Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040517/wm2040sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040517/wm2040Isup2.hkl |
CCDC reference: 628424
Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Bruker, 2004); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C24H20P)2[Mo6Cl8(CF3O3S)6]·C4H10O·CH2Cl2 | Z = 1 |
Mr = 2432.40 | F(000) = 1184 |
Triclinic, P1 | Dx = 1.927 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8710 (4) Å | Cell parameters from 5957 reflections |
b = 13.8264 (5) Å | θ = 3.1–36.9° |
c = 14.0267 (5) Å | µ = 1.41 mm−1 |
α = 74.640 (2)° | T = 100 K |
β = 75.367 (2)° | Irregular chunk, yellow |
γ = 74.263 (2)° | 0.26 × 0.20 × 0.20 mm |
V = 2095.87 (13) Å3 |
Bruker APEX2 CCD diffractometer | 9451 independent reflections |
Radiation source: fine-focus sealed tube | 7868 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003) | h = −15→15 |
Tmin = 0.53, Tmax = 0.75 | k = −17→17 |
24669 measured reflections | l = −18→16 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0615P)2] where P = (Fo2 + 2Fc2)/3 |
9451 reflections | (Δ/σ)max = 0.003 |
505 parameters | Δρmax = 1.40 e Å−3 |
0 restraints | Δρmin = −1.25 e Å−3 |
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. SQUEEZE in PLATON was used to remove the highly disordered solvent molecules. The. ins file, free of Q peaks was used in the SQUEEZE program, resulting in the removal of the electron density representing the solvent molecules. After convergence, the. res file was then used in PLATON to produce the table of structure factors reflecting the removal of solvent molecules. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 1.008560 (18) | −0.087774 (16) | 0.418910 (17) | 0.01547 (7) | |
Mo2 | 1.094110 (18) | 0.073010 (16) | 0.397219 (17) | 0.01534 (7) | |
Mo3 | 0.867195 (18) | 0.083276 (16) | 0.455328 (17) | 0.01520 (7) | |
Cl1 | 1.04601 (5) | −0.23196 (4) | 0.56319 (5) | 0.01801 (13) | |
Cl3 | 0.79305 (5) | −0.07246 (5) | 0.47757 (5) | 0.01844 (13) | |
Cl4 | 0.97092 (5) | 0.06468 (5) | 0.28296 (5) | 0.01911 (13) | |
Cl2 | 1.22541 (5) | −0.09320 (5) | 0.36740 (5) | 0.01843 (13) | |
P1 | 0.50929 (6) | 0.67065 (5) | 0.20173 (5) | 0.01805 (14) | |
C24 | 0.7475 (2) | 0.6585 (2) | 0.1147 (2) | 0.0240 (6) | |
H24 | 0.7241 | 0.7296 | 0.0866 | 0.029* | |
C20 | 0.6968 (2) | 0.5008 (2) | 0.2197 (2) | 0.0223 (6) | |
H20 | 0.6390 | 0.4645 | 0.2626 | 0.027* | |
