Bis­[1,2-bis­(di­phenyl­phosphino)­ethane-P,P'](di­thio­formato-S,S')­technetium tris­(benzene) solvate

Two Tc-containing products were isolated from the reaction between CS₂ and the electron-deficient complex TcCl(dppe)₂. The title di­thio­formate complex, [Tc(S₂CH)(dppe)₂]·3C₆H₆, where dppe is 1,2-bis­(di­phenyl­phosphino)­ethane (C₂₆H₂₄P₂), exhibits Tc-P bond lengths ranging from 2.3566 (14) to 2.3884 (14) Å, which are little shorter than normally found. The other product is [TcCl(CS)(dppe)₂], and is the first reported Tc-thio­carbonyl complex.

Key indicators

• Single-crystal X-ray study
• T = 193 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.035
• wR factor = 0.104
• Data-to-parameter ratio = 13.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_302  Alert C Anion/Solvent disorder .......................      40.00 Perc.

PLAT_733  Alert C Torsion Calc    179.9(3), Rep    179.9(7) ....       2.33 s.u-Ratio
                     P3  -C50 -C51 -C52    1.555   1.555   1.555   1.555


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

S1. Comment

The title compound was prepared during an examination of the reactivity of the 16-electron complex [TcCl(dppe)₂], where dppe is 1,2-bis(diphenylphosphino)ethane (Burrell, et al., 1994). It is the first structural characterization of the dithioformate ligand on Tc. Only one other Tc–dithioformate complex, [Tc(S₂CH)(CO)₂(PPh₃)₂,] has been previously reported, but its structure was not determined (Cook et al., 1995).

The structure of the title compound is quite similar to isoelectronic, and isostructural [Fe(S₂CH)(depe)₂]⁺ (Bianchini, et al., 1982), and the closely related technetium(II) complexes [Tc(S₂CNMe₂)(depe)₂]⁺ (Okamoto, et al., 1993) and [Tc(S₂CNMe₂)(dppe)₂]⁺ (Rochon, et al., 1992). The Tc—P bond lengths range from 2.3566 (14) to 2.3884 (14) Å, which are little shorter than normally observed. A search of the Cambridge Structural Database (Allen & Kennard, 1993) indicates that most Tc—P bonds range from 2.39 to 2.50 Å, with a mean value of 2.44 Å.

S2. Experimental

[TcCl(dppe)₂] (100 mg) was added to a benzene (50 ml) solution containing CS₂ (0.2 ml) triphenylphosphine (50 mg). This mixture was heated to reflux for 2 min and then allowed to cool. Hexane was added to the solution and then the mixture was allowed to stand. Over time, a mixture of orange and yellow crystals were deposited. The orange crystals proved to be [Tc(S₂CH)(dppe)₂]·C₆H₆ (C₇₁H₆₇P₄S₂Tc).

S3. Refinement

Two of the benzene solvate molecules are disordered and each is modeled over two sites (68:32 and 73:27). The 1,1- and 1,3-distances, as well as the U^ij components of bonded or closely spaced disordered atoms are restrained to be similar. Despite the restraints, three atoms exhibit unusual elongation, and two of these (C118 and C120) are refined isotropically. All other non-H atoms are refined anisotropically. The dithioformate H atom (H5) was located in a difference map, and its coordinates were allowed to refine, with U_iso(H) equal to 1.5U_iso(C5). All other H atoms were placed in calculated positions, refined using a riding model, and given an isotropic displacement parameter equal to 1.2 times the equivalent isotropic displacement parameter of the atom to which they were attached.

Computing details

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms, 1993); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: PLATON (Spek, 2000).

Figures

Fig. 1. The molecular structure of the title compound showing 50% probability displacement ellipsoids. The benzene solvate molecules, and all H atoms, except H5 have been omitted for clarity.

(I)

Crystal data

[Tc(CHS2)(C26H24P2)2]·3C6H6	Z = 2
Mr = 1207.2	F(000) = 1256
Triclinic, P1	Dx = 1.35 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 14.132 (4) Å	Cell parameters from 25 reflections
b = 14.738 (6) Å	θ = 7.6–11.9°
c = 17.031 (4) Å	µ = 0.46 mm^−1
α = 65.79 (3)°	T = 193 K
β = 88.10 (3)°	Block, red–orange
γ = 67.88 (3)°	0.35 × 0.23 × 0.15 mm
V = 2966 (2) Å^3

Data collection

Nonius CAD-4 diffractometer	7752 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 25.0°, θmin = 2.2°
ω scans	h = 0→16
Absorption correction: ψ scan (SHELXTL-Plus; Siemens, 1990)	k = −16→17
Tmin = 0.854, Tmax = 0.934	l = −20→20
10893 measured reflections	3 standard reflections every 120 min
10431 independent reflections	intensity decay: 8%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.104	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0493P)^2 + 0.5423P] where P = (Fo^2 + 2Fc^2)/3
10431 reflections	(Δ/σ)max = 0.008
768 parameters	Δρmax = 0.56 e Å^−3
219 restraints	Δρmin = −0.43 e Å^−3
0 constraints

