Tricaesium tris-(pyridine-2,6-dicarboxyl-ato-κO,N,O)lutetium(III) octa-hydrate.

Colourless block crystals of the title compound, Cs(3)[Lu(dipic)(3)]·8H(2)O [dipic is dipicolinate or pyridine-2,6-dicarboxyl-ate, C(7)H(3)NO(4)] were synthesized by slow evaporation of the solvent. The crystal structure of this Lu(III)-complex, isostructural with the Dy(III) and Eu(III) complexes, was determined from a crystal twinned by inversion and consists of discrete [Lu(dipic)(3)](3-) anions, Cs(+) cations and water mol-ecules involving hydrogen bonding. The Lu atom lies on a twofold rotation axis and is coordinated by six O atoms and three N atoms of three dipicolinate ligands. One Cs atom is also on a twofold axis. The unit cell can be regarded as successive layers along the crystallographic c-axis formed by [Lu(dipic)(3)](3-) anionic planes and [Cs(+), H(2)O] cationic planes. In the crystal structure, although the H atoms attached to water mol-ecules could not be located, short O-O contacts clearly indicate the occurrence of an intricate hydrogen-bonded network through contacts with other water mol-ecules, Cs cations or with the O atoms of the dipicolinate ligands.

Related literature

For potential applications of lanthanide complexes as second-order non-linear optical materials, see: Tancrez et al. (2005 ▶); Sénéchal et al. (2004 ▶). For the isostructural EuIII complex, see: Brayshaw et al. (1995 ▶). For other related complexes, see: Murray et al. (1990 ▶). For related literature, see: Flack & Bernardinelli (1999 ▶, 2000 ▶).

Experimental

Crystal data

Cs3[Lu(C7H3NO4)3]·8H2O

M = 1213.14

Orthorhombic,

a = 10.0406 (2) Å

b = 17.8109 (6) Å

c = 18.4221 (5) Å

V = 3294.46 (16) Å3

Z = 4

Mo Kα radiation

μ = 6.36 mm−1

T = 100 (2) K

0.20 × 0.19 × 0.19 mm

Data collection

Oxford Diffraction Xcalibur–Sapphire3 diffractometer

Absorption correction: Gaussian (ABSORB; DeTitta, 1985 ▶) T min = 0.307, T max = 0.425

51066 measured reflections

3520 independent reflections

3491 reflections with I > 2σ(I)

R int = 0.045

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.063

S = 1.46

3520 reflections

208 parameters

H-atom parameters constrained

Δρmax = 3.00 e Å−3

Δρmin = −0.94 e Å−3

Absolute structure: Flack (1983 ▶), 1501 Friedel pairs

Flack parameter: 0.270 (12)

Data collection: CrysAlis CCD (Oxford Diffraction 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction 2006 ▶); data reduction: SORTAV (Blessing, 1989 ▶); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808029243/dn2357sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808029243/dn2357Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Cs3[Lu(C7H3NO4)3]·8H2O	F(000) = 2312
Mr = 1213.14	Dx = 2.446 Mg m−3
Orthorhombic, C2221	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c 2	Cell parameters from 17659 reflections
a = 10.0406 (2) Å	θ = 3.2–59.9°
b = 17.8109 (6) Å	µ = 6.36 mm−1
c = 18.4221 (5) Å	T = 100 K
V = 3294.46 (16) Å3	Block, colourless
Z = 4	0.20 × 0.19 × 0.19 mm

Oxford Diffraction Xcalibur-Sapphire3 diffractometer	3520 independent reflections
Radiation source: fine-focus sealed tube	3491 reflections with I > 2σ(I)
graphite	Rint = 0.045
ω scans	θmax = 27.0°, θmin = 3.2°
Absorption correction: gaussian (ABSORB; DeTitta, 1985)	h = −12→12
Tmin = 0.308, Tmax = 0.425	k = −22→22
51066 measured reflections	l = −23→23

