Two phases of {[CsPH(η⁶-2,4,6-^tBu₃C₆H₂)]₂(η³-toluene)_0.5}_x: their structures and interconversions

The solvent-bridged caesium phosphide {[CsPH(η⁶-2,4,6-^tBu₃C₆H₂)]₂(η³-toluene)_0.5}_x, catena-[(μ-η³-toluene)-bis[caesium(2,4,6-tri-tert-butylphenylphosphide)]], undergoes a reversible solid-state, order–disorder phase transition characterized by the doubling of the unit-cell volume at low temperature achieved by doubling one unit-cell vector. The unit-cell parameters at 293 (2) K (form A) are: a = 11.147 (4), b = 14.615 (4), c = 14.806 (5) Å, α = 70.57 (3), β = 71.85 (3), γ = 72.93 (2)°, V = 2112.5 (12) ų, Z = 2, ρ_calc = 1.362 g cm⁻³, R₁ = 0.0513 for 5462 reflections, wR₂ = 0.0947 for all data. The unit-cell parameters at 173 (2) K (form B) are: a = 14.6241 (3), b = 14.7393 (3), c = 22.0720 (4) Å, α = 72.2117 (7), β = 73.3659 (8), γ = 70.2953 (7)°, V = 4174.8 (2) ų, Z = 4, ρ_calc = 1.379 g cm⁻³, R₁ = 0.0405 for 14 010 reflections, wR₂ = 0.1326 for all data. With a minor change, the key structural features discussed previously for form A [Rabe et al. (1998). Inorg. Chem. 37, 4235–4245] remain unchanged. The η³-toluene ligand is observed to be disordered at 293 (2) K and ordered at 173 (2) K, with the order–disorder phase transition occurring at approximately 278 (2) K.

Computing details

Data collection: Bruker SMART; cell refinement: Bruker SMART; data reduction: Bruker SHELXTL; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.

(IB)

Crystal data

{[Cs(C18H30P)]2.0.5(C7H8)}	Z = 4
Mr = 866.67	F(000) = 1764
Triclinic, P1	Dx = 1.379 Mg m^−3
a = 14.6241 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.7393 (3) Å	Cell parameters from 8192 reflections
c = 22.0720 (4) Å	θ = 2.0–25.0°
α = 72.2117 (7)°	µ = 1.85 mm^−1
β = 73.3659 (8)°	T = 173 K
γ = 70.2953 (7)°	Block, yellow
V = 4174.8 (2) Å^3	0.25 × 0.25 × 0.20 mm

Data collection

Siemens P4/CCD area detector diffractometer	14010 independent reflections
Radiation source: fine-focus sealed tube	12235 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
φ and ω scans	θmax = 25.0°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements)	h = −17→17
Tmin = 0.655, Tmax = 0.709	k = −16→17
25526 measured reflections	l = −26→24

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.149	H atoms treated by a mixture of independent and constrained refinement
S = 1.17	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
14010 reflections	(Δ/σ)max = 0.002
800 parameters	Δρmax = 0.70 e Å^−3
0 restraints	Δρmin = −0.83 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cs1	0.91459 (2)	0.87298 (2)	−0.186408 (15)	0.03716 (11)
Cs2	0.53824 (2)	1.11187 (2)	−0.124000 (15)	0.03565 (11)
Cs3	0.06400 (2)	1.11812 (2)	−0.338633 (14)	0.03208 (11)
Cs4	0.45865 (2)	0.89457 (2)	−0.368427 (15)	0.03522 (11)
P1	0.67376 (10)	0.86080 (10)	−0.06741 (6)	0.0336 (3)
H1	0.633 (5)	0.814 (5)	−0.093 (4)	0.09 (2)*
P2	0.78492 (10)	1.12002 (10)	−0.24817 (7)	0.0339 (3)
H2	0.761 (4)	1.111 (4)	−0.304 (3)	0.051 (16)*
P3	0.20183 (9)	0.87909 (9)	−0.26236 (6)	0.0330 (3)
H3	0.211 (4)	0.910 (4)	−0.212 (3)	0.041 (14)*
P4	0.31261 (10)	1.12661 (10)	−0.44819 (6)	0.0366 (3)
H4	0.354 (5)	1.150 (4)	−0.413 (3)	0.063 (19)*
C1	0.6662 (3)	0.7834 (3)	0.0155 (2)	0.0236 (9)
C2	0.6139 (3)	0.7061 (3)	0.0419 (2)	0.0236 (9)
C3	0.6119 (3)	0.6536 (3)	0.1053 (2)	0.0247 (9)
H3A	0.5773	0.6041	0.1211	0.030*
C4	0.6568 (3)	0.6677 (3)	0.1480 (2)	0.0236 (9)
C5	0.7069 (3)	0.7400 (3)	0.1231 (2)	0.0239 (9)
H5A	0.7382	0.7520	0.1509	0.029*
C6	0.7140 (3)	0.7968 (3)	0.0589 (2)	0.0246 (9)
C7	0.5561 (3)	0.6811 (4)	0.0036 (2)	0.0317 (10)
C8	0.5042 (4)	0.5982 (4)	0.0450 (3)	0.0454 (14)
H8A	0.4581	0.6195	0.0833	0.068*
H8B	0.5545	0.5371	0.0589	0.068*
H8C	0.4676	0.5862	0.0187	0.068*
C9	0.6259 (4)	0.6388 (5)	−0.0545 (3)	0.0477 (14)
H9A	0.6616	0.6867	−0.0832	0.072*
H9B	0.5867	0.6259	−0.0788	0.072*
H9C	0.6736	0.5768	−0.0385	0.072*
C10	0.4700 (4)	0.7702 (4)	−0.0159 (2)	0.0402 (12)
H10A	0.4958	0.8264	−0.0424	0.060*
H10B	0.4236	0.7881	0.0233	0.060*
H10C	0.4354	0.7531	−0.0411	0.060*
C11	0.6477 (3)	0.6071 (3)	0.2188 (2)	0.0257 (9)
