The title compound, (C
7H
11N
2O)
4[Mo
8O
26], was synthesized by hydrothermal reaction of an acidified aqueous solution of Na
2Mo
2O
4·2H
2O,
N-(2-hydroxyethyl)-4-aminopyridine sulfate and Zn(CH
3COO)
2·4H
2O. Single X-ray crystal analysis reveals that the structure of the title compound consists of a centrosymmetric β-octamolybdate anion and
N-(2-hydroxyethyl)-4-aminopyridinium cations. The Mo—O bond lengths are in the range 1.687 (4)–1.708 (4) Å for terminal Mo—O bonds and 1.759 (4)–2.437 (4) Å for the Mo—O bonds shared by two or more neighboring {MoO
6} octahedra. The O—H
O hydrogen-bond lengths are 2.677 (8)–2.804 (8) Å, and the N—H
N hydrogen-bond lengths are 2.905 (8)–3.033 (7) Å.
Supporting information
CCDC reference: 206736
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.011 Å
- R factor = 0.037
- wR factor = 0.104
- Data-to-parameter ratio = 12.8
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
General Notes
FORMU_01 There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C28 H44 Mo8 N8 O30
Atom count from _chemical_formula_moiety:C280 H440 N80 O40
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: SMART and SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
Crystal data top
(C7H11N2O)4[Mo8O26] | F(000) = 1688 |
Mr = 1740.23 | Dx = 2.380 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.657 (3) Å | Cell parameters from 4440 reflections |
b = 13.816 (3) Å | θ = 2.1–25.1° |
c = 14.892 (3) Å | µ = 2.10 mm−1 |
β = 111.15 (1)° | T = 293 K |
V = 2428.8 (9) Å3 | Prism, colorless |
Z = 2 | 0.47 × 0.38 × 0.27 mm |
Data collection top
SMART CCD diffractometer | 4280 independent reflections |
Radiation source: fine-focus sealed tube | 3561 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 25.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −4→15 |
Tmin = 0.363, Tmax = 0.568 | k = −14→16 |
7194 measured reflections | l = −17→17 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.104 | w = 1/[σ2(Fo2) + (0.0471P)2 + 9.0016P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
4280 reflections | Δρmax = 1.10 e Å−3 |
335 parameters | Δρmin = −0.82 e Å−3 |
3 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00024 (1) |
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 | Uiso*/Ueq | |
Mo1 | 1.01296 (4) | 0.87781 (4) | −0.65165 (3) | 0.02796 (15) | |
Mo2 | 1.21918 (4) | 0.91046 (4) | −0.42635 (4) | 0.02803 (15) | |
