Poly[diaqua­penta­kis(μ4-benzene-1,2-dicarboxyl­ato)(μ3-benzene-1,2-dicarboxyl­ato)tetra­thulium(III)]

Wang, G.-M.; Duan, C.-S.; Liu, H.-L.; Li, H.

doi:10.1107/S1600536808003620

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 3| March 2008| Pages m468-m469

doi:10.1107/S1600536808003620

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Poly[diaquapentakis(μ₄-benzene-1,2-dicarboxylato)(μ₃-benzene-1,2-dicarboxylato)tetrathulium(III)]

Guo-Ming Wang,^a ^* Chun-Sheng Duan,^a Hui-Luan Liu ^a and Hui Li ^a

^aDepartment of Chemistry, Teachers College of Qingdao University, Qingdao, Shandong 266071, People's Republic of China
^*Correspondence e-mail: gmwang_pub@163.com

(Received 12 September 2007; accepted 1 February 2008; online 13 February 2008)

The title compound, [Tm₄(C₈H₄O₄)₆(H₂O)₂]_n, has been synthesized hydrothermally. The asymmetric unit has four unique Tm^III ions that are six-, seven-, eight- and nine-coordinate. The cations are interconnected by bridging benzene-1,2-dicarboxylate (BDC) anions to form an infinite two-dimensional framework, in which the BDC ligands adopt three different coordination modes. Adjacent sheets are further packed to form a three-dimensional supramolecular framework through O—H⋯O hydrogen bonds.

Related literature

For background to the structures and applications of coordination polymers, see: Meares & Wensel, (1984 ); Scott & Horrocks, (1992 ); Reineke et al. (1999 ); Eddaoudi et al. (2001 ). For related structures involving multi-dimensional networks formed by multi-functional carboxylate ligands, see: Choi et al. (1998 ); MacGillivray et al. (1998 ); Evans et al. (1999 ); Chen et al. (2001 ); Suresh et al. (2001 ); Kumagai et al. (2002 ); Lu & Babb (2003 ); Song et al. (2003 ); Zhang et al. (2004 ); Wang et al. (2007 ).

Experimental

Crystal data

[Tm₄(C₈H₄O₄)₆(H₂O)₂]
M_r = 1696.42
Triclinic, $[P \overline 1]$
a = 12.5716 (4) Å
b = 13.7737 (2) Å
c = 15.8867 (3) Å
α = 75.301 (4)°
β = 69.112 (2)°
γ = 65.617 (2)°
V = 2322.45 (9) Å³
Z = 2
Mo Kα radiation
μ = 7.67 mm⁻¹
T = 295 (2) K
0.30 × 0.14 × 0.02 mm

Data collection

Bruker APEX area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.207, T_max = 0.862
18519 measured reflections
9421 independent reflections
8260 reflections with I > 2σ(I)
R_int = 0.044

Refinement

R[F² > 2σ(F²)] = 0.042
wR(F²) = 0.108
S = 1.02
9421 reflections
715 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 2.34 e Å⁻³
Δρ_min = −2.67 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O25—H25A⋯O14ⁱ	0.824 (10)	2.06 (2)	2.872 (7)	169 (9)
O25—H25B⋯O17ⁱ	0.821 (10)	2.32 (7)	2.729 (7)	111 (6)
O25—H25B⋯O19ⁱ	0.821 (10)	2.45 (3)	3.232 (7)	161 (7)
O26—H26A⋯O7ⁱⁱ	0.816 (10)	2.08 (5)	2.822 (7)	151 (9)
O26—H26B⋯O22ⁱⁱⁱ	0.817 (10)	2.40 (2)	3.208 (7)	168 (9)
O26—H26B⋯O5ⁱⁱ	0.817 (10)	2.62 (6)	3.072 (7)	116 (5)
Symmetry codes: (i) -x+1, -y, -z; (ii) -x, -y, -z; (iii) -x+1, -y, -z-1.

Data collection: SMART (Bruker, 2002 ); cell refinement: SAINT-Plus (Bruker, 2002); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808003620/sj2461sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808003620/sj2461Isup2.hkl

checkCIF report

Comment top

Research into the design, synthesis and characterization of metal coordination polymers is still of great interest because of their intriguing topological architectures and their potential applications as functional materials (Meares & Wensel, 1984; Scott & Horrocks, 1992; Reineke et al., 1999; Eddaoudi et al., 2001). In these studies, multifunctional ligands such as poly-carboxylate compounds are used as bridging groups to construct one-, two- and three-dimensional networks (Choi et al., 1998; MacGillivray et al., 1998; Evans et al., 1999; Chen et al., 2001; Suresh et al., 2001; Kumagai et al., 2002; Lu & Babb, 2003; Song et al., 2003; Zhang et al., 2004). Numerous architectures have been assembled from particular combinations of appropriate metal centers and versatile polydentate ligands. In our pursuit of the synthesis of novel coordination polymers in the presence of benzene-1,2-dicarboxylic and isonicotinic acids (Wang et al., 2007), we obtained the title compound (I), Fig. 1, which exhibits an infinite two dimensional structure.

The asymmetric unit of (I) contains four independent thulium cations, six BDC ligands and two coordinated water molecules. Tm1 is coordinated to eight carboxylate oxygen atoms of six BDC anions; Tm2 binds to six carboxylate oxygen atoms of six individual BDC anions; Tm3 is nine-coordinated binding to nine carboxylate oxygen atoms from six BDC anions; finally, Tm4 is seven-coordinate binding to carboxylate oxygen atoms from five BDC anions and two coordinated water molecules. Compounds with four different types of metal ion coordination environments are rarely found in lanthanide coordination chemistry.

The Tm centers are each interconnected by BDC bridges to form an infinite two-dimensional network in the ac plane, as shown in Fig. 2. Interestingly, the sheet is made up from alternating infinite chains, in which the four Tm ions of the asymmetric unit are arranged in reverse order with Tm···Tm distances in the range 4.214 (6)–4.625 (9) Å. The six independent BDC ligands, however, adopt three discrete coordination modes (Fig. 3) linking the Tm cations into an extended network. O—H···O hydrogen bonds join adjacent sheets into a three dimensional supramolecular framework with O···O distances in the range 2.729 (7)–3.232 (7) Å, Table 1.

Related literature top

For background to the structures and applications of coordination polymers, see: Meares & Wensel, (1984); Scott & Horrocks, (1992); Reineke et al. (1999); Eddaoudi et al. (2001). For related structures involving multi-dimensional networks formed by multi-functional carboxylate ligands, see: Choi et al. (1998); MacGillivray et al. (1998); Evans et al. (1999); Chen et al. (2001); Suresh et al. (2001); Kumagai et al. (2002); Lu & Babb (2003); Song et al. (2003); Zhang et al. (2004); Wang et al. (2007).

Experimental top

The title compound was prepared under mild hydrothermal conditions. Typically, a mixture of Tm₂O₃ (0.193 g,0.5 mmol), isonicotinic acid (0.10 g,0.80 mmol), H₂BDC (0.251 g,1.50 mmol) and H₂O (10 mL) was sealed in a 25 ml Teflon-lined steel autoclave and heated under autogenous pressure at 443 K for 5 days. The colorless plate-like crystals obtained were recovered by filtration, washed with distilled water and dried in air.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2002); data reduction: SAINT-Plus (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) -2 - x, 2 - y, 2 - z; (ii) -1 - x, 2 - y, 2 - z; (iii) -1 + x, y, 1 + z; (iiii) -2 - x, 2 - y, 3 - z].
	Fig. 2. Crystal packing of (I) showing the two-dimensional layer structure.
	Fig. 3. Coordination modes of the BDC ligand found in (I).

Poly[diaquapentakis(µ₄-benzene-1,2-dicarboxylato)(µ₃-benzene-1,2- dicarboxylato)tetrathulium(III)] top

Crystal data top

[Tm₄(C₈H₄O₄)₆(H₂O)₂]	Z = 2
M_r = 1696.42	F(000) = 1600
Triclinic, P1	D_x = 2.426 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.5716 (4) Å	Cell parameters from 9365 reflections
b = 13.7737 (2) Å	θ = 2.8–28.3°
c = 15.8867 (3) Å	µ = 7.67 mm⁻¹
α = 75.301 (4)°	T = 295 K
β = 69.112 (2)°	Plate, colorless
γ = 65.617 (2)°	0.30 × 0.14 × 0.02 mm
V = 2322.45 (9) Å³

Data collection top

Bruker APEX area-detector diffractometer	9421 independent reflections
Radiation source: fine-focus sealed tube	8260 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ϕ and ω scans	θ_max = 26.5°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→15
T_min = 0.207, T_max = 0.862	k = −17→17
18519 measured reflections	l = −19→19

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.108	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ²(F_o²) + (0.0519P)²] where P = (F_o² + 2F_c²)/3
9421 reflections	(Δ/σ)_max = 0.002
715 parameters	Δρ_max = 2.34 e Å⁻³
6 restraints	Δρ_min = −2.67 e Å⁻³

Crystal data top

[Tm₄(C₈H₄O₄)₆(H₂O)₂]	γ = 65.617 (2)°
M_r = 1696.42	V = 2322.45 (9) Å³
Triclinic, P1	Z = 2
a = 12.5716 (4) Å	Mo Kα radiation
b = 13.7737 (2) Å	µ = 7.67 mm⁻¹
c = 15.8867 (3) Å	T = 295 K
α = 75.301 (4)°	0.30 × 0.14 × 0.02 mm
β = 69.112 (2)°