C13 | 0.4358 (2) | 0.6626 (2) | 0.1079 (2) | 0.0219 (6) | |
C21 | 0.8153 (3) | 0.4501 (2) | 0.1978 (2) | 0.0256 (6) | |
H21 | 0.8390 | 0.3791 | 0.2264 | 0.031* | |
C19 | 0.6634 (2) | 0.6048 (2) | 0.1787 (2) | 0.0191 (5) | |
C6 | 0.4330 (3) | 0.8816 (2) | 0.1387 (2) | 0.0258 (6) | |
H6 | 0.3867 | 0.8659 | 0.1009 | 0.031* | |
C8 | 0.4138 (2) | 0.6517 (2) | 0.4072 (2) | 0.0219 (6) | |
H8 | 0.4391 | 0.7127 | 0.4022 | 0.026* | |
C7 | 0.4336 (2) | 0.6113 (2) | 0.3221 (2) | 0.0195 (5) | |
C4 | 0.4991 (3) | 1.0056 (2) | 0.1912 (2) | 0.0332 (7) | |
H4 | 0.4970 | 1.0753 | 0.1893 | 0.040* | |
C12 | 0.3944 (2) | 0.5224 (2) | 0.3300 (2) | 0.0244 (6) | |
H12 | 0.4070 | 0.4948 | 0.2720 | 0.029* | |
C1 | 0.5042 (2) | 0.8028 (2) | 0.1970 (2) | 0.0196 (5) | |
C11 | 0.3371 (3) | 0.4743 (2) | 0.4224 (2) | 0.0263 (6) | |
H11 | 0.3109 | 0.4136 | 0.4278 | 0.032* | |
C3 | 0.5708 (3) | 0.9275 (2) | 0.2485 (2) | 0.0285 (6) | |
H3 | 0.6176 | 0.9435 | 0.2856 | 0.034* | |
C14 | 0.5022 (3) | 0.6416 (2) | 0.0160 (2) | 0.0267 (6) | |
H14 | 0.5869 | 0.6275 | 0.0037 | 0.032* | |
C16 | 0.3205 (3) | 0.6607 (3) | −0.0394 (3) | 0.0442 (9) | |
H16 | 0.2811 | 0.6609 | −0.0906 | 0.053* | |
C9 | 0.3571 (3) | 0.6030 (2) | 0.4994 (2) | 0.0244 (6) | |
H9 | 0.3449 | 0.6301 | 0.5577 | 0.029* | |
C10 | 0.3183 (2) | 0.5152 (2) | 0.5068 (2) | 0.0249 (6) | |
H10 | 0.2786 | 0.4827 | 0.5700 | 0.030* | |
C5 | 0.4306 (3) | 0.9832 (2) | 0.1366 (2) | 0.0315 (7) | |
H5 | 0.3818 | 1.0375 | 0.0977 | 0.038* | |
C2 | 0.5736 (2) | 0.8264 (2) | 0.2513 (2) | 0.0238 (6) | |
H2 | 0.6228 | 0.7726 | 0.2902 | 0.029* | |
C17 | 0.2551 (3) | 0.6796 (4) | 0.0523 (3) | 0.0507 (10) | |
H17 | 0.1706 | 0.6908 | 0.0649 | 0.061* | |
C15 | 0.4438 (3) | 0.6414 (3) | −0.0571 (2) | 0.0358 (7) | |
H15 | 0.4887 | 0.6279 | −0.1204 | 0.043* | |
C22 | 0.8997 (3) | 0.5033 (2) | 0.1335 (2) | 0.0267 (6) | |
H22 | 0.9806 | 0.4683 | 0.1180 | 0.032* | |
C23 | 0.8658 (3) | 0.6071 (2) | 0.0923 (2) | 0.0277 (6) | |
H23 | 0.9235 | 0.6431 | 0.0488 | 0.033* | |
S1 | 0.63441 (6) | 0.19045 (5) | 0.34168 (5) | 0.01865 (14) | |
S3 | 1.19429 (6) | 0.24088 (5) | 0.19454 (5) | 0.02082 (15) | |
S2 | 0.95144 (6) | −0.24132 (5) | 0.29128 (6) | 0.02637 (16) | |
O1 | 0.71551 (16) | 0.18964 (14) | 0.40749 (15) | 0.0215 (4) | |
O7 | 1.02673 (17) | −0.19195 (14) | 0.32565 (16) | 0.0245 (4) | |
O4 | 1.21051 (16) | 0.15499 (13) | 0.28338 (14) | 0.0208 (4) | |
O6 | 1.07361 (18) | 0.27269 (15) | 0.17971 (18) | 0.0309 (5) | |
