metal-organic compounds
Diammonium bis[(2-aminoacetato-κ2N,O)(2,2′-bipyridine-κ2N,N′)(N,N-dimethylformamide-κO)copper(II)] hexacosaoxidooctamolybdate(VI)
aCollege of Chemistry and Pharmacy, Jiamusi University, Jiamusi 154007, People's Republic of China
*Correspondence e-mail: hyliu2007@yahoo.cn
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 CuII 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.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2004); cell 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
10.1107/S1600536808000020/hy2114sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808000020/hy2114Isup2.hkl
(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.
H atoms of ammonium were located in difference Fourier maps and fixed in their as-found positions (N—H = 0.90–0.98 Å) with Uiso(H) = 1.2Ueq(N). The other H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93Å (CH), 0.97Å (CH2), N—H = 0.90Å and Uiso(H) = 1.2Ueq(C,N), and with C—H = 0.96Å (CH3) and Uiso(H) = 1.5Ueq(C).
Data collection: APEX2 (Bruker, 2004); cell
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.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. |
(NH4)2[Cu(C2H4NO2)(C10H8N2)(C3H7NO)]2[Mo8O26] | Z = 1 |
Mr = 1953.38 | F(000) = 946 |
Triclinic, P1 | Dx = 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 |
Bruker SMART APEXII diffractometer | 4889 independent reflections |
Radiation source: fine-focus sealed tube | 3591 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.071 |
ϕ and ω scans | θmax = 25.6°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→12 |
Tmin = 0.530, Tmax = 0.690 | k = −13→13 |
10864 measured reflections | l = −15→14 |
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(Fo2) + (0.0226P)2] where P = (Fo2 + 2Fc2)/3 |
4889 reflections | (Δ/σ)max < 0.001 |
370 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.83 e Å−3 |
(NH4)2[Cu(C2H4NO2)(C10H8N2)(C3H7NO)]2[Mo8O26] | γ = 81.61 (3)° |
Mr = 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)° |
Bruker SMART APEXII diffractometer | 4889 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3591 reflections with I > 2σ(I) |
Tmin = 0.530, Tmax = 0.690 | Rint = 0.071 |
10864 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.110 | H-atom parameters constrained |
S = 0.99 | Δρmax = 0.86 e Å−3 |
4889 reflections | Δρmin = −0.83 e Å−3 |
370 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
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* |
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) |
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. |
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] |
Mr | 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) |
Tmin, Tmax | 0.530, 0.690 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10864, 4889, 3591 |
Rint | 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 |
Δρmax, Δρmin (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).
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. |
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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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 CuII 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.