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The crystal structure of the title compound, (C24H20P)2[Mo6Cl8(CF3O3S)6]·C4H10O·CH2Cl2, consists of a centrosymmetric [Mo6Cl8]4+ cluster core that is bonded to six trifluoro­methane­sulfonate groups via O atoms and two tetra­phenyl­phospho­nium counter-cations. The packing of the cations and anions leads to voids with a size of ca 230 Å3 that are filled with disordered dichloro­methane and diethyl ether solvent mol­ecules. The title compound affords facile ligand substitution on the hexa­nuclear [Mo6Cl8]4+ cluster.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040517/wm2040sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040517/wm2040Isup2.hkl
Contains datablock I

CCDC reference: 628424

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • Some non-H atoms missing
  • R factor = 0.032
  • wR factor = 0.097
  • Data-to-parameter ratio = 18.7

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 227.00 A   3
Author Response: In an attempt to achieve a higher quality structure solution, SQUEEZE in PLATON was used to remove the highly disordered solvent molecules. This resulted in the void described above.

Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.530 0.750 Tmin(prime) and Tmax expected: 0.687 0.754 RR(prime) = 0.776 Please check that your absorption correction is appropriate. CHEMW01_ALERT_1_C The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.99 <> 1.01 Calculated formula weight = 2520.5911 Formula weight given = 2432.3999 CHEMW01_ALERT_1_C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76 PLAT220_ALERT_2_C Large Non-Solvent F Ueq(max)/Ueq(min) ... 2.57 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.68 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.65 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - Cl1 .. 5.04 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - Cl4 .. 5.68 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - Cl3_a .. 5.24 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C27 PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. F2 .. 3.02 Ang.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C59 H52 Cl8 F18 Mo6 O19 P2 Atom count from _chemical_formula_moiety:C59 H52 Cl10 F18 Mo6 O19 P2 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C59 H52 Cl8 F18 Mo6 O19 P2 S6 Atom count from the _atom_site data: C54 H40 Cl8 F18 Mo6 O18 P2 S6 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_sum C59 H52 Cl8 F18 Mo6 O19 P2 S6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 59.00 54.00 5.00 H 52.00 40.00 12.00 Cl 8.00 8.00 0.00 F 18.00 18.00 0.00 Mo 6.00 6.00 0.00 O 19.00 18.00 1.00 P 2.00 2.00 0.00 S 6.00 6.00 0.00
