Hexa­aqua­[μ-di-μ-oxo-bis­(hydroxo­dioxo­iodate)]dieuropium(III) bis­(perchlorate) dihydrate

The title compound, [Eu₂(H₂I₂O₁₀)(H₂O)₆](ClO₄)₂·2H₂O, is iso­structural with the corresponding Pr, Sm and Gd phases. It features Eu³⁺ cations, which are coordinated by centrosymmetric H₂I₂O₁₀⁴⁻ anions and water mol­ecules, forming positively charged sheets, separated by perchlorate anions and non-coordinated water mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 299 K
• Mean [sigma](l-O) = 0.005 Å
• H-atom completeness 12%
• R factor = 0.031
• wR factor = 0.077
• Data-to-parameter ratio = 22.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O13

Author Response: No H atoms could be located on the water of crystallization. (On all water molecules in the structure, to be accurate ...)

Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O13     ..       2.83 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O9      ..       2.83 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O4     ..  O10     ..       2.84 Ang.

Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight           531.38
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           Cl       35.45    1.00   35.45
           Eu      151.96    1.00  151.96
           I       126.90    1.00  126.90
           O        16.00   13.00  207.99
           H         1.01    1.00    1.01
           Calculated formula weight              523.31
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................     531.38
PLAT044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.47 Ratio
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         Cl
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.28

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:H9 Cl1 Eu1 I1 O13
            Atom count from the _atom_site data:  H1 Cl1 Eu1 I1 O13
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  Cl Eu H9 I O13
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           Cl         4.00      4.00    0.00
           Eu         4.00      4.00    0.00
           H         36.00      4.00   32.00
           I          4.00      4.00    0.00
           O         52.00     52.00    0.00

   1 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   9 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

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Computing details

Data collection: COLLECT (Nonius, 1999); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: maXus (Mackay et al., 1999).

hexaaqua[µ-di-µ-oxo-bis(hydroxodioxoiodate)]dieuropium(III) bis(perchlorate) dihydrate

Crystal data

[Eu2(H2I2O10)(H2O)6](ClO4)2·2H2O	Z = 4
Mr = 531.38	Dx = 3.348 Mg m^−3
Monoclinic, P21/c	Ag Kα radiation, λ = 0.5608 Å
Hall symbol: -P 2ybc	Cell parameters from 17576 reflections
a = 10.8602 (4) Å	θ = 4.1–23.6°
b = 7.1828 (3) Å	µ = 4.88 mm^−1
c = 13.7933 (5) Å	T = 299 K
β = 101.584 (2)°	Plate, colourless
V = 1054.05 (7) Å^3	0.12 × 0.07 × 0.04 mm

Data collection

Bruker–Nonius KappaCCD diffractometer	2723 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.060
ω and φ scans	θmax = 23.6°, θmin = 4.1°
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1997)	h = −15→15
Tmin = 0.593, Tmax = 0.866	k = −10→10
17576 measured reflections	l = −19→19
3211 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.077	w = 1/[σ^2(Fo^2) + (0.0346P)^2 + 3.015P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
3211 reflections	Δρmax = 1.84 e Å^−3
145 parameters	Δρmin = −1.65 e Å^−3
0 restraints

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Eu	−0.014649 (19)	0.14236 (3)	0.182210 (13)	0.01049 (7)
Cl	0.53872 (12)	0.26539 (18)	0.38506 (9)	0.0250 (2)
I	0.06359 (2)	0.13666 (3)	0.441684 (16)	0.00817 (7)
O1	0.2106 (3)	0.1575 (6)	0.2297 (3)	0.0301 (9)
O2	−0.1879 (3)	0.0887 (5)	0.0454 (2)	0.0202 (7)
O3	−0.0060 (3)	−0.1894 (4)	0.1552 (2)	0.0130 (6)
O4	−0.2189 (4)	0.1169 (7)	0.2317 (3)	0.0366 (10)
O5	0.0471 (3)	−0.0344 (4)	0.3387 (2)	0.0122 (6)
O6	−0.1038 (3)	0.0680 (4)	0.4616 (2)	0.0105 (5)
O7	0.0802 (3)	0.3064 (4)	0.5415 (2)	0.0128 (6)
O8	0.2341 (3)	0.1488 (4)	0.4368 (2)	0.0163 (6)
O9	0.5844 (5)	0.2121 (7)	0.4858 (3)	0.0442 (11)
O10	0.6429 (4)	0.3315 (8)	0.3465 (4)	0.0489 (13)
O11	0.4826 (6)	0.1071 (8)	0.3316 (4)	0.0554 (14)
O12	0.4477 (5)	0.4100 (7)	0.3802 (4)	0.0500 (12)
O13	0.3799 (4)	0.2357 (6)	0.6084 (3)	0.0300 (8)
H8	0.2813	0.1741	0.4846	0.020*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Eu	0.01720 (12)	0.00812 (12)	0.00664 (11)	−0.00004 (7)	0.00355 (7)	0.00033 (6)
Cl	0.0225 (5)	0.0274 (6)	0.0242 (5)	0.0006 (5)	0.0020 (4)	−0.0028 (4)
I	0.01491 (13)	0.00619 (13)	0.00394 (11)	−0.00051 (9)	0.00317 (8)	0.00009 (7)
O1	0.0179 (16)	0.058 (3)	0.0138 (15)	0.0003 (17)	0.0025 (12)	0.0086 (16)
O2	0.0214 (16)	0.0223 (17)	0.0145 (14)	0.0000 (13)	−0.0018 (11)	−0.0004 (12)
O3	0.0236 (15)	0.0077 (13)	0.0073 (12)	−0.0005 (12)	0.0022 (10)	−0.0028 (10)
O4	0.0250 (19)	0.063 (3)	0.0246 (19)	−0.0118 (19)	0.0128 (15)	−0.0142 (19)
O5	0.0219 (14)	0.0098 (14)	0.0057 (11)	−0.0021 (11)	0.0046 (10)	−0.0027 (10)
O6	0.0141 (13)	0.0086 (13)	0.0095 (12)	0.0003 (10)	0.0042 (10)	0.0033 (10)
O7	0.0210 (15)	0.0102 (14)	0.0083 (12)	−0.0032 (12)	0.0053 (11)	−0.0038 (10)
O8	0.0151 (14)	0.0229 (18)	0.0113 (13)	−0.0019 (12)	0.0039 (11)	−0.0021 (11)
O9	0.048 (3)	0.055 (3)	0.027 (2)	−0.014 (2)	−0.0003 (18)	0.007 (2)
O10	0.039 (3)	0.064 (4)	0.051 (3)	0.000 (2)	0.025 (2)	0.007 (2)
O11	0.063 (3)	0.039 (3)	0.054 (3)	−0.003 (3)	−0.015 (2)	−0.014 (2)
O12	0.037 (3)	0.044 (3)	0.070 (3)	0.015 (2)	0.014 (2)	0.000 (2)
O13	0.0246 (18)	0.037 (2)	0.0267 (18)	0.0011 (16)	0.0022 (14)	−0.0066 (16)