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F² for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The observed criterion of F² > σ(F²) is used only for calculating -R-factor-obs 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Tc	0.68692 (2)	0.67315 (2)	0.61216 (2)	0.0124 (1)
S1	0.69885 (7)	0.77850 (7)	0.69129 (5)	0.0187 (2)
S2	0.55321 (7)	0.85846 (7)	0.54825 (6)	0.0195 (2)
P1	0.59799 (7)	0.59135 (7)	0.72035 (5)	0.0152 (2)
P2	0.61640 (7)	0.60808 (7)	0.53325 (5)	0.0146 (2)
P3	0.84407 (6)	0.51919 (7)	0.66499 (5)	0.0138 (2)
P4	0.79020 (7)	0.74527 (7)	0.51157 (5)	0.0157 (2)
C1	0.5795 (3)	0.4860 (3)	0.6984 (2)	0.0184 (10)
C2	0.5363 (3)	0.5400 (3)	0.6021 (2)	0.0175 (10)
C3	0.9215 (3)	0.5270 (3)	0.5740 (2)	0.0178 (10)
C4	0.9228 (3)	0.6399 (3)	0.5326 (2)	0.0193 (10)
C5	0.6008 (3)	0.8864 (3)	0.6197 (2)	0.0211 (11)
C10	0.6493 (3)	0.5237 (3)	0.8367 (2)	0.0173 (10)
C11	0.7350 (3)	0.5332 (3)	0.8652 (2)	0.0207 (10)
C12	0.7744 (3)	0.4837 (3)	0.9526 (2)	0.0261 (11)
C13	0.7274 (3)	0.4250 (3)	1.0136 (2)	0.0302 (11)
C14	0.6414 (3)	0.4159 (3)	0.9870 (2)	0.0311 (12)
C15	0.6026 (3)	0.4647 (3)	0.8996 (2)	0.0247 (11)
C20	0.4656 (3)	0.6714 (3)	0.7318 (2)	0.0173 (10)
C21	0.4522 (3)	0.7593 (3)	0.7498 (2)	0.0246 (11)
C22	0.3571 (3)	0.8202 (3)	0.7651 (3)	0.0295 (12)
C23	0.2735 (3)	0.7935 (3)	0.7616 (2)	0.0298 (12)
C24	0.2846 (3)	0.7078 (3)	0.7427 (2)	0.0274 (11)
C25	0.3803 (3)	0.6466 (3)	0.7275 (2)	0.0227 (11)
C30	0.6933 (2)	0.5106 (3)	0.4903 (2)	0.0157 (9)
C31	0.6947 (3)	0.4075 (3)	0.5175 (2)	0.0210 (10)
C32	0.7518 (3)	0.3390 (3)	0.4801 (3)	0.0265 (11)
C33	0.8076 (3)	0.3730 (3)	0.4151 (3)	0.0305 (12)
C34	0.8089 (3)	0.4758 (3)	0.3870 (2)	0.0256 (11)
C35	0.7523 (3)	0.5434 (3)	0.4246 (2)	0.0206 (10)
C40	0.5145 (3)	0.7032 (3)	0.4366 (2)	0.0175 (10)
C41	0.5156 (3)	0.6958 (3)	0.3573 (2)	0.0201 (10)
C42	0.4376 (3)	0.7702 (3)	0.2885 (2)	0.0241 (11)
C43	0.3572 (3)	0.8552 (3)	0.2956 (2)	0.0282 (11)
C44	0.3554 (3)	0.8629 (3)	0.3746 (2)	0.0255 (11)
C45	0.4323 (3)	0.7872 (3)	0.4443 (2)	0.0196 (10)
C50	0.8583 (3)	0.3764 (3)	0.7085 (2)	0.0183 (10)
C51	0.8445 (3)	0.3242 (3)	0.7953 (2)	0.0241 (11)
C52	0.8546 (3)	0.2176 (3)	0.8293 (3)	0.0286 (11)
C53	0.8780 (3)	0.1607 (3)	0.7788 (3)	0.0287 (11)
C54	0.8928 (3)	0.2108 (3)	0.6935 (3)	0.0271 (11)
C55	0.8824 (3)	0.3183 (3)	0.6588 (2)	0.0216 (11)
C60	0.9481 (3)	0.4991 (3)	0.7430 (2)	0.0179 (10)
C61	0.9472 (3)	0.5847 (3)	0.7584 (2)	0.0232 (11)
C62	1.0301 (3)	0.5737 (3)	0.8085 (3)	0.0287 (12)
C63	1.1150 (3)	0.4762 (3)	0.8439 (2)	0.0298 (11)
C64	1.1172 (3)	0.3902 (3)	0.8296 (2)	0.0288 (11)
C65	1.0346 (3)	0.4006 (3)	0.7797 (2)	0.0235 (11)
C70	0.7575 (3)	0.8042 (3)	0.3924 (2)	0.0192 (10)
C71	0.6558 (3)	0.8479 (3)	0.3552 (2)	0.0297 (14)
C72	0.6300 (4)	0.8977 (4)	0.2650 (3)	0.0437 (16)
C73	0.7059 (4)	0.9041 (4)	0.2118 (3)	0.0455 (18)
C74	0.8070 (4)	0.8611 (3)	0.2487 (3)	0.0425 (14)
C75	0.8323 (4)	0.8129 (3)	0.3378 (3)	0.0362 (14)
C80	0.8167 (3)	0.8584 (3)	0.5141 (2)	0.0190 (10)
C81	0.7497 (3)	0.9648 (3)	0.4639 (2)	0.0236 (11)
C82	0.7672 (3)	1.0513 (3)	0.4633 (3)	0.0325 (13)
C83	0.8534 (3)	1.0330 (3)	0.5135 (3)	0.0339 (14)
C84	0.9192 (3)	0.9276 (3)	0.5653 (3)	0.0322 (12)
C85	0.9014 (3)	0.8411 (3)	0.5670 (2)	0.0247 (11)
C90	0.2282 (3)	0.8795 (3)	0.9528 (3)	0.0340 (14)
C91	0.3118 (3)	0.8622 (3)	1.0053 (3)	0.0329 (12)
C92	0.3021 (3)	0.9316 (3)	1.0433 (3)	0.0353 (12)
C93	0.2087 (3)	1.0187 (3)	1.0286 (3)	0.0352 (14)
C94	0.1267 (3)	1.0348 (3)	0.9771 (3)	0.0344 (12)
C95	0.1359 (3)	0.9650 (3)	0.9393 (3)	0.0329 (12)
C100	0.8798 (13)	0.7290 (17)	0.9410 (8)	0.036 (3)	0.680
C101	0.9752 (16)	0.726 (2)	0.9628 (9)	0.051 (5)	0.680
C102	1.0166 (14)	0.791 (2)	0.9018 (11)	0.044 (6)	0.680
C103	0.9663 (11)	0.8543 (15)	0.8176 (9)	0.041 (4)	0.680
C104	0.8750 (8)	0.8552 (7)	0.7944 (6)	0.028 (3)	0.680
C105	0.8296 (7)	0.7921 (9)	0.8575 (6)	0.035 (3)	0.680
C112	0.41759 (16)	0.2985 (3)	1.0245 (2)	0.042 (2)	0.730
C113	0.39980 (16)	0.3366 (3)	0.9348 (2)	0.042 (2)	0.730
C114	0.39480 (16)	0.2689 (3)	0.8989 (2)	0.061 (3)	0.730
C115	0.40758 (16)	0.1631 (3)	0.9528 (2)	0.046 (3)	0.730
C116	0.42537 (16)	0.1250 (3)	1.0426 (2)	0.058 (3)	0.730
C117	0.43037 (16)	0.1927 (3)	1.0784 (2)	0.040 (2)	0.730
C106	0.869 (3)	0.745 (4)	0.9174 (15)	0.055 (10)	0.320
C107	0.960 (3)	0.722 (4)	0.9661 (18)	0.038 (7)	0.320
C108	1.021 (3)	0.777 (3)	0.924 (2)	0.030 (6)	0.320
C109	0.991 (2)	0.854 (3)	0.8382 (17)	0.029 (6)	0.320
C110	0.9012 (19)	0.881 (2)	0.7926 (12)	0.043 (7)	0.320
C111	0.84101 (16)	0.8187 (3)	0.8353 (2)	0.040 (7)	0.320
C118	0.40322 (16)	0.3277 (3)	0.9738 (2)	0.045 (6)*	0.270
C119	0.39618 (16)	0.3167 (3)	0.8909 (2)	0.061 (9)	0.270
C120	0.39773 (16)	0.2207 (3)	0.8978 (2)	0.039 (5)*	0.270
C121	0.40643 (16)	0.1401 (3)	0.9838 (2)	0.055 (6)	0.270
C122	0.41054 (16)	0.1490 (3)	1.0512 (2)	0.078 (9)	0.270
C123	0.41992 (16)	0.2676 (3)	1.0440 (2)	0.067 (8)	0.270
H1A	0.64600	0.42330	0.71110	0.0220*
H1B	0.53050	0.46050	0.73470	0.0220*
H2A	0.46490	0.59410	0.59250	0.0210*
H2B	0.53390	0.48450	0.58450	0.0210*
H3A	0.99270	0.47110	0.59600	0.0210*
H3B	0.89040	0.51410	0.53040	0.0210*
H4A	0.95160	0.65130	0.47730	0.0230*
H4B	0.96760	0.64600	0.57200	0.0230*
H5	0.575 (3)	0.953 (3)	0.620 (2)	0.0320*
H11	0.76690	0.57430	0.82380	0.0250*
H12	0.83360	0.49000	0.97070	0.0310*
H13	0.75430	0.39110	1.07360	0.0360*
H14	0.60890	0.37610	1.02880	0.0370*
H15	0.54340	0.45800	0.88190	0.0300*
H21	0.50920	0.77810	0.75160	0.0290*
H22	0.34950	0.87940	0.77780	0.0360*
H23	0.20840	0.83430	0.77240	0.0360*
H24	0.22700	0.69030	0.73990	0.0330*
H25	0.38730	0.58800	0.71420	0.0270*
H31	0.65620	0.38310	0.56230	0.0250*
H32	0.75200	0.26860	0.49980	0.0320*
H33	0.84530	0.32670	0.38920	0.0360*
H34	0.84810	0.49930	0.34260	0.0310*
H35	0.75350	0.61320	0.40550	0.0250*
H41	0.57060	0.63890	0.35060	0.0240*
H42	0.43920	0.76290	0.23550	0.0290*
H43	0.30450	0.90710	0.24780	0.0340*
H44	0.30080	0.92060	0.38070	0.0310*
H45	0.42890	0.79270	0.49810	0.0240*
H51	0.82820	0.36230	0.83070	0.0290*
H52	0.84540	0.18300	0.88810	0.0350*
H53	0.88380	0.08780	0.80250	0.0340*
H54	0.90990	0.17200	0.65860	0.0330*
H55	0.89210	0.35240	0.60000	0.0260*
H61	0.88910	0.65200	0.73440	0.0280*
H62	1.02830	0.63320	0.81840	0.0340*
H63	1.17170	0.46850	0.87810	0.0360*
H64	1.17560	0.32320	0.85400	0.0340*
H65	1.03680	0.34060	0.77050	0.0280*
H71	0.60340	0.84390	0.39120	0.0360*
H72	0.56000	0.92740	0.23980	0.0520*
H73	0.68820	0.93790	0.15030	0.0550*
H74	0.85960	0.86460	0.21270	0.0510*
H75	0.90220	0.78490	0.36260	0.0430*
H81	0.69040	0.97850	0.42900	0.0290*
H82	0.71990	1.12350	0.42840	0.0390*
H83	0.86700	1.09200	0.51210	0.0400*
H84	0.97790	0.91430	0.60060	0.0380*
H85	0.94690	0.76920	0.60420	0.0300*
H90	0.23460	0.83240	0.92620	0.0410*
H91	0.37570	0.80280	1.01530	0.0400*
H92	0.35930	0.91970	1.07940	0.0420*
H93	0.20220	1.06670	1.05430	0.0420*
H94	0.06270	1.09410	0.96710	0.0410*
H95	0.07820	0.97650	0.90390	0.0400*
H100	0.84970	0.68710	0.98390	0.0430*	0.680
H101	1.01170	0.68020	1.01990	0.0610*	0.680
H102	1.08010	0.79120	0.91770	0.0540*	0.680
H103	0.99590	0.89770	0.77560	0.0490*	0.680
H104	0.84140	0.89800	0.73610	0.0340*	0.680
H105	0.76490	0.79360	0.84200	0.0410*	0.680
H112	0.42100	0.34490	1.04910	0.0500*	0.730
H113	0.39110	0.40890	0.89790	0.0500*	0.730
H114	0.38260	0.29490	0.83750	0.0730*	0.730
H115	0.40420	0.11670	0.92830	0.0550*	0.730
H116	0.43410	0.05270	1.07940	0.0700*	0.730
H117	0.44250	0.16670	1.13980	0.0480*	0.730
H106	0.82640	0.70740	0.94380	0.0670*	0.320
H107	0.97890	0.67150	1.02550	0.0470*	0.320
H108	1.08390	0.76200	0.95390	0.0350*	0.320
H109	1.03550	0.88850	0.81070	0.0350*	0.320
H110	0.87850	0.93710	0.73530	0.0520*	0.320
H111	0.77980	0.83100	0.80380	0.0480*	0.320
H118	0.39130	0.39910	0.96550	0.0540*	0.270
H119	0.39090	0.37400	0.83600	0.0740*	0.270
H120	0.39320	0.20790	0.84800	0.0460*	0.270
H121	0.40930	0.07260	0.98860	0.0660*	0.270
H122	0.40880	0.09440	1.10530	0.0940*	0.270
H123	0.43650	0.27910	1.09190	0.0810*	0.270

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tc	0.0114 (1)	0.0122 (1)	0.0133 (1)	−0.0046 (1)	0.0016 (1)	−0.0054 (1)
S1	0.0178 (4)	0.0192 (4)	0.0209 (4)	−0.0064 (4)	0.0014 (3)	−0.0111 (4)
S2	0.0172 (4)	0.0149 (4)	0.0226 (4)	−0.0030 (4)	−0.0020 (3)	−0.0073 (3)
P1	0.0149 (4)	0.0156 (4)	0.0155 (4)	−0.0064 (4)	0.0038 (3)	−0.0069 (3)
P2	0.0134 (4)	0.0156 (4)	0.0158 (4)	−0.0063 (4)	0.0025 (3)	−0.0073 (3)
P3	0.0116 (4)	0.0137 (4)	0.0156 (4)	−0.0046 (3)	0.0024 (3)	−0.0062 (3)
P4	0.0160 (4)	0.0142 (4)	0.0163 (4)	−0.0064 (4)	0.0041 (3)	−0.0057 (3)
C1	0.0201 (18)	0.0171 (17)	0.0187 (17)	−0.0089 (15)	0.0067 (14)	−0.0073 (14)
C2	0.0145 (17)	0.0205 (17)	0.0214 (18)	−0.0094 (15)	0.0030 (14)	−0.0104 (15)
C3	0.0191 (18)	0.0151 (17)	0.0190 (17)	−0.0061 (14)	0.0045 (14)	−0.0078 (14)
C4	0.0154 (17)	0.0160 (17)	0.0259 (19)	−0.0079 (15)	0.0062 (14)	−0.0073 (15)
C5	0.0235 (19)	0.0168 (17)	0.0249 (19)	−0.0084 (16)	0.0075 (15)	−0.0106 (15)
C10	0.0164 (17)	0.0151 (16)	0.0158 (17)	−0.0022 (14)	0.0044 (14)	−0.0062 (14)
C11	0.0185 (18)	0.0225 (18)	0.0176 (17)	−0.0044 (15)	0.0033 (14)	−0.0089 (15)
C12	0.0210 (19)	0.029 (2)	0.025 (2)	−0.0046 (17)	−0.0008 (16)	−0.0130 (17)
C13	0.038 (2)	0.0239 (19)	0.0160 (18)	−0.0017 (18)	−0.0011 (17)	−0.0062 (15)
C14	0.040 (2)	0.026 (2)	0.023 (2)	−0.0142 (19)	0.0094 (18)	−0.0061 (16)
C15	0.024 (2)	0.0241 (19)	0.0234 (19)	−0.0107 (16)	0.0025 (15)	−0.0066 (15)
C20	0.0166 (17)	0.0185 (17)	0.0137 (16)	−0.0074 (14)	0.0032 (13)	−0.0037 (14)
C21	0.022 (2)	0.0261 (19)	0.026 (2)	−0.0104 (16)	0.0071 (16)	−0.0110 (16)
C22	0.030 (2)	0.028 (2)	0.033 (2)	−0.0084 (18)	0.0103 (17)	−0.0187 (18)
C23	0.020 (2)	0.039 (2)	0.027 (2)	−0.0056 (18)	0.0099 (16)	−0.0171 (18)
C24	0.0159 (19)	0.041 (2)	0.025 (2)	−0.0112 (17)	0.0054 (15)	−0.0143 (18)
C25	0.0199 (19)	0.029 (2)	0.0216 (18)	−0.0119 (16)	0.0042 (15)	−0.0112 (16)
C30	0.0110 (16)	0.0205 (17)	0.0164 (16)	−0.0058 (14)	−0.0005 (13)	−0.0089 (14)
C31	0.0125 (17)	0.0228 (18)	0.0274 (19)	−0.0057 (15)	−0.0003 (14)	−0.0115 (16)
C32	0.0181 (19)	0.026 (2)	0.044 (2)	−0.0109 (16)	0.0026 (17)	−0.0210 (18)
C33	0.021 (2)	0.040 (2)	0.044 (2)	−0.0071 (18)	0.0057 (17)	−0.035 (2)
C34	0.0176 (19)	0.042 (2)	0.0251 (19)	−0.0141 (17)	0.0058 (15)	−0.0198 (18)
C35	0.0194 (18)	0.0251 (18)	0.0217 (18)	−0.0112 (16)	0.0035 (14)	−0.0121 (15)
C40	0.0176 (18)	0.0186 (17)	0.0185 (17)	−0.0100 (15)	0.0019 (14)	−0.0074 (14)
C41	0.0170 (18)	0.0227 (18)	0.0215 (18)	−0.0089 (15)	0.0019 (14)	−0.0094 (15)
C42	0.027 (2)	0.029 (2)	0.0159 (18)	−0.0113 (17)	−0.0003 (15)	−0.0088 (15)
C43	0.023 (2)	0.029 (2)	0.0238 (19)	−0.0067 (17)	−0.0063 (16)	−0.0059 (16)
C44	0.0162 (18)	0.0232 (19)	0.033 (2)	−0.0027 (16)	0.0018 (16)	−0.0128 (16)
C45	0.0136 (17)	0.0225 (18)	0.0248 (18)	−0.0067 (15)	0.0054 (14)	−0.0127 (15)
C50	0.0128 (16)	0.0151 (16)	0.0244 (18)	−0.0047 (14)	0.0019 (14)	−0.0068 (14)
C51	0.0204 (19)	0.0177 (18)	0.029 (2)	−0.0034 (15)	0.0064 (16)	−0.0092 (16)
C52	0.026 (2)	0.0224 (19)	0.027 (2)	−0.0091 (17)	0.0064 (16)	−0.0016 (16)
C53	0.024 (2)	0.0163 (18)	0.038 (2)	−0.0094 (16)	−0.0007 (17)	−0.0029 (16)
C54	0.024 (2)	0.0216 (19)	0.037 (2)	−0.0076 (16)	0.0006 (17)	−0.0147 (17)
C55	0.0192 (18)	0.0188 (18)	0.0234 (19)	−0.0066 (15)	0.0012 (15)	−0.0066 (15)
C60	0.0144 (17)	0.0251 (18)	0.0146 (16)	−0.0080 (15)	0.0039 (13)	−0.0089 (14)
C61	0.0156 (18)	0.0251 (19)	0.029 (2)	−0.0054 (16)	0.0028 (15)	−0.0142 (16)
C62	0.027 (2)	0.033 (2)	0.035 (2)	−0.0142 (18)	0.0046 (17)	−0.0207 (18)
C63	0.0170 (19)	0.042 (2)	0.031 (2)	−0.0092 (18)	−0.0015 (16)	−0.0183 (19)
C64	0.0174 (19)	0.029 (2)	0.030 (2)	−0.0017 (16)	−0.0052 (16)	−0.0097 (17)
C65	0.0212 (19)	0.0232 (19)	0.0228 (19)	−0.0052 (16)	0.0024 (15)	−0.0100 (15)
C70	0.030 (2)	0.0161 (17)	0.0119 (16)	−0.0119 (16)	0.0046 (14)	−0.0041 (13)
C71	0.045 (3)	0.030 (2)	0.0207 (19)	−0.028 (2)	0.0039 (17)	−0.0051 (16)
C72	0.062 (3)	0.045 (3)	0.029 (2)	−0.039 (2)	−0.012 (2)	−0.003 (2)
C73	0.097 (4)	0.039 (3)	0.0137 (19)	−0.044 (3)	0.009 (2)	−0.0083 (18)
C74	0.066 (3)	0.035 (2)	0.023 (2)	−0.020 (2)	0.020 (2)	−0.0103 (19)
C75	0.042 (3)	0.027 (2)	0.027 (2)	−0.0082 (19)	0.0136 (19)	−0.0055 (17)
C80	0.0208 (18)	0.0178 (17)	0.0206 (18)	−0.0106 (15)	0.0102 (14)	−0.0083 (14)
C81	0.025 (2)	0.0208 (18)	0.0241 (19)	−0.0075 (16)	0.0043 (15)	−0.0104 (15)
C82	0.047 (3)	0.0167 (18)	0.032 (2)	−0.0125 (18)	0.0188 (19)	−0.0100 (17)
C83	0.039 (2)	0.033 (2)	0.049 (3)	−0.025 (2)	0.025 (2)	−0.027 (2)
C84	0.032 (2)	0.037 (2)	0.045 (2)	−0.023 (2)	0.0142 (19)	−0.026 (2)
C85	0.0205 (19)	0.0251 (19)	0.032 (2)	−0.0129 (16)	0.0049 (16)	−0.0120 (16)
C90	0.045 (3)	0.032 (2)	0.036 (2)	−0.021 (2)	0.017 (2)	−0.0203 (19)
C91	0.021 (2)	0.031 (2)	0.044 (2)	−0.0102 (18)	0.0123 (18)	−0.0143 (19)
C92	0.030 (2)	0.039 (2)	0.035 (2)	−0.019 (2)	0.0000 (18)	−0.0091 (19)
C93	0.048 (3)	0.030 (2)	0.035 (2)	−0.021 (2)	0.011 (2)	−0.0162 (19)
C94	0.032 (2)	0.024 (2)	0.035 (2)	−0.0074 (18)	0.0086 (19)	−0.0050 (18)
C95	0.031 (2)	0.036 (2)	0.027 (2)	−0.017 (2)	0.0023 (17)	−0.0058 (18)
C100	0.044 (6)	0.038 (6)	0.028 (4)	−0.012 (5)	0.003 (4)	−0.020 (4)
C101	0.045 (10)	0.049 (8)	0.051 (7)	−0.001 (7)	−0.013 (7)	−0.028 (7)
C102	0.021 (5)	0.059 (12)	0.066 (12)	−0.011 (6)	−0.006 (6)	−0.042 (9)
C103	0.023 (7)	0.040 (5)	0.067 (9)	−0.013 (6)	0.004 (6)	−0.030 (6)
C104	0.021 (5)	0.034 (5)	0.031 (4)	−0.011 (3)	0.004 (3)	−0.015 (3)
C105	0.029 (4)	0.057 (5)	0.031 (4)	−0.025 (4)	0.010 (3)	−0.024 (4)
C112	0.026 (4)	0.037 (3)	0.058 (5)	−0.005 (3)	0.007 (3)	−0.024 (3)
C113	0.017 (3)	0.062 (4)	0.043 (4)	−0.013 (3)	0.003 (3)	−0.021 (3)
C114	0.024 (4)	0.101 (7)	0.076 (5)	−0.018 (4)	0.008 (4)	−0.061 (4)
C115	0.034 (4)	0.059 (4)	0.060 (5)	−0.017 (4)	0.006 (3)	−0.042 (4)
C116	0.048 (5)	0.061 (5)	0.085 (6)	−0.024 (4)	0.005 (5)	−0.048 (5)
C117	0.034 (4)	0.049 (4)	0.057 (4)	−0.026 (3)	0.015 (3)	−0.033 (3)
C106	0.056 (15)	0.057 (19)	0.08 (2)	−0.036 (15)	0.012 (15)	−0.042 (16)
C107	0.020 (11)	0.033 (13)	0.048 (12)	−0.001 (9)	0.020 (7)	−0.014 (11)
C108	0.030 (10)	0.011 (8)	0.032 (11)	0.002 (7)	−0.003 (8)	−0.003 (9)
C109	0.019 (12)	0.032 (9)	0.031 (10)	−0.006 (9)	0.002 (9)	−0.012 (8)
C110	0.040 (15)	0.058 (14)	0.045 (9)	−0.018 (10)	−0.001 (9)	−0.037 (8)
C111	0.026 (9)	0.068 (15)	0.058 (13)	−0.019 (8)	0.014 (8)	−0.058 (12)
C119	0.028 (11)	0.091 (17)	0.103 (18)	−0.018 (10)	0.008 (11)	−0.082 (15)
C121	0.058 (14)	0.042 (10)	0.026 (9)	−0.006 (10)	0.015 (9)	0.009 (8)
C122	0.063 (18)	0.110 (16)	0.048 (12)	−0.028 (15)	0.022 (13)	−0.028 (14)
C123	0.048 (16)	0.085 (15)	0.047 (12)	−0.009 (12)	0.026 (11)	−0.025 (12)