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)] = 0.025	H-atom parameters constrained
wR(F2) = 0.063	w = 1/[σ2(Fo2) + (0.0149P)2 + 27.044P] where P = (Fo2 + 2Fc2)/3
S = 1.46	(Δ/σ)max < 0.001
3520 reflections	Δρmax = 3.00 e Å−3
208 parameters	Δρmin = −0.94 e Å−3
0 restraints	Absolute structure: Flack (1983),1501 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.270 (12)

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Lu1	0.75054 (5)	0.0000	0.0000	0.00950 (7)
Cs1	0.74407 (4)	0.021678 (17)	−0.24335 (2)	0.01702 (8)
Cs2	0.5000	−0.26389 (3)	−0.2500	0.01796 (11)
N11	0.8713 (4)	−0.1197 (2)	−0.0042 (3)	0.0107 (8)
O11	0.6846 (4)	−0.0835 (2)	−0.0950 (2)	0.0149 (8)
O12	0.7226 (5)	−0.1846 (3)	−0.1649 (2)	0.0228 (12)
O13	1.0389 (5)	−0.0907 (3)	0.1601 (2)	0.0174 (11)
O14	0.9174 (4)	−0.01382 (19)	0.0906 (2)	0.0124 (8)
C12	0.9612 (6)	−0.1355 (3)	0.0466 (3)	0.0131 (12)
C13	1.0349 (6)	−0.2016 (3)	0.0468 (3)	0.0187 (13)
H13	1.1001	−0.2089	0.0819	0.022*
C14	1.0140 (14)	−0.2518 (3)	−0.0006 (8)	0.040 (2)
H14	1.0567	−0.2980	0.0026	0.048*
C15	0.9185 (7)	−0.2357 (4)	−0.0624 (3)	0.0199 (13)
H15	0.9073	−0.2688	−0.1010	0.024*
C16	0.8496 (6)	−0.1693 (3)	−0.0580 (3)	0.0132 (11)
C17	0.7438 (8)	−0.1440 (3)	−0.1112 (3)	0.0146 (6)
C18	0.9756 (6)	−0.0754 (3)	0.1041 (4)	0.0146 (6)
N21	0.5071 (8)	0.0000	0.0000	0.0173 (12)
O21	0.4794 (7)	−0.1104 (3)	0.1573 (3)	0.0323 (15)
O22	0.6543 (5)	−0.0785 (2)	0.0880 (2)	0.0168 (9)
C22	0.4415 (7)	−0.0390 (4)	0.0490 (3)	0.0242 (9)
C23	0.3047 (7)	−0.0426 (4)	0.0509 (3)	0.0242 (9)
H23	0.2584	−0.0719	0.0843	0.029*
C24	0.2430 (13)	0.0000	0.0000	0.0242 (9)
H24	0.1503	0.0000	0.0000	0.029*
C25	0.5310 (6)	−0.0805 (4)	0.1040 (4)	0.0146 (6)
O1W	0.7467 (9)	−0.1739 (4)	−0.3818 (4)	0.0584 (17)
O2W	0.9514 (7)	−0.0907 (4)	−0.3228 (4)	0.0424 (18)
O3W	0.5456 (5)	−0.0888 (3)	−0.3207 (3)	0.0240 (12)
O4WA	0.6970 (8)	0.2031 (4)	−0.2207 (6)	0.032 (3)	0.69 (2)
O4WB	0.7228 (15)	0.1956 (8)	−0.1715 (11)	0.023 (6)	0.31 (2)