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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

Computing details top

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.

Bis(tetraphenylphosphonium) [octa(µ3-chloro)hexakis (trifluoromethanesulfonato)-octahedro-hexamolybdate] dichloromethane/diethylether solvate top
Crystal data top
(C24H20P)2[Mo6Cl8(CF3O3S)6]·C4H10O·CH2Cl2Z = 1
Mr = 2432.40F(000) = 1184
Triclinic, P1Dx = 1.927 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.8710 (4) ÅCell parameters from 5957 reflections
b = 13.8264 (5) Åθ = 3.1–36.9°
c = 14.0267 (5) ŵ = 1.41 mm1
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
Data collection top
Bruker APEX2 CCD
diffractometer
9451 independent reflections
Radiation source: fine-focus sealed tube7868 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
φ and ω scansθmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS in SAINT-Plus; Bruker, 2003)
h = 1515
Tmin = 0.53, Tmax = 0.75k = 1717
24669 measured reflectionsl = 1816
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.097H-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 parametersΔρmax = 1.40 e Å3
0 restraintsΔρmin = 1.25 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo11.008560 (18)0.087774 (16)0.418910 (17)0.01547 (7)
Mo21.094110 (18)0.073010 (16)0.397219 (17)0.01534 (7)
Mo30.867195 (18)0.083276 (16)0.455328 (17)0.01520 (7)
Cl11.04601 (5)0.23196 (4)0.56319 (5)0.01801 (13)
Cl30.79305 (5)0.07246 (5)0.47757 (5)0.01844 (13)
Cl40.97092 (5)0.06468 (5)0.28296 (5)0.01911 (13)
Cl21.22541 (5)0.09320 (5)0.36740 (5)0.01843 (13)
P10.50929 (6)0.67065 (5)0.20173 (5)0.01805 (14)
C240.7475 (2)0.6585 (2)0.1147 (2)0.0240 (6)
H240.72410.72960.08660.029*
C200.6968 (2)0.5008 (2)0.2197 (2)0.0223 (6)
H200.63900.46450.26260.027*
C130.4358 (2)0.6626 (2)0.1079 (2)0.0219 (6)
C210.8153 (3)0.4501 (2)0.1978 (2)0.0256 (6)
H210.83900.37910.22640.031*
C190.6634 (2)0.6048 (2)0.1787 (2)0.0191 (5)
C60.4330 (3)0.8816 (2)0.1387 (2)0.0258 (6)
H60.38670.86590.10090.031*
C80.4138 (2)0.6517 (2)0.4072 (2)0.0219 (6)
H80.43910.71270.40220.026*
C70.4336 (2)0.6113 (2)0.3221 (2)0.0195 (5)
C40.4991 (3)1.0056 (2)0.1912 (2)0.0332 (7)
H40.49701.07530.18930.040*
C120.3944 (2)0.5224 (2)0.3300 (2)0.0244 (6)
H120.40700.49480.27200.029*
