Poly[di-μ-aqua-di-aqua-bis-(μ7-oxalato-κ(9) O (1):O (1):O (1),O (2):O (2):O (2'):O (2'),O (1'):O (1'))calciumdicaesium].

In the title compound, [CaCs2(C2O4)2(H2O)4] n , the Ca(2+) ion, lying on a twofold rotation axis, is coordinated by four O atoms from two oxalate ligands and two bridging water mol-ecules in an octa-hedral geometry. The Cs(+) ion is coordinated by seven O atoms from six oxalate ligands, one bridging water and one terminal water mol-ecule. The oxalate ligand displays a scarce high denticity. The structure contains parallel chain units runnig along [10-1], formed by two edge-sharing Cs polyhedra connected by CsO9 polyhedra connected by a face-sharing CaO6 octahedron. These chains are further linked by the oxalate ligands to build up a three-dimensional framework. O-H⋯O hydrogen bonds involving the water mol-ecules and the carboxyl-ate O atoms enhance the extended structure.

Related literature

For related compounds or structures, see: Chen et al. (2008 ▶); Hursthouse et al. (2004 ▶); Kolitsch (2004 ▶); Price et al. (1999 ▶); Schwendtner & Kolitsch (2004 ▶); Wu & Liu (2010 ▶).

Experimental

Crystal data

[CaCs2(C2O4)2(H2O)4]

M = 554.00

Monoclinic,

a = 16.8808 (4) Å

b = 7.3212 (2) Å

c = 13.5268 (3) Å

β = 128.364 (1)°

V = 1310.79 (6) Å3

Z = 4

Mo Kα radiation

μ = 6.01 mm−1

T = 100 K

0.26 × 0.22 × 0.16 mm

Data collection

Agilent Xcalibur EOS CCD diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012 ▶) T min = 0.229, T max = 0.382

14337 measured reflections

2196 independent reflections

2189 reflections with I > 2σ(I)

R int = 0.056

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.060

S = 1.25

2196 reflections

104 parameters

6 restraints

All H-atom parameters refined

Δρmax = 1.65 e Å−3

Δρmin = −1.14 e Å−3

Data collection: CrysAlis PRO (Agilent, 2012 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: WinGX (Farrugia, 2012 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536813022654/hy2635sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813022654/hy2635Isup2.hkl

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

[CaCs2(C2O4)2(H2O)4]	F(000) = 1032
Mr = 554.00	Dx = 2.807 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1722 reflections
a = 16.8808 (4) Å	θ = 1.9–32.0°
b = 7.3212 (2) Å	µ = 6.01 mm−1
c = 13.5268 (3) Å	T = 100 K
β = 128.364 (1)°	Prismatic, pink
V = 1310.79 (6) Å3	0.26 × 0.22 × 0.16 mm
Z = 4

Agilent Xcalibur EOS CCD diffractometer	2196 independent reflections
Radiation source: fine-focus sealed tube	2189 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.056
w scans	θmax = 32.0°, θmin = 3.1°
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	h = −25→25
Tmin = 0.229, Tmax = 0.382	k = −10→10
14337 measured reflections	l = −20→20

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)] = 0.024	All H-atom parameters refined
wR(F2) = 0.060	w = 1/[σ2(Fo2) + (0.0199P)2 + 5.1138P] where P = (Fo2 + 2Fc2)/3
S = 1.25	(Δ/σ)max < 0.001
2196 reflections	Δρmax = 1.65 e Å−3
104 parameters	Δρmin = −1.14 e Å−3
6 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0048 (4)

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
Cs1	0.152844 (10)	0.314498 (19)	0.109026 (12)	0.01416 (8)
Ca1	0.0000	0.33665 (10)	0.2500	0.01801 (14)
C1	0.12874 (17)	0.1846 (3)	0.4980 (2)	0.0118 (4)
O1	0.06123 (14)	0.3069 (2)	0.43831 (17)	0.0135 (3)
O2	0.17036 (14)	0.1342 (3)	0.60819 (16)	0.0183 (3)
C2	0.15913 (16)	0.0871 (3)	0.4234 (2)	0.0114 (3)
O4	0.22599 (14)	−0.0311 (3)	0.47650 (17)	0.0179 (3)
O3	0.10886 (13)	0.1373 (2)	0.30886 (16)	0.0133 (3)
O1W	−0.03349 (15)	0.1582 (2)	−0.15099 (18)	0.0161 (3)
H1	−0.071 (3)	0.159 (6)	−0.133 (5)	0.033 (12)*
H2	−0.049 (4)	0.079 (5)	−0.202 (4)	0.037 (12)*
O2W	0.10155 (13)	0.5272 (2)	0.28003 (17)	0.0162 (3)
H3	0.088 (4)	0.632 (4)	0.254 (4)	0.027 (10)*
H4	0.154 (3)	0.532 (8)	0.351 (3)	0.050 (15)*