O5 | 1.28803 (19) | 0.22638 (15) | 0.11008 (16) | 0.0300 (5) | |
F1 | 0.53633 (15) | 0.08116 (13) | 0.50813 (13) | 0.0324 (4) | |
F2 | 0.42934 (15) | 0.13940 (15) | 0.39353 (15) | 0.0380 (5) | |
O2 | 0.67538 (18) | 0.10750 (16) | 0.29069 (17) | 0.0292 (5) | |
F3 | 0.44794 (16) | 0.23997 (14) | 0.47964 (15) | 0.0388 (5) | |
F4 | 1.14049 (19) | 0.36600 (15) | 0.31855 (17) | 0.0489 (6) | |
F6 | 1.32786 (17) | 0.32458 (14) | 0.25758 (16) | 0.0394 (5) | |
O3 | 0.59391 (18) | 0.29215 (15) | 0.28697 (16) | 0.0271 (4) | |
F5 | 1.21048 (18) | 0.43092 (13) | 0.16414 (17) | 0.0428 (5) | |
F8 | 0.9270 (2) | −0.43049 (16) | 0.34287 (18) | 0.0519 (6) | |
C25 | 0.5043 (2) | 0.1611 (2) | 0.4361 (2) | 0.0242 (6) | |
C26 | 1.2193 (3) | 0.3463 (2) | 0.2370 (3) | 0.0294 (7) | |
O9 | 0.9963 (3) | −0.2521 (2) | 0.18949 (19) | 0.0488 (7) | |
F7 | 1.0979 (2) | −0.41236 (16) | 0.3480 (3) | 0.0821 (10) | |
O8 | 0.8279 (2) | −0.2034 (2) | 0.3216 (3) | 0.0555 (8) | |
F9 | 0.9458 (3) | −0.3709 (2) | 0.46296 (19) | 0.0833 (10) | |
C27 | 0.9831 (3) | −0.3714 (3) | 0.3662 (3) | 0.0421 (9) | |
C18 | 0.3114 (3) | 0.6823 (3) | 0.1263 (3) | 0.0370 (8) | |
H18 | 0.2660 | 0.6973 | 0.1890 | 0.044* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01319 (11) | 0.01394 (11) | 0.01941 (13) | −0.00191 (8) | −0.00443 (9) | −0.00363 (9) |
Mo2 | 0.01223 (11) | 0.01409 (11) | 0.01891 (13) | −0.00211 (8) | −0.00366 (9) | −0.00232 (9) |
Mo3 | 0.01187 (11) | 0.01377 (11) | 0.01971 (13) | −0.00143 (8) | −0.00504 (9) | −0.00268 (9) |
Cl1 | 0.0153 (3) | 0.0142 (3) | 0.0243 (3) | −0.0022 (2) | −0.0059 (2) | −0.0028 (2) |
Cl3 | 0.0147 (3) | 0.0174 (3) | 0.0243 (3) | −0.0038 (2) | −0.0055 (2) | −0.0042 (2) |
Cl4 | 0.0184 (3) | 0.0188 (3) | 0.0200 (3) | −0.0031 (2) | −0.0059 (2) | −0.0029 (2) |
Cl2 | 0.0139 (3) | 0.0178 (3) | 0.0222 (3) | −0.0012 (2) | −0.0031 (2) | −0.0046 (2) |
P1 | 0.0180 (3) | 0.0189 (3) | 0.0182 (4) | −0.0021 (2) | −0.0067 (3) | −0.0043 (3) |
C24 | 0.0250 (14) | 0.0204 (13) | 0.0255 (15) | −0.0022 (10) | −0.0078 (11) | −0.0030 (11) |
C20 | 0.0235 (13) | 0.0216 (13) | 0.0221 (14) | −0.0025 (10) | −0.0083 (11) | −0.0042 (11) |
C13 | 0.0215 (13) | 0.0261 (13) | 0.0193 (14) | −0.0061 (11) | −0.0075 (11) | −0.0028 (11) |
C21 | 0.0267 (14) | 0.0214 (13) | 0.0285 (16) | −0.0008 (11) | −0.0103 (12) | −0.0047 (12) |
C19 | 0.0202 (12) | 0.0197 (12) | 0.0187 (14) | −0.0011 (10) | −0.0084 (10) | −0.0052 (10) |
