Tetra­kis(2,3,5,6-tetra­fluoro­benzene­thiol­ato-κS)(tri­phenyl­phosphane-κP)osmium(IV): a monoclinic polymorph

Zeleny, P.; Arroyo, M.; Meléndez, L.; Bernès, S.

doi:10.1107/S2414314619016225

Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphane-κP)osmium(IV): a monoclinic polymorph

P. Zeleny, M. Arroyo, L. Meléndez and S. Bernès

The structure of the title compound, [Os(C₆HF₄S)₄{P(C₆H₅)₃}], has been previously reported [Arroyo et al. (1994). J. Chem. Soc. Dalton Trans. pp. 1819–1824], in the space group P $\overline{1}$ . We have now obtained a monoclinic polymorph for this compound, crystallized from ethanol, while the previous form was obtained from a hexane/chloroform mixture. The molecular structure is based on a trigonal–bipyramidal Os^IV coordination geometry, close to that observed previously in the triclinic form.

Keywords: crystal structure; osmium(IV); polymorphism; tetrafluorobenzenethiolate.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314619016225/zl4036sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2414314619016225/zl4036Isup2.hkl Contains datablock I

CCDC reference: 1969511

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.013 Å
R factor = 0.045
wR factor = 0.092
Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
RINTA01_ALERT_3_B  The value of Rint is greater than 0.18
            Rint given   0.186

Alert level C
GOODF01_ALERT_2_C  The least squares goodness of fit parameter lies
            outside the range 0.80 <> 2.00
            Goodness of fit given =      0.795
PLAT220_ALERT_2_C Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.1 Ratio
PLAT234_ALERT_4_C Large Hirshfeld Difference F3       --C23      .       0.19 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C19      --C20      .       0.18 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C21      --C22      .       0.24 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C23      --C24      .       0.18 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C31      --C36      .       0.19 Ang.
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C22 Check
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C28 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C19 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C21 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C23 Check
PLAT334_ALERT_2_C Small Aver. Benzene C-C Dist C25      -C30             1.37 Ang.
PLAT334_ALERT_2_C Small Aver. Benzene C-C Dist C37      -C42             1.37 Ang.
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01324 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H12      ..S2       .       2.98 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H14      ..S4       .       2.96 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H34      ..F15      .       2.58 Ang.
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          9 Note
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
PLAT020_ALERT_3_G The Value of Rint is Greater Than 0.12 .........      0.186 Report
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Os1      --S2       .        6.5 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Os1      --S3       .        5.1 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Os1      --S4       .        5.2 s.u.
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         12 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          7 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
  20 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   8 ALERT level G = General information/check it is not something unexpected

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

Computing details top

Data collection: X-AREA (Stoe & Cie, 2018); cell refinement: X-AREA (Stoe & Cie, 2018); data reduction: X-AREA (Stoe & Cie, 2018); program(s) used to solve structure: SHELXT2018 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2018); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphane-κP)osmium(IV) top

Crystal data top

[Os(C₆HF₄S)₄(C₁₈H₁₅P)]	F(000) = 2280
M_r = 1176.98	D_x = 1.832 Mg m⁻³
Monoclinic, P2₁/c	Ag Kα radiation, λ = 0.56083 Å
a = 12.4008 (5) Å	Cell parameters from 22104 reflections
b = 13.8892 (7) Å	θ = 2.0–23.5°
c = 25.2321 (11) Å	µ = 1.80 mm⁻¹
β = 100.991 (3)°	T = 295 K
V = 4266.2 (3) Å³	Plate, brown
Z = 4	0.20 × 0.06 × 0.03 mm

Data collection top

Stoe Stadivari diffractometer	8692 independent reflections
Radiation source: Sealed X-ray tube, Axo Astix-f Microfocus source	4264 reflections with I > 2σ(I)
Graded multilayer mirror monochromator	R_int = 0.186
Detector resolution: 5.81 pixels mm^-1	θ_max = 20.5°, θ_min = 2.0°
ω scans	h = −15→15
Absorption correction: multi-scan (X-AREA; Stoe & Cie, 2018)	k = −17→17
T_min = 0.388, T_max = 1.000	l = −31→31
93107 measured reflections

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.092	H-atom parameters constrained
S = 0.80	w = 1/[σ²(F_o²) + (0.0305P)²] where P = (F_o² + 2F_c²)/3
8692 reflections	(Δ/σ)_max = 0.002
577 parameters	Δρ_max = 0.71 e Å⁻³
12 restraints	Δρ_min = −1.05 e Å⁻³
0 constraints

Special details top

Refinement. All H atoms were placed in idealized positions, with C—H bond lengths of 0.93 Å and U_iso(H) = 1.2×U_eq(carrier C atom).

