The hydrothermally synthesized title compound, {(C
5H
7N
2)
2[Mo
3O
10]}
n, contains [Mo
3O
10]
n2n− chains, which are generated through inversion symmetry. An extensive N—H
O hydrogen-bonding network is observed between the C
5H
7N
2+ cations and the chains.
Supporting information
CCDC reference: 610795
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.005 Å
- R factor = 0.022
- wR factor = 0.046
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.84
PLAT432_ALERT_2_C Short Inter X...Y Contact O8 .. C5 .. 2.99 Ang.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrysAlis CCD (Oxford Diffraction, 2004); cell refinement: CrysAlis RED; data reduction: CrysAlis RED (Oxford Diffraction, 2004); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ATOMS (Dowty, 2002); software used to prepare material for publication: CRYSTALS.
poly[bis(4-aminopyridinium) decaoxotrimolybdenum]
top
Crystal data top
(C5H7N2)2[Mo3O10] | Z = 2 |
Mr = 638.06 | F(000) = 616 |
Triclinic, P1 | Dx = 2.565 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.045 (3) Å | Cell parameters from 6705 reflections |
b = 10.376 (5) Å | θ = 3.8–32.0° |
c = 11.538 (4) Å | µ = 2.31 mm−1 |
α = 65.05 (4)° | T = 110 K |
β = 89.94 (3)° | Needle, colorless |
γ = 72.91 (3)° | 0.22 × 0.10 × 0.07 mm |
V = 826.3 (7) Å3 | |
Data collection top
CrysAlis CCD diffractometer | 3432 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.02 |
ω scans | θmax = 32.2°, θmin = 3.8° |
Absorption correction: analytical multifaceted crystal model (Clark & Reid, 1995) | h = −11→11 |
Tmin = 0.76, Tmax = 0.85 | k = −15→15 |
11942 measured reflections | l = −17→17 |
5309 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.046 | w = [1-(Fo-Fc)2/36σ2(F)]2/[(0.176 × 105)To(x)-
(0.227 × 105)T1(x) + (0.215 × 105)T2(x)-
(0.768 × 104)T3(x) + (0.406 × 104)T4(x)]
where Ti are the Chebychev polynomials and x = Fc/Fmax
(Prince, 1982; Watkin, 1994) |
S = 0.86 | (Δ/σ)max = 0.001 |
3432 reflections | Δρmax = 1.56 e Å−3 |
244 parameters | Δρmin = −0.55 e Å−3 |
0 restraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mo1 | 0.70361 (3) | 0.13745 (3) | 0.77090 (2) | 0.0070 | |
Mo2 | 0.85271 (3) | 0.12633 (3) | 1.03909 (2) | 0.0066 | |
Mo3 | 0.36820 (3) | 0.16537 (3) | 0.90934 (2) | 0.0066 | |
O1 | 0.7593 (3) | 0.2900 (3) | 0.6703 (2) | 0.0124 | |
O2 | 0.7372 (3) | 0.0265 (3) | 0.6918 (2) | 0.0121 | |
O3 | 0.4522 (3) | 0.2343 (2) | 0.7382 (2) | 0.0088 | |
O4 | 0.9085 (3) | 0.0290 (2) | 0.9023 (2) | 0.0082 | |
O5 | 0.6353 (3) | 0.1904 (2) | 0.9383 (2) | 0.0084 | |