	U11	U22	U33	U12	U13	U23
Cs1	0.01329 (9)	0.01645 (10)	0.01254 (9)	−0.00098 (4)	0.00792 (7)	−0.00063 (4)
Ca1	0.0185 (3)	0.0180 (3)	0.0172 (3)	0.000	0.0109 (3)	0.000
C1	0.0101 (8)	0.0146 (9)	0.0100 (9)	−0.0015 (6)	0.0060 (7)	−0.0013 (6)
O1	0.0136 (7)	0.0154 (7)	0.0114 (7)	0.0021 (5)	0.0077 (6)	−0.0001 (5)
O2	0.0168 (7)	0.0263 (9)	0.0110 (7)	0.0042 (7)	0.0082 (6)	0.0034 (6)
C2	0.0111 (8)	0.0115 (8)	0.0113 (8)	−0.0003 (7)	0.0068 (7)	−0.0013 (6)
O4	0.0160 (7)	0.0200 (8)	0.0154 (7)	0.0066 (6)	0.0086 (6)	0.0012 (6)
O3	0.0151 (7)	0.0138 (7)	0.0110 (7)	0.0018 (6)	0.0082 (6)	0.0005 (5)
O1W	0.0188 (8)	0.0156 (7)	0.0158 (8)	−0.0026 (6)	0.0117 (7)	−0.0031 (6)
O2W	0.0132 (7)	0.0142 (7)	0.0154 (7)	−0.0014 (6)	0.0060 (6)	0.0022 (6)