Data collection top

Bruker APEX area-detector diffractometer	9421 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	8260 reflections with I > 2σ(I)
T_min = 0.207, T_max = 0.862	R_int = 0.044
18519 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.042	6 restraints
wR(F²) = 0.108	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 2.34 e Å⁻³
9421 reflections	Δρ_min = −2.67 e Å⁻³
715 parameters

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
Tm1	−0.31816 (2)	0.12071 (2)	0.463579 (18)	0.01666 (9)
Tm2	−0.00120 (2)	0.00357 (2)	0.241350 (18)	0.01670 (9)
Tm3	0.30710 (2)	−0.11202 (2)	0.002946 (18)	0.01663 (9)
Tm4	0.51486 (2)	0.04932 (2)	−0.258514 (18)	0.01669 (9)
O1	−0.1567 (4)	0.1696 (5)	0.4135 (4)	0.0365 (13)
O2	0.0298 (4)	0.0745 (4)	0.3378 (3)	0.0289 (12)
O3	0.2956 (4)	0.0633 (4)	0.3023 (3)	0.0354 (13)
O4	0.2189 (4)	−0.0054 (4)	0.4425 (3)	0.0282 (11)
O5	−0.3224 (4)	0.1930 (4)	0.3206 (3)	0.0265 (11)
O6	−0.1474 (4)	0.1583 (4)	0.2105 (3)	0.0241 (11)
O7	−0.3531 (4)	0.1884 (4)	0.1302 (3)	0.0249 (11)
O8	−0.3630 (4)	0.3019 (4)	0.0065 (3)	0.0276 (11)
O9	−0.0324 (4)	−0.0860 (4)	0.1619 (3)	0.0265 (11)
O10	0.1308 (4)	−0.1341 (4)	0.0439 (4)	0.0355 (13)
O11	−0.3142 (4)	−0.1192 (4)	0.2113 (3)	0.0302 (12)
O12	−0.2293 (4)	−0.0281 (4)	0.0877 (3)	0.0274 (11)
O13	0.1513 (4)	−0.1479 (4)	0.2665 (3)	0.0275 (11)
O14	0.3183 (4)	−0.1874 (4)	0.1483 (3)	0.0275 (11)
O15	0.3801 (4)	−0.2562 (4)	0.4525 (3)	0.0253 (11)
O16	0.3972 (5)	−0.1774 (4)	0.3097 (3)	0.0296 (12)
O17	0.5130 (4)	−0.1881 (4)	−0.0108 (3)	0.0254 (11)
O18	0.5131 (4)	−0.0711 (4)	−0.1315 (3)	0.0279 (11)
O19	0.6707 (4)	−0.0348 (4)	−0.0425 (3)	0.0249 (11)
O20	0.8564 (4)	−0.0430 (4)	−0.1219 (3)	0.0251 (11)
O21	0.5023 (4)	0.1011 (4)	−0.4038 (3)	0.0197 (10)
O22	0.4733 (4)	0.1920 (4)	−0.5335 (3)	0.0253 (11)
O23	0.1458 (4)	0.0407 (4)	−0.3581 (3)	0.0261 (11)
O24	0.3314 (4)	0.0309 (4)	−0.4389 (3)	0.0261 (11)
O25	0.4742 (5)	0.1444 (5)	−0.1427 (3)	0.0359 (13)
O26	0.4781 (5)	−0.0892 (5)	−0.2904 (4)	0.0360 (13)
C1	−0.0433 (6)	0.1453 (6)	0.3882 (4)	0.0216 (14)
C2	0.0057 (6)	0.2099 (6)	0.4160 (4)	0.0208 (14)
C3	−0.0740 (7)	0.3070 (6)	0.4508 (5)	0.0333 (18)
H3	−0.1578	0.3266	0.4630	0.040*
C4	−0.0269 (8)	0.3731 (7)	0.4667 (6)	0.043 (2)
H4	−0.0795	0.4363	0.4915	0.052*
C5	0.0940 (8)	0.3469 (7)	0.4466 (6)	0.042 (2)
H5	0.1237	0.3949	0.4541	0.050*
C6	0.1761 (7)	0.2499 (7)	0.4150 (5)	0.0347 (18)
H6	0.2595	0.2316	0.4032	0.042*
C7	0.1294 (6)	0.1807 (5)	0.4014 (4)	0.0205 (14)
C8	0.2211 (6)	0.0706 (6)	0.3786 (5)	0.0242 (15)
C9	−0.2531 (5)	0.2181 (5)	0.2461 (4)	0.0189 (13)
C10	−0.3008 (6)	0.3307 (6)	0.2024 (4)	0.0198 (14)
C11	−0.2968 (7)	0.4109 (6)	0.2387 (5)	0.0290 (16)
H11	−0.2646	0.3919	0.2874	0.035*
C12	−0.3396 (8)	0.5178 (7)	0.2041 (5)	0.0366 (19)
H12	−0.3377	0.5702	0.2301	0.044*
C13	−0.3853 (7)	0.5465 (6)	0.1304 (6)	0.040 (2)
H13	−0.4120	0.6182	0.1057	0.048*
C14	−0.3913 (7)	0.4700 (6)	0.0937 (5)	0.0306 (17)
H14	−0.4231	0.4901	0.0447	0.037*
C15	−0.3498 (6)	0.3608 (6)	0.1294 (4)	0.0203 (14)
C16	−0.3577 (5)	0.2801 (6)	0.0867 (4)	0.0204 (14)
C17	0.0328 (6)	−0.1417 (5)	0.0971 (5)	0.0193 (14)
C18	−0.0077 (6)	−0.2241 (6)	0.0859 (4)	0.0210 (14)
C19	0.0831 (6)	−0.3190 (6)	0.0542 (5)	0.0285 (16)
H19	0.1648	−0.3266	0.0367	0.034*
C20	0.0510 (8)	−0.4018 (7)	0.0489 (6)	0.040 (2)
H20	0.1114	−0.4645	0.0272	0.049*
C21	−0.0675 (7)	−0.3920 (7)	0.0751 (6)	0.043 (2)
H21	−0.0882	−0.4479	0.0711	0.052*
C22	−0.1584 (6)	−0.2989 (6)	0.1079 (5)	0.0279 (16)
H22	−0.2395	−0.2932	0.1269	0.034*
C23	−0.1287 (6)	−0.2141 (6)	0.1125 (4)	0.0214 (14)
C24	−0.2311 (5)	−0.1127 (6)	0.1400 (4)	0.0194 (14)
C25	0.2553 (6)	−0.2075 (6)	0.2276 (4)	0.0208 (14)
C26	0.3052 (5)	−0.3180 (5)	0.2776 (4)	0.0188 (14)
C27	0.2949 (7)	−0.4028 (6)	0.2527 (5)	0.0305 (17)
H27	0.2622	−0.3910	0.2053	0.037*
C28	0.3340 (8)	−0.5060 (7)	0.2992 (6)	0.043 (2)
H28	0.3290	−0.5631	0.2816	0.052*
C29	0.3802 (8)	−0.5236 (6)	0.3712 (6)	0.039 (2)
H29	0.4050	−0.5921	0.4025	0.047*
C30	0.3891 (7)	−0.4394 (6)	0.3960 (5)	0.0295 (16)
H30	0.4182	−0.4510	0.4453	0.035*
C31	0.3552 (6)	−0.3363 (6)	0.3483 (4)	0.0216 (15)
C32	0.3785 (6)	−0.2512 (6)	0.3731 (4)	0.0206 (14)
C33	0.5698 (5)	−0.1514 (5)	−0.0863 (4)	0.0179 (13)
C34	0.7019 (5)	−0.2149 (5)	−0.1220 (4)	0.0182 (13)
C35	0.7286 (7)	−0.3091 (6)	−0.1544 (5)	0.0303 (17)
H35	0.6656	−0.3291	−0.1526	0.036*
C36	0.8467 (7)	−0.3730 (7)	−0.1891 (6)	0.041 (2)
H36	0.8634	−0.4350	−0.2122	0.049*
C37	0.9415 (7)	−0.3461 (7)	−0.1900 (6)	0.040 (2)
H37	1.0218	−0.3908	−0.2120	0.048*
C38	0.9158 (6)	−0.2520 (6)	−0.1578 (5)	0.0271 (16)
H38	0.9793	−0.2334	−0.1585	0.033*
C39	0.7962 (5)	−0.1850 (5)	−0.1247 (4)	0.0194 (14)
C40	0.7718 (6)	−0.0829 (6)	−0.0942 (4)	0.0202 (14)
C41	0.4315 (6)	0.1676 (5)	−0.4498 (4)	0.0182 (13)
C42	0.3013 (5)	0.2301 (5)	−0.4029 (4)	0.0183 (13)
C43	0.2790 (7)	0.3312 (6)	−0.3869 (5)	0.0297 (17)
H43	0.3426	0.3570	−0.4059	0.036*
C44	0.1616 (7)	0.3961 (7)	−0.3424 (5)	0.0370 (19)
H44	0.1477	0.4632	−0.3294	0.044*
C45	0.0666 (7)	0.3585 (6)	−0.3180 (5)	0.0360 (19)
H45	−0.0123	0.4019	−0.2906	0.043*
C46	0.0882 (6)	0.2577 (6)	−0.3339 (5)	0.0265 (16)
H46	0.0235	0.2336	−0.3170	0.032*
C47	0.2054 (5)	0.1908 (6)	−0.3752 (4)	0.0193 (14)
C48	0.2280 (6)	0.0824 (6)	−0.3906 (4)	0.0198 (14)
H25A	0.528 (6)	0.165 (7)	−0.146 (5)	0.050*
H25B	0.440 (7)	0.127 (7)	−0.0899 (18)	0.050*
H26A	0.422 (5)	−0.096 (7)	−0.246 (3)	0.050*
