Tetra­kis(2,3,5,6-tetra­fluoro­benzene­thiol­ato-κS)(triphenyl­phosphine-κP)osmium(IV) n-hexane hemisolvate

Cerón, M.; Arroyo, M.; Bernès, S.

doi:10.1107/S1600536806029230

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Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphine-κP)osmium(IV) n-hexane hemisolvate

M. Cerón, M. Arroyo and S. Bernès

The title compound, [Os(C₆HF₄S)₄(PPh₃)]·0.5C₆H₁₄, includes a trigonal–bipyramidal Os^IV complex with a coordination geometry close to that known for the analogous unsolvated complex, and hexane disordered around an inversion centre. Significant libration and rotation are observed for the thiolate ligands in the crystal structure when compared with the unsolvated species.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806029230/kp2044sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806029230/kp2044Isup2.hkl Contains datablock I

CCDC reference: 621397

checkCIF report

Key indicators

Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.015 Å
Disorder in solvent or counterion
R factor = 0.064
wR factor = 0.174
Data-to-parameter ratio = 13.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT223_ALERT_4_B Large Solvent/Anion  H     Ueq(max)/Ueq(min) ...       4.60 Ratio

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.566     0.778
            Tmin and Tmax expected:      0.450     0.780
            RR =      1.261
            Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.28
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1
PLAT220_ALERT_2_C Large Non-Solvent    F     Ueq(max)/Ueq(min) ...       2.86 Ratio
PLAT221_ALERT_4_C Large Solvent/Anion  C     Ueq(max)/Ueq(min) ...       3.66 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C17
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       C101
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       C103
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C102
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C201
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C202
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      40.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         15
PLAT731_ALERT_1_C Bond    Calc     1.53(3), Rep   1.530(10) ......       3.00 su-Ra
              C103 -C103    1.555   2.756
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C42 H19 F16 Os P S4

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  16 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   9 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1998); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: SHELXTL-Plus and Mercury (Version 1.4.1; Macrae et al., 2006); software used to prepare material for publication: SHELXTL-Plus.

Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphine- κP)osmium(IV) n-hexane hemisolvate top

Crystal data top

[Os(C₆HF₄S)₄(C₁₈H₁₅P)]·0.5C₆H₁₄	Z = 2
M_r = 1220.07	F(000) = 1190
Triclinic, P1	D_x = 1.777 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.209 (3) Å	Cell parameters from 60 reflections
b = 13.513 (3) Å	θ = 3.8–12.2°
c = 13.865 (3) Å	µ = 3.11 mm⁻¹
α = 89.20 (2)°	T = 296 K
β = 87.40 (2)°	Plate, dark red
γ = 86.454 (15)°	0.60 × 0.22 × 0.08 mm
V = 2280.5 (9) Å³

Data collection top

Bruker P4 diffractometer	6378 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4	R_int = 0.042
Graphite monochromator	θ_max = 25.0°, θ_min = 2.1°
ω scans	h = −14→1
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −16→16
T_min = 0.566, T_max = 0.778	l = −16→16
8756 measured reflections	3 standard reflections every 97 reflections
8033 independent reflections	intensity decay: 28.1%