Cs1—O2i	3.0837 (18)	Ca1—O1	2.0823 (18)
Cs1—O4ii	3.1206 (18)	C1—O2	1.246 (3)
Cs1—O1W	3.1369 (19)	C1—O1	1.269 (3)
Cs1—O1iii	3.2557 (18)	C1—C2	1.559 (3)
Cs1—O2iv	3.299 (2)	C2—O4	1.238 (3)
Cs1—O1v	3.3124 (17)	C2—O3	1.275 (3)
Cs1—O2W	3.318 (2)	O1W—H1	0.81 (3)
Cs1—O4iv	3.434 (2)	O1W—H2	0.81 (3)
Cs1—O3	3.4688 (17)	O2W—H3	0.82 (3)
Ca1—O2W	2.0456 (18)	O2W—H4	0.81 (3)
Ca1—O3	2.0797 (18)
O2i—Cs1—O4ii	93.63 (5)	O3iii—Ca1—C2iii	23.63 (6)
O2i—Cs1—O1W	163.78 (5)	O3—Ca1—C2iii	91.29 (7)
O4ii—Cs1—O1W	98.53 (5)	O1—Ca1—C2iii	115.82 (7)
O2i—Cs1—O1iii	110.34 (5)	O1iii—Ca1—C2iii	55.35 (6)
O4ii—Cs1—O1iii	146.74 (5)	C1iii—Ca1—C2iii	31.60 (6)
O1W—Cs1—O1iii	63.58 (5)	C1—Ca1—C2iii	110.84 (6)
O2i—Cs1—O2iv	96.06 (5)	O2Wiii—Ca1—C2	147.17 (7)
O4ii—Cs1—O2iv	106.19 (5)	O2W—Ca1—C2	91.60 (6)
O1W—Cs1—O2iv	70.28 (5)	O3iii—Ca1—C2	91.29 (7)
O1iii—Cs1—O2iv	94.20 (5)	O3—Ca1—C2	23.63 (6)
O2i—Cs1—O1v	115.89 (5)	O1—Ca1—C2	55.35 (6)
O4ii—Cs1—O1v	64.42 (5)	O1iii—Ca1—C2	115.82 (7)
O1W—Cs1—O1v	79.29 (5)	C1iii—Ca1—C2	110.84 (6)
O1iii—Cs1—O1v	84.04 (4)	C1—Ca1—C2	31.60 (6)
O2iv—Cs1—O1v	146.60 (4)	C2iii—Ca1—C2	100.91 (9)
O2i—Cs1—O2W	63.16 (5)	O2Wiii—Ca1—Cs1iii	54.62 (5)
O4ii—Cs1—O2W	127.09 (5)	O2W—Ca1—Cs1iii	129.31 (6)
O1W—Cs1—O2W	116.03 (5)	O3iii—Ca1—Cs1iii	58.85 (5)
O1iii—Cs1—O2W	53.63 (4)	O3—Ca1—Cs1iii	117.46 (5)
O2iv—Cs1—O2W	122.16 (4)	O1—Ca1—Cs1iii	52.98 (5)
O1v—Cs1—O2W	83.25 (4)	O1iii—Ca1—Cs1iii	126.43 (5)
O2i—Cs1—O4iv	109.66 (5)	C1iii—Ca1—Cs1iii	107.11 (5)
O4ii—Cs1—O4iv	59.65 (6)	C1—Ca1—Cs1iii	71.01 (5)
O1W—Cs1—O4iv	68.25 (5)	C2iii—Ca1—Cs1iii	79.22 (4)
O1iii—Cs1—O4iv	127.01 (4)	C2—Ca1—Cs1iii	97.83 (4)
O2iv—Cs1—O4iv	48.27 (4)	O2Wiii—Ca1—Cs1	129.31 (6)
O1v—Cs1—O4iv	107.77 (4)	O2W—Ca1—Cs1	54.62 (5)
O2W—Cs1—O4iv	168.93 (4)	O3iii—Ca1—Cs1	117.46 (5)
O2i—Cs1—O3	65.75 (5)	O3—Ca1—Cs1	58.85 (5)
O4ii—Cs1—O3	158.59 (4)	O1—Ca1—Cs1	126.43 (5)
O1W—Cs1—O3	100.76 (5)	O1iii—Ca1—Cs1	52.98 (5)
O1iii—Cs1—O3	53.03 (4)	C1iii—Ca1—Cs1	71.01 (5)
O2iv—Cs1—O3	72.14 (4)	C1—Ca1—Cs1	107.11 (5)
O1v—Cs1—O3	128.54 (4)	C2iii—Ca1—Cs1	97.83 (4)
O2W—Cs1—O3	50.03 (4)	C2—Ca1—Cs1	79.22 (4)
O4iv—Cs1—O3	120.07 (4)	Cs1iii—Ca1—Cs1	175.41 (2)
O2i—Cs1—C1iv	112.56 (5)	O2Wiii—Ca1—H3	80.6 (9)
O4ii—Cs1—C1iv	97.66 (5)	O2W—Ca1—H3	14.7 (9)
O1W—Cs1—C1iv	55.28 (5)	O3iii—Ca1—H3	161.3 (9)
O1iii—Cs1—C1iv	94.08 (4)	O3—Ca1—H3	102.5 (9)
O2iv—Cs1—C1iv	17.78 (4)	O1—Ca1—H3	102.7 (10)
O1v—Cs1—C1iv	128.86 (4)	O1iii—Ca1—H3	87.3 (10)
O2W—Cs1—C1iv	134.64 (5)	C1iii—Ca1—H3	110.7 (10)
O4iv—Cs1—C1iv	38.09 (4)	C1—Ca1—H3	107.0 (10)
O3—Cs1—C1iv	85.85 (4)	C2iii—Ca1—H3	141.0 (10)
O2i—Cs1—C1v	98.81 (5)	C2—Ca1—H3	106.2 (9)
O4ii—Cs1—C1v	56.66 (5)	Cs1iii—Ca1—H3	123.2 (10)
O1W—Cs1—C1v	96.84 (5)	Cs1—Ca1—H3	61.3 (10)
