Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229620011626/ef3009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229620011626/ef3009Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229620011626/ef3009sup3.pdf |
CCDC reference: 2013034
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).
[MoCl3O(C4H10O)2] | Dx = 1.700 Mg m−3 |
Mr = 366.53 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 3727 reflections |
a = 8.6186 (7) Å | θ = 2.2–30.5° |
b = 12.250 (1) Å | µ = 1.46 mm−1 |
c = 13.5681 (11) Å | T = 100 K |
V = 1432.5 (2) Å3 | Block, green |
Z = 4 | 0.6 × 0.21 × 0.16 mm |
F(000) = 740 |
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 = 0.831 | h = −11→10 |
7488 measured reflections | k = −15→15 |
3179 independent reflections | l = −17→16 |
2959 reflections with I > 2σ(I) |
Refinement on F2 | H 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) = 0.069 | Δρmax = 0.53 e Å−3 |
S = 1.01 | Δρmin = −0.87 e Å−3 |
3179 reflections | Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
153 parameters | Extinction coefficient: 0.0042 (6) |
0 restraints | Absolute structure: Flack x determined using 1123 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
Hydrogen site location: mixed | Absolute structure parameter: 0.01 (5) |
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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.14299 (5) | 0.44571 (3) | 0.49142 (3) | 0.01453 (13) | |
Cl3 | 0.28566 (14) | 0.58992 (10) | 0.56149 (9) | 0.0189 (3) | |
Cl1 | −0.00756 (16) | 0.33468 (10) | 0.38785 (9) | 0.0220 (3) | |
Cl2 | −0.07724 (14) | 0.49900 (10) | 0.57657 (9) | 0.0209 (3) | |
O2 | 0.3298 (4) | 0.4174 (3) | 0.3888 (2) | 0.0174 (8) | |
O3 | 0.0863 (4) | 0.5768 (2) | 0.3751 (2) | 0.0144 (7) | |
O1 | 0.2054 (4) | 0.3474 (3) | 0.5698 (2) | 0.0168 (8) | |
C5 | 0.0851 (6) | 0.5576 (4) | 0.2693 (3) | 0.0182 (11) | |
H5A | 0.135 (6) | 0.491 (4) | 0.258 (4) | 0.022* | |
H5B | 0.160 (6) | 0.612 (4) | 0.235 (4) | 0.022* | |
C6 | −0.0733 (6) | 0.5618 (4) | 0.2246 (4) | 0.0236 (12) | |
H6A | −0.066049 | 0.547134 | 0.153769 | 0.035* | |
H6B | −0.118133 | 0.634422 | 0.235048 | 0.035* | |
H6C | −0.139516 | 0.506695 | 0.255753 | 0.035* | |
C7 | 0.0422 (6) | 0.6881 (4) | 0.4026 (4) | 0.0190 (12) | |
H7A | 0.027585 | 0.691699 | 0.474858 | 0.023* | |
H7B | −0.058213 | 0.706262 | 0.371106 | 0.023* | |