Refinement top

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)] = 0.065	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.174	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.1011P)² + 7.7358P] where P = (F_o² + 2F_c²)/3
8033 reflections	(Δ/σ)_max = 0.001
597 parameters	Δρ_max = 2.48 e Å⁻³
336 restraints	Δρ_min = −2.06 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Os1	0.33011 (3)	−0.17279 (3)	0.76817 (3)	0.04135 (15)
S1	0.3421 (2)	−0.35227 (18)	0.77036 (19)	0.0503 (6)
S2	0.3226 (3)	−0.15757 (19)	0.92742 (18)	0.0560 (7)
S3	0.4928 (2)	−0.17719 (18)	0.68960 (19)	0.0512 (6)
S4	0.1886 (2)	−0.14481 (19)	0.6763 (2)	0.0532 (6)
P1	0.3427 (2)	0.00344 (18)	0.76363 (18)	0.0452 (6)
C1	0.4802 (8)	0.0429 (6)	0.7808 (6)	0.055 (3)
C2	0.5484 (8)	−0.0078 (7)	0.8441 (7)	0.066 (3)
H2A	0.5243	−0.0626	0.8784	0.079*
C3	0.6525 (8)	0.0233 (8)	0.8563 (8)	0.074 (3)
H3A	0.6981	−0.0108	0.8991	0.089*
C4	0.6892 (10)	0.1029 (9)	0.8066 (9)	0.089 (4)
H4A	0.7596	0.1229	0.8153	0.106*
C5	0.6226 (10)	0.1534 (10)	0.7442 (10)	0.092 (5)
H5A	0.6480	0.2074	0.7095	0.111*
C6	0.5185 (8)	0.1249 (8)	0.7324 (8)	0.070 (3)
H6A	0.4729	0.1612	0.6912	0.084*
C7	0.3064 (8)	0.0634 (6)	0.6492 (6)	0.056 (3)
C8	0.3407 (8)	0.0198 (7)	0.5624 (7)	0.066 (3)
H8A	0.3799	−0.0414	0.5622	0.079*
C9	0.3169 (9)	0.0666 (9)	0.4761 (7)	0.074 (4)
H9A	0.3402	0.0366	0.4181	0.089*
C10	0.2599 (10)	0.1559 (9)	0.4751 (9)	0.089 (5)
H10A	0.2446	0.1871	0.4166	0.106*
C11	0.2251 (11)	0.1999 (9)	0.5597 (9)	0.092 (5)
H11A	0.1849	0.2606	0.5587	0.110*
C12	0.2489 (9)	0.1551 (7)	0.6474 (8)	0.072 (3)
H12A	0.2264	0.1864	0.7049	0.086*
C13	0.2530 (8)	0.0670 (6)	0.8538 (7)	0.056 (3)
C14	0.1438 (8)	0.0482 (7)	0.8617 (8)	0.078 (4)
H14A	0.1168	0.0019	0.8214	0.093*
C15	0.0730 (9)	0.0970 (9)	0.9287 (10)	0.098 (5)
H15A	−0.0009	0.0835	0.9328	0.118*
C16	0.1114 (11)	0.1644 (9)	0.9885 (9)	0.092 (5)
H16A	0.0642	0.1964	1.0342	0.111*
C17	0.2191 (12)	0.1849 (10)	0.9814 (10)	0.099 (5)
H17A	0.2447	0.2313	1.0224	0.119*
C18	0.2913 (9)	0.1381 (8)	0.9142 (8)	0.074 (3)
H18A	0.3645	0.1537	0.9094	0.089*
C19	0.2257 (6)	−0.4152 (5)	0.8082 (6)	0.046 (2)
C20	0.2260 (7)	−0.5159 (6)	0.7876 (6)	0.056 (3)
C21	0.1398 (8)	−0.5710 (6)	0.8125 (7)	0.068 (3)
C22	0.0452 (8)	−0.5312 (6)	0.8585 (8)	0.070 (3)
H22A	−0.0146	−0.5689	0.8734	0.084*
C23	0.0443 (7)	−0.4331 (7)	0.8808 (7)	0.060 (3)
C24	0.1310 (6)	−0.3767 (5)	0.8562 (6)	0.044 (2)
F20	0.3148 (6)	−0.5604 (4)	0.7419 (5)	0.079 (2)
F21	0.1446 (8)	−0.6678 (5)	0.7875 (8)	0.116 (3)
F23	−0.0482 (5)	−0.3876 (5)	0.9223 (6)	0.086 (2)
F24	0.1191 (5)	−0.2789 (4)	0.8763 (4)	0.0575 (15)
C25	0.3557 (7)	−0.2682 (7)	0.9925 (6)	0.059 (3)
C26	0.4638 (8)	−0.3062 (7)	0.9930 (7)	0.069 (3)
C27	0.4955 (8)	−0.3827 (8)	1.0532 (8)	0.089 (4)
C28	0.4233 (9)	−0.4249 (10)	1.1155 (10)	0.107 (6)
H28A	0.4461	−0.4756	1.1575	0.129*
C29	0.3163 (9)	−0.3905 (10)	1.1147 (10)	0.104 (6)
C30	0.2832 (8)	−0.3117 (8)	1.0563 (8)	0.077 (4)
F26	0.5408 (6)	−0.2666 (6)	0.9352 (5)	0.084 (2)
F27	0.6037 (7)	−0.4136 (8)	1.0520 (7)	0.124 (3)
F29	0.2389 (9)	−0.4314 (10)	1.1744 (8)	0.165 (5)