	U11	U22	U33	U12	U13	U23
Lu1	0.00740 (14)	0.01013 (12)	0.01097 (13)	0.000	0.000	−0.00081 (10)
Cs1	0.01540 (16)	0.02237 (15)	0.01327 (15)	−0.00244 (13)	0.00109 (19)	−0.00051 (11)
Cs2	0.0245 (3)	0.01430 (19)	0.0151 (2)	0.000	−0.0028 (2)	0.000
N11	0.008 (2)	0.0127 (18)	0.011 (2)	−0.0017 (15)	0.0012 (18)	0.0004 (17)
O11	0.013 (2)	0.013 (2)	0.018 (2)	−0.0015 (16)	−0.0019 (16)	−0.0004 (16)
O12	0.023 (4)	0.023 (2)	0.022 (2)	0.0013 (18)	−0.0084 (19)	−0.0097 (17)
O13	0.019 (3)	0.023 (3)	0.010 (2)	0.0014 (18)	−0.0035 (16)	0.0022 (17)
O14	0.010 (2)	0.008 (2)	0.018 (2)	0.0010 (14)	−0.0021 (15)	−0.0017 (14)
C12	0.015 (3)	0.011 (2)	0.014 (3)	−0.0009 (19)	0.001 (2)	0.002 (2)
C13	0.018 (4)	0.017 (3)	0.021 (3)	0.004 (2)	−0.004 (2)	0.001 (2)
C14	0.033 (6)	0.023 (3)	0.066 (5)	−0.003 (3)	−0.040 (5)	0.009 (3)
C15	0.026 (4)	0.018 (3)	0.016 (3)	0.007 (3)	−0.002 (2)	−0.005 (2)
C16	0.015 (3)	0.012 (3)	0.012 (3)	−0.002 (2)	0.003 (2)	0.001 (2)
C17	0.0135 (16)	0.0138 (13)	0.0166 (13)	−0.0096 (16)	0.0027 (15)	−0.0028 (10)
C18	0.0135 (16)	0.0138 (13)	0.0166 (13)	−0.0096 (16)	0.0027 (15)	−0.0028 (10)
N21	0.009 (3)	0.027 (3)	0.016 (3)	0.000	0.000	−0.010 (3)
O21	0.038 (4)	0.039 (3)	0.021 (2)	−0.021 (3)	0.014 (2)	−0.009 (2)
O22	0.020 (3)	0.013 (2)	0.0168 (19)	−0.0027 (17)	0.0040 (17)	−0.0020 (15)
C22	0.0106 (19)	0.048 (2)	0.0143 (17)	−0.007 (2)	0.0024 (15)	−0.0146 (17)
C23	0.0106 (19)	0.048 (2)	0.0143 (17)	−0.007 (2)	0.0024 (15)	−0.0146 (17)
C24	0.0106 (19)	0.048 (2)	0.0143 (17)	−0.007 (2)	0.0024 (15)	−0.0146 (17)
C25	0.0135 (16)	0.0138 (13)	0.0166 (13)	−0.0096 (16)	0.0027 (15)	−0.0028 (10)
O1W	0.046 (4)	0.079 (5)	0.051 (3)	0.016 (5)	−0.002 (4)	−0.012 (3)
O2W	0.047 (4)	0.021 (3)	0.059 (4)	0.003 (3)	0.028 (3)	0.001 (3)
O3W	0.018 (3)	0.032 (3)	0.022 (3)	−0.004 (2)	−0.005 (2)	0.004 (2)
O4WA	0.028 (4)	0.030 (4)	0.039 (6)	−0.002 (3)	−0.003 (3)	0.007 (3)
O4WB	0.012 (11)	0.018 (7)	0.038 (13)	0.005 (5)	0.011 (7)	0.015 (6)

