Download citation
Download citation
link to html
The crystal structures of two crown-ether-coordinated caesium halogen salt hydrates, namely di-μ-bromido-bis­[aqua(1,4,7,10,13,16-hexa­oxa­cyclo­octa­decane)caesium(I)] dihydrate, [Cs2Br2(C12H24O6)2(H2O)2]·2H2O, (I), and poly[[diaquadi-μ-chlorido-μ-(1,4,7,10,13,16-hexa­oxa­cyclo­octadecane)dicaesium(I)] dihydrate], {[Cs2Cl2(C12H24O6)(H2O)2]·2H2O}n, (II), are re­ported. In (I), all atoms are located on general positions. In (II), the Cs+ cation is located on a mirror plane perpendicular to the a axis, the chloride anion is located on a mirror plane perpendicular to the c axis and the crown-ether ring is located around a special position with site symmetry 2/m, with two opposite O atoms exactly on the mirror plane perpendicular to the a axis; of one water mol­ecule, only the O atom is located on a mirror plane perpendicular on the a axis, while the other water mol­ecule is completely located on a mirror plane perpendicular to the c axis. Whereas in (I), hydrogen bonds between bromide ligands and water mol­ecules lead to one-dimensional chains running along the b axis, in (II) two-dimensional sheets of water mol­ecules and chloride ligands are formed which combine with the polymeric caesium–crown polymer to give a three-dimensional network. Although both compounds have a similar composition, i.e. a Cs+ cation with a halogen, an 18-crown-6 ether and a water ligand, the crystal structures are rather different. On the other hand, it is remarkable that (I) is isomorphous with the already published iodide compound.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614006809/sk3535sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614006809/sk3535Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614006809/sk3535IIsup3.hkl
Contains datablock II

CCDC references: 994052; 994053

Computing details top

For both structures, data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Di-µ-bromido-bis[aqua(1,4,7,10,13,16-hexaoxacyclooctadecane)caesium(I)] dihydrate (I) top
Crystal data top
[Cs2Br2(C12H24O6)2(H2O)2]·2H2OF(000) = 1016
Mr = 1026.31Dx = 1.771 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.7379 (5) ÅCell parameters from 44249 reflections
b = 8.4198 (3) Åθ = 2.3–30.6°
c = 21.4724 (11) ŵ = 4.03 mm1
β = 97.618 (4)°T = 173 K
V = 1924.21 (15) Å3Block, colourless
Z = 20.28 × 0.23 × 0.18 mm
Data collection top
Stoe IPDSII two-circle
diffractometer