C12	0.7132 (4)	0.6216 (5)	0.2549 (2)	0.0469 (14)
H12A	0.7044	0.5813	0.2995	0.070*
H12B	0.6952	0.6916	0.2557	0.070*
H12C	0.7827	0.6012	0.2329	0.070*
C13	0.5402 (4)	0.6398 (4)	0.2551 (2)	0.0472 (15)
H13A	0.5336	0.6016	0.3003	0.071*
H13B	0.4959	0.6282	0.2341	0.071*
H13C	0.5224	0.7105	0.2541	0.071*
C14	0.6754 (5)	0.4973 (4)	0.2196 (3)	0.0491 (14)
H14A	0.6698	0.4585	0.2647	0.074*
H14B	0.7439	0.4769	0.1958	0.074*
H14C	0.6305	0.4861	0.1989	0.074*
C15	0.7776 (3)	0.8731 (4)	0.0395 (2)	0.0305 (10)
C16	0.7151 (5)	0.9794 (4)	0.0190 (3)	0.0520 (15)
H16A	0.7566	1.0248	0.0073	0.078*
H16B	0.6601	0.9960	0.0550	0.078*
H16C	0.6887	0.9857	−0.0186	0.078*
C17	0.8193 (4)	0.8726 (4)	0.0955 (3)	0.0456 (14)
H17A	0.8579	0.9211	0.0808	0.068*
H17B	0.8622	0.8064	0.1102	0.068*
H17C	0.7645	0.8899	0.1315	0.068*
C18	0.8688 (4)	0.8416 (5)	−0.0142 (3)	0.0456 (14)
H18A	0.9095	0.8880	−0.0270	0.068*
H18B	0.8461	0.8423	−0.0521	0.068*
H18C	0.9085	0.7747	0.0026	0.068*
C19	0.8323 (3)	1.2298 (3)	−0.2836 (2)	0.0233 (9)
C20	0.8767 (3)	1.2589 (3)	−0.2451 (2)	0.0210 (8)
C21	0.9369 (3)	1.3237 (3)	−0.2754 (2)	0.0235 (9)
H21A	0.9678	1.3398	−0.2492	0.028*
C22	0.9535 (3)	1.3653 (3)	−0.3418 (2)	0.0210 (9)
C23	0.8981 (3)	1.3483 (3)	−0.3767 (2)	0.0221 (9)
H23A	0.9016	1.3824	−0.4211	0.027*
C24	0.8375 (3)	1.2840 (3)	−0.3506 (2)	0.0221 (9)
C25	0.8663 (4)	1.2209 (4)	−0.1701 (2)	0.0312 (10)
C26	0.7570 (4)	1.2341 (5)	−0.1355 (3)	0.0570 (17)
H26A	0.7527	1.2096	−0.0885	0.085*
H26B	0.7277	1.1966	−0.1508	0.085*
H26C	0.7209	1.3044	−0.1451	0.085*
C27	0.9051 (5)	1.2796 (4)	−0.1412 (2)	0.0492 (15)
H27A	0.8972	1.2533	−0.0941	0.074*
H27B	0.8675	1.3495	−0.1504	0.074*
H27C	0.9755	1.2735	−0.1607	0.074*
C28	0.9259 (5)	1.1136 (4)	−0.1516 (3)	0.0552 (16)
H28A	0.9178	1.0921	−0.1042	0.083*
H28B	0.9962	1.1076	−0.1714	0.083*
H28C	0.9023	1.0719	−0.1673	0.083*
C29	1.0218 (3)	1.4333 (3)	−0.3750 (2)	0.0225 (9)
C30	1.0957 (4)	1.4192 (4)	−0.3327 (2)	0.0334 (11)
H30A	1.0589	1.4342	−0.2906	0.050*
H30B	1.1379	1.4640	−0.3548	0.050*
H30C	1.1371	1.3505	−0.3259	0.050*
C31	1.0830 (3)	1.4089 (4)	−0.4404 (2)	0.0317 (10)
H31A	1.0380	1.4173	−0.4684	0.048*
H31B	1.1245	1.3403	−0.4328	0.048*
H31C	1.1254	1.4537	−0.4617	0.048*
C32	0.9586 (3)	1.5409 (3)	−0.3862 (2)	0.0298 (10)
H32A	0.9116	1.5502	−0.4129	0.045*
H32B	1.0017	1.5847	−0.4085	0.045*
H32C	0.9221	1.5566	−0.3442	0.045*
C33	0.7814 (3)	1.2769 (3)	−0.3983 (2)	0.0269 (10)
C34	0.7805 (4)	1.3622 (4)	−0.4589 (2)	0.0422 (13)
H34A	0.7446	1.3547	−0.4876	0.063*
H34B	0.8488	1.3611	−0.4819	0.063*
H34C	0.7474	1.4253	−0.4460	0.063*
C35	0.8331 (4)	1.1803 (4)	−0.4224 (3)	0.0483 (14)
H35A	0.7971	1.1766	−0.4525	0.072*
H35B	0.8334	1.1232	−0.3852	0.072*
H35C	0.9015	1.1798	−0.4449	0.072*
C36	0.6705 (3)	1.2873 (4)	−0.3669 (2)	0.0371 (12)
H36A	0.6366	1.2826	−0.3977	0.056*
H36B	0.6402	1.3517	−0.3554	0.056*
H36C	0.6644	1.2343	−0.3276	0.056*
C37	0.5719 (5)	0.9600 (5)	−0.2349 (3)	0.0547 (15)
H37A	0.6386	0.9120	−0.2439	0.066*
C38	0.5529 (5)	1.0482 (5)	−0.2806 (3)	0.0544 (16)
H38A	0.6091	1.0612	−0.3173	0.065*
C39	0.4575 (4)	1.0972 (4)	−0.2912 (3)	0.0455 (13)
H39A	0.4434	1.1676	−0.3167	0.055*
C40	0.3779 (4)	1.0585 (4)	−0.2552 (2)	0.0353 (11)
C41	0.3985 (4)	0.9694 (4)	−0.2096 (2)	0.0413 (12)
H41A	0.3420	0.9504	−0.1754	0.050*
C42	0.4944 (5)	0.9207 (4)	−0.1993 (3)	0.0483 (14)
H42A	0.5064	0.8601	−0.1676	0.058*
C43	0.2753 (4)	1.1096 (4)	−0.2666 (3)	0.0448 (13)
H43A	0.2422	1.1576	−0.2392	0.067*
H43B	0.2380	1.0606	−0.2556	0.067*
H43C	0.2782	1.1443	−0.3124	0.067*
C44	0.1579 (3)	0.7685 (3)	−0.2231 (2)	0.0226 (9)
C45	0.1219 (3)	0.7285 (3)	−0.2608 (2)	0.0214 (9)
C46	0.0636 (3)	0.6620 (3)	−0.2288 (2)	0.0212 (8)
H46A	0.0387	0.6381	−0.2544	0.025*
C47	0.0406 (3)	0.6296 (3)	−0.1614 (2)	0.0219 (9)
C48	0.0878 (3)	0.6578 (3)	−0.1265 (2)	0.0251 (9)
H48A	0.0792	0.6311	−0.0809	0.030*
C49	0.1467 (3)	0.7225 (3)	−0.1543 (2)	0.0226 (9)
C50	0.1407 (3)	0.7570 (3)	−0.3364 (2)	0.0288 (10)
C51	0.1069 (5)	0.6913 (4)	−0.3630 (2)	0.0469 (14)
H51A	0.1197	0.7114	−0.4106	0.070*
H51B	0.0358	0.6988	−0.3461	0.070*
H51C	0.1438	0.6219	−0.3493	0.070*
C52	0.2529 (4)	0.7402 (5)	−0.3655 (3)	0.0492 (15)
