Temperature-resolved study of three [M(M′O4)4(TBPO)4] complexes (MM′ = URe, ThRe, ThTc)

Helliwell, M.; Collison, D.; John, G.H.; May, I.; Sarsfield, M.J.; Sharrad, C.A.; Sutton, A.D.

doi:10.1107/S0108768105036931

research papers

STRUCTURAL SCIENCE
CRYSTAL ENGINEERING
MATERIALS

ISSN: 2052-5206

Volume 62| Part 1| February 2006| Pages 68-85

doi:10.1107/S0108768105036931

Temperature-resolved study of three [M(M′O₄)₄(TBPO)₄] complexes (MM′ = URe, ThRe, ThTc)

Madeleine Helliwell,^a ^* David Collison,^a Gordon H. John,^b Iain May,^a Mark J. Sarsfield,^a,^c Clint A. Sharrad ^a and Andrew D. Sutton ^a

^aSchool of Chemistry, The University of Manchester, Manchester M13 9PL, England, ^bCentre for Radiochemistry Research, School of Chemistry, The University of Manchester, Manchester M13 9PL, England, and ^cBNFL, Sellafield, Seascale, Cumbria CA20 1PG, England
^*Correspondence e-mail: madeleine.helliwell@manchester.ac.uk

(Received 24 February 2005; accepted 9 November 2005)

The crystal structures of the title complexes were measured at several temperatures between room temperature and 100 K. Each sample shows reversible crystal-to-crystal phase transitions as the temperature is varied. The behaviour of [U(ReO₄)₄(TBPO)₄] (I) and [Th(ReO₄)₄(TBPO)₄] (II) (TBPO = tri-n-butylphosphine oxide) is very similar; at room temperature, crystals of (I) and (II) are isostructural, with space group $[I\bar 42m]$ , and reducing the temperature to 100 K causes a lowering of the space-group symmetry to C-centred cells, space groups Cc for (I) and Cmc2₁ for (II). The variation of lattice symmetry of [Th(TcO₄)₄(TBPO)₄] (III) was found to be somewhat different, with the body-centred cubic space group, $[I\bar 43m]$ , occurring at 293 K, a reduction of symmetry at 230 K to the C-centred orthorhombic space group, Cmc2₁, and a further transition to the primitive orthorhombic space group, Pbc2₁, below 215 K. Elucidation of the correct space-group symmetry and the subsequent refinement was complicated in some cases by the twinning by pseudo-merohedry that arises from the lowering of the space-group symmetry, occurring as the temperature is reduced. All three of the crystal structures determined at room temperature have high atomic displacement parameters, particularly of the ⁿBu groups, and (III) shows disorder of some of the O atoms. The structures in the space group Cmc2₁, show some disorder of ⁿBu groups, but are otherwise reasonably well ordered; the structures of (I) in Cc and (III) in Pbc2₁ are ordered, even to the ends of the alkyl chains. Inter-comparison of the structures measured below 293 K, using the program OFIT from the SHELXTL package, showed that generally, they are remarkably alike, with weighted r.m.s. deviations of the M, M′ and P atoms of less than 0.1 Å, as are the 293 K structures of (I) and (II) with their low-temperature counterparts. However, the structure of (III) measured in the space group Cmc2₁ is significantly different from both the structure of (III) at 293 K and that found below 215 K, with weighted r.m.s. deviations of the Th, Tc and P atoms of 0.40 and 0.37 Å, respectively. An extensive network of weak intra- and intermolecular C—H⋯O hydrogen bonds found between the atoms of the ⁿBu and [M′O₄] groups probably influences the packing and the overall geometry of the molecules.

Keywords: phase transitions; twinning; merohedry; hydrogen bonds.

1. Introduction

Research into the coordination chemistry of actinides is important for the design of the safe processing of irradiated nuclear fuel. Uranium and plutonium are separated from fission products for recovery in the PUREX process (plutonium and uranium recovery by extraction). Extraction of U and Pu is achieved using a 30% TBP/kerosene mixture (TBP = tri-n-butylphosphate) as the organic phase, with an approximately 3 M nitric acid aqueous phase, containing the majority of the fission products. However, it is well established that the fission product technetium (as [TcO₄]⁻) follows the organic phase with indirect evidence, suggesting this anion coordinates to hexavalent {UO₂²⁺} and tetravalent (Pu⁴⁺, Zr⁴⁺) metal centres (Wilson, 1996 ). Technetium-99 was first identified as a fission product of uranium-238 when it was isolated in very small quantities from African pitchblende (Kenna & Kuroda, 1961 ). It is a β emitter (t_½ = 2.1 × 10⁵ years) and has a specific activity of 6.2 × 10⁸ Bq g⁻¹. The chemistry of technetium is similar to that of rhenium and the anions, [TcO₄]⁻ and [ReO₄]⁻, are closely related `weakly coordinating anions', although much less is known about the former because of its radioactivity. [ReO₄]⁻ is known to bind to transition elements and lanthanides (Chakravorti, 1990 ), but there are few crystal structures of [ReO₄]⁻ and [TcO₄]⁻ binding to actinides, although there is spectroscopic evidence for their existence (Bol'shakov et al., 1967 ). Recently, we reported the isostructural crystal structures of [UO₂(ReO₄)₂(TPPO)₃] and [UO₂(TcO₄)₂(TPPO)₃] (TPPO = triphenylphosphine oxide), in which ReO₄^- and TcO₄^- are bound to U(VI) (John et al., 2004 ; Sarsfield et al., 2004 ) and the neptunyl(VI) pertechnetate complex [(NpO₂)₂(TcO₄)₂·3H₂O)] has also been reported (Fedosseev et al., 2003 ). Here we describe the structural characterization of model complexes of pertechnetate coordinating to tetravalent actinides, namely, [U(ReO₄)₄(TBPO)₄] (I), [Th(ReO₄)₄(TBPO)₄] (II) and [Th(TcO₄)₄(TBPO)₄] (III) (TBPO = tri-n-butylphosphine oxide)], which may be related to the extracted species formed in solution during the PUREX process; compound (III) is the first example of a tetravalent actinide coordinated to pertechnetate. Interestingly, all three complexes exhibit a number of temperature-resolved reversible crystal-to-crystal phase transitions, which we describe in this paper; the crystal structure of (III) at 100 K has been reported previously in Sarsfield et al. (2004).

2. Experimental

The synthesis and method of crystal growth for (I)–(III) have been reported previously (John, 2003 ; Sutton, 2003 ; Sarsfield et al. 2004).

Crystals of (I) and (II) were mounted on glass fibres, but owing to the radioactive hazard of (III) it was necessary to triply contain a crystal in a Lindemann capillary tube; triple containment involves coating the crystal in oil or epoxy resin and it is then placed in a capillary, the second layer of containment being provided by the glass of the tube. The third layer is gained by painting the capillary tube with clear nail varnish. Data were collected on a Bruker Apex CCD diffractometer (Bruker, 2001 ) or in one case [(I) at 100 K, §2.2.3 below] a Rigaku RAXIS IIc image-plate diffractometer, with temperature variation achieved using an Oxford Cryostream. Data processing was carried out using the SAINT package for the Bruker APEX data (Bruker, 2002 ), DENZO and SCALEPACK (Otwinowski, 1988 ) for the RAXIS data, and the SHELXTL package was used for structure solution and refinement and graphical work (Bruker, 2001). The crystal structures were solved by direct methods, unless an isostructural model was used as the starting point, and H atoms were included in calculated positions. Additional details applying to individual crystal structures are described below. Tables 1, 2 and 3 summarize the crystal data measured at the various temperatures, for (I), (II) and (III), respectively. Fig. 1 shows the numbering scheme adopted for the structures and ORTEP plots for each crystal structure are illustrated in Figs. 2(a) to (m).

Table 1
Experimental details for (I)

	(I) at 293 K	(I) at 230 K	(I) at 165 K	(I) at 100 K
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U
M_r	2112.05	2112.05	2112.05	2112.05
Cell setting, space group	Tetragonal, $[I\bar 42m]$	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁	Monoclinic, Cc
a, b, c (Å)	15.5404 (6), 15.5404 (6), 14.8191 (11)	21.5289 (15), 21.9148 (16), 14.8288 (11)	21.4344 (15), 21.7929 (15), 14.7782 (10)	21.40 (2), 21.68 (2), 14.78 (2)
α, β, γ (°)	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00 (3), 90.00
V (Å³)	3578.9 (3)	6996.3 (9)	6903.2 (8)	6857 (13)
Z	2	4	4	4
Dx (Mg m⁻³)	1.960	2.005	2.032	2.046
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
No. of reflections for cell parameters	3188	5703	7236	49029
θ range (°)	2.6–20.8	2.6–26.2	2.7–26.4	2.3–25.0
μ (mm⁻¹)	9.14	9.35	9.48	9.55
Temperature (K)	293 (2)	230 (2)	165 (2)	100 (2)
Crystal form, colour	Block, green	Block, green	Block, green	Prismatic, green
Crystal size (mm)	0.15 × 0.15 × 0.10	0.15 × 0.15 × 0.10	0.15 × 0.15 × 0.10	0.12 × 0.1 × 0.08

Data collection
Diffractometer	CCD area detector	CCD area detector	CCD area detector	Rigaku RAXIS
Data collection method	φ and ω scans	φ and ω scans	φ and ω scans	103 × 3° φ scans
Absorption correction	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	None
T_min	0.341	0.334	0.331	–
T_max	0.462	0.455	0.451	–
No. of measured, independent and observed reflections	10 483, 1941, 1699	25 273, 6529, 6180	24 887, 6428, 6171	49 029, 11 595, 11431
Criterion for observed reflections	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)
R_int	0.029	0.027	0.029	0.06
θ_max (°)	26.4	25.0	25.0	25.0
Range of h, k, l	−19 → h → 15	−25 → h → 25	−25 → h → 25	−25 → h → 25
	−17 → k → 19	−26 → k → 26	−25 → k → 25	−25 → k → 25
	−18 → l → 17	−17 → l → 17	−17 → l → 17	−17 → l → 17

Refinement
Refinement on	F²	F²	F²	F²
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.099, 1.09	0.027, 0.068, 1.12	0.025, 0.065, 1.11	0.032, 0.080, 1.05
No. of reflections	1941	6529	6428	11 595
No. of parameters	102	377	417	698
H-atom treatment	Constrained to parent site	Constrained to parent site	Constrained to parent site	Constrained to parent site
Weighting scheme	w = 1/[σ²(F_o²) + (0.0614P)²], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0273P)² + 21.6652P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0227P)² + 46.403P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0247P)² + 70.409P], where P = (F_o² + 2F_c²)/3
(Δ/σ)_max	0.001	0.002	0.007	0.001
Δρ_max, Δρ_min (e Å⁻³)	1.03, −0.38	2.23, −1.05	2.33, −1.21	1.77, −1.87
Extinction method	None	None	None	SHELXL
Extinction coefficient	–	–	–	0.000349 (19)
Absolute structure	Flack (1983 )	Flack (1983)	Flack (1983)	Flack (1983)
Flack parameter	0.03 (2)	0.025 (9)	0.020 (9)	0

Table 2
Experimental details for (II)

	(II) at 293 K	(II) at 230 K	(II) at 165 K	(II) at 100 K
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th
M_r	2106.06	2106.06	2106.06	2106.06
Cell setting, space group	Tetragonal, $[I\bar 42m]$	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁
a, b, c (Å)	15.5577 (12), 15.5577 (12), 14.8730 (17)	21.721 (3), 21.738 (3), 14.8793 (19)	21.610 (3), 21.623 (3), 14.8324 (19)	21.535 (3), 21.548 (3), 14.7950 (19)
α, β, γ (°)	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00
V (Å³)	3599.9 (6)	7025.4 (16)	6930.7 (15)	6865.4 (15)
Z	2	4	4	4
D_x (Mg m⁻³)	1.943	1.991	2.018	2.038
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
No. of reflections for cell parameters	1544	5355	5437	8488
θ range (°)	2.7–20.5	2.6–23.0	2.7–25.9	2.7–26.5
μ (mm⁻¹)	8.91	9.13	9.25	9.34
Temperature (K)	293 (2)	230 (2)	165 (2)	100 (2)
Crystal form, colour	Plate, colourless	Plate, colourless	Plate, colourless	Block, colourless
Crystal size (mm)	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10

Data collection
Diffractometer	CCD area detector	CCD area detector	CCD area detector	CCD area detector
Data collection method	φ and ω scans	φ and ω scans	φ and ω scans	φ and ω scans
Absorption correction	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)
T_min	0.297	0.290	0.689	0.284
T_max	0.470	0.462	1.000	0.455
No. of measured, independent and observed reflections	5728, 1932, 1605	18 098, 6391, 6029	24 808, 6458, 6367	24 358, 6390, 6376
Criterion for observed reflections	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)
R_int	0.028	0.042	0.036	0.034
θ_max (°)	26.4	25.0	25.0	25.0
Range of h, k, l	−19 → h → 7	−25 → h → 25	−25 → h → 25	−25 → h → 25
	−12 → k → 16	−12 → k → 25	−25 → k → 25	−25 → k → 25
	−16 → l → 18	−16 → l → 17	−17 → l → 17	−17 → l → 17

Refinement
Refinement on	F²	F²	F²	F²
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.117, 1.01	0.036, 0.076, 1.07	0.026, 0.054, 1.06	0.027, 0.059, 1.16
No. of reflections	1932	6391	6458	6390
No. of parameters	102	393	372	393
H-atom treatment	Constrained to parent site	Constrained to parent site	Constrained to parent site	Constrained to parent site
Weighting scheme	w = 1/[σ²(F_o²) + (0.0736P)²], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0314P)² + 8.8462P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0201P)² + 25.4516P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0121P)² + 76.2392P], where P = (F_o² + 2F_c²)/3
(Δ/σ)max	<0.0001	<0.0001	0.002	0.002
Δρ_max, Δρ_min (e Å⁻³)	0.79, −0.59	1.13, −1.55	1.10, −1.05	1.62, −1.34
Extinction method	None	None	None	None
Absolute structure	Flack (1983)	Flack (1983)	Flack (1983)	Flack (1983)
Flack parameter	0.09 (4)	0.037 (15)	0.011 (11)	0.027 (13)

Table 3
Experimental details for (III)

	(III) at 293 K	(III) at 230 K	(III) at 170 K	(III) at 130 K	(III) at 100 K
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th
M_r	1753.26	1753.26	1753.26	1753.26	1753.26
Cell setting, space group	Cubic, $[I\bar 43m]$	Orthorhombic, Cmc2₁	Orthorhombic, Pbc2₁	Orthorhombic, Pbc2₁	Orthorhombic, Pbc2₁
a, b, c (Å)	15.3423 (10), 15.3423 (10), 15.3423 (10)	21.444 (2), 21.582 (2), 14.736 (2)	21.417 (6), 21.649 (6), 14.848 (4)	21.358 (13), 21.651 (13), 14.790 (9)	21.386 (4), 21.732 (4), 14.820 (2)
α, β, γ (°)	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00	90.00, 90.00, 90.00
V (Å³)	3611.4 (4)	6819.9 (13)	6885 (3)	6839 (7)	6888 (2)
Z	2	4	4	4	4
D_x (Mg m⁻³)	1.612	1.708	1.692	1.703	1.691
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα	Mo Kα
No. of reflections for cell parameters	1959	5437	7727	5490	5577
θ range (°)	2.6–20.0	2.7–25.9	2.7–26.3	2.7–26.1	2.3–26.4
μ (mm⁻¹)	2.95	3.12	3.09	3.11	3.09
Temperature (K)	293 (2)	230 (2)	170 (2)	130 (2)	100 (2)
Crystal form, colour	Prism, colourless	Block, colourless	Block, colourless	Block, colourless	Block, colourless
Crystal size (mm)	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10

Data collection
Diffractometer	CCD area detector	CCD area detector	CCD area detector	CCD area detector	CCD area detector
Data collection method	φ and ω scans	φ and ω scans	φ and ω scans	φ and ω scans	φ and ω scans
Absorption correction	None	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)	Multi-scan (based on symmetry-related measurements)
T_min	–	0.746	0.748	0.746	0.748
T_max	–	0.746	0.748	0.746	0.748
No. of measured, independent and observed reflections	6235, 723, 651	26 789, 7255, 6041	54 013, 14 267, 12 482	50 705, 14 038, 12 090	35 481, 13 901, 12 000
Criterion for observed reflections	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)	I > 2σ(I)
R_int	0.041	0.055	0.074	0.090	0.073
θ_max (°)	26.3	26.5	26.5	26.4	26.6
Range of h, k, l	−12 → h → 18	−26 → h → 26	−26 → h → 26	−26 → h → 26	−25 → h → 26
	−3 → k → 19	−26 → k → 26	−27 → k → 27	−26 → k → 26	−25 → k → 27
	−19 → l → 18	−17 → l → 18	−18 → l → 18	−17 → l → 18	−18 → l → 18

Refinement
Refinement on	F²	F²	F²	F²	F²
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.101, 1.01	0.037, 0.088, 0.97	0.050, 0.127, 1.08	0.053, 0.130, 1.05	0.062, 0.161, 1.09
No. of reflections	723	7255	14 267	14 038	13 901
No. of parameters	50	354	707	707	707
H-atom treatment	Constrained to parent site	Constrained to parent site	Constrained to parent site	Constrained to parent site	Constrained to parent site
Weighting scheme	w = 1/[σ²(F_o²) + (0.0666P)²], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0428P)²], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.042P)² + 14.969P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0001P)² + 21.3104P], where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0606P)² + 22.3563P], where P = (F_o² + 2F_c²)/3
(Δσ)_max	0.002	0.004	0.002	0.004	0.003
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.27	1.43, −0.77	3.57, −0.88	3.15, −1.14	4.83, −3.49
Extinction method	None	None	None	None	None
Absolute structure	Flack (1983)	Flack (1983)	Flack (1983)	Flack (1983)	Flack (1983)
Flack parameter	0.00 (2)	0.034 (7)	0.016 (6)	0.017 (6)	0.020 (8)
Computer programs used: Bruker SMART (Bruker, 2001), MSC RAXIS11 Control, DENZO (Otwinowski, 1988), SAINT (Bruker, 2002), SHELXS97 (Sheldrick, 1997 ), SIR97 (Altomare et al. 1999 ), SHELXL97 (Sheldrick, 1997), SHELXTL, TEXSAN (Molecular Structure Corporation, 1995 ).

Figure 1
Ball-and-stick plot showing the numbering scheme for all the structures at 230 K and below.

Figure 2
Plots of (I), (II) and (III) with H atoms omitted for clarity. The same view has been used for all plots to allow comparison of the structures. For (I) M = U and M′ = Re, for (II) M = Th and M′ = Re and for (III) M = Th and M′ = Tc. ORTEP plots are with 30% probablility displacement ellipsoids. (a) (I) at 293 K; (b) (I) at 230 K; (c) (I) at 165 K; (d) (I) at 100 K; (e) (II) at 293 K; (f) (II) at 230 K; (g) (II) at 165 K; (h) (II) at 100 K; (i) (III) at 293 K; (j) (III) at 230 K; (k) (III) at 170 K; (l) (III) at 130 K; (m) (III) at 100 K.

2.1. Investigation of possible pseudo-merohedral twinning

To assess whether the lowering of the symmetry with temperature led to any pseudo-merohedral twinning, which is commonly seen in such cases (see Herbst-Irmer & Sheldrick, 1998 ; Parsons, 2003 , for example), careful examination of the raw diffraction images was made of each of the data sets of the lower-symmetry space groups, measured at 230 K and below. This showed that some reflections were slightly split, i.e not into individual components, but rather into a peak with a shoulder. Evaluation trials were made increasing the box sizes (i.e. integration limits) by 25 and 50%, respectively, of the initially determined box size. It was, however, found that the box size optimized originally in the matrix determination from the raw images, and then during the SAINT data processing, had in fact led to the optimum precision in terms of the R_int and final R values. For instance, for the 100 K structure of (II), which showed the greatest degree of pseudo-merohedral twinning, increasing the box size by 25% led to an R_int of 0.0441 and a final conventional R value of 0.0339, and increasing the box size by 50% gave an R_int = 0.0406 and a conventional R = 0.0297. These values are both higher than those obtained by the normal SAINT data reduction procedures which gave an R_int = 0.0336 and a conventional R value of 0.0268, presumably because when the box size was increased too much background was being included with the peak. Similar results were obtained for the other low-temperature crystal structures and therefore normal data processing procedures, with optimized box sizes, were adopted for all the data sets measured using the Bruker APEX diffractometer. For the crystal structure of (I) at 100 K, measured on the RAXIS II, the box size was chosen manually to fully encompass the reflections, during the DENZO data processing.

In some cases the application of more than one twin law might in theory be necessary for the possible monoclinic space groups and tests were made, for data collected using the Bruker APEX diffractometer, using the program TWINABS (Sheldrick, 2002 ), which allows the application of multiple twin laws; the treatment adopted for each compound is described fully in the supplementary information¹ and the results are summarized here.

Each compound showed a reduction of symmetry at 230 K. The lattice type became primitive owing to a doubling of the number of diffraction spots and although the cell dimensions were still similar, the crystals were no longer tetragonal; the primitive unit cells could be transformed to C-centred lattices. Three space-group choices were possible, either Cmc2₁ or Cc in the C-centred lattice or P2₁ in the primitive lattice. Refinement in Cmc2₁ was carried out using the twin law (0 1 0/ 1 0 0/ 0 0 −1) to account for the possible pseudo-merohedral twinning arising from the fact that the metric symmetry of the unit cells, which appears to be tetragonal due to the similarity of a and b, was higher than the symmetry of the structures. However, although the agreement factors for each structure refined in the space group Cmc2₁ were excellent (see Tables 1, 2 and 3), there was disorder seen in the ⁿBu group C13–C16, and for the atom C25. Therefore, the space groups Cc and P2₁ were also investigated to see whether by lowering the symmetry still further, this disorder could be removed.

For the space group Cc, because the metric symmetry was approximately tetragonal, but the symmetry to be tested was monoclinic, to fully deal with possible pseudo-merohedral twinning, the twin laws (0 1 0/1 0 0/0 0 −1), (1 0 0/0 −1 0/0 0 −1) and (0 1 0/−1 0 0/0 0 1), together with inversion twinning for each domain might, in theory, all be necessary. Likewise, for the space group P2₁, the possible twin laws are (1 0 0/0 −1 0/0 0 −1), (0 0 1/0 −1 0/1 0 0) and (0 0 1/0 1 0/−1 0 0), together with inversion twinning for each domain. Therefore, for each structure which could be refined in the space group Cmc2₁, the lower-symmetry space groups Cc and P2₁ were also investigated, with the application of the multiple twin laws using the program TWINABS (Sheldrick, 2002). The treatment used for each compound, at each possible temperature, is fully described in the supplementary information and the final choice of space groups is discussed in §3.1. However, in summary, for (I), the space group Cmc2₁ was found to be best for all temperatures from 230 K and below, except for the RAXIS II data measured at 100 K, for which Cc gave the optimal results. Also, there was essentially no twinning observed for the structures of (I) in Cmc2₁. There was, however, a degree of twinning for the structure of (I) in Cc, arising from the orthorhombic metric symmetry, but monoclinic symmetry of the structure; the extent of this twinning was ca 14% and the twin law used to account for it was (1 0 0/0 −1 0/0 0 −1). For (II), the space group Cmc2₁ was optimal for all the structures at 230 K and below, including that at 100 K; for this sample a high degree of pseudo-merohedral twinning (twin fraction, approximately 50%) was observed at each of the temperatures, arising from the fact that the metric symmetry was approximately tetragonal, but the symmetry of the structure was orthorhombic [twin law (0 1 0/ 1 0 0/ 0 0 −1)]; for (III), the space group at 230 K was found to be Cmc2₁, rather than Cc or P2₁, and a much lower degree of pseudo-merohedral twinning [twin law (0 1 0/ 1 0 0/ 0 0 −1)] was observed than for (II), of 17.4 (1)%. At lower temperatures, the space-group symmetry of (III) was Pbc2₁ and the twin fraction refined to values between ca 7 and 8%.

Therefore, in all cases it was possible to describe the twinning using a single twin law in the instruction file, with in one case [(I) at 100 K], additional racemic twinning. That the twinning is suitably explained using a single twin law is also indicated by the precision of the structures, in terms of the excellent R values, the stability of the refinements and the fact that the geometry was reasonable.

Further details about all the refinements for (I), (II) and (III) are reported in the experimental details below (§§2.2–2.4 ) and the choice of space groups is discussed in §3.1.

2.2. [U(ReO₄)₄(TBPO)₄] (I)

2.2.1. 293 K

An initial structure solution located the U, Re and O atoms. The C atoms of the ⁿBu groups were then found by successive difference-Fourier cycling techniques; their thermal motion is very high and restraints were used on their bond lengths and angles. The non-H atoms were refined anisotropically, with restraints applied to those of the ⁿBu C atoms.

2.2.2. 230 and 165 K

The structures, which were found to be in the space group Cmc2₁ (see above and the supplementary information ) are isostructural with (III), measured at 230 K (see §2.4.2), whose structure was used as a starting point, and a similar refinement method was used. Tests were made to determine whether the crystal was twinned with the twin matrix (0 1 0/1 0 0/0 0 −1); the twin fraction refined to values of 0.0131 (4) and 0.0200 (4) for the 230 and 165 K structures, respectively. These refined values showed that there was essentially no twinning seen for the structures of (I) in the space group Cmc2₁. C25 is disordered, with the other component related by mirror symmetry; the ⁿBu group, C13–C16, is disordered over two sites, whose occupancy was constrained to sum to 1.0.

2.2.3. 100 K

The data were collected using the RAXIS in 105 × 3° phi oscillations of 10 min per exposure on a Mo Kα Rigaku rotating-anode generator. The crystal was a racemic twin, as well as having twinning arising from the approximate 90° β angle. The extent of the latter twinning was ∼ 13.8 (9)% and the matrix employed to account for this was (1 0 0/0 −1 0/0 0 −1); the application of the twin law reduced the R value from 0.0418 to 0.0321. Clearly, there might have been additional twinning arising from the similarity of a and b, but with the excellent precision, stability of the refinement and lack of the need for restraints on the parameters, it was assumed that the single twin matrix, with account taken of the additional racemic twinning was sufficient to describe the situation properly. Moreover, this corresponds with the lack of such twinning found in the 230 and 165 K crystal structures (see above and the supplementary information ).

2.3. [Th(ReO₄)₄(TBPO)₄] (II)

2.3.1. 293 K

The model for the 293 K structure of (I) (the isostructural U/Re equivalent) was used as a starting point and the refinement details are as described above (§2.2.1).

2.3.2. 230 and 165 K

The structures are isostructural with (III), measured at 230 K, i.e. in space group Cmc2₁ (see the supplementary information and §3.1 for a full discussion of the choice of space group), whose parameters were used initially and the refinement details and patterns of disorder are similar (see §2.4.2). The crystal was twinned such that the twin matrix was (0 1 0/ 1 0 0/ 0 0 −1) and the twin fraction refined to similar values of 0.478 (1) and 0.489 (1) for the 230 and 165 K structures, respectively; without the application of the twin matrix, the refinement of the structure was unstable and the R values were around 0.19, whereas introducing the twin law reduced the R values to 0.0398 and 0.0260, respectively, and led to stable refinements. As is often the case with a high degree of twinning, some restraints of the geometric parameters of the ⁿBu groups, as well as the anisotropic thermal parameters, was required (Herbst-Irmer & Sheldrick, 1998).

2.3.3. 100 K

The structure is isostructural with that of (II) measured at 165 K and the refined model was used as a starting point (see supplementary information and §3.1 for a full discussion of the choice of space group). The crystal was twinned with the twin matrix (0 1 0/ 1 0 0/ 0 0 −1) and the twin fraction refined to 0.496 (1). As in the case of the 230 and 165 K structures of (II), the application of the twin law was essential in providing a stable refinement, with an excellent final R value of 0.0268. Further details of the structure refinement are the same as in §2.3.2.

2.4. [Th(TcO₄)₄(TBPO)₄] (III)

2.4.1. 293 K

Non-H atoms were refined anisotropically, with restraints on the a.d.p.s of the O and C atoms and the geometry of the ⁿBu group. The O atoms bonded to Th are disordered over three sites, related by space-group symmetry; this disorder was not removed when the symmetry was lowered.

2.4.2. 230 K

The space group was found to be Cmc2₁ (see supplementary information and §3.1 for a full discussion of the choice of space group). The crystal was twinned such that the twin matrix was (0 1 0/1 0 0/0 0 −1) and the twin fraction refined to a value of 0.174 (1); the introduction of the twin law to the refinement significantly reduced the R value from 0.0557 to 0.0373. The asymmetric unit contains ½ of the molecule. C25 is disordered over two sites related by mirror symmetry. C13 is also disordered over two sites whose occupancies were constrained to sum to unity. Restraints were applied to the bond lengths and angles of some of the atoms of the ⁿBu groups. The non-H atoms, except the disordered C atoms, were refined anisotropically, using restraints for those of the partially occupied C atoms.

2.4.3. 170, 130 and 100 K

Initially, the crystal structure was solved by direct methods in the space group Pbc2₁, then having verified that this indeed was the correct space-group symmetry, the expanded structure solution at 230 K was used as a starting point with the origin shifted by 0.25 −0.25 −0.15. This was to obtain an equivalent numbering scheme in the lower symmetry for ease of comparison of the structures with the higher temperature structures in the space group Cmc2₁. The structures obtained by direct solution and by expansion and shifting of the origin were exactly equivalent. The crystal was twinned such that the twin matrix was (0 1 0/ 1 0 0/ 0 0 −1) and the twin fractions refined to values of 0.088 (1), 0.071 (1) and 0.073 (1), respectively. A few restraints were applied to the bond lengths and angles of the atoms of the ⁿBu groups.

2.5. Determination of C—H hydrogen bonds

An extensive network of possible weak intra- and intermolecular C—H⋯O hydrogen bonds was found between the C atoms of the ⁿBu groups and the O atoms of the [M′O₄] groups. The H-atom positions were calculated and are reasonably certain, except for those of the methyl groups; for these H atoms, it was necessary to calculate the H-atom positions to provide a staggered conformation with respect to the bonding CH₂, rather than from the torsion angle that maximized the electron density. The latter method is preferable, particularly for hydrogen-bond determination, since it allows the optimum positioning of the methyl H atoms, but was not possible in this study because the H-atom electron density was masked by that from the heavy atoms. PARST, from the WinGX system (PARST, Nardelli, 1995 ; WinGX, Farrugia, 1999 ) was used to determine the C—H hydrogen bonds for distances between the donor C atom and the acceptor O atom of less than 4 Å. These hydrogen bonds were then included in the SHELXL97 refinement for the structures measured at 230 and 100 K.

3. Results

3.1. Thermotropic phase transitions

3.1.1. (I) and (II)

At 293 and 260 K, (I) and (II) crystallize in the body-centred tetragonal space group $[I\bar 42 m]$ and the asymmetric unit contains 1/8 of the molecule. The M atom [M = U for (I) and Th for (II)] lies on a special position ( $[\bar 42m]$ ) and also a number of the atoms lie on a mirror plane. Plots of the 293 K structures of (I) and (II) are shown in Figs. 2(a) and (e), which indicate the very high a.d.p.s, particularly of the ⁿBu groups. A number of lower symmetry space groups were investigated, but reducing the symmetry did not lead to an improved structural model.

Reducing the temperature to 230 K, however, did lead to a striking improvement, not just by virtue of the temperature change but also due to a change in lattice symmetry. This was manifested by a doubling of the number of diffraction spots, arising from the removal of body-centering (see Figs. 3a and b), to give a primitive unit cell of similar dimensions to that at 293 K; the primitive lattice could be transformed to a C-centred lattice. The merging R factor of 0.277 for the diffraction intensities for the crystal of (I) clearly indicated that the lattice was no longer tetragonal, but instead was either C-centred orthorhombic, monoclinic or primitive monoclinic, space groups Cmc2₁, Cc or P2₁, respectively (the latter space group using the primitive setting of the unit cell prior to transformation to the C-centred lattice); all three space groups were tried and a detailed description of the investigation and handling of possible pseudo-merohedral twinning for the possible monoclinic space groups is described in the supplementary information and summarized in §2. Eventually, the space group Cmc2₁ was selected as the most satisfactory for the final refinement, for a number of reasons; firstly, the solution in P2₁ showed the same patterns of high a.d.p.s or disorder as were observed in Cmc2₁, and in fact in many cases, the thermal ellipsoids were found to be more eccentric; the conventional R value was also higher, at 0.032 (versus 0.027), although the R_int values were very similar at 0.024 and 0.027, for P2₁ and Cmc2₁, respectively. For Cc the conventional R factor was 0.028 and the R_int was 0.023, but there were problems with the a.d.p.s of the C and O atoms, including a non-positive definite C atom. Finally, the C—C bond length precision was best in the space group Cmc2₁ at 0.018 Å (versus 0.021 and 0.028 Å for P2₁ and Cc, respectively). The final structure in Cmc2₁ is shown in Fig. 2(b).

Figure 3
Diffraction patterns showing the differing lattice types at different temperatures [at identical setting for (a) and (b), and for (c), (d) and (e)]. (a) (I) at 293 K, showing the body-centred tetragonal lattice; (b) (I) at 230 K, where the lattice has become C-centred orthorhombic; (c) (III) at 260 K, showing the body-centred cubic lattice; (d) (III) at 230 K, where the lattice has become C-centred orthorhombic; (e) (III) at 205 K, where the lattice has become primitive orthorhombic.

The choice of space group for (II) at 230 K was complicated still further by the fact that the merging R value suggested that the lattice symmetry was primitive tetragonal; a number of space groups were tried, but it became clear that the symmetry was lower, as for (I); again the space groups Cmc2₁, Cc and P2₁ were all tested, but for analogous reasons as for (I), Cmc2₁ was finally selected as the optimum (see the supplementary information for a detailed description of the investigation and handling of possible pseudo-merohedral twinning for the possible monoclinic space groups); the structure is shown in Fig. 2(f). In this case the degree of pseudo-merohedral twinning with the twin law (0 1 0/ 1 0 / 0 0 −1) was found to be very high at 47.8 (1)%, probably because the a and b unit-cell parameters are much more similar than for (I), where essentially no such twinning was seen (§2). The high degree of twinning explains the apparent tetragonal symmetry of the diffraction pattern (Herbst-Irmer & Sheldrick 1998; Parsons, 2003). The space group of the crystal structures of (I) and (II), measured at 165 K, were also deduced to be Cmc2₁ after trials in all three possible space groups; plots are shown in Fig. 2(c) and (g).

Somewhat ambiguous results were obtained for (I) at 100 K; data collection was originally carried out using the RAXIS 11 image-plate diffractometer, and again structure solution and refinement were carried out in the space groups Cmc2₁, Cc and P2₁. Both the P2₁ and Cmc2₁ groups were discounted, owing to the presence of regions of disorder and/or non-positive definite thermal parameters not present in Cc. Moreover, refinement in the space group Cc was possible without any restraints on the geometry or the thermal parameters, in contrast to refinement in P2₁ and Cmc2₁, and the structure was well ordered, even to the ends of the ⁿBu groups. The R value was also better in Cc than in P2₁ and Cmc2₁ (0.032 versus 0.041 and 0.037, respectively). Thus, on balance, the space group Cc was preferred for the final refinement, using this particular data set, and the structure is plotted in Fig. 2(d). Later, a further set of data on a different crystal was collected at 100 K, using the Bruker APEX CCD diffractometer; this time, the space group Cmc2₁ seemed to be superior, since the disordered regions were not improved significantly by reducing the symmetry and, moreover, ADDSYM (from PLATON; Spek, 2003 ) detected additional symmetry suggesting Cmc2₁ for both the monoclinic space groups. Possible explanations for the differing result in the later experiment are firstly that the transition to Cc occurs close to 100 K and perhaps the crystal was better positioned in the cold stream in the RAXIS experiment, and therefore the crystal was kept at a slightly lower temperature during the data collection; another possibility is that there is some variation in behaviour from crystal to crystal. A further possibility is that the rate of cooling to the data-collection temperature might lead to different behaviour; for the RAXIS II data collection, flash cooling was used to cool the crystal to 100 K; for data collection using the Bruker APEX diffractometer, three data sets were collected at 100 K involving both flash cooling and more gradual cooling to the desired temperature, but similar results were obtained for each of the 100 K Bruker APEX data sets. A data collection at 95 K was carried out, but since the cryostream is at its limit at this temperature, the temperature was not as stable as usual, varying by about a degree. However, there were signs that some adjustment towards Cc had occurred at this temperature; the atoms particularly affected by the lowering of symmetry are those of the disordered ⁿBu group (C13–C16) and C25 (see Fig. 1), which is disordered in Cmc2₁ because it is removed slightly from the mirror plane, on which the other atoms of that ⁿBu lie (C26–C28). Of the heavier atoms, P2, O7 and O11 have higher and more eccentric a.d.p.s than the average for atoms of the same type, in Cmc2₁. If the reduction of symmetry to Cc leads to a reduction of the a.d.p.s of these atoms in particular, then this is a sign of the transition towards the space group Cc. This was clearly seen for the data measured using the RAXIS 11c at 100 K; for the data measured at 95 K on the Bruker APEX, there is no great difference between the a.d.p.s of the P and O atoms, but there are indications of improvement for some of the C atoms. Firstly, C13–C16 could be refined anisotropically, without the need to split the atoms into disordered components; secondly, C25–C28 are reasonably well ordered in Cc, whereas in Cmc2₁, C25 is (as always) disordered and C26–C28 show such eccentric a.d.p.s that it was suggested in the SHELXL list file that they should be split into two components. However, the conventional R value was marginally better for the Cmc2₁ refinement than for Cc (0.036 versus 0.039) and ADDSYM detected the possible higher symmetry of Cmc2₁. Thus, the choice of space group was not clear-cut and one would therefore probably select the higher-symmetry space group. Ideally, further data collection using helium cryocooling to achieve a significantly lower temperature would resolve this issue and the authors are seeking to carry out such experiments. In addition, differential scanning calorimetry (DSC) measurements would allow the temperature of the transition to the space group Cc to be measured precisely and again a suitable apparatus is being sought in order to carry out these further investigations.

For (II) at 100 K, the situation was straightforward; those atoms which were disordered or showed high thermal motion in Cmc2₁, showed the same patterns in Cc, ADDSYM detected higher symmetry and the R value in Cmc2₁ was significantly better than it was in Cc (0.027 versus 0.031). Note that refinement in Cc was carried out using a single twin law, (0 1 0/ 1 0 0/ 0 0 −1). Extensive tests of the possible additional twin laws arising from the fact that the metric symmetry is tetragonal, but the structure is monoclinic, are described in §2 and the supplementary information . These showed that the application of additional twin laws led to less satisfactory and less stable refinements, thus indicating that the application of a single twin law was appropriate. The refined structure in Cmc2₁ is plotted in Fig. 2(h). However, it seems very likely that further reduction of the temperature would lead to a transition to Cc, since the behaviour of (II) is so similar to that of (I) and a suitable location to carry out further experiments to investigate this is being sought.

3.1.2. (III)

Complex (III), [Th(TcO₄)₄(TBPO)₄], crystallizes in the body-centred cubic space group $[I\bar 43m]$ at 293 K, with the Th atom lying on the $[\bar 4]$ 3m special position and the asymmetric unit consisting of 1/24 of the molecule, Fig. 2(i). In this structure, not only do the ⁿBu groups show extremely high thermal motion, but the O atoms linking the Th and Tc atoms, and the Th and P atoms are disordered over three sites about a 3m axis. Again, a number of lower symmetry space groups were tested to see if this disorder could be removed, but to no avail. The body-centred cubic space group was also seen at 260 K, but by 230 K the body centring was no longer present, as was very apparent by the number of diffraction spots doubling and the unit cell becoming primitive (Figs. 3c and d). As for (I) and (II), this primitive cell transformed to a C-centred cell, with possible space groups Cmc2₁, Cc or P2₁, the latter using the primitive setting of the unit cell. Refinement was tried first in P2₁, but ADDSYM indicated that this model could be converted to Cmc2₁, which in fact led to a more satisfactory refinement. Cc was also tried, but the R value was higher (0.052 versus 0.037) and there were problems with the thermal parameters, so that as for (I) and (II) the space group Cmc2₁ was clearly the most acceptable at a temperature of 230 K (Fig. 2j). Note that TWINABS (Sheldrick, 2002) was used to investigate the application of the multiple twin laws, which might be possible in the monoclinic space groups owing to the fact that the metric symmetry is close to tetragonal and these trials are described in the supplementary information and summarized in §2; however, this did not change the conclusion that the orthorhombic space group was the correct choice. Moreover, a further transition to the space group Pbc2₁ takes place below 215 K (described in the next paragraph), which can be rationalized because it is a maximal subgroup of Cmc2₁; in contrast, the space group Pbc2₁ is not a maximal subgroup of P2₁ or Cc and a possible transition from one of these monoclinic space groups to Pbc2₁ would instead represent an increase in symmetry at the lower temperature rather than a decrease, and would therefore be unlikely.

Further reduction of the temperature below 230 K was carried out, and by 205 K the space group Cmc2₁ no longer gave an adequate refinement. The R value was higher and increased thermal motion was observed for the Tc, P and O atoms. P2₁ did not give an improved solution, but the solution in Cc was better although still showed some problems with not only the a.d.p.s, but also the geometry, initially thought to arise from twinning. Eventually, it became clear, once the temperature was lowered still further, that the number of diffraction spots had again doubled, as shown in Fig. 3(e) (i.e. quadrupled overall versus the 293 K diffraction pattern), marking a transition to a primitive unit cell of similar dimensions to the C centred cell, and the space group was found to be Pbc2₁ (a non-standard setting of Pca2₁, used here for ease of comparison with the other crystal structures). Re-examination of the data set measured at 215 K showed that although the systematic absence condition h+k = 2n+1 was obeyed, except for two weak reflections, refinement in Cmc2₁ was not satisfactory, nor was the solution in Pbc2₁. However, by 205 K the systematic absence condition no longer held and refinement was possible in Pbc2₁. It is likely that the transformation to the primitive orthorhombic space group occurs close to 215 K, explaining the difficulty in refining the structure in either space group at this temperature. As a further detail, the average I/σ for the h+k = 2n+1 class of reflections for the 100 K structure, for example, was 4.4 versus 9.75 for the whole data set. Of the total 13 900 independent reflections used in the refinement, 12 000 had I > 2σ(I), very clearly showing that C-centring was no longer present. These average values are typical for the data sets below 205 K, marking the transition to the primitive orthorhombic unit cell. The fact that the R_int and conventional R values are generally higher for the Pbc2₁ crystal structures than for the other structures is explained by the weaker h+k odd reflection subset.

All structures of (III) determined between 205 and 100 K were extremely well behaved in Pbc2₁ (see Figs. 2k, l and m); some degree of twinning was observed due to the similarity of a and b, but the disorder of the C13 and C25 atoms was no longer seen.

3.2. Unit-cell parameters

3.2.1. (I) and (II)

Plots of the unit-cell parameters are shown in the supplementary data [Figs. S1a and b for (I) and (II), respectively]; the tetragonal cells were transformed to cells equivalent to C-centred cells using the matrix (−1 −1 0/ 1 −1 0/ 0 0 1). For (I) the transition from tetragonal to C-centred leads to discontinuities in the reduction in the cell parameters seen as the temperature is lowered, which occur between 260 and 230 K. This is particularly marked for a, which reduces significantly more than b, and for c, which increases appreciably, due to the transition to the C-centred cell. The reduction in a, b, c and V is then steady from 230 to 95 K, with no obvious sign of a change around 100 K, which might be expected for the transition from Cmc2₁ to Cc.

For (II) again there are discontinuities between 260 and 230 K, and this is most obvious for c, which again increases slightly during the transition from tetragonal to C-centred; the similarity of a and b, even for the C-centred unit cells is obvious (Fig. S1b) .

3.2.2. (III)

Plots of the unit-cell parameters are shown for (III) in the supplementary data (Fig. S1c). The a parameter decreases and b increases, between 260 and 230 K, accompanying the transition from body-centred cubic to C-centred orthorhombic; then there is a sharp increase at 215 K, which is close to the probable transition temperature to the primitive orthorhombic cell. c and V show similar trends to one another, with significant reductions between 260 and 230 K accompanying the transition from cubic to C-centred orthorhombic. Then there is a further discontinuity at ∼ 215 K, marked by increases in c and V, arising from the transition to the primitive orthorhombic cell. A gradual reduction in all parameters takes place from 205 to 130 K, but there does seem to be a slight rise, particularly in b, between 130 and 100 K. This could signify further symmetry reduction, and the space groups Pc and P2₁ were investigated, but neither provided an improved model over the model in Pbc2₁.

4. Discussion

4.1. Space-group conversion pathways

The thermotropic behaviour observed as the temperature was reduced can be understood in terms of transitions down chains of maximal subgroups (International Tables, Vol. A, 1992, and the program SYMMODES; Capillas et al., 2003 ); the space-group pathways for (I) and (II), are somewhat different, although related to that of (III), and these are shown in Fig. 4.

Figure 4
Relationship between the space groups seen for complexes (I), (II) and (III). Note that the space group $[I\bar 21m]$ is a non-standard setting of the space group Fmm2. This space group is not seen for any of the complexes, but it is the likely space group linking between $[I\bar 42m]$ and Cmc2₁.

Complex (III) at 293 K exists in the space group $[I\bar 43m]$ , whilst (I) and (II) have the space group $[I\bar 42m]$ , which is a maximal subgroup of $[I\bar 43m]$ of type I and index 3. The reduction of symmetry arises from the loss of threefold point symmetry; the symmetry of the M-atom site which lies on the $[\bar 43m]$ special position in $[I\bar 43m]$ is reduced to $[\bar 42m]$ in the space group $[I\bar 42m]$ ; similarly, the symmetry of the M′ and P atom sites is reduced from 3m to m, and all other atoms, which lie on mirror planes in $[I\bar 43m]$ , either remain on mirror planes or have their symmetry reduced to general positions.

The $[I\bar 42m]$ space group is not seen for (III), but at 230 K all three complexes are found in the orthorhombic space group Cmc2₁. The route to this space group is somewhat more complex, being accessible by several space-group pathways; the most direct is via the maximal subgroup $[I\bar 21m]$ , which is equivalent to the orthorhombic space group Fmm2. The reduction in symmetry arises from the removal of the $[\bar 4]$ point symmetry; the symmetry of the M atom position is reduced from $[\bar 42m]$ to mm2 and the atoms which lie on a mirror plane in $[I\bar 42m]$ may or may not have that symmetry reduced to general positions. Although the space group $[I\bar 21m]$ (Fmm2) is not seen for any of the complexes, one of its maximal subgroups of the type (IIa), and index 2, is Cmc2₁. This change of space group causes the symmetry of the M-atom position to be reduced from mm2 to m, and atoms which lie on the m special positions may become general.

When the temperature is lowered still further, (III) transforms to the space group Pbc2₁, which is a maximal subgroup of Cmc2₁ of type (IIa) and index 2. This space group is not seen for (I) and (II), but the space-group symmetry of complex (I) reduces to Cc, at 100 K, which is another maximal subgroup of Cmc2₁ of type I and index 2. In either case, the change of space group removes the mirror symmetry from those atoms lying on m special positions and all atom positions become general.

4.2. Description of the structures

The molecules are distorted triangular dodecahedra (Haigh, 1995 ), with four [M′O₄]⁻ ions and four TBPO ligands placed alternately at the vertices. Selected bond lengths and angles are shown in Tables 4 and 5 for the complexes at 293, 230 and 100 K [except for those of (III) at 293 K, owing to the high degree of disorder of this structure]; other parameters for all the crystal structures have been deposited. For each molecule at the various temperatures, the bond lengths generally agree within experimental error, although for (III) there are several examples of slight differences in bond lengths between the structures at 230 and 100 K. The bond lengths around M [M = U for (I), and Th for (II) and (III)] fall into two groups, namely M—OTBPO and M—OM′ [M′ = Re for (I) and (II), and Tc for (III)]. For (I) the M—O bond lengths are slightly shorter than those found in complexes (II) and (III), reflecting the larger ionic radius of Th⁴⁺ versus U⁴⁺ (119 and 114 pm, respectively, for the eight coordinate M⁴⁺ ions; from https://www.webelements.com/webelements/elements/text/U/radii.html ); for example, for the 100 K crystal structures (I) has average M—OTBPO bond distances of 2.302 (5) Å and M—OM′ of 2.421 (5) Å, whilst the same average distances for (II) are 2.329 (5) and 2.461 (5) Å, and for (III) are 2.356 (4) and 2.450 (4) Å, respectively. Re—O and Tc—O bond lengths also fall into two groups, i.e. those that arise from the terminal O atoms and those from the O atoms bonded to the central M atom, and overall the equivalent bond lengths agree for all three complexes within experimental error, reflecting the similar ionic radii of Re⁷⁺ and Tc⁷⁺ (52 and 51 pm, respectively, for the four coordinate M′⁷⁺ ions; from https://www.webelements.com/webelements/elements ).

Table 4
Selected bond lengths (Å)

	(I) at 293 K	(I) at 230 K	(I) at 100 K	(II) at 293 K	(II) at 230 K	(II) at 100 K	(III) at 230 K	(III) at 100 K
M1—O13	2.272 (10)	2.261 (8)	2.280 (7)	2.320 (11)	2.280 (15)	2.287 (12)	2.302 (8)	2.337 (9)
M1—O9	–	2.272 (8)	2.305 (8)	–	2.337 (15)	2.293 (11)	2.290 (9)	2.348 (8)
M1—O5	–	2.297 (6)	2.311 (11)	–	2.362 (11)	2.368 (8)	2.314 (7)	2.374 (8)
M1—O5A	–	2.297 (6)	2.305 (11)	–	2.362 (11)	2.368 (8)	2.313 (7)	2.368 (8)
M1—O10	2.411 (10)	2.396 (8)	2.434 (7)	2.436 (11)	2.462 (13)	2.454 (11)	2.438 (10)	2.437 (9)
M1—O6	–	2.404 (8)	2.426 (7)	–	2.489 (11)	2.461 (11)	2.398 (10)	2.444 (9)
M1—O1	–	2.428 (6)	2.440 (10)	–	2.489 (11)	2.464 (8)	2.433 (7)	2.465 (8)
M1—O1A	–	2.428 (6)	2.419 (10)	–	2.502 (14)	2.464 (8)	2.433 (7)	2.449 (8)
M′1—O2	–	1.667 (8)	1.675 (12)	–	1.681 (11)	1.693 (9)	1.613 (9)	1.691 (10)
M′1—O3	–	1.690 (8)	1.698 (13)	–	1.690 (11)	1.703 (9)	1.663 (9)	1.704 (10)
M′1—O4	–	1.700 (7)	1.798 (11)	–	1.715 (11)	1.711 (8)	1.672 (7)	1.683 (11)
M′1—O1	1.749 (10)	1.748 (6)	1.752 (11)	1.742 (12)	1.720 (11)	1.756 (9)	1.710 (7)	1.759 (9)
M′2—O8A	–	1.688 (7)	1.691 (12)	–	1.701 (12)	1.668 (9)	1.621 (8)	1.676 (10)
M′2—O8	–	1.688 (7)	1.697 (11)	–	1.701 (12)	1.668 (9)	1.621 (8)	1.703 (10)
M′2—O7	–	1.705 (10)	1.652 (12)	–	1.722 (13)	1.737 (11)	1.630 (10)	1.723 (10)
M′2—O6	–	1.770 (8)	1.757 (7)	–	1.761 (14)	1.743 (11)	1.752 (10)	1.750 (9)
M′3—O11A	–	1.646 (8)	1.676 (12)	–	1.550 (13)	1.660 (11)	1.603 (9)	1.670 (11)
M′3—O11	–	1.646 (8)	1.651 (11)	–	1.550 (13)	1.660 (11)	1.603 (9)	1.697 (10)
M′3—O12	–	1.675 (10)	1.689 (9)	–	1.706 (13)	1.691 (10)	1.626 (11)	1.706 (9)
M′3—O10	–	1.756 (8)	1.737 (7)	–	1.711 (13)	1.753 (10)	1.705 (10)	1.758 (10)
M′1A—O3A	–	–	1.667 (14)	–	–	–	–	1.683 (10)
M′1A—O2A	–	–	1.681 (12)	–	–	–	–	1.703 (9)
M′1A—O4A	–	–	1.724 (12)	–	–	–	–	1.671 (11)
M′1A—O1A	–	–	1.771 (11)	–	–	–	–	1.751 (9)
P1—O5	1.506 (11)	1.508 (6)	1.520 (11)	1.522 (12)	1.513 (11)	1.515 (8)	1.503 (7)	1.509 (9)
P2—O9	–	1.506 (9)	1.528 (8)	–	1.531 (15)	1.535 (12)	1.497 (11)	1.516 (9)
P3—O13	–	1.520 (8)	1.524 (8)	–	1.477 (16)	1.518 (12)	1.474 (9)	1.499 (10)
P1A—O5A	–	–	1.520 (11)	–	–	–	–	1.515 (8)

Table 5
Bond angles about M (°)

	(I) at 293 K	(I) at 230 K	(I) at 100 K	(II) at 293 K	(II) at 230 K	(II) at 100 K	(III) at 230 K	(III) at 100 K
O9—M1—O13	138.7 (6)	136.6 (4)	136.9 (3)	137.7 (3)	135.3 (6)	134.9 (5)	133.6 (4)	117.7 (4)
O9—M1—O5	97.1 (2)	98.88 (18)	103.2 (4)	97.7 (3)	100.2 (3)	100.1 (2)	99.49 (18)	127.2 (3)
O13—M1—O5	–	96.00 (18)	91.2 (4)	–	95.6 (3)	95.1 (2)	97.02 (18)	83.5 (3)
O9—M1—O5A	–	98.88 (18)	95.5 (4)	–	100.2 (3)	100.2 (2)	99.49 (18)	83.2 (3)
O13—M1—O5A	–	96.00 (18)	99.1 (4)	–	95.6 (3)	95.1 (2)	97.02 (18)	131.1 (3)
O5—M1—O5A	–	138.9 (3)	139.6 (3)	–	137.3 (6)	139.2 (4)	137.2 (4)	120.1 (3)
O9—M1—O6	71.6 (4)	70.6 (3)	70.1 (3)	70.8 (5)	70.9 (5)	71.3 (4)	71.8 (4)	73.4 (3)
O13—M1—O6	149.6 (4)	152.8 (3)	152.8 (3)	152.2 (5)	153.7 (5)	153.8 (4)	154.6 (4)	153.8 (3)
O5—M1—O6	74.1 (2)	75.76 (16)	77.5 (4)	73.9 (3)	76.0 (3)	76.8 (2)	75.04 (19)	71.7 (3)
O5A—M1—O6	–	75.76 (16)	75.7 (4)	–	76.0 (3)	76.8 (2)	75.04 (19)	71.3 (3)
O9—M1—O1A	–	72.2 (2)	72.7 (3)	–	72.3 (4)	71.3 (4)	71.1 (3)	74.5 (3)
O13—M1—O1A	–	74.1 (2)	73.6 (3)	–	73.7 (4)	74.1 (3)	73.8 (3)	71.4 (3)
O5—M1—O1A	–	149.0 (2)	147.3 (4)	–	151.0 (4)	148.6 (3)	151.6 (3)	153.3 (3)
O5A—M1—O1A	–	72.0 (2)	72.5 (4)	–	71.5 (4)	72.0 (3)	71.0 (3)	73.4 (3)
O9—M1—O1	–	72.2 (2)	72.7 (3)	–	72.3 (4)	70.9 (3)	71.1 (3)	70.3 (3)
O13—M1—O1	–	74.1 (2)	74.0 (3)	–	73.7 (4)	74.1 (3)	73.8 (3)	71.3 (3)
O5—M1—O1	–	72.0 (2)	71.5 (4)	–	71.5 (4)	72.0 (3)	71.0 (3)	73.1 (3)
O5A—M1—O1	–	149.0 (2)	148.9 (4)	–	151.0 (4)	148.6 (3)	151.6 (3)	152.2 (3)
O9—M1—O10	–	149.0 (3)	148.3 (3)	–	149.6 (5)	149.3 (4)	152.0 (4)	154.5 (3)
O13—M1—O10	–	74.4 (3)	74.7 (3)	–	75.1 (5)	75.8 (4)	74.6 (3)	75.5 (4)
O5—M1—O10	–	72.88 (16)	73.0 (4)	–	71.7 (3)	72.2 (2)	72.54 (18)	73.5 (3)
O5A—M1—O10	–	72.88 (16)	72.3 (4)	–	71.7 (3)	72.2 (2)	72.54 (18)	72.4 (3)
O6—M1—O10	78.0 (6)	78.4 (3)	78.4 (3)	81.4 (7)	78.7 (4)	78.0 (3)	79.9 (4)	104.6 (3)
O1A—M1—O10	127.1 (4)	129.2 (2)	127.3 (4)	125.1 (4)	128.3 (3)	130.2 (3)	127.6 (2)	91.1 (3)
O1—M1—O10	–	129.2 (2)	131.4 (4)	–	128.3 (3)	130.2 (3)	127.6 (2)	134.9 (3)
O6—M1—O1A	–	125.4 (2)	127.6 (4)	–	124.6 (3)	124.8 (3)	123.9 (2)	134.3 (3)
O6—M1—O1	–	125.4 (2)	123.6 (3)	–	124.6 (3)	124.8 (3)	12397 (2)	92.8 (3)
O1A—M1—O1	–	76.9 (3)	76.5 (3)	–	79.6 (5)	76.7 (4)	80.7 (4)	105.9 (3)

Looking at the bond angles about the central M atom (Table 5), for all the crystal structures in the space group Cmc2₁, in general, there is no significant difference between equivalent bond angles. Also, the agreement between these bond angles for (I) and (II) measured at all temperatures is reasonably close, even though there are one or two space-group transitions in the whole temperature range. However, there are major differences between the bond angles about M in (III) in the space Pbc2₁ and any of the other crystal structures, including that of (III) at 230 K, indicating that the space-group transition between Cmc2₁ and Pbc2₁ causes a major change in conformation of the molecule. In general, the particularly large differences are seen for the OTBPO—Th—OTBPO and OTc—Th—OTc bond angles, while the OTBPO—Th—OTc match reasonably closely with the equivalent angles of the other crystal structures. For example, the OTBPO—M—OTBPO angle, O9—M1—O13, varies from 133.6 (4) to 138.7 (6)° for all the structures from 293 to 100 K, except (III) at 100 K [also not including the disordered 293 K structure of (III)], whereas for (III) at 100 K the corresponding angle is 117.7 (4)° (Table 5). Similarly, the OM′—M—OM′ angle, O1A—M1—O1, varies from 76.5 (3) to 80.7 (4)° for all the structures except for (III) at 100 K, where the corresponding angle is 105.9 (3)°. This is in contrast to the OTBPO—M—OM′ angles, which show much smaller differences; for example, the O13—M1—O1A angle varies from 73.6 (3) to 74.1 (2)° for all the structures except (III) at 100 K, where this angle is 71.4 (3)°.

4.3. Comparison of the structures

The similarities and differences seen in geometric parameters are clarified further by comparison of the complexes using the program OFIT from the SHELXTL package (Bruker, 2001), where equivalent M, M′ and P atoms were fitted. Firstly, for (I) the r.m.s. deviation of these atoms between the 293 and 230 K structures was 0.043 Å, and it is clear from Fig. 5(a) that the heavy atoms are very well matched at the two different temperatures; most of the O atoms fit fairly well, but there are some more significant deviations of the C atoms of the ⁿBu groups. Similar results were seen in comparing (II) at 293 and 230 K (r.m.s. deviation = 0.065 Å). The r.m.s. deviation of the 230 and 100 K structures of (I) was 0.090 Å (Fig. 5b) and it is clear that generally the lighter atoms fit reasonably closely, except in the disordered ⁿBu regions of the 230 K structure. The structures of (II) at 230 and 100 K are much more similar (r.m.s. deviation = 0.029 Å), with the main differences again found in the regions of disorder in the ⁿBu groups (Fig. 5c); since these two structures are both in Cmc2₁, their correspondence is to be expected. It was also found that different complexes in the same space group showed very close resemblance; for example, the r.m.s. deviation of structures (I) and (II) at 293 K was found to be 0.058 Å; similarly, all the structures at 230 K (in the space group Cmc2₁) match very closely, with the r.m.s. deviation of the structures of (I) and (II) of 0.055 Å, structures (I) and (III) 0.069 Å, and (II) and (III) 0.056 Å.

Figure 5
Comparison of the structures using the program OFIT from the SHELTL program suite (Bruker, 2001

). The same view has been used as in Figs. 1

and 2

. (a) Overlay of (I) at 293 K (dashed lines) and 230 K. (b) Overlay of (I) at 230 K (dashed lines) and 100 K. (c) Overlay of (II) at 230 K (dashed lines) and 100 K. (d) Overlay of (III) at 293 K (dashed lines) and 230 K. (e) Overlay of (III) at 230 K (dashed lines) and 100 K.

However, the structures of (III) at 293 and below 205 K (space groups $[I\bar43m]$ and Pbc2₁, respectively) are both quite different from all the other structures, including the structure of (III) at 230 K; for example, comparing the M, M′ and P atoms of the structures of (III) at the different temperatures, between the 293 and 230 K structures, the r.m.s. deviation = 0.366 Å (Fig. 5d), and between the 230 and 100 K structures, the r.m.s. deviation = 0.399 Å (Fig. 5e); the r.m.s. deviation between the 293 and 100 K structures is slightly reduced to 0.279 Å showing that the Th, Tc and P atoms are a little better matched but due to the disorder of (III) at 293 K, the C and O atoms positions do not correspond well.

The crystal structures can also be evaluated by comparing their polyhedron plots, a selection of which are shown in Fig. 6; these show the central M atom as a dodecahedron, and the M′ and P atoms as tetrahedra, and the dodecahedron is linked to the tetrahedra by corner sharing; the variation of the four molecules contained in the C-centred and primitive unit cells seen at 230 K and below is displayed The 293 K structures of (III) and (II) in the space groups $[I\bar 43m]$ and $[I\bar 42m]$ , respectively, show the high symmetry of these two structures (Figs. 6a and b). At 230 K each structure is found in the orthorhombic space group Cmc2₁, which is shown for (III) in Fig. 6(c). This shows some tilting of the polyhedra relative to one another, compared with those seen in Figs. 6(a) and (b). For (I), reduction of the temperature leads to the transition to Cc, as shown in Fig. 6(d), which shows only minor differences in tilt angles compared with Fig. 6(c). Finally, Fig. 6(e) shows (III) in the space group Pbc2₁, which has a much larger change in the relative tilt angles of the three different polyhedra types, illustrating the significant difference of this structure to all the others.

Figure 6
Polyhedron plots of the four molecules contained in the unit cells at 230 K and below, viewed down the c axis. The M atom is shown in green, M′ in blue and P in purple; C atoms have been omitted for clarity. The plot for (III) at 293 K was prepared by using one component of the disordered O1 and O3 atoms. (a) (III) at 293 K; (b) (II) at 293 K; (c) (III) at 230 K; (d) (I) at 100 K; (e) (III) at 100 K.

The changes of space group also lead to changes in the packing arrangement of the molecules. Firstly, there are adjustments of the distances between the central M atoms, which have 14 neighbours in the closest coordination shell. Fig. 7 shows the arrangement for (III) at 293 K. The distances are either 15.342 or 13.287 Å, between the six neighbours in the direction of the faces or eight neighbours towards the vertices of the cell, respectively; the former distance is the unit-cell dimension. Reduction of the symmetry leads to changes in these two distances. Firstly, in the direction of the faces, the distances change from 15.342 Å to the ranges 14.736–15.212 Å at 230 K and 14.820–15.297 Å at 100 K, with the two shortest distances arising from the reduction of the c unit-cell dimension. Secondly, at the same time, the distances to the vertices change from 13.287 Å to the ranges 12.981–13.152 Å at 230 K and 12.948–13.357 Å at 100 K. Thus, the space-group transition to Cmc2₁ leads to an overall reduction in all these distances, but the transition to Pbc2₁ leads, in some cases, to small increases. For (I) and (II), the distances generally reduce with temperature; for example, for (I), the distances in the direction of the faces of the unit cell are in the range 14.819–15.540 Å at 293 K, 14.829–15.360 Å at 230 K and 14.784–15.229 Å at 100 K, and the distances to the vertices are 13.253 Å at 293 K, and in the range 13.071–13.285 Å at 230 K and 13.004–13.175 Å at 100 K.

Figure 7
Packing arrangement for the central Th atom to its 14 nearest-neighbour Th atoms for (III) at 293 K, showing the body-centred cubic unit cell. The distances are either 15.342 or 13.287 Å between the neighbours in the direction of the faces or vertices of the cell, respectively.

The molecules are arranged so that the M′O₄^- groups point towards TBPO groups of adjacent molecules. This probably arises firstly because the M′O₄ groups do not protrude as far from the central M atom as the TBPO groups; the former distance is around 4.6–4.8 Å to the outer most O atoms, whilst the latter is between 6.5–9 Å to the furthest C atoms. Thus, the ⁿBu groups of one molecule fit into the cavity of the smaller M′O₄ group of the next molecule to provide the optimum filling of the space between the molecules (see Fig. 8). The ⁿBu groups form a layer around the M′O₄ groups and so this configuration allows stabilization owing to a possible network of 20–30 weak intermolecular C—H⋯O hydrogen bonds per molecule; these are marked by the many contacts of less than 4 Å, which are present between the ⁿBu C atoms and the terminal O atoms of the M′O₄ groups of the neighbouring molecules. In addition, there are numerous (around 40 per molecule) intramolecular C⋯O contacts less than 4 Å, arising from the proximity of adjacent TBPO and M′O₄ groups in the alternate arrangement of the ligands about the central M atom. Determination of these hydrogen bonds was carried out for the crystal structures at 230 and 100 K; those at 293 K were omitted from this analysis owing to the uncertainty of the C atom and especially the H-atom positions of the structures at this temperature. For the crystal structures at 230 K and below the calculated position of the H atoms should be accurate, except for those of the methyl groups where the torsion angle may not be correct (see §2.5). Owing to the uncertainty specifically of the methyl H-atom positions, these structures would be excellent candidates for neutron crystal structure analyses to determine their H-atom position and therefore their hydrogen bonding, precisely in the presence of these very heavy elements.

Figure 8
Space-filling diagram showing how the TBPO groups and [M′O₄] groups from adjacent molecules fit together (MERCURY; Bruno et al., 2002

Comparison of the hydrogen-bonding interactions revealed that they are very similar for all the cryostructures in the space group Cmc2₁, namely (I), (II) and (III) at 230 K, and (II) at 100 K. Also, the hydrogen bonding in (I) in the space group Cc, at 100 K, is closely comparable with the structures in Cmc2₁. However, because of the large differences of conformation between the structures of (III) at 230 and 100 K, there are also some differences in hydrogen bonding. There are other similar contacts where there is disorder of the ⁿBu chains at the higher temperature, but since these are less certain they will not be discussed here. The contacts for (III) at 230 and 100 K are listed in Table 6, between atoms where there is no disorder of the ⁿBu groups at the either temperature. Also, Fig. 9 shows the intermolecular hydrogen bonds between these atoms at the two temperatures, with differences arising from the changes in conformation at the two temperatures. Interaction cooperativity, where a number of hydrogen bonds work together, which appears to be the case for these complexes, tends to increase the strength of the hydrogen bonds to be greater than the sum of their individual energies (Desiraju, 1996 ; Desiraju & Steiner, 1999 ). Thus, it is very probable that these weak interactions influence both the way that the molecules pack together and also their conformations at the different temperatures.

Table 6
Selected intra- and intermolecular hydrogen bonds for (III) at 100 and 230 K

D—H⋯A	d(D—H)	d(H⋯A)	d(D⋯A)	<(DHA)
(III) at 100 K
C1—H1A⋯O11	0.99	2.83	3.696 (18)	147.0
C2—H2B⋯O5	0.99	2.85	3.265 (16)	105.7
C2—H2B⋯O6	0.99	2.90	3.578 (15)	126.7
C3—H3A⋯O(12)	0.99	2.77	3.602 (19)	142.5
C5—H5A⋯O2	0.99	2.73	3.614 (17)	148.8
C5—H5B⋯O6	0.99	2.49	3.230 (16)	131.6
C5—H5B⋯O8	0.99	2.79	3.736 (17)	160.3
C9—H9A⋯O2	0.99	2.84	3.689 (17)	144.1
C10—H10A⋯O11	0.99	2.62	3.318 (18)	127.3
C10—H10B⋯O4	0.99	2.87	3.608 (17)	132.3
C10—H10B⋯O5	0.99	2.85	3.179 (18)	100.3
C1A—H1C⋯O10	0.99	2.71	3.477 (15)	134.7
C1A—H1C⋯O12	0.99	2.60	3.549 (17)	160.8
C1A—H1D⋯O7	0.99	2.51	3.381 (16)	147.2
C5A—H5D⋯O7	0.99	2.81	3.612 (17)	139.0
C5A—H5D⋯O8A	0.99	2.99	3.606 (16)	121.2
C6A—H6C⋯O5A	0.99	2.97	3.262 (14)	98.2
C6A—H6C⋯O8A	0.99	2.87	3.557 (16)	127.3
C6A—H6D⋯O2A	0.99	2.70	3.363 (16)	124.3
C9A—H9D⋯O2A	0.99	2.78	3.690 (15)	152.6
C10A—H10C⋯O10	0.99	2.68	3.390 (15)	128.5
C10A—H10C⋯O1A	0.99	2.77	3.574 (15)	138.2
C10A—H10C⋯O5A	0.99	2.95	3.325 (14)	103.4
C1—H1B⋯O2ⁱ	0.99	2.77	3.674 (17)	152.1
C6—H6B⋯O3ⁱ	0.99	2.82	3.611 (16)	137.8
C4—H4A⋯O2ⁱ	0.98	2.75	3.72 (2)	168.3
C12—H12B⋯O3ⁱ	0.98	3.01	3.69 (2)	127.7
C9—H9B⋯O3ⁱ	0.99	2.60	3.573 (17)	167.3
C12—H12C⋯O8ⁱⁱ	0.98	2.76	3.697 (18)	160.0
C2A—H2C⋯O2Aⁱⁱⁱ	0.99	2.97	3.569 (16)	119.8
C2A—H2D⋯O4Aⁱⁱⁱ	0.99	2.79	3.645 (17)	145.4
C5A—H5C⋯O4Aⁱⁱⁱ	0.99	2.80	3.784 (16)	171.7
C12A—H12F⋯O3Aⁱⁱⁱ	0.98	2.69	3.552 (18)	146.4
C4A—H4E⋯O3A^iv	0.98	2.68	3.549 (17)	148.2

(III) at 230 K
C2—H2A⋯O5	0.97	2.94	3.337 (14)	105.6
C2—H2A⋯O6	0.97	2.60	3.454 (14)	147.4
C2—H2A⋯O7	0.97	3.00	3.464 (16)	110.4
C2—H2A⋯O10	0.97	2.92	3.650 (16)	133.3
C3—H3B⋯O12	0.97	2.68	3.537 (19)	147.3
C5—H5B⋯O8	0.97	2.58	3.533 (14)	167.1
C5—H5A⋯O2	0.97	2.59	3.449 (14)	147.6
C9—H9A⋯O2	0.97	2.82	3.624 (15)	141.3
C9—H9A⋯O4	0.97	2.97	3.633 (14)	126.9
C10—H10A⋯O11	0.97	3.07	3.564 (16)	113.3
C10—H10B⋯O4	0.97	3.02	3.565 (15)	116.9
C10—H10B⋯O5	0.97	2.87	3.228 (14)	102.7
C4—H4A⋯O2^v	0.96	3.02	3.880 (19)	149.4
C6—H6B⋯O4^v	0.97	2.88	3.559 (13)	127.7
C6—H6A⋯O3^v	0.97	2.74	3.523 (13)	138.1
C9—H9B⋯O3^v	0.97	2.72	3.682 (13)	172.9
Symmetry codes: (i) $[-x+1,-y,z+{1\over 2}]$ ; (ii) $[-x+1,y-{1\over 2},z]$ ; (iii) $[-x,-y,z+{1\over 2}]$ ; (iv) x,y,z+1; (v) $[-x+{1\over 2},-y+{1\over 2},z+{1\over 2}]$ .

Figure 9
Comparison of the intermolecular C—H⋯O hydrogen-bonding interactions between C1—C12 and C1A—C12A and O1—O4 and O1A—O4A for (III) at (a) 230 K and (b) 100 K; note that at 230 K the two components, C1—C12 and C1A—C12A, and likewise O1—O4 and O1A—O4A, are related by mirror symmetry.

To summarize, all the crystal structures agree remarkably closely, except the structures of (III) at 293 K and those of (III) below 205 K, in the space groups $[I\bar 43m]$ and Pbc2₁, respectively. These two space groups are not seen for complexes (I) and (II). It is clear that as well as the possible increase of mobility, particularly of the ⁿBu groups as the temperature is increased, there is also an unexpected freedom of movement of the atoms bonded to the central M atom. This is indicated by the fact that some of the OTBPO—Th—OTBPO and OTc—Th—OTc bond angles in (III) differ by a surprising amount at different temperatures, and also illustrated by changes in the relative tilt angles of the linked polyhedra. Thus, the space-group transitions seen for (I) and (II) may be largely attributed to the altered degrees of mobility, especially of the ⁿBu groups. However, the much larger conformational changes seen for (III) presumably also arise from the differing packing constraints in the space groups $[I\bar 43m]$ and Pbc2₁.

The change of M from U in (I) to Th in (II), where M′ is Re in each case, gives complexes that have very similar behaviour with temperature, although the ionic radius of Th⁴⁺ is somewhat larger than that of U⁴⁺; however, the change of M′ from Re in (II) to Tc in (III) causes a much greater alteration in the behaviour with temperature, even though the atomic radii of Tc⁷⁺ and Re⁷⁺ are similar, and the bond lengths about the M′ atoms correspond very closely from structure to structure. Therefore, from a consideration of the bond lengths it is not clear why the apparently similar complex (III) shows this difference in behaviour compared with complexes (I) and (II). Also, a detailed study of the vibrational spectroscopy proved to be unhelpful; firstly, the [TcO₄]⁻ stretches come at lower energy than the [ReO₄]⁻ stretches and hence a direct comparison is impossible; secondly, for the TBPO ligand, the spectral features are almost identical for the three complexes, with the major P=O stretch coming at 1059, 1060 and 1057 cm⁻¹, respectively, for (I), (II) and (III). However, the different conformations and packing arrangements may be influenced by variations in the strength of the weak C—H⋯O intra- and intermolecular hydrogen-bonding interactions. These differences could in turn arise because of the possible variations in charge density on the O atoms of the pertechnetate ion versus the perrhenate ion; such differences in the basicity of the acceptor atoms would lead to variations in hydrogen-bond lengths and therefore strengths (Desiraju, 1996; Desiraju & Steiner, 1999).

Of particular interest in determining the reasons for the differing behaviour seen for (III) versus (I) and (II) would be to carry out temperature-resolved studies of the [M(M′O₄)₄(TBPO)₄] structure, where M = U and M′ = Tc, to find out whether its behaviour would be analogous to that of (I) and (II) or that of (III); unfortunately, the U⁴⁺ ion would be oxidized by pertechnetate, making the synthesis of this complex impossible. However, we intend to explore the chemistry of lanthanide analogues, which might show similar interesting behaviour with temperature and lead to greater insight into the causes for the variation in behaviour of these closely related complexes.

5. Conclusions

This ensemble of experiments demonstrates that for each complex the crystal structures show a stepwise improvement of order as the temperature is reduced, which is marked by changes of lattice centring and reduction of space-group symmetry. Liquid nitrogen cooling removes all or almost all the disorder seen at ambient temperature and it seems likely that cooling to temperatures lower than 100 K might induce further phase transitions. In one case repetition of the experiment on two different diffractometers suggested a fine sensitivity to temperature setting close to the liquid nitrogen cryostream lower-temperature limit; in order to investigate this and any possible further space-group transitions, a liquid helium temperature facility would be required for future experiments. In addition, heat-capacity experiments using DSC would be helpful for investigating the space-group transitions.

The various results obtained suggest that firstly the freezing, particularly of the ⁿBu groups, which are highly mobile at 293 K, leads to space-group transitions as the temperature is reduced. Also, the constraints of the crystal packing for different space groups, together with the weak C—H⋯O hydrogen bonding, probably influence the overall geometry of these compounds and lead in some cases to some large changes of conformation between structures measured at different temperatures. We would expect that the changes are cooperatively intermolecular, although it is not possible to resolve whether the drive is enthalpic or entropic. The changes of the distances between the central M atoms of up to 0.6 Å represent a significant fraction of a hydrogen bond and must presumably affect the 25 to 30 intermolecular hydrogen bonds in each structure to a greater or lesser extent.

Finally, the formation of these complexes demonstrates that perrhenate and pertechnetate are sufficiently strong ligands to compete with TBPO and bind to actinide metal centres. Further studies are in progress to explore whether these complexes are stable in solution and therefore might be model complexes for species involved in the PUREX process.

Supporting information

Crystal structure: contains datablocks Iat293, Iat230, Iat165, Iat100, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100. DOI: 10.1107/S0108768105036931/ws5025sup1.cif

Structure factors: contains datablock s989-121a. DOI: 10.1107/S0108768105036931/ws5025Iat293sup2.hkl

Structure factors: contains datablock s989-36a. DOI: 10.1107/S0108768105036931/ws5025Iat230sup3.hkl

Structure factors: contains datablock s989-165-36a. DOI: 10.1107/S0108768105036931/ws5025Iat165sup4.hkl

Structure factors: contains datablock s989100cc. DOI: 10.1107/S0108768105036931/ws5025Iat100sup5.hkl

Structure factors: contains datablock ads293a. DOI: 10.1107/S0108768105036931/ws5025IIat293sup6.hkl

Structure factors: contains datablock ads-36a. DOI: 10.1107/S0108768105036931/ws5025IIat230sup7.hkl

Structure factors: contains datablock ads-36a. DOI: 10.1107/S0108768105036931/ws5025IIat165sup8.hkl

Structure factors: contains datablock ads100b-36a. DOI: 10.1107/S0108768105036931/ws5025IIat100sup9.hkl

Structure factors: contains datablock h:\s1884\work\s1884m. DOI: 10.1107/S0108768105036931/ws5025IIIat293sup10.hkl

Structure factors: contains datablock s1884ca. DOI: 10.1107/S0108768105036931/ws5025IIIat230sup11.hkl

Structure factors: contains datablock s1884-170. DOI: 10.1107/S0108768105036931/ws5025IIIat170sup12.hkl

Structure factors: contains datablock s1884-130. DOI: 10.1107/S0108768105036931/ws5025IIIat130sup13.hkl

Structure factors: contains datablock s1879-29ba. DOI: 10.1107/S0108768105036931/ws5025IIIat100sup14.hkl

Comment top

ENTER TEXT

Experimental top

ENTER EXPERIMENTAL SECTION

Computing details top

Data collection: Bruker SMART for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100; MSC RAXIS11 Control for Iat100. Cell refinement: Bruker SMART for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100; DENZO (Otwinowski, Z. 1988) for Iat100. Data reduction: Bruker SAINT for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100; DENZO (Otwinowski, Z. 1988) for Iat100. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990) for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100; SIR97 (Altomare, et al. 1997) for Iat100. For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: Bruker SHELXTL for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100. Software used to prepare material for publication: Bruker SHELXTL for Iat293, Iat230, Iat165, IIat293, IIat230, IIat165, IIat100, IIIat293, IIIat230, IIIat170, IIIat130, IIIat100; TEXSAN (MSC, 1995) for Iat100.