C3 | 0.4417 (6) | 0.4994 (4) | 0.3559 (4) | 0.0224 (12) | |
H3A | 0.396033 | 0.572873 | 0.364903 | 0.027* | |
H3B | 0.461479 | 0.489161 | 0.284577 | 0.027* | |
C1 | 0.3840 (7) | 0.3043 (5) | 0.3786 (4) | 0.0229 (13) | |
H1A | 0.289 (6) | 0.265 (4) | 0.396 (4) | 0.027* | |
H1B | 0.467 (6) | 0.293 (4) | 0.421 (4) | 0.027* | |
C8 | 0.1614 (7) | 0.7714 (4) | 0.3723 (4) | 0.0286 (13) | |
H8A | 0.174268 | 0.769715 | 0.300548 | 0.043* | |
H8B | 0.260723 | 0.754567 | 0.404031 | 0.043* | |
H8C | 0.126930 | 0.844267 | 0.392619 | 0.043* | |
C2 | 0.4275 (8) | 0.2761 (4) | 0.2751 (4) | 0.0314 (14) | |
H2A | 0.340121 | 0.291847 | 0.231139 | 0.047* | |
H2B | 0.453518 | 0.198366 | 0.271139 | 0.047* | |
H2C | 0.517573 | 0.319693 | 0.255101 | 0.047* | |
C4 | 0.5935 (6) | 0.4942 (5) | 0.4102 (4) | 0.0346 (15) | |
H4A | 0.647842 | 0.426657 | 0.392671 | 0.052* | |
H4B | 0.573964 | 0.495383 | 0.481324 | 0.052* | |
H4C | 0.657549 | 0.557115 | 0.391958 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01522 (19) | 0.0139 (2) | 0.0144 (2) | −0.00072 (17) | 0.00121 (18) | −0.00088 (18) |
Cl3 | 0.0200 (6) | 0.0202 (6) | 0.0165 (6) | −0.0034 (5) | −0.0024 (5) | −0.0025 (5) |
Cl1 | 0.0286 (7) | 0.0161 (6) | 0.0213 (7) | −0.0050 (6) | −0.0044 (6) | −0.0019 (6) |
Cl2 | 0.0174 (6) | 0.0251 (7) | 0.0202 (7) | 0.0015 (6) | 0.0047 (6) | −0.0008 (6) |
O2 | 0.0203 (18) | 0.0119 (17) | 0.0200 (18) | 0.0030 (14) | 0.0045 (15) | 0.0044 (14) |
O3 | 0.0205 (17) | 0.0124 (18) | 0.0103 (16) | 0.0035 (14) | −0.0016 (14) | −0.0012 (14) |
O1 | 0.0164 (17) | 0.0174 (18) | 0.0166 (18) | 0.0003 (15) | 0.0010 (15) | −0.0014 (16) |
C5 | 0.025 (3) | 0.021 (3) | 0.009 (2) | 0.002 (3) | 0.002 (2) | −0.002 (2) |
C6 | 0.029 (3) | 0.023 (3) | 0.019 (3) | 0.000 (3) | −0.007 (2) | −0.001 (3) |
C7 | 0.024 (3) | 0.008 (2) | 0.024 (3) | 0.004 (2) | −0.001 (2) | −0.001 (2) |
C3 | 0.022 (3) | 0.023 (3) | 0.022 (3) | −0.004 (2) | 0.007 (2) | 0.003 (2) |
C1 | 0.031 (3) | 0.018 (3) | 0.020 (3) | 0.012 (2) | 0.002 (3) | 0.002 (2) |
C8 | 0.041 (3) | 0.014 (3) | 0.031 (3) | −0.001 (3) | −0.003 (3) | 0.000 (2) |
C2 | 0.051 (4) | 0.021 (3) | 0.022 (3) | 0.011 (3) | 0.007 (3) | −0.003 (3) |
C4 | 0.019 (3) | 0.050 (4) | 0.035 (3) | −0.001 (3) | 0.005 (3) | −0.001 (3) |
Mo1—Cl1 | 2.3469 (13) | C7—H7B | 0.9900 |
Mo1—Cl3 | 2.3530 (13) | C7—C8 | 1.506 (7) |
Mo1—Cl2 | 2.3159 (13) | C3—H3A | 0.9900 |
Mo1—O1 | 1.694 (3) | C3—H3B | 0.9900 |
