Chloridotris(penta-fluoro-benzene-thiol-ato-κS)[tris-(4-fluoro-phen-yl)phosphine-κP]osmium(IV).

The title complex, [Os(C(6)F(5)S)(3)Cl(C(18)H(12)F(3)P)], displays a trigonal-bipyramidal Os(IV) coordination geometry with the S atoms of three thiol-ate ligands occupying the equatorial positions. The thiol-ate penta-fluoro-phenyl substituents are all placed above the equatorial plane, forming a claw-like cavity which accommodates the chloride ligand with a normal Os-Cl bond length. The phosphine ligand trans to the chloride ligand reveals a short Os-P bond length compared to other chloride-phosphine Os(IV) complexes (average = 2.40 Å). This strong bonding indicates that the inductive effect of the F atoms in the phosphine does not affect significantly its basicity, compared to triphenyl-phosphine. This feature is also consistent with the known poor trans influence of Cl(-). The crystal packing involves π-π contacts between inversion-related thiol-ate C(6)F(5) rings, with a centroid-centroid separation of 3.659 (8) Å.

Related literature

For the structures of related five-coordinated OsIV complexes, see: Hills et al. (1991 ▶); Arroyo et al. (1994 ▶, 2007 ▶, 2009 ▶); Cerón et al. (2006 ▶); Mendoza et al. (2006 ▶). For the structure and basicity of free tris­(4-fluoro­phen­yl)phosphine, see: bin Shawkataly et al. (1996 ▶) and Allman & Goel (1982 ▶), respectively. For geometrical analysis using the Cambridge Structural Database, see: Bruno et al. (2002 ▶).

Experimental

Crystal data

[Os(C6F5S)3Cl(C18H12F3P)]

M = 1139.26

Monoclinic,

a = 17.983 (7) Å

b = 10.446 (5) Å

c = 21.521 (8) Å

β = 107.62 (2)°

V = 3853 (3) Å3

Z = 4

Mo Kα radiation

μ = 3.70 mm−1

T = 298 K

0.5 × 0.4 × 0.3 mm

Data collection

Siemens P4 diffractometer

Absorption correction: ψ scan (XSCANS; Siemens, 1996 ▶) T min = 0.215, T max = 0.330

13694 measured reflections

6749 independent reflections

5120 reflections with I > 2σ(I)

R int = 0.052

3 standard reflections every 97 reflections intensity decay: 0.5%

Refinement

R[F 2 > 2σ(F 2)] = 0.048

wR(F 2) = 0.135

S = 1.33

6749 reflections

542 parameters

H-atom parameters constrained

Δρmax = 1.96 e Å−3

Δρmin = −2.11 e Å−3

Data collection: XSCANS (Siemens, 1996 ▶); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: Mercury (Macrae et al., 2008 ▶); software used to prepare material for publication: SHELXTL-Plus.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810011281/kp2255sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810011281/kp2255Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Os(C6F5S)3Cl(C18H12F3P)]	F(000) = 2184
Mr = 1139.26	Dx = 1.964 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 84 reflections
a = 17.983 (7) Å	θ = 5.2–12.5°
b = 10.446 (5) Å	µ = 3.70 mm−1
c = 21.521 (8) Å	T = 298 K
β = 107.62 (2)°	Prism, dark-brown
V = 3853 (3) Å3	0.5 × 0.4 × 0.3 mm
Z = 4

Siemens P4 diffractometer	5120 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.052
graphite	θmax = 25.0°, θmin = 2.0°
ω scans	h = −21→11
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −12→1
Tmin = 0.215, Tmax = 0.330	l = −24→25
13694 measured reflections	3 standard reflections every 97 reflections
6749 independent reflections	intensity decay: 0.5%