5351 reflections with I > 2σ(I)
Radiation source: Genix 3D IµS microfocus X-ray sourceRint = 0.073
ω scansθmax = 30.2°, θmin = 2.6°
Absorption correction: multi-scan
(X-AREA; Stoe & Cie, 2001)
h = 1515
Tmin = 0.398, Tmax = 0.531k = 1111
32488 measured reflectionsl = 3030
5665 independent reflections
Refinement top
Refinement on F2Hydrogen site location: mixed
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.035 w = 1/[σ2(Fo2) + (0.0468P)2 + 1.741P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.090(Δ/σ)max = 0.001
S = 1.09Δρmax = 1.18 e Å3
5665 reflectionsΔρmin = 1.17 e Å3
216 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
4 restraintsExtinction coefficient: 0.0154 (7)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cs10.83923 (2)0.52538 (2)0.60297 (2)0.02701 (8)
Br11.12489 (3)0.32691 (4)0.56604 (2)0.03532 (9)
O10.76052 (19)0.8885 (2)0.60244 (9)0.0328 (4)
O20.57087 (19)0.6532 (3)0.57151 (10)0.0369 (4)
O30.58421 (17)0.3840 (2)0.65021 (9)0.0296 (4)
O40.82764 (16)0.2818 (2)0.70794 (9)0.0276 (3)
O51.01419 (17)0.5182 (2)0.73457 (10)0.0296 (4)
O61.00371 (18)0.7926 (2)0.66133 (10)0.0328 (4)
C10.6713 (3)0.8918 (4)0.54736 (13)0.0382 (6)
H1A0.70420.83240.51330.046*
H1B0.65601.00300.53330.046*
C20.5507 (3)0.8183 (4)0.56094 (14)0.0385 (6)
H2A0.52320.86830.59850.046*
H2B0.48420.83490.52490.046*
C30.4621 (3)0.5731 (4)0.58557 (14)0.0392 (6)
H3A0.39330.58500.55030.047*
H3B0.43390.61900.62380.047*
C40.4935 (3)0.4011 (4)0.59591 (14)0.0384 (6)
H4A0.41660.34100.60160.046*
H4B0.52730.35770.55870.046*
C50.6208 (3)0.2228 (3)0.66045 (14)0.0322 (5)
H5A0.65960.18300.62410.039*
H5B0.54600.15700.66470.039*
C60.7126 (2)0.2104 (3)0.71876 (13)0.0303 (5)
H6A0.67910.26490.75390.036*
H6B0.72670.09740.73030.036*
C70.9171 (2)0.2806 (3)0.76312 (12)0.0298 (5)
H7A0.93330.16990.77750.036*
H7B0.88370.34020.79700.036*
C81.0373 (2)0.3555 (3)0.74917 (13)0.0305 (5)
H8A1.10260.34580.78610.037*
H8B1.06770.30100.71320.037*
C91.1250 (2)0.6014 (4)0.72459 (15)0.0349 (6)
H9A1.15780.55900.68700.042*
H9B1.19030.58730.76120.042*
C101.0941 (3)0.7744 (4)0.71551 (15)0.0354 (6)
H10A1.06010.81640.75290.043*
H10B1.17110.83480.71020.043*
C110.9668 (3)0.9538 (3)0.65176 (17)0.0372 (6)
H11A1.04141.02040.64800.045*
H11B0.92730.99230.68810.045*
C120.8754 (3)0.9662 (4)0.59298 (17)0.0406 (7)
H12A0.85881.07930.58240.049*
H12B0.91100.91560.55760.049*
O1W0.8425 (2)0.2870 (3)0.47605 (13)0.0459 (5)
H1WA0.9145 (17)0.272 (5)0.4954 (16)0.034 (9)*
H1WB0.852 (4)0.361 (3)0.4510 (15)0.038 (10)*