H52A	0.2635	0.7586	−0.4131	0.074*
H52B	0.2875	0.6703	−0.3513	0.074*
H52C	0.2787	0.7812	−0.3507	0.074*
C53	0.0833 (4)	0.8635 (4)	−0.3632 (3)	0.0455 (14)
H53A	0.0977	0.8776	−0.4108	0.068*
H53B	0.1035	0.9096	−0.3493	0.068*
H53C	0.0120	0.8714	−0.3468	0.068*
C54	−0.0261 (3)	0.5595 (3)	−0.1267 (2)	0.0250 (9)
C55	−0.0967 (4)	0.5681 (4)	−0.1690 (3)	0.0422 (13)
H55A	−0.1383	0.5229	−0.1462	0.063*
H55B	−0.0580	0.5507	−0.2102	0.063*
H55C	−0.1390	0.6363	−0.1779	0.063*
C56	−0.0903 (3)	0.5863 (4)	−0.0631 (2)	0.0352 (11)
H56A	−0.1321	0.5410	−0.0417	0.053*
H56B	−0.1324	0.6545	−0.0724	0.053*
H56C	−0.0474	0.5807	−0.0344	0.053*
C57	0.0393 (4)	0.4530 (4)	−0.1129 (3)	0.0384 (12)
H57A	−0.0027	0.4080	−0.0909	0.058*
H57B	0.0835	0.4469	−0.0850	0.058*
H57C	0.0789	0.4359	−0.1539	0.058*
C58	0.1990 (3)	0.7387 (4)	−0.1083 (2)	0.0322 (11)
C59	0.1491 (4)	0.8410 (4)	−0.0901 (3)	0.0497 (15)
H59A	0.0783	0.8475	−0.0718	0.075*
H59B	0.1568	0.8941	−0.1292	0.075*
H59C	0.1806	0.8457	−0.0580	0.075*
C60	0.3115 (3)	0.7243 (4)	−0.1376 (2)	0.0331 (11)
H60A	0.3404	0.6595	−0.1485	0.050*
H60B	0.3444	0.7279	−0.1058	0.050*
H60C	0.3206	0.7766	−0.1770	0.050*
C61	0.1956 (5)	0.6615 (5)	−0.0430 (3)	0.0532 (17)
H61A	0.2261	0.5948	−0.0509	0.080*
H61B	0.1264	0.6675	−0.0201	0.080*
H61C	0.2320	0.6730	−0.0163	0.080*
C62	0.3286 (3)	1.2091 (3)	−0.5295 (2)	0.0234 (9)
C63	0.2862 (3)	1.2021 (3)	−0.5788 (2)	0.0265 (9)
C64	0.2988 (3)	1.2646 (3)	−0.6410 (2)	0.0252 (9)
H64A	0.2710	1.2577	−0.6728	0.030*
C65	0.3492 (3)	1.3354 (3)	−0.6583 (2)	0.0251 (9)
C66	0.3893 (3)	1.3428 (3)	−0.6109 (2)	0.0264 (9)
H66A	0.4242	1.3915	−0.6219	0.032*
C67	0.3820 (3)	1.2835 (3)	−0.5481 (2)	0.0255 (9)
C68	0.2260 (4)	1.1271 (4)	−0.5682 (3)	0.0358 (11)
C69	0.2865 (5)	1.0190 (4)	−0.5489 (3)	0.0554 (16)
H69A	0.3468	1.0057	−0.5823	0.083*
H69B	0.2466	0.9749	−0.5450	0.083*
H69C	0.3045	1.0072	−0.5071	0.083*
C70	0.1283 (4)	1.1533 (5)	−0.5168 (3)	0.0511 (15)
H70A	0.0897	1.1067	−0.5097	0.077*
H70B	0.0892	1.2209	−0.5327	0.077*
H70C	0.1449	1.1488	−0.4758	0.077*
C71	0.1907 (4)	1.1348 (5)	−0.6297 (3)	0.0499 (15)
H71A	0.2485	1.1192	−0.6644	0.075*
H71B	0.1498	1.2023	−0.6439	0.075*
H71C	0.1515	1.0878	−0.6198	0.075*
C72	0.3635 (3)	1.4023 (4)	−0.7277 (2)	0.0299 (10)
C73	0.2966 (5)	1.3989 (6)	−0.7674 (3)	0.0643 (19)
H73A	0.3082	1.4425	−0.8107	0.096*
H73B	0.2271	1.4211	−0.7458	0.096*
H73C	0.3110	1.3308	−0.7716	0.096*
C74	0.4701 (4)	1.3659 (5)	−0.7627 (3)	0.0633 (19)
H74A	0.4803	1.4078	−0.8068	0.095*
H74B	0.4833	1.2973	−0.7651	0.095*
H74C	0.5155	1.3694	−0.7389	0.095*
C75	0.3410 (6)	1.5083 (5)	−0.7236 (3)	0.068 (2)
H75A	0.3500	1.5506	−0.7676	0.103*
H75B	0.3862	1.5128	−0.7000	0.103*
H75C	0.2723	1.5303	−0.7007	0.103*
C76	0.4344 (3)	1.3023 (4)	−0.5027 (2)	0.0282 (10)
C77	0.5183 (4)	1.2092 (4)	−0.4826 (2)	0.0392 (12)
H77A	0.5507	1.2219	−0.4540	0.059*
H77B	0.5672	1.1934	−0.5215	0.059*
H77C	0.4902	1.1532	−0.4594	0.059*
C78	0.3590 (4)	1.3368 (4)	−0.4431 (2)	0.0410 (12)
H78A	0.3942	1.3480	−0.4155	0.062*
H78B	0.3251	1.2856	−0.4181	0.062*
H78C	0.3101	1.3985	−0.4580	0.062*
C79	0.4866 (4)	1.3865 (4)	−0.5365 (3)	0.0435 (13)
H79A	0.5183	1.3952	−0.5058	0.065*
H79B	0.4374	1.4484	−0.5506	0.065*
H79C	0.5371	1.3689	−0.5744	0.065*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cs1	0.03140 (17)	0.02770 (17)	0.03594 (18)	−0.00039 (13)	0.00625 (13)	−0.00522 (13)
Cs2	0.02675 (17)	0.03255 (18)	0.03943 (19)	0.00065 (13)	−0.00231 (13)	−0.01078 (14)
Cs3	0.02394 (16)	0.02736 (17)	0.03519 (18)	−0.00266 (12)	0.00235 (12)	−0.00632 (13)
Cs4	0.02658 (17)	0.03339 (18)	0.03916 (19)	−0.00056 (13)	−0.00228 (13)	−0.01194 (14)
P1	0.0336 (7)	0.0399 (7)	0.0246 (6)	−0.0114 (6)	−0.0081 (5)	−0.0001 (5)
P2	0.0341 (6)	0.0301 (7)	0.0392 (7)	−0.0187 (6)	−0.0089 (5)	0.0018 (5)
P3	0.0351 (7)	0.0286 (7)	0.0390 (7)	−0.0182 (6)	−0.0116 (6)	0.0012 (6)
P4	0.0331 (7)	0.0417 (7)	0.0299 (6)	−0.0141 (6)	−0.0062 (5)	0.0027 (6)
C1	0.019 (2)	0.025 (2)	0.022 (2)	−0.0004 (17)	−0.0045 (16)	−0.0057 (18)
C2	0.0165 (19)	0.029 (2)	0.026 (2)	−0.0013 (18)	−0.0038 (17)	−0.0126 (19)
C3	0.0173 (19)	0.027 (2)	0.029 (2)	−0.0068 (17)	−0.0014 (17)	−0.0076 (19)