Figures top

ENTER FIGURE CAPTIONS

(Iat293) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	D_x = 1.960 Mg m⁻³
M_r = 2112.05	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4₂m	Cell parameters from 3188 reflections
a = 15.5404 (6) Å	θ = 2.6–20.8°
c = 14.8191 (11) Å	µ = 9.14 mm⁻¹
V = 3578.9 (3) Å³	T = 293 K
Z = 2	Block, green
F(000) = 2016	0.15 × 0.15 × 0.10 mm

Data collection top

CCD area detector diffractometer	1941 independent reflections
Radiation source: fine-focus sealed tube	1699 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.029
phi and ω scans	θ_max = 26.4°, θ_min = 1.9°
Absorption correction: multi-scan SADABS	h = −19→15
T_min = 0.341, T_max = 0.462	k = −17→19
10483 measured reflections	l = −18→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.039	H-atom parameters constrained
wR(F²) = 0.099	w = 1/[σ²(F_o²) + (0.0614P)²] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.001
1941 reflections	Δρ_max = 1.04 e Å⁻³
102 parameters	Δρ_min = −0.38 e Å⁻³
58 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.03 (2)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	Z = 2
M_r = 2112.05	Mo Kα radiation
Tetragonal, I4₂m	µ = 9.14 mm⁻¹
a = 15.5404 (6) Å	T = 293 K
c = 14.8191 (11) Å	0.15 × 0.15 × 0.10 mm
V = 3578.9 (3) Å³

Data collection top

CCD area detector diffractometer	1941 independent reflections
Absorption correction: multi-scan SADABS	1699 reflections with I > 2σ(I)
T_min = 0.341, T_max = 0.462	R_int = 0.029
10483 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	H-atom parameters constrained
wR(F²) = 0.099	Δρ_max = 1.04 e Å⁻³
S = 1.09	Δρ_min = −0.38 e Å⁻³
1941 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
102 parameters	Absolute structure parameter: 0.03 (2)
58 restraints

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	0.5000	0.5000	0.5000	0.0546 (2)
Re1	0.64207 (3)	0.35793 (3)	0.32660 (4)	0.0848 (2)
P1	0.6509 (2)	0.3491 (2)	0.6164 (3)	0.1132 (16)
O1	0.5690 (5)	0.4310 (5)	0.3736 (7)	0.101 (3)
O2	0.7410 (6)	0.3795 (10)	0.3602 (9)	0.163 (4)
O3	0.6374 (7)	0.3626 (7)	0.2164 (9)	0.158 (6)
O4	0.5967 (4)	0.4033 (4)	0.5540 (8)	0.108 (4)
C1	0.6012 (14)	0.2422 (10)	0.6023 (15)	0.200 (8)
H1A	0.5456	0.2438	0.6320	0.240*
H1B	0.5902	0.2343	0.5383	0.240*
C2	0.6459 (15)	0.1659 (11)	0.6342 (16)	0.215 (8)
H2A	0.6447	0.1642	0.6996	0.257*
H2B	0.7055	0.1676	0.6149	0.257*
C3	0.6024 (16)	0.0862 (13)	0.596 (2)	0.218 (9)
H3A	0.6140	0.0792	0.5325	0.261*
H3B	0.5408	0.0872	0.6064	0.261*
C4	0.6465 (16)	0.0161 (15)	0.6527 (13)	0.203 (9)
H4A	0.6275	−0.0395	0.6326	0.305*
H4B	0.6317	0.0234	0.7151	0.305*
H4C	0.7077	0.0204	0.6456	0.305*
C5	0.6193 (14)	0.3807 (14)	0.7268 (13)	0.247 (15)
H5A	0.6285	0.4423	0.7308	0.296*	0.50
H5B	0.5577	0.3715	0.7308	0.296*	0.50
C6	0.6578 (14)	0.3422 (14)	0.8090 (18)	0.266 (15)
H6A	0.7193	0.3525	0.8110	0.319*	0.50
H6B	0.6475	0.2807	0.8110	0.319*	0.50
C7	0.6111 (16)	0.3889 (16)	0.889 (2)	0.275 (17)
H7A	0.6215	0.4504	0.8873	0.330*	0.50
H7B	0.5496	0.3785	0.8873	0.330*	0.50
C8	0.651 (2)	0.349 (2)	0.972 (2)	0.36 (3)
H8A	0.6209	0.3696	1.0246	0.533*	0.50
H8B	0.7102	0.3654	0.9756	0.533*	0.50
H8C	0.6461	0.2878	0.9685	0.533*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.0507 (3)	0.0507 (3)	0.0622 (4)	0.000	0.000	0.000
Re1	0.0849 (3)	0.0849 (3)	0.0846 (4)	0.0082 (3)	0.0175 (2)	−0.0175 (2)
P1	0.120 (3)	0.120 (3)	0.099 (3)	0.054 (3)	−0.0176 (14)	0.0176 (14)
O1	0.101 (4)	0.101 (4)	0.102 (7)	0.007 (6)	0.022 (4)	−0.022 (4)
O2	0.092 (6)	0.213 (12)	0.183 (11)	0.008 (7)	0.012 (6)	−0.037 (10)
O3	0.193 (10)	0.193 (10)	0.086 (8)	0.030 (14)	0.030 (6)	−0.030 (6)
O4	0.113 (6)	0.113 (6)	0.099 (7)	0.049 (7)	−0.011 (4)	0.011 (4)
C1	0.22 (2)	0.217 (15)	0.160 (16)	0.056 (14)	−0.034 (14)	0.068 (14)
C2	0.21 (2)	0.189 (13)	0.248 (19)	0.039 (12)	−0.090 (16)	−0.032 (15)
C3	0.183 (18)	0.211 (16)	0.26 (3)	−0.048 (15)	−0.058 (16)	−0.024 (16)
C4	0.23 (3)	0.219 (16)	0.160 (16)	−0.042 (16)	−0.013 (18)	−0.015 (16)
C5	0.28 (2)	0.28 (2)	0.19 (2)	0.11 (3)	−0.005 (14)	0.005 (14)
C6	0.31 (2)	0.31 (2)	0.18 (2)	0.10 (3)	0.004 (12)	−0.004 (12)
C7	0.32 (3)	0.32 (3)	0.19 (2)	0.04 (3)	0.042 (16)	−0.042 (16)
C8	0.43 (4)	0.43 (4)	0.20 (2)	0.07 (6)	0.01 (2)	−0.01 (2)

Geometric parameters (Å, º) top

U1—O4ⁱ	2.272 (10)	C2—H2A	0.9700
U1—O4ⁱⁱ	2.272 (10)	C2—H2B	0.9700
U1—O4ⁱⁱⁱ	2.272 (10)	C3—C4	1.533 (18)
U1—O4	2.272 (10)	C3—H3A	0.9700
U1—O1ⁱⁱ	2.411 (10)	C3—H3B	0.9700
U1—O1ⁱ	2.411 (10)	C4—H4A	0.9600
U1—O1ⁱⁱⁱ	2.411 (10)	C4—H4B	0.9600
U1—O1	2.411 (10)	C4—H4C	0.9600
Re1—O3	1.636 (13)	C5—C6	1.484 (19)
Re1—O2	1.651 (10)	C5—H5A	0.9700
Re1—O2^iv	1.651 (10)	C5—H5B	0.9700
Re1—O1	1.749 (10)	C6—C7	1.569 (19)
P1—O4	1.506 (11)	C6—H6A	0.9700
P1—C5	1.778 (18)	C6—H6B	0.9700
P1—C1^iv	1.844 (15)	C7—C8	1.50 (2)
P1—C1	1.844 (15)	C7—H7A	0.9700
C1—C2	1.454 (16)	C7—H7B	0.9700
C1—H1A	0.9700	C8—H8A	0.9600
C1—H1B	0.9700	C8—H8B	0.9600
C2—C3	1.518 (17)	C8—H8C	0.9600

O4ⁱ—U1—O4ⁱⁱ	97.1 (2)	C2—C1—H1B	107.4
O4ⁱ—U1—O4ⁱⁱⁱ	138.7 (6)	P1—C1—H1B	107.4
O4ⁱⁱ—U1—O4ⁱⁱⁱ	97.1 (2)	H1A—C1—H1B	106.9
O4ⁱ—U1—O4	97.1 (2)	C1—C2—C3	109.5 (15)
O4ⁱⁱ—U1—O4	138.7 (6)	C1—C2—H2A	109.8
O4ⁱⁱⁱ—U1—O4	97.1 (2)	C3—C2—H2A	109.8
O4ⁱ—U1—O1ⁱⁱ	74.1 (2)	C1—C2—H2B	109.8
O4ⁱⁱ—U1—O1ⁱⁱ	71.6 (4)	C3—C2—H2B	109.8
O4ⁱⁱⁱ—U1—O1ⁱⁱ	74.1 (2)	H2A—C2—H2B	108.2
O4—U1—O1ⁱⁱ	149.6 (4)	C2—C3—C4	100.4 (16)
O4ⁱ—U1—O1ⁱ	71.6 (4)	C2—C3—H3A	111.7
O4ⁱⁱ—U1—O1ⁱ	74.1 (2)	C4—C3—H3A	111.7
O4ⁱⁱⁱ—U1—O1ⁱ	149.6 (4)	C2—C3—H3B	111.7
O4—U1—O1ⁱ	74.1 (2)	C4—C3—H3B	111.7
O1ⁱⁱ—U1—O1ⁱ	127.1 (4)	H3A—C3—H3B	109.5
O4ⁱ—U1—O1ⁱⁱⁱ	149.6 (4)	C3—C4—H4A	109.5
O4ⁱⁱ—U1—O1ⁱⁱⁱ	74.1 (2)	C3—C4—H4B	109.5
O4ⁱⁱⁱ—U1—O1ⁱⁱⁱ	71.6 (4)	H4A—C4—H4B	109.5
O4—U1—O1ⁱⁱⁱ	74.1 (2)	C3—C4—H4C	109.5
O1ⁱⁱ—U1—O1ⁱⁱⁱ	127.1 (4)	H4A—C4—H4C	109.5
O1ⁱ—U1—O1ⁱⁱⁱ	78.0 (6)	H4B—C4—H4C	109.5
O4ⁱ—U1—O1	74.1 (2)	C6—C5—P1	122 (2)
O4ⁱⁱ—U1—O1	149.6 (4)	C6—C5—H5A	106.8
O4ⁱⁱⁱ—U1—O1	74.1 (2)	P1—C5—H5A	106.8
O4—U1—O1	71.6 (4)	C6—C5—H5B	106.8
O1ⁱⁱ—U1—O1	78.0 (6)	P1—C5—H5B	106.8
O1ⁱ—U1—O1	127.1 (4)	H5A—C5—H5B	106.6
O1ⁱⁱⁱ—U1—O1	127.1 (4)	C5—C6—C7	104 (2)
O3—Re1—O2	109.5 (6)	C5—C6—H6A	110.9
O3—Re1—O2^iv	109.5 (6)	C7—C6—H6A	110.9
O2—Re1—O2^iv	106.8 (11)	C5—C6—H6B	110.9
O3—Re1—O1	109.8 (7)	C7—C6—H6B	110.9
O2—Re1—O1	110.6 (5)	H6A—C6—H6B	108.9
O2^iv—Re1—O1	110.6 (5)	C8—C7—C6	104 (2)
O4—P1—C5	104.8 (12)	C8—C7—H7A	111.0
O4—P1—C1^iv	101.5 (6)	C6—C7—H7A	111.0
C5—P1—C1^iv	103.8 (8)	C8—C7—H7B	111.0
O4—P1—C1	101.5 (6)	C6—C7—H7B	111.0
C5—P1—C1	103.8 (8)	H7A—C7—H7B	109.0
C1^iv—P1—C1	137.9 (15)	C7—C8—H8A	109.5
Re1—O1—U1	152.5 (7)	C7—C8—H8B	109.5
P1—O4—U1	162.8 (8)	H8A—C8—H8B	109.5
C2—C1—P1	119.9 (13)	C7—C8—H8C	109.5
C2—C1—H1A	107.4	H8A—C8—H8C	109.5
P1—C1—H1A	107.4	H8B—C8—H8C	109.5

O3—Re1—O1—U1	180.000 (2)	O4ⁱⁱⁱ—U1—O4—P1	−109.4 (2)
O2—Re1—O1—U1	−59.0 (6)	O1ⁱⁱ—U1—O4—P1	180.000 (3)
O2^iv—Re1—O1—U1	59.1 (6)	O1ⁱ—U1—O4—P1	40.9 (3)
O4ⁱ—U1—O1—Re1	103.3 (2)	O1ⁱⁱⁱ—U1—O4—P1	−40.9 (3)
O4ⁱⁱ—U1—O1—Re1	180.0	O1—U1—O4—P1	180.000 (6)
O4ⁱⁱⁱ—U1—O1—Re1	−103.3 (2)	O4—P1—C1—C2	166 (2)
O4—U1—O1—Re1	0.000 (2)	C5—P1—C1—C2	−86 (2)
O1ⁱⁱ—U1—O1—Re1	180.000 (3)	C1^iv—P1—C1—C2	44 (3)
O1ⁱ—U1—O1—Re1	52.15 (11)	P1—C1—C2—C3	−167 (2)
O1ⁱⁱⁱ—U1—O1—Re1	−52.15 (11)	C1—C2—C3—C4	−169 (2)
C5—P1—O4—U1	0.000 (9)	O4—P1—C5—C6	180.000 (6)
C1^iv—P1—O4—U1	−107.8 (8)	C1^iv—P1—C5—C6	−73.9 (7)
C1—P1—O4—U1	107.8 (8)	C1—P1—C5—C6	73.9 (7)
O4ⁱ—U1—O4—P1	109.4 (3)	P1—C5—C6—C7	180.000 (10)
O4ⁱⁱ—U1—O4—P1	0.000 (7)	C5—C6—C7—C8	180.000 (9)

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

(Iat230) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	D_x = 2.005 Mg m⁻³
M_r = 2112.05	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 5703 reflections
a = 21.5289 (15) Å	θ = 2.7–26.2°
b = 21.9148 (16) Å	µ = 9.35 mm⁻¹
c = 14.8288 (11) Å	T = 230 K
V = 6996.3 (9) Å³	Block, green
Z = 4	0.15 × 0.15 × 0.10 mm
F(000) = 4032

Data collection top

CCD area detector diffractometer	6529 independent reflections
Radiation source: fine-focus sealed tube	6180 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
phi and ω scans	θ_max = 25.0°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→25
T_min = 0.334, T_max = 0.455	k = −26→26
25273 measured reflections	l = −17→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.027	H-atom parameters constrained
wR(F²) = 0.068	w = 1/[σ²(F_o²) + (0.0273P)² + 21.6652P] where P = (F_o² + 2F_c²)/3
S = 1.12	(Δ/σ)_max = 0.002
6529 reflections	Δρ_max = 2.23 e Å⁻³
377 parameters	Δρ_min = −1.05 e Å⁻³
324 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.025 (9)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	V = 6996.3 (9) Å³
M_r = 2112.05	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.5289 (15) Å	µ = 9.35 mm⁻¹
b = 21.9148 (16) Å	T = 230 K
c = 14.8288 (11) Å	0.15 × 0.15 × 0.10 mm

Data collection top

CCD area detector diffractometer	6529 independent reflections
Absorption correction: multi-scan SADABS	6180 reflections with I > 2σ(I)
T_min = 0.334, T_max = 0.455	R_int = 0.027
25273 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.027	H-atom parameters constrained
wR(F²) = 0.068	w = 1/[σ²(F_o²) + (0.0273P)² + 21.6652P] where P = (F_o² + 2F_c²)/3
S = 1.12	Δρ_max = 2.23 e Å⁻³
6529 reflections	Δρ_min = −1.05 e Å⁻³
377 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
324 restraints	Absolute structure parameter: 0.025 (9)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	1.0000	0.748499 (15)	0.70272 (3)	0.02929 (9)
Re1	0.855048 (15)	0.760328 (15)	0.87493 (2)	0.04713 (10)
Re2	1.0000	0.59478 (2)	0.55071 (3)	0.04392 (12)
Re3	1.0000	0.87951 (2)	0.51085 (3)	0.04368 (12)
P1	0.84363 (11)	0.73937 (12)	0.59017 (17)	0.0530 (6)
P2	1.0000	0.60898 (17)	0.8435 (3)	0.0723 (11)
P3	1.0000	0.90773 (15)	0.7991 (2)	0.0585 (9)
O1	0.9299 (3)	0.7516 (3)	0.8307 (4)	0.0598 (14)
O2	0.8071 (3)	0.7078 (4)	0.8317 (6)	0.083 (2)
O3	0.8576 (4)	0.7521 (4)	0.9881 (5)	0.083 (2)
O4	0.8267 (4)	0.8306 (3)	0.8506 (5)	0.085 (2)
O5	0.9002 (3)	0.7491 (3)	0.6483 (4)	0.0594 (14)
O6	1.0000	0.6717 (4)	0.5867 (5)	0.0562 (18)
O7	1.0000	0.5926 (5)	0.4359 (7)	0.092 (3)
O8	0.9353 (4)	0.5585 (3)	0.5865 (6)	0.087 (2)
O9	1.0000	0.6545 (4)	0.7673 (6)	0.064 (2)
O10	1.0000	0.8097 (4)	0.5690 (6)	0.0577 (18)
O11	0.9372 (5)	0.9205 (4)	0.5343 (5)	0.109 (3)
O12	1.0000	0.8672 (4)	0.3992 (6)	0.081 (3)
O13	1.0000	0.8465 (4)	0.7505 (7)	0.067 (2)
C1	0.8557 (5)	0.7557 (6)	0.4746 (7)	0.079 (3)
H1A	0.8153	0.7538	0.4441	0.094*
H1B	0.8705	0.7979	0.4698	0.094*
C2	0.8995 (7)	0.7161 (7)	0.4245 (8)	0.104 (4)
H2A	0.8833	0.6743	0.4238	0.125*
H2B	0.9395	0.7156	0.4562	0.125*
C3	0.9102 (7)	0.7380 (6)	0.3247 (8)	0.101 (4)
H3A	0.9216	0.7813	0.3248	0.121*
H3B	0.9448	0.7150	0.2984	0.121*
C4	0.8544 (8)	0.7293 (9)	0.2687 (12)	0.131 (6)
H4A	0.8222	0.7574	0.2881	0.197*
H4B	0.8396	0.6877	0.2751	0.197*
H4C	0.8645	0.7371	0.2060	0.197*
C5	0.8160 (4)	0.6626 (4)	0.6086 (7)	0.063 (2)
H5A	0.8497	0.6343	0.5931	0.075*
H5B	0.8076	0.6577	0.6731	0.075*
C6	0.7587 (4)	0.6432 (4)	0.5573 (8)	0.066 (2)
H6A	0.7666	0.6463	0.4924	0.080*
H6B	0.7243	0.6708	0.5721	0.080*
C7	0.7401 (5)	0.5777 (5)	0.5804 (8)	0.077 (3)
H7A	0.7317	0.5748	0.6452	0.092*
H7B	0.7747	0.5503	0.5663	0.092*
C8	0.6824 (7)	0.5571 (6)	0.5281 (9)	0.114 (5)
H8A	0.6823	0.5130	0.5232	0.171*
H8B	0.6830	0.5750	0.4682	0.171*
H8C	0.6453	0.5704	0.5597	0.171*
C9	0.7818 (4)	0.7903 (4)	0.6221 (7)	0.0598 (19)
H9A	0.7461	0.7833	0.5823	0.072*
H9B	0.7687	0.7806	0.6838	0.072*
C10	0.7998 (5)	0.8571 (4)	0.6175 (8)	0.075 (2)
H10A	0.8126	0.8668	0.5557	0.090*
H10B	0.8356	0.8640	0.6569	0.090*
C11	0.7478 (5)	0.9002 (5)	0.6450 (9)	0.088 (3)
H11A	0.7324	0.8883	0.7046	0.106*
H11B	0.7645	0.9417	0.6497	0.106*
C12	0.6949 (6)	0.9000 (6)	0.5794 (11)	0.113 (5)
H12A	0.6714	0.8625	0.5861	0.169*
H12B	0.7110	0.9027	0.5185	0.169*
H12C	0.6681	0.9346	0.5912	0.169*
C13A	1.0468 (7)	0.5465 (7)	0.8263 (14)	0.088 (5)*	0.637 (15)
H13A	1.0411	0.5167	0.8749	0.105*	0.637 (15)
H13B	1.0365	0.5268	0.7688	0.105*	0.637 (15)
C14A	1.1123 (7)	0.5691 (7)	0.8250 (13)	0.081 (5)*	0.637 (15)
H14A	1.1231	0.5846	0.8850	0.097*	0.637 (15)
H14B	1.1156	0.6030	0.7822	0.097*	0.637 (15)
C15A	1.1593 (9)	0.5188 (8)	0.7981 (14)	0.090 (6)*	0.637 (15)
H15A	1.1487	0.5037	0.7378	0.108*	0.637 (15)
H15B	1.2009	0.5369	0.7946	0.108*	0.637 (15)
C16A	1.1611 (10)	0.4651 (9)	0.8634 (15)	0.094 (6)*	0.637 (15)
H16A	1.1351	0.4324	0.8405	0.140*	0.637 (15)
H16B	1.1458	0.4780	0.9219	0.140*	0.637 (15)
H16C	1.2035	0.4506	0.8694	0.140*	0.637 (15)
C13B	1.0821 (9)	0.5819 (11)	0.847 (2)	0.070 (7)*	0.363 (15)
H13C	1.0998	0.5929	0.7881	0.084*	0.363 (15)
H13D	1.1029	0.6081	0.8912	0.084*	0.363 (15)
C14B	1.1050 (12)	0.5184 (11)	0.866 (2)	0.089 (7)*	0.363 (15)
H14C	1.0758	0.4895	0.8384	0.107*	0.363 (15)
H14D	1.1038	0.5118	0.9311	0.107*	0.363 (15)
C15B	1.1709 (13)	0.5027 (15)	0.832 (3)	0.094 (9)*	0.363 (15)
H15C	1.1726	0.5050	0.7662	0.113*	0.363 (15)
H15D	1.2011	0.5315	0.8571	0.113*	0.363 (15)
C16B	1.1857 (19)	0.4379 (16)	0.864 (4)	0.133 (14)*	0.363 (15)
H16D	1.1531	0.4104	0.8440	0.200*	0.363 (15)
H16E	1.1884	0.4372	0.9290	0.200*	0.363 (15)
H16F	1.2250	0.4250	0.8382	0.200*	0.363 (15)
C17	1.0000	0.6438 (6)	0.9514 (8)	0.073 (4)
H17A	1.0367	0.6701	0.9557	0.088*	0.50
H17B	0.9633	0.6701	0.9557	0.088*	0.50
C18	1.0000	0.6010 (6)	1.0319 (7)	0.072 (4)
H18A	1.0369	0.5748	1.0298	0.086*	0.50
H18B	0.9631	0.5748	1.0298	0.086*	0.50
C19	1.0000	0.6380 (7)	1.1199 (8)	0.091 (5)
H19A	1.0369	0.6641	1.1229	0.109*	0.50
H19B	0.9631	0.6641	1.1229	0.109*	0.50
C20	1.0000	0.5928 (8)	1.1978 (10)	0.115 (7)
H20A	1.0000	0.6149	1.2545	0.173*
H20B	1.0368	0.5674	1.1942	0.173*	0.50
H20C	0.9632	0.5674	1.1942	0.173*	0.50
C21	1.0675 (5)	0.9465 (5)	0.7688 (9)	0.086 (3)
H21A	1.1023	0.9179	0.7755	0.103*
H21B	1.0644	0.9563	0.7045	0.103*
C22	1.0851 (4)	1.0049 (5)	0.8179 (9)	0.083 (3)
H22A	1.0872	0.9965	0.8828	0.100*
H22B	1.0525	1.0353	0.8082	0.100*
C23	1.1469 (5)	1.0312 (6)	0.7872 (11)	0.104 (4)
H23A	1.1797	1.0011	0.7983	0.125*
H23B	1.1452	1.0386	0.7220	0.125*
C24	1.1635 (6)	1.0894 (6)	0.8338 (13)	0.141 (7)
H24A	1.2058	1.1006	0.8187	0.211*
H24B	1.1600	1.0839	0.8985	0.211*
H24C	1.1355	1.1215	0.8145	0.211*
C25	1.0227 (14)	0.9056 (10)	0.9130 (13)	0.116 (8)	0.50
H25A	1.0681	0.9032	0.9136	0.139*	0.50
H25B	1.0117	0.9453	0.9390	0.139*	0.50
C26	1.0000	0.8589 (10)	0.9760 (10)	0.135 (7)
H26A	1.0254	0.8222	0.9680	0.163*	0.50
H26B	0.9574	0.8484	0.9588	0.163*	0.50
C27	1.0000	0.8749 (11)	1.0745 (11)	0.150 (7)
H27A	1.0366	0.9004	1.0858	0.180*	0.50
H27B	0.9634	0.9004	1.0858	0.180*	0.50
C28	1.0000	0.8271 (15)	1.1404 (18)	0.252 (14)
H28A	1.0000	0.8448	1.2003	0.379*
H28B	1.0368	0.8021	1.1327	0.379*	0.50
H28C	0.9632	0.8021	1.1327	0.379*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.02811 (17)	0.02851 (15)	0.03126 (18)	0.000	0.000	−0.00197 (15)
Re1	0.04165 (18)	0.05385 (19)	0.04588 (19)	0.00563 (14)	0.01205 (15)	0.00054 (18)
Re2	0.0556 (3)	0.0362 (2)	0.0400 (2)	0.000	0.000	−0.0066 (2)
Re3	0.0494 (3)	0.0401 (2)	0.0415 (2)	0.000	0.000	0.0099 (2)
P1	0.0397 (12)	0.0718 (16)	0.0474 (12)	−0.0067 (10)	−0.0118 (10)	−0.0023 (11)
P2	0.127 (3)	0.0391 (17)	0.051 (2)	0.000	0.000	0.0109 (14)
P3	0.078 (2)	0.0377 (16)	0.060 (2)	0.000	0.000	−0.0174 (14)
O1	0.045 (3)	0.089 (4)	0.046 (3)	0.000 (2)	0.010 (2)	−0.007 (3)
O2	0.051 (3)	0.084 (4)	0.113 (5)	−0.004 (3)	0.001 (4)	−0.005 (4)
O3	0.084 (5)	0.113 (6)	0.052 (3)	0.013 (4)	0.024 (3)	0.005 (3)
O4	0.087 (5)	0.070 (3)	0.096 (5)	0.025 (3)	0.005 (4)	0.000 (3)
O5	0.036 (3)	0.089 (4)	0.054 (3)	−0.002 (2)	−0.008 (2)	−0.004 (3)
O6	0.089 (5)	0.037 (3)	0.042 (3)	0.000	0.000	−0.007 (3)
O7	0.161 (11)	0.072 (7)	0.043 (4)	0.000	0.000	−0.016 (4)
O8	0.085 (5)	0.053 (4)	0.122 (6)	−0.011 (3)	0.025 (4)	−0.011 (4)
O9	0.109 (6)	0.039 (3)	0.044 (3)	0.000	0.000	0.007 (3)
O10	0.078 (5)	0.045 (3)	0.050 (3)	0.000	0.000	0.014 (3)
O11	0.136 (7)	0.103 (6)	0.087 (6)	0.062 (5)	0.027 (5)	0.033 (4)
O12	0.126 (9)	0.069 (6)	0.047 (3)	0.000	0.000	0.010 (4)
O13	0.095 (6)	0.038 (3)	0.069 (5)	0.000	0.000	−0.018 (3)
C1	0.085 (7)	0.101 (8)	0.050 (3)	−0.019 (5)	−0.007 (4)	−0.012 (4)
C2	0.107 (8)	0.128 (9)	0.077 (5)	0.012 (7)	0.015 (5)	−0.003 (6)
C3	0.106 (9)	0.122 (10)	0.073 (6)	0.009 (8)	0.020 (5)	−0.007 (6)
C4	0.139 (13)	0.153 (15)	0.102 (9)	0.009 (11)	−0.013 (8)	−0.023 (11)
C5	0.056 (5)	0.065 (4)	0.067 (6)	0.007 (3)	−0.020 (4)	−0.008 (4)
C6	0.053 (5)	0.067 (4)	0.079 (6)	−0.005 (4)	−0.020 (4)	−0.001 (5)
C7	0.077 (6)	0.072 (5)	0.082 (7)	−0.013 (5)	−0.020 (5)	0.016 (5)
C8	0.119 (10)	0.101 (9)	0.122 (13)	−0.044 (7)	−0.055 (8)	0.011 (9)
C9	0.049 (4)	0.063 (4)	0.067 (5)	0.000 (3)	−0.021 (4)	0.007 (4)
C10	0.081 (6)	0.066 (4)	0.078 (6)	−0.017 (4)	−0.020 (5)	−0.001 (5)
C11	0.101 (7)	0.056 (5)	0.107 (9)	−0.006 (5)	−0.021 (6)	0.004 (6)
C12	0.114 (9)	0.079 (8)	0.146 (13)	0.012 (7)	−0.046 (8)	0.005 (8)
C17	0.126 (11)	0.049 (7)	0.045 (4)	0.000	0.000	0.018 (4)
C18	0.113 (10)	0.057 (7)	0.044 (4)	0.000	0.000	0.021 (4)
C19	0.150 (13)	0.080 (9)	0.044 (5)	0.000	0.000	0.015 (5)
C20	0.22 (2)	0.088 (11)	0.039 (5)	0.000	0.000	0.011 (7)
C21	0.070 (6)	0.082 (6)	0.106 (7)	−0.014 (4)	0.010 (6)	−0.054 (5)
C22	0.062 (5)	0.071 (6)	0.116 (8)	−0.008 (4)	0.002 (5)	−0.048 (5)
C23	0.068 (7)	0.094 (8)	0.150 (11)	−0.017 (5)	0.017 (7)	−0.051 (8)
C24	0.086 (9)	0.112 (11)	0.224 (19)	−0.039 (7)	0.014 (11)	−0.077 (11)
C25	0.19 (2)	0.091 (13)	0.062 (5)	0.006 (12)	−0.020 (8)	−0.023 (6)
C26	0.222 (19)	0.119 (13)	0.066 (6)	0.000	0.000	−0.013 (6)
C27	0.21 (2)	0.167 (17)	0.067 (7)	0.000	0.000	−0.007 (8)
C28	0.38 (4)	0.27 (3)	0.104 (12)	0.000	0.000	0.065 (17)

Geometric parameters (Å, º) top

U1—O13	2.262 (8)	C11—H11A	0.9800
U1—O9	2.271 (8)	C11—H11B	0.9800
U1—O5ⁱ	2.294 (6)	C12—H12A	0.9700
U1—O5	2.294 (6)	C12—H12B	0.9700
U1—O10	2.393 (8)	C12—H12C	0.9700
U1—O6	2.407 (8)	C13A—C14A	1.497 (16)
U1—O1ⁱ	2.426 (6)	C13A—H13A	0.9800
U1—O1	2.426 (6)	C13A—H13B	0.9800
Re1—O2	1.674 (8)	C14A—C15A	1.548 (16)
Re1—O3	1.688 (8)	C14A—H14A	0.9800
Re1—O4	1.696 (7)	C14A—H14B	0.9800
Re1—O1	1.750 (6)	C15A—C16A	1.526 (17)
Re2—O8	1.689 (7)	C15A—H15A	0.9800
Re2—O8ⁱ	1.689 (7)	C15A—H15B	0.9800
Re2—O7	1.703 (10)	C16A—H16A	0.9700
Re2—O6	1.769 (8)	C16A—H16B	0.9700
Re3—O11ⁱ	1.661 (8)	C16A—H16C	0.9700
Re3—O11	1.661 (8)	C13B—C14B	1.504 (18)
Re3—O12	1.677 (9)	C13B—H13C	0.9800
Re3—O10	1.757 (8)	C13B—H13D	0.9800
P1—O5	1.508 (6)	C14B—C15B	1.543 (19)
P1—C1	1.770 (12)	C14B—H14C	0.9800
P1—C9	1.801 (10)	C14B—H14D	0.9800
P1—C5	1.806 (10)	C15B—C16B	1.527 (19)
P2—O9	1.508 (9)	C15B—H15C	0.9800
P2—C13Aⁱ	1.719 (14)	C15B—H15D	0.9800
P2—C13A	1.719 (14)	C16B—H16D	0.9700
P2—C17	1.773 (14)	C16B—H16E	0.9700
P2—C13B	1.865 (16)	C16B—H16F	0.9700
P2—C13Bⁱ	1.865 (16)	C17—C18	1.518 (12)
P3—O13	1.523 (8)	C17—H17A	0.9800
P3—C21	1.742 (11)	C17—H17B	0.9800
P3—C21ⁱ	1.742 (11)	C18—C19	1.537 (14)
P3—C25	1.76 (2)	C18—H18A	0.9800
P3—C25ⁱ	1.76 (2)	C18—H18B	0.9800
C1—C2	1.481 (13)	C19—C20	1.521 (15)
C1—H1A	0.9800	C19—H19A	0.9800
C1—H1B	0.9800	C19—H19B	0.9800
C2—C3	1.573 (13)	C20—H20A	0.9700
C2—H2A	0.9800	C20—H20B	0.9700
C2—H2B	0.9800	C20—H20C	0.9700
C3—C4	1.474 (14)	C21—C22	1.521 (11)
C3—H3A	0.9800	C21—H21A	0.9800
C3—H3B	0.9800	C21—H21B	0.9800
C4—H4A	0.9700	C22—C23	1.521 (12)
C4—H4B	0.9700	C22—H22A	0.9800
C4—H4C	0.9700	C22—H22B	0.9800
C5—C6	1.512 (10)	C23—C24	1.494 (13)
C5—H5A	0.9800	C23—H23A	0.9800
C5—H5B	0.9800	C23—H23B	0.9800
C6—C7	1.528 (11)	C24—H24A	0.9700
C6—H6A	0.9800	C24—H24B	0.9700
C6—H6B	0.9800	C24—H24C	0.9700
C7—C8	1.532 (12)	C25—C26	1.469 (17)
C7—H7A	0.9800	C25—H25A	0.9800
C7—H7B	0.9800	C25—H25B	0.9800
C8—H8A	0.9700	C26—C27	1.501 (17)
C8—H8B	0.9700	C26—H26A	0.9800
C8—H8C	0.9700	C26—H26B	0.9800
C9—C10	1.516 (11)	C27—C28	1.432 (18)
C9—H9A	0.9800	C27—H27A	0.9800
C9—H9B	0.9800	C27—H27B	0.9800
C10—C11	1.520 (12)	C28—H28A	0.9700
C10—H10A	0.9800	C28—H28B	0.9700
C10—H10B	0.9800	C28—H28C	0.9700
C11—C12	1.498 (13)

O13—U1—O9	136.8 (3)	C9—C10—H10A	108.9
O13—U1—O5ⁱ	96.00 (18)	C11—C10—H10A	108.9
O9—U1—O5ⁱ	98.84 (18)	C9—C10—H10B	108.9
O13—U1—O5	96.00 (18)	C11—C10—H10B	108.9
O9—U1—O5	98.84 (18)	H10A—C10—H10B	107.7
O5ⁱ—U1—O5	138.8 (3)	C12—C11—C10	112.6 (10)
O13—U1—O10	74.2 (3)	C12—C11—H11A	109.1
O9—U1—O10	149.0 (3)	C10—C11—H11A	109.1
O5ⁱ—U1—O10	72.86 (17)	C12—C11—H11B	109.1
O5—U1—O10	72.86 (17)	C10—C11—H11B	109.1
O13—U1—O6	152.6 (3)	H11A—C11—H11B	107.8
O9—U1—O6	70.6 (3)	C11—C12—H12A	109.5
O5ⁱ—U1—O6	75.69 (17)	C11—C12—H12B	109.5
O5—U1—O6	75.68 (17)	H12A—C12—H12B	109.5
O10—U1—O6	78.4 (3)	C11—C12—H12C	109.5
O13—U1—O1ⁱ	74.2 (2)	H12A—C12—H12C	109.5
O9—U1—O1ⁱ	72.3 (2)	H12B—C12—H12C	109.5
O5ⁱ—U1—O1ⁱ	72.1 (2)	C14A—C13A—P2	106.9 (11)
O5—U1—O1ⁱ	149.0 (2)	C14A—C13A—H13A	110.3
O10—U1—O1ⁱ	129.2 (2)	P2—C13A—H13A	110.3
O6—U1—O1ⁱ	125.4 (2)	C14A—C13A—H13B	110.3
O13—U1—O1	74.2 (2)	P2—C13A—H13B	110.3
O9—U1—O1	72.3 (2)	H13A—C13A—H13B	108.6
O5ⁱ—U1—O1	149.0 (2)	C13A—C14A—C15A	112.6 (14)
O5—U1—O1	72.1 (2)	C13A—C14A—H14A	109.1
O10—U1—O1	129.2 (2)	C15A—C14A—H14A	109.1
O6—U1—O1	125.4 (2)	C13A—C14A—H14B	109.1
O1ⁱ—U1—O1	77.0 (3)	C15A—C14A—H14B	109.1
O2—Re1—O3	109.1 (4)	H14A—C14A—H14B	107.8
O2—Re1—O4	108.7 (4)	C16A—C15A—C14A	113.7 (15)
O3—Re1—O4	108.7 (4)	C16A—C15A—H15A	108.8
O2—Re1—O1	110.5 (3)	C14A—C15A—H15A	108.8
O3—Re1—O1	109.3 (3)	C16A—C15A—H15B	108.8
O4—Re1—O1	110.5 (4)	C14A—C15A—H15B	108.8
O8—Re2—O8ⁱ	111.0 (6)	H15A—C15A—H15B	107.7
O8—Re2—O7	107.5 (4)	C15A—C16A—H16A	109.5
O8ⁱ—Re2—O7	107.5 (4)	C15A—C16A—H16B	109.5
O8—Re2—O6	110.7 (3)	H16A—C16A—H16B	109.5
O8ⁱ—Re2—O6	110.7 (3)	C15A—C16A—H16C	109.5
O7—Re2—O6	109.1 (4)	H16A—C16A—H16C	109.5
O11ⁱ—Re3—O11	109.1 (8)	H16B—C16A—H16C	109.5
O11ⁱ—Re3—O12	107.1 (3)	C14B—C13B—P2	127.5 (18)
O11—Re3—O12	107.1 (3)	C14B—C13B—H13C	105.4
O11ⁱ—Re3—O10	111.6 (3)	P2—C13B—H13C	105.4
O11—Re3—O10	111.6 (3)	C14B—C13B—H13D	105.4
O12—Re3—O10	110.2 (4)	P2—C13B—H13D	105.4
O5—P1—C1	114.0 (5)	H13C—C13B—H13D	106.0
O5—P1—C9	111.1 (4)	C13B—C14B—C15B	117 (2)
C1—P1—C9	103.7 (5)	C13B—C14B—H14C	108.2
O5—P1—C5	108.2 (4)	C15B—C14B—H14C	108.2
C1—P1—C5	112.5 (5)	C13B—C14B—H14D	108.2
C9—P1—C5	107.1 (4)	C15B—C14B—H14D	108.2
O9—P2—C13Aⁱ	114.6 (7)	H14C—C14B—H14D	107.3
O9—P2—C13A	114.6 (7)	C16B—C15B—C14B	107 (2)
C13Aⁱ—P2—C13A	71.7 (11)	C16B—C15B—H15C	110.2
O9—P2—C17	113.1 (5)	C14B—C15B—H15C	110.2
C13Aⁱ—P2—C17	118.5 (8)	C16B—C15B—H15D	110.2
C13A—P2—C17	118.5 (8)	C14B—C15B—H15D	110.2
O9—P2—C13B	103.3 (8)	H15C—C15B—H15D	108.5
C13Aⁱ—P2—C13B	107.8 (10)	C15B—C16B—H16D	109.5
C13A—P2—C13B	36.5 (9)	C15B—C16B—H16E	109.5
C17—P2—C13B	96.5 (10)	H16D—C16B—H16E	109.5
O9—P2—C13Bⁱ	103.3 (8)	C15B—C16B—H16F	109.5
C13Aⁱ—P2—C13Bⁱ	36.5 (9)	H16D—C16B—H16F	109.5
C13A—P2—C13Bⁱ	107.8 (10)	H16E—C16B—H16F	109.5
C17—P2—C13Bⁱ	96.5 (10)	C18—C17—P2	116.4 (10)
C13B—P2—C13Bⁱ	142.8 (16)	C18—C17—H17A	108.2
O13—P3—C21	107.9 (4)	P2—C17—H17A	108.2
O13—P3—C21ⁱ	107.9 (4)	C18—C17—H17B	108.2
C21—P3—C21ⁱ	113.1 (9)	P2—C17—H17B	108.2
O13—P3—C25	115.5 (8)	H17A—C17—H17B	107.3
C21—P3—C25	91.6 (10)	C17—C18—C19	110.0 (11)
C21ⁱ—P3—C25	119.5 (10)	C17—C18—H18A	109.7
O13—P3—C25ⁱ	115.5 (8)	C19—C18—H18A	109.7
C21—P3—C25ⁱ	119.5 (10)	C17—C18—H18B	109.7
C21ⁱ—P3—C25ⁱ	91.6 (10)	C19—C18—H18B	109.7
C25—P3—C25ⁱ	32.2 (19)	H18A—C18—H18B	108.2
Re1—O1—U1	150.4 (4)	C20—C19—C18	107.5 (12)
P1—O5—U1	163.1 (4)	C20—C19—H19A	110.2
Re2—O6—U1	151.9 (4)	C18—C19—H19A	110.2
P2—O9—U1	156.4 (6)	C20—C19—H19B	110.2
Re3—O10—U1	153.5 (5)	C18—C19—H19B	110.2
P3—O13—U1	170.1 (7)	H19A—C19—H19B	108.5
C2—C1—P1	117.4 (9)	C19—C20—H20A	109.5
C2—C1—H1A	108.0	C19—C20—H20B	109.5
P1—C1—H1A	108.0	H20A—C20—H20B	109.5
C2—C1—H1B	108.0	C19—C20—H20C	109.5
P1—C1—H1B	108.0	H20A—C20—H20C	109.5
H1A—C1—H1B	107.2	H20B—C20—H20C	109.5
C1—C2—C3	112.7 (11)	C22—C21—P3	119.6 (8)
C1—C2—H2A	109.0	C22—C21—H21A	107.4
C3—C2—H2A	109.0	P3—C21—H21A	107.4
C1—C2—H2B	109.0	C22—C21—H21B	107.4
C3—C2—H2B	109.0	P3—C21—H21B	107.4
H2A—C2—H2B	107.8	H21A—C21—H21B	106.9
C4—C3—C2	111.8 (13)	C21—C22—C23	113.2 (9)
C4—C3—H3A	109.3	C21—C22—H22A	108.9
C2—C3—H3A	109.3	C23—C22—H22A	108.9
C4—C3—H3B	109.3	C21—C22—H22B	108.9
C2—C3—H3B	109.3	C23—C22—H22B	108.9
H3A—C3—H3B	107.9	H22A—C22—H22B	107.8
C3—C4—H4A	109.5	C24—C23—C22	113.2 (10)
C3—C4—H4B	109.5	C24—C23—H23A	108.9
H4A—C4—H4B	109.5	C22—C23—H23A	108.9
C3—C4—H4C	109.5	C24—C23—H23B	108.9
H4A—C4—H4C	109.5	C22—C23—H23B	108.9
H4B—C4—H4C	109.5	H23A—C23—H23B	107.7
C6—C5—P1	117.0 (7)	C23—C24—H24A	109.5
C6—C5—H5A	108.0	C23—C24—H24B	109.5
P1—C5—H5A	108.0	H24A—C24—H24B	109.5
C6—C5—H5B	108.0	C23—C24—H24C	109.5
P1—C5—H5B	108.0	H24A—C24—H24C	109.5
H5A—C5—H5B	107.3	H24B—C24—H24C	109.5
C5—C6—C7	111.4 (8)	C26—C25—P3	122.5 (16)
C5—C6—H6A	109.3	C26—C25—H25A	106.7
C7—C6—H6A	109.3	P3—C25—H25A	106.7
C5—C6—H6B	109.3	C26—C25—H25B	106.7
C7—C6—H6B	109.3	P3—C25—H25B	106.7
H6A—C6—H6B	108.0	H25A—C25—H25B	106.6
C6—C7—C8	112.1 (8)	C25—C26—C27	117.2 (16)
C6—C7—H7A	109.2	C25—C26—H26A	108.0
C8—C7—H7A	109.2	C27—C26—H26A	108.0
C6—C7—H7B	109.2	C25—C26—H26B	108.0
C8—C7—H7B	109.2	C27—C26—H26B	108.0
H7A—C7—H7B	107.9	H26A—C26—H26B	107.3
C7—C8—H8A	109.5	C28—C27—C26	120 (2)
C7—C8—H8B	109.5	C28—C27—H27A	107.4
H8A—C8—H8B	109.5	C26—C27—H27A	107.4
C7—C8—H8C	109.5	C28—C27—H27B	107.4
H8A—C8—H8C	109.5	C26—C27—H27B	107.4
H8B—C8—H8C	109.5	H27A—C27—H27B	107.0
C10—C9—P1	113.4 (7)	C27—C28—H28A	109.5
C10—C9—H9A	108.9	C27—C28—H28B	109.5
P1—C9—H9A	108.9	H28A—C28—H28B	109.5
C10—C9—H9B	108.9	C27—C28—H28C	109.5
P1—C9—H9B	108.9	H28A—C28—H28C	109.5
H9A—C9—H9B	107.7	H28B—C28—H28C	109.5
C9—C10—C11	113.6 (9)

O2—Re1—O1—U1	59.0 (8)	O9—U1—O13—P3	0.000 (15)
O3—Re1—O1—U1	179.0 (7)	O5ⁱ—U1—O13—P3	−109.74 (17)
O4—Re1—O1—U1	−61.4 (8)	O5—U1—O13—P3	109.74 (17)
O13—U1—O1—Re1	91.9 (7)	O10—U1—O13—P3	180.000 (13)
O9—U1—O1—Re1	−115.8 (7)	O6—U1—O13—P3	180.000 (10)
O5ⁱ—U1—O1—Re1	166.8 (5)	O1ⁱ—U1—O13—P3	−40.29 (17)
O5—U1—O1—Re1	−10.0 (7)	O1—U1—O13—P3	40.29 (17)
O10—U1—O1—Re1	38.4 (8)	O5—P1—C1—C2	65.8 (11)
O6—U1—O1—Re1	−66.8 (8)	C9—P1—C1—C2	−173.3 (10)
O1ⁱ—U1—O1—Re1	168.9 (6)	C5—P1—C1—C2	−57.8 (12)
C1—P1—O5—U1	−46.2 (16)	P1—C1—C2—C3	−175.7 (9)
C9—P1—O5—U1	−162.9 (13)	C1—C2—C3—C4	−69.1 (17)
C5—P1—O5—U1	79.8 (15)	O5—P1—C5—C6	179.3 (7)
O13—U1—O5—P1	137.7 (14)	C1—P1—C5—C6	−53.9 (10)
O9—U1—O5—P1	−83.0 (14)	C9—P1—C5—C6	59.5 (9)
O5ⁱ—U1—O5—P1	31.4 (18)	P1—C5—C6—C7	−179.2 (8)
O10—U1—O5—P1	66.2 (14)	C5—C6—C7—C8	−179.3 (11)
O6—U1—O5—P1	−15.8 (14)	O5—P1—C9—C10	57.5 (8)
O1ⁱ—U1—O5—P1	−153.2 (12)	C1—P1—C9—C10	−65.4 (8)
O1—U1—O5—P1	−151.1 (15)	C5—P1—C9—C10	175.4 (7)
O8—Re2—O6—U1	61.8 (3)	P1—C9—C10—C11	−179.6 (8)
O8ⁱ—Re2—O6—U1	−61.8 (3)	C9—C10—C11—C12	−67.7 (14)
O7—Re2—O6—U1	180.000 (2)	O9—P2—C13A—C14A	66.3 (15)
O13—U1—O6—Re2	180.0	C13Aⁱ—P2—C13A—C14A	175.6 (9)
O9—U1—O6—Re2	0.000 (3)	C17—P2—C13A—C14A	−71.3 (15)
O5ⁱ—U1—O6—Re2	104.97 (17)	C13B—P2—C13A—C14A	−12.5 (18)
O5—U1—O6—Re2	−104.96 (17)	C13Bⁱ—P2—C13A—C14A	−179.3 (14)
O10—U1—O6—Re2	180.000 (4)	P2—C13A—C14A—C15A	−172.8 (13)
O1ⁱ—U1—O6—Re2	49.8 (2)	C13A—C14A—C15A—C16A	−62 (2)
O1—U1—O6—Re2	−49.8 (2)	O9—P2—C13B—C14B	−143 (3)
C13Aⁱ—P2—O9—U1	139.9 (7)	C13Aⁱ—P2—C13B—C14B	−21 (3)
C13A—P2—O9—U1	−139.9 (7)	C13A—P2—C13B—C14B	−29 (2)
C17—P2—O9—U1	0.000 (5)	C17—P2—C13B—C14B	102 (3)
C13B—P2—O9—U1	−103.1 (9)	C13Bⁱ—P2—C13B—C14B	−8 (5)
C13Bⁱ—P2—O9—U1	103.1 (9)	P2—C13B—C14B—C15B	159 (3)
O13—U1—O9—P2	0.000 (5)	C13B—C14B—C15B—C16B	177 (3)
O5ⁱ—U1—O9—P2	108.68 (17)	O9—P2—C17—C18	180.000 (4)
O5—U1—O9—P2	−108.68 (17)	C13Aⁱ—P2—C17—C18	41.8 (6)
O10—U1—O9—P2	180.000 (3)	C13A—P2—C17—C18	−41.8 (6)
O6—U1—O9—P2	180.000 (4)	C13B—P2—C17—C18	−72.5 (8)
O1ⁱ—U1—O9—P2	40.78 (17)	C13Bⁱ—P2—C17—C18	72.5 (8)
O1—U1—O9—P2	−40.78 (17)	P2—C17—C18—C19	180.000 (6)
O11ⁱ—Re3—O10—U1	61.2 (4)	C17—C18—C19—C20	180.000 (7)
O11—Re3—O10—U1	−61.2 (4)	O13—P3—C21—C22	−170.7 (10)
O12—Re3—O10—U1	180.000 (3)	C21ⁱ—P3—C21—C22	70.0 (14)
O13—U1—O10—Re3	0.000 (3)	C25—P3—C21—C22	−53.1 (14)
O9—U1—O10—Re3	180.0	C25ⁱ—P3—C21—C22	−36.0 (15)
O5ⁱ—U1—O10—Re3	−101.59 (18)	P3—C21—C22—C23	176.9 (10)
O5—U1—O10—Re3	101.59 (18)	C21—C22—C23—C24	178.6 (14)
O6—U1—O10—Re3	180.000 (3)	O13—P3—C25—C26	−44 (2)
O1ⁱ—U1—O10—Re3	−53.4 (2)	C21—P3—C25—C26	−155 (2)
O1—U1—O10—Re3	53.4 (2)	C21ⁱ—P3—C25—C26	87 (2)
C21—P3—O13—U1	118.7 (5)	C25ⁱ—P3—C25—C26	54 (2)
C21ⁱ—P3—O13—U1	−118.7 (5)	P3—C25—C26—C27	−155.5 (13)
C25—P3—O13—U1	17.9 (11)	C25—C26—C27—C28	−158.1 (15)
C25ⁱ—P3—O13—U1	−17.9 (11)

Symmetry code: (i) −x+2, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C18—H18A···O8ⁱⁱ	0.98	3.10	3.849 (13)	134
C18—H18B···O8ⁱⁱⁱ	0.98	3.10	3.849 (13)	134
C2—H2B···O6	0.98	2.52	3.377 (15)	146
C2—H2B···O10	0.98	2.96	3.670 (17)	131
C3—H3A···O12	0.98	2.76	3.603 (17)	145
C5—H5A···O8	0.98	2.48	3.450 (12)	169
C5—H5B···O2	0.98	2.60	3.460 (13)	147
C9—H9B···O2	0.98	2.84	3.637 (13)	140
C9—H9B···O4	0.98	2.98	3.632 (12)	125
C10—H10A···O11	0.98	2.95	3.492 (15)	116
C10—H10B···O4	0.98	2.97	3.552 (14)	119
C10—H10B···O5	0.98	2.88	3.238 (12)	103
C14A—H14B···O9	0.98	2.74	3.176 (17)	108
C14A—H14B···O9	0.98	2.74	3.176 (17)	108
C17—H17B···O1	0.98	2.67	3.327 (12)	124
C17—H17B···O3	0.98	2.94	3.915 (11)	174
C26—H26B···O1	0.98	2.91	3.529 (18)	122
C4—H4A···O2^iv	0.97	2.96	3.854 (19)	154
C6—H6A···O4^iv	0.98	2.95	3.620 (12)	126
C6—H6B···O3^iv	0.98	2.74	3.548 (12)	140
C8—H8B···O4^iv	0.97	2.71	3.608 (14)	153
C9—H9A···O3^iv	0.98	2.75	3.717 (11)	171
C12—H12A···O3^iv	0.97	2.97	3.771 (15)	141
C14B—H14C···O7ⁱⁱ	0.98	2.83	3.48 (3)	125
C14B—H14D···O8ⁱⁱ	0.98	2.90	3.78 (3)	151
C13A—H13A···O7ⁱⁱ	0.98	2.71	3.60 (2)	151
C13A—H13A···O7ⁱⁱ	0.98	2.71	3.60 (2)	151
C14B—H14C···O7ⁱⁱ	0.98	2.83	3.48 (3)	125
C13A—H13A···O7ⁱⁱⁱ	0.98	2.71	3.60 (2)	151
C14B—H14C···O7ⁱⁱⁱ	0.98	2.83	3.48 (3)	125
C13A—H13A···O7ⁱⁱⁱ	0.98	2.71	3.60 (2)	151
C14B—H14C···O7ⁱⁱⁱ	0.98	2.83	3.48 (3)	125
C17—H17A···O1ⁱ	0.98	2.67	3.327 (12)	124
C17—H17A···O3ⁱ	0.98	2.94	3.915 (12)	174
C13A—H13B···O8ⁱ	0.98	2.86	3.59 (2)	132
C13B—H13D···O2ⁱ	0.98	3.05	3.65 (3)	121
C21—H21A···O4ⁱ	0.98	2.69	3.620 (15)	158
C21—H21B···O11ⁱ	0.98	2.64	3.524 (15)	150
C25—H25A···O4ⁱ	0.98	2.92	3.75 (3)	143
C26—H26A···O1ⁱ	0.98	2.73	3.529 (18)	139
C26—H26A···O3ⁱ	0.98	2.97	3.861 (15)	153
C14A—H14B···O2ⁱ	0.98	2.93	3.502 (18)	118
C20—H20A···O7^v	0.97	2.73	3.531 (18)	140
C28—H28A···O12^v	0.97	2.99	3.94 (3)	166
C20—H20A···O7^vi	0.97	2.73	3.531 (18)	140
C28—H28A···O12^vi	0.97	2.99	3.94 (3)	166
C22—H22A···O11^vii	0.98	2.94	3.634 (13)	129
C22—H22B···O12^vii	0.98	2.77	3.559 (13)	138
C24—H24B···O11^vii	0.97	2.91	3.69 (2)	138
C22—H22B···O12^viii	0.98	2.77	3.559 (13)	138
C16B—H16F···O4^ix	0.97	3.02	3.84 (3)	144
C16A—H16A···O7ⁱⁱ	0.97	3.28	3.84 (2)	119
C16A—H16B···O8ⁱⁱ	0.97	3.11	3.94 (2)	145

Symmetry codes: (i) −x+2, y, z; (ii) −x+2, −y+1, z+1/2; (iii) x, −y+1, z+1/2; (iv) −x+3/2, −y+3/2, z−1/2; (v) x, y, z+1; (vi) −x+2, y, z+1; (vii) −x+2, −y+2, z+1/2; (viii) x, −y+2, z+1/2; (ix) x+1/2, y−1/2, z.

(Iat165) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	D_x = 2.032 Mg m⁻³ D_m = 0 Mg m⁻³ D_m measured by not measured
M_r = 2112.05	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 7236 reflections
a = 21.4344 (15) Å	θ = 2.7–26.4°
b = 21.7929 (15) Å	µ = 9.48 mm⁻¹
c = 14.7782 (10) Å	T = 165 K
V = 6903.2 (8) Å³	Block, green
Z = 4	0.15 × 0.15 × 0.10 mm
F(000) = 4032

Data collection top

CCD area detector diffractometer	6428 independent reflections
Radiation source: fine-focus sealed tube	6171 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.029
phi and ω scans	θ_max = 25.0°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→25
T_min = 0.331, T_max = 0.451	k = −25→25
24887 measured reflections	l = −17→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.025	H-atom parameters constrained
wR(F²) = 0.065	w = 1/[σ²(F_o²) + (0.0227P)² + 46.403P] where P = (F_o² + 2F_c²)/3
S = 1.11	(Δ/σ)_max = 0.007
6428 reflections	Δρ_max = 2.33 e Å⁻³
417 parameters	Δρ_min = −1.21 e Å⁻³
152 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.020 (9)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	V = 6903.2 (8) Å³
M_r = 2112.05	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.4344 (15) Å	µ = 9.48 mm⁻¹
b = 21.7929 (15) Å	T = 165 K
c = 14.7782 (10) Å	0.15 × 0.15 × 0.10 mm

Data collection top

CCD area detector diffractometer	6428 independent reflections
Absorption correction: multi-scan SADABS	6171 reflections with I > 2σ(I)
T_min = 0.331, T_max = 0.451	R_int = 0.029
24887 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	H-atom parameters constrained
wR(F²) = 0.065	w = 1/[σ²(F_o²) + (0.0227P)² + 46.403P] where P = (F_o² + 2F_c²)/3
S = 1.11	Δρ_max = 2.33 e Å⁻³
6428 reflections	Δρ_min = −1.21 e Å⁻³
417 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
152 restraints	Absolute structure parameter: 0.020 (9)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	1.0000	0.748665 (16)	0.70241 (3)	0.01972 (9)
Re1	0.854642 (15)	0.762088 (15)	0.87518 (2)	0.03206 (9)
Re2	1.0000	0.59180 (2)	0.55403 (3)	0.02911 (11)
Re3	1.0000	0.87773 (2)	0.50691 (3)	0.02897 (11)
P1	0.84170 (10)	0.73947 (11)	0.59145 (15)	0.0319 (5)
P2	1.0000	0.61055 (18)	0.8492 (3)	0.0606 (12)
P3	1.0000	0.91022 (14)	0.7943 (2)	0.0391 (8)
O1	0.9298 (3)	0.7540 (3)	0.8311 (4)	0.0441 (16)
O2	0.8064 (3)	0.7095 (4)	0.8319 (6)	0.064 (2)
O3	0.8573 (3)	0.7524 (4)	0.9895 (5)	0.057 (2)
O4	0.8262 (4)	0.8328 (4)	0.8510 (5)	0.068 (2)
O5	0.8997 (3)	0.7497 (3)	0.6491 (4)	0.0359 (14)
O6	1.0000	0.6688 (3)	0.5899 (5)	0.037 (2)
O7	1.0000	0.5895 (5)	0.4374 (6)	0.061 (3)
O8	0.9351 (4)	0.5555 (3)	0.5909 (6)	0.064 (2)
O9	1.0000	0.6548 (4)	0.7699 (6)	0.053 (3)
O10	1.0000	0.8075 (4)	0.5641 (5)	0.039 (2)
O11	0.9373 (5)	0.9194 (4)	0.5316 (6)	0.090 (3)
O12	1.0000	0.8653 (4)	0.3935 (6)	0.062 (3)
O13	1.0000	0.8482 (4)	0.7462 (6)	0.050 (2)
C1	0.8548 (4)	0.7545 (5)	0.4730 (6)	0.041 (2)
H1A	0.8142	0.7518	0.4412	0.049*
H1B	0.8698	0.7973	0.4667	0.049*
C2	0.9000 (5)	0.7132 (5)	0.4261 (7)	0.052 (3)
H2A	0.8838	0.6706	0.4271	0.062*
H2B	0.9402	0.7137	0.4589	0.062*
C3	0.9108 (6)	0.7334 (6)	0.3261 (7)	0.064 (3)
H3A	0.9256	0.7764	0.3255	0.077*
H3B	0.9441	0.7076	0.2995	0.077*
C4	0.8546 (6)	0.7286 (6)	0.2692 (10)	0.073 (4)
H4A	0.8230	0.7577	0.2908	0.109*
H4B	0.8379	0.6868	0.2727	0.109*
H4C	0.8653	0.7382	0.2063	0.109*
C5	0.8157 (4)	0.6619 (4)	0.6081 (6)	0.038 (2)
H5A	0.8506	0.6341	0.5923	0.045*
H5B	0.8071	0.6562	0.6734	0.045*
C6	0.7585 (4)	0.6410 (4)	0.5559 (7)	0.045 (2)
H6A	0.7229	0.6680	0.5715	0.054*
H6B	0.7666	0.6454	0.4903	0.054*
C7	0.7413 (5)	0.5757 (5)	0.5759 (8)	0.058 (3)
H7A	0.7318	0.5719	0.6413	0.069*
H7B	0.7776	0.5491	0.5626	0.069*
C8	0.6852 (7)	0.5531 (6)	0.5215 (10)	0.090 (5)
H8A	0.6863	0.5082	0.5177	0.135*
H8B	0.6866	0.5705	0.4605	0.135*
H8C	0.6466	0.5659	0.5516	0.135*
C9	0.7800 (4)	0.7911 (4)	0.6246 (6)	0.038 (2)
H9A	0.7434	0.7839	0.5853	0.045*
H9B	0.7676	0.7817	0.6876	0.045*
C10	0.7985 (5)	0.8582 (4)	0.6185 (7)	0.046 (2)
H10A	0.8354	0.8653	0.6574	0.055*
H10B	0.8106	0.8677	0.5554	0.055*
C11	0.7467 (5)	0.9018 (4)	0.6473 (8)	0.053 (3)
H11A	0.7314	0.8896	0.7079	0.064*
H11B	0.7639	0.9439	0.6521	0.064*
C12	0.6931 (6)	0.9023 (6)	0.5827 (11)	0.080 (4)
H12A	0.6691	0.8643	0.5893	0.121*
H12B	0.7089	0.9055	0.5206	0.121*
H12C	0.6662	0.9376	0.5957	0.121*
C13A	1.0483 (7)	0.5488 (7)	0.8327 (12)	0.063 (4)	0.687 (16)
H13A	1.0443	0.5195	0.8835	0.076*	0.687 (16)
H13B	1.0372	0.5273	0.7759	0.076*	0.687 (16)
C14A	1.1110 (9)	0.5715 (8)	0.8276 (13)	0.066 (4)	0.687 (16)
H14A	1.1222	0.5897	0.8868	0.080*	0.687 (16)
H14B	1.1127	0.6046	0.7818	0.080*	0.687 (16)
C15A	1.1603 (11)	0.5221 (9)	0.8029 (14)	0.063 (4)	0.687 (16)
H15A	1.1546	0.5104	0.7387	0.075*	0.687 (16)
H15B	1.2024	0.5404	0.8089	0.075*	0.687 (16)
C16A	1.1576 (10)	0.4651 (11)	0.8598 (17)	0.065 (5)	0.687 (16)
H16A	1.1302	0.4349	0.8308	0.097*	0.687 (16)
H16B	1.1413	0.4752	0.9198	0.097*	0.687 (16)
H16C	1.1996	0.4478	0.8658	0.097*	0.687 (16)
C13B	1.0810 (10)	0.5803 (16)	0.860 (3)	0.061 (6)	0.313 (16)
H13C	1.1023	0.5966	0.8056	0.074*	0.313 (16)
H13D	1.0984	0.6036	0.9115	0.074*	0.313 (16)
C14B	1.1061 (17)	0.5231 (17)	0.870 (3)	0.066 (5)	0.313 (16)
H14C	1.0754	0.4942	0.8439	0.079*	0.313 (16)
H14D	1.1066	0.5150	0.9361	0.079*	0.313 (16)
C15B	1.170 (3)	0.503 (3)	0.834 (4)	0.070 (6)	0.313 (16)
H15C	1.1703	0.5029	0.7675	0.084*	0.313 (16)
H15D	1.2030	0.5312	0.8559	0.084*	0.313 (16)
C16B	1.181 (3)	0.448 (2)	0.864 (4)	0.076 (9)	0.313 (16)
H16D	1.1478	0.4199	0.8444	0.115*	0.313 (16)
H16E	1.1828	0.4481	0.9306	0.115*	0.313 (16)
H16F	1.2212	0.4330	0.8404	0.115*	0.313 (16)
C17	1.0000	0.6464 (6)	0.9574 (9)	0.045 (3)
H17A	1.0372	0.6731	0.9618	0.054*	0.50
H17B	0.9628	0.6731	0.9618	0.054*	0.50
C18	1.0000	0.6031 (6)	1.0370 (8)	0.047 (3)
H18A	0.9627	0.5765	1.0338	0.056*	0.50
H18B	1.0373	0.5765	1.0338	0.056*	0.50
C19	1.0000	0.6365 (7)	1.1246 (10)	0.066 (4)
H19A	0.9626	0.6630	1.1284	0.080*	0.50
H19B	1.0374	0.6630	1.1284	0.080*	0.50
C20	1.0000	0.5914 (8)	1.2030 (11)	0.081 (6)
H20A	1.0000	0.6141	1.2603	0.121*
H20B	1.0373	0.5656	1.1996	0.121*	0.50
H20C	0.9627	0.5656	1.1996	0.121*	0.50
C21	1.0683 (6)	0.9487 (6)	0.7648 (10)	0.084 (5)
H21A	1.1034	0.9198	0.7737	0.100*
H21B	1.0661	0.9577	0.6992	0.100*
C22	1.0850 (5)	1.0084 (5)	0.8131 (9)	0.065 (3)
H22A	1.0519	1.0390	0.8013	0.078*
H22B	1.0862	1.0008	0.8791	0.078*
C23	1.1462 (6)	1.0345 (7)	0.7843 (12)	0.094 (6)
H23A	1.1793	1.0042	0.7983	0.112*
H23B	1.1455	1.0401	0.7178	0.112*
C24	1.1628 (6)	1.0928 (7)	0.8262 (13)	0.109 (7)
H24A	1.2059	1.1034	0.8101	0.163*
H24B	1.1593	1.0893	0.8921	0.163*
H24C	1.1346	1.1250	0.8045	0.163*
C25	1.0227 (10)	0.9061 (10)	0.9119 (12)	0.059 (5)	0.50
H25A	1.0686	0.9014	0.9124	0.071*	0.50
H25B	1.0138	0.9470	0.9381	0.071*	0.50
C26	1.0000	0.8641 (9)	0.9724 (9)	0.084 (5)
H26A	1.0233	0.8255	0.9620	0.101*	0.50
H26B	0.9562	0.8559	0.9549	0.101*	0.50
C27	1.0000	0.8748 (8)	1.0714 (9)	0.087 (5)
H27A	1.0370	0.9003	1.0849	0.104*	0.50
H27B	0.9630	0.9003	1.0849	0.104*	0.50
C28	1.0000	0.8245 (12)	1.1371 (16)	0.191 (12)
H28A	1.0000	0.8415	1.1986	0.287*
H28B	1.0373	0.7993	1.1284	0.287*	0.50
H28C	0.9627	0.7993	1.1284	0.287*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.01978 (18)	0.02102 (17)	0.01835 (18)	0.000	0.000	−0.00105 (15)
Re1	0.02977 (17)	0.03902 (18)	0.02739 (17)	0.00533 (13)	0.00811 (14)	0.00139 (16)
Re2	0.0397 (3)	0.0247 (2)	0.0230 (2)	0.000	0.000	−0.00248 (19)
Re3	0.0358 (3)	0.0273 (2)	0.0239 (2)	0.000	0.000	0.00542 (19)
P1	0.0277 (11)	0.0451 (13)	0.0228 (10)	−0.0031 (9)	−0.0074 (9)	−0.0014 (9)
P2	0.123 (4)	0.0254 (17)	0.033 (2)	0.000	0.000	0.0057 (14)
P3	0.055 (2)	0.0254 (16)	0.0367 (18)	0.000	0.000	−0.0086 (13)
O1	0.040 (4)	0.065 (4)	0.027 (3)	−0.002 (3)	0.005 (3)	−0.004 (3)
O2	0.037 (4)	0.067 (5)	0.088 (6)	0.004 (4)	0.004 (4)	0.016 (4)
O3	0.056 (5)	0.083 (5)	0.031 (4)	0.013 (3)	0.014 (3)	0.005 (3)
O4	0.075 (5)	0.066 (5)	0.063 (5)	0.021 (4)	0.005 (4)	−0.010 (4)
O5	0.024 (3)	0.051 (4)	0.032 (3)	−0.001 (3)	−0.006 (2)	−0.002 (3)
O6	0.069 (6)	0.021 (4)	0.022 (4)	0.000	0.000	−0.007 (3)
O7	0.113 (9)	0.053 (6)	0.018 (5)	0.000	0.000	−0.006 (4)
O8	0.064 (5)	0.039 (4)	0.089 (6)	0.001 (3)	0.008 (4)	−0.001 (4)
O9	0.104 (8)	0.026 (5)	0.030 (5)	0.000	0.000	0.003 (4)
O10	0.066 (6)	0.027 (4)	0.023 (4)	0.000	0.000	0.010 (3)
O11	0.127 (9)	0.076 (6)	0.067 (6)	0.042 (6)	0.031 (5)	0.036 (4)
O12	0.116 (9)	0.040 (5)	0.029 (5)	0.000	0.000	0.005 (4)
O13	0.081 (7)	0.030 (5)	0.039 (5)	0.000	0.000	0.000 (4)
C1	0.045 (6)	0.059 (6)	0.019 (4)	−0.004 (4)	0.001 (4)	−0.006 (4)
C2	0.051 (6)	0.060 (7)	0.044 (6)	0.014 (5)	−0.007 (5)	−0.002 (5)
C3	0.066 (7)	0.092 (9)	0.034 (5)	0.007 (6)	0.002 (5)	−0.015 (6)
C4	0.067 (9)	0.078 (9)	0.074 (9)	−0.004 (7)	−0.002 (7)	−0.009 (7)
C5	0.036 (5)	0.042 (5)	0.035 (5)	0.010 (4)	−0.010 (4)	0.002 (4)
C6	0.038 (5)	0.043 (5)	0.054 (5)	−0.006 (4)	−0.016 (5)	0.004 (5)
C7	0.058 (7)	0.047 (6)	0.068 (7)	−0.014 (5)	−0.024 (6)	0.021 (5)
C8	0.080 (10)	0.077 (9)	0.112 (13)	−0.034 (7)	−0.050 (9)	0.010 (8)
C9	0.030 (4)	0.045 (5)	0.039 (5)	−0.004 (4)	−0.011 (4)	0.005 (4)
C10	0.048 (6)	0.046 (6)	0.044 (5)	−0.016 (4)	−0.008 (4)	0.002 (4)
C11	0.061 (7)	0.037 (5)	0.062 (7)	−0.008 (5)	−0.002 (5)	−0.002 (5)
C12	0.066 (8)	0.054 (7)	0.121 (12)	0.010 (6)	−0.039 (8)	0.001 (7)
C13A	0.075 (7)	0.053 (8)	0.061 (8)	−0.010 (6)	−0.006 (7)	0.010 (7)
C14A	0.074 (9)	0.052 (7)	0.073 (9)	−0.016 (6)	−0.009 (7)	0.028 (7)
C15A	0.076 (8)	0.067 (9)	0.045 (8)	−0.022 (7)	0.009 (8)	0.008 (6)
C16A	0.067 (12)	0.081 (10)	0.046 (10)	0.015 (8)	−0.017 (9)	0.023 (9)
C13B	0.069 (12)	0.049 (9)	0.066 (13)	−0.026 (9)	−0.004 (11)	−0.007 (11)
C14B	0.071 (10)	0.064 (9)	0.063 (10)	−0.013 (8)	−0.007 (9)	0.005 (9)
C15B	0.080 (12)	0.069 (13)	0.061 (14)	−0.010 (10)	0.003 (12)	0.001 (12)
C16B	0.10 (2)	0.097 (19)	0.030 (16)	0.019 (14)	−0.01 (2)	0.015 (17)
C17	0.075 (9)	0.036 (6)	0.025 (5)	0.000	0.000	0.010 (5)
C18	0.075 (9)	0.038 (6)	0.027 (5)	0.000	0.000	0.015 (4)
C19	0.120 (12)	0.050 (8)	0.030 (5)	0.000	0.000	0.012 (5)
C20	0.157 (18)	0.062 (9)	0.022 (5)	0.000	0.000	0.007 (6)
C21	0.053 (7)	0.084 (9)	0.114 (12)	−0.022 (6)	0.018 (7)	−0.067 (9)
C22	0.044 (6)	0.068 (7)	0.083 (9)	−0.004 (5)	0.001 (6)	−0.050 (6)
C23	0.053 (8)	0.088 (10)	0.140 (14)	−0.016 (7)	0.023 (8)	−0.070 (10)
C24	0.056 (8)	0.082 (10)	0.189 (19)	−0.024 (7)	0.019 (10)	−0.066 (11)
C25	0.081 (15)	0.072 (12)	0.025 (7)	0.016 (9)	−0.003 (7)	−0.012 (7)
C26	0.145 (14)	0.070 (10)	0.037 (7)	0.000	0.000	−0.012 (6)
C27	0.145 (15)	0.084 (11)	0.032 (7)	0.000	0.000	0.003 (6)
C28	0.37 (3)	0.127 (19)	0.073 (12)	0.000	0.000	0.043 (13)

Geometric parameters (Å, º) top

U1—O13	2.263 (9)	C11—H11A	0.9900
U1—O9	2.275 (9)	C11—H11B	0.9900
U1—O5	2.289 (6)	C12—H12A	0.9800
U1—O5ⁱ	2.289 (6)	C12—H12B	0.9800
U1—O6	2.406 (7)	C12—H12C	0.9800
U1—O10	2.413 (8)	C13A—C14A	1.43 (2)
U1—O1ⁱ	2.428 (6)	C13A—H13A	0.9900
U1—O1	2.428 (6)	C13A—H13B	0.9900
Re1—O2	1.670 (8)	C14A—C15A	1.55 (3)
Re1—O4	1.695 (8)	C14A—H14A	0.9900
Re1—O3	1.703 (7)	C14A—H14B	0.9900
Re1—O1	1.747 (7)	C15A—C16A	1.50 (3)
Re2—O8	1.691 (8)	C15A—H15A	0.9900
Re2—O8ⁱ	1.691 (8)	C15A—H15B	0.9900
Re2—O7	1.724 (9)	C16A—H16A	0.9800
Re2—O6	1.760 (7)	C16A—H16B	0.9800
Re3—O11ⁱ	1.663 (9)	C16A—H16C	0.9800
Re3—O11	1.663 (9)	C13B—C14B	1.37 (5)
Re3—O12	1.697 (9)	C13B—H13C	0.9900
Re3—O10	1.748 (8)	C13B—H13D	0.9900
P1—O5	1.524 (6)	C14B—C15B	1.54 (6)
P1—C5	1.798 (9)	C14B—H14C	0.9900
P1—C1	1.803 (9)	C14B—H14D	0.9900
P1—C9	1.803 (9)	C15B—C16B	1.30 (7)
P2—O9	1.518 (9)	C15B—H15C	0.9900
P2—C13Aⁱ	1.716 (14)	C15B—H15D	0.9900
P2—C13A	1.716 (14)	C16B—H16D	0.9800
P2—C17	1.780 (14)	C16B—H16E	0.9800
P2—C13B	1.863 (19)	C16B—H16F	0.9800
P2—C13Bⁱ	1.863 (19)	C17—C18	1.508 (16)
P3—O13	1.528 (9)	C17—H17A	0.9900
P3—C21ⁱ	1.743 (12)	C17—H17B	0.9900
P3—C21	1.743 (12)	C18—C19	1.49 (2)
P3—C25	1.807 (19)	C18—H18A	0.9900
P3—C25ⁱ	1.807 (19)	C18—H18B	0.9900
C1—C2	1.494 (14)	C19—C20	1.52 (2)
C1—H1A	0.9900	C19—H19A	0.9900
C1—H1B	0.9900	C19—H19B	0.9900
C2—C3	1.559 (14)	C20—H20A	0.9800
C2—H2A	0.9900	C20—H20B	0.9800
C2—H2B	0.9900	C20—H20C	0.9800
C3—C4	1.474 (17)	C21—C22	1.527 (14)
C3—H3A	0.9900	C21—H21A	0.9900
C3—H3B	0.9900	C21—H21B	0.9900
C4—H4A	0.9800	C22—C23	1.490 (16)
C4—H4B	0.9800	C22—H22A	0.9900
C4—H4C	0.9800	C22—H22B	0.9900
C5—C6	1.519 (12)	C23—C24	1.459 (17)
C5—H5A	0.9900	C23—H23A	0.9900
C5—H5B	0.9900	C23—H23B	0.9900
C6—C7	1.500 (13)	C24—H24A	0.9800
C6—H6A	0.9900	C24—H24B	0.9800
C6—H6B	0.9900	C24—H24C	0.9800
C7—C8	1.529 (15)	C25—C26	1.37 (3)
C7—H7A	0.9900	C25—H25A	0.9900
C7—H7B	0.9900	C25—H25B	0.9900
C8—H8A	0.9800	C26—C27	1.481 (15)
C8—H8B	0.9800	C26—H26A	0.9900
C8—H8C	0.9800	C26—H26B	0.9900
C9—C10	1.518 (12)	C27—C28	1.463 (17)
C9—H9A	0.9900	C27—H27A	0.9900
C9—H9B	0.9900	C27—H27B	0.9900
C10—C11	1.522 (14)	C28—H28A	0.9800
C10—H10A	0.9900	C28—H28B	0.9800
C10—H10B	0.9900	C28—H28C	0.9800
C11—C12	1.493 (15)