O2W0.7235 (3)0.0336 (4)0.39410 (14)0.0499 (6)
H2WA0.753 (5)0.055 (3)0.406 (3)0.080 (18)*
H2WB0.761 (5)0.101 (6)0.419 (2)0.09 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.02688 (10)0.02713 (11)0.02730 (10)0.00380 (5)0.00463 (6)0.00055 (5)
Br10.03321 (14)0.03525 (16)0.03854 (16)0.00666 (10)0.00860 (11)0.00002 (11)
O10.0365 (9)0.0316 (10)0.0311 (9)0.0053 (8)0.0072 (7)0.0067 (7)
O20.0330 (9)0.0371 (11)0.0395 (11)0.0106 (8)0.0005 (8)0.0005 (8)
O30.0277 (8)0.0315 (9)0.0282 (8)0.0009 (7)0.0009 (7)0.0038 (7)
O40.0264 (8)0.0298 (9)0.0263 (8)0.0015 (7)0.0027 (6)0.0027 (7)
O50.0226 (8)0.0269 (9)0.0390 (10)0.0001 (6)0.0033 (7)0.0006 (7)
O60.0331 (9)0.0243 (9)0.0413 (10)0.0005 (7)0.0062 (8)0.0013 (8)
C10.0522 (16)0.0338 (14)0.0276 (12)0.0159 (12)0.0015 (11)0.0034 (10)
C20.0427 (14)0.0412 (16)0.0284 (12)0.0197 (12)0.0066 (11)0.0028 (11)
C30.0266 (11)0.0551 (18)0.0337 (13)0.0077 (12)0.0043 (10)0.0032 (13)
C40.0314 (12)0.0476 (17)0.0333 (13)0.0039 (11)0.0056 (10)0.0058 (12)
C50.0307 (11)0.0297 (12)0.0367 (13)0.0033 (10)0.0065 (10)0.0051 (10)
C60.0306 (11)0.0294 (12)0.0318 (12)0.0028 (9)0.0077 (9)0.0050 (10)
C70.0324 (11)0.0279 (12)0.0285 (11)0.0028 (9)0.0017 (9)0.0031 (9)
C80.0267 (11)0.0309 (13)0.0327 (12)0.0045 (9)0.0002 (9)0.0022 (10)
C90.0221 (10)0.0373 (15)0.0450 (15)0.0016 (9)0.0035 (10)0.0004 (11)
C100.0283 (11)0.0335 (14)0.0445 (15)0.0065 (10)0.0048 (10)0.0027 (11)
C110.0379 (14)0.0227 (12)0.0540 (18)0.0005 (10)0.0174 (13)0.0006 (11)
C120.0479 (17)0.0308 (15)0.0472 (17)0.0066 (12)0.0216 (14)0.0097 (12)
O1W0.0459 (12)0.0426 (13)0.0481 (13)0.0005 (10)0.0020 (10)0.0012 (11)
O2W0.0449 (13)0.0547 (17)0.0491 (14)0.0102 (11)0.0025 (11)0.0058 (12)
Geometric parameters (Å, º) top
Cs1—O63.028 (2)C2—H2B0.9900
Cs1—O43.0622 (18)C3—C41.496 (5)
Cs1—O23.066 (2)C3—H3A0.9900
Cs1—O13.172 (2)C3—H3B0.9900
Cs1—O53.180 (2)C4—H4A0.9900
Cs1—O33.2682 (19)C4—H4B0.9900
Cs1—O1W3.388 (3)C5—C61.491 (4)
Cs1—Br13.6708 (3)C5—H5A0.9900
Cs1—C13.692 (3)C5—H5B0.9900
Cs1—C123.741 (3)C6—H6A0.9900
Cs1—C53.779 (3)C6—H6B0.9900
Cs1—C93.810 (3)C7—C81.502 (4)
Cs1—H1WA3.32 (4)C7—H7A0.9900
Br1—Cs1i3.9032 (4)C7—H7B0.9900
O1—C11.420 (3)C8—H8A0.9900
O1—C121.434 (4)C8—H8B0.9900
O2—C31.416 (4)C9—C101.501 (4)
O2—C21.420 (4)C9—H9A0.9900
O3—C51.422 (3)C9—H9B0.9900
O3—C41.424 (3)C10—H10A0.9900
O4—C61.420 (3)C10—H10B0.9900
O4—C71.423 (3)C11—C121.496 (5)
O5—C81.420 (3)C11—H11A0.9900
O5—C91.421 (3)C11—H11B0.9900
O6—C101.421 (4)C12—H12A0.9900