O1iii—Cs1—C1v	95.90 (5)	O2Wiii—Ca1—H4	100.2 (12)
O2iv—Cs1—C1v	157.84 (5)	O2W—Ca1—H4	16.9 (10)
O1v—Cs1—C1v	18.14 (4)	O3iii—Ca1—H4	169.1 (11)
O2W—Cs1—C1v	79.44 (5)	O3—Ca1—H4	79.6 (12)
O4iv—Cs1—C1v	110.71 (4)	O1—Ca1—H4	80.4 (10)
O3—Cs1—C1v	129.22 (4)	O1iii—Ca1—H4	106.6 (10)
C1iv—Cs1—C1v	141.18 (6)	C1iii—Ca1—H4	129.7 (10)
O2i—Cs1—C2iv	119.80 (5)	C1—Ca1—H4	78.8 (10)
O4ii—Cs1—C2iv	75.48 (5)	C2iii—Ca1—H4	159.8 (11)
O1W—Cs1—C2iv	54.11 (5)	C2—Ca1—H4	77.8 (11)
O1iii—Cs1—C2iv	109.27 (4)	Cs1iii—Ca1—H4	121.0 (11)
O2iv—Cs1—C2iv	37.89 (4)	Cs1—Ca1—H4	62.0 (11)
O1v—Cs1—C2iv	111.62 (4)	H3—Ca1—H4	29.4 (14)
O2W—Cs1—C2iv	157.40 (4)	O2—C1—O1	125.9 (2)
O4iv—Cs1—C2iv	17.93 (4)	O2—C1—C2	118.1 (2)
O3—Cs1—C2iv	108.86 (4)	O1—C1—C2	116.0 (2)
C1iv—Cs1—C2iv	23.10 (5)	O2—C1—Ca1	166.71 (17)
C1v—Cs1—C2iv	119.95 (4)	C2—C1—Ca1	74.64 (12)
O2i—Cs1—H1	154.3 (7)	O2—C1—Cs1vi	53.94 (13)
O4ii—Cs1—H1	111.6 (6)	O1—C1—Cs1vi	138.48 (15)
O1W—Cs1—H1	14.1 (5)	C2—C1—Cs1vi	79.72 (11)
O1iii—Cs1—H1	49.6 (5)	Ca1—C1—Cs1vi	130.00 (7)
O2iv—Cs1—H1	72.7 (8)	O2—C1—Cs1vii	88.32 (14)
O1v—Cs1—H1	81.2 (8)	O1—C1—Cs1vii	54.36 (11)
O2W—Cs1—H1	102.6 (6)	C2—C1—Cs1vii	133.18 (13)
O4iv—Cs1—H1	80.5 (6)	Ca1—C1—Cs1vii	84.67 (5)
O3—Cs1—H1	88.6 (6)	Cs1vi—C1—Cs1vii	141.18 (6)
C1iv—Cs1—H1	60.7 (8)	C1—O1—Ca1	114.80 (15)
C1v—Cs1—H1	99.3 (8)	C1—O1—Cs1iii	125.89 (14)
C2iv—Cs1—H1	64.9 (6)	Ca1—O1—Cs1iii	96.32 (6)
O2Wiii—Ca1—O2W	94.03 (11)	C1—O1—Cs1vii	107.50 (14)
O2Wiii—Ca1—O3iii	88.28 (7)	Ca1—O1—Cs1vii	115.34 (7)
O2W—Ca1—O3iii	170.75 (7)	Cs1iii—O1—Cs1vii	95.96 (4)
O2Wiii—Ca1—O3	170.75 (7)	C1—O2—Cs1i	147.27 (17)
O2W—Ca1—O3	88.28 (7)	C1—O2—Cs1vi	108.28 (15)
O3iii—Ca1—O3	90.86 (10)	Cs1i—O2—Cs1vi	97.86 (5)
O2Wiii—Ca1—O1	91.87 (7)	O4—C2—O3	125.9 (2)
O2W—Ca1—O1	96.30 (7)	O4—C2—C1	119.50 (19)
O3iii—Ca1—O1	92.57 (7)	O3—C2—C1	114.60 (18)
O3—Ca1—O1	78.97 (7)	O4—C2—Ca1	166.69 (16)
O2Wiii—Ca1—O1iii	96.30 (7)	C1—C2—Ca1	73.76 (11)
O2W—Ca1—O1iii	91.87 (7)	O4—C2—Cs1vi	58.69 (13)
O3iii—Ca1—O1iii	78.97 (7)	O3—C2—Cs1vi	137.27 (14)
O3—Ca1—O1iii	92.57 (7)	C1—C2—Cs1vi	77.18 (11)
O1—Ca1—O1iii	168.01 (10)	Ca1—C2—Cs1vi	128.24 (7)
O2Wiii—Ca1—C1iii	95.70 (7)	C2—O4—Cs1viii	127.57 (15)
O2W—Ca1—C1iii	115.59 (7)	C2—O4—Cs1vi	103.37 (14)
O3iii—Ca1—C1iii	55.22 (6)	Cs1viii—O4—Cs1vi	120.35 (6)
O3—Ca1—C1iii	91.35 (7)	C2—O3—Ca1	115.54 (14)
O1—Ca1—C1iii	146.48 (7)	C2—O3—Cs1	138.80 (14)
O1iii—Ca1—C1iii	23.78 (6)	Ca1—O3—Cs1	90.28 (6)
O2Wiii—Ca1—C1	115.59 (7)	Cs1—O1W—H1	95 (4)
O2W—Ca1—C1	95.70 (7)	Cs1—O1W—H2	141 (4)
O3iii—Ca1—C1	91.35 (7)	H1—O1W—H2	111 (5)
O3—Ca1—C1	55.22 (6)	Ca1—O2W—Cs1	95.21 (6)
O1—Ca1—C1	23.78 (6)	Ca1—O2W—H3	126 (3)
O1iii—Ca1—C1	146.48 (7)	Cs1—O2W—H3	105 (3)