O13—U1—O9	137.4 (3)	C11—C10—H10A	108.9
O13—U1—O5	95.11 (17)	C9—C10—H10A	108.9
O9—U1—O5	99.17 (17)	C11—C10—H10B	108.9
O13—U1—O5ⁱ	95.11 (17)	C9—C10—H10B	108.9
O9—U1—O5ⁱ	99.17 (17)	H10A—C10—H10B	107.7
O5—U1—O5ⁱ	139.8 (3)	C12—C11—C10	112.8 (10)
O13—U1—O6	152.9 (3)	C12—C11—H11A	109.0
O9—U1—O6	69.7 (3)	C10—C11—H11A	109.0
O5—U1—O6	76.67 (16)	C12—C11—H11B	109.0
O5ⁱ—U1—O6	76.67 (16)	C10—C11—H11B	109.0
O13—U1—O10	74.5 (3)	H11A—C11—H11B	107.8
O9—U1—O10	148.1 (3)	C11—C12—H12A	109.5
O5—U1—O10	72.76 (15)	C11—C12—H12B	109.5
O5ⁱ—U1—O10	72.76 (15)	H12A—C12—H12B	109.5
O6—U1—O10	78.4 (3)	C11—C12—H12C	109.5
O13—U1—O1ⁱ	74.3 (2)	H12A—C12—H12C	109.5
O9—U1—O1ⁱ	72.5 (2)	H12B—C12—H12C	109.5
O5—U1—O1ⁱ	148.3 (2)	C14A—C13A—P2	107.6 (13)
O5ⁱ—U1—O1ⁱ	71.8 (2)	C14A—C13A—H13A	110.2
O6—U1—O1ⁱ	125.2 (2)	P2—C13A—H13A	110.2
O10—U1—O1ⁱ	129.6 (2)	C14A—C13A—H13B	110.2
O13—U1—O1	74.3 (2)	P2—C13A—H13B	110.2
O9—U1—O1	72.5 (2)	H13A—C13A—H13B	108.5
O5—U1—O1	71.8 (2)	C13A—C14A—C15A	114.2 (16)
O5ⁱ—U1—O1	148.3 (2)	C13A—C14A—H14A	108.7
O6—U1—O1	125.2 (2)	C15A—C14A—H14A	108.7
O10—U1—O1	129.6 (2)	C13A—C14A—H14B	108.7
O1ⁱ—U1—O1	76.6 (3)	C15A—C14A—H14B	108.7
O2—Re1—O4	108.7 (4)	H14A—C14A—H14B	107.6
O2—Re1—O3	108.3 (4)	C16A—C15A—C14A	114.6 (16)
O4—Re1—O3	109.5 (4)	C16A—C15A—H15A	108.6
O2—Re1—O1	111.0 (3)	C14A—C15A—H15A	108.6
O4—Re1—O1	110.1 (4)	C16A—C15A—H15B	108.6
O3—Re1—O1	109.1 (3)	C14A—C15A—H15B	108.6
O8—Re2—O8ⁱ	110.7 (5)	H15A—C15A—H15B	107.6
O8—Re2—O7	108.0 (3)	C15A—C16A—H16A	109.5
O8ⁱ—Re2—O7	108.0 (3)	C15A—C16A—H16B	109.5
O8—Re2—O6	110.4 (3)	H16A—C16A—H16B	109.5
O8ⁱ—Re2—O6	110.4 (3)	C15A—C16A—H16C	109.5
O7—Re2—O6	109.2 (4)	H16A—C16A—H16C	109.5
O11ⁱ—Re3—O11	107.9 (8)	H16B—C16A—H16C	109.5
O11ⁱ—Re3—O12	107.7 (4)	C14B—C13B—P2	134 (3)
O11—Re3—O12	107.7 (4)	C14B—C13B—H13C	103.6
O11ⁱ—Re3—O10	111.8 (3)	P2—C13B—H13C	103.6
O11—Re3—O10	111.8 (3)	C14B—C13B—H13D	103.6
O12—Re3—O10	109.7 (4)	P2—C13B—H13D	103.6
O5—P1—C5	108.2 (4)	H13C—C13B—H13D	105.3
O5—P1—C1	112.9 (4)	C13B—C14B—C15B	125 (4)
C5—P1—C1	110.6 (4)	C13B—C14B—H14C	106.0
O5—P1—C9	110.8 (4)	C15B—C14B—H14C	106.0
C5—P1—C9	108.8 (4)	C13B—C14B—H14D	106.0
C1—P1—C9	105.3 (5)	C15B—C14B—H14D	106.0
O9—P2—C13Aⁱ	112.9 (7)	H14C—C14B—H14D	106.3
O9—P2—C13A	112.9 (7)	C16B—C15B—C14B	108 (5)
C13Aⁱ—P2—C13A	74.3 (12)	C16B—C15B—H15C	110.1
O9—P2—C17	114.5 (6)	C14B—C15B—H15C	110.1
C13Aⁱ—P2—C17	118.2 (7)	C16B—C15B—H15D	110.0
C13A—P2—C17	118.2 (7)	C14B—C15B—H15D	110.1
O9—P2—C13B	106.9 (13)	H15C—C15B—H15D	108.4
C13Aⁱ—P2—C13B	107.3 (14)	C15B—C16B—H16D	109.5
C13A—P2—C13B	34.1 (12)	C15B—C16B—H16E	109.5
C17—P2—C13B	94.5 (13)	H16D—C16B—H16E	109.5
O9—P2—C13Bⁱ	106.9 (13)	C15B—C16B—H16F	109.5
C13Aⁱ—P2—C13Bⁱ	34.1 (12)	H16D—C16B—H16F	109.5
C13A—P2—C13Bⁱ	107.3 (14)	H16E—C16B—H16F	109.5
C17—P2—C13Bⁱ	94.5 (13)	C18—C17—P2	115.2 (9)
C13B—P2—C13Bⁱ	137 (2)	C18—C17—H17A	108.5
O13—P3—C21ⁱ	108.0 (4)	P2—C17—H17A	108.5
O13—P3—C21	108.0 (4)	C18—C17—H17B	108.5
C21ⁱ—P3—C21	114.3 (11)	P2—C17—H17B	108.5
O13—P3—C25	113.8 (8)	H17A—C17—H17B	107.5
C21ⁱ—P3—C25	119.4 (8)	C19—C18—C17	111.9 (11)
C21—P3—C25	92.2 (9)	C19—C18—H18A	109.2
O13—P3—C25ⁱ	113.8 (8)	C17—C18—H18A	109.2
C21ⁱ—P3—C25ⁱ	92.2 (9)	C19—C18—H18B	109.2
C21—P3—C25ⁱ	119.4 (8)	C17—C18—H18B	109.2
C25—P3—C25ⁱ	31.2 (14)	H18A—C18—H18B	107.9
Re1—O1—U1	150.3 (4)	C18—C19—C20	110.4 (13)
P1—O5—U1	163.2 (4)	C18—C19—H19A	109.6
Re2—O6—U1	153.9 (4)	C20—C19—H19A	109.6
P2—O9—U1	155.5 (6)	C18—C19—H19B	109.6
Re3—O10—U1	151.0 (5)	C20—C19—H19B	109.6
P3—O13—U1	168.9 (6)	H19A—C19—H19B	108.1
C2—C1—P1	116.2 (8)	C19—C20—H20A	109.5
C2—C1—H1A	108.2	C19—C20—H20B	109.5
P1—C1—H1A	108.2	H20A—C20—H20B	109.5
C2—C1—H1B	108.2	C19—C20—H20C	109.5
P1—C1—H1B	108.2	H20A—C20—H20C	109.5
H1A—C1—H1B	107.4	H20B—C20—H20C	109.5
C1—C2—C3	111.5 (9)	C22—C21—P3	119.4 (9)
C1—C2—H2A	109.3	C22—C21—H21A	107.5
C3—C2—H2A	109.3	P3—C21—H21A	107.5
C1—C2—H2B	109.3	C22—C21—H21B	107.5
C3—C2—H2B	109.3	P3—C21—H21B	107.5
H2A—C2—H2B	108.0	H21A—C21—H21B	107.0
C4—C3—C2	113.5 (11)	C23—C22—C21	113.4 (9)
C4—C3—H3A	108.9	C23—C22—H22A	108.9
C2—C3—H3A	108.9	C21—C22—H22A	108.9
C4—C3—H3B	108.9	C23—C22—H22B	108.9
C2—C3—H3B	108.9	C21—C22—H22B	108.9
H3A—C3—H3B	107.7	H22A—C22—H22B	107.7
C3—C4—H4A	109.5	C24—C23—C22	115.2 (11)
C3—C4—H4B	109.5	C24—C23—H23A	108.5
H4A—C4—H4B	109.5	C22—C23—H23A	108.5
C3—C4—H4C	109.5	C24—C23—H23B	108.5
H4A—C4—H4C	109.5	C22—C23—H23B	108.5
H4B—C4—H4C	109.5	H23A—C23—H23B	107.5
C6—C5—P1	117.5 (6)	C23—C24—H24A	109.5
C6—C5—H5A	107.9	C23—C24—H24B	109.5
P1—C5—H5A	107.9	H24A—C24—H24B	109.5
C6—C5—H5B	107.9	C23—C24—H24C	109.5
P1—C5—H5B	107.9	H24A—C24—H24C	109.5
H5A—C5—H5B	107.2	H24B—C24—H24C	109.5
C7—C6—C5	112.4 (8)	C26—C25—P3	124.5 (15)
C7—C6—H6A	109.1	C26—C25—H25A	106.2
C5—C6—H6A	109.1	P3—C25—H25A	106.2
C7—C6—H6B	109.1	C26—C25—H25B	106.2
C5—C6—H6B	109.1	P3—C25—H25B	106.2
H6A—C6—H6B	107.9	H25A—C25—H25B	106.4
C6—C7—C8	113.3 (9)	C25—C26—C27	122.7 (16)
C6—C7—H7A	108.9	C25—C26—H26A	106.7
C8—C7—H7A	108.9	C27—C26—H26A	106.7
C6—C7—H7B	108.9	C25—C26—H26B	106.7
C8—C7—H7B	108.9	C27—C26—H26B	106.7
H7A—C7—H7B	107.7	H26A—C26—H26B	106.6
C7—C8—H8A	109.5	C28—C27—C26	123 (2)
C7—C8—H8B	109.5	C28—C27—H27A	106.7
H8A—C8—H8B	109.5	C26—C27—H27A	106.7
C7—C8—H8C	109.5	C28—C27—H27B	106.7
H8A—C8—H8C	109.5	C26—C27—H27B	106.7
H8B—C8—H8C	109.5	H27A—C27—H27B	106.6
C10—C9—P1	113.2 (7)	C27—C28—H28A	109.5
C10—C9—H9A	108.9	C27—C28—H28B	109.5
P1—C9—H9A	108.9	H28A—C28—H28B	109.5
C10—C9—H9B	108.9	C27—C28—H28C	109.5
P1—C9—H9B	108.9	H28A—C28—H28C	109.5
H9A—C9—H9B	107.7	H28B—C28—H28C	109.5
C11—C10—C9	113.3 (8)

O2—Re1—O1—U1	55.6 (8)	O9—U1—O13—P3	0.000 (12)
O4—Re1—O1—U1	−64.9 (8)	O5—U1—O13—P3	109.49 (15)
O3—Re1—O1—U1	175.0 (7)	O5ⁱ—U1—O13—P3	−109.49 (15)
O13—U1—O1—Re1	93.8 (8)	O6—U1—O13—P3	180.000 (8)
O9—U1—O1—Re1	−113.4 (8)	O10—U1—O13—P3	180.000 (11)
O5—U1—O1—Re1	−7.1 (7)	O1ⁱ—U1—O13—P3	−40.06 (17)
O5ⁱ—U1—O1—Re1	167.7 (6)	O1—U1—O13—P3	40.06 (17)
O6—U1—O1—Re1	−65.2 (8)	O5—P1—C1—C2	64.7 (9)
O10—U1—O1—Re1	40.2 (9)	C5—P1—C1—C2	−56.9 (9)
O1ⁱ—U1—O1—Re1	171.0 (6)	C9—P1—C1—C2	−174.3 (8)
C5—P1—O5—U1	76.3 (14)	P1—C1—C2—C3	−176.1 (8)
C1—P1—O5—U1	−46.6 (14)	C1—C2—C3—C4	−64.4 (14)
C9—P1—O5—U1	−164.5 (12)	O5—P1—C5—C6	−179.3 (7)
O13—U1—O5—P1	138.0 (13)	C1—P1—C5—C6	−55.0 (9)
O9—U1—O5—P1	−82.3 (13)	C9—P1—C5—C6	60.2 (8)
O5ⁱ—U1—O5—P1	33.9 (17)	P1—C5—C6—C7	−179.7 (8)
O6—U1—O5—P1	−15.8 (13)	C5—C6—C7—C8	−177.9 (11)
O10—U1—O5—P1	66.0 (13)	O5—P1—C9—C10	57.6 (7)
O1ⁱ—U1—O5—P1	−153.8 (12)	C5—P1—C9—C10	176.5 (6)
O1—U1—O5—P1	−150.4 (14)	C1—P1—C9—C10	−64.8 (7)
O8—Re2—O6—U1	61.4 (3)	P1—C9—C10—C11	−179.5 (7)
O8ⁱ—Re2—O6—U1	−61.4 (3)	C9—C10—C11—C12	−68.6 (12)
O7—Re2—O6—U1	180.000 (2)	O9—P2—C13A—C14A	64.6 (14)
O13—U1—O6—Re2	180.0	C13Aⁱ—P2—C13A—C14A	173.2 (10)
O9—U1—O6—Re2	0.000 (2)	C17—P2—C13A—C14A	−72.8 (14)
O5—U1—O6—Re2	−105.21 (16)	C13B—P2—C13A—C14A	−22 (3)
O5ⁱ—U1—O6—Re2	105.21 (16)	C13Bⁱ—P2—C13A—C14A	−178.0 (18)
O10—U1—O6—Re2	180.000 (3)	P2—C13A—C14A—C15A	−174.1 (13)
O1ⁱ—U1—O6—Re2	49.3 (2)	C13A—C14A—C15A—C16A	−51 (3)
O1—U1—O6—Re2	−49.3 (2)	O9—P2—C13B—C14B	−133 (5)
C13Aⁱ—P2—O9—U1	139.1 (7)	C13Aⁱ—P2—C13B—C14B	−11 (5)
C13A—P2—O9—U1	−139.1 (7)	C13A—P2—C13B—C14B	−27 (4)
C17—P2—O9—U1	0.000 (7)	C17—P2—C13B—C14B	110 (5)
C13B—P2—O9—U1	−103.3 (13)	C13Bⁱ—P2—C13B—C14B	8 (8)
C13Bⁱ—P2—O9—U1	103.3 (13)	P2—C13B—C14B—C15B	149 (4)
O13—U1—O9—P2	0.000 (6)	C13B—C14B—C15B—C16B	174 (5)
O5—U1—O9—P2	−107.99 (16)	O9—P2—C17—C18	180.000 (4)
O5ⁱ—U1—O9—P2	107.99 (16)	C13Aⁱ—P2—C17—C18	43.2 (7)
O6—U1—O9—P2	180.000 (5)	C13A—P2—C17—C18	−43.2 (7)
O10—U1—O9—P2	180.000 (3)	C13B—P2—C17—C18	−69.1 (12)
O1ⁱ—U1—O9—P2	40.51 (17)	C13Bⁱ—P2—C17—C18	69.1 (12)
O1—U1—O9—P2	−40.51 (17)	P2—C17—C18—C19	180.000 (7)
O11ⁱ—Re3—O10—U1	60.6 (4)	C17—C18—C19—C20	180.000 (7)
O11—Re3—O10—U1	−60.6 (4)	O13—P3—C21—C22	−171.8 (11)
O12—Re3—O10—U1	180.000 (3)	C21ⁱ—P3—C21—C22	68.0 (17)
O13—U1—O10—Re3	0.000 (2)	C25—P3—C21—C22	−55.8 (14)
O9—U1—O10—Re3	180.0	C25ⁱ—P3—C21—C22	−39.6 (17)
O5—U1—O10—Re3	100.54 (17)	P3—C21—C22—C23	177.0 (12)
O5ⁱ—U1—O10—Re3	−100.54 (17)	C21—C22—C23—C24	177.7 (15)
O6—U1—O10—Re3	180.000 (3)	O13—P3—C25—C26	−46.8 (19)
O1ⁱ—U1—O10—Re3	−53.6 (2)	C21ⁱ—P3—C25—C26	82.8 (19)
O1—U1—O10—Re3	53.6 (2)	C21—P3—C25—C26	−157.6 (17)
C21ⁱ—P3—O13—U1	−117.9 (6)	C25ⁱ—P3—C25—C26	50.3 (18)
C21—P3—O13—U1	117.9 (6)	P3—C25—C26—C27	−156.5 (10)
C25—P3—O13—U1	17.1 (8)	C25—C26—C27—C28	−155.0 (13)
C25ⁱ—P3—O13—U1	−17.1 (8)

Symmetry code: (i) −x+2, y, z.

(Iat100) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	F(000) = 4032
M_r = 2112.05	D_x = 2.046 Mg m⁻³
Monoclinic, Cc	Mo Kα radiation, λ = 0.71069 Å
a = 21.40 (2) Å	Cell parameters from 49029 reflections
b = 21.68 (2) Å	θ = 2.3–25.0°
c = 14.78 (2) Å	µ = 9.55 mm⁻¹
β = 90.00 (3)°	T = 100 K
V = 6857 (13) Å³	Prismatic, green
Z = 4	0.12 × 0.1 × 0.08 mm

Data collection top

Rigaku RAXIS diffractometer	11431 reflections with I > 2σ(I)
Radiation source: Rigaku rotating anode	R_int = 0.06
Graphite monochromator	θ_max = 25.0°, θ_min = 2.3°
103 x 3 degree phi scans	h = −25→25
49029 measured reflections	k = −25→25
11595 independent reflections	l = −17→17

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.032	w = 1/[σ²(F_o²) + (0.0247P)² + 70.409P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.080	(Δ/σ)_max = 0.001
S = 1.05	Δρ_max = 1.77 e Å⁻³
11595 reflections	Δρ_min = −1.88 e Å⁻³
698 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
2 restraints	Extinction coefficient: 0.000349 (19)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier map	Absolute structure parameter: 0.00

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄U	V = 6857 (13) Å³
M_r = 2112.05	Z = 4
Monoclinic, Cc	Mo Kα radiation
a = 21.40 (2) Å	µ = 9.55 mm⁻¹
b = 21.68 (2) Å	T = 100 K
c = 14.78 (2) Å	0.12 × 0.1 × 0.08 mm
β = 90.00 (3)°

Data collection top

Rigaku RAXIS diffractometer	11431 reflections with I > 2σ(I)
49029 measured reflections	R_int = 0.06
11595 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	H-atom parameters constrained
wR(F²) = 0.080	w = 1/[σ²(F_o²) + (0.0247P)² + 70.409P] where P = (F_o² + 2F_c²)/3
S = 1.05	Δρ_max = 1.77 e Å⁻³
11595 reflections	Δρ_min = −1.88 e Å⁻³
698 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
2 restraints	Absolute structure parameter: 0.00

Special details top

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

	x	y	z	U_iso*/U_eq
U1	0.65587 (3)	0.748434 (14)	0.85693 (2)	0.01537 (9)
Re1	0.51126 (3)	0.76338 (3)	0.68382 (4)	0.02347 (14)
Re2	0.65481 (3)	0.589605 (17)	1.00499 (3)	0.02138 (11)
Re3	0.65297 (4)	0.877000 (17)	1.05446 (3)	0.02059 (10)
Re1A	0.80268 (2)	0.76204 (3)	0.68646 (4)	0.02141 (14)
P1	0.4959 (2)	0.73669 (19)	0.9664 (3)	0.0239 (8)
P2	0.6676 (2)	0.61073 (16)	0.7051 (2)	0.0344 (10)
P3	0.6479 (2)	0.91147 (13)	0.7673 (2)	0.0235 (7)
P1A	0.81419 (19)	0.74164 (17)	0.9705 (3)	0.0191 (8)
O1	0.5860 (5)	0.7477 (5)	0.7265 (7)	0.023 (2)
O2	0.4589 (5)	0.7122 (5)	0.7221 (9)	0.038 (3)
O3	0.5127 (6)	0.7593 (6)	0.5692 (9)	0.042 (3)
O4	0.4889 (5)	0.8355 (5)	0.7149 (8)	0.036 (3)
O5	0.5539 (5)	0.7454 (5)	0.9085 (7)	0.022 (2)
O6	0.6594 (6)	0.6667 (3)	0.9689 (5)	0.0247 (17)
O7	0.6492 (8)	0.5873 (4)	1.1164 (8)	0.048 (3)
O8	0.5921 (6)	0.5521 (5)	0.9612 (9)	0.040 (3)
O9	0.6676 (5)	0.6544 (4)	0.7862 (6)	0.032 (3)
O10	0.6528 (7)	0.8070 (3)	0.9973 (5)	0.0290 (17)
O11	0.5854 (6)	0.9127 (5)	1.0419 (8)	0.044 (3)
O12	0.6639 (6)	0.8657 (4)	1.1664 (6)	0.034 (2)
O13	0.6449 (6)	0.8489 (3)	0.8142 (6)	0.032 (3)
O1A	0.7256 (5)	0.7638 (4)	0.7302 (7)	0.028 (2)
O2A	0.8429 (6)	0.7046 (5)	0.7361 (7)	0.035 (3)
O3A	0.8001 (6)	0.7494 (5)	0.5753 (10)	0.036 (3)
O4A	0.8388 (6)	0.8316 (6)	0.7080 (10)	0.045 (3)
O5A	0.7562 (5)	0.7526 (5)	0.9132 (8)	0.028 (2)
O8A	0.7218 (6)	0.5523 (5)	0.9787 (11)	0.049 (4)
O11A	0.7093 (6)	0.9238 (5)	1.0157 (7)	0.042 (3)
C1	0.5090 (9)	0.7500 (9)	1.0859 (13)	0.037 (4)
H1A	0.5220	0.7926	1.0932	0.045*
H1B	0.4691	0.7456	1.1165	0.045*
C2	0.5550 (8)	0.7106 (8)	1.1341 (10)	0.032 (4)
H2A	0.5938	0.7103	1.1002	0.039*
H2B	0.5393	0.6686	1.1358	0.039*
C3	0.5683 (10)	0.7316 (10)	1.2297 (11)	0.043 (5)
H3A	0.5800	0.7748	1.2286	0.051*
H3B	0.6037	0.7085	1.2530	0.051*
C4	0.5116 (10)	0.7231 (10)	1.2955 (13)	0.045 (5)
H4A	0.5174	0.6864	1.3307	0.067*
H4B	0.4737	0.7197	1.2610	0.067*
H4C	0.5089	0.7581	1.3351	0.067*
C5	0.4674 (7)	0.6584 (7)	0.9495 (11)	0.030 (4)
H5A	0.4587	0.6529	0.8857	0.036*
H5B	0.5008	0.6300	0.9652	0.036*
C6	0.4098 (8)	0.6402 (7)	1.0021 (12)	0.034 (4)
H6A	0.3755	0.6675	0.9868	0.040*
H6B	0.4179	0.6439	1.0665	0.040*
C7	0.3921 (8)	0.5732 (7)	0.9792 (10)	0.030 (4)
H7A	0.3846	0.5698	0.9147	0.037*
H7B	0.4269	0.5463	0.9941	0.037*
C8	0.3346 (10)	0.5519 (8)	1.0298 (14)	0.055 (6)
H8A	0.2987	0.5740	1.0081	0.083*
H8B	0.3399	0.5598	1.0933	0.083*
H8C	0.3287	0.5085	1.0203	0.083*
C9	0.4362 (7)	0.7898 (7)	0.9337 (13)	0.032 (4)
H9A	0.4263	0.7831	0.8705	0.038*
H9B	0.3989	0.7812	0.9687	0.038*
C10	0.4536 (7)	0.8569 (8)	0.9467 (11)	0.029 (3)
H10A	0.4922	0.8649	0.9143	0.035*
H10B	0.4617	0.8639	1.0105	0.035*
C11	0.4042 (8)	0.9032 (7)	0.9150 (12)	0.033 (4)
H11A	0.4221	0.9443	0.9149	0.040*
H11B	0.3919	0.8933	0.8536	0.040*
C12	0.3469 (9)	0.9023 (9)	0.9759 (16)	0.045 (5)
H12A	0.3574	0.9192	1.0339	0.068*
H12B	0.3327	0.8606	0.9832	0.068*
H12C	0.3143	0.9266	0.9489	0.068*
C13	0.7460 (9)	0.5746 (7)	0.6924 (12)	0.052 (5)
H13A	0.7428	0.5418	0.6480	0.063*
H13B	0.7745	0.6053	0.6685	0.063*
C14	0.7716 (9)	0.5504 (8)	0.7699 (12)	0.048 (4)
H14A	0.7399	0.5263	0.8007	0.057*
H14B	0.7831	0.5842	0.8095	0.057*
C15	0.8293 (10)	0.5096 (9)	0.7551 (13)	0.053 (5)
H15A	0.8595	0.5314	0.7180	0.064*
H15B	0.8487	0.5005	0.8129	0.064*
C16	0.8107 (9)	0.4494 (8)	0.7085 (11)	0.044 (4)
H16A	0.7830	0.4582	0.6591	0.066*
H16B	0.7899	0.4230	0.7512	0.066*
H16C	0.8475	0.4291	0.6861	0.066*
C17	0.6564 (11)	0.6492 (5)	0.5998 (7)	0.033 (3)
H17A	0.6186	0.6738	0.6030	0.040*
H17B	0.6912	0.6770	0.5894	0.040*
C18	0.6513 (9)	0.6040 (5)	0.5195 (8)	0.029 (3)
H18A	0.6879	0.5775	0.5190	0.034*
H18B	0.6149	0.5780	0.5280	0.034*
C19	0.6463 (10)	0.6358 (6)	0.4301 (10)	0.039 (4)
H19A	0.6828	0.6616	0.4203	0.047*
H19B	0.6095	0.6620	0.4293	0.047*
C20	0.6416 (9)	0.5876 (7)	0.3553 (9)	0.047 (5)
H20A	0.5992	0.5737	0.3504	0.070*
H20B	0.6682	0.5533	0.3696	0.070*
H20C	0.6546	0.6055	0.2990	0.070*
C21	0.7251 (6)	0.9425 (6)	0.7821 (9)	0.026 (3)
H21A	0.7323	0.9477	0.8464	0.031*
H21B	0.7548	0.9121	0.7605	0.031*
C22	0.7395 (6)	1.0037 (7)	0.7354 (11)	0.028 (3)
H22A	0.7077	1.0338	0.7511	0.033*
H22B	0.7388	0.9981	0.6703	0.033*
C23	0.8036 (6)	1.0274 (7)	0.7647 (10)	0.028 (3)
H23A	0.8047	1.0319	0.8299	0.034*
H23B	0.8356	0.9980	0.7472	0.034*
C24	0.8165 (9)	1.0886 (8)	0.7209 (12)	0.045 (5)
H24A	0.7819	1.1159	0.7313	0.067*
H24B	0.8221	1.0829	0.6570	0.067*
H24C	0.8538	1.1061	0.7463	0.067*
C25	0.6288 (7)	0.9096 (6)	0.6507 (9)	0.029 (3)
H25A	0.5850	0.8986	0.6457	0.035*
H25B	0.6331	0.9513	0.6274	0.035*
C26	0.6674 (7)	0.8648 (6)	0.5851 (9)	0.034 (4)
H26A	0.7117	0.8732	0.5910	0.041*
H26B	0.6602	0.8222	0.6026	0.041*
C27	0.6480 (11)	0.8737 (6)	0.4898 (9)	0.039 (4)
H27A	0.6545	0.9164	0.4724	0.046*
H271	0.6039	0.8644	0.4834	0.046*
C28	0.6867 (10)	0.8309 (8)	0.4278 (14)	0.064 (5)
H28A	0.6768	0.7886	0.4410	0.096*
H28B	0.7305	0.8379	0.4381	0.096*
H28C	0.6770	0.8396	0.3657	0.096*
C1A	0.7993 (6)	0.7570 (6)	1.0890 (10)	0.016 (3)
H1C	0.8388	0.7548	1.1212	0.019*
H1D	0.7840	0.7989	1.0945	0.019*
C2A	0.7533 (8)	0.7143 (8)	1.1356 (13)	0.034 (4)
H2C	0.7680	0.6721	1.1306	0.041*
H2D	0.7132	0.7169	1.1052	0.041*
C3A	0.7445 (8)	0.7306 (7)	1.2375 (12)	0.032 (4)
H3C	0.7254	0.7711	1.2417	0.038*
H3D	0.7156	0.7012	1.2640	0.038*
C4A	0.8044 (10)	0.7308 (7)	1.2934 (14)	0.046 (5)
H4D	0.8337	0.7591	1.2672	0.069*
H4E	0.8221	0.6901	1.2939	0.069*
H4F	0.7950	0.7433	1.3542	0.069*
C5A	0.8385 (7)	0.6632 (7)	0.9570 (11)	0.027 (3)
H5C	0.8031	0.6368	0.9707	0.032*
H5D	0.8489	0.6568	0.8938	0.032*
C6A	0.8929 (7)	0.6422 (7)	1.0133 (11)	0.027 (3)
H6C	0.8844	0.6505	1.0765	0.032*
H6D	0.9299	0.6653	0.9962	0.032*
C7A	0.9059 (7)	0.5720 (6)	1.0009 (11)	0.029 (3)
H7C	0.8688	0.5490	1.0178	0.034*
H7D	0.9143	0.5638	0.9376	0.034*
C8A	0.9613 (9)	0.5492 (8)	1.0578 (11)	0.041 (4)
H8D	0.9935	0.5801	1.0582	0.062*
H8E	0.9774	0.5118	1.0321	0.062*
H8F	0.9476	0.5415	1.1186	0.062*
C9A	0.8756 (7)	0.7922 (7)	0.9354 (10)	0.023 (3)
H9C	0.9112	0.7864	0.9751	0.028*
H9D	0.8884	0.7809	0.8747	0.028*
C10A	0.8571 (7)	0.8610 (7)	0.9360 (12)	0.029 (4)
H10C	0.8231	0.8674	0.8936	0.035*
H10D	0.8421	0.8720	0.9958	0.035*
C11A	0.9105 (7)	0.9030 (7)	0.9112 (12)	0.030 (3)
H11C	0.8945	0.9446	0.9043	0.036*
H11D	0.9270	0.8902	0.8530	0.036*
C12A	0.9647 (10)	0.9041 (8)	0.9804 (18)	0.057 (6)
H12D	0.9805	0.8630	0.9887	0.086*
H12E	0.9498	0.9198	1.0371	0.086*
H12F	0.9976	0.9302	0.9583	0.086*
C13A	0.6118 (6)	0.5521 (6)	0.7266 (10)	0.031 (3)
H13C	0.6149	0.5205	0.6802	0.037*
H13D	0.6207	0.5329	0.7845	0.037*
C14A	0.5466 (8)	0.5775 (7)	0.7276 (10)	0.038 (4)
H14C	0.5368	0.5943	0.6684	0.045*
H14D	0.5442	0.6109	0.7711	0.045*
C15A	0.4970 (9)	0.5267 (8)	0.7529 (14)	0.046 (5)
H15C	0.5063	0.5119	0.8133	0.055*
H15D	0.4562	0.5461	0.7550	0.055*
C16A	0.4929 (9)	0.4720 (8)	0.6913 (12)	0.047 (5)
H16D	0.5340	0.4553	0.6819	0.070*
H16E	0.4755	0.4845	0.6343	0.070*
H16F	0.4667	0.4411	0.7182	0.070*
C21A	0.5881 (7)	0.9603 (6)	0.8170 (9)	0.031 (3)
H21C	0.5514	0.9351	0.8275	0.037*
H21D	0.6031	0.9740	0.8757	0.037*
C22A	0.5674 (8)	1.0188 (7)	0.7621 (11)	0.039 (4)
H22C	0.6014	1.0484	0.7601	0.046*
H22D	0.5572	1.0072	0.7005	0.046*
C23A	0.5106 (7)	1.0476 (7)	0.8073 (12)	0.039 (4)
H23C	0.4761	1.0187	0.8071	0.047*
H23D	0.5203	1.0580	0.8696	0.047*
C24A	0.4930 (11)	1.1055 (9)	0.7552 (16)	0.064 (6)
H24D	0.4883	1.0957	0.6923	0.097*
H24E	0.5252	1.1360	0.7624	0.097*
H24F	0.4542	1.1215	0.7782	0.097*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.01384 (18)	0.01380 (16)	0.01846 (18)	0.0001 (2)	−0.0006 (2)	0.00007 (12)
Re1	0.0190 (3)	0.0251 (3)	0.0263 (3)	0.0038 (2)	−0.0058 (2)	−0.0015 (2)
Re2	0.0250 (2)	0.01674 (19)	0.0224 (2)	−0.0012 (3)	−0.0009 (3)	0.00163 (16)
Re3	0.0220 (2)	0.01755 (19)	0.0222 (2)	−0.0004 (3)	−0.0017 (3)	−0.00329 (15)
Re1A	0.0192 (3)	0.0237 (3)	0.0213 (3)	−0.0013 (2)	0.0026 (2)	0.0013 (2)
P1	0.023 (2)	0.028 (2)	0.021 (2)	−0.0044 (15)	0.0028 (16)	−0.0026 (16)
P2	0.051 (3)	0.0238 (14)	0.0282 (19)	−0.0016 (16)	−0.0038 (17)	−0.0015 (12)
P3	0.028 (2)	0.0174 (13)	0.0255 (14)	−0.0022 (15)	0.0008 (16)	0.0023 (10)
P1A	0.017 (2)	0.0230 (18)	0.0171 (18)	−0.0008 (14)	−0.0018 (15)	−0.0001 (13)
O1	0.022 (5)	0.038 (5)	0.008 (4)	−0.003 (4)	−0.007 (4)	−0.013 (4)
O2	0.013 (5)	0.029 (6)	0.073 (8)	0.004 (4)	−0.018 (5)	−0.012 (5)
O3	0.033 (7)	0.063 (8)	0.030 (6)	0.014 (6)	−0.021 (5)	0.008 (5)
O4	0.035 (6)	0.033 (6)	0.040 (6)	0.010 (5)	−0.005 (5)	−0.003 (5)
O5	0.015 (6)	0.032 (5)	0.019 (5)	−0.002 (4)	−0.002 (4)	0.006 (4)
O6	0.036 (5)	0.023 (4)	0.015 (3)	0.005 (5)	−0.007 (5)	0.012 (3)
O7	0.045 (7)	0.028 (4)	0.072 (7)	0.000 (6)	−0.006 (7)	−0.001 (4)
O8	0.041 (7)	0.033 (6)	0.046 (7)	−0.008 (5)	−0.016 (5)	−0.014 (5)
O9	0.054 (8)	0.011 (3)	0.029 (4)	0.006 (4)	−0.006 (5)	−0.012 (3)
O10	0.037 (5)	0.032 (4)	0.018 (4)	−0.005 (6)	0.010 (5)	−0.009 (3)
O11	0.052 (8)	0.052 (7)	0.029 (6)	0.028 (6)	−0.014 (5)	−0.022 (5)
O12	0.031 (7)	0.029 (4)	0.041 (5)	0.003 (5)	−0.007 (5)	−0.008 (4)
O13	0.052 (8)	0.008 (3)	0.036 (4)	0.007 (4)	−0.001 (5)	0.003 (3)
O1A	0.029 (6)	0.026 (5)	0.027 (5)	−0.001 (4)	0.002 (4)	0.012 (4)
O2A	0.036 (7)	0.045 (6)	0.024 (5)	−0.001 (5)	−0.007 (5)	−0.005 (5)
O3A	0.027 (7)	0.021 (5)	0.060 (8)	0.002 (4)	−0.009 (6)	−0.001 (5)
O4A	0.037 (7)	0.036 (6)	0.063 (8)	−0.010 (5)	0.007 (6)	−0.004 (6)
O5A	0.023 (6)	0.036 (6)	0.025 (6)	0.004 (4)	−0.014 (5)	0.000 (4)
O8A	0.033 (7)	0.020 (6)	0.095 (11)	0.000 (5)	−0.003 (6)	0.008 (6)
O11A	0.072 (9)	0.032 (6)	0.023 (6)	−0.014 (5)	0.005 (5)	0.003 (4)
C1	0.022 (9)	0.050 (10)	0.040 (10)	−0.013 (7)	−0.011 (7)	−0.023 (8)
C2	0.044 (10)	0.034 (9)	0.018 (8)	−0.010 (7)	0.006 (7)	−0.003 (6)
C3	0.045 (12)	0.068 (13)	0.015 (8)	0.012 (9)	0.008 (7)	−0.001 (8)
C4	0.035 (11)	0.059 (12)	0.041 (10)	0.022 (9)	0.004 (8)	0.006 (9)
C5	0.034 (9)	0.028 (8)	0.029 (8)	0.023 (6)	−0.003 (7)	−0.018 (6)
C6	0.035 (9)	0.020 (8)	0.046 (10)	−0.011 (6)	0.007 (7)	−0.004 (7)
C7	0.042 (9)	0.027 (8)	0.022 (7)	0.006 (6)	0.008 (6)	−0.011 (6)
C8	0.066 (13)	0.033 (9)	0.067 (14)	−0.022 (9)	0.029 (10)	0.000 (9)
C9	0.022 (8)	0.022 (8)	0.050 (11)	−0.005 (6)	0.013 (7)	0.006 (7)
C10	0.021 (8)	0.037 (9)	0.030 (8)	−0.007 (7)	−0.008 (6)	−0.002 (7)
C11	0.042 (10)	0.022 (8)	0.035 (9)	0.002 (7)	0.005 (8)	−0.009 (7)
C12	0.029 (10)	0.038 (10)	0.069 (13)	−0.016 (8)	0.011 (9)	−0.009 (9)
C13	0.085 (14)	0.027 (8)	0.045 (11)	−0.018 (8)	0.003 (10)	−0.016 (8)
C14	0.060 (12)	0.041 (9)	0.041 (10)	0.005 (8)	0.007 (8)	−0.010 (7)
C15	0.084 (15)	0.042 (10)	0.034 (9)	−0.014 (10)	−0.005 (9)	−0.006 (8)
C16	0.063 (12)	0.039 (9)	0.030 (9)	0.004 (8)	−0.005 (8)	−0.010 (7)
C17	0.052 (8)	0.032 (6)	0.015 (5)	−0.023 (9)	0.009 (8)	0.004 (4)
C18	0.027 (7)	0.019 (5)	0.039 (7)	0.003 (7)	−0.008 (8)	−0.006 (5)
C19	0.040 (10)	0.018 (6)	0.060 (9)	−0.006 (7)	0.005 (8)	0.003 (6)
C20	0.075 (16)	0.052 (8)	0.013 (6)	0.020 (8)	0.015 (8)	0.012 (6)
C21	0.018 (7)	0.037 (8)	0.024 (7)	0.002 (6)	−0.007 (5)	−0.001 (6)
C22	0.009 (6)	0.029 (7)	0.046 (9)	−0.004 (5)	0.001 (6)	0.017 (6)
C23	0.018 (7)	0.036 (8)	0.030 (7)	−0.002 (6)	−0.013 (6)	0.019 (6)
C24	0.042 (10)	0.044 (10)	0.048 (10)	−0.020 (8)	−0.003 (8)	0.027 (8)
C25	0.034 (8)	0.020 (6)	0.034 (8)	0.012 (5)	0.001 (6)	0.004 (5)
C26	0.036 (11)	0.027 (6)	0.040 (8)	0.001 (6)	0.010 (6)	0.004 (5)
C27	0.053 (11)	0.039 (7)	0.023 (6)	0.022 (8)	−0.003 (8)	0.000 (5)
C28	0.086 (14)	0.042 (9)	0.064 (12)	0.029 (10)	0.003 (10)	−0.016 (8)
C1A	0.007 (7)	0.021 (7)	0.021 (7)	0.005 (5)	0.006 (5)	0.011 (5)
C2A	0.022 (8)	0.022 (8)	0.058 (11)	−0.009 (6)	−0.001 (7)	0.011 (7)
C3A	0.023 (9)	0.029 (8)	0.044 (10)	0.013 (6)	0.015 (7)	0.005 (7)
C4A	0.063 (13)	0.020 (8)	0.056 (12)	0.019 (8)	0.033 (10)	0.004 (7)
C5A	0.026 (8)	0.026 (8)	0.029 (8)	−0.003 (6)	0.000 (6)	0.003 (6)
C6A	0.018 (7)	0.029 (8)	0.034 (8)	−0.006 (6)	−0.001 (6)	−0.020 (6)
C7A	0.033 (8)	0.013 (6)	0.040 (8)	0.011 (5)	−0.010 (7)	−0.013 (6)
C8A	0.054 (11)	0.039 (9)	0.031 (9)	0.020 (8)	−0.001 (8)	0.002 (7)
C9A	0.016 (7)	0.025 (8)	0.028 (8)	0.005 (6)	−0.004 (6)	−0.001 (6)
C10A	0.019 (8)	0.020 (7)	0.049 (10)	0.004 (6)	−0.006 (7)	−0.001 (7)
C11A	0.036 (9)	0.014 (7)	0.039 (9)	0.006 (6)	0.000 (7)	−0.003 (7)
C12A	0.046 (12)	0.021 (8)	0.105 (19)	−0.022 (8)	−0.014 (12)	0.007 (10)
C13A	0.024 (7)	0.036 (8)	0.033 (7)	0.008 (6)	−0.008 (6)	0.003 (6)
C14A	0.066 (11)	0.032 (8)	0.016 (7)	0.015 (7)	0.014 (7)	0.002 (6)
C15A	0.036 (10)	0.045 (10)	0.058 (12)	0.003 (8)	0.012 (8)	0.011 (8)
C16A	0.051 (11)	0.060 (12)	0.029 (8)	0.010 (9)	−0.013 (8)	0.005 (8)
C21A	0.050 (9)	0.018 (6)	0.024 (7)	0.007 (6)	−0.004 (6)	0.002 (5)
C22A	0.050 (11)	0.029 (8)	0.038 (9)	−0.005 (7)	0.006 (8)	0.018 (7)
C23A	0.034 (9)	0.037 (8)	0.046 (10)	0.010 (7)	0.003 (7)	−0.002 (7)
C24A	0.070 (14)	0.040 (10)	0.083 (16)	0.030 (10)	0.002 (12)	0.009 (10)

Geometric parameters (Å, º) top

U1—O13	2.280 (7)	C18—H18A	0.9700
U1—O9	2.305 (8)	C18—H18B	0.9700
U1—O5A	2.305 (11)	C19—C20	1.52 (2)
U1—O5	2.311 (11)	C19—H19A	0.9700
U1—O1A	2.419 (11)	C19—H19B	0.9700
U1—O6	2.426 (7)	C20—H20A	0.9600
U1—O10	2.434 (7)	C20—H20B	0.9600
U1—O1	2.440 (10)	C20—H20C	0.9600
Re1—O2	1.675 (12)	C21—C22	1.528 (19)
Re1—O3	1.698 (13)	C21—H21A	0.9700
Re1—O4	1.698 (11)	C21—H21B	0.9700
Re1—O1	1.752 (11)	C22—C23	1.528 (18)
Re2—O7	1.652 (12)	C22—H22A	0.9700
Re2—O8A	1.691 (12)	C22—H22B	0.9700
Re2—O8	1.697 (11)	C23—C24	1.50 (2)
Re2—O6	1.757 (7)	C23—H23A	0.9700
Re3—O11	1.651 (11)	C23—H23B	0.9700
Re3—O11A	1.676 (12)	C24—H24A	0.9600
Re3—O12	1.689 (9)	C24—H24B	0.9600
Re3—O10	1.737 (7)	C24—H24C	0.9600
Re1A—O3A	1.667 (14)	C25—C26	1.602 (18)
Re1A—O2A	1.681 (12)	C25—H25A	0.9700
Re1A—O4A	1.724 (12)	C25—H25B	0.9700
Re1A—O1A	1.771 (11)	C26—C27	1.48 (2)
P1—O5	1.520 (11)	C26—H26A	0.9700
P1—C9	1.786 (17)	C26—H26B	0.9700
P1—C1	1.812 (18)	C27—C28	1.55 (2)
P1—C5	1.821 (16)	C27—H27A	0.9700
P2—O9	1.528 (8)	C27—H271	0.9700
P2—C13A	1.774 (15)	C28—H28A	0.9600
P2—C17	1.782 (12)	C28—H28B	0.9600
P2—C13	1.86 (2)	C28—H28C	0.9600
P3—O13	1.524 (8)	C1A—C2A	1.52 (2)
P3—C25	1.772 (14)	C1A—H1C	0.9700
P3—C21	1.795 (14)	C1A—H1D	0.9700
P3—C21A	1.816 (15)	C2A—C3A	1.56 (3)
P1A—O5A	1.520 (11)	C2A—H2C	0.9700
P1A—C9A	1.787 (16)	C2A—H2D	0.9700
P1A—C5A	1.789 (15)	C3A—C4A	1.53 (3)
P1A—C1A	1.811 (15)	C3A—H3C	0.9700
C1—C2	1.48 (3)	C3A—H3D	0.9700
C1—H1A	0.9700	C4A—H4D	0.9600
C1—H1B	0.9700	C4A—H4E	0.9600
C2—C3	1.51 (2)	C4A—H4F	0.9600
C2—H2A	0.9700	C5A—C6A	1.50 (2)
C2—H2B	0.9700	C5A—H5C	0.9700
C3—C4	1.57 (3)	C5A—H5D	0.9700
C3—H3A	0.9700	C6A—C7A	1.556 (19)
C3—H3B	0.9700	C6A—H6C	0.9700
C4—H4A	0.9600	C6A—H6D	0.9700
C4—H4B	0.9600	C7A—C8A	1.54 (2)
C4—H4C	0.9600	C7A—H7C	0.9700
C5—C6	1.51 (2)	C7A—H7D	0.9700
C5—H5A	0.9700	C8A—H8D	0.9600
C5—H5B	0.9700	C8A—H8E	0.9600
C6—C7	1.54 (2)	C8A—H8F	0.9600
C6—H6A	0.9700	C9A—C10A	1.54 (2)
C6—H6B	0.9700	C9A—H9C	0.9700
C7—C8	1.51 (2)	C9A—H9D	0.9700
C7—H7A	0.9700	C10A—C11A	1.51 (2)
C7—H7B	0.9700	C10A—H10C	0.9700
C8—H8A	0.9600	C10A—H10D	0.9700
C8—H8B	0.9600	C11A—C12A	1.55 (3)
C8—H8C	0.9600	C11A—H11C	0.9700
C9—C10	1.51 (2)	C11A—H11D	0.9700
C9—H9A	0.9700	C12A—H12D	0.9600
C9—H9B	0.9700	C12A—H12E	0.9600
C10—C11	1.53 (2)	C12A—H12F	0.9600
C10—H10A	0.9700	C13A—C14A	1.50 (2)
C10—H10B	0.9700	C13A—H13C	0.9700
C11—C12	1.52 (2)	C13A—H13D	0.9700
C11—H11A	0.9700	C14A—C15A	1.58 (2)
C11—H11B	0.9700	C14A—H14C	0.9700
C12—H12A	0.9600	C14A—H14D	0.9700
C12—H12B	0.9600	C15A—C16A	1.50 (3)
C12—H12C	0.9600	C15A—H15C	0.9700
C13—C14	1.37 (3)	C15A—H15D	0.9700
C13—H13A	0.9700	C16A—H16D	0.9600
C13—H13B	0.9700	C16A—H16E	0.9600
C14—C15	1.53 (3)	C16A—H16F	0.9600
C14—H14A	0.9700	C21A—C22A	1.571 (19)
C14—H14B	0.9700	C21A—H21C	0.9700
C15—C16	1.53 (2)	C21A—H21D	0.9700
C15—H15A	0.9700	C22A—C23A	1.52 (2)
C15—H15B	0.9700	C22A—H22C	0.9700
C16—H16A	0.9600	C22A—H22D	0.9700
C16—H16B	0.9600	C23A—C24A	1.52 (2)
C16—H16C	0.9600	C23A—H23C	0.9700
C17—C18	1.544 (15)	C23A—H23D	0.9700
C17—H17A	0.9700	C24A—H24D	0.9600
C17—H17B	0.9700	C24A—H24E	0.9600
C18—C19	1.495 (18)	C24A—H24F	0.9600

O13—U1—O9	136.9 (3)	C19—C18—C17	113.1 (9)
O13—U1—O5A	99.1 (4)	C19—C18—H18A	109.0
O9—U1—O5A	95.5 (4)	C17—C18—H18A	109.0
O13—U1—O5	91.2 (4)	C19—C18—H18B	109.0
O9—U1—O5	103.2 (4)	C17—C18—H18B	109.0
O5A—U1—O5	139.6 (3)	H18A—C18—H18B	107.8
O13—U1—O1A	73.6 (3)	C18—C19—C20	109.2 (10)
O9—U1—O1A	72.7 (3)	C18—C19—H19A	109.8
O5A—U1—O1A	72.5 (4)	C20—C19—H19A	109.8
O5—U1—O1A	147.3 (4)	C18—C19—H19B	109.8
O13—U1—O6	152.8 (3)	C20—C19—H19B	109.8
O9—U1—O6	70.1 (3)	H19A—C19—H19B	108.3
O5A—U1—O6	75.7 (4)	C19—C20—H20A	109.5
O5—U1—O6	77.5 (4)	C19—C20—H20B	109.5
O1A—U1—O6	127.6 (4)	H20A—C20—H20B	109.5
O13—U1—O10	74.7 (3)	C19—C20—H20C	109.5
O9—U1—O10	148.3 (3)	H20A—C20—H20C	109.5
O5A—U1—O10	72.3 (5)	H20B—C20—H20C	109.5
O5—U1—O10	73.0 (4)	C22—C21—P3	117.1 (10)
O1A—U1—O10	127.3 (4)	C22—C21—H21A	108.0
O6—U1—O10	78.4 (3)	P3—C21—H21A	108.0
O13—U1—O1	74.0 (3)	C22—C21—H21B	108.0
O9—U1—O1	72.7 (3)	P3—C21—H21B	108.0
O5A—U1—O1	148.9 (4)	H21A—C21—H21B	107.3
O5—U1—O1	71.5 (4)	C21—C22—C23	110.2 (11)
O1A—U1—O1	76.5 (3)	C21—C22—H22A	109.6
O6—U1—O1	123.6 (4)	C23—C22—H22A	109.6
O10—U1—O1	131.4 (4)	C21—C22—H22B	109.6
O2—Re1—O3	108.4 (6)	C23—C22—H22B	109.6
O2—Re1—O4	109.3 (6)	H22A—C22—H22B	108.1
O3—Re1—O4	108.9 (6)	C24—C23—C22	109.9 (12)
O2—Re1—O1	111.1 (5)	C24—C23—H23A	109.7
O3—Re1—O1	109.4 (6)	C22—C23—H23A	109.7
O4—Re1—O1	109.7 (5)	C24—C23—H23B	109.7
O7—Re2—O8A	106.0 (8)	C22—C23—H23B	109.7
O7—Re2—O8	108.0 (7)	H23A—C23—H23B	108.2
O8A—Re2—O8	110.7 (5)	C23—C24—H24A	109.5
O7—Re2—O6	109.6 (4)	C23—C24—H24B	109.5
O8A—Re2—O6	109.7 (6)	H24A—C24—H24B	109.5
O8—Re2—O6	112.6 (6)	C23—C24—H24C	109.5
O11—Re3—O11A	107.9 (7)	H24A—C24—H24C	109.5
O11—Re3—O12	107.4 (6)	H24B—C24—H24C	109.5
O11A—Re3—O12	108.9 (5)	C26—C25—P3	118.9 (9)
O11—Re3—O10	110.7 (6)	C26—C25—H25A	107.6
O11A—Re3—O10	111.4 (6)	P3—C25—H25A	107.6
O12—Re3—O10	110.5 (4)	C26—C25—H25B	107.6
O3A—Re1A—O2A	109.0 (5)	P3—C25—H25B	107.6
O3A—Re1A—O4A	109.9 (6)	H25A—C25—H25B	107.0
O2A—Re1A—O4A	109.7 (6)	C27—C26—C25	110.6 (12)
O3A—Re1A—O1A	109.4 (6)	C27—C26—H26A	109.5
O2A—Re1A—O1A	109.4 (5)	C25—C26—H26A	109.5
O4A—Re1A—O1A	109.3 (5)	C27—C26—H26B	109.5
O5—P1—C9	110.6 (7)	C25—C26—H26B	109.5
O5—P1—C1	113.8 (8)	H26A—C26—H26B	108.1
C9—P1—C1	105.7 (9)	C26—C27—C28	109.6 (15)
O5—P1—C5	108.2 (7)	C26—C27—H27A	109.7
C9—P1—C5	109.0 (7)	C28—C27—H27A	109.7
C1—P1—C5	109.4 (8)	C26—C27—H271	109.7
O9—P2—C13A	107.7 (7)	C28—C27—H271	109.7
O9—P2—C17	113.3 (5)	H27A—C27—H271	108.2
C13A—P2—C17	113.7 (8)	C27—C28—H28A	109.5
O9—P2—C13	109.9 (7)	C27—C28—H28B	109.5
C13A—P2—C13	108.8 (7)	H28A—C28—H28B	109.5
C17—P2—C13	103.3 (9)	C27—C28—H28C	109.5
O13—P3—C25	114.4 (6)	H28A—C28—H28C	109.5
O13—P3—C21	108.5 (7)	H28B—C28—H28C	109.5
C25—P3—C21	109.8 (7)	C2A—C1A—P1A	116.2 (12)
O13—P3—C21A	107.6 (6)	C2A—C1A—H1C	108.2
C25—P3—C21A	104.2 (6)	P1A—C1A—H1C	108.2
C21—P3—C21A	112.3 (7)	C2A—C1A—H1D	108.2
O5A—P1A—C9A	110.0 (7)	P1A—C1A—H1D	108.2
O5A—P1A—C5A	108.8 (7)	H1C—C1A—H1D	107.4
C9A—P1A—C5A	109.7 (7)	C1A—C2A—C3A	112.3 (14)
O5A—P1A—C1A	111.5 (7)	C1A—C2A—H2C	109.1
C9A—P1A—C1A	107.3 (7)	C3A—C2A—H2C	109.1
C5A—P1A—C1A	109.5 (7)	C1A—C2A—H2D	109.1
Re1—O1—U1	147.4 (5)	C3A—C2A—H2D	109.1
P1—O5—U1	163.7 (6)	H2C—C2A—H2D	107.9
Re2—O6—U1	154.2 (4)	C4A—C3A—C2A	115.0 (13)
P2—O9—U1	154.7 (6)	C4A—C3A—H3C	108.5
Re3—O10—U1	150.5 (4)	C2A—C3A—H3C	108.5
P3—O13—U1	166.2 (6)	C4A—C3A—H3D	108.5
Re1A—O1A—U1	148.7 (6)	C2A—C3A—H3D	108.5
P1A—O5A—U1	162.7 (7)	H3C—C3A—H3D	107.5
C2—C1—P1	118.6 (13)	C3A—C4A—H4D	109.5
C2—C1—H1A	107.7	C3A—C4A—H4E	109.5
P1—C1—H1A	107.7	H4D—C4A—H4E	109.5
C2—C1—H1B	107.7	C3A—C4A—H4F	109.5
P1—C1—H1B	107.7	H4D—C4A—H4F	109.5
H1A—C1—H1B	107.1	H4E—C4A—H4F	109.5
C1—C2—C3	113.6 (15)	C6A—C5A—P1A	116.8 (11)
C1—C2—H2A	108.8	C6A—C5A—H5C	108.1
C3—C2—H2A	108.8	P1A—C5A—H5C	108.1
C1—C2—H2B	108.8	C6A—C5A—H5D	108.1
C3—C2—H2B	108.8	P1A—C5A—H5D	108.1
H2A—C2—H2B	107.7	H5C—C5A—H5D	107.3
C2—C3—C4	113.5 (17)	C5A—C6A—C7A	111.7 (12)
C2—C3—H3A	108.9	C5A—C6A—H6C	109.3
C4—C3—H3A	108.9	C7A—C6A—H6C	109.3
C2—C3—H3B	108.9	C5A—C6A—H6D	109.3
C4—C3—H3B	108.9	C7A—C6A—H6D	109.3
H3A—C3—H3B	107.7	H6C—C6A—H6D	107.9
C3—C4—H4A	109.5	C8A—C7A—C6A	112.8 (13)
C3—C4—H4B	109.5	C8A—C7A—H7C	109.0
H4A—C4—H4B	109.5	C6A—C7A—H7C	109.0
C3—C4—H4C	109.5	C8A—C7A—H7D	109.0
H4A—C4—H4C	109.5	C6A—C7A—H7D	109.0
H4B—C4—H4C	109.5	H7C—C7A—H7D	107.8
C6—C5—P1	116.5 (10)	C7A—C8A—H8D	109.5
C6—C5—H5A	108.2	C7A—C8A—H8E	109.5
P1—C5—H5A	108.2	H8D—C8A—H8E	109.5
C6—C5—H5B	108.2	C7A—C8A—H8F	109.5
P1—C5—H5B	108.2	H8D—C8A—H8F	109.5
H5A—C5—H5B	107.3	H8E—C8A—H8F	109.5
C5—C6—C7	109.5 (13)	C10A—C9A—P1A	113.8 (10)
C5—C6—H6A	109.8	C10A—C9A—H9C	108.8
C7—C6—H6A	109.8	P1A—C9A—H9C	108.8
C5—C6—H6B	109.8	C10A—C9A—H9D	108.8
C7—C6—H6B	109.8	P1A—C9A—H9D	108.8
H6A—C6—H6B	108.2	H9C—C9A—H9D	107.7
C8—C7—C6	112.3 (13)	C11A—C10A—C9A	112.8 (13)
C8—C7—H7A	109.2	C11A—C10A—H10C	109.0
C6—C7—H7A	109.2	C9A—C10A—H10C	109.0
C8—C7—H7B	109.2	C11A—C10A—H10D	109.0
C6—C7—H7B	109.2	C9A—C10A—H10D	109.0
H7A—C7—H7B	107.9	H10C—C10A—H10D	107.8
C7—C8—H8A	109.5	C10A—C11A—C12A	114.7 (15)
C7—C8—H8B	109.5	C10A—C11A—H11C	108.6
H8A—C8—H8B	109.5	C12A—C11A—H11C	108.6
C7—C8—H8C	109.5	C10A—C11A—H11D	108.6
H8A—C8—H8C	109.5	C12A—C11A—H11D	108.6
H8B—C8—H8C	109.5	H11C—C11A—H11D	107.6
C10—C9—P1	114.2 (12)	C11A—C12A—H12D	109.5
C10—C9—H9A	108.7	C11A—C12A—H12E	109.5
P1—C9—H9A	108.7	H12D—C12A—H12E	109.5
C10—C9—H9B	108.7	C11A—C12A—H12F	109.5
P1—C9—H9B	108.7	H12D—C12A—H12F	109.5
H9A—C9—H9B	107.6	H12E—C12A—H12F	109.5
C9—C10—C11	114.9 (14)	C14A—C13A—P2	111.4 (10)
C9—C10—H10A	108.5	C14A—C13A—H13C	109.4
C11—C10—H10A	108.5	P2—C13A—H13C	109.4
C9—C10—H10B	108.5	C14A—C13A—H13D	109.4
C11—C10—H10B	108.5	P2—C13A—H13D	109.4
H10A—C10—H10B	107.5	H13C—C13A—H13D	108.0
C12—C11—C10	111.6 (15)	C13A—C14A—C15A	111.8 (13)
C12—C11—H11A	109.3	C13A—C14A—H14C	109.3
C10—C11—H11A	109.3	C15A—C14A—H14C	109.3
C12—C11—H11B	109.3	C13A—C14A—H14D	109.3
C10—C11—H11B	109.3	C15A—C14A—H14D	109.3
H11A—C11—H11B	108.0	H14C—C14A—H14D	107.9
C11—C12—H12A	109.5	C16A—C15A—C14A	116.7 (15)
C11—C12—H12B	109.5	C16A—C15A—H15C	108.1
H12A—C12—H12B	109.5	C14A—C15A—H15C	108.1
C11—C12—H12C	109.5	C16A—C15A—H15D	108.1
H12A—C12—H12C	109.5	C14A—C15A—H15D	108.1
H12B—C12—H12C	109.5	H15C—C15A—H15D	107.3
C14—C13—P2	115.9 (14)	C15A—C16A—H16D	109.5
C14—C13—H13A	108.3	C15A—C16A—H16E	109.5
P2—C13—H13A	108.3	H16D—C16A—H16E	109.5
C14—C13—H13B	108.3	C15A—C16A—H16F	109.5
P2—C13—H13B	108.3	H16D—C16A—H16F	109.5
H13A—C13—H13B	107.4	H16E—C16A—H16F	109.5
C13—C14—C15	115.0 (16)	C22A—C21A—P3	117.4 (11)
C13—C14—H14A	108.5	C22A—C21A—H21C	108.0
C15—C14—H14A	108.5	P3—C21A—H21C	108.0
C13—C14—H14B	108.5	C22A—C21A—H21D	108.0
C15—C14—H14B	108.5	P3—C21A—H21D	108.0
H14A—C14—H14B	107.5	H21C—C21A—H21D	107.2
C16—C15—C14	110.3 (17)	C23A—C22A—C21A	109.2 (13)
C16—C15—H15A	109.6	C23A—C22A—H22C	109.8
C14—C15—H15A	109.6	C21A—C22A—H22C	109.8
C16—C15—H15B	109.6	C23A—C22A—H22D	109.8
C14—C15—H15B	109.6	C21A—C22A—H22D	109.8
H15A—C15—H15B	108.1	H22C—C22A—H22D	108.3
C15—C16—H16A	109.5	C24A—C23A—C22A	108.3 (15)
C15—C16—H16B	109.5	C24A—C23A—H23C	110.0
H16A—C16—H16B	109.5	C22A—C23A—H23C	110.0
C15—C16—H16C	109.5	C24A—C23A—H23D	110.0
H16A—C16—H16C	109.5	C22A—C23A—H23D	110.0
H16B—C16—H16C	109.5	H23C—C23A—H23D	108.4
C18—C17—P2	112.6 (8)	C23A—C24A—H24D	109.5
C18—C17—H17A	109.1	C23A—C24A—H24E	109.5
P2—C17—H17A	109.1	H24D—C24A—H24E	109.5
C18—C17—H17B	109.1	C23A—C24A—H24F	109.5
P2—C17—H17B	109.1	H24D—C24A—H24F	109.5
H17A—C17—H17B	107.8	H24E—C24A—H24F	109.5

O2—Re1—O1—U1	−71.8 (11)	C9A—P1A—O5A—U1	−174 (2)
O3—Re1—O1—U1	168.5 (10)	C5A—P1A—O5A—U1	66 (3)
O4—Re1—O1—U1	49.1 (11)	C1A—P1A—O5A—U1	−55 (2)
O13—U1—O1—Re1	−73.6 (10)	O13—U1—O5A—P1A	144 (2)
O9—U1—O1—Re1	134.1 (11)	O9—U1—O5A—P1A	−77 (2)
O5A—U1—O1—Re1	−154.6 (8)	O5—U1—O5A—P1A	41 (3)
O5—U1—O1—Re1	23.2 (10)	O1A—U1—O5A—P1A	−147 (2)
O1A—U1—O1—Re1	−150.1 (11)	O6—U1—O5A—P1A	−9 (2)
O6—U1—O1—Re1	83.4 (11)	O10—U1—O5A—P1A	73 (2)
O10—U1—O1—Re1	−21.9 (12)	O1—U1—O5A—P1A	−142 (2)
C9—P1—O5—U1	151 (2)	O5—P1—C1—C2	−60.7 (16)
C1—P1—O5—U1	33 (3)	C9—P1—C1—C2	177.7 (14)
C5—P1—O5—U1	−89 (2)	C5—P1—C1—C2	60.5 (16)
O13—U1—O5—P1	−128 (2)	P1—C1—C2—C3	172.0 (13)
O9—U1—O5—P1	93 (2)	C1—C2—C3—C4	68 (2)
O5A—U1—O5—P1	−22 (2)	O5—P1—C5—C6	179.6 (12)
O1A—U1—O5—P1	172 (2)	C9—P1—C5—C6	−60.1 (15)
O6—U1—O5—P1	27 (2)	C1—P1—C5—C6	55.0 (15)
O10—U1—O5—P1	−54 (2)	P1—C5—C6—C7	179.5 (11)
O1—U1—O5—P1	160 (2)	C5—C6—C7—C8	180.0 (16)
O7—Re2—O6—U1	−166.0 (16)	O5—P1—C9—C10	−62.6 (14)
O8A—Re2—O6—U1	78.0 (17)	C1—P1—C9—C10	61.0 (14)
O8—Re2—O6—U1	−45.8 (17)	C5—P1—C9—C10	178.6 (12)
O13—U1—O6—Re2	159.4 (12)	P1—C9—C10—C11	177.3 (12)
O9—U1—O6—Re2	−17.1 (15)	C9—C10—C11—C12	69.9 (19)
O5A—U1—O6—Re2	−118.5 (17)	O9—P2—C13—C14	47.9 (14)
O5—U1—O6—Re2	92.1 (16)	C13A—P2—C13—C14	−69.8 (14)
O1A—U1—O6—Re2	−64.5 (18)	C17—P2—C13—C14	169.1 (13)
O10—U1—O6—Re2	167.0 (17)	P2—C13—C14—C15	168.1 (13)
O1—U1—O6—Re2	34.7 (18)	C13—C14—C15—C16	−69 (2)
C13A—P2—O9—U1	−120.1 (15)	O9—P2—C17—C18	−175.5 (13)
C17—P2—O9—U1	6 (2)	C13A—P2—C17—C18	−52.1 (18)
C13—P2—O9—U1	121.5 (16)	C13—P2—C17—C18	65.7 (16)
O13—U1—O9—P2	−11.6 (19)	P2—C17—C18—C19	−176.1 (15)
O5A—U1—O9—P2	−121.3 (16)	C17—C18—C19—C20	179.9 (17)
O5—U1—O9—P2	94.8 (16)	O13—P3—C21—C22	176.6 (11)
O1A—U1—O9—P2	−51.6 (16)	C25—P3—C21—C22	50.9 (13)
O6—U1—O9—P2	166.1 (17)	C21A—P3—C21—C22	−64.5 (13)
O10—U1—O9—P2	173.7 (13)	P3—C21—C22—C23	172.7 (10)
O1—U1—O9—P2	29.3 (15)	C21—C22—C23—C24	−178.2 (14)
O11—Re3—O10—U1	73.0 (17)	O13—P3—C25—C26	−56.3 (13)
O11A—Re3—O10—U1	−47.1 (18)	C21—P3—C25—C26	65.9 (12)
O12—Re3—O10—U1	−168.2 (15)	C21A—P3—C25—C26	−173.6 (11)
O13—U1—O10—Re3	−8.7 (16)	P3—C25—C26—C27	−175.3 (12)
O9—U1—O10—Re3	167.5 (12)	C25—C26—C27—C28	178.9 (14)
O5A—U1—O10—Re3	96.4 (17)	O5A—P1A—C1A—C2A	65.7 (12)
O5—U1—O10—Re3	−104.8 (17)	C9A—P1A—C1A—C2A	−173.8 (11)
O1A—U1—O10—Re3	46.0 (19)	C5A—P1A—C1A—C2A	−54.8 (13)
O6—U1—O10—Re3	174.9 (17)	P1A—C1A—C2A—C3A	179.1 (10)
O1—U1—O10—Re3	−60.2 (18)	C1A—C2A—C3A—C4A	−56.6 (18)
C25—P3—O13—U1	53 (3)	O5A—P1A—C5A—C6A	−176.2 (11)
C21—P3—O13—U1	−70 (3)	C9A—P1A—C5A—C6A	63.5 (14)
C21A—P3—O13—U1	169 (3)	C1A—P1A—C5A—C6A	−54.0 (14)
O9—U1—O13—P3	−34 (3)	P1A—C5A—C6A—C7A	175.5 (11)
O5A—U1—O13—P3	74 (3)	C5A—C6A—C7A—C8A	−179.9 (14)
O5—U1—O13—P3	−145 (3)	O5A—P1A—C9A—C10A	54.9 (13)
O1A—U1—O13—P3	5 (3)	C5A—P1A—C9A—C10A	174.6 (11)
O6—U1—O13—P3	150 (3)	C1A—P1A—C9A—C10A	−66.5 (13)
O10—U1—O13—P3	143 (3)	P1A—C9A—C10A—C11A	176.8 (12)
O1—U1—O13—P3	−75 (3)	C9A—C10A—C11A—C12A	−66 (2)
O3A—Re1A—O1A—U1	152.9 (10)	O9—P2—C13A—C14A	67.0 (11)
O2A—Re1A—O1A—U1	33.6 (12)	C17—P2—C13A—C14A	−59.4 (13)
O4A—Re1A—O1A—U1	−86.6 (11)	C13—P2—C13A—C14A	−173.9 (11)
O13—U1—O1A—Re1A	121.0 (11)	P2—C13A—C14A—C15A	−176.3 (12)
O9—U1—O1A—Re1A	−86.2 (10)	C13A—C14A—C15A—C16A	−60 (2)
O5A—U1—O1A—Re1A	15.5 (10)	O13—P3—C21A—C22A	−161.5 (11)
O5—U1—O1A—Re1A	−173.8 (8)	C25—P3—C21A—C22A	−39.7 (13)
O6—U1—O1A—Re1A	−39.8 (12)	C21—P3—C21A—C22A	79.2 (13)
O10—U1—O1A—Re1A	65.8 (12)	P3—C21A—C22A—C23A	171.3 (12)
O1—U1—O1A—Re1A	−162.0 (11)	C21A—C22A—C23A—C24A	177.8 (15)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.97	2.57	3.44 (2)	149
C2—H2A···O7	0.97	2.93	3.36 (2)	108
C2—H2A···O10	0.97	2.88	3.583 (19)	130
C2—H2A···O7	0.97	2.93	3.36 (2)	108
C3—H3A···O12	0.97	2.82	3.67 (2)	148
C5—H5A···O2	0.97	2.74	3.56 (2)	143
C5—H5B···O8	0.97	2.58	3.529 (19)	165
C9—H9A···O2	0.97	2.77	3.59 (2)	142
C9—H9A···O4	0.97	2.89	3.57 (2)	127
C10—H10A···O5	0.97	2.91	3.28 (2)	104
C10—H10B···O11	0.97	2.89	3.37 (2)	112
C10—H10B···O11	0.97	2.89	3.37 (2)	112
C13—H13B···O2A	0.97	2.79	3.56 (2)	137
C14—H14A···O8A	0.97	2.72	3.27 (2)	116
C14—H14B···O9	0.97	2.92	3.18 (2)	96
C14—H14A···O8A	0.97	2.72	3.27 (2)	116
C17—H17A···O1	0.97	2.53	3.215 (19)	128
C17—H17A···O3	0.97	2.97	3.92 (3)	166
C17—H17B···O1A	0.97	2.90	3.475 (18)	119
C17—H17B···O3A	0.97	2.82	3.78 (2)	173
C21—H21A···O11A	0.97	2.60	3.494 (18)	153
C21—H21B···O4A	0.97	2.62	3.591 (19)	177
C25—H25A···O4	0.97	2.67	3.528 (19)	147
C26—H26B···O1	0.97	2.91	3.720 (17)	141
C26—H26B···O1A	0.97	2.67	3.308 (17)	124
C2A—H2D···O6	0.97	2.56	3.34 (2)	137
C2A—H2D···O10	0.97	2.83	3.58 (2)	135
C3A—H3C···O12	0.97	2.68	3.556 (18)	151
C5A—H5C···O8A	0.97	2.53	3.479 (19)	167
C5A—H5D···O2A	0.97	2.56	3.39 (2)	144
C9A—H9D···O2A	0.97	2.81	3.574 (19)	137
C9A—H9D···O4A	0.97	2.90	3.56 (2)	126
C10A—H10C···O4A	0.97	2.87	3.45 (2)	119
C10A—H10C···O5A	0.97	2.89	3.209 (19)	101
C13A—H13D···O8	0.97	2.71	3.49 (2)	138
C14A—H14D···O2	0.97	2.95	3.471 (18)	115
C14A—H14D···O9	0.97	2.81	3.20 (2)	105
C15A—H15C···O8	0.97	2.98	3.73 (2)	135
C21A—H21D···O11	0.97	2.82	3.481 (19)	126
C6—H6A···O3Aⁱ	0.97	2.75	3.52 (2)	137
C6—H6B···O4Aⁱ	0.97	2.74	3.46 (2)	131
C12—H12B···O3Aⁱ	0.96	2.83	3.74 (2)	158
C9—H9B···O3Aⁱ	0.97	2.72	3.69 (2)	175
C8—H8B···O4Aⁱ	0.96	2.90	3.65 (2)	136
C13A—H13C···O7ⁱⁱ	0.97	2.63	3.524 (17)	154
C16—H16A···O8Aⁱⁱ	0.96	2.98	3.89 (2)	160
C16A—H16D···O7ⁱⁱ	0.96	2.81	3.75 (2)	168
C18—H18A···O8Aⁱⁱ	0.97	2.97	3.757 (17)	140
C20—H20C···O7ⁱⁱⁱ	0.96	2.73	3.537 (18)	142
C22—H22B···O11A^iv	0.97	2.91	3.665 (19)	135
C24—H24A···O12^iv	0.96	2.73	3.51 (2)	138
C22—H22A···O12^iv	0.97	2.68	3.417 (17)	133
C22A—H22C···O12^iv	0.97	2.68	3.540 (18)	148
C22A—H22D···O11^iv	0.97	2.98	3.598 (19)	123
C12A—H12D···O3^v	0.96	2.99	3.92 (2)	163
C4A—H4D···O2^v	0.96	2.83	3.68 (2)	149
C6A—H6D···O3^v	0.97	2.64	3.437 (18)	140
C8A—H8D···O4^v	0.96	2.96	3.46 (2)	114
C9A—H9C···O3^v	0.97	2.76	3.712 (19)	166
C8—H8C···O11A^vi	0.96	3.15	3.87 (2)	133
C20—H20B···O8ⁱⁱ	0.96	3.11	3.57 (2)	111
C20—H20B···O8Aⁱⁱ	0.96	3.03	3.93 (2)	158
C24—H24B···O11A^iv	0.96	3.19	3.81 (2)	124
C28—H28C···O12ⁱⁱⁱ	0.96	3.01	3.97 (2)	173
C8A—H8E···O11^vii	0.96	3.16	3.98 (2)	145
C16A—H16D···O7ⁱⁱ	0.96	2.81	3.75 (2)	168
C24A—H24D···O11^iv	0.96	3.05	3.74 (3)	131
C24A—H24E···O12^iv	0.96	3.29	3.94 (3)	126

Symmetry codes: (i) x−1/2, −y+3/2, z+1/2; (ii) x, −y+1, z−1/2; (iii) x, y, z−1; (iv) x, −y+2, z−1/2; (v) x+1/2, −y+3/2, z+1/2; (vi) x−1/2, y−1/2, z; (vii) x+1/2, y−1/2, z.