C6 | 0.0252 (14) | 0.0284 (14) | 0.0222 (15) | 0.0006 (11) | −0.0084 (12) | −0.0056 (12) |
C8 | 0.0231 (13) | 0.0203 (12) | 0.0238 (15) | −0.0031 (10) | −0.0083 (11) | −0.0054 (11) |
C7 | 0.0189 (12) | 0.0188 (12) | 0.0197 (14) | −0.0021 (10) | −0.0052 (10) | −0.0028 (10) |
C4 | 0.0431 (18) | 0.0203 (13) | 0.0328 (18) | −0.0057 (12) | 0.0001 (14) | −0.0082 (12) |
C12 | 0.0271 (14) | 0.0260 (14) | 0.0240 (15) | −0.0081 (11) | −0.0056 (12) | −0.0091 (12) |
C1 | 0.0204 (12) | 0.0190 (12) | 0.0180 (13) | −0.0018 (10) | −0.0047 (10) | −0.0034 (10) |
C11 | 0.0238 (14) | 0.0260 (14) | 0.0295 (16) | −0.0088 (11) | −0.0048 (12) | −0.0036 (12) |
C3 | 0.0301 (15) | 0.0295 (15) | 0.0284 (16) | −0.0090 (12) | −0.0036 (12) | −0.0101 (13) |
C14 | 0.0244 (14) | 0.0347 (15) | 0.0227 (15) | −0.0085 (12) | −0.0060 (12) | −0.0054 (12) |
C16 | 0.0405 (19) | 0.075 (3) | 0.0275 (18) | −0.0242 (18) | −0.0144 (15) | −0.0089 (18) |
C9 | 0.0291 (14) | 0.0241 (13) | 0.0187 (14) | −0.0005 (11) | −0.0060 (11) | −0.0067 (11) |
C10 | 0.0225 (13) | 0.0261 (14) | 0.0227 (15) | −0.0022 (11) | −0.0049 (11) | −0.0018 (11) |
C5 | 0.0392 (17) | 0.0207 (13) | 0.0274 (17) | 0.0048 (12) | −0.0085 (14) | −0.0028 (12) |
C2 | 0.0233 (13) | 0.0254 (13) | 0.0233 (15) | −0.0047 (11) | −0.0077 (11) | −0.0039 (11) |
C17 | 0.0262 (17) | 0.098 (3) | 0.035 (2) | −0.0202 (19) | −0.0113 (15) | −0.014 (2) |
C15 | 0.0376 (17) | 0.054 (2) | 0.0184 (16) | −0.0137 (15) | −0.0067 (13) | −0.0076 (14) |
C22 | 0.0230 (14) | 0.0298 (15) | 0.0280 (16) | 0.0007 (11) | −0.0097 (12) | −0.0093 (12) |
C23 | 0.0212 (13) | 0.0292 (14) | 0.0305 (17) | −0.0062 (11) | −0.0029 (12) | −0.0038 (12) |
S1 | 0.0182 (3) | 0.0194 (3) | 0.0204 (3) | −0.0056 (2) | −0.0077 (2) | −0.0024 (2) |
S3 | 0.0202 (3) | 0.0165 (3) | 0.0232 (4) | −0.0024 (2) | −0.0059 (3) | 0.0001 (3) |
S2 | 0.0251 (3) | 0.0261 (3) | 0.0322 (4) | 0.0002 (3) | −0.0123 (3) | −0.0129 (3) |
O1 | 0.0177 (9) | 0.0195 (9) | 0.0307 (11) | 0.0003 (7) | −0.0138 (8) | −0.0068 (8) |
O7 | 0.0241 (10) | 0.0206 (9) | 0.0315 (11) | −0.0038 (7) | −0.0056 (8) | −0.0112 (8) |
O4 | 0.0178 (9) | 0.0180 (9) | 0.0214 (10) | −0.0025 (7) | −0.0042 (7) | 0.0033 (7) |
O6 | 0.0238 (10) | 0.0228 (10) | 0.0442 (14) | −0.0018 (8) | −0.0170 (9) | 0.0029 (9) |
O5 | 0.0352 (11) | 0.0238 (10) | 0.0257 (11) | −0.0069 (9) | −0.0002 (9) | −0.0011 (8) |
F1 | 0.0316 (9) | 0.0343 (9) | 0.0251 (9) | −0.0078 (8) | −0.0080 (7) | 0.0071 (7) |