O6 | 0.4196 (3) | 0.0373 (2) | 1.0843 (2) | 0.0079 | |
O7 | 0.9133 (3) | 0.2824 (3) | 0.9646 (2) | 0.0112 | |
O8 | 0.8108 (3) | 0.1256 (3) | 1.1855 (2) | 0.0108 | |
O9 | 0.2041 (3) | 0.1114 (2) | 0.8643 (2) | 0.0094 | |
O10 | 0.2642 (3) | 0.3350 (3) | 0.9085 (2) | 0.0108 | |
N1 | 0.5752 (4) | −0.2276 (3) | 0.7936 (3) | 0.0113 | |
N2 | 0.3959 (4) | −0.4380 (3) | 0.6132 (3) | 0.0133 | |
N3 | 0.8192 (5) | −0.2675 (4) | 0.4450 (3) | 0.0231 | |
N4 | 1.0494 (4) | −0.3557 (4) | 0.7974 (3) | 0.0214 | |
C1 | 0.5932 (4) | −0.3743 (4) | 0.8591 (3) | 0.0122 | |
C2 | 0.5347 (4) | −0.4477 (4) | 0.8019 (3) | 0.0121 | |
C3 | 0.4523 (4) | −0.3684 (3) | 0.6721 (3) | 0.0093 | |
C4 | 0.4337 (4) | −0.2145 (4) | 0.6074 (3) | 0.0109 | |
C5 | 0.4964 (4) | −0.1487 (4) | 0.6702 (3) | 0.0117 | |
C6 | 0.8392 (5) | −0.4000 (4) | 0.5461 (4) | 0.0208 | |
C7 | 0.9199 (5) | −0.4360 (4) | 0.6640 (3) | 0.0137 | |
C8 | 0.9788 (4) | −0.3286 (4) | 0.6818 (3) | 0.0108 | |
C9 | 0.9591 (5) | −0.1914 (4) | 0.5728 (4) | 0.0169 | |
C10 | 0.8817 (5) | −0.1654 (4) | 0.4562 (4) | 0.0210 | |
H1 | 0.6210 | −0.1768 | 0.8369 | 0.0147* | |
H2 | 0.6501 | −0.4307 | 0.9512 | 0.0144* | |
H3 | 0.5504 | −0.5571 | 0.8517 | 0.0135* | |
H4 | 0.3750 | −0.1539 | 0.5159 | 0.0133* | |
H5 | 0.4831 | −0.0394 | 0.6235 | 0.0146* | |
H6 | 0.4108 | −0.5474 | 0.6614 | 0.0167* | |
H7 | 0.3391 | −0.3806 | 0.5211 | 0.0167* | |
H8 | 0.7571 | −0.2438 | 0.3599 | 0.0238* | |
H9 | 0.7936 | −0.4742 | 0.5344 | 0.0268* | |
H10 | 0.9374 | −0.5369 | 0.7376 | 0.0173* | |
H11 | 1.0013 | −0.1138 | 0.5811 | 0.0198* | |
H12 | 0.8716 | −0.0697 | 0.3783 | 0.0211* | |
H13 | 1.0890 | −0.2781 | 0.8080 | 0.0251* | |
H14 | 1.0624 | −0.4536 | 0.8737 | 0.0251* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.00710 (11) | 0.00792 (11) | 0.00564 (11) | −0.00268 (9) | −0.00009 (8) | −0.00263 (9) |
Mo2 | 0.00644 (11) | 0.00693 (11) | 0.00677 (11) | −0.00194 (9) | −0.00027 (8) | −0.00354 (9) |
Mo3 | 0.00656 (11) | 0.00625 (11) | 0.00653 (11) | −0.00215 (9) | −0.00025 (8) | −0.00245 (9) |
O1 | 0.0135 (11) | 0.0105 (10) | 0.0105 (10) | −0.0054 (8) | 0.0004 (8) | −0.0011 (8) |
O2 | 0.0134 (11) | 0.0140 (11) | 0.0103 (10) | −0.0043 (9) | 0.0011 (8) | −0.0068 (9) |
O3 | 0.0095 (10) | 0.0093 (10) | 0.0064 (9) | −0.0031 (8) | 0.0002 (7) | −0.0022 (8) |
O4 | 0.0089 (9) | 0.0096 (10) | 0.0072 (9) | −0.0026 (8) | 0.0007 (7) | −0.0050 (8) |
O5 | 0.0076 (9) | 0.0100 (10) | 0.0070 (9) | −0.0017 (8) | −0.0012 (7) | −0.0040 (8) |
O6 | 0.0092 (9) | 0.0067 (9) | 0.0073 (9) | −0.0023 (7) | 0.0010 (7) | −0.0029 (8) |