H26B	0.481 (7)	−0.107 (7)	−0.337 (3)	0.050*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tm1	0.01355 (14)	0.01940 (17)	0.01543 (15)	−0.00609 (12)	−0.00262 (11)	−0.00136 (11)
Tm2	0.01188 (15)	0.01966 (18)	0.01674 (15)	−0.00620 (13)	0.00029 (11)	−0.00466 (12)
Tm3	0.01472 (15)	0.01797 (17)	0.01583 (15)	−0.00678 (12)	−0.00276 (11)	−0.00056 (12)
Tm4	0.01315 (14)	0.02015 (17)	0.01376 (15)	−0.00586 (12)	−0.00174 (10)	−0.00035 (11)
O1	0.016 (2)	0.043 (4)	0.051 (3)	−0.013 (2)	−0.008 (2)	−0.005 (3)
O2	0.028 (3)	0.034 (3)	0.030 (3)	−0.012 (2)	−0.005 (2)	−0.015 (2)
O3	0.016 (2)	0.036 (3)	0.036 (3)	−0.003 (2)	0.006 (2)	−0.004 (2)
O4	0.026 (3)	0.027 (3)	0.024 (3)	−0.002 (2)	−0.010 (2)	−0.001 (2)
O5	0.019 (2)	0.034 (3)	0.020 (2)	−0.011 (2)	−0.0013 (19)	0.004 (2)
O6	0.018 (2)	0.025 (3)	0.022 (2)	−0.006 (2)	0.0006 (19)	−0.002 (2)
O7	0.030 (3)	0.022 (3)	0.023 (2)	−0.013 (2)	−0.006 (2)	0.001 (2)
O8	0.035 (3)	0.027 (3)	0.020 (2)	−0.009 (2)	−0.009 (2)	−0.004 (2)
O9	0.024 (2)	0.032 (3)	0.025 (3)	−0.010 (2)	−0.004 (2)	−0.010 (2)
O10	0.024 (3)	0.036 (3)	0.044 (3)	−0.017 (2)	0.007 (2)	−0.012 (3)
O11	0.017 (2)	0.042 (3)	0.026 (3)	−0.010 (2)	−0.004 (2)	0.001 (2)
O12	0.027 (3)	0.023 (3)	0.027 (3)	−0.006 (2)	−0.011 (2)	0.005 (2)
O13	0.019 (2)	0.023 (3)	0.026 (3)	0.001 (2)	−0.001 (2)	0.000 (2)
O14	0.027 (3)	0.030 (3)	0.021 (2)	−0.009 (2)	−0.003 (2)	−0.002 (2)
O15	0.028 (3)	0.029 (3)	0.019 (2)	−0.011 (2)	−0.0050 (19)	−0.004 (2)
O16	0.043 (3)	0.033 (3)	0.022 (3)	−0.025 (3)	−0.012 (2)	0.005 (2)
O17	0.020 (2)	0.031 (3)	0.019 (2)	−0.012 (2)	0.0006 (19)	0.003 (2)
O18	0.023 (2)	0.025 (3)	0.028 (3)	0.001 (2)	−0.011 (2)	−0.001 (2)
O19	0.018 (2)	0.029 (3)	0.026 (3)	−0.008 (2)	0.0003 (19)	−0.010 (2)
O20	0.020 (2)	0.034 (3)	0.023 (2)	−0.017 (2)	−0.0003 (19)	0.000 (2)
O21	0.017 (2)	0.025 (3)	0.017 (2)	−0.010 (2)	−0.0047 (18)	0.0013 (19)
O22	0.016 (2)	0.034 (3)	0.019 (2)	−0.007 (2)	−0.0030 (18)	0.002 (2)
O23	0.021 (2)	0.037 (3)	0.020 (2)	−0.019 (2)	0.0019 (19)	−0.001 (2)
O24	0.015 (2)	0.025 (3)	0.033 (3)	−0.007 (2)	0.004 (2)	−0.013 (2)
O25	0.033 (3)	0.058 (4)	0.022 (3)	−0.018 (3)	−0.005 (2)	−0.014 (3)
O26	0.048 (3)	0.046 (4)	0.024 (3)	−0.029 (3)	−0.006 (2)	−0.006 (3)
C1	0.021 (3)	0.026 (4)	0.017 (3)	−0.011 (3)	−0.003 (3)	0.001 (3)
C2	0.019 (3)	0.024 (4)	0.018 (3)	−0.005 (3)	−0.006 (3)	−0.003 (3)
C3	0.030 (4)	0.022 (4)	0.040 (4)	0.003 (3)	−0.012 (3)	−0.009 (3)
C4	0.051 (5)	0.027 (5)	0.051 (5)	0.002 (4)	−0.022 (4)	−0.018 (4)
C5	0.066 (6)	0.033 (5)	0.047 (5)	−0.029 (5)	−0.029 (4)	0.001 (4)
C6	0.043 (4)	0.039 (5)	0.037 (4)	−0.025 (4)	−0.018 (4)	−0.002 (4)
C7	0.021 (3)	0.019 (4)	0.017 (3)	−0.005 (3)	−0.005 (3)	0.000 (3)
C8	0.021 (3)	0.025 (4)	0.029 (4)	−0.011 (3)	−0.006 (3)	−0.004 (3)
C9	0.014 (3)	0.018 (4)	0.025 (3)	−0.003 (3)	−0.009 (3)	−0.003 (3)
C10	0.016 (3)	0.022 (4)	0.018 (3)	−0.006 (3)	−0.001 (2)	−0.004 (3)
C11	0.035 (4)	0.031 (4)	0.027 (4)	−0.015 (3)	−0.009 (3)	−0.006 (3)
C12	0.049 (5)	0.028 (5)	0.037 (4)	−0.018 (4)	−0.008 (4)	−0.010 (4)
C13	0.039 (5)	0.012 (4)	0.053 (5)	−0.003 (4)	−0.006 (4)	−0.002 (4)
C14	0.035 (4)	0.023 (4)	0.031 (4)	−0.010 (3)	−0.010 (3)	0.001 (3)
C15	0.020 (3)	0.018 (4)	0.016 (3)	−0.004 (3)	0.000 (2)	−0.001 (3)
C16	0.014 (3)	0.021 (4)	0.025 (4)	−0.006 (3)	0.000 (3)	−0.009 (3)
C17	0.016 (3)	0.016 (3)	0.028 (4)	−0.008 (3)	−0.007 (3)	−0.001 (3)
C18	0.022 (3)	0.026 (4)	0.018 (3)	−0.010 (3)	−0.005 (3)	−0.006 (3)
C19	0.025 (4)	0.025 (4)	0.031 (4)	−0.007 (3)	0.000 (3)	−0.010 (3)
C20	0.039 (5)	0.028 (5)	0.048 (5)	−0.005 (4)	−0.003 (4)	−0.019 (4)
C21	0.037 (4)	0.031 (5)	0.068 (6)	−0.017 (4)	−0.013 (4)	−0.013 (4)
C22	0.028 (4)	0.024 (4)	0.037 (4)	−0.015 (3)	−0.010 (3)	−0.002 (3)
C23	0.019 (3)	0.022 (4)	0.020 (3)	−0.010 (3)	0.000 (3)	0.000 (3)
C24	0.013 (3)	0.028 (4)	0.015 (3)	−0.006 (3)	−0.003 (2)	−0.003 (3)
C25	0.020 (3)	0.027 (4)	0.020 (3)	−0.011 (3)	−0.008 (3)	−0.004 (3)
C26	0.016 (3)	0.018 (4)	0.018 (3)	−0.004 (3)	0.000 (2)	−0.005 (3)
C27	0.031 (4)	0.026 (4)	0.038 (4)	−0.010 (3)	−0.015 (3)	−0.005 (3)
C28	0.060 (6)	0.023 (5)	0.051 (5)	−0.019 (4)	−0.021 (4)	0.000 (4)
C29	0.049 (5)	0.016 (4)	0.045 (5)	−0.010 (4)	−0.012 (4)	0.003 (4)
C30	0.036 (4)	0.020 (4)	0.027 (4)	−0.005 (3)	−0.012 (3)	0.004 (3)
C31	0.019 (3)	0.020 (4)	0.023 (3)	−0.009 (3)	0.000 (3)	−0.002 (3)
C32	0.015 (3)	0.025 (4)	0.021 (3)	−0.007 (3)	−0.003 (2)	−0.004 (3)
C33	0.013 (3)	0.022 (4)	0.019 (3)	−0.003 (3)	−0.007 (2)	−0.006 (3)
C34	0.015 (3)	0.018 (4)	0.017 (3)	−0.008 (3)	0.000 (2)	0.001 (3)
C35	0.030 (4)	0.023 (4)	0.037 (4)	−0.007 (3)	−0.005 (3)	−0.014 (3)
C36	0.036 (4)	0.031 (5)	0.050 (5)	−0.006 (4)	−0.001 (4)	−0.022 (4)
C37	0.025 (4)	0.025 (5)	0.047 (5)	0.003 (3)	0.003 (3)	−0.005 (4)
C38	0.013 (3)	0.028 (4)	0.032 (4)	−0.007 (3)	0.000 (3)	0.000 (3)
C39	0.017 (3)	0.016 (4)	0.018 (3)	−0.004 (3)	−0.002 (2)	0.001 (3)
C40	0.022 (3)	0.029 (4)	0.015 (3)	−0.015 (3)	−0.008 (3)	0.003 (3)
C41	0.021 (3)	0.021 (4)	0.017 (3)	−0.012 (3)	−0.005 (2)	−0.001 (3)
C42	0.015 (3)	0.022 (4)	0.014 (3)	−0.008 (3)	−0.001 (2)	0.002 (3)
C43	0.031 (4)	0.020 (4)	0.031 (4)	−0.008 (3)	−0.008 (3)	0.005 (3)
C44	0.044 (5)	0.025 (4)	0.036 (4)	−0.010 (4)	−0.005 (4)	−0.007 (4)
C45	0.031 (4)	0.026 (4)	0.034 (4)	−0.001 (3)	0.002 (3)	−0.005 (3)
C46	0.015 (3)	0.025 (4)	0.027 (4)	−0.001 (3)	0.003 (3)	−0.004 (3)
C47	0.015 (3)	0.024 (4)	0.016 (3)	−0.006 (3)	−0.001 (2)	−0.005 (3)
C48	0.023 (3)	0.024 (4)	0.015 (3)	−0.012 (3)	−0.007 (3)	0.000 (3)