O6—C111.421 (3)C12—H12B0.9900
C1—C21.498 (5)O1W—H1WA0.838 (10)
C1—H1A0.9900O1W—H1WB0.839 (10)
C1—H1B0.9900O2W—H2WA0.840 (10)
C2—H2A0.9900O2W—H2WB0.840 (10)
O6—Cs1—O4105.75 (5)C2—C1—Cs189.39 (16)
O6—Cs1—O2108.05 (6)O1—C1—H1A109.8
O4—Cs1—O2105.58 (5)C2—C1—H1A109.8
O6—Cs1—O154.94 (5)Cs1—C1—H1A67.0
O4—Cs1—O1127.70 (5)O1—C1—H1B109.8
O2—Cs1—O154.45 (6)C2—C1—H1B109.8
O6—Cs1—O553.33 (5)Cs1—C1—H1B160.4
O4—Cs1—O553.84 (5)H1A—C1—H1B108.2
O2—Cs1—O5129.03 (5)O2—C2—C1108.5 (2)
O1—Cs1—O598.47 (5)O2—C2—H2A110.0
O6—Cs1—O3127.52 (5)C1—C2—H2A110.0
O4—Cs1—O353.85 (5)O2—C2—H2B110.0
O2—Cs1—O352.75 (6)C1—C2—H2B110.0
O1—Cs1—O396.80 (5)H2A—C2—H2B108.4
O5—Cs1—O397.92 (5)O2—C3—C4108.5 (2)
O6—Cs1—O1W134.87 (6)O2—C3—H3A110.0
O4—Cs1—O1W101.60 (6)C4—C3—H3A110.0
O2—Cs1—O1W98.07 (6)O2—C3—H3B110.0
O1—Cs1—O1W126.82 (6)C4—C3—H3B110.0
O5—Cs1—O1W129.47 (6)H3A—C3—H3B108.4
O3—Cs1—O1W97.60 (6)O3—C4—C3109.6 (2)
O6—Cs1—Br188.25 (4)O3—C4—Cs156.12 (13)
O4—Cs1—Br188.32 (3)C3—C4—Cs186.56 (17)
O2—Cs1—Br1154.16 (4)O3—C4—H4A109.7
O1—Cs1—Br1131.91 (4)C3—C4—H4A109.7
O5—Cs1—Br176.77 (4)Cs1—C4—H4A162.2
O3—Cs1—Br1131.28 (4)O3—C4—H4B109.7
O1W—Cs1—Br157.22 (4)C3—C4—H4B109.7
O6—Cs1—C175.28 (6)Cs1—C4—H4B71.1
O4—Cs1—C1137.06 (6)H4A—C4—H4B108.2
O2—Cs1—C139.71 (7)O3—C5—C6109.6 (2)
O1—Cs1—C122.27 (6)O3—C5—Cs158.47 (12)
O5—Cs1—C1120.61 (6)C6—C5—Cs187.24 (15)
O3—Cs1—C190.64 (6)O3—C5—H5A109.8
O1W—Cs1—C1106.95 (6)C6—C5—H5A109.8
Br1—Cs1—C1134.19 (5)Cs1—C5—H5A68.1
O6—Cs1—C1239.39 (7)O3—C5—H5B109.8
O4—Cs1—C12136.17 (7)C6—C5—H5B109.8
O2—Cs1—C1274.97 (7)Cs1—C5—H5B162.5
O1—Cs1—C1222.03 (6)H5A—C5—H5B108.2
O5—Cs1—C1290.93 (7)O4—C6—C5109.0 (2)
O3—Cs1—C12118.47 (6)O4—C6—H6A109.9
O1W—Cs1—C12121.96 (7)C5—C6—H6A109.9
Br1—Cs1—C12110.08 (5)O4—C6—H6B109.9
C1—Cs1—C1237.08 (8)C5—C6—H6B109.9
O6—Cs1—C5135.98 (6)H6A—C6—H6B108.3
O4—Cs1—C538.79 (6)O4—C7—C8109.5 (2)
O2—Cs1—C572.71 (6)O4—C7—H7A109.8
O1—Cs1—C5118.32 (6)C8—C7—H7A109.8
O5—Cs1—C590.92 (6)O4—C7—H7B109.8
O3—Cs1—C521.76 (5)C8—C7—H7B109.8
O1W—Cs1—C586.35 (6)H7A—C7—H7B108.2
Br1—Cs1—C5109.65 (4)O5—C8—C7108.7 (2)
C1—Cs1—C5111.79 (7)O5—C8—Cs152.89 (12)
C12—Cs1—C5139.56 (6)C7—C8—Cs185.53 (14)
O6—Cs1—C938.64 (6)O5—C8—H8A110.0
O4—Cs1—C973.48 (6)C7—C8—H8A110.0
O2—Cs1—C9137.71 (6)Cs1—C8—H8A161.0
O1—Cs1—C991.75 (6)O5—C8—H8B110.0
O5—Cs1—C921.08 (6)C7—C8—H8B110.0
O3—Cs1—C9118.69 (6)Cs1—C8—H8B74.8
O1W—Cs1—C9123.89 (6)H8A—C8—H8B108.3
Br1—Cs1—C966.71 (5)O5—C9—C10108.9 (2)
C1—Cs1—C9113.31 (7)O5—C9—Cs153.59 (13)
C12—Cs1—C978.02 (8)C10—C9—Cs185.99 (16)
C5—Cs1—C9111.57 (6)O5—C9—H9A109.9