Geometric parameters (Å, º)

Tc—S1	2.4866 (14)	C32—H32	0.9494
Tc—S2	2.4548 (15)	C33—H33	0.9495
Tc—P1	2.3650 (14)	C34—H34	0.9490
Tc—P2	2.3632 (14)	C35—H35	0.9501
Tc—P3	2.3566 (14)	C41—H41	0.9498
Tc—P4	2.3884 (14)	C42—H42	0.9504
S1—C5	1.673 (4)	C43—H43	0.9502
S2—C5	1.666 (4)	C44—H44	0.9499
P1—C1	1.846 (5)	C45—H45	0.9505
P1—C10	1.838 (3)	C51—H51	0.9502
P1—C20	1.853 (5)	C52—H52	0.9499
P2—C2	1.862 (4)	C53—H53	0.9509
P2—C30	1.848 (4)	C54—H54	0.9507
P2—C40	1.869 (4)	C55—H55	0.9509
P3—C3	1.857 (4)	C61—H61	0.9495
P3—C50	1.852 (4)	C62—H62	0.9499
P3—C60	1.869 (4)	C63—H63	0.9500
P4—C4	1.857 (5)	C64—H64	0.9494
P4—C70	1.844 (3)	C65—H65	0.9487
P4—C80	1.858 (5)	C71—H71	0.9491
C1—C2	1.525 (5)	C72—H72	0.9499
C3—C4	1.525 (6)	C73—H73	0.9505
C10—C11	1.394 (6)	C74—H74	0.9507
C10—C15	1.400 (6)	C75—H75	0.9498
C11—C12	1.384 (5)	C81—H81	0.9505
C12—C13	1.385 (6)	C82—H82	0.9510
C13—C14	1.382 (6)	C83—H83	0.9498
C14—C15	1.383 (5)	C84—H84	0.9497
C20—C21	1.395 (6)	C85—H85	0.9492
C20—C25	1.397 (6)	C90—C91	1.384 (7)
C21—C22	1.393 (6)	C90—C95	1.374 (7)
C22—C23	1.389 (6)	C91—C92	1.384 (7)
C23—C24	1.380 (6)	C92—C93	1.391 (7)
C24—C25	1.400 (6)	C93—C94	1.363 (7)
C30—C31	1.387 (6)	C94—C95	1.388 (7)
C30—C35	1.407 (5)	C90—H90	0.9504
C31—C32	1.399 (6)	C91—H91	0.9505
C32—C33	1.372 (7)	C92—H92	0.9487
C33—C34	1.397 (6)	C93—H93	0.9502
C34—C35	1.390 (6)	C94—H94	0.9506
C40—C41	1.398 (5)	C95—H95	0.9496
C40—C45	1.393 (6)	C100—C101	1.39 (3)
C41—C42	1.383 (5)	C100—C105	1.370 (17)
C42—C43	1.385 (6)	C101—C102	1.38 (3)
C43—C44	1.394 (5)	C102—C103	1.38 (2)
C44—C45	1.386 (5)	C103—C104	1.36 (2)
C50—C51	1.406 (5)	C104—C105	1.420 (15)
C50—C55	1.386 (6)	C100—H100	0.9504
C51—C52	1.384 (6)	C101—H101	0.9487
C52—C53	1.384 (7)	C102—H102	0.9473
C53—C54	1.384 (7)	C103—H103	0.9498
C54—C55	1.394 (6)	C104—H104	0.9493
C60—C61	1.385 (6)	C105—H105	0.9498
C60—C65	1.401 (6)	C112—C113	1.388 (4)
C61—C62	1.392 (6)	C112—C117	1.390 (5)
C62—C63	1.381 (6)	C113—C114	1.389 (6)
C63—C64	1.375 (6)	C114—C115	1.390 (5)
C64—C65	1.390 (6)	C115—C116	1.390 (4)
C70—C71	1.382 (6)	C116—C117	1.388 (6)
C70—C75	1.392 (7)	C112—H112	0.9522
C71—C72	1.394 (6)	C113—H113	0.9501
C72—C73	1.386 (8)	C114—H114	0.9506
C73—C74	1.374 (8)	C115—H115	0.9508
C74—C75	1.377 (7)	C116—H116	0.9496
C80—C81	1.387 (6)	C117—H117	0.9505
C80—C85	1.401 (6)	C106—C107	1.40 (6)
C81—C82	1.383 (6)	C106—C111	1.33 (3)
C82—C83	1.386 (6)	C107—C108	1.39 (6)
C83—C84	1.378 (7)	C108—C109	1.39 (4)
C84—C85	1.378 (6)	C109—C110	1.34 (4)
C1—H1A	0.9897	C110—C111	1.45 (3)
C1—H1B	0.9899	C106—H106	0.9490
C2—H2A	0.9893	C107—H107	0.9484
C2—H2B	0.9913	C108—H108	0.9424
C3—H3A	0.9895	C109—H109	0.9483
C3—H3B	0.9905	C110—H110	0.9477
C4—H4A	0.9885	C111—H111	0.9497
C4—H4B	0.9898	C118—C119	1.496 (5)
C5—H5	0.91 (4)	C118—C123	1.124 (5)
C11—H11	0.9495	C119—C120	1.363 (6)
C12—H12	0.9501	C120—C121	1.431 (5)
C13—H13	0.9499	C121—C122	1.213 (5)
C14—H14	0.9490	C122—C123	1.757 (6)
C15—H15	0.9507	C118—H118	0.9496
C21—H21	0.9504	C119—H119	0.9500
C22—H22	0.9499	C120—H120	0.9502
C23—H23	0.9511	C121—H121	0.9493
C24—H24	0.9498	C122—H122	0.9499
C25—H25	0.9495	C123—H123	0.9514
C31—H31	0.9499
S1—Tc—S2	68.38 (4)	C24—C25—H25	119.90
S1—Tc—P1	89.52 (4)	C30—C31—H31	119.36
S1—Tc—P2	160.79 (5)	C32—C31—H31	119.52
S1—Tc—P3	103.41 (5)	C31—C32—H32	119.84
S1—Tc—P4	89.41 (4)	C33—C32—H32	119.83
S2—Tc—P1	98.18 (5)	C32—C33—H33	120.05
S2—Tc—P2	95.66 (5)	C34—C33—H33	119.98
S2—Tc—P3	165.10 (5)	C33—C34—H34	120.28
S2—Tc—P4	85.93 (5)	C35—C34—H34	120.28
P1—Tc—P2	82.05 (4)	C30—C35—H35	119.36
P1—Tc—P3	94.05 (4)	C34—C35—H35	119.28
P1—Tc—P4	175.03 (5)	C40—C41—H41	119.58
P2—Tc—P3	94.42 (5)	C42—C41—H41	119.56
P2—Tc—P4	100.39 (4)	C41—C42—H42	119.48
P3—Tc—P4	81.48 (4)	C43—C42—H42	119.48
Tc—S1—C5	88.86 (15)	C42—C43—H43	120.85
Tc—S2—C5	90.09 (15)	C44—C43—H43	120.73
Tc—P1—C1	108.38 (12)	C43—C44—H44	119.60
Tc—P1—C10	122.16 (15)	C45—C44—H44	119.68
Tc—P1—C20	120.93 (13)	C40—C45—H45	119.53
C1—P1—C10	104.39 (18)	C44—C45—H45	119.55
C1—P1—C20	102.2 (2)	C50—C51—H51	119.84
C10—P1—C20	96.09 (18)	C52—C51—H51	119.94
Tc—P2—C2	108.60 (12)	C51—C52—H52	119.54
Tc—P2—C30	124.61 (12)	C53—C52—H52	119.57
Tc—P2—C40	121.23 (15)	C52—C53—H53	120.27
C2—P2—C30	102.85 (18)	C54—C53—H53	120.26
C2—P2—C40	96.65 (18)	C53—C54—H54	120.05
C30—P2—C40	98.28 (17)	C55—C54—H54	120.06
Tc—P3—C3	107.82 (13)	C50—C55—H55	119.36
Tc—P3—C50	125.77 (15)	C54—C55—H55	119.44
Tc—P3—C60	123.40 (15)	C60—C61—H61	119.51
C3—P3—C50	100.72 (19)	C62—C61—H61	119.40
C3—P3—C60	95.27 (18)	C61—C62—H62	120.04
C50—P3—C60	97.90 (18)	C63—C62—H62	119.98
Tc—P4—C4	110.12 (13)	C62—C63—H63	120.14
Tc—P4—C70	123.82 (15)	C64—C63—H63	120.06
Tc—P4—C80	118.82 (13)	C63—C64—H64	119.72
C4—P4—C70	102.99 (18)	C65—C64—H64	119.77
C4—P4—C80	101.5 (2)	C60—C65—H65	119.81
C70—P4—C80	96.34 (17)	C64—C65—H65	119.79
P1—C1—C2	105.7 (3)	C70—C71—H71	119.89
P2—C2—C1	111.6 (3)	C72—C71—H71	119.92
P3—C3—C4	108.0 (3)	C71—C72—H72	119.82
P4—C4—C3	110.4 (3)	C73—C72—H72	119.78
S1—C5—S2	112.5 (3)	C72—C73—H73	120.29
P1—C10—C11	120.2 (3)	C74—C73—H73	120.24
P1—C10—C15	121.9 (3)	C73—C74—H74	120.01
C11—C10—C15	117.8 (3)	C75—C74—H74	119.89
C10—C11—C12	121.2 (4)	C70—C75—H75	119.24
C11—C12—C13	119.9 (4)	C74—C75—H75	119.42
C12—C13—C14	119.9 (3)	C80—C81—H81	119.10
C13—C14—C15	120.1 (4)	C82—C81—H81	119.30
C10—C15—C14	121.0 (4)	C81—C82—H82	119.90
P1—C20—C21	117.1 (3)	C83—C82—H82	119.94
P1—C20—C25	124.4 (3)	C82—C83—H83	120.63
C21—C20—C25	118.4 (4)	C84—C83—H83	120.61
C20—C21—C22	121.4 (4)	C83—C84—H84	119.34
C21—C22—C23	119.3 (4)	C85—C84—H84	119.36
C22—C23—C24	120.2 (4)	C80—C85—H85	119.65
C23—C24—C25	120.3 (4)	C84—C85—H85	119.82
C20—C25—C24	120.3 (4)	C91—C90—C95	119.8 (4)
P2—C30—C31	124.0 (3)	C90—C91—C92	119.8 (4)
P2—C30—C35	118.3 (3)	C91—C92—C93	120.1 (4)
C31—C30—C35	117.8 (4)	C92—C93—C94	119.6 (4)
C30—C31—C32	121.1 (4)	C93—C94—C95	120.4 (4)
C31—C32—C33	120.3 (4)	C90—C95—C94	120.2 (4)
C32—C33—C34	120.0 (4)	C91—C90—H90	120.16
C33—C34—C35	119.4 (4)	C95—C90—H90	120.09
C30—C35—C34	121.4 (4)	C90—C91—H91	120.15
P2—C40—C41	124.4 (3)	C92—C91—H91	120.03
P2—C40—C45	117.6 (3)	C91—C92—H92	119.88
C41—C40—C45	118.0 (3)	C93—C92—H92	120.01
C40—C41—C42	120.9 (4)	C92—C93—H93	120.11
C41—C42—C43	121.0 (3)	C94—C93—H93	120.25
C42—C43—C44	118.4 (3)	C93—C94—H94	119.83
C43—C44—C45	120.7 (4)	C95—C94—H94	119.72
C40—C45—C44	120.9 (3)	C90—C95—H95	119.91
P3—C50—C51	119.1 (3)	C94—C95—H95	119.86
P3—C50—C55	122.6 (3)	C101—C100—C105	119.8 (15)
C51—C50—C55	118.3 (4)	C100—C101—C102	120.1 (16)
C50—C51—C52	120.2 (4)	C101—C102—C103	120 (2)
C51—C52—C53	120.9 (4)	C102—C103—C104	120.6 (16)
C52—C53—C54	119.5 (4)	C103—C104—C105	119.9 (10)
C53—C54—C55	119.9 (4)	C100—C105—C104	119.5 (12)
C50—C55—C54	121.2 (3)	C101—C100—H100	120.03
P3—C60—C61	120.7 (3)	C105—C100—H100	120.15
P3—C60—C65	120.7 (3)	C100—C101—H101	120.26
C61—C60—C65	118.2 (4)	C102—C101—H101	119.62
C60—C61—C62	121.1 (4)	C101—C102—H102	119.83
C61—C62—C63	120.0 (4)	C103—C102—H102	120.14
C62—C63—C64	119.8 (4)	C102—C103—H103	119.64
C63—C64—C65	120.5 (4)	C104—C103—H103	119.79
C60—C65—C64	120.4 (4)	C103—C104—H104	120.11
P4—C70—C71	119.9 (3)	C105—C104—H104	120.02
P4—C70—C75	121.4 (3)	C100—C105—H105	120.20
C71—C70—C75	118.5 (3)	C104—C105—H105	120.32
C70—C71—C72	120.2 (4)	C113—C112—C117	120.0 (4)
C71—C72—C73	120.4 (5)	C112—C113—C114	120.0 (4)
C72—C73—C74	119.5 (4)	C113—C114—C115	120.0 (3)
C73—C74—C75	120.1 (5)	C114—C115—C116	120.0 (4)
C70—C75—C74	121.3 (5)	C115—C116—C117	120.0 (4)
P4—C80—C81	119.8 (3)	C112—C117—C116	120.0 (3)
P4—C80—C85	122.6 (3)	C113—C112—H112	119.98
C81—C80—C85	117.6 (4)	C117—C112—H112	119.98
C80—C81—C82	121.6 (4)	C112—C113—H113	120.10
C81—C82—C83	120.2 (4)	C114—C113—H113	119.92
C82—C83—C84	118.8 (4)	C113—C114—H114	120.06
C83—C84—C85	121.3 (4)	C115—C114—H114	119.97
C80—C85—C84	120.5 (4)	C114—C115—H115	120.05
P1—C1—H1A	110.52	C116—C115—H115	119.93
P1—C1—H1B	110.58	C115—C116—H116	119.99
C2—C1—H1A	110.69	C117—C116—H116	120.06
C2—C1—H1B	110.62	C112—C117—H117	119.99
H1A—C1—H1B	108.76	C116—C117—H117	119.99
P2—C2—H2A	109.32	C107—C106—C111	121 (4)
P2—C2—H2B	109.27	C106—C107—C108	117 (3)
C1—C2—H2A	109.42	C107—C108—C109	121 (4)
C1—C2—H2B	109.29	C108—C109—C110	122 (3)
H2A—C2—H2B	107.89	C109—C110—C111	116 (2)
P3—C3—H3A	110.15	C106—C111—C110	122 (2)
P3—C3—H3B	110.09	C107—C106—H106	119.38
C4—C3—H3A	110.20	C111—C106—H106	119.31
C4—C3—H3B	110.11	C106—C107—H107	121.59
H3A—C3—H3B	108.32	C108—C107—H107	121.18
P4—C4—H4A	109.60	C107—C108—H108	119.79
P4—C4—H4B	109.56	C109—C108—H108	119.21
C3—C4—H4A	109.61	C108—C109—H109	118.92
C3—C4—H4B	109.46	C110—C109—H109	118.91
H4A—C4—H4B	108.14	C109—C110—H110	122.17
S1—C5—H5	124 (2)	C111—C110—H110	121.47
S2—C5—H5	123 (2)	C106—C111—H111	119.11
C10—C11—H11	119.28	C110—C111—H111	119.20
C12—C11—H11	119.50	C119—C118—C123	132.3 (4)
C11—C12—H12	120.02	C118—C119—C120	116.9 (3)
C13—C12—H12	120.06	C119—C120—C121	116.7 (3)
C12—C13—H13	119.99	C120—C121—C122	126.8 (4)
C14—C13—H13	120.12	C121—C122—C123	116.8 (3)
C13—C14—H14	119.92	C118—C123—C122	109.1 (3)
C15—C14—H14	119.95	C119—C118—H118	113.87
C10—C15—H15	119.45	C123—C118—H118	113.86
C14—C15—H15	119.55	C118—C119—H119	121.53
C20—C21—H21	119.27	C120—C119—H119	121.55
C22—C21—H21	119.28	C119—C120—H120	121.71
C21—C22—H22	120.34	C121—C120—H120	121.63
C23—C22—H22	120.33	C120—C121—H121	116.56
C22—C23—H23	119.90	C122—C121—H121	116.63
C24—C23—H23	119.88	C121—C122—H122	121.58
C23—C24—H24	119.86	C123—C122—H122	121.59
C25—C24—H24	119.81	C118—C123—H123	125.44
C20—C25—H25	119.84	C122—C123—H123	125.43
S2—Tc—S1—C5	−2.29 (15)	C80—P4—C70—C75	69.8 (4)
P1—Tc—S1—C5	−101.29 (15)	C80—P4—C4—C3	154.0 (2)
P3—Tc—S1—C5	164.66 (15)	Tc—P4—C4—C3	27.2 (3)
P4—Tc—S1—C5	83.56 (15)	C70—P4—C4—C3	−106.7 (3)
S1—Tc—S2—C5	2.30 (15)	P1—C1—C2—P2	51.2 (3)
P1—Tc—S2—C5	88.52 (15)	P3—C3—C4—P4	−48.2 (3)
P2—Tc—S2—C5	171.26 (15)	C15—C10—C11—C12	1.6 (7)
P4—Tc—S2—C5	−88.68 (15)	P1—C10—C15—C14	−178.9 (3)
S1—Tc—P1—C1	−174.01 (14)	C11—C10—C15—C14	−1.1 (6)
S1—Tc—P1—C10	−52.80 (17)	P1—C10—C11—C12	179.4 (3)
S1—Tc—P1—C20	68.72 (16)	C10—C11—C12—C13	−1.1 (7)
S2—Tc—P1—C1	117.92 (14)	C11—C12—C13—C14	0.1 (7)
S2—Tc—P1—C10	−120.86 (17)	C12—C13—C14—C15	0.4 (7)
S2—Tc—P1—C20	0.65 (16)	C13—C14—C15—C10	0.1 (8)
P2—Tc—P1—C1	23.30 (14)	C21—C20—C25—C24	−1.2 (5)
P2—Tc—P1—C10	144.51 (17)	P1—C20—C21—C22	−175.8 (3)
P2—Tc—P1—C20	−93.97 (16)	C25—C20—C21—C22	1.4 (5)
P3—Tc—P1—C1	−70.60 (14)	P1—C20—C25—C24	175.7 (2)
P3—Tc—P1—C10	50.61 (17)	C20—C21—C22—C23	−0.6 (6)
P3—Tc—P1—C20	172.13 (15)	C21—C22—C23—C24	−0.3 (6)
S2—Tc—P2—C2	−96.07 (15)	C22—C23—C24—C25	0.4 (5)
S2—Tc—P2—C30	142.78 (14)	C23—C24—C25—C20	0.3 (5)
S2—Tc—P2—C40	14.24 (16)	P2—C30—C31—C32	177.7 (3)
P1—Tc—P2—C2	1.44 (15)	C35—C30—C31—C32	−0.8 (6)
P1—Tc—P2—C30	−119.71 (14)	P2—C30—C35—C34	−177.6 (3)
P1—Tc—P2—C40	111.74 (16)	C31—C30—C35—C34	1.0 (5)
P3—Tc—P2—C2	94.92 (15)	C30—C31—C32—C33	−0.2 (6)
P3—Tc—P2—C30	−26.23 (14)	C31—C32—C33—C34	1.1 (7)
P3—Tc—P2—C40	−154.78 (16)	C32—C33—C34—C35	−0.8 (6)
P4—Tc—P2—C2	177.05 (15)	C33—C34—C35—C30	−0.2 (6)
P4—Tc—P2—C30	55.90 (14)	P2—C40—C45—C44	178.0 (3)
P4—Tc—P2—C40	−72.65 (16)	C45—C40—C41—C42	0.4 (7)
S1—Tc—P3—C3	−112.45 (15)	P2—C40—C41—C42	−179.4 (3)
S1—Tc—P3—C50	129.35 (14)	C41—C40—C45—C44	−1.7 (7)
S1—Tc—P3—C60	−3.33 (15)	C40—C41—C42—C43	1.2 (7)
P1—Tc—P3—C3	157.07 (15)	C41—C42—C43—C44	−1.3 (7)
P1—Tc—P3—C50	38.88 (14)	C42—C43—C44—C45	0.0 (7)
P1—Tc—P3—C60	−93.81 (15)	C43—C44—C45—C40	1.6 (7)
P2—Tc—P3—C3	74.75 (15)	P3—C50—C55—C54	179.9 (5)
P2—Tc—P3—C50	−43.44 (14)	P3—C50—C51—C52	179.9 (7)
P2—Tc—P3—C60	−176.12 (15)	C51—C50—C55—C54	0.0 (7)
P4—Tc—P3—C3	−25.11 (15)	C55—C50—C51—C52	−0.2 (7)
P4—Tc—P3—C50	−143.30 (14)	C50—C51—C52—C53	−0.2 (7)
P4—Tc—P3—C60	84.01 (15)	C51—C52—C53—C54	0.9 (7)
S1—Tc—P4—C4	105.74 (14)	C52—C53—C54—C55	−1.1 (7)
S1—Tc—P4—C70	−132.01 (18)	C53—C54—C55—C50	0.6 (7)
S1—Tc—P4—C80	−10.66 (15)	C61—C60—C65—C64	−0.5 (5)
S2—Tc—P4—C4	174.11 (14)	P3—C60—C65—C64	172.5 (3)
S2—Tc—P4—C70	−63.65 (18)	P3—C60—C61—C62	−172.6 (3)
S2—Tc—P4—C80	57.71 (15)	C65—C60—C61—C62	0.4 (6)
P2—Tc—P4—C4	−90.87 (14)	C60—C61—C62—C63	−0.1 (6)
P2—Tc—P4—C70	31.38 (18)	C61—C62—C63—C64	−0.1 (6)
P2—Tc—P4—C80	152.73 (15)	C62—C63—C64—C65	0.0 (6)
P3—Tc—P4—C4	2.09 (15)	C63—C64—C65—C60	0.3 (6)
P3—Tc—P4—C70	124.34 (18)	P4—C70—C71—C72	176.6 (4)
P3—Tc—P4—C80	−114.31 (15)	C75—C70—C71—C72	1.1 (7)
Tc—S1—C5—S2	3.4 (2)	C71—C70—C75—C74	−1.8 (7)
Tc—S2—C5—S1	−3.4 (2)	P4—C70—C75—C74	−177.2 (4)
C20—P1—C1—C2	80.1 (3)	C70—C71—C72—C73	−0.1 (8)
C1—P1—C10—C15	−49.4 (4)	C71—C72—C73—C74	−0.1 (9)
C20—P1—C10—C15	54.9 (4)	C72—C73—C74—C75	−0.5 (8)
Tc—P1—C1—C2	−48.7 (3)	C73—C74—C75—C70	1.5 (8)
Tc—P1—C20—C21	−60.1 (3)	P4—C80—C85—C84	178.6 (3)
Tc—P1—C10—C11	9.8 (4)	P4—C80—C81—C82	−179.4 (3)
C1—P1—C10—C11	132.8 (4)	C81—C80—C85—C84	−3.1 (6)
C20—P1—C10—C11	−122.9 (4)	C85—C80—C81—C82	2.2 (6)
Tc—P1—C10—C15	−172.5 (3)	C80—C81—C82—C83	0.1 (7)
C10—P1—C20—C25	−103.6 (3)	C81—C82—C83—C84	−1.7 (7)
C1—P1—C20—C25	2.6 (3)	C82—C83—C84—C85	0.8 (7)
C10—P1—C20—C21	73.4 (3)	C83—C84—C85—C80	1.6 (6)
Tc—P1—C20—C25	122.9 (3)	C95—C90—C91—C92	−0.5 (7)
C1—P1—C20—C21	179.5 (3)	C91—C90—C95—C94	0.9 (7)
C10—P1—C1—C2	179.7 (3)	C90—C91—C92—C93	−0.2 (7)
C40—P2—C2—C1	−158.6 (3)	C91—C92—C93—C94	0.5 (7)
C40—P2—C30—C31	−106.6 (3)	C92—C93—C94—C95	−0.1 (7)
C30—P2—C2—C1	101.3 (3)	C93—C94—C95—C90	−0.6 (7)
C30—P2—C40—C41	−5.8 (4)	C105—C100—C101—C102	4 (4)
Tc—P2—C40—C41	133.6 (3)	C101—C100—C105—C104	−1 (3)
Tc—P2—C30—C31	115.9 (3)	C105—C100—C101—H101	−177.41
Tc—P2—C40—C45	−46.2 (4)	H100—C100—C101—C102	−176.66
Tc—P2—C2—C1	−32.4 (3)	H100—C100—C101—H101	2.31
Tc—P2—C30—C35	−65.7 (3)	C101—C100—C105—H105	179.01
C2—P2—C30—C31	−7.8 (3)	H100—C100—C105—C104	179.27
C2—P2—C40—C41	−109.9 (4)	H100—C100—C105—H105	−0.70
C40—P2—C30—C35	71.8 (3)	C100—C101—C102—H102	177.06
C2—P2—C30—C35	170.6 (3)	H101—C101—C102—C103	177.16
C2—P2—C40—C45	70.3 (4)	H101—C101—C102—H102	−1.91
C30—P2—C40—C45	174.4 (3)	C101—C102—C103—H103	−178.67
C50—P3—C3—C4	−177.2 (3)	H102—C102—C103—C104	−179.48
Tc—P3—C3—C4	49.5 (3)	H102—C102—C103—H103	0.40
Tc—P3—C60—C61	−14.6 (4)	C102—C103—C104—H104	−178.92
C3—P3—C60—C61	100.8 (3)	H103—C103—C104—C105	−178.71
C60—P3—C3—C4	−78.1 (3)	H103—C103—C104—H104	1.20
C60—P3—C50—C51	59.9 (4)	C103—C104—C105—H105	178.59
C3—P3—C50—C55	−23.0 (4)	H104—C104—C105—C100	178.70
C60—P3—C50—C55	−120.0 (4)	H104—C104—C105—H105	−1.32
C50—P3—C60—C61	−157.5 (3)	C117—C112—C113—H113	−179.97
Tc—P3—C60—C65	172.7 (3)	H112—C112—C113—C114	−180.00
C3—P3—C60—C65	−71.9 (3)	H112—C112—C113—H113	0.07
C50—P3—C60—C65	29.7 (3)	C113—C112—C117—H117	−179.96
Tc—P3—C50—C51	−81.8 (4)	H112—C112—C117—C116	179.96
C3—P3—C50—C51	156.8 (4)	H112—C112—C117—H117	0.02
Tc—P3—C50—C55	98.3 (4)	C112—C113—C114—H114	180.00
C70—P4—C80—C81	45.0 (3)	H113—C113—C114—C115	179.97
Tc—P4—C70—C75	−159.0 (3)	H113—C113—C114—H114	−0.08
Tc—P4—C70—C71	25.6 (4)	C113—C114—C115—H115	−179.98
C80—P4—C70—C71	−105.6 (4)	H114—C114—C115—C116	−179.96
C4—P4—C70—C75	−33.6 (4)	H114—C114—C115—H115	0.07
Tc—P4—C80—C85	88.8 (3)	C114—C115—C116—H116	−180.00
C4—P4—C70—C71	151.0 (4)	H115—C115—C116—C117	179.96
C4—P4—C80—C81	149.7 (3)	H115—C115—C116—H116	−0.03
C70—P4—C80—C85	−136.7 (3)	C115—C116—C117—H117	179.98
Tc—P4—C80—C81	−89.5 (3)	H116—C116—C117—C112	180.00
C4—P4—C80—C85	−32.0 (3)	H116—C116—C117—H117	−0.03

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C11—H11···S1	0.9495	2.7329	3.469 (4)	134.85
C21—H21···S1	0.9504	2.8395	3.675 (5)	147.23
C45—H45···S2	0.9505	2.6107	3.199 (4)	120.44
C61—H61···S1	0.9495	2.5450	3.438 (5)	156.84
C71—H71···S2	0.9491	2.8167	3.587 (4)	139.00
C105—H105···S1	0.9498	2.8797	3.544 (11)	127.94