Geometric parameters (Å, º) top

Tm1—O4ⁱ	2.190 (5)	O26—H26B	0.817 (10)
Tm1—O1	2.216 (5)	C1—C2	1.488 (9)
Tm1—O5	2.248 (5)	C2—C7	1.380 (9)
Tm1—O15ⁱ	2.278 (5)	C2—C3	1.403 (10)
Tm1—O24ⁱⁱ	2.300 (5)	C3—C4	1.383 (12)
Tm1—O22ⁱⁱⁱ	2.377 (4)	C3—H3	0.9300
Tm1—O21ⁱⁱⁱ	2.536 (4)	C4—C5	1.343 (12)
Tm1—O23ⁱⁱ	2.787 (5)	C4—H4	0.9300
Tm1—C41ⁱⁱⁱ	2.811 (6)	C5—C6	1.391 (12)
Tm1—C48ⁱⁱ	2.924 (7)	C5—H5	0.9300
Tm2—O9	2.194 (5)	C6—C7	1.400 (10)
Tm2—O2	2.225 (5)	C6—H6	0.9300
Tm2—O13	2.238 (5)	C7—C8	1.516 (9)
Tm2—O20^iv	2.244 (4)	C9—C10	1.493 (9)
Tm2—O6	2.244 (5)	C10—C11	1.395 (9)
Tm2—O23ⁱⁱ	2.248 (4)	C10—C15	1.396 (9)
Tm3—O12ⁱⁱ	2.188 (5)	C11—C12	1.381 (11)
Tm3—O10	2.203 (4)	C11—H11	0.9300
Tm3—O17	2.306 (4)	C12—C13	1.383 (12)
Tm3—O14	2.308 (5)	C12—H12	0.9300
Tm3—O7ⁱⁱ	2.380 (5)	C13—C14	1.366 (11)
Tm3—O19^iv	2.408 (5)	C13—H13	0.9300
Tm3—O8ⁱⁱ	2.442 (5)	C14—C15	1.409 (10)
Tm3—C16ⁱⁱ	2.758 (7)	C14—H14	0.9300
Tm3—O20^iv	2.830 (5)	C15—C16	1.493 (9)
Tm3—O18	2.870 (5)	C16—Tm3ⁱⁱ	2.758 (7)
Tm3—C33	2.963 (6)	C17—C18	1.491 (9)
Tm4—O11ⁱⁱ	2.205 (4)	C18—C23	1.381 (9)
Tm4—O3^iv	2.210 (5)	C18—C19	1.400 (10)
Tm4—O18	2.264 (5)	C19—C20	1.386 (11)
Tm4—O21	2.278 (4)	C19—H19	0.9300
Tm4—O16^iv	2.289 (5)	C20—C21	1.354 (11)
Tm4—O25	2.315 (5)	C20—H20	0.9300
Tm4—O26	2.344 (5)	C21—C22	1.388 (11)
O1—C1	1.254 (8)	C21—H21	0.9300
O2—C1	1.253 (8)	C22—C23	1.389 (9)
O3—C8	1.237 (8)	C22—H22	0.9300
O3—Tm4^iv	2.210 (5)	C23—C24	1.492 (9)
O4—C8	1.261 (8)	C25—C26	1.515 (9)
O4—Tm1ⁱ	2.190 (5)	C26—C27	1.390 (9)
O5—C9	1.258 (7)	C26—C31	1.396 (9)
O6—C9	1.250 (7)	C27—C28	1.398 (11)
O7—C16	1.267 (8)	C27—H27	0.9300
O7—Tm3ⁱⁱ	2.380 (5)	C28—C29	1.386 (12)
O8—C16	1.252 (8)	C28—H28	0.9300
O8—Tm3ⁱⁱ	2.442 (5)	C29—C30	1.373 (11)
O9—C17	1.265 (8)	C29—H29	0.9300
O10—C17	1.251 (7)	C30—C31	1.399 (10)
O11—C24	1.252 (7)	C30—H30	0.9300
O11—Tm4ⁱⁱ	2.205 (4)	C31—C32	1.487 (9)
O12—C24	1.251 (8)	C33—C34	1.492 (8)
O12—Tm3ⁱⁱ	2.188 (5)	C34—C35	1.386 (9)
O13—C25	1.249 (8)	C34—C39	1.391 (9)
O14—C25	1.258 (7)	C35—C36	1.366 (10)
O15—C32	1.253 (8)	C35—H35	0.9300
O15—Tm1ⁱ	2.278 (5)	C36—C37	1.380 (11)
O16—C32	1.270 (8)	C36—H36	0.9300
O16—Tm4^iv	2.289 (5)	C37—C38	1.386 (11)
O17—C33	1.258 (7)	C37—H37	0.9300
O18—C33	1.248 (8)	C38—C39	1.387 (9)
O19—C40	1.251 (8)	C38—H38	0.9300
O19—Tm3^iv	2.408 (5)	C39—C40	1.480 (9)
O20—C40	1.286 (7)	C41—C42	1.506 (8)
O20—Tm2^iv	2.244 (4)	C41—Tm1^v	2.811 (6)
O20—Tm3^iv	2.830 (5)	C42—C43	1.375 (10)
O21—C41	1.272 (8)	C42—C47	1.406 (8)
O21—Tm1^v	2.536 (4)	C43—C44	1.401 (10)
O22—C41	1.256 (7)	C43—H43	0.9300
O22—Tm1^v	2.377 (4)	C44—C45	1.387 (11)
O23—C48	1.274 (7)	C44—H44	0.9300
O23—Tm2ⁱⁱ	2.248 (4)	C45—C46	1.373 (10)
O23—Tm1ⁱⁱ	2.787 (5)	C45—H45	0.9300
O24—C48	1.259 (8)	C46—C47	1.396 (9)
O24—Tm1ⁱⁱ	2.300 (5)	C46—H46	0.9300
O25—H25A	0.824 (10)	C47—C48	1.468 (9)
O25—H25B	0.821 (10)	C48—Tm1ⁱⁱ	2.924 (7)
O26—H26A	0.816 (10)