C1iii—Ca1—C1	134.14 (9)	Ca1—O2W—H4	116 (4)
O2Wiii—Ca1—C2iii	91.60 (7)	Cs1—O2W—H4	106 (4)
O2W—Ca1—C2iii	147.17 (7)	H3—O2W—H4	106 (5)
O2i—Cs1—Ca1—O2Wiii	115.19 (8)	O2—C1—O1—Cs1vii	55.7 (3)
O4ii—Cs1—Ca1—O2Wiii	39.97 (10)	C2—C1—O1—Cs1vii	−125.96 (15)
O1W—Cs1—Ca1—O2Wiii	−79.43 (7)	Ca1—C1—O1—Cs1vii	−129.79 (16)
O1iii—Cs1—Ca1—O2Wiii	−63.90 (9)	Cs1vi—C1—O1—Cs1vii	129.51 (16)
O2iv—Cs1—Ca1—O2Wiii	−149.93 (7)	O2Wiii—Ca1—O1—C1	175.89 (16)
O1v—Cs1—Ca1—O2Wiii	0.17 (7)	O2W—Ca1—O1—C1	−89.85 (17)
O2W—Cs1—Ca1—O2Wiii	61.95 (13)	O3iii—Ca1—O1—C1	87.52 (16)
O4iv—Cs1—Ca1—O2Wiii	−135.51 (8)	O3—Ca1—O1—C1	−2.85 (16)
O3—Cs1—Ca1—O2Wiii	174.67 (9)	O1iii—Ca1—O1—C1	42.85 (15)
C1iv—Cs1—Ca1—O2Wiii	−134.13 (7)	C1iii—Ca1—O1—C1	72.6 (2)
C1v—Cs1—Ca1—O2Wiii	18.20 (7)	C2iii—Ca1—O1—C1	83.21 (17)
C2iv—Cs1—Ca1—O2Wiii	−125.01 (8)	C2—Ca1—O1—C1	−2.27 (14)
O2i—Cs1—Ca1—O2W	53.23 (7)	Cs1iii—Ca1—O1—C1	134.50 (17)
O4ii—Cs1—Ca1—O2W	−21.98 (10)	Cs1—Ca1—O1—C1	−39.83 (18)
O1W—Cs1—Ca1—O2W	−141.38 (7)	O2Wiii—Ca1—O1—Cs1iii	41.39 (6)
O1iii—Cs1—Ca1—O2W	−125.86 (9)	O2W—Ca1—O1—Cs1iii	135.65 (6)
O2iv—Cs1—Ca1—O2W	148.11 (7)	O3iii—Ca1—O1—Cs1iii	−46.97 (6)
O1v—Cs1—Ca1—O2W	−61.78 (7)	O3—Ca1—O1—Cs1iii	−137.35 (7)
O4iv—Cs1—Ca1—O2W	162.53 (8)	O1iii—Ca1—O1—Cs1iii	−91.7 (5)
O3—Cs1—Ca1—O2W	112.72 (8)	C1iii—Ca1—O1—Cs1iii	−61.87 (12)
C1iv—Cs1—Ca1—O2W	163.92 (7)	C1—Ca1—O1—Cs1iii	−134.50 (18)
C1v—Cs1—Ca1—O2W	−43.75 (7)	C2iii—Ca1—O1—Cs1iii	−51.29 (7)
C2iv—Cs1—Ca1—O2W	173.04 (7)	C2—Ca1—O1—Cs1iii	−136.77 (8)
O2i—Cs1—Ca1—O3iii	−132.36 (7)	Cs1—Ca1—O1—Cs1iii	−174.33 (3)
O4ii—Cs1—Ca1—O3iii	152.42 (10)	O2Wiii—Ca1—O1—Cs1vii	−58.29 (8)
O1W—Cs1—Ca1—O3iii	33.02 (7)	O2W—Ca1—O1—Cs1vii	35.97 (8)
O1iii—Cs1—Ca1—O3iii	48.55 (8)	O3iii—Ca1—O1—Cs1vii	−146.65 (8)
O2iv—Cs1—Ca1—O3iii	−37.49 (6)	O3—Ca1—O1—Cs1vii	122.98 (8)
O1v—Cs1—Ca1—O3iii	112.62 (6)	O1iii—Ca1—O1—Cs1vii	168.7 (4)
O2W—Cs1—Ca1—O3iii	174.40 (8)	C1iii—Ca1—O1—Cs1vii	−161.55 (9)
O4iv—Cs1—Ca1—O3iii	−23.07 (8)	C1—Ca1—O1—Cs1vii	125.83 (19)
O3—Cs1—Ca1—O3iii	−72.88 (11)	C2iii—Ca1—O1—Cs1vii	−150.97 (6)
C1iv—Cs1—Ca1—O3iii	−21.68 (7)	C2—Ca1—O1—Cs1vii	123.55 (10)
C1v—Cs1—Ca1—O3iii	130.65 (7)	Cs1iii—Ca1—O1—Cs1vii	−99.68 (7)
C2iv—Cs1—Ca1—O3iii	−12.56 (7)	Cs1—Ca1—O1—Cs1vii	86.00 (7)
O2i—Cs1—Ca1—O3	−59.48 (7)	O1—C1—O2—Cs1i	−90.7 (4)
O4ii—Cs1—Ca1—O3	−134.70 (10)	C2—C1—O2—Cs1i	91.0 (3)
O1W—Cs1—Ca1—O3	105.90 (7)	Ca1—C1—O2—Cs1i	−106.6 (7)
O1iii—Cs1—Ca1—O3	121.43 (8)	Cs1vi—C1—O2—Cs1i	141.3 (3)
O2iv—Cs1—Ca1—O3	35.39 (7)	Cs1vii—C1—O2—Cs1i	−48.5 (3)
O1v—Cs1—Ca1—O3	−174.50 (6)	O1—C1—O2—Cs1vi	128.0 (2)
O2W—Cs1—Ca1—O3	−112.72 (8)	C2—C1—O2—Cs1vi	−50.3 (2)
O4iv—Cs1—Ca1—O3	49.81 (8)	Ca1—C1—O2—Cs1vi	112.1 (7)
C1iv—Cs1—Ca1—O3	51.20 (7)	Cs1vii—C1—O2—Cs1vi	170.22 (7)