F30	0.1768 (6)	−0.2769 (7)	1.0631 (6)	0.100 (3)
C31	0.5257 (6)	−0.2872 (6)	0.6229 (5)	0.048 (2)
C32	0.4987 (6)	−0.2887 (6)	0.5274 (6)	0.051 (2)
C33	0.5406 (8)	−0.3627 (7)	0.4673 (6)	0.065 (3)
C34	0.6110 (8)	−0.4373 (7)	0.4991 (6)	0.067 (3)
H34A	0.6406	−0.4863	0.4575	0.081*
C35	0.6366 (8)	−0.4375 (7)	0.5935 (7)	0.063 (3)
C36	0.5946 (7)	−0.3638 (6)	0.6546 (6)	0.054 (3)
F32	0.4319 (6)	−0.2164 (5)	0.4912 (4)	0.0712 (18)
F33	0.5097 (7)	−0.3625 (6)	0.3751 (5)	0.087 (2)
F35	0.7058 (6)	−0.5103 (5)	0.6284 (6)	0.090 (2)
F36	0.6229 (5)	−0.3666 (5)	0.7472 (4)	0.0709 (18)
C37	0.1084 (7)	−0.2467 (6)	0.6590 (7)	0.056 (3)
C38	0.1429 (7)	−0.3297 (7)	0.6057 (6)	0.065 (3)
C39	0.0755 (9)	−0.4055 (8)	0.5948 (8)	0.086 (4)
C40	−0.0278 (8)	−0.4027 (8)	0.6366 (9)	0.092 (5)
H40A	−0.0722	−0.4556	0.6309	0.110*
C41	−0.0644 (8)	−0.3200 (8)	0.6871 (9)	0.081 (4)
C42	0.0023 (7)	−0.2435 (7)	0.6983 (8)	0.069 (3)
F38	0.2418 (6)	−0.3349 (6)	0.5596 (5)	0.085 (2)
F39	0.1150 (8)	−0.4882 (6)	0.5466 (7)	0.120 (3)
F41	−0.1679 (6)	−0.3120 (8)	0.7274 (7)	0.122 (3)
F42	−0.0365 (5)	−0.1653 (5)	0.7525 (6)	0.086 (2)
C101	1.074 (8)	−0.160 (3)	0.349 (5)	0.34 (7)*	0.50
H10B	1.1071	−0.1668	0.2851	0.515*	0.50
H10C	1.0062	−0.1924	0.3528	0.515*	0.50
H10D	1.1229	−0.1891	0.3950	0.515*	0.50
C102	1.051 (3)	−0.048 (2)	0.3714 (13)	0.093 (9)*	0.50
H10E	1.1186	−0.0150	0.3742	0.112*	0.50
H10F	1.0064	−0.0157	0.3222	0.112*	0.50
C201	1.070 (4)	−0.202 (3)	0.377 (4)	0.161 (19)*	0.50
H20A	1.1391	−0.2321	0.3548	0.241*	0.50
H20B	1.0240	−0.1886	0.3231	0.241*	0.50
H20C	1.0341	−0.2456	0.4219	0.241*	0.50
C202	1.088 (2)	−0.104 (2)	0.427 (3)	0.114 (11)*	0.50
H20D	1.1376	−0.1189	0.4788	0.137*	0.50
H20E	1.1247	−0.0617	0.3810	0.137*	0.50
C103	0.9876 (14)	−0.0449 (13)	0.4702 (14)	0.266 (19)*
H10G	0.9093	−0.0432	0.4603	0.319*
H10H	1.0071	−0.1050	0.5062	0.319*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Os1	0.0511 (2)	0.0332 (2)	0.0378 (2)	0.00230 (14)	0.01119 (15)	0.00072 (14)
S1	0.0550 (14)	0.0356 (13)	0.0581 (15)	0.0014 (10)	0.0161 (12)	−0.0015 (11)
S2	0.0861 (19)	0.0435 (14)	0.0375 (13)	−0.0046 (13)	0.0092 (12)	−0.0002 (11)
S3	0.0582 (14)	0.0424 (13)	0.0508 (14)	−0.0009 (11)	0.0180 (11)	0.0002 (11)
S4	0.0597 (15)	0.0417 (14)	0.0571 (16)	0.0043 (11)	−0.0004 (12)	0.0032 (11)
P1	0.0599 (15)	0.0366 (13)	0.0378 (13)	−0.0014 (11)	0.0094 (11)	−0.0016 (10)
C1	0.068 (6)	0.042 (6)	0.053 (6)	0.006 (5)	0.014 (5)	−0.009 (5)
C2	0.081 (8)	0.059 (7)	0.058 (7)	−0.012 (6)	−0.003 (6)	0.009 (6)
C3	0.078 (8)	0.068 (8)	0.078 (9)	−0.012 (7)	−0.015 (7)	−0.012 (7)
C4	0.083 (9)	0.098 (11)	0.089 (10)	−0.038 (8)	−0.003 (8)	0.011 (9)
C5	0.106 (11)	0.097 (11)	0.079 (9)	−0.053 (9)	−0.003 (8)	0.015 (8)
C6	0.084 (8)	0.058 (7)	0.069 (8)	−0.022 (6)	0.002 (6)	0.013 (6)
C7	0.067 (6)	0.043 (6)	0.056 (6)	0.009 (5)	0.014 (5)	0.014 (5)
C8	0.078 (7)	0.049 (6)	0.067 (7)	0.008 (5)	0.015 (6)	0.017 (6)
C9	0.080 (8)	0.091 (10)	0.051 (7)	−0.022 (7)	0.006 (6)	0.019 (6)
C10	0.081 (9)	0.094 (11)	0.090 (11)	−0.009 (8)	−0.013 (8)	0.052 (9)
C11	0.104 (11)	0.073 (9)	0.092 (11)	0.025 (8)	0.012 (9)	0.031 (8)
C12	0.082 (8)	0.054 (7)	0.075 (8)	0.016 (6)	0.009 (6)	0.012 (6)