F2 | 0.0260 (9) | 0.0523 (11) | 0.0411 (11) | −0.0200 (8) | −0.0138 (8) | −0.0003 (9) |
O2 | 0.0281 (11) | 0.0316 (11) | 0.0332 (12) | −0.0074 (9) | −0.0063 (9) | −0.0148 (9) |
F3 | 0.0296 (9) | 0.0381 (10) | 0.0415 (12) | 0.0017 (8) | 0.0010 (8) | −0.0131 (9) |
F4 | 0.0511 (12) | 0.0423 (11) | 0.0577 (14) | −0.0222 (10) | 0.0151 (11) | −0.0302 (10) |
F6 | 0.0351 (10) | 0.0381 (10) | 0.0509 (13) | −0.0121 (8) | −0.0180 (9) | −0.0058 (9) |
O3 | 0.0285 (10) | 0.0245 (10) | 0.0291 (12) | −0.0083 (8) | −0.0152 (9) | 0.0046 (8) |
F5 | 0.0463 (11) | 0.0197 (8) | 0.0597 (14) | −0.0101 (8) | −0.0148 (10) | 0.0032 (8) |
F8 | 0.0689 (14) | 0.0458 (12) | 0.0581 (14) | −0.0372 (11) | −0.0111 (12) | −0.0159 (11) |
C25 | 0.0211 (13) | 0.0242 (13) | 0.0251 (15) | −0.0046 (10) | −0.0079 (11) | 0.0016 (11) |
C26 | 0.0269 (15) | 0.0226 (14) | 0.0379 (18) | −0.0087 (11) | −0.0027 (13) | −0.0052 (13) |
O9 | 0.0737 (18) | 0.0538 (15) | 0.0296 (13) | −0.0267 (14) | −0.0080 (13) | −0.0158 (12) |
F7 | 0.0549 (15) | 0.0274 (11) | 0.174 (3) | 0.0060 (10) | −0.0611 (18) | −0.0168 (15) |
O8 | 0.0241 (12) | 0.0697 (18) | 0.092 (2) | 0.0110 (11) | −0.0261 (13) | −0.0564 (18) |
F9 | 0.169 (3) | 0.0722 (17) | 0.0354 (14) | −0.080 (2) | −0.0311 (16) | 0.0088 (12) |
C27 | 0.054 (2) | 0.0346 (18) | 0.049 (2) | −0.0241 (16) | −0.0178 (18) | −0.0051 (16) |
C18 | 0.0225 (15) | 0.067 (2) | 0.0242 (17) | −0.0080 (14) | −0.0066 (13) | −0.0130 (16) |
Mo1—O7 | 2.1259 (19) | C4—C5 | 1.386 (5) |
Mo1—Cl3 | 2.4499 (6) | C4—C3 | 1.387 (5) |
Mo1—Cl4 | 2.4636 (7) | C4—H4 | 0.9500 |
Mo1—Cl1 | 2.4707 (6) | C12—C11 | 1.389 (4) |
Mo1—Cl2 | 2.4776 (6) | C12—H12 | 0.9500 |
Mo1—Mo3i | 2.5911 (3) | C1—C2 | 1.401 (4) |
Mo1—Mo3 | 2.5931 (3) | C11—C10 | 1.387 (4) |
Mo1—Mo2i | 2.5952 (3) | C11—H11 | 0.9500 |
Mo1—Mo2 | 2.6031 (3) | C3—C2 | 1.379 (4) |
Mo2—O4 | 2.1260 (17) | C3—H3 | 0.9500 |
Mo2—Cl3i | 2.4609 (7) | C14—C15 | 1.376 (4) |
Mo2—Cl4 | 2.4686 (7) | C14—H14 | 0.9500 |
Mo2—Cl1i | 2.4702 (6) | C16—C17 | 1.375 (5) |
Mo2—Cl2 | 2.4744 (6) | C16—C15 | 1.384 (5) |
Mo2—Mo3 | 2.5856 (3) | C16—H16 | 0.9500 |
Mo2—Mo3i | 2.5946 (3) | C9—C10 | 1.381 (4) |
Mo2—Mo1i | 2.5951 (3) | C9—H9 | 0.9500 |
Mo3—O1 | 2.1229 (18) | C10—H10 | 0.9500 |
Mo3—Cl3 | 2.4581 (6) | C5—H5 | 0.9500 |
Mo3—Cl4 | 2.4661 (7) | C2—H2 | 0.9500 |
Mo3—Cl1i | 2.4671 (6) | C17—C18 | 1.382 (5) |
Mo3—Cl2i | 2.4756 (7) | C17—H17 | 0.9500 |