O4ⁱ—Tm1—O1	82.99 (19)	C48—O23—Tm1ⁱⁱ	83.2 (4)
O4ⁱ—Tm1—O5	149.43 (17)	Tm2ⁱⁱ—O23—Tm1ⁱⁱ	116.9 (2)
O1—Tm1—O5	78.74 (18)	C48—O24—Tm1ⁱⁱ	106.8 (4)
O4ⁱ—Tm1—O15ⁱ	91.43 (18)	Tm4—O25—H25A	115 (5)
O1—Tm1—O15ⁱ	78.58 (18)	Tm4—O25—H25B	122 (6)
O5—Tm1—O15ⁱ	108.50 (18)	H25A—O25—H25B	112 (3)
O4ⁱ—Tm1—O24ⁱⁱ	82.45 (19)	Tm4—O26—H26A	102 (5)
O1—Tm1—O24ⁱⁱ	127.61 (18)	Tm4—O26—H26B	134 (6)
O5—Tm1—O24ⁱⁱ	89.52 (18)	H26A—O26—H26B	115 (3)
O15ⁱ—Tm1—O24ⁱⁱ	151.59 (15)	O2—C1—O1	124.3 (6)
O4ⁱ—Tm1—O22ⁱⁱⁱ	133.10 (16)	O2—C1—C2	118.5 (6)
O1—Tm1—O22ⁱⁱⁱ	139.67 (19)	O1—C1—C2	117.1 (6)
O5—Tm1—O22ⁱⁱⁱ	73.92 (15)	C7—C2—C3	119.3 (7)
O15ⁱ—Tm1—O22ⁱⁱⁱ	82.61 (17)	C7—C2—C1	121.1 (6)
O24ⁱⁱ—Tm1—O22ⁱⁱⁱ	81.57 (17)	C3—C2—C1	119.4 (6)
O4ⁱ—Tm1—O21ⁱⁱⁱ	80.83 (16)	C4—C3—C2	119.4 (7)
O1—Tm1—O21ⁱⁱⁱ	147.00 (18)	C4—C3—H3	120.3
O5—Tm1—O21ⁱⁱⁱ	126.42 (15)	C2—C3—H3	120.3
O15ⁱ—Tm1—O21ⁱⁱⁱ	73.30 (15)	C5—C4—C3	120.7 (8)
O24ⁱⁱ—Tm1—O21ⁱⁱⁱ	78.34 (15)	C5—C4—H4	119.6
O22ⁱⁱⁱ—Tm1—O21ⁱⁱⁱ	52.83 (15)	C3—C4—H4	119.6
O4ⁱ—Tm1—O23ⁱⁱ	76.67 (16)	C4—C5—C6	121.7 (7)
O1—Tm1—O23ⁱⁱ	77.80 (17)	C4—C5—H5	119.2
O5—Tm1—O23ⁱⁱ	75.65 (16)	C6—C5—H5	119.2
O15ⁱ—Tm1—O23ⁱⁱ	154.64 (15)	C5—C6—C7	118.1 (7)
O24ⁱⁱ—Tm1—O23ⁱⁱ	49.89 (13)	C5—C6—H6	121.0
O22ⁱⁱⁱ—Tm1—O23ⁱⁱ	121.86 (15)	C7—C6—H6	121.0
O21ⁱⁱⁱ—Tm1—O23ⁱⁱ	125.32 (15)	C2—C7—C6	120.7 (7)
O4ⁱ—Tm1—C41ⁱⁱⁱ	107.72 (18)	C2—C7—C8	123.4 (6)
O1—Tm1—C41ⁱⁱⁱ	149.9 (2)	C6—C7—C8	115.7 (6)
O5—Tm1—C41ⁱⁱⁱ	100.28 (17)	O3—C8—O4	125.6 (7)
O15ⁱ—Tm1—C41ⁱⁱⁱ	73.19 (17)	O3—C8—C7	118.4 (6)
O24ⁱⁱ—Tm1—C41ⁱⁱⁱ	82.27 (17)	O4—C8—C7	115.8 (6)
O22ⁱⁱⁱ—Tm1—C41ⁱⁱⁱ	26.36 (17)	O6—C9—O5	124.8 (6)
O21ⁱⁱⁱ—Tm1—C41ⁱⁱⁱ	26.89 (16)	O6—C9—C10	119.3 (6)
O23ⁱⁱ—Tm1—C41ⁱⁱⁱ	131.59 (16)	O5—C9—C10	115.8 (5)
O4ⁱ—Tm1—C48ⁱⁱ	77.03 (18)	C11—C10—C15	118.4 (7)
O1—Tm1—C48ⁱⁱ	103.25 (19)	C11—C10—C9	116.7 (6)
O5—Tm1—C48ⁱⁱ	83.54 (18)	C15—C10—C9	124.9 (6)
O15ⁱ—Tm1—C48ⁱⁱ	167.89 (18)	C12—C11—C10	121.6 (7)
O24ⁱⁱ—Tm1—C48ⁱⁱ	24.35 (15)	C12—C11—H11	119.2
O22ⁱⁱⁱ—Tm1—C48ⁱⁱ	102.50 (17)	C10—C11—H11	119.2
O21ⁱⁱⁱ—Tm1—C48ⁱⁱ	100.86 (16)	C11—C12—C13	119.6 (7)
O23ⁱⁱ—Tm1—C48ⁱⁱ	25.63 (15)	C11—C12—H12	120.2
C41ⁱⁱⁱ—Tm1—C48ⁱⁱ	106.56 (18)	C13—C12—H12	120.2
O9—Tm2—O2	171.67 (18)	C14—C13—C12	120.3 (8)
O9—Tm2—O13	86.46 (19)	C14—C13—H13	119.9
O2—Tm2—O13	88.27 (19)	C12—C13—H13	119.9
O9—Tm2—O20^iv	91.61 (17)	C13—C14—C15	120.7 (8)
O2—Tm2—O20^iv	94.30 (17)	C13—C14—H14	119.7
O13—Tm2—O20^iv	84.49 (17)	C15—C14—H14	119.7
O9—Tm2—O6	93.86 (18)	C10—C15—C14	119.5 (7)
O2—Tm2—O6	91.72 (19)	C10—C15—C16	121.8 (6)
O13—Tm2—O6	177.17 (15)	C14—C15—C16	118.6 (6)
O20^iv—Tm2—O6	92.69 (17)	O8—C16—O7	120.4 (6)
O9—Tm2—O23ⁱⁱ	86.23 (17)	O8—C16—C15	119.7 (6)
O2—Tm2—O23ⁱⁱ	87.80 (17)	O7—C16—C15	119.8 (6)
O13—Tm2—O23ⁱⁱ	94.83 (17)	O8—C16—Tm3ⁱⁱ	62.3 (4)
O20^iv—Tm2—O23ⁱⁱ	177.77 (16)	O7—C16—Tm3ⁱⁱ	59.5 (3)
O6—Tm2—O23ⁱⁱ	87.99 (17)	C15—C16—Tm3ⁱⁱ	165.0 (4)
O12ⁱⁱ—Tm3—O10	85.95 (19)	O10—C17—O9	123.9 (6)
O12ⁱⁱ—Tm3—O17	122.74 (16)	O10—C17—C18	118.2 (6)
O10—Tm3—O17	147.99 (19)	O9—C17—C18	117.8 (5)
O12ⁱⁱ—Tm3—O14	148.40 (18)	C23—C18—C19	119.7 (6)
O10—Tm3—O14	86.65 (19)	C23—C18—C17	122.9 (6)
O17—Tm3—O14	75.42 (16)	C19—C18—C17	117.2 (6)
O12ⁱⁱ—Tm3—O7ⁱⁱ	77.54 (18)	C20—C19—C18	119.8 (7)
O10—Tm3—O7ⁱⁱ	86.24 (18)	C20—C19—H19	120.1
O17—Tm3—O7ⁱⁱ	86.73 (17)	C18—C19—H19	120.1
O14—Tm3—O7ⁱⁱ	132.48 (17)	C21—C20—C19	120.5 (8)
O12ⁱⁱ—Tm3—O19^iv	75.28 (18)	C21—C20—H20	119.7
O10—Tm3—O19^iv	122.56 (17)	C19—C20—H20	119.7
O17—Tm3—O19^iv	81.89 (17)	C20—C21—C22	120.2 (7)
O14—Tm3—O19^iv	83.07 (17)	C20—C21—H21	119.9
O7ⁱⁱ—Tm3—O19^iv	138.07 (15)	C22—C21—H21	119.9
O12ⁱⁱ—Tm3—O8ⁱⁱ	128.53 (17)	C21—C22—C23	120.4 (7)
O10—Tm3—O8ⁱⁱ	75.95 (18)	C21—C22—H22	119.8
O17—Tm3—O8ⁱⁱ	74.70 (17)	C23—C22—H22	119.8
O14—Tm3—O8ⁱⁱ	78.84 (17)	C18—C23—C22	119.4 (7)
O7ⁱⁱ—Tm3—O8ⁱⁱ	53.88 (16)	C18—C23—C24	122.9 (6)
O19^iv—Tm3—O8ⁱⁱ	153.32 (16)	C22—C23—C24	117.5 (6)
O12ⁱⁱ—Tm3—C16ⁱⁱ	102.3 (2)	O12—C24—O11	125.1 (6)
O10—Tm3—C16ⁱⁱ	76.62 (18)	O12—C24—C23	117.1 (5)
O17—Tm3—C16ⁱⁱ	82.96 (18)	O11—C24—C23	117.7 (6)
O14—Tm3—C16ⁱⁱ	105.80 (19)	O13—C25—O14	126.1 (7)
O7ⁱⁱ—Tm3—C16ⁱⁱ	27.30 (18)	O13—C25—C26	116.6 (6)
O19^iv—Tm3—C16ⁱⁱ	159.87 (16)	O14—C25—C26	117.0 (6)
O8ⁱⁱ—Tm3—C16ⁱⁱ	26.99 (18)	C27—C26—C31	119.9 (7)
O12ⁱⁱ—Tm3—O20^iv	76.45 (17)	C27—C26—C25	116.9 (6)
O10—Tm3—O20^iv	74.39 (16)	C31—C26—C25	123.1 (6)
O17—Tm3—O20^iv	122.62 (15)	C26—C27—C28	119.7 (7)
O14—Tm3—O20^iv	71.97 (16)	C26—C27—H27	120.1
O7ⁱⁱ—Tm3—O20^iv	148.42 (15)	C28—C27—H27	120.1
O19^iv—Tm3—O20^iv	48.69 (13)	C29—C28—C27	120.4 (8)
O8ⁱⁱ—Tm3—O20^iv	139.11 (14)	C29—C28—H28	119.8
C16ⁱⁱ—Tm3—O20^iv	151.00 (15)	C27—C28—H28	119.8
O12ⁱⁱ—Tm3—O18	74.97 (16)	C30—C29—C28	119.6 (8)
O10—Tm3—O18	152.24 (18)	C30—C29—H29	120.2
O17—Tm3—O18	48.03 (15)	C28—C29—H29	120.2
O14—Tm3—O18	119.99 (15)	C29—C30—C31	121.1 (7)
O7ⁱⁱ—Tm3—O18	70.26 (15)	C29—C30—H30	119.5
O19^iv—Tm3—O18	72.22 (14)	C31—C30—H30	119.5
O8ⁱⁱ—Tm3—O18	100.23 (15)	C26—C31—C30	119.2 (7)
C16ⁱⁱ—Tm3—O18	87.78 (16)	C26—C31—C32	122.6 (6)
O20^iv—Tm3—O18	118.94 (14)	C30—C31—C32	118.2 (7)
O12ⁱⁱ—Tm3—C33	99.60 (18)	O15—C32—O16	124.0 (6)
O10—Tm3—C33	158.80 (18)	O15—C32—C31	119.9 (6)
O17—Tm3—C33	23.68 (17)	O16—C32—C31	116.1 (6)
O14—Tm3—C33	98.32 (17)	O18—C33—O17	119.9 (6)
O7ⁱⁱ—Tm3—C33	75.17 (16)	O18—C33—C34	122.8 (6)
O19^iv—Tm3—C33	78.59 (16)	O17—C33—C34	117.0 (6)
O8ⁱⁱ—Tm3—C33	84.77 (17)	O18—C33—Tm3	73.5 (3)
C16ⁱⁱ—Tm3—C33	82.21 (17)	O17—C33—Tm3	47.4 (3)
O20^iv—Tm3—C33	126.77 (15)	C34—C33—Tm3	157.5 (4)
O18—Tm3—C33	24.63 (15)	C35—C34—C39	119.7 (6)
O11ⁱⁱ—Tm4—O3^iv	163.2 (2)	C35—C34—C33	115.8 (6)
O11ⁱⁱ—Tm4—O18	89.47 (17)	C39—C34—C33	124.5 (6)
O3^iv—Tm4—O18	81.73 (18)	C36—C35—C34	120.6 (7)
O11ⁱⁱ—Tm4—O21	88.24 (16)	C36—C35—H35	119.7
O3^iv—Tm4—O21	92.44 (18)	C34—C35—H35	119.7
O18—Tm4—O21	150.61 (17)	C35—C36—C37	120.5 (7)
O11ⁱⁱ—Tm4—O16^iv	112.53 (19)	C35—C36—H36	119.8
O3^iv—Tm4—O16^iv	83.94 (19)	C37—C36—H36	119.8
O18—Tm4—O16^iv	129.82 (17)	C36—C37—C38	119.3 (7)
O21—Tm4—O16^iv	77.53 (16)	C36—C37—H37	120.3
O11ⁱⁱ—Tm4—O25	75.59 (19)	C38—C37—H37	120.3
O3^iv—Tm4—O25	115.2 (2)	C37—C38—C39	120.7 (6)
O18—Tm4—O25	74.5 (2)	C37—C38—H38	119.6
O21—Tm4—O25	132.8 (2)	C39—C38—H38	119.6
O16^iv—Tm4—O25	68.97 (18)	C38—C39—C34	119.1 (6)
O11ⁱⁱ—Tm4—O26	83.4 (2)	C38—C39—C40	119.4 (6)
O3^iv—Tm4—O26	80.5 (2)	C34—C39—C40	121.4 (6)
O18—Tm4—O26	74.75 (19)	O19—C40—O20	119.6 (6)
O21—Tm4—O26	75.88 (18)	O19—C40—C39	121.3 (5)
O16^iv—Tm4—O26	148.45 (17)	O20—C40—C39	119.0 (6)
O25—Tm4—O26	142.58 (19)	O22—C41—O21	120.1 (6)
C1—O1—Tm1	150.0 (5)	O22—C41—C42	118.8 (6)
C1—O2—Tm2	130.1 (4)	O21—C41—C42	120.4 (5)
C8—O3—Tm4^iv	130.2 (5)	O22—C41—Tm1^v	57.2 (3)
C8—O4—Tm1ⁱ	144.7 (4)	O21—C41—Tm1^v	64.4 (3)
C9—O5—Tm1	139.6 (4)	C42—C41—Tm1^v	159.4 (4)
C9—O6—Tm2	141.4 (4)	C43—C42—C47	120.0 (6)
C16—O7—Tm3ⁱⁱ	93.2 (4)	C43—C42—C41	115.9 (5)
C16—O8—Tm3ⁱⁱ	90.7 (4)	C47—C42—C41	124.1 (6)
C17—O9—Tm2	135.3 (4)	C42—C43—C44	120.9 (7)
C17—O10—Tm3	156.6 (5)	C42—C43—H43	119.5
C24—O11—Tm4ⁱⁱ	137.6 (4)	C44—C43—H43	119.5
C24—O12—Tm3ⁱⁱ	152.0 (4)	C45—C44—C43	118.9 (7)
C25—O13—Tm2	142.0 (4)	C45—C44—H44	120.5
C25—O14—Tm3	143.2 (4)	C43—C44—H44	120.5
C32—O15—Tm1ⁱ	129.4 (5)	C46—C45—C44	120.4 (7)
C32—O16—Tm4^iv	145.1 (4)	C46—C45—H45	119.8
C33—O17—Tm3	108.9 (4)	C44—C45—H45	119.8
C33—O18—Tm4	149.3 (4)	C45—C46—C47	121.1 (6)
C33—O18—Tm3	81.9 (4)	C45—C46—H46	119.4
Tm4—O18—Tm3	128.13 (19)	C47—C46—H46	119.4
C40—O19—Tm3^iv	106.2 (4)	C46—C47—C42	118.5 (6)
C40—O20—Tm2^iv	145.9 (4)	C46—C47—C48	120.7 (6)
C40—O20—Tm3^iv	85.1 (4)	C42—C47—C48	120.7 (6)
Tm2^iv—O20—Tm3^iv	120.00 (19)	O24—C48—O23	119.7 (6)
C41—O21—Tm4	141.4 (4)	O24—C48—C47	118.3 (5)
C41—O21—Tm1^v	88.7 (3)	O23—C48—C47	122.0 (6)
Tm4—O21—Tm1^v	122.08 (18)	O24—C48—Tm1ⁱⁱ	48.9 (3)
C41—O22—Tm1^v	96.5 (4)	O23—C48—Tm1ⁱⁱ	71.2 (4)
C48—O23—Tm2ⁱⁱ	151.2 (4)	C47—C48—Tm1ⁱⁱ	165.3 (4)