O7 | 0.0118 (10) | 0.0087 (10) | 0.0134 (10) | −0.0041 (8) | 0.0013 (8) | −0.0045 (9) |
O8 | 0.0112 (10) | 0.0134 (11) | 0.0084 (10) | −0.0032 (8) | 0.0008 (8) | −0.0059 (8) |
O9 | 0.0056 (9) | 0.0060 (9) | 0.0161 (11) | −0.0007 (7) | −0.0025 (8) | −0.0051 (9) |
O10 | 0.0115 (10) | 0.0082 (10) | 0.0110 (10) | −0.0019 (8) | −0.0005 (8) | −0.0035 (8) |
N1 | 0.0123 (12) | 0.0135 (13) | 0.0112 (12) | −0.0053 (10) | 0.0009 (10) | −0.0078 (10) |
N2 | 0.0180 (13) | 0.0093 (12) | 0.0123 (12) | −0.0041 (10) | −0.0034 (10) | −0.0047 (10) |
N3 | 0.0284 (17) | 0.0209 (16) | 0.0108 (13) | 0.0034 (13) | −0.0072 (12) | −0.0060 (12) |
N4 | 0.0277 (17) | 0.0144 (14) | 0.0192 (15) | 0.0013 (12) | −0.0096 (12) | −0.0101 (12) |
C1 | 0.0131 (14) | 0.0133 (14) | 0.0096 (13) | −0.0042 (11) | −0.0012 (11) | −0.0046 (11) |
C2 | 0.0129 (14) | 0.0107 (14) | 0.0106 (13) | −0.0035 (11) | −0.0017 (11) | −0.0030 (11) |
C3 | 0.0095 (13) | 0.0110 (13) | 0.0083 (13) | −0.0019 (10) | 0.0019 (10) | −0.0060 (11) |
C4 | 0.0131 (14) | 0.0109 (13) | 0.0088 (13) | −0.0042 (11) | 0.0007 (10) | −0.0040 (11) |
C5 | 0.0137 (14) | 0.0095 (13) | 0.0124 (14) | −0.0038 (11) | 0.0019 (11) | −0.0053 (11) |
C6 | 0.0173 (16) | 0.0227 (18) | 0.0270 (19) | −0.0053 (14) | −0.0020 (14) | −0.0160 (16) |
C7 | 0.0166 (15) | 0.0130 (14) | 0.0131 (14) | −0.0058 (12) | 0.0021 (12) | −0.0066 (12) |
C8 | 0.0115 (13) | 0.0094 (13) | 0.0121 (13) | −0.0008 (11) | 0.0002 (11) | −0.0069 (11) |
C9 | 0.0185 (16) | 0.0104 (14) | 0.0206 (17) | −0.0046 (12) | 0.0016 (13) | −0.0058 (13) |
C10 | 0.0258 (19) | 0.0132 (16) | 0.0142 (15) | −0.0008 (14) | 0.0044 (14) | −0.0006 (13) |
Geometric parameters (Å, º) top
Mo1—O1 | 1.709 (2) | N2—H7 | 1.000 |
Mo1—O2 | 1.713 (2) | N3—C6 | 1.339 (5) |
Mo1—O3 | 1.931 (2) | N3—C10 | 1.349 (5) |
Mo1—O4 | 1.938 (2) | N3—H8 | 1.000 |
Mo1—O5 | 2.247 (2) | N4—C8 | 1.332 (4) |
Mo1—O6i | 2.358 (2) | N4—H13 | 1.000 |
Mo2—O4 | 2.188 (2) | N4—H14 | 1.000 |
Mo2—O4ii | 2.002 (2) | C1—C2 | 1.368 (4) |
Mo2—O5 | 1.877 (2) | C1—H2 | 1.000 |
Mo2—O7 | 1.700 (2) | C2—C3 | 1.415 (4) |
Mo2—O8 | 1.720 (2) | C2—H3 | 1.000 |
Mo2—O9i | 2.424 (2) | C3—C4 | 1.409 (4) |
Mo3—O3 | 1.990 (2) | C4—C5 | 1.367 (4) |
Mo3—O5 | 2.280 (2) | C4—H4 | 1.000 |
Mo3—O6 | 1.852 (2) | C5—H5 | 1.000 |
Mo3—O6i | 2.258 (2) | C6—C7 | 1.357 (5) |
Mo3—O9 | 1.735 (2) | C6—H9 | 1.000 |
Mo3—O10 | 1.708 (2) | C7—C8 | 1.418 (4) |
N1—C1 | 1.345 (4) | C7—H10 | 1.000 |
N1—C5 | 1.346 (4) | C8—C9 | 1.411 (5) |
N1—H1 | 1.000 | C9—C10 | 1.366 (5) |
N2—C3 | 1.339 (4) | C9—H11 | 1.000 |
N2—H6 | 1.000 | C10—H12 | 1.000 |
| | | |