C10.5042 (2)0.8028 (2)0.1970 (2)0.0196 (5)
C110.3371 (3)0.4743 (2)0.4224 (2)0.0263 (6)
H110.31090.41360.42780.032*
C30.5708 (3)0.9275 (2)0.2485 (2)0.0285 (6)
H30.61760.94350.28560.034*
C140.5022 (3)0.6416 (2)0.0160 (2)0.0267 (6)
H140.58690.62750.00370.032*
C160.3205 (3)0.6607 (3)0.0394 (3)0.0442 (9)
H160.28110.66090.09060.053*
C90.3571 (3)0.6030 (2)0.4994 (2)0.0244 (6)
H90.34490.63010.55770.029*
C100.3183 (2)0.5152 (2)0.5068 (2)0.0249 (6)
H100.27860.48270.57000.030*
C50.4306 (3)0.9832 (2)0.1366 (2)0.0315 (7)
H50.38181.03750.09770.038*
C20.5736 (2)0.8264 (2)0.2513 (2)0.0238 (6)
H20.62280.77260.29020.029*
C170.2551 (3)0.6796 (4)0.0523 (3)0.0507 (10)
H170.17060.69080.06490.061*
C150.4438 (3)0.6414 (3)0.0571 (2)0.0358 (7)
H150.48870.62790.12040.043*
C220.8997 (3)0.5033 (2)0.1335 (2)0.0267 (6)
H220.98060.46830.11800.032*
C230.8658 (3)0.6071 (2)0.0923 (2)0.0277 (6)
H230.92350.64310.04880.033*
S10.63441 (6)0.19045 (5)0.34168 (5)0.01865 (14)
S31.19429 (6)0.24088 (5)0.19454 (5)0.02082 (15)
S20.95144 (6)0.24132 (5)0.29128 (6)0.02637 (16)
O10.71551 (16)0.18964 (14)0.40749 (15)0.0215 (4)
O71.02673 (17)0.19195 (14)0.32565 (16)0.0245 (4)
O41.21051 (16)0.15499 (13)0.28338 (14)0.0208 (4)
O61.07361 (18)0.27269 (15)0.17971 (18)0.0309 (5)
O51.28803 (19)0.22638 (15)0.11008 (16)0.0300 (5)
F10.53633 (15)0.08116 (13)0.50813 (13)0.0324 (4)
F20.42934 (15)0.13940 (15)0.39353 (15)0.0380 (5)
O20.67538 (18)0.10750 (16)0.29069 (17)0.0292 (5)
F30.44794 (16)0.23997 (14)0.47964 (15)0.0388 (5)
F41.14049 (19)0.36600 (15)0.31855 (17)0.0489 (6)
F61.32786 (17)0.32458 (14)0.25758 (16)0.0394 (5)
O30.59391 (18)0.29215 (15)0.28697 (16)0.0271 (4)
F51.21048 (18)0.43092 (13)0.16414 (17)0.0428 (5)
F80.9270 (2)0.43049 (16)0.34287 (18)0.0519 (6)
C250.5043 (2)0.1611 (2)0.4361 (2)0.0242 (6)
C261.2193 (3)0.3463 (2)0.2370 (3)0.0294 (7)
O90.9963 (3)0.2521 (2)0.18949 (19)0.0488 (7)
F71.0979 (2)0.41236 (16)0.3480 (3)0.0821 (10)
O80.8279 (2)0.2034 (2)0.3216 (3)0.0555 (8)
F90.9458 (3)0.3709 (2)0.46296 (19)0.0833 (10)
C270.9831 (3)0.3714 (3)0.3662 (3)0.0421 (9)
C180.3114 (3)0.6823 (3)0.1263 (3)0.0370 (8)
H180.26600.69730.18900.044*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01319 (11)0.01394 (11)0.01941 (13)0.00191 (8)0.00443 (9)0.00363 (9)
Mo20.01223 (11)0.01409 (11)0.01891 (13)0.00211 (8)0.00366 (9)0.00232 (9)
Mo30.01187 (11)0.01377 (11)0.01971 (13)0.00143 (8)0.00504 (9)0.00268 (9)
Cl10.0153 (3)0.0142 (3)0.0243 (3)0.0022 (2)0.0059 (2)0.0028 (2)