O4ⁱ—Tm1—O1—C1	47.0 (10)	C10—C15—C16—O8	−156.4 (6)
O5—Tm1—O1—C1	−108.4 (10)	C14—C15—C16—O8	22.5 (9)
O15ⁱ—Tm1—O1—C1	139.9 (10)	C10—C15—C16—O7	20.2 (9)
O24ⁱⁱ—Tm1—O1—C1	−27.8 (11)	C14—C15—C16—O7	−160.9 (6)
O22ⁱⁱⁱ—Tm1—O1—C1	−156.3 (9)	C10—C15—C16—Tm3ⁱⁱ	−63 (2)
O21ⁱⁱⁱ—Tm1—O1—C1	108.0 (10)	C14—C15—C16—Tm3ⁱⁱ	116.0 (18)
O23ⁱⁱ—Tm1—O1—C1	−30.8 (10)	Tm3—O10—C17—O9	37.6 (17)
C41ⁱⁱⁱ—Tm1—O1—C1	160.5 (9)	Tm3—O10—C17—C18	−140.1 (10)
C48ⁱⁱ—Tm1—O1—C1	−27.9 (10)	Tm2—O9—C17—O10	−21.7 (11)
O9—Tm2—O2—C1	−100.3 (12)	Tm2—O9—C17—C18	155.9 (5)
O13—Tm2—O2—C1	−151.1 (6)	O10—C17—C18—C23	−153.5 (7)
O20^iv—Tm2—O2—C1	124.6 (6)	O9—C17—C18—C23	28.7 (10)
O6—Tm2—O2—C1	31.8 (6)	O10—C17—C18—C19	32.2 (10)
O23ⁱⁱ—Tm2—O2—C1	−56.1 (6)	O9—C17—C18—C19	−145.6 (7)
O4ⁱ—Tm1—O5—C9	−36.3 (9)	C23—C18—C19—C20	0.6 (11)
O1—Tm1—O5—C9	18.1 (7)	C17—C18—C19—C20	175.1 (7)
O15ⁱ—Tm1—O5—C9	91.9 (7)	C18—C19—C20—C21	−0.7 (13)
O24ⁱⁱ—Tm1—O5—C9	−110.5 (7)	C19—C20—C21—C22	−0.2 (14)
O22ⁱⁱⁱ—Tm1—O5—C9	168.2 (7)	C20—C21—C22—C23	1.2 (13)
O21ⁱⁱⁱ—Tm1—O5—C9	174.4 (6)	C19—C18—C23—C22	0.4 (11)
O23ⁱⁱ—Tm1—O5—C9	−62.0 (7)	C17—C18—C23—C22	−173.8 (6)
C41ⁱⁱⁱ—Tm1—O5—C9	167.5 (7)	C19—C18—C23—C24	−175.0 (6)
C48ⁱⁱ—Tm1—O5—C9	−86.8 (7)	C17—C18—C23—C24	10.8 (11)
O9—Tm2—O6—C9	105.1 (7)	C21—C22—C23—C18	−1.3 (11)
O2—Tm2—O6—C9	−68.7 (7)	C21—C22—C23—C24	174.3 (7)
O13—Tm2—O6—C9	−158 (3)	Tm3ⁱⁱ—O12—C24—O11	−59.1 (13)
O20^iv—Tm2—O6—C9	−163.1 (7)	Tm3ⁱⁱ—O12—C24—C23	117.8 (9)
O23ⁱⁱ—Tm2—O6—C9	19.0 (7)	Tm4ⁱⁱ—O11—C24—O12	38.9 (11)
O2—Tm2—O9—C17	−103.5 (12)	Tm4ⁱⁱ—O11—C24—C23	−138.0 (6)
O13—Tm2—O9—C17	−52.7 (7)	C18—C23—C24—O12	50.0 (9)
O20^iv—Tm2—O9—C17	31.7 (7)	C22—C23—C24—O12	−125.5 (7)
O6—Tm2—O9—C17	124.5 (7)	C18—C23—C24—O11	−132.9 (7)
O23ⁱⁱ—Tm2—O9—C17	−147.8 (7)	C22—C23—C24—O11	51.6 (9)
O12ⁱⁱ—Tm3—O10—C17	−119.9 (13)	Tm2—O13—C25—O14	8.4 (12)
O17—Tm3—O10—C17	84.6 (13)	Tm2—O13—C25—C26	−166.0 (5)
O14—Tm3—O10—C17	29.3 (12)	Tm3—O14—C25—O13	−39.0 (11)
O7ⁱⁱ—Tm3—O10—C17	162.3 (13)	Tm3—O14—C25—C26	135.4 (6)
O19^iv—Tm3—O10—C17	−50.3 (13)	O13—C25—C26—C27	98.5 (7)
O8ⁱⁱ—Tm3—O10—C17	108.7 (13)	O14—C25—C26—C27	−76.4 (8)
C16ⁱⁱ—Tm3—O10—C17	136.4 (13)	O13—C25—C26—C31	−78.8 (8)
O20^iv—Tm3—O10—C17	−42.9 (12)	O14—C25—C26—C31	106.2 (7)
O18—Tm3—O10—C17	−166.1 (11)	C31—C26—C27—C28	0.4 (10)
C33—Tm3—O10—C17	133.8 (11)	C25—C26—C27—C28	−177.0 (7)
O9—Tm2—O13—C25	70.2 (7)	C26—C27—C28—C29	1.5 (12)
O2—Tm2—O13—C25	−116.2 (7)	C27—C28—C29—C30	−1.0 (13)
O20^iv—Tm2—O13—C25	−21.7 (7)	C28—C29—C30—C31	−1.6 (12)
O6—Tm2—O13—C25	−26 (4)	C27—C26—C31—C30	−2.9 (9)
O23ⁱⁱ—Tm2—O13—C25	156.2 (7)	C25—C26—C31—C30	174.4 (6)
O12ⁱⁱ—Tm3—O14—C25	57.0 (9)	C27—C26—C31—C32	174.7 (6)
O10—Tm3—O14—C25	−19.7 (8)	C25—C26—C31—C32	−8.1 (9)
O17—Tm3—O14—C25	−172.9 (8)	C29—C30—C31—C26	3.5 (10)
O7ⁱⁱ—Tm3—O14—C25	−101.5 (8)	C29—C30—C31—C32	−174.1 (7)
O19^iv—Tm3—O14—C25	103.7 (8)	Tm1ⁱ—O15—C32—O16	35.3 (9)
O8ⁱⁱ—Tm3—O14—C25	−96.0 (8)	Tm1ⁱ—O15—C32—C31	−145.6 (5)
C16ⁱⁱ—Tm3—O14—C25	−94.8 (8)	Tm4^iv—O16—C32—O15	23.4 (13)
O20^iv—Tm3—O14—C25	55.0 (7)	Tm4^iv—O16—C32—C31	−155.8 (6)
O18—Tm3—O14—C25	168.5 (7)	C26—C31—C32—O15	154.0 (6)
C33—Tm3—O14—C25	−179.0 (7)	C30—C31—C32—O15	−28.4 (9)
O12ⁱⁱ—Tm3—O17—C33	−13.4 (5)	C26—C31—C32—O16	−26.8 (9)
O10—Tm3—O17—C33	137.0 (4)	C30—C31—C32—O16	150.8 (6)
O14—Tm3—O17—C33	−165.0 (5)	Tm4—O18—C33—O17	−179.0 (6)
O7ⁱⁱ—Tm3—O17—C33	59.5 (4)	Tm3—O18—C33—O17	−10.2 (6)
O19^iv—Tm3—O17—C33	−80.1 (4)	Tm4—O18—C33—C34	−5.9 (13)
O8ⁱⁱ—Tm3—O17—C33	112.9 (4)	Tm3—O18—C33—C34	162.9 (6)
C16ⁱⁱ—Tm3—O17—C33	86.6 (4)	Tm4—O18—C33—Tm3	−168.8 (9)
O20^iv—Tm3—O17—C33	−108.1 (4)	Tm3—O17—C33—O18	13.3 (7)
O18—Tm3—O17—C33	−6.7 (4)	Tm3—O17—C33—C34	−160.1 (4)
O11ⁱⁱ—Tm4—O18—C33	175.0 (9)	O12ⁱⁱ—Tm3—C33—O18	0.6 (4)
O3^iv—Tm4—O18—C33	9.4 (9)	O10—Tm3—C33—O18	104.4 (6)
O21—Tm4—O18—C33	89.6 (10)	O17—Tm3—C33—O18	−168.0 (7)
O16^iv—Tm4—O18—C33	−65.6 (10)	O14—Tm3—C33—O18	−153.3 (4)
O25—Tm4—O18—C33	−109.8 (9)	O7ⁱⁱ—Tm3—C33—O18	74.9 (4)
O26—Tm4—O18—C33	91.8 (9)	O19^iv—Tm3—C33—O18	−72.1 (4)
O11ⁱⁱ—Tm4—O18—Tm3	9.2 (3)	O8ⁱⁱ—Tm3—C33—O18	128.8 (4)
O3^iv—Tm4—O18—Tm3	−156.5 (3)	C16ⁱⁱ—Tm3—C33—O18	101.8 (4)
O21—Tm4—O18—Tm3	−76.3 (4)	O20^iv—Tm3—C33—O18	−79.6 (4)
O16^iv—Tm4—O18—Tm3	128.6 (3)	O12ⁱⁱ—Tm3—C33—O17	168.6 (4)
O25—Tm4—O18—Tm3	84.4 (3)	O10—Tm3—C33—O17	−87.7 (7)
O26—Tm4—O18—Tm3	−74.1 (3)	O14—Tm3—C33—O17	14.7 (4)
O12ⁱⁱ—Tm3—O18—C33	−179.4 (4)	O7ⁱⁱ—Tm3—C33—O17	−117.2 (4)
O10—Tm3—O18—C33	−131.2 (5)	O19^iv—Tm3—C33—O17	95.8 (4)
O17—Tm3—O18—C33	6.5 (4)	O8ⁱⁱ—Tm3—C33—O17	−63.2 (4)
O14—Tm3—O18—C33	30.9 (4)	C16ⁱⁱ—Tm3—C33—O17	−90.2 (4)