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

	x	y	z	U_iso*/U_eq
Os1	0.26257 (2)	0.72225 (2)	0.54794 (2)	0.05251 (10)
P1	0.23237 (15)	0.63058 (14)	0.46496 (8)	0.0522 (5)
S1	0.30213 (16)	0.82548 (15)	0.62659 (8)	0.0668 (6)
S2	0.38093 (16)	0.60874 (16)	0.58113 (8)	0.0670 (6)
S3	0.08383 (15)	0.70369 (16)	0.54370 (8)	0.0656 (6)
S4	0.32211 (17)	0.83611 (16)	0.49853 (8)	0.0695 (6)
C1	0.2366 (5)	0.5002 (5)	0.4732 (3)	0.0554 (19)
C2	0.2910 (6)	0.4419 (6)	0.4430 (3)	0.065 (2)
H2	0.329275	0.469588	0.418569	0.077*
C3	0.2900 (7)	0.3425 (6)	0.4483 (4)	0.074 (2)
H3	0.326374	0.304047	0.427095	0.089*
C4	0.2349 (6)	0.3008 (6)	0.4851 (3)	0.067 (2)
H4	0.234290	0.234273	0.489147	0.080*
C5	0.1808 (6)	0.3593 (7)	0.5158 (3)	0.067 (2)
H5	0.142517	0.331698	0.540215	0.081*
C6	0.1826 (6)	0.4577 (6)	0.5106 (3)	0.059 (2)
H6	0.147568	0.496165	0.532308	0.071*
C7	0.3332 (5)	0.6512 (5)	0.4226 (3)	0.0505 (18)
C8	0.3022 (6)	0.6737 (6)	0.3679 (3)	0.071 (2)
H8	0.228602	0.685311	0.353508	0.085*
C9	0.3789 (7)	0.6791 (6)	0.3349 (3)	0.079 (3)
H9	0.355914	0.690868	0.298149	0.095*
C10	0.4878 (7)	0.6673 (6)	0.3555 (4)	0.068 (2)
H10	0.539175	0.671926	0.333165	0.081*
C11	0.5213 (6)	0.6485 (5)	0.4097 (3)	0.062 (2)
H11	0.595667	0.640958	0.423953	0.075*
C12	0.4450 (6)	0.6406 (5)	0.4432 (3)	0.060 (2)
H12	0.468844	0.628102	0.479744	0.071*
C13	0.1013 (5)	0.6534 (5)	0.4210 (3)	0.0491 (18)
C14	0.0643 (6)	0.7474 (5)	0.4116 (3)	0.062 (2)
H14	0.105932	0.798161	0.428677	0.074*
C15	−0.0352 (7)	0.7661 (7)	0.3766 (3)	0.076 (2)
H15	−0.058204	0.829321	0.369675	0.092*
C16	−0.0999 (6)	0.6912 (8)	0.3522 (3)	0.075 (3)
H16	−0.166895	0.703585	0.329645	0.090*
C17	−0.0634 (6)	0.5979 (7)	0.3619 (3)	0.071 (2)
H17	−0.105422	0.547273	0.344834	0.086*
C18	0.0359 (6)	0.5783 (6)	0.3969 (3)	0.064 (2)
H18	0.058057	0.514870	0.404097	0.077*
C19	0.2201 (6)	0.8136 (6)	0.6755 (3)	0.060 (2)
C20	0.1820 (8)	0.8938 (9)	0.6965 (4)	0.094 (3)
C21	0.1238 (10)	0.8909 (13)	0.7386 (6)	0.133 (6)
C22	0.0940 (10)	0.8069 (16)	0.7575 (5)	0.155 (9)
H22	0.047515	0.804355	0.782347	0.186*
C23	0.1340 (8)	0.7267 (12)	0.7392 (4)	0.108 (4)
C24	0.1917 (6)	0.7276 (9)	0.6974 (3)	0.081 (3)
C25	0.4434 (6)	0.6181 (6)	0.6500 (3)	0.064 (2)
C26	0.5247 (7)	0.6827 (7)	0.6702 (3)	0.073 (2)
C27	0.5792 (7)	0.6786 (9)	0.7224 (4)	0.095 (3)
C28	0.5575 (10)	0.6084 (12)	0.7576 (4)	0.117 (4)
H28	0.596547	0.604811	0.792873	0.140*
C29	0.4772 (11)	0.5456 (9)	0.7386 (5)	0.106 (3)
C30	0.4203 (8)	0.5490 (8)	0.6859 (4)	0.082 (3)
C31	0.0172 (5)	0.7771 (6)	0.5852 (3)	0.0599 (18)
C32	−0.0365 (6)	0.7385 (6)	0.6231 (3)	0.063 (2)
C33	−0.1025 (7)	0.7926 (8)	0.6505 (4)	0.079 (3)
C34	−0.1176 (7)	0.8872 (9)	0.6387 (4)	0.095 (3)
H34	−0.160757	0.924662	0.657037	0.114*
C35	−0.0691 (7)	0.9272 (7)	0.6000 (5)	0.089 (3)