Mo3 | 0.75292 (4) | 0.86928 (4) | −0.65751 (4) | 0.03127 (16) | |
Mo4 | 0.96264 (4) | 0.90512 (3) | −0.43275 (3) | 0.02434 (15) | |
O1 | 0.8783 (3) | 1.0199 (3) | −0.4206 (3) | 0.0277 (8) | |
O2 | 0.8859 (3) | 0.8008 (3) | −0.6575 (3) | 0.0332 (9) | |
O3 | 1.0689 (3) | 0.8454 (3) | −0.4835 (3) | 0.0287 (8) | |
O4 | 1.3006 (3) | 1.0291 (3) | −0.4027 (3) | 0.0354 (9) | |
O5 | 1.2951 (3) | 0.8442 (3) | −0.4787 (3) | 0.0385 (10) | |
O6 | 1.1070 (4) | 0.7930 (3) | −0.6557 (3) | 0.0443 (11) | |
O7 | 0.7084 (4) | 0.9123 (4) | −0.7719 (3) | 0.0482 (12) | |
O8 | 0.9114 (3) | 0.9802 (3) | −0.5890 (3) | 0.0259 (8) | |
O9 | 0.8438 (3) | 0.8342 (3) | −0.4962 (3) | 0.0320 (9) | |
O10 | 1.2578 (4) | 0.8629 (3) | −0.3135 (3) | 0.0373 (10) | |
O11 | 0.6620 (4) | 0.7771 (3) | −0.6609 (3) | 0.0430 (11) | |
O12 | 1.0068 (4) | 0.8625 (3) | −0.3190 (3) | 0.0344 (9) | |
O13 | 0.9690 (4) | 0.9323 (3) | −0.7620 (3) | 0.0394 (10) | |
O14 | 1.5970 (8) | 0.7425 (5) | −0.5026 (6) | 0.118 (3) | |
H14B | 1.6163 | 0.7484 | −0.5493 | 0.178* | |
O15 | 1.4365 (5) | 0.6248 (4) | −0.4869 (4) | 0.0593 (14) | |
H15A | 1.4853 | 0.6605 | −0.4928 | 0.089* | |
N1 | 1.6294 (6) | 0.9376 (5) | −0.3288 (5) | 0.0631 (19) | |
N2 | 1.6046 (5) | 1.1852 (4) | −0.1846 (5) | 0.0525 (15) | |
H2A | 1.5730 | 1.1831 | −0.1422 | 0.063* | |
H2B | 1.6337 | 1.2383 | −0.1947 | 0.063* | |
N3 | 1.2055 (4) | 0.5492 (4) | −0.5325 (4) | 0.0359 (12) | |
N4 | 1.0890 (5) | 0.4169 (4) | −0.3387 (4) | 0.0457 (14) | |
H4A | 1.0630 | 0.4505 | −0.3026 | 0.055* | |
H4B | 1.0917 | 0.3549 | −0.3339 | 0.055* | |
C1 | 1.5737 (8) | 0.8348 (8) | −0.4729 (7) | 0.090 (3) | |
H1A | 1.4953 | 0.8392 | −0.4779 | 0.108* | |
H1B | 1.5884 | 0.8854 | −0.5121 | 0.108* | |
C2 | 1.6523 (8) | 0.8442 (8) | −0.3696 (6) | 0.081 (3) | |
H2C | 1.6408 | 0.7903 | −0.3324 | 0.097* | |
H2D | 1.7303 | 0.8427 | −0.3661 | 0.097* | |
C3 | 1.6708 (7) | 1.0226 (7) | −0.3459 (6) | 0.066 (2) | |
H3A | 1.7077 | 1.0238 | −0.3898 | 0.079* | |
C4 | 1.6615 (6) | 1.1060 (6) | −0.3025 (5) | 0.0514 (19) | |
H4C | 1.6901 | 1.1632 | −0.3175 | 0.062* | |
C5 | 1.6082 (5) | 1.1060 (5) | −0.2344 (5) | 0.0381 (14) | |
C6 | 1.5616 (5) | 1.0179 (5) | −0.2200 (5) | 0.0441 (16) | |
H6A | 1.5222 | 1.0151 | −0.1781 | 0.053* | |
C7 | 1.5734 (7) | 0.9373 (6) | −0.2663 (6) | 0.0541 (19) | |
H7A | 1.5422 | 0.8797 | −0.2551 | 0.065* | |
C8 | 1.3738 (6) | 0.5828 (6) | −0.5765 (5) | 0.0482 (17) | |
H8A | 1.3908 | 0.5142 | −0.5742 | 0.058* | |
H8B | 1.3970 | 0.6118 | −0.6258 | 0.058* | |
C9 | 1.2490 (6) | 0.5958 (5) | −0.6035 (5) | 0.0471 (17) | |
H9A | 1.2103 | 0.5680 | −0.6667 | 0.056* | |
H9B | 1.2317 | 0.6644 | −0.6073 | 0.056* | |
C10 | 1.2059 (6) | 0.4513 (4) | −0.5250 (5) | 0.0385 (14) | |
H10A | 1.2334 | 0.4141 | −0.5638 | 0.046* | |
C11 | 1.1674 (6) | 0.4070 (5) | −0.4624 (5) | 0.0412 (15) | |
H11A | 1.1683 | 0.3398 | −0.4590 | 0.049* | |
C12 | 1.1253 (5) | 0.4610 (5) | −0.4017 (4) | 0.0339 (13) | |
C13 | 1.1234 (5) | 0.5626 (5) | −0.4133 (4) | 0.0343 (13) | |
H13A | 1.0950 | 0.6016 | −0.3764 | 0.041* | |
C14 | 1.1627 (5) | 0.6032 (4) | −0.4775 (4) | 0.0351 (14) | |
H14A | 1.1604 | 0.6702 | −0.4842 | 0.042* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.0334 (3) | 0.0255 (3) | 0.0292 (3) | 0.0013 (2) | 0.0164 (2) | −0.00157 (19) |
Mo2 | 0.0276 (3) | 0.0262 (3) | 0.0327 (3) | 0.0048 (2) | 0.0138 (2) | 0.0022 (2) |
Mo3 | 0.0325 (3) | 0.0291 (3) | 0.0328 (3) | −0.0007 (2) | 0.0125 (2) | 0.0007 (2) |
Mo4 | 0.0286 (3) | 0.0215 (3) | 0.0272 (3) | 0.00185 (19) | 0.0153 (2) | 0.00257 (18) |
O1 | 0.029 (2) | 0.027 (2) | 0.031 (2) | −0.0018 (17) | 0.0167 (16) | −0.0005 (16) |
O2 | 0.044 (2) | 0.023 (2) | 0.035 (2) | −0.0040 (18) | 0.0168 (19) | −0.0018 (17) |
O3 | 0.033 (2) | 0.025 (2) | 0.030 (2) | 0.0023 (17) | 0.0138 (17) | 0.0015 (16) |
O4 | 0.025 (2) | 0.037 (2) | 0.046 (2) | 0.0013 (18) | 0.0151 (18) | 0.0001 (19) |
O5 | 0.033 (2) | 0.037 (2) | 0.050 (3) | 0.0073 (19) | 0.022 (2) | 0.002 (2) |
O6 | 0.049 (3) | 0.037 (2) | 0.052 (3) | 0.010 (2) | 0.023 (2) | −0.007 (2) |
O7 | 0.050 (3) | 0.050 (3) | 0.042 (3) | 0.005 (2) | 0.013 (2) | 0.005 (2) |
O8 | 0.0270 (19) | 0.025 (2) | 0.0287 (19) | 0.0032 (16) | 0.0135 (15) | 0.0024 (16) |
O9 | 0.033 (2) | 0.030 (2) | 0.037 (2) | −0.0014 (18) | 0.0164 (18) | 0.0015 (18) |
O10 | 0.040 (2) | 0.036 (2) | 0.037 (2) | 0.0035 (19) | 0.0157 (19) | 0.0026 (19) |
O11 | 0.040 (2) | 0.038 (3) | 0.049 (3) | −0.010 (2) | 0.014 (2) | −0.003 (2) |
O12 | 0.043 (2) | 0.031 (2) | 0.033 (2) | 0.0004 (18) | 0.0191 (19) | 0.0066 (17) |
O13 | 0.047 (3) | 0.041 (3) | 0.035 (2) | −0.003 (2) | 0.020 (2) | 0.0010 (19) |
O14 | 0.188 (8) | 0.081 (5) | 0.156 (7) | −0.076 (5) | 0.147 (7) | −0.064 (5) |
O15 | 0.060 (3) | 0.072 (4) | 0.054 (3) | −0.012 (3) | 0.030 (3) | −0.007 (3) |
N1 | 0.072 (5) | 0.064 (4) | 0.075 (5) | −0.012 (4) | 0.053 (4) | −0.017 (4) |
N2 | 0.050 (4) | 0.045 (4) | 0.065 (4) | −0.005 (3) | 0.024 (3) | −0.004 (3) |
N3 | 0.034 (3) | 0.034 (3) | 0.040 (3) | 0.001 (2) | 0.014 (2) | 0.003 (2) |
N4 | 0.059 (4) | 0.034 (3) | 0.052 (3) | −0.002 (3) | 0.030 (3) | −0.001 (3) |
C1 | 0.056 (5) | 0.128 (10) | 0.089 (7) | −0.018 (6) | 0.030 (5) | 0.028 (7) |
C2 | 0.067 (6) | 0.104 (8) | 0.069 (6) | 0.003 (6) | 0.020 (5) | 0.012 (6) |
C3 | 0.063 (5) | 0.086 (7) | 0.067 (5) | −0.004 (5) | 0.045 (4) | 0.006 (5) |
C4 | 0.051 (4) | 0.059 (5) | 0.049 (4) | −0.016 (4) | 0.024 (3) | 0.010 (4) |
C5 | 0.033 (3) | 0.043 (4) | 0.035 (3) | 0.000 (3) | 0.009 (3) | 0.008 (3) |
C6 | 0.040 (4) | 0.050 (4) | 0.050 (4) | −0.001 (3) | 0.025 (3) | 0.006 (3) |
C7 | 0.065 (5) | 0.045 (4) | 0.070 (5) | −0.012 (4) | 0.045 (4) | 0.002 (4) |
C8 | 0.055 (4) | 0.050 (4) | 0.046 (4) | −0.001 (3) | 0.026 (3) | −0.001 (3) |
C9 | 0.053 (4) | 0.049 (4) | 0.045 (4) | 0.009 (3) | 0.025 (3) | 0.012 (3) |
C10 | 0.047 (4) | 0.030 (3) | 0.041 (3) | 0.003 (3) | 0.019 (3) | −0.006 (3) |
C11 | 0.045 (4) | 0.031 (3) | 0.049 (4) | 0.001 (3) | 0.019 (3) | −0.001 (3) |
C12 | 0.027 (3) | 0.036 (3) | 0.038 (3) | −0.001 (3) | 0.011 (3) | −0.003 (3) |
C13 | 0.029 (3) | 0.037 (3) | 0.037 (3) | 0.001 (3) | 0.013 (3) | −0.006 (3) |
C14 | 0.034 (3) | 0.028 (3) | 0.042 (3) | 0.007 (3) | 0.012 (3) | −0.004 (3) |
Geometric parameters (Å, º) top
Mo1—O6 | 1.687 (4) | N1—C2 | 1.499 (11) |
Mo1—O13 | 1.708 (4) | N2—C5 | 1.332 (9) |
Mo1—O2 | 1.904 (4) | N2—H2A | 0.8600 |
Mo1—O1i | 1.996 (4) | N2—H2B | 0.8600 |
Mo1—O8 | 2.321 (4) | N3—C14 | 1.357 (8) |
Mo1—O3 | 2.386 (4) | N3—C10 | 1.358 (8) |
Mo2—O10 | 1.704 (4) | N3—C9 | 1.502 (8) |
Mo2—O5 | 1.706 (4) | N4—C12 | 1.333 (8) |
Mo2—O4 | 1.901 (4) | N4—H4A | 0.8600 |
Mo2—O3 | 1.995 (4) | N4—H4B | 0.8600 |
Mo2—O8i | 2.311 (4) | C1—C2 | 1.505 (11) |
Mo2—O1i | 2.369 (4) | C1—H1A | 0.9700 |
Mo2—Mo4 | 3.2145 (9) | C1—H1B | 0.9700 |
Mo3—O7 | 1.696 (5) | C2—H2C | 0.9700 |
Mo3—O11 | 1.705 (4) | C2—H2D | 0.9700 |
Mo3—O4i | 1.916 (4) | C3—C4 | 1.346 (12) |
Mo3—O2 | 1.931 (4) | C3—H3A | 0.9300 |
Mo3—O9 | 2.309 (4) | C4—C5 | 1.405 (9) |
Mo3—O8 | 2.437 (4) | C4—H4C | 0.9300 |
Mo4—O12 | 1.687 (4) | C5—C6 | 1.403 (9) |
Mo4—O9 | 1.758 (4) | C6—C7 | 1.344 (10) |
Mo4—O3 | 1.948 (4) | C6—H6A | 0.9300 |
Mo4—O1 | 1.956 (4) | C7—H7A | 0.9300 |
Mo4—O8i | 2.187 (4) | C8—C9 | 1.493 (10) |
Mo4—O8 | 2.413 (4) | C8—H8A | 0.9700 |
O1—Mo1i | 1.996 (4) | C8—H8B | 0.9700 |
O1—Mo2i | 2.369 (4) | C9—H9A | 0.9700 |
O4—Mo3i | 1.916 (4) | C9—H9B | 0.9700 |
O8—Mo4i | 2.187 (4) | C10—C11 | 1.345 (9) |
O8—Mo2i | 2.311 (4) | C10—H10A | 0.9300 |
O14—C1 | 1.416 (11) | C11—C12 | 1.416 (9) |
O14—H14B | 0.8200 | C11—H11A | 0.9300 |
O15—C8 | 1.409 (8) | C12—C13 | 1.413 (9) |
O15—H15A | 0.8200 | C13—C14 | 1.349 (9) |
N1—C3 | 1.349 (11) | C13—H13A | 0.9300 |
N1—C7 | 1.358 (9) | C14—H14A | 0.9300 |
| | | |
O6—Mo1—O13 | 105.2 (2) | Mo4i—O8—Mo2i | 91.18 (14) |
O6—Mo1—O2 | 101.9 (2) | Mo4i—O8—Mo1 | 91.25 (13) |
O13—Mo1—O2 | 103.0 (2) | Mo2i—O8—Mo1 | 163.29 (18) |
O6—Mo1—O1i | 98.8 (2) | Mo4i—O8—Mo4 | 103.92 (14) |
O13—Mo1—O1i | 97.4 (2) | Mo2i—O8—Mo4 | 97.95 (13) |
O2—Mo1—O1i | 145.9 (2) | Mo1—O8—Mo4 | 97.50 (13) |
O6—Mo1—O8 | 159.7 (2) | Mo4i—O8—Mo3 | 164.51 (18) |
O13—Mo1—O8 | 94.7 (2) | Mo2i—O8—Mo3 | 86.68 (12) |
O2—Mo1—O8 | 77.2 (2) | Mo1—O8—Mo3 | 86.57 (12) |
O1i—Mo1—O8 | 74.1 (1) | Mo4—O8—Mo3 | 91.58 (12) |
O6—Mo1—O3 | 87.8 (2) | Mo4—O9—Mo3 | 116.78 (19) |
O13—Mo1—O3 | 164.3 (2) | C1—O14—H14B | 109.5 |
O2—Mo1—O3 | 82.5 (2) | C8—O15—H15A | 109.5 |
O1i—Mo1—O3 | 71.4 (1) | C3—N1—C7 | 117.8 (7) |
O8—Mo1—O3 | 72.0 (1) | C3—N1—C2 | 121.9 (7) |
O10—Mo2—O5 | 103.6 (2) | C7—N1—C2 | 120.1 (7) |
O10—Mo2—O4 | 101.9 (2) | C5—N2—H2A | 120.0 |
O5—Mo2—O4 | 101.0 (2) | C5—N2—H2B | 120.0 |
O10—Mo2—O3 | 97.9 (2) | H2A—N2—H2B | 120.0 |
O5—Mo2—O3 | 99.8 (2) | C14—N3—C10 | 119.2 (6) |
O4—Mo2—O3 | 146.9 (2) | C14—N3—C9 | 121.1 (5) |
O10—Mo2—O8i | 96.6 (2) | C10—N3—C9 | 119.6 (6) |
O5—Mo2—O8i | 159.6 (2) | C12—N4—H4A | 120.0 |
O4—Mo2—O8i | 77.1 (2) | C12—N4—H4B | 120.0 |
O3—Mo2—O8i | 74.4 (2) | H4A—N4—H4B | 120.0 |
O10—Mo2—O1i | 166.0 (2) | O14—C1—C2 | 105.1 (9) |
O5—Mo2—O1i | 87.8 (2) | O14—C1—H1A | 110.7 |
O4—Mo2—O1i | 83.5 (2) | C2—C1—H1A | 110.7 |
O3—Mo2—O1i | 71.8 (1) | O14—C1—H1B | 110.7 |
O8i—Mo2—O1i | 71.8 (1) | C2—C1—H1B | 110.7 |
O10—Mo2—Mo4 | 87.0 (2) | H1A—C1—H1B | 108.8 |
O5—Mo2—Mo4 | 134.7 (2) | N1—C2—C1 | 109.6 (8) |
O4—Mo2—Mo4 | 120.0 (1) | N1—C2—H2C | 109.8 |
O3—Mo2—Mo4 | 34.9 (1) | C1—C2—H2C | 109.8 |
O8i—Mo2—Mo4 | 42.9 (1) | N1—C2—H2D | 109.8 |
O1i—Mo2—Mo4 | 79.11 (9) | C1—C2—H2D | 109.8 |
O7—Mo3—O11 | 104.8 (2) | H2C—C2—H2D | 108.2 |
O7—Mo3—O4i | 99.7 (2) | C4—C3—N1 | 123.1 (7) |
O11—Mo3—O4i | 102.3 (2) | C4—C3—H3A | 118.4 |
O7—Mo3—O2 | 98.4 (2) | N1—C3—H3A | 118.4 |
O11—Mo3—O2 | 102.3 (2) | C3—C4—C5 | 119.7 (7) |
O4i—Mo3—O2 | 144.5 (2) | C3—C4—H4C | 120.2 |
O7—Mo3—O9 | 168.0 (2) | C5—C4—H4C | 120.2 |
O11—Mo3—O9 | 87.2 (2) | N2—C5—C6 | 121.8 (6) |
O4i—Mo3—O9 | 78.2 (2) | N2—C5—C4 | 121.6 (7) |
O2—Mo3—O9 | 77.9 (2) | C6—C5—C4 | 116.6 (7) |
O7—Mo3—O8 | 97.2 (2) | C7—C6—C5 | 120.6 (6) |
O11—Mo3—O8 | 158.0 (2) | C7—C6—H6A | 119.7 |
O4i—Mo3—O8 | 73.8 (2) | C5—C6—H6A | 119.7 |
O2—Mo3—O8 | 73.9 (2) | C6—C7—N1 | 122.1 (7) |
O9—Mo3—O8 | 70.8 (1) | C6—C7—H7A | 119.0 |
O12—Mo4—O9 | 104.7 (2) | N1—C7—H7A | 119.0 |
O12—Mo4—O3 | 102.5 (2) | O15—C8—C9 | 112.6 (6) |
O9—Mo4—O3 | 97.6 (2) | O15—C8—H8A | 109.1 |
O12—Mo4—O1 | 100.6 (2) | C9—C8—H8A | 109.1 |
O9—Mo4—O1 | 96.4 (2) | O15—C8—H8B | 109.1 |
O3—Mo4—O1 | 148.8 (2) | C9—C8—H8B | 109.1 |
O12—Mo4—O8i | 98.3 (2) | H8A—C8—H8B | 107.8 |
O9—Mo4—O8i | 156.9 (2) | C8—C9—N3 | 112.3 (6) |
O3—Mo4—O8i | 78.2 (2) | C8—C9—H9A | 109.1 |
O1—Mo4—O8i | 78.0 (2) | N3—C9—H9A | 109.1 |
O12—Mo4—O8 | 174.2 (2) | C8—C9—H9B | 109.1 |
O9—Mo4—O8 | 80.9 (2) | N3—C9—H9B | 109.1 |
O3—Mo4—O8 | 77.9 (1) | H9A—C9—H9B | 107.9 |
O1—Mo4—O8 | 77.0 (1) | C11—C10—N3 | 121.3 (6) |
O8i—Mo4—O8 | 76.1 (1) | C11—C10—H10A | 119.4 |
O12—Mo4—Mo2 | 90.76 (14) | N3—C10—H10A | 119.4 |
O9—Mo4—Mo2 | 133.45 (13) | C10—C11—C12 | 121.0 (6) |
O3—Mo4—Mo2 | 35.88 (11) | C10—C11—H11A | 119.5 |
O1—Mo4—Mo2 | 123.91 (11) | C12—C11—H11A | 119.5 |
O8i—Mo4—Mo2 | 45.96 (9) | N4—C12—C13 | 123.0 (6) |
O8—Mo4—Mo2 | 86.32 (8) | N4—C12—C11 | 120.9 (6) |
Mo4—O1—Mo1i | 109.30 (18) | C13—C12—C11 | 116.1 (6) |
Mo4—O1—Mo2i | 110.65 (16) | C14—C13—C12 | 120.3 (6) |
Mo1i—O1—Mo2i | 104.45 (16) | C14—C13—H13A | 119.8 |
Mo1—O2—Mo3 | 116.6 (2) | C12—C13—H13A | 119.8 |
Mo4—O3—Mo2 | 109.21 (18) | C13—C14—N3 | 121.9 (6) |
Mo4—O3—Mo1 | 110.03 (17) | C13—C14—H14A | 119.0 |
Mo2—O3—Mo1 | 103.87 (16) | N3—C14—H14A | 119.0 |
Mo2—O4—Mo3i | 117.3 (2) | | |
Symmetry code: (i) −x+2, −y+2, −z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O14—H14B···O11ii | 0.82 | 1.99 | 2.804 (8) | 174 |
O15—H15A···O14 | 0.82 | 1.86 | 2.677 (8) | 178 |
N2—H2A···O15iii | 0.86 | 2.13 | 2.905 (8) | 150 |
N2—H2B···O10iii | 0.86 | 2.18 | 3.017 (7) | 165 |
N4—H4A···O13iv | 0.86 | 2.22 | 3.033 (7) | 158 |
N4—H4B···O2v | 0.86 | 2.18 | 3.028 (7) | 169 |
Symmetry codes: (ii) x+1, y, z; (iii) −x+3, y+1/2, −z−1/2; (iv) x, −y+3/2, z+1/2; (v) −x+2, −y+1, −z−1. |