O3105.76 (15)O11—As1—O1098.94 (13)
O2—Mo1—O1102.98 (14)O11—As2—O12100.25 (13)
O3—Mo1—O198.34 (13)O11—As2—O15i100.87 (15)
O2—Mo1—O494.47 (13)O12—As2—O15i98.60 (13)
O3—Mo1—O4100.78 (13)O14—As3—O1599.93 (14)
O1—Mo1—O4149.46 (12)O14—As3—O1399.56 (13)
O2—Mo1—O13161.51 (13)O15—As3—O1399.65 (13)
O3—Mo1—O1388.59 (12)Mo1—O1—Mo3i122.20 (14)
O1—Mo1—O1385.98 (11)Mo2—O4—Mo1121.87 (14)
O4—Mo1—O1370.99 (10)Mo2—O7—Mo3121.00 (14)
O2—Mo1—O1291.53 (13)As1—O10—Cu1125.93 (14)
O3—Mo1—O12162.04 (13)As1—O10—Mo2115.77 (13)
O1—Mo1—O1272.51 (10)Cu1—O10—Mo299.64 (10)
O4—Mo1—O1282.27 (10)As1—O10—Mo3116.41 (13)
O13—Mo1—O1275.58 (9)Cu1—O10—Mo399.92 (11)
O6—Mo2—O5105.65 (16)Mo2—O10—Mo393.11 (9)
O6—Mo2—O7103.19 (14)As2—O11—As1130.91 (17)
O5—Mo2—O796.23 (14)As2—O12—Cu1126.82 (14)
O6—Mo2—O496.59 (13)As2—O12—Mo1117.47 (13)
O5—Mo2—O4100.89 (13)Cu1—O12—Mo198.60 (10)
O7—Mo2—O4149.22 (11)As2—O12—Mo3i116.78 (13)
O6—Mo2—O1090.01 (13)Cu1—O12—Mo3i98.95 (10)
O5—Mo2—O10162.31 (13)Mo1—O12—Mo3i91.05 (9)
O7—Mo2—O1071.73 (10)As3—O13—Cu1126.18 (14)
O4—Mo2—O1085.07 (11)As3—O13—Mo1115.12 (13)
O6—Mo2—O13160.76 (13)Cu1—O13—Mo199.30 (10)
O5—Mo2—O1391.16 (13)As3—O13—Mo2117.13 (13)
O7—Mo2—O1383.77 (11)Cu1—O13—Mo299.54 (11)
O4—Mo2—O1370.57 (10)Mo1—O13—Mo293.50 (10)
O10—Mo2—O1375.00 (9)As3—O14—As1i132.63 (17)
O8—Mo3—O9105.69 (16)As2i—O15—As3130.07 (17)
O8—Mo3—O1i97.38 (14)N2—C1—N1108.0 (5)
O9—Mo3—O1i103.31 (14)N2—C1—H1126.0
O8—Mo3—O7100.96 (14)N1—C1—H1126.0
O9—Mo3—O795.87 (13)C3—C2—N1107.2 (5)
O1i—Mo3—O7148.71 (11)C3—C2—H2126.4
O8—Mo3—O1092.78 (13)N1—C2—H2126.4
O9—Mo3—O10159.45 (13)C2—C3—N2107.0 (5)
O1i—Mo3—O1082.70 (11)C2—C3—H3126.5
O7—Mo3—O1071.35 (10)N2—C3—H3126.5
O8—Mo3—O12i163.96 (13)C5—C4—N3109.5 (6)
O9—Mo3—O12i88.23 (13)C5—C4—H4125.2
O1i—Mo3—O12i71.15 (10)N3—C4—H4125.2
O7—Mo3—O12i85.17 (11)C4—C5—N4106.7 (7)
O10—Mo3—O12i74.99 (9)C4—C5—H5126.7
O13—Cu1—O13i180.0N4—C5—H5126.7
O13—Cu1—O1286.42 (10)N3—C6—N4107.7 (6)
O13i—Cu1—O1293.58 (10)N3—C6—H6126.2
O13—Cu1—O12i93.58 (10)N4—C6—H6126.2
O13i—Cu1—O12i86.42 (10)C1—N1—C2108.8 (4)
O12—Cu1—O12i180.0C1—N1—H1A125.6
O13—Cu1—O10i94.21 (10)C2—N1—H1A125.6
O13i—Cu1—O10i85.79 (10)C1—N2—C3109.1 (5)
O12—Cu1—O10i86.14 (10)C1—N2—H2A125.5
O12i—Cu1—O10i93.86 (10)C3—N2—H2A125.5
O13—Cu1—O1085.79 (10)C6—N3—C4107.6 (6)
O13i—Cu1—O1094.21 (10)C6—N3—H3A126.2
O12—Cu1—O1093.86 (10)C4—N3—H3A126.2
O12i—Cu1—O1086.14 (10)C6—N4—C5108.5 (5)
O10i—Cu1—O10180.0C6—N4—H4A125.8
O14i—As1—O1199.33 (14)C5—N4—H4A125.8
O14i—As1—O1099.24 (13)
Symmetry code: (i) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4ii0.861.812.664 (5)173
N2—H2A···O30.861.992.748 (5)146
N2—H2A···O9iii0.862.423.020 (5)127
N3—H3A···O7iii0.862.092.867 (6)150
N4—H4A···O2iv0.862.002.834 (6)165
Symmetry codes: (ii) x, y+1/2, z+1/2; (iii) x1, y, z; (iv) x, y, z+1.

Experimental details

Crystal data
Chemical formula(C3H5N2)4[As6CuMo6O30]
Mr1845.07
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)10.5696 (7), 19.2842 (12), 10.4678 (7)
β (°) 106.747 (1)
V3)2043.1 (2)
Z2
Radiation typeMo Kα
µ (mm1)7.22
Crystal size (mm)0.28 × 0.25 × 0.20
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.237, 0.326
No. of measured, independent and
observed [I > 2σ(I)] reflections
12666, 4906, 4057
Rint0.029
(sin θ/λ)max1)0.666
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.073, 1.03
No. of reflections4906
No. of parameters286
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.56, 1.94

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4i0.861.812.664 (5)173
N2—H2A···O30.861.992.748 (5)146
N2—H2A···O9ii0.862.423.020 (5)127
N3—H3A···O7ii0.862.092.867 (6)150
N4—H4A···O2iii0.862.002.834 (6)165
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x1, y, z; (iii) x, y, z+1.
 

Acknowledgements

This work was supported by the Science and Technology Project of the Education Office of Heilongjiang Province (11531249), the Scientific Research Foundation for Doctors of Harbin Normal University (09XBKQ11) and the Research Project of Harbin Normal University (KM2007–09).

References

First citationBruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationBruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationFidalgo, E. G., Neels, A., Stoeckli-Evans, H. & Süss-Fink, G. (2002). Polyhedron, 21, 1921–1928.  Web of Science CSD CrossRef CAS Google Scholar
First citationMüller, A., Peters, F., Pope, M. T. & Gatteschi, D. (1998). Chem. Rev. 98, 239–271.  Web of Science CrossRef PubMed Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSun, C.-Y., Li, Y.-G., Wang, E.-B., Xiao, D.-R., An, H.-Y. & Xu, L. (2007). Inorg. Chem. 46, 1563–1574.  Web of Science CSD CrossRef PubMed CAS Google Scholar

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