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A single crystal of commercially available `iron(III) perchlor­ate hexa­hydrate' has been structurally characterized and shown to be hexa­aqua­iron(III) tris­(perchlorate) trihydrate, [Fe(H2O)6](ClO4)3·3H2O. The structure contains [Fe(H2O)6]3+ complex ions, charge-balancing perchlorate ions and three water mol­ecules of crystallization per Fe atom. A network of O—H...O hydrogen bonds helps to stabilize the crystal packing. Fe, Cl and one water O atom occupy special positions with site symmetries \overline{3}, 2, and 2, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806008555/hb2019sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806008555/hb2019Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 250 K
  • Mean [sigma](l-O) = 0.005 Å
  • R factor = 0.046
  • wR factor = 0.114
  • Data-to-parameter ratio = 16.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cl1
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX/LSQ (Duisenberg et al., 2003); data reduction: EVALCCD (Duisenberg, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: maXus (Mackay et al., 1999).

hexaaquairon(III) tris(perchlorate) trihydrate top
Crystal data top
[Fe(H2O)6](ClO4)3·3H2ODx = 2.031 Mg m3
Mr = 516.33Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3cCell parameters from 44 reflections
Hall symbol: -R 3 2"cθ = 9.2–20.2°
a = 16.047 (2) ŵ = 1.47 mm1
c = 11.3561 (13) ÅT = 250 K
V = 2532.5 (5) Å3Needle, colourless
Z = 60.45 × 0.10 × 0.09 mm
F(000) = 1578
Data collection top
Bruker-Nonius KappaCCD
diffractometer
Rint = 0.044
Radiation source: fine-focus sealed tubeθmax = 27.5°, θmin = 4.6°
φ and ω scansh = 1620
8799 measured reflectionsk = 2020
652 independent reflectionsl = 1414
555 reflections with I > 2σ(I)
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046H-atom parameters constrained
wR(F2) = 0.114 w = 1/[σ2(Fo2) + (0.0447P)2 + 20.7174P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
652 reflectionsΔρmax = 0.68 e Å3
39 parametersΔρmin = 0.43 e Å3
0 restraints
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 &gt; 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
Fe10.00000.00000.00000.0241 (3)
Cl10.25203 (7)0.33330.08330.0443 (4)
O40.18680.00000.25000.0336 (7)
O10.11625 (16)0.07358 (16)0.0997 (2)0.0339 (6)
O20.1873 (3)0.3021 (4)0.1797 (5)0.1152 (19)
O30.2653 (2)0.2565 (2)0.0453 (4)0.0675 (10)
H40.24200.04770.29310.040*
H1A0.16250.13280.08900.041*
H1B0.14060.04990.14140.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0200 (3)0.0200 (3)0.0322 (6)0.0100.0000.000
Cl10.0220 (4)0.0266 (6)0.0859 (10)0.0133 (3)0.0034 (3)0.0068 (6)
O40.0274 (12)0.0346 (18)0.0413 (19)0.0173 (9)0.0028 (7)0.0055 (14)
O10.0275 (12)0.0228 (11)0.0461 (13)0.0085 (9)0.0102 (10)0.0006 (9)
O20.068 (3)0.123 (4)0.167 (5)0.057 (3)0.069 (3)0.054 (3)
O30.059 (2)0.0368 (17)0.104 (3)0.0218 (15)0.0059 (18)0.0167 (17)
Geometric parameters (Å, º) top
Fe1—O1i1.988 (2)Cl1—O21.417 (4)
Fe1—O1ii1.988 (2)Cl1—O31.419 (3)
Fe1—O11.988 (2)Cl1—O3vi1.419 (3)
Fe1—O1iii1.988 (2)O4—H40.9654
Fe1—O1iv1.988 (2)O1—H1A0.8732
Fe1—O1v1.988 (2)O1—H1B0.8189
Cl1—O2vi1.417 (4)
O1i—Fe1—O1ii180.0O1—Fe1—O1v90.80 (10)
O1i—Fe1—O189.20 (10)O1iii—Fe1—O1v89.20 (10)
O1ii—Fe1—O190.80 (10)O1iv—Fe1—O1v180.0
O1i—Fe1—O1iii90.80 (10)O2vi—Cl1—O2112.5 (4)
O1ii—Fe1—O1iii89.20 (10)O2vi—Cl1—O3108.7 (3)
O1—Fe1—O1iii180.0O2—Cl1—O3109.2 (3)
O1i—Fe1—O1iv90.80 (10)O2vi—Cl1—O3vi109.2 (3)
O1ii—Fe1—O1iv89.20 (10)O2—Cl1—O3vi108.7 (3)
O1—Fe1—O1iv89.20 (10)O3—Cl1—O3vi108.5 (3)
O1iii—Fe1—O1iv90.80 (10)Fe1—O1—H1A127.0
O1i—Fe1—O1v89.20 (10)Fe1—O1—H1B125.3
O1ii—Fe1—O1v90.80 (10)H1A—O1—H1B104.0
Symmetry codes: (i) y, x+y, z; (ii) y, xy, z; (iii) x, y, z; (iv) xy, x, z; (v) x+y, x, z; (vi) xy+1/3, y+2/3, z+1/6.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···O2vii0.971.972.745 (4)136
O4—H4···O3viii0.972.363.052 (3)128
O1—H1A···O30.871.912.775 (4)172
O1—H1B···O40.821.822.632 (2)173
Symmetry codes: (vii) y, x, z+1/2; (viii) x+2/3, y+1/3, z+1/3.
 

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