Cl30.0147 (3)0.0174 (3)0.0243 (3)0.0038 (2)0.0055 (2)0.0042 (2)
Cl40.0184 (3)0.0188 (3)0.0200 (3)0.0031 (2)0.0059 (2)0.0029 (2)
Cl20.0139 (3)0.0178 (3)0.0222 (3)0.0012 (2)0.0031 (2)0.0046 (2)
P10.0180 (3)0.0189 (3)0.0182 (4)0.0021 (2)0.0067 (3)0.0043 (3)
C240.0250 (14)0.0204 (13)0.0255 (15)0.0022 (10)0.0078 (11)0.0030 (11)
C200.0235 (13)0.0216 (13)0.0221 (14)0.0025 (10)0.0083 (11)0.0042 (11)
C130.0215 (13)0.0261 (13)0.0193 (14)0.0061 (11)0.0075 (11)0.0028 (11)
C210.0267 (14)0.0214 (13)0.0285 (16)0.0008 (11)0.0103 (12)0.0047 (12)
C190.0202 (12)0.0197 (12)0.0187 (14)0.0011 (10)0.0084 (10)0.0052 (10)
C60.0252 (14)0.0284 (14)0.0222 (15)0.0006 (11)0.0084 (12)0.0056 (12)
C80.0231 (13)0.0203 (12)0.0238 (15)0.0031 (10)0.0083 (11)0.0054 (11)
C70.0189 (12)0.0188 (12)0.0197 (14)0.0021 (10)0.0052 (10)0.0028 (10)
C40.0431 (18)0.0203 (13)0.0328 (18)0.0057 (12)0.0001 (14)0.0082 (12)
C120.0271 (14)0.0260 (14)0.0240 (15)0.0081 (11)0.0056 (12)0.0091 (12)
C10.0204 (12)0.0190 (12)0.0180 (13)0.0018 (10)0.0047 (10)0.0034 (10)
C110.0238 (14)0.0260 (14)0.0295 (16)0.0088 (11)0.0048 (12)0.0036 (12)
C30.0301 (15)0.0295 (15)0.0284 (16)0.0090 (12)0.0036 (12)0.0101 (13)
C140.0244 (14)0.0347 (15)0.0227 (15)0.0085 (12)0.0060 (12)0.0054 (12)
C160.0405 (19)0.075 (3)0.0275 (18)0.0242 (18)0.0144 (15)0.0089 (18)
C90.0291 (14)0.0241 (13)0.0187 (14)0.0005 (11)0.0060 (11)0.0067 (11)
C100.0225 (13)0.0261 (14)0.0227 (15)0.0022 (11)0.0049 (11)0.0018 (11)
C50.0392 (17)0.0207 (13)0.0274 (17)0.0048 (12)0.0085 (14)0.0028 (12)
C20.0233 (13)0.0254 (13)0.0233 (15)0.0047 (11)0.0077 (11)0.0039 (11)
C170.0262 (17)0.098 (3)0.035 (2)0.0202 (19)0.0113 (15)0.014 (2)
C150.0376 (17)0.054 (2)0.0184 (16)0.0137 (15)0.0067 (13)0.0076 (14)
C220.0230 (14)0.0298 (15)0.0280 (16)0.0007 (11)0.0097 (12)0.0093 (12)
C230.0212 (13)0.0292 (14)0.0305 (17)0.0062 (11)0.0029 (12)0.0038 (12)
S10.0182 (3)0.0194 (3)0.0204 (3)0.0056 (2)0.0077 (2)0.0024 (2)
S30.0202 (3)0.0165 (3)0.0232 (4)0.0024 (2)0.0059 (3)0.0001 (3)
S20.0251 (3)0.0261 (3)0.0322 (4)0.0002 (3)0.0123 (3)0.0129 (3)
O10.0177 (9)0.0195 (9)0.0307 (11)0.0003 (7)0.0138 (8)0.0068 (8)
O70.0241 (10)0.0206 (9)0.0315 (11)0.0038 (7)0.0056 (8)0.0112 (8)
O40.0178 (9)0.0180 (9)0.0214 (10)0.0025 (7)0.0042 (7)0.0033 (7)
O60.0238 (10)0.0228 (10)0.0442 (14)0.0018 (8)0.0170 (9)0.0029 (9)
O50.0352 (11)0.0238 (10)0.0257 (11)0.0069 (9)0.0002 (9)0.0011 (8)
F10.0316 (9)0.0343 (9)0.0251 (9)0.0078 (8)0.0080 (7)0.0071 (7)
F20.0260 (9)0.0523 (11)0.0411 (11)0.0200 (8)0.0138 (8)0.0003 (9)
