research communications
Synthesis and
of a new hybrid organic–inorganic material containing neutral molecules, cations and heptamolybdate anionsaLaboratoire de Chimie Minérale et Analytique, Département de Chimie, Faculté des Sciences et Téchniques, Université Cheikh Anta Diop, Dakar, Senegal, bLaboratoire de Chimie et de Physique des Matériaux (LCPM) de l'Université Assane Seck de Ziguinchor (UASZ), BP 523 Ziguinchor, Senegal, and cService Commun d'Analyse par Diffraction des Rayons X, Universite de Bretagne Occidentale, 6, avenue Victor Le Gorgeu, CS 93837, F-29238 Brest cedex 3, France
*Correspondence e-mail: bouks89@gmail.com
The title compound, hexakis(2-methyl-1H-imidazol-3-ium) heptamolybdate 2-methyl-1H-imidazole disolvate dihydrate, (C4H7N2)6[Mo7O24]·2C4H6N2·2H2O, was prepared from 2-methylimidazole and ammonium heptamolybdate tetrahydrate in acid solution. The [Mo7O24]6− heptamolybdate cluster anion is accompanied by six protonated (C4H7N2)+ 2-methylimidazolium cations, two neutral C4H6N2 2-methylimidazole molecules and two water molecules of crystallization. The cluster consists of seven distorted MoO6 octahedra sharing edges or vertices. In the crystal, the components are linked by N—H⋯N, N—H⋯O, O—H⋯O, N—H⋯(O,O) and O—H⋯(O,O) hydrogen bonds, generating a three-dimensional network. Weak C—H⋯O interactions consolidate the packing.
CCDC reference: 1922927
1. Chemical context
Polyoxometalates (POMs) are clusters of transition metals (M = V, Nb, Ta, Mo, W, ⋯) and oxygen atoms with a structural and compositional diversity that lead to numerous applications because of their electrochemical, optical, catalytic and photochromic properties as well as their antiviral and antitumor activities (Katsoulis, 1998; Hasenknopf, 2005; Gerth et al., 2005; Coué et al., 2007). In this context, the [Mo7O24]6− heptamolybdate anion has been isolated with numerous different counter-cations such as 4-aminopyridinium, N-pentylammonium, diethylenetriammonium, N,N,N′,N′-tetramethylethylenediammonium, tetramethylammonium, guanidinium, hexanediammonium, butan-1-aminium, ammonium, potassium and sodium (Román et al., 1985, 1988, 1990, 1992; Don & Weakly, 1981; Gatehouse & Leverett, 1968; Sjöbom & Hedman, 1973; Niu et al., 1996; Himeno et al., 1997; Reinoso et al., 2008; Ftini, 2015; Khandolkar et al., 2016). As a continuation of our work in this area (Sarr et al., 2018), we now describe the synthesis and structure of the title compound (I), which is notable for the incorporation of both protonated [C4H7N2]+ 2-methylimidazolium cations and neutral C4H6N2 2-methylimidazole molecules in the crystal.
2. Structural commentary
The title compound is characterized by the presence of the familiar [Mo7O24]6− heptamolybdate cluster anion (Fig. 1).
There are four categories of oxygen atoms within the polyanion: Ot (terminal oxygen atoms), μ2-O (oxygen atoms bridging two molybdenum atoms), μ3-O (oxygen atoms bridging three molybdenum atoms) and μ4-O (oxygen atoms bridging four molybdenum atoms). All of the Mo atoms are bound to two terminal oxygen atoms except for Mo7, which is located in the `core' of the cluster. The geometrical data for the cluster in (I) are consistent with those found in previous studies (Román et al., 1992; Reinoso et al., 2008): the Mo—O bond lengths vary between 1.707 (2) and 1.726 (2) Å for Ot, 1.754 (2)—2.453 (2) Å for μ2-O, 1.8945 (19)–2.3057 (19) Å for μ3-O and 2.1329 (19)–2.3011 (18) Å for μ4-O. The variations of Mo—O bond lengths and O—Mo—O angles indicate that all seven octahedra (MoO6) within the cluster are highly distorted. As in the compound (H3dien)2[Mo7O24]·4H2O (Román et al., 1988), we note that the longest Mo—O bond length derives from an oxygen atom bridging two molybdenum atoms (μ2-O). As well as the [Mo7O24]6− anion, six (C4H7N2)+ cations, two neutral C4H6N2 molecules and two water molecules of crystallization are present in the (Fig. 2).
3. Supramolecular features
In the crystal, each heptamolybdate anion interacts with six neighbours via the water molecules, (C4H7N2)+ cations and/or neutral 2-methylimidazole molecules (Fig. 3). These interactions occur through simple O—H⋯O, N—H⋯O and N—H⋯N and bifurcated N—H⋯(O,O) and O—H⋯(O,O) hydrogen bonds (Table 1) involving three categories of oxygen atoms of the polyanion: Ot, μ2-O and μ3-O. The N—H⋯N hydrogen bonds from N9 and N12 link (C4H7N2)+ cations to neutral molecules. The packing is consolidated by weak C—H⋯O links (Table 1). The overall hydrogen-bonding topology is an infinite three-dimensional network.
4. Database survey
A search of the Cambridge Structural Database (CSD, version 5.40, update November 2018; Groom et al., 2016) resulted in 35 hits for the heptamolybdate anion and 90 hits for the 2-methylimidazolium cation.
5. Synthesis and crystallization
Sulfuric acid (2.1 g, 21.7 mmol), 2-methylimidazole (3.5 g, 43.4 mmol) and ammonium heptamolybdate tetrahydrate (2.2 g, 1.8 mmol) in a ratio of 1:2:1/12 were dissolved in water (60 ml). The solution was stirred for one h and evaporated in the oven at 333 K to yield a whitish precipitate. The precipitate was recrystallized from methanol solution: after two weeks at room temperature, colourless prisms of (I) were recovered.
The IR spectrum of (I) is included in the supporting information. The absorption bands at 3400 and 3395 cm−1 correspond to ν(O—H) stretches and indicate the presence of water molecules and those at 1621 and 1564 cm−1 to the deformation vibrations δ(O—H). The bands centered at 3132 and 1431 cm−1 with shoulders are respectively attributed to the stretching and deformation vibrations of the N—H bonds of the protonated and/or non-protonated entities of 2-methylimidazole (Jinnah et al., 2004). The bands between 2904–2686 cm−1 are attributed to the stretching vibrations of the C—H bonds, while that at 1291 cm−1 is a δ(C—H) deformation vibration (Jinnah et al., 2004). The two bands at 929 and 900 cm−1 correspond to ν(Mo—Ot) stretching vibrations while the bands between 838 and 650 cm−1 are typical for the vibrations of ν(Mo—O—Mo) and ν[Mo—(μ-O)] groupings (Dey et al., 2011).