Mo3—Mo1i | 2.5911 (3) | C15—H15 | 0.9500 |
Mo3—Mo2i | 2.5947 (3) | C22—C23 | 1.386 (4) |
Cl1—Mo3i | 2.4671 (6) | C22—H22 | 0.9500 |
Cl1—Mo2i | 2.4702 (6) | C23—H23 | 0.9500 |
Cl3—Mo2i | 2.4608 (7) | S1—O2 | 1.421 (2) |
Cl2—Mo3i | 2.4755 (7) | S1—O3 | 1.430 (2) |
P1—C13 | 1.793 (3) | S1—O1 | 1.489 (2) |
P1—C1 | 1.795 (3) | S1—C25 | 1.823 (3) |
P1—C19 | 1.798 (3) | S3—O5 | 1.421 (2) |
P1—C7 | 1.797 (3) | S3—O6 | 1.432 (2) |
C24—C23 | 1.388 (4) | S3—O4 | 1.4877 (19) |
C24—C19 | 1.397 (4) | S3—C26 | 1.832 (3) |
C24—H24 | 0.9500 | S2—O8 | 1.411 (2) |
C20—C21 | 1.387 (4) | S2—O9 | 1.425 (2) |
C20—C19 | 1.388 (4) | S2—O7 | 1.490 (2) |
C20—H20 | 0.9500 | S2—C27 | 1.820 (4) |
C13—C14 | 1.388 (4) | F1—C25 | 1.327 (3) |
C13—C18 | 1.396 (4) | F2—C25 | 1.322 (3) |
C21—C22 | 1.396 (4) | F3—C25 | 1.327 (3) |
C21—H21 | 0.9500 | F4—C26 | 1.320 (4) |
C6—C5 | 1.391 (4) | F6—C26 | 1.329 (4) |
C6—C1 | 1.395 (4) | F5—C26 | 1.333 (4) |
C6—H6 | 0.9500 | F8—C27 | 1.329 (4) |
C8—C9 | 1.387 (4) | F7—C27 | 1.314 (5) |
C8—C7 | 1.391 (4) | F9—C27 | 1.318 (5) |
C8—H8 | 0.9500 | C18—H18 | 0.9500 |
C7—C12 | 1.396 (4) | ||
O7—Mo1—Cl3 | 94.61 (5) | Mo3i—Cl2—Mo1 | 63.084 (16) |
O7—Mo1—Cl4 | 93.27 (6) | C13—P1—C1 | 109.85 (13) |
Cl3—Mo1—Cl4 | 89.77 (2) | C13—P1—C19 | 110.30 (13) |
O7—Mo1—Cl1 | 90.96 (6) | C1—P1—C19 | 107.99 (12) |
Cl3—Mo1—Cl1 | 90.21 (2) | C13—P1—C7 | 107.40 (13) |
Cl4—Mo1—Cl1 | 175.75 (2) | C1—P1—C7 | 111.23 (12) |
O7—Mo1—Cl2 | 89.89 (5) | C19—P1—C7 | 110.09 (13) |
Cl3—Mo1—Cl2 | 175.50 (2) | C23—C24—C19 | 119.6 (3) |
Cl4—Mo1—Cl2 | 89.75 (2) | C23—C24—H24 | 120.2 |
Cl1—Mo1—Cl2 | 89.93 (2) | C19—C24—H24 | 120.2 |
O7—Mo1—Mo3i | 132.73 (6) | C21—C20—C19 | 119.5 (3) |
Cl3—Mo1—Mo3i | 118.085 (18) | C21—C20—H20 | 120.2 |
Cl4—Mo1—Mo3i | 118.158 (17) | C19—C20—H20 | 120.2 |
Cl1—Mo1—Mo3i | 58.282 (15) | C14—C13—C18 | 120.4 (3) |
Cl2—Mo1—Mo3i | 58.419 (17) | C14—C13—P1 | 120.1 (2) |
O7—Mo1—Mo3 | 137.66 (6) | C18—C13—P1 | 119.4 (2) |
Cl3—Mo1—Mo3 | 58.260 (15) | C20—C21—C22 | 120.1 (3) |
Cl4—Mo1—Mo3 | 58.310 (16) | C20—C21—H21 | 120.0 |
Cl1—Mo1—Mo3 | 118.297 (17) | C22—C21—H21 | 120.0 |
Cl2—Mo1—Mo3 | 117.891 (16) | C20—C19—C24 | 120.6 (2) |
Mo3i—Mo1—Mo3 | 89.601 (10) | C20—C19—P1 | 120.2 (2) |
O7—Mo1—Mo2i | 135.78 (5) | C24—C19—P1 | 119.1 (2) |
Cl3—Mo1—Mo2i | 58.302 (17) | C5—C6—C1 | 119.3 (3) |
Cl4—Mo1—Mo2i | 118.312 (17) | C5—C6—H6 | 120.3 |
Cl1—Mo1—Mo2i | 58.307 (16) | C1—C6—H6 | 120.3 |
Cl2—Mo1—Mo2i | 118.212 (18) | C9—C8—C7 | 120.1 (2) |