C13	0.074 (7)	0.037 (5)	0.055 (6)	0.005 (5)	0.015 (5)	−0.006 (5)
C14	0.077 (8)	0.072 (8)	0.083 (9)	−0.007 (6)	0.020 (7)	−0.029 (7)
C15	0.098 (10)	0.070 (9)	0.119 (13)	0.013 (8)	0.053 (9)	−0.001 (9)
C16	0.119 (12)	0.065 (9)	0.085 (10)	0.031 (8)	0.040 (9)	−0.015 (7)
C17	0.121 (13)	0.077 (10)	0.096 (11)	0.023 (9)	0.008 (10)	−0.033 (8)
C18	0.099 (9)	0.055 (7)	0.066 (8)	0.004 (6)	0.010 (7)	−0.016 (6)
C19	0.055 (5)	0.031 (5)	0.049 (6)	0.006 (4)	0.001 (4)	0.000 (4)
C20	0.070 (7)	0.048 (6)	0.048 (6)	0.004 (5)	0.013 (5)	−0.006 (5)
C21	0.098 (9)	0.030 (6)	0.076 (8)	−0.010 (6)	0.003 (7)	−0.003 (5)
C22	0.079 (8)	0.052 (7)	0.079 (8)	−0.020 (6)	0.017 (7)	−0.001 (6)
C23	0.061 (6)	0.068 (7)	0.049 (6)	−0.012 (5)	0.020 (5)	−0.008 (5)
C24	0.062 (6)	0.031 (5)	0.040 (5)	0.001 (4)	0.008 (4)	−0.004 (4)
F20	0.096 (5)	0.045 (4)	0.093 (5)	0.013 (3)	0.029 (4)	−0.018 (3)
F21	0.137 (8)	0.039 (4)	0.171 (9)	−0.011 (4)	0.025 (7)	−0.013 (5)
F23	0.074 (4)	0.083 (5)	0.097 (5)	−0.005 (4)	0.038 (4)	−0.014 (4)
F24	0.067 (4)	0.047 (3)	0.058 (4)	0.002 (3)	0.015 (3)	−0.014 (3)
C25	0.080 (8)	0.057 (7)	0.040 (6)	−0.011 (6)	0.001 (5)	−0.002 (5)
C26	0.088 (9)	0.065 (8)	0.056 (7)	−0.009 (7)	−0.013 (6)	0.008 (6)
C27	0.089 (10)	0.078 (9)	0.100 (11)	0.011 (8)	−0.022 (8)	0.015 (8)
C28	0.131 (14)	0.087 (11)	0.104 (12)	−0.007 (10)	−0.020 (11)	0.055 (10)
C29	0.115 (12)	0.114 (13)	0.087 (10)	−0.043 (10)	−0.009 (9)	0.056 (10)
C30	0.098 (10)	0.081 (9)	0.053 (7)	−0.028 (8)	0.000 (7)	0.018 (6)
F26	0.080 (5)	0.092 (5)	0.079 (5)	0.002 (4)	0.005 (4)	0.016 (4)
F27	0.130 (8)	0.125 (8)	0.114 (7)	0.030 (6)	−0.023 (6)	0.027 (6)
F29	0.172 (10)	0.204 (12)	0.125 (8)	−0.070 (9)	−0.007 (7)	0.115 (9)
F30	0.092 (6)	0.136 (8)	0.072 (5)	−0.023 (5)	0.009 (4)	0.032 (5)
C31	0.047 (5)	0.043 (5)	0.051 (6)	0.005 (4)	0.024 (4)	0.006 (4)
C32	0.059 (6)	0.040 (5)	0.052 (6)	0.012 (5)	0.013 (5)	0.003 (4)
C33	0.074 (7)	0.062 (7)	0.057 (7)	0.004 (6)	0.016 (6)	0.002 (6)
C34	0.073 (7)	0.052 (7)	0.073 (8)	0.016 (6)	0.020 (6)	−0.009 (6)
C35	0.064 (7)	0.045 (6)	0.077 (8)	0.007 (5)	0.005 (6)	0.005 (6)
C36	0.052 (5)	0.058 (6)	0.048 (6)	0.006 (5)	0.012 (5)	0.011 (5)
F32	0.093 (5)	0.065 (4)	0.051 (4)	0.024 (3)	0.006 (3)	0.004 (3)
F33	0.118 (6)	0.083 (5)	0.056 (4)	0.019 (4)	0.010 (4)	−0.011 (4)
F35	0.093 (5)	0.066 (4)	0.106 (6)	0.037 (4)	0.003 (4)	0.007 (4)
F36	0.069 (4)	0.073 (4)	0.068 (4)	0.009 (3)	0.004 (3)	0.017 (3)
C37	0.064 (6)	0.047 (6)	0.057 (6)	−0.004 (5)	−0.007 (5)	−0.003 (5)
C38	0.070 (7)	0.067 (8)	0.057 (7)	−0.002 (6)	−0.001 (6)	−0.008 (6)
C39	0.093 (10)	0.091 (11)	0.077 (9)	−0.008 (8)	−0.022 (8)	−0.015 (8)
C40	0.103 (11)	0.077 (10)	0.102 (11)	−0.041 (9)	−0.027 (9)	−0.009 (8)
C41	0.063 (7)	0.092 (10)	0.089 (10)	−0.013 (7)	−0.014 (7)	0.023 (8)
C42	0.070 (7)	0.062 (8)	0.072 (8)	0.009 (6)	0.005 (6)	0.008 (6)
F38	0.086 (5)	0.094 (6)	0.074 (5)	0.002 (4)	0.007 (4)	−0.027 (4)
F39	0.156 (9)	0.092 (6)	0.113 (7)	−0.014 (6)	−0.009 (6)	−0.048 (5)
F41	0.060 (5)	0.163 (9)	0.144 (8)	−0.030 (5)	0.003 (5)	0.029 (7)
F42	0.062 (4)	0.087 (5)	0.103 (6)	0.017 (4)	0.010 (4)	0.004 (4)

Geometric parameters (Å, º) top

Os1—S4	2.204 (3)	C23—F23	1.361 (9)
Os1—S2	2.218 (3)	C23—C24	1.369 (10)
Os1—S3	2.219 (2)	C24—F24	1.352 (8)
Os1—P1	2.396 (3)	C25—C30	1.374 (10)
Os1—S1	2.420 (2)	C25—C26	1.387 (10)
S1—C19	1.757 (8)	C26—F26	1.340 (10)
S2—C25	1.770 (9)	C26—C27	1.368 (10)
S3—C31	1.777 (9)	C27—C28	1.352 (11)
S4—C37	1.763 (9)	C27—F27	1.360 (11)
P1—C13	1.813 (9)	C28—C29	1.360 (11)
P1—C1	1.819 (10)	C28—H28A	0.9300
P1—C7	1.831 (9)	C29—F29	1.365 (11)
C1—C6	1.383 (10)	C29—C30	1.381 (11)
C1—C2	1.383 (11)	C30—F30	1.354 (10)
C2—C3	1.380 (11)	C31—C36	1.373 (9)
C2—H2A	0.9300	C31—C32	1.381 (9)
C3—C4	1.358 (12)	C32—F32	1.341 (9)
C3—H3A	0.9300	C32—C33	1.370 (10)
C4—C5	1.362 (12)	C33—F33	1.349 (10)
C4—H4A	0.9300	C33—C34	1.365 (10)
C5—C6	1.368 (12)	C34—C35	1.359 (10)
C5—H5A	0.9300	C34—H34A	0.9300
C6—H6A	0.9300	C35—F35	1.355 (9)
C7—C8	1.384 (11)	C35—C36	1.376 (10)
C7—C12	1.386 (10)	C36—F36	1.344 (9)
C8—C9	1.380 (11)	C37—C42	1.382 (10)
C8—H8A	0.9300	C37—C38	1.385 (10)
C9—C10	1.355 (12)	C38—F38	1.338 (10)
C9—H9A	0.9300	C38—C39	1.368 (11)
C10—C11	1.363 (12)	C39—F39	1.361 (11)
C10—H10A	0.9300	C39—C40	1.363 (11)
C11—C12	1.385 (12)	C40—C41	1.368 (11)
C11—H11A	0.9300	C40—H40A	0.9300
C12—H12A	0.9300	C41—F41	1.356 (10)
C13—C14	1.372 (11)	C41—C42	1.369 (11)
C13—C18	1.398 (11)	C42—F42	1.355 (10)
C14—C15	1.385 (11)	C101—C102	1.553 (10)
C14—H14A	0.9300	C101—H10B	0.9600
C15—C16	1.359 (12)	C101—H10C	0.9600
C15—H15A	0.9300	C101—H10D	0.9600
C16—C17	1.358 (12)	C102—C103	1.541 (10)
C16—H16A	0.9300	C102—H10E	0.9700
C17—C18	1.385 (12)	C102—H10F	0.9700
C17—H17A	0.9300	C201—C202	1.533 (10)
C18—H18A	0.9300	C201—H20A	0.9600
C19—C24	1.385 (9)	C201—H20B	0.9600
C19—C20	1.393 (9)	C201—H20C	0.9600
C20—F20	1.344 (9)	C202—C103	1.521 (10)
C20—C21	1.356 (10)	C202—H20D	0.9700
C21—F21	1.355 (10)	C202—H20E	0.9700
C21—C22	1.376 (10)	C103—C103ⁱ	1.530 (10)
C22—C23	1.365 (10)	C103—H10G	0.9700
C22—H22A	0.9300	C103—H10H	0.9700

S4—Os1—S2	124.39 (11)	F24—C24—C23	117.3 (7)
S4—Os1—S3	114.73 (10)	F24—C24—C19	120.0 (7)
S2—Os1—S3	118.87 (11)	C23—C24—C19	122.6 (7)
S4—Os1—P1	85.47 (10)	C30—C25—C26	115.9 (8)
S2—Os1—P1	85.53 (9)	C30—C25—S2	123.4 (7)
S3—Os1—P1	84.86 (9)	C26—C25—S2	119.8 (6)
S4—Os1—S1	99.87 (10)	F26—C26—C27	118.2 (8)
S2—Os1—S1	95.23 (10)	F26—C26—C25	120.1 (8)
S3—Os1—S1	88.55 (9)	C27—C26—C25	121.7 (8)
P1—Os1—S1	172.84 (9)	C28—C27—F27	119.9 (9)
C19—S1—Os1	119.0 (2)	C28—C27—C26	121.8 (9)
C25—S2—Os1	114.9 (3)	F27—C27—C26	118.2 (9)
C31—S3—Os1	114.4 (3)	C27—C28—C29	117.6 (9)
C37—S4—Os1	115.9 (3)	C27—C28—H28A	121.2
C13—P1—C1	106.4 (4)	C29—C28—H28A	121.2
C13—P1—C7	104.5 (4)	C28—C29—F29	120.5 (9)
C1—P1—C7	103.1 (4)	C28—C29—C30	121.4 (8)
C13—P1—Os1	113.0 (3)	F29—C29—C30	118.1 (9)
C1—P1—Os1	114.0 (3)	F30—C30—C25	119.9 (8)
C7—P1—Os1	114.8 (3)	F30—C30—C29	118.5 (8)
C6—C1—C2	118.4 (9)	C25—C30—C29	121.6 (8)
C6—C1—P1	121.1 (7)	C36—C31—C32	116.9 (7)
C2—C1—P1	120.5 (7)	C36—C31—S3	123.4 (6)
C3—C2—C1	119.7 (8)	C32—C31—S3	118.4 (5)
C3—C2—H2A	120.1	F32—C32—C33	118.7 (7)
C1—C2—H2A	120.1	F32—C32—C31	120.3 (7)
C4—C3—C2	121.0 (9)	C33—C32—C31	121.0 (7)
C4—C3—H3A	119.5	F33—C33—C34	119.5 (8)
C2—C3—H3A	119.5	F33—C33—C32	118.9 (8)
C3—C4—C5	119.8 (10)	C34—C33—C32	121.5 (8)
C3—C4—H4A	120.1	C35—C34—C33	117.9 (8)
C5—C4—H4A	120.1	C35—C34—H34A	121.0
C4—C5—C6	120.2 (9)	C33—C34—H34A	121.0
C4—C5—H5A	119.9	F35—C35—C34	120.0 (8)
C6—C5—H5A	119.9	F35—C35—C36	119.0 (8)
C5—C6—C1	120.9 (9)	C34—C35—C36	121.0 (7)
C5—C6—H6A	119.5	F36—C36—C31	119.5 (7)
C1—C6—H6A	119.5	F36—C36—C35	119.0 (7)
C8—C7—C12	118.6 (8)	C31—C36—C35	121.6 (7)
C8—C7—P1	120.3 (6)	C42—C37—C38	116.7 (8)
C12—C7—P1	121.1 (7)	C42—C37—S4	118.7 (6)
C9—C8—C7	120.4 (8)	C38—C37—S4	124.6 (6)
C9—C8—H8A	119.8	F38—C38—C39	118.5 (8)
C7—C8—H8A	119.8	F38—C38—C37	120.2 (8)
C10—C9—C8	120.5 (9)	C39—C38—C37	121.2 (8)
C10—C9—H9A	119.7	F39—C39—C40	119.3 (9)
C8—C9—H9A	119.7	F39—C39—C38	119.3 (9)
C9—C10—C11	120.0 (10)	C40—C39—C38	121.3 (8)
C9—C10—H10A	120.0	C39—C40—C41	118.3 (9)
C11—C10—H10A	120.0	C39—C40—H40A	120.9
C10—C11—C12	120.6 (9)	C41—C40—H40A	120.9
C10—C11—H11A	119.7	F41—C41—C40	120.7 (9)
C12—C11—H11A	119.7	F41—C41—C42	118.4 (9)
C11—C12—C7	119.8 (9)	C40—C41—C42	120.9 (8)
C11—C12—H12A	120.1	F42—C42—C41	118.5 (8)
C7—C12—H12A	120.1	F42—C42—C37	119.9 (8)
C14—C13—C18	118.3 (8)	C41—C42—C37	121.5 (8)
C14—C13—P1	120.0 (7)	C102—C101—H10B	109.5
C18—C13—P1	121.7 (7)	C102—C101—H10C	109.5
C13—C14—C15	121.2 (9)	H10B—C101—H10C	109.5
C13—C14—H14A	119.4	C102—C101—H10D	109.5
C15—C14—H14A	119.4	H10B—C101—H10D	109.5
C16—C15—C14	120.0 (10)	H10C—C101—H10D	109.5
C16—C15—H15A	120.0	C103—C102—C101	105.4 (14)
C14—C15—H15A	120.0	C103—C102—H10E	110.7
C17—C16—C15	119.8 (10)	C101—C102—H10E	110.7
C17—C16—H16A	120.1	C103—C102—H10F	110.7
C15—C16—H16A	120.1	C101—C102—H10F	110.7
C16—C17—C18	121.3 (10)	H10E—C102—H10F	108.8
C16—C17—H17A	119.4	C202—C201—H20A	109.5
C18—C17—H17A	119.4	C202—C201—H20B	109.5
C17—C18—C13	119.3 (9)	H20A—C201—H20B	109.5
C17—C18—H18A	120.3	C202—C201—H20C	109.5
C13—C18—H18A	120.3	H20A—C201—H20C	109.5
C24—C19—C20	114.6 (7)	H20B—C201—H20C	109.5
C24—C19—S1	127.8 (6)	C103—C202—C201	118.0 (15)
C20—C19—S1	117.6 (5)	C103—C202—H20D	107.8
F20—C20—C21	118.5 (7)	C201—C202—H20D	107.8
F20—C20—C19	119.2 (7)	C103—C202—H20E	107.8
C21—C20—C19	122.3 (7)	C201—C202—H20E	107.8
F21—C21—C20	119.0 (8)	H20D—C202—H20E	107.1
F21—C21—C22	118.5 (8)	C202—C103—C103ⁱ	115.3 (15)
C20—C21—C22	122.4 (7)	C103ⁱ—C103—C102	112.6 (15)
C23—C22—C21	116.0 (8)	C103ⁱ—C103—H10G	109.1
C23—C22—H22A	122.0	C102—C103—H10G	109.1
C21—C22—H22A	122.0	C103ⁱ—C103—H10H	109.1
F23—C23—C22	119.3 (7)	C102—C103—H10H	109.1
F23—C23—C24	118.5 (7)	H10G—C103—H10H	107.8
C22—C23—C24	122.0 (7)

S4—Os1—S1—C19	−55.2 (4)	C21—C22—C23—C24	2.0 (17)
S2—Os1—S1—C19	71.0 (4)	F23—C23—C24—F24	0.9 (14)
S3—Os1—S1—C19	−170.1 (4)	C22—C23—C24—F24	175.9 (10)
S4—Os1—S2—C25	118.2 (3)	F23—C23—C24—C19	−175.8 (9)
S3—Os1—S2—C25	−78.8 (3)	C22—C23—C24—C19	−0.7 (16)
P1—Os1—S2—C25	−160.4 (3)	C20—C19—C24—F24	−177.0 (8)
S1—Os1—S2—C25	12.4 (3)	S1—C19—C24—F24	2.4 (13)
S4—Os1—S3—C31	−75.0 (3)	C20—C19—C24—C23	−0.5 (13)
S2—Os1—S3—C31	120.4 (3)	S1—C19—C24—C23	178.9 (8)
P1—Os1—S3—C31	−157.6 (3)	Os1—S2—C25—C30	−118.2 (8)
S1—Os1—S3—C31	25.2 (3)	Os1—S2—C25—C26	72.7 (7)
S2—Os1—S4—C37	−88.0 (3)	C30—C25—C26—F26	−178.1 (10)
S3—Os1—S4—C37	108.3 (3)	S2—C25—C26—F26	−8.2 (11)
P1—Os1—S4—C37	−169.5 (3)	C30—C25—C26—C27	0.4 (9)
S1—Os1—S4—C37	15.4 (3)	S2—C25—C26—C27	170.3 (8)
S4—Os1—P1—C13	84.7 (4)	F26—C26—C27—C28	178.2 (13)
S2—Os1—P1—C13	−40.4 (4)	C25—C26—C27—C28	−0.3 (11)
S3—Os1—P1—C13	−160.0 (4)	F26—C26—C27—F27	0.8 (12)
S4—Os1—P1—C1	−153.6 (3)	C25—C26—C27—F27	−177.7 (12)
S2—Os1—P1—C1	81.3 (3)	F27—C27—C28—C29	179.2 (14)
S3—Os1—P1—C1	−38.3 (3)	C26—C27—C28—C29	2 (2)
S4—Os1—P1—C7	−35.0 (3)	C27—C28—C29—F29	178.6 (14)
S2—Os1—P1—C7	−160.1 (3)	C27—C28—C29—C30	−4 (2)
S3—Os1—P1—C7	80.4 (3)	C26—C25—C30—F30	177.7 (10)
C13—P1—C1—C6	−90.3 (9)	S2—C25—C30—F30	8.2 (16)
C7—P1—C1—C6	19.3 (9)	C26—C25—C30—C29	−2.1 (16)
Os1—P1—C1—C6	144.4 (7)	S2—C25—C30—C29	−171.6 (11)
C13—P1—C1—C2	88.6 (7)	C28—C29—C30—F30	−176.0 (14)
C7—P1—C1—C2	−161.7 (6)	F29—C29—C30—F30	2 (2)
Os1—P1—C1—C2	−36.6 (7)	C28—C29—C30—C25	4 (2)
C6—C1—C2—C3	−1.0 (9)	F29—C29—C30—C25	−178.3 (13)
P1—C1—C2—C3	−180.0 (7)	Os1—S3—C31—C36	−101.0 (7)
C1—C2—C3—C4	−0.2 (10)	Os1—S3—C31—C32	91.9 (5)
C2—C3—C4—C5	0.3 (18)	C36—C31—C32—F32	−180.0 (9)
C3—C4—C5—C6	1 (2)	S3—C31—C32—F32	−12.1 (9)
C4—C5—C6—C1	−2 (2)	C36—C31—C32—C33	−0.9 (8)
C2—C1—C6—C5	2.1 (15)	S3—C31—C32—C33	166.9 (7)
P1—C1—C6—C5	−178.8 (10)	F32—C32—C33—F33	−2.6 (10)
C13—P1—C7—C8	−165.5 (6)	C31—C32—C33—F33	178.3 (9)
C1—P1—C7—C8	83.4 (7)	F32—C32—C33—C34	178.5 (10)
Os1—P1—C7—C8	−41.1 (7)	C31—C32—C33—C34	−0.6 (9)
C13—P1—C7—C12	17.6 (10)	F33—C33—C34—C35	−177.1 (10)
C1—P1—C7—C12	−93.5 (9)	C32—C33—C34—C35	1.7 (14)
Os1—P1—C7—C12	141.9 (8)	C33—C34—C35—F35	179.7 (10)
C12—C7—C8—C9	−0.6 (9)	C33—C34—C35—C36	−1.4 (16)
P1—C7—C8—C9	−177.6 (7)	C32—C31—C36—F36	−179.4 (8)
C7—C8—C9—C10	0.1 (10)	S3—C31—C36—F36	13.4 (12)
C8—C9—C10—C11	−0.3 (17)	C32—C31—C36—C35	1.2 (13)
C9—C10—C11—C12	1 (2)	S3—C31—C36—C35	−166.0 (8)
C10—C11—C12—C7	−2 (2)	F35—C35—C36—F36	−0.5 (15)
C8—C7—C12—C11	1.3 (15)	C34—C35—C36—F36	−179.4 (10)
P1—C7—C12—C11	178.3 (10)	F35—C35—C36—C31	178.8 (9)
C1—P1—C13—C14	−176.9 (7)	C34—C35—C36—C31	−0.1 (16)
C7—P1—C13—C14	74.5 (7)	Os1—S4—C37—C42	112.6 (8)
Os1—P1—C13—C14	−51.0 (7)	Os1—S4—C37—C38	−69.6 (8)
C1—P1—C13—C18	5.3 (9)	C42—C37—C38—F38	175.2 (10)
C7—P1—C13—C18	−103.4 (9)	S4—C37—C38—F38	−2.6 (11)
Os1—P1—C13—C18	131.2 (8)	C42—C37—C38—C39	−1.6 (9)
C18—C13—C14—C15	−1.0 (9)	S4—C37—C38—C39	−179.4 (8)
P1—C13—C14—C15	−178.9 (8)	F38—C38—C39—F39	7.0 (12)
C13—C14—C15—C16	−0.4 (10)	C37—C38—C39—F39	−176.1 (11)
C14—C15—C16—C17	1.0 (18)	F38—C38—C39—C40	−177.3 (12)
C15—C16—C17—C18	0 (2)	C37—C38—C39—C40	−0.4 (10)
C16—C17—C18—C13	−1 (2)	F39—C39—C40—C41	178.1 (12)
C14—C13—C18—C17	1.7 (15)	C38—C39—C40—C41	2.4 (17)
P1—C13—C18—C17	179.6 (10)	C39—C40—C41—F41	177.9 (11)
Os1—S1—C19—C24	−14.2 (10)	C39—C40—C41—C42	−2.3 (19)
Os1—S1—C19—C20	165.2 (5)	F41—C41—C42—F42	2.7 (17)
C24—C19—C20—F20	−179.4 (9)	C40—C41—C42—F42	−177.2 (12)
S1—C19—C20—F20	1.2 (10)	F41—C41—C42—C37	−179.9 (10)
C24—C19—C20—C21	0.3 (8)	C40—C41—C42—C37	0.2 (19)
S1—C19—C20—C21	−179.2 (7)	C38—C37—C42—F42	179.1 (9)
F20—C20—C21—F21	−2.3 (12)	S4—C37—C42—F42	−3.0 (14)
C19—C20—C21—F21	178.0 (10)	C38—C37—C42—C41	1.7 (15)
F20—C20—C21—C22	−179.2 (11)	S4—C37—C42—C41	179.6 (9)
C19—C20—C21—C22	1.1 (10)	C201—C202—C103—C103ⁱ	173 (4)
F21—C21—C22—C23	−179.1 (11)	C201—C202—C103—C102	−90 (4)
C20—C21—C22—C23	−2.2 (15)	C101—C102—C103—C202	44 (5)
C21—C22—C23—F23	177.0 (10)	C101—C102—C103—C103ⁱ	147 (5)

Symmetry code: (i) −x+2, −y, −z+1.

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