Lu1—O22i	2.348 (4)	O11—C17	1.267 (8)
Lu1—O22	2.348 (4)	O12—C17	1.244 (7)
Lu1—O14	2.377 (4)	O13—C18	1.242 (9)
Lu1—O14i	2.377 (4)	O13—Cs1ix	3.070 (5)
Lu1—O11	2.390 (4)	O13—Cs2x	3.100 (5)
Lu1—O11i	2.390 (4)	O13—Cs1i	3.553 (5)
Lu1—N21	2.445 (8)	O14—C18	1.267 (8)
Lu1—N11i	2.454 (4)	O14—Cs1i	3.312 (4)
Lu1—N11	2.454 (4)	C12—C13	1.390 (8)
Lu1—Cs1	4.5002 (4)	C12—C18	1.513 (8)
Lu1—Cs1i	4.5002 (4)	C13—C14	1.267 (13)
Cs1—O13ii	3.070 (5)	C13—Cs2x	3.810 (6)
Cs1—O3W	3.142 (5)	C13—H13	0.9300
Cs1—O22i	3.167 (4)	C14—C15	1.517 (12)
Cs1—O2W	3.237 (6)	C14—H14	0.9300
Cs1—O4WA	3.293 (8)	C15—C16	1.373 (9)
Cs1—O21iii	3.299 (6)	C15—H15	0.9300
Cs1—O14i	3.312 (4)	C16—C17	1.514 (9)
Cs1—O11	3.367 (4)	C18—Cs1i	3.592 (6)
Cs1—O4WB	3.375 (16)	N21—C22i	1.315 (8)
Cs1—O21i	3.474 (6)	N21—C22	1.315 (8)
Cs1—C25i	3.502 (6)	O21—C25	1.230 (9)
Cs1—O13i	3.553 (5)	O21—Cs1xi	3.299 (6)
Cs2—O12	3.073 (5)	O21—Cs1i	3.474 (6)
Cs2—O12iv	3.073 (5)	O22—C25	1.273 (8)
Cs2—O13v	3.100 (5)	O22—Cs1i	3.167 (4)
Cs2—O13vi	3.100 (5)	C22—C23	1.376 (10)
Cs2—O4WAvii	3.145 (8)	C22—C25	1.544 (10)
Cs2—O4WAviii	3.145 (8)	C23—C24	1.356 (9)
Cs2—O4WBvii	3.219 (14)	C23—Cs1xi	3.840 (6)
Cs2—O4WBviii	3.219 (14)	C23—H23	0.9300
Cs2—O3W	3.410 (6)	C24—C23i	1.356 (9)
Cs2—O3Wiv	3.410 (6)	C24—H24	0.9300
Cs2—C13v	3.810 (6)	C25—Cs1i	3.502 (6)
Cs2—C13vi	3.810 (6)	O3W—Cs1iv	3.705 (6)
N11—C12	1.330 (7)	O4WA—Cs2xii	3.145 (8)
N11—C16	1.345 (7)	O4WB—Cs2xii	3.219 (14)
O22i—Lu1—O22	131.4 (2)	O13v—Cs2—O4WAviii	82.77 (19)
O22i—Lu1—O14	146.72 (14)	O13vi—Cs2—O4WAviii	79.26 (18)
O22—Lu1—O14	75.16 (15)	O4WAvii—Cs2—O4WAviii	158.5 (3)
O22i—Lu1—O14i	75.16 (15)	O12—Cs2—O4WBvii	120.2 (4)
O22—Lu1—O14i	146.72 (14)	O12iv—Cs2—O4WBvii	72.8 (3)
O14—Lu1—O14i	90.4 (2)	O13v—Cs2—O4WBvii	86.8 (3)
O22i—Lu1—O11	75.58 (13)	O13vi—Cs2—O4WBvii	71.4 (3)
O22—Lu1—O11	91.20 (14)	O4WAvii—Cs2—O4WBvii	17.2 (3)
O14—Lu1—O11	130.16 (14)	O4WAviii—Cs2—O4WBvii	150.6 (3)
O14i—Lu1—O11	75.28 (14)	O12—Cs2—O4WBviii	72.8 (3)
O22i—Lu1—O11i	91.20 (14)	O12iv—Cs2—O4WBviii	120.2 (4)
O22—Lu1—O11i	75.58 (13)	O13v—Cs2—O4WBviii	71.4 (3)
O14—Lu1—O11i	75.28 (14)	O13vi—Cs2—O4WBviii	86.8 (3)
O14i—Lu1—O11i	130.16 (14)	O4WAvii—Cs2—O4WBviii	150.6 (3)
O11—Lu1—O11i	147.8 (2)	O4WAviii—Cs2—O4WBviii	17.2 (3)
O22i—Lu1—N21	65.71 (12)	O4WBvii—Cs2—O4WBviii	154.1 (5)
O22—Lu1—N21	65.71 (12)	O12—Cs2—O3W	71.14 (12)
O14—Lu1—N21	134.81 (10)	O12iv—Cs2—O3W	58.84 (12)
O14i—Lu1—N21	134.81 (10)	O13v—Cs2—O3W	125.24 (14)
O11—Lu1—N21	73.90 (11)	O13vi—Cs2—O3W	162.07 (13)
O11i—Lu1—N21	73.90 (11)	O4WAvii—Cs2—O3W	111.48 (18)
O22i—Lu1—N11i	73.00 (16)	O4WAviii—Cs2—O3W	88.59 (17)
O22—Lu1—N11i	134.33 (16)	O4WBvii—Cs2—O3W	119.5 (3)
O14—Lu1—N11i	73.72 (14)	O4WBviii—Cs2—O3W	85.3 (3)
O14i—Lu1—N11i	65.42 (14)	O12—Cs2—O3Wiv	58.84 (12)
O11—Lu1—N11i	134.47 (16)	O12iv—Cs2—O3Wiv	71.14 (12)
O11i—Lu1—N11i	64.75 (15)	O13v—Cs2—O3Wiv	162.07 (13)
N21—Lu1—N11i	119.60 (10)	O13vi—Cs2—O3Wiv	125.24 (14)
O22i—Lu1—N11	134.33 (16)	O4WAvii—Cs2—O3Wiv	88.59 (17)
O22—Lu1—N11	73.00 (16)	O4WAviii—Cs2—O3Wiv	111.48 (19)
O14—Lu1—N11	65.42 (14)	O4WBvii—Cs2—O3Wiv	85.3 (3)
O14i—Lu1—N11	73.72 (14)	O4WBviii—Cs2—O3Wiv	119.5 (3)
O11—Lu1—N11	64.75 (15)	O3W—Cs2—O3Wiv	47.76 (19)
O11i—Lu1—N11	134.47 (16)	O12—Cs2—C13v	129.96 (13)
N21—Lu1—N11	119.60 (10)	O12iv—Cs2—C13v	60.42 (13)
N11i—Lu1—N11	120.8 (2)	O13v—Cs2—C13v	47.80 (13)
O22i—Lu1—Cs1	41.88 (11)	O13vi—Cs2—C13v	113.68 (13)
O22—Lu1—Cs1	137.11 (11)	O4WAvii—Cs2—C13v	92.8 (2)
O14—Lu1—Cs1	135.91 (10)	O4WAviii—Cs2—C13v	83.7 (2)
O14i—Lu1—Cs1	45.74 (10)	O4WBvii—Cs2—C13v	109.0 (4)
O11—Lu1—Cs1	47.15 (10)	O4WBviii—Cs2—C13v	66.5 (4)
O11i—Lu1—Cs1	132.23 (10)	O3W—Cs2—C13v	77.57 (13)
N21—Lu1—Cs1	89.173 (8)	O3Wiv—Cs2—C13v	120.70 (13)
N11i—Lu1—Cs1	87.94 (12)	O12—Cs2—C13vi	60.42 (13)
N11—Lu1—Cs1	92.88 (12)	O12iv—Cs2—C13vi	129.96 (13)
O22i—Lu1—Cs1i	137.11 (11)	O13v—Cs2—C13vi	113.68 (13)
O22—Lu1—Cs1i	41.88 (11)	O13vi—Cs2—C13vi	47.80 (13)
O14—Lu1—Cs1i	45.74 (10)	O4WAvii—Cs2—C13vi	83.7 (2)
O14i—Lu1—Cs1i	135.91 (10)	O4WAviii—Cs2—C13vi	92.8 (2)
O11—Lu1—Cs1i	132.23 (10)	O4WBvii—Cs2—C13vi	66.5 (4)
O11i—Lu1—Cs1i	47.15 (10)	O4WBviii—Cs2—C13vi	109.0 (4)
N21—Lu1—Cs1i	89.173 (8)	O3W—Cs2—C13vi	120.70 (13)
N11i—Lu1—Cs1i	92.88 (12)	O3Wiv—Cs2—C13vi	77.57 (13)
N11—Lu1—Cs1i	87.94 (12)	C13v—Cs2—C13vi	161.41 (18)
Cs1—Lu1—Cs1i	178.347 (17)	C12—N11—C16	119.3 (5)
O13ii—Cs1—O3W	115.98 (14)	C12—N11—Lu1	119.8 (4)
O13ii—Cs1—O22i	126.72 (12)	C16—N11—Lu1	120.9 (4)
O3W—Cs1—O22i	115.44 (13)	C17—O11—Lu1	124.9 (4)
O13ii—Cs1—O2W	61.89 (12)	C17—O11—Cs1	101.4 (3)
O3W—Cs1—O2W	79.37 (13)	Lu1—O11—Cs1	101.50 (14)
O22i—Cs1—O2W	142.10 (16)	C17—O12—Cs2	142.9 (5)
O13ii—Cs1—O4WA	77.43 (18)	C18—O13—Cs1ix	139.2 (4)
O3W—Cs1—O4WA	125.53 (19)	C18—O13—Cs2x	124.2 (4)
O22i—Cs1—O4WA	62.0 (2)	Cs1ix—O13—Cs2x	96.56 (13)
O2W—Cs1—O4WA	139.14 (19)	C18—O13—Cs1i	81.8 (4)
O13ii—Cs1—O21iii	88.27 (12)	Cs1ix—O13—Cs1i	101.70 (14)
O3W—Cs1—O21iii	67.47 (13)	Cs2x—O13—Cs1i	87.33 (12)
O22i—Cs1—O21iii	98.92 (14)	C18—O14—Lu1	123.5 (4)
O2W—Cs1—O21iii	118.85 (19)	C18—O14—Cs1i	92.2 (4)
O4WA—Cs1—O21iii	60.2 (2)	Lu1—O14—Cs1i	103.33 (13)
O13ii—Cs1—O14i	97.84 (11)	N11—C12—C13	122.8 (5)
O3W—Cs1—O14i	133.79 (12)	N11—C12—C18	114.0 (5)
O22i—Cs1—O14i	52.77 (10)	C13—C12—C18	123.1 (5)
O2W—Cs1—O14i	91.16 (16)	C14—C13—C12	120.5 (7)
O4WA—Cs1—O14i	90.54 (19)	C14—C13—Cs2x	123.1 (7)
O21iii—Cs1—O14i	148.13 (12)	C12—C13—Cs2x	95.2 (4)
O13ii—Cs1—O11	144.99 (12)	C14—C13—H13	119.7
O3W—Cs1—O11	84.68 (12)	C12—C13—H13	119.7
O22i—Cs1—O11	52.66 (10)	Cs2x—C13—H13	50.1
O2W—Cs1—O11	97.89 (14)	C13—C14—C15	119.3 (7)
O4WA—Cs1—O11	114.7 (2)	C13—C14—H14	120.4
O21iii—Cs1—O11	126.59 (13)	C15—C14—H14	120.4
O14i—Cs1—O11	51.67 (10)	C16—C15—C14	115.9 (6)
O13ii—Cs1—O4WB	84.6 (3)	C16—C15—H15	122.1
O3W—Cs1—O4WB	135.4 (3)	C14—C15—H15	122.1
O22i—Cs1—O4WB	48.2 (3)	N11—C16—C15	121.9 (5)
O2W—Cs1—O4WB	141.8 (3)	N11—C16—C17	113.3 (5)
O4WA—Cs1—O4WB	16.4 (3)	C15—C16—C17	124.8 (5)
O21iii—Cs1—O4WB	74.7 (4)	O12—C17—O11	127.0 (7)
O14i—Cs1—O4WB	74.8 (4)	O12—C17—C16	117.5 (6)
O11—Cs1—O4WB	100.4 (3)	O11—C17—C16	115.5 (5)