C1v—Cs1—Ca1—O3	−156.47 (7)	O2—C1—C2—O4	−3.0 (3)
C2iv—Cs1—Ca1—O3	60.32 (7)	O1—C1—C2—O4	178.5 (2)
O2i—Cs1—Ca1—O1	−15.86 (8)	Ca1—C1—C2—O4	−178.8 (2)
O4ii—Cs1—Ca1—O1	−91.08 (11)	Cs1vi—C1—C2—O4	−42.18 (19)
O1W—Cs1—Ca1—O1	149.52 (7)	Cs1vii—C1—C2—O4	114.1 (2)
O1iii—Cs1—Ca1—O1	165.05 (12)	O2—C1—C2—O3	175.6 (2)
O2iv—Cs1—Ca1—O1	79.01 (7)	O1—C1—C2—O3	−2.9 (3)
O1v—Cs1—Ca1—O1	−130.88 (6)	Ca1—C1—C2—O3	−0.25 (16)
O2W—Cs1—Ca1—O1	−69.10 (9)	Cs1vi—C1—C2—O3	136.42 (18)
O4iv—Cs1—Ca1—O1	93.43 (8)	Cs1vii—C1—C2—O3	−67.3 (2)
O3—Cs1—Ca1—O1	43.62 (8)	O2—C1—C2—Ca1	175.9 (2)
C1iv—Cs1—Ca1—O1	94.82 (7)	O1—C1—C2—Ca1	−2.63 (16)
C1v—Cs1—Ca1—O1	−112.85 (7)	Cs1vi—C1—C2—Ca1	136.67 (5)
C2iv—Cs1—Ca1—O1	103.94 (7)	Cs1vii—C1—C2—Ca1	−67.05 (14)
O2i—Cs1—Ca1—O1iii	179.09 (7)	O2—C1—C2—Cs1vi	39.20 (19)
O4ii—Cs1—Ca1—O1iii	103.88 (10)	O1—C1—C2—Cs1vi	−139.29 (19)
O1W—Cs1—Ca1—O1iii	−15.53 (7)	Ca1—C1—C2—Cs1vi	−136.67 (5)
O2iv—Cs1—Ca1—O1iii	−86.03 (7)	Cs1vii—C1—C2—Cs1vi	156.28 (15)
O1v—Cs1—Ca1—O1iii	64.08 (8)	O2Wiii—Ca1—C2—O4	174.0 (7)
O2W—Cs1—Ca1—O1iii	125.86 (9)	O2W—Ca1—C2—O4	−86.1 (7)
O4iv—Cs1—Ca1—O1iii	−71.61 (8)	O3iii—Ca1—C2—O4	85.2 (7)
O3—Cs1—Ca1—O1iii	−121.43 (8)	O3—Ca1—C2—O4	−4.0 (7)
C1iv—Cs1—Ca1—O1iii	−70.23 (7)	O1—Ca1—C2—O4	177.4 (8)
C1v—Cs1—Ca1—O1iii	82.10 (7)	O1iii—Ca1—C2—O4	6.8 (7)
C2iv—Cs1—Ca1—O1iii	−61.11 (7)	C1iii—Ca1—C2—O4	32.2 (7)
O2i—Cs1—Ca1—C1iii	−163.20 (6)	C1—Ca1—C2—O4	175.6 (8)
O4ii—Cs1—Ca1—C1iii	121.58 (10)	C2iii—Ca1—C2—O4	63.4 (7)
O1W—Cs1—Ca1—C1iii	2.18 (6)	Cs1iii—Ca1—C2—O4	143.9 (7)
O1iii—Cs1—Ca1—C1iii	17.71 (7)	Cs1—Ca1—C2—O4	−32.6 (7)
O2iv—Cs1—Ca1—C1iii	−68.32 (6)	O2Wiii—Ca1—C2—O3	178.02 (16)
O1v—Cs1—Ca1—C1iii	81.78 (6)	O2W—Ca1—C2—O3	−82.03 (17)
O2W—Cs1—Ca1—C1iii	143.56 (8)	O3iii—Ca1—C2—O3	89.18 (18)
O4iv—Cs1—Ca1—C1iii	−53.90 (7)	O1—Ca1—C2—O3	−178.59 (19)
O3—Cs1—Ca1—C1iii	−103.72 (7)	O1iii—Ca1—C2—O3	10.82 (18)
C1iv—Cs1—Ca1—C1iii	−52.52 (7)	C1iii—Ca1—C2—O3	36.19 (17)
C1v—Cs1—Ca1—C1iii	99.81 (5)	C1—Ca1—C2—O3	179.7 (2)
C2iv—Cs1—Ca1—C1iii	−43.40 (6)	C2iii—Ca1—C2—O3	67.45 (15)
O2i—Cs1—Ca1—C1	−31.54 (6)	Cs1iii—Ca1—C2—O3	147.91 (15)
O4ii—Cs1—Ca1—C1	−106.76 (10)	Cs1—Ca1—C2—O3	−28.54 (15)
O1W—Cs1—Ca1—C1	133.84 (6)	O2Wiii—Ca1—C2—C1	−1.64 (19)
O1iii—Cs1—Ca1—C1	149.37 (8)	O2W—Ca1—C2—C1	98.31 (12)
O2iv—Cs1—Ca1—C1	63.34 (6)	O3iii—Ca1—C2—C1	−90.48 (12)
O1v—Cs1—Ca1—C1	−146.56 (6)	O3—Ca1—C2—C1	−179.7 (2)
O2W—Cs1—Ca1—C1	−84.78 (8)	O1—Ca1—C2—C1	1.75 (11)
O4iv—Cs1—Ca1—C1	77.76 (7)	O1iii—Ca1—C2—C1	−168.84 (11)
O3—Cs1—Ca1—C1	27.94 (7)	C1iii—Ca1—C2—C1	−143.47 (10)
C1iv—Cs1—Ca1—C1	79.14 (4)	C2iii—Ca1—C2—C1	−112.21 (12)
C1v—Cs1—Ca1—C1	−128.53 (6)	Cs1iii—Ca1—C2—C1	−31.75 (11)
C2iv—Cs1—Ca1—C1	88.26 (6)	Cs1—Ca1—C2—C1	151.80 (11)