O6—Cs1—H1WA125.6 (5)C10—C9—H9A109.9
O4—Cs1—H1WA96.8 (6)Cs1—C9—H9A73.8
O2—Cs1—H1WA112.36 (19)O5—C9—H9B109.9
O1—Cs1—H1WA134.9 (6)C10—C9—H9B109.9
O5—Cs1—H1WA115.9 (3)Cs1—C9—H9B161.2
O3—Cs1—H1WA105.8 (6)H9A—C9—H9B108.3
O1W—Cs1—H1WA14.30 (17)O6—C10—C9109.0 (2)
Br1—Cs1—H1WA43.1 (2)O6—C10—H10A109.9
C1—Cs1—H1WA117.7 (5)C9—C10—H10A109.9
C12—Cs1—H1WA124.1 (7)O6—C10—H10B109.9
C5—Cs1—H1WA90.7 (6)C9—C10—H10B109.9
C9—Cs1—H1WA109.7 (2)H10A—C10—H10B108.3
Cs1—Br1—Cs1i104.126 (8)O6—C11—C12109.2 (3)
C1—O1—C12111.8 (2)O6—C11—H11A109.8
C1—O1—Cs199.90 (16)C12—C11—H11A109.8
C12—O1—Cs1101.91 (15)O6—C11—H11B109.8
C3—O2—C2112.8 (2)C12—C11—H11B109.8
C3—O2—Cs1124.30 (17)H11A—C11—H11B108.3
C2—O2—Cs1119.86 (18)O1—C12—C11109.2 (2)
C5—O3—C4111.6 (2)O1—C12—Cs156.06 (13)
C5—O3—Cs199.77 (14)C11—C12—Cs186.77 (16)
C4—O3—Cs1102.67 (16)O1—C12—H12A109.8
C6—O4—C7111.50 (19)C11—C12—H12A109.8
C6—O4—Cs1121.67 (14)Cs1—C12—H12A162.0
C7—O4—Cs1121.93 (15)O1—C12—H12B109.8
C8—O5—C9112.6 (2)C11—C12—H12B109.8
C8—O5—Cs1106.26 (15)Cs1—C12—H12B70.8
C9—O5—Cs1105.33 (16)H12A—C12—H12B108.3
C10—O6—C11111.6 (2)Cs1—O1W—H1WA78 (3)
C10—O6—Cs1123.81 (16)Cs1—O1W—H1WB95 (3)
C11—O6—Cs1120.90 (18)H1WA—O1W—H1WB104 (4)
O1—C1—C2109.6 (2)H2WA—O2W—H2WB106 (6)
O1—C1—Cs157.83 (13)
C12—O1—C1—C2176.5 (2)C6—O4—C7—C8179.4 (2)
Cs1—O1—C1—C276.3 (2)Cs1—O4—C7—C825.0 (3)
C12—O1—C1—Cs1107.2 (2)C9—O5—C8—C7176.2 (2)
C3—O2—C2—C1179.3 (2)Cs1—O5—C8—C769.0 (2)
Cs1—O2—C2—C118.1 (3)C9—O5—C8—Cs1114.8 (2)
O1—C1—C2—O268.3 (3)O4—C7—C8—O565.1 (3)
Cs1—C1—C2—O212.9 (2)O4—C7—C8—Cs116.76 (18)
C2—O2—C3—C4179.9 (2)C8—O5—C9—C10174.7 (2)
Cs1—O2—C3—C419.7 (3)Cs1—O5—C9—C1069.9 (2)
C5—O3—C4—C3177.6 (2)C8—O5—C9—Cs1115.4 (2)
Cs1—O3—C4—C371.6 (2)C11—O6—C10—C9177.6 (2)
C5—O3—C4—Cs1106.04 (19)Cs1—O6—C10—C919.1 (3)
O2—C3—C4—O365.0 (3)O5—C9—C10—O661.8 (3)
O2—C3—C4—Cs112.9 (2)Cs1—C9—C10—O612.51 (19)
C4—O3—C5—C6178.2 (2)C10—O6—C11—C12178.0 (2)
Cs1—O3—C5—C673.8 (2)Cs1—O6—C11—C1222.8 (3)
C4—O3—C5—Cs1107.9 (2)C1—O1—C12—C11178.0 (2)
C7—O4—C6—C5177.1 (2)Cs1—O1—C12—C1172.2 (2)
Cs1—O4—C6—C521.4 (3)C1—O1—C12—Cs1105.9 (2)
O3—C5—C6—O469.7 (3)O6—C11—C12—O167.9 (3)
Cs1—C5—C6—O414.61 (19)O6—C11—C12—Cs115.7 (2)
Symmetry code: (i) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···Br10.84 (1)2.59 (2)3.390 (3)160 (4)
O1W—H1WB···Br1i0.84 (1)2.67 (2)3.405 (3)147 (4)
O2W—H2WA···Br1ii0.84 (1)2.67 (2)3.497 (3)170 (5)
O2W—H2WB···O1W0.84 (1)2.11 (1)2.947 (4)174 (6)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+2, y, z+1.