O7ⁱⁱ—Tm3—O18—C33	−97.5 (4)	O20^iv—Tm3—C33—O17	88.4 (4)
O19^iv—Tm3—O18—C33	101.6 (4)	O18—Tm3—C33—O17	168.0 (7)
O8ⁱⁱ—Tm3—O18—C33	−52.0 (4)	O12ⁱⁱ—Tm3—C33—C34	−139.0 (11)
C16ⁱⁱ—Tm3—O18—C33	−76.1 (4)	O10—Tm3—C33—C34	−35.2 (14)
O20^iv—Tm3—O18—C33	115.8 (4)	O17—Tm3—C33—C34	52.4 (11)
O12ⁱⁱ—Tm3—O18—Tm4	−6.6 (3)	O14—Tm3—C33—C34	67.1 (11)
O10—Tm3—O18—Tm4	41.5 (5)	O7ⁱⁱ—Tm3—C33—C34	−64.7 (11)
O17—Tm3—O18—Tm4	179.2 (4)	O19^iv—Tm3—C33—C34	148.3 (12)
O14—Tm3—O18—Tm4	−156.3 (2)	O8ⁱⁱ—Tm3—C33—C34	−10.8 (11)
O7ⁱⁱ—Tm3—O18—Tm4	75.3 (3)	C16ⁱⁱ—Tm3—C33—C34	−37.8 (11)
O19^iv—Tm3—O18—Tm4	−85.7 (3)	O20^iv—Tm3—C33—C34	140.8 (11)
O8ⁱⁱ—Tm3—O18—Tm4	120.7 (3)	O18—Tm3—C33—C34	−139.6 (13)
C16ⁱⁱ—Tm3—O18—Tm4	96.7 (3)	O18—C33—C34—C35	−99.9 (8)
O20^iv—Tm3—O18—Tm4	−71.4 (3)	O17—C33—C34—C35	73.3 (8)
C33—Tm3—O18—Tm4	172.7 (6)	Tm3—C33—C34—C35	32.4 (15)
O11ⁱⁱ—Tm4—O21—C41	22.2 (6)	O18—C33—C34—C39	79.7 (9)
O3^iv—Tm4—O21—C41	−174.6 (6)	O17—C33—C34—C39	−107.0 (7)
O18—Tm4—O21—C41	108.0 (7)	Tm3—C33—C34—C39	−147.9 (9)
O16^iv—Tm4—O21—C41	−91.3 (6)	C39—C34—C35—C36	−0.1 (11)
O25—Tm4—O21—C41	−46.2 (7)	C33—C34—C35—C36	179.6 (7)
O26—Tm4—O21—C41	105.8 (6)	C34—C35—C36—C37	1.8 (13)
O11ⁱⁱ—Tm4—O21—Tm1^v	160.1 (2)	C35—C36—C37—C38	−1.9 (13)
O3^iv—Tm4—O21—Tm1^v	−36.7 (2)	C36—C37—C38—C39	0.2 (12)
O18—Tm4—O21—Tm1^v	−114.2 (3)	C37—C38—C39—C34	1.6 (11)
O16^iv—Tm4—O21—Tm1^v	46.5 (2)	C37—C38—C39—C40	−177.5 (7)
O25—Tm4—O21—Tm1^v	91.6 (3)	C35—C34—C39—C38	−1.6 (10)
O26—Tm4—O21—Tm1^v	−116.3 (3)	C33—C34—C39—C38	178.7 (6)
Tm2—O2—C1—O1	21.3 (10)	C35—C34—C39—C40	177.5 (6)
Tm2—O2—C1—C2	−154.8 (5)	C33—C34—C39—C40	−2.2 (10)
Tm1—O1—C1—O2	41.8 (14)	Tm3^iv—O19—C40—O20	−6.7 (7)
Tm1—O1—C1—C2	−142.0 (8)	Tm3^iv—O19—C40—C39	173.4 (5)
O2—C1—C2—C7	−11.8 (10)	Tm2^iv—O20—C40—O19	−134.8 (7)
O1—C1—C2—C7	171.7 (6)	Tm3^iv—O20—C40—O19	5.5 (6)
O2—C1—C2—C3	162.8 (7)	Tm2^iv—O20—C40—C39	45.1 (11)
O1—C1—C2—C3	−13.7 (10)	Tm3^iv—O20—C40—C39	−174.6 (6)
C7—C2—C3—C4	2.2 (11)	C38—C39—C40—O19	−160.5 (6)
C1—C2—C3—C4	−172.5 (7)	C34—C39—C40—O19	20.4 (10)
C2—C3—C4—C5	2.1 (13)	C38—C39—C40—O20	19.6 (9)
C3—C4—C5—C6	−4.3 (14)	C34—C39—C40—O20	−159.4 (6)
C4—C5—C6—C7	2.1 (13)	Tm1^v—O22—C41—O21	−14.6 (6)
C3—C2—C7—C6	−4.3 (10)	Tm1^v—O22—C41—C42	156.4 (5)
C1—C2—C7—C6	170.3 (6)	Tm4—O21—C41—O22	158.9 (5)
C3—C2—C7—C8	169.9 (7)	Tm1^v—O21—C41—O22	13.6 (6)
C1—C2—C7—C8	−15.5 (10)	Tm4—O21—C41—C42	−11.9 (10)
C5—C6—C7—C2	2.2 (11)	Tm1^v—O21—C41—C42	−157.2 (5)
C5—C6—C7—C8	−172.4 (7)	Tm4—O21—C41—Tm1^v	145.3 (6)
Tm4^iv—O3—C8—O4	−27.1 (10)	O22—C41—C42—C43	−75.5 (8)
Tm4^iv—O3—C8—C7	148.1 (5)	O21—C41—C42—C43	95.5 (7)
Tm1ⁱ—O4—C8—O3	64.5 (12)	Tm1^v—C41—C42—C43	−2.6 (16)
Tm1ⁱ—O4—C8—C7	−110.8 (8)	O22—C41—C42—C47	105.0 (8)
C2—C7—C8—O3	113.1 (8)	O21—C41—C42—C47	−84.0 (8)
C6—C7—C8—O3	−72.4 (9)	Tm1^v—C41—C42—C47	177.9 (9)
C2—C7—C8—O4	−71.3 (9)	C47—C42—C43—C44	0.6 (11)
C6—C7—C8—O4	103.2 (7)	C41—C42—C43—C44	−178.9 (7)
Tm2—O6—C9—O5	−11.6 (11)	C42—C43—C44—C45	−2.8 (12)
Tm2—O6—C9—C10	164.1 (5)	C43—C44—C45—C46	2.6 (12)
Tm1—O5—C9—O6	48.3 (11)	C44—C45—C46—C47	−0.3 (12)
Tm1—O5—C9—C10	−127.5 (6)	C45—C46—C47—C42	−1.9 (11)
O6—C9—C10—C11	−99.1 (7)	C45—C46—C47—C48	178.9 (7)
O5—C9—C10—C11	76.9 (7)	C43—C42—C47—C46	1.7 (10)
O6—C9—C10—C15	81.8 (8)	C41—C42—C47—C46	−178.8 (6)
O5—C9—C10—C15	−102.2 (8)	C43—C42—C47—C48	−179.1 (6)
C15—C10—C11—C12	−0.2 (10)	C41—C42—C47—C48	0.4 (10)
C9—C10—C11—C12	−179.4 (6)	Tm1ⁱⁱ—O24—C48—O23	7.2 (7)
C10—C11—C12—C13	−1.4 (11)	Tm1ⁱⁱ—O24—C48—C47	−171.4 (5)
C11—C12—C13—C14	1.9 (12)	Tm2ⁱⁱ—O23—C48—O24	130.9 (8)
C12—C13—C14—C15	−0.8 (12)	Tm1ⁱⁱ—O23—C48—O24	−5.7 (6)
C11—C10—C15—C14	1.2 (9)	Tm2ⁱⁱ—O23—C48—C47	−50.5 (13)
C9—C10—C15—C14	−179.7 (6)	Tm1ⁱⁱ—O23—C48—C47	172.8 (6)
C11—C10—C15—C16	−179.9 (6)	Tm2ⁱⁱ—O23—C48—Tm1ⁱⁱ	136.7 (9)
C9—C10—C15—C16	−0.8 (9)	C46—C47—C48—O24	170.4 (6)
C13—C14—C15—C10	−0.8 (10)	C42—C47—C48—O24	−8.8 (9)
C13—C14—C15—C16	−179.7 (6)	C46—C47—C48—O23	−8.2 (10)
Tm3ⁱⁱ—O8—C16—O7	−13.5 (6)	C42—C47—C48—O23	172.7 (6)
Tm3ⁱⁱ—O8—C16—C15	163.1 (5)	C46—C47—C48—Tm1ⁱⁱ	143.9 (15)
Tm3ⁱⁱ—O7—C16—O8	13.9 (6)	C42—C47—C48—Tm1ⁱⁱ	−35 (2)
Tm3ⁱⁱ—O7—C16—C15	−162.7 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O25—H25A···O14^iv	0.82 (1)	2.06 (2)	2.872 (7)	169 (9)
O25—H25B···O17^iv	0.82 (1)	2.32 (7)	2.729 (7)	111 (6)
O25—H25B···O19^iv	0.82 (1)	2.45 (3)	3.232 (7)	161 (7)
O26—H26A···O7ⁱⁱ	0.82 (1)	2.08 (5)	2.822 (7)	151 (9)
O26—H26B···O22^vi	0.82 (1)	2.40 (2)	3.208 (7)	168 (9)
O26—H26B···O5ⁱⁱ	0.82 (1)	2.62 (6)	3.072 (7)	116 (5)