C4	0.0174 (19)	0.029 (2)	0.022 (2)	−0.0033 (18)	0.0000 (16)	−0.0093 (19)
C5	0.0184 (19)	0.029 (2)	0.024 (2)	−0.0030 (17)	−0.0038 (16)	−0.0105 (18)
C6	0.0148 (19)	0.028 (2)	0.030 (2)	−0.0061 (17)	0.0014 (17)	−0.0104 (19)
C7	0.026 (2)	0.040 (3)	0.033 (2)	−0.010 (2)	−0.0058 (19)	−0.014 (2)
C8	0.055 (3)	0.053 (3)	0.046 (3)	−0.030 (3)	−0.016 (3)	−0.013 (3)
C9	0.042 (3)	0.067 (4)	0.046 (3)	−0.008 (3)	−0.007 (2)	−0.039 (3)
C10	0.028 (2)	0.062 (4)	0.037 (3)	−0.012 (2)	−0.013 (2)	−0.015 (3)
C11	0.019 (2)	0.028 (2)	0.026 (2)	−0.0044 (18)	−0.0008 (17)	−0.0074 (19)
C12	0.047 (3)	0.073 (4)	0.026 (2)	−0.027 (3)	−0.015 (2)	0.000 (3)
C13	0.029 (3)	0.059 (4)	0.030 (3)	−0.003 (2)	0.001 (2)	0.005 (3)
C14	0.068 (4)	0.035 (3)	0.042 (3)	−0.009 (3)	−0.023 (3)	−0.002 (2)
C15	0.027 (2)	0.035 (3)	0.032 (2)	−0.012 (2)	−0.0022 (19)	−0.011 (2)
C16	0.061 (4)	0.034 (3)	0.068 (4)	−0.020 (3)	−0.018 (3)	−0.010 (3)
C17	0.053 (3)	0.053 (3)	0.045 (3)	−0.033 (3)	−0.007 (3)	−0.012 (3)
C18	0.031 (3)	0.068 (4)	0.042 (3)	−0.027 (3)	0.005 (2)	−0.015 (3)
C19	0.0143 (19)	0.027 (2)	0.025 (2)	−0.0039 (17)	0.0008 (16)	−0.0079 (18)
C20	0.0181 (19)	0.020 (2)	0.019 (2)	−0.0016 (16)	0.0022 (16)	−0.0072 (17)
C21	0.021 (2)	0.029 (2)	0.024 (2)	−0.0045 (18)	−0.0040 (17)	−0.0133 (18)
C22	0.0171 (19)	0.024 (2)	0.025 (2)	−0.0092 (17)	−0.0013 (16)	−0.0086 (18)
C23	0.022 (2)	0.022 (2)	0.022 (2)	−0.0053 (17)	−0.0068 (17)	−0.0030 (17)
C24	0.0176 (19)	0.026 (2)	0.025 (2)	−0.0055 (17)	−0.0034 (16)	−0.0111 (18)
C25	0.037 (3)	0.034 (3)	0.021 (2)	−0.013 (2)	−0.0010 (19)	−0.0028 (19)
C26	0.049 (3)	0.084 (5)	0.028 (3)	−0.026 (3)	0.011 (2)	−0.007 (3)
C27	0.073 (4)	0.059 (4)	0.022 (2)	−0.032 (3)	−0.010 (2)	−0.003 (2)
C28	0.085 (5)	0.039 (3)	0.042 (3)	−0.014 (3)	−0.029 (3)	0.002 (3)
C29	0.026 (2)	0.021 (2)	0.023 (2)	−0.0123 (18)	−0.0065 (17)	−0.0026 (17)
C30	0.033 (2)	0.038 (3)	0.040 (3)	−0.021 (2)	−0.014 (2)	−0.006 (2)
C31	0.025 (2)	0.038 (3)	0.032 (2)	−0.017 (2)	0.0012 (19)	−0.005 (2)
C32	0.028 (2)	0.026 (2)	0.037 (3)	−0.0120 (19)	−0.0015 (19)	−0.009 (2)
C33	0.021 (2)	0.039 (3)	0.029 (2)	−0.0153 (19)	−0.0001 (18)	−0.015 (2)
C34	0.042 (3)	0.069 (4)	0.027 (2)	−0.029 (3)	−0.008 (2)	−0.010 (2)
C35	0.045 (3)	0.059 (4)	0.058 (3)	−0.021 (3)	−0.002 (3)	−0.038 (3)
C36	0.019 (2)	0.052 (3)	0.045 (3)	−0.013 (2)	−0.008 (2)	−0.013 (2)
C37	0.047 (3)	0.070 (4)	0.051 (3)	−0.010 (3)	−0.013 (3)	−0.022 (3)
C38	0.052 (4)	0.077 (4)	0.050 (3)	−0.036 (3)	0.004 (3)	−0.030 (3)
C39	0.057 (3)	0.048 (3)	0.036 (3)	−0.028 (3)	0.004 (2)	−0.014 (3)
C40	0.050 (3)	0.043 (3)	0.023 (2)	−0.020 (2)	−0.005 (2)	−0.017 (2)
C41	0.056 (3)	0.040 (3)	0.035 (3)	−0.022 (3)	−0.005 (2)	−0.012 (2)
C42	0.067 (4)	0.047 (3)	0.032 (3)	−0.013 (3)	−0.015 (3)	−0.009 (2)
C43	0.055 (3)	0.050 (3)	0.034 (3)	−0.022 (3)	−0.009 (2)	−0.007 (2)
C44	0.0140 (18)	0.019 (2)	0.033 (2)	−0.0018 (16)	−0.0036 (17)	−0.0074 (18)
C45	0.0198 (19)	0.020 (2)	0.023 (2)	−0.0060 (17)	−0.0007 (16)	−0.0054 (17)
C46	0.0185 (19)	0.023 (2)	0.023 (2)	−0.0054 (17)	−0.0023 (16)	−0.0099 (18)
C47	0.0171 (19)	0.024 (2)	0.023 (2)	−0.0064 (17)	0.0001 (16)	−0.0062 (18)
C48	0.021 (2)	0.027 (2)	0.025 (2)	−0.0053 (18)	−0.0019 (17)	−0.0085 (19)
C49	0.0178 (19)	0.024 (2)	0.026 (2)	−0.0037 (17)	−0.0030 (17)	−0.0093 (18)
C50	0.031 (2)	0.032 (2)	0.022 (2)	−0.012 (2)	0.0007 (18)	−0.0074 (19)
C51	0.080 (4)	0.045 (3)	0.025 (2)	−0.032 (3)	−0.002 (3)	−0.012 (2)
C52	0.037 (3)	0.060 (4)	0.031 (3)	−0.011 (3)	0.013 (2)	−0.005 (3)
C53	0.062 (4)	0.038 (3)	0.044 (3)	−0.016 (3)	−0.030 (3)	0.000 (2)
C54	0.023 (2)	0.028 (2)	0.024 (2)	−0.0111 (19)	−0.0016 (17)	−0.0034 (18)
C55	0.043 (3)	0.055 (3)	0.041 (3)	−0.035 (3)	−0.012 (2)	−0.001 (2)
C56	0.029 (2)	0.041 (3)	0.036 (3)	−0.018 (2)	0.008 (2)	−0.012 (2)
C57	0.035 (3)	0.027 (3)	0.046 (3)	−0.007 (2)	0.004 (2)	−0.010 (2)
C58	0.027 (2)	0.046 (3)	0.031 (2)	−0.016 (2)	0.0011 (19)	−0.020 (2)
C59	0.032 (3)	0.063 (4)	0.068 (4)	−0.015 (3)	0.002 (3)	−0.043 (3)
C60	0.026 (2)	0.041 (3)	0.040 (3)	−0.012 (2)	−0.008 (2)	−0.015 (2)
C61	0.059 (4)	0.090 (5)	0.029 (3)	−0.049 (4)	−0.010 (2)	−0.007 (3)
C62	0.0160 (19)	0.024 (2)	0.025 (2)	0.0016 (17)	−0.0013 (16)	−0.0084 (18)