O13ii—Cs1—O21i	128.72 (14)	O12—C17—Cs1	86.7 (3)
O3W—Cs1—O21i	90.39 (15)	O11—C17—Cs1	59.6 (3)
O22i—Cs1—O21i	39.15 (12)	C16—C17—Cs1	129.9 (4)
O2W—Cs1—O21i	168.30 (16)	O13—C18—O14	126.1 (6)
O4WA—Cs1—O21i	52.14 (18)	O13—C18—C12	118.4 (6)
O21iii—Cs1—O21i	61.01 (17)	O14—C18—C12	115.5 (5)
O14i—Cs1—O21i	91.90 (11)	O13—C18—Cs1i	78.2 (4)
O11—Cs1—O21i	75.32 (12)	O14—C18—Cs1i	67.2 (3)
O4WB—Cs1—O21i	49.9 (3)	C12—C18—Cs1i	128.8 (4)
O13ii—Cs1—C25i	137.62 (15)	C22i—N21—C22	119.9 (9)
O3W—Cs1—C25i	97.62 (14)	C22i—N21—Lu1	120.0 (4)
O22i—Cs1—C25i	21.25 (13)	C22—N21—Lu1	120.0 (4)
O2W—Cs1—C25i	155.39 (16)	C25—O21—Cs1xi	121.5 (5)
O4WA—Cs1—C25i	61.7 (2)	C25—O21—Cs1i	81.1 (4)
O21iii—Cs1—C25i	81.26 (15)	Cs1xi—O21—Cs1i	92.82 (13)
O14i—Cs1—C25i	73.18 (12)	C25—O22—Lu1	125.2 (4)
O11—Cs1—C25i	57.51 (13)	C25—O22—Cs1i	94.4 (4)
O4WB—Cs1—C25i	53.1 (3)	Lu1—O22—Cs1i	108.45 (15)
O21i—Cs1—C25i	20.31 (14)	N21—C22—C23	122.8 (7)
O13ii—Cs1—O13i	61.34 (14)	N21—C22—C25	114.3 (6)
O3W—Cs1—O13i	160.15 (13)	C23—C22—C25	122.8 (6)
O22i—Cs1—O13i	74.71 (11)	C24—C23—C22	114.3 (8)
O2W—Cs1—O13i	82.72 (16)	C24—C23—Cs1xi	124.7 (4)
O4WA—Cs1—O13i	74.07 (18)	C22—C23—Cs1xi	98.5 (4)
O21iii—Cs1—O13i	129.85 (12)	C24—C23—H23	122.8
O14i—Cs1—O13i	37.82 (10)	C22—C23—H23	122.8
O11—Cs1—O13i	89.41 (11)	Cs1xi—C23—H23	48.6
O4WB—Cs1—O13i	64.3 (3)	C23i—C24—C23	125.6 (11)
O21i—Cs1—O13i	106.43 (12)	C23i—C24—H24	117.2
C25i—Cs1—O13i	95.10 (14)	C23—C24—H24	117.2
O12—Cs2—O12iv	125.26 (18)	O21—C25—O22	127.3 (7)
O12—Cs2—O13v	138.44 (13)	O21—C25—C22	119.0 (6)
O12iv—Cs2—O13v	91.16 (13)	O22—C25—C22	113.6 (5)
O12—Cs2—O13vi	91.16 (13)	O21—C25—Cs1i	78.6 (4)
O12iv—Cs2—O13vi	138.44 (13)	O22—C25—Cs1i	64.4 (3)
O13v—Cs2—O13vi	66.60 (18)	C22—C25—Cs1i	133.9 (4)
O12—Cs2—O4WAvii	134.6 (2)	Cs1—O3W—Cs2	119.00 (16)
O12iv—Cs2—O4WAvii	58.0 (2)	Cs1—O3W—Cs1iv	91.19 (14)
O13v—Cs2—O4WAvii	79.26 (18)	Cs2—O3W—Cs1iv	104.99 (14)
O13vi—Cs2—O4WAvii	82.77 (19)	Cs2xii—O4WA—Cs1	91.3 (2)
O12—Cs2—O4WAviii	58.0 (2)	Cs2xii—O4WB—Cs1	88.6 (4)
O12iv—Cs2—O4WAviii	134.6 (2)