O20.0281 (11)0.0316 (11)0.0332 (12)0.0074 (9)0.0063 (9)0.0148 (9)
F30.0296 (9)0.0381 (10)0.0415 (12)0.0017 (8)0.0010 (8)0.0131 (9)
F40.0511 (12)0.0423 (11)0.0577 (14)0.0222 (10)0.0151 (11)0.0302 (10)
F60.0351 (10)0.0381 (10)0.0509 (13)0.0121 (8)0.0180 (9)0.0058 (9)
O30.0285 (10)0.0245 (10)0.0291 (12)0.0083 (8)0.0152 (9)0.0046 (8)
F50.0463 (11)0.0197 (8)0.0597 (14)0.0101 (8)0.0148 (10)0.0032 (8)
F80.0689 (14)0.0458 (12)0.0581 (14)0.0372 (11)0.0111 (12)0.0159 (11)
C250.0211 (13)0.0242 (13)0.0251 (15)0.0046 (10)0.0079 (11)0.0016 (11)
C260.0269 (15)0.0226 (14)0.0379 (18)0.0087 (11)0.0027 (13)0.0052 (13)
O90.0737 (18)0.0538 (15)0.0296 (13)0.0267 (14)0.0080 (13)0.0158 (12)
F70.0549 (15)0.0274 (11)0.174 (3)0.0060 (10)0.0611 (18)0.0168 (15)
O80.0241 (12)0.0697 (18)0.092 (2)0.0110 (11)0.0261 (13)0.0564 (18)
F90.169 (3)0.0722 (17)0.0354 (14)0.080 (2)0.0311 (16)0.0088 (12)
C270.054 (2)0.0346 (18)0.049 (2)0.0241 (16)0.0178 (18)0.0051 (16)
C180.0225 (15)0.067 (2)0.0242 (17)0.0080 (14)0.0066 (13)0.0130 (16)
Geometric parameters (Å, º) top
Mo1—O72.1259 (19)C4—C51.386 (5)
Mo1—Cl32.4499 (6)C4—C31.387 (5)
Mo1—Cl42.4636 (7)C4—H40.9500
Mo1—Cl12.4707 (6)C12—C111.389 (4)
Mo1—Cl22.4776 (6)C12—H120.9500
Mo1—Mo3i2.5911 (3)C1—C21.401 (4)
Mo1—Mo32.5931 (3)C11—C101.387 (4)
Mo1—Mo2i2.5952 (3)C11—H110.9500
Mo1—Mo22.6031 (3)C3—C21.379 (4)
Mo2—O42.1260 (17)C3—H30.9500
Mo2—Cl3i2.4609 (7)C14—C151.376 (4)
Mo2—Cl42.4686 (7)C14—H140.9500
Mo2—Cl1i2.4702 (6)C16—C171.375 (5)
Mo2—Cl22.4744 (6)C16—C151.384 (5)
Mo2—Mo32.5856 (3)C16—H160.9500
Mo2—Mo3i2.5946 (3)C9—C101.381 (4)
Mo2—Mo1i2.5951 (3)C9—H90.9500
Mo3—O12.1229 (18)C10—H100.9500
Mo3—Cl32.4581 (6)C5—H50.9500
Mo3—Cl42.4661 (7)C2—H20.9500
Mo3—Cl1i2.4671 (6)C17—C181.382 (5)
Mo3—Cl2i2.4756 (7)C17—H170.9500
Mo3—Mo1i2.5911 (3)C15—H150.9500
Mo3—Mo2i2.5947 (3)C22—C231.386 (4)
Cl1—Mo3i2.4671 (6)C22—H220.9500
Cl1—Mo2i2.4702 (6)C23—H230.9500
Cl3—Mo2i2.4608 (7)S1—O21.421 (2)
Cl2—Mo3i2.4755 (7)S1—O31.430 (2)
P1—C131.793 (3)S1—O11.489 (2)
P1—C11.795 (3)S1—C251.823 (3)
P1—C191.798 (3)S3—O51.421 (2)
P1—C71.797 (3)S3—O61.432 (2)
C24—C231.388 (4)S3—O41.4877 (19)
C24—C191.397 (4)S3—C261.832 (3)
C24—H240.9500S2—O81.411 (2)
C20—C211.387 (4)S2—O91.425 (2)
C20—C191.388 (4)S2—O71.490 (2)
C20—H200.9500S2—C271.820 (4)
C13—C141.388 (4)F1—C251.327 (3)
C13—C181.396 (4)F2—C251.322 (3)
C21—C221.396 (4)F3—C251.327 (3)
C21—H210.9500F4—C261.320 (4)
C6—C51.391 (4)F6—C261.329 (4)
C6—C11.395 (4)F5—C261.333 (4)
C6—H60.9500F8—C271.329 (4)
C8—C91.387 (4)F7—C271.314 (5)
C8—C71.391 (4)F9—C271.318 (5)