O2i—Cs1—Ca1—C2iii	−146.25 (6)	O2Wiii—Ca1—C2—Cs1vi	56.78 (16)
O4ii—Cs1—Ca1—C2iii	138.54 (9)	O2W—Ca1—C2—Cs1vi	156.73 (9)
O1W—Cs1—Ca1—C2iii	19.14 (6)	O3iii—Ca1—C2—Cs1vi	−32.05 (9)
O1iii—Cs1—Ca1—C2iii	34.66 (7)	O3—Ca1—C2—Cs1vi	−121.23 (19)
O2iv—Cs1—Ca1—C2iii	−51.37 (5)	O1—Ca1—C2—Cs1vi	60.17 (9)
O1v—Cs1—Ca1—C2iii	98.74 (5)	O1iii—Ca1—C2—Cs1vi	−110.41 (9)
O2W—Cs1—Ca1—C2iii	160.52 (8)	C1iii—Ca1—C2—Cs1vi	−85.05 (9)
O4iv—Cs1—Ca1—C2iii	−36.95 (7)	C1—Ca1—C2—Cs1vi	58.42 (11)
O3—Cs1—Ca1—C2iii	−86.76 (7)	C2iii—Ca1—C2—Cs1vi	−53.78 (6)
C1iv—Cs1—Ca1—C2iii	−35.56 (6)	Cs1iii—Ca1—C2—Cs1vi	26.67 (8)
C1v—Cs1—Ca1—C2iii	116.76 (6)	Cs1—Ca1—C2—Cs1vi	−149.78 (8)
C2iv—Cs1—Ca1—C2iii	−26.45 (8)	O3—C2—O4—Cs1viii	18.6 (3)
O2i—Cs1—Ca1—C2	−46.56 (6)	C1—C2—O4—Cs1viii	−163.01 (13)
O4ii—Cs1—Ca1—C2	−121.77 (9)	Ca1—C2—O4—Cs1viii	21.8 (8)
O1W—Cs1—Ca1—C2	118.83 (6)	Cs1vi—C2—O4—Cs1viii	146.96 (19)
O1iii—Cs1—Ca1—C2	134.35 (7)	O3—C2—O4—Cs1vi	−128.4 (2)
O2iv—Cs1—Ca1—C2	48.32 (5)	C1—C2—O4—Cs1vi	50.0 (2)
O1v—Cs1—Ca1—C2	−161.57 (5)	Ca1—C2—O4—Cs1vi	−125.2 (7)
O2W—Cs1—Ca1—C2	−99.79 (7)	O4—C2—O3—Ca1	178.86 (19)
O4iv—Cs1—Ca1—C2	62.74 (7)	C1—C2—O3—Ca1	0.4 (2)
O3—Cs1—Ca1—C2	12.93 (7)	Cs1vi—C2—O3—Ca1	98.19 (19)
C1iv—Cs1—Ca1—C2	64.13 (6)	O4—C2—O3—Cs1	−57.5 (3)
C1v—Cs1—Ca1—C2	−143.54 (6)	C1—C2—O3—Cs1	123.99 (18)
C2iv—Cs1—Ca1—C2	73.24 (2)	Ca1—C2—O3—Cs1	123.6 (2)
O2Wiii—Ca1—C1—O2	15.1 (8)	Cs1vi—C2—O3—Cs1	−138.18 (13)
O2W—Ca1—C1—O2	112.3 (7)	O2W—Ca1—O3—C2	97.94 (16)
O3iii—Ca1—C1—O2	−73.7 (8)	O3iii—Ca1—O3—C2	−91.27 (16)
O3—Ca1—C1—O2	−163.8 (8)	O1—Ca1—O3—C2	1.18 (16)
O1—Ca1—C1—O2	19.6 (7)	O1iii—Ca1—O3—C2	−170.26 (16)
O1iii—Ca1—C1—O2	−145.6 (7)	C1iii—Ca1—O3—C2	−146.50 (16)
C1iii—Ca1—C1—O2	−113.1 (8)	C1—Ca1—O3—C2	−0.22 (14)
C2iii—Ca1—C1—O2	−87.4 (7)	C2iii—Ca1—O3—C2	−114.89 (16)
C2—Ca1—C1—O2	−164.0 (8)	Cs1iii—Ca1—O3—C2	−36.38 (17)
Cs1iii—Ca1—C1—O2	−17.4 (7)	Cs1—Ca1—O3—C2	146.74 (17)
Cs1—Ca1—C1—O2	167.0 (7)	O2W—Ca1—O3—Cs1	−48.80 (6)
O2Wiii—Ca1—C1—O1	−4.56 (18)	O3iii—Ca1—O3—Cs1	121.99 (6)
O2W—Ca1—C1—O1	92.68 (17)	O1—Ca1—O3—Cs1	−145.56 (6)
O3iii—Ca1—C1—O1	−93.30 (16)	O1iii—Ca1—O3—Cs1	43.00 (6)
O3—Ca1—C1—O1	176.60 (19)	C1iii—Ca1—O3—Cs1	66.76 (5)
O1iii—Ca1—C1—O1	−165.18 (13)	C1—Ca1—O3—Cs1	−146.96 (8)
C1iii—Ca1—C1—O1	−132.75 (17)	C2iii—Ca1—O3—Cs1	98.37 (5)
C2iii—Ca1—C1—O1	−106.99 (16)	C2—Ca1—O3—Cs1	−146.74 (17)
C2—Ca1—C1—O1	176.4 (2)	Cs1iii—Ca1—O3—Cs1	176.877 (14)
Cs1iii—Ca1—C1—O1	−37.03 (15)	O2i—Cs1—O3—C2	−19.6 (2)
Cs1—Ca1—C1—O1	147.37 (15)	O4ii—Cs1—O3—C2	−3.0 (3)
O2Wiii—Ca1—C1—C2	179.01 (11)	O1W—Cs1—O3—C2	150.9 (2)
O2W—Ca1—C1—C2	−83.74 (12)	O1iii—Cs1—O3—C2	−164.4 (2)
O3iii—Ca1—C1—C2	90.27 (12)	O2iv—Cs1—O3—C2	85.8 (2)