Mo1—O2 | 2.157 (3) | C3—C4 | 1.502 (7) |
Mo1—O3 | 2.304 (3) | C1—H1A | 0.97 (5) |
O2—C1 | 1.468 (6) | C1—H1B | 0.93 (5) |
O2—C3 | 1.463 (6) | C1—C2 | 1.493 (7) |
O3—C5 | 1.455 (5) | C8—H8A | 0.9800 |
O3—C7 | 1.463 (5) | C8—H8B | 0.9800 |
C5—H5A | 0.93 (5) | C8—H8C | 0.9800 |
C5—H5B | 1.04 (5) | C2—H2A | 0.9800 |
C5—C6 | 1.494 (7) | C2—H2B | 0.9800 |
C6—H6A | 0.9800 | C2—H2C | 0.9800 |
C6—H6B | 0.9800 | C4—H4A | 0.9800 |
C6—H6C | 0.9800 | C4—H4B | 0.9800 |
C7—H7A | 0.9900 | C4—H4C | 0.9800 |
O1—Mo1—O3 | 173.06 (14) | O3—C7—C8 | 112.6 (4) |
O2—Mo1—Cl2 | 168.30 (9) | H7A—C7—H7B | 107.8 |
Cl1—Mo1—Cl3 | 165.00 (5) | C8—C7—H7A | 109.1 |
O1—Mo1—Cl2 | 98.48 (12) | C8—C7—H7B | 109.1 |
O1—Mo1—Cl1 | 98.02 (11) | O2—C3—H3A | 108.9 |
O1—Mo1—Cl3 | 96.55 (11) | O2—C3—H3B | 108.9 |
O1—Mo1—O2 | 93.09 (14) | O2—C3—C4 | 113.3 (4) |
O3—Mo1—Cl2 | 88.37 (9) | H3A—C3—H3B | 107.7 |
O3—Mo1—Cl1 | 82.92 (8) | C4—C3—H3A | 108.9 |
O3—Mo1—Cl3 | 82.19 (8) | C4—C3—H3B | 108.9 |
O2—Mo1—O3 | 80.10 (11) | O2—C1—H1A | 100 (3) |
Cl2—Mo1—Cl3 | 90.87 (5) | O2—C1—H1B | 109 (3) |
Cl2—Mo1—Cl1 | 90.51 (5) | O2—C1—C2 | 112.7 (4) |
O2—Mo1—Cl3 | 89.52 (9) | H1A—C1—H1B | 115 (4) |
O2—Mo1—Cl1 | 86.14 (10) | C2—C1—H1A | 109 (3) |
C3—O2—Mo1 | 125.4 (3) | C2—C1—H1B | 110 (3) |
C3—O2—C1 | 114.2 (4) | C7—C8—H8A | 109.5 |
C1—O2—Mo1 | 116.8 (3) | C7—C8—H8B | 109.5 |
C5—O3—Mo1 | 124.4 (3) | C7—C8—H8C | 109.5 |
C5—O3—C7 | 113.6 (4) | H8A—C8—H8B | 109.5 |
C7—O3—Mo1 | 122.0 (3) | H8A—C8—H8C | 109.5 |
O3—C5—H5A | 107 (3) | H8B—C8—H8C | 109.5 |
O3—C5—H5B | 110 (3) | C1—C2—H2A | 109.5 |
O3—C5—C6 | 113.7 (4) | C1—C2—H2B | 109.5 |
H5A—C5—H5B | 101 (4) | C1—C2—H2C | 109.5 |
C6—C5—H5A | 113 (3) | H2A—C2—H2B | 109.5 |
C6—C5—H5B | 111 (3) | H2A—C2—H2C | 109.5 |
C5—C6—H6A | 109.5 | H2B—C2—H2C | 109.5 |
C5—C6—H6B | 109.5 | C3—C4—H4A | 109.5 |
C5—C6—H6C | 109.5 | C3—C4—H4B | 109.5 |
H6A—C6—H6B | 109.5 | C3—C4—H4C | 109.5 |
H6A—C6—H6C | 109.5 | H4A—C4—H4B | 109.5 |
H6B—C6—H6C | 109.5 | H4A—C4—H4C | 109.5 |
O3—C7—H7A | 109.1 | H4B—C4—H4C | 109.5 |
O3—C7—H7B | 109.1 | ||
Mo1—O2—C3—C4 | 98.5 (5) | C5—O3—C7—C8 | −68.7 (5) |
Mo1—O2—C1—C2 | 143.0 (4) | C7—O3—C5—C6 | −67.0 (5) |
Mo1—O3—C5—C6 | 110.8 (4) | C3—O2—C1—C2 | −57.5 (6) |
Mo1—O3—C7—C8 | 113.4 (4) | C1—O2—C3—C4 | −58.9 (6) |
MoCl3O(Et2O)2 | MoCl3O(thf)2 | MoCl3O(MeOH)2 | MoCl3O(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) |