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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800017840/na6006sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536800017840/na6006Isup2.hkl
Contains datablock I

CCDC reference: 155810

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


Yellow Alert 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

Comment top

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.

Experimental top

[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).

Refinement top

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 Uij 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 Uiso(H) equal to 1.5Uiso(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 top

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 top
[Figure 1] 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) top
Crystal data top
[Tc(CHS2)(C26H24P2)2]·3C6H6Z = 2
Mr = 1207.2F(000) = 1256
Triclinic, P1Dx = 1.35 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.132 (4) ÅCell parameters from 25 reflections
b = 14.738 (6) Åθ = 7.6–11.9°
c = 17.031 (4) ŵ = 0.46 mm1
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) Å3
Data collection top
Nonius CAD-4
diffractometer
7752 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.029
Graphite monochromatorθmax = 25.0°, θmin = 2.2°
ω scansh = 016
Absorption correction: ψ scan
(SHELXTL-Plus; Siemens, 1990)
k = 1617
Tmin = 0.854, Tmax = 0.934l = 2020
10893 measured reflections3 standard reflections every 120 min
10431 independent reflections intensity decay: 8%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0493P)2 + 0.5423P]
where P = (Fo2 + 2Fc2)/3
10431 reflections(Δ/σ)max = 0.008
768 parametersΔρmax = 0.56 e Å3
219 restraintsΔρmin = 0.43 e Å3
0 constraints
Crystal data top
[Tc(CHS2)(C26H24P2)2]·3C6H6γ = 67.88 (3)°
Mr = 1207.2V = 2966 (2) Å3
Triclinic, P1Z = 2
a = 14.132 (4) ÅMo Kα radiation
b = 14.738 (6) ŵ = 0.46 mm1
c = 17.031 (4) ÅT = 193 K
α = 65.79 (3)°0.35 × 0.23 × 0.15 mm
β = 88.10 (3)°
Data collection top
Nonius CAD-4
diffractometer
7752 reflections with I > 2σ(I)
Absorption correction: ψ scan
(SHELXTL-Plus; Siemens, 1990)
Rint = 0.029
Tmin = 0.854, Tmax = 0.9343 standard reflections every 120 min
10893 measured reflections intensity decay: 8%
10431 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.035219 restraints
wR(F2) = 0.104H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.56 e Å3
10431 reflectionsΔρmin = 0.43 e Å3
768 parameters
Special details top