Poly[[diaquadi-µ-chlorido-µ-(1,4,7,10,13,16-hexaoxacyclooctadecane)-dicaesium(I)] dihydrate] (II) top
Crystal data top
[Cs2Cl2(C12H24O6)(H2O)2]·2H2ODx = 1.870 Mg m3
Mr = 673.09Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, CmcmCell parameters from 51072 reflections
a = 14.2567 (6) Åθ = 2.5–30.8°
b = 10.4542 (4) ŵ = 3.31 mm1
c = 16.0386 (5) ÅT = 173 K
V = 2390.43 (16) Å3Block, colourless
Z = 40.23 × 0.17 × 0.13 mm
F(000) = 1312
Data collection top
Stoe IPDSII two-circle
diffractometer
1905 reflections with I > 2σ(I)
Radiation source: Genix 3D IµS microfocus X-ray sourceRint = 0.082
ω scansθmax = 30.4°, θmin = 2.4°
Absorption correction: multi-scan
(X-AREA; Stoe & Cie, 2001)
h = 2020
Tmin = 0.516, Tmax = 0.673k = 1414
31362 measured reflectionsl = 2222
1911 independent reflections
Refinement top
Refinement on F2Hydrogen site location: mixed
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.030 w = 1/[σ2(Fo2) + (0.0379P)2 + 6.3049P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.083(Δ/σ)max = 0.001
S = 1.21Δρmax = 0.66 e Å3
1911 reflectionsΔρmin = 1.05 e Å3
78 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0144 (6)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cs10.50000.59962 (2)0.60079 (2)0.02645 (13)
Cl10.32395 (7)0.61640 (8)0.75000.02649 (18)
O10.50000.7086 (3)0.38765 (19)0.0313 (6)
O20.33290 (14)0.62067 (18)0.46040 (13)0.0294 (4)
C10.4177 (2)0.7842 (3)0.38969 (18)0.0341 (6)
H1A0.41660.84280.34130.041*
H1B0.41640.83620.44120.041*
C20.3342 (2)0.6976 (3)0.38717 (18)0.0326 (5)
H2A0.27610.74910.38390.039*
H2B0.33740.64230.33720.039*
C30.25343 (18)0.5382 (3)0.46063 (16)0.0308 (5)
H3A0.25600.48020.41190.037*
H3B0.19520.58940.45690.037*
O1W0.50000.8914 (3)0.6284 (3)0.0420 (7)
H1WA0.547 (5)0.908 (5)0.657 (4)0.08 (2)*
O2W0.6480 (2)0.9205 (3)0.75000.0377 (6)
H2WA0.706 (5)0.960 (7)0.75000.058 (18)*
H2WB0.673 (5)0.849 (6)0.75000.052 (17)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.02644 (16)0.02666 (16)0.02626 (16)0.0000.0000.00422 (7)
Cl10.0276 (4)0.0258 (4)0.0261 (4)0.0003 (3)0.0000.000
O10.0316 (13)0.0212 (12)0.0412 (14)0.0000.0000.0025 (10)
O20.0267 (9)0.0299 (8)0.0315 (9)0.0002 (7)0.0073 (7)0.0013 (7)
C10.0402 (14)0.0202 (11)0.0421 (14)0.0040 (10)0.0039 (11)0.0032 (9)
C20.0347 (13)0.0273 (11)0.0359 (12)0.0038 (10)0.0100 (10)0.0018 (10)
C30.0223 (10)0.0387 (13)0.0312 (11)0.0001 (9)0.0032 (9)0.0039 (10)
O1W0.0419 (19)0.0340 (16)0.050 (2)0.0000.0000.0028 (14)
O2W0.0272 (13)0.0314 (13)0.0543 (19)0.0010 (11)0.0000.000
Geometric parameters (Å, º) top
Cs1—O1W3.082 (3)O1—Cs1i3.227 (3)
Cs1—O1i3.227 (3)O2—C21.424 (3)
Cs1—O23.2853 (19)O2—C31.424 (3)
Cs1—O2ii3.2853 (19)O2—Cs1i3.456 (2)
Cs1—O2iii3.456 (2)C1—C21.495 (4)
Cs1—O2i3.456 (2)C1—H1A0.9900
Cs1—Cl1iv3.4724 (7)C1—H1B0.9900
Cs1—Cl13.4724 (7)C2—Cs1i3.909 (3)
Cs1—O13.603 (3)C2—H2A0.9900
Cs1—Cs1i3.8458 (4)C2—H2B0.9900
Cs1—C2iii3.909 (3)C3—C3iii1.494 (5)
Cs1—C2i3.909 (3)C3—H3A0.9900
Cs1—H1WA3.41 (5)C3—H3B0.9900
Cl1—Cs1v3.4724 (7)O1W—H1WA0.83 (7)
O1—C1ii1.415 (3)O2W—H2WA0.92 (7)
O1—C11.415 (3)O2W—H2WB0.83 (7)
O1W—Cs1—O1i168.43 (11)O2ii—Cs1—C2i69.43 (6)
O1W—Cs1—O291.85 (7)O2iii—Cs1—C2i84.32 (5)
O1i—Cs1—O296.10 (5)O2i—Cs1—C2i21.16 (5)
O1W—Cs1—O2ii91.85 (7)Cl1iv—Cs1—C2i64.48 (4)
O1i—Cs1—O2ii96.10 (5)Cl1—Cs1—C2i116.30 (5)
O2—Cs1—O2ii92.96 (7)O1—Cs1—C2i107.35 (6)
O1W—Cs1—O2iii134.45 (4)Cs1i—Cs1—C2i67.11 (4)
O1i—Cs1—O2iii49.53 (4)C2iii—Cs1—C2i74.40 (9)
O2—Cs1—O2iii49.47 (7)O1W—Cs1—H1WA13.5 (11)
O2ii—Cs1—O2iii110.48 (4)O1i—Cs1—H1WA158.1 (11)
O1W—Cs1—O2i134.45 (4)O2—Cs1—H1WA105.1 (11)
O1i—Cs1—O2i49.53 (4)O2ii—Cs1—H1WA88.6 (11)
O2—Cs1—O2i110.48 (4)O2iii—Cs1—H1WA147.1 (11)
O2ii—Cs1—O2i49.47 (7)O2i—Cs1—H1WA124.7 (11)
O2iii—Cs1—O2i87.16 (6)Cl1iv—Cs1—H1WA68.2 (11)
O1W—Cs1—Cl1iv81.42 (6)Cl1—Cs1—H1WA85.0 (11)
O1i—Cs1—Cl1iv90.62 (4)O1—Cs1—H1WA87.2 (11)
O2—Cs1—Cl1iv173.26 (4)Cs1i—Cs1—H1WA137.2 (11)
O2ii—Cs1—Cl1iv86.84 (4)C2iii—Cs1—H1WA148.9 (11)
O2iii—Cs1—Cl1iv136.69 (4)C2i—Cs1—H1WA128.2 (11)
O2i—Cs1—Cl1iv74.40 (4)Cs1v—Cl1—Cs187.13 (2)
O1W—Cs1—Cl181.42 (6)C1ii—O1—C1112.1 (3)
O1i—Cs1—Cl190.62 (4)C1ii—O1—Cs1i123.78 (16)
O2—Cs1—Cl186.84 (4)C1—O1—Cs1i123.78 (16)
O2ii—Cs1—Cl1173.26 (4)C1ii—O1—Cs198.89 (17)
O2iii—Cs1—Cl174.40 (4)C1—O1—Cs198.89 (17)
O2i—Cs1—Cl1136.69 (4)Cs1i—O1—Cs168.28 (5)
Cl1iv—Cs1—Cl192.57 (2)C2—O2—C3110.8 (2)
O1W—Cs1—O179.84 (10)C2—O2—Cs1126.41 (16)
O1i—Cs1—O1111.72 (5)C3—O2—Cs1122.32 (15)
O2—Cs1—O147.83 (4)C2—O2—Cs1i97.64 (16)
O2ii—Cs1—O147.83 (4)C3—O2—Cs1i98.37 (14)
O2iii—Cs1—O186.63 (5)Cs1—O2—Cs1i69.52 (4)
O2i—Cs1—O186.63 (5)O1—C1—C2108.7 (2)
Cl1iv—Cs1—O1129.63 (2)O1—C1—H1A109.9
Cl1—Cs1—O1129.63 (2)C2—C1—H1A109.9
O1W—Cs1—Cs1i131.06 (9)O1—C1—H1B109.9
O1i—Cs1—Cs1i60.50 (5)C2—C1—H1B109.9
O2—Cs1—Cs1i57.33 (4)H1A—C1—H1B108.3
O2ii—Cs1—Cs1i57.33 (4)O2—C2—C1109.3 (2)
O2iii—Cs1—Cs1i53.16 (3)O2—C2—Cs1i61.20 (13)
O2i—Cs1—Cs1i53.16 (3)C1—C2—Cs1i89.93 (16)
Cl1iv—Cs1—Cs1i127.355 (13)O2—C2—H2A109.8
Cl1—Cs1—Cs1i127.355 (13)C1—C2—H2A109.8
O1—Cs1—Cs1i51.22 (5)Cs1i—C2—H2A160.3
O1W—Cs1—C2iii141.23 (5)O2—C2—H2B109.8
O1i—Cs1—C2iii37.20 (4)C1—C2—H2B109.8
O2—Cs1—C2iii69.43 (6)Cs1i—C2—H2B63.1
O2ii—Cs1—C2iii121.70 (5)H2A—C2—H2B108.3
O2iii—Cs1—C2iii21.16 (5)O2—C3—C3iii109.01 (18)
O2i—Cs1—C2iii84.32 (5)O2—C3—H3A109.9
Cl1iv—Cs1—C2iii116.30 (5)C3iii—C3—H3A109.9
Cl1—Cs1—C2iii64.48 (4)O2—C3—H3B109.9
O1—Cs1—C2iii107.35 (6)C3iii—C3—H3B109.9
Cs1i—Cs1—C2iii67.11 (4)H3A—C3—H3B108.3
O1W—Cs1—C2i141.23 (5)Cs1—O1W—H1WA107 (3)
O1i—Cs1—C2i37.20 (4)H2WA—O2W—H2WB91 (6)
O2—Cs1—C2i121.70 (5)
C1ii—O1—C1—C2179.88 (19)Cs1—O2—C2—Cs1i70.14 (13)
Cs1i—O1—C1—C26.9 (3)O1—C1—C2—O264.0 (3)
Cs1—O1—C1—C276.7 (2)O1—C1—C2—Cs1i4.8 (2)
C3—O2—C2—C1179.2 (2)C2—O2—C3—C3iii178.5 (2)
Cs1—O2—C2—C18.7 (3)Cs1—O2—C3—C3iii8.9 (3)
Cs1i—O2—C2—C178.8 (2)Cs1i—O2—C3—C3iii79.9 (2)
C3—O2—C2—Cs1i102.01 (19)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z; (iii) x, y+1, z+1; (iv) x+1, y, z+3/2; (v) x, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2A···Cl1vi0.992.943.702 (3)135
C3—H3A···Cl1vii0.992.953.877 (3)156
O1W—H1WA···O2W0.83 (7)2.08 (7)2.889 (4)166 (6)
O2W—H2WA···Cl1viii0.92 (7)2.35 (7)3.239 (3)162 (6)
O2W—H2WB···Cl1iv0.83 (7)2.43 (7)3.205 (3)156 (6)
Symmetry codes: (iv) x+1, y, z+3/2; (vi) x+1/2, y+3/2, z+1; (vii) x, y+1, z1/2; (viii) x+1/2, y+1/2, z.
Atomic ratios of Cs, Cl and Br as determined by EDX analysis top
CompoundElementat.%
(I)Cs51.6
(I)Br48.4
(II)Cs48.2
(II)Cl51.8
 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds