Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807019423/pk2017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807019423/pk2017Isup2.hkl |
CCDC reference: 646648
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.016 Å
- R factor = 0.044
- wR factor = 0.114
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Guo & Li (2007); Deng et al. (2005); Wang et al. (1993); Wilson et al. (1984).
A solution of n-hexylpyridinium bromide (1.80 g, 7 mmol) in 10 ml of distilled water was added dropwise to a mixture of 20 ml aqueous solution of dihydrate sodium molybdate (1.2 g, 5 mmol) and 12% dilute hydrogen chloride (1.8 ml, 7 mmol) under stirring at 70°C. A white precipitate was immediately formed. After continuously stirring for 20 min, the resulting product was filtered, washed with water and dried at room temperature to produce the tetra-n-hexylpyridinium octamolybdate in 89% yield. Single crystals were separated from the above filtrate by slowly evaporating over a period of 1 d at 40°C.
The H atoms bonded to C atoms were included in the refinement with a riding model approximation, with C–H = 0.93–0.97 Å and Uiso (H) = 1.2 Ueq (C atom). For the H atoms attached to C atoms of methyl groups, their Uiso(H) =1.5Ueq(C).
Polymolybdates have attracted considerable interest for application in selective catalysis of oxidation reactions with hydrogen peroxide. The synthesis and crystal structure reported here is part of this study (Guo and Li, 2007).
The title compound, (I), consists of a centrosymmetric β-octamolybdate anion and four n-hexylpyridinium cations. The structure of the anion is constructed from an array of eight edge-shared MoO6 octahedra. The Mo–O bond lengths can be grouped into four sets: Mo–O(t) 1.672 (6)–1.694 (5) Å, Mo–O(µ2) 1.725 (5)–2.311 (5) Å, Mo–O(µ3) 1.939 (5)–2.311 (5) Å, Mo–O(µ5) 2.128 (5)–2.374 (5) Å. The molecule of the compound is shown in Fig. 1.
In the structure of (I), no classic hydrogen bonds are found, but there exist a number of weak C–H···O interactions (see Table 1). These are further loosely aggregated into a three-dimensional framework via van der Waals forces. A packing diagram for the structure of (I) is shown in Fig. 2.
For related literature, see: Guo & Li (2007); Deng et al. (2005); Wang et al. (1993); Wilson et al. (1984).
Data collection: SMART (Bruker 1997); cell refinement: SAINT (Bruker 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C11H18N)4[Mo8O26] | F(000) = 1816 |
Mr = 1840.58 | Dx = 1.983 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2002 reflections |
a = 15.474 (4) Å | θ = 2.4–21.6° |
b = 12.051 (3) Å | µ = 1.65 mm−1 |
c = 16.592 (4) Å | T = 294 K |
β = 94.964 (5)° | Block, colorless |
V = 3082.4 (13) Å3 | 0.22 × 0.20 × 0.16 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 5450 independent reflections |
Radiation source: fine-focus sealed tube | 2782 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.082 |
φ and ω scans | θmax = 25.0°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→11 |
Tmin = 0.698, Tmax = 0.765 | k = −14→14 |
15694 measured reflections | l = −19→19 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.114 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0421P)2] where P = (Fo2 + 2Fc2)/3 |
5450 reflections | (Δ/σ)max < 0.001 |
370 parameters | Δρmax = 0.63 e Å−3 |
78 restraints | Δρmin = −0.62 e Å−3 |
(C11H18N)4[Mo8O26] | V = 3082.4 (13) Å3 |
Mr = 1840.58 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 15.474 (4) Å | µ = 1.65 mm−1 |
b = 12.051 (3) Å | T = 294 K |
c = 16.592 (4) Å | 0.22 × 0.20 × 0.16 mm |
β = 94.964 (5)° |
Bruker SMART CCD area-detector diffractometer | 5450 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2782 reflections with I > 2σ(I) |
Tmin = 0.698, Tmax = 0.765 | Rint = 0.082 |
15694 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 78 restraints |
wR(F2) = 0.114 | H-atom parameters constrained |
S = 0.95 | Δρmax = 0.63 e Å−3 |
5450 reflections | Δρmin = −0.62 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. |
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 > 2σ(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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.41536 (5) | 0.20179 (6) | 0.04058 (5) | 0.0450 (2) | |
Mo2 | 0.48353 (5) | 0.07732 (7) | 0.20537 (5) | 0.0499 (3) | |
Mo3 | 0.53068 (5) | 0.16326 (7) | −0.12012 (5) | 0.0476 (2) | |
Mo4 | 0.39661 (5) | −0.03796 (6) | −0.04320 (5) | 0.0408 (2) | |
O1 | 0.4177 (4) | 0.3339 (5) | 0.0102 (4) | 0.0603 (18) | |
O2 | 0.3120 (4) | 0.1786 (5) | 0.0627 (4) | 0.0545 (17) | |
O3 | 0.5349 (4) | 0.1230 (6) | 0.2923 (4) | 0.0670 (19) | |
O4 | 0.3787 (4) | 0.0657 (5) | 0.2242 (4) | 0.0588 (18) | |
O5 | 0.4897 (4) | 0.2894 (5) | −0.1449 (4) | 0.0638 (19) | |
O6 | 0.6361 (4) | 0.1711 (5) | −0.1393 (4) | 0.0618 (19) | |
O7 | 0.2955 (3) | −0.0510 (5) | −0.0137 (3) | 0.0504 (16) | |
O8 | 0.4487 (3) | −0.1747 (4) | 0.0012 (3) | 0.0404 (14) | |
O9 | 0.4740 (3) | 0.2126 (5) | 0.1435 (3) | 0.0497 (16) | |
O10 | 0.4588 (3) | 0.0179 (4) | 0.0689 (3) | 0.0412 (14) | |
O11 | 0.4034 (3) | 0.1201 (4) | −0.0639 (3) | 0.0424 (15) | |
O12 | 0.4840 (3) | 0.0770 (5) | −0.2070 (3) | 0.0494 (16) | |
O13 | 0.3885 (3) | −0.0793 (5) | −0.1431 (3) | 0.0484 (15) | |
N1 | 0.2719 (6) | 0.4703 (7) | 0.8434 (5) | 0.063 (2) | |
N2 | 0.1678 (5) | 0.0741 (6) | 0.2113 (5) | 0.0553 (18) | |
C1 | 0.2063 (8) | 0.5384 (10) | 0.8243 (7) | 0.078 (3) | |
H1 | 0.1574 | 0.5123 | 0.7935 | 0.094* | |
C2 | 0.2091 (9) | 0.6445 (10) | 0.8486 (9) | 0.095 (4) | |
H2 | 0.1626 | 0.6918 | 0.8354 | 0.114* | |
C3 | 0.2804 (12) | 0.6813 (11) | 0.8924 (9) | 0.113 (5) | |
H3 | 0.2836 | 0.7549 | 0.9092 | 0.136* | |
C4 | 0.3472 (10) | 0.6120 (14) | 0.9121 (9) | 0.109 (5) | |
H4 | 0.3958 | 0.6377 | 0.9435 | 0.131* | |
C5 | 0.3441 (8) | 0.5047 (11) | 0.8863 (7) | 0.081 (3) | |
H5 | 0.3906 | 0.4569 | 0.8981 | 0.097* | |
C6 | 0.2610 (6) | 0.3530 (8) | 0.8199 (6) | 0.072 (2) | |
H6A | 0.3178 | 0.3195 | 0.8179 | 0.086* | |
H6B | 0.2312 | 0.3490 | 0.7661 | 0.086* | |
C7 | 0.2105 (6) | 0.2877 (8) | 0.8775 (6) | 0.070 (2) | |
H7A | 0.2436 | 0.2828 | 0.9297 | 0.084* | |
H7B | 0.1564 | 0.3254 | 0.8848 | 0.084* | |
C8 | 0.1920 (6) | 0.1735 (8) | 0.8450 (7) | 0.073 (2) | |
H8A | 0.2466 | 0.1354 | 0.8405 | 0.088* | |
H8B | 0.1628 | 0.1796 | 0.7911 | 0.088* | |
C9 | 0.1370 (7) | 0.1045 (9) | 0.8962 (7) | 0.078 (2) | |
H9A | 0.0820 | 0.1418 | 0.9006 | 0.094* | |
H9B | 0.1659 | 0.0978 | 0.9502 | 0.094* | |
C10 | 0.1201 (7) | −0.0099 (9) | 0.8613 (7) | 0.084 (2) | |
H10A | 0.0911 | −0.0031 | 0.8073 | 0.101* | |
H10B | 0.1751 | −0.0471 | 0.8568 | 0.101* | |
C11 | 0.0653 (8) | −0.0788 (10) | 0.9123 (7) | 0.103 (4) | |
H11A | 0.0974 | −0.0949 | 0.9632 | 0.155* | |
H11B | 0.0500 | −0.1470 | 0.8848 | 0.155* | |
H11C | 0.0136 | −0.0387 | 0.9218 | 0.155* | |
C12 | 0.1944 (6) | 0.0055 (8) | 0.1554 (6) | 0.053 (3) | |
H12 | 0.2310 | 0.0314 | 0.1180 | 0.064* | |
C13 | 0.1683 (6) | −0.1019 (9) | 0.1532 (7) | 0.067 (3) | |
H13 | 0.1884 | −0.1507 | 0.1155 | 0.080* | |
C14 | 0.1128 (7) | −0.1372 (9) | 0.2062 (8) | 0.078 (3) | |
H14 | 0.0915 | −0.2094 | 0.2032 | 0.094* | |
C15 | 0.0881 (7) | −0.0664 (11) | 0.2643 (7) | 0.091 (4) | |
H15 | 0.0536 | −0.0917 | 0.3036 | 0.109* | |
C16 | 0.1140 (7) | 0.0401 (10) | 0.2642 (6) | 0.076 (3) | |
H16 | 0.0942 | 0.0900 | 0.3012 | 0.092* | |
C17 | 0.1953 (6) | 0.1912 (7) | 0.2100 (6) | 0.0611 (19) | |
H17A | 0.2547 | 0.1946 | 0.1958 | 0.073* | |
H17B | 0.1939 | 0.2221 | 0.2639 | 0.073* | |
C18 | 0.1401 (6) | 0.2599 (8) | 0.1522 (6) | 0.068 (2) | |
H18A | 0.0831 | 0.2671 | 0.1718 | 0.082* | |
H18B | 0.1332 | 0.2220 | 0.1005 | 0.082* | |
C19 | 0.1760 (7) | 0.3735 (9) | 0.1398 (6) | 0.074 (2) | |
H19A | 0.1864 | 0.4092 | 0.1922 | 0.088* | |
H19B | 0.2316 | 0.3658 | 0.1175 | 0.088* | |
C20 | 0.1206 (7) | 0.4467 (9) | 0.0863 (7) | 0.084 (2) | |
H20A | 0.0653 | 0.4567 | 0.1087 | 0.101* | |
H20B | 0.1096 | 0.4118 | 0.0337 | 0.101* | |
C21 | 0.1629 (8) | 0.5616 (9) | 0.0757 (7) | 0.092 (3) | |
H21A | 0.1800 | 0.5928 | 0.1285 | 0.111* | |
H21B | 0.2147 | 0.5526 | 0.0473 | 0.111* | |
C22 | 0.1029 (8) | 0.6387 (11) | 0.0300 (8) | 0.119 (4) | |
H22A | 0.0886 | 0.6101 | −0.0235 | 0.179* | |
H22B | 0.1302 | 0.7099 | 0.0265 | 0.179* | |
H22C | 0.0510 | 0.6464 | 0.0572 | 0.179* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0468 (5) | 0.0387 (5) | 0.0525 (6) | 0.0037 (4) | 0.0212 (4) | −0.0021 (4) |
Mo2 | 0.0500 (5) | 0.0571 (6) | 0.0447 (6) | 0.0045 (4) | 0.0156 (4) | −0.0054 (4) |
Mo3 | 0.0508 (5) | 0.0426 (5) | 0.0529 (6) | −0.0015 (4) | 0.0245 (4) | 0.0059 (4) |
Mo4 | 0.0381 (4) | 0.0379 (5) | 0.0484 (5) | −0.0023 (4) | 0.0154 (4) | −0.0029 (4) |
O1 | 0.071 (4) | 0.036 (4) | 0.078 (5) | 0.005 (3) | 0.029 (4) | 0.001 (3) |
O2 | 0.048 (4) | 0.059 (4) | 0.061 (4) | 0.003 (3) | 0.027 (3) | 0.004 (3) |
O3 | 0.070 (5) | 0.079 (5) | 0.054 (4) | 0.010 (4) | 0.013 (3) | −0.016 (4) |
O4 | 0.045 (4) | 0.073 (5) | 0.061 (4) | 0.007 (3) | 0.023 (3) | 0.003 (4) |
O5 | 0.073 (5) | 0.053 (4) | 0.069 (5) | 0.004 (4) | 0.027 (4) | 0.017 (4) |
O6 | 0.051 (4) | 0.069 (5) | 0.070 (5) | −0.008 (3) | 0.031 (3) | 0.013 (4) |
O7 | 0.040 (4) | 0.045 (4) | 0.069 (4) | −0.004 (3) | 0.021 (3) | −0.001 (3) |
O8 | 0.043 (3) | 0.038 (3) | 0.043 (4) | 0.001 (3) | 0.020 (3) | −0.001 (3) |
O9 | 0.050 (4) | 0.045 (4) | 0.056 (4) | −0.001 (3) | 0.015 (3) | −0.013 (3) |
O10 | 0.043 (3) | 0.033 (3) | 0.050 (4) | −0.002 (3) | 0.018 (3) | −0.002 (3) |
O11 | 0.040 (3) | 0.042 (4) | 0.046 (4) | 0.003 (3) | 0.015 (3) | 0.007 (3) |
O12 | 0.050 (4) | 0.063 (4) | 0.038 (4) | 0.013 (3) | 0.017 (3) | 0.006 (3) |
O13 | 0.047 (4) | 0.049 (4) | 0.050 (4) | −0.001 (3) | 0.011 (3) | −0.007 (3) |
N1 | 0.065 (6) | 0.053 (6) | 0.072 (6) | −0.011 (5) | 0.011 (5) | 0.000 (5) |
N2 | 0.054 (4) | 0.049 (4) | 0.066 (4) | 0.010 (3) | 0.027 (4) | −0.001 (4) |
C1 | 0.082 (9) | 0.058 (8) | 0.095 (10) | −0.017 (7) | 0.019 (7) | 0.000 (7) |
C2 | 0.100 (11) | 0.055 (9) | 0.133 (13) | −0.013 (7) | 0.020 (9) | −0.009 (8) |
C3 | 0.169 (17) | 0.053 (9) | 0.121 (14) | −0.023 (10) | 0.027 (12) | −0.004 (9) |
C4 | 0.109 (12) | 0.092 (12) | 0.123 (13) | −0.048 (10) | −0.002 (9) | 0.008 (10) |
C5 | 0.082 (9) | 0.081 (10) | 0.080 (9) | −0.010 (7) | 0.007 (7) | 0.018 (7) |
C6 | 0.066 (5) | 0.055 (5) | 0.093 (6) | −0.008 (4) | 0.008 (4) | −0.003 (5) |
C7 | 0.066 (4) | 0.054 (4) | 0.090 (5) | −0.005 (4) | 0.004 (4) | 0.001 (4) |
C8 | 0.070 (4) | 0.057 (4) | 0.093 (5) | −0.002 (4) | 0.004 (4) | 0.003 (4) |
C9 | 0.072 (4) | 0.062 (4) | 0.099 (5) | −0.003 (4) | 0.002 (4) | 0.005 (4) |
C10 | 0.079 (5) | 0.068 (5) | 0.105 (5) | −0.005 (4) | 0.001 (4) | 0.007 (5) |
C11 | 0.101 (5) | 0.096 (5) | 0.111 (5) | −0.003 (4) | 0.001 (4) | 0.006 (4) |
C12 | 0.048 (6) | 0.054 (7) | 0.059 (7) | −0.002 (5) | 0.020 (5) | −0.004 (5) |
C13 | 0.052 (7) | 0.058 (8) | 0.094 (9) | 0.011 (5) | 0.022 (6) | 0.007 (6) |
C14 | 0.070 (8) | 0.048 (7) | 0.117 (11) | 0.008 (6) | 0.013 (7) | 0.013 (7) |
C15 | 0.077 (9) | 0.104 (11) | 0.099 (10) | 0.013 (8) | 0.047 (7) | 0.051 (9) |
C16 | 0.073 (8) | 0.078 (9) | 0.085 (9) | 0.030 (7) | 0.049 (7) | 0.022 (7) |
C17 | 0.064 (4) | 0.053 (4) | 0.070 (4) | 0.007 (4) | 0.024 (4) | −0.005 (4) |
C18 | 0.071 (4) | 0.060 (4) | 0.078 (5) | 0.005 (4) | 0.024 (4) | −0.003 (4) |
C19 | 0.081 (5) | 0.065 (5) | 0.079 (5) | 0.002 (4) | 0.026 (4) | −0.003 (4) |
C20 | 0.091 (5) | 0.077 (5) | 0.086 (5) | 0.003 (4) | 0.025 (4) | −0.001 (4) |
C21 | 0.102 (5) | 0.086 (5) | 0.091 (5) | 0.005 (5) | 0.026 (5) | 0.004 (5) |
C22 | 0.126 (5) | 0.115 (5) | 0.117 (5) | −0.002 (4) | 0.014 (4) | 0.003 (4) |
Mo1—O1 | 1.672 (6) | C6—H6A | 0.9700 |
Mo1—O2 | 1.694 (5) | C6—H6B | 0.9700 |
Mo2—O3 | 1.678 (6) | C7—C8 | 1.496 (12) |
Mo2—O4 | 1.684 (5) | C7—H7A | 0.9700 |
Mo3—O5 | 1.684 (6) | C7—H7B | 0.9700 |
Mo3—O6 | 1.692 (5) | C8—C9 | 1.504 (13) |
Mo4—O7 | 1.686 (5) | C8—H8A | 0.9700 |
Mo1—O9 | 1.867 (6) | C8—H8B | 0.9700 |
Mo2—O12i | 1.925 (6) | C9—C10 | 1.510 (13) |
Mo2—O9 | 1.926 (6) | C9—H9A | 0.9700 |
Mo2—O13i | 2.311 (5) | C9—H9B | 0.9700 |
Mo3—O12 | 1.870 (6) | C10—C11 | 1.501 (14) |
Mo4—O13 | 1.725 (5) | C10—H10A | 0.9700 |
Mo1—O11 | 1.989 (5) | C10—H10B | 0.9700 |
Mo1—O8i | 2.295 (5) | C11—H11A | 0.9600 |
Mo3—O8i | 1.976 (5) | C11—H11B | 0.9600 |
Mo3—O11 | 2.311 (5) | C11—H11C | 0.9600 |
Mo4—O11 | 1.939 (5) | C12—C13 | 1.355 (12) |
Mo4—O8 | 1.951 (5) | C12—H12 | 0.9300 |
Mo2—O10 | 2.374 (5) | C13—C14 | 1.351 (13) |
Mo1—O10 | 2.351 (5) | C13—H13 | 0.9300 |
Mo3—O10i | 2.344 (5) | C14—C15 | 1.367 (15) |
Mo4—O10 | 2.128 (5) | C14—H14 | 0.9300 |
Mo4—O10i | 2.327 (5) | C15—C16 | 1.345 (15) |
Mo1—Mo4 | 3.2085 (13) | C15—H15 | 0.9300 |
Mo1—Mo2 | 3.2154 (14) | C16—H16 | 0.9300 |
Mo3—Mo4i | 3.2188 (13) | C17—C18 | 1.481 (12) |
Mo4—Mo3i | 3.2188 (13) | C17—H17A | 0.9700 |
N1—C1 | 1.322 (12) | C17—H17B | 0.9700 |
N1—C5 | 1.338 (13) | C18—C19 | 1.499 (13) |
N1—C6 | 1.472 (12) | C18—H18A | 0.9700 |
N2—C16 | 1.325 (10) | C18—H18B | 0.9700 |
N2—C12 | 1.333 (10) | C19—C20 | 1.474 (13) |
N2—C17 | 1.475 (11) | C19—H19A | 0.9700 |
C1—C2 | 1.340 (14) | C19—H19B | 0.9700 |
C1—H1 | 0.9300 | C20—C21 | 1.547 (14) |
C2—C3 | 1.342 (17) | C20—H20A | 0.9700 |
C2—H2 | 0.9300 | C20—H20B | 0.9700 |
C3—C4 | 1.347 (17) | C21—C22 | 1.476 (15) |
C3—H3 | 0.9300 | C21—H21A | 0.9700 |
C4—C5 | 1.362 (17) | C21—H21B | 0.9700 |
C4—H4 | 0.9300 | C22—H22A | 0.9600 |
C5—H5 | 0.9300 | C22—H22B | 0.9600 |
C6—C7 | 1.507 (12) | C22—H22C | 0.9600 |
O1—Mo1—O2 | 105.6 (3) | Mo4—O11—Mo3 | 110.7 (2) |
O1—Mo1—O9 | 100.8 (3) | Mo1—O11—Mo3 | 102.8 (2) |
O2—Mo1—O9 | 101.9 (3) | Mo3—O12—Mo2i | 116.3 (3) |
O1—Mo1—O11 | 102.2 (3) | Mo4—O13—Mo2i | 115.7 (3) |
O2—Mo1—O11 | 95.1 (2) | C1—N1—C5 | 121.6 (10) |
O9—Mo1—O11 | 146.4 (2) | C1—N1—C6 | 117.7 (9) |
O1—Mo1—O8i | 90.0 (2) | C5—N1—C6 | 120.6 (10) |
O2—Mo1—O8i | 161.6 (2) | C16—N2—C12 | 121.2 (9) |
O9—Mo1—O8i | 84.3 (2) | C16—N2—C17 | 120.2 (8) |
O11—Mo1—O8i | 71.63 (19) | C12—N2—C17 | 118.5 (8) |
O1—Mo1—O10 | 160.9 (2) | N1—C1—C2 | 121.0 (12) |
O2—Mo1—O10 | 93.4 (2) | N1—C1—H1 | 119.5 |
O9—Mo1—O10 | 77.0 (2) | C2—C1—H1 | 119.5 |
O11—Mo1—O10 | 73.2 (2) | C1—C2—C3 | 118.8 (14) |
O8i—Mo1—O10 | 70.90 (17) | C1—C2—H2 | 120.6 |
O1—Mo1—Mo4 | 136.9 (2) | C3—C2—H2 | 120.6 |
O2—Mo1—Mo4 | 83.9 (2) | C2—C3—C4 | 120.3 (14) |
O9—Mo1—Mo4 | 118.54 (17) | C2—C3—H3 | 119.9 |
O11—Mo1—Mo4 | 34.73 (15) | C4—C3—H3 | 119.9 |
O8i—Mo1—Mo4 | 77.98 (13) | C3—C4—C5 | 120.4 (14) |
O10—Mo1—Mo4 | 41.53 (13) | C3—C4—H4 | 119.8 |
O1—Mo1—Mo2 | 133.4 (2) | C5—C4—H4 | 119.8 |
O2—Mo1—Mo2 | 89.1 (2) | N1—C5—C4 | 117.8 (12) |
O9—Mo1—Mo2 | 32.60 (17) | N1—C5—H5 | 121.1 |
O11—Mo1—Mo2 | 120.61 (16) | C4—C5—H5 | 121.1 |
O8i—Mo1—Mo2 | 87.06 (14) | N1—C6—C7 | 112.8 (8) |
O10—Mo1—Mo2 | 47.42 (13) | N1—C6—H6A | 109.0 |
Mo4—Mo1—Mo2 | 87.65 (3) | C7—C6—H6A | 109.0 |
O3—Mo2—O4 | 105.1 (3) | N1—C6—H6B | 109.0 |
O3—Mo2—O12i | 101.6 (3) | C7—C6—H6B | 109.0 |
O4—Mo2—O12i | 99.9 (3) | H6A—C6—H6B | 107.8 |
O3—Mo2—O9 | 100.9 (3) | C8—C7—C6 | 110.3 (9) |
O4—Mo2—O9 | 98.0 (3) | C8—C7—H7A | 109.6 |
O12i—Mo2—O9 | 146.4 (2) | C6—C7—H7A | 109.6 |
O3—Mo2—O13i | 91.2 (2) | C8—C7—H7B | 109.6 |
O4—Mo2—O13i | 163.7 (3) | C6—C7—H7B | 109.6 |
O12i—Mo2—O13i | 77.5 (2) | H7A—C7—H7B | 108.1 |
O9—Mo2—O13i | 77.4 (2) | C7—C8—C9 | 113.9 (9) |
O3—Mo2—O10 | 160.7 (2) | C7—C8—H8A | 108.8 |
O4—Mo2—O10 | 94.2 (2) | C9—C8—H8A | 108.8 |
O12i—Mo2—O10 | 75.1 (2) | C7—C8—H8B | 108.8 |
O9—Mo2—O10 | 75.4 (2) | C9—C8—H8B | 108.8 |
O13i—Mo2—O10 | 69.54 (18) | H8A—C8—H8B | 107.7 |
O3—Mo2—Mo1 | 132.4 (2) | C8—C9—C10 | 112.0 (9) |
O4—Mo2—Mo1 | 86.9 (2) | C8—C9—H9A | 109.2 |
O12i—Mo2—Mo1 | 121.87 (17) | C10—C9—H9A | 109.2 |
O9—Mo2—Mo1 | 31.49 (17) | C8—C9—H9B | 109.2 |
O13i—Mo2—Mo1 | 81.13 (15) | C10—C9—H9B | 109.2 |
O10—Mo2—Mo1 | 46.81 (13) | H9A—C9—H9B | 107.9 |
O5—Mo3—O6 | 104.6 (3) | C11—C10—C9 | 112.1 (10) |
O5—Mo3—O12 | 101.6 (3) | C11—C10—H10A | 109.2 |
O6—Mo3—O12 | 101.6 (3) | C9—C10—H10A | 109.2 |
O5—Mo3—O8i | 101.9 (3) | C11—C10—H10B | 109.2 |
O6—Mo3—O8i | 96.3 (3) | C9—C10—H10B | 109.2 |
O12—Mo3—O8i | 145.7 (2) | H10A—C10—H10B | 107.9 |
O5—Mo3—O11 | 89.2 (2) | C10—C11—H11A | 109.5 |
O6—Mo3—O11 | 163.4 (2) | C10—C11—H11B | 109.5 |
O12—Mo3—O11 | 84.3 (2) | H11A—C11—H11B | 109.5 |
O8i—Mo3—O11 | 71.48 (19) | C10—C11—H11C | 109.5 |
O5—Mo3—O10i | 160.5 (2) | H11A—C11—H11C | 109.5 |
O6—Mo3—O10i | 94.7 (2) | H11B—C11—H11C | 109.5 |
O12—Mo3—O10i | 76.8 (2) | N2—C12—C13 | 120.1 (9) |
O8i—Mo3—O10i | 72.70 (19) | N2—C12—H12 | 119.9 |
O11—Mo3—O10i | 71.27 (18) | C13—C12—H12 | 119.9 |
O5—Mo3—Mo4i | 136.5 (2) | C14—C13—C12 | 119.2 (10) |
O6—Mo3—Mo4i | 85.0 (2) | C14—C13—H13 | 120.4 |
O12—Mo3—Mo4i | 118.11 (17) | C12—C13—H13 | 120.4 |
O8i—Mo3—Mo4i | 34.68 (15) | C13—C14—C15 | 119.7 (11) |
O11—Mo3—Mo4i | 78.62 (13) | C13—C14—H14 | 120.2 |
O10i—Mo3—Mo4i | 41.35 (13) | C15—C14—H14 | 120.2 |
O7—Mo4—O13 | 105.1 (3) | C16—C15—C14 | 119.6 (10) |
O7—Mo4—O11 | 102.0 (2) | C16—C15—H15 | 120.2 |
O13—Mo4—O11 | 96.5 (2) | C14—C15—H15 | 120.2 |
O7—Mo4—O8 | 100.1 (2) | N2—C16—C15 | 120.0 (10) |
O13—Mo4—O8 | 96.5 (2) | N2—C16—H16 | 120.0 |
O11—Mo4—O8 | 150.4 (2) | C15—C16—H16 | 120.0 |
O7—Mo4—O10 | 97.8 (2) | N2—C17—C18 | 113.2 (8) |
O13—Mo4—O10 | 157.1 (2) | N2—C17—H17A | 108.9 |
O11—Mo4—O10 | 79.4 (2) | C18—C17—H17A | 108.9 |
O8—Mo4—O10 | 78.3 (2) | N2—C17—H17B | 108.9 |
O7—Mo4—O10i | 173.7 (2) | C18—C17—H17B | 108.9 |
O13—Mo4—O10i | 81.1 (2) | H17A—C17—H17B | 107.8 |
O11—Mo4—O10i | 78.36 (19) | C17—C18—C19 | 113.5 (9) |
O8—Mo4—O10i | 77.54 (19) | C17—C18—H18A | 108.9 |
O10—Mo4—O10i | 76.0 (2) | C19—C18—H18A | 108.9 |
O7—Mo4—Mo1 | 90.55 (19) | C17—C18—H18B | 108.9 |
O13—Mo4—Mo1 | 132.26 (19) | C19—C18—H18B | 108.9 |
O11—Mo4—Mo1 | 35.74 (16) | H18A—C18—H18B | 107.7 |
O8—Mo4—Mo1 | 125.31 (16) | C20—C19—C18 | 115.2 (9) |
O10—Mo4—Mo1 | 47.10 (14) | C20—C19—H19A | 108.5 |
O10i—Mo4—Mo1 | 86.19 (13) | C18—C19—H19A | 108.5 |
O7—Mo4—Mo3i | 88.7 (2) | C20—C19—H19B | 108.5 |
O13—Mo4—Mo3i | 131.65 (19) | C18—C19—H19B | 108.5 |
O11—Mo4—Mo3i | 126.12 (16) | H19A—C19—H19B | 107.5 |
O8—Mo4—Mo3i | 35.19 (15) | C19—C20—C21 | 111.9 (10) |
O10—Mo4—Mo3i | 46.69 (14) | C19—C20—H20A | 109.2 |
O10i—Mo4—Mo3i | 86.06 (13) | C21—C20—H20A | 109.2 |
Mo1—Mo4—Mo3i | 92.62 (3) | C19—C20—H20B | 109.2 |
Mo4—O8—Mo3i | 110.1 (2) | C21—C20—H20B | 109.2 |
Mo4—O8—Mo1i | 111.4 (2) | H20A—C20—H20B | 107.9 |
Mo3i—O8—Mo1i | 103.8 (2) | C22—C21—C20 | 111.6 (11) |
Mo1—O9—Mo2 | 115.9 (3) | C22—C21—H21A | 109.3 |
Mo4—O10—Mo4i | 104.0 (2) | C20—C21—H21A | 109.3 |
Mo4—O10—Mo3i | 91.96 (19) | C22—C21—H21B | 109.3 |
Mo4i—O10—Mo3i | 97.19 (19) | C20—C21—H21B | 109.3 |
Mo4—O10—Mo1 | 91.4 (2) | H21A—C21—H21B | 108.0 |
Mo4i—O10—Mo1 | 97.37 (18) | C21—C22—H22A | 109.5 |
Mo3i—O10—Mo1 | 163.8 (2) | C21—C22—H22B | 109.5 |
Mo4—O10—Mo2 | 162.3 (2) | H22A—C22—H22B | 109.5 |
Mo4i—O10—Mo2 | 93.72 (19) | C21—C22—H22C | 109.5 |
Mo3i—O10—Mo2 | 86.24 (18) | H22A—C22—H22C | 109.5 |
Mo1—O10—Mo2 | 85.76 (17) | H22B—C22—H22C | 109.5 |
Mo4—O11—Mo1 | 109.5 (2) | ||
O1—Mo1—Mo2—O3 | −0.1 (4) | O8—Mo4—O10—Mo2 | −101.8 (9) |
O2—Mo1—Mo2—O3 | −110.9 (3) | O10i—Mo4—O10—Mo2 | 178.3 (10) |
O9—Mo1—Mo2—O3 | 3.0 (4) | Mo1—Mo4—O10—Mo2 | 80.4 (8) |
O11—Mo1—Mo2—O3 | 153.7 (3) | Mo3i—Mo4—O10—Mo2 | −83.8 (8) |
O8i—Mo1—Mo2—O3 | 87.1 (3) | O1—Mo1—O10—Mo4 | −96.1 (8) |
O10—Mo1—Mo2—O3 | 153.6 (3) | O2—Mo1—O10—Mo4 | 76.8 (2) |
Mo4—Mo1—Mo2—O3 | 165.2 (3) | O9—Mo1—O10—Mo4 | 178.2 (2) |
O1—Mo1—Mo2—O4 | 107.6 (3) | O11—Mo1—O10—Mo4 | −17.47 (18) |
O2—Mo1—Mo2—O4 | −3.2 (3) | O8i—Mo1—O10—Mo4 | −93.4 (2) |
O9—Mo1—Mo2—O4 | 110.7 (4) | Mo2—Mo1—O10—Mo4 | 162.5 (2) |
O11—Mo1—Mo2—O4 | −98.6 (3) | O1—Mo1—O10—Mo4i | 8.2 (9) |
O8i—Mo1—Mo2—O4 | −165.2 (2) | O2—Mo1—O10—Mo4i | −178.9 (2) |
O10—Mo1—Mo2—O4 | −98.7 (3) | O9—Mo1—O10—Mo4i | −77.5 (2) |
Mo4—Mo1—Mo2—O4 | −87.1 (2) | O11—Mo1—O10—Mo4i | 86.8 (2) |
O1—Mo1—Mo2—O12i | −152.7 (3) | O8i—Mo1—O10—Mo4i | 10.94 (18) |
O2—Mo1—Mo2—O12i | 96.5 (3) | Mo4—Mo1—O10—Mo4i | 104.3 (2) |
O9—Mo1—Mo2—O12i | −149.6 (4) | Mo2—Mo1—O10—Mo4i | −93.2 (2) |
O11—Mo1—Mo2—O12i | 1.1 (3) | O1—Mo1—O10—Mo3i | 162.0 (9) |
O8i—Mo1—Mo2—O12i | −65.6 (2) | O2—Mo1—O10—Mo3i | −25.0 (10) |
O10—Mo1—Mo2—O12i | 1.0 (2) | O9—Mo1—O10—Mo3i | 76.4 (10) |
Mo4—Mo1—Mo2—O12i | 12.53 (19) | O11—Mo1—O10—Mo3i | −119.3 (10) |
O1—Mo1—Mo2—O9 | −3.2 (4) | O8i—Mo1—O10—Mo3i | 164.8 (10) |
O2—Mo1—Mo2—O9 | −114.0 (4) | Mo4—Mo1—O10—Mo3i | −101.9 (10) |
O11—Mo1—Mo2—O9 | 150.7 (3) | Mo2—Mo1—O10—Mo3i | 60.6 (9) |
O8i—Mo1—Mo2—O9 | 84.0 (3) | O1—Mo1—O10—Mo2 | 101.4 (8) |
O10—Mo1—Mo2—O9 | 150.6 (3) | O2—Mo1—O10—Mo2 | −85.7 (2) |
Mo4—Mo1—Mo2—O9 | 162.1 (3) | O9—Mo1—O10—Mo2 | 15.75 (18) |
O1—Mo1—Mo2—O13i | −83.5 (3) | O11—Mo1—O10—Mo2 | −180.0 (2) |
O2—Mo1—Mo2—O13i | 165.7 (2) | O8i—Mo1—O10—Mo2 | 104.2 (2) |
O9—Mo1—Mo2—O13i | −80.4 (3) | Mo4—Mo1—O10—Mo2 | −162.5 (2) |
O11—Mo1—Mo2—O13i | 70.3 (2) | O3—Mo2—O10—Mo4 | −177.9 (8) |
O8i—Mo1—Mo2—O13i | 3.65 (19) | O4—Mo2—O10—Mo4 | 0.6 (9) |
O10—Mo1—Mo2—O13i | 70.2 (2) | O12i—Mo2—O10—Mo4 | 99.7 (9) |
Mo4—Mo1—Mo2—O13i | 81.73 (14) | O9—Mo2—O10—Mo4 | −96.6 (9) |
O1—Mo1—Mo2—O10 | −153.8 (3) | O13i—Mo2—O10—Mo4 | −178.4 (9) |
O2—Mo1—Mo2—O10 | 95.4 (3) | Mo1—Mo2—O10—Mo4 | −81.2 (8) |
O9—Mo1—Mo2—O10 | −150.6 (3) | O3—Mo2—O10—Mo4i | 0.5 (9) |
O11—Mo1—Mo2—O10 | 0.1 (2) | O4—Mo2—O10—Mo4i | 178.9 (2) |
O8i—Mo1—Mo2—O10 | −66.6 (2) | O12i—Mo2—O10—Mo4i | −82.0 (2) |
Mo4—Mo1—Mo2—O10 | 11.52 (16) | O9—Mo2—O10—Mo4i | 81.8 (2) |
O1—Mo1—Mo4—O7 | −108.3 (4) | O13i—Mo2—O10—Mo4i | −0.02 (17) |
O2—Mo1—Mo4—O7 | −2.0 (3) | Mo1—Mo2—O10—Mo4i | 97.12 (18) |
O9—Mo1—Mo4—O7 | 98.2 (3) | O3—Mo2—O10—Mo3i | 97.4 (8) |
O11—Mo1—Mo4—O7 | −110.1 (3) | O4—Mo2—O10—Mo3i | −84.1 (2) |
O8i—Mo1—Mo4—O7 | 174.9 (2) | O12i—Mo2—O10—Mo3i | 14.98 (19) |
O10—Mo1—Mo4—O7 | 100.2 (3) | O9—Mo2—O10—Mo3i | 178.7 (2) |
Mo2—Mo1—Mo4—O7 | 87.4 (2) | O13i—Mo2—O10—Mo3i | 97.0 (2) |
O1—Mo1—Mo4—O13 | 2.8 (4) | Mo1—Mo2—O10—Mo3i | −165.9 (2) |
O2—Mo1—Mo4—O13 | 109.1 (3) | O3—Mo2—O10—Mo1 | −96.7 (8) |
O9—Mo1—Mo4—O13 | −150.6 (3) | O4—Mo2—O10—Mo1 | 81.8 (2) |
O11—Mo1—Mo4—O13 | 1.0 (3) | O12i—Mo2—O10—Mo1 | −179.1 (2) |
O8i—Mo1—Mo4—O13 | −74.0 (3) | O9—Mo2—O10—Mo1 | −15.36 (18) |
O10—Mo1—Mo4—O13 | −148.7 (3) | O13i—Mo2—O10—Mo1 | −97.14 (19) |
Mo2—Mo1—Mo4—O13 | −161.5 (2) | O7—Mo4—O11—Mo1 | 73.8 (3) |
O1—Mo1—Mo4—O11 | 1.8 (4) | O13—Mo4—O11—Mo1 | −179.2 (3) |
O2—Mo1—Mo4—O11 | 108.1 (3) | O8—Mo4—O11—Mo1 | −63.7 (5) |
O9—Mo1—Mo4—O11 | −151.7 (3) | O10—Mo4—O11—Mo1 | −22.1 (2) |
O8i—Mo1—Mo4—O11 | −75.0 (3) | O10i—Mo4—O11—Mo1 | −99.8 (3) |
O10—Mo1—Mo4—O11 | −149.7 (3) | Mo3i—Mo4—O11—Mo1 | −23.5 (3) |
Mo2—Mo1—Mo4—O11 | −162.5 (2) | O7—Mo4—O11—Mo3 | −173.5 (3) |
O1—Mo1—Mo4—O8 | 148.9 (3) | O13—Mo4—O11—Mo3 | −66.6 (3) |
O2—Mo1—Mo4—O8 | −104.8 (3) | O8—Mo4—O11—Mo3 | 48.9 (5) |
O9—Mo1—Mo4—O8 | −4.5 (3) | O10—Mo4—O11—Mo3 | 90.6 (2) |
O11—Mo1—Mo4—O8 | 147.1 (3) | O10i—Mo4—O11—Mo3 | 12.9 (2) |
O8i—Mo1—Mo4—O8 | 72.1 (2) | Mo1—Mo4—O11—Mo3 | 112.7 (3) |
O10—Mo1—Mo4—O8 | −2.6 (2) | Mo3i—Mo4—O11—Mo3 | 89.2 (2) |
Mo2—Mo1—Mo4—O8 | −15.39 (17) | O1—Mo1—O11—Mo4 | −178.8 (3) |
O1—Mo1—Mo4—O10 | 151.5 (4) | O2—Mo1—O11—Mo4 | −71.6 (3) |
O2—Mo1—Mo4—O10 | −102.2 (3) | O9—Mo1—O11—Mo4 | 48.9 (5) |
O9—Mo1—Mo4—O10 | −2.0 (3) | O8i—Mo1—O11—Mo4 | 95.4 (3) |
O11—Mo1—Mo4—O10 | 149.7 (3) | O10—Mo1—O11—Mo4 | 20.4 (2) |
O8i—Mo1—Mo4—O10 | 74.7 (2) | Mo2—Mo1—O11—Mo4 | 20.4 (3) |
Mo2—Mo1—Mo4—O10 | −12.82 (18) | O1—Mo1—O11—Mo3 | 63.5 (3) |
O1—Mo1—Mo4—O10i | 77.1 (3) | O2—Mo1—O11—Mo3 | 170.7 (2) |
O2—Mo1—Mo4—O10i | −176.6 (2) | O9—Mo1—O11—Mo3 | −68.8 (5) |
O9—Mo1—Mo4—O10i | −76.4 (2) | O8i—Mo1—O11—Mo3 | −22.35 (18) |
O11—Mo1—Mo4—O10i | 75.3 (3) | O10—Mo1—O11—Mo3 | −97.3 (2) |
O8i—Mo1—Mo4—O10i | 0.28 (19) | Mo4—Mo1—O11—Mo3 | −117.7 (3) |
O10—Mo1—Mo4—O10i | −74.4 (2) | Mo2—Mo1—O11—Mo3 | −97.32 (18) |
Mo2—Mo1—Mo4—O10i | −87.21 (14) | O5—Mo3—O11—Mo4 | 166.5 (3) |
O1—Mo1—Mo4—Mo3i | 163.0 (3) | O6—Mo3—O11—Mo4 | −46.8 (10) |
O2—Mo1—Mo4—Mo3i | −90.7 (2) | O12—Mo3—O11—Mo4 | 64.7 (3) |
O9—Mo1—Mo4—Mo3i | 9.51 (18) | O8i—Mo3—O11—Mo4 | −90.7 (3) |
O11—Mo1—Mo4—Mo3i | 161.2 (2) | O10i—Mo3—O11—Mo4 | −13.2 (2) |
O8i—Mo1—Mo4—Mo3i | 86.15 (14) | Mo4i—Mo3—O11—Mo4 | −55.5 (2) |
O10—Mo1—Mo4—Mo3i | 11.47 (18) | O5—Mo3—O11—Mo1 | −76.6 (3) |
Mo2—Mo1—Mo4—Mo3i | −1.34 (3) | O6—Mo3—O11—Mo1 | 70.1 (9) |
O7—Mo4—O8—Mo3i | −73.0 (3) | O12—Mo3—O11—Mo1 | −178.4 (3) |
O13—Mo4—O8—Mo3i | −179.7 (3) | O8i—Mo3—O11—Mo1 | 26.2 (2) |
O11—Mo4—O8—Mo3i | 64.8 (5) | O10i—Mo3—O11—Mo1 | 103.7 (2) |
O10—Mo4—O8—Mo3i | 23.0 (2) | Mo4i—Mo3—O11—Mo1 | 61.42 (18) |
O10i—Mo4—O8—Mo3i | 101.0 (3) | O5—Mo3—O12—Mo2i | 178.7 (3) |
Mo1—Mo4—O8—Mo3i | 24.9 (3) | O6—Mo3—O12—Mo2i | 70.9 (3) |
O7—Mo4—O8—Mo1i | 172.3 (3) | O8i—Mo3—O12—Mo2i | −48.9 (5) |
O13—Mo4—O8—Mo1i | 65.7 (3) | O11—Mo3—O12—Mo2i | −93.3 (3) |
O11—Mo4—O8—Mo1i | −49.8 (5) | O10i—Mo3—O12—Mo2i | −21.3 (2) |
O10—Mo4—O8—Mo1i | −91.7 (2) | Mo4i—Mo3—O12—Mo2i | −19.5 (3) |
O10i—Mo4—O8—Mo1i | −13.6 (2) | O7—Mo4—O13—Mo2i | −178.5 (3) |
Mo1—Mo4—O8—Mo1i | −89.8 (2) | O11—Mo4—O13—Mo2i | 77.1 (3) |
Mo3i—Mo4—O8—Mo1i | −114.7 (4) | O8—Mo4—O13—Mo2i | −76.2 (3) |
O1—Mo1—O9—Mo2 | 177.7 (3) | O10—Mo4—O13—Mo2i | −1.2 (8) |
O2—Mo1—O9—Mo2 | 69.0 (3) | O10i—Mo4—O13—Mo2i | 0.0 (3) |
O11—Mo1—O9—Mo2 | −49.7 (5) | Mo1—Mo4—O13—Mo2i | 76.5 (3) |
O8i—Mo1—O9—Mo2 | −93.4 (3) | Mo3i—Mo4—O13—Mo2i | −76.5 (3) |
O10—Mo1—O9—Mo2 | −21.8 (2) | C5—N1—C1—C2 | −1.2 (17) |
Mo4—Mo1—O9—Mo2 | −20.4 (3) | C6—N1—C1—C2 | 175.2 (10) |
O3—Mo2—O9—Mo1 | −177.7 (3) | N1—C1—C2—C3 | 1 (2) |
O4—Mo2—O9—Mo1 | −70.6 (3) | C1—C2—C3—C4 | −1 (2) |
O12i—Mo2—O9—Mo1 | 50.9 (6) | C2—C3—C4—C5 | 1 (2) |
O13i—Mo2—O9—Mo1 | 93.5 (3) | C1—N1—C5—C4 | 1.9 (17) |
O10—Mo2—O9—Mo1 | 21.7 (2) | C6—N1—C5—C4 | −174.4 (10) |
O7—Mo4—O10—Mo4i | 178.6 (2) | C3—C4—C5—N1 | −2 (2) |
O13—Mo4—O10—Mo4i | 1.3 (7) | C1—N1—C6—C7 | −80.5 (12) |
O11—Mo4—O10—Mo4i | −80.5 (2) | C5—N1—C6—C7 | 95.9 (11) |
O8—Mo4—O10—Mo4i | 79.9 (2) | N1—C6—C7—C8 | 172.8 (9) |
O10i—Mo4—O10—Mo4i | 0.0 | C6—C7—C8—C9 | −176.4 (9) |
Mo1—Mo4—O10—Mo4i | −97.9 (2) | C7—C8—C9—C10 | −179.9 (9) |
Mo3i—Mo4—O10—Mo4i | 97.9 (2) | C8—C9—C10—C11 | 179.9 (10) |
O7—Mo4—O10—Mo3i | 80.7 (2) | C16—N2—C12—C13 | −1.7 (15) |
O13—Mo4—O10—Mo3i | −96.7 (6) | C17—N2—C12—C13 | −178.0 (9) |
O11—Mo4—O10—Mo3i | −178.4 (2) | N2—C12—C13—C14 | 2.3 (16) |
O8—Mo4—O10—Mo3i | −18.00 (17) | C12—C13—C14—C15 | −4.0 (17) |
O10i—Mo4—O10—Mo3i | −97.9 (2) | C13—C14—C15—C16 | 5.1 (19) |
Mo1—Mo4—O10—Mo3i | 164.2 (2) | C12—N2—C16—C15 | 2.7 (17) |
O7—Mo4—O10—Mo1 | −83.4 (2) | C17—N2—C16—C15 | 179.0 (10) |
O13—Mo4—O10—Mo1 | 99.2 (6) | C14—C15—C16—N2 | −4.4 (19) |
O11—Mo4—O10—Mo1 | 17.44 (17) | C16—N2—C17—C18 | −93.2 (11) |
O8—Mo4—O10—Mo1 | 177.9 (2) | C12—N2—C17—C18 | 83.2 (10) |
O10i—Mo4—O10—Mo1 | 97.9 (2) | N2—C17—C18—C19 | −170.0 (8) |
Mo3i—Mo4—O10—Mo1 | −164.2 (2) | C17—C18—C19—C20 | −176.7 (9) |
O7—Mo4—O10—Mo2 | −3.1 (9) | C18—C19—C20—C21 | −179.2 (9) |
O13—Mo4—O10—Mo2 | 179.6 (7) | C19—C20—C21—C22 | −173.3 (10) |
O11—Mo4—O10—Mo2 | 97.8 (9) |
Symmetry code: (i) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C19—H19A···O4ii | 0.97 | 2.60 | 3.391 (12) | 139 |
C17—H17B···O6iii | 0.97 | 2.30 | 3.200 (11) | 154 |
C17—H17A···O4 | 0.97 | 2.48 | 3.207 (11) | 131 |
C17—H17A···O2 | 0.97 | 2.46 | 3.166 (10) | 130 |
C16—H16···O5iii | 0.93 | 2.40 | 3.271 (11) | 155 |
C15—H15···O9iv | 0.93 | 2.56 | 3.257 (13) | 132 |
C12—H12···O2 | 0.93 | 2.40 | 3.243 (11) | 151 |
C7—H7B···O3iii | 0.97 | 2.40 | 3.143 (12) | 133 |
C5—H5···O1v | 0.93 | 2.39 | 3.059 (13) | 129 |
C4—H4···O8vi | 0.93 | 2.56 | 3.295 (15) | 136 |
C1—H1···O3iii | 0.93 | 2.50 | 3.295 (13) | 144 |
Symmetry codes: (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1/2, −y+1/2, z+1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) x, y, z+1; (vi) x, y+1, z+1. |
Experimental details
Crystal data | |
Chemical formula | (C11H18N)4[Mo8O26] |
Mr | 1840.58 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 15.474 (4), 12.051 (3), 16.592 (4) |
β (°) | 94.964 (5) |
V (Å3) | 3082.4 (13) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.65 |
Crystal size (mm) | 0.22 × 0.20 × 0.16 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.698, 0.765 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15694, 5450, 2782 |
Rint | 0.082 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.114, 0.95 |
No. of reflections | 5450 |
No. of parameters | 370 |
No. of restraints | 78 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.63, −0.62 |
Computer programs: SMART (Bruker 1997), SAINT (Bruker 1997), SAINT, SHELXTL (Bruker, 2001), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
C19—H19A···O4i | 0.97 | 2.60 | 3.391 (12) | 139.4 |
C17—H17B···O6ii | 0.97 | 2.30 | 3.200 (11) | 154.1 |
C17—H17A···O4 | 0.97 | 2.48 | 3.207 (11) | 131.4 |
C17—H17A···O2 | 0.97 | 2.46 | 3.166 (10) | 129.7 |
C16—H16···O5ii | 0.93 | 2.40 | 3.271 (11) | 155.1 |
C15—H15···O9iii | 0.93 | 2.56 | 3.257 (13) | 131.6 |
C12—H12···O2 | 0.93 | 2.40 | 3.243 (11) | 150.7 |
C7—H7B···O3ii | 0.97 | 2.40 | 3.143 (12) | 132.6 |
C5—H5···O1iv | 0.93 | 2.39 | 3.059 (13) | 129.1 |
C4—H4···O8v | 0.93 | 2.56 | 3.295 (15) | 136.0 |
C1—H1···O3ii | 0.93 | 2.50 | 3.295 (13) | 143.7 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) x, y, z+1; (v) x, y+1, z+1. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
Polymolybdates have attracted considerable interest for application in selective catalysis of oxidation reactions with hydrogen peroxide. The synthesis and crystal structure reported here is part of this study (Guo and Li, 2007).
The title compound, (I), consists of a centrosymmetric β-octamolybdate anion and four n-hexylpyridinium cations. The structure of the anion is constructed from an array of eight edge-shared MoO6 octahedra. The Mo–O bond lengths can be grouped into four sets: Mo–O(t) 1.672 (6)–1.694 (5) Å, Mo–O(µ2) 1.725 (5)–2.311 (5) Å, Mo–O(µ3) 1.939 (5)–2.311 (5) Å, Mo–O(µ5) 2.128 (5)–2.374 (5) Å. The molecule of the compound is shown in Fig. 1.
In the structure of (I), no classic hydrogen bonds are found, but there exist a number of weak C–H···O interactions (see Table 1). These are further loosely aggregated into a three-dimensional framework via van der Waals forces. A packing diagram for the structure of (I) is shown in Fig. 2.