O3—Ca1—C1—C2	0.17 (11)	O1v—Cs1—O3—C2	−124.3 (2)
O1—Ca1—C1—C2	−176.4 (2)	O2W—Cs1—O3—C2	−94.1 (2)
O1iii—Ca1—C1—C2	18.39 (18)	O4iv—Cs1—O3—C2	79.9 (2)
C1iii—Ca1—C1—C2	50.82 (10)	C1iv—Cs1—O3—C2	97.4 (2)
C2iii—Ca1—C1—C2	76.58 (14)	C1v—Cs1—O3—C2	−101.0 (2)
Cs1iii—Ca1—C1—C2	146.54 (11)	C2iv—Cs1—O3—C2	95.3 (2)
Cs1—Ca1—C1—C2	−29.06 (11)	O2i—Cs1—O3—Ca1	111.65 (7)
O2Wiii—Ca1—C1—Cs1vi	117.19 (10)	O4ii—Cs1—O3—Ca1	128.25 (11)
O2W—Ca1—C1—Cs1vi	−145.57 (10)	O1W—Cs1—O3—Ca1	−77.83 (6)
O3iii—Ca1—C1—Cs1vi	28.45 (10)	O1iii—Cs1—O3—Ca1	−33.05 (5)
O3—Ca1—C1—Cs1vi	−61.65 (9)	O2iv—Cs1—O3—Ca1	−142.87 (7)
O1—Ca1—C1—Cs1vi	121.8 (2)	O1v—Cs1—O3—Ca1	6.97 (8)
O1iii—Ca1—C1—Cs1vi	−43.43 (17)	O2W—Cs1—O3—Ca1	37.23 (5)
C1iii—Ca1—C1—Cs1vi	−11.00 (6)	O4iv—Cs1—O3—Ca1	−148.82 (5)
C2iii—Ca1—C1—Cs1vi	14.76 (11)	C1iv—Cs1—O3—Ca1	−131.32 (6)
C2—Ca1—C1—Cs1vi	−61.82 (11)	C1v—Cs1—O3—Ca1	30.32 (8)
Cs1iii—Ca1—C1—Cs1vi	84.72 (8)	C2iv—Cs1—O3—Ca1	−133.39 (5)
Cs1—Ca1—C1—Cs1vi	−90.88 (8)	O2Wiii—Ca1—O2W—Cs1	−136.80 (8)
O2Wiii—Ca1—C1—Cs1vii	−43.40 (8)	O3—Ca1—O2W—Cs1	52.16 (6)
O2W—Ca1—C1—Cs1vii	53.84 (7)	O1—Ca1—O2W—Cs1	130.87 (6)
O3iii—Ca1—C1—Cs1vii	−132.14 (6)	O1iii—Ca1—O2W—Cs1	−40.35 (6)
O3—Ca1—C1—Cs1vii	137.76 (8)	C1iii—Ca1—O2W—Cs1	−38.51 (8)
O1—Ca1—C1—Cs1vii	−38.84 (15)	C1—Ca1—O2W—Cs1	106.96 (6)
O1iii—Ca1—C1—Cs1vii	155.98 (10)	C2iii—Ca1—O2W—Cs1	−37.56 (14)
C1iii—Ca1—C1—Cs1vii	−171.59 (5)	C2—Ca1—O2W—Cs1	75.56 (5)
C2iii—Ca1—C1—Cs1vii	−145.83 (5)	Cs1iii—Ca1—O2W—Cs1	177.031 (16)
C2—Ca1—C1—Cs1vii	137.59 (12)	O2i—Cs1—O2W—Ca1	−117.98 (8)
Cs1iii—Ca1—C1—Cs1vii	−75.87 (3)	O4ii—Cs1—O2W—Ca1	169.09 (5)
Cs1—Ca1—C1—Cs1vii	108.53 (3)	O1W—Cs1—O2W—Ca1	43.91 (7)
O2—C1—O1—Ca1	−174.53 (19)	O1iii—Cs1—O2W—Ca1	30.93 (5)
C2—C1—O1—Ca1	3.8 (2)	O2iv—Cs1—O2W—Ca1	−38.25 (8)
Cs1vi—C1—O1—Ca1	−100.7 (2)	O1v—Cs1—O2W—Ca1	118.48 (6)
Cs1vii—C1—O1—Ca1	129.79 (16)	O4iv—Cs1—O2W—Ca1	−66.5 (2)
O2—C1—O1—Cs1iii	−55.6 (3)	O3—Cs1—O2W—Ca1	−38.14 (5)
C2—C1—O1—Cs1iii	122.78 (17)	C1iv—Cs1—O2W—Ca1	−21.98 (9)
Ca1—C1—O1—Cs1iii	118.94 (19)	C1v—Cs1—O2W—Ca1	136.42 (7)
Cs1vi—C1—O1—Cs1iii	18.2 (3)	C2iv—Cs1—O2W—Ca1	−14.46 (15)
Cs1vii—C1—O1—Cs1iii	−111.26 (16)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1···O2iii	0.81 (7)	1.91 (7)	2.714 (4)	172 (6)
O1W—H2···O3ix	0.81 (4)	1.95 (4)	2.736 (2)	163 (7)
O2W—H3···O1Wx	0.82 (3)	1.89 (3)	2.680 (2)	164 (5)
O2W—H4···O4i	0.81 (4)	1.92 (3)	2.724 (3)	176 (7)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1⋯O2i	0.81 (7)	1.91 (7)	2.714 (4)	172 (6)
O1W—H2⋯O3ii	0.81 (4)	1.95 (4)	2.736 (2)	163 (7)
O2W—H3⋯O1W iii	0.82 (3)	1.89 (3)	2.680 (2)	164 (5)
O2W—H4⋯O4iv	0.81 (4)	1.92 (3)	2.724 (3)	176 (7)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .