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First reported in 1930, MoCl3O(Et2O)2 is a by-product of the reductive synthesis of MoCl4(OEt2)2 from MoCl5. We report herein the X-ray crystal structure and Hirshfeld surface characteristics of mer-MoCl3O(Et2O)2, or [MoCl3O(C4H10O)2]. The com­pound crystallizes in the ortho­rhom­bic space group P212121. The molyb­denyl (Mo=O) bond length is 1.694 (3) Å and the cis- and trans-Mo—O distances are 2.157 (3) and 2.304 (3) Å, respectively. Inter­molecular Mo=O...H bonding is present in the lattice, with the shortest distance being 2.572 Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229620011626/ef3009sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229620011626/ef3009Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229620011626/ef3009sup3.pdf
Supplementary material

CCDC reference: 2013034

Computing details top

Data collection: CrysAlis PRO (Rigaku Oxford Diffraction, 2020); cell refinement: CrysAlis PRO (Rigaku Oxford Diffraction, 2020); data reduction: CrysAlis PRO (Rigaku Oxford Diffraction, 2020); program(s) used to solve structure: SHELXT2018 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Trichloridobis(diethyl ether)oxidomolybdenum(V) top
Crystal data top
[MoCl3O(C4H10O)2]Dx = 1.700 Mg m3
Mr = 366.53Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 3727 reflections
a = 8.6186 (7) Åθ = 2.2–30.5°
b = 12.250 (1) ŵ = 1.46 mm1
c = 13.5681 (11) ÅT = 100 K
V = 1432.5 (2) Å3Block, green
Z = 40.6 × 0.21 × 0.16 mm
F(000) = 740
Data collection top
Rigaku XtaLAB Mini II
diffractometer
Rint = 0.042
Absorption correction: gaussian
(CrysAlis PRO; Rigaku Oxford Diffraction, 2020)
θmax = 27.5°, θmin = 2.2°
Tmin = 0.614, Tmax = 0.831h = 1110
7488 measured reflectionsk = 1515
3179 independent reflectionsl = 1716
2959 reflections with I > 2σ(I)
Refinement top
Refinement on F2H atoms treated by a mixture of independent and constrained refinement
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0278P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.033(Δ/σ)max < 0.001
wR(F2) = 0.069Δρmax = 0.53 e Å3
S = 1.01Δρmin = 0.87 e Å3
3179 reflectionsExtinction correction: SHELXL2018 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
153 parametersExtinction coefficient: 0.0042 (6)
0 restraintsAbsolute structure: Flack x determined using 1123 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Hydrogen site location: mixedAbsolute structure parameter: 0.01 (5)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.14299 (5)0.44571 (3)0.49142 (3)0.01453 (13)
Cl30.28566 (14)0.58992 (10)0.56149 (9)0.0189 (3)
Cl10.00756 (16)0.33468 (10)0.38785 (9)0.0220 (3)
Cl20.07724 (14)0.49900 (10)0.57657 (9)0.0209 (3)
O20.3298 (4)0.4174 (3)0.3888 (2)0.0174 (8)
O30.0863 (4)0.5768 (2)0.3751 (2)0.0144 (7)
O10.2054 (4)0.3474 (3)0.5698 (2)0.0168 (8)
C50.0851 (6)0.5576 (4)0.2693 (3)0.0182 (11)
H5A0.135 (6)0.491 (4)0.258 (4)0.022*
H5B0.160 (6)0.612 (4)0.235 (4)0.022*
C60.0733 (6)0.5618 (4)0.2246 (4)0.0236 (12)
H6A0.0660490.5471340.1537690.035*
H6B0.1181330.6344220.2350480.035*
H6C0.1395160.5066950.2557530.035*
C70.0422 (6)0.6881 (4)0.4026 (4)0.0190 (12)
H7A0.0275850.6916990.4748580.023*
H7B0.0582130.7062620.3711060.023*
C30.4417 (6)0.4994 (4)0.3559 (4)0.0224 (12)
H3A0.3960330.5728730.3649030.027*
H3B0.4614790.4891610.2845770.027*
C10.3840 (7)0.3043 (5)0.3786 (4)0.0229 (13)
H1A0.289 (6)0.265 (4)0.396 (4)0.027*
H1B0.467 (6)0.293 (4)0.421 (4)0.027*
C80.1614 (7)0.7714 (4)0.3723 (4)0.0286 (13)
H8A0.1742680.7697150.3005480.043*
H8B0.2607230.7545670.4040310.043*
H8C0.1269300.8442670.3926190.043*
C20.4275 (8)0.2761 (4)0.2751 (4)0.0314 (14)
H2A0.3401210.2918470.2311390.047*
H2B0.4535180.1983660.2711390.047*
H2C0.5175730.3196930.2551010.047*
C40.5935 (6)0.4942 (5)0.4102 (4)0.0346 (15)
H4A0.6478420.4266570.3926710.052*
H4B0.5739640.4953830.4813240.052*
H4C0.6575490.5571150.3919580.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01522 (19)0.0139 (2)0.0144 (2)0.00072 (17)0.00121 (18)0.00088 (18)
Cl30.0200 (6)0.0202 (6)0.0165 (6)0.0034 (5)0.0024 (5)0.0025 (5)
Cl10.0286 (7)0.0161 (6)0.0213 (7)0.0050 (6)0.0044 (6)0.0019 (6)
Cl20.0174 (6)0.0251 (7)0.0202 (7)0.0015 (6)0.0047 (6)0.0008 (6)
O20.0203 (18)0.0119 (17)0.0200 (18)0.0030 (14)0.0045 (15)0.0044 (14)
O30.0205 (17)0.0124 (18)0.0103 (16)0.0035 (14)0.0016 (14)0.0012 (14)
O10.0164 (17)0.0174 (18)0.0166 (18)0.0003 (15)0.0010 (15)0.0014 (16)
C50.025 (3)0.021 (3)0.009 (2)0.002 (3)0.002 (2)0.002 (2)
C60.029 (3)0.023 (3)0.019 (3)0.000 (3)0.007 (2)0.001 (3)
C70.024 (3)0.008 (2)0.024 (3)0.004 (2)0.001 (2)0.001 (2)
C30.022 (3)0.023 (3)0.022 (3)0.004 (2)0.007 (2)0.003 (2)
C10.031 (3)0.018 (3)0.020 (3)0.012 (2)0.002 (3)0.002 (2)
C80.041 (3)0.014 (3)0.031 (3)0.001 (3)0.003 (3)0.000 (2)
C20.051 (4)0.021 (3)0.022 (3)0.011 (3)0.007 (3)0.003 (3)
C40.019 (3)0.050 (4)0.035 (3)0.001 (3)0.005 (3)0.001 (3)
Geometric parameters (Å, º) top
Mo1—Cl12.3469 (13)C7—H7B0.9900