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

Experimental details

Crystal data
Chemical formula	[Tm₄(C₈H₄O₄)₆(H₂O)₂]
M_r	1696.42
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	12.5716 (4), 13.7737 (2), 15.8867 (3)
α, β, γ (°)	75.301 (4), 69.112 (2), 65.617 (2)
V (Å³)	2322.45 (9)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	7.67
Crystal size (mm)	0.30 × 0.14 × 0.02

Data collection
Diffractometer	Bruker APEX area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.207, 0.862
No. of measured, independent and observed [I > 2σ(I)] reflections	18519, 9421, 8260
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.628

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.042, 0.108, 1.02
No. of reflections	9421
No. of parameters	715
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	2.34, −2.67

Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O25—H25A···O14ⁱ	0.824 (10)	2.06 (2)	2.872 (7)	169 (9)
O25—H25B···O17ⁱ	0.821 (10)	2.32 (7)	2.729 (7)	111 (6)
O25—H25B···O19ⁱ	0.821 (10)	2.45 (3)	3.232 (7)	161 (7)
O26—H26A···O7ⁱⁱ	0.816 (10)	2.08 (5)	2.822 (7)	151 (9)
O26—H26B···O22ⁱⁱⁱ	0.817 (10)	2.40 (2)	3.208 (7)	168 (9)
O26—H26B···O5ⁱⁱ	0.817 (10)	2.62 (6)	3.072 (7)	116 (5)

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

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