C36	−0.0021 (7)	0.8743 (7)	0.5736 (4)	0.077 (3)
C37	0.3850 (6)	0.9313 (5)	0.5385 (3)	0.061 (2)
C38	0.3314 (6)	1.0133 (6)	0.5508 (3)	0.063 (2)
C39	0.3847 (7)	1.0855 (6)	0.5819 (4)	0.069 (2)
C40	0.4944 (7)	1.0825 (7)	0.5998 (3)	0.075 (2)
H40	0.529985	1.132860	0.620328	0.091*
C41	0.5525 (7)	1.0049 (7)	0.5876 (4)	0.072 (2)
C42	0.4977 (7)	0.9318 (6)	0.5572 (3)	0.069 (2)
F1	0.2049 (5)	0.9820 (5)	0.6771 (3)	0.129 (2)
F2	0.0878 (6)	0.9748 (7)	0.7556 (4)	0.205 (4)
F3	0.1098 (5)	0.6368 (7)	0.7576 (3)	0.166 (3)
F4	0.2212 (4)	0.6441 (4)	0.6780 (3)	0.110 (2)
F5	0.5539 (4)	0.7526 (4)	0.6381 (2)	0.0948 (17)
F6	0.6577 (4)	0.7465 (6)	0.7405 (2)	0.142 (3)
F7	0.4529 (6)	0.4739 (6)	0.7704 (3)	0.155 (3)
F8	0.3406 (4)	0.4832 (4)	0.6691 (2)	0.0977 (16)
F9	−0.0231 (4)	0.6436 (4)	0.6353 (2)	0.0864 (14)
F10	−0.1503 (4)	0.7474 (5)	0.6865 (2)	0.118 (2)
F11	−0.0839 (5)	1.0212 (4)	0.5886 (3)	0.141 (2)
F12	0.0411 (4)	0.9153 (4)	0.5348 (2)	0.1025 (18)
F13	0.2227 (4)	1.0214 (3)	0.5329 (2)	0.0893 (15)
F14	0.3251 (4)	1.1613 (3)	0.5948 (2)	0.0964 (16)
F15	0.6604 (4)	0.9994 (4)	0.6038 (2)	0.1128 (19)
F16	0.5587 (4)	0.8562 (3)	0.5443 (2)	0.0889 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Os1	0.04872 (15)	0.06055 (18)	0.04846 (16)	−0.00044 (17)	0.00977 (11)	−0.00498 (19)
P1	0.0462 (10)	0.0602 (13)	0.0503 (13)	−0.0004 (9)	0.0095 (10)	−0.0050 (10)
S1	0.0724 (13)	0.0704 (14)	0.0611 (13)	−0.0117 (10)	0.0219 (11)	−0.0167 (11)
S2	0.0684 (13)	0.0770 (16)	0.0533 (12)	0.0080 (10)	0.0062 (10)	−0.0093 (11)
S3	0.0563 (11)	0.0772 (17)	0.0641 (13)	−0.0016 (10)	0.0139 (10)	−0.0169 (11)
S4	0.0823 (14)	0.0682 (15)	0.0600 (13)	−0.0109 (11)	0.0183 (11)	−0.0089 (11)
C1	0.044 (4)	0.062 (5)	0.058 (5)	0.004 (3)	0.003 (4)	−0.006 (4)
C2	0.066 (5)	0.073 (6)	0.059 (5)	0.005 (4)	0.023 (4)	−0.003 (5)
C3	0.083 (6)	0.060 (6)	0.082 (6)	0.007 (5)	0.023 (5)	−0.010 (5)
C4	0.059 (5)	0.061 (6)	0.075 (6)	0.002 (4)	−0.001 (4)	0.002 (5)
C5	0.065 (5)	0.080 (7)	0.058 (5)	−0.004 (4)	0.015 (4)	0.008 (5)
C6	0.061 (5)	0.054 (5)	0.063 (5)	0.000 (4)	0.011 (4)	−0.003 (4)
C7	0.043 (4)	0.057 (5)	0.052 (5)	−0.001 (3)	0.009 (3)	−0.011 (4)
C8	0.049 (5)	0.110 (7)	0.052 (5)	−0.004 (4)	0.008 (4)	0.006 (5)
C9	0.059 (5)	0.119 (8)	0.062 (6)	−0.001 (5)	0.019 (5)	0.002 (5)
C10	0.068 (6)	0.072 (6)	0.071 (6)	−0.001 (4)	0.034 (5)	−0.010 (5)
C11	0.050 (4)	0.071 (6)	0.070 (6)	−0.001 (4)	0.022 (4)	−0.003 (5)
C12	0.054 (5)	0.069 (6)	0.056 (5)	−0.004 (4)	0.011 (4)	−0.010 (4)
C13	0.046 (4)	0.049 (5)	0.053 (5)	−0.005 (3)	0.011 (3)	0.001 (4)
C14	0.055 (4)	0.061 (7)	0.063 (5)	−0.001 (3)	−0.005 (4)	0.005 (4)
C15	0.073 (5)	0.088 (7)	0.067 (5)	0.011 (5)	0.009 (4)	0.011 (5)
C16	0.048 (5)	0.117 (9)	0.058 (5)	0.010 (5)	0.005 (4)	0.002 (5)
C17	0.052 (5)	0.092 (7)	0.066 (6)	−0.011 (4)	0.001 (4)	−0.016 (5)
C18	0.048 (4)	0.077 (6)	0.065 (5)	−0.005 (4)	0.007 (4)	−0.002 (4)
C19	0.046 (4)	0.082 (7)	0.055 (5)	0.010 (4)	0.013 (4)	−0.017 (4)
C20	0.081 (7)	0.129 (10)	0.072 (7)	0.018 (7)	0.013 (5)	−0.024 (7)
C21	0.080 (9)	0.223 (19)	0.100 (11)	0.017 (9)	0.027 (7)	−0.084 (12)
C22	0.053 (7)	0.34 (3)	0.068 (8)	0.009 (11)	0.008 (6)	−0.057 (13)
C23	0.065 (6)	0.170 (12)	0.088 (8)	−0.007 (8)	0.009 (6)	0.046 (9)
C24	0.060 (5)	0.118 (9)	0.069 (6)	−0.004 (6)	0.023 (4)	0.019 (7)
C25	0.061 (5)	0.075 (6)	0.055 (5)	0.014 (4)	0.012 (4)	−0.011 (5)
C26	0.056 (5)	0.108 (8)	0.053 (5)	0.001 (5)	0.007 (4)	0.000 (5)
C27	0.063 (6)	0.158 (11)	0.060 (6)	−0.007 (6)	−0.003 (5)	−0.022 (7)
C28	0.107 (9)	0.177 (14)	0.057 (7)	0.037 (9)	−0.007 (7)	−0.004 (8)
C29	0.125 (10)	0.116 (11)	0.077 (9)	0.014 (7)	0.023 (8)	0.026 (8)
C30	0.084 (7)	0.095 (8)	0.067 (7)	0.004 (6)	0.009 (5)	−0.007 (6)
C31	0.058 (4)	0.059 (5)	0.060 (5)	0.002 (4)	0.004 (4)	0.005 (5)
C32	0.061 (5)	0.062 (6)	0.067 (5)	−0.005 (4)	0.015 (4)	−0.005 (4)
C33	0.067 (5)	0.104 (8)	0.071 (6)	0.008 (6)	0.024 (5)	−0.006 (6)
C34	0.073 (6)	0.112 (10)	0.102 (9)	0.021 (6)	0.021 (6)	−0.032 (7)
C35	0.071 (6)	0.075 (8)	0.120 (9)	0.018 (5)	0.014 (6)	−0.007 (7)
C36	0.057 (5)	0.097 (8)	0.074 (6)	0.000 (5)	0.008 (5)	0.006 (6)
C37	0.072 (5)	0.057 (5)	0.056 (5)	0.004 (4)	0.017 (4)	0.000 (4)
C38	0.057 (5)	0.052 (5)	0.075 (6)	−0.008 (4)	0.006 (4)	−0.006 (4)
C39	0.070 (6)	0.062 (6)	0.077 (6)	0.005 (4)	0.016 (5)	−0.008 (5)
C40	0.076 (6)	0.072 (7)	0.073 (6)	−0.010 (5)	−0.001 (5)	−0.010 (5)
C41	0.054 (5)	0.076 (7)	0.082 (6)	−0.012 (5)	0.004 (5)	0.011 (5)
C42	0.083 (6)	0.063 (6)	0.068 (6)	0.017 (5)	0.029 (5)	0.003 (5)
F1	0.131 (5)	0.094 (5)	0.157 (6)	0.027 (4)	0.018 (4)	−0.046 (5)
F2	0.158 (6)	0.260 (10)	0.207 (8)	0.046 (6)	0.061 (6)	−0.127 (8)
F3	0.117 (5)	0.245 (10)	0.144 (6)	−0.008 (5)	0.042 (4)	0.087 (6)
F4	0.095 (4)	0.096 (5)	0.148 (6)	0.003 (3)	0.043 (4)	0.019 (4)
F5	0.076 (3)	0.127 (5)	0.084 (3)	−0.018 (3)	0.024 (3)	−0.006 (3)
F6	0.088 (4)	0.240 (8)	0.089 (4)	−0.033 (4)	−0.007 (3)	−0.040 (5)
F7	0.203 (7)	0.158 (7)	0.101 (5)	0.005 (5)	0.018 (5)	0.048 (5)
F8	0.112 (4)	0.080 (4)	0.100 (4)	−0.002 (3)	0.016 (3)	0.007 (3)
F9	0.087 (3)	0.080 (4)	0.096 (4)	−0.011 (3)	0.030 (3)	−0.001 (3)
F10	0.094 (4)	0.167 (6)	0.105 (4)	0.010 (3)	0.054 (3)	0.003 (4)
F11	0.135 (5)	0.076 (4)	0.200 (7)	0.040 (4)	0.005 (5)	0.000 (4)
F12	0.087 (4)	0.092 (4)	0.132 (5)	0.007 (3)	0.028 (3)	0.038 (4)
F13	0.065 (3)	0.072 (3)	0.126 (4)	−0.001 (2)	0.008 (3)	−0.010 (3)
F14	0.093 (3)	0.063 (3)	0.133 (5)	0.010 (3)	0.022 (3)	−0.019 (3)
F15	0.054 (3)	0.120 (5)	0.153 (5)	−0.003 (3)	−0.008 (3)	0.009 (4)
F16	0.079 (3)	0.078 (4)	0.116 (4)	0.013 (2)	0.034 (3)	0.003 (3)

Geometric parameters (Å, º) top

Os1—S2	2.207 (2)	C19—C20	1.358 (11)
Os1—S3	2.2138 (19)	C19—C24	1.391 (11)
Os1—S4	2.225 (2)	C20—F1	1.368 (11)
Os1—P1	2.4178 (19)	C20—C21	1.394 (13)
Os1—S1	2.421 (2)	C21—C22	1.339 (15)
P1—C13	1.812 (7)	C21—F2	1.346 (15)
P1—C7	1.817 (7)	C22—C23	1.336 (15)
P1—C1	1.822 (8)	C22—H22	0.9300
S1—C19	1.749 (8)	C23—C24	1.381 (11)
S2—C25	1.768 (8)	C23—F3	1.386 (13)
S3—C31	1.773 (8)	C24—F4	1.337 (11)
S4—C37	1.754 (8)	C25—C26	1.373 (11)
C1—C2	1.373 (9)	C25—C30	1.386 (12)
C1—C6	1.389 (10)	C26—F5	1.358 (9)
C2—C3	1.388 (10)	C26—C27	1.362 (12)
C2—H2	0.9300	C27—F6	1.370 (11)
C3—C4	1.380 (10)	C27—C28	1.379 (15)
C3—H3	0.9300	C28—C29	1.341 (15)
C4—C5	1.382 (10)	C28—H28	0.9300
C4—H4	0.9300	C29—F7	1.350 (12)
C5—C6	1.374 (10)	C29—C30	1.381 (13)
C5—H5	0.9300	C30—F8	1.353 (10)
C6—H6	0.9300	C31—C32	1.375 (9)
C7—C12	1.393 (9)	C31—C36	1.393 (10)
C7—C8	1.394 (9)	C32—F9	1.356 (8)
C8—C9	1.382 (10)	C32—C33	1.388 (10)
C8—H8	0.9300	C33—F10	1.332 (10)
C9—C10	1.362 (10)	C33—C34	1.353 (11)
C9—H9	0.9300	C34—C35	1.359 (12)
C10—C11	1.375 (10)	C34—H34	0.9300
C10—H10	0.9300	C35—F11	1.344 (10)
C11—C12	1.388 (9)	C35—C36	1.374 (11)
C11—H11	0.9300	C36—F12	1.329 (9)
C12—H12	0.9300	C37—C38	1.383 (10)
C13—C14	1.389 (9)	C37—C42	1.386 (10)
C13—C18	1.389 (9)	C38—F13	1.342 (8)
C14—C15	1.398 (9)	C38—C39	1.364 (10)
C14—H14	0.9300	C39—C40	1.350 (10)
C15—C16	1.384 (11)	C39—F14	1.361 (8)
C15—H15	0.9300	C40—C41	1.364 (11)
C16—C17	1.378 (11)	C40—H40	0.9300
C16—H16	0.9300	C41—F15	1.324 (8)
C17—C18	1.399 (10)	C41—C42	1.372 (11)
C17—H17	0.9300	C42—F16	1.370 (8)
C18—H18	0.9300