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.048	H-atom parameters constrained
wR(F2) = 0.135	w = 1/[σ2(Fo2) + (0.026P)2 + 24.9505P] where P = (Fo2 + 2Fc2)/3
S = 1.33	(Δ/σ)max = 0.002
6749 reflections	Δρmax = 1.96 e Å−3
542 parameters	Δρmin = −2.11 e Å−3
0 restraints	Extinction correction: SHELXTL-Plus (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 constraints	Extinction coefficient: 0.00165 (11)
Primary atom site location: structure-invariant direct methods

	x	y	z	Uiso*/Ueq
Os1	0.76039 (2)	0.56074 (3)	0.715615 (17)	0.04286 (15)
Cl1	0.78380 (14)	0.6117 (2)	0.61374 (11)	0.0508 (6)
P1	0.73741 (14)	0.5076 (2)	0.81355 (11)	0.0428 (5)
S1	0.78307 (18)	0.7581 (3)	0.75283 (13)	0.0589 (7)
S2	0.85683 (16)	0.4221 (3)	0.74230 (12)	0.0572 (6)
S3	0.63988 (15)	0.4992 (3)	0.66494 (12)	0.0549 (6)
C1	0.8010 (6)	0.5869 (9)	0.8837 (5)	0.053 (2)
C2	0.8829 (7)	0.5691 (12)	0.8998 (5)	0.072 (3)
H2A	0.9022	0.5170	0.8732	0.086*
C3	0.9347 (8)	0.6259 (14)	0.9531 (6)	0.082 (4)
H3A	0.9883	0.6133	0.9632	0.099*
C4	0.9038 (9)	0.7011 (13)	0.9902 (5)	0.076 (4)
F4	0.9545 (6)	0.7575 (9)	1.0432 (4)	0.120 (3)
C5	0.8274 (9)	0.7246 (12)	0.9780 (5)	0.076 (4)
H5A	0.8099	0.7783	1.0051	0.092*
C6	0.7743 (7)	0.6666 (11)	0.9236 (5)	0.066 (3)
H6A	0.7211	0.6819	0.9144	0.079*
C7	0.7474 (5)	0.3408 (9)	0.8337 (4)	0.045 (2)
C8	0.7133 (7)	0.2499 (10)	0.7861 (5)	0.063 (3)
H8A	0.6900	0.2766	0.7434	0.075*
C9	0.7135 (9)	0.1221 (12)	0.8007 (6)	0.083 (4)
H9A	0.6925	0.0622	0.7682	0.099*
C10	0.7446 (9)	0.0850 (11)	0.8631 (6)	0.075 (4)
F10	0.7452 (6)	−0.0411 (7)	0.8774 (4)	0.110 (3)
C11	0.7818 (7)	0.1675 (11)	0.9110 (6)	0.073 (3)
H11A	0.8066	0.1385	0.9530	0.087*
C12	0.7819 (6)	0.2956 (11)	0.8956 (5)	0.057 (3)
H12A	0.8062	0.3534	0.9283	0.069*
C13	0.6421 (5)	0.5476 (10)	0.8168 (4)	0.048 (2)
C14	0.6033 (7)	0.4718 (12)	0.8503 (6)	0.071 (3)
H14A	0.6261	0.3952	0.8685	0.085*
C15	0.5324 (7)	0.5062 (13)	0.8573 (6)	0.075 (3)
H15A	0.5088	0.4560	0.8817	0.090*
C16	0.4974 (6)	0.6154 (12)	0.8278 (5)	0.060 (3)
F16	0.4288 (4)	0.6488 (8)	0.8350 (4)	0.089 (2)
C17	0.5316 (7)	0.6903 (12)	0.7939 (6)	0.074 (3)
H17A	0.5066	0.7644	0.7742	0.089*
C18	0.6040 (6)	0.6581 (11)	0.7881 (5)	0.061 (3)
H18A	0.6273	0.7111	0.7647	0.073*
C19	0.7813 (7)	0.8609 (9)	0.6869 (5)	0.062 (3)
C20	0.7086 (8)	0.9076 (11)	0.6483 (6)	0.070 (3)
F20	0.6449 (5)	0.8800 (8)	0.6635 (4)	0.092 (2)
C21	0.7051 (9)	0.9799 (12)	0.5942 (7)	0.084 (4)
F21	0.6339 (6)	1.0171 (9)	0.5564 (4)	0.120 (3)
C22	0.7686 (11)	1.0100 (13)	0.5801 (7)	0.088 (4)
F22	0.7646 (7)	1.0821 (8)	0.5264 (4)	0.137 (4)
C23	0.8428 (10)	0.9711 (13)	0.6153 (7)	0.083 (4)
F23	0.9054 (6)	0.9989 (10)	0.6012 (5)	0.133 (4)
C24	0.8443 (8)	0.8931 (12)	0.6702 (6)	0.076 (3)
F24	0.9150 (5)	0.8441 (9)	0.7039 (4)	0.100 (3)
C25	0.9160 (6)	0.4406 (10)	0.6912 (5)	0.054 (2)
C26	0.9050 (6)	0.3713 (11)	0.6354 (5)	0.059 (3)
F26	0.8450 (4)	0.2905 (7)	0.6162 (4)	0.088 (2)
C27	0.9505 (7)	0.3856 (13)	0.5952 (5)	0.070 (3)
F27	0.9364 (5)	0.3208 (10)	0.5399 (4)	0.107 (3)
C28	1.0114 (7)	0.4685 (15)	0.6120 (6)	0.078 (4)
F28	1.0582 (5)	0.4826 (11)	0.5748 (5)	0.125 (3)
C29	1.0258 (7)	0.5396 (14)	0.6685 (8)	0.085 (4)
F29	1.0851 (5)	0.6206 (11)	0.6855 (5)	0.138 (4)
C30	0.9755 (6)	0.5254 (12)	0.7056 (6)	0.067 (3)
F30	0.9929 (4)	0.5951 (8)	0.7607 (4)	0.095 (2)
C31	0.6220 (6)	0.4927 (10)	0.5789 (5)	0.054 (2)
C32	0.5926 (7)	0.5966 (12)	0.5394 (6)	0.069 (3)
F32	0.5806 (5)	0.7067 (7)	0.5659 (4)	0.104 (3)
C33	0.5783 (8)	0.5886 (16)	0.4740 (6)	0.085 (4)
F33	0.5500 (6)	0.6898 (11)	0.4365 (4)	0.139 (4)
C34	0.5880 (7)	0.4766 (19)	0.4461 (6)	0.087 (4)
F34	0.5699 (6)	0.4657 (13)	0.3809 (4)	0.140 (4)
C35	0.6150 (8)	0.3715 (15)	0.4836 (6)	0.081 (4)
F35	0.6243 (6)	0.2614 (11)	0.4560 (4)	0.133 (4)
C36	0.6326 (6)	0.3817 (11)	0.5496 (5)	0.063 (3)
F36	0.6620 (5)	0.2803 (7)	0.5865 (4)	0.088 (2)