6. details
Crystal data, data collection and structure . All H atoms treated by a mixture of independent and were placed in geometrically idealized positions and constrained to ride on their parent atoms, with N—H distances of 0.87 (2), 0.88 (2) and 0.89 (2) Å, Cmethyl—H = 0.97/0.98 Å and Cmethine—H = 0.94/0.95 Å, and with Uiso (H) = 1.2Ueq(C,N) or 1.5Ueq(C-methyl).
details are summarized in Table 2
|
Supporting information
CCDC reference: 1922927
https://doi.org/10.1107/S2056989019008454/hb7831sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989019008454/hb7831Isup2.hkl
The IR spectrum of compound (I). DOI: https://doi.org/10.1107/S2056989019008454/hb7831sup3.tif
Data collection: CrysAlis PRO (Agilent, 2014); cell
CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRO (Agilent, 2014); program(s) used to solve structure: SIR92 (Altomare et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008); software used to prepare material for publication: WinGX (Farrugia, 2012) and PLATON (Spek, 2009).(C4H7N2)6[Mo7O24]·2C4H6N2·2H2O | F(000) = 3456 |
Mr = 1754.52 | Dx = 2.016 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 38522 reflections |
a = 16.5325 (2) Å | θ = 3.5–37.4° |
b = 17.5842 (2) Å | µ = 1.56 mm−1 |
c = 19.8873 (2) Å | T = 170 K |
β = 90.653 (1)° | Fragment of prism, colourless |
V = 5781.08 (11) Å3 | 0.38 × 0.28 × 0.19 mm |
Z = 4 |
Agilent Xcalibur, Sapphire2, large Be window diffractometer | 27993 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 21593 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 8.3622 pixels mm-1 | θmax = 36.3°, θmin = 3.3° |
ω scans | h = −24→27 |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | k = −29→29 |
Tmin = 0.476, Tmax = 0.756 | l = −33→33 |
104921 measured reflections |
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) = 0.120 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.15 | w = 1/[σ2(Fo2) + (0.0397P)2 + 11.2859P] where P = (Fo2 + 2Fc2)/3 |
27993 reflections | (Δ/σ)max = 0.011 |
792 parameters | Δρmax = 1.83 e Å−3 |
58 restraints | Δρmin = −2.87 e Å−3 |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 | ||
O1 | −0.04305 (13) | 0.24793 (14) | 0.39565 (12) | 0.0280 (4) | |
O2 | 0.00551 (14) | 0.27946 (14) | 0.26843 (11) | 0.0284 (5) | |
O3 | 0.07596 (13) | 0.15830 (12) | 0.34241 (10) | 0.0230 (4) | |
O4 | 0.07336 (14) | 0.12579 (14) | 0.48407 (11) | 0.0269 (4) | |
O5 | 0.15457 (15) | 0.03530 (13) | 0.39571 (12) | 0.0295 (5) | |
O6 | 0.23807 (12) | 0.13563 (11) | 0.47918 (9) | 0.0185 (3) | |
O7 | 0.40034 (14) | 0.12283 (14) | 0.50582 (12) | 0.0284 (5) | |
O8 | 0.33831 (15) | 0.04054 (13) | 0.40157 (12) | 0.0280 (4) | |
O9 | 0.42573 (14) | 0.16391 (13) | 0.36926 (12) | 0.0268 (4) | |
O10 | 0.52563 (15) | 0.25984 (16) | 0.44633 (15) | 0.0364 (6) | |
O11 | 0.50709 (16) | 0.28585 (17) | 0.31122 (14) | 0.0393 (6) | |
O12 | 0.41549 (13) | 0.37036 (12) | 0.40412 (11) | 0.0223 (4) | |
O13 | 0.39387 (13) | 0.34235 (15) | 0.54308 (11) | 0.0277 (4) | |
O14 | 0.32385 (14) | 0.46326 (12) | 0.47845 (11) | 0.0246 (4) | |
O15 | 0.23109 (12) | 0.33656 (12) | 0.51719 (9) | 0.0197 (3) | |
O16 | 0.06318 (13) | 0.33595 (15) | 0.52098 (11) | 0.0278 (5) | |
O17 | 0.13927 (14) | 0.45859 (13) | 0.46625 (11) | 0.0251 (4) | |
O18 | 0.06704 (13) | 0.36491 (12) | 0.37905 (10) | 0.0213 (4) | |
O19 | 0.16800 (13) | 0.28094 (12) | 0.28601 (10) | 0.0227 (4) | |
O20 | 0.24914 (12) | 0.16416 (11) | 0.35550 (9) | 0.0191 (3) | |
O21 | 0.33322 (14) | 0.28445 (13) | 0.29412 (11) | 0.0253 (4) | |
O22 | 0.24226 (12) | 0.36427 (11) | 0.39099 (9) | 0.0171 (3) | |
O23 | 0.14447 (11) | 0.25197 (11) | 0.41666 (9) | 0.0164 (3) | |
O24 | 0.33781 (11) | 0.25392 (11) | 0.42940 (9) | 0.0172 (3) | |
Mo1 | 0.042356 (14) | 0.264056 (14) | 0.348758 (11) | 0.01907 (5) | |
Mo2 | 0.142420 (14) | 0.128403 (13) | 0.420960 (11) | 0.01805 (4) | |
Mo3 | 0.342279 (14) | 0.130828 (14) | 0.434127 (12) | 0.01888 (4) | |
Mo4 | 0.454713 (15) | 0.269540 (15) | 0.383726 (13) | 0.02328 (5) | |
Mo5 | 0.333156 (14) | 0.365314 (13) | 0.475739 (11) | 0.01745 (4) | |
Mo6 | 0.134696 (14) | 0.360541 (13) | 0.463691 (11) | 0.01669 (4) | |
Mo7 | 0.248954 (14) | 0.271359 (12) | 0.343147 (10) | 0.01554 (4) | |
C1 | 0.2405 (3) | 0.0776 (2) | 0.1309 (2) | 0.0436 (9) | |
H1 | 0.235 | 0.0891 | 0.0844 | 0.052* | |
C2 | 0.2374 (3) | 0.1281 (2) | 0.18283 (19) | 0.0366 (8) | |
H2 | 0.2294 | 0.1814 | 0.1794 | 0.044* | |
C3 | 0.25571 (18) | 0.01393 (18) | 0.22512 (16) | 0.0243 (5) | |
C4 | 0.2682 (3) | −0.0505 (2) | 0.2726 (2) | 0.0466 (10) | |
H4A | 0.2705 | −0.031 | 0.3188 | 0.07* | |
H4B | 0.3192 | −0.0763 | 0.2623 | 0.07* | |
H4C | 0.2233 | −0.0865 | 0.2681 | 0.07* | |
N1 | 0.25288 (17) | 0.00771 (16) | 0.15858 (13) | 0.0265 (5) | |
N2 | 0.24786 (16) | 0.08720 (15) | 0.24065 (13) | 0.0236 (5) | |
H1N | 0.255 (2) | −0.0354 (12) | 0.1362 (13) | 0.028* | |
H2N | 0.248 (2) | 0.1084 (15) | 0.2801 (10) | 0.028* | |
C5 | 0.4466 (3) | 0.0710 (3) | 0.1457 (2) | 0.0472 (10) | |
H5 | 0.4409 | 0.0769 | 0.0984 | 0.057* | |
C6 | 0.4432 (3) | 0.1273 (3) | 0.1927 (2) | 0.0429 (9) | |
H6 | 0.4352 | 0.1801 | 0.1847 | 0.051* | |
C7 | 0.46291 (19) | 0.0184 (2) | 0.2452 (2) | 0.0338 (7) | |
C8 | 0.4797 (3) | −0.0370 (3) | 0.3006 (2) | 0.0458 (10) | |
H8A | 0.5322 | −0.0253 | 0.3215 | 0.069* | |
H8B | 0.4807 | −0.0887 | 0.2822 | 0.069* | |
H8C | 0.4372 | −0.0333 | 0.3344 | 0.069* | |
N3 | 0.45995 (18) | 0.00367 (19) | 0.18011 (18) | 0.0356 (7) | |
N4 | 0.45352 (17) | 0.09260 (18) | 0.25376 (18) | 0.0343 (6) | |
H3N | 0.457 (3) | −0.0409 (12) | 0.1597 (14) | 0.041* | |
H4N | 0.450 (3) | 0.1166 (16) | 0.2926 (10) | 0.041* | |
C9 | 0.4628 (3) | 0.5730 (2) | 0.3839 (2) | 0.0417 (9) | |
H9 | 0.4661 | 0.5816 | 0.431 | 0.05* | |
C10 | 0.4672 (2) | 0.6261 (2) | 0.3346 (2) | 0.0389 (8) | |
H10 | 0.4739 | 0.6794 | 0.3407 | 0.047* | |
C11 | 0.45236 (19) | 0.5147 (2) | 0.28609 (19) | 0.0308 (7) | |
C12 | 0.4469 (3) | 0.4532 (3) | 0.2355 (2) | 0.0536 (12) | |
H12A | 0.4124 | 0.4697 | 0.1979 | 0.08* | |
H12B | 0.4235 | 0.4077 | 0.2561 | 0.08* | |
H12C | 0.5011 | 0.4413 | 0.219 | 0.08* | |
N5 | 0.45244 (17) | 0.50405 (18) | 0.35196 (16) | 0.0316 (6) | |
N6 | 0.46028 (17) | 0.58857 (17) | 0.27414 (16) | 0.0316 (6) | |
H5N | 0.446 (3) | 0.4604 (12) | 0.3735 (13) | 0.038* | |
H6N | 0.456 (3) | 0.6126 (15) | 0.2346 (10) | 0.038* | |
C13 | 0.4092 (3) | 0.3119 (4) | 0.0588 (3) | 0.0606 (14) | |
H13 | 0.4644 | 0.327 | 0.0599 | 0.073* | |
C14 | 0.3540 (3) | 0.3234 (3) | 0.1070 (3) | 0.0549 (12) | |
H14 | 0.363 | 0.3476 | 0.1492 | 0.066* | |
C15 | 0.2921 (3) | 0.2642 (2) | 0.02298 (19) | 0.0364 (8) | |
C16 | 0.2296 (4) | 0.2267 (3) | −0.0190 (3) | 0.0564 (12) | |
H16A | 0.2271 | 0.1726 | −0.0075 | 0.085* | |
H16B | 0.2433 | 0.2323 | −0.0666 | 0.085* | |
H16C | 0.177 | 0.2503 | −0.0108 | 0.085* | |
N7 | 0.3698 (2) | 0.2740 (2) | 0.00784 (19) | 0.0475 (9) | |
N8 | 0.2818 (2) | 0.2935 (2) | 0.08359 (17) | 0.0398 (7) | |
H7N | 0.3920 (18) | 0.263 (3) | −0.0313 (13) | 0.048* | |
H8N | 0.2341 (13) | 0.301 (3) | 0.1029 (17) | 0.048* | |
C17 | 0.3403 (2) | 0.3084 (2) | 0.75070 (18) | 0.0319 (7) | |
H17 | 0.3787 | 0.2916 | 0.7834 | 0.038* | |
C18 | 0.34305 (19) | 0.2954 (2) | 0.68388 (18) | 0.0300 (6) | |
H18 | 0.3836 | 0.2681 | 0.6606 | 0.036* | |
C19 | 0.23323 (18) | 0.36274 (19) | 0.70469 (15) | 0.0251 (5) | |
C20 | 0.1568 (2) | 0.4053 (3) | 0.6948 (2) | 0.0404 (9) | |
H20A | 0.119 | 0.392 | 0.7305 | 0.061* | |
H20B | 0.1328 | 0.392 | 0.651 | 0.061* | |
H20C | 0.1679 | 0.46 | 0.6962 | 0.061* | |
N9 | 0.27156 (17) | 0.35055 (18) | 0.76280 (14) | 0.0292 (5) | |
N10 | 0.27544 (16) | 0.32947 (17) | 0.65606 (13) | 0.0260 (5) | |
H9N | 0.2597 (19) | 0.369 (2) | 0.8029 (10) | 0.031* | |
H10N | 0.2612 (19) | 0.328 (2) | 0.6133 (9) | 0.031* | |
C21 | 0.1295 (2) | 0.2036 (2) | 0.62572 (16) | 0.0294 (6) | |
H21 | 0.0909 | 0.2298 | 0.5985 | 0.035* | |
C22 | 0.12795 (19) | 0.1954 (2) | 0.69351 (15) | 0.0289 (6) | |
H22 | 0.0878 | 0.2144 | 0.7228 | 0.035* | |
C23 | 0.23697 (19) | 0.13713 (18) | 0.65689 (14) | 0.0241 (5) | |
C24 | 0.3139 (2) | 0.0943 (2) | 0.6550 (2) | 0.0356 (7) | |
H24A | 0.3575 | 0.1257 | 0.6739 | 0.053* | |
H24B | 0.3264 | 0.0813 | 0.6083 | 0.053* | |
H24C | 0.3088 | 0.0476 | 0.6815 | 0.053* | |
N11 | 0.19766 (16) | 0.16674 (17) | 0.60401 (12) | 0.0262 (5) | |
N12 | 0.19571 (16) | 0.15416 (17) | 0.71190 (12) | 0.0257 (5) | |
H11N | 0.2134 (19) | 0.164 (2) | 0.5621 (9) | 0.031* | |
H12N | 0.2122 (19) | 0.145 (2) | 0.7531 (9) | 0.031* | |
C25 | 0.3331 (3) | −0.0694 (3) | 0.5204 (2) | 0.0543 (12) | |
H25 | 0.3753 | −0.0638 | 0.4888 | 0.065* | |
C26 | 0.3380 (3) | −0.1023 (3) | 0.5821 (2) | 0.0498 (11) | |
H26 | 0.3853 | −0.1248 | 0.6009 | 0.06* | |
C27 | 0.2140 (3) | −0.0632 (2) | 0.5699 (2) | 0.0439 (10) | |
C28 | 0.1286 (4) | −0.0448 (3) | 0.5815 (3) | 0.0625 (14) | |
H28A | 0.0994 | −0.0912 | 0.5938 | 0.094* | |
H28B | 0.1046 | −0.0234 | 0.5404 | 0.094* | |
H28C | 0.1248 | −0.0077 | 0.618 | 0.094* | |
N13 | 0.2543 (3) | −0.0461 (2) | 0.51329 (18) | 0.0523 (10) | |
N14 | 0.2641 (2) | −0.0981 (2) | 0.61320 (16) | 0.0421 (8) | |
H13N | 0.2347 (18) | −0.022 (3) | 0.4779 (15) | 0.05* | |
C29 | 0.1459 (2) | 0.5736 (2) | 0.59154 (18) | 0.0331 (7) | |
H29 | 0.0966 | 0.5697 | 0.5669 | 0.04* | |
C30 | 0.1591 (2) | 0.6127 (2) | 0.64964 (18) | 0.0325 (7) | |
H30 | 0.1195 | 0.6411 | 0.673 | 0.039* | |
C31 | 0.2732 (2) | 0.5611 (2) | 0.62385 (16) | 0.0289 (6) | |
C32 | 0.3600 (2) | 0.5372 (3) | 0.6246 (2) | 0.0472 (11) | |
H32A | 0.3916 | 0.5723 | 0.6526 | 0.071* | |
H32B | 0.3807 | 0.5378 | 0.5786 | 0.071* | |
H32C | 0.3645 | 0.4856 | 0.643 | 0.071* | |
N15 | 0.21866 (17) | 0.54082 (17) | 0.57597 (14) | 0.0287 (5) | |
N16 | 0.23894 (17) | 0.60467 (18) | 0.66955 (14) | 0.0302 (6) | |
H15N | 0.2266 (18) | 0.511 (2) | 0.5419 (15) | 0.036* | |
O25 | 0.14267 (16) | 0.30433 (19) | 0.14871 (12) | 0.0369 (6) | |
H25V | 0.134 (3) | 0.300 (3) | 0.1909 (10) | 0.055* | |
H25W | 0.0957 (17) | 0.302 (3) | 0.130 (2) | 0.055* | |
O26 | 0.4963 (2) | 0.2100 (2) | 0.58818 (17) | 0.0519 (8) | |
H26V | 0.482 (4) | 0.248 (2) | 0.566 (3) | 0.078* | |
H26W | 0.482 (4) | 0.172 (2) | 0.566 (3) | 0.078* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0214 (9) | 0.0333 (12) | 0.0294 (11) | −0.0021 (8) | 0.0030 (8) | 0.0072 (9) |
O2 | 0.0330 (11) | 0.0339 (12) | 0.0182 (9) | −0.0065 (9) | −0.0104 (8) | 0.0047 (8) |
O3 | 0.0288 (10) | 0.0217 (9) | 0.0183 (9) | −0.0051 (8) | −0.0051 (7) | 0.0004 (7) |
O4 | 0.0258 (10) | 0.0345 (12) | 0.0206 (9) | −0.0030 (9) | 0.0017 (8) | 0.0070 (8) |
O5 | 0.0382 (12) | 0.0218 (10) | 0.0285 (11) | −0.0060 (9) | −0.0035 (9) | −0.0020 (8) |
O6 | 0.0218 (8) | 0.0208 (9) | 0.0129 (7) | −0.0003 (7) | 0.0016 (6) | 0.0024 (6) |
O7 | 0.0255 (10) | 0.0328 (12) | 0.0268 (11) | 0.0018 (9) | −0.0034 (8) | 0.0067 (9) |
O8 | 0.0375 (12) | 0.0221 (10) | 0.0247 (10) | 0.0050 (9) | 0.0080 (9) | 0.0008 (8) |
O9 | 0.0295 (10) | 0.0258 (10) | 0.0253 (10) | 0.0044 (8) | 0.0119 (8) | 0.0025 (8) |
O10 | 0.0240 (11) | 0.0398 (14) | 0.0452 (15) | 0.0009 (10) | −0.0018 (10) | 0.0059 (12) |
O11 | 0.0371 (13) | 0.0433 (15) | 0.0379 (14) | 0.0011 (11) | 0.0227 (11) | 0.0077 (11) |
O12 | 0.0239 (9) | 0.0206 (9) | 0.0223 (9) | −0.0029 (7) | 0.0041 (7) | 0.0025 (7) |
O13 | 0.0233 (10) | 0.0389 (13) | 0.0206 (9) | −0.0016 (9) | −0.0060 (8) | 0.0031 (9) |
O14 | 0.0312 (10) | 0.0204 (9) | 0.0222 (9) | −0.0040 (8) | −0.0020 (8) | −0.0034 (7) |
O15 | 0.0219 (9) | 0.0257 (9) | 0.0116 (7) | −0.0001 (7) | −0.0011 (6) | 0.0004 (7) |
O16 | 0.0256 (10) | 0.0402 (13) | 0.0177 (9) | 0.0037 (9) | 0.0059 (8) | 0.0036 (8) |
O17 | 0.0310 (11) | 0.0228 (10) | 0.0215 (9) | 0.0033 (8) | −0.0038 (8) | −0.0032 (7) |
O18 | 0.0242 (9) | 0.0206 (9) | 0.0189 (9) | 0.0013 (7) | −0.0031 (7) | 0.0008 (7) |
O19 | 0.0306 (10) | 0.0237 (9) | 0.0137 (8) | −0.0029 (8) | −0.0038 (7) | 0.0018 (7) |
O20 | 0.0283 (9) | 0.0160 (8) | 0.0129 (7) | −0.0013 (7) | 0.0032 (7) | −0.0007 (6) |
O21 | 0.0321 (11) | 0.0255 (10) | 0.0186 (9) | 0.0004 (8) | 0.0110 (8) | 0.0020 (7) |
O22 | 0.0229 (8) | 0.0167 (8) | 0.0117 (7) | −0.0007 (6) | 0.0003 (6) | −0.0007 (6) |
O23 | 0.0187 (8) | 0.0189 (8) | 0.0117 (7) | −0.0014 (6) | 0.0007 (6) | 0.0008 (6) |
O24 | 0.0198 (8) | 0.0175 (8) | 0.0143 (7) | 0.0004 (6) | 0.0029 (6) | 0.0014 (6) |
Mo1 | 0.01912 (9) | 0.02215 (10) | 0.01584 (9) | −0.00268 (8) | −0.00351 (7) | 0.00174 (7) |
Mo2 | 0.02159 (10) | 0.01762 (9) | 0.01494 (9) | −0.00348 (7) | −0.00019 (7) | 0.00209 (7) |
Mo3 | 0.02075 (10) | 0.01832 (10) | 0.01763 (9) | 0.00146 (8) | 0.00352 (7) | 0.00293 (7) |
Mo4 | 0.01970 (10) | 0.02472 (11) | 0.02561 (11) | 0.00006 (8) | 0.00868 (8) | 0.00360 (9) |
Mo5 | 0.01950 (9) | 0.01916 (10) | 0.01367 (9) | −0.00115 (7) | −0.00133 (7) | −0.00076 (7) |
Mo6 | 0.01876 (9) | 0.01945 (10) | 0.01188 (8) | 0.00120 (7) | 0.00054 (7) | −0.00103 (7) |
Mo7 | 0.02116 (9) | 0.01513 (9) | 0.01035 (8) | −0.00110 (7) | 0.00168 (7) | −0.00035 (6) |
C1 | 0.069 (3) | 0.0360 (19) | 0.0254 (16) | 0.0063 (19) | −0.0037 (17) | −0.0048 (14) |
C2 | 0.054 (2) | 0.0268 (15) | 0.0291 (16) | 0.0069 (15) | −0.0016 (15) | −0.0060 (12) |
C3 | 0.0225 (12) | 0.0242 (13) | 0.0263 (13) | 0.0004 (10) | 0.0014 (10) | −0.0075 (10) |
C4 | 0.076 (3) | 0.0280 (17) | 0.036 (2) | −0.0038 (18) | 0.002 (2) | −0.0050 (15) |
N1 | 0.0293 (12) | 0.0281 (12) | 0.0222 (11) | 0.0017 (10) | 0.0000 (9) | −0.0128 (9) |
N2 | 0.0248 (11) | 0.0248 (11) | 0.0211 (11) | 0.0002 (9) | 0.0014 (9) | −0.0092 (9) |
C5 | 0.052 (2) | 0.051 (3) | 0.038 (2) | 0.000 (2) | −0.0123 (18) | −0.0113 (18) |
C6 | 0.047 (2) | 0.041 (2) | 0.041 (2) | 0.0030 (17) | −0.0089 (17) | −0.0061 (17) |
C7 | 0.0215 (13) | 0.0335 (17) | 0.047 (2) | −0.0041 (12) | 0.0096 (13) | −0.0113 (14) |
C8 | 0.045 (2) | 0.046 (2) | 0.046 (2) | 0.0079 (18) | 0.0100 (18) | −0.0030 (18) |
N3 | 0.0256 (13) | 0.0373 (16) | 0.0439 (17) | −0.0015 (11) | 0.0025 (12) | −0.0179 (13) |
N4 | 0.0231 (12) | 0.0330 (15) | 0.0469 (18) | −0.0027 (11) | 0.0027 (11) | −0.0127 (13) |
C9 | 0.050 (2) | 0.037 (2) | 0.038 (2) | −0.0067 (17) | 0.0036 (17) | 0.0054 (15) |
C10 | 0.043 (2) | 0.0313 (17) | 0.043 (2) | −0.0031 (15) | 0.0023 (16) | 0.0063 (15) |
C11 | 0.0230 (13) | 0.0311 (15) | 0.0380 (17) | −0.0034 (11) | −0.0103 (12) | 0.0118 (13) |
C12 | 0.073 (3) | 0.040 (2) | 0.047 (2) | −0.004 (2) | −0.020 (2) | 0.0017 (19) |
N5 | 0.0250 (12) | 0.0308 (14) | 0.0389 (16) | −0.0056 (10) | −0.0032 (11) | 0.0133 (12) |
N6 | 0.0261 (12) | 0.0306 (14) | 0.0380 (15) | −0.0036 (10) | −0.0054 (11) | 0.0120 (12) |
C13 | 0.037 (2) | 0.077 (4) | 0.068 (3) | 0.002 (2) | 0.012 (2) | −0.008 (3) |
C14 | 0.045 (2) | 0.070 (3) | 0.050 (3) | −0.003 (2) | 0.005 (2) | −0.020 (2) |
C15 | 0.047 (2) | 0.0326 (17) | 0.0296 (16) | 0.0093 (15) | 0.0081 (14) | 0.0016 (13) |
C16 | 0.077 (4) | 0.044 (3) | 0.047 (3) | 0.002 (2) | −0.011 (2) | −0.005 (2) |
N7 | 0.053 (2) | 0.052 (2) | 0.0381 (18) | 0.0154 (17) | 0.0202 (16) | 0.0027 (16) |
N8 | 0.0393 (16) | 0.0454 (19) | 0.0350 (16) | 0.0044 (14) | 0.0116 (13) | −0.0041 (14) |
C17 | 0.0242 (13) | 0.0393 (18) | 0.0321 (16) | 0.0027 (12) | −0.0053 (12) | 0.0007 (13) |
C18 | 0.0220 (13) | 0.0359 (17) | 0.0322 (16) | 0.0035 (12) | 0.0030 (11) | −0.0006 (13) |
C19 | 0.0228 (12) | 0.0309 (15) | 0.0215 (12) | 0.0022 (11) | 0.0018 (10) | −0.0001 (10) |
C20 | 0.0333 (17) | 0.048 (2) | 0.040 (2) | 0.0146 (16) | −0.0022 (14) | 0.0057 (17) |
N9 | 0.0293 (13) | 0.0380 (15) | 0.0203 (11) | 0.0040 (11) | −0.0012 (9) | −0.0007 (10) |
N10 | 0.0266 (12) | 0.0338 (13) | 0.0177 (10) | −0.0006 (10) | 0.0024 (9) | −0.0001 (9) |
C21 | 0.0277 (14) | 0.0417 (18) | 0.0190 (12) | 0.0009 (13) | 0.0000 (10) | 0.0026 (12) |
C22 | 0.0268 (13) | 0.0415 (18) | 0.0187 (12) | −0.0004 (12) | 0.0069 (10) | 0.0002 (11) |
C23 | 0.0288 (13) | 0.0282 (14) | 0.0155 (11) | −0.0015 (11) | 0.0017 (10) | −0.0007 (9) |
C24 | 0.0362 (17) | 0.0365 (18) | 0.0343 (17) | 0.0089 (14) | 0.0056 (14) | 0.0012 (14) |
N11 | 0.0289 (12) | 0.0374 (14) | 0.0124 (9) | −0.0002 (10) | 0.0027 (8) | 0.0008 (9) |
N12 | 0.0293 (12) | 0.0347 (14) | 0.0132 (9) | −0.0017 (10) | 0.0013 (8) | 0.0037 (9) |
C25 | 0.081 (3) | 0.039 (2) | 0.043 (2) | 0.008 (2) | 0.026 (2) | 0.0121 (18) |
C26 | 0.066 (3) | 0.042 (2) | 0.042 (2) | 0.003 (2) | 0.013 (2) | 0.0089 (18) |
C27 | 0.074 (3) | 0.0266 (16) | 0.0306 (17) | −0.0031 (18) | 0.0014 (18) | 0.0015 (13) |
C28 | 0.075 (4) | 0.054 (3) | 0.058 (3) | −0.001 (3) | −0.006 (3) | 0.005 (2) |
N13 | 0.095 (3) | 0.0330 (17) | 0.0288 (16) | 0.0064 (19) | 0.0075 (18) | 0.0112 (13) |
N14 | 0.065 (2) | 0.0348 (16) | 0.0260 (14) | −0.0038 (15) | 0.0053 (14) | 0.0052 (12) |
C29 | 0.0285 (15) | 0.0419 (19) | 0.0286 (15) | 0.0052 (13) | −0.0094 (12) | −0.0013 (13) |
C30 | 0.0307 (15) | 0.0369 (17) | 0.0298 (15) | 0.0115 (13) | −0.0028 (12) | −0.0057 (13) |
C31 | 0.0290 (14) | 0.0355 (16) | 0.0222 (13) | 0.0043 (12) | −0.0059 (11) | −0.0094 (12) |
C32 | 0.0322 (18) | 0.068 (3) | 0.041 (2) | 0.0155 (19) | −0.0086 (15) | −0.019 (2) |
N15 | 0.0315 (13) | 0.0327 (14) | 0.0217 (11) | 0.0048 (11) | −0.0046 (10) | −0.0109 (10) |
N16 | 0.0302 (13) | 0.0364 (15) | 0.0240 (12) | 0.0088 (11) | −0.0057 (10) | −0.0092 (11) |
O25 | 0.0344 (12) | 0.0563 (17) | 0.0199 (10) | 0.0001 (12) | 0.0025 (9) | 0.0003 (11) |
O26 | 0.066 (2) | 0.0466 (18) | 0.0422 (17) | −0.0038 (16) | −0.0272 (15) | 0.0040 (14) |
O1—Mo1 | 1.724 (2) | C11—N6 | 1.328 (4) |
O2—Mo1 | 1.725 (2) | C11—C12 | 1.479 (6) |
O3—Mo1 | 1.945 (2) | C12—H12A | 0.98 |
O3—Mo2 | 1.971 (2) | C12—H12B | 0.98 |
O4—Mo2 | 1.707 (2) | C12—H12C | 0.98 |
O5—Mo2 | 1.725 (2) | N5—H5N | 0.886 (17) |
O6—Mo3 | 1.9528 (19) | N6—H6N | 0.895 (17) |
O6—Mo2 | 1.953 (2) | C13—C14 | 1.347 (7) |
O7—Mo3 | 1.715 (2) | C13—N7 | 1.372 (7) |
O8—Mo3 | 1.716 (2) | C13—H13 | 0.95 |
O9—Mo4 | 1.939 (2) | C14—N8 | 1.379 (6) |
O9—Mo3 | 1.987 (2) | C14—H14 | 0.95 |
O10—Mo4 | 1.709 (3) | C15—N8 | 1.324 (5) |
O11—Mo4 | 1.715 (2) | C15—N7 | 1.333 (5) |
O12—Mo4 | 1.932 (2) | C15—C16 | 1.476 (6) |
O12—Mo5 | 1.983 (2) | C16—H16A | 0.98 |
O13—Mo5 | 1.713 (2) | C16—H16B | 0.98 |
O14—Mo5 | 1.730 (2) | C16—H16C | 0.98 |
O15—Mo6 | 1.9521 (19) | N7—H7N | 0.887 (17) |
O15—Mo5 | 1.953 (2) | N8—H8N | 0.893 (17) |
O16—Mo6 | 1.707 (2) | C17—C18 | 1.350 (5) |
O17—Mo6 | 1.726 (2) | C17—N9 | 1.380 (4) |
O18—Mo1 | 1.916 (2) | C17—H17 | 0.95 |
O18—Mo6 | 2.012 (2) | C18—N10 | 1.379 (4) |
O19—Mo7 | 1.754 (2) | C18—H18 | 0.95 |
O19—Mo1 | 2.453 (2) | C19—N9 | 1.329 (4) |
O20—Mo7 | 1.901 (2) | C19—N10 | 1.334 (4) |
O20—Mo3 | 2.259 (2) | C19—C20 | 1.480 (5) |
O20—Mo2 | 2.292 (2) | C20—H20A | 0.98 |
O21—Mo7 | 1.725 (2) | C20—H20B | 0.98 |
O22—Mo7 | 1.8945 (19) | C20—H20C | 0.98 |
O22—Mo5 | 2.2453 (19) | N9—H9N | 0.886 (17) |
O22—Mo6 | 2.3057 (19) | N10—H10N | 0.880 (17) |
O23—Mo6 | 2.1329 (19) | C21—C22 | 1.356 (4) |
O23—Mo1 | 2.1604 (19) | C21—N11 | 1.374 (4) |
O23—Mo2 | 2.1748 (19) | C21—H21 | 0.95 |
O23—Mo7 | 2.3011 (18) | C22—N12 | 1.380 (4) |
O24—Mo4 | 2.1624 (19) | C22—H22 | 0.95 |
O24—Mo5 | 2.1665 (19) | C23—N12 | 1.330 (4) |
O24—Mo3 | 2.1677 (19) | C23—N11 | 1.336 (4) |
O24—Mo7 | 2.2665 (19) | C23—C24 | 1.479 (5) |
Mo1—Mo6 | 3.2178 (3) | C24—H24A | 0.98 |
Mo4—Mo5 | 3.2105 (3) | C24—H24B | 0.98 |
C1—C2 | 1.362 (5) | C24—H24C | 0.98 |
C1—N1 | 1.362 (5) | N11—H11N | 0.877 (17) |
C1—H1 | 0.95 | N12—H12N | 0.876 (17) |
C2—N2 | 1.365 (5) | C25—C26 | 1.357 (6) |
C2—H2 | 0.95 | C25—N13 | 1.371 (7) |
C3—N1 | 1.328 (4) | C25—H25 | 0.95 |
C3—N2 | 1.332 (4) | C26—N14 | 1.377 (6) |
C3—C4 | 1.488 (5) | C26—H26 | 0.95 |
C4—H4A | 0.98 | C27—N14 | 1.338 (6) |
C4—H4B | 0.98 | C27—N13 | 1.348 (6) |
C4—H4C | 0.98 | C27—C28 | 1.470 (8) |
N1—H1N | 0.881 (17) | C28—H28A | 0.98 |
N2—H2N | 0.868 (17) | C28—H28B | 0.98 |
C5—C6 | 1.363 (6) | C28—H28C | 0.98 |
C5—N3 | 1.384 (6) | N13—H13N | 0.880 (19) |
C5—H5 | 0.95 | C29—C30 | 1.360 (5) |
C6—N4 | 1.367 (6) | C29—N15 | 1.372 (4) |
C6—H6 | 0.95 | C29—H29 | 0.95 |
C7—N3 | 1.321 (5) | C30—N16 | 1.380 (4) |
C7—N4 | 1.325 (5) | C30—H30 | 0.95 |
C7—C8 | 1.493 (6) | C31—N16 | 1.321 (4) |
C8—H8A | 0.98 | C31—N15 | 1.352 (4) |
C8—H8B | 0.98 | C31—C32 | 1.495 (5) |
C8—H8C | 0.98 | C32—H32A | 0.98 |
N3—H3N | 0.884 (17) | C32—H32B | 0.98 |
N4—H4N | 0.884 (17) | C32—H32C | 0.98 |
C9—C10 | 1.357 (6) | N15—H15N | 0.867 (19) |
C9—N5 | 1.378 (5) | O25—H25V | 0.857 (19) |
C9—H9 | 0.95 | O25—H25W | 0.856 (18) |
C10—N6 | 1.375 (5) | O26—H26V | 0.842 (19) |
C10—H10 | 0.95 | O26—H26W | 0.843 (19) |
C11—N5 | 1.323 (5) | ||
Mo1—O3—Mo2 | 111.13 (10) | C3—C4—H4A | 109.5 |
Mo3—O6—Mo2 | 115.96 (9) | C3—C4—H4B | 109.5 |
Mo4—O9—Mo3 | 110.89 (11) | H4A—C4—H4B | 109.5 |
Mo4—O12—Mo5 | 110.14 (10) | C3—C4—H4C | 109.5 |
Mo6—O15—Mo5 | 114.70 (9) | H4A—C4—H4C | 109.5 |
Mo1—O18—Mo6 | 110.01 (10) | H4B—C4—H4C | 109.5 |
Mo7—O19—Mo1 | 107.64 (9) | C3—N1—C1 | 109.4 (3) |
Mo7—O20—Mo3 | 110.29 (9) | C3—N1—H1N | 125.1 (19) |
Mo7—O20—Mo2 | 110.20 (9) | C1—N1—H1N | 125.4 (19) |
Mo3—O20—Mo2 | 93.36 (7) | C3—N2—C2 | 109.0 (3) |
Mo7—O22—Mo5 | 109.98 (9) | C3—N2—H2N | 128.7 (19) |
Mo7—O22—Mo6 | 109.89 (9) | C2—N2—H2N | 122.3 (19) |
Mo5—O22—Mo6 | 92.51 (7) | C6—C5—N3 | 106.9 (4) |
Mo6—O23—Mo1 | 97.09 (8) | C6—C5—H5 | 126.6 |
Mo6—O23—Mo2 | 151.14 (9) | N3—C5—H5 | 126.6 |
Mo1—O23—Mo2 | 96.34 (7) | C5—C6—N4 | 106.2 (4) |
Mo6—O23—Mo7 | 101.96 (8) | C5—C6—H6 | 126.9 |
Mo1—O23—Mo7 | 100.09 (7) | N4—C6—H6 | 126.9 |
Mo2—O23—Mo7 | 100.67 (7) | N3—C7—N4 | 108.4 (4) |
Mo4—O24—Mo5 | 95.74 (8) | N3—C7—C8 | 126.8 (4) |
Mo4—O24—Mo3 | 96.60 (8) | N4—C7—C8 | 124.7 (4) |
Mo5—O24—Mo3 | 152.34 (9) | C7—C8—H8A | 109.5 |
Mo4—O24—Mo7 | 103.86 (7) | C7—C8—H8B | 109.5 |
Mo5—O24—Mo7 | 100.00 (8) | H8A—C8—H8B | 109.5 |
Mo3—O24—Mo7 | 100.92 (8) | C7—C8—H8C | 109.5 |
O1—Mo1—O2 | 104.12 (11) | H8A—C8—H8C | 109.5 |
O1—Mo1—O18 | 98.92 (11) | H8B—C8—H8C | 109.5 |
O2—Mo1—O18 | 102.57 (10) | C7—N3—C5 | 108.7 (3) |
O1—Mo1—O3 | 96.55 (11) | C7—N3—H3N | 129 (2) |
O2—Mo1—O3 | 100.84 (10) | C5—N3—H3N | 122 (2) |
O18—Mo1—O3 | 147.73 (9) | C7—N4—C6 | 109.9 (3) |
O1—Mo1—O23 | 106.54 (9) | C7—N4—H4N | 126 (2) |
O2—Mo1—O23 | 149.29 (10) | C6—N4—H4N | 124 (2) |
O18—Mo1—O23 | 74.47 (8) | C10—C9—N5 | 106.3 (4) |