S2—Os1—S3	121.49 (8)	C17—C18—H18	120.0
S2—Os1—S4	116.91 (8)	C20—C19—C24	114.5 (9)
S3—Os1—S4	119.46 (8)	C20—C19—S1	119.4 (8)
S2—Os1—P1	86.24 (7)	C24—C19—S1	126.0 (6)
S3—Os1—P1	84.75 (7)	C19—C20—F1	118.9 (9)
S4—Os1—P1	84.39 (7)	C19—C20—C21	122.9 (12)
S2—Os1—S1	95.50 (7)	F1—C20—C21	118.1 (11)
S3—Os1—S1	98.80 (7)	C22—C21—F2	120.7 (15)
S4—Os1—S1	90.08 (7)	C22—C21—C20	120.9 (14)
P1—Os1—S1	174.40 (7)	F2—C21—C20	117.9 (15)
C13—P1—C7	104.5 (3)	C23—C22—C21	117.2 (14)
C13—P1—C1	104.3 (3)	C23—C22—H22	121.4
C7—P1—C1	102.4 (3)	C21—C22—H22	121.4
C13—P1—Os1	114.2 (2)	C22—C23—C24	122.5 (13)
C7—P1—Os1	114.6 (2)	C22—C23—F3	121.0 (13)
C1—P1—Os1	115.4 (2)	C24—C23—F3	116.2 (13)
C19—S1—Os1	117.9 (3)	F4—C24—C23	119.3 (11)
C25—S2—Os1	117.1 (3)	F4—C24—C19	119.4 (7)
C31—S3—Os1	118.6 (2)	C23—C24—C19	121.2 (11)
C37—S4—Os1	111.8 (3)	C26—C25—C30	116.0 (8)
C2—C1—C6	118.5 (8)	C26—C25—S2	124.5 (7)
C2—C1—P1	122.0 (6)	C30—C25—S2	119.0 (7)
C6—C1—P1	119.5 (6)	F5—C26—C27	117.8 (9)
C1—C2—C3	121.3 (8)	F5—C26—C25	120.4 (7)
C1—C2—H2	119.3	C27—C26—C25	121.7 (10)
C3—C2—H2	119.3	C26—C27—F6	118.9 (11)
C4—C3—C2	119.7 (8)	C26—C27—C28	122.0 (11)
C4—C3—H3	120.1	F6—C27—C28	119.1 (10)
C2—C3—H3	120.1	C29—C28—C27	116.9 (10)
C3—C4—C5	119.1 (8)	C29—C28—H28	121.6
C3—C4—H4	120.5	C27—C28—H28	121.6
C5—C4—H4	120.5	C28—C29—F7	120.1 (12)
C6—C5—C4	120.9 (8)	C28—C29—C30	122.1 (11)
C6—C5—H5	119.6	F7—C29—C30	117.8 (13)
C4—C5—H5	119.6	F8—C30—C29	119.3 (11)
C5—C6—C1	120.4 (7)	F8—C30—C25	119.4 (8)
C5—C6—H6	119.8	C29—C30—C25	121.3 (10)
C1—C6—H6	119.8	C32—C31—C36	115.9 (7)
C12—C7—C8	117.4 (7)	C32—C31—S3	121.9 (7)
C12—C7—P1	120.8 (6)	C36—C31—S3	120.9 (6)
C8—C7—P1	121.8 (5)	F9—C32—C31	118.8 (7)
C9—C8—C7	121.2 (7)	F9—C32—C33	118.1 (8)
C9—C8—H8	119.4	C31—C32—C33	123.1 (9)
C7—C8—H8	119.4	F10—C33—C34	123.1 (9)
C10—C9—C8	120.6 (8)	F10—C33—C32	117.8 (10)
C10—C9—H9	119.7	C34—C33—C32	119.1 (9)
C8—C9—H9	119.7	C33—C34—C35	119.5 (9)
C9—C10—C11	119.5 (8)	C33—C34—H34	120.2
C9—C10—H10	120.2	C35—C34—H34	120.2
C11—C10—H10	120.2	F11—C35—C34	119.4 (10)
C10—C11—C12	120.6 (7)	F11—C35—C36	119.1 (10)
C10—C11—H11	119.7	C34—C35—C36	121.5 (10)
C12—C11—H11	119.7	F12—C36—C35	119.6 (10)
C11—C12—C7	120.7 (7)	F12—C36—C31	119.5 (8)
C11—C12—H12	119.7	C35—C36—C31	120.8 (9)
C7—C12—H12	119.7	C38—C37—C42	114.6 (7)
C14—C13—C18	119.0 (7)	C38—C37—S4	124.7 (6)
C14—C13—P1	119.9 (5)	C42—C37—S4	120.5 (6)
C18—C13—P1	121.1 (6)	F13—C38—C39	118.5 (7)
C13—C14—C15	120.4 (7)	F13—C38—C37	119.3 (7)
C13—C14—H14	119.8	C39—C38—C37	122.2 (8)
C15—C14—H14	119.8	C40—C39—F14	120.1 (8)
C16—C15—C14	120.5 (8)	C40—C39—C38	121.1 (8)
C16—C15—H15	119.7	F14—C39—C38	118.7 (8)
C14—C15—H15	119.7	C39—C40—C41	119.4 (8)
C17—C16—C15	119.0 (8)	C39—C40—H40	120.3
C17—C16—H16	120.5	C41—C40—H40	120.3
C15—C16—H16	120.5	F15—C41—C40	121.5 (8)
C16—C17—C18	120.9 (8)	F15—C41—C42	119.5 (9)
C16—C17—H17	119.5	C40—C41—C42	119.0 (8)
C18—C17—H17	119.5	F16—C42—C41	117.6 (8)
C13—C18—C17	120.1 (8)	F16—C42—C37	118.8 (8)
C13—C18—H18	120.0	C41—C42—C37	123.6 (8)

C13—P1—C1—C2	97.8 (6)	Os1—S2—C25—C30	113.9 (7)
C7—P1—C1—C2	−10.9 (7)	C30—C25—C26—F5	179.4 (7)
Os1—P1—C1—C2	−136.1 (5)	S2—C25—C26—F5	7.7 (11)
C13—P1—C1—C6	−81.6 (6)	C30—C25—C26—C27	0.2 (13)
C7—P1—C1—C6	169.7 (6)	S2—C25—C26—C27	−171.6 (7)
Os1—P1—C1—C6	44.5 (6)	F5—C26—C27—F6	2.2 (13)
C6—C1—C2—C3	1.9 (11)	C25—C26—C27—F6	−178.5 (8)
P1—C1—C2—C3	−177.5 (6)	F5—C26—C27—C28	−178.0 (9)
C1—C2—C3—C4	−1.0 (12)	C25—C26—C27—C28	1.3 (16)
C2—C3—C4—C5	0.6 (11)	C26—C27—C28—C29	−2.0 (18)
C3—C4—C5—C6	−1.0 (11)	F6—C27—C28—C29	177.7 (10)
C4—C5—C6—C1	1.9 (11)	C27—C28—C29—F7	178.7 (10)
C2—C1—C6—C5	−2.3 (10)	C27—C28—C29—C30	1.4 (18)
P1—C1—C6—C5	177.1 (5)	C28—C29—C30—F8	179.6 (10)
C13—P1—C7—C12	179.8 (6)	F7—C29—C30—F8	2.3 (15)
C1—P1—C7—C12	−71.7 (6)	C28—C29—C30—C25	−0.1 (17)
Os1—P1—C7—C12	54.0 (6)	F7—C29—C30—C25	−177.4 (9)
C13—P1—C7—C8	−3.3 (7)	C26—C25—C30—F8	179.6 (7)
C1—P1—C7—C8	105.2 (7)	S2—C25—C30—F8	−8.2 (11)
Os1—P1—C7—C8	−129.1 (6)	C26—C25—C30—C29	−0.7 (14)
C12—C7—C8—C9	4.1 (12)	S2—C25—C30—C29	171.5 (8)
P1—C7—C8—C9	−173.0 (6)	Os1—S3—C31—C32	−119.9 (6)
C7—C8—C9—C10	−3.4 (13)	Os1—S3—C31—C36	73.1 (6)
C8—C9—C10—C11	1.0 (13)	C36—C31—C32—F9	178.4 (6)
C9—C10—C11—C12	0.6 (12)	S3—C31—C32—F9	10.9 (9)
C10—C11—C12—C7	0.2 (11)	C36—C31—C32—C33	−2.7 (11)
C8—C7—C12—C11	−2.5 (10)	S3—C31—C32—C33	−170.3 (6)
P1—C7—C12—C11	174.5 (6)	F9—C32—C33—F10	−1.0 (11)
C7—P1—C13—C14	−81.0 (6)	C31—C32—C33—F10	−179.8 (7)
C1—P1—C13—C14	171.8 (6)	F9—C32—C33—C34	−179.6 (7)
Os1—P1—C13—C14	45.0 (6)	C31—C32—C33—C34	1.6 (13)
C7—P1—C13—C18	99.8 (6)	F10—C33—C34—C35	−177.6 (8)
C1—P1—C13—C18	−7.3 (7)	C32—C33—C34—C35	0.9 (14)
Os1—P1—C13—C18	−134.2 (5)	C33—C34—C35—F11	−179.8 (8)
C18—C13—C14—C15	−2.6 (11)	C33—C34—C35—C36	−2.1 (15)
P1—C13—C14—C15	178.2 (6)	F11—C35—C36—F12	−4.2 (13)
C13—C14—C15—C16	2.0 (12)	C34—C35—C36—F12	178.0 (8)
C14—C15—C16—C17	−1.6 (12)	F11—C35—C36—C31	178.6 (7)
C15—C16—C17—C18	1.8 (12)	C34—C35—C36—C31	0.8 (14)
C14—C13—C18—C17	2.8 (11)	C32—C31—C36—F12	−175.7 (7)
P1—C13—C18—C17	−178.0 (6)	S3—C31—C36—F12	−8.0 (10)
C16—C17—C18—C13	−2.4 (12)	C32—C31—C36—C35	1.5 (11)
Os1—S1—C19—C20	−135.1 (6)	S3—C31—C36—C35	169.2 (7)
Os1—S1—C19—C24	47.4 (8)	Os1—S4—C37—C38	−91.8 (7)
C24—C19—C20—F1	−179.4 (8)	Os1—S4—C37—C42	93.2 (6)
S1—C19—C20—F1	2.9 (12)	C42—C37—C38—F13	177.7 (7)
C24—C19—C20—C21	3.1 (13)	S4—C37—C38—F13	2.4 (11)
S1—C19—C20—C21	−174.7 (8)	C42—C37—C38—C39	−4.3 (12)
C19—C20—C21—C22	−6 (2)	S4—C37—C38—C39	−179.6 (6)
F1—C20—C21—C22	176.6 (13)	F13—C38—C39—C40	−178.2 (8)
C19—C20—C21—F2	−178.6 (9)	C37—C38—C39—C40	3.8 (13)
F1—C20—C21—F2	3.8 (15)	F13—C38—C39—F14	1.8 (12)
F2—C21—C22—C23	−179.3 (9)	C37—C38—C39—F14	−176.2 (8)
C20—C21—C22—C23	8 (2)	F14—C39—C40—C41	178.5 (8)
C21—C22—C23—C24	−8 (2)	C38—C39—C40—C41	−1.5 (14)
C21—C22—C23—F3	178.3 (11)	C39—C40—C41—F15	179.2 (8)
C22—C23—C24—F4	−174.3 (10)	C39—C40—C41—C42	0.1 (13)
F3—C23—C24—F4	−0.6 (12)	F15—C41—C42—F16	−1.1 (12)
C22—C23—C24—C19	6.1 (15)	C40—C41—C42—F16	178.2 (8)
F3—C23—C24—C19	179.7 (8)	F15—C41—C42—C37	180.0 (7)
C20—C19—C24—F4	177.2 (7)	C40—C41—C42—C37	−0.8 (13)
S1—C19—C24—F4	−5.2 (11)	C38—C37—C42—F16	−176.1 (7)
C20—C19—C24—C23	−3.1 (12)	S4—C37—C42—F16	−0.6 (10)
S1—C19—C24—C23	174.5 (6)	C38—C37—C42—C41	2.9 (12)
Os1—S2—C25—C26	−74.5 (7)	S4—C37—C42—C41	178.4 (7)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12···S2	0.93	2.98	3.742 (8)	140
C14—H14···S4	0.93	2.96	3.725 (7)	140
C14—H14···F11ⁱ	0.93	2.55	3.223 (10)	129
C18—H18···F9ⁱⁱ	0.93	2.42	3.183 (10)	139
C34—H34···F15ⁱⁱⁱ	0.93	2.58	3.140 (11)	119

Symmetry codes: (i) −x, −y+2, −z+1; (ii) −x, −y+1, −z+1; (iii) x−1, y, z.

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Tetra­kis(2,3,5,6-tetra­fluoro­benzene­thiol­ato-κS)(tri­phenyl­phosphane-κP)osmium(IV): a monoclinic polymorph

Supporting information

Key indicators

checkCIF/PLATON results

Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphane-κP)osmium(IV): a monoclinic polymorph