(IIat293) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	D_x = 1.943 Mg m⁻³
M_r = 2106.06	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4₂m	Cell parameters from 1544 reflections
a = 15.5577 (12) Å	θ = 2.7–20.5°
c = 14.8730 (17) Å	µ = 8.91 mm⁻¹
V = 3599.9 (6) Å³	T = 293 K
Z = 2	Plate, colourless
F(000) = 2012	0.18 × 0.18 × 0.10 mm

Data collection top

CCD area detector diffractometer	1932 independent reflections
Radiation source: fine-focus sealed tube	1605 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.028
phi and ω scans	θ_max = 26.4°, θ_min = 1.9°
Absorption correction: multi-scan SADABS	h = −19→7
T_min = 0.297, T_max = 0.470	k = −12→16
5728 measured reflections	l = −16→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.044	H-atom parameters constrained
wR(F²) = 0.117	w = 1/[σ²(F_o²) + (0.0736P)²] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max < 0.001
1932 reflections	Δρ_max = 0.79 e Å⁻³
102 parameters	Δρ_min = −0.59 e Å⁻³
95 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.09 (4)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	Z = 2
M_r = 2106.06	Mo Kα radiation
Tetragonal, I4₂m	µ = 8.91 mm⁻¹
a = 15.5577 (12) Å	T = 293 K
c = 14.8730 (17) Å	0.18 × 0.18 × 0.10 mm
V = 3599.9 (6) Å³

Data collection top

CCD area detector diffractometer	1932 independent reflections
Absorption correction: multi-scan SADABS	1605 reflections with I > 2σ(I)
T_min = 0.297, T_max = 0.470	R_int = 0.028
5728 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	H-atom parameters constrained
wR(F²) = 0.117	Δρ_max = 0.79 e Å⁻³
S = 1.01	Δρ_min = −0.59 e Å⁻³
1932 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
102 parameters	Absolute structure parameter: 0.09 (4)
95 restraints

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.5000	0.5000	0.5000	0.0554 (3)
Re1	0.35587 (3)	0.35587 (3)	0.67317 (4)	0.0863 (3)
P1	0.3470 (3)	0.3470 (3)	0.3806 (4)	0.124 (2)
O1	0.4278 (6)	0.4278 (6)	0.6242 (9)	0.104 (3)
O2	0.2561 (7)	0.3779 (11)	0.6402 (9)	0.156 (4)
O3	0.3608 (9)	0.3608 (9)	0.7830 (9)	0.152 (6)
O4	0.4019 (5)	0.4019 (5)	0.4429 (10)	0.106 (4)
C1	0.2387 (9)	0.3958 (17)	0.3955 (18)	0.209 (10)
H1A	0.2318	0.4086	0.4589	0.250*
H1B	0.2387	0.4504	0.3640	0.250*
C2	0.1629 (11)	0.3490 (17)	0.367 (2)	0.222 (10)
H2A	0.1647	0.2904	0.3892	0.266*
H2B	0.1598	0.3473	0.3017	0.266*
C3	0.0842 (13)	0.3970 (17)	0.406 (2)	0.217 (11)
H3A	0.0765	0.3852	0.4694	0.261*
H3B	0.0884	0.4586	0.3966	0.261*
C4	0.0121 (14)	0.3571 (17)	0.3490 (16)	0.212 (11)
H4A	−0.0424	0.3793	0.3684	0.318*
H4B	0.0128	0.2957	0.3562	0.318*
H4C	0.0209	0.3712	0.2868	0.318*
C5	0.3937 (16)	0.3937 (16)	0.2812 (15)	0.31 (2)
H5A	0.3837	0.4553	0.2801	0.367*	0.50
H5B	0.4553	0.3837	0.2801	0.367*	0.50
C6	0.3519 (17)	0.3519 (17)	0.2023 (18)	0.32 (2)
H6A	0.2903	0.3619	0.2036	0.382*	0.50
H6B	0.3619	0.2903	0.2036	0.382*	0.50
C7	0.3915 (16)	0.3915 (16)	0.1167 (17)	0.30 (2)
H7A	0.3814	0.4530	0.1149	0.354*	0.50
H7B	0.4530	0.3814	0.1149	0.354*	0.50
C8	0.347 (2)	0.347 (2)	0.037 (2)	0.35 (3)
H8A	0.3687	0.3705	−0.0181	0.528*
H8B	0.2863	0.3566	0.0408	0.528*	0.50
H8C	0.3587	0.2866	0.0393	0.528*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0521 (3)	0.0521 (3)	0.0620 (5)	0.000	0.000	0.000
Re1	0.0868 (4)	0.0868 (4)	0.0853 (4)	−0.0083 (4)	0.0170 (3)	0.0170 (3)
P1	0.128 (3)	0.128 (3)	0.115 (4)	−0.060 (4)	−0.0159 (19)	−0.0159 (19)
O1	0.103 (5)	0.103 (5)	0.107 (7)	−0.013 (7)	0.023 (4)	0.023 (4)
O2	0.098 (6)	0.191 (12)	0.178 (10)	−0.002 (7)	0.002 (6)	0.019 (10)
O3	0.184 (9)	0.184 (9)	0.089 (6)	−0.006 (15)	0.028 (5)	0.028 (5)
O4	0.097 (5)	0.097 (5)	0.126 (8)	−0.038 (7)	−0.017 (4)	−0.017 (4)
C1	0.130 (7)	0.29 (3)	0.209 (18)	−0.032 (11)	−0.070 (10)	−0.048 (19)
C2	0.128 (8)	0.24 (2)	0.30 (2)	−0.018 (12)	0.020 (15)	−0.097 (19)
C3	0.150 (10)	0.20 (2)	0.31 (3)	0.004 (15)	0.062 (17)	−0.085 (19)
C4	0.142 (11)	0.25 (3)	0.25 (3)	0.017 (16)	0.045 (18)	−0.04 (3)
C5	0.40 (3)	0.40 (3)	0.120 (9)	0.10 (4)	0.087 (16)	0.087 (16)
C6	0.41 (3)	0.41 (3)	0.140 (9)	0.12 (4)	0.076 (18)	0.076 (18)
C7	0.38 (3)	0.38 (3)	0.124 (11)	0.14 (4)	0.069 (18)	0.069 (18)
C8	0.45 (4)	0.45 (4)	0.154 (13)	0.08 (6)	0.05 (2)	0.05 (2)

Geometric parameters (Å, º) top

Th1—O4ⁱ	2.320 (11)	C2—H2A	0.9700
Th1—O4	2.320 (11)	C2—H2B	0.9700
Th1—O4ⁱⁱ	2.320 (11)	C3—C4	1.536 (18)
Th1—O4ⁱⁱⁱ	2.320 (11)	C3—H3A	0.9700
Th1—O1	2.436 (11)	C3—H3B	0.9700
Th1—O1ⁱ	2.436 (11)	C4—H4A	0.9600
Th1—O1ⁱⁱⁱ	2.436 (11)	C4—H4B	0.9600
Th1—O1ⁱⁱ	2.436 (11)	C4—H4C	0.9600
Re1—O3	1.637 (14)	C5—C6	1.49 (2)
Re1—O2^iv	1.664 (11)	C5—H5A	0.9700
Re1—O2	1.664 (11)	C5—H5B	0.9700
Re1—O1	1.742 (12)	C6—C7	1.544 (19)
P1—O4	1.522 (12)	C6—H6A	0.9700
P1—C5	1.800 (18)	C6—H6B	0.9700
P1—C1	1.862 (15)	C7—C8	1.53 (2)
P1—C1^iv	1.862 (15)	C7—H7A	0.9700
C1—C2	1.449 (17)	C7—H7B	0.9700
C1—H1A	0.9700	C8—H8A	0.9600
C1—H1B	0.9700	C8—H8B	0.9600
C2—C3	1.548 (17)	C8—H8C	0.9600

O4ⁱ—Th1—O4	97.7 (3)	C2—C1—H1B	107.4
O4ⁱ—Th1—O4ⁱⁱ	137.0 (7)	P1—C1—H1B	107.4
O4—Th1—O4ⁱⁱ	97.7 (3)	H1A—C1—H1B	106.9
O4ⁱ—Th1—O4ⁱⁱⁱ	97.7 (3)	C1—C2—C3	106.9 (16)
O4—Th1—O4ⁱⁱⁱ	137.0 (7)	C1—C2—H2A	110.3
O4ⁱⁱ—Th1—O4ⁱⁱⁱ	97.7 (3)	C3—C2—H2A	110.3
O4ⁱ—Th1—O1	73.9 (3)	C1—C2—H2B	110.3
O4—Th1—O1	70.8 (5)	C3—C2—H2B	110.3
O4ⁱⁱ—Th1—O1	73.9 (3)	H2A—C2—H2B	108.6
O4ⁱⁱⁱ—Th1—O1	152.2 (5)	C4—C3—C2	100.1 (16)
O4ⁱ—Th1—O1ⁱ	70.8 (5)	C4—C3—H3A	111.7
O4—Th1—O1ⁱ	73.9 (3)	C2—C3—H3A	111.7
O4ⁱⁱ—Th1—O1ⁱ	152.2 (5)	C4—C3—H3B	111.7
O4ⁱⁱⁱ—Th1—O1ⁱ	73.9 (3)	C2—C3—H3B	111.7
O1—Th1—O1ⁱ	125.1 (4)	H3A—C3—H3B	109.5
O4ⁱ—Th1—O1ⁱⁱⁱ	73.9 (3)	C3—C4—H4A	109.5
O4—Th1—O1ⁱⁱⁱ	152.2 (5)	C3—C4—H4B	109.5
O4ⁱⁱ—Th1—O1ⁱⁱⁱ	73.9 (3)	H4A—C4—H4B	109.5
O4ⁱⁱⁱ—Th1—O1ⁱⁱⁱ	70.8 (5)	C3—C4—H4C	109.5
O1—Th1—O1ⁱⁱⁱ	81.4 (7)	H4A—C4—H4C	109.5
O1ⁱ—Th1—O1ⁱⁱⁱ	125.1 (4)	H4B—C4—H4C	109.5
O4ⁱ—Th1—O1ⁱⁱ	152.2 (5)	C6—C5—P1	107 (2)
O4—Th1—O1ⁱⁱ	73.9 (3)	C6—C5—H5A	110.3
O4ⁱⁱ—Th1—O1ⁱⁱ	70.8 (5)	P1—C5—H5A	110.3
O4ⁱⁱⁱ—Th1—O1ⁱⁱ	73.9 (3)	C6—C5—H5B	110.3
O1—Th1—O1ⁱⁱ	125.1 (4)	P1—C5—H5B	110.3
O1ⁱ—Th1—O1ⁱⁱ	81.4 (7)	H5A—C5—H5B	108.6
O1ⁱⁱⁱ—Th1—O1ⁱⁱ	125.1 (4)	C5—C6—C7	107 (2)
O3—Re1—O2^iv	109.2 (6)	C5—C6—H6A	110.2
O3—Re1—O2	109.2 (6)	C7—C6—H6A	110.2
O2^iv—Re1—O2	107.3 (12)	C5—C6—H6B	110.2
O3—Re1—O1	110.9 (8)	C7—C6—H6B	110.2
O2^iv—Re1—O1	110.1 (6)	H6A—C6—H6B	108.5
O2—Re1—O1	110.1 (6)	C8—C7—C6	106 (2)
O4—P1—C5	92.7 (13)	C8—C7—H7A	110.5
O4—P1—C1	101.9 (7)	C6—C7—H7A	110.5
C5—P1—C1	107.4 (10)	C8—C7—H7B	110.5
O4—P1—C1^iv	101.9 (7)	C6—C7—H7B	110.5
C5—P1—C1^iv	107.4 (10)	H7A—C7—H7B	108.7
C1—P1—C1^iv	136.4 (18)	C7—C8—H8A	109.5
Re1—O1—Th1	155.4 (8)	C7—C8—H8B	109.5
P1—O4—Th1	164.0 (9)	H8A—C8—H8B	109.5
C2—C1—P1	119.7 (15)	C7—C8—H8C	109.5
C2—C1—H1A	107.4	H8A—C8—H8C	109.5
P1—C1—H1A	107.4	H8B—C8—H8C	109.5

O3—Re1—O1—Th1	180.000 (2)	O4ⁱⁱⁱ—Th1—O4—P1	0.001 (4)
O2^iv—Re1—O1—Th1	59.1 (6)	O1—Th1—O4—P1	180.000 (3)
O2—Re1—O1—Th1	−59.1 (6)	O1ⁱ—Th1—O4—P1	−42.7 (3)
O4ⁱ—Th1—O1—Re1	−104.4 (3)	O1ⁱⁱⁱ—Th1—O4—P1	179.999 (2)
O4—Th1—O1—Re1	0.000 (2)	O1ⁱⁱ—Th1—O4—P1	42.7 (3)
O4ⁱⁱ—Th1—O1—Re1	104.4 (3)	O4—P1—C1—C2	−163 (3)
O4ⁱⁱⁱ—Th1—O1—Re1	179.999 (1)	C5—P1—C1—C2	100 (3)
O1ⁱ—Th1—O1—Re1	−52.83 (14)	C1^iv—P1—C1—C2	−42 (4)
O1ⁱⁱⁱ—Th1—O1—Re1	180.000 (2)	P1—C1—C2—C3	168 (2)
O1ⁱⁱ—Th1—O1—Re1	52.83 (14)	C1—C2—C3—C4	164 (3)
C5—P1—O4—Th1	0.000 (2)	O4—P1—C5—C6	180.000 (2)
C1—P1—O4—Th1	−108.4 (10)	C1—P1—C5—C6	−76.6 (8)
C1^iv—P1—O4—Th1	108.4 (10)	C1^iv—P1—C5—C6	76.6 (8)
O4ⁱ—Th1—O4—P1	−110.1 (3)	P1—C5—C6—C7	180.000 (2)
O4ⁱⁱ—Th1—O4—P1	110.1 (3)	C5—C6—C7—C8	180.000 (3)

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

(IIat230) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	D_x = 1.991 Mg m⁻³
M_r = 2106.06	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 5355 reflections
a = 21.721 (3) Å	θ = 2.7–23.0°
b = 21.738 (3) Å	µ = 9.13 mm⁻¹
c = 14.8793 (19) Å	T = 230 K
V = 7025.4 (16) Å³	Plate, colourless
Z = 4	0.18 × 0.18 × 0.10 mm
F(000) = 4024

Data collection top

CCD area detector diffractometer	6391 independent reflections
Radiation source: fine-focus sealed tube	6029 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.042
phi and ω scans	θ_max = 25.0°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→25
T_min = 0.290, T_max = 0.462	k = −12→25
18098 measured reflections	l = −16→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.036	H-atom parameters constrained
wR(F²) = 0.076	w = 1/[σ²(F_o²) + (0.0314P)² + 8.8462P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max < 0.001
6391 reflections	Δρ_max = 1.13 e Å⁻³
393 parameters	Δρ_min = −1.55 e Å⁻³
387 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.037 (15)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	V = 7025.4 (16) Å³
M_r = 2106.06	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.721 (3) Å	µ = 9.13 mm⁻¹
b = 21.738 (3) Å	T = 230 K
c = 14.8793 (19) Å	0.18 × 0.18 × 0.10 mm

Data collection top

CCD area detector diffractometer	6391 independent reflections
Absorption correction: multi-scan SADABS	6029 reflections with I > 2σ(I)
T_min = 0.290, T_max = 0.462	R_int = 0.042
18098 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	H-atom parameters constrained
wR(F²) = 0.076	Δρ_max = 1.13 e Å⁻³
S = 1.07	Δρ_min = −1.55 e Å⁻³
6391 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
393 parameters	Absolute structure parameter: 0.037 (15)
387 restraints

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.0000	0.25227 (3)	0.29686 (6)	0.02841 (13)
Re1	0.14631 (3)	0.23960 (3)	0.12490 (4)	0.04611 (17)
Re2	0.0000	0.40884 (4)	0.44881 (5)	0.0425 (2)
Re3	0.0000	0.12049 (4)	0.49115 (5)	0.0436 (2)
P1	0.15854 (18)	0.2620 (2)	0.4101 (3)	0.0498 (9)
P2	0.0000	0.3924 (3)	0.1503 (4)	0.0676 (16)
P3	0.0000	0.0902 (3)	0.2015 (4)	0.0569 (14)
O1	0.0733 (5)	0.2466 (5)	0.1686 (8)	0.060 (2)
O2	0.1922 (6)	0.2943 (6)	0.1683 (9)	0.077 (3)
O3	0.1427 (6)	0.2490 (5)	0.0106 (7)	0.076 (3)
O4	0.1735 (7)	0.1686 (5)	0.1485 (8)	0.085 (3)
O5	0.1013 (5)	0.2508 (4)	0.3546 (8)	0.0570 (18)
O6	0.0000	0.3338 (6)	0.4117 (9)	0.051 (3)
O7	0.0000	0.4072 (7)	0.5671 (9)	0.088 (6)
O8	0.0659 (7)	0.4441 (6)	0.4148 (10)	0.096 (5)
O9	0.0000	0.3457 (8)	0.2273 (10)	0.065 (2)
O10	0.0000	0.1902 (6)	0.4385 (10)	0.052 (3)
O11	0.0571 (8)	0.0811 (6)	0.4670 (8)	0.095 (4)
O12	0.0000	0.1315 (8)	0.6050 (9)	0.086 (5)
O13	0.0000	0.1499 (7)	0.2491 (10)	0.059 (3)
C1	0.1483 (9)	0.2425 (8)	0.5274 (10)	0.077 (4)
H1A	0.1343	0.2002	0.5317	0.092*
H1B	0.1877	0.2453	0.5577	0.092*
C2	0.1028 (9)	0.2834 (9)	0.5749 (10)	0.081 (4)
H2A	0.0644	0.2833	0.5416	0.098*
H2B	0.1184	0.3252	0.5749	0.098*
C3	0.0898 (8)	0.2637 (9)	0.6728 (10)	0.079 (4)
H3A	0.0570	0.2890	0.6971	0.095*
H3B	0.0760	0.2213	0.6734	0.095*
C4	0.1460 (9)	0.2699 (10)	0.7313 (12)	0.094 (5)
H4A	0.1772	0.2418	0.7111	0.140*
H4B	0.1354	0.2605	0.7924	0.140*
H4C	0.1614	0.3112	0.7279	0.140*
C5	0.1858 (6)	0.3380 (7)	0.3939 (11)	0.057 (3)
H5A	0.1940	0.3431	0.3303	0.069*
H5B	0.1524	0.3658	0.4090	0.069*
C6	0.2428 (6)	0.3596 (6)	0.4448 (11)	0.060 (3)
H6A	0.2362	0.3529	0.5086	0.072*
H6B	0.2775	0.3343	0.4268	0.072*
C7	0.2592 (7)	0.4254 (6)	0.4305 (13)	0.066 (4)
H7A	0.2249	0.4506	0.4506	0.080*
H7B	0.2642	0.4323	0.3666	0.080*
C8	0.3177 (9)	0.4474 (8)	0.4786 (12)	0.085 (6)
H8A	0.3172	0.4915	0.4831	0.128*
H8B	0.3533	0.4346	0.4451	0.128*
H8C	0.3193	0.4299	0.5378	0.128*
C9	0.2171 (6)	0.2111 (6)	0.3780 (10)	0.051 (2)
H9A	0.2295	0.2214	0.3172	0.062*
H9B	0.2523	0.2182	0.4167	0.062*
C10	0.2018 (7)	0.1434 (6)	0.3808 (12)	0.063 (3)
H10A	0.1897	0.1329	0.4417	0.075*
H10B	0.1665	0.1362	0.3423	0.075*
C11	0.2525 (7)	0.1006 (7)	0.3526 (11)	0.069 (3)
H11A	0.2661	0.1121	0.2928	0.083*
H11B	0.2361	0.0592	0.3491	0.083*
C12	0.3075 (8)	0.1004 (9)	0.4145 (14)	0.089 (5)
H12A	0.3303	0.1379	0.4069	0.134*
H12B	0.3334	0.0659	0.4004	0.134*
H12C	0.2937	0.0972	0.4757	0.134*
C13A	−0.0489 (12)	0.4566 (10)	0.165 (2)	0.078 (3)	0.61 (2)
H13A	−0.0331	0.4822	0.2127	0.094*	0.61 (2)
H13B	−0.0491	0.4809	0.1099	0.094*	0.61 (2)
C14A	−0.1130 (13)	0.4378 (12)	0.186 (2)	0.085 (3)	0.61 (2)
H14A	−0.1118	0.4133	0.2408	0.102*	0.61 (2)
H14B	−0.1274	0.4112	0.1384	0.102*	0.61 (2)
C15A	−0.1609 (13)	0.4890 (13)	0.200 (2)	0.084 (3)	0.61 (2)
H15A	−0.2014	0.4704	0.1950	0.101*	0.61 (2)
H15B	−0.1567	0.5041	0.2607	0.101*	0.61 (2)
C16A	−0.1595 (18)	0.5443 (13)	0.137 (3)	0.085 (5)	0.61 (2)
H16A	−0.1334	0.5756	0.1621	0.128*	0.61 (2)
H16B	−0.2004	0.5603	0.1300	0.128*	0.61 (2)
H16C	−0.1437	0.5321	0.0795	0.128*	0.61 (2)
C13B	−0.0764 (11)	0.4274 (18)	0.135 (3)	0.078 (3)	0.39 (2)
H13C	−0.0711	0.4683	0.1604	0.094*	0.39 (2)
H13D	−0.0788	0.4337	0.0708	0.094*	0.39 (2)
C14B	−0.1428 (16)	0.4112 (16)	0.161 (3)	0.085 (3)	0.39 (2)
H14C	−0.1426	0.3776	0.2036	0.102*	0.39 (2)
H14D	−0.1648	0.3977	0.1076	0.102*	0.39 (2)
C15B	−0.176 (2)	0.4672 (19)	0.202 (3)	0.084 (3)	0.39 (2)
H15C	−0.2184	0.4563	0.2144	0.101*	0.39 (2)
H15D	−0.1565	0.4776	0.2587	0.101*	0.39 (2)
C16B	−0.175 (3)	0.5233 (18)	0.140 (4)	0.085 (5)	0.39 (2)
H16D	−0.1454	0.5526	0.1629	0.128*	0.39 (2)
H16E	−0.2147	0.5418	0.1384	0.128*	0.39 (2)
H16F	−0.1628	0.5108	0.0809	0.128*	0.39 (2)
C17	0.0000	0.3565 (11)	0.0448 (12)	0.074 (4)
H17A	0.0359	0.3301	0.0418	0.089*	0.50
H17B	−0.0359	0.3301	0.0418	0.089*	0.50
C18	0.0000	0.3971 (9)	−0.0395 (10)	0.076 (4)
H18A	0.0361	0.4233	−0.0391	0.091*	0.50
H18B	−0.0361	0.4233	−0.0391	0.091*	0.50
C19	0.0000	0.3574 (9)	−0.1266 (11)	0.080 (5)
H19A	0.0363	0.3314	−0.1285	0.096*	0.50
H19B	−0.0363	0.3314	−0.1285	0.096*	0.50
C20	0.0000	0.4020 (12)	−0.2062 (14)	0.098 (7)
H20A	0.0000	0.3791	−0.2614	0.147*
H20B	0.0361	0.4274	−0.2036	0.147*	0.50
H20C	−0.0361	0.4274	−0.2036	0.147*	0.50
C21	−0.0697 (9)	0.0525 (8)	0.2342 (13)	0.090 (4)
H21A	−0.0678	0.0446	0.2983	0.108*
H21B	−0.1036	0.0806	0.2240	0.108*
C22	−0.0840 (7)	−0.0069 (8)	0.1875 (13)	0.091 (4)
H22A	−0.0517	−0.0364	0.2004	0.109*
H22B	−0.0846	0.0000	0.1231	0.109*
C23	−0.1460 (8)	−0.0337 (8)	0.2168 (13)	0.097 (5)
H23A	−0.1446	−0.0418	0.2809	0.117*
H23B	−0.1778	−0.0032	0.2065	0.117*
C24	−0.1636 (10)	−0.0922 (9)	0.1686 (15)	0.114 (7)
H24A	−0.2052	−0.1030	0.1837	0.172*
H24B	−0.1364	−0.1248	0.1867	0.172*
H24C	−0.1603	−0.0861	0.1049	0.172*
C25	−0.025 (3)	0.0916 (16)	0.0871 (17)	0.155 (11)	0.50
H25A	−0.0169	0.0516	0.0613	0.186*	0.50
H25B	−0.0698	0.0966	0.0876	0.186*	0.50
C26	0.0000	0.1383 (14)	0.0259 (13)	0.161 (11)
H26A	0.0421	0.1466	0.0439	0.193*	0.50
H26B	−0.0232	0.1761	0.0339	0.193*	0.50
C27	0.0000	0.1226 (13)	−0.0728 (13)	0.167 (11)
H27A	−0.0359	0.0974	−0.0848	0.200*	0.50
H27B	0.0359	0.0974	−0.0848	0.200*	0.50
C28	0.0000	0.1751 (16)	−0.139 (2)	0.196 (13)
H28A	0.0000	0.1589	−0.1993	0.295*
H28B	0.0361	0.1998	−0.1304	0.295*	0.50
H28C	−0.0361	0.1998	−0.1304	0.295*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0281 (4)	0.0320 (5)	0.0251 (3)	0.000	0.000	−0.0017 (3)
Re1	0.0424 (3)	0.0563 (4)	0.0397 (3)	0.0068 (3)	0.0107 (3)	0.0005 (3)
Re2	0.0551 (7)	0.0408 (5)	0.0315 (4)	0.000	0.000	−0.0049 (4)
Re3	0.0520 (6)	0.0462 (5)	0.0328 (4)	0.000	0.000	0.0092 (4)
P1	0.0342 (19)	0.072 (2)	0.0432 (18)	−0.0010 (17)	−0.0096 (15)	−0.0030 (18)
P2	0.114 (4)	0.045 (3)	0.044 (3)	0.000	0.000	0.013 (2)
P3	0.070 (4)	0.041 (3)	0.061 (3)	0.000	0.000	−0.019 (2)
O1	0.045 (3)	0.098 (6)	0.037 (3)	−0.008 (3)	0.012 (3)	−0.011 (4)
O2	0.049 (6)	0.085 (5)	0.098 (6)	−0.010 (5)	0.006 (6)	−0.012 (6)
O3	0.098 (9)	0.093 (9)	0.036 (3)	0.019 (6)	0.029 (4)	0.009 (4)
O4	0.111 (8)	0.068 (4)	0.077 (7)	0.027 (5)	0.001 (7)	0.011 (5)
O5	0.031 (3)	0.093 (5)	0.047 (4)	−0.004 (2)	−0.006 (3)	−0.006 (3)
O6	0.082 (7)	0.040 (3)	0.031 (4)	0.000	0.000	−0.005 (3)
O7	0.184 (18)	0.047 (10)	0.034 (3)	0.000	0.000	−0.007 (4)
O8	0.089 (8)	0.083 (8)	0.116 (9)	−0.035 (7)	0.038 (8)	−0.026 (8)
O9	0.116 (6)	0.045 (3)	0.034 (4)	0.000	0.000	0.009 (3)
O10	0.069 (7)	0.045 (4)	0.044 (3)	0.000	0.000	0.013 (3)
O11	0.118 (9)	0.091 (7)	0.077 (7)	0.054 (7)	0.026 (7)	0.027 (6)
O12	0.139 (16)	0.089 (12)	0.030 (3)	0.000	0.000	0.009 (4)
O13	0.077 (6)	0.041 (3)	0.060 (6)	0.000	0.000	−0.017 (3)
C1	0.088 (10)	0.102 (10)	0.041 (3)	0.001 (7)	−0.005 (4)	0.000 (5)
C2	0.090 (9)	0.107 (9)	0.047 (4)	−0.003 (7)	0.004 (5)	−0.003 (6)
C3	0.088 (9)	0.107 (10)	0.043 (5)	0.006 (8)	−0.004 (5)	−0.001 (6)
C4	0.099 (12)	0.125 (14)	0.057 (7)	−0.029 (11)	−0.013 (8)	−0.009 (9)
C5	0.041 (7)	0.065 (4)	0.066 (7)	0.006 (3)	−0.019 (6)	−0.002 (5)
C6	0.046 (6)	0.060 (5)	0.075 (6)	−0.001 (4)	−0.025 (6)	0.010 (6)
C7	0.054 (8)	0.063 (6)	0.081 (9)	−0.006 (5)	−0.022 (7)	0.017 (7)
C8	0.087 (12)	0.074 (9)	0.095 (13)	−0.029 (7)	−0.045 (9)	0.026 (9)
C9	0.037 (5)	0.061 (4)	0.055 (6)	−0.001 (4)	−0.009 (5)	0.012 (6)
C10	0.062 (7)	0.062 (4)	0.065 (7)	−0.008 (5)	−0.006 (6)	0.004 (6)
C11	0.069 (8)	0.061 (6)	0.076 (8)	−0.001 (6)	−0.006 (6)	0.009 (7)
C12	0.082 (10)	0.091 (12)	0.094 (12)	0.012 (9)	−0.021 (8)	0.011 (10)
C13A	0.109 (4)	0.041 (4)	0.086 (6)	−0.003 (4)	−0.005 (4)	0.014 (4)
C14A	0.109 (4)	0.054 (5)	0.092 (5)	−0.006 (4)	−0.003 (5)	0.015 (5)
C15A	0.107 (5)	0.053 (6)	0.094 (6)	−0.007 (5)	−0.002 (5)	0.018 (5)
C16A	0.110 (10)	0.055 (7)	0.091 (9)	−0.010 (8)	−0.016 (9)	0.019 (7)
C13B	0.109 (4)	0.041 (4)	0.086 (6)	−0.003 (4)	−0.005 (4)	0.014 (4)
C14B	0.109 (4)	0.054 (5)	0.092 (5)	−0.006 (4)	−0.003 (5)	0.015 (5)
C15B	0.107 (5)	0.053 (6)	0.094 (6)	−0.007 (5)	−0.002 (5)	0.018 (5)
C16B	0.110 (10)	0.055 (7)	0.091 (9)	−0.010 (8)	−0.016 (9)	0.019 (7)
C17	0.123 (10)	0.065 (8)	0.034 (4)	0.000	0.000	0.020 (4)
C18	0.121 (11)	0.064 (9)	0.044 (4)	0.000	0.000	0.027 (5)
C19	0.129 (13)	0.075 (10)	0.035 (4)	0.000	0.000	0.030 (6)
C20	0.158 (19)	0.092 (15)	0.045 (5)	0.000	0.000	0.043 (9)
C21	0.075 (8)	0.093 (9)	0.103 (8)	−0.027 (6)	0.026 (7)	−0.066 (7)
C22	0.062 (8)	0.096 (8)	0.115 (9)	−0.030 (6)	0.028 (7)	−0.068 (7)
C23	0.064 (8)	0.104 (10)	0.123 (10)	−0.028 (6)	0.038 (8)	−0.065 (8)
C24	0.072 (12)	0.111 (13)	0.160 (15)	−0.043 (9)	0.023 (12)	−0.068 (11)
C25	0.33 (3)	0.099 (17)	0.041 (6)	0.005 (8)	−0.011 (7)	−0.023 (6)
C26	0.33 (3)	0.104 (16)	0.048 (7)	0.000	0.000	−0.025 (6)
C27	0.34 (3)	0.113 (17)	0.046 (7)	0.000	0.000	−0.017 (8)
C28	0.38 (4)	0.14 (2)	0.067 (9)	0.000	0.000	0.008 (12)

Geometric parameters (Å, º) top

Th1—O9	2.280 (15)	C11—H11A	0.9700
Th1—O13	2.337 (15)	C11—H11B	0.9700
Th1—O5ⁱ	2.362 (11)	C12—H12A	0.9600
Th1—O5	2.362 (11)	C12—H12B	0.9600
Th1—O6	2.462 (13)	C12—H12C	0.9600
Th1—O1ⁱ	2.489 (11)	C13A—C14A	1.486 (18)
Th1—O1	2.489 (11)	C13A—H13A	0.9700
Th1—O10	2.502 (14)	C13A—H13B	0.9700
Re1—O2	1.681 (11)	C14A—C15A	1.537 (18)
Re1—O4	1.690 (11)	C14A—H14A	0.9700
Re1—O3	1.715 (11)	C14A—H14B	0.9700
Re1—O1	1.720 (11)	C15A—C16A	1.522 (18)
Re2—O8	1.701 (12)	C15A—H15A	0.9700
Re2—O8ⁱ	1.701 (12)	C15A—H15B	0.9700
Re2—O6	1.722 (13)	C16A—H16A	0.9600
Re2—O7	1.761 (14)	C16A—H16B	0.9600
Re3—O11ⁱ	1.550 (13)	C16A—H16C	0.9600
Re3—O11	1.550 (13)	C13B—C14B	1.532 (19)
Re3—O10	1.706 (13)	C13B—H13C	0.9700
Re3—O12	1.711 (13)	C13B—H13D	0.9700
P1—O5	1.513 (11)	C14B—C15B	1.543 (19)
P1—C9	1.751 (14)	C14B—H14C	0.9700
P1—C5	1.772 (15)	C14B—H14D	0.9700
P1—C1	1.809 (16)	C15B—C16B	1.528 (19)
P2—O9	1.531 (15)	C15B—H15C	0.9700
P2—C17	1.75 (2)	C15B—H15D	0.9700
P2—C13A	1.767 (16)	C16B—H16D	0.9600
P2—C13Aⁱ	1.767 (16)	C16B—H16E	0.9600
P2—C13Bⁱ	1.840 (18)	C16B—H16F	0.9600
P2—C13B	1.840 (18)	C17—C18	1.533 (15)
P3—O13	1.477 (16)	C17—H17A	0.9700
P3—C21	1.788 (17)	C17—H17B	0.9700
P3—C21ⁱ	1.788 (17)	C18—C19	1.557 (17)
P3—C25	1.79 (3)	C18—H18A	0.9700
P3—C25ⁱ	1.79 (3)	C18—H18B	0.9700
C1—C2	1.506 (15)	C19—C20	1.530 (16)
C1—H1A	0.9700	C19—H19A	0.9700
C1—H1B	0.9700	C19—H19B	0.9700
C2—C3	1.544 (15)	C20—H20A	0.9600
C2—H2A	0.9700	C20—H20B	0.9600
C2—H2B	0.9700	C20—H20C	0.9600
C3—C4	1.506 (16)	C21—C22	1.498 (14)
C3—H3A	0.9700	C21—H21A	0.9700
C3—H3B	0.9700	C21—H21B	0.9700
C4—H4A	0.9600	C22—C23	1.531 (15)
C4—H4B	0.9600	C22—H22A	0.9700
C4—H4C	0.9600	C22—H22B	0.9700
C5—C6	1.526 (14)	C23—C24	1.509 (15)
C5—H5A	0.9700	C23—H23A	0.9700
C5—H5B	0.9700	C23—H23B	0.9700
C6—C7	1.491 (14)	C24—H24A	0.9600
C6—H6A	0.9700	C24—H24B	0.9600
C6—H6B	0.9700	C24—H24C	0.9600
C7—C8	1.536 (15)	C25—C26	1.471 (18)
C7—H7A	0.9700	C25—H25A	0.9700
C7—H7B	0.9700	C25—H25B	0.9700
C8—H8A	0.9600	C26—C27	1.508 (18)
C8—H8B	0.9600	C26—H26A	0.9700
C8—H8C	0.9600	C26—H26B	0.9700
C9—C10	1.510 (14)	C27—C28	1.509 (18)
C9—H9A	0.9700	C27—H27A	0.9700
C9—H9B	0.9700	C27—H27B	0.9700
C10—C11	1.502 (15)	C28—H28A	0.9600
C10—H10A	0.9700	C28—H28B	0.9600
C10—H10B	0.9700	C28—H28C	0.9600
C11—C12	1.508 (15)

O9—Th1—O13	135.3 (6)	C11—C10—H10A	108.3
O9—Th1—O5ⁱ	100.2 (3)	C9—C10—H10A	108.3
O13—Th1—O5ⁱ	95.6 (3)	C11—C10—H10B	108.3
O9—Th1—O5	100.2 (3)	C9—C10—H10B	108.3
O13—Th1—O5	95.6 (3)	H10A—C10—H10B	107.4
O5ⁱ—Th1—O5	137.3 (6)	C10—C11—C12	114.3 (14)
O9—Th1—O6	70.9 (5)	C10—C11—H11A	108.7
O13—Th1—O6	153.7 (5)	C12—C11—H11A	108.7
O5ⁱ—Th1—O6	76.0 (3)	C10—C11—H11B	108.7
O5—Th1—O6	76.0 (3)	C12—C11—H11B	108.7
O9—Th1—O1ⁱ	72.3 (4)	H11A—C11—H11B	107.6
O13—Th1—O1ⁱ	73.7 (4)	C11—C12—H12A	109.5
O5ⁱ—Th1—O1ⁱ	71.5 (4)	C11—C12—H12B	109.5
O5—Th1—O1ⁱ	151.0 (4)	H12A—C12—H12B	109.5
O6—Th1—O1ⁱ	124.6 (3)	C11—C12—H12C	109.5
O9—Th1—O1	72.3 (4)	H12A—C12—H12C	109.5
O13—Th1—O1	73.7 (4)	H12B—C12—H12C	109.5
O5ⁱ—Th1—O1	151.0 (4)	C14A—C13A—P2	111.8 (16)
O5—Th1—O1	71.5 (4)	C14A—C13A—H13A	109.3
O6—Th1—O1	124.6 (3)	P2—C13A—H13A	109.3
O1ⁱ—Th1—O1	79.6 (5)	C14A—C13A—H13B	109.3
O9—Th1—O10	149.6 (5)	P2—C13A—H13B	109.3
O13—Th1—O10	75.1 (5)	H13A—C13A—H13B	107.9
O5ⁱ—Th1—O10	71.7 (3)	C13A—C14A—C15A	117.5 (19)
O5—Th1—O10	71.7 (3)	C13A—C14A—H14A	107.9
O6—Th1—O10	78.7 (4)	C15A—C14A—H14A	107.9
O1ⁱ—Th1—O10	128.3 (3)	C13A—C14A—H14B	107.9
O1—Th1—O10	128.3 (3)	C15A—C14A—H14B	107.9
O2—Re1—O4	111.1 (7)	H14A—C14A—H14B	107.2
O2—Re1—O3	108.9 (6)	C16A—C15A—C14A	119 (2)
O4—Re1—O3	109.3 (5)	C16A—C15A—H15A	107.6
O2—Re1—O1	109.8 (6)	C14A—C15A—H15A	107.6
O4—Re1—O1	108.9 (6)	C16A—C15A—H15B	107.6
O3—Re1—O1	108.8 (6)	C14A—C15A—H15B	107.6
O8—Re2—O8ⁱ	114.6 (12)	H15A—C15A—H15B	107.1
O8—Re2—O6	109.4 (5)	C15A—C16A—H16A	109.5
O8ⁱ—Re2—O6	109.4 (5)	C15A—C16A—H16B	109.5
O8—Re2—O7	107.9 (6)	H16A—C16A—H16B	109.5
O8ⁱ—Re2—O7	107.9 (6)	C15A—C16A—H16C	109.5
O6—Re2—O7	107.5 (7)	H16A—C16A—H16C	109.5
O11ⁱ—Re3—O11	106.4 (13)	H16B—C16A—H16C	109.5
O11ⁱ—Re3—O10	112.6 (6)	C14B—C13B—P2	136 (3)
O11—Re3—O10	112.6 (6)	C14B—C13B—H13C	103.1
O11ⁱ—Re3—O12	107.9 (5)	P2—C13B—H13C	103.1
O11—Re3—O12	107.9 (5)	C14B—C13B—H13D	103.1
O10—Re3—O12	109.3 (8)	P2—C13B—H13D	103.1
O5—P1—C9	110.3 (6)	H13C—C13B—H13D	105.1
O5—P1—C5	110.5 (6)	C13B—C14B—C15B	111 (2)
C9—P1—C5	108.0 (7)	C13B—C14B—H14C	109.5
O5—P1—C1	112.8 (8)	C15B—C14B—H14C	109.5
C9—P1—C1	101.8 (7)	C13B—C14B—H14D	109.5
C5—P1—C1	113.0 (8)	C15B—C14B—H14D	109.5
O9—P2—C17	112.1 (9)	H14C—C14B—H14D	108.1
O9—P2—C13A	115.6 (11)	C16B—C15B—C14B	112 (2)
C17—P2—C13A	117.3 (13)	C16B—C15B—H15C	109.1
O9—P2—C13Aⁱ	115.6 (11)	C14B—C15B—H15C	109.1
C17—P2—C13Aⁱ	117.3 (13)	C16B—C15B—H15D	109.1
C13A—P2—C13Aⁱ	74 (2)	C14B—C15B—H15D	109.1
O9—P2—C13Bⁱ	111.4 (13)	H15C—C15B—H15D	107.9
C17—P2—C13Bⁱ	94.3 (17)	C15B—C16B—H16D	109.5
C13A—P2—C13Bⁱ	103.3 (19)	C15B—C16B—H16E	109.5
C13Aⁱ—P2—C13Bⁱ	31.2 (15)	H16D—C16B—H16E	109.5
O9—P2—C13B	111.4 (13)	C15B—C16B—H16F	109.5
C17—P2—C13B	94.3 (17)	H16D—C16B—H16F	109.5
C13A—P2—C13B	31.2 (15)	H16E—C16B—H16F	109.5
C13Aⁱ—P2—C13B	103.3 (19)	C18—C17—P2	118.5 (16)
C13Bⁱ—P2—C13B	129 (3)	C18—C17—H17A	107.7
O13—P3—C21	105.8 (6)	P2—C17—H17A	107.7
O13—P3—C21ⁱ	105.8 (6)	C18—C17—H17B	107.7
C21—P3—C21ⁱ	115.6 (16)	P2—C17—H17B	107.7
O13—P3—C25	116.1 (15)	H17A—C17—H17B	107.1
C21—P3—C25	90.3 (17)	C17—C18—C19	111.2 (15)
C21ⁱ—P3—C25	122 (2)	C17—C18—H18A	109.4
O13—P3—C25ⁱ	116.1 (15)	C19—C18—H18A	109.4
C21—P3—C25ⁱ	122 (2)	C17—C18—H18B	109.4
C21ⁱ—P3—C25ⁱ	90.3 (17)	C19—C18—H18B	109.4
C25—P3—C25ⁱ	36 (4)	H18A—C18—H18B	108.0
Re1—O1—Th1	152.1 (6)	C20—C19—C18	107.0 (16)
P1—O5—Th1	164.2 (7)	C20—C19—H19A	110.3
Re2—O6—Th1	154.7 (7)	C18—C19—H19A	110.3
P2—O9—Th1	158.5 (11)	C20—C19—H19B	110.3
Re3—O10—Th1	149.9 (8)	C18—C19—H19B	110.3
P3—O13—Th1	169.0 (11)	H19A—C19—H19B	108.6
C2—C1—P1	113.3 (11)	C19—C20—H20A	109.5
C2—C1—H1A	108.9	C19—C20—H20B	109.5
P1—C1—H1A	108.9	H20A—C20—H20B	109.5
C2—C1—H1B	108.9	C19—C20—H20C	109.5
P1—C1—H1B	108.9	H20A—C20—H20C	109.5
H1A—C1—H1B	107.7	H20B—C20—H20C	109.5
C1—C2—C3	113.5 (14)	C22—C21—P3	116.4 (12)
C1—C2—H2A	108.9	C22—C21—H21A	108.2
C3—C2—H2A	108.9	P3—C21—H21A	108.2
C1—C2—H2B	108.9	C22—C21—H21B	108.2
C3—C2—H2B	108.9	P3—C21—H21B	108.2
H2A—C2—H2B	107.7	H21A—C21—H21B	107.3
C4—C3—C2	111.9 (15)	C21—C22—C23	112.3 (12)
C4—C3—H3A	109.2	C21—C22—H22A	109.1
C2—C3—H3A	109.2	C23—C22—H22A	109.1
C4—C3—H3B	109.2	C21—C22—H22B	109.1
C2—C3—H3B	109.2	C23—C22—H22B	109.1
H3A—C3—H3B	107.9	H22A—C22—H22B	107.9
C3—C4—H4A	109.5	C24—C23—C22	114.1 (13)
C3—C4—H4B	109.5	C24—C23—H23A	108.7
H4A—C4—H4B	109.5	C22—C23—H23A	108.7
C3—C4—H4C	109.5	C24—C23—H23B	108.7
H4A—C4—H4C	109.5	C22—C23—H23B	108.7
H4B—C4—H4C	109.5	H23A—C23—H23B	107.6
C6—C5—P1	119.3 (10)	C23—C24—H24A	109.5
C6—C5—H5A	107.5	C23—C24—H24B	109.5
P1—C5—H5A	107.5	H24A—C24—H24B	109.5
C6—C5—H5B	107.5	C23—C24—H24C	109.5
P1—C5—H5B	107.5	H24A—C24—H24C	109.5
H5A—C5—H5B	107.0	H24B—C24—H24C	109.5
C7—C6—C5	114.7 (11)	C26—C25—P3	119 (3)
C7—C6—H6A	108.6	C26—C25—H25A	107.6
C5—C6—H6A	108.6	P3—C25—H25A	107.6
C7—C6—H6B	108.6	C26—C25—H25B	107.6
C5—C6—H6B	108.6	P3—C25—H25B	107.6
H6A—C6—H6B	107.6	H25A—C25—H25B	107.0
C6—C7—C8	115.5 (12)	C25—C26—C27	117 (2)
C6—C7—H7A	108.4	C25—C26—H26A	108.2
C8—C7—H7A	108.4	C27—C26—H26A	108.2
C6—C7—H7B	108.4	C25—C26—H26B	108.2
C8—C7—H7B	108.4	C27—C26—H26B	108.2
H7A—C7—H7B	107.5	H26A—C26—H26B	107.3
C7—C8—H8A	109.5	C26—C27—C28	118 (2)
C7—C8—H8B	109.5	C26—C27—H27A	107.9
H8A—C8—H8B	109.5	C28—C27—H27A	107.9
C7—C8—H8C	109.5	C26—C27—H27B	107.9
H8A—C8—H8C	109.5	C28—C27—H27B	107.9
H8B—C8—H8C	109.5	H27A—C27—H27B	107.2
C10—C9—P1	116.6 (10)	C27—C28—H28A	109.5
C10—C9—H9A	108.1	C27—C28—H28B	109.5
P1—C9—H9A	108.1	H28A—C28—H28B	109.5
C10—C9—H9B	108.1	C27—C28—H28C	109.5
P1—C9—H9B	108.1	H28A—C28—H28C	109.5
H9A—C9—H9B	107.3	H28B—C28—H28C	109.5
C11—C10—C9	115.8 (13)

O2—Re1—O1—Th1	−55.5 (14)	O9—Th1—O13—P3	0.000 (6)
O4—Re1—O1—Th1	66.3 (13)	O5ⁱ—Th1—O13—P3	110.6 (3)
O3—Re1—O1—Th1	−174.6 (11)	O5—Th1—O13—P3	−110.6 (3)
O9—Th1—O1—Re1	113.3 (13)	O6—Th1—O13—P3	180.000 (4)
O13—Th1—O1—Re1	−96.1 (13)	O1ⁱ—Th1—O13—P3	41.8 (3)
O5ⁱ—Th1—O1—Re1	−167.7 (9)	O1—Th1—O13—P3	−41.8 (3)
O5—Th1—O1—Re1	5.7 (11)	O10—Th1—O13—P3	180.000 (6)
O6—Th1—O1—Re1	62.9 (13)	O5—P1—C1—C2	−66.2 (17)
O1ⁱ—Th1—O1—Re1	−172.1 (10)	C9—P1—C1—C2	175.6 (15)
O10—Th1—O1—Re1	−41.0 (14)	C5—P1—C1—C2	60.0 (17)
C9—P1—O5—Th1	171 (2)	P1—C1—C2—C3	175.3 (13)
C5—P1—O5—Th1	−70 (3)	C1—C2—C3—C4	65 (2)
C1—P1—O5—Th1	58 (3)	O5—P1—C5—C6	179.1 (12)
O9—Th1—O5—P1	76 (3)	C9—P1—C5—C6	−60.2 (15)
O13—Th1—O5—P1	−146 (2)	C1—P1—C5—C6	51.6 (15)
O5ⁱ—Th1—O5—P1	−42 (3)	P1—C5—C6—C7	−176.3 (13)
O6—Th1—O5—P1	9 (2)	C5—C6—C7—C8	−178.0 (16)
O1ⁱ—Th1—O5—P1	148 (2)	O5—P1—C9—C10	−55.3 (14)
O1—Th1—O5—P1	143 (3)	C5—P1—C9—C10	−176.1 (12)
O10—Th1—O5—P1	−74 (3)	C1—P1—C9—C10	64.7 (14)
O8—Re2—O6—Th1	−63.1 (6)	P1—C9—C10—C11	179.7 (12)
O8ⁱ—Re2—O6—Th1	63.1 (6)	C9—C10—C11—C12	66 (2)
O7—Re2—O6—Th1	180.000 (4)	O9—P2—C13A—C14A	−53 (3)
O9—Th1—O6—Re2	0.000 (1)	C17—P2—C13A—C14A	83 (2)
O13—Th1—O6—Re2	180.0	C13Aⁱ—P2—C13A—C14A	−164.0 (18)
O5ⁱ—Th1—O6—Re2	−106.2 (3)	C13Bⁱ—P2—C13A—C14A	−175 (3)
O5—Th1—O6—Re2	106.2 (3)	C13B—P2—C13A—C14A	37 (3)
O1ⁱ—Th1—O6—Re2	−51.0 (4)	P2—C13A—C14A—C15A	−179 (3)
O1—Th1—O6—Re2	51.0 (4)	C13A—C14A—C15A—C16A	40 (5)
O10—Th1—O6—Re2	180.000 (2)	O9—P2—C13B—C14B	−20 (5)
C17—P2—O9—Th1	0.000 (6)	C17—P2—C13B—C14B	95 (5)
C13A—P2—O9—Th1	138.2 (12)	C13A—P2—C13B—C14B	−125 (7)
C13Aⁱ—P2—O9—Th1	−138.2 (12)	C13Aⁱ—P2—C13B—C14B	−145 (5)
C13Bⁱ—P2—O9—Th1	−104.3 (17)	C13Bⁱ—P2—C13B—C14B	−166 (3)
C13B—P2—O9—Th1	104.3 (17)	P2—C13B—C14B—C15B	133 (5)
O13—Th1—O9—P2	0.000 (5)	C13B—C14B—C15B—C16B	56 (5)
O5ⁱ—Th1—O9—P2	−108.8 (3)	O9—P2—C17—C18	180.000 (2)
O5—Th1—O9—P2	108.8 (3)	C13A—P2—C17—C18	42.6 (10)
O6—Th1—O9—P2	180.000 (4)	C13Aⁱ—P2—C17—C18	−42.6 (10)
O1ⁱ—Th1—O9—P2	−42.2 (3)	C13Bⁱ—P2—C17—C18	−64.8 (13)
O1—Th1—O9—P2	42.2 (3)	C13B—P2—C17—C18	64.8 (13)
O10—Th1—O9—P2	180.000 (2)	P2—C17—C18—C19	180.000 (3)
O11ⁱ—Re3—O10—Th1	−60.2 (7)	C17—C18—C19—C20	180.000 (2)
O11—Re3—O10—Th1	60.2 (7)	O13—P3—C21—C22	174.0 (18)
O12—Re3—O10—Th1	180.000 (2)	C21ⁱ—P3—C21—C22	−69 (2)
O9—Th1—O10—Re3	180.0	C25—P3—C21—C22	57 (2)
O13—Th1—O10—Re3	0.000 (2)	C25ⁱ—P3—C21—C22	38 (2)
O5ⁱ—Th1—O10—Re3	101.2 (3)	P3—C21—C22—C23	−177.1 (17)
O5—Th1—O10—Re3	−101.2 (3)	C21—C22—C23—C24	178 (2)
O6—Th1—O10—Re3	180.000 (2)	O13—P3—C25—C26	48 (5)
O1ⁱ—Th1—O10—Re3	54.6 (4)	C21—P3—C25—C26	156 (4)
O1—Th1—O10—Re3	−54.6 (4)	C21ⁱ—P3—C25—C26	−83 (4)
C21—P3—O13—Th1	−118.4 (8)	C25ⁱ—P3—C25—C26	−51 (4)
C21ⁱ—P3—O13—Th1	118.4 (8)	P3—C25—C26—C27	154 (2)
C25—P3—O13—Th1	−20 (2)	C25—C26—C27—C28	155 (3)
C25ⁱ—P3—O13—Th1	20 (2)

Symmetry code: (i) −x, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.97	2.63	3.476 (19)	146
C2—H2A···O10	0.97	2.90	3.63 (2)	133
C3—H3B···O12	0.97	2.75	3.62 (2)	149
C5—H5B···O8	0.97	2.54	3.49 (2)	168
C5—H5A···O2	0.97	2.63	3.492 (19)	148
C9—H9A···O2	0.97	2.84	3.65 (2)	141
C9—H9A···O4	0.97	3.02	3.663 (19)	125
C10—H10A···O11	0.97	3.11	3.65 (2)	117
C10—H10B···O4	0.97	2.97	3.55 (2)	120
C10—H10B···O5	0.97	2.87	3.220 (17)	102
C14A—H14A···O9	0.97	2.84	3.22 (3)	104
C14A—H14A···O9	0.97	2.84	3.22 (3)	104
C17—H17A···O1	0.97	2.74	3.41 (2)	127
C17—H17A···O3	0.97	2.95	3.915 (19)	174
C26—H26A···O1	0.97	2.94	3.55 (3)	122
C4—H4A···O2ⁱⁱ	0.96	3.01	3.90 (3)	154
C6—H6A···O4ⁱⁱ	0.97	2.90	3.587 (19)	129
C6—H6B···O3ⁱⁱ	0.97	2.80	3.565 (18)	136
C8—H8C···O4ⁱⁱ	0.96	2.71	3.58 (2)	151
C9—H9B···O3ⁱⁱ	0.97	2.77	3.731 (18)	172
C12—H12A···O3ⁱⁱ	0.96	2.96	3.73 (2)	138
C13A—H13B···O7ⁱⁱⁱ	0.97	2.73	3.46 (3)	133
C13A—H13B···O7ⁱⁱⁱ	0.97	2.73	3.46 (3)	133
C13B—H13C···O7ⁱⁱⁱ	0.97	3.41	4.09 (4)	129
C13A—H13B···O7^iv	0.97	2.73	3.46 (3)	133
C13A—H13B···O7^iv	0.97	2.73	3.46 (3)	133
C13A—H13B···O7^iv	0.97	2.73	3.46 (3)	133
C13B—H13C···O7^iv	0.97	3.41	4.09 (4)	129
C18—H18B···O8ⁱⁱⁱ	0.97	3.03	3.80 (2)	137
C18—H18A···O8^iv	0.97	3.03	3.80 (2)	137
C17—H17B···O1ⁱ	0.97	2.74	3.41 (2)	127
C17—H17B···O3ⁱ	0.97	2.95	3.915 (19)	174
C13A—H13A···O8ⁱ	0.97	3.20	3.75 (3)	118
C14A—H14A···O8ⁱ	0.97	2.85	3.55 (4)	130
C21—H21B···O4ⁱ	0.97	2.69	3.62 (3)	161
C21—H21A···O11ⁱ	0.97	2.64	3.53 (2)	152
C25—H25B···O4ⁱ	0.97	2.89	3.74 (6)	147
C26—H26B···O1ⁱ	0.97	2.75	3.55 (3)	140
C26—H26B···O3ⁱ	0.97	3.06	3.93 (2)	150
C14A—H14B···O2ⁱ	0.97	2.94	3.57 (3)	124
C20—H20A···O7^v	0.96	2.62	3.37 (3)	135
C28—H28A···O12^v	0.96	2.97	3.92 (4)	170
C20—H20A···O7^vi	0.96	2.62	3.37 (3)	135
C28—H28A···O12^vi	0.96	2.97	3.92 (4)	170
C22—H22B···O11^vii	0.97	2.98	3.702 (19)	133
C22—H22A···O12^vii	0.97	2.75	3.49 (2)	134
C24—H24C···O11^vii	0.96	3.04	3.79 (3)	137
C22—H22A···O12^viii	0.97	2.75	3.49 (2)	134
C16B—H16D···O7ⁱⁱⁱ	0.96	3.57	4.22 (6)	127
C16A—H16A···O7ⁱⁱⁱ	0.96	3.25	3.77 (4)	116
C16A—H16C···O8ⁱⁱⁱ	0.96	3.02	3.89 (4)	151

Symmetry codes: (i) −x, y, z; (ii) −x+1/2, −y+1/2, z+1/2; (iii) −x, −y+1, z−1/2; (iv) x, −y+1, z−1/2; (v) x, y, z−1; (vi) −x, y, z−1; (vii) −x, −y, z−1/2; (viii) x, −y, z−1/2.

(IIat165) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	D_x = 2.018 Mg m⁻³
M_r = 2106.06	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 5437 reflections
a = 21.610 (3) Å	θ = 2.7–25.9°
b = 21.623 (3) Å	µ = 9.25 mm⁻¹
c = 14.8324 (19) Å	T = 165 K
V = 6930.7 (15) Å³	Plate, colourless
Z = 4	0.18 × 0.18 × 0.10 mm
F(000) = 4024

Data collection top

CCD area detector diffractometer	6458 independent reflections
Radiation source: fine-focus sealed tube	6367 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.036
phi and ω scans	θ_max = 25.0°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→25
T_min = 0.689, T_max = 1.000	k = −25→25
24808 measured reflections	l = −17→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.026	H-atom parameters constrained
wR(F²) = 0.054	w = 1/[σ²(F_o²) + (0.0201P)² + 25.4516P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.002
6458 reflections	Δρ_max = 1.10 e Å⁻³
372 parameters	Δρ_min = −1.05 e Å⁻³
312 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.011 (11)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	V = 6930.7 (15) Å³
M_r = 2106.06	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.610 (3) Å	µ = 9.25 mm⁻¹
b = 21.623 (3) Å	T = 165 K
c = 14.8324 (19) Å	0.18 × 0.18 × 0.10 mm

Data collection top

CCD area detector diffractometer	6458 independent reflections
Absorption correction: multi-scan SADABS	6367 reflections with I > 2σ(I)
T_min = 0.689, T_max = 1.000	R_int = 0.036
24808 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	H-atom parameters constrained
wR(F²) = 0.054	w = 1/[σ²(F_o²) + (0.0201P)² + 25.4516P] where P = (F_o² + 2F_c²)/3
S = 1.06	Δρ_max = 1.10 e Å⁻³
6458 reflections	Δρ_min = −1.05 e Å⁻³
372 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
312 restraints	Absolute structure parameter: 0.011 (11)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.0000	0.25246 (2)	0.29706 (4)	0.01592 (10)
Re1	0.14655 (2)	0.23822 (2)	0.12481 (3)	0.02848 (10)
Re2	0.0000	0.41190 (3)	0.44636 (4)	0.02472 (14)
Re3	0.0000	0.12233 (3)	0.49449 (4)	0.02571 (13)
P1	0.16001 (12)	0.26172 (13)	0.40944 (17)	0.0265 (6)
P2	0.0000	0.3913 (2)	0.1447 (3)	0.0516 (14)
P3	0.0000	0.0881 (2)	0.2060 (3)	0.0367 (9)
O1	0.0714 (4)	0.2460 (4)	0.1674 (5)	0.0418 (15)
O2	0.1926 (4)	0.2919 (4)	0.1705 (6)	0.055 (2)
O3	0.1449 (4)	0.2481 (3)	0.0109 (5)	0.049 (2)
O4	0.1747 (5)	0.1667 (4)	0.1488 (5)	0.060 (2)
O5	0.1020 (3)	0.2510 (3)	0.3525 (5)	0.0341 (13)
O6	0.0000	0.3355 (4)	0.4091 (6)	0.0286 (18)
O7	0.0000	0.4137 (5)	0.5642 (7)	0.073 (4)
O8	0.0648 (4)	0.4488 (4)	0.4111 (7)	0.061 (2)
O9	0.0000	0.3465 (5)	0.2228 (8)	0.048 (2)
O10	0.0000	0.1926 (4)	0.4383 (7)	0.0338 (18)
O11	0.0625 (6)	0.0812 (5)	0.4691 (6)	0.080 (4)
O12	0.0000	0.1346 (5)	0.6075 (6)	0.048 (3)
O13	0.0000	0.1498 (5)	0.2513 (7)	0.041 (2)
C1	0.1464 (5)	0.2455 (5)	0.5267 (6)	0.033 (2)
H1A	0.1308	0.2026	0.5319	0.040*
H1B	0.1865	0.2474	0.5588	0.040*
C2	0.1015 (5)	0.2878 (5)	0.5740 (7)	0.041 (2)
H2A	0.0619	0.2882	0.5404	0.049*
H2B	0.1183	0.3304	0.5736	0.049*
C3	0.0891 (5)	0.2679 (6)	0.6723 (7)	0.041 (2)
H3A	0.0559	0.2942	0.6975	0.049*
H3B	0.0742	0.2246	0.6726	0.049*
C4	0.1451 (6)	0.2727 (6)	0.7315 (8)	0.053 (3)
H4A	0.1768	0.2438	0.7103	0.080*
H4B	0.1337	0.2624	0.7937	0.080*
H4C	0.1614	0.3150	0.7293	0.080*
C5	0.1857 (5)	0.3387 (5)	0.3945 (7)	0.0326 (19)
H5A	0.1949	0.3445	0.3297	0.039*
H5B	0.1507	0.3665	0.4094	0.039*
C6	0.2417 (5)	0.3606 (4)	0.4477 (8)	0.0372 (19)
H6A	0.2337	0.3543	0.5128	0.045*
H6B	0.2779	0.3349	0.4311	0.045*
C7	0.2573 (5)	0.4270 (5)	0.4320 (9)	0.045 (3)
H7A	0.2217	0.4527	0.4510	0.054*
H7B	0.2635	0.4335	0.3666	0.054*
C8	0.3148 (7)	0.4488 (6)	0.4820 (9)	0.061 (4)
H8A	0.3143	0.4940	0.4866	0.091*
H8B	0.3518	0.4357	0.4490	0.091*
H8C	0.3153	0.4308	0.5427	0.091*
C9	0.2198 (4)	0.2096 (4)	0.3750 (6)	0.0251 (16)
H9A	0.2311	0.2189	0.3118	0.030*
H9B	0.2569	0.2171	0.4127	0.030*
C10	0.2025 (5)	0.1420 (4)	0.3817 (8)	0.033 (2)
H10A	0.1655	0.1345	0.3441	0.040*
H10B	0.1914	0.1325	0.4450	0.040*
C11	0.2538 (5)	0.0982 (5)	0.3520 (8)	0.039 (2)
H11A	0.2369	0.0557	0.3480	0.047*
H11B	0.2681	0.1103	0.2911	0.047*
C12	0.3073 (6)	0.0984 (6)	0.4148 (9)	0.052 (3)
H12A	0.3308	0.1368	0.4071	0.078*
H12B	0.3342	0.0630	0.4016	0.078*
H12C	0.2924	0.0955	0.4770	0.078*
C13A	−0.0500 (8)	0.4539 (8)	0.1609 (14)	0.048 (5)*	0.620 (18)
H13A	−0.0307	0.4826	0.2046	0.058*	0.620 (18)
H13B	−0.0540	0.4764	0.1030	0.058*	0.620 (18)
C14A	−0.1124 (9)	0.4384 (10)	0.1933 (17)	0.065 (4)*	0.620 (18)
H14A	−0.1072	0.4248	0.2566	0.078*	0.620 (18)
H14B	−0.1253	0.4013	0.1589	0.078*	0.620 (18)
C15A	−0.1675 (12)	0.4814 (12)	0.1930 (19)	0.068 (5)*	0.620 (18)
H15A	−0.1765	0.4942	0.2558	0.081*	0.620 (18)
H15B	−0.2041	0.4586	0.1702	0.081*	0.620 (18)
C16A	−0.1578 (11)	0.5391 (9)	0.1352 (16)	0.054 (6)*	0.620 (18)
H16A	−0.1300	0.5677	0.1666	0.081*	0.620 (18)
H16B	−0.1977	0.5594	0.1247	0.081*	0.620 (18)
H16C	−0.1394	0.5273	0.0773	0.081*	0.620 (18)
C13B	−0.0777 (9)	0.4265 (13)	0.126 (2)	0.045 (5)*	0.380 (18)
H13C	−0.0693	0.4708	0.1376	0.053*	0.380 (18)
H13D	−0.0819	0.4236	0.0596	0.053*	0.380 (18)
C14B	−0.1432 (13)	0.4205 (14)	0.156 (3)	0.075 (6)*	0.380 (18)
H14C	−0.1478	0.3833	0.1945	0.090*	0.380 (18)
H14D	−0.1707	0.4159	0.1032	0.090*	0.380 (18)
C15B	−0.161 (2)	0.4783 (18)	0.210 (2)	0.070 (6)*	0.380 (18)
H15C	−0.1941	0.4674	0.2540	0.084*	0.380 (18)
H15D	−0.1251	0.4936	0.2439	0.084*	0.380 (18)
C16B	−0.185 (2)	0.5295 (16)	0.147 (3)	0.061 (9)*	0.380 (18)
H16D	−0.1593	0.5664	0.1542	0.092*	0.380 (18)
H16E	−0.2281	0.5396	0.1632	0.092*	0.380 (18)
H16F	−0.1835	0.5152	0.0847	0.092*	0.380 (18)
C17	0.0000	0.3536 (8)	0.0387 (9)	0.050 (4)
H17A	0.0369	0.3266	0.0354	0.060*	0.50
H17B	−0.0369	0.3266	0.0354	0.060*	0.50
C18	0.0000	0.3958 (7)	−0.0433 (9)	0.049 (3)
H18A	0.0370	0.4227	−0.0412	0.059*	0.50
H18B	−0.0370	0.4227	−0.0412	0.059*	0.50
C19	0.0000	0.3595 (8)	−0.1320 (9)	0.059 (4)
H19A	−0.0371	0.3327	−0.1350	0.070*	0.50
H19B	0.0371	0.3327	−0.1350	0.070*	0.50
C20	0.0000	0.4052 (9)	−0.2130 (11)	0.070 (6)
H20A	0.0000	0.3818	−0.2696	0.105*
H20B	0.0370	0.4313	−0.2102	0.105*	0.50
H20C	−0.0370	0.4313	−0.2102	0.105*	0.50
C21	−0.0693 (6)	0.0481 (6)	0.2398 (11)	0.071 (4)
H21A	−0.0656	0.0382	0.3047	0.085*
H21B	−0.1045	0.0770	0.2331	0.085*
C22	−0.0854 (5)	−0.0111 (6)	0.1901 (10)	0.066 (3)
H22A	−0.0888	−0.0024	0.1248	0.079*
H22B	−0.0518	−0.0416	0.1987	0.079*
C23	−0.1459 (5)	−0.0386 (6)	0.2234 (10)	0.069 (3)
H23A	−0.1793	−0.0077	0.2156	0.083*
H23B	−0.1422	−0.0476	0.2886	0.083*
C24	−0.1637 (7)	−0.0978 (6)	0.1738 (11)	0.081 (5)
H24A	−0.2063	−0.1090	0.1891	0.121*
H24B	−0.1357	−0.1313	0.1918	0.121*
H24C	−0.1604	−0.0911	0.1086	0.121*
C25	−0.0248 (12)	0.0913 (11)	0.0907 (14)	0.059 (5)*	0.50
H25A	−0.0160	0.0504	0.0636	0.071*	0.50
H25B	−0.0704	0.0962	0.0911	0.071*	0.50
C26	0.0000	0.1382 (9)	0.0293 (10)	0.073 (4)
H26A	0.0432	0.1467	0.0475	0.088*	0.50
H26B	−0.0238	0.1768	0.0387	0.088*	0.50
C27	0.0000	0.1245 (9)	−0.0699 (10)	0.080 (5)
H27A	−0.0369	0.0989	−0.0832	0.096*	0.50
H27B	0.0369	0.0989	−0.0832	0.096*	0.50
C28	0.0000	0.1783 (12)	−0.1343 (16)	0.137 (9)
H28A	0.0000	0.1628	−0.1964	0.205*
H28B	0.0370	0.2035	−0.1242	0.205*	0.50
H28C	−0.0370	0.2035	−0.1242	0.205*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0163 (3)	0.0180 (3)	0.0135 (2)	0.000	0.000	−0.00064 (18)
Re1	0.0256 (2)	0.0351 (2)	0.0248 (2)	0.00541 (19)	0.0070 (2)	0.0015 (2)
Re2	0.0344 (4)	0.0228 (3)	0.0169 (3)	0.000	0.000	−0.0026 (3)
Re3	0.0324 (4)	0.0258 (3)	0.0190 (3)	0.000	0.000	0.0055 (3)
P1	0.0187 (13)	0.0355 (14)	0.0253 (12)	−0.0003 (11)	−0.0046 (10)	−0.0010 (11)
P2	0.108 (4)	0.023 (2)	0.024 (2)	0.000	0.000	0.0067 (14)
P3	0.052 (3)	0.0227 (18)	0.036 (2)	0.000	0.000	−0.0086 (16)
O1	0.029 (3)	0.074 (4)	0.023 (2)	−0.010 (3)	0.008 (2)	−0.010 (3)
O2	0.035 (4)	0.058 (4)	0.071 (5)	−0.012 (4)	0.008 (4)	−0.006 (4)
O3	0.055 (5)	0.064 (6)	0.027 (2)	0.018 (4)	0.020 (3)	0.011 (3)
O4	0.098 (6)	0.046 (3)	0.037 (4)	0.027 (4)	−0.006 (4)	0.000 (3)
O5	0.018 (2)	0.056 (4)	0.029 (3)	0.0008 (19)	−0.005 (2)	−0.005 (3)
O6	0.047 (5)	0.021 (2)	0.018 (3)	0.000	0.000	0.000 (2)
O7	0.162 (14)	0.036 (7)	0.022 (3)	0.000	0.000	−0.008 (4)
O8	0.049 (5)	0.041 (4)	0.092 (6)	−0.015 (3)	0.018 (4)	−0.011 (5)
O9	0.092 (6)	0.029 (3)	0.022 (3)	0.000	0.000	0.011 (3)
O10	0.050 (5)	0.025 (3)	0.026 (3)	0.000	0.000	0.008 (3)
O11	0.100 (7)	0.081 (6)	0.058 (6)	0.059 (5)	0.045 (5)	0.039 (4)
O12	0.083 (8)	0.042 (6)	0.019 (2)	0.000	0.000	0.003 (3)
O13	0.061 (5)	0.024 (2)	0.038 (4)	0.000	0.000	−0.012 (3)
C1	0.035 (5)	0.041 (5)	0.023 (2)	−0.008 (4)	−0.004 (3)	−0.003 (3)
C2	0.039 (5)	0.053 (6)	0.030 (3)	−0.005 (4)	0.000 (3)	−0.009 (4)
C3	0.037 (5)	0.048 (6)	0.038 (4)	−0.006 (5)	0.011 (4)	−0.001 (4)
C4	0.070 (8)	0.049 (7)	0.040 (5)	−0.018 (7)	−0.013 (5)	−0.002 (5)
C5	0.023 (5)	0.037 (3)	0.038 (5)	0.001 (3)	−0.007 (4)	0.006 (4)
C6	0.031 (5)	0.032 (4)	0.048 (5)	−0.003 (3)	−0.008 (4)	−0.005 (4)
C7	0.043 (6)	0.034 (4)	0.057 (6)	−0.006 (4)	−0.008 (5)	−0.003 (5)
C8	0.061 (9)	0.047 (6)	0.075 (9)	−0.031 (5)	−0.026 (6)	0.024 (6)
C9	0.017 (3)	0.034 (3)	0.025 (4)	−0.003 (3)	−0.005 (3)	0.008 (4)
C10	0.032 (4)	0.030 (3)	0.038 (5)	−0.006 (3)	−0.009 (4)	−0.004 (4)
C11	0.032 (5)	0.032 (4)	0.053 (6)	−0.008 (4)	−0.002 (4)	−0.005 (5)
C12	0.055 (7)	0.042 (7)	0.058 (7)	0.021 (6)	−0.018 (5)	0.002 (6)
C17	0.083 (10)	0.047 (7)	0.021 (3)	0.000	0.000	0.005 (3)
C18	0.082 (9)	0.041 (7)	0.025 (3)	0.000	0.000	0.006 (4)
C19	0.104 (11)	0.051 (8)	0.021 (3)	0.000	0.000	0.008 (5)
C20	0.128 (16)	0.058 (10)	0.024 (4)	0.000	0.000	0.012 (7)
C21	0.038 (6)	0.066 (6)	0.108 (9)	−0.014 (4)	0.021 (6)	−0.059 (6)
C22	0.030 (5)	0.062 (6)	0.105 (8)	−0.014 (4)	0.020 (5)	−0.054 (6)
C23	0.032 (6)	0.062 (7)	0.113 (8)	−0.009 (4)	0.033 (6)	−0.051 (6)
C24	0.040 (8)	0.060 (8)	0.142 (12)	−0.019 (5)	0.016 (8)	−0.045 (8)
C26	0.101 (9)	0.065 (8)	0.053 (5)	0.000	0.000	0.018 (6)
C27	0.121 (11)	0.068 (9)	0.051 (6)	0.000	0.000	0.021 (7)
C28	0.23 (2)	0.102 (15)	0.075 (9)	0.000	0.000	0.051 (11)

Geometric parameters (Å, º) top

Th1—O9	2.313 (11)	C11—H11A	0.9900
Th1—O13	2.321 (10)	C11—H11B	0.9900
Th1—O5ⁱ	2.352 (7)	C12—H12A	0.9800
Th1—O5	2.352 (7)	C12—H12B	0.9800
Th1—O6	2.446 (10)	C12—H12C	0.9800
Th1—O10	2.463 (10)	C13A—C14A	1.471 (17)
Th1—O1ⁱ	2.470 (8)	C13A—H13A	0.9900
Th1—O1	2.470 (8)	C13A—H13B	0.9900
Re1—O2	1.672 (9)	C14A—C15A	1.510 (17)
Re1—O4	1.700 (8)	C14A—H14A	0.9900
Re1—O3	1.703 (7)	C14A—H14B	0.9900
Re1—O1	1.750 (8)	C15A—C16A	1.530 (18)
Re2—O8	1.695 (8)	C15A—H15A	0.9900
Re2—O8ⁱ	1.695 (8)	C15A—H15B	0.9900
Re2—O6	1.742 (10)	C16A—H16A	0.9800
Re2—O7	1.748 (11)	C16A—H16B	0.9800
Re3—O11	1.660 (10)	C16A—H16C	0.9800
Re3—O11ⁱ	1.660 (10)	C13B—C14B	1.492 (19)
Re3—O12	1.698 (9)	C13B—H13C	0.9900
Re3—O10	1.733 (10)	C13B—H13D	0.9900
P1—O5	1.530 (8)	C14B—C15B	1.534 (19)
P1—C5	1.769 (10)	C14B—H14C	0.9900
P1—C9	1.789 (10)	C14B—H14D	0.9900
P1—C1	1.798 (10)	C15B—C16B	1.533 (19)
P2—O9	1.510 (11)	C15B—H15C	0.9900
P2—C13A	1.749 (14)	C15B—H15D	0.9900
P2—C13Aⁱ	1.749 (14)	C16B—H16D	0.9800
P2—C17	1.771 (16)	C16B—H16E	0.9800
P2—C13B	1.864 (17)	C16B—H16F	0.9800
P2—C13Bⁱ	1.865 (17)	C17—C18	1.519 (14)
P3—O13	1.494 (11)	C17—H17A	0.9900
P3—C25	1.79 (2)	C17—H17B	0.9900
P3—C25ⁱ	1.79 (2)	C18—C19	1.533 (15)
P3—C21ⁱ	1.801 (13)	C18—H18A	0.9900
P3—C21	1.801 (13)	C18—H18B	0.9900
C1—C2	1.506 (12)	C19—C20	1.556 (15)
C1—H1A	0.9900	C19—H19A	0.9900
C1—H1B	0.9900	C19—H19B	0.9900
C2—C3	1.543 (12)	C20—H20A	0.9800
C2—H2A	0.9900	C20—H20B	0.9800
C2—H2B	0.9900	C20—H20C	0.9800
C3—C4	1.498 (13)	C21—C22	1.519 (12)
C3—H3A	0.9900	C21—H21A	0.9900
C3—H3B	0.9900	C21—H21B	0.9900
C4—H4A	0.9800	C22—C23	1.518 (13)
C4—H4B	0.9800	C22—H22A	0.9900
C4—H4C	0.9800	C22—H22B	0.9900
C5—C6	1.522 (11)	C23—C24	1.526 (13)
C5—H5A	0.9900	C23—H23A	0.9900
C5—H5B	0.9900	C23—H23B	0.9900
C6—C7	1.491 (11)	C24—H24A	0.9800
C6—H6A	0.9900	C24—H24B	0.9800
C6—H6B	0.9900	C24—H24C	0.9800
C7—C8	1.523 (13)	C25—C26	1.464 (16)
C7—H7A	0.9900	C25—H25A	0.9900
C7—H7B	0.9900	C25—H25B	0.9900
C8—H8A	0.9800	C26—C27	1.500 (16)
C8—H8B	0.9800	C26—H26A	0.9900
C8—H8C	0.9800	C26—H26B	0.9900
C9—C10	1.512 (11)	C27—C28	1.504 (16)
C9—H9A	0.9900	C27—H27A	0.9900
C9—H9B	0.9900	C27—H27B	0.9900
C10—C11	1.523 (12)	C28—H28A	0.9800
C10—H10A	0.9900	C28—H28B	0.9800
C10—H10B	0.9900	C28—H28C	0.9800
C11—C12	1.485 (13)

O9—Th1—O13	134.6 (4)	C9—C10—H10A	108.8
O9—Th1—O5ⁱ	100.27 (19)	C11—C10—H10A	108.8
O13—Th1—O5ⁱ	95.12 (19)	C9—C10—H10B	108.8
O9—Th1—O5	100.28 (19)	C11—C10—H10B	108.8
O13—Th1—O5	95.12 (19)	H10A—C10—H10B	107.7
O5ⁱ—Th1—O5	139.0 (4)	C12—C11—C10	112.5 (9)
O9—Th1—O6	71.2 (4)	C12—C11—H11A	109.1
O13—Th1—O6	154.2 (4)	C10—C11—H11A	109.1
O5ⁱ—Th1—O6	76.85 (19)	C12—C11—H11B	109.1
O5—Th1—O6	76.85 (19)	C10—C11—H11B	109.1
O9—Th1—O10	150.1 (4)	H11A—C11—H11B	107.8
O13—Th1—O10	75.3 (4)	C11—C12—H12A	109.5
O5ⁱ—Th1—O10	72.27 (19)	C11—C12—H12B	109.5
O5—Th1—O10	72.27 (19)	H12A—C12—H12B	109.5
O6—Th1—O10	78.9 (3)	C11—C12—H12C	109.5
O9—Th1—O1ⁱ	71.3 (3)	H12A—C12—H12C	109.5
O13—Th1—O1ⁱ	73.6 (3)	H12B—C12—H12C	109.5
O5ⁱ—Th1—O1ⁱ	71.7 (3)	C14A—C13A—P2	115.7 (13)
O5—Th1—O1ⁱ	148.9 (3)	C14A—C13A—H13A	108.3
O6—Th1—O1ⁱ	124.8 (2)	P2—C13A—H13A	108.3
O10—Th1—O1ⁱ	129.2 (2)	C14A—C13A—H13B	108.3
O9—Th1—O1	71.3 (3)	P2—C13A—H13B	108.3
O13—Th1—O1	73.6 (3)	H13A—C13A—H13B	107.4
O5ⁱ—Th1—O1	148.9 (3)	C13A—C14A—C15A	125.6 (17)
O5—Th1—O1	71.7 (3)	C13A—C14A—H14A	105.9
O6—Th1—O1	124.8 (2)	C15A—C14A—H14A	105.9
O10—Th1—O1	129.2 (2)	C13A—C14A—H14B	105.9
O1ⁱ—Th1—O1	77.3 (4)	C15A—C14A—H14B	105.9
O2—Re1—O4	109.5 (5)	H14A—C14A—H14B	106.2
O2—Re1—O3	109.1 (4)	C14A—C15A—C16A	113.3 (18)
O4—Re1—O3	109.2 (4)	C14A—C15A—H15A	108.9
O2—Re1—O1	109.9 (4)	C16A—C15A—H15A	108.9
O4—Re1—O1	110.1 (5)	C14A—C15A—H15B	108.9
O3—Re1—O1	109.1 (4)	C16A—C15A—H15B	108.9
O8—Re2—O8ⁱ	111.5 (7)	H15A—C15A—H15B	107.7
O8—Re2—O6	110.4 (3)	C15A—C16A—H16A	109.5
O8ⁱ—Re2—O6	110.4 (3)	C15A—C16A—H16B	109.5
O8—Re2—O7	107.3 (4)	H16A—C16A—H16B	109.5
O8ⁱ—Re2—O7	107.3 (4)	C15A—C16A—H16C	109.5
O6—Re2—O7	109.8 (5)	H16A—C16A—H16C	109.5
O11—Re3—O11ⁱ	108.8 (10)	H16B—C16A—H16C	109.5
O11—Re3—O12	107.9 (4)	C14B—C13B—P2	141 (2)
O11ⁱ—Re3—O12	107.9 (4)	C14B—C13B—H13C	101.8
O11—Re3—O10	111.1 (4)	P2—C13B—H13C	101.8
O11ⁱ—Re3—O10	111.1 (4)	C14B—C13B—H13D	101.8
O12—Re3—O10	109.8 (5)	P2—C13B—H13D	101.8
O5—P1—C5	109.3 (4)	H13C—C13B—H13D	104.7
O5—P1—C9	109.8 (4)	C13B—C14B—C15B	109 (2)
C5—P1—C9	109.3 (5)	C13B—C14B—H14C	109.8
O5—P1—C1	111.7 (5)	C15B—C14B—H14C	109.8
C5—P1—C1	110.9 (5)	C13B—C14B—H14D	109.8
C9—P1—C1	105.7 (5)	C15B—C14B—H14D	109.8
O9—P2—C13A	113.0 (7)	H14C—C14B—H14D	108.3
O9—P2—C13Aⁱ	113.0 (8)	C16B—C15B—C14B	111 (2)
C13A—P2—C13Aⁱ	76.3 (13)	C16B—C15B—H15C	109.4
O9—P2—C17	112.8 (7)	C14B—C15B—H15C	109.4
C13A—P2—C17	118.5 (8)	C16B—C15B—H15D	109.4
C13Aⁱ—P2—C17	118.5 (8)	C14B—C15B—H15D	109.4
O9—P2—C13B	112.1 (9)	H15C—C15B—H15D	108.0
C13A—P2—C13B	31.5 (10)	C15B—C16B—H16D	109.5
C13Aⁱ—P2—C13B	105.1 (13)	C15B—C16B—H16E	109.5
C17—P2—C13B	93.2 (11)	H16D—C16B—H16E	109.5
O9—P2—C13Bⁱ	112.1 (9)	C15B—C16B—H16F	109.5
C13A—P2—C13Bⁱ	105.1 (13)	H16D—C16B—H16F	109.5
C13Aⁱ—P2—C13Bⁱ	31.5 (10)	H16E—C16B—H16F	109.5
C17—P2—C13Bⁱ	93.2 (11)	C18—C17—P2	115.8 (11)
C13B—P2—C13Bⁱ	128.4 (18)	C18—C17—H17A	108.3
O13—P3—C25	113.2 (9)	P2—C17—H17A	108.3
O13—P3—C25ⁱ	113.2 (9)	C18—C17—H17B	108.3
C25—P3—C25ⁱ	34.8 (17)	P2—C17—H17B	108.3
O13—P3—C21ⁱ	107.7 (4)	H17A—C17—H17B	107.4
C25—P3—C21ⁱ	122.2 (11)	C17—C18—C19	112.4 (11)
C25ⁱ—P3—C21ⁱ	92.0 (9)	C17—C18—H18A	109.1
O13—P3—C21	107.7 (4)	C19—C18—H18A	109.1
C25—P3—C21	92.0 (9)	C17—C18—H18B	109.1
C25ⁱ—P3—C21	122.2 (11)	C19—C18—H18B	109.1
C21ⁱ—P3—C21	112.5 (11)	H18A—C18—H18B	107.9
Re1—O1—Th1	150.0 (4)	C18—C19—C20	109.8 (13)
P1—O5—Th1	163.5 (5)	C18—C19—H19A	109.7
Re2—O6—Th1	155.7 (5)	C20—C19—H19A	109.7
P2—O9—Th1	158.3 (8)	C18—C19—H19B	109.7
Re3—O10—Th1	150.4 (6)	C20—C19—H19B	109.7
P3—O13—Th1	170.2 (7)	H19A—C19—H19B	108.2
C2—C1—P1	115.9 (7)	C19—C20—H20A	109.5
C2—C1—H1A	108.3	C19—C20—H20B	109.5
P1—C1—H1A	108.3	H20A—C20—H20B	109.5
C2—C1—H1B	108.3	C19—C20—H20C	109.5
P1—C1—H1B	108.3	H20A—C20—H20C	109.5
H1A—C1—H1B	107.4	H20B—C20—H20C	109.5
C1—C2—C3	112.5 (9)	C22—C21—P3	117.5 (9)
C1—C2—H2A	109.1	C22—C21—H21A	107.9
C3—C2—H2A	109.1	P3—C21—H21A	107.9
C1—C2—H2B	109.1	C22—C21—H21B	107.9
C3—C2—H2B	109.1	P3—C21—H21B	107.9
H2A—C2—H2B	107.8	H21A—C21—H21B	107.2
C4—C3—C2	113.2 (9)	C23—C22—C21	111.7 (10)
C4—C3—H3A	108.9	C23—C22—H22A	109.3
C2—C3—H3A	108.9	C21—C22—H22A	109.3
C4—C3—H3B	108.9	C23—C22—H22B	109.3
C2—C3—H3B	108.9	C21—C22—H22B	109.3
H3A—C3—H3B	107.7	H22A—C22—H22B	107.9
C3—C4—H4A	109.5	C22—C23—C24	112.8 (10)
C3—C4—H4B	109.5	C22—C23—H23A	109.0
H4A—C4—H4B	109.5	C24—C23—H23A	109.0
C3—C4—H4C	109.5	C22—C23—H23B	109.0
H4A—C4—H4C	109.5	C24—C23—H23B	109.0
H4B—C4—H4C	109.5	H23A—C23—H23B	107.8
C6—C5—P1	118.6 (7)	C23—C24—H24A	109.5
C6—C5—H5A	107.7	C23—C24—H24B	109.5
P1—C5—H5A	107.7	H24A—C24—H24B	109.5
C6—C5—H5B	107.7	C23—C24—H24C	109.5
P1—C5—H5B	107.7	H24A—C24—H24C	109.5
H5A—C5—H5B	107.1	H24B—C24—H24C	109.5
C7—C6—C5	113.4 (9)	C26—C25—P3	120.7 (16)
C7—C6—H6A	108.9	C26—C25—H25A	107.2
C5—C6—H6A	108.9	P3—C25—H25A	107.2
C7—C6—H6B	108.9	C26—C25—H25B	107.2
C5—C6—H6B	108.9	P3—C25—H25B	107.2
H6A—C6—H6B	107.7	H25A—C25—H25B	106.8
C6—C7—C8	113.9 (9)	C25—C26—C27	118.3 (16)
C6—C7—H7A	108.8	C25—C26—H26A	107.7
C8—C7—H7A	108.8	C27—C26—H26A	107.7
C6—C7—H7B	108.8	C25—C26—H26B	107.7
C8—C7—H7B	108.8	C27—C26—H26B	107.7
H7A—C7—H7B	107.7	H26A—C26—H26B	107.1
C7—C8—H8A	109.5	C26—C27—C28	118.1 (18)
C7—C8—H8B	109.5	C26—C27—H27A	107.8
H8A—C8—H8B	109.5	C28—C27—H27A	107.8
C7—C8—H8C	109.5	C26—C27—H27B	107.8
H8A—C8—H8C	109.5	C28—C27—H27B	107.8
H8B—C8—H8C	109.5	H27A—C27—H27B	107.1
C10—C9—P1	114.3 (7)	C27—C28—H28A	109.5
C10—C9—H9A	108.7	C27—C28—H28B	109.5
P1—C9—H9A	108.7	H28A—C28—H28B	109.5
C10—C9—H9B	108.7	C27—C28—H28C	109.5
P1—C9—H9B	108.7	H28A—C28—H28C	109.5
H9A—C9—H9B	107.6	H28B—C28—H28C	109.5
C9—C10—C11	113.8 (9)

O2—Re1—O1—Th1	−53.9 (10)	O9—Th1—O13—P3	0.000 (6)
O4—Re1—O1—Th1	66.8 (9)	O5ⁱ—Th1—O13—P3	109.85 (19)
O3—Re1—O1—Th1	−173.4 (8)	O5—Th1—O13—P3	−109.86 (19)
O9—Th1—O1—Re1	113.6 (9)	O6—Th1—O13—P3	180.000 (3)
O13—Th1—O1—Re1	−95.7 (9)	O10—Th1—O13—P3	180.000 (5)
O5ⁱ—Th1—O1—Re1	−167.7 (6)	O1ⁱ—Th1—O13—P3	40.6 (2)
O5—Th1—O1—Re1	5.6 (8)	O1—Th1—O13—P3	−40.6 (2)
O6—Th1—O1—Re1	64.1 (10)	O5—P1—C1—C2	−66.0 (9)
O10—Th1—O1—Re1	−41.3 (10)	C5—P1—C1—C2	56.2 (10)
O1ⁱ—Th1—O1—Re1	−172.1 (7)	C9—P1—C1—C2	174.6 (8)
C5—P1—O5—Th1	−72.6 (17)	P1—C1—C2—C3	176.0 (8)
C9—P1—O5—Th1	167.5 (15)	C1—C2—C3—C4	65.2 (14)
C1—P1—O5—Th1	50.5 (17)	O5—P1—C5—C6	177.7 (8)
O9—Th1—O5—P1	81.4 (17)	C9—P1—C5—C6	−62.0 (10)
O13—Th1—O5—P1	−141.5 (16)	C1—P1—C5—C6	54.1 (10)
O5ⁱ—Th1—O5—P1	−38 (2)	P1—C5—C6—C7	−177.7 (8)
O6—Th1—O5—P1	13.6 (16)	C5—C6—C7—C8	−177.7 (11)
O10—Th1—O5—P1	−68.7 (16)	O5—P1—C9—C10	−58.1 (8)
O1ⁱ—Th1—O5—P1	152.1 (14)	C5—P1—C9—C10	−178.1 (7)
O1—Th1—O5—P1	147.6 (17)	C1—P1—C9—C10	62.6 (9)
O8—Re2—O6—Th1	−61.9 (4)	P1—C9—C10—C11	179.9 (7)
O8ⁱ—Re2—O6—Th1	61.9 (4)	C9—C10—C11—C12	68.6 (13)
O7—Re2—O6—Th1	180.000 (3)	O9—P2—C13A—C14A	−46.8 (19)
O9—Th1—O6—Re2	0.000 (1)	C13Aⁱ—P2—C13A—C14A	−156.3 (14)
O13—Th1—O6—Re2	180.0	C17—P2—C13A—C14A	88.4 (18)
O5ⁱ—Th1—O6—Re2	−105.84 (19)	C13B—P2—C13A—C14A	48 (2)
O5—Th1—O6—Re2	105.84 (19)	C13Bⁱ—P2—C13A—C14A	−169.4 (19)
O10—Th1—O6—Re2	180.000 (2)	P2—C13A—C14A—C15A	−166 (2)
O1ⁱ—Th1—O6—Re2	−49.5 (3)	C13A—C14A—C15A—C16A	14 (4)
O1—Th1—O6—Re2	49.5 (3)	O9—P2—C13B—C14B	−9 (4)
C13A—P2—O9—Th1	137.8 (8)	C13A—P2—C13B—C14B	−108 (5)
C13Aⁱ—P2—O9—Th1	−137.9 (8)	C13Aⁱ—P2—C13B—C14B	−132 (4)
C17—P2—O9—Th1	0.000 (4)	C17—P2—C13B—C14B	107 (4)
C13B—P2—O9—Th1	103.6 (12)	C13Bⁱ—P2—C13B—C14B	−156 (2)
C13Bⁱ—P2—O9—Th1	−103.6 (12)	P2—C13B—C14B—C15B	113 (4)
O13—Th1—O9—P2	0.000 (4)	C13B—C14B—C15B—C16B	87 (4)
O5ⁱ—Th1—O9—P2	−107.8 (2)	O9—P2—C17—C18	180.000 (1)
O5—Th1—O9—P2	107.8 (2)	C13A—P2—C17—C18	44.7 (7)
O6—Th1—O9—P2	180.000 (3)	C13Aⁱ—P2—C17—C18	−44.7 (7)
O10—Th1—O9—P2	180.000 (1)	C13B—P2—C17—C18	64.4 (9)
O1ⁱ—Th1—O9—P2	−41.3 (2)	C13Bⁱ—P2—C17—C18	−64.4 (9)
O1—Th1—O9—P2	41.3 (2)	P2—C17—C18—C19	180.000 (2)
O11—Re3—O10—Th1	60.7 (5)	C17—C18—C19—C20	180.000 (2)
O11ⁱ—Re3—O10—Th1	−60.7 (5)	O13—P3—C21—C22	169.7 (13)
O12—Re3—O10—Th1	180.000 (2)	C25—P3—C21—C22	54.5 (16)
O9—Th1—O10—Re3	180.0	C25ⁱ—P3—C21—C22	36.0 (18)
O13—Th1—O10—Re3	0.000 (1)	C21ⁱ—P3—C21—C22	−71.8 (17)
O5ⁱ—Th1—O10—Re3	100.4 (2)	P3—C21—C22—C23	−178.1 (12)
O5—Th1—O10—Re3	−100.4 (2)	C21—C22—C23—C24	179.3 (15)
O6—Th1—O10—Re3	180.000 (2)	O13—P3—C25—C26	47 (2)
O1ⁱ—Th1—O10—Re3	53.8 (3)	C25ⁱ—P3—C25—C26	−51 (2)
O1—Th1—O10—Re3	−53.8 (3)	C21ⁱ—P3—C25—C26	−84 (2)
C25—P3—O13—Th1	−19.0 (9)	C21—P3—C25—C26	157 (2)
C25ⁱ—P3—O13—Th1	19.0 (9)	P3—C25—C26—C27	154.8 (13)
C21ⁱ—P3—O13—Th1	119.2 (6)	C25—C26—C27—C28	155.4 (14)
C21—P3—O13—Th1	−119.2 (6)

Symmetry code: (i) −x, y, z.

(IIat100) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	D_x = 2.038 Mg m⁻³
M_r = 2106.06	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 8488 reflections
a = 21.535 (3) Å	θ = 2.7–26.5°
b = 21.548 (3) Å	µ = 9.34 mm⁻¹
c = 14.7950 (19) Å	T = 100 K
V = 6865.4 (15) Å³	Block, colourless
Z = 4	0.18 × 0.18 × 0.10 mm
F(000) = 4024

Data collection top

CCD area detector diffractometer	6390 independent reflections
Radiation source: fine-focus sealed tube	6376 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
phi and ω scans	θ_max = 25.0°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→25
T_min = 0.284, T_max = 0.455	k = −25→25
24358 measured reflections	l = −17→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.027	H-atom parameters constrained
wR(F²) = 0.059	w = 1/[σ²(F_o²) + (0.0121P)² + 76.2392P] where P = (F_o² + 2F_c²)/3
S = 1.16	(Δ/σ)_max = 0.002
6390 reflections	Δρ_max = 1.62 e Å⁻³
393 parameters	Δρ_min = −1.34 e Å⁻³
399 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.027 (13)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Re₄Th	V = 6865.4 (15) Å³
M_r = 2106.06	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.535 (3) Å	µ = 9.34 mm⁻¹
b = 21.548 (3) Å	T = 100 K
c = 14.7950 (19) Å	0.18 × 0.18 × 0.10 mm

Data collection top

CCD area detector diffractometer	6390 independent reflections
Absorption correction: multi-scan SADABS	6376 reflections with I > 2σ(I)
T_min = 0.284, T_max = 0.455	R_int = 0.034
24358 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.027	H-atom parameters constrained
wR(F²) = 0.059	w = 1/[σ²(F_o²) + (0.0121P)² + 76.2392P] where P = (F_o² + 2F_c²)/3
S = 1.16	Δρ_max = 1.62 e Å⁻³
6390 reflections	Δρ_min = −1.34 e Å⁻³
393 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
399 restraints	Absolute structure parameter: 0.027 (13)

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.0000	0.25213 (3)	0.29653 (4)	0.00999 (11)
Re1	0.14695 (2)	0.23760 (2)	0.12466 (3)	0.01727 (9)
Re2	0.0000	0.41287 (3)	0.44558 (4)	0.01414 (13)
Re3	0.0000	0.12284 (3)	0.49589 (4)	0.01718 (14)
P1	0.16069 (13)	0.26198 (15)	0.40888 (18)	0.0186 (6)
P2	0.0000	0.3906 (2)	0.1422 (3)	0.0461 (13)
P3	0.0000	0.0869 (2)	0.2075 (3)	0.0317 (10)
O1	0.0710 (4)	0.2456 (4)	0.1663 (6)	0.0335 (16)
O2	0.1934 (5)	0.2931 (5)	0.1709 (7)	0.043 (2)
O3	0.1453 (4)	0.2475 (4)	0.0100 (5)	0.036 (2)
O4	0.1769 (6)	0.1669 (4)	0.1490 (5)	0.049 (3)
O5	0.1030 (4)	0.2511 (4)	0.3523 (5)	0.0266 (13)
O6	0.0000	0.3363 (5)	0.4090 (7)	0.0165 (18)
O7	0.0000	0.4134 (6)	0.5634 (7)	0.047 (4)
O8	0.0636 (5)	0.4502 (4)	0.4112 (7)	0.040 (2)
O9	0.0000	0.3452 (6)	0.2221 (9)	0.047 (2)
O10	0.0000	0.1944 (5)	0.4394 (8)	0.0204 (18)
O11	0.0619 (7)	0.0806 (5)	0.4699 (7)	0.067 (4)
O12	0.0000	0.1341 (5)	0.6090 (7)	0.035 (3)
O13	0.0000	0.1500 (5)	0.2530 (8)	0.033 (2)
C1	0.1482 (5)	0.2474 (5)	0.5266 (7)	0.021 (2)
H1A	0.1343	0.2038	0.5336	0.025*
H1B	0.1885	0.2514	0.5583	0.025*
C2	0.1009 (5)	0.2895 (5)	0.5740 (7)	0.024 (2)
H2A	0.0613	0.2886	0.5400	0.029*
H2B	0.1165	0.3327	0.5735	0.029*
C3	0.0889 (5)	0.2694 (6)	0.6720 (7)	0.025 (2)
H3A	0.0561	0.2963	0.6979	0.030*
H3B	0.0730	0.2263	0.6720	0.030*
C4	0.1460 (6)	0.2726 (6)	0.7325 (8)	0.029 (3)
H4A	0.1774	0.2434	0.7105	0.043*
H4B	0.1344	0.2617	0.7945	0.043*
H4C	0.1629	0.3148	0.7314	0.043*
C5	0.1837 (5)	0.3397 (5)	0.3959 (8)	0.025 (2)
H5A	0.1917	0.3471	0.3308	0.030*
H5B	0.1483	0.3664	0.4134	0.030*
C6	0.2416 (5)	0.3618 (4)	0.4493 (8)	0.0263 (19)
H6A	0.2348	0.3546	0.5146	0.032*
H6B	0.2781	0.3370	0.4305	0.032*
C7	0.2550 (6)	0.4299 (5)	0.4337 (10)	0.037 (3)
H7A	0.2190	0.4549	0.4537	0.044*
H7B	0.2612	0.4374	0.3683	0.044*
C8	0.3131 (7)	0.4506 (6)	0.4854 (11)	0.054 (4)
H8A	0.3133	0.4959	0.4906	0.081*
H8B	0.3503	0.4370	0.4528	0.081*
H8C	0.3128	0.4321	0.5460	0.081*
C9	0.2192 (5)	0.2102 (4)	0.3757 (7)	0.0177 (17)
H9A	0.2306	0.2195	0.3122	0.021*
H9B	0.2564	0.2181	0.4133	0.021*
C10	0.2032 (5)	0.1419 (5)	0.3824 (8)	0.021 (2)
H10A	0.1934	0.1322	0.4462	0.026*
H10B	0.1651	0.1342	0.3465	0.026*
C11	0.2531 (5)	0.0978 (5)	0.3505 (8)	0.024 (2)
H11A	0.2356	0.0554	0.3459	0.029*
H11B	0.2673	0.1104	0.2896	0.029*
C12	0.3073 (6)	0.0971 (5)	0.4138 (9)	0.033 (3)
H12A	0.3312	0.1355	0.4066	0.050*
H12B	0.3339	0.0614	0.4001	0.050*
H12C	0.2923	0.0940	0.4762	0.050*
C13A	−0.0531 (12)	0.4509 (10)	0.1595 (18)	0.051 (2)	0.491 (15)
H13A	−0.0297	0.4833	0.1926	0.061*	0.491 (15)
H13B	−0.0613	0.4683	0.0987	0.061*	0.491 (15)
C14A	−0.1158 (12)	0.4479 (12)	0.2051 (18)	0.050 (2)	0.491 (15)
H14A	−0.1309	0.4050	0.1956	0.060*	0.491 (15)
H14B	−0.1074	0.4518	0.2707	0.060*	0.491 (15)
C15A	−0.1700 (13)	0.4891 (12)	0.187 (2)	0.049 (2)	0.491 (15)
H15A	−0.1933	0.4948	0.2437	0.059*	0.491 (15)
H15B	−0.1979	0.4676	0.1436	0.059*	0.491 (15)
C16A	−0.1548 (18)	0.5531 (12)	0.148 (2)	0.046 (4)	0.491 (15)
H16A	−0.1265	0.5748	0.1893	0.069*	0.491 (15)
H16B	−0.1932	0.5771	0.1418	0.069*	0.491 (15)
H16C	−0.1351	0.5484	0.0889	0.069*	0.491 (15)
C13B	−0.0725 (9)	0.4303 (10)	0.1138 (16)	0.051 (2)	0.509 (15)
H13C	−0.0643	0.4755	0.1127	0.061*	0.509 (15)
H13D	−0.0845	0.4178	0.0518	0.061*	0.509 (15)
C14B	−0.1235 (13)	0.4196 (10)	0.1712 (17)	0.050 (2)	0.509 (15)
H14C	−0.1075	0.3984	0.2258	0.060*	0.509 (15)
H14D	−0.1512	0.3898	0.1401	0.060*	0.509 (15)
C15B	−0.1633 (16)	0.4732 (11)	0.2028 (17)	0.049 (2)	0.509 (15)
H15C	−0.1465	0.4880	0.2613	0.059*	0.509 (15)
H15D	−0.2056	0.4573	0.2143	0.059*	0.509 (15)
C16B	−0.1684 (18)	0.5288 (11)	0.1394 (19)	0.046 (4)	0.509 (15)
H16D	−0.1392	0.5611	0.1585	0.069*	0.509 (15)
H16E	−0.2108	0.5453	0.1415	0.069*	0.509 (15)
H16F	−0.1586	0.5158	0.0776	0.069*	0.509 (15)
C17	0.0000	0.3542 (9)	0.0371 (10)	0.039 (3)
H17A	0.0370	0.3270	0.0339	0.046*	0.50
H17B	−0.0370	0.3270	0.0339	0.046*	0.50
C18	0.0000	0.3959 (7)	−0.0458 (9)	0.038 (3)
H18A	−0.0372	0.4229	−0.0440	0.046*	0.50
H18B	0.0372	0.4229	−0.0440	0.046*	0.50
C19	0.0000	0.3596 (8)	−0.1333 (10)	0.048 (4)
H19A	−0.0372	0.3327	−0.1357	0.058*	0.50
H19B	0.0372	0.3327	−0.1357	0.058*	0.50
C20	0.0000	0.4039 (9)	−0.2157 (11)	0.061 (6)
H20A	0.0000	0.3795	−0.2716	0.092*
H20B	0.0372	0.4302	−0.2138	0.092*	0.50
H20C	−0.0372	0.4302	−0.2138	0.092*	0.50
C21	−0.0694 (7)	0.0472 (6)	0.2409 (10)	0.046 (3)
H21A	−0.0663	0.0382	0.3064	0.055*
H21B	−0.1047	0.0760	0.2326	0.055*
C22	−0.0851 (6)	−0.0134 (6)	0.1925 (11)	0.054 (3)
H22A	−0.0864	−0.0059	0.1265	0.065*
H22B	−0.0521	−0.0442	0.2046	0.065*
C23	−0.1467 (6)	−0.0391 (7)	0.2232 (12)	0.063 (4)
H23A	−0.1791	−0.0071	0.2140	0.076*
H23B	−0.1444	−0.0479	0.2888	0.076*
C24	−0.1661 (7)	−0.0979 (7)	0.1742 (13)	0.065 (5)
H24A	−0.2090	−0.1083	0.1905	0.097*
H24B	−0.1386	−0.1321	0.1918	0.097*
H24C	−0.1633	−0.0914	0.1088	0.097*
C25	−0.0307 (13)	0.0904 (11)	0.0910 (13)	0.038 (4)	0.50
H25A	−0.0270	0.0486	0.0638	0.046*	0.50
H25B	−0.0755	0.1005	0.0942	0.046*	0.50
C26	0.0000	0.1361 (9)	0.0287 (9)	0.049 (4)
H26A	−0.0201	0.1769	0.0382	0.059*	0.50
H26B	0.0438	0.1404	0.0482	0.059*	0.50
C27	0.0000	0.1233 (9)	−0.0709 (9)	0.053 (4)
H27A	−0.0371	0.0980	−0.0854	0.064*	0.50
H27B	0.0371	0.0980	−0.0854	0.064*	0.50
C28	0.0000	0.1796 (12)	−0.1317 (16)	0.099 (8)
H28A	0.0000	0.1662	−0.1950	0.148*
H28B	0.0372	0.2045	−0.1197	0.148*	0.50
H28C	−0.0372	0.2045	−0.1197	0.148*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0114 (3)	0.0100 (3)	0.0085 (2)	0.000	0.000	−0.00019 (19)
Re1	0.0170 (2)	0.02032 (19)	0.0145 (2)	0.00218 (19)	0.0038 (2)	0.0001 (2)
Re2	0.0204 (4)	0.0130 (3)	0.0090 (3)	0.000	0.000	−0.0012 (3)
Re3	0.0258 (4)	0.0149 (3)	0.0108 (3)	0.000	0.000	0.0026 (3)
P1	0.0153 (14)	0.0275 (14)	0.0131 (12)	0.0027 (11)	−0.0032 (10)	0.0001 (11)
P2	0.116 (4)	0.011 (2)	0.011 (2)	0.000	0.000	0.0029 (14)
P3	0.064 (3)	0.0136 (18)	0.0175 (19)	0.000	0.000	−0.0048 (16)
O1	0.019 (3)	0.069 (5)	0.013 (2)	−0.013 (3)	0.007 (2)	−0.006 (3)
O2	0.035 (5)	0.042 (4)	0.052 (5)	−0.026 (4)	0.004 (4)	0.005 (4)
O3	0.035 (5)	0.056 (6)	0.017 (2)	0.017 (4)	0.014 (3)	0.009 (3)
O4	0.094 (7)	0.031 (3)	0.021 (4)	0.027 (4)	−0.007 (5)	−0.007 (3)
O5	0.012 (2)	0.052 (4)	0.015 (3)	0.001 (2)	0.002 (2)	−0.010 (3)
O6	0.028 (5)	0.013 (2)	0.009 (3)	0.000	0.000	0.003 (2)
O7	0.110 (13)	0.019 (6)	0.012 (3)	0.000	0.000	−0.003 (3)
O8	0.033 (5)	0.026 (4)	0.061 (5)	−0.009 (3)	0.009 (4)	−0.002 (4)
O9	0.112 (6)	0.017 (3)	0.012 (3)	0.000	0.000	0.009 (3)
O10	0.034 (5)	0.016 (3)	0.011 (3)	0.000	0.000	0.004 (2)
O11	0.091 (8)	0.058 (6)	0.054 (6)	0.051 (5)	0.045 (6)	0.033 (5)
O12	0.076 (9)	0.018 (5)	0.010 (2)	0.000	0.000	0.004 (3)
O13	0.067 (5)	0.014 (2)	0.017 (4)	0.000	0.000	−0.005 (3)
C1	0.026 (5)	0.023 (5)	0.014 (2)	−0.006 (4)	−0.003 (3)	−0.006 (3)
C2	0.028 (5)	0.024 (5)	0.020 (3)	−0.008 (4)	0.004 (3)	−0.007 (4)
C3	0.026 (5)	0.028 (5)	0.022 (4)	−0.007 (5)	0.006 (3)	−0.003 (4)
C4	0.035 (7)	0.024 (6)	0.028 (5)	−0.007 (5)	−0.001 (5)	−0.004 (5)
C5	0.019 (5)	0.025 (3)	0.033 (6)	0.006 (3)	−0.004 (4)	0.007 (4)
C6	0.022 (5)	0.015 (4)	0.041 (5)	0.005 (3)	−0.007 (4)	0.001 (4)
C7	0.038 (6)	0.018 (4)	0.054 (7)	0.002 (4)	−0.007 (6)	0.001 (5)
C8	0.057 (10)	0.031 (6)	0.074 (10)	−0.025 (6)	−0.023 (7)	0.028 (7)
C9	0.017 (4)	0.022 (3)	0.015 (4)	−0.001 (3)	−0.002 (3)	0.005 (4)
C10	0.023 (4)	0.023 (3)	0.019 (5)	−0.003 (3)	−0.004 (4)	−0.004 (4)
C11	0.023 (5)	0.019 (4)	0.031 (5)	−0.008 (4)	−0.001 (4)	−0.008 (4)
C12	0.046 (7)	0.017 (6)	0.036 (6)	0.021 (5)	−0.017 (5)	−0.011 (5)
C13A	0.116 (4)	0.016 (4)	0.020 (5)	0.007 (4)	−0.010 (3)	−0.006 (3)
C14A	0.113 (4)	0.016 (5)	0.022 (5)	0.005 (4)	−0.013 (4)	0.000 (4)
C15A	0.109 (5)	0.020 (5)	0.019 (5)	0.005 (4)	−0.012 (4)	0.002 (4)
C16A	0.091 (9)	0.024 (6)	0.024 (7)	0.003 (6)	−0.031 (7)	0.006 (6)
C13B	0.116 (4)	0.016 (4)	0.020 (5)	0.007 (4)	−0.010 (3)	−0.006 (3)
C14B	0.113 (4)	0.016 (5)	0.022 (5)	0.005 (4)	−0.013 (4)	0.000 (4)
C15B	0.109 (5)	0.020 (5)	0.019 (5)	0.005 (4)	−0.012 (4)	0.002 (4)
C16B	0.091 (9)	0.024 (6)	0.024 (7)	0.003 (6)	−0.031 (7)	0.006 (6)
C17	0.069 (8)	0.038 (7)	0.009 (3)	0.000	0.000	0.000 (3)
C18	0.068 (9)	0.035 (7)	0.011 (3)	0.000	0.000	0.000 (4)
C19	0.099 (11)	0.038 (8)	0.009 (3)	0.000	0.000	0.003 (5)
C20	0.138 (17)	0.035 (10)	0.010 (4)	0.000	0.000	0.003 (7)
C21	0.047 (6)	0.040 (6)	0.049 (5)	−0.005 (4)	0.022 (6)	−0.035 (5)
C22	0.028 (6)	0.055 (6)	0.078 (7)	−0.008 (4)	0.017 (5)	−0.052 (5)
C23	0.017 (6)	0.066 (7)	0.106 (9)	−0.004 (4)	0.014 (6)	−0.058 (7)
C24	0.020 (7)	0.061 (9)	0.113 (12)	−0.008 (5)	0.016 (8)	−0.054 (8)
C25	0.054 (12)	0.034 (10)	0.026 (4)	0.003 (7)	−0.009 (5)	−0.015 (4)
C26	0.082 (11)	0.048 (9)	0.018 (4)	0.000	0.000	−0.008 (5)
C27	0.090 (12)	0.049 (9)	0.022 (5)	0.000	0.000	−0.013 (6)
C28	0.18 (2)	0.083 (14)	0.033 (8)	0.000	0.000	0.015 (9)

Geometric parameters (Å, º) top

Th1—O9	2.287 (12)	C11—H11A	0.9900
Th1—O13	2.293 (11)	C11—H11B	0.9900
Th1—O5	2.368 (8)	C12—H12A	0.9800
Th1—O5ⁱ	2.368 (8)	C12—H12B	0.9800
Th1—O10	2.454 (11)	C12—H12C	0.9800
Th1—O6	2.461 (11)	C13A—C14A	1.510 (18)
Th1—O1ⁱ	2.464 (8)	C13A—H13A	0.9900
Th1—O1	2.464 (8)	C13A—H13B	0.9900
Re1—O4	1.693 (9)	C14A—C15A	1.492 (18)
Re1—O2	1.703 (9)	C14A—H14A	0.9900
Re1—O3	1.711 (8)	C14A—H14B	0.9900
Re1—O1	1.756 (9)	C15A—C16A	1.526 (18)
Re2—O8	1.668 (9)	C15A—H15A	0.9900
Re2—O8ⁱ	1.668 (9)	C15A—H15B	0.9900
Re2—O6	1.737 (11)	C16A—H16A	0.9800
Re2—O7	1.743 (11)	C16A—H16B	0.9800
Re3—O11ⁱ	1.660 (11)	C16A—H16C	0.9800
Re3—O11	1.660 (11)	C13B—C14B	1.406 (18)
Re3—O12	1.691 (10)	C13B—H13C	0.9900
Re3—O10	1.753 (10)	C13B—H13D	0.9900
P1—O5	1.515 (8)	C14B—C15B	1.512 (18)
P1—C9	1.754 (11)	C14B—H14C	0.9900
P1—C5	1.758 (12)	C14B—H14D	0.9900
P1—C1	1.791 (10)	C15B—C16B	1.525 (17)
P2—O9	1.535 (12)	C15B—H15C	0.9900
P2—C17	1.742 (17)	C15B—H15D	0.9900
P2—C13Aⁱ	1.749 (16)	C16B—H16D	0.9800
P2—C13A	1.750 (16)	C16B—H16E	0.9800
P2—C13Bⁱ	1.828 (17)	C16B—H16F	0.9800
P2—C13B	1.828 (17)	C17—C18	1.521 (15)
P3—O13	1.518 (12)	C17—H17A	0.9900
P3—C21ⁱ	1.791 (14)	C17—H17B	0.9900
P3—C21	1.792 (14)	C18—C19	1.513 (15)
P3—C25	1.85 (2)	C18—H18A	0.9900
P3—C25ⁱ	1.85 (2)	C18—H18B	0.9900
C1—C2	1.533 (12)	C19—C20	1.549 (16)
C1—H1A	0.9900	C19—H19A	0.9900
C1—H1B	0.9900	C19—H19B	0.9900
C2—C3	1.536 (12)	C20—H20A	0.9800
C2—H2A	0.9900	C20—H20B	0.9800
C2—H2B	0.9900	C20—H20C	0.9800
C3—C4	1.522 (13)	C21—C22	1.526 (13)
C3—H3A	0.9900	C21—H21A	0.9900
C3—H3B	0.9900	C21—H21B	0.9900
C4—H4A	0.9800	C22—C23	1.508 (14)
C4—H4B	0.9800	C22—H22A	0.9900
C4—H4C	0.9800	C22—H22B	0.9900
C5—C6	1.551 (12)	C23—C24	1.519 (14)
C5—H5A	0.9900	C23—H23A	0.9900
C5—H5B	0.9900	C23—H23B	0.9900
C6—C7	1.514 (12)	C24—H24A	0.9800
C6—H6A	0.9900	C24—H24B	0.9800
C6—H6B	0.9900	C24—H24C	0.9800
C7—C8	1.531 (14)	C25—C26	1.502 (17)
C7—H7A	0.9900	C25—H25A	0.9900
C7—H7B	0.9900	C25—H25B	0.9900
C8—H8A	0.9800	C26—C27	1.500 (16)
C8—H8B	0.9800	C26—H26A	0.9900
C8—H8C	0.9800	C26—H26B	0.9900
C9—C10	1.515 (12)	C27—C28	1.510 (17)
C9—H9A	0.9900	C27—H27A	0.9900
C9—H9B	0.9900	C27—H27B	0.9900
C10—C11	1.511 (13)	C28—H28A	0.9800
C10—H10A	0.9900	C28—H28B	0.9800
C10—H10B	0.9900	C28—H28C	0.9800
C11—C12	1.498 (13)

O9—Th1—O13	134.9 (5)	C11—C10—H10A	108.4
O9—Th1—O5	100.1 (2)	C9—C10—H10A	108.4
O13—Th1—O5	95.1 (2)	C11—C10—H10B	108.4
O9—Th1—O5ⁱ	100.2 (2)	C9—C10—H10B	108.4
O13—Th1—O5ⁱ	95.1 (2)	H10A—C10—H10B	107.5
O5—Th1—O5ⁱ	139.2 (4)	C12—C11—C10	111.4 (9)
O9—Th1—O10	149.3 (4)	C12—C11—H11A	109.3
O13—Th1—O10	75.8 (4)	C10—C11—H11A	109.3
O5—Th1—O10	72.2 (2)	C12—C11—H11B	109.3
O5ⁱ—Th1—O10	72.2 (2)	C10—C11—H11B	109.3
O9—Th1—O6	71.3 (4)	H11A—C11—H11B	108.0
O13—Th1—O6	153.8 (4)	C11—C12—H12A	109.5
O5—Th1—O6	76.8 (2)	C11—C12—H12B	109.5
O5ⁱ—Th1—O6	76.8 (2)	H12A—C12—H12B	109.5
O10—Th1—O6	78.0 (3)	C11—C12—H12C	109.5
O9—Th1—O1ⁱ	70.9 (3)	H12A—C12—H12C	109.5
O13—Th1—O1ⁱ	74.1 (3)	H12B—C12—H12C	109.5
O5—Th1—O1ⁱ	148.6 (3)	C14A—C13A—P2	128.1 (18)
O5ⁱ—Th1—O1ⁱ	72.0 (3)	C14A—C13A—H13A	105.3
O10—Th1—O1ⁱ	130.2 (3)	P2—C13A—H13A	105.3
O6—Th1—O1ⁱ	124.8 (3)	C14A—C13A—H13B	105.3
O9—Th1—O1	70.9 (3)	P2—C13A—H13B	105.3
O13—Th1—O1	74.1 (3)	H13A—C13A—H13B	106.0
O5—Th1—O1	72.0 (3)	C15A—C14A—C13A	126.3 (19)
O5ⁱ—Th1—O1	148.6 (3)	C15A—C14A—H14A	105.7
O10—Th1—O1	130.2 (3)	C13A—C14A—H14A	105.8
O6—Th1—O1	124.8 (3)	C15A—C14A—H14B	105.8
O1ⁱ—Th1—O1	76.7 (4)	C13A—C14A—H14B	105.8
O4—Re1—O2	108.8 (5)	H14A—C14A—H14B	106.2
O4—Re1—O3	109.4 (4)	C14A—C15A—C16A	116 (2)
O2—Re1—O3	108.8 (4)	C14A—C15A—H15A	108.3
O4—Re1—O1	111.6 (5)	C16A—C15A—H15A	108.3
O2—Re1—O1	109.7 (5)	C14A—C15A—H15B	108.3
O3—Re1—O1	108.4 (4)	C16A—C15A—H15B	108.3
O8—Re2—O8ⁱ	110.5 (7)	H15A—C15A—H15B	107.4
O8—Re2—O6	111.3 (4)	C15A—C16A—H16A	109.5
O8ⁱ—Re2—O6	111.3 (4)	C15A—C16A—H16B	109.5
O8—Re2—O7	107.6 (4)	H16A—C16A—H16B	109.5
O8ⁱ—Re2—O7	107.6 (4)	C15A—C16A—H16C	109.5
O6—Re2—O7	108.5 (5)	H16A—C16A—H16C	109.5
O11ⁱ—Re3—O11	106.9 (11)	H16B—C16A—H16C	109.5
O11ⁱ—Re3—O12	107.9 (4)	C14B—C13B—P2	116.9 (17)
O11—Re3—O12	107.9 (4)	C14B—C13B—H13C	108.1
O11ⁱ—Re3—O10	111.8 (4)	P2—C13B—H13C	108.1
O11—Re3—O10	111.8 (4)	C14B—C13B—H13D	108.1
O12—Re3—O10	110.2 (5)	P2—C13B—H13D	108.1
O5—P1—C9	109.6 (5)	H13C—C13B—H13D	107.3
O5—P1—C5	108.6 (5)	C13B—C14B—C15B	120.3 (19)
C9—P1—C5	111.9 (5)	C13B—C14B—H14C	107.2
O5—P1—C1	112.8 (5)	C15B—C14B—H14C	107.2
C9—P1—C1	105.6 (5)	C13B—C14B—H14D	107.3
C5—P1—C1	108.5 (5)	C15B—C14B—H14D	107.3
O9—P2—C17	113.5 (8)	H14C—C14B—H14D	106.9
O9—P2—C13Aⁱ	111.2 (10)	C14B—C15B—C16B	116.8 (19)
C17—P2—C13Aⁱ	117.7 (10)	C14B—C15B—H15C	108.1
O9—P2—C13A	111.2 (10)	C16B—C15B—H15C	108.1
C17—P2—C13A	117.7 (10)	C14B—C15B—H15D	108.1
C13Aⁱ—P2—C13A	82 (2)	C16B—C15B—H15D	108.1
O9—P2—C13Bⁱ	118.4 (8)	H15C—C15B—H15D	107.3
C17—P2—C13Bⁱ	90.3 (9)	C15B—C16B—H16D	109.5
C13Aⁱ—P2—C13Bⁱ	29.4 (10)	C15B—C16B—H16E	109.5
C13A—P2—C13Bⁱ	104.2 (13)	H16D—C16B—H16E	109.5
O9—P2—C13B	118.4 (8)	C15B—C16B—H16F	109.5
C17—P2—C13B	90.3 (9)	H16D—C16B—H16F	109.5
C13Aⁱ—P2—C13B	104.2 (13)	H16E—C16B—H16F	109.5
C13A—P2—C13B	29.4 (10)	C18—C17—P2	117.0 (13)
C13Bⁱ—P2—C13B	117.3 (15)	C18—C17—H17A	108.1
O13—P3—C21ⁱ	107.8 (4)	P2—C17—H17A	108.1
O13—P3—C21	107.8 (4)	C18—C17—H17B	108.1
C21ⁱ—P3—C21	113.1 (11)	P2—C17—H17B	108.1
O13—P3—C25	112.2 (9)	H17A—C17—H17B	107.3
C21ⁱ—P3—C25	125.1 (10)	C19—C18—C17	112.6 (12)
C21—P3—C25	88.8 (9)	C19—C18—H18A	109.1
O13—P3—C25ⁱ	112.2 (9)	C17—C18—H18A	109.1
C21ⁱ—P3—C25ⁱ	88.8 (9)	C19—C18—H18B	109.1
C21—P3—C25ⁱ	125.1 (10)	C17—C18—H18B	109.1
C25—P3—C25ⁱ	41.9 (17)	H18A—C18—H18B	107.8
Re1—O1—Th1	149.1 (5)	C18—C19—C20	110.8 (14)
P1—O5—Th1	163.5 (5)	C18—C19—H19A	109.5
Re2—O6—Th1	155.6 (6)	C20—C19—H19A	109.5
P2—O9—Th1	158.4 (9)	C18—C19—H19B	109.5
Re3—O10—Th1	148.9 (6)	C20—C19—H19B	109.5
P3—O13—Th1	170.0 (7)	H19A—C19—H19B	108.1
C2—C1—P1	116.1 (8)	C19—C20—H20A	109.5
C2—C1—H1A	108.3	C19—C20—H20B	109.5
P1—C1—H1A	108.3	H20A—C20—H20B	109.5
C2—C1—H1B	108.3	C19—C20—H20C	109.5
P1—C1—H1B	108.3	H20A—C20—H20C	109.5
H1A—C1—H1B	107.4	H20B—C20—H20C	109.5
C1—C2—C3	112.2 (9)	C22—C21—P3	117.6 (9)
C1—C2—H2A	109.2	C22—C21—H21A	107.9
C3—C2—H2A	109.2	P3—C21—H21A	107.9
C1—C2—H2B	109.2	C22—C21—H21B	107.9
C3—C2—H2B	109.2	P3—C21—H21B	107.9
H2A—C2—H2B	107.9	H21A—C21—H21B	107.2
C4—C3—C2	113.9 (10)	C23—C22—C21	111.6 (10)
C4—C3—H3A	108.8	C23—C22—H22A	109.3
C2—C3—H3A	108.8	C21—C22—H22A	109.3
C4—C3—H3B	108.8	C23—C22—H22B	109.3
C2—C3—H3B	108.8	C21—C22—H22B	109.3
H3A—C3—H3B	107.7	H22A—C22—H22B	108.0
C3—C4—H4A	109.5	C22—C23—C24	114.0 (11)
C3—C4—H4B	109.5	C22—C23—H23A	108.8
H4A—C4—H4B	109.5	C24—C23—H23A	108.8
C3—C4—H4C	109.5	C22—C23—H23B	108.8
H4A—C4—H4C	109.5	C24—C23—H23B	108.8
H4B—C4—H4C	109.5	H23A—C23—H23B	107.7
C6—C5—P1	117.6 (8)	C23—C24—H24A	109.5
C6—C5—H5A	107.9	C23—C24—H24B	109.5
P1—C5—H5A	107.9	H24A—C24—H24B	109.5
C6—C5—H5B	107.9	C23—C24—H24C	109.5
P1—C5—H5B	107.9	H24A—C24—H24C	109.5
H5A—C5—H5B	107.2	H24B—C24—H24C	109.5
C7—C6—C5	111.9 (9)	C26—C25—P3	116.2 (15)
C7—C6—H6A	109.2	C26—C25—H25A	108.2
C5—C6—H6A	109.2	P3—C25—H25A	108.2
C7—C6—H6B	109.2	C26—C25—H25B	108.2
C5—C6—H6B	109.2	P3—C25—H25B	108.2
H6A—C6—H6B	107.9	H25A—C25—H25B	107.4
C6—C7—C8	111.2 (10)	C27—C26—C25	118.8 (15)
C6—C7—H7A	109.4	C27—C26—H26A	107.6
C8—C7—H7A	109.4	C25—C26—H26A	107.6
C6—C7—H7B	109.4	C27—C26—H26B	107.6
C8—C7—H7B	109.4	C25—C26—H26B	107.6
H7A—C7—H7B	108.0	H26A—C26—H26B	107.0
C7—C8—H8A	109.5	C26—C27—C28	116.0 (16)
C7—C8—H8B	109.5	C26—C27—H27A	108.3
H8A—C8—H8B	109.5	C28—C27—H27A	108.3
C7—C8—H8C	109.5	C26—C27—H27B	108.3
H8A—C8—H8C	109.5	C28—C27—H27B	108.3
H8B—C8—H8C	109.5	H27A—C27—H27B	107.4
C10—C9—P1	115.8 (8)	C27—C28—H28A	109.5
C10—C9—H9A	108.3	C27—C28—H28B	109.5
P1—C9—H9A	108.3	H28A—C28—H28B	109.5
C10—C9—H9B	108.3	C27—C28—H28C	109.5
P1—C9—H9B	108.3	H28A—C28—H28C	109.5
H9A—C9—H9B	107.4	H28B—C28—H28C	109.5
C11—C10—C9	115.4 (9)

O4—Re1—O1—Th1	65.9 (10)	O9—Th1—O13—P3	0.000 (5)
O2—Re1—O1—Th1	−54.8 (11)	O5—Th1—O13—P3	−109.8 (2)
O3—Re1—O1—Th1	−173.5 (9)	O5ⁱ—Th1—O13—P3	109.8 (2)
O9—Th1—O1—Re1	114.0 (10)	O10—Th1—O13—P3	180.000 (5)
O13—Th1—O1—Re1	−94.9 (10)	O6—Th1—O13—P3	180.000 (4)
O5—Th1—O1—Re1	6.0 (9)	O1ⁱ—Th1—O13—P3	40.2 (2)
O5ⁱ—Th1—O1—Re1	−168.0 (7)	O1—Th1—O13—P3	−40.2 (2)
O10—Th1—O1—Re1	−40.0 (12)	O5—P1—C1—C2	−63.5 (9)
O6—Th1—O1—Re1	64.7 (11)	C9—P1—C1—C2	176.9 (8)
O1ⁱ—Th1—O1—Re1	−171.9 (8)	C5—P1—C1—C2	56.8 (10)
C9—P1—O5—Th1	166.6 (17)	P1—C1—C2—C3	174.5 (8)
C5—P1—O5—Th1	−70.9 (19)	C1—C2—C3—C4	62.3 (13)
C1—P1—O5—Th1	49 (2)	O5—P1—C5—C6	179.0 (9)
O9—Th1—O5—P1	82.0 (19)	C9—P1—C5—C6	−59.9 (11)
O13—Th1—O5—P1	−140.6 (18)	C1—P1—C5—C6	56.2 (11)
O5ⁱ—Th1—O5—P1	−37 (2)	P1—C5—C6—C7	−178.5 (9)
O10—Th1—O5—P1	−67.3 (18)	C5—C6—C7—C8	−178.9 (12)
O6—Th1—O5—P1	14.1 (18)	O5—P1—C9—C10	−58.1 (9)
O1ⁱ—Th1—O5—P1	151.9 (16)	C5—P1—C9—C10	−178.6 (8)
O1—Th1—O5—P1	148.0 (19)	C1—P1—C9—C10	63.6 (9)
O8—Re2—O6—Th1	−61.8 (4)	P1—C9—C10—C11	177.9 (8)
O8ⁱ—Re2—O6—Th1	61.8 (4)	C9—C10—C11—C12	70.2 (13)
O7—Re2—O6—Th1	180.000 (3)	O9—P2—C13A—C14A	−36 (3)
O9—Th1—O6—Re2	0.000 (1)	C17—P2—C13A—C14A	98 (3)
O13—Th1—O6—Re2	180.0	C13Aⁱ—P2—C13A—C14A	−145 (2)
O5—Th1—O6—Re2	105.7 (2)	C13Bⁱ—P2—C13A—C14A	−164 (2)
O5ⁱ—Th1—O6—Re2	−105.7 (2)	C13B—P2—C13A—C14A	75 (3)
O10—Th1—O6—Re2	180.000 (2)	P2—C13A—C14A—C15A	−152 (3)
O1ⁱ—Th1—O6—Re2	−49.1 (3)	C13A—C14A—C15A—C16A	−25 (4)
O1—Th1—O6—Re2	49.1 (3)	O9—P2—C13B—C14B	4 (2)
C17—P2—O9—Th1	0.000 (5)	C17—P2—C13B—C14B	121 (2)
C13Aⁱ—P2—O9—Th1	−135.5 (11)	C13Aⁱ—P2—C13B—C14B	−120.0 (19)
C13A—P2—O9—Th1	135.5 (11)	C13A—P2—C13B—C14B	−79 (3)
C13Bⁱ—P2—O9—Th1	−104.0 (10)	C13Bⁱ—P2—C13B—C14B	−148.2 (14)
C13B—P2—O9—Th1	104.0 (10)	P2—C13B—C14B—C15B	135 (2)
O13—Th1—O9—P2	0.000 (4)	C13B—C14B—C15B—C16B	30 (5)
O5—Th1—O9—P2	107.8 (2)	O9—P2—C17—C18	180.000 (1)
O5ⁱ—Th1—O9—P2	−107.8 (2)	C13Aⁱ—P2—C17—C18	−47.6 (11)
O10—Th1—O9—P2	180.000 (2)	C13A—P2—C17—C18	47.6 (11)
O6—Th1—O9—P2	180.000 (3)	C13Bⁱ—P2—C17—C18	−58.6 (8)
O1ⁱ—Th1—O9—P2	−41.0 (2)	C13B—P2—C17—C18	58.6 (8)
O1—Th1—O9—P2	41.0 (2)	P2—C17—C18—C19	180.000 (2)
O11ⁱ—Re3—O10—Th1	−59.9 (6)	C17—C18—C19—C20	180.000 (2)
O11—Re3—O10—Th1	59.9 (6)	O13—P3—C21—C22	170.7 (13)
O12—Re3—O10—Th1	180.000 (1)	C21ⁱ—P3—C21—C22	−70.3 (17)
O9—Th1—O10—Re3	180.0	C25—P3—C21—C22	57.8 (16)
O13—Th1—O10—Re3	0.000 (1)	C25ⁱ—P3—C21—C22	35.5 (19)
O5—Th1—O10—Re3	−100.2 (2)	P3—C21—C22—C23	−176.1 (13)
O5ⁱ—Th1—O10—Re3	100.2 (2)	C21—C22—C23—C24	177.4 (16)
O6—Th1—O10—Re3	180.000 (2)	O13—P3—C25—C26	55 (2)
O1ⁱ—Th1—O10—Re3	54.3 (3)	C21ⁱ—P3—C25—C26	−79 (2)
O1—Th1—O10—Re3	−54.3 (3)	C21—P3—C25—C26	163.2 (19)
C21ⁱ—P3—O13—Th1	118.8 (6)	C25ⁱ—P3—C25—C26	−44 (2)
C21—P3—O13—Th1	−118.8 (6)	P3—C25—C26—C27	152.4 (12)
C25—P3—O13—Th1	−22.7 (9)	C25—C26—C27—C28	149.9 (15)
C25ⁱ—P3—O13—Th1	22.7 (9)

Symmetry code: (i) −x, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.99	2.56	3.421 (14)	145
C2—H2A···O10	0.99	2.84	3.590 (15)	133
C3—H3B···O12	0.99	2.70	3.611 (15)	153
C5—H5B···O8	0.99	2.57	3.522 (17)	162
C5—H5A···O2	0.99	2.64	3.483 (16)	144
C9—H9A···O2	0.99	2.74	3.561 (14)	140
C9—H9A···O4	0.99	2.91	3.598 (13)	128
C10—H10A···O11	0.99	3.06	3.561 (18)	113
C10—H10B···O4	0.99	3.02	3.539 (14)	114
C10—H10B···O5	0.99	2.85	3.222 (13)	103
C14A—H14A···O9	0.99	3.12	3.34 (2)	94
C14A—H14A···O9	0.99	3.12	3.34 (2)	94
C17—H17A···O1	0.99	2.73	3.386 (18)	124
C17—H17A···O3	0.99	2.91	3.903 (15)	176
C26—H26B···O1	0.99	2.92	3.471 (18)	116
C4—H4A···O2ⁱⁱ	0.98	2.95	3.847 (18)	153
C6—H6A···O4ⁱⁱ	0.99	2.79	3.491 (15)	128
C6—H6B···O3ⁱⁱ	0.99	2.72	3.505 (13)	136
C8—H8C···O4ⁱⁱ	0.98	2.63	3.509 (15)	149
C9—H9B···O3ⁱⁱ	0.99	2.66	3.646 (14)	174
C12—H12A···O3ⁱⁱ	0.98	2.99	3.778 (14)	138
C13A—H13B···O7ⁱⁱⁱ	0.99	2.92	3.45 (3)	114
C13A—H13B···O7ⁱⁱⁱ	0.99	2.92	3.45 (3)	114
C13B—H13C···O7ⁱⁱⁱ	0.99	2.86	3.79 (3)	156
C13A—H13B···O7^iv	0.99	2.92	3.45 (3)	114
C13A—H13B···O7^iv	0.99	2.92	3.45 (3)	114
C13A—H13B···O7^iv	0.99	2.92	3.45 (3)	114
C13B—H13C···O7^iv	0.99	2.86	3.79 (3)	156
C18—H18A···O8ⁱⁱⁱ	0.99	2.87	3.645 (18)	136
C18—H18B···O8^iv	0.99	2.87	3.645 (18)	136
C17—H17B···O1ⁱ	0.99	2.73	3.386 (18)	124
C17—H17B···O3ⁱ	0.99	2.91	3.903 (15)	176
C13A—H13A···O8ⁱ	0.99	3.39	3.73 (3)	102
C14A—H14B···O8ⁱ	0.99	2.28	3.25 (3)	165
C21—H21B···O4ⁱ	0.99	2.79	3.72 (2)	158
C21—H21A···O11ⁱ	0.99	2.59	3.467 (17)	148
C25—H25B···O4ⁱ	0.99	2.73	3.66 (3)	155
C26—H26A···O1ⁱ	0.99	2.64	3.471 (18)	141
C26—H26A···O3ⁱ	0.99	3.12	3.953 (16)	142
C14A—H14A···O2ⁱ	0.99	2.79	3.76 (3)	170
C20—H20A···O7^v	0.98	2.55	3.275 (19)	131
C28—H28A···O12^v	0.98	2.98	3.96 (3)	176
C20—H20A···O7^vi	0.98	2.55	3.275 (19)	131
C28—H28A···O12^vi	0.98	2.98	3.96 (3)	176
C22—H22A···O11^vii	0.99	2.87	3.632 (16)	134
C22—H22B···O12^vii	0.99	2.65	3.413 (15)	134
C24—H24C···O11^vii	0.98	3.01	3.78 (2)	137
C22—H22B···O12^viii	0.99	2.65	3.413 (15)	134
C16B—H16D···O7ⁱⁱⁱ	0.98	3.36	4.00 (4)	125
C16A—H16C···O7ⁱⁱⁱ	0.98	3.05	3.64 (4)	120
C16A—H16C···O8ⁱⁱⁱ	0.98	3.05	4.02 (4)	172

(IIIat293) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	Mo Kα radiation, λ = 0.71073 Å
M_r = 1753.26	Cell parameters from 1959 reflections
Cubic, I4₃m	θ = 2.7–20.0°
a = 15.3423 (10) Å	µ = 2.95 mm⁻¹
V = 3611.4 (4) Å³	T = 293 K
Z = 2	Prism, colourless
F(000) = 1756	0.10 × 0.10 × 0.10 mm
D_x = 1.612 Mg m⁻³

Data collection top

CCD area detector diffractometer	651 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.041
Graphite monochromator	θ_max = 26.3°, θ_min = 1.9°
phi and ω scans	h = −12→18
6235 measured reflections	k = −3→19
723 independent reflections	l = −19→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.039	H-atom parameters constrained
wR(F²) = 0.101	w = 1/[σ²(F_o²) + (0.0666P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.002
723 reflections	Δρ_max = 0.63 e Å⁻³
50 parameters	Δρ_min = −0.27 e Å⁻³
29 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.00 (2)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	Z = 2
M_r = 1753.26	Mo Kα radiation
Cubic, I4₃m	µ = 2.95 mm⁻¹
a = 15.3423 (10) Å	T = 293 K
V = 3611.4 (4) Å³	0.10 × 0.10 × 0.10 mm

Data collection top

CCD area detector diffractometer	651 reflections with I > 2σ(I)
6235 measured reflections	R_int = 0.041
723 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	H-atom parameters constrained
wR(F²) = 0.101	Δρ_max = 0.63 e Å⁻³
S = 1.02	Δρ_min = −0.27 e Å⁻³
723 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
50 parameters	Absolute structure parameter: 0.00 (2)
29 restraints

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.0000	0.0000	0.0000	0.0657 (3)
Tc1	0.15344 (9)	0.15344 (9)	−0.15344 (9)	0.1127 (8)
P1	0.1432 (4)	0.1432 (4)	0.1432 (4)	0.177 (5)
O1	0.0724 (10)	0.0724 (10)	−0.1226 (14)	0.116 (13)	0.33
O2	0.1348 (6)	0.1348 (6)	−0.2538 (7)	0.204 (7)
O3	0.0752 (9)	0.0752 (9)	0.1099 (12)	0.088 (9)	0.33
C1	0.1055 (9)	0.2482 (12)	0.1055 (9)	0.281 (12)
H1A	0.1147	0.2498	0.0429	0.337*	0.50
H1B	0.0429	0.2498	0.1147	0.337*	0.50
C2	0.1401 (8)	0.3273 (15)	0.1401 (8)	0.279 (10)
H2A	0.2025	0.3295	0.1301	0.335*	0.50
H2B	0.1301	0.3295	0.2025	0.335*	0.50
C3	0.0962 (9)	0.4061 (17)	0.0962 (9)	0.290 (11)
H3A	0.0339	0.4077	0.1070	0.348*	0.50
H3B	0.1070	0.4077	0.0339	0.348*	0.50
C4	0.1451 (11)	0.479 (2)	0.1451 (11)	0.286 (12)
H4A	0.1252	0.5349	0.1246	0.428*
H4B	0.2065	0.4739	0.1346	0.428*	0.50
H4C	0.1339	0.4744	0.2064	0.428*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0657 (3)	0.0657 (3)	0.0657 (3)	0.000	0.000	0.000
Tc1	0.1127 (8)	0.1127 (8)	0.1127 (8)	−0.0223 (6)	0.0223 (6)	0.0223 (6)
P1	0.177 (5)	0.177 (5)	0.177 (5)	−0.045 (4)	−0.045 (4)	−0.045 (4)
O1	0.117 (14)	0.117 (14)	0.112 (19)	−0.018 (14)	0.037 (11)	0.037 (11)
O2	0.255 (12)	0.255 (12)	0.102 (7)	−0.094 (14)	0.007 (5)	0.007 (5)
O3	0.110 (12)	0.110 (12)	0.045 (9)	−0.041 (12)	0.008 (6)	0.008 (6)
C1	0.196 (12)	0.45 (3)	0.196 (12)	−0.053 (11)	−0.087 (15)	−0.053 (11)
C2	0.213 (12)	0.41 (3)	0.213 (12)	−0.030 (9)	−0.073 (14)	−0.030 (9)
C3	0.204 (12)	0.46 (3)	0.204 (12)	−0.001 (11)	−0.064 (14)	−0.001 (11)
C4	0.225 (13)	0.41 (3)	0.225 (13)	−0.001 (14)	−0.016 (18)	−0.001 (14)

Geometric parameters (Å, º) top

Th1—O3ⁱ	2.35 (2)	P1—O3^v	1.56 (2)
Th1—O3ⁱⁱ	2.35 (2)	P1—C1^v	1.807 (17)
Th1—O3ⁱⁱⁱ	2.35 (2)	P1—C1	1.807 (17)
Th1—O3	2.35 (2)	P1—C1^iv	1.807 (17)
Th1—O3^iv	2.35 (2)	O1—O1^viii	1.09 (4)
Th1—O3^v	2.35 (2)	O1—O1^ix	1.09 (4)
Th1—O3^vi	2.35 (2)	O3—O3^iv	0.75 (3)
Th1—O3^vii	2.35 (2)	O3—O3^v	0.75 (3)
Th1—O3^viii	2.35 (2)	C1—C2	1.428 (17)
Th1—O3^ix	2.35 (2)	C1—H1A	0.9700
Th1—O3^x	2.35 (2)	C1—H1B	0.9700
Th1—O3^xi	2.35 (2)	C2—C3	1.539 (18)
Tc1—O2^viii	1.591 (11)	C2—H2A	0.9700
Tc1—O2^ix	1.591 (11)	C2—H2B	0.9700
Tc1—O2	1.591 (11)	C3—C4	1.544 (19)
Tc1—O1^viii	1.82 (2)	C3—H3A	0.9700
Tc1—O1^ix	1.82 (2)	C3—H3B	0.9700
Tc1—O1	1.82 (2)	C4—H4A	0.9600
P1—O3	1.56 (2)	C4—H4B	0.9600
P1—O3^iv	1.56 (2)	C4—H4C	0.9600

O3ⁱ—Th1—O3ⁱⁱ	121.1 (5)	O2^viii—Tc1—O2^ix	108.4 (5)
O3ⁱ—Th1—O3ⁱⁱⁱ	121.1 (5)	O2^viii—Tc1—O2	108.4 (5)
O3ⁱⁱ—Th1—O3ⁱⁱⁱ	88.1 (8)	O2^ix—Tc1—O2	108.4 (5)
O3ⁱ—Th1—O3	88.1 (8)	O2^viii—Tc1—O1^viii	90.4 (9)
O3ⁱⁱ—Th1—O3	121.1 (5)	O2^ix—Tc1—O1^viii	119.4 (5)
O3ⁱⁱⁱ—Th1—O3	121.1 (5)	O2—Tc1—O1^viii	119.4 (5)
O3ⁱ—Th1—O3^iv	104.0 (2)	O2^viii—Tc1—O1^ix	119.4 (5)
O3ⁱⁱ—Th1—O3^iv	117.7 (2)	O2^ix—Tc1—O1^ix	90.4 (9)
O3ⁱⁱⁱ—Th1—O3^iv	104.0 (2)	O2—Tc1—O1^ix	119.4 (5)
O3—Th1—O3^iv	18.4 (7)	O1^viii—Tc1—O1^ix	34.8 (13)
O3ⁱ—Th1—O3^v	104.0 (2)	O2^viii—Tc1—O1	119.4 (5)
O3ⁱⁱ—Th1—O3^v	104.0 (2)	O2^ix—Tc1—O1	119.4 (5)
O3ⁱⁱⁱ—Th1—O3^v	117.7 (2)	O2—Tc1—O1	90.4 (9)
O3—Th1—O3^v	18.4 (7)	O1^viii—Tc1—O1	34.8 (13)
O3^iv—Th1—O3^v	18.4 (7)	O1^ix—Tc1—O1	34.8 (13)
O3ⁱ—Th1—O3^vi	18.4 (7)	O3—P1—O3^iv	27.9 (11)
O3ⁱⁱ—Th1—O3^vi	104.0 (2)	O3—P1—O3^v	27.9 (11)
O3ⁱⁱⁱ—Th1—O3^vi	117.7 (2)	O3^iv—P1—O3^v	27.9 (11)
O3—Th1—O3^vi	104.0 (2)	O3—P1—C1^v	82.2 (10)
O3^iv—Th1—O3^vi	121.1 (5)	O3^iv—P1—C1^v	106.0 (9)
O3^v—Th1—O3^vi	117.7 (2)	O3^v—P1—C1^v	106.0 (9)
O3ⁱ—Th1—O3^vii	18.4 (7)	O3—P1—C1	106.0 (9)
O3ⁱⁱ—Th1—O3^vii	117.7 (2)	O3^iv—P1—C1	82.2 (10)
O3ⁱⁱⁱ—Th1—O3^vii	104.0 (2)	O3^v—P1—C1	106.0 (9)
O3—Th1—O3^vii	104.0 (2)	C1^v—P1—C1	118.0 (4)
O3^iv—Th1—O3^vii	117.7 (2)	O3—P1—C1^iv	106.0 (9)
O3^v—Th1—O3^vii	121.1 (5)	O3^iv—P1—C1^iv	106.0 (9)
O3^vi—Th1—O3^vii	18.4 (7)	O3^v—P1—C1^iv	82.2 (10)
O3ⁱ—Th1—O3^viii	104.0 (2)	C1^v—P1—C1^iv	118.0 (4)
O3ⁱⁱ—Th1—O3^viii	18.4 (7)	C1—P1—C1^iv	118.0 (4)
O3ⁱⁱⁱ—Th1—O3^viii	104.0 (2)	O1^viii—O1—O1^ix	59.993 (4)
O3—Th1—O3^viii	117.7 (2)	O1^viii—O1—Tc1	72.6 (6)
O3^iv—Th1—O3^viii	121.1 (5)	O1^ix—O1—Tc1	72.6 (6)
O3^v—Th1—O3^viii	104.0 (2)	O1^viii—O1—Th1	77.2 (5)
O3^vi—Th1—O3^viii	88.1 (8)	O1^ix—O1—Th1	77.2 (5)
O3^vii—Th1—O3^viii	104.0 (2)	Tc1—O1—Th1	144.9 (13)
O3ⁱ—Th1—O3^ix	104.0 (2)	O3^iv—O3—O3^v	60.002 (8)
O3ⁱⁱ—Th1—O3^ix	104.0 (2)	O3^iv—O3—P1	76.1 (5)
O3ⁱⁱⁱ—Th1—O3^ix	18.4 (7)	O3^v—O3—P1	76.1 (5)
O3—Th1—O3^ix	117.7 (2)	O3^iv—O3—Th1	80.8 (4)
O3^iv—Th1—O3^ix	104.0 (2)	O3^v—O3—Th1	80.8 (4)
O3^v—Th1—O3^ix	121.1 (5)	P1—O3—Th1	153.2 (10)
O3^vi—Th1—O3^ix	104.0 (2)	C2—C1—P1	121.3 (17)
O3^vii—Th1—O3^ix	88.1 (8)	C2—C1—H1A	107.0
O3^viii—Th1—O3^ix	117.7 (2)	P1—C1—H1A	107.0
O3ⁱ—Th1—O3^x	117.7 (2)	C2—C1—H1B	107.0
O3ⁱⁱ—Th1—O3^x	104.0 (2)	P1—C1—H1B	107.0
O3ⁱⁱⁱ—Th1—O3^x	18.4 (7)	H1A—C1—H1B	106.8
O3—Th1—O3^x	104.0 (2)	C1—C2—C3	109.9 (17)
O3^iv—Th1—O3^x	88.1 (8)	C1—C2—H2A	109.7
O3^v—Th1—O3^x	104.0 (2)	C3—C2—H2A	109.7
O3^vi—Th1—O3^x	121.1 (5)	C1—C2—H2B	109.7
O3^vii—Th1—O3^x	104.0 (2)	C3—C2—H2B	109.7
O3^viii—Th1—O3^x	121.1 (5)	H2A—C2—H2B	108.2
O3^ix—Th1—O3^x	18.4 (7)	C2—C3—C4	98.3 (17)
O3ⁱ—Th1—O3^xi	117.7 (2)	C2—C3—H3A	112.1
O3ⁱⁱ—Th1—O3^xi	18.4 (7)	C4—C3—H3A	112.1
O3ⁱⁱⁱ—Th1—O3^xi	104.0 (2)	C2—C3—H3B	112.1
O3—Th1—O3^xi	104.0 (2)	C4—C3—H3B	112.1
O3^iv—Th1—O3^xi	104.0 (2)	H3A—C3—H3B	109.7
O3^v—Th1—O3^xi	88.1 (8)	C3—C4—H4A	109.5
O3^vi—Th1—O3^xi	104.0 (2)	C3—C4—H4B	109.5
O3^vii—Th1—O3^xi	121.1 (5)	H4A—C4—H4B	109.5
O3^viii—Th1—O3^xi	18.4 (7)	C3—C4—H4C	109.5
O3^ix—Th1—O3^xi	121.1 (5)	H4A—C4—H4C	109.5
O3^x—Th1—O3^xi	117.7 (2)	H4B—C4—H4C	109.5

O2^viii—Tc1—O1—O1^viii	−37.0 (3)	C1^v—P1—O3—O3^iv	148.99 (8)
O2^ix—Tc1—O1—O1^viii	100.2 (5)	C1—P1—O3—O3^iv	32.1 (2)
O2—Tc1—O1—O1^viii	−148.41 (12)	C1^iv—P1—O3—O3^iv	−94.1 (3)
O1^ix—Tc1—O1—O1^viii	63.2 (2)	O3^iv—P1—O3—O3^v	62.02 (16)
O2^viii—Tc1—O1—O1^ix	−100.2 (5)	C1^v—P1—O3—O3^v	−148.99 (8)
O2^ix—Tc1—O1—O1^ix	37.0 (3)	C1—P1—O3—O3^v	94.1 (3)
O2—Tc1—O1—O1^ix	148.41 (12)	C1^iv—P1—O3—O3^v	−32.1 (2)
O1^viii—Tc1—O1—O1^ix	−63.2 (2)	O3^iv—P1—O3—Th1	31.01 (8)
O2^viii—Tc1—O1—Th1	−68.6 (4)	O3^v—P1—O3—Th1	−31.01 (8)
O2^ix—Tc1—O1—Th1	68.6 (4)	C1^v—P1—O3—Th1	180.0
O2—Tc1—O1—Th1	180.0	C1—P1—O3—Th1	63.1 (3)
O1^viii—Tc1—O1—Th1	−31.59 (12)	C1^iv—P1—O3—Th1	−63.1 (3)
O1^ix—Tc1—O1—Th1	31.59 (12)	O3ⁱ—Th1—O3—O3^iv	−149.56 (3)
O3ⁱ—Th1—O1—O1^viii	149.15 (7)	O3ⁱⁱ—Th1—O3—O3^iv	84.74 (15)
O3ⁱⁱ—Th1—O1—O1^viii	−154.4 (5)	O3ⁱⁱⁱ—Th1—O3—O3^iv	−23.9 (2)
O3ⁱⁱⁱ—Th1—O1—O1^viii	92.7 (6)	O3^v—Th1—O3—O3^iv	60.87 (7)
O3—Th1—O1—O1^viii	−30.85 (7)	O3^vi—Th1—O3—O3^iv	−159.1 (3)
O3^iv—Th1—O1—O1^viii	−21.5 (4)	O3^vii—Th1—O3—O3^iv	−140.1 (4)
O3^v—Th1—O1—O1^viii	−40.2 (3)	O3^viii—Th1—O3—O3^iv	105.6 (7)
O3^vi—Th1—O1—O1^viii	174.3 (11)	O3^ix—Th1—O3—O3^iv	−44.7 (6)
O3^vii—Th1—O1—O1^viii	124.0 (10)	O3^x—Th1—O3—O3^iv	−31.450 (14)
O3^viii—Th1—O1—O1^viii	−147.97 (15)	O3^xi—Th1—O3—O3^iv	92.32 (5)
O3^ix—Th1—O1—O1^viii	86.3 (3)	O3ⁱ—Th1—O3—O3^v	149.56 (3)
O3^x—Th1—O1—O1^viii	71.8 (5)	O3ⁱⁱ—Th1—O3—O3^v	23.9 (2)
O3^xi—Th1—O1—O1^viii	−133.5 (4)	O3ⁱⁱⁱ—Th1—O3—O3^v	−84.74 (16)
O3ⁱ—Th1—O1—O1^ix	−149.15 (7)	O3^iv—Th1—O3—O3^v	−60.87 (7)
O3ⁱⁱ—Th1—O1—O1^ix	−92.7 (6)	O3^vi—Th1—O3—O3^v	140.1 (4)
O3ⁱⁱⁱ—Th1—O1—O1^ix	154.4 (5)	O3^vii—Th1—O3—O3^v	159.1 (3)
O3—Th1—O1—O1^ix	30.85 (7)	O3^viii—Th1—O3—O3^v	44.7 (6)
O3^iv—Th1—O1—O1^ix	40.2 (3)	O3^ix—Th1—O3—O3^v	−105.6 (7)
O3^v—Th1—O1—O1^ix	21.5 (4)	O3^x—Th1—O3—O3^v	−92.32 (5)
O3^vi—Th1—O1—O1^ix	−124.0 (10)	O3^xi—Th1—O3—O3^v	31.449 (13)
O3^vii—Th1—O1—O1^ix	−174.3 (11)	O3ⁱ—Th1—O3—P1	180.0
O3^viii—Th1—O1—O1^ix	−86.3 (3)	O3ⁱⁱ—Th1—O3—P1	54.30 (19)
O3^ix—Th1—O1—O1^ix	147.97 (15)	O3ⁱⁱⁱ—Th1—O3—P1	−54.30 (19)
O3^x—Th1—O1—O1^ix	133.5 (4)	O3^iv—Th1—O3—P1	−30.44 (3)
O3^xi—Th1—O1—O1^ix	−71.8 (5)	O3^v—Th1—O3—P1	30.44 (3)
O3ⁱ—Th1—O1—Tc1	180.001 (3)	O3^vi—Th1—O3—P1	170.5 (4)
O3ⁱⁱ—Th1—O1—Tc1	−123.5 (6)	O3^vii—Th1—O3—P1	−170.5 (4)
O3ⁱⁱⁱ—Th1—O1—Tc1	123.5 (6)	O3^viii—Th1—O3—P1	75.1 (7)
O3—Th1—O1—Tc1	0.0	O3^ix—Th1—O3—P1	−75.1 (7)
O3^iv—Th1—O1—Tc1	9.4 (4)	O3^x—Th1—O3—P1	−61.89 (2)
O3^v—Th1—O1—Tc1	−9.4 (4)	O3^xi—Th1—O3—P1	61.88 (2)
O3^vi—Th1—O1—Tc1	−154.9 (10)	O3—P1—C1—C2	165.5 (6)
O3^vii—Th1—O1—Tc1	154.9 (10)	O3^iv—P1—C1—C2	180.001 (2)
O3^viii—Th1—O1—Tc1	−117.1 (2)	O3^v—P1—C1—C2	−165.5 (6)
O3^ix—Th1—O1—Tc1	117.1 (2)	C1^v—P1—C1—C2	76.0 (13)
O3^x—Th1—O1—Tc1	102.7 (4)	C1^iv—P1—C1—C2	−76.0 (13)
O3^xi—Th1—O1—Tc1	−102.7 (4)	P1—C1—C2—C3	180.000 (2)
O3^v—P1—O3—O3^iv	−62.02 (16)	C1—C2—C3—C4	180.000 (3)

Symmetry codes: (i) −x, −y, z; (ii) x, −y, −z; (iii) −x, y, −z; (iv) y, z, x; (v) z, x, y; (vi) −y, −z, x; (vii) −z, −x, y; (viii) y, −z, −x; (ix) −z, x, −y; (x) −y, z, −x; (xi) z, −x, −y.

(IIIat230) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	D_x = 1.708 Mg m⁻³
M_r = 1753.26	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmc2₁	Cell parameters from 5437 reflections
a = 21.444 (2) Å	θ = 2.7–25.9°
b = 21.582 (2) Å	µ = 3.12 mm⁻¹
c = 14.736 (2) Å	T = 230 K
V = 6819.9 (13) Å³	Block, colourless
Z = 4	0.10 × 0.10 × 0.10 mm
F(000) = 3512

Data collection top

CCD area detector diffractometer	7255 independent reflections
Radiation source: fine-focus sealed tube	6041 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.055
phi and ω scans	θ_max = 26.5°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −26→26
T_min = 0.746, T_max = 0.746	k = −26→26
26789 measured reflections	l = −17→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.037	H-atom parameters constrained
wR(F²) = 0.088	w = 1/[σ²(F_o²) + (0.0428P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max = 0.004
7255 reflections	Δρ_max = 1.43 e Å⁻³
354 parameters	Δρ_min = −0.77 e Å⁻³
57 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.034 (7)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	V = 6819.9 (13) Å³
M_r = 1753.26	Z = 4
Orthorhombic, Cmc2₁	Mo Kα radiation
a = 21.444 (2) Å	µ = 3.12 mm⁻¹
b = 21.582 (2) Å	T = 230 K
c = 14.736 (2) Å	0.10 × 0.10 × 0.10 mm

Data collection top

CCD area detector diffractometer	7255 independent reflections
Absorption correction: multi-scan SADABS	6041 reflections with I > 2σ(I)
T_min = 0.746, T_max = 0.746	R_int = 0.055
26789 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	H-atom parameters constrained
wR(F²) = 0.088	Δρ_max = 1.43 e Å⁻³
S = 0.97	Δρ_min = −0.77 e Å⁻³
7255 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
354 parameters	Absolute structure parameter: 0.034 (7)
57 restraints

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.0000	0.252390 (18)	0.29670 (4)	0.03378 (9)
Tc1	0.14670 (4)	0.24064 (4)	0.12697 (6)	0.0547 (2)
Tc2	0.0000	0.40819 (5)	0.44940 (9)	0.0497 (3)
Tc3	0.0000	0.11885 (5)	0.48817 (8)	0.0522 (3)
P1	0.15719 (12)	0.26123 (13)	0.4123 (2)	0.0581 (7)
P2	0.0000	0.3926 (2)	0.1491 (3)	0.0823 (15)
P3	0.0000	0.09153 (19)	0.1978 (3)	0.0742 (12)
O1	0.0734 (3)	0.2490 (3)	0.1709 (5)	0.071 (2)
O2	0.1928 (4)	0.2943 (4)	0.1704 (7)	0.100 (3)
O3	0.1443 (5)	0.2490 (3)	0.0148 (6)	0.092 (3)
O4	0.1757 (4)	0.1704 (4)	0.1500 (6)	0.094 (3)
O5	0.1005 (3)	0.2522 (3)	0.3538 (5)	0.068 (2)
O6	0.0000	0.3313 (5)	0.4112 (7)	0.082 (4)
O7	0.0000	0.4045 (7)	0.5599 (8)	0.121 (5)
O8	0.0611 (5)	0.4457 (4)	0.4150 (8)	0.122 (4)
O9	0.0000	0.3466 (4)	0.2251 (7)	0.089 (4)
O10	0.0000	0.1882 (4)	0.4329 (7)	0.070 (3)
O11	0.0585 (6)	0.0760 (5)	0.4627 (6)	0.134 (4)
O12	0.0000	0.1320 (5)	0.5968 (7)	0.102 (4)
O13	0.0000	0.1516 (4)	0.2453 (7)	0.075 (3)
C1	0.1473 (6)	0.2430 (5)	0.5296 (8)	0.076 (3)
H1A	0.1343	0.2001	0.5347	0.091*
H1B	0.1873	0.2470	0.5598	0.091*
C2	0.1027 (6)	0.2811 (6)	0.5762 (9)	0.096 (4)
H2A	0.0642	0.2814	0.5416	0.115*
H2B	0.1183	0.3232	0.5780	0.115*
C3	0.0875 (8)	0.2598 (7)	0.6766 (9)	0.122 (6)
H3A	0.0542	0.2854	0.7008	0.146*
H3B	0.0730	0.2172	0.6758	0.146*
C4	0.1422 (7)	0.2646 (7)	0.7357 (10)	0.116 (6)
H4A	0.1794	0.2614	0.6998	0.174*
H4B	0.1414	0.2317	0.7795	0.174*
H4C	0.1417	0.3038	0.7664	0.174*
C5	0.1846 (5)	0.3381 (5)	0.3952 (7)	0.065 (3)
H5A	0.1925	0.3434	0.3308	0.078*
H5B	0.1511	0.3663	0.4112	0.078*
C6	0.2414 (5)	0.3580 (4)	0.4450 (8)	0.072 (3)
H6A	0.2755	0.3306	0.4290	0.086*
H6B	0.2340	0.3537	0.5096	0.086*
C7	0.2608 (5)	0.4243 (4)	0.4255 (8)	0.071 (3)
H7A	0.2675	0.4288	0.3607	0.085*
H7B	0.2270	0.4517	0.4425	0.085*
C8	0.3181 (7)	0.4437 (6)	0.4740 (9)	0.116 (5)
H8A	0.3454	0.4088	0.4810	0.174*
H8B	0.3072	0.4596	0.5327	0.174*
H8C	0.3389	0.4754	0.4398	0.174*
C9	0.2159 (5)	0.2116 (5)	0.3818 (8)	0.082 (4)
H9A	0.2286	0.2216	0.3204	0.099*
H9B	0.2513	0.2194	0.4211	0.099*
C10	0.2009 (5)	0.1430 (5)	0.3858 (9)	0.084 (4)
H10A	0.1892	0.1329	0.4476	0.101*
H10B	0.1647	0.1355	0.3478	0.101*
C11	0.2509 (6)	0.0994 (5)	0.3574 (9)	0.087 (4)
H11A	0.2337	0.0580	0.3524	0.105*
H11B	0.2664	0.1114	0.2981	0.105*
C12	0.3023 (6)	0.0987 (6)	0.4216 (11)	0.111 (5)
H12A	0.3327	0.1291	0.4041	0.167*
H12B	0.3213	0.0584	0.4219	0.167*
H12C	0.2870	0.1081	0.4812	0.167*
C13A	−0.0500 (8)	0.4546 (9)	0.1684 (19)	0.111 (6)*	0.605 (19)
H13A	−0.0343	0.4787	0.2190	0.133*	0.605 (19)
H13B	−0.0500	0.4812	0.1153	0.133*	0.605 (19)
C13B	−0.0755 (10)	0.4234 (17)	0.1134 (17)	0.111 (6)*	0.395 (19)
H13C	−0.0691	0.4612	0.0790	0.133*	0.395 (19)
H13D	−0.0959	0.3936	0.0741	0.133*	0.395 (19)
C14	−0.1139 (7)	0.4359 (8)	0.1879 (12)	0.147 (5)
H14A	−0.1130	0.4139	0.2453	0.177*
H14B	−0.1255	0.4058	0.1420	0.177*
C15	−0.1663 (8)	0.4816 (7)	0.1937 (12)	0.143 (5)
H15A	−0.2043	0.4592	0.1796	0.172*
H15B	−0.1694	0.4941	0.2568	0.172*
C16	−0.1673 (7)	0.5385 (7)	0.1395 (12)	0.141 (6)
H16A	−0.1387	0.5680	0.1649	0.212*
H16B	−0.2087	0.5555	0.1398	0.212*
H16C	−0.1553	0.5291	0.0782	0.212*
C17	0.0000	0.3538 (7)	0.0417 (11)	0.076 (4)*
H17A	0.0366	0.3275	0.0378	0.091*	0.50
H17B	−0.0366	0.3275	0.0378	0.091*	0.50
C18	0.0000	0.3959 (7)	−0.0328 (9)	0.083 (5)*
H18A	0.0366	0.4222	−0.0294	0.100*	0.50
H18B	−0.0366	0.4222	−0.0294	0.100*	0.50
C19	0.0000	0.3605 (8)	−0.1244 (12)	0.084 (5)*
H19A	0.0367	0.3343	−0.1283	0.101*	0.50
H19B	−0.0367	0.3343	−0.1283	0.101*	0.50
C20	0.0000	0.4064 (10)	−0.2012 (19)	0.127 (7)*
H20A	0.0000	0.3846	−0.2580	0.190*
H20B	0.0366	0.4320	−0.1973	0.190*	0.50
H20C	−0.0366	0.4320	−0.1973	0.190*	0.50
C21	−0.0697 (6)	0.0530 (6)	0.2307 (9)	0.101 (5)
H21A	−0.0671	0.0443	0.2951	0.121*
H21B	−0.1042	0.0815	0.2220	0.121*
C22	−0.0853 (5)	−0.0058 (6)	0.1833 (10)	0.101 (4)
H22A	−0.0869	0.0019	0.1185	0.121*
H22B	−0.0522	−0.0356	0.1943	0.121*
C23	−0.1452 (6)	−0.0333 (7)	0.2123 (11)	0.133 (7)
H23A	−0.1427	−0.0410	0.2771	0.160*
H23B	−0.1775	−0.0024	0.2031	0.160*
C24	−0.1656 (6)	−0.0905 (6)	0.1685 (13)	0.145 (7)
H24A	−0.1768	−0.0820	0.1067	0.218*
H24B	−0.2010	−0.1069	0.2002	0.218*
H24C	−0.1323	−0.1202	0.1699	0.218*
C25	0.0267 (11)	0.0976 (12)	0.0829 (11)	0.099 (8)*	0.50
H25A	0.0713	0.1052	0.0852	0.118*	0.50
H25B	0.0211	0.0573	0.0550	0.118*	0.50
C26	0.0000	0.1434 (11)	0.0213 (15)	0.154 (9)*
H26A	0.0184	0.1825	0.0396	0.185*	0.50
H26B	−0.0436	0.1459	0.0383	0.185*	0.50
C27	0.0000	0.1451 (13)	−0.0806 (16)	0.170 (10)*
H27A	−0.0440	0.1456	−0.0959	0.204*	0.50
H27B	0.0150	0.1864	−0.0944	0.204*	0.50
C28	0.027 (3)	0.107 (2)	−0.152 (2)	0.29 (3)*	0.50
H28A	−0.0048	0.0832	−0.1806	0.440*	0.50
H28B	0.0579	0.0800	−0.1261	0.440*	0.50
H28C	0.0468	0.1335	−0.1962	0.440*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.02838 (17)	0.03701 (19)	0.03595 (15)	0.000	0.000	−0.0021 (2)
Tc1	0.0442 (5)	0.0639 (5)	0.0559 (5)	0.0067 (4)	0.0138 (4)	0.0002 (5)
Tc2	0.0632 (7)	0.0427 (6)	0.0431 (5)	0.000	0.000	−0.0068 (5)
Tc3	0.0508 (7)	0.0550 (6)	0.0507 (6)	0.000	0.000	0.0144 (5)
P1	0.0442 (14)	0.0778 (18)	0.0524 (15)	−0.0067 (12)	−0.0095 (12)	0.0027 (12)
P2	0.137 (5)	0.049 (2)	0.060 (3)	0.000	0.000	0.012 (2)
P3	0.093 (3)	0.052 (2)	0.077 (3)	0.000	0.000	−0.022 (2)
O1	0.046 (4)	0.118 (7)	0.050 (4)	−0.005 (4)	0.016 (3)	−0.009 (3)
O2	0.058 (5)	0.094 (6)	0.149 (8)	−0.011 (4)	0.002 (5)	−0.009 (6)
O3	0.088 (6)	0.125 (8)	0.062 (5)	0.018 (4)	0.020 (5)	0.019 (4)
O4	0.118 (7)	0.083 (5)	0.080 (5)	0.040 (5)	0.009 (5)	0.008 (4)
O5	0.047 (4)	0.101 (6)	0.057 (4)	−0.005 (3)	−0.005 (3)	−0.002 (4)
O6	0.142 (11)	0.059 (6)	0.046 (6)	0.000	0.000	−0.008 (5)
O7	0.153 (13)	0.143 (12)	0.068 (7)	0.000	0.000	0.048 (8)
O8	0.136 (8)	0.059 (5)	0.171 (9)	−0.027 (5)	0.074 (7)	−0.026 (5)
O9	0.180 (12)	0.027 (5)	0.059 (6)	0.000	0.000	0.005 (4)
O10	0.077 (7)	0.070 (6)	0.063 (6)	0.000	0.000	0.009 (5)
O11	0.167 (11)	0.134 (8)	0.100 (8)	0.073 (7)	0.048 (6)	0.035 (6)
O12	0.155 (12)	0.089 (8)	0.063 (7)	0.000	0.000	0.009 (6)
O13	0.111 (9)	0.036 (5)	0.076 (7)	0.000	0.000	−0.023 (5)
C1	0.080 (9)	0.084 (8)	0.063 (7)	0.003 (6)	−0.004 (7)	−0.005 (6)
C2	0.073 (9)	0.101 (9)	0.114 (10)	0.007 (7)	−0.002 (7)	−0.005 (8)
C3	0.126 (14)	0.161 (15)	0.077 (9)	0.035 (11)	−0.013 (9)	−0.020 (9)
C4	0.105 (12)	0.129 (13)	0.114 (13)	−0.034 (9)	0.006 (10)	−0.036 (10)
C5	0.052 (6)	0.084 (7)	0.059 (6)	0.007 (5)	−0.008 (4)	0.007 (5)
C6	0.059 (6)	0.072 (6)	0.085 (6)	−0.005 (5)	−0.024 (6)	0.012 (6)
C7	0.063 (7)	0.062 (6)	0.088 (8)	0.002 (5)	−0.006 (6)	0.016 (5)
C8	0.104 (11)	0.116 (10)	0.128 (13)	−0.040 (9)	−0.045 (9)	0.024 (10)
C9	0.066 (7)	0.077 (8)	0.103 (9)	−0.011 (6)	−0.044 (7)	0.015 (7)
C10	0.078 (8)	0.084 (8)	0.090 (8)	−0.038 (7)	−0.021 (7)	−0.002 (7)
C11	0.105 (10)	0.066 (7)	0.091 (9)	−0.009 (7)	−0.018 (7)	0.003 (6)
C12	0.103 (11)	0.090 (9)	0.141 (13)	0.026 (8)	−0.027 (10)	0.005 (9)
C14	0.131 (10)	0.152 (9)	0.158 (10)	0.013 (7)	0.039 (9)	0.069 (9)
C15	0.130 (12)	0.147 (12)	0.153 (12)	0.007 (8)	0.017 (11)	0.036 (9)
C16	0.128 (14)	0.173 (13)	0.124 (12)	0.018 (10)	−0.019 (11)	0.045 (11)
C21	0.076 (9)	0.099 (9)	0.127 (12)	0.008 (7)	−0.022 (8)	−0.055 (9)
C22	0.074 (9)	0.096 (9)	0.132 (11)	0.008 (7)	−0.014 (8)	−0.040 (8)
C23	0.060 (9)	0.169 (15)	0.170 (15)	−0.038 (9)	0.044 (9)	−0.100 (13)
C24	0.072 (10)	0.130 (13)	0.23 (2)	−0.042 (9)	0.006 (11)	−0.071 (13)

Geometric parameters (Å, º) top

Th1—O9	2.290 (9)	C9—H9B	0.9700
Th1—O13	2.302 (8)	C10—C11	1.487 (16)
Th1—O5ⁱ	2.313 (7)	C10—H10A	0.9700
Th1—O5	2.314 (7)	C10—H10B	0.9700
Th1—O6	2.398 (10)	C11—C12	1.452 (17)
Th1—O1ⁱ	2.433 (7)	C11—H11A	0.9700
Th1—O1	2.433 (7)	C11—H11B	0.9700
Th1—O10	2.438 (10)	C12—H12A	0.9600
Tc1—O2	1.651 (9)	C12—H12B	0.9600
Tc1—O3	1.663 (9)	C12—H12C	0.9600
Tc1—O4	1.672 (7)	C13A—C14	1.457 (16)
Tc1—O1	1.710 (7)	C13A—H13A	0.9700
Tc2—O8	1.621 (8)	C13A—H13B	0.9700
Tc2—O8ⁱ	1.621 (8)	C13B—C14	1.400 (18)
Tc2—O7	1.630 (11)	C13B—H13C	0.9700
Tc2—O6	1.752 (10)	C13B—H13D	0.9700
Tc3—O11ⁱ	1.603 (9)	C14—C15	1.497 (14)
Tc3—O11	1.603 (9)	C14—H14A	0.9700
Tc3—O12	1.626 (11)	C14—H14B	0.9700
Tc3—O10	1.705 (10)	C15—C16	1.465 (14)
P1—O5	1.503 (8)	C15—H15A	0.9700
P1—C9	1.712 (12)	C15—H15B	0.9700
P1—C5	1.779 (11)	C16—H16A	0.9600
P1—C1	1.785 (12)	C16—H16B	0.9600
P2—O9	1.497 (11)	C16—H16C	0.9600
P2—C13A	1.737 (15)	C17—C18	1.42 (2)
P2—C13Aⁱ	1.737 (15)	C17—H17A	0.9700
P2—C17	1.791 (17)	C17—H17B	0.9700
P2—C13B	1.827 (18)	C18—C19	1.55 (2)
P2—C13Bⁱ	1.827 (18)	C18—H18A	0.9700
P3—O13	1.474 (9)	C18—H18B	0.9700
P3—C21	1.778 (14)	C19—C20	1.51 (3)
P3—C21ⁱ	1.778 (14)	C19—H19A	0.9700
P3—C25ⁱ	1.793 (15)	C19—H19B	0.9700
P3—C25	1.793 (15)	C20—H20A	0.9600
C1—C2	1.436 (13)	C20—H20B	0.9600
C1—H1A	0.9700	C20—H20C	0.9600
C1—H1B	0.9700	C21—C22	1.487 (15)
C2—C3	1.583 (14)	C21—H21A	0.9700
C2—H2A	0.9700	C21—H21B	0.9700
C2—H2B	0.9700	C22—C23	1.477 (17)
C3—C4	1.465 (15)	C22—H22A	0.9700
C3—H3A	0.9700	C22—H22B	0.9700
C3—H3B	0.9700	C23—C24	1.460 (13)
C4—H4A	0.9600	C23—H23A	0.9700
C4—H4B	0.9600	C23—H23B	0.9700
C4—H4C	0.9600	C24—H24A	0.9600
C5—C6	1.486 (13)	C24—H24B	0.9600
C5—H5A	0.9700	C24—H24C	0.9600
C5—H5B	0.9700	C25—C26	1.458 (17)
C6—C7	1.517 (12)	C25—H25A	0.9700
C6—H6A	0.9700	C25—H25B	0.9700
C6—H6B	0.9700	C26—C27	1.503 (17)
C7—C8	1.483 (16)	C26—H26A	0.9700
C7—H7A	0.9700	C26—H26B	0.9700
C7—H7B	0.9700	C27—C28	1.454 (19)
C8—H8A	0.9600	C27—H27A	0.9700
C8—H8B	0.9600	C27—H27B	0.9700
C8—H8C	0.9600	C28—H28A	0.9600
C9—C10	1.516 (14)	C28—H28B	0.9600
C9—H9A	0.9700	C28—H28C	0.9600

O9—Th1—O13	133.4 (4)	C10—C9—P1	116.5 (9)
O9—Th1—O5ⁱ	99.72 (18)	C10—C9—H9A	108.2
O13—Th1—O5ⁱ	96.79 (18)	P1—C9—H9A	108.2
O9—Th1—O5	99.72 (18)	C10—C9—H9B	108.2
O13—Th1—O5	96.79 (18)	P1—C9—H9B	108.2
O5ⁱ—Th1—O5	137.4 (4)	H9A—C9—H9B	107.3
O9—Th1—O6	72.2 (4)	C11—C10—C9	117.1 (10)
O13—Th1—O6	154.5 (4)	C11—C10—H10A	108.0
O5ⁱ—Th1—O6	75.23 (18)	C9—C10—H10A	108.0
O5—Th1—O6	75.23 (18)	C11—C10—H10B	108.0
O9—Th1—O1ⁱ	71.1 (3)	C9—C10—H10B	108.0
O13—Th1—O1ⁱ	73.8 (3)	H10A—C10—H10B	107.3
O5ⁱ—Th1—O1ⁱ	71.0 (3)	C12—C11—C10	111.8 (11)
O5—Th1—O1ⁱ	151.6 (3)	C12—C11—H11A	109.3
O6—Th1—O1ⁱ	123.9 (2)	C10—C11—H11A	109.3
O9—Th1—O1	71.1 (3)	C12—C11—H11B	109.3
O13—Th1—O1	73.8 (3)	C10—C11—H11B	109.3
O5ⁱ—Th1—O1	151.6 (3)	H11A—C11—H11B	107.9
O5—Th1—O1	71.0 (3)	C11—C12—H12A	109.5
O6—Th1—O1	123.9 (2)	C11—C12—H12B	109.5
O1ⁱ—Th1—O1	80.6 (4)	H12A—C12—H12B	109.5
O9—Th1—O10	152.0 (4)	C11—C12—H12C	109.5
O13—Th1—O10	74.6 (3)	H12A—C12—H12C	109.5
O5ⁱ—Th1—O10	72.54 (18)	H12B—C12—H12C	109.5
O5—Th1—O10	72.54 (18)	C14—C13A—P2	113.6 (13)
O6—Th1—O10	79.9 (4)	C14—C13A—H13A	108.9
O1ⁱ—Th1—O10	127.6 (2)	P2—C13A—H13A	108.8
O1—Th1—O10	127.6 (2)	C14—C13A—H13B	108.8
O2—Tc1—O3	109.1 (5)	P2—C13A—H13B	108.8
O2—Tc1—O4	109.5 (4)	H13A—C13A—H13B	107.7
O3—Tc1—O4	108.2 (4)	C14—C13B—P2	111.4 (16)
O2—Tc1—O1	109.3 (4)	C14—C13B—H13C	109.3
O3—Tc1—O1	109.6 (4)	P2—C13B—H13C	109.3
O4—Tc1—O1	111.1 (4)	C14—C13B—H13D	109.3
O8—Tc2—O8ⁱ	107.9 (8)	P2—C13B—H13D	109.3
O8—Tc2—O7	109.6 (5)	H13C—C13B—H13D	108.0
O8ⁱ—Tc2—O7	109.6 (5)	C13B—C14—C13A	49.0 (15)
O8—Tc2—O6	111.9 (3)	C13B—C14—C15	127.9 (16)
O8ⁱ—Tc2—O6	111.9 (3)	C13A—C14—C15	122.3 (14)
O7—Tc2—O6	105.9 (6)	C13B—C14—H14A	125.3
O11ⁱ—Tc3—O11	103.0 (10)	C13A—C14—H14A	106.7
O11ⁱ—Tc3—O12	109.3 (4)	C15—C14—H14A	106.7
O11—Tc3—O12	109.3 (4)	C13B—C14—H14B	58.3
O11ⁱ—Tc3—O10	113.3 (4)	C13A—C14—H14B	106.7
O11—Tc3—O10	113.3 (4)	C15—C14—H14B	106.7
O12—Tc3—O10	108.5 (6)	H14A—C14—H14B	106.6
O5—P1—C9	111.3 (5)	C16—C15—C14	122.1 (14)
O5—P1—C5	107.8 (4)	C16—C15—H15A	106.8
C9—P1—C5	107.7 (5)	C14—C15—H15A	106.8
O5—P1—C1	115.5 (5)	C16—C15—H15B	106.8
C9—P1—C1	101.8 (6)	C14—C15—H15B	106.8
C5—P1—C1	112.5 (5)	H15A—C15—H15B	106.6
O9—P2—C13A	112.9 (9)	C15—C16—H16A	109.5
O9—P2—C13Aⁱ	112.9 (9)	C15—C16—H16B	109.5
C13A—P2—C13Aⁱ	76.3 (14)	H16A—C16—H16B	109.5
O9—P2—C17	110.5 (7)	C15—C16—H16C	109.5
C13A—P2—C17	120.3 (10)	H16A—C16—H16C	109.5
C13Aⁱ—P2—C17	120.3 (10)	H16B—C16—H16C	109.5
O9—P2—C13B	117.2 (10)	C18—C17—P2	112.6 (11)
C13A—P2—C13B	38.8 (11)	C18—C17—H17A	109.1
C13Aⁱ—P2—C13B	108.3 (14)	P2—C17—H17A	109.1
C17—P2—C13B	85.1 (9)	C18—C17—H17B	109.1
O9—P2—C13Bⁱ	117.2 (10)	P2—C17—H17B	109.1
C13A—P2—C13Bⁱ	108.3 (14)	H17A—C17—H17B	107.8
C13Aⁱ—P2—C13Bⁱ	38.8 (11)	C17—C18—C19	110.9 (13)
C17—P2—C13Bⁱ	85.1 (9)	C17—C18—H18A	109.5
C13B—P2—C13Bⁱ	125 (2)	C19—C18—H18A	109.5
O13—P3—C21	106.4 (4)	C17—C18—H18B	109.5
O13—P3—C21ⁱ	106.4 (4)	C19—C18—H18B	109.5
C21—P3—C21ⁱ	114.5 (9)	H18A—C18—H18B	108.0
O13—P3—C25ⁱ	112.6 (10)	C20—C19—C18	109.3 (16)
C21—P3—C25ⁱ	91.3 (8)	C20—C19—H19A	109.8
C21ⁱ—P3—C25ⁱ	124.1 (10)	C18—C19—H19A	109.8
O13—P3—C25	112.6 (10)	C20—C19—H19B	109.8
C21—P3—C25	124.1 (10)	C18—C19—H19B	109.8
C21ⁱ—P3—C25	91.3 (8)	H19A—C19—H19B	108.3
C25ⁱ—P3—C25	37.3 (15)	C19—C20—H20A	109.5
Tc1—O1—Th1	152.4 (4)	C19—C20—H20B	109.5
P1—O5—Th1	164.1 (5)	H20A—C20—H20B	109.5
Tc2—O6—Th1	154.0 (6)	C19—C20—H20C	109.5
P2—O9—Th1	159.1 (7)	H20A—C20—H20C	109.5
Tc3—O10—Th1	153.1 (6)	H20B—C20—H20C	109.5
P3—O13—Th1	170.8 (7)	C22—C21—P3	117.4 (10)
C2—C1—P1	114.6 (9)	C22—C21—H21A	107.9
C2—C1—H1A	108.6	P3—C21—H21A	107.9
P1—C1—H1A	108.6	C22—C21—H21B	107.9
C2—C1—H1B	108.6	P3—C21—H21B	107.9
P1—C1—H1B	108.6	H21A—C21—H21B	107.2
H1A—C1—H1B	107.6	C23—C22—C21	113.7 (11)
C1—C2—C3	114.7 (11)	C23—C22—H22A	108.8
C1—C2—H2A	108.6	C21—C22—H22A	108.8
C3—C2—H2A	108.6	C23—C22—H22B	108.8
C1—C2—H2B	108.6	C21—C22—H22B	108.8
C3—C2—H2B	108.6	H22A—C22—H22B	107.7
H2A—C2—H2B	107.6	C24—C23—C22	118.1 (11)
C4—C3—C2	111.7 (13)	C24—C23—H23A	107.8
C4—C3—H3A	109.3	C22—C23—H23A	107.8
C2—C3—H3A	109.3	C24—C23—H23B	107.8
C4—C3—H3B	109.3	C22—C23—H23B	107.8
C2—C3—H3B	109.3	H23A—C23—H23B	107.1
H3A—C3—H3B	107.9	C23—C24—H24A	109.5
C3—C4—H4A	109.5	C23—C24—H24B	109.5
C3—C4—H4B	109.5	H24A—C24—H24B	109.5
H4A—C4—H4B	109.5	C23—C24—H24C	109.5
C3—C4—H4C	109.5	H24A—C24—H24C	109.5
H4A—C4—H4C	109.5	H24B—C24—H24C	109.5
H4B—C4—H4C	109.5	C26—C25—P3	120.8 (16)
C6—C5—P1	118.0 (7)	C26—C25—H25A	107.1
C6—C5—H5A	107.8	P3—C25—H25A	107.1
P1—C5—H5A	107.8	C26—C25—H25B	107.1
C6—C5—H5B	107.8	P3—C25—H25B	107.1
P1—C5—H5B	107.8	H25A—C25—H25B	106.8
H5A—C5—H5B	107.1	C25—C26—C27	129.7 (19)
C5—C6—C7	113.8 (9)	C25—C26—H26A	104.9
C5—C6—H6A	108.8	C27—C26—H26A	104.9
C7—C6—H6A	108.8	C25—C26—H26B	104.9
C5—C6—H6B	108.8	C27—C26—H26B	104.9
C7—C6—H6B	108.8	H26A—C26—H26B	105.8
H6A—C6—H6B	107.7	C28—C27—C26	135 (3)
C8—C7—C6	113.8 (9)	C28—C27—H27A	103.4
C8—C7—H7A	108.8	C26—C27—H27A	103.4
C6—C7—H7A	108.8	C28—C27—H27B	103.4
C8—C7—H7B	108.8	C26—C27—H27B	103.4
C6—C7—H7B	108.8	H27A—C27—H27B	105.2
H7A—C7—H7B	107.7	C27—C28—H28A	109.5
C7—C8—H8A	109.5	C27—C28—H28B	109.5
C7—C8—H8B	109.5	H28A—C28—H28B	109.5
H8A—C8—H8B	109.5	C27—C28—H28C	109.5
C7—C8—H8C	109.5	H28A—C28—H28C	109.5
H8A—C8—H8C	109.5	H28B—C28—H28C	109.5
H8B—C8—H8C	109.5

O2—Tc1—O1—Th1	−59.5 (9)	O5ⁱ—Th1—O13—P3	110.3 (2)
O3—Tc1—O1—Th1	−179.0 (7)	O5—Th1—O13—P3	−110.3 (2)
O4—Tc1—O1—Th1	61.4 (9)	O6—Th1—O13—P3	180.000 (4)
O9—Th1—O1—Tc1	118.2 (8)	O1ⁱ—Th1—O13—P3	42.4 (2)
O13—Th1—O1—Tc1	−93.0 (8)	O1—Th1—O13—P3	−42.4 (2)
O5ⁱ—Th1—O1—Tc1	−166.8 (6)	O10—Th1—O13—P3	180.000 (5)
O5—Th1—O1—Tc1	10.3 (7)	O5—P1—C1—C2	−63.2 (11)
O6—Th1—O1—Tc1	66.5 (8)	C9—P1—C1—C2	176.1 (10)
O1ⁱ—Th1—O1—Tc1	−168.8 (6)	C5—P1—C1—C2	61.1 (12)
O10—Th1—O1—Tc1	−38.0 (9)	P1—C1—C2—C3	172.7 (10)
C9—P1—O5—Th1	160.9 (14)	C1—C2—C3—C4	64.5 (18)
C5—P1—O5—Th1	−81.2 (16)	O5—P1—C5—C6	−179.0 (8)
C1—P1—O5—Th1	45.5 (17)	C9—P1—C5—C6	−58.8 (10)
O9—Th1—O5—P1	87.3 (16)	C1—P1—C5—C6	52.5 (10)
O13—Th1—O5—P1	−136.4 (15)	P1—C5—C6—C7	179.9 (8)
O5ⁱ—Th1—O5—P1	−28.7 (19)	C5—C6—C7—C8	−179.0 (11)
O6—Th1—O5—P1	18.8 (15)	O5—P1—C9—C10	−58.4 (10)
O1ⁱ—Th1—O5—P1	155.3 (13)	C5—P1—C9—C10	−176.4 (9)
O1—Th1—O5—P1	153.3 (16)	C1—P1—C9—C10	65.2 (10)
O10—Th1—O5—P1	−65.0 (15)	P1—C9—C10—C11	178.6 (9)
O8—Tc2—O6—Th1	−60.6 (5)	C9—C10—C11—C12	69.2 (15)
O8ⁱ—Tc2—O6—Th1	60.6 (5)	O9—P2—C13A—C14	−55 (2)
O7—Tc2—O6—Th1	180.000 (3)	C13Aⁱ—P2—C13A—C14	−164.1 (13)
O9—Th1—O6—Tc2	0.000 (1)	C17—P2—C13A—C14	79 (2)
O13—Th1—O6—Tc2	180.0	C13B—P2—C13A—C14	50.7 (16)
O5ⁱ—Th1—O6—Tc2	−105.55 (19)	C13Bⁱ—P2—C13A—C14	173.8 (19)
O5—Th1—O6—Tc2	105.55 (19)	O9—P2—C13B—C14	41 (3)
O1ⁱ—Th1—O6—Tc2	−51.2 (3)	C13A—P2—C13B—C14	−52.4 (17)
O1—Th1—O6—Tc2	51.2 (3)	C13Aⁱ—P2—C13B—C14	−88 (2)
O10—Th1—O6—Tc2	180.000 (2)	C17—P2—C13B—C14	152 (3)
C13A—P2—O9—Th1	137.9 (9)	C13Bⁱ—P2—C13B—C14	−127.9 (18)
C13Aⁱ—P2—O9—Th1	−137.9 (9)	P2—C13B—C14—C13A	51.7 (16)
C17—P2—O9—Th1	0.000 (4)	P2—C13B—C14—C15	154.5 (19)
C13B—P2—O9—Th1	95.2 (12)	P2—C13A—C14—C13B	−56.9 (18)
C13Bⁱ—P2—O9—Th1	−95.2 (12)	P2—C13A—C14—C15	−171.3 (16)
O13—Th1—O9—P2	0.000 (3)	C13B—C14—C15—C16	−29 (4)
O5ⁱ—Th1—O9—P2	−109.1 (2)	C13A—C14—C15—C16	32 (3)
O5—Th1—O9—P2	109.1 (2)	O9—P2—C17—C18	180.000 (2)
O6—Th1—O9—P2	180.000 (3)	C13A—P2—C17—C18	45.6 (8)
O1ⁱ—Th1—O9—P2	−43.1 (2)	C13Aⁱ—P2—C17—C18	−45.6 (8)
O1—Th1—O9—P2	43.1 (2)	C13B—P2—C17—C18	62.8 (12)
O10—Th1—O9—P2	180.000 (2)	C13Bⁱ—P2—C17—C18	−62.8 (12)
O11ⁱ—Tc3—O10—Th1	−58.4 (5)	P2—C17—C18—C19	180.000 (2)
O11—Tc3—O10—Th1	58.4 (5)	C17—C18—C19—C20	180.000 (2)
O12—Tc3—O10—Th1	180.000 (2)	O13—P3—C21—C22	172.6 (11)
O9—Th1—O10—Tc3	180.0	C21ⁱ—P3—C21—C22	−70.2 (15)
O13—Th1—O10—Tc3	0.000 (1)	C25ⁱ—P3—C21—C22	58.5 (14)
O5ⁱ—Th1—O10—Tc3	102.43 (19)	C25—P3—C21—C22	39.5 (16)
O5—Th1—O10—Tc3	−102.43 (19)	P3—C21—C22—C23	−177.6 (12)
O6—Th1—O10—Tc3	180.000 (2)	C21—C22—C23—C24	178.7 (15)
O1ⁱ—Th1—O10—Tc3	54.7 (3)	O13—P3—C25—C26	−51 (2)
O1—Th1—O10—Tc3	−54.7 (3)	C21—P3—C25—C26	79 (2)
C21—P3—O13—Th1	−118.8 (5)	C21ⁱ—P3—C25—C26	−159.6 (19)
C21ⁱ—P3—O13—Th1	118.8 (5)	C25ⁱ—P3—C25—C26	47 (2)
C25ⁱ—P3—O13—Th1	−20.3 (8)	P3—C25—C26—C27	−159.5 (13)
C25—P3—O13—Th1	20.3 (8)	C25—C26—C27—C28	−4 (5)
O9—Th1—O13—P3	0.000 (5)

Symmetry code: (i) −x, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O5	0.97	2.94	3.337 (14)	106
C2—H2A···O6	0.97	2.60	3.454 (14)	147
C2—H2A···O7	0.97	3.00	3.464 (16)	110
C2—H2A···O10	0.97	2.92	3.650 (16)	133
C3—H3B···O12	0.97	2.68	3.537 (19)	147
C5—H5B···O8	0.97	2.58	3.533 (14)	167
C5—H5A···O2	0.97	2.59	3.449 (14)	148
C9—H9A···O2	0.97	2.82	3.624 (15)	141
C9—H9A···O4	0.97	2.97	3.633 (14)	127
C10—H10A···O11	0.97	3.07	3.564 (16)	113
C10—H10B···O4	0.97	3.02	3.565 (15)	117
C10—H10B···O5	0.97	2.87	3.228 (14)	103
C17—H17A···O1	0.97	2.71	3.350 (16)	124
C17—H17A···O3	0.97	2.88	3.853 (13)	177
C26—H26A···O1	0.97	2.68	3.54 (2)	148
C4—H4A···O2ⁱⁱ	0.96	3.02	3.880 (19)	149
C6—H6B···O4ⁱⁱ	0.97	2.88	3.559 (13)	128
C6—H6A···O3ⁱⁱ	0.97	2.74	3.523 (13)	138
C8—H8A···O4ⁱⁱ	0.96	3.05	3.580 (15)	116
C9—H9B···O3ⁱⁱ	0.97	2.72	3.682 (13)	173
C12—H12A···O3ⁱⁱ	0.96	3.13	3.741 (15)	123
C13A—H13B···O7ⁱⁱⁱ	0.97	2.81	3.60 (3)	139
C13A—H13B···O7ⁱⁱⁱ	0.97	2.81	3.60 (3)	139
C13B—H13C···O7ⁱⁱⁱ	0.97	3.27	4.13 (4)	149
C13A—H13B···O7^iv	0.97	2.81	3.60 (3)	139
C13A—H13B···O7^iv	0.97	2.81	3.60 (3)	139
C13A—H13B···O7^iv	0.97	2.81	3.60 (3)	139
C13B—H13C···O7^iv	0.97	3.27	4.13 (4)	149
C18—H18B···O8ⁱⁱⁱ	0.97	3.01	3.742 (16)	133
C18—H18A···O8^iv	0.97	3.01	3.742 (16)	133
C17—H17B···O1ⁱ	0.97	2.71	3.350 (16)	124
C17—H17B···O3ⁱ	0.97	2.88	3.853 (13)	177
C13A—H13A···O8ⁱ	0.97	3.03	3.65 (3)	123
C13B—H13D···O2ⁱ	0.97	3.31	3.85 (4)	117
C21—H21B···O4ⁱ	0.97	2.68	3.605 (17)	161
C21—H21A···O11ⁱ	0.97	2.57	3.464 (16)	153
C26—H26B···O1ⁱ	0.97	3.03	3.54 (2)	114
C26—H26B···O3ⁱ	0.97	3.12	3.845 (18)	133
C20—H20A···O7^v	0.96	2.72	3.52 (3)	142
C28—H28C···O12^v	0.96	3.21	3.79 (4)	120
C20—H20A···O7^vi	0.96	2.72	3.52 (3)	142
C28—H28C···O12^vi	0.96	3.21	3.79 (4)	120
C22—H22A···O11^vii	0.97	2.91	3.633 (16)	132
C22—H22B···O12^vii	0.97	2.77	3.519 (15)	135
C24—H24A···O11^vii	0.96	3.31	3.82 (2)	115
C22—H22B···O12^viii	0.97	2.77	3.519 (15)	135

(IIIat170) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	D_x = 1.692 Mg m⁻³
M_r = 1753.26	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbc2₁	Cell parameters from 7727 reflections
a = 21.417 (6) Å	θ = 2.7–26.3°
b = 21.649 (6) Å	µ = 3.09 mm⁻¹
c = 14.848 (4) Å	T = 170 K
V = 6885 (3) Å³	Block, colourless
Z = 4	0.10 × 0.10 × 0.10 mm
F(000) = 3512

Data collection top

CCD area detector diffractometer	14267 independent reflections
Radiation source: fine-focus sealed tube	12482 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.074
phi and ω scans	θ_max = 26.5°, θ_min = 1.4°
Absorption correction: multi-scan SADABS	h = −26→26
T_min = 0.748, T_max = 0.748	k = −27→27
54013 measured reflections	l = −18→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.050	H-atom parameters constrained
wR(F²) = 0.127	w = 1/[σ²(F_o²) + (0.042P)² + 14.969P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.002
14267 reflections	Δρ_max = 3.57 e Å⁻³
707 parameters	Δρ_min = −0.88 e Å⁻³
25 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.016 (6)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	V = 6885 (3) Å³
M_r = 1753.26	Z = 4
Orthorhombic, Pbc2₁	Mo Kα radiation
a = 21.417 (6) Å	µ = 3.09 mm⁻¹
b = 21.649 (6) Å	T = 170 K
c = 14.848 (4) Å	0.10 × 0.10 × 0.10 mm

Data collection top

CCD area detector diffractometer	14267 independent reflections
Absorption correction: multi-scan SADABS	12482 reflections with I > 2σ(I)
T_min = 0.748, T_max = 0.748	R_int = 0.074
54013 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.050	H-atom parameters constrained
wR(F²) = 0.127	w = 1/[σ²(F_o²) + (0.042P)² + 14.969P] where P = (F_o² + 2F_c²)/3
S = 1.08	Δρ_max = 3.57 e Å⁻³
14267 reflections	Δρ_min = −0.88 e Å⁻³
707 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
25 restraints	Absolute structure parameter: 0.016 (6)

Special details top

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

	x	y	z	U_iso*/U_eq
Th1	0.252041 (13)	0.004857 (13)	0.15862 (4)	0.02047 (8)
Tc1	0.39882 (4)	−0.00347 (4)	−0.01205 (7)	0.0324 (2)
Tc2	0.26165 (4)	0.16558 (4)	0.29452 (6)	0.02978 (18)
Tc3	0.25042 (4)	−0.13843 (4)	0.34041 (7)	0.0357 (2)
Tc1A	0.09106 (4)	−0.01308 (4)	0.01682 (6)	0.03061 (19)
P1	0.40972 (12)	0.00209 (12)	0.2759 (2)	0.0339 (6)
P2	0.22759 (14)	0.13538 (12)	−0.00605 (18)	0.0350 (6)
P3	0.26010 (16)	−0.15100 (15)	0.0450 (3)	0.0491 (8)
P1A	0.11770 (11)	0.03550 (12)	0.32124 (17)	0.0320 (6)
O1	0.3297 (4)	0.0202 (4)	0.0401 (6)	0.053 (2)
O2	0.4584 (4)	0.0396 (5)	0.0227 (8)	0.076 (3)
O3	0.3905 (5)	0.0057 (4)	−0.1248 (6)	0.068 (3)
O4	0.4153 (4)	−0.0771 (4)	0.0102 (6)	0.066 (3)
O5	0.3512 (3)	−0.0116 (3)	0.2247 (5)	0.0407 (18)
O6	0.2833 (3)	0.0977 (3)	0.2382 (6)	0.0433 (19)
O7	0.2377 (5)	0.1503 (5)	0.4018 (6)	0.069 (3)
O8	0.3246 (4)	0.2124 (4)	0.2973 (6)	0.0526 (19)
O9	0.2232 (4)	0.0877 (3)	0.0687 (5)	0.0405 (17)
O10	0.2377 (4)	−0.0725 (5)	0.2761 (6)	0.057 (3)
O11	0.3256 (4)	−0.1616 (5)	0.3304 (6)	0.069 (3)
O12	0.2371 (4)	−0.1209 (4)	0.4489 (6)	0.057 (2)
O13	0.2683 (4)	−0.0891 (4)	0.0860 (6)	0.050 (2)
O1A	0.1568 (4)	−0.0280 (4)	0.0822 (6)	0.051 (2)
O2A	0.0481 (4)	0.0436 (4)	0.0611 (6)	0.061 (3)
O3A	0.1116 (5)	0.0066 (5)	−0.0847 (9)	0.085 (4)
O4A	0.0482 (4)	−0.0768 (4)	0.0124 (7)	0.072 (3)
O5A	0.1679 (3)	0.0368 (3)	0.2488 (5)	0.0399 (18)
O8A	0.2039 (4)	0.2005 (4)	0.2389 (6)	0.055 (2)
O11A	0.2010 (5)	−0.1949 (4)	0.3086 (6)	0.068 (3)
C1	0.3985 (5)	−0.0114 (5)	0.3930 (8)	0.039 (3)
H1A	0.3888	−0.0547	0.4020	0.047*
H1B	0.4373	−0.0027	0.4244	0.047*
C2	0.3462 (5)	0.0279 (6)	0.4348 (8)	0.047 (3)
H2A	0.3089	0.0248	0.3979	0.056*
H2B	0.3589	0.0709	0.4362	0.056*
C3	0.3315 (6)	0.0059 (6)	0.5309 (10)	0.061 (4)
H3A	0.2953	0.0283	0.5530	0.074*
H3B	0.3208	−0.0376	0.5291	0.074*
C4	0.3849 (7)	0.0150 (9)	0.5963 (10)	0.085 (6)
H4A	0.4219	−0.0038	0.5724	0.128*
H4B	0.3745	−0.0038	0.6529	0.128*
H4C	0.3920	0.0584	0.6050	0.128*
C5	0.4329 (5)	0.0811 (4)	0.2583 (7)	0.032 (2)
H5A	0.4407	0.0867	0.1945	0.039*
H5B	0.3979	0.1073	0.2741	0.039*
C6	0.4898 (5)	0.1038 (5)	0.3095 (8)	0.047 (3)
H6A	0.4830	0.0986	0.3736	0.056*
H6B	0.5259	0.0792	0.2927	0.056*
C7	0.5024 (5)	0.1709 (5)	0.2891 (9)	0.047 (3)
H7A	0.5095	0.1762	0.2251	0.056*
H7B	0.4665	0.1957	0.3060	0.056*
C8	0.5585 (7)	0.1918 (6)	0.3405 (10)	0.067 (4)
H8A	0.5487	0.1933	0.4035	0.100*
H8B	0.5706	0.2321	0.3202	0.100*
H8C	0.5921	0.1633	0.3308	0.100*
C9	0.4728 (4)	−0.0473 (5)	0.2408 (7)	0.035 (2)
H9A	0.4859	−0.0349	0.1810	0.042*
H9B	0.5078	−0.0409	0.2811	0.042*
C10	0.4576 (5)	−0.1148 (5)	0.2391 (8)	0.047 (3)
H10A	0.4425	−0.1269	0.2981	0.057*
H10B	0.4240	−0.1217	0.1964	0.057*
C11	0.5112 (6)	−0.1546 (5)	0.2144 (8)	0.047 (3)
H11A	0.4958	−0.1963	0.2057	0.057*
H11B	0.5274	−0.1404	0.1571	0.057*
C12	0.5625 (7)	−0.1569 (6)	0.2783 (12)	0.074 (4)
H12A	0.5462	−0.1596	0.3384	0.112*
H12B	0.5874	−0.1203	0.2726	0.112*
H12C	0.5879	−0.1925	0.2661	0.112*
C13	0.1505 (6)	0.1724 (6)	−0.0200 (11)	0.066 (4)
H13C	0.1456	0.1837	−0.0828	0.079*
H13D	0.1185	0.1422	−0.0060	0.079*
C14	0.1396 (6)	0.2274 (7)	0.0352 (11)	0.087 (5)
H14C	0.1738	0.2561	0.0264	0.104*
H14D	0.1392	0.2155	0.0981	0.104*
C15	0.0786 (6)	0.2598 (6)	0.0129 (10)	0.062 (4)
H15A	0.0781	0.2721	−0.0499	0.074*
H15B	0.0436	0.2322	0.0234	0.074*
C16	0.0736 (8)	0.3145 (7)	0.0715 (11)	0.093 (5)
H16A	0.0740	0.3018	0.1334	0.139*
H16B	0.0352	0.3358	0.0589	0.139*
H16C	0.1082	0.3416	0.0603	0.139*
C17	0.2422 (6)	0.0984 (6)	−0.1114 (8)	0.046 (3)
H17A	0.2794	0.0731	−0.1054	0.056*
H17B	0.2076	0.0709	−0.1245	0.056*
C18	0.2510 (5)	0.1422 (6)	−0.1917 (8)	0.050 (3)
H18A	0.2154	0.1697	−0.1952	0.060*
H18B	0.2879	0.1673	−0.1815	0.060*
C19	0.2576 (8)	0.1099 (7)	−0.2766 (10)	0.079 (5)
H19A	0.2217	0.0834	−0.2855	0.095*
H19B	0.2945	0.0839	−0.2742	0.095*
C20	0.2632 (10)	0.1538 (8)	−0.3564 (11)	0.095 (6)
H20A	0.2332	0.1865	−0.3503	0.143*
H20B	0.2555	0.1316	−0.4113	0.143*
H20C	0.3045	0.1710	−0.3580	0.143*
C21	0.1848 (6)	−0.1812 (5)	0.0758 (7)	0.045 (3)
H21A	0.1831	−0.1838	0.1409	0.054*
H21B	0.1534	−0.1515	0.0572	0.054*
C22	0.1667 (5)	−0.2433 (6)	0.0381 (8)	0.048 (3)
H22A	0.1987	−0.2732	0.0536	0.057*
H22B	0.1649	−0.2406	−0.0270	0.057*
C23	0.1044 (6)	−0.2659 (5)	0.0730 (9)	0.053 (3)
H23A	0.1059	−0.2675	0.1383	0.063*
H23B	0.0723	−0.2366	0.0560	0.063*
C24	0.0873 (7)	−0.3288 (6)	0.0374 (13)	0.076 (5)
H24A	0.0991	−0.3318	−0.0248	0.114*
H24B	0.0430	−0.3348	0.0428	0.114*
H24C	0.1087	−0.3600	0.0714	0.114*
C25	0.2714 (9)	−0.1476 (7)	−0.0718 (10)	0.073 (4)
H25A	0.3139	−0.1344	−0.0842	0.088*
H25B	0.2660	−0.1885	−0.0972	0.088*
C26	0.2272 (11)	−0.1044 (10)	−0.1160 (12)	0.149 (12)
H26A	0.2226	−0.0676	−0.0794	0.179*
H26B	0.1866	−0.1238	−0.1214	0.179*
C27	0.2514 (7)	−0.0861 (8)	−0.2110 (15)	0.107 (8)
H27A	0.2282	−0.0507	−0.2329	0.129*
H27B	0.2951	−0.0747	−0.2074	0.129*
C28	0.2435 (9)	−0.1400 (9)	−0.2758 (14)	0.103 (8)
H28A	0.2777	−0.1682	−0.2687	0.155*
H28B	0.2428	−0.1248	−0.3366	0.155*
H28C	0.2050	−0.1610	−0.2631	0.155*
C1A	0.1523 (5)	0.0174 (5)	0.4266 (8)	0.038 (2)
H1C	0.1771	−0.0198	0.4192	0.045*
H1D	0.1807	0.0505	0.4425	0.045*
C2A	0.1074 (5)	0.0072 (4)	0.5062 (6)	0.036 (3)
H2C	0.0794	0.0423	0.5110	0.044*
H2D	0.0823	−0.0293	0.4949	0.044*
C3A	0.1422 (6)	−0.0007 (6)	0.5943 (8)	0.052 (3)
H3C	0.1699	0.0342	0.6032	0.063*
H3D	0.1676	−0.0378	0.5913	0.063*
C4A	0.0970 (6)	−0.0057 (8)	0.6757 (9)	0.069 (4)
H4D	0.0653	0.0254	0.6707	0.103*
H4E	0.1199	0.0002	0.7306	0.103*
H4F	0.0779	−0.0458	0.6760	0.103*
C5A	0.0800 (5)	0.1085 (5)	0.3344 (8)	0.045 (3)
H5C	0.0483	0.1049	0.3806	0.054*
H5D	0.1105	0.1385	0.3549	0.054*
C6A	0.0496 (6)	0.1326 (6)	0.2484 (8)	0.051 (3)
H6C	0.0816	0.1407	0.2036	0.061*
H6D	0.0216	0.1015	0.2244	0.061*
C7A	0.0133 (7)	0.1918 (6)	0.2671 (8)	0.060 (4)
H7C	0.0408	0.2207	0.2974	0.072*
H7D	0.0017	0.2101	0.2099	0.072*
C8A	−0.0451 (7)	0.1845 (7)	0.3233 (10)	0.074 (5)
H8D	−0.0730	0.2182	0.3113	0.111*
H8E	−0.0341	0.1845	0.3860	0.111*
H8F	−0.0652	0.1462	0.3084	0.111*
C9A	0.0588 (4)	−0.0188 (4)	0.2934 (7)	0.036 (2)
H9C	0.0259	−0.0160	0.3381	0.043*
H9D	0.0410	−0.0073	0.2358	0.043*
C10A	0.0804 (4)	−0.0860 (4)	0.2879 (8)	0.037 (2)
H10C	0.1154	−0.0885	0.2467	0.045*
H10D	0.0951	−0.0988	0.3469	0.045*
C11A	0.0300 (5)	−0.1303 (5)	0.2569 (8)	0.047 (3)
H11C	0.0480	−0.1713	0.2522	0.057*
H11D	0.0165	−0.1181	0.1972	0.057*
C12A	−0.0270 (5)	−0.1335 (5)	0.3181 (8)	0.051 (3)
H12D	−0.0142	−0.1454	0.3776	0.076*
H12E	−0.0559	−0.1633	0.2948	0.076*
H12F	−0.0467	−0.0937	0.3205	0.076*
C13A	0.2819 (5)	0.1919 (6)	0.0175 (8)	0.048 (3)
H13A	0.2804	0.2224	−0.0302	0.058*
H13B	0.2697	0.2123	0.0729	0.058*
C14A	0.3490 (5)	0.1705 (5)	0.0275 (10)	0.056 (3)
H14A	0.3629	0.1545	−0.0302	0.067*
H14B	0.3498	0.1364	0.0700	0.067*
C15A	0.3966 (6)	0.2195 (6)	0.0592 (9)	0.056 (3)
H15C	0.3836	0.2338	0.1182	0.067*
H15D	0.4367	0.1991	0.0667	0.067*
C16A	0.4064 (8)	0.2745 (7)	0.0013 (7)	0.068 (4)
H16D	0.4215	0.2616	−0.0566	0.102*
H16E	0.4364	0.3014	0.0289	0.102*
H16F	0.3675	0.2961	−0.0060	0.102*
C21A	0.3247 (6)	−0.2001 (6)	0.0905 (10)	0.066 (4)
H21C	0.3616	−0.1744	0.0952	0.079*
H21D	0.3133	−0.2121	0.1512	0.079*
C22A	0.3424 (6)	−0.2561 (6)	0.0421 (10)	0.058 (3)
H22C	0.3487	−0.2462	−0.0209	0.069*
H22D	0.3086	−0.2858	0.0460	0.069*
C23A	0.4013 (7)	−0.2851 (7)	0.0790 (10)	0.073 (4)
H23C	0.4354	−0.2559	0.0728	0.088*
H23D	0.3956	−0.2931	0.1428	0.088*
C24A	0.4187 (9)	−0.3436 (8)	0.0336 (13)	0.092 (5)
H24D	0.3863	−0.3736	0.0427	0.138*
H24E	0.4571	−0.3588	0.0585	0.138*
H24F	0.4240	−0.3363	−0.0297	0.138*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.01633 (15)	0.02440 (15)	0.02068 (14)	0.00034 (11)	−0.00022 (12)	0.00073 (18)
Tc1	0.0275 (4)	0.0373 (5)	0.0324 (5)	0.0042 (3)	0.0096 (4)	0.0020 (3)
Tc2	0.0334 (4)	0.0279 (4)	0.0280 (4)	0.0002 (3)	−0.0020 (4)	−0.0039 (4)
Tc3	0.0331 (5)	0.0410 (5)	0.0330 (5)	0.0058 (4)	0.0041 (3)	0.0152 (4)
Tc1A	0.0220 (4)	0.0396 (4)	0.0302 (4)	0.0006 (3)	−0.0059 (3)	−0.0027 (4)
P1	0.0252 (13)	0.0380 (15)	0.0385 (16)	−0.0020 (10)	−0.0080 (11)	−0.0008 (11)
P2	0.0478 (16)	0.0286 (13)	0.0287 (15)	0.0061 (12)	−0.0029 (12)	0.0053 (10)
P3	0.0574 (19)	0.0311 (15)	0.059 (2)	−0.0044 (13)	0.0165 (16)	−0.0151 (14)
P1A	0.0260 (12)	0.0338 (13)	0.0363 (15)	0.0024 (10)	0.0103 (10)	0.0004 (11)
O1	0.055 (5)	0.052 (5)	0.051 (5)	0.018 (4)	0.032 (4)	0.017 (4)
O2	0.047 (5)	0.080 (7)	0.101 (8)	−0.010 (5)	0.011 (6)	−0.007 (7)
O3	0.069 (7)	0.096 (8)	0.040 (5)	0.015 (5)	0.016 (5)	0.006 (5)
O4	0.065 (6)	0.068 (6)	0.066 (6)	0.022 (5)	0.020 (5)	0.009 (5)
O5	0.024 (4)	0.045 (4)	0.052 (5)	0.002 (3)	−0.018 (3)	−0.002 (4)
O6	0.033 (4)	0.035 (4)	0.062 (5)	−0.001 (3)	−0.010 (4)	−0.016 (4)
O7	0.100 (7)	0.078 (7)	0.028 (4)	−0.020 (5)	0.014 (4)	0.007 (5)
O8	0.055 (5)	0.055 (5)	0.048 (5)	−0.007 (4)	−0.007 (4)	−0.006 (4)
O9	0.048 (4)	0.045 (4)	0.028 (4)	0.009 (4)	0.005 (3)	0.008 (3)
O10	0.039 (4)	0.076 (6)	0.058 (6)	0.019 (4)	0.014 (4)	0.033 (5)
O11	0.050 (5)	0.096 (7)	0.061 (6)	0.033 (5)	0.018 (4)	0.034 (5)
O12	0.079 (6)	0.056 (5)	0.036 (5)	0.007 (5)	0.002 (4)	0.009 (4)
O13	0.043 (4)	0.038 (4)	0.068 (6)	0.008 (4)	0.004 (4)	−0.022 (4)
O1A	0.038 (4)	0.047 (5)	0.069 (6)	0.005 (3)	−0.026 (4)	−0.014 (4)
O2A	0.044 (5)	0.081 (7)	0.060 (5)	0.023 (4)	−0.005 (4)	−0.021 (5)
O3A	0.065 (7)	0.096 (9)	0.093 (9)	0.024 (6)	−0.007 (7)	0.021 (6)
O4A	0.066 (6)	0.070 (6)	0.079 (7)	−0.025 (5)	−0.016 (5)	0.001 (5)
O5A	0.042 (4)	0.040 (4)	0.037 (4)	0.011 (3)	0.019 (3)	0.003 (3)
O8A	0.064 (6)	0.048 (5)	0.052 (5)	0.008 (4)	−0.003 (4)	−0.009 (4)
O11A	0.097 (7)	0.066 (6)	0.041 (5)	−0.016 (5)	−0.011 (5)	−0.004 (4)
C1	0.029 (5)	0.044 (6)	0.044 (7)	0.003 (5)	−0.008 (5)	0.009 (5)
C2	0.031 (6)	0.062 (8)	0.047 (7)	0.007 (5)	−0.007 (5)	−0.003 (6)
C3	0.046 (7)	0.073 (9)	0.065 (9)	−0.005 (6)	−0.001 (7)	−0.024 (8)
C4	0.068 (10)	0.144 (16)	0.044 (8)	0.000 (10)	−0.008 (7)	−0.044 (10)
C5	0.031 (5)	0.035 (5)	0.031 (5)	0.007 (4)	−0.012 (4)	0.000 (4)
C6	0.049 (6)	0.043 (6)	0.049 (7)	−0.005 (5)	−0.018 (5)	0.005 (5)
C7	0.040 (6)	0.046 (6)	0.054 (7)	−0.010 (5)	0.001 (6)	0.005 (6)
C8	0.069 (9)	0.061 (8)	0.071 (9)	−0.021 (7)	−0.021 (8)	0.027 (7)
C9	0.029 (5)	0.040 (6)	0.036 (6)	−0.002 (4)	−0.005 (4)	−0.001 (5)
C10	0.042 (7)	0.054 (7)	0.045 (7)	−0.006 (5)	0.001 (5)	−0.004 (6)
C11	0.063 (8)	0.032 (6)	0.047 (7)	0.002 (5)	0.007 (6)	0.002 (5)
C12	0.068 (9)	0.060 (9)	0.095 (13)	0.026 (7)	−0.014 (9)	−0.012 (8)
C13	0.059 (8)	0.046 (7)	0.093 (10)	−0.008 (6)	−0.016 (8)	0.023 (8)
C14	0.075 (10)	0.117 (14)	0.068 (10)	0.043 (10)	0.002 (9)	−0.010 (10)
C15	0.045 (7)	0.076 (9)	0.065 (9)	−0.001 (6)	0.012 (6)	0.004 (8)
C16	0.098 (13)	0.088 (12)	0.093 (13)	−0.006 (10)	0.022 (10)	−0.004 (10)
C17	0.070 (8)	0.042 (7)	0.027 (6)	−0.008 (5)	−0.013 (5)	−0.001 (5)
C18	0.065 (9)	0.044 (7)	0.040 (7)	−0.005 (5)	0.010 (5)	0.003 (5)
C19	0.145 (16)	0.051 (8)	0.041 (7)	−0.004 (8)	−0.022 (8)	−0.005 (6)
C20	0.190 (19)	0.062 (8)	0.033 (8)	−0.006 (10)	0.004 (9)	−0.009 (6)
C21	0.052 (7)	0.049 (7)	0.033 (6)	−0.006 (5)	−0.007 (5)	−0.010 (5)
C22	0.047 (6)	0.053 (7)	0.043 (7)	0.001 (6)	0.007 (6)	−0.001 (5)
C23	0.048 (7)	0.041 (7)	0.070 (9)	−0.005 (5)	0.003 (6)	−0.004 (6)
C24	0.061 (9)	0.045 (7)	0.123 (14)	0.002 (6)	0.008 (9)	−0.029 (9)
C25	0.122 (13)	0.051 (8)	0.046 (9)	0.005 (9)	0.010 (9)	0.003 (7)
C26	0.21 (2)	0.16 (2)	0.076 (15)	0.13 (2)	−0.062 (16)	−0.065 (15)
C27	0.12 (2)	0.053 (10)	0.14 (2)	0.002 (9)	−0.042 (15)	0.013 (12)
C28	0.14 (2)	0.089 (14)	0.080 (14)	0.007 (12)	−0.052 (12)	−0.009 (11)
C1A	0.026 (5)	0.044 (6)	0.043 (6)	0.006 (5)	0.010 (4)	−0.006 (5)
C2A	0.031 (5)	0.036 (5)	0.043 (7)	−0.001 (4)	0.003 (4)	−0.007 (4)
C3A	0.053 (8)	0.070 (9)	0.035 (6)	0.005 (6)	−0.007 (5)	−0.002 (6)
C4A	0.046 (7)	0.127 (13)	0.032 (7)	−0.005 (8)	0.000 (5)	0.006 (7)
C5A	0.047 (7)	0.042 (6)	0.045 (6)	0.017 (5)	0.008 (5)	0.000 (5)
C6A	0.060 (8)	0.048 (7)	0.044 (7)	−0.005 (6)	0.002 (6)	−0.002 (6)
C7A	0.083 (10)	0.056 (8)	0.042 (7)	0.021 (7)	−0.005 (6)	−0.001 (6)
C8A	0.065 (9)	0.073 (10)	0.084 (12)	0.024 (7)	0.002 (8)	−0.012 (8)
C9A	0.042 (5)	0.034 (4)	0.031 (5)	0.005 (3)	−0.011 (5)	0.000 (4)
C10A	0.042 (5)	0.033 (4)	0.038 (5)	0.007 (4)	0.006 (5)	0.001 (4)
C11A	0.048 (7)	0.044 (7)	0.051 (7)	−0.011 (5)	0.014 (5)	−0.002 (5)
C12A	0.041 (6)	0.055 (7)	0.056 (8)	−0.012 (5)	0.009 (5)	0.004 (6)
C13A	0.042 (6)	0.066 (8)	0.036 (6)	−0.021 (6)	−0.004 (5)	0.015 (6)
C14A	0.045 (7)	0.049 (7)	0.073 (9)	0.002 (5)	0.006 (6)	0.017 (7)
C15A	0.064 (9)	0.058 (8)	0.045 (7)	−0.003 (6)	−0.018 (6)	−0.007 (6)
C16A	0.106 (13)	0.073 (10)	0.026 (7)	−0.015 (8)	0.008 (6)	−0.003 (5)
C21A	0.049 (8)	0.058 (8)	0.091 (11)	0.012 (6)	0.010 (7)	−0.018 (8)
C22A	0.050 (7)	0.062 (8)	0.062 (8)	−0.002 (6)	−0.010 (7)	−0.003 (6)
C23A	0.052 (9)	0.103 (12)	0.065 (9)	0.028 (8)	−0.014 (7)	0.014 (9)
C24A	0.098 (13)	0.095 (12)	0.082 (12)	0.004 (10)	−0.022 (11)	−0.021 (11)

Geometric parameters (Å, º) top

Th1—O9	2.319 (7)	C18—H18A	0.9700
Th1—O13	2.327 (7)	C18—H18B	0.9700
Th1—O5A	2.350 (6)	C19—C20	1.52 (2)
Th1—O5	2.367 (6)	C19—H19A	0.9700
Th1—O6	2.425 (7)	C19—H19B	0.9700
Th1—O10	2.438 (8)	C20—H20A	0.9600
Th1—O1A	2.440 (7)	C20—H20B	0.9600
Th1—O1	2.444 (7)	C20—H20C	0.9600
Tc1—O2	1.664 (10)	C21—C22	1.508 (15)
Tc1—O4	1.665 (9)	C21—H21A	0.9700
Tc1—O3	1.696 (9)	C21—H21B	0.9700
Tc1—O1	1.748 (7)	C22—C23	1.512 (16)
Tc2—O8A	1.668 (8)	C22—H22A	0.9700
Tc2—O8	1.688 (7)	C22—H22B	0.9700
Tc2—O7	1.705 (9)	C23—C24	1.508 (16)
Tc2—O6	1.753 (7)	C23—H23A	0.9700
Tc3—O12	1.679 (9)	C23—H23B	0.9700
Tc3—O11A	1.683 (9)	C24—H24A	0.9600
Tc3—O11	1.694 (8)	C24—H24B	0.9600
Tc3—O10	1.739 (8)	C24—H24C	0.9600
Tc1A—O3A	1.627 (13)	C25—C26	1.484 (15)
Tc1A—O4A	1.659 (9)	C25—H25A	0.9700
Tc1A—O2A	1.669 (8)	C25—H25B	0.9700
Tc1A—O1A	1.740 (7)	C26—C27	1.552 (17)
P1—O5	1.495 (7)	C26—H26A	0.9700
P1—C1	1.779 (12)	C26—H26B	0.9700
P1—C5	1.799 (10)	C27—C28	1.522 (16)
P1—C9	1.800 (10)	C27—H27A	0.9700
P2—O9	1.519 (7)	C27—H27B	0.9700
P2—C13A	1.724 (11)	C28—H28A	0.9600
P2—C17	1.784 (12)	C28—H28B	0.9600
P2—C13	1.846 (13)	C28—H28C	0.9600
P3—O13	1.484 (8)	C1A—C2A	1.540 (14)
P3—C25	1.753 (15)	C1A—H1C	0.9700
P3—C21	1.799 (12)	C1A—H1D	0.9700
P3—C21A	1.872 (14)	C2A—C3A	1.516 (15)
P1A—O5A	1.521 (7)	C2A—H2C	0.9700
P1A—C9A	1.772 (9)	C2A—H2D	0.9700
P1A—C1A	1.775 (12)	C3A—C4A	1.551 (18)
P1A—C5A	1.785 (10)	C3A—H3C	0.9700
C1—C2	1.537 (15)	C3A—H3D	0.9700
C1—H1A	0.9700	C4A—H4D	0.9600
C1—H1B	0.9700	C4A—H4E	0.9600
C2—C3	1.538 (18)	C4A—H4F	0.9600
C2—H2A	0.9700	C5A—C6A	1.525 (15)
C2—H2B	0.9700	C5A—H5C	0.9700
C3—C4	1.512 (18)	C5A—H5D	0.9700
C3—H3A	0.9700	C6A—C7A	1.525 (17)
C3—H3B	0.9700	C6A—H6C	0.9700
C4—H4A	0.9600	C6A—H6D	0.9700
C4—H4B	0.9600	C7A—C8A	1.511 (18)
C4—H4C	0.9600	C7A—H7C	0.9700
C5—C6	1.519 (13)	C7A—H7D	0.9700
C5—H5A	0.9700	C8A—H8D	0.9600
C5—H5B	0.9700	C8A—H8E	0.9600
C6—C7	1.510 (15)	C8A—H8F	0.9600
C6—H6A	0.9700	C9A—C10A	1.528 (13)
C6—H6B	0.9700	C9A—H9C	0.9700
C7—C8	1.492 (16)	C9A—H9D	0.9700
C7—H7A	0.9700	C10A—C11A	1.516 (15)
C7—H7B	0.9700	C10A—H10C	0.9700
C8—H8A	0.9600	C10A—H10D	0.9700
C8—H8B	0.9600	C11A—C12A	1.523 (15)
C8—H8C	0.9600	C11A—H11C	0.9700
C9—C10	1.496 (15)	C11A—H11D	0.9700
C9—H9A	0.9700	C12A—H12D	0.9600
C9—H9B	0.9700	C12A—H12E	0.9600
C10—C11	1.481 (16)	C12A—H12F	0.9600
C10—H10A	0.9700	C13A—C14A	1.517 (16)
C10—H10B	0.9700	C13A—H13A	0.9700
C11—C12	1.454 (18)	C13A—H13B	0.9700
C11—H11A	0.9700	C14A—C15A	1.545 (17)
C11—H11B	0.9700	C14A—H14A	0.9700
C12—H12A	0.9600	C14A—H14B	0.9700
C12—H12B	0.9600	C15A—C16A	1.484 (17)
C12—H12C	0.9600	C15A—H15C	0.9700
C13—C14	1.464 (14)	C15A—H15D	0.9700
C13—H13C	0.9700	C16A—H16D	0.9600
C13—H13D	0.9700	C16A—H16E	0.9600
C14—C15	1.520 (14)	C16A—H16F	0.9600
C14—H14C	0.9700	C21A—C22A	1.458 (17)
C14—H14D	0.9700	C21A—H21C	0.9700
C15—C16	1.474 (14)	C21A—H21D	0.9700
C15—H15A	0.9700	C22A—C23A	1.511 (17)
C15—H15B	0.9700	C22A—H22C	0.9700
C16—H16A	0.9600	C22A—H22D	0.9700
C16—H16B	0.9600	C23A—C24A	1.48 (2)
C16—H16C	0.9600	C23A—H23C	0.9700
C17—C18	1.535 (16)	C23A—H23D	0.9700
C17—H17A	0.9700	C24A—H24D	0.9600
C17—H17B	0.9700	C24A—H24E	0.9600
C18—C19	1.449 (19)	C24A—H24F	0.9600

O9—Th1—O13	116.7 (3)	C19—C18—C17	113.0 (11)
O9—Th1—O5A	84.0 (2)	C19—C18—H18A	109.0
O13—Th1—O5A	129.5 (3)	C17—C18—H18A	109.0
O9—Th1—O5	126.4 (3)	C19—C18—H18B	109.0
O13—Th1—O5	85.7 (3)	C17—C18—H18B	109.0
O5A—Th1—O5	119.8 (3)	H18A—C18—H18B	107.8
O9—Th1—O6	73.3 (3)	C18—C19—C20	112.6 (13)
O13—Th1—O6	155.2 (3)	C18—C19—H19A	109.1
O5A—Th1—O6	71.9 (3)	C20—C19—H19A	109.1
O5—Th1—O6	71.1 (2)	C18—C19—H19B	109.1
O9—Th1—O10	155.4 (2)	C20—C19—H19B	109.1
O13—Th1—O10	75.5 (4)	H19A—C19—H19B	107.8
O5A—Th1—O10	72.4 (3)	C19—C20—H20A	109.5
O5—Th1—O10	73.3 (3)	C19—C20—H20B	109.5
O6—Th1—O10	104.8 (3)	H20A—C20—H20B	109.5
O9—Th1—O1A	74.6 (3)	C19—C20—H20C	109.5
O13—Th1—O1A	69.9 (3)	H20A—C20—H20C	109.5
O5A—Th1—O1A	73.1 (3)	H20B—C20—H20C	109.5
O5—Th1—O1A	154.1 (3)	C22—C21—P3	117.4 (8)
O6—Th1—O1A	134.3 (2)	C22—C21—H21A	108.0
O10—Th1—O1A	91.6 (3)	P3—C21—H21A	108.0
O9—Th1—O1	70.2 (3)	C22—C21—H21B	108.0
O13—Th1—O1	71.6 (3)	P3—C21—H21B	108.0
O5A—Th1—O1	153.2 (3)	H21A—C21—H21B	107.2
O5—Th1—O1	73.1 (3)	C21—C22—C23	112.8 (10)
O6—Th1—O1	92.9 (3)	C21—C22—H22A	109.0
O10—Th1—O1	134.0 (3)	C23—C22—H22A	109.0
O1A—Th1—O1	105.9 (3)	C21—C22—H22B	109.0
O2—Tc1—O4	108.2 (5)	C23—C22—H22B	109.0
O2—Tc1—O3	108.8 (6)	H22A—C22—H22B	107.8
O4—Tc1—O3	109.3 (5)	C24—C23—C22	112.7 (11)
O2—Tc1—O1	110.4 (5)	C24—C23—H23A	109.0
O4—Tc1—O1	111.9 (4)	C22—C23—H23A	109.0
O3—Tc1—O1	108.3 (5)	C24—C23—H23B	109.0
O8A—Tc2—O8	109.4 (4)	C22—C23—H23B	109.0
O8A—Tc2—O7	109.1 (5)	H23A—C23—H23B	107.8
O8—Tc2—O7	109.5 (5)	C23—C24—H24A	109.5
O8A—Tc2—O6	109.8 (4)	C23—C24—H24B	109.5
O8—Tc2—O6	107.7 (4)	H24A—C24—H24B	109.5
O7—Tc2—O6	111.2 (5)	C23—C24—H24C	109.5
O12—Tc3—O11A	109.0 (5)	H24A—C24—H24C	109.5
O12—Tc3—O11	108.2 (4)	H24B—C24—H24C	109.5
O11A—Tc3—O11	111.0 (5)	C26—C25—P3	112.1 (13)
O12—Tc3—O10	108.4 (5)	C26—C25—H25A	109.2
O11A—Tc3—O10	110.1 (5)	P3—C25—H25A	109.2
O11—Tc3—O10	110.1 (4)	C26—C25—H25B	109.2
O3A—Tc1A—O4A	109.3 (6)	P3—C25—H25B	109.2
O3A—Tc1A—O2A	108.8 (5)	H25A—C25—H25B	107.9
O4A—Tc1A—O2A	108.8 (5)	C25—C26—C27	110.5 (16)
O3A—Tc1A—O1A	110.3 (5)	C25—C26—H26A	109.6
O4A—Tc1A—O1A	108.4 (4)	C27—C26—H26A	109.6
O2A—Tc1A—O1A	111.2 (4)	C25—C26—H26B	109.6
O5—P1—C1	110.6 (5)	C27—C26—H26B	109.6
O5—P1—C5	110.2 (4)	H26A—C26—H26B	108.1
C1—P1—C5	109.6 (5)	C28—C27—C26	110.0 (16)
O5—P1—C9	111.3 (5)	C28—C27—H27A	109.7
C1—P1—C9	106.6 (5)	C26—C27—H27A	109.7
C5—P1—C9	108.4 (5)	C28—C27—H27B	109.7
O9—P2—C13A	112.1 (5)	C26—C27—H27B	109.7
O9—P2—C17	110.3 (5)	H27A—C27—H27B	108.2
C13A—P2—C17	112.2 (6)	C27—C28—H28A	109.5
O9—P2—C13	108.8 (6)	C27—C28—H28B	109.5
C13A—P2—C13	108.6 (6)	H28A—C28—H28B	109.5
C17—P2—C13	104.6 (6)	C27—C28—H28C	109.5
O13—P3—C25	110.6 (7)	H28A—C28—H28C	109.5
O13—P3—C21	109.3 (5)	H28B—C28—H28C	109.5
C25—P3—C21	113.0 (7)	C2A—C1A—P1A	116.6 (7)
O13—P3—C21A	106.1 (6)	C2A—C1A—H1C	108.1
C25—P3—C21A	106.2 (7)	P1A—C1A—H1C	108.1
C21—P3—C21A	111.4 (7)	C2A—C1A—H1D	108.1
O5A—P1A—C9A	110.5 (5)	P1A—C1A—H1D	108.2
O5A—P1A—C1A	109.4 (4)	H1C—C1A—H1D	107.3
C9A—P1A—C1A	110.8 (5)	C3A—C2A—C1A	111.8 (9)
O5A—P1A—C5A	112.4 (5)	C3A—C2A—H2C	109.3
C9A—P1A—C5A	106.9 (5)	C1A—C2A—H2C	109.3
C1A—P1A—C5A	106.8 (5)	C3A—C2A—H2D	109.3
Tc1—O1—Th1	148.8 (4)	C1A—C2A—H2D	109.3
P1—O5—Th1	158.9 (5)	H2C—C2A—H2D	107.9
Tc2—O6—Th1	148.7 (4)	C2A—C3A—C4A	111.9 (10)
P2—O9—Th1	158.4 (5)	C2A—C3A—H3C	109.2
Tc3—O10—Th1	159.6 (5)	C4A—C3A—H3C	109.2
P3—O13—Th1	164.2 (5)	C2A—C3A—H3D	109.2
Tc1A—O1A—Th1	151.9 (4)	C4A—C3A—H3D	109.2
P1A—O5A—Th1	160.1 (4)	H3C—C3A—H3D	107.9
C2—C1—P1	113.7 (8)	C3A—C4A—H4D	109.5
C2—C1—H1A	108.8	C3A—C4A—H4E	109.5
P1—C1—H1A	108.8	H4D—C4A—H4E	109.5
C2—C1—H1B	108.8	C3A—C4A—H4F	109.5
P1—C1—H1B	108.8	H4D—C4A—H4F	109.5
H1A—C1—H1B	107.7	H4E—C4A—H4F	109.5
C1—C2—C3	110.7 (10)	C6A—C5A—P1A	113.9 (8)
C1—C2—H2A	109.5	C6A—C5A—H5C	108.8
C3—C2—H2A	109.5	P1A—C5A—H5C	108.8
C1—C2—H2B	109.5	C6A—C5A—H5D	108.8
C3—C2—H2B	109.5	P1A—C5A—H5D	108.8
H2A—C2—H2B	108.1	H5C—C5A—H5D	107.7
C4—C3—C2	113.7 (12)	C7A—C6A—C5A	110.7 (10)
C4—C3—H3A	108.8	C7A—C6A—H6C	109.5
C2—C3—H3A	108.8	C5A—C6A—H6C	109.5
C4—C3—H3B	108.8	C7A—C6A—H6D	109.5
C2—C3—H3B	108.8	C5A—C6A—H6D	109.5
H3A—C3—H3B	107.7	H6C—C6A—H6D	108.1
C3—C4—H4A	109.5	C8A—C7A—C6A	115.8 (11)
C3—C4—H4B	109.5	C8A—C7A—H7C	108.3
H4A—C4—H4B	109.5	C6A—C7A—H7C	108.3
C3—C4—H4C	109.5	C8A—C7A—H7D	108.3
H4A—C4—H4C	109.5	C6A—C7A—H7D	108.3
H4B—C4—H4C	109.5	H7C—C7A—H7D	107.4
C6—C5—P1	117.1 (7)	C7A—C8A—H8D	109.5
C6—C5—H5A	108.0	C7A—C8A—H8E	109.5
P1—C5—H5A	108.0	H8D—C8A—H8E	109.5
C6—C5—H5B	108.0	C7A—C8A—H8F	109.5
P1—C5—H5B	108.0	H8D—C8A—H8F	109.5
H5A—C5—H5B	107.3	H8E—C8A—H8F	109.5
C7—C6—C5	110.8 (9)	C10A—C9A—P1A	115.3 (7)
C7—C6—H6A	109.5	C10A—C9A—H9C	108.4
C5—C6—H6A	109.5	P1A—C9A—H9C	108.4
C7—C6—H6B	109.5	C10A—C9A—H9D	108.4
C5—C6—H6B	109.5	P1A—C9A—H9D	108.4
H6A—C6—H6B	108.1	H9C—C9A—H9D	107.5
C8—C7—C6	109.4 (10)	C11A—C10A—C9A	113.7 (9)
C8—C7—H7A	109.8	C11A—C10A—H10C	108.8
C6—C7—H7A	109.8	C9A—C10A—H10C	108.8
C8—C7—H7B	109.8	C11A—C10A—H10D	108.8
C6—C7—H7B	109.8	C9A—C10A—H10D	108.8
H7A—C7—H7B	108.2	H10C—C10A—H10D	107.7
C7—C8—H8A	109.5	C10A—C11A—C12A	114.7 (10)
C7—C8—H8B	109.5	C10A—C11A—H11C	108.6
H8A—C8—H8B	109.5	C12A—C11A—H11C	108.6
C7—C8—H8C	109.5	C10A—C11A—H11D	108.6
H8A—C8—H8C	109.5	C12A—C11A—H11D	108.6
H8B—C8—H8C	109.5	H11C—C11A—H11D	107.6
C10—C9—P1	114.9 (7)	C11A—C12A—H12D	109.5
C10—C9—H9A	108.5	C11A—C12A—H12E	109.5
P1—C9—H9A	108.5	H12D—C12A—H12E	109.5
C10—C9—H9B	108.5	C11A—C12A—H12F	109.5
P1—C9—H9B	108.5	H12D—C12A—H12F	109.5
H9A—C9—H9B	107.5	H12E—C12A—H12F	109.5
C11—C10—C9	113.8 (10)	C14A—C13A—P2	116.3 (9)
C11—C10—H10A	108.8	C14A—C13A—H13A	108.2
C9—C10—H10A	108.8	P2—C13A—H13A	108.2
C11—C10—H10B	108.8	C14A—C13A—H13B	108.2
C9—C10—H10B	108.8	P2—C13A—H13B	108.2
H10A—C10—H10B	107.7	H13A—C13A—H13B	107.4
C12—C11—C10	116.4 (11)	C13A—C14A—C15A	116.4 (11)
C12—C11—H11A	108.2	C13A—C14A—H14A	108.2
C10—C11—H11A	108.2	C15A—C14A—H14A	108.2
C12—C11—H11B	108.2	C13A—C14A—H14B	108.2
C10—C11—H11B	108.2	C15A—C14A—H14B	108.2
H11A—C11—H11B	107.3	H14A—C14A—H14B	107.3
C11—C12—H12A	109.5	C16A—C15A—C14A	117.9 (11)
C11—C12—H12B	109.5	C16A—C15A—H15C	107.8
H12A—C12—H12B	109.5	C14A—C15A—H15C	107.8
C11—C12—H12C	109.5	C16A—C15A—H15D	107.8
H12A—C12—H12C	109.5	C14A—C15A—H15D	107.8
H12B—C12—H12C	109.5	H15C—C15A—H15D	107.2
C14—C13—P2	115.6 (10)	C15A—C16A—H16D	109.5
C14—C13—H13C	108.4	C15A—C16A—H16E	109.5
P2—C13—H13C	108.4	H16D—C16A—H16E	109.5
C14—C13—H13D	108.4	C15A—C16A—H16F	109.5
P2—C13—H13D	108.4	H16D—C16A—H16F	109.5
H13C—C13—H13D	107.4	H16E—C16A—H16F	109.5
C13—C14—C15	113.0 (12)	C22A—C21A—P3	119.2 (11)
C13—C14—H14C	109.0	C22A—C21A—H21C	107.5
C15—C14—H14C	109.0	P3—C21A—H21C	107.5
C13—C14—H14D	109.0	C22A—C21A—H21D	107.5
C15—C14—H14D	109.0	P3—C21A—H21D	107.5
H14C—C14—H14D	107.8	H21C—C21A—H21D	107.0
C16—C15—C14	107.8 (12)	C21A—C22A—C23A	112.6 (12)
C16—C15—H15A	110.2	C21A—C22A—H22C	109.1
C14—C15—H15A	110.2	C23A—C22A—H22C	109.1
C16—C15—H15B	110.2	C21A—C22A—H22D	109.1
C14—C15—H15B	110.2	C23A—C22A—H22D	109.1
H15A—C15—H15B	108.5	H22C—C22A—H22D	107.8
C15—C16—H16A	109.5	C24A—C23A—C22A	113.6 (13)
C15—C16—H16B	109.5	C24A—C23A—H23C	108.8
H16A—C16—H16B	109.5	C22A—C23A—H23C	108.8
C15—C16—H16C	109.5	C24A—C23A—H23D	108.8
H16A—C16—H16C	109.5	C22A—C23A—H23D	108.8
H16B—C16—H16C	109.5	H23C—C23A—H23D	107.7
C18—C17—P2	115.1 (8)	C23A—C24A—H24D	109.5
C18—C17—H17A	108.5	C23A—C24A—H24E	109.5
P2—C17—H17A	108.5	H24D—C24A—H24E	109.5
C18—C17—H17B	108.5	C23A—C24A—H24F	109.5
P2—C17—H17B	108.5	H24D—C24A—H24F	109.5
H17A—C17—H17B	107.5	H24E—C24A—H24F	109.5

O2—Tc1—O1—Th1	−99.2 (11)	C9A—P1A—O5A—Th1	−69.6 (15)
O4—Tc1—O1—Th1	21.4 (12)	C1A—P1A—O5A—Th1	52.7 (15)
O3—Tc1—O1—Th1	141.9 (10)	C5A—P1A—O5A—Th1	171.1 (13)
O9—Th1—O1—Tc1	−178.3 (11)	O9—Th1—O5A—P1A	166.7 (15)
O13—Th1—O1—Tc1	−49.7 (10)	O13—Th1—O5A—P1A	46.8 (16)
O5A—Th1—O1—Tc1	164.6 (7)	O5—Th1—O5A—P1A	−64.4 (15)
O5—Th1—O1—Tc1	41.4 (10)	O6—Th1—O5A—P1A	−118.9 (15)
O6—Th1—O1—Tc1	110.6 (10)	O10—Th1—O5A—P1A	−6.3 (14)
O10—Th1—O1—Tc1	−3.2 (13)	O1A—Th1—O5A—P1A	91.0 (15)
O1A—Th1—O1—Tc1	−111.5 (10)	O1—Th1—O5A—P1A	−177.1 (11)
C1—P1—O5—Th1	86.7 (14)	O5—P1—C1—C2	−59.3 (10)
C5—P1—O5—Th1	−34.6 (15)	C5—P1—C1—C2	62.3 (9)
C9—P1—O5—Th1	−154.9 (13)	C9—P1—C1—C2	179.5 (8)
O9—Th1—O5—P1	48.6 (15)	P1—C1—C2—C3	170.1 (8)
O13—Th1—O5—P1	168.9 (14)	C1—C2—C3—C4	65.0 (15)
O5A—Th1—O5—P1	−57.3 (15)	O5—P1—C5—C6	177.0 (8)
O6—Th1—O5—P1	−2.3 (14)	C1—P1—C5—C6	55.1 (10)
O10—Th1—O5—P1	−114.9 (14)	C9—P1—C5—C6	−61.0 (10)
O1A—Th1—O5—P1	−171.5 (11)	P1—C5—C6—C7	−178.8 (8)
O1—Th1—O5—P1	96.9 (14)	C5—C6—C7—C8	179.9 (11)
O8A—Tc2—O6—Th1	−42.6 (10)	O5—P1—C9—C10	−50.4 (9)
O8—Tc2—O6—Th1	−161.7 (8)	C1—P1—C9—C10	70.3 (9)
O7—Tc2—O6—Th1	78.3 (10)	C5—P1—C9—C10	−171.8 (8)
O9—Th1—O6—Tc2	66.4 (9)	P1—C9—C10—C11	−177.1 (8)
O13—Th1—O6—Tc2	−175.5 (7)	C9—C10—C11—C12	66.9 (15)
O5A—Th1—O6—Tc2	−22.6 (8)	O9—P2—C13—C14	89.6 (12)
O5—Th1—O6—Tc2	−154.2 (9)	C13A—P2—C13—C14	−32.5 (14)
O10—Th1—O6—Tc2	−88.1 (9)	C17—P2—C13—C14	−152.5 (12)
O1A—Th1—O6—Tc2	19.2 (11)	P2—C13—C14—C15	173.4 (11)
O1—Th1—O6—Tc2	134.8 (9)	C13—C14—C15—C16	−179.1 (14)
C13A—P2—O9—Th1	−73.5 (15)	O9—P2—C17—C18	−176.9 (8)
C17—P2—O9—Th1	52.3 (15)	C13A—P2—C17—C18	−51.3 (10)
C13—P2—O9—Th1	166.5 (13)	C13—P2—C17—C18	66.3 (10)
O13—Th1—O9—P2	−58.6 (14)	P2—C17—C18—C19	−175.3 (11)
O5A—Th1—O9—P2	169.9 (14)	C17—C18—C19—C20	177.2 (13)
O5—Th1—O9—P2	46.9 (15)	O13—P3—C21—C22	178.2 (9)
O6—Th1—O9—P2	97.0 (14)	C25—P3—C21—C22	54.6 (11)
O10—Th1—O9—P2	−173.9 (11)	C21A—P3—C21—C22	−64.9 (11)
O1A—Th1—O9—P2	−116.1 (14)	P3—C21—C22—C23	176.4 (9)
O1—Th1—O9—P2	−2.5 (13)	C21—C22—C23—C24	−178.4 (12)
O12—Tc3—O10—Th1	141.2 (16)	O13—P3—C25—C26	−59.1 (19)
O11A—Tc3—O10—Th1	−99.7 (17)	C21—P3—C25—C26	63.8 (18)
O11—Tc3—O10—Th1	23.0 (19)	C21A—P3—C25—C26	−173.9 (16)
O9—Th1—O10—Tc3	165.1 (12)	P3—C25—C26—C27	161.6 (13)
O13—Th1—O10—Tc3	41.7 (17)	C25—C26—C27—C28	73 (2)
O5A—Th1—O10—Tc3	−177.9 (18)	O5A—P1A—C1A—C2A	−173.7 (7)
O5—Th1—O10—Tc3	−48.2 (16)	C9A—P1A—C1A—C2A	−51.6 (9)
O6—Th1—O10—Tc3	−112.7 (17)	C5A—P1A—C1A—C2A	64.5 (9)
O1A—Th1—O10—Tc3	110.4 (17)	P1A—C1A—C2A—C3A	−173.5 (8)
O1—Th1—O10—Tc3	−4 (2)	C1A—C2A—C3A—C4A	175.4 (11)
C25—P3—O13—Th1	114 (2)	O5A—P1A—C5A—C6A	57.8 (10)
C21—P3—O13—Th1	−11 (2)	C9A—P1A—C5A—C6A	−63.6 (10)
C21A—P3—O13—Th1	−131 (2)	C1A—P1A—C5A—C6A	177.8 (9)
O9—Th1—O13—P3	−90 (2)	P1A—C5A—C6A—C7A	174.5 (9)
O5A—Th1—O13—P3	16 (2)	C5A—C6A—C7A—C8A	−69.2 (15)
O5—Th1—O13—P3	141 (2)	O5A—P1A—C9A—C10A	63.0 (9)
O6—Th1—O13—P3	161.4 (18)	C1A—P1A—C9A—C10A	−58.4 (9)
O10—Th1—O13—P3	67 (2)	C5A—P1A—C9A—C10A	−174.4 (8)
O1A—Th1—O13—P3	−30 (2)	P1A—C9A—C10A—C11A	−175.5 (8)
O1—Th1—O13—P3	−145 (2)	C9A—C10A—C11A—C12A	−61.3 (14)
O3A—Tc1A—O1A—Th1	66.3 (12)	O9—P2—C13A—C14A	62.3 (11)
O4A—Tc1A—O1A—Th1	−174.0 (10)	C17—P2—C13A—C14A	−62.4 (11)
O2A—Tc1A—O1A—Th1	−54.5 (12)	C13—P2—C13A—C14A	−177.6 (10)
O9—Th1—O1A—Tc1A	−11.2 (10)	P2—C13A—C14A—C15A	−173.2 (9)
O13—Th1—O1A—Tc1A	−137.8 (11)	C13A—C14A—C15A—C16A	−61.6 (18)
O5A—Th1—O1A—Tc1A	77.2 (10)	O13—P3—C21A—C22A	−159.7 (11)
O5—Th1—O1A—Tc1A	−158.7 (7)	C25—P3—C21A—C22A	−42.0 (14)
O6—Th1—O1A—Tc1A	35.7 (13)	C21—P3—C21A—C22A	81.5 (13)
O10—Th1—O1A—Tc1A	148.2 (11)	P3—C21A—C22A—C23A	171.1 (11)
O1—Th1—O1A—Tc1A	−74.9 (11)	C21A—C22A—C23A—C24A	177.4 (14)

(IIIat130) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	D_x = 1.703 Mg m⁻³
M_r = 1753.26	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbc2₁	Cell parameters from 5490 reflections
a = 21.358 (13) Å	θ = 2.7–26.1°
b = 21.651 (13) Å	µ = 3.11 mm⁻¹
c = 14.790 (9) Å	T = 130 K
V = 6839 (7) Å³	Block, colourless
Z = 4	0.10 × 0.10 × 0.10 mm
F(000) = 3512

Data collection top

CCD area detector diffractometer	14038 independent reflections
Radiation source: fine-focus sealed tube	12090 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.090
phi and ω scans	θ_max = 26.4°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −26→26
T_min = 0.746, T_max = 0.746	k = −26→26
50705 measured reflections	l = −17→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.053	H-atom parameters constrained
wR(F²) = 0.130	w = 1/[σ²(F_o²) + (0.0001P)² + 21.3104P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.004
14038 reflections	Δρ_max = 3.15 e Å⁻³
707 parameters	Δρ_min = −1.14 e Å⁻³
23 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.017 (6)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	V = 6839 (7) Å³
M_r = 1753.26	Z = 4
Orthorhombic, Pbc2₁	Mo Kα radiation
a = 21.358 (13) Å	µ = 3.11 mm⁻¹
b = 21.651 (13) Å	T = 130 K
c = 14.790 (9) Å	0.10 × 0.10 × 0.10 mm

Data collection top

CCD area detector diffractometer	14038 independent reflections
Absorption correction: multi-scan SADABS	12090 reflections with I > 2σ(I)
T_min = 0.746, T_max = 0.746	R_int = 0.090
50705 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.053	H-atom parameters constrained
wR(F²) = 0.130	w = 1/[σ²(F_o²) + (0.0001P)² + 21.3104P] where P = (F_o² + 2F_c²)/3
S = 1.05	Δρ_max = 3.15 e Å⁻³
14038 reflections	Δρ_min = −1.14 e Å⁻³
707 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
23 restraints	Absolute structure parameter: 0.017 (6)

Special details top

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

	x	y	z	U_iso*/U_eq
Th1	0.251916 (15)	0.005307 (14)	0.15872 (4)	0.01725 (9)
Tc1	0.39834 (4)	−0.00417 (4)	−0.01338 (7)	0.0257 (2)
Tc2	0.26231 (4)	0.16605 (4)	0.29377 (6)	0.02333 (18)
Tc3	0.25049 (4)	−0.13768 (5)	0.34153 (7)	0.0292 (2)
Tc1A	0.09090 (4)	−0.01248 (4)	0.01686 (6)	0.0241 (2)
P1	0.41066 (14)	0.00275 (13)	0.2745 (2)	0.0287 (7)
P2	0.22668 (14)	0.13502 (13)	−0.00784 (19)	0.0259 (6)
P3	0.25961 (16)	−0.15109 (15)	0.0463 (3)	0.0403 (8)
P1A	0.11828 (12)	0.03693 (12)	0.32300 (17)	0.0237 (6)
O1	0.3287 (4)	0.0192 (4)	0.0381 (6)	0.041 (2)
O2	0.4577 (4)	0.0383 (4)	0.0226 (7)	0.055 (2)
O3	0.3906 (5)	0.0058 (4)	−0.1261 (6)	0.057 (3)
O4	0.4128 (4)	−0.0774 (4)	0.0080 (6)	0.053 (3)
O5	0.3519 (3)	−0.0112 (4)	0.2235 (5)	0.0319 (18)
O6	0.2839 (4)	0.0993 (3)	0.2365 (5)	0.0312 (18)
O7	0.2384 (5)	0.1486 (5)	0.4007 (6)	0.053 (3)
O8	0.3252 (4)	0.2132 (4)	0.2971 (6)	0.0401 (19)
O9	0.2208 (4)	0.0872 (3)	0.0674 (5)	0.0303 (17)
O10	0.2379 (4)	−0.0712 (4)	0.2774 (6)	0.044 (2)
O11	0.3258 (4)	−0.1610 (4)	0.3316 (6)	0.052 (2)
O12	0.2352 (4)	−0.1213 (4)	0.4505 (6)	0.044 (2)
O13	0.2682 (4)	−0.0888 (3)	0.0874 (6)	0.040 (2)
O1A	0.1554 (4)	−0.0289 (4)	0.0855 (6)	0.038 (2)
O2A	0.0470 (4)	0.0437 (4)	0.0620 (6)	0.045 (2)
O3A	0.1146 (5)	0.0101 (5)	−0.0843 (8)	0.063 (3)
O4A	0.0473 (4)	−0.0763 (4)	0.0071 (6)	0.051 (2)
O5A	0.1687 (3)	0.0390 (3)	0.2502 (5)	0.0300 (17)
O8A	0.2043 (4)	0.2013 (4)	0.2404 (6)	0.045 (2)
O11A	0.2020 (5)	−0.1937 (4)	0.3072 (6)	0.052 (2)
C1	0.3985 (5)	−0.0110 (5)	0.3923 (8)	0.030 (3)
H1A	0.3889	−0.0544	0.4010	0.037*
H1B	0.4371	−0.0024	0.4244	0.037*
C2	0.3458 (6)	0.0279 (7)	0.4338 (9)	0.044 (3)
H2A	0.3087	0.0251	0.3961	0.052*
H2B	0.3585	0.0708	0.4364	0.052*
C3	0.3305 (6)	0.0045 (6)	0.5301 (10)	0.047 (3)
H3A	0.2937	0.0259	0.5524	0.056*
H3B	0.3207	−0.0392	0.5275	0.056*
C4	0.3850 (7)	0.0146 (8)	0.5967 (10)	0.069 (5)
H4A	0.4209	−0.0085	0.5768	0.104*
H4B	0.3728	0.0008	0.6558	0.104*
H4C	0.3953	0.0577	0.5989	0.104*
C5	0.4333 (5)	0.0813 (5)	0.2579 (7)	0.025 (2)
H5A	0.4413	0.0873	0.1939	0.030*
H5B	0.3980	0.1073	0.2737	0.030*
C6	0.4903 (5)	0.1046 (5)	0.3099 (8)	0.036 (3)
H6A	0.4831	0.1002	0.3744	0.044*
H6B	0.5267	0.0800	0.2941	0.044*
C7	0.5026 (5)	0.1716 (5)	0.2875 (10)	0.039 (3)
H7A	0.4662	0.1963	0.3029	0.047*
H7B	0.5103	0.1760	0.2232	0.047*
C8	0.5593 (6)	0.1944 (6)	0.3407 (9)	0.054 (4)
H8A	0.5509	0.1914	0.4043	0.082*
H8B	0.5678	0.2366	0.3252	0.082*
H8C	0.5951	0.1694	0.3260	0.082*
C9	0.4732 (5)	−0.0466 (5)	0.2410 (7)	0.029 (2)
H9A	0.4876	−0.0337	0.1817	0.035*
H9B	0.5077	−0.0409	0.2829	0.035*
C10	0.4577 (6)	−0.1137 (6)	0.2372 (8)	0.040 (3)
H10A	0.4412	−0.1262	0.2955	0.048*
H10B	0.4248	−0.1198	0.1928	0.048*
C11	0.5111 (6)	−0.1544 (5)	0.2138 (8)	0.039 (3)
H11A	0.4951	−0.1959	0.2048	0.047*
H11B	0.5283	−0.1407	0.1566	0.047*
C12	0.5614 (7)	−0.1574 (6)	0.2788 (11)	0.060 (4)
H12A	0.5444	−0.1564	0.3389	0.090*
H12B	0.5888	−0.1227	0.2704	0.090*
H12C	0.5845	−0.1950	0.2705	0.090*
C13	0.1508 (6)	0.1734 (5)	−0.0231 (10)	0.045 (3)
H13C	0.1468	0.1850	−0.0862	0.054*
H13D	0.1180	0.1437	−0.0101	0.054*
C14	0.1398 (6)	0.2290 (6)	0.0328 (9)	0.049 (3)
H14C	0.1731	0.2584	0.0211	0.059*
H14D	0.1423	0.2173	0.0960	0.059*
C15	0.0784 (5)	0.2603 (6)	0.0170 (9)	0.040 (3)
H15A	0.0748	0.2706	−0.0466	0.048*
H15B	0.0448	0.2318	0.0318	0.048*
C16	0.0708 (7)	0.3166 (7)	0.0706 (10)	0.062 (4)
H16A	0.0680	0.3060	0.1335	0.093*
H16B	0.0333	0.3375	0.0524	0.093*
H16C	0.1062	0.3432	0.0612	0.093*
C17	0.2444 (5)	0.0987 (5)	−0.1135 (8)	0.033 (3)
H17A	0.2826	0.0749	−0.1063	0.040*
H17B	0.2111	0.0700	−0.1277	0.040*
C18	0.2528 (5)	0.1421 (6)	−0.1929 (8)	0.042 (3)
H18A	0.2162	0.1686	−0.1975	0.050*
H18B	0.2888	0.1683	−0.1820	0.050*
C19	0.2615 (9)	0.1092 (8)	−0.2793 (10)	0.072 (5)
H19A	0.2262	0.0818	−0.2893	0.086*
H19B	0.2990	0.0840	−0.2758	0.086*
C20	0.2672 (10)	0.1537 (7)	−0.3594 (9)	0.080 (6)
H20A	0.2356	0.1851	−0.3547	0.120*
H20B	0.2616	0.1313	−0.4149	0.120*
H20C	0.3078	0.1725	−0.3589	0.120*
C21	0.1844 (6)	−0.1817 (5)	0.0752 (7)	0.033 (3)
H21A	0.1819	−0.1837	0.1406	0.039*
H21B	0.1530	−0.1523	0.0553	0.039*
C22	0.1669 (5)	−0.2437 (6)	0.0387 (8)	0.037 (3)
H22A	0.1990	−0.2733	0.0554	0.044*
H22B	0.1656	−0.2416	−0.0268	0.044*
C23	0.1041 (6)	−0.2662 (5)	0.0731 (9)	0.040 (3)
H23A	0.1051	−0.2675	0.1387	0.048*
H23B	0.0719	−0.2371	0.0552	0.048*
C24	0.0876 (7)	−0.3287 (6)	0.0381 (12)	0.059 (4)
H24A	0.0976	−0.3310	−0.0252	0.089*
H24B	0.0437	−0.3359	0.0464	0.089*
H24C	0.1110	−0.3595	0.0704	0.089*
C25	0.2705 (8)	−0.1487 (7)	−0.0718 (9)	0.055 (4)
H25A	0.3132	−0.1367	−0.0850	0.066*
H25B	0.2637	−0.1896	−0.0968	0.066*
C26	0.2270 (11)	−0.1047 (10)	−0.1147 (11)	0.132 (11)
H26A	0.2236	−0.0678	−0.0777	0.159*
H26B	0.1857	−0.1232	−0.1194	0.159*
C27	0.2511 (7)	−0.0872 (7)	−0.2104 (15)	0.091 (7)
H27A	0.2282	−0.0515	−0.2322	0.109*
H27B	0.2951	−0.0761	−0.2067	0.109*
C28	0.2434 (9)	−0.1397 (9)	−0.2762 (13)	0.091 (7)
H28A	0.2749	−0.1703	−0.2649	0.137*
H28B	0.2477	−0.1244	−0.3368	0.137*
H28C	0.2027	−0.1577	−0.2687	0.137*
C1A	0.1529 (5)	0.0179 (5)	0.4291 (7)	0.026 (2)
H1C	0.1782	−0.0189	0.4211	0.031*
H1D	0.1809	0.0512	0.4462	0.031*
C2A	0.1075 (5)	0.0066 (4)	0.5069 (6)	0.026 (2)
H2C	0.0788	0.0412	0.5116	0.031*
H2D	0.0830	−0.0302	0.4946	0.031*
C3A	0.1419 (6)	−0.0013 (6)	0.5960 (8)	0.042 (3)
H3C	0.1691	0.0340	0.6056	0.051*
H3D	0.1681	−0.0379	0.5926	0.051*
C4A	0.0969 (6)	−0.0076 (7)	0.6770 (8)	0.052 (4)
H4D	0.0698	0.0278	0.6793	0.078*
H4E	0.1207	−0.0100	0.7320	0.078*
H4F	0.0722	−0.0443	0.6702	0.078*
C5A	0.0802 (5)	0.1097 (5)	0.3344 (7)	0.029 (2)
H5C	0.0480	0.1060	0.3803	0.035*
H5D	0.1106	0.1396	0.3558	0.035*
C6A	0.0502 (6)	0.1346 (6)	0.2480 (8)	0.038 (3)
H6C	0.0826	0.1420	0.2033	0.046*
H6D	0.0218	0.1038	0.2237	0.046*
C7A	0.0145 (6)	0.1941 (5)	0.2649 (8)	0.039 (3)
H7C	0.0032	0.2118	0.2069	0.047*
H7D	0.0423	0.2230	0.2947	0.047*
C8A	−0.0450 (7)	0.1879 (6)	0.3218 (10)	0.059 (4)
H8D	−0.0725	0.2219	0.3091	0.089*
H8E	−0.0342	0.1881	0.3848	0.089*
H8F	−0.0657	0.1498	0.3072	0.089*
C9A	0.0593 (5)	−0.0175 (4)	0.2944 (7)	0.026 (2)
H9C	0.0262	−0.0148	0.3391	0.031*
H9D	0.0415	−0.0059	0.2365	0.031*
C10A	0.0810 (5)	−0.0848 (4)	0.2886 (8)	0.028 (2)
H10C	0.1163	−0.0874	0.2476	0.033*
H10D	0.0951	−0.0981	0.3478	0.033*
C11A	0.0295 (6)	−0.1285 (5)	0.2559 (8)	0.037 (3)
H11C	0.0154	−0.1148	0.1969	0.044*
H11D	0.0473	−0.1695	0.2488	0.044*
C12A	−0.0258 (5)	−0.1327 (5)	0.3173 (8)	0.039 (3)
H12D	−0.0119	−0.1407	0.3780	0.058*
H12E	−0.0526	−0.1658	0.2978	0.058*
H12F	−0.0486	−0.0945	0.3158	0.058*
C13A	0.2829 (5)	0.1921 (5)	0.0168 (8)	0.029 (2)
H13A	0.2822	0.2226	−0.0312	0.035*
H13B	0.2706	0.2129	0.0722	0.035*
C14A	0.3504 (5)	0.1686 (5)	0.0279 (9)	0.038 (3)
H14A	0.3505	0.1348	0.0709	0.046*
H14B	0.3648	0.1525	−0.0297	0.046*
C15A	0.3961 (6)	0.2178 (6)	0.0600 (8)	0.043 (3)
H15C	0.3819	0.2324	0.1185	0.052*
H15D	0.4365	0.1982	0.0691	0.052*
C16A	0.4056 (7)	0.2727 (7)	0.0004 (7)	0.051 (4)
H16D	0.4200	0.2594	−0.0579	0.077*
H16E	0.4362	0.2996	0.0271	0.077*
H16F	0.3667	0.2945	−0.0062	0.077*
C21A	0.3235 (6)	−0.2013 (6)	0.0917 (9)	0.049 (3)
H21C	0.3609	−0.1762	0.0970	0.058*
H21D	0.3117	−0.2137	0.1524	0.058*
C22A	0.3403 (6)	−0.2568 (6)	0.0423 (9)	0.046 (3)
H22C	0.3461	−0.2468	−0.0211	0.056*
H22D	0.3066	−0.2867	0.0468	0.056*
C23A	0.4005 (6)	−0.2850 (7)	0.0798 (10)	0.058 (4)
H23C	0.4345	−0.2557	0.0727	0.069*
H23D	0.3953	−0.2929	0.1439	0.069*
C24A	0.4176 (8)	−0.3444 (7)	0.0329 (12)	0.071 (5)
H24D	0.3826	−0.3722	0.0346	0.107*
H24E	0.4527	−0.3630	0.0630	0.107*
H24F	0.4285	−0.3359	−0.0289	0.107*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.01293 (16)	0.02320 (17)	0.01561 (14)	−0.00018 (13)	−0.00026 (13)	0.0005 (2)
Tc1	0.0208 (5)	0.0312 (5)	0.0251 (5)	0.0031 (4)	0.0063 (4)	0.0019 (4)
Tc2	0.0248 (4)	0.0249 (4)	0.0202 (4)	0.0000 (4)	−0.0006 (4)	−0.0029 (4)
Tc3	0.0251 (5)	0.0370 (5)	0.0254 (5)	0.0041 (4)	0.0037 (4)	0.0124 (4)
Tc1A	0.0162 (4)	0.0335 (5)	0.0226 (4)	−0.0002 (4)	−0.0030 (4)	−0.0015 (4)
P1	0.0251 (15)	0.0311 (16)	0.0299 (16)	−0.0018 (12)	−0.0069 (12)	0.0003 (11)
P2	0.0334 (16)	0.0237 (14)	0.0206 (15)	0.0016 (12)	−0.0007 (11)	0.0034 (11)
P3	0.0399 (18)	0.0303 (16)	0.051 (2)	−0.0055 (14)	0.0143 (15)	−0.0117 (15)
P1A	0.0202 (13)	0.0283 (14)	0.0225 (14)	0.0005 (10)	0.0061 (10)	−0.0009 (11)
O1	0.041 (5)	0.044 (5)	0.038 (5)	0.012 (4)	0.018 (4)	0.010 (4)
O2	0.049 (6)	0.054 (6)	0.062 (6)	−0.002 (4)	0.006 (5)	−0.002 (5)
O3	0.068 (7)	0.076 (7)	0.028 (5)	0.017 (5)	0.019 (5)	0.010 (4)
O4	0.047 (6)	0.063 (6)	0.050 (6)	0.020 (5)	0.016 (4)	0.010 (5)
O5	0.021 (4)	0.039 (5)	0.036 (4)	0.002 (3)	−0.013 (3)	−0.001 (4)
O6	0.032 (5)	0.028 (4)	0.033 (4)	−0.004 (3)	0.001 (3)	−0.006 (3)
O7	0.072 (7)	0.065 (6)	0.022 (4)	−0.019 (5)	0.016 (4)	0.008 (4)
O8	0.045 (5)	0.043 (5)	0.032 (4)	0.000 (4)	−0.001 (4)	−0.005 (4)
O9	0.034 (4)	0.040 (5)	0.017 (4)	0.005 (4)	0.002 (3)	0.005 (3)
O10	0.027 (4)	0.062 (6)	0.044 (6)	0.010 (4)	0.014 (4)	0.020 (4)
O11	0.048 (6)	0.067 (6)	0.040 (5)	0.021 (5)	0.009 (4)	0.021 (5)
O12	0.060 (6)	0.046 (5)	0.028 (5)	0.006 (4)	0.001 (4)	0.005 (4)
O13	0.038 (5)	0.025 (4)	0.057 (6)	0.005 (4)	0.007 (4)	−0.020 (4)
O1A	0.029 (4)	0.034 (4)	0.050 (5)	−0.001 (3)	−0.019 (4)	−0.003 (4)
O2A	0.033 (5)	0.063 (6)	0.040 (5)	0.015 (4)	−0.003 (4)	−0.008 (4)
O3A	0.049 (6)	0.067 (7)	0.074 (8)	0.003 (5)	−0.019 (6)	0.034 (6)
O4A	0.044 (5)	0.057 (6)	0.053 (6)	−0.018 (4)	−0.017 (4)	0.001 (4)
O5A	0.032 (4)	0.032 (4)	0.026 (4)	0.001 (3)	0.017 (3)	−0.001 (3)
O8A	0.048 (6)	0.038 (5)	0.048 (5)	0.000 (4)	0.003 (4)	−0.005 (4)
O11A	0.082 (7)	0.051 (5)	0.023 (5)	−0.001 (5)	−0.007 (4)	0.001 (4)
C1	0.020 (6)	0.032 (6)	0.039 (7)	−0.002 (5)	−0.004 (5)	0.001 (5)
C2	0.026 (7)	0.055 (8)	0.049 (8)	0.011 (6)	−0.002 (5)	0.000 (7)
C3	0.035 (7)	0.062 (9)	0.043 (8)	0.001 (6)	−0.004 (6)	−0.014 (7)
C4	0.063 (11)	0.114 (14)	0.031 (8)	0.004 (10)	−0.017 (7)	−0.035 (9)
C5	0.018 (5)	0.036 (6)	0.020 (5)	0.008 (4)	−0.011 (4)	−0.005 (4)
C6	0.032 (6)	0.037 (7)	0.040 (7)	−0.004 (5)	−0.013 (5)	0.008 (5)
C7	0.034 (6)	0.035 (7)	0.049 (7)	−0.006 (5)	−0.005 (6)	0.011 (6)
C8	0.056 (9)	0.058 (9)	0.050 (8)	−0.019 (7)	−0.008 (7)	0.023 (7)
C9	0.019 (5)	0.040 (7)	0.029 (6)	0.005 (5)	−0.006 (4)	0.006 (5)
C10	0.041 (7)	0.048 (8)	0.031 (6)	−0.010 (6)	−0.006 (5)	0.003 (6)
C11	0.049 (8)	0.028 (7)	0.039 (7)	−0.005 (5)	0.009 (6)	−0.003 (5)
C12	0.067 (10)	0.045 (8)	0.069 (11)	0.027 (7)	−0.017 (8)	−0.013 (7)
C13	0.041 (7)	0.030 (6)	0.064 (8)	0.005 (5)	0.000 (7)	0.015 (6)
C14	0.040 (7)	0.057 (8)	0.050 (8)	0.012 (6)	0.011 (6)	−0.002 (7)
C15	0.031 (7)	0.042 (7)	0.048 (7)	0.014 (5)	0.003 (5)	0.010 (6)
C16	0.067 (11)	0.062 (10)	0.056 (9)	0.004 (8)	0.010 (8)	−0.002 (8)
C17	0.044 (8)	0.027 (6)	0.028 (6)	0.001 (5)	−0.005 (5)	0.000 (5)
C18	0.056 (9)	0.038 (7)	0.032 (7)	0.002 (5)	0.012 (6)	0.008 (5)
C19	0.135 (16)	0.058 (9)	0.022 (7)	−0.007 (10)	−0.004 (8)	0.000 (6)
C20	0.165 (18)	0.057 (9)	0.018 (7)	−0.010 (10)	0.006 (8)	−0.003 (6)
C21	0.042 (7)	0.031 (6)	0.025 (6)	0.001 (5)	0.001 (5)	−0.001 (5)
C22	0.034 (6)	0.045 (7)	0.032 (7)	0.004 (5)	0.011 (5)	0.004 (5)
C23	0.037 (7)	0.027 (6)	0.057 (8)	−0.008 (5)	0.000 (6)	−0.002 (6)
C24	0.050 (9)	0.035 (7)	0.092 (12)	0.003 (6)	0.010 (8)	−0.020 (8)
C25	0.098 (12)	0.047 (8)	0.021 (7)	0.003 (8)	0.011 (7)	−0.001 (6)
C26	0.143 (19)	0.18 (2)	0.075 (15)	0.121 (18)	−0.052 (14)	−0.084 (16)
C27	0.076 (15)	0.046 (10)	0.15 (2)	0.002 (8)	−0.001 (14)	−0.005 (12)
C28	0.113 (18)	0.093 (15)	0.068 (13)	0.007 (12)	−0.055 (12)	−0.009 (11)
C1A	0.018 (5)	0.032 (6)	0.028 (6)	−0.002 (4)	0.007 (4)	−0.003 (5)
C2A	0.019 (5)	0.025 (5)	0.033 (7)	−0.002 (4)	−0.001 (4)	−0.007 (4)
C3A	0.047 (8)	0.057 (8)	0.022 (6)	−0.007 (6)	−0.009 (5)	−0.001 (5)
C4A	0.036 (7)	0.099 (12)	0.020 (7)	−0.001 (7)	−0.001 (5)	−0.004 (6)
C5A	0.023 (6)	0.032 (6)	0.033 (6)	0.013 (5)	0.001 (4)	0.007 (5)
C6A	0.042 (7)	0.040 (7)	0.033 (6)	0.004 (6)	0.006 (5)	0.007 (5)
C7A	0.048 (8)	0.033 (7)	0.037 (7)	0.005 (6)	−0.005 (5)	0.002 (5)
C8A	0.056 (9)	0.054 (9)	0.068 (11)	0.016 (7)	0.001 (7)	0.000 (8)
C9A	0.030 (5)	0.030 (4)	0.018 (5)	0.006 (3)	−0.016 (4)	0.003 (4)
C10A	0.030 (5)	0.026 (4)	0.027 (5)	0.003 (4)	0.005 (5)	0.003 (4)
C11A	0.038 (7)	0.035 (7)	0.037 (7)	−0.005 (5)	0.009 (5)	−0.008 (5)
C12A	0.030 (6)	0.044 (7)	0.043 (8)	−0.011 (5)	0.005 (5)	0.001 (6)
C13A	0.020 (5)	0.043 (7)	0.025 (5)	−0.016 (5)	−0.004 (4)	0.011 (5)
C14A	0.029 (6)	0.044 (7)	0.042 (7)	−0.003 (5)	−0.004 (5)	0.005 (6)
C15A	0.047 (8)	0.048 (8)	0.035 (7)	−0.004 (6)	−0.015 (6)	−0.004 (6)
C16A	0.073 (11)	0.059 (9)	0.022 (8)	−0.012 (7)	0.010 (6)	−0.010 (5)
C21A	0.039 (7)	0.051 (8)	0.056 (8)	0.015 (6)	0.000 (6)	−0.015 (7)
C22A	0.038 (7)	0.057 (8)	0.045 (8)	0.000 (6)	−0.009 (6)	−0.002 (6)
C23A	0.036 (8)	0.085 (11)	0.052 (9)	0.024 (7)	−0.015 (6)	0.014 (8)
C24A	0.070 (11)	0.080 (11)	0.064 (10)	−0.003 (9)	−0.027 (9)	−0.012 (10)

Geometric parameters (Å, º) top

Th1—O13	2.321 (7)	C18—H18A	0.9700
Th1—O9	2.325 (7)	C18—H18B	0.9700
Th1—O5A	2.350 (7)	C19—C20	1.53 (2)
Th1—O5	2.367 (7)	C19—H19A	0.9700
Th1—O10	2.433 (8)	C19—H19B	0.9700
Th1—O6	2.435 (7)	C20—H20A	0.9600
Th1—O1	2.441 (8)	C20—H20B	0.9600
Th1—O1A	2.443 (8)	C20—H20C	0.9600
Tc1—O4	1.647 (9)	C21—C22	1.494 (16)
Tc1—O2	1.653 (10)	C21—H21A	0.9700
Tc1—O3	1.689 (9)	C21—H21B	0.9700
Tc1—O1	1.747 (8)	C22—C23	1.515 (16)
Tc2—O8A	1.655 (9)	C22—H22A	0.9700
Tc2—O8	1.688 (8)	C22—H22B	0.9700
Tc2—O7	1.704 (8)	C23—C24	1.492 (16)
Tc2—O6	1.737 (7)	C23—H23A	0.9700
Tc3—O11A	1.673 (9)	C23—H23B	0.9700
Tc3—O12	1.682 (8)	C24—H24A	0.9600
Tc3—O11	1.693 (9)	C24—H24B	0.9600
Tc3—O10	1.743 (9)	C24—H24C	0.9600
Tc1A—O3A	1.653 (11)	C25—C26	1.475 (15)
Tc1A—O4A	1.672 (8)	C25—H25A	0.9700
Tc1A—O2A	1.675 (8)	C25—H25B	0.9700
Tc1A—O1A	1.749 (8)	C26—C27	1.553 (17)
P1—O5	1.495 (7)	C26—H26A	0.9700
P1—C9	1.781 (11)	C26—H26B	0.9700
P1—C5	1.786 (11)	C27—C28	1.505 (16)
P1—C1	1.786 (13)	C27—H27A	0.9700
P2—O9	1.526 (8)	C27—H27B	0.9700
P2—C13A	1.761 (10)	C28—H28A	0.9600
P2—C17	1.789 (12)	C28—H28B	0.9600
P2—C13	1.835 (12)	C28—H28C	0.9600
P3—O13	1.491 (8)	C1A—C2A	1.526 (13)
P3—C25	1.762 (14)	C1A—H1C	0.9700
P3—C21	1.790 (12)	C1A—H1D	0.9700
P3—C21A	1.870 (13)	C2A—C3A	1.518 (15)
P1A—O5A	1.523 (7)	C2A—H2C	0.9700
P1A—C9A	1.776 (9)	C2A—H2D	0.9700
P1A—C5A	1.780 (10)	C3A—C4A	1.543 (17)
P1A—C1A	1.783 (11)	C3A—H3C	0.9700
C1—C2	1.535 (16)	C3A—H3D	0.9700
C1—H1A	0.9700	C4A—H4D	0.9600
C1—H1B	0.9700	C4A—H4E	0.9600
C2—C3	1.547 (18)	C4A—H4F	0.9600
C2—H2A	0.9700	C5A—C6A	1.528 (15)
C2—H2B	0.9700	C5A—H5C	0.9700
C3—C4	1.540 (18)	C5A—H5D	0.9700
C3—H3A	0.9700	C6A—C7A	1.518 (16)
C3—H3B	0.9700	C6A—H6C	0.9700
C4—H4A	0.9600	C6A—H6D	0.9700
C4—H4B	0.9600	C7A—C8A	1.530 (17)
C4—H4C	0.9600	C7A—H7C	0.9700
C5—C6	1.526 (13)	C7A—H7D	0.9700
C5—H5A	0.9700	C8A—H8D	0.9600
C5—H5B	0.9700	C8A—H8E	0.9600
C6—C7	1.512 (15)	C8A—H8F	0.9600
C6—H6A	0.9700	C9A—C10A	1.532 (13)
C6—H6B	0.9700	C9A—H9C	0.9700
C7—C8	1.526 (16)	C9A—H9D	0.9700
C7—H7A	0.9700	C10A—C11A	1.528 (15)
C7—H7B	0.9700	C10A—H10C	0.9700
C8—H8A	0.9600	C10A—H10D	0.9700
C8—H8B	0.9600	C11A—C12A	1.494 (15)
C8—H8C	0.9600	C11A—H11C	0.9700
C9—C10	1.491 (16)	C11A—H11D	0.9700
C9—H9A	0.9700	C12A—H12D	0.9600
C9—H9B	0.9700	C12A—H12E	0.9600
C10—C11	1.483 (17)	C12A—H12F	0.9600
C10—H10A	0.9700	C13A—C14A	1.539 (15)
C10—H10B	0.9700	C13A—H13A	0.9700
C11—C12	1.443 (18)	C13A—H13B	0.9700
C11—H11A	0.9700	C14A—C15A	1.520 (16)
C11—H11B	0.9700	C14A—H14A	0.9700
C12—H12A	0.9600	C14A—H14B	0.9700
C12—H12B	0.9600	C15A—C16A	1.494 (16)
C12—H12C	0.9600	C15A—H15C	0.9700
C13—C14	1.479 (13)	C15A—H15D	0.9700
C13—H13C	0.9700	C16A—H16D	0.9600
C13—H13D	0.9700	C16A—H16E	0.9600
C14—C15	1.494 (16)	C16A—H16F	0.9600
C14—H14C	0.9700	C21A—C22A	1.450 (17)
C14—H14D	0.9700	C21A—H21C	0.9700
C15—C16	1.463 (18)	C21A—H21D	0.9700
C15—H15A	0.9700	C22A—C23A	1.527 (16)
C15—H15B	0.9700	C22A—H22C	0.9700
C16—H16A	0.9600	C22A—H22D	0.9700
C16—H16B	0.9600	C23A—C24A	1.51 (2)
C16—H16C	0.9600	C23A—H23C	0.9700
C17—C18	1.515 (15)	C23A—H23D	0.9700
C17—H17A	0.9700	C24A—H24D	0.9600
C17—H17B	0.9700	C24A—H24E	0.9600
C18—C19	1.476 (19)	C24A—H24F	0.9600

O13—Th1—O9	116.6 (3)	C19—C18—C17	112.7 (11)
O13—Th1—O5A	130.4 (3)	C19—C18—H18A	109.0
O9—Th1—O5A	83.2 (2)	C17—C18—H18A	109.0
O13—Th1—O5	85.2 (3)	C19—C18—H18B	109.0
O9—Th1—O5	127.5 (3)	C17—C18—H18B	109.0
O5A—Th1—O5	119.7 (3)	H18A—C18—H18B	107.8
O13—Th1—O10	75.4 (3)	C18—C19—C20	112.1 (13)
O9—Th1—O10	154.6 (3)	C18—C19—H19A	109.2
O5A—Th1—O10	72.8 (3)	C20—C19—H19A	109.2
O5—Th1—O10	73.5 (3)	C18—C19—H19B	109.2
O13—Th1—O6	155.0 (3)	C20—C19—H19B	109.2
O9—Th1—O6	73.6 (3)	H19A—C19—H19B	107.9
O5A—Th1—O6	71.4 (3)	C19—C20—H20A	109.5
O5—Th1—O6	71.4 (3)	C19—C20—H20B	109.5
O10—Th1—O6	105.2 (3)	H20A—C20—H20B	109.5
O13—Th1—O1	71.1 (3)	C19—C20—H20C	109.5
O9—Th1—O1	71.0 (3)	H20A—C20—H20C	109.5
O5A—Th1—O1	152.9 (3)	H20B—C20—H20C	109.5
O5—Th1—O1	73.1 (3)	C22—C21—P3	118.0 (8)
O10—Th1—O1	133.9 (3)	C22—C21—H21A	107.8
O6—Th1—O1	93.1 (3)	P3—C21—H21A	107.8
O13—Th1—O1A	70.0 (3)	C22—C21—H21B	107.8
O9—Th1—O1A	74.5 (3)	P3—C21—H21B	107.8
O5A—Th1—O1A	73.2 (3)	H21A—C21—H21B	107.1
O5—Th1—O1A	153.5 (3)	C21—C22—C23	112.9 (10)
O10—Th1—O1A	90.5 (3)	C21—C22—H22A	109.0
O6—Th1—O1A	134.4 (3)	C23—C22—H22A	109.0
O1—Th1—O1A	106.3 (3)	C21—C22—H22B	109.0
O4—Tc1—O2	109.2 (5)	C23—C22—H22B	109.0
O4—Tc1—O3	109.3 (5)	H22A—C22—H22B	107.8
O2—Tc1—O3	108.8 (5)	C24—C23—C22	112.6 (11)
O4—Tc1—O1	110.8 (4)	C24—C23—H23A	109.1
O2—Tc1—O1	110.6 (5)	C22—C23—H23A	109.1
O3—Tc1—O1	108.1 (4)	C24—C23—H23B	109.1
O8A—Tc2—O8	109.3 (4)	C22—C23—H23B	109.1
O8A—Tc2—O7	108.8 (5)	H23A—C23—H23B	107.8
O8—Tc2—O7	110.2 (4)	C23—C24—H24A	109.5
O8A—Tc2—O6	110.4 (4)	C23—C24—H24B	109.5
O8—Tc2—O6	107.8 (4)	H24A—C24—H24B	109.5
O7—Tc2—O6	110.3 (4)	C23—C24—H24C	109.5
O11A—Tc3—O12	108.8 (4)	H24A—C24—H24C	109.5
O11A—Tc3—O11	110.2 (4)	H24B—C24—H24C	109.5
O12—Tc3—O11	109.3 (4)	C26—C25—P3	111.2 (12)
O11A—Tc3—O10	109.8 (4)	C26—C25—H25A	109.4
O12—Tc3—O10	108.5 (4)	P3—C25—H25A	109.4
O11—Tc3—O10	110.2 (4)	C26—C25—H25B	109.4
O3A—Tc1A—O4A	109.7 (5)	P3—C25—H25B	109.4
O3A—Tc1A—O2A	108.5 (5)	H25A—C25—H25B	108.0
O4A—Tc1A—O2A	108.8 (5)	C25—C26—C27	109.9 (15)
O3A—Tc1A—O1A	110.2 (5)	C25—C26—H26A	109.7
O4A—Tc1A—O1A	108.7 (4)	C27—C26—H26A	109.7
O2A—Tc1A—O1A	111.0 (4)	C25—C26—H26B	109.7
O5—P1—C9	111.6 (5)	C27—C26—H26B	109.7
O5—P1—C5	110.5 (5)	H26A—C26—H26B	108.2
C9—P1—C5	109.3 (5)	C28—C27—C26	111.6 (15)
O5—P1—C1	109.7 (5)	C28—C27—H27A	109.3
C9—P1—C1	106.2 (5)	C26—C27—H27A	109.3
C5—P1—C1	109.4 (5)	C28—C27—H27B	109.3
O9—P2—C13A	112.5 (5)	C26—C27—H27B	109.3
O9—P2—C17	110.9 (5)	H27A—C27—H27B	108.0
C13A—P2—C17	110.2 (6)	C27—C28—H28A	109.5
O9—P2—C13	108.9 (5)	C27—C28—H28B	109.5
C13A—P2—C13	108.0 (5)	H28A—C28—H28B	109.5
C17—P2—C13	106.2 (6)	C27—C28—H28C	109.5
O13—P3—C25	111.3 (7)	H28A—C28—H28C	109.5
O13—P3—C21	110.3 (5)	H28B—C28—H28C	109.5
C25—P3—C21	111.5 (7)	C2A—C1A—P1A	115.9 (7)
O13—P3—C21A	106.9 (6)	C2A—C1A—H1C	108.3
C25—P3—C21A	106.0 (7)	P1A—C1A—H1C	108.3
C21—P3—C21A	110.7 (6)	C2A—C1A—H1D	108.3
O5A—P1A—C9A	110.6 (5)	P1A—C1A—H1D	108.3
O5A—P1A—C5A	111.3 (5)	H1C—C1A—H1D	107.4
C9A—P1A—C5A	106.6 (5)	C3A—C2A—C1A	111.4 (9)
O5A—P1A—C1A	109.6 (4)	C3A—C2A—H2C	109.4
C9A—P1A—C1A	110.5 (5)	C1A—C2A—H2C	109.4
C5A—P1A—C1A	108.1 (5)	C3A—C2A—H2D	109.4
Tc1—O1—Th1	148.7 (4)	C1A—C2A—H2D	109.4
P1—O5—Th1	158.6 (5)	H2C—C2A—H2D	108.0
Tc2—O6—Th1	148.3 (4)	C2A—C3A—C4A	112.4 (11)
P2—O9—Th1	156.5 (5)	C2A—C3A—H3C	109.1
Tc3—O10—Th1	159.3 (4)	C4A—C3A—H3C	109.1
P3—O13—Th1	164.1 (5)	C2A—C3A—H3D	109.1
Tc1A—O1A—Th1	149.4 (4)	C4A—C3A—H3D	109.1
P1A—O5A—Th1	158.8 (5)	H3C—C3A—H3D	107.9
C2—C1—P1	113.8 (8)	C3A—C4A—H4D	109.5
C2—C1—H1A	108.8	C3A—C4A—H4E	109.5
P1—C1—H1A	108.8	H4D—C4A—H4E	109.5
C2—C1—H1B	108.8	C3A—C4A—H4F	109.5
P1—C1—H1B	108.8	H4D—C4A—H4F	109.5
H1A—C1—H1B	107.7	H4E—C4A—H4F	109.5
C1—C2—C3	110.1 (11)	C6A—C5A—P1A	115.1 (8)
C1—C2—H2A	109.6	C6A—C5A—H5C	108.5
C3—C2—H2A	109.6	P1A—C5A—H5C	108.5
C1—C2—H2B	109.6	C6A—C5A—H5D	108.5
C3—C2—H2B	109.6	P1A—C5A—H5D	108.5
H2A—C2—H2B	108.2	H5C—C5A—H5D	107.5
C4—C3—C2	112.5 (12)	C7A—C6A—C5A	111.9 (10)
C4—C3—H3A	109.1	C7A—C6A—H6C	109.2
C2—C3—H3A	109.1	C5A—C6A—H6C	109.2
C4—C3—H3B	109.1	C7A—C6A—H6D	109.2
C2—C3—H3B	109.1	C5A—C6A—H6D	109.2
H3A—C3—H3B	107.8	H6C—C6A—H6D	107.9
C3—C4—H4A	109.5	C6A—C7A—C8A	115.7 (10)
C3—C4—H4B	109.5	C6A—C7A—H7C	108.4
H4A—C4—H4B	109.5	C8A—C7A—H7C	108.4
C3—C4—H4C	109.5	C6A—C7A—H7D	108.4
H4A—C4—H4C	109.5	C8A—C7A—H7D	108.4
H4B—C4—H4C	109.5	H7C—C7A—H7D	107.4
C6—C5—P1	117.4 (7)	C7A—C8A—H8D	109.5
C6—C5—H5A	107.9	C7A—C8A—H8E	109.5
P1—C5—H5A	107.9	H8D—C8A—H8E	109.5
C6—C5—H5B	107.9	C7A—C8A—H8F	109.5
P1—C5—H5B	107.9	H8D—C8A—H8F	109.5
H5A—C5—H5B	107.2	H8E—C8A—H8F	109.5
C7—C6—C5	110.1 (9)	C10A—C9A—P1A	115.5 (7)
C7—C6—H6A	109.6	C10A—C9A—H9C	108.4
C5—C6—H6A	109.6	P1A—C9A—H9C	108.4
C7—C6—H6B	109.6	C10A—C9A—H9D	108.4
C5—C6—H6B	109.6	P1A—C9A—H9D	108.4
H6A—C6—H6B	108.1	H9C—C9A—H9D	107.5
C6—C7—C8	109.5 (10)	C11A—C10A—C9A	112.9 (9)
C6—C7—H7A	109.8	C11A—C10A—H10C	109.0
C8—C7—H7A	109.8	C9A—C10A—H10C	109.0
C6—C7—H7B	109.8	C11A—C10A—H10D	109.0
C8—C7—H7B	109.8	C9A—C10A—H10D	109.0
H7A—C7—H7B	108.2	H10C—C10A—H10D	107.8
C7—C8—H8A	109.5	C12A—C11A—C10A	114.6 (9)
C7—C8—H8B	109.5	C12A—C11A—H11C	108.6
H8A—C8—H8B	109.5	C10A—C11A—H11C	108.6
C7—C8—H8C	109.5	C12A—C11A—H11D	108.6
H8A—C8—H8C	109.5	C10A—C11A—H11D	108.6
H8B—C8—H8C	109.5	H11C—C11A—H11D	107.6
C10—C9—P1	115.4 (8)	C11A—C12A—H12D	109.5
C10—C9—H9A	108.4	C11A—C12A—H12E	109.5
P1—C9—H9A	108.4	H12D—C12A—H12E	109.5
C10—C9—H9B	108.4	C11A—C12A—H12F	109.5
P1—C9—H9B	108.4	H12D—C12A—H12F	109.5
H9A—C9—H9B	107.5	H12E—C12A—H12F	109.5
C11—C10—C9	114.7 (10)	C14A—C13A—P2	115.4 (8)
C11—C10—H10A	108.6	C14A—C13A—H13A	108.4
C9—C10—H10A	108.6	P2—C13A—H13A	108.4
C11—C10—H10B	108.6	C14A—C13A—H13B	108.4
C9—C10—H10B	108.6	P2—C13A—H13B	108.4
H10A—C10—H10B	107.6	H13A—C13A—H13B	107.5
C12—C11—C10	116.4 (11)	C15A—C14A—C13A	113.8 (10)
C12—C11—H11A	108.2	C15A—C14A—H14A	108.8
C10—C11—H11A	108.2	C13A—C14A—H14A	108.8
C12—C11—H11B	108.2	C15A—C14A—H14B	108.8
C10—C11—H11B	108.2	C13A—C14A—H14B	108.8
H11A—C11—H11B	107.3	H14A—C14A—H14B	107.7
C11—C12—H12A	109.5	C16A—C15A—C14A	117.5 (11)
C11—C12—H12B	109.5	C16A—C15A—H15C	107.9
H12A—C12—H12B	109.5	C14A—C15A—H15C	107.9
C11—C12—H12C	109.5	C16A—C15A—H15D	107.9
H12A—C12—H12C	109.5	C14A—C15A—H15D	107.9
H12B—C12—H12C	109.5	H15C—C15A—H15D	107.2
C14—C13—P2	116.1 (9)	C15A—C16A—H16D	109.5
C14—C13—H13C	108.3	C15A—C16A—H16E	109.5
P2—C13—H13C	108.3	H16D—C16A—H16E	109.5
C14—C13—H13D	108.3	C15A—C16A—H16F	109.5
P2—C13—H13D	108.3	H16D—C16A—H16F	109.5
H13C—C13—H13D	107.4	H16E—C16A—H16F	109.5
C13—C14—C15	114.9 (11)	C22A—C21A—P3	118.8 (10)
C13—C14—H14C	108.5	C22A—C21A—H21C	107.6
C15—C14—H14C	108.5	P3—C21A—H21C	107.6
C13—C14—H14D	108.5	C22A—C21A—H21D	107.6
C15—C14—H14D	108.5	P3—C21A—H21D	107.6
H14C—C14—H14D	107.5	H21C—C21A—H21D	107.0
C16—C15—C14	112.9 (12)	C21A—C22A—C23A	110.9 (11)
C16—C15—H15A	109.0	C21A—C22A—H22C	109.5
C14—C15—H15A	109.0	C23A—C22A—H22C	109.5
C16—C15—H15B	109.0	C21A—C22A—H22D	109.5
C14—C15—H15B	109.0	C23A—C22A—H22D	109.5
H15A—C15—H15B	107.8	H22C—C22A—H22D	108.0
C15—C16—H16A	109.5	C24A—C23A—C22A	112.3 (12)
C15—C16—H16B	109.5	C24A—C23A—H23C	109.2
H16A—C16—H16B	109.5	C22A—C23A—H23C	109.2
C15—C16—H16C	109.5	C24A—C23A—H23D	109.2
H16A—C16—H16C	109.5	C22A—C23A—H23D	109.2
H16B—C16—H16C	109.5	H23C—C23A—H23D	107.9
C18—C17—P2	115.5 (8)	C23A—C24A—H24D	109.5
C18—C17—H17A	108.4	C23A—C24A—H24E	109.5
P2—C17—H17A	108.4	H24D—C24A—H24E	109.5
C18—C17—H17B	108.4	C23A—C24A—H24F	109.5
P2—C17—H17B	108.4	H24D—C24A—H24F	109.5
H17A—C17—H17B	107.5	H24E—C24A—H24F	109.5

O4—Tc1—O1—Th1	25.6 (11)	C9A—P1A—O5A—Th1	−66.5 (14)
O2—Tc1—O1—Th1	−95.7 (10)	C5A—P1A—O5A—Th1	175.2 (12)
O3—Tc1—O1—Th1	145.4 (9)	C1A—P1A—O5A—Th1	55.7 (14)
O13—Th1—O1—Tc1	−51.8 (9)	O13—Th1—O5A—P1A	42.7 (15)
O9—Th1—O1—Tc1	179.9 (10)	O9—Th1—O5A—P1A	162.1 (13)
O5A—Th1—O1—Tc1	161.8 (7)	O5—Th1—O5A—P1A	−68.4 (14)
O5—Th1—O1—Tc1	38.9 (9)	O10—Th1—O5A—P1A	−9.7 (13)
O10—Th1—O1—Tc1	−6.2 (12)	O6—Th1—O5A—P1A	−122.9 (14)
O6—Th1—O1—Tc1	108.4 (10)	O1—Th1—O5A—P1A	179.3 (10)
O1A—Th1—O1—Tc1	−113.4 (9)	O1A—Th1—O5A—P1A	86.3 (13)
C9—P1—O5—Th1	−156.5 (12)	O5—P1—C1—C2	−59.2 (10)
C5—P1—O5—Th1	−34.7 (15)	C9—P1—C1—C2	180.0 (9)
C1—P1—O5—Th1	86.0 (14)	C5—P1—C1—C2	62.1 (10)
O13—Th1—O5—P1	170.1 (14)	P1—C1—C2—C3	169.5 (8)
O9—Th1—O5—P1	49.9 (15)	C1—C2—C3—C4	66.0 (15)
O5A—Th1—O5—P1	−55.5 (15)	O5—P1—C5—C6	176.3 (8)
O10—Th1—O5—P1	−113.8 (14)	C9—P1—C5—C6	−60.5 (10)
O6—Th1—O5—P1	−0.9 (13)	C1—P1—C5—C6	55.5 (10)
O1—Th1—O5—P1	98.4 (14)	P1—C5—C6—C7	179.9 (8)
O1A—Th1—O5—P1	−169.0 (11)	C5—C6—C7—C8	179.5 (11)
O8A—Tc2—O6—Th1	−45.1 (9)	O5—P1—C9—C10	−48.2 (10)
O8—Tc2—O6—Th1	−164.5 (7)	C5—P1—C9—C10	−170.7 (8)
O7—Tc2—O6—Th1	75.2 (9)	C1—P1—C9—C10	71.3 (9)
O13—Th1—O6—Tc2	−173.4 (7)	P1—C9—C10—C11	−176.9 (8)
O9—Th1—O6—Tc2	68.2 (8)	C9—C10—C11—C12	65.8 (15)
O5A—Th1—O6—Tc2	−19.9 (8)	O9—P2—C13—C14	89.3 (11)
O5—Th1—O6—Tc2	−151.6 (9)	C13A—P2—C13—C14	−33.1 (12)
O10—Th1—O6—Tc2	−85.3 (8)	C17—P2—C13—C14	−151.3 (10)
O1—Th1—O6—Tc2	137.4 (8)	P2—C13—C14—C15	178.3 (9)
O1A—Th1—O6—Tc2	20.9 (10)	C13—C14—C15—C16	−177.3 (12)
C13A—P2—O9—Th1	−69.1 (13)	O9—P2—C17—C18	−178.8 (8)
C17—P2—O9—Th1	54.7 (13)	C13A—P2—C17—C18	−53.6 (10)
C13—P2—O9—Th1	171.2 (11)	C13—P2—C17—C18	63.1 (10)
O13—Th1—O9—P2	−63.6 (12)	P2—C17—C18—C19	−174.7 (11)
O5A—Th1—O9—P2	164.4 (12)	C17—C18—C19—C20	177.7 (14)
O5—Th1—O9—P2	41.9 (13)	O13—P3—C21—C22	179.1 (9)
O10—Th1—O9—P2	−177.0 (10)	C25—P3—C21—C22	55.0 (11)
O6—Th1—O9—P2	91.9 (12)	C21A—P3—C21—C22	−62.8 (10)
O1—Th1—O9—P2	−7.4 (12)	P3—C21—C22—C23	176.1 (9)
O1A—Th1—O9—P2	−121.2 (12)	C21—C22—C23—C24	−178.7 (11)
O11A—Tc3—O10—Th1	−96.0 (15)	O13—P3—C25—C26	−57.8 (18)
O12—Tc3—O10—Th1	145.2 (15)	C21—P3—C25—C26	65.8 (17)
O11—Tc3—O10—Th1	25.5 (17)	C21A—P3—C25—C26	−173.6 (16)
O13—Th1—O10—Tc3	39.2 (15)	P3—C25—C26—C27	161.3 (13)
O9—Th1—O10—Tc3	161.3 (11)	C25—C26—C27—C28	72 (2)
O5A—Th1—O10—Tc3	−179.4 (16)	O5A—P1A—C1A—C2A	−173.1 (7)
O5—Th1—O10—Tc3	−50.1 (15)	C9A—P1A—C1A—C2A	−50.9 (9)
O6—Th1—O10—Tc3	−114.9 (15)	C5A—P1A—C1A—C2A	65.4 (9)
O1—Th1—O10—Tc3	−5.1 (18)	P1A—C1A—C2A—C3A	−173.0 (8)
O1A—Th1—O10—Tc3	108.4 (16)	C1A—C2A—C3A—C4A	175.3 (10)
C25—P3—O13—Th1	112 (2)	O5A—P1A—C5A—C6A	57.0 (10)
C21—P3—O13—Th1	−12 (2)	C9A—P1A—C5A—C6A	−63.7 (9)
C21A—P3—O13—Th1	−133 (2)	C1A—P1A—C5A—C6A	177.4 (8)
O9—Th1—O13—P3	−87 (2)	P1A—C5A—C6A—C7A	175.5 (8)
O5A—Th1—O13—P3	18 (2)	C5A—C6A—C7A—C8A	−68.7 (14)
O5—Th1—O13—P3	143 (2)	O5A—P1A—C9A—C10A	63.5 (9)
O10—Th1—O13—P3	69 (2)	C5A—P1A—C9A—C10A	−175.3 (8)
O6—Th1—O13—P3	164.1 (18)	C1A—P1A—C9A—C10A	−58.1 (9)
O1—Th1—O13—P3	−143 (2)	P1A—C9A—C10A—C11A	−175.1 (8)
O1A—Th1—O13—P3	−27 (2)	C9A—C10A—C11A—C12A	−63.3 (13)
O3A—Tc1A—O1A—Th1	59.4 (10)	O9—P2—C13A—C14A	62.3 (10)
O4A—Tc1A—O1A—Th1	179.6 (9)	C17—P2—C13A—C14A	−62.0 (10)
O2A—Tc1A—O1A—Th1	−60.8 (10)	C13—P2—C13A—C14A	−177.5 (9)
O13—Th1—O1A—Tc1A	−133.0 (10)	P2—C13A—C14A—C15A	−173.1 (9)
O9—Th1—O1A—Tc1A	−6.4 (9)	C13A—C14A—C15A—C16A	−61.7 (16)
O5A—Th1—O1A—Tc1A	81.0 (9)	O13—P3—C21A—C22A	−159.2 (11)
O5—Th1—O1A—Tc1A	−155.3 (7)	C25—P3—C21A—C22A	−40.5 (14)
O10—Th1—O1A—Tc1A	152.8 (9)	C21—P3—C21A—C22A	80.6 (12)
O6—Th1—O1A—Tc1A	40.6 (11)	P3—C21A—C22A—C23A	169.6 (10)
O1—Th1—O1A—Tc1A	−70.7 (10)	C21A—C22A—C23A—C24A	177.2 (13)

(IIIat100) top

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	D_x = 1.691 Mg m⁻³
M_r = 1753.26	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbc2₁	Cell parameters from 5577 reflections
a = 21.386 (4) Å	θ = 2.3–26.4°
b = 21.732 (4) Å	µ = 3.09 mm⁻¹
c = 14.820 (2) Å	T = 100 K
V = 6888 (2) Å³	Block, colourless
Z = 4	0.10 × 0.10 × 0.10 mm
F(000) = 3512

Data collection top

CCD area detector diffractometer	13901 independent reflections
Radiation source: fine-focus sealed tube	12000 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.073
phi and ω scans	θ_max = 26.6°, θ_min = 1.3°
Absorption correction: multi-scan SADABS	h = −25→26
T_min = 0.748, T_max = 0.748	k = −25→27
35481 measured reflections	l = −18→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycle	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.062	H-atom parameters constrained
wR(F²) = 0.161	w = 1/[σ²(F_o²) + (0.0606P)² + 22.3563P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.003
13901 reflections	Δρ_max = 4.83 e Å⁻³
707 parameters	Δρ_min = −3.50 e Å⁻³
19 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.020 (8)

Crystal data top

C₄₈H₁₀₈O₂₀P₄Tc₄Th	V = 6888 (2) Å³
M_r = 1753.26	Z = 4
Orthorhombic, Pbc2₁	Mo Kα radiation
a = 21.386 (4) Å	µ = 3.09 mm⁻¹
b = 21.732 (4) Å	T = 100 K
c = 14.820 (2) Å	0.10 × 0.10 × 0.10 mm

Data collection top

CCD area detector diffractometer	13901 independent reflections
Absorption correction: multi-scan SADABS	12000 reflections with I > 2σ(I)
T_min = 0.748, T_max = 0.748	R_int = 0.073
35481 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.062	H-atom parameters constrained
wR(F²) = 0.161	w = 1/[σ²(F_o²) + (0.0606P)² + 22.3563P] where P = (F_o² + 2F_c²)/3
S = 1.09	Δρ_max = 4.83 e Å⁻³
13901 reflections	Δρ_min = −3.50 e Å⁻³
707 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
19 restraints	Absolute structure parameter: 0.020 (8)

Special details top

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

	x	y	z	U_iso*/U_eq
Th1	0.251703 (17)	0.005694 (17)	0.15904 (5)	0.01577 (10)
Tc1	0.39783 (5)	−0.00505 (5)	−0.01416 (8)	0.0230 (2)
Tc2	0.26247 (5)	0.16646 (5)	0.29380 (7)	0.0211 (2)
Tc3	0.25072 (5)	−0.13665 (5)	0.34308 (8)	0.0250 (2)
Tc1A	0.09095 (5)	−0.01162 (5)	0.01687 (7)	0.0216 (2)
P1	0.41131 (16)	0.00325 (15)	0.2737 (2)	0.0235 (7)
P2	0.22621 (16)	0.13474 (15)	−0.0084 (2)	0.0214 (7)
P3	0.25976 (18)	−0.15147 (18)	0.0481 (3)	0.0320 (8)
P1A	0.11870 (15)	0.03809 (15)	0.32417 (19)	0.0210 (6)
O1	0.3276 (4)	0.0199 (4)	0.0356 (6)	0.034 (2)
O2	0.4587 (5)	0.0372 (5)	0.0241 (8)	0.044 (3)
O3	0.3918 (6)	0.0062 (5)	−0.1276 (7)	0.045 (3)
O4	0.4109 (5)	−0.0800 (5)	0.0070 (7)	0.043 (3)
O5	0.3525 (4)	−0.0111 (4)	0.2213 (6)	0.030 (2)
O6	0.2846 (4)	0.1000 (4)	0.2354 (5)	0.028 (2)
O7	0.2384 (5)	0.1484 (5)	0.4015 (6)	0.044 (3)
O8	0.3257 (5)	0.2140 (5)	0.2986 (7)	0.040 (2)
O9	0.2201 (4)	0.0879 (4)	0.0669 (6)	0.0256 (19)
O10	0.2385 (4)	−0.0692 (5)	0.2800 (6)	0.035 (2)
O11	0.3264 (5)	−0.1593 (5)	0.3342 (7)	0.043 (3)
O12	0.2350 (5)	−0.1214 (5)	0.4537 (6)	0.040 (2)
O13	0.2694 (5)	−0.0894 (4)	0.0899 (7)	0.037 (2)
O1A	0.1545 (4)	−0.0283 (4)	0.0872 (6)	0.029 (2)
O2A	0.0465 (5)	0.0448 (5)	0.0645 (6)	0.039 (2)
O3A	0.1161 (5)	0.0113 (5)	−0.0854 (7)	0.042 (3)
O4A	0.0479 (5)	−0.0753 (5)	0.0052 (6)	0.047 (3)
O5A	0.1689 (4)	0.0404 (4)	0.2521 (5)	0.0242 (19)
O8A	0.2039 (5)	0.2017 (5)	0.2393 (6)	0.039 (2)
O11A	0.2029 (5)	−0.1923 (5)	0.3072 (7)	0.046 (3)
C1	0.3992 (6)	−0.0099 (6)	0.3907 (9)	0.030 (3)
H1A	0.3894	−0.0541	0.3997	0.036*
H1B	0.4387	−0.0012	0.4231	0.036*
C2	0.3467 (6)	0.0286 (7)	0.4337 (9)	0.030 (3)
H2A	0.3602	0.0721	0.4372	0.036*
H2B	0.3091	0.0266	0.3949	0.036*
C3	0.3300 (7)	0.0056 (7)	0.5285 (11)	0.040 (3)
H3A	0.3198	−0.0388	0.5257	0.047*
H3B	0.2924	0.0277	0.5502	0.047*
C4	0.3837 (8)	0.0156 (9)	0.5960 (10)	0.053 (5)
H4A	0.4219	−0.0035	0.5726	0.080*
H4B	0.3727	−0.0033	0.6540	0.080*
H4C	0.3906	0.0598	0.6045	0.080*
C5	0.4339 (6)	0.0822 (6)	0.2561 (8)	0.026 (3)
H5A	0.4424	0.0880	0.1910	0.031*
H5B	0.3978	0.1087	0.2718	0.031*
C6	0.4912 (6)	0.1055 (6)	0.3091 (9)	0.032 (3)
H6A	0.4840	0.0999	0.3745	0.039*
H6B	0.5285	0.0811	0.2920	0.039*
C7	0.5033 (6)	0.1729 (6)	0.2897 (10)	0.028 (3)
H7A	0.5103	0.1787	0.2242	0.034*
H7B	0.4662	0.1975	0.3072	0.034*
C8	0.5595 (7)	0.1952 (7)	0.3410 (10)	0.043 (4)
H8A	0.5498	0.1963	0.4056	0.064*
H8B	0.5707	0.2366	0.3203	0.064*
H8C	0.5946	0.1672	0.3304	0.064*
C9	0.4752 (6)	−0.0467 (6)	0.2392 (8)	0.028 (3)
H9A	0.4899	−0.0337	0.1787	0.033*
H9B	0.5104	−0.0414	0.2819	0.033*
C10	0.4578 (7)	−0.1139 (7)	0.2356 (9)	0.037 (3)
H10A	0.4413	−0.1266	0.2952	0.045*
H10B	0.4241	−0.1197	0.1906	0.045*
C11	0.5118 (7)	−0.1544 (7)	0.2114 (9)	0.037 (3)
H11A	0.4960	−0.1966	0.2014	0.044*
H11B	0.5296	−0.1398	0.1536	0.044*
C12	0.5625 (7)	−0.1569 (8)	0.2792 (12)	0.052 (4)
H12A	0.5447	−0.1521	0.3397	0.078*
H12B	0.5924	−0.1236	0.2677	0.078*
H12C	0.5840	−0.1966	0.2750	0.078*
C13	0.1512 (6)	0.1737 (6)	−0.0263 (9)	0.026 (3)
H13C	0.1482	0.1858	−0.0905	0.032*
H13D	0.1171	0.1441	−0.0140	0.032*
C14	0.1410 (6)	0.2301 (6)	0.0313 (8)	0.032 (3)
H14C	0.1742	0.2604	0.0174	0.039*
H14D	0.1455	0.2184	0.0955	0.039*
C15	0.0775 (6)	0.2611 (7)	0.0186 (10)	0.032 (3)
H15A	0.0718	0.2707	−0.0462	0.038*
H15B	0.0443	0.2318	0.0362	0.038*
C16	0.0697 (7)	0.3178 (7)	0.0707 (10)	0.043 (4)
H16A	0.0735	0.3086	0.1352	0.065*
H16B	0.0283	0.3353	0.0585	0.065*
H16C	0.1020	0.3475	0.0532	0.065*
C17	0.2451 (6)	0.0987 (7)	−0.1130 (9)	0.028 (3)
H17A	0.2840	0.0747	−0.1049	0.034*
H17B	0.2113	0.0692	−0.1282	0.034*
C18	0.2541 (6)	0.1431 (7)	−0.1943 (9)	0.031 (3)
H18A	0.2168	0.1698	−0.1999	0.038*
H18B	0.2906	0.1699	−0.1827	0.038*
C19	0.2639 (9)	0.1093 (8)	−0.2814 (10)	0.046 (4)
H19A	0.2278	0.0820	−0.2931	0.055*
H19B	0.3019	0.0834	−0.2769	0.055*
C20	0.2712 (12)	0.1550 (8)	−0.3599 (9)	0.065 (6)
H20A	0.2359	0.1837	−0.3599	0.098*
H20B	0.2721	0.1324	−0.4171	0.098*
H20C	0.3104	0.1779	−0.3527	0.098*
C21	0.1832 (6)	−0.1817 (6)	0.0758 (8)	0.027 (3)
H21A	0.1799	−0.1838	0.1424	0.033*
H21B	0.1515	−0.1518	0.0547	0.033*
C22	0.1663 (6)	−0.2438 (7)	0.0386 (9)	0.035 (3)
H22A	0.1991	−0.2739	0.0553	0.042*
H22B	0.1647	−0.2415	−0.0281	0.042*
C23	0.1039 (6)	−0.2659 (6)	0.0738 (10)	0.037 (4)
H23A	0.0709	−0.2364	0.0558	0.045*
H23B	0.1052	−0.2672	0.1405	0.045*
C24	0.0876 (7)	−0.3295 (6)	0.0377 (12)	0.042 (4)
H24A	0.1041	−0.3339	−0.0237	0.064*
H24B	0.0421	−0.3345	0.0369	0.064*
H24C	0.1063	−0.3609	0.0767	0.064*
C25	0.2692 (9)	−0.1474 (7)	−0.0721 (9)	0.042 (4)
H25A	0.3130	−0.1361	−0.0859	0.050*
H25B	0.2613	−0.1886	−0.0982	0.050*
C26	0.2280 (13)	−0.1035 (14)	−0.1149 (14)	0.106 (11)
H26A	0.2265	−0.0653	−0.0787	0.127*
H26B	0.1851	−0.1207	−0.1177	0.127*
C27	0.2519 (7)	−0.0880 (9)	−0.2152 (16)	0.062 (6)
H27A	0.2298	−0.0511	−0.2379	0.074*
H27B	0.2972	−0.0785	−0.2134	0.074*
C28	0.2410 (11)	−0.1399 (11)	−0.2776 (14)	0.079 (8)
H28A	0.2742	−0.1705	−0.2701	0.118*
H28B	0.2411	−0.1247	−0.3399	0.118*
H28C	0.2004	−0.1587	−0.2641	0.118*
C1A	0.1525 (6)	0.0194 (6)	0.4307 (8)	0.021 (2)
H1C	0.1794	−0.0172	0.4225	0.025*
H1D	0.1799	0.0539	0.4490	0.025*
C2A	0.1073 (6)	0.0062 (5)	0.5088 (8)	0.023 (3)
H2C	0.0832	−0.0316	0.4953	0.028*
H2D	0.0774	0.0407	0.5146	0.028*
C3A	0.1424 (8)	−0.0022 (7)	0.5984 (9)	0.040 (4)
H3C	0.1700	0.0337	0.6088	0.048*
H3D	0.1691	−0.0393	0.5948	0.048*
C4A	0.0968 (7)	−0.0088 (8)	0.6786 (9)	0.044 (4)
H4D	0.0643	0.0229	0.6744	0.066*
H4E	0.1198	−0.0039	0.7353	0.066*
H4F	0.0773	−0.0496	0.6769	0.066*
C5A	0.0802 (6)	0.1106 (5)	0.3369 (8)	0.025 (3)
H5C	0.0464	0.1062	0.3821	0.029*
H5D	0.1106	0.1410	0.3607	0.029*
C6A	0.0515 (5)	0.1362 (6)	0.2474 (8)	0.023 (3)
H6C	0.0855	0.1445	0.2037	0.028*
H6D	0.0235	0.1049	0.2207	0.028*
C7A	0.0145 (7)	0.1957 (7)	0.2645 (8)	0.035 (3)
H7C	0.0425	0.2254	0.2950	0.042*
H7D	0.0029	0.2135	0.2054	0.042*
C8A	−0.0441 (8)	0.1891 (7)	0.3204 (11)	0.049 (4)
H8D	−0.0723	0.2236	0.3077	0.074*
H8E	−0.0331	0.1890	0.3846	0.074*
H8F	−0.0650	0.1503	0.3051	0.074*
C9A	0.0593 (6)	−0.0164 (5)	0.2960 (8)	0.024 (2)
H9C	0.0261	−0.0142	0.3425	0.029*
H9D	0.0403	−0.0040	0.2378	0.029*
C10A	0.0808 (6)	−0.0833 (5)	0.2881 (8)	0.024 (2)
H10C	0.1164	−0.0852	0.2455	0.029*
H10D	0.0960	−0.0972	0.3477	0.029*
C11A	0.0305 (7)	−0.1271 (6)	0.2561 (9)	0.032 (3)
H11C	0.0491	−0.1686	0.2495	0.038*
H11D	0.0162	−0.1138	0.1956	0.038*
C12A	−0.0261 (7)	−0.1319 (6)	0.3178 (8)	0.035 (3)
H12D	−0.0123	−0.1413	0.3793	0.052*
H12E	−0.0537	−0.1647	0.2962	0.052*
H12F	−0.0488	−0.0927	0.3176	0.052*
C13A	0.2839 (5)	0.1925 (6)	0.0183 (8)	0.023 (3)
H13A	0.2832	0.2244	−0.0294	0.027*
H13B	0.2721	0.2125	0.0758	0.027*
C14A	0.3512 (6)	0.1674 (6)	0.0269 (10)	0.033 (3)
H14A	0.3514	0.1323	0.0695	0.039*
H14B	0.3653	0.1520	−0.0326	0.039*
C15A	0.3973 (7)	0.2166 (6)	0.0604 (9)	0.033 (3)
H15C	0.3833	0.2308	0.1205	0.040*
H15D	0.4387	0.1969	0.0684	0.040*
C16A	0.4053 (8)	0.2720 (8)	0.0007 (7)	0.042 (4)
H16D	0.4199	0.2588	−0.0590	0.062*
H16E	0.4362	0.2999	0.0275	0.062*
H16F	0.3652	0.2933	−0.0054	0.062*
C21A	0.3222 (7)	−0.2015 (7)	0.0938 (10)	0.036 (3)
H21C	0.3601	−0.1759	0.1017	0.043*
H21D	0.3091	−0.2151	0.1547	0.043*
C22A	0.3407 (7)	−0.2573 (7)	0.0421 (9)	0.040 (3)
H22C	0.3487	−0.2458	−0.0215	0.047*
H22D	0.3058	−0.2873	0.0428	0.047*
C23A	0.3989 (7)	−0.2873 (8)	0.0813 (9)	0.046 (4)
H23C	0.4339	−0.2576	0.0786	0.055*
H23D	0.3912	−0.2972	0.1455	0.055*
C24A	0.4173 (8)	−0.3445 (8)	0.0332 (11)	0.050 (4)
H24D	0.3833	−0.3745	0.0370	0.075*
H24E	0.4550	−0.3616	0.0612	0.075*
H24F	0.4258	−0.3349	−0.0303	0.075*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.0138 (2)	0.0226 (2)	0.01092 (16)	0.00007 (15)	−0.00024 (15)	0.0007 (2)
Tc1	0.0198 (5)	0.0303 (6)	0.0187 (5)	0.0026 (4)	0.0049 (4)	0.0007 (4)
Tc2	0.0237 (5)	0.0252 (5)	0.0144 (4)	0.0005 (4)	−0.0011 (4)	−0.0024 (4)
Tc3	0.0240 (6)	0.0325 (6)	0.0185 (5)	0.0033 (4)	0.0017 (4)	0.0096 (5)
Tc1A	0.0171 (5)	0.0322 (6)	0.0155 (4)	0.0000 (4)	−0.0025 (4)	−0.0027 (5)
P1	0.0228 (18)	0.0281 (18)	0.0197 (16)	−0.0014 (13)	−0.0038 (13)	0.0017 (12)
P2	0.0288 (18)	0.0233 (17)	0.0123 (14)	0.0012 (13)	0.0005 (12)	−0.0006 (11)
P3	0.034 (2)	0.0272 (19)	0.034 (2)	−0.0060 (15)	0.0092 (15)	−0.0078 (15)
P1A	0.0190 (16)	0.0308 (17)	0.0133 (13)	−0.0002 (12)	0.0026 (11)	−0.0024 (12)
O1	0.032 (5)	0.039 (5)	0.030 (5)	0.004 (4)	0.011 (4)	0.006 (4)
O2	0.035 (6)	0.046 (6)	0.052 (6)	−0.013 (5)	0.000 (5)	−0.002 (6)
O3	0.053 (7)	0.060 (7)	0.022 (5)	0.001 (5)	0.007 (5)	0.006 (4)
O4	0.040 (6)	0.049 (7)	0.041 (7)	0.013 (5)	0.013 (5)	−0.005 (4)
O5	0.024 (5)	0.031 (5)	0.034 (5)	0.002 (4)	−0.013 (4)	−0.006 (4)
O6	0.026 (5)	0.042 (6)	0.016 (4)	0.003 (4)	0.005 (4)	−0.003 (4)
O7	0.066 (7)	0.059 (7)	0.006 (4)	−0.010 (5)	0.008 (4)	0.001 (4)
O8	0.049 (6)	0.049 (6)	0.022 (4)	−0.003 (5)	0.007 (5)	−0.005 (5)
O9	0.026 (5)	0.034 (5)	0.017 (4)	−0.003 (4)	0.004 (4)	−0.002 (4)
O10	0.029 (5)	0.053 (6)	0.023 (5)	0.011 (4)	0.004 (4)	0.014 (4)
O11	0.035 (6)	0.062 (7)	0.033 (5)	0.021 (5)	0.003 (4)	0.010 (5)
O12	0.055 (6)	0.047 (6)	0.018 (5)	0.005 (5)	0.005 (4)	0.012 (4)
O13	0.027 (5)	0.032 (6)	0.052 (7)	0.003 (4)	0.002 (5)	−0.008 (5)
O1A	0.027 (5)	0.038 (5)	0.023 (4)	0.000 (4)	−0.009 (4)	−0.004 (4)
O2A	0.034 (6)	0.057 (7)	0.026 (5)	0.015 (5)	0.003 (4)	−0.015 (5)
O3A	0.036 (6)	0.055 (7)	0.036 (6)	0.002 (5)	−0.001 (5)	0.019 (5)
O4A	0.055 (7)	0.050 (7)	0.036 (6)	−0.005 (5)	−0.020 (5)	−0.002 (5)
O5A	0.024 (5)	0.033 (5)	0.015 (4)	0.001 (4)	0.010 (3)	−0.005 (4)
O8A	0.046 (6)	0.046 (6)	0.024 (5)	0.002 (5)	0.003 (4)	−0.006 (4)
O11A	0.072 (8)	0.046 (6)	0.021 (5)	0.000 (5)	−0.005 (5)	−0.004 (4)
C1	0.016 (7)	0.041 (8)	0.033 (8)	0.000 (5)	−0.002 (5)	−0.004 (6)
C2	0.016 (7)	0.046 (9)	0.028 (7)	0.002 (6)	−0.008 (5)	0.003 (6)
C3	0.039 (9)	0.047 (9)	0.033 (8)	0.001 (6)	−0.002 (7)	−0.009 (7)
C4	0.051 (11)	0.089 (13)	0.020 (7)	0.013 (10)	−0.009 (7)	−0.015 (8)
C5	0.023 (7)	0.037 (8)	0.019 (6)	−0.002 (5)	−0.003 (5)	0.003 (5)
C6	0.035 (8)	0.037 (8)	0.024 (6)	0.002 (6)	−0.006 (5)	0.011 (6)
C7	0.021 (6)	0.034 (7)	0.029 (6)	−0.006 (5)	−0.007 (6)	−0.004 (6)
C8	0.051 (10)	0.047 (9)	0.030 (7)	−0.023 (7)	−0.005 (7)	0.016 (7)
C9	0.020 (7)	0.044 (8)	0.020 (6)	0.011 (5)	0.003 (5)	0.001 (5)
C10	0.041 (9)	0.050 (9)	0.021 (6)	−0.008 (7)	−0.007 (6)	0.002 (6)
C11	0.053 (10)	0.029 (8)	0.029 (7)	−0.004 (7)	0.004 (6)	−0.005 (6)
C12	0.038 (9)	0.058 (11)	0.060 (11)	0.018 (8)	−0.007 (8)	−0.001 (9)
C13	0.027 (7)	0.025 (7)	0.028 (6)	0.010 (5)	−0.001 (5)	0.004 (5)
C14	0.032 (8)	0.049 (9)	0.015 (6)	0.009 (6)	0.004 (5)	−0.002 (6)
C15	0.019 (7)	0.049 (9)	0.029 (6)	0.001 (6)	0.005 (5)	0.010 (7)
C16	0.048 (10)	0.043 (9)	0.039 (8)	0.007 (7)	0.004 (7)	0.011 (7)
C17	0.031 (8)	0.036 (8)	0.018 (6)	−0.002 (5)	−0.005 (5)	0.000 (6)
C18	0.039 (9)	0.041 (8)	0.015 (5)	0.007 (5)	0.008 (5)	0.000 (5)
C19	0.087 (12)	0.033 (8)	0.019 (6)	−0.002 (8)	−0.003 (7)	0.002 (5)
C20	0.140 (17)	0.047 (9)	0.008 (7)	−0.011 (11)	0.004 (8)	−0.001 (6)
C21	0.023 (7)	0.041 (8)	0.018 (6)	0.003 (6)	0.007 (5)	0.003 (5)
C22	0.025 (7)	0.048 (9)	0.032 (7)	−0.002 (6)	0.012 (6)	−0.002 (6)
C23	0.019 (7)	0.038 (8)	0.055 (9)	−0.008 (6)	0.006 (6)	−0.014 (7)
C24	0.037 (9)	0.025 (8)	0.065 (11)	0.004 (6)	0.008 (8)	−0.009 (7)
C25	0.071 (11)	0.042 (9)	0.012 (6)	−0.013 (8)	0.005 (7)	0.002 (6)
C26	0.116 (18)	0.15 (3)	0.048 (12)	0.079 (19)	−0.039 (13)	−0.057 (15)
C27	0.059 (14)	0.051 (11)	0.076 (15)	0.003 (8)	−0.029 (11)	0.001 (10)
C28	0.11 (2)	0.082 (16)	0.044 (11)	0.008 (13)	−0.050 (12)	0.001 (11)
C1A	0.019 (7)	0.021 (6)	0.023 (6)	−0.002 (5)	0.002 (5)	−0.001 (5)
C2A	0.027 (7)	0.021 (7)	0.023 (7)	−0.001 (5)	−0.001 (5)	−0.001 (4)
C3A	0.045 (10)	0.058 (10)	0.016 (6)	−0.007 (7)	−0.008 (6)	0.000 (6)
C4A	0.032 (8)	0.082 (12)	0.017 (7)	−0.002 (8)	−0.008 (6)	0.004 (6)
C5A	0.022 (7)	0.029 (7)	0.023 (5)	0.006 (5)	−0.001 (5)	0.005 (5)
C6A	0.014 (6)	0.039 (8)	0.018 (6)	0.004 (5)	0.008 (4)	0.011 (5)
C7A	0.046 (9)	0.040 (8)	0.019 (6)	0.004 (7)	−0.009 (6)	0.004 (5)
C8A	0.051 (10)	0.046 (10)	0.051 (10)	0.023 (8)	0.009 (7)	−0.006 (8)
C9A	0.036 (7)	0.026 (5)	0.011 (5)	0.003 (4)	−0.018 (5)	−0.004 (5)
C10A	0.032 (6)	0.026 (4)	0.013 (5)	0.001 (4)	0.004 (5)	0.002 (4)
C11A	0.037 (8)	0.030 (7)	0.028 (6)	−0.004 (6)	0.008 (6)	−0.007 (6)
C12A	0.038 (8)	0.044 (8)	0.021 (7)	−0.009 (6)	0.004 (5)	0.000 (6)
C13A	0.016 (6)	0.039 (7)	0.013 (5)	−0.010 (5)	−0.006 (5)	0.004 (5)
C14A	0.036 (8)	0.033 (7)	0.030 (7)	0.007 (6)	−0.003 (6)	−0.001 (6)
C15A	0.041 (9)	0.038 (8)	0.021 (6)	−0.010 (6)	−0.010 (6)	−0.006 (5)
C16A	0.061 (11)	0.051 (10)	0.012 (7)	−0.008 (8)	0.005 (6)	0.005 (5)
C21A	0.033 (8)	0.038 (8)	0.037 (7)	0.007 (6)	−0.008 (6)	−0.009 (6)
C22A	0.038 (8)	0.056 (10)	0.025 (7)	0.001 (7)	−0.005 (6)	−0.001 (6)
C23A	0.036 (9)	0.076 (12)	0.025 (7)	0.016 (8)	−0.003 (6)	0.012 (7)
C24A	0.055 (11)	0.063 (11)	0.032 (8)	−0.003 (8)	−0.003 (7)	−0.017 (8)

Geometric parameters (Å, º) top

Th1—O13	2.337 (9)	C18—H18A	0.9900
Th1—O9	2.348 (9)	C18—H18B	0.9900
Th1—O5A	2.368 (8)	C19—C20	1.54 (2)
Th1—O5	2.374 (8)	C19—H19A	0.9900
Th1—O10	2.437 (9)	C19—H19B	0.9900
Th1—O6	2.444 (9)	C20—H20A	0.9800
Th1—O1A	2.449 (9)	C20—H20B	0.9800
Th1—O1	2.465 (9)	C20—H20C	0.9800
Tc1—O4	1.683 (11)	C21—C22	1.502 (19)
Tc1—O2	1.691 (10)	C21—H21A	0.9900
Tc1—O3	1.704 (10)	C21—H21B	0.9900
Tc1—O1	1.759 (9)	C22—C23	1.511 (18)
Tc2—O8A	1.676 (10)	C22—H22A	0.9900
Tc2—O8	1.703 (10)	C22—H22B	0.9900
Tc2—O7	1.723 (10)	C23—C24	1.522 (18)
Tc2—O6	1.750 (9)	C23—H23A	0.9900
Tc3—O11A	1.670 (11)	C23—H23B	0.9900
Tc3—O11	1.697 (10)	C24—H24A	0.9800
Tc3—O12	1.706 (9)	C24—H24B	0.9800
Tc3—O10	1.758 (10)	C24—H24C	0.9800
Tc1A—O4A	1.671 (11)	C25—C26	1.44 (3)
Tc1A—O3A	1.683 (10)	C25—H25A	0.9900
Tc1A—O2A	1.703 (9)	C25—H25B	0.9900
Tc1A—O1A	1.751 (9)	C26—C27	1.61 (3)
P1—O5	1.509 (9)	C26—H26A	0.9900
P1—C1	1.778 (15)	C26—H26B	0.9900
P1—C5	1.803 (13)	C27—C28	1.48 (3)
P1—C9	1.818 (12)	C27—H27A	0.9900
P2—O9	1.516 (9)	C27—H27B	0.9900
P2—C17	1.783 (14)	C28—H28A	0.9800
P2—C13A	1.804 (12)	C28—H28B	0.9800
P2—C13	1.833 (12)	C28—H28C	0.9800
P3—O13	1.499 (10)	C1A—C2A	1.534 (16)
P3—C25	1.795 (14)	C1A—H1C	0.9900
P3—C21	1.811 (13)	C1A—H1D	0.9900
P3—C21A	1.852 (14)	C2A—C3A	1.537 (17)
P1A—O5A	1.515 (8)	C2A—H2C	0.9900
P1A—C9A	1.786 (11)	C2A—H2D	0.9900
P1A—C1A	1.783 (12)	C3A—C4A	1.54 (2)
P1A—C5A	1.789 (12)	C3A—H3C	0.9900
C1—C2	1.538 (18)	C3A—H3D	0.9900
C1—H1A	0.9900	C4A—H4D	0.9800
C1—H1B	0.9900	C4A—H4E	0.9800
C2—C3	1.53 (2)	C4A—H4F	0.9800
C2—H2A	0.9900	C5A—C6A	1.563 (15)
C2—H2B	0.9900	C5A—H5C	0.9900
C3—C4	1.54 (2)	C5A—H5D	0.9900
C3—H3A	0.9900	C6A—C7A	1.536 (18)
C3—H3B	0.9900	C6A—H6C	0.9900
C4—H4A	0.9800	C6A—H6D	0.9900
C4—H4B	0.9800	C7A—C8A	1.51 (2)
C4—H4C	0.9800	C7A—H7C	0.9900
C5—C6	1.541 (17)	C7A—H7D	0.9900
C5—H5A	0.9900	C8A—H8D	0.9800
C5—H5B	0.9900	C8A—H8E	0.9800
C6—C7	1.515 (17)	C8A—H8F	0.9800
C6—H6A	0.9900	C9A—C10A	1.528 (16)
C6—H6B	0.9900	C9A—H9C	0.9900
C7—C8	1.501 (18)	C9A—H9D	0.9900
C7—H7A	0.9900	C10A—C11A	1.513 (17)
C7—H7B	0.9900	C10A—H10C	0.9900
C8—H8A	0.9800	C10A—H10D	0.9900
C8—H8B	0.9800	C11A—C12A	1.520 (18)
C8—H8C	0.9800	C11A—H11C	0.9900
C9—C10	1.51 (2)	C11A—H11D	0.9900
C9—H9A	0.9900	C12A—H12D	0.9800
C9—H9B	0.9900	C12A—H12E	0.9800
C10—C11	1.50 (2)	C12A—H12F	0.9800
C10—H10A	0.9900	C13A—C14A	1.545 (17)
C10—H10B	0.9900	C13A—H13A	0.9900
C11—C12	1.48 (2)	C13A—H13B	0.9900
C11—H11A	0.9900	C14A—C15A	1.536 (18)
C11—H11B	0.9900	C14A—H14A	0.9900
C12—H12A	0.9800	C14A—H14B	0.9900
C12—H12B	0.9800	C15A—C16A	1.505 (18)
C12—H12C	0.9800	C15A—H15C	0.9900
C13—C14	1.509 (17)	C15A—H15D	0.9900
C13—H13C	0.9900	C16A—H16D	0.9800
C13—H13D	0.9900	C16A—H16E	0.9800
C14—C15	1.528 (17)	C16A—H16F	0.9800
C14—H14C	0.9900	C21A—C22A	1.488 (19)
C14—H14D	0.9900	C21A—H21C	0.9900
C15—C16	1.46 (2)	C21A—H21D	0.9900
C15—H15A	0.9900	C22A—C23A	1.520 (19)
C15—H15B	0.9900	C22A—H22C	0.9900
C16—H16A	0.9800	C22A—H22D	0.9900
C16—H16B	0.9800	C23A—C24A	1.49 (2)
C16—H16C	0.9800	C23A—H23C	0.9900
C17—C18	1.556 (18)	C23A—H23D	0.9900
C17—H17A	0.9900	C24A—H24D	0.9800
C17—H17B	0.9900	C24A—H24E	0.9800
C18—C19	1.500 (19)	C24A—H24F	0.9800

O13—Th1—O9	117.7 (4)	C19—C18—C17	112.3 (12)
O13—Th1—O5A	131.1 (3)	C19—C18—H18A	109.1
O9—Th1—O5A	83.2 (3)	C17—C18—H18A	109.1
O13—Th1—O5	83.5 (3)	C19—C18—H18B	109.1
O9—Th1—O5	127.2 (3)	C17—C18—H18B	109.1
O5A—Th1—O5	120.1 (3)	H18A—C18—H18B	107.9
O13—Th1—O10	75.5 (4)	C18—C19—C20	110.4 (13)
O9—Th1—O10	154.5 (3)	C18—C19—H19A	109.6
O5A—Th1—O10	72.4 (3)	C20—C19—H19A	109.6
O5—Th1—O10	73.5 (3)	C18—C19—H19B	109.6
O13—Th1—O6	153.8 (3)	C20—C19—H19B	109.6
O9—Th1—O6	73.4 (3)	H19A—C19—H19B	108.1
O5A—Th1—O6	71.3 (3)	C19—C20—H20A	109.5
O5—Th1—O6	71.7 (3)	C19—C20—H20B	109.5
O10—Th1—O6	104.6 (3)	H20A—C20—H20B	109.5
O13—Th1—O1A	71.4 (3)	C19—C20—H20C	109.5
O9—Th1—O1A	74.5 (3)	H20A—C20—H20C	109.5
O5A—Th1—O1A	73.4 (3)	H20B—C20—H20C	109.5
O5—Th1—O1A	153.3 (3)	C22—C21—P3	117.4 (9)
O10—Th1—O1A	91.1 (3)	C22—C21—H21A	107.9
O6—Th1—O1A	134.3 (3)	P3—C21—H21A	107.9
O13—Th1—O1	71.3 (3)	C22—C21—H21B	107.9
O9—Th1—O1	70.3 (3)	P3—C21—H21B	107.9
O5A—Th1—O1	152.2 (3)	H21A—C21—H21B	107.2
O5—Th1—O1	73.1 (3)	C21—C22—C23	111.8 (11)
O10—Th1—O1	134.9 (3)	C21—C22—H22A	109.3
O6—Th1—O1	92.8 (3)	C23—C22—H22A	109.3
O1A—Th1—O1	105.9 (3)	C21—C22—H22B	109.3
O4—Tc1—O2	109.6 (5)	C23—C22—H22B	109.3
O4—Tc1—O3	109.6 (5)	H22A—C22—H22B	107.9
O2—Tc1—O3	108.2 (6)	C22—C23—C24	111.6 (12)
O4—Tc1—O1	111.2 (5)	C22—C23—H23A	109.3
O2—Tc1—O1	110.5 (5)	C24—C23—H23A	109.3
O3—Tc1—O1	107.7 (5)	C22—C23—H23B	109.3
O8A—Tc2—O8	109.7 (5)	C24—C23—H23B	109.3
O8A—Tc2—O7	109.1 (5)	H23A—C23—H23B	108.0
O8—Tc2—O7	109.6 (5)	C23—C24—H24A	109.5
O8A—Tc2—O6	110.0 (4)	C23—C24—H24B	109.5
O8—Tc2—O6	107.9 (4)	H24A—C24—H24B	109.5
O7—Tc2—O6	110.6 (5)	C23—C24—H24C	109.5
O11A—Tc3—O11	110.4 (5)	H24A—C24—H24C	109.5
O11A—Tc3—O12	109.0 (5)	H24B—C24—H24C	109.5
O11—Tc3—O12	108.6 (5)	C26—C25—P3	113.6 (14)
O11A—Tc3—O10	110.1 (5)	C26—C25—H25A	108.9
O11—Tc3—O10	110.0 (5)	P3—C25—H25A	108.9
O12—Tc3—O10	108.6 (5)	C26—C25—H25B	108.8
O4A—Tc1A—O3A	109.2 (5)	P3—C25—H25B	108.9
O4A—Tc1A—O2A	109.4 (5)	H25A—C25—H25B	107.7
O3A—Tc1A—O2A	109.7 (5)	C25—C26—C27	110.5 (17)
O4A—Tc1A—O1A	108.5 (5)	C25—C26—H26A	109.6
O3A—Tc1A—O1A	110.5 (5)	C27—C26—H26A	109.6
O2A—Tc1A—O1A	109.6 (4)	C25—C26—H26B	109.6
O5—P1—C1	110.3 (6)	C27—C26—H26B	109.6
O5—P1—C5	110.2 (6)	H26A—C26—H26B	108.1
C1—P1—C5	109.5 (6)	C28—C27—C26	111.5 (19)
O5—P1—C9	111.0 (6)	C28—C27—H27A	109.3
C1—P1—C9	106.7 (6)	C26—C27—H27A	109.3
C5—P1—C9	109.0 (6)	C28—C27—H27B	109.3
O9—P2—C17	111.3 (6)	C26—C27—H27B	109.3
O9—P2—C13A	111.4 (5)	H27A—C27—H27B	108.0
C17—P2—C13A	110.0 (6)	C27—C28—H28A	109.5
O9—P2—C13	109.9 (6)	C27—C28—H28B	109.5
C17—P2—C13	106.0 (6)	H28A—C28—H28B	109.5
C13A—P2—C13	108.0 (6)	C27—C28—H28C	109.5
O13—P3—C25	110.5 (7)	H28A—C28—H28C	109.5
O13—P3—C21	111.0 (6)	H28B—C28—H28C	109.5
C25—P3—C21	110.2 (7)	C2A—C1A—P1A	117.1 (9)
O13—P3—C21A	106.1 (6)	C2A—C1A—H1C	108.0
C25—P3—C21A	108.2 (8)	P1A—C1A—H1C	108.0
C21—P3—C21A	110.8 (7)	C2A—C1A—H1D	108.0
O5A—P1A—C9A	111.1 (6)	P1A—C1A—H1D	108.0
O5A—P1A—C1A	110.2 (5)	H1C—C1A—H1D	107.3
C9A—P1A—C1A	110.1 (6)	C1A—C2A—C3A	111.5 (11)
O5A—P1A—C5A	111.8 (5)	C1A—C2A—H2C	109.3
C9A—P1A—C5A	106.4 (6)	C3A—C2A—H2C	109.3
C1A—P1A—C5A	107.1 (6)	C1A—C2A—H2D	109.3
Tc1—O1—Th1	146.6 (5)	C3A—C2A—H2D	109.3
P1—O5—Th1	157.6 (6)	H2C—C2A—H2D	108.0
Tc2—O6—Th1	147.5 (5)	C2A—C3A—C4A	111.6 (12)
P2—O9—Th1	156.1 (5)	C2A—C3A—H3C	109.3
Tc3—O10—Th1	158.6 (5)	C4A—C3A—H3C	109.3
P3—O13—Th1	162.6 (6)	C2A—C3A—H3D	109.3
Tc1A—O1A—Th1	148.8 (5)	C4A—C3A—H3D	109.3
P1A—O5A—Th1	158.5 (5)	H3C—C3A—H3D	108.0
C2—C1—P1	115.0 (10)	C3A—C4A—H4D	109.5
C2—C1—H1A	108.5	C3A—C4A—H4E	109.5
P1—C1—H1A	108.5	H4D—C4A—H4E	109.5
C2—C1—H1B	108.5	C3A—C4A—H4F	109.5
P1—C1—H1B	108.5	H4D—C4A—H4F	109.5
H1A—C1—H1B	107.5	H4E—C4A—H4F	109.5
C3—C2—C1	111.8 (12)	C6A—C5A—P1A	113.8 (9)
C3—C2—H2A	109.2	C6A—C5A—H5C	108.8
C1—C2—H2A	109.2	P1A—C5A—H5C	108.8
C3—C2—H2B	109.2	C6A—C5A—H5D	108.8
C1—C2—H2B	109.2	P1A—C5A—H5D	108.8
H2A—C2—H2B	107.9	H5C—C5A—H5D	107.7
C2—C3—C4	112.1 (13)	C7A—C6A—C5A	111.1 (10)
C2—C3—H3A	109.2	C7A—C6A—H6C	109.4
C4—C3—H3A	109.2	C5A—C6A—H6C	109.4
C2—C3—H3B	109.2	C7A—C6A—H6D	109.4
C4—C3—H3B	109.2	C5A—C6A—H6D	109.4
H3A—C3—H3B	107.9	H6C—C6A—H6D	108.0
C3—C4—H4A	109.5	C8A—C7A—C6A	116.0 (12)
C3—C4—H4B	109.5	C8A—C7A—H7C	108.3
H4A—C4—H4B	109.5	C6A—C7A—H7C	108.3
C3—C4—H4C	109.5	C8A—C7A—H7D	108.3
H4A—C4—H4C	109.5	C6A—C7A—H7D	108.3
H4B—C4—H4C	109.5	H7C—C7A—H7D	107.4
C6—C5—P1	116.9 (9)	C7A—C8A—H8D	109.5
C6—C5—H5A	108.1	C7A—C8A—H8E	109.5
P1—C5—H5A	108.1	H8D—C8A—H8E	109.5
C6—C5—H5B	108.1	C7A—C8A—H8F	109.5
P1—C5—H5B	108.1	H8D—C8A—H8F	109.5
H5A—C5—H5B	107.3	H8E—C8A—H8F	109.5
C7—C6—C5	110.9 (10)	C10A—C9A—P1A	115.8 (8)
C7—C6—H6A	109.5	C10A—C9A—H9C	108.3
C5—C6—H6A	109.5	P1A—C9A—H9C	108.3
C7—C6—H6B	109.5	C10A—C9A—H9D	108.3
C5—C6—H6B	109.5	P1A—C9A—H9D	108.3
H6A—C6—H6B	108.1	H9C—C9A—H9D	107.4
C8—C7—C6	110.6 (11)	C11A—C10A—C9A	114.2 (10)
C8—C7—H7A	109.5	C11A—C10A—H10C	108.7
C6—C7—H7A	109.5	C9A—C10A—H10C	108.7
C8—C7—H7B	109.5	C11A—C10A—H10D	108.7
C6—C7—H7B	109.5	C9A—C10A—H10D	108.7
H7A—C7—H7B	108.1	H10C—C10A—H10D	107.6
C7—C8—H8A	109.5	C10A—C11A—C12A	114.8 (10)
C7—C8—H8B	109.5	C10A—C11A—H11C	108.6
H8A—C8—H8B	109.5	C12A—C11A—H11C	108.6
C7—C8—H8C	109.5	C10A—C11A—H11D	108.6
H8A—C8—H8C	109.5	C12A—C11A—H11D	108.6
H8B—C8—H8C	109.5	H11C—C11A—H11D	107.5
C10—C9—P1	113.7 (10)	C11A—C12A—H12D	109.5
C10—C9—H9A	108.8	C11A—C12A—H12E	109.5
P1—C9—H9A	108.8	H12D—C12A—H12E	109.5
C10—C9—H9B	108.8	C11A—C12A—H12F	109.5
P1—C9—H9B	108.8	H12D—C12A—H12F	109.5
H9A—C9—H9B	107.7	H12E—C12A—H12F	109.5
C11—C10—C9	112.8 (12)	C14A—C13A—P2	114.3 (9)
C11—C10—H10A	109.0	C14A—C13A—H13A	108.7
C9—C10—H10A	109.0	P2—C13A—H13A	108.7
C11—C10—H10B	109.0	C14A—C13A—H13B	108.7
C9—C10—H10B	109.0	P2—C13A—H13B	108.7
H10A—C10—H10B	107.8	H13A—C13A—H13B	107.6
C12—C11—C10	115.2 (12)	C15A—C14A—C13A	112.3 (11)
C12—C11—H11A	108.5	C15A—C14A—H14A	109.1
C10—C11—H11A	108.5	C13A—C14A—H14A	109.1
C12—C11—H11B	108.5	C15A—C14A—H14B	109.1
C10—C11—H11B	108.5	C13A—C14A—H14B	109.1
H11A—C11—H11B	107.5	H14A—C14A—H14B	107.9
C11—C12—H12A	109.5	C16A—C15A—C14A	116.1 (11)
C11—C12—H12B	109.5	C16A—C15A—H15C	108.3
H12A—C12—H12B	109.5	C14A—C15A—H15C	108.3
C11—C12—H12C	109.5	C16A—C15A—H15D	108.3
H12A—C12—H12C	109.5	C14A—C15A—H15D	108.3
H12B—C12—H12C	109.5	H15C—C15A—H15D	107.4
C14—C13—P2	114.9 (9)	C15A—C16A—H16D	109.5
C14—C13—H13C	108.6	C15A—C16A—H16E	109.5
P2—C13—H13C	108.6	H16D—C16A—H16E	109.5
C14—C13—H13D	108.6	C15A—C16A—H16F	109.5
P2—C13—H13D	108.6	H16D—C16A—H16F	109.5
H13C—C13—H13D	107.5	H16E—C16A—H16F	109.5
C13—C14—C15	114.6 (11)	C22A—C21A—P3	118.8 (10)
C13—C14—H14C	108.6	C22A—C21A—H21C	107.6
C15—C14—H14C	108.6	P3—C21A—H21C	107.6
C13—C14—H14D	108.6	C22A—C21A—H21D	107.6
C15—C14—H14D	108.6	P3—C21A—H21D	107.6
H14C—C14—H14D	107.6	H21C—C21A—H21D	107.1
C16—C15—C14	114.0 (12)	C21A—C22A—C23A	111.7 (12)
C16—C15—H15A	108.7	C21A—C22A—H22C	109.3
C14—C15—H15A	108.7	C23A—C22A—H22C	109.3
C16—C15—H15B	108.7	C21A—C22A—H22D	109.3
C14—C15—H15B	108.7	C23A—C22A—H22D	109.3
H15A—C15—H15B	107.6	H22C—C22A—H22D	107.9
C15—C16—H16A	109.5	C24A—C23A—C22A	113.1 (13)
C15—C16—H16B	109.5	C24A—C23A—H23C	109.0
H16A—C16—H16B	109.5	C22A—C23A—H23C	109.0
C15—C16—H16C	109.5	C24A—C23A—H23D	109.0
H16A—C16—H16C	109.5	C22A—C23A—H23D	109.0
H16B—C16—H16C	109.5	H23C—C23A—H23D	107.8
C18—C17—P2	115.4 (10)	C23A—C24A—H24D	109.5
C18—C17—H17A	108.4	C23A—C24A—H24E	109.5
P2—C17—H17A	108.4	H24D—C24A—H24E	109.5
C18—C17—H17B	108.4	C23A—C24A—H24F	109.5
P2—C17—H17B	108.4	H24D—C24A—H24F	109.5
H17A—C17—H17B	107.5	H24E—C24A—H24F	109.5

O4—Tc1—O1—Th1	28.2 (11)	C9A—P1A—O5A—Th1	−63.8 (15)
O2—Tc1—O1—Th1	−93.8 (10)	C1A—P1A—O5A—Th1	58.5 (15)
O3—Tc1—O1—Th1	148.3 (9)	C5A—P1A—O5A—Th1	177.5 (13)
O13—Th1—O1—Tc1	−51.3 (10)	O13—Th1—O5A—P1A	38.2 (16)
O9—Th1—O1—Tc1	178.8 (11)	O9—Th1—O5A—P1A	159.3 (14)
O5A—Th1—O1—Tc1	160.8 (7)	O5—Th1—O5A—P1A	−71.3 (15)
O5—Th1—O1—Tc1	37.5 (9)	O10—Th1—O5A—P1A	−13.1 (14)
O10—Th1—O1—Tc1	−6.5 (13)	O6—Th1—O5A—P1A	−125.9 (15)
O6—Th1—O1—Tc1	107.5 (10)	O1A—Th1—O5A—P1A	83.6 (14)
O1A—Th1—O1—Tc1	−114.7 (10)	O1—Th1—O5A—P1A	176.3 (11)
C1—P1—O5—Th1	82.2 (17)	O5—P1—C1—C2	−59.6 (12)
C5—P1—O5—Th1	−38.8 (17)	C5—P1—C1—C2	61.8 (12)
C9—P1—O5—Th1	−159.7 (14)	C9—P1—C1—C2	179.7 (10)
O13—Th1—O5—P1	174.2 (16)	P1—C1—C2—C3	168.3 (10)
O9—Th1—O5—P1	54.2 (17)	C1—C2—C3—C4	66.7 (17)
O5A—Th1—O5—P1	−51.4 (17)	O5—P1—C5—C6	176.7 (9)
O10—Th1—O5—P1	−109.0 (16)	C1—P1—C5—C6	55.2 (11)
O6—Th1—O5—P1	3.1 (15)	C9—P1—C5—C6	−61.2 (11)
O1A—Th1—O5—P1	−166.1 (12)	P1—C5—C6—C7	−178.3 (9)
O1—Th1—O5—P1	101.9 (16)	C5—C6—C7—C8	−179.6 (11)
O8A—Tc2—O6—Th1	−47.1 (10)	O5—P1—C9—C10	−48.4 (10)
O8—Tc2—O6—Th1	−166.7 (8)	C1—P1—C9—C10	71.8 (10)
O7—Tc2—O6—Th1	73.5 (10)	C5—P1—C9—C10	−170.0 (9)
O13—Th1—O6—Tc2	−170.7 (8)	P1—C9—C10—C11	−177.3 (9)
O9—Th1—O6—Tc2	69.7 (9)	C9—C10—C11—C12	66.5 (16)
O5A—Th1—O6—Tc2	−18.5 (8)	O9—P2—C13—C14	88.3 (10)
O5—Th1—O6—Tc2	−150.6 (9)	C17—P2—C13—C14	−151.3 (10)
O10—Th1—O6—Tc2	−83.8 (9)	C13A—P2—C13—C14	−33.5 (11)
O1A—Th1—O6—Tc2	22.7 (11)	P2—C13—C14—C15	−177.9 (9)
O1—Th1—O6—Tc2	138.2 (9)	C13—C14—C15—C16	−176.5 (12)
C17—P2—O9—Th1	53.2 (15)	O9—P2—C17—C18	−178.5 (8)
C13A—P2—O9—Th1	−70.0 (14)	C13A—P2—C17—C18	−54.5 (11)
C13—P2—O9—Th1	170.3 (12)	C13—P2—C17—C18	62.0 (10)
O13—Th1—O9—P2	−62.3 (14)	P2—C17—C18—C19	−174.7 (11)
O5A—Th1—O9—P2	164.4 (13)	C17—C18—C19—C20	178.8 (15)
O5—Th1—O9—P2	41.5 (14)	O13—P3—C21—C22	179.8 (10)
O10—Th1—O9—P2	−178.7 (10)	C25—P3—C21—C22	57.1 (12)
O6—Th1—O9—P2	92.0 (13)	C21A—P3—C21—C22	−62.5 (12)
O1A—Th1—O9—P2	−121.0 (13)	P3—C21—C22—C23	174.8 (10)
O1—Th1—O9—P2	−7.3 (12)	C21—C22—C23—C24	−178.6 (13)
O11A—Tc3—O10—Th1	−90.1 (16)	O13—P3—C25—C26	−57 (2)
O11—Tc3—O10—Th1	31.8 (17)	C21—P3—C25—C26	66 (2)
O12—Tc3—O10—Th1	150.5 (15)	C21A—P3—C25—C26	−172.7 (18)
O13—Th1—O10—Tc3	33.4 (16)	P3—C25—C26—C27	163.6 (14)
O9—Th1—O10—Tc3	158.3 (12)	C25—C26—C27—C28	73 (2)
O5A—Th1—O10—Tc3	176.0 (17)	O5A—P1A—C1A—C2A	−171.6 (9)
O5—Th1—O10—Tc3	−54.1 (16)	C9A—P1A—C1A—C2A	−48.7 (11)
O6—Th1—O10—Tc3	−119.5 (16)	C5A—P1A—C1A—C2A	66.6 (10)
O1A—Th1—O10—Tc3	103.8 (16)	P1A—C1A—C2A—C3A	−173.8 (10)
O1—Th1—O10—Tc3	−10.2 (19)	C1A—C2A—C3A—C4A	174.1 (12)
C25—P3—O13—Th1	106 (2)	O5A—P1A—C5A—C6A	55.4 (10)
C21—P3—O13—Th1	−17 (3)	C9A—P1A—C5A—C6A	−66.1 (10)
C21A—P3—O13—Th1	−137 (2)	C1A—P1A—C5A—C6A	176.2 (9)
O9—Th1—O13—P3	−82 (2)	P1A—C5A—C6A—C7A	175.2 (9)
O5A—Th1—O13—P3	25 (3)	C5A—C6A—C7A—C8A	−66.7 (15)
O5—Th1—O13—P3	150 (2)	O5A—P1A—C9A—C10A	62.1 (10)
O10—Th1—O13—P3	75 (2)	C1A—P1A—C9A—C10A	−60.2 (10)
O6—Th1—O13—P3	168.8 (19)	C5A—P1A—C9A—C10A	−175.9 (9)
O1A—Th1—O13—P3	−21 (2)	P1A—C9A—C10A—C11A	−174.9 (8)
O1—Th1—O13—P3	−136 (2)	C9A—C10A—C11A—C12A	−61.6 (15)
O4A—Tc1A—O1A—Th1	176.1 (9)	O9—P2—C13A—C14A	64.4 (11)
O3A—Tc1A—O1A—Th1	56.5 (10)	C17—P2—C13A—C14A	−59.6 (11)
O2A—Tc1A—O1A—Th1	−64.5 (10)	C13—P2—C13A—C14A	−174.8 (10)
O13—Th1—O1A—Tc1A	−130.8 (10)	P2—C13A—C14A—C15A	−173.3 (9)
O9—Th1—O1A—Tc1A	−3.7 (9)	C13A—C14A—C15A—C16A	−61.8 (17)
O5A—Th1—O1A—Tc1A	83.7 (10)	O13—P3—C21A—C22A	−157.2 (12)
O5—Th1—O1A—Tc1A	−151.4 (8)	C25—P3—C21A—C22A	−38.6 (14)
O10—Th1—O1A—Tc1A	154.9 (9)	C21—P3—C21A—C22A	82.2 (13)
O6—Th1—O1A—Tc1A	43.0 (11)	P3—C21A—C22A—C23A	171.1 (11)
O1—Th1—O1A—Tc1A	−67.4 (10)	C21A—C22A—C23A—C24A	178.0 (14)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1A···O11	0.99	2.83	3.696 (18)	147
C2—H2B···O5	0.99	2.85	3.265 (16)	106
C2—H2B···O6	0.99	2.90	3.578 (15)	127
C3—H3A···O12	0.99	2.77	3.602 (19)	143
C5—H5A···O2	0.99	2.73	3.614 (17)	149
C5—H5B···O6	0.99	2.49	3.230 (16)	132
C5—H5B···O8	0.99	2.79	3.736 (17)	160
C9—H9A···O2	0.99	2.84	3.689 (17)	144
C10—H10A···O11	0.99	2.62	3.318 (18)	127
C10—H10B···O4	0.99	2.87	3.608 (17)	132
C10—H10B···O5	0.99	2.85	3.179 (18)	100
C13—H13D···O2A	0.99	2.88	3.831 (17)	161
C14—H14D···O8A	0.99	2.50	3.420 (16)	155
C17—H17A···O1	0.99	2.57	3.301 (16)	130
C17—H17A···O3	0.99	2.76	3.732 (18)	166
C17—H17B···O3A	0.99	2.48	3.373 (17)	150
C21—H21A···O11A	0.99	2.50	3.462 (15)	164
C21—H21B···O1A	0.99	2.73	3.396 (16)	125
C21—H21B···O4A	0.99	2.87	3.849 (17)	172
C25—H25A···O4	0.99	2.79	3.56 (2)	136
C26—H26A···O13	0.99	2.71	3.18 (2)	109
C26—H26A···O3A	0.99	2.89	3.49 (2)	119
C27—H27B···O3	0.99	3.02	3.85 (2)	143
C1A—H1C···O10	0.99	2.71	3.477 (15)	135
C1A—H1C···O12	0.99	2.60	3.549 (17)	161
C1A—H1D···O7	0.99	2.51	3.381 (16)	147
C5A—H5D···O7	0.99	2.81	3.612 (17)	139
C5A—H5D···O8A	0.99	2.99	3.606 (16)	121
C6A—H6C···O5A	0.99	2.97	3.262 (14)	98
C6A—H6C···O8A	0.99	2.87	3.557 (16)	127
C6A—H6D···O2A	0.99	2.70	3.363 (16)	124
C9A—H9D···O2A	0.99	2.78	3.690 (15)	153
C10A—H10C···O10	0.99	2.68	3.390 (15)	129
C10A—H10C···O1A	0.99	2.77	3.574 (15)	138
C10A—H10C···O5A	0.99	2.95	3.325 (14)	103
C13A—H13B···O8A	0.99	2.84	3.702 (16)	146
C14A—H14A···O1	0.99	2.55	3.248 (17)	128
C14A—H14A···O6	0.99	2.93	3.705 (17)	136
C14A—H14A···O9	0.99	2.97	3.348 (16)	104
C15A—H15C···O8	0.99	2.93	3.849 (16)	154
C21A—H21C···O4	0.99	2.74	3.496 (19)	134
C21A—H21D···O11	0.99	2.95	3.680 (17)	132
C1—H1B···O2ⁱ	0.99	2.77	3.674 (17)	152
C6—H6B···O3ⁱ	0.99	2.82	3.611 (16)	138
C4—H4A···O2ⁱ	0.98	2.75	3.72 (2)	168
C12—H12B···O3ⁱ	0.98	3.01	3.69 (2)	128
C9—H9B···O3ⁱ	0.99	2.60	3.573 (17)	167
C12—H12C···O8ⁱⁱ	0.98	2.76	3.697 (18)	160
C24A—H24E···O2ⁱⁱ	0.98	2.92	3.70 (2)	137
C20—H20A···O8Aⁱⁱⁱ	0.98	2.97	3.73 (2)	135
C16A—H16D···O8ⁱⁱⁱ	0.98	2.98	3.459 (16)	112
C14—H14C···O7ⁱⁱⁱ	0.99	2.96	3.873 (18)	154
C18—H18A···O8Aⁱⁱⁱ	0.99	2.95	3.675 (18)	131
C18—H18B···O8ⁱⁱⁱ	0.99	2.65	3.463 (18)	140
C16—H16B···O4A^iv	0.98	2.66	3.558 (18)	153
C20—H20B···O7^v	0.98	2.80	3.607 (17)	140
C22—H22B···O11A^vi	0.99	2.95	3.781 (17)	142
C24—H24A···O12^vi	0.98	2.98	3.554 (19)	118
C22A—H22C···O11^vi	0.99	3.01	3.586 (17)	118
C22A—H22D···O12^vi	0.99	2.82	3.711 (18)	149
C22—H22A···O12^vi	0.99	2.84	3.511 (18)	126
C24A—H24F···O11^vi	0.98	2.93	3.533 (19)	121
C2A—H2C···O2A^vii	0.99	2.97	3.569 (16)	120
C2A—H2D···O4A^vii	0.99	2.79	3.645 (17)	145
C5A—H5C···O4A^vii	0.99	2.80	3.784 (16)	172
C12A—H12F···O3A^vii	0.98	2.69	3.552 (18)	146
C4A—H4E···O3A^viii	0.98	2.68	3.549 (17)	148

Symmetry codes: (i) −x+1, −y, z+1/2; (ii) −x+1, y−1/2, z; (iii) x, −y+1/2, z−1/2; (iv) −x, y+1/2, z; (v) x, y, z−1; (vi) x, −y−1/2, z−1/2; (vii) −x, −y, z+1/2; (viii) x, y, z+1.

Experimental details

	(Iat293)	(Iat230)	(Iat165)	(Iat100)
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U	C₄₈H₁₀₈O₂₀P₄Re₄U
M_r	2112.05	2112.05	2112.05	2112.05
Crystal system, space group	Tetragonal, I4₂m	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁	Monoclinic, Cc
Temperature (K)	293	230	165	100
a, b, c (Å)	15.5404 (6), 15.5404 (6), 14.8191 (11)	21.5289 (15), 21.9148 (16), 14.8288 (11)	21.4344 (15), 21.7929 (15), 14.7782 (10)	21.40 (2), 21.68 (2), 14.78 (2)
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 90	90, 90.00 (3), 90
V (Å³)	3578.9 (3)	6996.3 (9)	6903.2 (8)	6857 (13)
Z	2	4	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	9.14	9.35	9.48	9.55
Crystal size (mm)	0.15 × 0.15 × 0.10	0.15 × 0.15 × 0.10	0.15 × 0.15 × 0.10	0.12 × 0.1 × 0.08

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	Rigaku RAXIS diffractometer
Absorption correction	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS	–
T_min, T_max	0.341, 0.462	0.334, 0.455	0.331, 0.451	–
No. of measured, independent and observed [I > 2σ(I)] reflections	10483, 1941, 1699	25273, 6529, 6180	24887, 6428, 6171	49029, 11595, 11431
R_int	0.029	0.027	0.029	0.06
(sin θ/λ)_max (Å⁻¹)	0.626	0.595	0.595	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.099, 1.09	0.027, 0.068, 1.12	0.025, 0.065, 1.11	0.032, 0.080, 1.05
No. of reflections	1941	6529	6428	11595
No. of parameters	102	377	417	698
No. of restraints	58	324	152	2
H-atom treatment	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0614P)²] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0273P)² + 21.6652P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0227P)² + 46.403P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0247P)² + 70.409P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.04, −0.38	2.23, −1.05	2.33, −1.21	1.77, −1.88
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter	0.03 (2)	0.025 (9)	0.020 (9)	0.00

	(IIat293)	(IIat230)	(IIat165)	(IIat100)
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th	C₄₈H₁₀₈O₂₀P₄Re₄Th
M_r	2106.06	2106.06	2106.06	2106.06
Crystal system, space group	Tetragonal, I4₂m	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁
Temperature (K)	293	230	165	100
a, b, c (Å)	15.5577 (12), 15.5577 (12), 14.8730 (17)	21.721 (3), 21.738 (3), 14.8793 (19)	21.610 (3), 21.623 (3), 14.8324 (19)	21.535 (3), 21.548 (3), 14.7950 (19)
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 90	90, 90, 90
V (Å³)	3599.9 (6)	7025.4 (16)	6930.7 (15)	6865.4 (15)
Z	2	4	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	8.91	9.13	9.25	9.34
Crystal size (mm)	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10	0.18 × 0.18 × 0.10

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer
Absorption correction	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS
T_min, T_max	0.297, 0.470	0.290, 0.462	0.689, 1.000	0.284, 0.455
No. of measured, independent and observed [I > 2σ(I)] reflections	5728, 1932, 1605	18098, 6391, 6029	24808, 6458, 6367	24358, 6390, 6376
R_int	0.028	0.042	0.036	0.034
(sin θ/λ)_max (Å⁻¹)	0.625	0.595	0.595	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.117, 1.01	0.036, 0.076, 1.07	0.026, 0.054, 1.06	0.027, 0.059, 1.16
No. of reflections	1932	6391	6458	6390
No. of parameters	102	393	372	393
No. of restraints	95	387	312	399
H-atom treatment	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0736P)²] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0314P)² + 8.8462P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0201P)² + 25.4516P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0121P)² + 76.2392P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.79, −0.59	1.13, −1.55	1.10, −1.05	1.62, −1.34
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter	0.09 (4)	0.037 (15)	0.011 (11)	0.027 (13)

	(IIIat293)	(IIIat230)	(IIIat170)	(IIIat130)
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th	C₄₈H₁₀₈O₂₀P₄Tc₄Th
M_r	1753.26	1753.26	1753.26	1753.26
Crystal system, space group	Cubic, I4₃m	Orthorhombic, Cmc2₁	Orthorhombic, Pbc2₁	Orthorhombic, Pbc2₁
Temperature (K)	293	230	170	130
a, b, c (Å)	15.3423 (10), 15.3423 (10), 15.3423 (10)	21.444 (2), 21.582 (2), 14.736 (2)	21.417 (6), 21.649 (6), 14.848 (4)	21.358 (13), 21.651 (13), 14.790 (9)
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 90	90, 90, 90
V (Å³)	3611.4 (4)	6819.9 (13)	6885 (3)	6839 (7)
Z	2	4	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	2.95	3.12	3.09	3.11
Crystal size (mm)	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10	0.10 × 0.10 × 0.10

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer	CCD area detector diffractometer
Absorption correction	–	Multi-scan SADABS	Multi-scan SADABS	Multi-scan SADABS
T_min, T_max	–	0.746, 0.746	0.748, 0.748	0.746, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	6235, 723, 651	26789, 7255, 6041	54013, 14267, 12482	50705, 14038, 12090
R_int	0.041	0.055	0.074	0.090
(sin θ/λ)_max (Å⁻¹)	0.623	0.627	0.627	0.626

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.101, 1.02	0.037, 0.088, 0.97	0.050, 0.127, 1.08	0.053, 0.130, 1.05
No. of reflections	723	7255	14267	14038
No. of parameters	50	354	707	707
No. of restraints	29	57	25	23
H-atom treatment	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0666P)²] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0428P)²] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.042P)² + 14.969P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0001P)² + 21.3104P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.27	1.43, −0.77	3.57, −0.88	3.15, −1.14
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter	0.00 (2)	0.034 (7)	0.016 (6)	0.017 (6)

	(IIIat100)
Crystal data
Chemical formula	C₄₈H₁₀₈O₂₀P₄Tc₄Th
M_r	1753.26
Crystal system, space group	Orthorhombic, Pbc2₁
Temperature (K)	100
a, b, c (Å)	21.386 (4), 21.732 (4), 14.820 (2)
α, β, γ (°)	90, 90, 90
V (Å³)	6888 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.09
Crystal size (mm)	0.10 × 0.10 × 0.10

Data collection
Diffractometer	CCD area detector diffractometer
Absorption correction	Multi-scan SADABS
T_min, T_max	0.748, 0.748
No. of measured, independent and observed [I > 2σ(I)] reflections	35481, 13901, 12000
R_int	0.073
(sin θ/λ)_max (Å⁻¹)	0.629

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.062, 0.161, 1.09
No. of reflections	13901
No. of parameters	707
No. of restraints	19
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0606P)² + 22.3563P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	4.83, −3.50
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter	0.020 (8)

Computer programs: Bruker SMART, MSC RAXIS11 Control, DENZO (Otwinowski, Z. 1988), Bruker SAINT, SHELXS97 (Sheldrick, 1990), SIR97 (Altomare, et al. 1997), SHELXL97 (Sheldrick, 1997), Bruker SHELXTL, TEXSAN (MSC, 1995).

Hydrogen-bond geometry (Å, º) for (Iat230) top

D—H···A	D—H	H···A	D···A	D—H···A
C18—H18A···O8ⁱ	0.98	3.10	3.849 (13)	134.4
C18—H18B···O8ⁱⁱ	0.98	3.10	3.849 (13)	134.4
C2—H2B···O6	0.98	2.52	3.377 (15)	145.6
C2—H2B···O10	0.98	2.96	3.670 (17)	130.5
C3—H3A···O12	0.98	2.76	3.603 (17)	144.5
C5—H5A···O8	0.98	2.48	3.450 (12)	168.6
C5—H5B···O2	0.98	2.60	3.460 (13)	147.1
C9—H9B···O2	0.98	2.84	3.637 (13)	139.5
C9—H9B···O4	0.98	2.98	3.632 (12)	125.2
C10—H10A···O11	0.98	2.95	3.492 (15)	116.2
C10—H10B···O4	0.98	2.97	3.552 (14)	119.2
C10—H10B···O5	0.98	2.88	3.238 (12)	102.7
C14A—H14B···O9	0.98	2.74	3.176 (17)	107.5
C14A—H14B···O9	0.98	2.74	3.176 (17)	107.5
C17—H17B···O1	0.98	2.67	3.327 (12)	124.4
C17—H17B···O3	0.98	2.94	3.915 (11)	174.0
C26—H26B···O1	0.98	2.91	3.529 (18)	122.3
C4—H4A···O2ⁱⁱⁱ	0.97	2.96	3.854 (19)	154.2
C6—H6A···O4ⁱⁱⁱ	0.98	2.95	3.620 (12)	126.4
C6—H6B···O3ⁱⁱⁱ	0.98	2.74	3.548 (12)	139.8
C8—H8B···O4ⁱⁱⁱ	0.97	2.71	3.608 (14)	153.4
C9—H9A···O3ⁱⁱⁱ	0.98	2.75	3.717 (11)	170.8
C12—H12A···O3ⁱⁱⁱ	0.97	2.97	3.771 (15)	140.9
C14B—H14C···O7ⁱ	0.98	2.83	3.48 (3)	124.7
C14B—H14D···O8ⁱ	0.98	2.90	3.78 (3)	150.7
C13A—H13A···O7ⁱ	0.98	2.71	3.60 (2)	151.0
C13A—H13A···O7ⁱ	0.98	2.71	3.60 (2)	151.0
C14B—H14C···O7ⁱ	0.98	2.83	3.48 (3)	124.7
C13A—H13A···O7ⁱⁱ	0.98	2.71	3.60 (2)	151.0
C14B—H14C···O7ⁱⁱ	0.98	2.83	3.48 (3)	124.7
C13A—H13A···O7ⁱⁱ	0.98	2.71	3.60 (2)	151.0
C14B—H14C···O7ⁱⁱ	0.98	2.83	3.48 (3)	124.7
C17—H17A···O1^iv	0.98	2.67	3.327 (12)	124.4
C17—H17A···O3^iv	0.98	2.94	3.915 (12)	174.0
C13A—H13B···O8^iv	0.98	2.86	3.59 (2)	131.9
C13B—H13D···O2^iv	0.98	3.05	3.65 (3)	121.0
C21—H21A···O4^iv	0.98	2.69	3.620 (15)	158.4
C21—H21B···O11^iv	0.98	2.64	3.524 (15)	149.9
C25—H25A···O4^iv	0.98	2.92	3.75 (3)	143.2
C26—H26A···O1^iv	0.98	2.73	3.529 (18)	138.7
C26—H26A···O3^iv	0.98	2.97	3.861 (15)	152.5
C14A—H14B···O2^iv	0.98	2.93	3.502 (18)	118.3
C20—H20A···O7^v	0.97	2.73	3.531 (18)	139.8
C28—H28A···O12^v	0.97	2.99	3.94 (3)	165.9
C20—H20A···O7^vi	0.97	2.73	3.531 (18)	139.8
C28—H28A···O12^vi	0.97	2.99	3.94 (3)	165.9
C22—H22A···O11^vii	0.98	2.94	3.634 (13)	128.8
C22—H22B···O12^vii	0.98	2.77	3.559 (13)	138.3
C24—H24B···O11^vii	0.97	2.91	3.69 (2)	138.3
C22—H22B···O12^viii	0.98	2.77	3.559 (13)	138.3
C16B—H16F···O4^ix	0.97	3.02	3.84 (3)	144.0
C16A—H16A···O7ⁱ	0.97	3.28	3.84 (2)	118.9
C16A—H16B···O8ⁱ	0.97	3.11	3.94 (2)	144.9

Symmetry codes: (i) −x+2, −y+1, z+1/2; (ii) x, −y+1, z+1/2; (iii) −x+3/2, −y+3/2, z−1/2; (iv) −x+2, y, z; (v) x, y, z+1; (vi) −x+2, y, z+1; (vii) −x+2, −y+2, z+1/2; (viii) x, −y+2, z+1/2; (ix) x+1/2, y−1/2, z.

Hydrogen-bond geometry (Å, º) for (Iat100) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.97	2.57	3.44 (2)	149.1
C2—H2A···O7	0.97	2.93	3.36 (2)	108.0
C2—H2A···O10	0.97	2.88	3.583 (19)	130.1
C2—H2A···O7	0.97	2.93	3.36 (2)	108.0
C3—H3A···O12	0.97	2.82	3.67 (2)	147.6
C5—H5A···O2	0.97	2.74	3.56 (2)	143.3
C5—H5B···O8	0.97	2.58	3.529 (19)	164.8
C9—H9A···O2	0.97	2.77	3.59 (2)	142.3
C9—H9A···O4	0.97	2.89	3.57 (2)	127.2
C10—H10A···O5	0.97	2.91	3.28 (2)	104.0
C10—H10B···O11	0.97	2.89	3.37 (2)	112.2
C10—H10B···O11	0.97	2.89	3.37 (2)	112.2
C13—H13B···O2A	0.97	2.79	3.56 (2)	136.9
C14—H14A···O8A	0.97	2.72	3.27 (2)	116.2
C14—H14B···O9	0.97	2.92	3.18 (2)	96.2
C14—H14A···O8A	0.97	2.72	3.27 (2)	116.2
C17—H17A···O1	0.97	2.53	3.215 (19)	127.8
C17—H17A···O3	0.97	2.97	3.92 (3)	166.2
C17—H17B···O1A	0.97	2.90	3.475 (18)	119.0
C17—H17B···O3A	0.97	2.82	3.78 (2)	172.9
C21—H21A···O11A	0.97	2.60	3.494 (18)	152.8
C21—H21B···O4A	0.97	2.62	3.591 (19)	177.4
C25—H25A···O4	0.97	2.67	3.528 (19)	147.2
C26—H26B···O1	0.97	2.91	3.720 (17)	141.4
C26—H26B···O1A	0.97	2.67	3.308 (17)	123.8
C2A—H2D···O6	0.97	2.56	3.34 (2)	137.4
C2A—H2D···O10	0.97	2.83	3.58 (2)	134.8
C3A—H3C···O12	0.97	2.68	3.556 (18)	150.8
C5A—H5C···O8A	0.97	2.53	3.479 (19)	166.8
C5A—H5D···O2A	0.97	2.56	3.39 (2)	143.9
C9A—H9D···O2A	0.97	2.81	3.574 (19)	136.5
C9A—H9D···O4A	0.97	2.90	3.56 (2)	125.9
C10A—H10C···O4A	0.97	2.87	3.45 (2)	119.4
C10A—H10C···O5A	0.97	2.89	3.209 (19)	100.6
C13A—H13D···O8	0.97	2.71	3.49 (2)	137.7
C14A—H14D···O2	0.97	2.95	3.471 (18)	115.2
C14A—H14D···O9	0.97	2.81	3.20 (2)	104.7
C15A—H15C···O8	0.97	2.98	3.73 (2)	134.8
C21A—H21D···O11	0.97	2.82	3.481 (19)	126.2
C6—H6A···O3Aⁱ	0.97	2.75	3.52 (2)	137.1
C6—H6B···O4Aⁱ	0.97	2.74	3.46 (2)	130.9
C12—H12B···O3Aⁱ	0.96	2.83	3.74 (2)	157.6
C9—H9B···O3Aⁱ	0.97	2.72	3.69 (2)	175.2
C8—H8B···O4Aⁱ	0.96	2.90	3.65 (2)	135.6
C13A—H13C···O7ⁱⁱ	0.97	2.63	3.524 (17)	154.2
C16—H16A···O8Aⁱⁱ	0.96	2.98	3.89 (2)	159.6
C16A—H16D···O7ⁱⁱ	0.96	2.81	3.75 (2)	168.0
C18—H18A···O8Aⁱⁱ	0.97	2.97	3.757 (17)	139.5
C20—H20C···O7ⁱⁱⁱ	0.96	2.73	3.537 (18)	142.0
C22—H22B···O11A^iv	0.97	2.91	3.665 (19)	135.1
C24—H24A···O12^iv	0.96	2.73	3.51 (2)	138.3
C22—H22A···O12^iv	0.97	2.68	3.417 (17)	132.8
C22A—H22C···O12^iv	0.97	2.68	3.540 (18)	148.2
C22A—H22D···O11^iv	0.97	2.98	3.598 (19)	122.7
C12A—H12D···O3^v	0.96	2.99	3.92 (2)	162.9
C4A—H4D···O2^v	0.96	2.83	3.68 (2)	148.8
C6A—H6D···O3^v	0.97	2.64	3.437 (18)	139.5
C8A—H8D···O4^v	0.96	2.96	3.46 (2)	114.4
C9A—H9C···O3^v	0.97	2.76	3.712 (19)	165.6
C8—H8C···O11A^vi	0.96	3.15	3.87 (2)	133.0
C20—H20B···O8ⁱⁱ	0.96	3.11	3.57 (2)	110.8
C20—H20B···O8Aⁱⁱ	0.96	3.03	3.93 (2)	158.2
C24—H24B···O11A^iv	0.96	3.19	3.81 (2)	123.7
C28—H28C···O12ⁱⁱⁱ	0.96	3.01	3.97 (2)	172.7
C8A—H8E···O11^vii	0.96	3.16	3.98 (2)	145.1
C16A—H16D···O7ⁱⁱ	0.96	2.81	3.75 (2)	168.0
C24A—H24D···O11^iv	0.96	3.05	3.74 (3)	130.6
C24A—H24E···O12^iv	0.96	3.29	3.94 (3)	126.4

Symmetry codes: (i) x−1/2, −y+3/2, z+1/2; (ii) x, −y+1, z−1/2; (iii) x, y, z−1; (iv) x, −y+2, z−1/2; (v) x+1/2, −y+3/2, z+1/2; (vi) x−1/2, y−1/2, z; (vii) x+1/2, y−1/2, z.

Hydrogen-bond geometry (Å, º) for (IIat230) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.97	2.63	3.476 (19)	146.3
C2—H2A···O10	0.97	2.90	3.63 (2)	133.4
C3—H3B···O12	0.97	2.75	3.62 (2)	148.9
C5—H5B···O8	0.97	2.54	3.49 (2)	168.3
C5—H5A···O2	0.97	2.63	3.492 (19)	147.7
C9—H9A···O2	0.97	2.84	3.65 (2)	140.9
C9—H9A···O4	0.97	3.02	3.663 (19)	125.2
C10—H10A···O11	0.97	3.11	3.65 (2)	116.7
C10—H10B···O4	0.97	2.97	3.55 (2)	119.7
C10—H10B···O5	0.97	2.87	3.220 (17)	102.3
C14A—H14A···O9	0.97	2.84	3.22 (3)	104.3
C14A—H14A···O9	0.97	2.84	3.22 (3)	104.3
C17—H17A···O1	0.97	2.74	3.41 (2)	126.8
C17—H17A···O3	0.97	2.95	3.915 (19)	173.5
C26—H26A···O1	0.97	2.94	3.55 (3)	122.0
C4—H4A···O2ⁱ	0.96	3.01	3.90 (3)	153.7
C6—H6A···O4ⁱ	0.97	2.90	3.587 (19)	128.7
C6—H6B···O3ⁱ	0.97	2.80	3.565 (18)	136.3
C8—H8C···O4ⁱ	0.96	2.71	3.58 (2)	151.0
C9—H9B···O3ⁱ	0.97	2.77	3.731 (18)	172.1
C12—H12A···O3ⁱ	0.96	2.96	3.73 (2)	138.2
C13A—H13B···O7ⁱⁱ	0.97	2.73	3.46 (3)	132.8
C13A—H13B···O7ⁱⁱ	0.97	2.73	3.46 (3)	132.8
C13B—H13C···O7ⁱⁱ	0.97	3.41	4.09 (4)	128.5
C13A—H13B···O7ⁱⁱⁱ	0.97	2.73	3.46 (3)	132.8
C13A—H13B···O7ⁱⁱⁱ	0.97	2.73	3.46 (3)	132.8
C13A—H13B···O7ⁱⁱⁱ	0.97	2.73	3.46 (3)	132.8
C13B—H13C···O7ⁱⁱⁱ	0.97	3.41	4.09 (4)	128.5
C18—H18B···O8ⁱⁱ	0.97	3.03	3.80 (2)	136.8
C18—H18A···O8ⁱⁱⁱ	0.97	3.03	3.80 (2)	136.8
C17—H17B···O1^iv	0.97	2.74	3.41 (2)	126.8
C17—H17B···O3^iv	0.97	2.95	3.915 (19)	173.5
C13A—H13A···O8^iv	0.97	3.20	3.75 (3)	117.8
C14A—H14A···O8^iv	0.97	2.85	3.55 (4)	129.7
C21—H21B···O4^iv	0.97	2.69	3.62 (3)	160.6
C21—H21A···O11^iv	0.97	2.64	3.53 (2)	152.2
C25—H25B···O4^iv	0.97	2.89	3.74 (6)	146.8
C26—H26B···O1^iv	0.97	2.75	3.55 (3)	140.1
C26—H26B···O3^iv	0.97	3.06	3.93 (2)	149.8
C14A—H14B···O2^iv	0.97	2.94	3.57 (3)	124.0
C20—H20A···O7^v	0.96	2.62	3.37 (3)	135.3
C28—H28A···O12^v	0.96	2.97	3.92 (4)	170.1
C20—H20A···O7^vi	0.96	2.62	3.37 (3)	135.3
C28—H28A···O12^vi	0.96	2.97	3.92 (4)	170.1
C22—H22B···O11^vii	0.97	2.98	3.702 (19)	132.6
C22—H22A···O12^vii	0.97	2.75	3.49 (2)	133.8
C24—H24C···O11^vii	0.96	3.04	3.79 (3)	136.5
C22—H22A···O12^viii	0.97	2.75	3.49 (2)	133.8
C16B—H16D···O7ⁱⁱ	0.96	3.57	4.22 (6)	127.4
C16A—H16A···O7ⁱⁱ	0.96	3.25	3.77 (4)	116.1
C16A—H16C···O8ⁱⁱ	0.96	3.02	3.89 (4)	151.0

Symmetry codes: (i) −x+1/2, −y+1/2, z+1/2; (ii) −x, −y+1, z−1/2; (iii) x, −y+1, z−1/2; (iv) −x, y, z; (v) x, y, z−1; (vi) −x, y, z−1; (vii) −x, −y, z−1/2; (viii) x, −y, z−1/2.

Hydrogen-bond geometry (Å, º) for (IIat100) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O6	0.99	2.56	3.421 (14)	145.2
C2—H2A···O10	0.99	2.84	3.590 (15)	132.8
C3—H3B···O12	0.99	2.70	3.611 (15)	153.1
C5—H5B···O8	0.99	2.57	3.522 (17)	162.3
C5—H5A···O2	0.99	2.64	3.483 (16)	143.5
C9—H9A···O2	0.99	2.74	3.561 (14)	140.1
C9—H9A···O4	0.99	2.91	3.598 (13)	127.6
C10—H10A···O11	0.99	3.06	3.561 (18)	112.5
C10—H10B···O4	0.99	3.02	3.539 (14)	114.2
C10—H10B···O5	0.99	2.85	3.222 (13)	103.0
C14A—H14A···O9	0.99	3.12	3.34 (2)	94.0
C14A—H14A···O9	0.99	3.12	3.34 (2)	94.0
C17—H17A···O1	0.99	2.73	3.386 (18)	124.1
C17—H17A···O3	0.99	2.91	3.903 (15)	175.8
C26—H26B···O1	0.99	2.92	3.471 (18)	115.9
C4—H4A···O2ⁱ	0.98	2.95	3.847 (18)	152.7
C6—H6A···O4ⁱ	0.99	2.79	3.491 (15)	128.3
C6—H6B···O3ⁱ	0.99	2.72	3.505 (13)	136.1
C8—H8C···O4ⁱ	0.98	2.63	3.509 (15)	149.1
C9—H9B···O3ⁱ	0.99	2.66	3.646 (14)	173.7
C12—H12A···O3ⁱ	0.98	2.99	3.778 (14)	138.1
C13A—H13B···O7ⁱⁱ	0.99	2.92	3.45 (3)	114.3
C13A—H13B···O7ⁱⁱ	0.99	2.92	3.45 (3)	114.3
C13B—H13C···O7ⁱⁱ	0.99	2.86	3.79 (3)	156.2
C13A—H13B···O7ⁱⁱⁱ	0.99	2.92	3.45 (3)	114.3
C13A—H13B···O7ⁱⁱⁱ	0.99	2.92	3.45 (3)	114.3
C13A—H13B···O7ⁱⁱⁱ	0.99	2.92	3.45 (3)	114.3
C13B—H13C···O7ⁱⁱⁱ	0.99	2.86	3.79 (3)	156.2
C18—H18A···O8ⁱⁱ	0.99	2.87	3.645 (18)	135.6
C18—H18B···O8ⁱⁱⁱ	0.99	2.87	3.645 (18)	135.6
C17—H17B···O1^iv	0.99	2.73	3.386 (18)	124.1
C17—H17B···O3^iv	0.99	2.91	3.903 (15)	175.8
C13A—H13A···O8^iv	0.99	3.39	3.73 (3)	102.4
C14A—H14B···O8^iv	0.99	2.28	3.25 (3)	165.0
C21—H21B···O4^iv	0.99	2.79	3.72 (2)	157.5
C21—H21A···O11^iv	0.99	2.59	3.467 (17)	148.1
C25—H25B···O4^iv	0.99	2.73	3.66 (3)	155.2
C26—H26A···O1^iv	0.99	2.64	3.471 (18)	141.3
C26—H26A···O3^iv	0.99	3.12	3.953 (16)	142.4
C14A—H14A···O2^iv	0.99	2.79	3.76 (3)	170.3
C20—H20A···O7^v	0.98	2.55	3.275 (19)	130.9
C28—H28A···O12^v	0.98	2.98	3.96 (3)	176.4
C20—H20A···O7^vi	0.98	2.55	3.275 (19)	130.9
C28—H28A···O12^vi	0.98	2.98	3.96 (3)	176.4
C22—H22A···O11^vii	0.99	2.87	3.632 (16)	134.4
C22—H22B···O12^vii	0.99	2.65	3.413 (15)	134.4
C24—H24C···O11^vii	0.98	3.01	3.78 (2)	137.0
C22—H22B···O12^viii	0.99	2.65	3.413 (15)	134.4
C16B—H16D···O7ⁱⁱ	0.98	3.36	4.00 (4)	124.7
C16A—H16C···O7ⁱⁱ	0.98	3.05	3.64 (4)	119.9
C16A—H16C···O8ⁱⁱ	0.98	3.05	4.02 (4)	172.2

Hydrogen-bond geometry (Å, º) for (IIIat230) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2A···O5	0.97	2.94	3.337 (14)	105.6
C2—H2A···O6	0.97	2.60	3.454 (14)	147.4
C2—H2A···O7	0.97	3.00	3.464 (16)	110.4
C2—H2A···O10	0.97	2.92	3.650 (16)	133.3
C3—H3B···O12	0.97	2.68	3.537 (19)	147.3
C5—H5B···O8	0.97	2.58	3.533 (14)	167.1
C5—H5A···O2	0.97	2.59	3.449 (14)	147.6
C9—H9A···O2	0.97	2.82	3.624 (15)	141.3
C9—H9A···O4	0.97	2.97	3.633 (14)	126.9
C10—H10A···O11	0.97	3.07	3.564 (16)	113.3
C10—H10B···O4	0.97	3.02	3.565 (15)	116.9
C10—H10B···O5	0.97	2.87	3.228 (14)	102.7
C17—H17A···O1	0.97	2.71	3.350 (16)	124.0
C17—H17A···O3	0.97	2.88	3.853 (13)	176.7
C26—H26A···O1	0.97	2.68	3.54 (2)	147.7
C4—H4A···O2ⁱ	0.96	3.02	3.880 (19)	149.4
C6—H6B···O4ⁱ	0.97	2.88	3.559 (13)	127.7
C6—H6A···O3ⁱ	0.97	2.74	3.523 (13)	138.1
C8—H8A···O4ⁱ	0.96	3.05	3.580 (15)	115.9
C9—H9B···O3ⁱ	0.97	2.72	3.682 (13)	172.9
C12—H12A···O3ⁱ	0.96	3.13	3.741 (15)	122.7
C13A—H13B···O7ⁱⁱ	0.97	2.81	3.60 (3)	138.8
C13A—H13B···O7ⁱⁱ	0.97	2.81	3.60 (3)	138.8
C13B—H13C···O7ⁱⁱ	0.97	3.27	4.13 (4)	148.7
C13A—H13B···O7ⁱⁱⁱ	0.97	2.81	3.60 (3)	138.8
C13A—H13B···O7ⁱⁱⁱ	0.97	2.81	3.60 (3)	138.8
C13A—H13B···O7ⁱⁱⁱ	0.97	2.81	3.60 (3)	138.8
C13B—H13C···O7ⁱⁱⁱ	0.97	3.27	4.13 (4)	148.7
C18—H18B···O8ⁱⁱ	0.97	3.01	3.742 (16)	132.9
C18—H18A···O8ⁱⁱⁱ	0.97	3.01	3.742 (16)	132.9
C17—H17B···O1^iv	0.97	2.71	3.350 (16)	124.0
C17—H17B···O3^iv	0.97	2.88	3.853 (13)	176.7
C13A—H13A···O8^iv	0.97	3.03	3.65 (3)	122.8
C13B—H13D···O2^iv	0.97	3.31	3.85 (4)	117.2
C21—H21B···O4^iv	0.97	2.68	3.605 (17)	160.7
C21—H21A···O11^iv	0.97	2.57	3.464 (16)	153.4
C26—H26B···O1^iv	0.97	3.03	3.54 (2)	114.2
C26—H26B···O3^iv	0.97	3.12	3.845 (18)	132.7
C20—H20A···O7^v	0.96	2.72	3.52 (3)	141.6
C28—H28C···O12^v	0.96	3.21	3.79 (4)	120.2
C20—H20A···O7^vi	0.96	2.72	3.52 (3)	141.6
C28—H28C···O12^vi	0.96	3.21	3.79 (4)	120.2
C22—H22A···O11^vii	0.97	2.91	3.633 (16)	132.0
C22—H22B···O12^vii	0.97	2.77	3.519 (15)	135.0
C24—H24A···O11^vii	0.96	3.31	3.82 (2)	115.1
C22—H22B···O12^viii	0.97	2.77	3.519 (15)	135.0

Hydrogen-bond geometry (Å, º) for (IIIat100) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1A···O11	0.99	2.83	3.696 (18)	147.0
C2—H2B···O5	0.99	2.85	3.265 (16)	105.7
C2—H2B···O6	0.99	2.90	3.578 (15)	126.7
C3—H3A···O12	0.99	2.77	3.602 (19)	142.5
C5—H5A···O2	0.99	2.73	3.614 (17)	148.8
C5—H5B···O6	0.99	2.49	3.230 (16)	131.6
C5—H5B···O8	0.99	2.79	3.736 (17)	160.3
C9—H9A···O2	0.99	2.84	3.689 (17)	144.1
C10—H10A···O11	0.99	2.62	3.318 (18)	127.3
C10—H10B···O4	0.99	2.87	3.608 (17)	132.3
C10—H10B···O5	0.99	2.85	3.179 (18)	100.3
C13—H13D···O2A	0.99	2.88	3.831 (17)	161.4
C14—H14D···O8A	0.99	2.50	3.420 (16)	155.1
C17—H17A···O1	0.99	2.57	3.301 (16)	130.3
C17—H17A···O3	0.99	2.76	3.732 (18)	166.0
C17—H17B···O3A	0.99	2.48	3.373 (17)	150.4
C21—H21A···O11A	0.99	2.50	3.462 (15)	164.4
C21—H21B···O1A	0.99	2.73	3.396 (16)	125.0
C21—H21B···O4A	0.99	2.87	3.849 (17)	172.4
C25—H25A···O4	0.99	2.79	3.56 (2)	135.9
C26—H26A···O13	0.99	2.71	3.18 (2)	109.1
C26—H26A···O3A	0.99	2.89	3.49 (2)	119.3
C27—H27B···O3	0.99	3.02	3.85 (2)	142.6
C1A—H1C···O10	0.99	2.71	3.477 (15)	134.7
C1A—H1C···O12	0.99	2.60	3.549 (17)	160.8
C1A—H1D···O7	0.99	2.51	3.381 (16)	147.2
C5A—H5D···O7	0.99	2.81	3.612 (17)	139.0
C5A—H5D···O8A	0.99	2.99	3.606 (16)	121.2
C6A—H6C···O5A	0.99	2.97	3.262 (14)	98.2
C6A—H6C···O8A	0.99	2.87	3.557 (16)	127.3
C6A—H6D···O2A	0.99	2.70	3.363 (16)	124.3
C9A—H9D···O2A	0.99	2.78	3.690 (15)	152.6
C10A—H10C···O10	0.99	2.68	3.390 (15)	128.5
C10A—H10C···O1A	0.99	2.77	3.574 (15)	138.2
C10A—H10C···O5A	0.99	2.95	3.325 (14)	103.4
C13A—H13B···O8A	0.99	2.84	3.702 (16)	146.1
C14A—H14A···O1	0.99	2.55	3.248 (17)	127.8
C14A—H14A···O6	0.99	2.93	3.705 (17)	135.9
C14A—H14A···O9	0.99	2.97	3.348 (16)	103.8
C15A—H15C···O8	0.99	2.93	3.849 (16)	153.9
C21A—H21C···O4	0.99	2.74	3.496 (19)	133.9
C21A—H21D···O11	0.99	2.95	3.680 (17)	131.6
C1—H1B···O2ⁱ	0.99	2.77	3.674 (17)	152.1
C6—H6B···O3ⁱ	0.99	2.82	3.611 (16)	137.8
C4—H4A···O2ⁱ	0.98	2.75	3.72 (2)	168.3
C12—H12B···O3ⁱ	0.98	3.01	3.69 (2)	127.7
C9—H9B···O3ⁱ	0.99	2.60	3.573 (17)	167.3
C12—H12C···O8ⁱⁱ	0.98	2.76	3.697 (18)	160.0
C24A—H24E···O2ⁱⁱ	0.98	2.92	3.70 (2)	136.5
C20—H20A···O8Aⁱⁱⁱ	0.98	2.97	3.73 (2)	135.4
C16A—H16D···O8ⁱⁱⁱ	0.98	2.98	3.459 (16)	111.5
C14—H14C···O7ⁱⁱⁱ	0.99	2.96	3.873 (18)	154.0
C18—H18A···O8Aⁱⁱⁱ	0.99	2.95	3.675 (18)	131.0
C18—H18B···O8ⁱⁱⁱ	0.99	2.65	3.463 (18)	140.0
C16—H16B···O4A^iv	0.98	2.66	3.558 (18)	153.3
C20—H20B···O7^v	0.98	2.80	3.607 (17)	139.7
C22—H22B···O11A^vi	0.99	2.95	3.781 (17)	142.3
C24—H24A···O12^vi	0.98	2.98	3.554 (19)	118.2
C22A—H22C···O11^vi	0.99	3.01	3.586 (17)	118.4
C22A—H22D···O12^vi	0.99	2.82	3.711 (18)	149.4
C22—H22A···O12^vi	0.99	2.84	3.511 (18)	126.1
C24A—H24F···O11^vi	0.98	2.93	3.533 (19)	121.0
C2A—H2C···O2A^vii	0.99	2.97	3.569 (16)	119.8
C2A—H2D···O4A^vii	0.99	2.79	3.645 (17)	145.4
C5A—H5C···O4A^vii	0.99	2.80	3.784 (16)	171.7
C12A—H12F···O3A^vii	0.98	2.69	3.552 (18)	146.4
C4A—H4E···O3A^viii	0.98	2.68	3.549 (17)	148.2

Footnotes

¹Supplementary data for this paper are available from the IUCr electronic archives (Reference: WS5025 ). Services for accessing these data are described at the back of the journal.

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119. Web of Science CrossRef CAS IUCr Journals Google Scholar
Bol'shakov, K. A., Sinitsyn, N. M., Travkin, V. F. & Borisov, V. V. (1967). Dokl. Akad. Nauk SSSR, 177, 344–346. CAS Google Scholar
Bruker (2001). SMART, Version 5.625, SADABS, Version 2.03a, and SHELXTL, Version 6.12. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2002). SAINT, Version 6.36a. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. & Taylor, R. (2002). Acta Cryst. B58, 389–397. Web of Science CrossRef CAS IUCr Journals Google Scholar
Capillas, C., Kroumova, E., Aroyo, M. I., Perez-Mato, J. M., Stokes, H. T. & Hatch, D. M. (2003). J. Appl. Cryst. 36, 953–954. CrossRef CAS IUCr Journals Google Scholar
Chakravorti, M. C. (1990). Coord. Chem. Rev. 106, 205–225. CrossRef CAS Web of Science Google Scholar
Desiraju, G. R. (1996). Acc. Chem. Res. 29, 441–449. CrossRef CAS PubMed Web of Science Google Scholar
Desiraju, G. R, & Steiner, T. (1999). The Weak Hydrogen Bond in Structural Chemistry and Biology, pp. 1–121. Oxford University Press. Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Fedosseev, A. M., Budantseva, N. A., Grigoriev, M. S., Guerman, K. E. & Krupa, J. C. (2003). Radiochim. Acta, 91, 147–152. Web of Science CrossRef CAS Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Haigh, C. W. (1995). Polyhedron, 14, 2871–2878. CrossRef CAS Web of Science Google Scholar
Herbst-Irmer, R. & Sheldrick, G. (1998). Acta Cryst. B54, 443–449. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
John, G. H. (2003). PhD. Thesis. The University of Manchester, England. Google Scholar
John, G. H., May, I., Sarsfield, M. J., Steele, H. M., Collison, D., Helliwell, M. & McKinney, J. D. (2004). Dalton Trans. pp. 734–740. Web of Science CSD CrossRef Google Scholar
Kenna, B. T. & Kuroda, P. K. (1961). J. Inorg. Nucl. Chem. 23, 142–144. CrossRef CAS Web of Science Google Scholar
Molecular Structure Corporation (1995). TEXSAN. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Google Scholar
Nardelli, M. (1995). J. Appl. Cryst. 28, 659. CrossRef IUCr Journals Google Scholar
Otwinowski, Z. (1988). DENZO. Department of Molecular Biophysics and Biochemistry, Yale University, New Haven, Connecticut. Google Scholar
Parsons, S. (2003). Acta Cryst. D59, 1995–2003. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sarsfield, M. J., Sutton, A. D., May, I., John, G. H., Sharrad, C. & Helliwell, M. (2004). Chem. Commun. pp. 2320–2321. CrossRef Google Scholar
Sheldrick, G. M. (1997). SHELX97. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2002). TWINABS. Bruker-AXS, Madison, Wisconsin, USA. Google Scholar
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sutton, A. D. (2003). PhD. Thesis. The University of Manchester, England. Google Scholar
Wilson, P. D. (1996). Editor. The Nuclear Fuel Cycle, pp. 116–183. BNFL plc, Oxford University Press. Google Scholar

© International Union of Crystallography. Prior permission is not required to reproduce short quotations, tables and figures from this article, provided the original authors and source are cited. For more information, click here.

STRUCTURAL SCIENCE
CRYSTAL ENGINEERING
MATERIALS

ISSN: 2052-5206

Volume 62| Part 1| February 2006| Pages 68-85

doi:10.1107/S0108768105036931

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

research papers\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)