Download citation
Download citation
link to html
The structure of the one-dimensional anti­ferromagnet caesium diaqua­trichloro­manganate(II) was re-refined based on area-detector data, including the positions of H atoms. The MnII atom, on a twofold rotation axis, is in a distorted octa­hedral coordination by two bridging Cl ligands in trans positions, two terminal Cl ligands and two aqua ligands, both in cis positions. Hydrogen bonds of the type O—H...Cl connect octa­hedra along the chain and link the chains into layers which are separated by the Cs ions (also on twofold axes). The structure is discussed in comparison with non-isotypic related compounds of the morphotropic series AMCl3(H2O)2 (A = Cs, Rb, K and M = Mn, Fe, Co).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806054742/wm2084sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806054742/wm2084Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](n-O) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.068
  • Data-to-parameter ratio = 27.8

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.596 0.625 Tmin and Tmax expected: 0.590 0.740 RR = 1.197 Please check that your absorption correction is appropriate. GOODF01_ALERT_2_C The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 0.784 PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.20 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.18
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 1.184 Tmax scaled 0.740 Tmin scaled 0.706 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: EXPOSE (Stoe & Cie, 1999); cell refinement: CELL (Stoe & Cie, 1999); data reduction: INTEGRATE (Stoe & Cie, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (version 1.0c; Westrip, 2006).

caesium diaquatrichloromanganate(II) top
Crystal data top
Cs[MnCl3(H2O)2]F(000) = 604
Mr = 330.23Dx = 2.925 Mg m3
Orthorhombic, PccaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2a 2acCell parameters from 2772 reflections
a = 9.0307 (12) Åθ = 3.5–29.3°
b = 7.2636 (8) ŵ = 7.52 mm1
c = 11.4312 (13) ÅT = 293 K
V = 749.83 (15) Å3Irregular, colourless
Z = 40.10 × 0.06 × 0.04 mm
Data collection top
Stoe IPDS
diffractometer
1002 independent reflections
Radiation source: fine-focus sealed tube529 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.099
Detector resolution: 6.7 pixels mm-1θmax = 29.0°, θmin = 3.6°
φ scansh = 1212
Absorption correction: multi-scan
(Blessing, 1995)
k = 99
Tmin = 0.596, Tmax = 0.625l = 1515
9154 measured reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: difference Fourier map
wR(F2) = 0.068H-atom parameters constrained
S = 0.78 w = 1/[σ2(Fo2) + (0.029P)2]
where P = (Fo2 + 2Fc2)/3
1002 reflections(Δ/σ)max < 0.001
36 parametersΔρmax = 1.38 e Å3
0 restraintsΔρmin = 0.94 e Å3
Special details top

Experimental. Owing to the small and irregular size of the crystal a semiempirical absorption correction was prefered

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
xyzUiso*/Ueq
Cs10.25000.00000.14585 (5)0.03770 (18)
Mn10.00000.46686 (15)0.25000.0235 (3)
Cl10.25000.50000.14997 (18)0.0261 (4)
Cl20.08913 (17)0.22201 (18)0.39016 (16)0.0284 (3)
O10.0707 (5)0.6819 (6)0.3712 (4)0.0345 (12)
H10.03130.70290.43750.07 (2)*
H20.16140.71330.37250.07 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.0404 (3)0.0344 (3)0.0383 (3)0.0127 (3)0.0000.000
Mn10.0217 (6)0.0237 (6)0.0252 (7)0.0000.0006 (5)0.000
Cl10.0205 (8)0.0322 (8)0.0256 (9)0.0010 (11)0.0000.000
Cl20.0257 (7)0.0328 (8)0.0267 (7)0.0001 (6)0.0011 (7)0.0030 (6)
O10.023 (3)0.045 (2)0.036 (4)0.008 (2)0.004 (2)0.016 (2)
Geometric parameters (Å, º) top
Cs1—Cl2i3.4856 (15)Mn1—O1ii2.183 (4)
Cs1—Cl2ii3.4856 (15)Mn1—Cl2ii2.5255 (18)
Cs1—Cl23.5371 (18)Mn1—Cl22.5255 (18)
Cs1—Cl2iii3.5371 (18)Mn1—Cl12.5422 (10)
Cs1—Cl13.6321 (4)Mn1—Cl1ix2.5422 (10)
Cs1—Cl1iv3.6321 (4)Mn1—Cs1x4.2443 (10)
Cs1—Cl2v3.6405 (18)Cl1—Mn1xi2.5422 (10)
Cs1—Cl2vi3.6405 (18)Cl1—Cs1xii3.6321 (4)
Cs1—O1vii3.710 (5)Cl2—Cs1x3.4856 (15)
Cs1—O1viii3.710 (5)Cl2—Cs1xiii3.6405 (18)
Mn1—O12.183 (4)
Cl2i—Cs1—Cl2ii166.43 (6)Cl2i—Cs1—O1viii66.18 (7)
Cl2i—Cs1—Cl2131.69 (3)Cl2ii—Cs1—O1viii113.05 (7)
Cl2ii—Cs1—Cl261.41 (5)Cl2—Cs1—O1viii94.48 (7)
Cl2i—Cs1—Cl2iii61.41 (5)Cl2iii—Cs1—O1viii90.28 (8)
Cl2ii—Cs1—Cl2iii131.69 (3)Cl1—Cs1—O1viii51.53 (7)
Cl2—Cs1—Cl2iii75.71 (5)Cl1iv—Cs1—O1viii128.57 (7)
Cl2i—Cs1—Cl1117.65 (2)Cl2v—Cs1—O1viii123.04 (8)
Cl2ii—Cs1—Cl162.54 (2)Cl2vi—Cs1—O1viii50.98 (7)
Cl2—Cs1—Cl162.22 (4)O1vii—Cs1—O1viii173.98 (15)
Cl2iii—Cs1—Cl1116.46 (4)O1—Mn1—O1ii88.7 (3)
Cl2i—Cs1—Cl1iv62.54 (2)O1—Mn1—Cl2ii178.37 (13)
Cl2ii—Cs1—Cl1iv117.65 (2)O1ii—Mn1—Cl2ii90.45 (13)
Cl2—Cs1—Cl1iv116.46 (4)O1—Mn1—Cl290.45 (13)
Cl2iii—Cs1—Cl1iv62.22 (4)O1ii—Mn1—Cl2178.37 (13)
Cl1—Cs1—Cl1iv178.51 (7)Cl2ii—Mn1—Cl290.47 (8)
Cl2i—Cs1—Cl2v92.92 (3)O1—Mn1—Cl187.59 (13)
Cl2ii—Cs1—Cl2v76.08 (4)O1ii—Mn1—Cl184.64 (13)
Cl2—Cs1—Cl2v132.22 (5)Cl2ii—Mn1—Cl193.69 (5)
Cl2iii—Cs1—Cl2v126.57 (4)Cl2—Mn1—Cl193.96 (5)
Cl1—Cs1—Cl2v116.96 (4)O1—Mn1—Cl1ix84.64 (13)
Cl1iv—Cs1—Cl2v64.37 (4)O1ii—Mn1—Cl1ix87.59 (13)
Cl2i—Cs1—Cl2vi76.08 (4)Cl2ii—Mn1—Cl1ix93.96 (5)
Cl2ii—Cs1—Cl2vi92.92 (3)Cl2—Mn1—Cl1ix93.69 (5)
Cl2—Cs1—Cl2vi126.57 (4)Cl1—Mn1—Cl1ix169.13 (5)
Cl2iii—Cs1—Cl2vi132.22 (5)Mn1xi—Cl1—Mn1126.54 (8)
Cl1—Cs1—Cl2vi64.37 (4)Mn1xi—Cl1—Cs195.77 (3)
Cl1iv—Cs1—Cl2vi116.96 (4)Mn1—Cl1—Cs184.90 (3)
Cl2v—Cs1—Cl2vi73.20 (5)Mn1xi—Cl1—Cs1xii84.90 (3)
Cl2i—Cs1—O1vii113.05 (7)Mn1—Cl1—Cs1xii95.77 (3)
Cl2ii—Cs1—O1vii66.18 (7)Cs1—Cl1—Cs1xii178.51 (7)
Cl2—Cs1—O1vii90.28 (8)Mn1—Cl2—Cs1x88.33 (5)
Cl2iii—Cs1—O1vii94.48 (7)Mn1—Cl2—Cs187.19 (5)
Cl1—Cs1—O1vii128.57 (7)Cs1x—Cl2—Cs193.25 (4)
Cl1iv—Cs1—O1vii51.53 (7)Mn1—Cl2—Cs1xiii161.53 (6)
Cl2v—Cs1—O1vii50.98 (7)Cs1x—Cl2—Cs1xiii103.92 (4)
Cl2vi—Cs1—O1vii123.04 (8)Cs1—Cl2—Cs1xiii105.55 (4)
Symmetry codes: (i) x+1/2, y, z+1/2; (ii) x, y, z+1/2; (iii) x+1/2, y, z; (iv) x, y1, z; (v) x, y, z1/2; (vi) x+1/2, y, z1/2; (vii) x, y1, z+1/2; (viii) x+1/2, y+1, z+1/2; (ix) x1/2, y+1, z+1/2; (x) x1/2, y, z+1/2; (xi) x+1/2, y+1, z; (xii) x, y+1, z; (xiii) x+1/2, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···Cl2xiv0.852.323.164 (5)175
O1—H2···Cl2xi0.852.313.158 (5)175
Symmetry codes: (xi) x+1/2, y+1, z; (xiv) x, y+1, z+1.
 

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