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 (Å2) top
xyzUiso*/UeqOcc. (<1)
Tc0.68692 (2)0.67315 (2)0.61216 (2)0.0124 (1)
S10.69885 (7)0.77850 (7)0.69129 (5)0.0187 (2)
S20.55321 (7)0.85846 (7)0.54825 (6)0.0195 (2)
P10.59799 (7)0.59135 (7)0.72035 (5)0.0152 (2)
P20.61640 (7)0.60808 (7)0.53325 (5)0.0146 (2)
P30.84407 (6)0.51919 (7)0.66499 (5)0.0138 (2)
P40.79020 (7)0.74527 (7)0.51157 (5)0.0157 (2)
C10.5795 (3)0.4860 (3)0.6984 (2)0.0184 (10)
C20.5363 (3)0.5400 (3)0.6021 (2)0.0175 (10)
C30.9215 (3)0.5270 (3)0.5740 (2)0.0178 (10)
C40.9228 (3)0.6399 (3)0.5326 (2)0.0193 (10)
C50.6008 (3)0.8864 (3)0.6197 (2)0.0211 (11)
C100.6493 (3)0.5237 (3)0.8367 (2)0.0173 (10)
C110.7350 (3)0.5332 (3)0.8652 (2)0.0207 (10)
C120.7744 (3)0.4837 (3)0.9526 (2)0.0261 (11)
C130.7274 (3)0.4250 (3)1.0136 (2)0.0302 (11)
C140.6414 (3)0.4159 (3)0.9870 (2)0.0311 (12)
C150.6026 (3)0.4647 (3)0.8996 (2)0.0247 (11)
C200.4656 (3)0.6714 (3)0.7318 (2)0.0173 (10)
C210.4522 (3)0.7593 (3)0.7498 (2)0.0246 (11)
C220.3571 (3)0.8202 (3)0.7651 (3)0.0295 (12)
C230.2735 (3)0.7935 (3)0.7616 (2)0.0298 (12)
C240.2846 (3)0.7078 (3)0.7427 (2)0.0274 (11)
C250.3803 (3)0.6466 (3)0.7275 (2)0.0227 (11)
C300.6933 (2)0.5106 (3)0.4903 (2)0.0157 (9)
C310.6947 (3)0.4075 (3)0.5175 (2)0.0210 (10)
C320.7518 (3)0.3390 (3)0.4801 (3)0.0265 (11)
C330.8076 (3)0.3730 (3)0.4151 (3)0.0305 (12)
C340.8089 (3)0.4758 (3)0.3870 (2)0.0256 (11)
C350.7523 (3)0.5434 (3)0.4246 (2)0.0206 (10)
C400.5145 (3)0.7032 (3)0.4366 (2)0.0175 (10)
C410.5156 (3)0.6958 (3)0.3573 (2)0.0201 (10)
C420.4376 (3)0.7702 (3)0.2885 (2)0.0241 (11)
C430.3572 (3)0.8552 (3)0.2956 (2)0.0282 (11)
C440.3554 (3)0.8629 (3)0.3746 (2)0.0255 (11)
C450.4323 (3)0.7872 (3)0.4443 (2)0.0196 (10)
C500.8583 (3)0.3764 (3)0.7085 (2)0.0183 (10)
C510.8445 (3)0.3242 (3)0.7953 (2)0.0241 (11)
C520.8546 (3)0.2176 (3)0.8293 (3)0.0286 (11)
C530.8780 (3)0.1607 (3)0.7788 (3)0.0287 (11)
C540.8928 (3)0.2108 (3)0.6935 (3)0.0271 (11)
C550.8824 (3)0.3183 (3)0.6588 (2)0.0216 (11)
C600.9481 (3)0.4991 (3)0.7430 (2)0.0179 (10)
C610.9472 (3)0.5847 (3)0.7584 (2)0.0232 (11)
C621.0301 (3)0.5737 (3)0.8085 (3)0.0287 (12)
C631.1150 (3)0.4762 (3)0.8439 (2)0.0298 (11)
C641.1172 (3)0.3902 (3)0.8296 (2)0.0288 (11)
C651.0346 (3)0.4006 (3)0.7797 (2)0.0235 (11)
C700.7575 (3)0.8042 (3)0.3924 (2)0.0192 (10)
C710.6558 (3)0.8479 (3)0.3552 (2)0.0297 (14)
C720.6300 (4)0.8977 (4)0.2650 (3)0.0437 (16)
C730.7059 (4)0.9041 (4)0.2118 (3)0.0455 (18)
C740.8070 (4)0.8611 (3)0.2487 (3)0.0425 (14)
C750.8323 (4)0.8129 (3)0.3378 (3)0.0362 (14)
C800.8167 (3)0.8584 (3)0.5141 (2)0.0190 (10)
C810.7497 (3)0.9648 (3)0.4639 (2)0.0236 (11)
C820.7672 (3)1.0513 (3)0.4633 (3)0.0325 (13)
C830.8534 (3)1.0330 (3)0.5135 (3)0.0339 (14)
C840.9192 (3)0.9276 (3)0.5653 (3)0.0322 (12)
C850.9014 (3)0.8411 (3)0.5670 (2)0.0247 (11)
C900.2282 (3)0.8795 (3)0.9528 (3)0.0340 (14)
C910.3118 (3)0.8622 (3)1.0053 (3)0.0329 (12)
C920.3021 (3)0.9316 (3)1.0433 (3)0.0353 (12)
C930.2087 (3)1.0187 (3)1.0286 (3)0.0352 (14)
C940.1267 (3)1.0348 (3)0.9771 (3)0.0344 (12)
C950.1359 (3)0.9650 (3)0.9393 (3)0.0329 (12)
C1000.8798 (13)0.7290 (17)0.9410 (8)0.036 (3)0.680
C1010.9752 (16)0.726 (2)0.9628 (9)0.051 (5)0.680
C1021.0166 (14)0.791 (2)0.9018 (11)0.044 (6)0.680
C1030.9663 (11)0.8543 (15)0.8176 (9)0.041 (4)0.680
C1040.8750 (8)0.8552 (7)0.7944 (6)0.028 (3)0.680
C1050.8296 (7)0.7921 (9)0.8575 (6)0.035 (3)0.680
C1120.41759 (16)0.2985 (3)1.0245 (2)0.042 (2)0.730
C1130.39980 (16)0.3366 (3)0.9348 (2)0.042 (2)0.730
C1140.39480 (16)0.2689 (3)0.8989 (2)0.061 (3)0.730
C1150.40758 (16)0.1631 (3)0.9528 (2)0.046 (3)0.730
C1160.42537 (16)0.1250 (3)1.0426 (2)0.058 (3)0.730
C1170.43037 (16)0.1927 (3)1.0784 (2)0.040 (2)0.730
C1060.869 (3)0.745 (4)0.9174 (15)0.055 (10)0.320
C1070.960 (3)0.722 (4)0.9661 (18)0.038 (7)0.320
C1081.021 (3)0.777 (3)0.924 (2)0.030 (6)0.320
C1090.991 (2)0.854 (3)0.8382 (17)0.029 (6)0.320
C1100.9012 (19)0.881 (2)0.7926 (12)0.043 (7)0.320
C1110.84101 (16)0.8187 (3)0.8353 (2)0.040 (7)0.320
C1180.40322 (16)0.3277 (3)0.9738 (2)0.045 (6)*0.270
C1190.39618 (16)0.3167 (3)0.8909 (2)0.061 (9)0.270
C1200.39773 (16)0.2207 (3)0.8978 (2)0.039 (5)*0.270
C1210.40643 (16)0.1401 (3)0.9838 (2)0.055 (6)0.270
C1220.41054 (16)0.1490 (3)1.0512 (2)0.078 (9)0.270
C1230.41992 (16)0.2676 (3)1.0440 (2)0.067 (8)0.270
H1A0.646000.423300.711100.0220*
H1B0.530500.460500.734700.0220*
H2A0.464900.594100.592500.0210*
H2B0.533900.484500.584500.0210*
H3A0.992700.471100.596000.0210*
H3B0.890400.514100.530400.0210*