Mo1—Cl32.3530 (13)C7—C81.506 (7)
Mo1—Cl22.3159 (13)C3—H3A0.9900
Mo1—O11.694 (3)C3—H3B0.9900
Mo1—O22.157 (3)C3—C41.502 (7)
Mo1—O32.304 (3)C1—H1A0.97 (5)
O2—C11.468 (6)C1—H1B0.93 (5)
O2—C31.463 (6)C1—C21.493 (7)
O3—C51.455 (5)C8—H8A0.9800
O3—C71.463 (5)C8—H8B0.9800
C5—H5A0.93 (5)C8—H8C0.9800
C5—H5B1.04 (5)C2—H2A0.9800
C5—C61.494 (7)C2—H2B0.9800
C6—H6A0.9800C2—H2C0.9800
C6—H6B0.9800C4—H4A0.9800
C6—H6C0.9800C4—H4B0.9800
C7—H7A0.9900C4—H4C0.9800
O1—Mo1—O3173.06 (14)O3—C7—C8112.6 (4)
O2—Mo1—Cl2168.30 (9)H7A—C7—H7B107.8
Cl1—Mo1—Cl3165.00 (5)C8—C7—H7A109.1
O1—Mo1—Cl298.48 (12)C8—C7—H7B109.1
O1—Mo1—Cl198.02 (11)O2—C3—H3A108.9
O1—Mo1—Cl396.55 (11)O2—C3—H3B108.9
O1—Mo1—O293.09 (14)O2—C3—C4113.3 (4)
O3—Mo1—Cl288.37 (9)H3A—C3—H3B107.7
O3—Mo1—Cl182.92 (8)C4—C3—H3A108.9
O3—Mo1—Cl382.19 (8)C4—C3—H3B108.9
O2—Mo1—O380.10 (11)O2—C1—H1A100 (3)
Cl2—Mo1—Cl390.87 (5)O2—C1—H1B109 (3)
Cl2—Mo1—Cl190.51 (5)O2—C1—C2112.7 (4)
O2—Mo1—Cl389.52 (9)H1A—C1—H1B115 (4)
O2—Mo1—Cl186.14 (10)C2—C1—H1A109 (3)
C3—O2—Mo1125.4 (3)C2—C1—H1B110 (3)
C3—O2—C1114.2 (4)C7—C8—H8A109.5
C1—O2—Mo1116.8 (3)C7—C8—H8B109.5
C5—O3—Mo1124.4 (3)C7—C8—H8C109.5
C5—O3—C7113.6 (4)H8A—C8—H8B109.5
C7—O3—Mo1122.0 (3)H8A—C8—H8C109.5
O3—C5—H5A107 (3)H8B—C8—H8C109.5
O3—C5—H5B110 (3)C1—C2—H2A109.5
O3—C5—C6113.7 (4)C1—C2—H2B109.5
H5A—C5—H5B101 (4)C1—C2—H2C109.5
C6—C5—H5A113 (3)H2A—C2—H2B109.5
C6—C5—H5B111 (3)H2A—C2—H2C109.5
C5—C6—H6A109.5H2B—C2—H2C109.5
C5—C6—H6B109.5C3—C4—H4A109.5
C5—C6—H6C109.5C3—C4—H4B109.5
H6A—C6—H6B109.5C3—C4—H4C109.5
H6A—C6—H6C109.5H4A—C4—H4B109.5
H6B—C6—H6C109.5H4A—C4—H4C109.5
O3—C7—H7A109.1H4B—C4—H4C109.5
O3—C7—H7B109.1
Mo1—O2—C3—C498.5 (5)C5—O3—C7—C868.7 (5)
Mo1—O2—C1—C2143.0 (4)C7—O3—C5—C667.0 (5)
Mo1—O3—C5—C6110.8 (4)C3—O2—C1—C257.5 (6)
Mo1—O3—C7—C8113.4 (4)C1—O2—C3—C458.9 (6)
Comparative Mo—L and Mo—X bond lengths of MoCl3O(Et2O)2 (2) and analogous complexes (Marchetti et al., 2013; Vitzthumecker et al., 2017; Di Nicola et al., 2015) top
MoCl3O(Et2O)2MoCl3O(thf)2MoCl3O(MeOH)2MoCl3O(MeO(CH2)2OCH2Cl)
Mo1—Cl1 2.353 (1)Mo—Cl2 2.3513 (9)Mo1—Cl2 2.3642 (8)Mo1—Cl5 2.3542 (8)
Mo1—Cl3 2.347 (1)Mo—Cl1 2.3646 (8)Mo1—Cl1 2.3434 (7)Mo1—Cl4 2.3453 (7)
Mo1—Cl2 2.316 (1)Mo—Cl3 2.3191 (9)Mo1—Cl3 2.3741 (9)Mo1—Cl2 2.3216 (7)
Mo1—O2 2.158 (3)Mo—O2(thf) 2.146 (2)Mo—O2 2.099 (2)Mo1—O2 2.161 (2)
Mo1—O3 2.305 (3)Mo—O3(thf) 2.277 (2)Mo—O3 2.266 (2)Mo1—O3 2.420 (2)
Mo1—O1 1.694 (3)Mo—O1(oxide) 1.682 (2)Mo1—O1 1.655 (2)Mo1—O1 1.666 (2)
 

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