	U11	U22	U33	U12	U13	U23
Os1	0.0543 (2)	0.0379 (2)	0.0388 (2)	−0.00019 (17)	0.01766 (16)	0.00087 (15)
Cl1	0.0629 (14)	0.0505 (13)	0.0431 (12)	−0.0031 (11)	0.0224 (11)	0.0043 (10)
P1	0.0553 (14)	0.0410 (13)	0.0371 (12)	−0.0003 (11)	0.0212 (10)	0.0003 (10)
S1	0.0863 (19)	0.0437 (14)	0.0519 (15)	−0.0079 (13)	0.0288 (14)	−0.0035 (11)
S2	0.0636 (15)	0.0599 (17)	0.0513 (14)	0.0123 (13)	0.0223 (12)	0.0082 (12)
S3	0.0617 (15)	0.0576 (16)	0.0481 (14)	−0.0056 (12)	0.0207 (12)	0.0031 (11)
C1	0.078 (7)	0.036 (5)	0.050 (6)	−0.007 (5)	0.026 (5)	−0.004 (4)
C2	0.085 (8)	0.078 (8)	0.058 (7)	−0.017 (7)	0.030 (6)	−0.016 (6)
C3	0.087 (9)	0.093 (10)	0.058 (7)	−0.027 (8)	0.008 (6)	−0.018 (7)
C4	0.099 (10)	0.079 (9)	0.043 (6)	−0.036 (8)	0.008 (6)	−0.013 (6)
F4	0.151 (8)	0.130 (8)	0.067 (5)	−0.062 (6)	0.017 (5)	−0.037 (5)
C5	0.116 (11)	0.064 (8)	0.051 (7)	−0.015 (7)	0.027 (7)	−0.022 (6)
C6	0.087 (8)	0.055 (7)	0.056 (6)	0.003 (6)	0.023 (6)	−0.002 (5)
C7	0.050 (5)	0.043 (5)	0.043 (5)	0.005 (4)	0.016 (4)	0.002 (4)
C8	0.083 (8)	0.051 (6)	0.045 (6)	−0.007 (6)	0.004 (5)	0.004 (5)
C9	0.134 (12)	0.043 (6)	0.070 (8)	−0.006 (7)	0.031 (8)	0.001 (6)
C10	0.123 (11)	0.041 (6)	0.071 (8)	0.014 (6)	0.045 (7)	0.015 (6)
F10	0.157 (8)	0.052 (5)	0.108 (6)	0.005 (5)	0.020 (5)	0.025 (4)
C11	0.095 (9)	0.057 (7)	0.057 (7)	0.013 (6)	0.009 (6)	0.019 (6)
C12	0.070 (7)	0.057 (7)	0.041 (5)	0.004 (5)	0.011 (5)	0.005 (5)
C13	0.053 (5)	0.056 (6)	0.035 (5)	−0.004 (5)	0.014 (4)	−0.004 (4)
C14	0.073 (7)	0.060 (7)	0.087 (8)	0.005 (6)	0.035 (7)	0.018 (6)
C15	0.061 (7)	0.078 (8)	0.096 (9)	0.014 (6)	0.039 (7)	0.020 (7)
C16	0.048 (6)	0.075 (8)	0.057 (6)	0.012 (5)	0.017 (5)	−0.004 (6)
F16	0.058 (4)	0.112 (6)	0.103 (5)	0.023 (4)	0.034 (4)	0.006 (5)
C17	0.090 (9)	0.072 (8)	0.064 (7)	0.028 (7)	0.028 (6)	0.010 (6)
C18	0.066 (7)	0.062 (7)	0.066 (7)	0.007 (5)	0.034 (5)	0.015 (5)
C19	0.101 (9)	0.030 (5)	0.055 (6)	−0.023 (5)	0.023 (6)	−0.007 (4)
C20	0.101 (10)	0.041 (6)	0.064 (7)	−0.006 (6)	0.019 (7)	−0.001 (5)