Mo3i—Mo1—Mo2i | 59.809 (9) | C9—C8—H8 | 120.0 |
Mo3—Mo1—Mo2i | 60.013 (9) | C7—C8—H8 | 120.0 |
O7—Mo1—Mo2 | 134.20 (5) | C8—C7—C12 | 119.5 (2) |
Cl3—Mo1—Mo2 | 117.928 (16) | C8—C7—P1 | 121.4 (2) |
Cl4—Mo1—Mo2 | 58.238 (16) | C12—C7—P1 | 119.1 (2) |
Cl1—Mo1—Mo2 | 118.207 (17) | C5—C4—C3 | 120.7 (3) |
Cl2—Mo1—Mo2 | 58.227 (15) | C5—C4—H4 | 119.6 |
Mo3i—Mo1—Mo2 | 59.937 (9) | C3—C4—H4 | 119.6 |
Mo3—Mo1—Mo2 | 59.680 (8) | C11—C12—C7 | 120.2 (3) |
Mo2i—Mo1—Mo2 | 89.913 (10) | C11—C12—H12 | 119.9 |
O4—Mo2—Cl3i | 89.45 (6) | C7—C12—H12 | 119.9 |
O4—Mo2—Cl4 | 95.32 (6) | C6—C1—C2 | 120.0 (2) |
Cl3i—Mo2—Cl4 | 175.21 (2) | C6—C1—P1 | 120.5 (2) |
O4—Mo2—Cl1i | 93.05 (5) | C2—C1—P1 | 119.5 (2) |
Cl3i—Mo2—Cl1i | 89.96 (2) | C10—C11—C12 | 119.7 (3) |
Cl4—Mo2—Cl1i | 90.12 (2) | C10—C11—H11 | 120.1 |
O4—Mo2—Cl2 | 91.02 (5) | C12—C11—H11 | 120.1 |
Cl3i—Mo2—Cl2 | 89.87 (2) | C2—C3—C4 | 119.6 (3) |
Cl4—Mo2—Cl2 | 89.71 (2) | C2—C3—H3 | 120.2 |
Cl1i—Mo2—Cl2 | 175.92 (2) | C4—C3—H3 | 120.2 |
O4—Mo2—Mo3 | 137.95 (5) | C15—C14—C13 | 119.2 (3) |
Cl3i—Mo2—Mo3 | 117.886 (17) | C15—C14—H14 | 120.4 |
Cl4—Mo2—Mo3 | 58.355 (16) | C13—C14—H14 | 120.4 |
Cl1i—Mo2—Mo3 | 58.362 (14) | C17—C16—C15 | 119.9 (3) |
Cl2—Mo2—Mo3 | 118.299 (16) | C17—C16—H16 | 120.0 |
O4—Mo2—Mo3i | 132.32 (5) | C15—C16—H16 | 120.0 |
Cl3i—Mo2—Mo3i | 58.114 (15) | C10—C9—C8 | 120.2 (3) |
Cl4—Mo2—Mo3i | 117.837 (16) | C10—C9—H9 | 119.9 |
Cl1i—Mo2—Mo3i | 118.258 (18) | C8—C9—H9 | 119.9 |
Cl2—Mo2—Mo3i | 58.408 (16) | C9—C10—C11 | 120.3 (3) |
Mo3—Mo2—Mo3i | 89.690 (9) | C9—C10—H10 | 119.8 |
O4—Mo2—Mo1i | 133.38 (5) | C11—C10—H10 | 119.8 |
Cl3i—Mo2—Mo1i | 57.892 (15) | C4—C5—C6 | 120.1 (3) |
Cl4—Mo2—Mo1i | 118.356 (16) | C4—C5—H5 | 119.9 |
Cl1i—Mo2—Mo1i | 58.325 (16) | C6—C5—H5 | 119.9 |
Cl2—Mo2—Mo1i | 118.357 (17) | C3—C2—C1 | 120.2 (3) |
Mo3—Mo2—Mo1i | 60.019 (9) | C3—C2—H2 | 119.9 |
Mo3i—Mo2—Mo1i | 59.956 (9) | C1—C2—H2 | 119.9 |
O4—Mo2—Mo1 | 136.39 (5) | C16—C17—C18 | 120.5 (3) |
Cl3i—Mo2—Mo1 | 117.899 (16) | C16—C17—H17 | 119.8 |
Cl4—Mo2—Mo1 | 58.051 (15) | C18—C17—H17 | 119.8 |
Cl1i—Mo2—Mo1 | 118.318 (16) | C14—C15—C16 | 120.7 (3) |
Cl2—Mo2—Mo1 | 58.347 (15) | C14—C15—H15 | 119.6 |
Mo3—Mo2—Mo1 | 59.968 (8) | C16—C15—H15 | 119.6 |
Mo3i—Mo2—Mo1 | 59.802 (9) | C23—C22—C21 | 120.2 (3) |
Mo1i—Mo2—Mo1 | 90.089 (10) | C23—C22—H22 | 119.9 |
O1—Mo3—Cl3 | 96.37 (5) | C21—C22—H22 | 119.9 |
O1—Mo3—Cl4 | 93.96 (6) | C22—C23—C24 | 120.0 (3) |
Cl3—Mo3—Cl4 | 89.52 (2) | C22—C23—H23 | 120.0 |
O1—Mo3—Cl1i | 87.53 (5) | C24—C23—H23 | 120.0 |
Cl3—Mo3—Cl1i | 176.10 (2) | O2—S1—O3 | 119.58 (14) |
Cl4—Mo3—Cl1i | 90.25 (2) | O2—S1—O1 | 112.77 (12) |
O1—Mo3—Cl2i | 89.93 (6) | O3—S1—O1 | 111.23 (11) |
Cl3—Mo3—Cl2i | 89.90 (2) | O2—S1—C25 | 105.45 (13) |
Cl4—Mo3—Cl2i | 176.11 (2) | O3—S1—C25 | 104.80 (12) |
Cl1i—Mo3—Cl2i | 90.06 (2) | O1—S1—C25 | 100.65 (13) |
O1—Mo3—Mo2 | 133.05 (5) | O5—S3—O6 | 118.86 (14) |
Cl3—Mo3—Mo2 | 118.291 (16) | O5—S3—O4 | 112.05 (12) |
Cl4—Mo3—Mo2 | 58.449 (16) | O6—S3—O4 | 112.74 (12) |
Cl1i—Mo3—Mo2 | 58.479 (15) | O5—S3—C26 | 104.56 (13) |
Cl2i—Mo3—Mo2 | 118.654 (17) | O6—S3—C26 | 105.06 (13) |
O1—Mo3—Mo1i | 130.42 (5) | O4—S3—C26 | 101.32 (13) |
Cl3—Mo3—Mo1i | 118.460 (18) | O8—S2—O9 | 118.57 (18) |
Cl4—Mo3—Mo1i | 118.604 (17) | O8—S2—O7 | 113.23 (13) |
Cl1i—Mo3—Mo1i | 58.416 (16) | O9—S2—O7 | 111.72 (14) |
Cl2i—Mo3—Mo1i | 58.496 (16) | O8—S2—C27 | 105.44 (19) |
Mo2—Mo3—Mo1i | 60.174 (9) | O9—S2—C27 | 104.84 (17) |
O1—Mo3—Mo1 | 139.14 (5) | O7—S2—C27 | 100.79 (14) |
Cl3—Mo3—Mo1 | 57.951 (15) | S1—O1—Mo3 | 134.15 (11) |
Cl4—Mo3—Mo1 | 58.216 (16) | S2—O7—Mo1 | 139.81 (12) |
Cl1i—Mo3—Mo1 | 118.819 (16) | S3—O4—Mo2 | 134.63 (11) |
Cl2i—Mo3—Mo1 | 118.390 (17) | F2—C25—F1 | 108.7 (2) |
Mo2—Mo3—Mo1 | 60.352 (8) | F2—C25—F3 | 108.7 (2) |
Mo1i—Mo3—Mo1 | 90.399 (10) | F1—C25—F3 | 107.5 (2) |
O1—Mo3—Mo2i | 136.31 (5) | F2—C25—S1 | 110.0 (2) |
Cl3—Mo3—Mo2i | 58.214 (17) | F1—C25—S1 | 110.76 (18) |
Cl4—Mo3—Mo2i | 118.237 (16) | F3—C25—S1 | 111.14 (19) |
Cl1i—Mo3—Mo2i | 118.667 (18) | F4—C26—F6 | 108.4 (3) |
Cl2i—Mo3—Mo2i | 58.366 (15) | F4—C26—F5 | 108.7 (2) |
Mo2—Mo3—Mo2i | 90.312 (10) | F6—C26—F5 | 107.5 (2) |
Mo1i—Mo3—Mo2i | 60.263 (9) | F4—C26—S3 | 111.38 (19) |
Mo1—Mo3—Mo2i | 60.032 (9) | F6—C26—S3 | 111.2 (2) |
Mo3i—Cl1—Mo2i | 63.160 (15) | F5—C26—S3 | 109.5 (2) |
Mo3i—Cl1—Mo1 | 63.302 (15) | F7—C27—F9 | 110.0 (4) |
Mo2i—Cl1—Mo1 | 63.369 (16) | F7—C27—F8 | 107.5 (3) |
Mo1—Cl3—Mo3 | 63.788 (15) | F9—C27—F8 | 108.1 (3) |
Mo1—Cl3—Mo2i | 63.804 (16) | F7—C27—S2 | 110.6 (3) |
Mo3—Cl3—Mo2i | 63.672 (16) | F9—C27—S2 | 110.3 (3) |
Mo1—Cl4—Mo3 | 63.474 (17) | F8—C27—S2 | 110.3 (3) |
Mo1—Cl4—Mo2 | 63.711 (17) | C17—C18—C13 | 119.2 (3) |
Mo3—Cl4—Mo2 | 63.196 (17) | C17—C18—H18 | 120.4 |
Mo2—Cl2—Mo3i | 63.226 (16) | C13—C18—H18 | 120.4 |
Mo2—Cl2—Mo1 | 63.427 (15) |
Symmetry code: (i) −x+2, −y, −z+1. |