C8—H80.9500C18—H180.9500
C7—C121.396 (4)
O7—Mo1—Cl394.61 (5)Mo3i—Cl2—Mo163.084 (16)
O7—Mo1—Cl493.27 (6)C13—P1—C1109.85 (13)
Cl3—Mo1—Cl489.77 (2)C13—P1—C19110.30 (13)
O7—Mo1—Cl190.96 (6)C1—P1—C19107.99 (12)
Cl3—Mo1—Cl190.21 (2)C13—P1—C7107.40 (13)
Cl4—Mo1—Cl1175.75 (2)C1—P1—C7111.23 (12)
O7—Mo1—Cl289.89 (5)C19—P1—C7110.09 (13)
Cl3—Mo1—Cl2175.50 (2)C23—C24—C19119.6 (3)
Cl4—Mo1—Cl289.75 (2)C23—C24—H24120.2
Cl1—Mo1—Cl289.93 (2)C19—C24—H24120.2
O7—Mo1—Mo3i132.73 (6)C21—C20—C19119.5 (3)
Cl3—Mo1—Mo3i118.085 (18)C21—C20—H20120.2
Cl4—Mo1—Mo3i118.158 (17)C19—C20—H20120.2
Cl1—Mo1—Mo3i58.282 (15)C14—C13—C18120.4 (3)
Cl2—Mo1—Mo3i58.419 (17)C14—C13—P1120.1 (2)
O7—Mo1—Mo3137.66 (6)C18—C13—P1119.4 (2)
Cl3—Mo1—Mo358.260 (15)C20—C21—C22120.1 (3)
Cl4—Mo1—Mo358.310 (16)C20—C21—H21120.0
Cl1—Mo1—Mo3118.297 (17)C22—C21—H21120.0
Cl2—Mo1—Mo3117.891 (16)C20—C19—C24120.6 (2)
Mo3i—Mo1—Mo389.601 (10)C20—C19—P1120.2 (2)
O7—Mo1—Mo2i135.78 (5)C24—C19—P1119.1 (2)
Cl3—Mo1—Mo2i58.302 (17)C5—C6—C1119.3 (3)
Cl4—Mo1—Mo2i118.312 (17)C5—C6—H6120.3
Cl1—Mo1—Mo2i58.307 (16)C1—C6—H6120.3
Cl2—Mo1—Mo2i118.212 (18)C9—C8—C7120.1 (2)
Mo3i—Mo1—Mo2i59.809 (9)C9—C8—H8120.0
Mo3—Mo1—Mo2i60.013 (9)C7—C8—H8120.0
O7—Mo1—Mo2134.20 (5)C8—C7—C12119.5 (2)
Cl3—Mo1—Mo2117.928 (16)C8—C7—P1121.4 (2)
Cl4—Mo1—Mo258.238 (16)C12—C7—P1119.1 (2)
Cl1—Mo1—Mo2118.207 (17)C5—C4—C3120.7 (3)
Cl2—Mo1—Mo258.227 (15)C5—C4—H4119.6
Mo3i—Mo1—Mo259.937 (9)C3—C4—H4119.6
Mo3—Mo1—Mo259.680 (8)C11—C12—C7120.2 (3)
Mo2i—Mo1—Mo289.913 (10)C11—C12—H12119.9
O4—Mo2—Cl3i89.45 (6)C7—C12—H12119.9
O4—Mo2—Cl495.32 (6)C6—C1—C2120.0 (2)
Cl3i—Mo2—Cl4175.21 (2)C6—C1—P1120.5 (2)
O4—Mo2—Cl1i93.05 (5)C2—C1—P1119.5 (2)
Cl3i—Mo2—Cl1i89.96 (2)C10—C11—C12119.7 (3)
Cl4—Mo2—Cl1i90.12 (2)C10—C11—H11120.1
O4—Mo2—Cl291.02 (5)C12—C11—H11120.1
Cl3i—Mo2—Cl289.87 (2)C2—C3—C4119.6 (3)
Cl4—Mo2—Cl289.71 (2)C2—C3—H3120.2
Cl1i—Mo2—Cl2175.92 (2)C4—C3—H3120.2
O4—Mo2—Mo3137.95 (5)C15—C14—C13119.2 (3)
Cl3i—Mo2—Mo3117.886 (17)C15—C14—H14120.4
Cl4—Mo2—Mo358.355 (16)C13—C14—H14120.4
Cl1i—Mo2—Mo358.362 (14)C17—C16—C15119.9 (3)
Cl2—Mo2—Mo3118.299 (16)C17—C16—H16120.0
O4—Mo2—Mo3i132.32 (5)C15—C16—H16120.0
Cl3i—Mo2—Mo3i58.114 (15)C10—C9—C8120.2 (3)
Cl4—Mo2—Mo3i117.837 (16)C10—C9—H9119.9
Cl1i—Mo2—Mo3i118.258 (18)C8—C9—H9119.9
Cl2—Mo2—Mo3i58.408 (16)C9—C10—C11120.3 (3)
Mo3—Mo2—Mo3i89.690 (9)C9—C10—H10119.8
O4—Mo2—Mo1i133.38 (5)C11—C10—H10119.8
Cl3i—Mo2—Mo1i57.892 (15)C4—C5—C6120.1 (3)
Cl4—Mo2—Mo1i118.356 (16)C4—C5—H5119.9
Cl1i—Mo2—Mo1i58.325 (16)C6—C5—H5119.9
Cl2—Mo2—Mo1i118.357 (17)C3—C2—C1120.2 (3)
Mo3—Mo2—Mo1i60.019 (9)C3—C2—H2119.9
Mo3i—Mo2—Mo1i59.956 (9)C1—C2—H2119.9
O4—Mo2—Mo1136.39 (5)C16—C17—C18120.5 (3)
Cl3i—Mo2—Mo1117.899 (16)C16—C17—H17119.8
Cl4—Mo2—Mo158.051 (15)C18—C17—H17119.8
Cl1i—Mo2—Mo1118.318 (16)C14—C15—C16120.7 (3)
Cl2—Mo2—Mo158.347 (15)C14—C15—H15119.6
Mo3—Mo2—Mo159.968 (8)C16—C15—H15119.6
Mo3i—Mo2—Mo159.802 (9)C23—C22—C21120.2 (3)
Mo1i—Mo2—Mo190.089 (10)C23—C22—H22119.9
O1—Mo3—Cl396.37 (5)C21—C22—H22119.9
O1—Mo3—Cl493.96 (6)C22—C23—C24120.0 (3)
Cl3—Mo3—Cl489.52 (2)C22—C23—H23120.0
O1—Mo3—Cl1i87.53 (5)C24—C23—H23120.0
Cl3—Mo3—Cl1i176.10 (2)O2—S1—O3119.58 (14)
Cl4—Mo3—Cl1i90.25 (2)O2—S1—O1112.77 (12)
O1—Mo3—Cl2i89.93 (6)O3—S1—O1111.23 (11)
Cl3—Mo3—Cl2i89.90 (2)O2—S1—C25105.45 (13)
Cl4—Mo3—Cl2i176.11 (2)O3—S1—C25104.80 (12)
Cl1i—Mo3—Cl2i90.06 (2)O1—S1—C25100.65 (13)
O1—Mo3—Mo2133.05 (5)O5—S3—O6118.86 (14)
Cl3—Mo3—Mo2118.291 (16)O5—S3—O4112.05 (12)
Cl4—Mo3—Mo258.449 (16)O6—S3—O4112.74 (12)
Cl1i—Mo3—Mo258.479 (15)O5—S3—C26104.56 (13)
Cl2i—Mo3—Mo2118.654 (17)O6—S3—C26105.06 (13)
O1—Mo3—Mo1i130.42 (5)O4—S3—C26101.32 (13)
Cl3—Mo3—Mo1i118.460 (18)O8—S2—O9118.57 (18)
Cl4—Mo3—Mo1i118.604 (17)O8—S2—O7113.23 (13)
Cl1i—Mo3—Mo1i58.416 (16)O9—S2—O7111.72 (14)
Cl2i—Mo3—Mo1i58.496 (16)O8—S2—C27105.44 (19)
Mo2—Mo3—Mo1i60.174 (9)O9—S2—C27104.84 (17)
O1—Mo3—Mo1139.14 (5)O7—S2—C27100.79 (14)
Cl3—Mo3—Mo157.951 (15)S1—O1—Mo3134.15 (11)
Cl4—Mo3—Mo158.216 (16)S2—O7—Mo1139.81 (12)
Cl1i—Mo3—Mo1118.819 (16)S3—O4—Mo2134.63 (11)
Cl2i—Mo3—Mo1118.390 (17)F2—C25—F1108.7 (2)
Mo2—Mo3—Mo160.352 (8)F2—C25—F3108.7 (2)
Mo1i—Mo3—Mo190.399 (10)F1—C25—F3107.5 (2)
O1—Mo3—Mo2i136.31 (5)F2—C25—S1110.0 (2)
Cl3—Mo3—Mo2i58.214 (17)F1—C25—S1110.76 (18)
Cl4—Mo3—Mo2i118.237 (16)F3—C25—S1111.14 (19)
Cl1i—Mo3—Mo2i118.667 (18)F4—C26—F6108.4 (3)
Cl2i—Mo3—Mo2i58.366 (15)F4—C26—F5108.7 (2)
Mo2—Mo3—Mo2i90.312 (10)F6—C26—F5107.5 (2)
Mo1i—Mo3—Mo2i60.263 (9)F4—C26—S3111.38 (19)
Mo1—Mo3—Mo2i60.032 (9)F6—C26—S3111.2 (2)
Mo3i—Cl1—Mo2i63.160 (15)F5—C26—S3109.5 (2)
Mo3i—Cl1—Mo163.302 (15)F7—C27—F9110.0 (4)
Mo2i—Cl1—Mo163.369 (16)F7—C27—F8107.5 (3)
Mo1—Cl3—Mo363.788 (15)F9—C27—F8108.1 (3)
Mo1—Cl3—Mo2i63.804 (16)F7—C27—S2110.6 (3)
Mo3—Cl3—Mo2i63.672 (16)F9—C27—S2110.3 (3)
Mo1—Cl4—Mo363.474 (17)F8—C27—S2110.3 (3)
Mo1—Cl4—Mo263.711 (17)C17—C18—C13119.2 (3)
Mo3—Cl4—Mo263.196 (17)C17—C18—H18120.4
Mo2—Cl2—Mo3i63.226 (16)C13—C18—H18120.4
Mo2—Cl2—Mo163.427 (15)
Symmetry code: (i) x+2, y, z+1.
 

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