H4A0.951600.651300.477300.0230*
H4B0.967600.646000.572000.0230*
H50.575 (3)0.953 (3)0.620 (2)0.0320*
H110.766900.574300.823800.0250*
H120.833600.490000.970700.0310*
H130.754300.391101.073600.0360*
H140.608900.376101.028800.0370*
H150.543400.458000.881900.0300*
H210.509200.778100.751600.0290*
H220.349500.879400.777800.0360*
H230.208400.834300.772400.0360*
H240.227000.690300.739900.0330*
H250.387300.588000.714200.0270*
H310.656200.383100.562300.0250*
H320.752000.268600.499800.0320*
H330.845300.326700.389200.0360*
H340.848100.499300.342600.0310*
H350.753500.613200.405500.0250*
H410.570600.638900.350600.0240*
H420.439200.762900.235500.0290*
H430.304500.907100.247800.0340*
H440.300800.920600.380700.0310*
H450.428900.792700.498100.0240*
H510.828200.362300.830700.0290*
H520.845400.183000.888100.0350*
H530.883800.087800.802500.0340*
H540.909900.172000.658600.0330*
H550.892100.352400.600000.0260*
H610.889100.652000.734400.0280*
H621.028300.633200.818400.0340*
H631.171700.468500.878100.0360*
H641.175600.323200.854000.0340*
H651.036800.340600.770500.0280*
H710.603400.843900.391200.0360*
H720.560000.927400.239800.0520*
H730.688200.937900.150300.0550*
H740.859600.864600.212700.0510*
H750.902200.784900.362600.0430*
H810.690400.978500.429000.0290*
H820.719901.123500.428400.0390*
H830.867001.092000.512100.0400*
H840.977900.914300.600600.0380*
H850.946900.769200.604200.0300*
H900.234600.832400.926200.0410*
H910.375700.802801.015300.0400*
H920.359300.919701.079400.0420*
H930.202201.066701.054300.0420*
H940.062701.094100.967100.0410*
H950.078200.976500.903900.0400*
H1000.849700.687100.983900.0430*0.680
H1011.011700.680201.019900.0610*0.680
H1021.080100.791200.917700.0540*0.680
H1030.995900.897700.775600.0490*0.680
H1040.841400.898000.736100.0340*0.680
H1050.764900.793600.842000.0410*0.680
H1120.421000.344901.049100.0500*0.730
H1130.391100.408900.897900.0500*0.730
H1140.382600.294900.837500.0730*0.730
H1150.404200.116700.928300.0550*0.730
H1160.434100.052701.079400.0700*0.730
H1170.442500.166701.139800.0480*0.730
H1060.826400.707400.943800.0670*0.320
H1070.978900.671501.025500.0470*0.320
H1081.083900.762000.953900.0350*0.320
H1091.035500.888500.810700.0350*0.320
H1100.878500.937100.735300.0520*0.320
H1110.779800.831000.803800.0480*0.320
H1180.391300.399100.965500.0540*0.270
H1190.390900.374000.836000.0740*0.270
H1200.393200.207900.848000.0460*0.270
H1210.409300.072600.988600.0660*0.270
H1220.408800.094401.105300.0940*0.270
H1230.436500.279101.091900.0810*0.270
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tc0.0114 (1)0.0122 (1)0.0133 (1)0.0046 (1)0.0016 (1)0.0054 (1)
S10.0178 (4)0.0192 (4)0.0209 (4)0.0064 (4)0.0014 (3)0.0111 (4)
S20.0172 (4)0.0149 (4)0.0226 (4)0.0030 (4)0.0020 (3)0.0073 (3)
P10.0149 (4)0.0156 (4)0.0155 (4)0.0064 (4)0.0038 (3)0.0069 (3)
P20.0134 (4)0.0156 (4)0.0158 (4)0.0063 (4)0.0025 (3)0.0073 (3)
P30.0116 (4)0.0137 (4)0.0156 (4)0.0046 (3)0.0024 (3)0.0062 (3)
P40.0160 (4)0.0142 (4)0.0163 (4)0.0064 (4)0.0041 (3)0.0057 (3)
C10.0201 (18)0.0171 (17)0.0187 (17)0.0089 (15)0.0067 (14)0.0073 (14)
C20.0145 (17)0.0205 (17)0.0214 (18)0.0094 (15)0.0030 (14)0.0104 (15)
C30.0191 (18)0.0151 (17)0.0190 (17)0.0061 (14)0.0045 (14)0.0078 (14)
C40.0154 (17)0.0160 (17)0.0259 (19)0.0079 (15)0.0062 (14)0.0073 (15)
C50.0235 (19)0.0168 (17)0.0249 (19)0.0084 (16)0.0075 (15)0.0106 (15)
C100.0164 (17)0.0151 (16)0.0158 (17)0.0022 (14)0.0044 (14)0.0062 (14)
C110.0185 (18)0.0225 (18)0.0176 (17)0.0044 (15)0.0033 (14)0.0089 (15)
C120.0210 (19)0.029 (2)0.025 (2)0.0046 (17)0.0008 (16)0.0130 (17)
C130.038 (2)0.0239 (19)0.0160 (18)0.0017 (18)0.0011 (17)0.0062 (15)
C140.040 (2)0.026 (2)0.023 (2)0.0142 (19)0.0094 (18)0.0061 (16)
C150.024 (2)0.0241 (19)0.0234 (19)0.0107 (16)0.0025 (15)0.0066 (15)
C200.0166 (17)0.0185 (17)0.0137 (16)0.0074 (14)0.0032 (13)0.0037 (14)
C210.022 (2)0.0261 (19)0.026 (2)0.0104 (16)0.0071 (16)0.0110 (16)
C220.030 (2)0.028 (2)0.033 (2)0.0084 (18)0.0103 (17)0.0187 (18)
C230.020 (2)0.039 (2)0.027 (2)0.0056 (18)0.0099 (16)0.0171 (18)
C240.0159 (19)0.041 (2)0.025 (2)0.0112 (17)0.0054 (15)0.0143 (18)
C250.0199 (19)0.029 (2)0.0216 (18)0.0119 (16)0.0042 (15)0.0112 (16)
C300.0110 (16)0.0205 (17)0.0164 (16)0.0058 (14)0.0005 (13)0.0089 (14)
C310.0125 (17)0.0228 (18)0.0274 (19)0.0057 (15)0.0003 (14)0.0115 (16)
C320.0181 (19)0.026 (2)0.044 (2)0.0109 (16)0.0026 (17)0.0210 (18)
C330.021 (2)0.040 (2)0.044 (2)0.0071 (18)0.0057 (17)0.035 (2)
C340.0176 (19)0.042 (2)0.0251 (19)0.0141 (17)0.0058 (15)0.0198 (18)
C350.0194 (18)0.0251 (18)0.0217 (18)0.0112 (16)0.0035 (14)0.0121 (15)
C400.0176 (18)0.0186 (17)0.0185 (17)0.0100 (15)0.0019 (14)0.0074 (14)
C410.0170 (18)0.0227 (18)0.0215 (18)0.0089 (15)0.0019 (14)0.0094 (15)
C420.027 (2)0.029 (2)0.0159 (18)0.0113 (17)0.0003 (15)0.0088 (15)
C430.023 (2)0.029 (2)0.0238 (19)0.0067 (17)0.0063 (16)0.0059 (16)
C440.0162 (18)0.0232 (19)0.033 (2)0.0027 (16)0.0018 (16)0.0128 (16)
C450.0136 (17)0.0225 (18)0.0248 (18)0.0067 (15)0.0054 (14)0.0127 (15)
C500.0128 (16)0.0151 (16)0.0244 (18)0.0047 (14)0.0019 (14)0.0068 (14)
C510.0204 (19)0.0177 (18)0.029 (2)0.0034 (15)0.0064 (16)0.0092 (16)
C520.026 (2)0.0224 (19)0.027 (2)0.0091 (17)0.0064 (16)0.0016 (16)
C530.024 (2)0.0163 (18)0.038 (2)0.0094 (16)0.0007 (17)0.0029 (16)
C540.024 (2)0.0216 (19)0.037 (2)0.0076 (16)0.0006 (17)0.0147 (17)
C550.0192 (18)0.0188 (18)0.0234 (19)0.0066 (15)0.0012 (15)0.0066 (15)
C600.0144 (17)0.0251 (18)0.0146 (16)0.0080 (15)0.0039 (13)0.0089 (14)
C610.0156 (18)0.0251 (19)0.029 (2)0.0054 (16)0.0028 (15)0.0142 (16)
C620.027 (2)0.033 (2)0.035 (2)0.0142 (18)0.0046 (17)0.0207 (18)
C630.0170 (19)0.042 (2)0.031 (2)0.0092 (18)0.0015 (16)0.0183 (19)
C640.0174 (19)0.029 (2)0.030 (2)0.0017 (16)0.0052 (16)0.0097 (17)
C650.0212 (19)0.0232 (19)0.0228 (19)0.0052 (16)0.0024 (15)0.0100 (15)
C700.030 (2)0.0161 (17)0.0119 (16)0.0119 (16)0.0046 (14)0.0041 (13)
C710.045 (3)0.030 (2)0.0207 (19)0.028 (2)0.0039 (17)0.0051 (16)
C720.062 (3)0.045 (3)0.029 (2)0.039 (2)0.012 (2)0.003 (2)
C730.097 (4)0.039 (3)0.0137 (19)0.044 (3)0.009 (2)0.0083 (18)
C740.066 (3)0.035 (2)0.023 (2)0.020 (2)0.020 (2)0.0103 (19)
C750.042 (3)0.027 (2)0.027 (2)0.0082 (19)0.0136 (19)0.0055 (17)
C800.0208 (18)0.0178 (17)0.0206 (18)0.0106 (15)0.0102 (14)0.0083 (14)
C810.025 (2)0.0208 (18)0.0241 (19)0.0075 (16)0.0043 (15)0.0104 (15)
C820.047 (3)0.0167 (18)0.032 (2)0.0125 (18)0.0188 (19)0.0100 (17)
C830.039 (2)0.033 (2)0.049 (3)0.025 (2)0.025 (2)0.027 (2)
C840.032 (2)0.037 (2)0.045 (2)0.023 (2)0.0142 (19)0.026 (2)
C850.0205 (19)0.0251 (19)0.032 (2)0.0129 (16)0.0049 (16)0.0120 (16)
C900.045 (3)0.032 (2)0.036 (2)0.021 (2)0.017 (2)0.0203 (19)
C910.021 (2)0.031 (2)0.044 (2)0.0102 (18)0.0123 (18)0.0143 (19)
C920.030 (2)0.039 (2)0.035 (2)0.019 (2)0.0000 (18)0.0091 (19)
C930.048 (3)0.030 (2)0.035 (2)0.021 (2)0.011 (2)0.0162 (19)
C940.032 (2)0.024 (2)0.035 (2)0.0074 (18)0.0086 (19)0.0050 (18)
C950.031 (2)0.036 (2)0.027 (2)0.017 (2)0.0023 (17)0.0058 (18)
C1000.044 (6)0.038 (6)0.028 (4)0.012 (5)0.003 (4)0.020 (4)
C1010.045 (10)0.049 (8)0.051 (7)0.001 (7)0.013 (7)0.028 (7)
C1020.021 (5)0.059 (12)0.066 (12)0.011 (6)0.006 (6)0.042 (9)
C1030.023 (7)0.040 (5)0.067 (9)0.013 (6)0.004 (6)0.030 (6)
C1040.021 (5)0.034 (5)0.031 (4)0.011 (3)0.004 (3)0.015 (3)
C1050.029 (4)0.057 (5)0.031 (4)0.025 (4)0.010 (3)0.024 (4)
C1120.026 (4)0.037 (3)0.058 (5)0.005 (3)0.007 (3)0.024 (3)
C1130.017 (3)0.062 (4)0.043 (4)0.013 (3)0.003 (3)0.021 (3)
C1140.024 (4)0.101 (7)0.076 (5)0.018 (4)0.008 (4)0.061 (4)
C1150.034 (4)0.059 (4)0.060 (5)0.017 (4)0.006 (3)0.042 (4)
C1160.048 (5)0.061 (5)0.085 (6)0.024 (4)0.005 (5)0.048 (5)
C1170.034 (4)0.049 (4)0.057 (4)0.026 (3)0.015 (3)0.033 (3)
C1060.056 (15)0.057 (19)0.08 (2)0.036 (15)0.012 (15)0.042 (16)
C1070.020 (11)0.033 (13)0.048 (12)0.001 (9)0.020 (7)0.014 (11)
C1080.030 (10)0.011 (8)0.032 (11)0.002 (7)0.003 (8)0.003 (9)
C1090.019 (12)0.032 (9)0.031 (10)0.006 (9)0.002 (9)0.012 (8)
C1100.040 (15)0.058 (14)0.045 (9)0.018 (10)0.001 (9)0.037 (8)
C1110.026 (9)0.068 (15)0.058 (13)0.019 (8)0.014 (8)0.058 (12)
C1190.028 (11)0.091 (17)0.103 (18)0.018 (10)0.008 (11)0.082 (15)
C1210.058 (14)0.042 (10)0.026 (9)0.006 (10)0.015 (9)0.009 (8)
C1220.063 (18)0.110 (16)0.048 (12)0.028 (15)0.022 (13)0.028 (14)
C1230.048 (16)0.085 (15)0.047 (12)0.009 (12)0.026 (11)0.025 (12)
Geometric parameters (Å, º) top
Tc—S12.4866 (14)C32—H320.9494
Tc—S22.4548 (15)C33—H330.9495
Tc—P12.3650 (14)C34—H340.9490
Tc—P22.3632 (14)C35—H350.9501
Tc—P32.3566 (14)C41—H410.9498
Tc—P42.3884 (14)C42—H420.9504
S1—C51.673 (4)C43—H430.9502
S2—C51.666 (4)C44—H440.9499
P1—C11.846 (5)C45—H450.9505
P1—C101.838 (3)C51—H510.9502
P1—C201.853 (5)C52—H520.9499
P2—C21.862 (4)C53—H530.9509
P2—C301.848 (4)C54—H540.9507
P2—C401.869 (4)C55—H550.9509
P3—C31.857 (4)C61—H610.9495
P3—C501.852 (4)C62—H620.9499
P3—C601.869 (4)C63—H630.9500
P4—C41.857 (5)C64—H640.9494
P4—C701.844 (3)C65—H650.9487
P4—C801.858 (5)C71—H710.9491
C1—C21.525 (5)C72—H720.9499
C3—C41.525 (6)C73—H730.9505
C10—C111.394 (6)C74—H740.9507
C10—C151.400 (6)C75—H750.9498
C11—C121.384 (5)C81—H810.9505
C12—C131.385 (6)C82—H820.9510
C13—C141.382 (6)C83—H830.9498
C14—C151.383 (5)C84—H840.9497
C20—C211.395 (6)C85—H850.9492
C20—C251.397 (6)C90—C911.384 (7)
C21—C221.393 (6)C90—C951.374 (7)
C22—C231.389 (6)C91—C921.384 (7)
C23—C241.380 (6)C92—C931.391 (7)
C24—C251.400 (6)C93—C941.363 (7)
C30—C311.387 (6)C94—C951.388 (7)
C30—C351.407 (5)C90—H900.9504
C31—C321.399 (6)C91—H910.9505
C32—C331.372 (7)C92—H920.9487
C33—C341.397 (6)C93—H930.9502
C34—C351.390 (6)C94—H940.9506
C40—C411.398 (5)C95—H950.9496
C40—C451.393 (6)C100—C1011.39 (3)
C41—C421.383 (5)C100—C1051.370 (17)
C42—C431.385 (6)C101—C1021.38 (3)
C43—C441.394 (5)C102—C1031.38 (2)
C44—C451.386 (5)C103—C1041.36 (2)
C50—C511.406 (5)C104—C1051.420 (15)
C50—C551.386 (6)C100—H1000.9504
C51—C521.384 (6)C101—H1010.9487
C52—C531.384 (7)C102—H1020.9473
C53—C541.384 (7)C103—H1030.9498
C54—C551.394 (6)C104—H1040.9493
C60—C611.385 (6)C105—H1050.9498
C60—C651.401 (6)C112—C1131.388 (4)
C61—C621.392 (6)C112—C1171.390 (5)
C62—C631.381 (6)C113—C1141.389 (6)
C63—C641.375 (6)C114—C1151.390 (5)
C64—C651.390 (6)C115—C1161.390 (4)
C70—C711.382 (6)C116—C1171.388 (6)
C70—C751.392 (7)C112—H1120.9522
C71—C721.394 (6)C113—H1130.9501
C72—C731.386 (8)C114—H1140.9506
C73—C741.374 (8)C115—H1150.9508
C74—C751.377 (7)C116—H1160.9496
C80—C811.387 (6)C117—H1170.9505
C80—C851.401 (6)C106—C1071.40 (6)
C81—C821.383 (6)C106—C1111.33 (3)
C82—C831.386 (6)C107—C1081.39 (6)
C83—C841.378 (7)C108—C1091.39 (4)
C84—C851.378 (6)C109—C1101.34 (4)
C1—H1A0.9897C110—C1111.45 (3)
C1—H1B0.9899C106—H1060.9490
C2—H2A0.9893C107—H1070.9484
C2—H2B0.9913C108—H1080.9424
C3—H3A0.9895C109—H1090.9483
C3—H3B0.9905C110—H1100.9477
C4—H4A0.9885C111—H1110.9497
C4—H4B0.9898C118—C1191.496 (5)
C5—H50.91 (4)C118—C1231.124 (5)
C11—H110.9495C119—C1201.363 (6)
C12—H120.9501C120—C1211.431 (5)
C13—H130.9499C121—C1221.213 (5)
C14—H140.9490C122—C1231.757 (6)
C15—H150.9507C118—H1180.9496
C21—H210.9504C119—H1190.9500
C22—H220.9499C120—H1200.9502
C23—H230.9511C121—H1210.9493
C24—H240.9498C122—H1220.9499
C25—H250.9495C123—H1230.9514
C31—H310.9499
S1—Tc—S268.38 (4)C24—C25—H25119.90
S1—Tc—P189.52 (4)C30—C31—H31119.36
S1—Tc—P2160.79 (5)C32—C31—H31119.52
S1—Tc—P3103.41 (5)C31—C32—H32119.84
S1—Tc—P489.41 (4)C33—C32—H32119.83
S2—Tc—P198.18 (5)C32—C33—H33120.05
S2—Tc—P295.66 (5)C34—C33—H33119.98
S2—Tc—P3165.10 (5)C33—C34—H34120.28
S2—Tc—P485.93 (5)C35—C34—H34120.28
P1—Tc—P282.05 (4)C30—C35—H35119.36
P1—Tc—P394.05 (4)C34—C35—H35119.28
P1—Tc—P4175.03 (5)C40—C41—H41119.58
P2—Tc—P394.42 (5)C42—C41—H41119.56
P2—Tc—P4100.39 (4)C41—C42—H42119.48
P3—Tc—P481.48 (4)C43—C42—H42119.48
Tc—S1—C588.86 (15)C42—C43—H43120.85
Tc—S2—C590.09 (15)C44—C43—H43120.73
Tc—P1—C1108.38 (12)C43—C44—H44119.60
Tc—P1—C10122.16 (15)C45—C44—H44119.68
Tc—P1—C20120.93 (13)C40—C45—H45119.53
C1—P1—C10104.39 (18)C44—C45—H45119.55
C1—P1—C20102.2 (2)C50—C51—H51119.84
C10—P1—C2096.09 (18)C52—C51—H51119.94
Tc—P2—C2108.60 (12)C51—C52—H52119.54
Tc—P2—C30124.61 (12)C53—C52—H52119.57
Tc—P2—C40121.23 (15)C52—C53—H53120.27
C2—P2—C30102.85 (18)C54—C53—H53120.26
C2—P2—C4096.65 (18)C53—C54—H54120.05
C30—P2—C4098.28 (17)C55—C54—H54120.06
Tc—P3—C3107.82 (13)C50—C55—H55119.36
Tc—P3—C50125.77 (15)C54—C55—H55119.44
Tc—P3—C60123.40 (15)C60—C61—H61119.51
C3—P3—C50100.72 (19)C62—C61—H61119.40
C3—P3—C6095.27 (18)C61—C62—H62120.04
C50—P3—C6097.90 (18)C63—C62—H62119.98
Tc—P4—C4110.12 (13)C62—C63—H63120.14
Tc—P4—C70123.82 (15)C64—C63—H63120.06
Tc—P4—C80118.82 (13)C63—C64—H64119.72
C4—P4—C70102.99 (18)C65—C64—H64119.77
C4—P4—C80101.5 (2)C60—C65—H65119.81
C70—P4—C8096.34 (17)C64—C65—H65119.79
P1—C1—C2105.7 (3)C70—C71—H71119.89
P2—C2—C1111.6 (3)C72—C71—H71119.92
P3—C3—C4108.0 (3)C71—C72—H72119.82
P4—C4—C3110.4 (3)C73—C72—H72119.78
S1—C5—S2112.5 (3)C72—C73—H73120.29
P1—C10—C11120.2 (3)C74—C73—H73120.24
P1—C10—C15121.9 (3)C73—C74—H74120.01
C11—C10—C15117.8 (3)C75—C74—H74119.89
C10—C11—C12121.2 (4)C70—C75—H75119.24
C11—C12—C13119.9 (4)C74—C75—H75119.42
C12—C13—C14119.9 (3)C80—C81—H81119.10
C13—C14—C15120.1 (4)C82—C81—H81119.30
C10—C15—C14121.0 (4)C81—C82—H82119.90
P1—C20—C21117.1 (3)C83—C82—H82119.94
P1—C20—C25124.4 (3)C82—C83—H83120.63
C21—C20—C25118.4 (4)C84—C83—H83120.61
C20—C21—C22121.4 (4)C83—C84—H84119.34
C21—C22—C23119.3 (4)C85—C84—H84119.36
C22—C23—C24120.2 (4)C80—C85—H85119.65
C23—C24—C25120.3 (4)C84—C85—H85119.82
C20—C25—C24120.3 (4)C91—C90—C95119.8 (4)
P2—C30—C31124.0 (3)C90—C91—C92119.8 (4)
P2—C30—C35118.3 (3)C91—C92—C93120.1 (4)
C31—C30—C35117.8 (4)C92—C93—C94119.6 (4)
C30—C31—C32121.1 (4)C93—C94—C95120.4 (4)
C31—C32—C33120.3 (4)C90—C95—C94120.2 (4)
C32—C33—C34120.0 (4)C91—C90—H90120.16
C33—C34—C35119.4 (4)C95—C90—H90120.09
C30—C35—C34121.4 (4)C90—C91—H91120.15
P2—C40—C41124.4 (3)C92—C91—H91120.03
P2—C40—C45117.6 (3)C91—C92—H92119.88
C41—C40—C45118.0 (3)C93—C92—H92120.01
C40—C41—C42120.9 (4)C92—C93—H93120.11
C41—C42—C43121.0 (3)C94—C93—H93120.25
C42—C43—C44118.4 (3)C93—C94—H94119.83
C43—C44—C45120.7 (4)C95—C94—H94119.72
C40—C45—C44120.9 (3)C90—C95—H95119.91
P3—C50—C51119.1 (3)C94—C95—H95119.86
P3—C50—C55122.6 (3)C101—C100—C105119.8 (15)
C51—C50—C55118.3 (4)C100—C101—C102120.1 (16)
C50—C51—C52120.2 (4)C101—C102—C103120 (2)
C51—C52—C53120.9 (4)C102—C103—C104120.6 (16)
C52—C53—C54119.5 (4)C103—C104—C105119.9 (10)
C53—C54—C55119.9 (4)C100—C105—C104119.5 (12)
C50—C55—C54121.2 (3)C101—C100—H100120.03
P3—C60—C61120.7 (3)C105—C100—H100120.15
P3—C60—C65120.7 (3)C100—C101—H101120.26
C61—C60—C65118.2 (4)C102—C101—H101119.62
C60—C61—C62121.1 (4)C101—C102—H102119.83
C61—C62—C63120.0 (4)C103—C102—H102120.14
C62—C63—C64119.8 (4)C102—C103—H103119.64
C63—C64—C65120.5 (4)C104—C103—H103119.79
C60—C65—C64120.4 (4)C103—C104—H104120.11
P4—C70—C71119.9 (3)C105—C104—H104120.02
P4—C70—C75121.4 (3)C100—C105—H105120.20
C71—C70—C75118.5 (3)C104—C105—H105120.32
C70—C71—C72120.2 (4)C113—C112—C117120.0 (4)
C71—C72—C73120.4 (5)C112—C113—C114120.0 (4)
C72—C73—C74119.5 (4)C113—C114—C115120.0 (3)
C73—C74—C75120.1 (5)C114—C115—C116120.0 (4)
C70—C75—C74121.3 (5)C115—C116—C117120.0 (4)
P4—C80—C81119.8 (3)C112—C117—C116120.0 (3)
P4—C80—C85122.6 (3)C113—C112—H112119.98
C81—C80—C85117.6 (4)C117—C112—H112119.98
C80—C81—C82121.6 (4)C112—C113—H113120.10
C81—C82—C83120.2 (4)C114—C113—H113119.92
C82—C83—C84118.8 (4)C113—C114—H114120.06
C83—C84—C85121.3 (4)C115—C114—H114119.97
C80—C85—C84120.5 (4)C114—C115—H115120.05
P1—C1—H1A110.52C116—C115—H115119.93
P1—C1—H1B110.58C115—C116—H116119.99
C2—C1—H1A110.69C117—C116—H116120.06
C2—C1—H1B110.62C112—C117—H117119.99
H1A—C1—H1B108.76C116—C117—H117119.99
P2—C2—H2A109.32C107—C106—C111121 (4)
P2—C2—H2B109.27C106—C107—C108117 (3)
C1—C2—H2A109.42C107—C108—C109121 (4)
C1—C2—H2B109.29C108—C109—C110122 (3)
H2A—C2—H2B107.89C109—C110—C111116 (2)
P3—C3—H3A110.15C106—C111—C110122 (2)
P3—C3—H3B110.09C107—C106—H106119.38
C4—C3—H3A110.20C111—C106—H106119.31
C4—C3—H3B110.11C106—C107—H107121.59
H3A—C3—H3B108.32C108—C107—H107121.18
P4—C4—H4A109.60C107—C108—H108119.79
P4—C4—H4B109.56C109—C108—H108119.21
C3—C4—H4A109.61C108—C109—H109118.92
C3—C4—H4B109.46C110—C109—H109118.91
H4A—C4—H4B108.14C109—C110—H110122.17
S1—C5—H5124 (2)C111—C110—H110121.47
S2—C5—H5123 (2)C106—C111—H111119.11
C10—C11—H11119.28C110—C111—H111119.20
C12—C11—H11119.50C119—C118—C123132.3 (4)
C11—C12—H12120.02C118—C119—C120116.9 (3)
C13—C12—H12120.06C119—C120—C121116.7 (3)
C12—C13—H13119.99C120—C121—C122126.8 (4)
C14—C13—H13120.12C121—C122—C123116.8 (3)
C13—C14—H14119.92C118—C123—C122109.1 (3)
C15—C14—H14119.95C119—C118—H118113.87
C10—C15—H15119.45C123—C118—H118113.86
C14—C15—H15119.55C118—C119—H119121.53
C20—C21—H21119.27C120—C119—H119121.55
C22—C21—H21119.28C119—C120—H120121.71
C21—C22—H22120.34C121—C120—H120121.63
C23—C22—H22120.33C120—C121—H121116.56
C22—C23—H23119.90C122—C121—H121116.63
C24—C23—H23119.88C121—C122—H122121.58
C23—C24—H24119.86C123—C122—H122121.59
C25—C24—H24119.81C118—C123—H123125.44
C20—C25—H25119.84C122—C123—H123125.43
S2—Tc—S1—C52.29 (15)C80—P4—C70—C7569.8 (4)
P1—Tc—S1—C5101.29 (15)C80—P4—C4—C3154.0 (2)
P3—Tc—S1—C5164.66 (15)Tc—P4—C4—C327.2 (3)
P4—Tc—S1—C583.56 (15)C70—P4—C4—C3106.7 (3)
S1—Tc—S2—C52.30 (15)P1—C1—C2—P251.2 (3)
P1—Tc—S2—C588.52 (15)P3—C3—C4—P448.2 (3)
P2—Tc—S2—C5171.26 (15)C15—C10—C11—C121.6 (7)
P4—Tc—S2—C588.68 (15)P1—C10—C15—C14178.9 (3)
S1—Tc—P1—C1174.01 (14)C11—C10—C15—C141.1 (6)
S1—Tc—P1—C1052.80 (17)P1—C10—C11—C12179.4 (3)
S1—Tc—P1—C2068.72 (16)C10—C11—C12—C131.1 (7)
S2—Tc—P1—C1117.92 (14)C11—C12—C13—C140.1 (7)
S2—Tc—P1—C10120.86 (17)C12—C13—C14—C150.4 (7)
S2—Tc—P1—C200.65 (16)C13—C14—C15—C100.1 (8)
P2—Tc—P1—C123.30 (14)C21—C20—C25—C241.2 (5)
P2—Tc—P1—C10144.51 (17)P1—C20—C21—C22175.8 (3)
P2—Tc—P1—C2093.97 (16)C25—C20—C21—C221.4 (5)
P3—Tc—P1—C170.60 (14)P1—C20—C25—C24175.7 (2)
P3—Tc—P1—C1050.61 (17)C20—C21—C22—C230.6 (6)
P3—Tc—P1—C20172.13 (15)C21—C22—C23—C240.3 (6)
S2—Tc—P2—C296.07 (15)C22—C23—C24—C250.4 (5)
S2—Tc—P2—C30142.78 (14)C23—C24—C25—C200.3 (5)
S2—Tc—P2—C4014.24 (16)P2—C30—C31—C32177.7 (3)
P1—Tc—P2—C21.44 (15)C35—C30—C31—C320.8 (6)
P1—Tc—P2—C30119.71 (14)P2—C30—C35—C34177.6 (3)
P1—Tc—P2—C40111.74 (16)C31—C30—C35—C341.0 (5)
P3—Tc—P2—C294.92 (15)C30—C31—C32—C330.2 (6)
P3—Tc—P2—C3026.23 (14)C31—C32—C33—C341.1 (7)
P3—Tc—P2—C40154.78 (16)C32—C33—C34—C350.8 (6)
P4—Tc—P2—C2177.05 (15)C33—C34—C35—C300.2 (6)
P4—Tc—P2—C3055.90 (14)P2—C40—C45—C44178.0 (3)
P4—Tc—P2—C4072.65 (16)C45—C40—C41—C420.4 (7)
S1—Tc—P3—C3112.45 (15)P2—C40—C41—C42179.4 (3)
S1—Tc—P3—C50129.35 (14)C41—C40—C45—C441.7 (7)
S1—Tc—P3—C603.33 (15)C40—C41—C42—C431.2 (7)
P1—Tc—P3—C3157.07 (15)C41—C42—C43—C441.3 (7)
P1—Tc—P3—C5038.88 (14)C42—C43—C44—C450.0 (7)
P1—Tc—P3—C6093.81 (15)C43—C44—C45—C401.6 (7)
P2—Tc—P3—C374.75 (15)P3—C50—C55—C54179.9 (5)
P2—Tc—P3—C5043.44 (14)P3—C50—C51—C52179.9 (7)
P2—Tc—P3—C60176.12 (15)C51—C50—C55—C540.0 (7)
P4—Tc—P3—C325.11 (15)C55—C50—C51—C520.2 (7)
P4—Tc—P3—C50143.30 (14)C50—C51—C52—C530.2 (7)
P4—Tc—P3—C6084.01 (15)C51—C52—C53—C540.9 (7)
S1—Tc—P4—C4105.74 (14)C52—C53—C54—C551.1 (7)
S1—Tc—P4—C70132.01 (18)C53—C54—C55—C500.6 (7)
S1—Tc—P4—C8010.66 (15)C61—C60—C65—C640.5 (5)
S2—Tc—P4—C4174.11 (14)P3—C60—C65—C64172.5 (3)
S2—Tc—P4—C7063.65 (18)P3—C60—C61—C62172.6 (3)
S2—Tc—P4—C8057.71 (15)C65—C60—C61—C620.4 (6)
P2—Tc—P4—C490.87 (14)C60—C61—C62—C630.1 (6)
P2—Tc—P4—C7031.38 (18)C61—C62—C63—C640.1 (6)
P2—Tc—P4—C80152.73 (15)C62—C63—C64—C650.0 (6)
P3—Tc—P4—C42.09 (15)C63—C64—C65—C600.3 (6)
P3—Tc—P4—C70124.34 (18)P4—C70—C71—C72176.6 (4)
P3—Tc—P4—C80114.31 (15)C75—C70—C71—C721.1 (7)
Tc—S1—C5—S23.4 (2)C71—C70—C75—C741.8 (7)
Tc—S2—C5—S13.4 (2)P4—C70—C75—C74177.2 (4)
C20—P1—C1—C280.1 (3)C70—C71—C72—C730.1 (8)
C1—P1—C10—C1549.4 (4)C71—C72—C73—C740.1 (9)
C20—P1—C10—C1554.9 (4)C72—C73—C74—C750.5 (8)
Tc—P1—C1—C248.7 (3)C73—C74—C75—C701.5 (8)
Tc—P1—C20—C2160.1 (3)P4—C80—C85—C84178.6 (3)
Tc—P1—C10—C119.8 (4)P4—C80—C81—C82179.4 (3)
C1—P1—C10—C11132.8 (4)C81—C80—C85—C843.1 (6)
C20—P1—C10—C11122.9 (4)C85—C80—C81—C822.2 (6)
Tc—P1—C10—C15172.5 (3)C80—C81—C82—C830.1 (7)
C10—P1—C20—C25103.6 (3)C81—C82—C83—C841.7 (7)
C1—P1—C20—C252.6 (3)C82—C83—C84—C850.8 (7)
C10—P1—C20—C2173.4 (3)C83—C84—C85—C801.6 (6)
Tc—P1—C20—C25122.9 (3)C95—C90—C91—C920.5 (7)
C1—P1—C20—C21179.5 (3)C91—C90—C95—C940.9 (7)
C10—P1—C1—C2179.7 (3)C90—C91—C92—C930.2 (7)
C40—P2—C2—C1158.6 (3)C91—C92—C93—C940.5 (7)
C40—P2—C30—C31106.6 (3)C92—C93—C94—C950.1 (7)
C30—P2—C2—C1101.3 (3)C93—C94—C95—C900.6 (7)
C30—P2—C40—C415.8 (4)C105—C100—C101—C1024 (4)
Tc—P2—C40—C41133.6 (3)C101—C100—C105—C1041 (3)
Tc—P2—C30—C31115.9 (3)C105—C100—C101—H101177.41
Tc—P2—C40—C4546.2 (4)H100—C100—C101—C102176.66
Tc—P2—C2—C132.4 (3)H100—C100—C101—H1012.31
Tc—P2—C30—C3565.7 (3)C101—C100—C105—H105179.01
C2—P2—C30—C317.8 (3)H100—C100—C105—C104179.27
C2—P2—C40—C41109.9 (4)H100—C100—C105—H1050.70
C40—P2—C30—C3571.8 (3)C100—C101—C102—H102177.06
C2—P2—C30—C35170.6 (3)H101—C101—C102—C103177.16
C2—P2—C40—C4570.3 (4)H101—C101—C102—H1021.91
C30—P2—C40—C45174.4 (3)C101—C102—C103—H103178.67
C50—P3—C3—C4177.2 (3)H102—C102—C103—C104179.48
Tc—P3—C3—C449.5 (3)H102—C102—C103—H1030.40
Tc—P3—C60—C6114.6 (4)C102—C103—C104—H104178.92
C3—P3—C60—C61100.8 (3)H103—C103—C104—C105178.71
C60—P3—C3—C478.1 (3)H103—C103—C104—H1041.20
C60—P3—C50—C5159.9 (4)C103—C104—C105—H105178.59
C3—P3—C50—C5523.0 (4)H104—C104—C105—C100178.70
C60—P3—C50—C55120.0 (4)H104—C104—C105—H1051.32
C50—P3—C60—C61157.5 (3)C117—C112—C113—H113179.97
Tc—P3—C60—C65172.7 (3)H112—C112—C113—C114180.00
C3—P3—C60—C6571.9 (3)H112—C112—C113—H1130.07
C50—P3—C60—C6529.7 (3)C113—C112—C117—H117179.96
Tc—P3—C50—C5181.8 (4)H112—C112—C117—C116179.96
C3—P3—C50—C51156.8 (4)H112—C112—C117—H1170.02
Tc—P3—C50—C5598.3 (4)C112—C113—C114—H114180.00
C70—P4—C80—C8145.0 (3)H113—C113—C114—C115179.97
Tc—P4—C70—C75159.0 (3)H113—C113—C114—H1140.08
Tc—P4—C70—C7125.6 (4)C113—C114—C115—H115179.98
C80—P4—C70—C71105.6 (4)H114—C114—C115—C116179.96
C4—P4—C70—C7533.6 (4)H114—C114—C115—H1150.07
Tc—P4—C80—C8588.8 (3)C114—C115—C116—H116180.00
C4—P4—C70—C71151.0 (4)H115—C115—C116—C117179.96
C4—P4—C80—C81149.7 (3)H115—C115—C116—H1160.03
C70—P4—C80—C85136.7 (3)C115—C116—C117—H117179.98
Tc—P4—C80—C8189.5 (3)H116—C116—C117—C112180.00
C4—P4—C80—C8532.0 (3)H116—C116—C117—H1170.03
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C11—H11···S10.94952.73293.469 (4)134.85
C21—H21···S10.95042.83953.675 (5)147.23
C45—H45···S20.95052.61073.199 (4)120.44
C61—H61···S10.94952.54503.438 (5)156.84
C71—H71···S20.94912.81673.587 (4)139.00
C105—H105···S10.94982.87973.544 (11)127.94

Experimental details

Crystal data
Chemical formula[Tc(CHS2)(C26H24P2)2]·3C6H6
Mr1207.2
Crystal system, space groupTriclinic, P1
Temperature (K)193
a, b, c (Å)14.132 (4), 14.738 (6), 17.031 (4)
α, β, γ (°)65.79 (3), 88.10 (3), 67.88 (3)
V3)2966 (2)
Z2
Radiation typeMo Kα
µ (mm1)0.46
Crystal size (mm)0.35 × 0.23 × 0.15
Data collection
DiffractometerNonius CAD-4
diffractometer
Absorption correctionψ scan
(SHELXTL-Plus; Siemens, 1990)
Tmin, Tmax0.854, 0.934
No. of measured, independent and
observed [I > 2σ(I)] reflections
10893, 10431, 7752
Rint0.029
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.104, 1.04
No. of reflections10431
No. of parameters768
No. of restraints219
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.56, 0.43

Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, XCAD4 (Harms, 1993), SHELXS86 (Sheldrick, 1985), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), PLATON (Spek, 2000).

Selected geometric parameters (Å, º) top
Tc—S12.4866 (14)Tc—P22.3632 (14)
Tc—S22.4548 (15)Tc—P32.3566 (14)
Tc—P12.3650 (14)Tc—P42.3884 (14)
S1—Tc—S268.38 (4)S2—Tc—P485.93 (5)
S1—Tc—P189.52 (4)P1—Tc—P282.05 (4)
S1—Tc—P2160.79 (5)P1—Tc—P394.05 (4)
S1—Tc—P3103.41 (5)P1—Tc—P4175.03 (5)
S1—Tc—P489.41 (4)P2—Tc—P394.42 (5)
S2—Tc—P198.18 (5)P2—Tc—P4100.39 (4)
S2—Tc—P295.66 (5)P3—Tc—P481.48 (4)
S2—Tc—P3165.10 (5)S1—C5—S2112.5 (3)
 

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