O3—Mo1—O23 | 74.03 (8) | C10—C9—H9 | 126.9 |
O1—Mo1—O19 | 176.53 (9) | N5—C9—H9 | 126.9 |
O2—Mo1—O19 | 78.58 (10) | C9—C10—N6 | 107.2 (4) |
O18—Mo1—O19 | 82.49 (8) | C9—C10—H10 | 126.4 |
O3—Mo1—O19 | 80.71 (8) | N6—C10—H10 | 126.4 |
O23—Mo1—O19 | 70.72 (7) | N5—C11—N6 | 108.4 (3) |
O1—Mo1—Mo6 | 95.01 (8) | N5—C11—C12 | 124.7 (3) |
O2—Mo1—Mo6 | 137.30 (8) | N6—C11—C12 | 126.8 (4) |
O18—Mo1—Mo6 | 35.98 (6) | C11—C12—H12A | 109.5 |
O3—Mo1—Mo6 | 114.62 (6) | C11—C12—H12B | 109.5 |
O23—Mo1—Mo6 | 41.13 (5) | H12A—C12—H12B | 109.5 |
O19—Mo1—Mo6 | 84.26 (5) | C11—C12—H12C | 109.5 |
O4—Mo2—O5 | 105.64 (12) | H12A—C12—H12C | 109.5 |
O4—Mo2—O6 | 96.30 (9) | H12B—C12—H12C | 109.5 |
O5—Mo2—O6 | 97.94 (10) | C11—N5—C9 | 109.3 (3) |
O4—Mo2—O3 | 102.62 (10) | C11—N5—H5N | 127.0 (19) |
O5—Mo2—O3 | 95.05 (10) | C9—N5—H5N | 123.7 (19) |
O6—Mo2—O3 | 153.21 (8) | C11—N6—C10 | 108.7 (3) |
O4—Mo2—O23 | 93.82 (10) | C11—N6—H6N | 127.8 (19) |
O5—Mo2—O23 | 159.22 (10) | C10—N6—H6N | 123.1 (19) |
O6—Mo2—O23 | 86.87 (8) | C14—C13—N7 | 106.2 (4) |
O3—Mo2—O23 | 73.22 (8) | C14—C13—H13 | 126.9 |
O4—Mo2—O20 | 161.90 (10) | N7—C13—H13 | 126.9 |
O5—Mo2—O20 | 90.12 (10) | C13—C14—N8 | 107.0 (4) |
O6—Mo2—O20 | 72.28 (7) | C13—C14—H14 | 126.5 |
O3—Mo2—O20 | 84.40 (8) | N8—C14—H14 | 126.5 |
O23—Mo2—O20 | 72.01 (7) | N8—C15—N7 | 106.8 (4) |
O8—Mo3—O7 | 104.86 (12) | N8—C15—C16 | 126.4 (4) |
O8—Mo3—O6 | 100.55 (10) | N7—C15—C16 | 126.8 (4) |
O7—Mo3—O6 | 96.34 (10) | C15—C16—H16A | 109.5 |
O8—Mo3—O9 | 92.85 (10) | C15—C16—H16B | 109.5 |
O7—Mo3—O9 | 100.23 (11) | H16A—C16—H16B | 109.5 |
O6—Mo3—O9 | 155.25 (9) | C15—C16—H16C | 109.5 |
O8—Mo3—O24 | 155.03 (9) | H16A—C16—H16C | 109.5 |
O7—Mo3—O24 | 97.84 (10) | H16B—C16—H16C | 109.5 |
O6—Mo3—O24 | 86.96 (8) | C15—N7—C13 | 110.3 (4) |
O9—Mo3—O24 | 72.72 (8) | C15—N7—H7N | 125 (2) |
O8—Mo3—O20 | 87.48 (10) | C13—N7—H7N | 124 (2) |
O7—Mo3—O20 | 165.23 (10) | C15—N8—C14 | 109.7 (4) |
O6—Mo3—O20 | 73.05 (7) | C15—N8—H8N | 125 (2) |
O9—Mo3—O20 | 86.99 (9) | C14—N8—H8N | 124 (2) |
O24—Mo3—O20 | 71.84 (7) | C18—C17—N9 | 107.4 (3) |
O10—Mo4—O11 | 106.30 (14) | C18—C17—H17 | 126.3 |
O10—Mo4—O12 | 99.66 (12) | N9—C17—H17 | 126.3 |
O11—Mo4—O12 | 101.36 (12) | C17—C18—N10 | 106.6 (3) |
O10—Mo4—O9 | 100.30 (12) | C17—C18—H18 | 126.7 |
O11—Mo4—O9 | 99.31 (12) | N10—C18—H18 | 126.7 |
O12—Mo4—O9 | 145.80 (9) | N9—C19—N10 | 108.1 (3) |
O10—Mo4—O24 | 106.87 (10) | N9—C19—C20 | 126.5 (3) |
O11—Mo4—O24 | 146.81 (11) | N10—C19—C20 | 125.3 (3) |
O12—Mo4—O24 | 74.02 (8) | C19—C20—H20A | 109.5 |
O9—Mo4—O24 | 73.74 (8) | C19—C20—H20B | 109.5 |
O10—Mo4—Mo5 | 93.77 (10) | H20A—C20—H20B | 109.5 |
O11—Mo4—Mo5 | 135.81 (10) | C19—C20—H20C | 109.5 |
O12—Mo4—Mo5 | 35.45 (6) | H20A—C20—H20C | 109.5 |
O9—Mo4—Mo5 | 115.58 (6) | H20B—C20—H20C | 109.5 |
O24—Mo4—Mo5 | 42.18 (5) | C19—N9—C17 | 108.7 (3) |
O13—Mo5—O14 | 105.18 (11) | C19—N9—H9N | 128.0 (19) |
O13—Mo5—O15 | 96.34 (10) | C17—N9—H9N | 123.0 (19) |
O14—Mo5—O15 | 99.61 (10) | C19—N10—C18 | 109.2 (3) |
O13—Mo5—O12 | 99.85 (10) | C19—N10—H10N | 125.4 (19) |
O14—Mo5—O12 | 92.28 (10) | C18—N10—H10N | 125.4 (19) |
O15—Mo5—O12 | 156.65 (9) | C22—C21—N11 | 106.6 (3) |
O13—Mo5—O24 | 95.51 (10) | C22—C21—H21 | 126.7 |
O14—Mo5—O24 | 156.48 (9) | N11—C21—H21 | 126.7 |
O15—Mo5—O24 | 88.88 (8) | C21—C22—N12 | 107.2 (3) |
O12—Mo5—O24 | 72.96 (8) | C21—C22—H22 | 126.4 |
O13—Mo5—O22 | 165.08 (10) | N12—C22—H22 | 126.4 |
O14—Mo5—O22 | 88.42 (9) | N12—C23—N11 | 108.1 (3) |
O15—Mo5—O22 | 74.97 (7) | N12—C23—C24 | 125.8 (3) |
O12—Mo5—O22 | 85.42 (8) | N11—C23—C24 | 126.1 (3) |
O24—Mo5—O22 | 72.54 (7) | C23—C24—H24A | 109.5 |
O13—Mo5—Mo4 | 87.53 (8) | C23—C24—H24B | 109.5 |
O14—Mo5—Mo4 | 126.61 (8) | H24A—C24—H24B | 109.5 |
O15—Mo5—Mo4 | 130.86 (6) | C23—C24—H24C | 109.5 |
O12—Mo5—Mo4 | 34.41 (6) | H24A—C24—H24C | 109.5 |
O24—Mo5—Mo4 | 42.08 (5) | H24B—C24—H24C | 109.5 |
O22—Mo5—Mo4 | 89.18 (5) | C23—N11—C21 | 109.3 (2) |
O16—Mo6—O17 | 105.29 (12) | C23—N11—H11N | 125.3 (18) |
O16—Mo6—O15 | 98.56 (10) | C21—N11—H11N | 125.4 (18) |
O17—Mo6—O15 | 99.46 (10) | C23—N12—C22 | 108.8 (2) |
O16—Mo6—O18 | 100.69 (10) | C23—N12—H12N | 124.9 (19) |
O17—Mo6—O18 | 90.59 (9) | C22—N12—H12N | 125.9 (19) |
O15—Mo6—O18 | 155.08 (8) | C26—C25—N13 | 105.5 (4) |
O16—Mo6—O23 | 97.03 (10) | C26—C25—H25 | 127.2 |
O17—Mo6—O23 | 154.60 (9) | N13—C25—H25 | 127.2 |
O15—Mo6—O23 | 88.86 (8) | C25—C26—N14 | 109.8 (5) |
O18—Mo6—O23 | 73.23 (8) | C25—C26—H26 | 125.1 |
O16—Mo6—O22 | 166.13 (10) | N14—C26—H26 | 125.1 |
O17—Mo6—O22 | 87.49 (9) | N14—C27—N13 | 109.4 (4) |
O15—Mo6—O22 | 73.58 (7) | N14—C27—C28 | 126.1 (4) |
O18—Mo6—O22 | 84.24 (8) | N13—C27—C28 | 124.5 (4) |
O23—Mo6—O22 | 71.80 (7) | C27—C28—H28A | 109.5 |
O16—Mo6—Mo1 | 90.80 (8) | C27—C28—H28B | 109.5 |
O17—Mo6—Mo1 | 124.59 (7) | H28A—C28—H28B | 109.5 |
O15—Mo6—Mo1 | 130.62 (6) | C27—C28—H28C | 109.5 |
O18—Mo6—Mo1 | 34.01 (6) | H28A—C28—H28C | 109.5 |
O23—Mo6—Mo1 | 41.78 (5) | H28B—C28—H28C | 109.5 |
O22—Mo6—Mo1 | 86.14 (5) | C27—N13—C25 | 108.9 (4) |
O21—Mo7—O19 | 103.66 (11) | C27—N13—H13N | 126 (2) |
O21—Mo7—O22 | 102.76 (10) | C25—N13—H13N | 125 (2) |
O19—Mo7—O22 | 101.19 (9) | C27—N14—C26 | 106.3 (4) |
O21—Mo7—O20 | 101.84 (10) | C30—C29—N15 | 105.7 (3) |
O19—Mo7—O20 | 100.32 (9) | C30—C29—H29 | 127.1 |
O22—Mo7—O20 | 142.21 (8) | N15—C29—H29 | 127.1 |
O21—Mo7—O24 | 85.71 (9) | C29—C30—N16 | 109.6 (3) |
O19—Mo7—O24 | 170.59 (8) | C29—C30—H30 | 125.2 |
O22—Mo7—O24 | 77.15 (8) | N16—C30—H30 | 125.2 |
O20—Mo7—O24 | 76.58 (8) | N16—C31—N15 | 110.4 (3) |
O21—Mo7—O23 | 174.78 (9) | N16—C31—C32 | 125.2 (3) |
O19—Mo7—O23 | 81.55 (8) | N15—C31—C32 | 124.4 (3) |
O22—Mo7—O23 | 76.12 (8) | C31—C32—H32A | 109.5 |
O20—Mo7—O23 | 76.77 (8) | C31—C32—H32B | 109.5 |
O24—Mo7—O23 | 89.07 (6) | H32A—C32—H32B | 109.5 |
C2—C1—N1 | 106.8 (3) | C31—C32—H32C | 109.5 |
C2—C1—H1 | 126.6 | H32A—C32—H32C | 109.5 |
N1—C1—H1 | 126.6 | H32B—C32—H32C | 109.5 |
C1—C2—N2 | 106.9 (3) | C31—N15—C29 | 108.1 (3) |
C1—C2—H2 | 126.6 | C31—N15—H15N | 127.1 (19) |
N2—C2—H2 | 126.6 | C29—N15—H15N | 124.8 (19) |
N1—C3—N2 | 108.0 (3) | C31—N16—C30 | 106.1 (3) |
N1—C3—C4 | 125.0 (3) | H25V—O25—H25W | 105 (3) |
N2—C3—C4 | 127.0 (3) | H26V—O26—H26W | 107 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N···O22i | 0.88 (2) | 1.85 (2) | 2.710 (3) | 167 (2) |
N2—H2N···O20 | 0.87 (2) | 1.79 (2) | 2.655 (3) | 172 (2) |
N3—H3N···O18i | 0.88 (2) | 1.87 (2) | 2.743 (4) | 171 (5) |
N4—H4N···O9 | 0.88 (2) | 1.79 (2) | 2.662 (4) | 171 (5) |
N5—H5N···O12 | 0.89 (2) | 1.77 (3) | 2.644 (4) | 168 (4) |
N6—H6N···O3ii | 0.90 (2) | 1.80 (3) | 2.684 (4) | 168 (5) |
N7—H7N···O1iii | 0.89 (3) | 1.83 (3) | 2.697 (4) | 167 (3) |
N8—H8N···O25 | 0.89 (3) | 1.78 (3) | 2.659 (4) | 172 (5) |
N9—H9N···N14iv | 0.89 (2) | 1.81 (2) | 2.698 (4) | 177 (3) |
N10—H10N···O15 | 0.88 (2) | 1.98 (2) | 2.852 (3) | 174 (3) |
N11—H11N···O6 | 0.88 (2) | 1.78 (2) | 2.636 (3) | 166 (3) |
N12—H12N···N16v | 0.88 (2) | 1.87 (2) | 2.725 (4) | 165 (3) |
N13—H13N···O5 | 0.88 (4) | 2.32 (4) | 3.186 (5) | 167 (3) |
N13—H13N···O8 | 0.88 (4) | 2.55 (4) | 3.043 (5) | 116 (2) |
N15—H15N···O14 | 0.87 (3) | 2.22 (3) | 2.953 (4) | 142 (3) |
N15—H15N···O17 | 0.87 (3) | 2.27 (3) | 2.917 (4) | 132 (3) |
O25—H25V···O19 | 0.86 (2) | 2.00 (2) | 2.788 (3) | 154 (5) |
O25—H25W···O26vi | 0.86 (3) | 1.85 (3) | 2.702 (4) | 176 (5) |
O26—H26V···O10 | 0.83 (4) | 2.50 (6) | 2.999 (4) | 119 (5) |
O26—H26V···O13 | 0.83 (4) | 2.25 (5) | 3.009 (4) | 151 (6) |
O26—H26W···O7 | 0.83 (4) | 1.99 (6) | 2.737 (4) | 149 (6) |
C4—H4A···O8 | 0.98 | 2.35 | 3.228 (5) | 149 |
C8—H8B···O2i | 0.98 | 2.54 | 3.517 (6) | 176 |
C8—H8C···O8 | 0.98 | 2.49 | 3.386 (5) | 152 |
C10—H10···O26vii | 0.95 | 2.45 | 3.318 (5) | 151 |
C12—H12A···O5ii | 0.98 | 2.44 | 3.407 (5) | 167 |
C13—H13···O4iii | 0.95 | 2.50 | 3.297 (6) | 141 |
C17—H17···O2viii | 0.95 | 2.46 | 3.154 (4) | 130 |
C18—H18···O26 | 0.95 | 2.58 | 3.522 (5) | 172 |
C21—H21···O16 | 0.95 | 2.46 | 3.302 (4) | 147 |
C22—H22···O11ix | 0.95 | 2.22 | 3.113 (4) | 156 |
C24—H24B···O7 | 0.98 | 2.50 | 3.346 (5) | 145 |
C25—H25···O8 | 0.95 | 2.59 | 3.055 (5) | 110 |
C32—H32B···O14 | 0.98 | 2.55 | 3.234 (5) | 126 |
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+1/2, y+1/2, −z+3/2; (v) −x+1/2, y−1/2, −z+3/2; (vi) x−1/2, −y+1/2, z−1/2; (vii) −x+1, −y+1, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x−1/2, −y+1/2, z+1/2. |
Acknowledgements
The authors thank the Université Cheikh Anta Diop Dakar-Sénégal, the Laboratoire de Chimie et de Physique des Matériaux (LCPM) de l'Université Assane Seck de Ziguinchor, Sénégal and the service commun d'analyse par diffraction des rayons X, Universitée de Bretagne Occidentale, France for financial support. All measurements were performed in the institutes above quoted.
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