F20	0.094 (5)	0.073 (5)	0.112 (6)	0.012 (4)	0.034 (5)	0.008 (4)
C21	0.101 (11)	0.049 (7)	0.088 (10)	0.010 (7)	0.009 (8)	−0.003 (6)
F21	0.152 (8)	0.083 (6)	0.105 (6)	0.023 (6)	0.008 (6)	0.017 (5)
C22	0.130 (13)	0.060 (8)	0.088 (10)	−0.022 (9)	0.057 (10)	−0.014 (7)
F22	0.274 (13)	0.072 (6)	0.078 (5)	−0.008 (7)	0.074 (7)	0.013 (4)
C23	0.116 (12)	0.058 (8)	0.092 (10)	−0.036 (8)	0.054 (9)	−0.021 (7)
F23	0.179 (9)	0.118 (8)	0.142 (8)	−0.070 (7)	0.108 (7)	−0.026 (6)
C24	0.089 (9)	0.062 (8)	0.074 (8)	−0.030 (7)	0.020 (7)	−0.011 (6)
F24	0.091 (5)	0.106 (7)	0.110 (6)	−0.040 (5)	0.038 (5)	−0.015 (5)
C25	0.052 (5)	0.063 (7)	0.054 (6)	0.014 (5)	0.027 (5)	−0.002 (5)
C26	0.064 (6)	0.056 (7)	0.058 (6)	0.007 (5)	0.020 (5)	−0.007 (5)
F26	0.083 (5)	0.086 (5)	0.098 (5)	−0.016 (4)	0.033 (4)	−0.034 (4)
C27	0.063 (7)	0.090 (9)	0.053 (6)	0.022 (7)	0.010 (5)	−0.008 (6)
F27	0.103 (6)	0.149 (8)	0.076 (5)	0.023 (5)	0.036 (4)	−0.028 (5)
C28	0.067 (8)	0.100 (11)	0.073 (8)	0.020 (7)	0.028 (7)	0.007 (7)
F28	0.114 (7)	0.165 (9)	0.131 (7)	0.015 (6)	0.091 (6)	0.022 (7)
C29	0.054 (7)	0.081 (10)	0.116 (11)	−0.007 (7)	0.018 (7)	0.013 (8)
F29	0.095 (6)	0.150 (9)	0.180 (10)	−0.057 (6)	0.059 (6)	−0.036 (8)
C30	0.053 (6)	0.075 (8)	0.069 (7)	−0.014 (6)	0.011 (5)	−0.010 (6)
F30	0.087 (5)	0.103 (6)	0.089 (5)	−0.017 (4)	0.016 (4)	−0.033 (4)
C31	0.057 (6)	0.054 (6)	0.049 (6)	0.000 (5)	0.011 (5)	0.003 (5)
C32	0.072 (7)	0.068 (8)	0.065 (7)	0.004 (6)	0.015 (6)	0.007 (6)
F32	0.143 (7)	0.061 (5)	0.092 (5)	0.021 (5)	0.009 (5)	0.008 (4)
C33	0.086 (9)	0.099 (11)	0.061 (8)	0.003 (8)	0.005 (7)	0.030 (8)
F33	0.158 (9)	0.145 (9)	0.093 (6)	0.021 (7)	0.007 (6)	0.065 (6)
C34	0.064 (7)	0.144 (15)	0.047 (7)	−0.012 (9)	0.009 (6)	0.004 (8)
F34	0.134 (8)	0.236 (13)	0.047 (4)	0.001 (8)	0.022 (4)	−0.007 (6)
C35	0.089 (9)	0.096 (11)	0.064 (8)	0.003 (8)	0.030 (7)	−0.019 (8)
F35	0.151 (8)	0.149 (9)	0.099 (6)	0.022 (7)	0.038 (6)	−0.058 (6)
C36	0.061 (6)	0.060 (7)	0.061 (7)	0.007 (5)	0.010 (5)	−0.004 (6)
F36	0.112 (6)	0.059 (4)	0.096 (5)	0.018 (4)	0.034 (4)	−0.002 (4)

Os1—S1	2.205 (3)	C16—F16	1.336 (11)
Os1—S2	2.199 (3)	C16—C17	1.339 (16)
Os1—S3	2.206 (3)	C17—C18	1.386 (15)
Os1—Cl1	2.414 (2)	C17—H17A	0.9300
Os1—P1	2.334 (2)	C18—H18A	0.9300
P1—C13	1.787 (10)	C19—C24	1.331 (16)
P1—C7	1.791 (10)	C19—C20	1.407 (17)
P1—C1	1.797 (10)	C20—F20	1.316 (14)
S1—C19	1.772 (10)	C20—C21	1.374 (18)
S2—C25	1.759 (9)	C21—C22	1.306 (19)
S3—C31	1.783 (10)	C21—F21	1.349 (15)
C1—C6	1.382 (14)	C22—F22	1.362 (16)
C1—C2	1.420 (15)	C22—C23	1.38 (2)
C2—C3	1.375 (16)	C23—F23	1.284 (15)
C2—H2A	0.9300	C23—C24	1.429 (18)
C3—C4	1.354 (18)	C24—F24	1.360 (15)
C3—H3A	0.9300	C25—C30	1.350 (15)
C4—C5	1.340 (18)	C25—C26	1.364 (14)
C4—F4	1.360 (12)	C26—F26	1.333 (12)
C5—C6	1.405 (16)	C26—C27	1.366 (15)
C5—H5A	0.9300	C27—F27	1.326 (13)
C6—H6A	0.9300	C27—C28	1.356 (18)
C7—C12	1.372 (13)	C28—F28	1.334 (13)
C7—C8	1.395 (14)	C28—C29	1.381 (19)
C8—C9	1.371 (15)	C29—F29	1.323 (15)
C8—H8A	0.9300	C29—C30	1.384 (17)
C9—C10	1.345 (16)	C30—F30	1.346 (13)
C9—H9A	0.9300	C31—C36	1.360 (15)
C10—F10	1.352 (13)	C31—C32	1.381 (15)
C10—C11	1.354 (17)	C32—F32	1.329 (14)
C11—C12	1.379 (15)	C32—C33	1.355 (17)
C11—H11A	0.9300	C33—F33	1.334 (15)
C12—H12A	0.9300	C33—C34	1.35 (2)
C13—C18	1.388 (14)	C34—F34	1.346 (14)
C13—C14	1.391 (14)	C34—C35	1.36 (2)
C14—C15	1.376 (15)	C35—F35	1.328 (16)
C14—H14A	0.9300	C35—C36	1.364 (16)
C15—C16	1.363 (16)	C36—F36	1.333 (13)
C15—H15A	0.9300
S2—Os1—S1	118.47 (11)	F16—C16—C17	120.2 (11)
S2—Os1—S3	121.08 (11)	F16—C16—C15	118.5 (10)
S1—Os1—S3	119.87 (11)	C17—C16—C15	121.3 (10)
S2—Os1—P1	87.06 (9)	C16—C17—C18	120.3 (11)
S1—Os1—P1	87.61 (9)	C16—C17—H17A	119.8
S3—Os1—P1	87.77 (9)	C18—C17—H17A	119.8
S2—Os1—Cl1	92.40 (9)	C17—C18—C13	120.9 (10)
S1—Os1—Cl1	93.42 (9)	C17—C18—H18A	119.6
S3—Os1—Cl1	91.75 (9)	C13—C18—H18A	119.6
P1—Os1—Cl1	178.96 (9)	C24—C19—C20	117.9 (11)
C13—P1—C7	104.2 (5)	C24—C19—S1	124.0 (11)
C13—P1—C1	103.5 (5)	C20—C19—S1	118.1 (9)
C7—P1—C1	104.7 (5)	F20—C20—C21	120.8 (13)
C13—P1—Os1	114.5 (3)	F20—C20—C19	120.1 (10)
C7—P1—Os1	114.7 (3)	C21—C20—C19	119.1 (13)
C1—P1—Os1	114.1 (3)	C22—C21—F21	121.9 (15)
C19—S1—Os1	108.6 (3)	C22—C21—C20	120.7 (15)
C25—S2—Os1	110.1 (4)	F21—C21—C20	117.4 (14)
C31—S3—Os1	111.5 (4)	C21—C22—F22	120.2 (17)
C6—C1—C2	117.2 (10)	C21—C22—C23	124.7 (14)
C6—C1—P1	123.2 (9)	F22—C22—C23	115.0 (14)
C2—C1—P1	119.6 (8)	F23—C23—C22	125.1 (14)
C3—C2—C1	122.5 (12)	F23—C23—C24	121.7 (16)
C3—C2—H2A	118.7	C22—C23—C24	113.2 (13)
C1—C2—H2A	118.7	C19—C24—F24	119.7 (12)
C4—C3—C2	116.5 (13)	C19—C24—C23	124.3 (14)
C4—C3—H3A	121.7	F24—C24—C23	115.9 (13)
C2—C3—H3A	121.7	C30—C25—C26	116.5 (10)
C5—C4—C3	124.7 (11)	C30—C25—S2	121.0 (8)
C5—C4—F4	118.2 (12)	C26—C25—S2	122.5 (9)
C3—C4—F4	117.1 (13)	F26—C26—C25	119.8 (10)
C4—C5—C6	118.9 (11)	F26—C26—C27	117.3 (10)
C4—C5—H5A	120.6	C25—C26—C27	122.8 (11)
C6—C5—H5A	120.6	F27—C27—C28	119.0 (12)
C1—C6—C5	120.1 (12)	F27—C27—C26	121.5 (12)
C1—C6—H6A	120.0	C28—C27—C26	119.5 (11)
C5—C6—H6A	120.0	F28—C28—C27	121.1 (13)
C12—C7—C8	116.6 (9)	F28—C28—C29	119.0 (14)
C12—C7—P1	123.5 (8)	C27—C28—C29	119.9 (11)
C8—C7—P1	119.7 (7)	F29—C29—C28	120.6 (13)
C9—C8—C7	121.6 (10)	F29—C29—C30	121.5 (14)
C9—C8—H8A	119.2	C28—C29—C30	118.0 (12)
C7—C8—H8A	119.2	F30—C30—C25	121.0 (10)
C10—C9—C8	118.7 (12)	F30—C30—C29	115.6 (11)
C10—C9—H9A	120.6	C25—C30—C29	123.2 (12)
C8—C9—H9A	120.6	C36—C31—C32	117.8 (10)
C9—C10—F10	118.7 (12)	C36—C31—S3	120.5 (8)
C9—C10—C11	122.4 (11)	C32—C31—S3	121.6 (9)
F10—C10—C11	118.6 (11)	F32—C32—C33	119.6 (12)
C10—C11—C12	118.1 (10)	F32—C32—C31	119.9 (10)
C10—C11—H11A	121.0	C33—C32—C31	120.5 (12)
C12—C11—H11A	121.0	F33—C33—C34	119.7 (13)
C7—C12—C11	122.3 (10)	F33—C33—C32	119.9 (15)
C7—C12—H12A	118.9	C34—C33—C32	120.4 (13)
C11—C12—H12A	118.9	F34—C34—C33	120.9 (15)
C18—C13—C14	116.5 (9)	F34—C34—C35	118.6 (16)
C18—C13—P1	121.8 (7)	C33—C34—C35	120.4 (12)
C14—C13—P1	121.7 (8)	F35—C35—C34	120.3 (13)
C15—C14—C13	122.3 (11)	F35—C35—C36	120.8 (14)
C15—C14—H14A	118.8	C34—C35—C36	118.9 (13)
C13—C14—H14A	118.8	F36—C36—C31	119.2 (10)
C16—C15—C14	118.7 (11)	F36—C36—C35	118.9 (11)
C16—C15—H15A	120.7	C31—C36—C35	121.9 (12)
C14—C15—H15A	120.7
S2—Os1—P1—C13	−160.3 (4)	S1—C19—C20—C21	−175.4 (9)
S1—Os1—P1—C13	81.0 (4)	F20—C20—C21—C22	178.3 (12)
S3—Os1—P1—C13	−39.0 (4)	C19—C20—C21—C22	−3.0 (19)
S2—Os1—P1—C7	−39.9 (4)	F20—C20—C21—F21	−2.3 (18)
S1—Os1—P1—C7	−158.6 (4)	C19—C20—C21—F21	176.4 (10)
S3—Os1—P1—C7	81.4 (4)	F21—C21—C22—F22	1(2)
S2—Os1—P1—C1	80.8 (4)	C20—C21—C22—F22	−179.7 (12)
S1—Os1—P1—C1	−37.9 (4)	F21—C21—C22—C23	−177.5 (13)
S3—Os1—P1—C1	−157.9 (4)	C20—C21—C22—C23	2(2)
S2—Os1—S1—C19	109.5 (5)	C21—C22—C23—F23	179.0 (13)
S3—Os1—S1—C19	−79.1 (5)	F22—C22—C23—F23	1(2)
P1—Os1—S1—C19	−165.2 (5)	C21—C22—C23—C24	0(2)
Cl1—Os1—S1—C19	14.9 (5)	F22—C22—C23—C24	−178.5 (11)
S1—Os1—S2—C25	−81.7 (4)	C20—C19—C24—F24	−176.3 (10)
S3—Os1—S2—C25	107.0 (4)	S1—C19—C24—F24	1.3 (16)
P1—Os1—S2—C25	−167.3 (4)	C20—C19—C24—C23	−0.6 (18)
Cl1—Os1—S2—C25	13.5 (4)	S1—C19—C24—C23	177.0 (9)
S2—Os1—S3—C31	−85.5 (4)	F23—C23—C24—C19	−179.7 (11)
S1—Os1—S3—C31	103.3 (4)	C22—C23—C24—C19	−0.5 (19)
P1—Os1—S3—C31	−170.7 (4)	F23—C23—C24—F24	−3.8 (18)
Cl1—Os1—S3—C31	8.4 (4)	C22—C23—C24—F24	175.3 (11)
C13—P1—C1—C6	−4.8 (10)	Os1—S2—C25—C30	87.0 (10)
C7—P1—C1—C6	−113.7 (9)	Os1—S2—C25—C26	−93.0 (9)
Os1—P1—C1—C6	120.2 (8)	C30—C25—C26—F26	−176.5 (10)
C13—P1—C1—C2	175.6 (9)	S2—C25—C26—F26	3.5 (15)
C7—P1—C1—C2	66.7 (9)	C30—C25—C26—C27	−0.3 (17)
Os1—P1—C1—C2	−59.4 (9)	S2—C25—C26—C27	179.7 (9)
C6—C1—C2—C3	1.1 (18)	F26—C26—C27—F27	−0.8 (17)
P1—C1—C2—C3	−179.3 (10)	C25—C26—C27—F27	−177.1 (11)
C1—C2—C3—C4	0(2)	F26—C26—C27—C28	178.8 (11)
C2—C3—C4—C5	−1(2)	C25—C26—C27—C28	2.5 (19)
C2—C3—C4—F4	179.8 (12)	F27—C27—C28—F28	−2.0 (19)
C3—C4—C5—C6	1(2)	C26—C27—C28—F28	178.3 (11)
F4—C4—C5—C6	−179.7 (11)	F27—C27—C28—C29	178.2 (12)
C2—C1—C6—C5	−1.0 (16)	C26—C27—C28—C29	−1(2)
P1—C1—C6—C5	179.4 (9)	F28—C28—C29—F29	0(2)
C4—C5—C6—C1	0.1 (18)	C27—C28—C29—F29	179.9 (13)
C13—P1—C7—C12	−94.5 (9)	F28—C28—C29—C30	178.6 (12)
C1—P1—C7—C12	13.8 (10)	C27—C28—C29—C30	−2(2)
Os1—P1—C7—C12	139.6 (8)	C26—C25—C30—F30	−177.6 (10)
C13—P1—C7—C8	80.0 (9)	S2—C25—C30—F30	2.4 (16)
C1—P1—C7—C8	−171.7 (8)	C26—C25—C30—C29	−3.0 (18)
Os1—P1—C7—C8	−46.0 (9)	S2—C25—C30—C29	177.0 (10)
C12—C7—C8—C9	0.8 (17)	F29—C29—C30—F30	−3(2)
P1—C7—C8—C9	−174.0 (10)	C28—C29—C30—F30	178.9 (12)
C7—C8—C9—C10	3(2)	F29—C29—C30—C25	−177.6 (12)
C8—C9—C10—F10	−179.6 (12)	C28—C29—C30—C25	4(2)
C8—C9—C10—C11	−6(2)	Os1—S3—C31—C36	92.6 (9)
C9—C10—C11—C12	5(2)	Os1—S3—C31—C32	−91.3 (9)
F10—C10—C11—C12	179.0 (11)	C36—C31—C32—F32	179.4 (11)
C8—C7—C12—C11	−1.4 (16)	S3—C31—C32—F32	3.3 (16)
P1—C7—C12—C11	173.2 (9)	C36—C31—C32—C33	−2.8 (18)
C10—C11—C12—C7	−1.5 (19)	S3—C31—C32—C33	−178.9 (10)
C7—P1—C13—C18	−162.8 (8)	F32—C32—C33—F33	−2(2)
C1—P1—C13—C18	87.9 (9)	C31—C32—C33—F33	−179.9 (12)
Os1—P1—C13—C18	−36.8 (9)	F32—C32—C33—C34	−178.1 (13)
C7—P1—C13—C14	19.5 (10)	C31—C32—C33—C34	4(2)
C1—P1—C13—C14	−89.8 (10)	F33—C33—C34—F34	0(2)
Os1—P1—C13—C14	145.5 (8)	C32—C33—C34—F34	176.3 (12)
C18—C13—C14—C15	−2.7 (18)	F33—C33—C34—C35	−178.4 (13)
P1—C13—C14—C15	175.1 (10)	C32—C33—C34—C35	−2(2)
C13—C14—C15—C16	3(2)	F34—C34—C35—F35	1(2)
C14—C15—C16—F16	−179.7 (11)	C33—C34—C35—F35	179.8 (13)
C14—C15—C16—C17	−1.7 (19)	F34—C34—C35—C36	−179.2 (11)
F16—C16—C17—C18	177.9 (10)	C33—C34—C35—C36	0(2)
C15—C16—C17—C18	0.0 (19)	C32—C31—C36—F36	178.9 (10)
C16—C17—C18—C13	0.4 (18)	S3—C31—C36—F36	−4.9 (15)
C14—C13—C18—C17	0.9 (16)	C32—C31—C36—C35	−0.1 (18)
P1—C13—C18—C17	−176.9 (9)	S3—C31—C36—C35	176.1 (10)
Os1—S1—C19—C24	−92.9 (10)	F35—C35—C36—F36	2.4 (19)
Os1—S1—C19—C20	84.7 (9)	C34—C35—C36—F36	−177.3 (11)
C24—C19—C20—F20	−178.9 (11)	F35—C35—C36—C31	−178.5 (12)
S1—C19—C20—F20	3.3 (14)	C34—C35—C36—C31	2(2)
C24—C19—C20—C21	2.3 (16)

Table 1

Selected bond lengths (Å)

Os1—S1	2.205 (3)
Os1—S2	2.199 (3)
Os1—S3	2.206 (3)
Os1—Cl1	2.414 (2)
Os1—P1	2.334 (2)