C63	0.0147 (19)	0.027 (2)	0.033 (2)	−0.0018 (17)	0.0005 (17)	−0.009 (2)
C64	0.019 (2)	0.032 (2)	0.028 (2)	−0.0053 (18)	−0.0048 (17)	−0.0129 (19)
C65	0.021 (2)	0.031 (2)	0.022 (2)	−0.0060 (18)	−0.0026 (17)	−0.0073 (19)
C66	0.018 (2)	0.035 (2)	0.025 (2)	−0.0081 (19)	−0.0015 (17)	−0.008 (2)
C67	0.0148 (19)	0.035 (2)	0.026 (2)	−0.0029 (18)	0.0000 (17)	−0.014 (2)
C68	0.033 (2)	0.037 (3)	0.041 (3)	−0.016 (2)	−0.008 (2)	−0.006 (2)
C69	0.057 (4)	0.035 (3)	0.078 (4)	−0.017 (3)	−0.022 (3)	−0.006 (3)
C70	0.026 (3)	0.068 (4)	0.057 (4)	−0.023 (3)	0.004 (2)	−0.011 (3)
C71	0.043 (3)	0.061 (4)	0.064 (4)	−0.030 (3)	−0.011 (3)	−0.022 (3)
C72	0.027 (2)	0.041 (3)	0.019 (2)	−0.012 (2)	−0.0038 (18)	−0.001 (2)
C73	0.065 (4)	0.105 (6)	0.028 (3)	−0.042 (4)	−0.014 (3)	0.001 (3)
C74	0.046 (3)	0.072 (4)	0.041 (3)	−0.008 (3)	0.005 (3)	0.009 (3)
C75	0.108 (6)	0.043 (4)	0.043 (4)	−0.015 (4)	−0.018 (4)	0.001 (3)
C76	0.027 (2)	0.039 (3)	0.026 (2)	−0.007 (2)	−0.0087 (18)	−0.016 (2)
C77	0.026 (2)	0.052 (3)	0.038 (3)	−0.002 (2)	−0.012 (2)	−0.012 (2)
C78	0.032 (3)	0.058 (3)	0.034 (3)	−0.002 (2)	−0.005 (2)	−0.025 (3)
C79	0.040 (3)	0.056 (3)	0.047 (3)	−0.020 (3)	−0.016 (2)	−0.014 (3)

Geometric parameters (Å, º)

Cs1—C44^i	3.332 (4)	C19—C20	1.434 (6)
Cs1—C46^i	3.366 (4)	C19—C24	1.443 (6)
Cs1—C45^i	3.370 (4)	C19—Cs3^i	3.282 (4)
Cs1—C47^i	3.389 (4)	C20—C21	1.405 (6)
Cs1—C48^i	3.488 (4)	C20—C25	1.557 (6)
Cs1—C49^i	3.505 (4)	C20—Cs3^i	3.408 (4)
Cs1—P2	3.5360 (13)	C21—C22	1.390 (6)
Cs1—P1	3.7653 (13)	C21—Cs3^i	3.447 (4)
Cs1—P3^i	4.0736 (12)	C22—C23	1.388 (6)
Cs1—Cs3^i	4.7772 (4)	C22—C29	1.532 (5)
Cs1—Cs2	5.4902 (4)	C22—Cs3^i	3.439 (4)
Cs2—C2^ii	3.474 (4)	C23—C24	1.399 (6)
Cs2—C1^ii	3.479 (4)	C23—Cs3^i	3.460 (4)
Cs2—C3^ii	3.489 (4)	C24—C33	1.552 (6)
Cs2—C6^ii	3.504 (4)	C24—Cs3^i	3.415 (4)
Cs2—C5^ii	3.510 (4)	C25—C28	1.519 (7)
Cs2—C4^ii	3.541 (4)	C25—C27	1.534 (7)
Cs2—P1	3.5818 (14)	C25—C26	1.535 (7)
Cs2—C37	3.629 (6)	C29—C32	1.527 (6)
Cs2—C38	3.780 (6)	C29—C31	1.542 (6)
Cs2—P2	3.8692 (13)	C29—C30	1.545 (6)
Cs2—Cs2^ii	5.4810 (6)	C33—C34	1.530 (7)
Cs3—C19^iii	3.282 (4)	C33—C36	1.546 (6)
Cs3—C20^iii	3.408 (4)	C33—C35	1.547 (7)
Cs3—C24^iii	3.415 (4)	C37—C42	1.375 (8)
Cs3—C22^iii	3.439 (4)	C37—C38	1.378 (9)
Cs3—C21^iii	3.447 (4)	C38—C39	1.389 (9)
Cs3—C23^iii	3.460 (4)	C39—C40	1.397 (7)
Cs3—P3	3.5832 (13)	C40—C41	1.389 (7)
Cs3—P4	3.7643 (13)	C40—C43	1.491 (8)
Cs3—C43	3.811 (6)	C41—C42	1.392 (8)
Cs3—P2^iii	3.9920 (13)	C44—C45	1.442 (6)
Cs3—Cs1^iii	4.7772 (4)	C44—C49	1.447 (6)
Cs3—Cs4	5.5610 (4)	C44—Cs1^iii	3.332 (4)
Cs4—C62^iv	3.461 (4)	C45—C46	1.407 (5)
Cs4—C67^iv	3.476 (4)	C45—C50	1.557 (6)
Cs4—C63^iv	3.500 (4)	C45—Cs1^iii	3.369 (4)
Cs4—C66^iv	3.541 (5)	C46—C47	1.393 (6)
Cs4—C64^iv	3.556 (4)	C46—Cs1^iii	3.366 (4)
Cs4—P4	3.5925 (14)	C47—C48	1.391 (6)
Cs4—C65^iv	3.611 (5)	C47—C54	1.541 (5)
Cs4—C40	3.682 (5)	C47—Cs1^iii	3.389 (4)
Cs4—C41	3.772 (5)	C48—C49	1.387 (6)
Cs4—P3	3.8543 (12)	C48—Cs1^iii	3.488 (4)
Cs4—C39	3.857 (5)	C49—C58	1.547 (6)
Cs4—C77^iv	3.920 (5)	C49—Cs1^iii	3.505 (4)
P1—H1	1.37 (8)	C50—C53	1.533 (7)
P1—C1	1.831 (4)	C50—C51	1.536 (7)
P2—H2	1.42 (6)	C50—C52	1.544 (6)
P2—C19	1.839 (4)	C54—C57	1.527 (6)
P2—Cs3^i	3.9920 (13)	C54—C55	1.531 (6)
P3—H3	1.37 (5)	C54—C56	1.531 (6)
P3—C44	1.828 (4)	C58—C61	1.539 (7)
P3—Cs1^iii	4.0737 (12)	C58—C60	1.552 (6)
P4—H4	1.29 (7)	C58—C59	1.557 (7)
P4—C62	1.836 (4)	C62—C63	1.441 (6)
C1—C6	1.426 (6)	C62—C67	1.449 (6)
C1—C2	1.467 (6)	C62—Cs4^iv	3.460 (4)
C1—Cs2^ii	3.479 (4)	C63—C64	1.401 (6)
C2—C3	1.375 (6)	C63—C68	1.559 (6)
C2—C7	1.541 (6)	C63—Cs4^iv	3.500 (4)
C2—Cs2^ii	3.474 (4)	C64—C65	1.377 (6)
C3—C4	1.390 (6)	C64—Cs4^iv	3.556 (4)
C3—Cs2^ii	3.489 (4)	C65—C66	1.384 (6)
C4—C5	1.383 (6)	C65—C72	1.547 (6)
C4—C11	1.538 (6)	C65—Cs4^iv	3.611 (5)
C4—Cs2^ii	3.541 (4)	C66—C67	1.390 (6)
C5—C6	1.403 (6)	C66—Cs4^iv	3.541 (5)
C5—Cs2^ii	3.510 (4)	C67—C76	1.558 (6)
C6—C15	1.580 (6)	C67—Cs4^iv	3.476 (4)
C6—Cs2^ii	3.504 (4)	C68—C69	1.535 (8)
C7—C10	1.531 (7)	C68—C71	1.547 (8)
C7—C9	1.545 (7)	C68—C70	1.563 (7)
C7—C8	1.564 (6)	C72—C73	1.510 (7)
C11—C12	1.507 (7)	C72—C75	1.510 (8)
C11—C14	1.526 (7)	C72—C74	1.522 (7)
C11—C13	1.532 (6)	C76—C77	1.546 (7)
C15—C17	1.523 (7)	C76—C78	1.551 (6)
C15—C16	1.528 (7)	C76—C79	1.557 (6)
C15—C18	1.554 (7)	C77—Cs4^iv	3.919 (5)
C44^i—Cs1—C46^i	43.12 (10)	C40—Cs4—C77^iv	161.35 (11)
C44^i—Cs1—C45^i	24.85 (10)	C41—Cs4—C77^iv	169.10 (11)
C46^i—Cs1—C45^i	24.11 (9)	P3—Cs4—C77^iv	104.60 (7)
C44^i—Cs1—C47^i	50.81 (9)	C39—Cs4—C77^iv	152.78 (11)
C46^i—Cs1—C47^i	23.79 (10)	H1—P1—C1	99 (3)
C45^i—Cs1—C47^i	42.76 (9)	H1—P1—Cs2	99 (3)
C44^i—Cs1—C48^i	42.07 (10)	C1—P1—Cs2	129.32 (15)
C46^i—Cs1—C48^i	40.27 (10)	H1—P1—Cs1	104 (3)
C45^i—Cs1—C48^i	47.83 (10)	C1—P1—Cs1	123.61 (14)
C47^i—Cs1—C48^i	23.28 (10)	Cs2—P1—Cs1	96.68 (3)
C44^i—Cs1—C49^i	24.27 (10)	H2—P2—C19	100 (2)
C46^i—Cs1—C49^i	47.71 (10)	H2—P2—Cs1	101 (2)
C45^i—Cs1—C49^i	41.70 (10)	C19—P2—Cs1	128.76 (14)
C47^i—Cs1—C49^i	41.61 (9)	H2—P2—Cs2	100 (2)
C48^i—Cs1—C49^i	22.88 (9)	C19—P2—Cs2	125.18 (14)
C44^i—Cs1—P2	127.08 (7)	Cs1—P2—Cs2	95.60 (3)
C46^i—Cs1—P2	143.79 (7)	H2—P2—Cs3^i	93 (2)
C45^i—Cs1—P2	128.47 (7)	C19—P2—Cs3^i	54.40 (13)
C47^i—Cs1—P2	166.74 (8)	Cs1—P2—Cs3^i	78.52 (3)
C48^i—Cs1—P2	165.37 (7)	Cs2—P2—Cs3^i	166.36 (4)
C49^i—Cs1—P2	142.95 (7)	H3—P3—C44	105 (2)
C44^i—Cs1—P1	146.55 (7)	H3—P3—Cs3	95 (2)
C46^i—Cs1—P1	117.62 (7)	C44—P3—Cs3	127.41 (14)
C45^i—Cs1—P1	141.61 (7)	H3—P3—Cs4	96 (2)
C47^i—Cs1—P1	100.52 (7)	C44—P3—Cs4	128.00 (14)
C48^i—Cs1—P1	104.61 (7)	Cs3—P3—Cs4	96.72 (3)
C49^i—Cs1—P1	123.32 (7)	H3—P3—Cs1^iii	95 (2)
P2—Cs1—P1	84.91 (3)	C44—P3—Cs1^iii	53.63 (13)
C44^i—Cs1—P3^i	26.22 (7)	Cs3—P3—Cs1^iii	76.91 (2)
C46^i—Cs1—P3^i	66.35 (7)	Cs4—P3—Cs1^iii	168.03 (4)
C45^i—Cs1—P3^i	43.32 (7)	H4—P4—C62	108 (3)
C47^i—Cs1—P3^i	77.02 (7)	H4—P4—Cs4	75 (3)
C48^i—Cs1—P3^i	66.09 (7)	C62—P4—Cs4	134.98 (14)
C49^i—Cs1—P3^i	44.33 (7)	H4—P4—Cs3	102 (3)
P2—Cs1—P3^i	101.55 (3)	C62—P4—Cs3	123.79 (14)
P1—Cs1—P3^i	161.69 (3)	Cs4—P4—Cs3	98.18 (3)
C44^i—Cs1—Cs3^i	72.10 (7)	C6—C1—C2	115.8 (4)
C46^i—Cs1—Cs3^i	102.53 (7)	C6—C1—P1	119.5 (3)
C45^i—Cs1—Cs3^i	79.26 (7)	C2—C1—P1	124.6 (3)
C47^i—Cs1—Cs3^i	120.93 (6)	C6—C1—Cs2^ii	79.2 (2)
C48^i—Cs1—Cs3^i	113.02 (7)	C2—C1—Cs2^ii	77.6 (2)
C49^i—Cs1—Cs3^i	90.82 (7)	P1—C1—Cs2^ii	112.43 (18)
P2—Cs1—Cs3^i	54.98 (2)	C3—C2—C1	119.5 (4)
P1—Cs1—Cs3^i	138.53 (2)	C3—C2—C7	116.3 (4)
P3^i—Cs1—Cs3^i	46.935 (18)	C1—C2—C7	124.1 (4)
C44^i—Cs1—Cs2	167.75 (7)	C3—C2—Cs2^ii	79.2 (3)
C46^i—Cs1—Cs2	149.08 (7)	C1—C2—Cs2^ii	78.0 (2)
C45^i—Cs1—Cs2	163.89 (7)	C7—C2—Cs2^ii	111.1 (3)
C47^i—Cs1—Cs2	139.89 (6)	C2—C3—C4	124.7 (4)
C48^i—Cs1—Cs2	143.50 (7)	C2—C3—Cs2^ii	78.0 (3)
C49^i—Cs1—Cs2	154.18 (7)	C4—C3—Cs2^ii	80.7 (3)
P2—Cs1—Cs2	44.54 (2)	C5—C4—C3	115.8 (4)
P1—Cs1—Cs2	40.39 (2)	C5—C4—C11	123.4 (4)
P3^i—Cs1—Cs2	142.568 (19)	C3—C4—C11	120.8 (4)
Cs3^i—Cs1—Cs2	98.732 (7)	C5—C4—Cs2^ii	77.4 (3)
C2^ii—Cs2—C1^ii	24.36 (10)	C3—C4—Cs2^ii	76.5 (3)
C2^ii—Cs2—C3^ii	22.77 (10)	C11—C4—Cs2^ii	113.8 (3)
C1^ii—Cs2—C3^ii	41.27 (9)	C4—C5—C6	123.7 (4)
C2^ii—Cs2—C6^ii	41.14 (10)	C4—C5—Cs2^ii	79.9 (2)
C1^ii—Cs2—C6^ii	23.57 (10)	C6—C5—Cs2^ii	78.2 (2)
C3^ii—Cs2—C6^ii	46.63 (10)	C5—C6—C1	120.4 (4)
C2^ii—Cs2—C5^ii	46.86 (10)	C5—C6—C15	115.6 (4)
C1^ii—Cs2—C5^ii	41.12 (10)	C1—C6—C15	124.0 (4)
C3^ii—Cs2—C5^ii	39.21 (10)	C5—C6—Cs2^ii	78.7 (2)
C6^ii—Cs2—C5^ii	23.07 (10)	C1—C6—Cs2^ii	77.2 (2)
C2^ii—Cs2—C4^ii	40.86 (10)	C15—C6—Cs2^ii	115.2 (3)
C1^ii—Cs2—C4^ii	48.66 (10)	C10—C7—C2	110.9 (4)
C3^ii—Cs2—C4^ii	22.79 (10)	C10—C7—C9	113.2 (4)
C6^ii—Cs2—C4^ii	40.81 (10)	C2—C7—C9	111.5 (4)
C5^ii—Cs2—C4^ii	22.61 (9)	C10—C7—C8	103.7 (4)
C2^ii—Cs2—P1	131.81 (8)	C2—C7—C8	112.8 (4)
C1^ii—Cs2—P1	117.28 (7)	C9—C7—C8	104.3 (4)
C3^ii—Cs2—P1	154.46 (8)	C12—C11—C14	108.5 (4)
C6^ii—Cs2—P1	121.77 (7)	C12—C11—C13	107.5 (4)
C5^ii—Cs2—P1	140.38 (7)	C14—C11—C13	109.7 (4)
C4^ii—Cs2—P1	162.41 (7)	C12—C11—C4	113.1 (4)
C2^ii—Cs2—C37	149.38 (12)	C14—C11—C4	109.2 (4)
C1^ii—Cs2—C37	133.18 (12)	C13—C11—C4	108.8 (4)
C3^ii—Cs2—C37	134.49 (13)	C17—C15—C16	105.3 (4)
C6^ii—Cs2—C37	110.94 (12)	C17—C15—C18	106.1 (4)
C5^ii—Cs2—C37	102.55 (12)	C16—C15—C18	113.0 (4)
C4^ii—Cs2—C37	112.08 (13)	C17—C15—C6	113.0 (4)
P1—Cs2—C37	68.36 (11)	C16—C15—C6	111.4 (4)
C2^ii—Cs2—C38	135.72 (13)	C18—C15—C6	108.1 (4)
C1^ii—Cs2—C38	130.38 (12)	C20—C19—C24	116.5 (4)
C3^ii—Cs2—C38	115.93 (13)	C20—C19—P2	118.9 (3)
C6^ii—Cs2—C38	106.92 (12)	C24—C19—P2	124.3 (3)
C5^ii—Cs2—C38	91.56 (13)	C20—C19—Cs3^i	82.6 (2)
C4^ii—Cs2—C38	95.05 (13)	C24—C19—Cs3^i	82.8 (2)
P1—Cs2—C38	88.51 (11)	P2—C19—Cs3^i	98.49 (17)
C37—Cs2—C38	21.31 (14)	C21—C20—C19	119.7 (4)
C2^ii—Cs2—P2	126.84 (7)	C21—C20—C25	115.6 (4)
C1^ii—Cs2—P2	151.18 (7)	C19—C20—C25	124.6 (4)
C3^ii—Cs2—P2	112.89 (7)	C21—C20—Cs3^i	79.7 (2)
C6^ii—Cs2—P2	155.03 (7)	C19—C20—Cs3^i	72.7 (2)
C5^ii—Cs2—P2	132.69 (7)	C25—C20—Cs3^i	116.8 (3)
C4^ii—Cs2—P2	114.40 (7)	C22—C21—C20	123.3 (4)
P1—Cs2—P2	82.79 (3)	C22—C21—Cs3^i	78.0 (3)
C37—Cs2—P2	71.80 (10)	C20—C21—Cs3^i	76.6 (2)
C38—Cs2—P2	66.12 (9)	C23—C22—C21	116.0 (4)
C2^ii—Cs2—Cs2^ii	79.05 (7)	C23—C22—C29	120.7 (4)
C1^ii—Cs2—Cs2^ii	62.43 (7)	C21—C22—C29	123.1 (4)
C3^ii—Cs2—Cs2^ii	101.32 (7)	C23—C22—Cs3^i	79.3 (3)
C6^ii—Cs2—Cs2^ii	72.70 (7)	C21—C22—Cs3^i	78.7 (3)
C5^ii—Cs2—Cs2^ii	95.69 (7)	C29—C22—Cs3^i	115.3 (3)
C4^ii—Cs2—Cs2^ii	110.55 (7)	C22—C23—C24	124.0 (4)
P1—Cs2—Cs2^ii	54.95 (2)	C22—C23—Cs3^i	77.5 (3)
C37—Cs2—Cs2^ii	107.54 (10)	C24—C23—Cs3^i	76.5 (2)
C38—Cs2—Cs2^ii	127.42 (9)	C23—C24—C19	119.1 (4)
P2—Cs2—Cs2^ii	131.30 (2)	C23—C24—C33	115.3 (4)
C2^ii—Cs2—Cs1	146.53 (7)	C19—C24—C33	125.5 (4)
C1^ii—Cs2—Cs1	153.19 (7)	C23—C24—Cs3^i	80.1 (2)
C3^ii—Cs2—Cs1	147.66 (7)	C19—C24—Cs3^i	72.4 (2)
C6^ii—Cs2—Cs1	164.46 (7)	C33—C24—Cs3^i	117.7 (3)
C5^ii—Cs2—Cs1	165.18 (7)	C28—C25—C27	105.9 (5)
C4^ii—Cs2—Cs1	154.19 (7)	C28—C25—C26	110.6 (4)
P1—Cs2—Cs1	42.93 (2)	C27—C25—C26	105.0 (5)
C37—Cs2—Cs1	63.94 (10)	C28—C25—C20	111.6 (4)
C38—Cs2—Cs1	73.68 (10)	C27—C25—C20	112.2 (4)
P2—Cs2—Cs1	39.87 (2)	C26—C25—C20	111.2 (4)
Cs2^ii—Cs2—Cs1	94.405 (8)	C32—C29—C22	109.0 (3)
C19^iii—Cs3—C20^iii	24.65 (10)	C32—C29—C31	109.9 (4)
C19^iii—Cs3—C24^iii	24.79 (10)	C22—C29—C31	110.0 (3)
C20^iii—Cs3—C24^iii	42.01 (10)	C32—C29—C30	109.1 (4)
C19^iii—Cs3—C22^iii	50.69 (10)	C22—C29—C30	111.2 (3)
C20^iii—Cs3—C22^iii	42.10 (9)	C31—C29—C30	107.6 (4)
C24^iii—Cs3—C22^iii	42.08 (9)	C34—C33—C36	104.2 (4)
C19^iii—Cs3—C21^iii	42.71 (10)	C34—C33—C35	106.5 (4)
C20^iii—Cs3—C21^iii	23.65 (9)	C36—C33—C35	112.8 (4)
C24^iii—Cs3—C21^iii	47.90 (10)	C34—C33—C24	112.3 (4)
C22^iii—Cs3—C21^iii	23.28 (10)	C36—C33—C24	110.8 (4)
C19^iii—Cs3—C23^iii	42.53 (10)	C35—C33—C24	110.2 (4)
C20^iii—Cs3—C23^iii	47.64 (10)	C42—C37—C38	118.9 (6)
C24^iii—Cs3—C23^iii	23.47 (9)	C42—C37—Cs2	94.3 (4)
C22^iii—Cs3—C23^iii	23.21 (10)	C38—C37—Cs2	85.6 (4)
C21^iii—Cs3—C23^iii	39.88 (10)	C37—C38—C39	121.1 (5)
C19^iii—Cs3—P3	125.53 (8)	C37—C38—Cs2	73.1 (4)
C20^iii—Cs3—P3	119.28 (7)	C39—C38—Cs2	101.0 (4)
C24^iii—Cs3—P3	147.70 (7)	C38—C39—C40	120.6 (5)
C22^iii—Cs3—P3	150.11 (7)	C38—C39—Cs4	91.6 (4)
C21^iii—Cs3—P3	129.38 (7)	C40—C39—Cs4	72.3 (3)
C23^iii—Cs3—P3	166.84 (7)	C41—C40—C39	117.5 (5)
C19^iii—Cs3—P4	150.34 (8)	C41—C40—C43	121.3 (4)
C20^iii—Cs3—P4	138.94 (7)	C39—C40—C43	121.2 (5)
C24^iii—Cs3—P4	128.72 (7)	C41—C40—Cs4	82.9 (3)
C22^iii—Cs3—P4	101.13 (7)	C39—C40—Cs4	86.5 (3)
C21^iii—Cs3—P4	115.39 (7)	C43—C40—Cs4	98.8 (3)
C23^iii—Cs3—P4	108.06 (7)	C40—C41—C42	121.5 (5)
P3—Cs3—P4	83.16 (3)	C40—C41—Cs4	75.6 (3)
C19^iii—Cs3—C43	121.87 (12)	C42—C41—Cs4	91.8 (3)
C20^iii—Cs3—C43	97.32 (11)	C37—C42—C41	120.3 (5)
C24^iii—Cs3—C43	132.65 (11)	C40—C43—Cs3	147.9 (4)
C22^iii—Cs3—C43	93.15 (11)	C45—C44—C49	116.0 (3)
C21^iii—Cs3—C43	85.03 (11)	C45—C44—P3	119.0 (3)
C23^iii—Cs3—C43	116.04 (11)	C49—C44—P3	124.8 (3)
P3—Cs3—C43	62.90 (9)	C45—C44—Cs1^iii	79.0 (2)
P4—Cs3—C43	60.71 (8)	C49—C44—Cs1^iii	84.6 (2)
C19^iii—Cs3—P2^iii	27.11 (8)	P3—C44—Cs1^iii	100.15 (16)
C20^iii—Cs3—P2^iii	44.02 (7)	C46—C45—C44	119.5 (4)
C24^iii—Cs3—P2^iii	45.42 (7)	C46—C45—C50	116.7 (4)
C22^iii—Cs3—P2^iii	77.77 (7)	C44—C45—C50	123.7 (3)
C21^iii—Cs3—P2^iii	66.72 (7)	C46—C45—Cs1^iii	77.8 (2)
C23^iii—Cs3—P2^iii	67.52 (7)	C44—C45—Cs1^iii	76.1 (2)
P3—Cs3—P2^iii	102.29 (3)	C50—C45—Cs1^iii	114.9 (3)
P4—Cs3—P2^iii	171.00 (3)	C47—C46—C45	123.3 (4)
C43—Cs3—P2^iii	128.12 (8)	C47—C46—Cs1^iii	79.0 (3)
C19^iii—Cs3—Cs1^iii	72.24 (7)	C45—C46—Cs1^iii	78.1 (2)
C20^iii—Cs3—Cs1^iii	78.81 (7)	C48—C47—C46	116.1 (4)
C24^iii—Cs3—Cs1^iii	91.64 (7)	C48—C47—C54	120.9 (4)
C22^iii—Cs3—Cs1^iii	120.25 (6)	C46—C47—C54	122.8 (4)
C21^iii—Cs3—Cs1^iii	101.40 (7)	C48—C47—Cs1^iii	82.3 (3)
C23^iii—Cs3—Cs1^iii	114.00 (7)	C46—C47—Cs1^iii	77.2 (2)
P3—Cs3—Cs1^iii	56.157 (19)	C54—C47—Cs1^iii	113.8 (3)
P4—Cs3—Cs1^iii	137.39 (2)	C49—C48—C47	123.9 (4)
C43—Cs3—Cs1^iii	104.42 (8)	C49—C48—Cs1^iii	79.3 (3)
P2^iii—Cs3—Cs1^iii	46.500 (19)	C47—C48—Cs1^iii	74.4 (3)
C19^iii—Cs3—Cs4	166.16 (8)	C48—C49—C44	119.8 (4)
C20^iii—Cs3—Cs4	144.81 (7)	C48—C49—C58	116.1 (4)
C24^iii—Cs3—Cs4	168.33 (7)	C44—C49—C58	124.0 (4)
C22^iii—Cs3—Cs4	132.30 (6)	C48—C49—Cs1^iii	77.9 (2)
C21^iii—Cs3—Cs4	132.80 (7)	C44—C49—Cs1^iii	71.2 (2)
C23^iii—Cs3—Cs4	146.76 (7)	C58—C49—Cs1^iii	123.5 (3)
P3—Cs3—Cs4	43.499 (19)	C53—C50—C51	105.4 (4)
P4—Cs3—Cs4	39.75 (2)	C53—C50—C52	110.6 (4)
C43—Cs3—Cs4	48.68 (9)	C51—C50—C52	105.6 (4)
P2^iii—Cs3—Cs4	145.61 (2)	C53—C50—C45	112.7 (4)
Cs1^iii—Cs3—Cs4	99.122 (7)	C51—C50—C45	111.7 (3)
C62^iv—Cs4—C67^iv	24.11 (10)	C52—C50—C45	110.4 (4)
C62^iv—Cs4—C63^iv	23.89 (11)	C57—C54—C55	109.2 (4)
C67^iv—Cs4—C63^iv	41.23 (10)	C57—C54—C56	110.0 (4)
C62^iv—Cs4—C66^iv	40.95 (9)	C55—C54—C56	107.2 (4)
C67^iv—Cs4—C66^iv	22.83 (10)	C57—C54—C47	109.0 (4)
C63^iv—Cs4—C66^iv	46.34 (10)	C55—C54—C47	110.8 (4)
C62^iv—Cs4—C64^iv	41.04 (10)	C56—C54—C47	110.6 (4)
C67^iv—Cs4—C64^iv	46.67 (10)	C61—C58—C49	112.5 (4)
C63^iv—Cs4—C64^iv	22.88 (10)	C61—C58—C60	104.1 (4)
C66^iv—Cs4—C64^iv	38.68 (10)	C49—C58—C60	110.8 (4)
C62^iv—Cs4—P4	113.41 (7)	C61—C58—C59	105.2 (5)
C67^iv—Cs4—P4	122.42 (8)	C49—C58—C59	112.2 (4)
C63^iv—Cs4—P4	124.29 (7)	C60—C58—C59	111.7 (4)
C66^iv—Cs4—P4	143.78 (8)	C63—C62—C67	116.4 (4)
C64^iv—Cs4—P4	146.25 (7)	C63—C62—P4	119.9 (3)
C62^iv—Cs4—C65^iv	48.00 (10)	C67—C62—P4	123.7 (3)
C67^iv—Cs4—C65^iv	40.42 (10)	C63—C62—Cs4^iv	79.6 (2)
C63^iv—Cs4—C65^iv	40.18 (10)	C67—C62—Cs4^iv	78.5 (2)
C66^iv—Cs4—C65^iv	22.28 (10)	P4—C62—Cs4^iv	111.40 (17)
C64^iv—Cs4—C65^iv	22.13 (9)	C64—C63—C62	120.0 (4)
P4—Cs4—C65^iv	161.32 (7)	C64—C63—C68	116.0 (4)
C62^iv—Cs4—C40	139.53 (11)	C62—C63—C68	124.0 (4)
C67^iv—Cs4—C40	157.52 (11)	C64—C63—Cs4^iv	80.8 (2)
C63^iv—Cs4—C40	117.92 (11)	C62—C63—Cs4^iv	76.5 (2)
C66^iv—Cs4—C40	142.04 (11)	C68—C63—Cs4^iv	112.8 (3)
C64^iv—Cs4—C40	110.96 (11)	C65—C64—C63	123.4 (4)
P4—Cs4—C40	73.92 (9)	C65—C64—Cs4^iv	81.2 (3)
C65^iv—Cs4—C40	120.46 (11)	C63—C64—Cs4^iv	76.3 (2)
C62^iv—Cs4—C41	136.16 (11)	C64—C65—C66	116.8 (4)
C67^iv—Cs4—C41	142.38 (12)	C64—C65—C72	122.3 (4)
C63^iv—Cs4—C41	112.27 (12)	C66—C65—C72	121.0 (4)
C66^iv—Cs4—C41	122.13 (11)	C64—C65—Cs4^iv	76.7 (3)
C64^iv—Cs4—C41	98.13 (11)	C66—C65—Cs4^iv	76.0 (3)
P4—Cs4—C41	94.07 (9)	C72—C65—Cs4^iv	115.4 (3)
C65^iv—Cs4—C41	102.09 (11)	C65—C66—C67	124.2 (4)
C40—Cs4—C41	21.44 (11)	C65—C66—Cs4^iv	81.7 (3)
C62^iv—Cs4—P3	148.28 (7)	C67—C66—Cs4^iv	76.0 (3)
C67^iv—Cs4—P3	124.19 (7)	C66—C67—C62	119.3 (4)
C63^iv—Cs4—P3	153.59 (7)	C66—C67—C76	116.0 (4)
C66^iv—Cs4—P3	110.82 (7)	C62—C67—C76	124.7 (4)
C64^iv—Cs4—P3	131.84 (7)	C66—C67—Cs4^iv	81.2 (3)
P4—Cs4—P3	81.77 (3)	C62—C67—Cs4^iv	77.3 (2)
C65^iv—Cs4—P3	113.45 (7)	C76—C67—Cs4^iv	111.0 (3)
C40—Cs4—P3	70.06 (8)	C69—C68—C71	105.5 (5)
C41—Cs4—P3	65.12 (8)	C69—C68—C63	112.7 (4)
C62^iv—Cs4—C39	119.79 (11)	C71—C68—C63	113.0 (4)
C67^iv—Cs4—C39	141.91 (11)	C69—C68—C70	112.1 (4)
C63^iv—Cs4—C39	100.73 (11)	C71—C68—C70	104.7 (4)
C66^iv—Cs4—C39	138.03 (12)	C63—C68—C70	108.7 (4)
C64^iv—Cs4—C39	100.20 (12)	C73—C72—C75	108.1 (5)
P4—Cs4—C39	72.27 (10)	C73—C72—C74	107.4 (5)
C65^iv—Cs4—C39	116.33 (12)	C75—C72—C74	110.6 (5)
C40—Cs4—C39	21.19 (10)	C73—C72—C65	112.6 (4)
C41—Cs4—C39	36.36 (11)	C75—C72—C65	109.5 (4)
P3—Cs4—C39	90.91 (8)	C74—C72—C65	108.6 (4)
C62^iv—Cs4—C77^iv	51.43 (10)	C77—C76—C78	112.2 (4)
C67^iv—Cs4—C77^iv	39.71 (10)	C77—C76—C79	105.0 (4)
C63^iv—Cs4—C77^iv	75.10 (10)	C78—C76—C79	104.9 (4)
C66^iv—Cs4—C77^iv	56.56 (10)	C77—C76—C67	110.2 (4)
C64^iv—Cs4—C77^iv	86.12 (10)	C78—C76—C67	111.4 (4)
P4—Cs4—C77^iv	87.73 (8)	C79—C76—C67	113.0 (4)
C65^iv—Cs4—C77^iv	78.18 (10)	C76—C77—Cs4^iv	93.0 (3)

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