O1—Mo1—O2 | 104.11 (11) | O9—Mo3—O10 | 105.75 (11) |
O1—Mo1—O3 | 97.43 (10) | C1—N1—C5 | 120.6 (3) |
O2—Mo1—O3 | 103.93 (10) | C1—N1—H1 | 119.7 |
O1—Mo1—O4 | 100.82 (10) | C5—N1—H1 | 119.7 |
O2—Mo1—O4 | 100.31 (10) | C3—N2—H6 | 120.0 |
O3—Mo1—O4 | 144.92 (9) | C3—N2—H7 | 120.0 |
O1—Mo1—O5 | 101.74 (10) | H6—N2—H7 | 120.000 |
O2—Mo1—O5 | 154.09 (10) | C6—N3—C10 | 121.0 (3) |
O3—Mo1—O5 | 74.31 (8) | C6—N3—H8 | 119.5 |
O1—Mo1—O6i | 168.53 (10) | C10—N3—H8 | 119.5 |
O2—Mo1—O6i | 84.69 (10) | C8—N4—H13 | 120.0 |
O3—Mo1—O6i | 73.00 (8) | C8—N4—H14 | 120.0 |
O4—Mo1—O5 | 72.80 (8) | H13—N4—H14 | 120.000 |
O4—Mo1—O6i | 84.53 (8) | N1—C1—C2 | 121.2 (3) |
O5—Mo1—O6i | 69.95 (8) | N1—C1—H2 | 119.5 |
O4—Mo2—O4ii | 71.07 (10) | C2—C1—H2 | 119.4 |
O4—Mo2—O5 | 75.31 (9) | C1—C2—C3 | 119.8 (3) |
O4ii—Mo2—O5 | 143.92 (9) | C1—C2—H3 | 120.1 |
O4—Mo2—O7 | 100.90 (10) | C3—C2—H3 | 120.1 |
O4ii—Mo2—O7 | 98.92 (10) | N2—C3—C2 | 121.0 (3) |
O5—Mo2—O7 | 99.90 (10) | N2—C3—C4 | 121.6 (3) |
O4—Mo2—O8 | 155.51 (10) | C2—C3—C4 | 117.3 (3) |
O4ii—Mo2—O8 | 98.10 (10) | C3—C4—C5 | 119.7 (3) |
O5—Mo2—O8 | 107.44 (10) | C3—C4—H4 | 120.1 |
O7—Mo2—O8 | 102.49 (11) | C5—C4—H4 | 120.2 |
O4—Mo2—O9i | 73.53 (8) | N1—C5—C4 | 121.4 (3) |
O4ii—Mo2—O9i | 75.48 (8) | N1—C5—H5 | 119.4 |
O5—Mo2—O9i | 82.88 (8) | C4—C5—H5 | 119.2 |
O7—Mo2—O9i | 173.05 (10) | N3—C6—C7 | 121.6 (3) |
O8—Mo2—O9i | 82.58 (10) | N3—C6—H9 | 119.2 |
O3—Mo3—O5 | 72.52 (8) | C7—C6—H9 | 119.2 |
O3—Mo3—O6 | 147.82 (9) | C6—C7—C8 | 119.2 (3) |
O5—Mo3—O6 | 83.90 (9) | C6—C7—H10 | 120.5 |
O3—Mo3—O6i | 74.29 (8) | C8—C7—H10 | 120.4 |
O5—Mo3—O6i | 71.17 (8) | N4—C8—C7 | 121.2 (3) |
O6—Mo3—O6i | 77.59 (10) | N4—C8—C9 | 121.0 (3) |
O3—Mo3—O9 | 95.72 (10) | C7—C8—C9 | 117.7 (3) |
O5—Mo3—O9 | 161.37 (9) | C8—C9—C10 | 119.6 (3) |
O6—Mo3—O9 | 100.61 (10) | C8—C9—H11 | 120.1 |
O3—Mo3—O10 | 99.86 (10) | C10—C9—H11 | 120.4 |
O5—Mo3—O10 | 90.75 (10) | N3—C10—C9 | 120.7 (3) |
O6—Mo3—O10 | 102.07 (10) | N3—C10—H12 | 119.7 |
O6i—Mo3—O9 | 91.99 (9) | C9—C10—H12 | 119.6 |
O6i—Mo3—O10 | 161.89 (10) | | |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+2, −y, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O6i | 1.00 | 1.96 | 2.877 (3) | 151 |
N2—H6···O3iii | 1.00 | 1.97 | 2.967 (4) | 173 |
N2—H7···O1iv | 1.00 | 2.05 | 3.043 (4) | 172 |
N3—H8···O3iv | 1.00 | 1.99 | 2.883 (4) | 148 |
N4—H13···O8ii | 1.00 | 2.00 | 2.997 (4) | 173 |
N4—H14···O10v | 1.00 | 2.19 | 2.864 (4) | 124 |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+2, −y, −z+2; (iii) x, y−1, z; (iv) −x+1, −y, −z+1; (v) x+1, y−1, z. |