Geometric parameters (Å, º)

Eu—O5^i	2.357 (3)	Cl—O9	1.431 (4)
Eu—O7^ii	2.402 (3)	I—O7	1.820 (3)
Eu—O1	2.404 (4)	I—O3^i	1.844 (3)
Eu—O2	2.413 (3)	I—O5	1.859 (3)
Eu—O3	2.417 (3)	I—O8	1.868 (3)
Eu—O4	2.455 (4)	I—O6	1.955 (3)
Eu—O5	2.478 (3)	I—O6^iv	1.974 (3)
Eu—O3^i	2.518 (3)	I—I^iv	3.0401 (5)
Eu—I	3.5087 (3)	O3—I^iii	1.844 (3)
Eu—Eu^i	4.0321 (2)	O3—Eu^iii	2.518 (3)
Eu—Eu^iii	4.0322 (2)	O5—Eu^iii	2.357 (3)
Cl—O11	1.424 (5)	O6—I^iv	1.974 (3)
Cl—O10	1.425 (5)	O7—Eu^v	2.402 (3)
Cl—O12	1.426 (5)	O8—H8	0.7705
O5^i—Eu—O7^ii	80.08 (10)	O11—Cl—O12	109.7 (3)
O5^i—Eu—O1	96.19 (13)	O10—Cl—O12	109.5 (3)
O7^ii—Eu—O1	68.61 (11)	O11—Cl—O9	108.6 (3)
O5^i—Eu—O2	89.29 (11)	O10—Cl—O9	107.8 (3)
O7^ii—Eu—O2	77.65 (11)	O12—Cl—O9	110.0 (3)
O1—Eu—O2	144.21 (12)	O7—I—O3^i	93.54 (14)
O5^i—Eu—O3	164.09 (10)	O7—I—O5	179.29 (13)
O7^ii—Eu—O3	89.44 (10)	O3^i—I—O5	85.87 (13)
O1—Eu—O3	91.01 (13)	O7—I—O8	92.71 (14)
O2—Eu—O3	76.71 (11)	O3^i—I—O8	97.87 (14)
O5^i—Eu—O4	89.21 (14)	O5—I—O8	86.98 (13)
O7^ii—Eu—O4	142.59 (12)	O7—I—O6	90.95 (13)
O1—Eu—O4	148.66 (13)	O3^i—I—O6	94.76 (13)
O2—Eu—O4	66.39 (12)	O5—I—O6	89.49 (13)
O3—Eu—O4	91.99 (14)	O8—I—O6	166.60 (13)
O5^i—Eu—O5	128.25 (8)	O7—I—O6^iv	90.75 (13)
O7^ii—Eu—O5	134.24 (10)	O3^i—I—O6^iv	172.20 (13)
O1—Eu—O5	72.73 (11)	O5—I—O6^iv	89.88 (12)
O2—Eu—O5	129.16 (11)	O8—I—O6^iv	88.42 (13)
O3—Eu—O5	67.49 (9)	O6—I—O6^iv	78.64 (13)
O4—Eu—O5	79.70 (13)	I^iii—O3—Eu	139.61 (15)
O5^i—Eu—O3^i	67.73 (9)	I^iii—O3—Eu^iii	106.07 (13)
O7^ii—Eu—O3^i	132.11 (10)	Eu—O3—Eu^iii	109.57 (11)
O1—Eu—O3^i	80.32 (12)	I—O5—Eu^iii	137.20 (15)
O2—Eu—O3^i	133.57 (11)	I—O5—Eu	107.11 (13)
O3—Eu—O3^i	127.69 (8)	Eu^iii—O5—Eu	112.97 (11)
O4—Eu—O3^i	73.25 (12)	I—O6—I^iv	101.36 (13)
O5—Eu—O3^i	60.64 (9)	I—O7—Eu^v	136.08 (15)
O11—Cl—O10	111.2 (4)	I—O8—H8	118.3

Symmetry codes: (i) −x, y+1/2, −z+1/2; (ii) x, −y+1/2, z−1/2; (iii) −x, y−1/2, −z+1/2; (iv) −x, −y, −z+1; (v) x, −y+1/2, z+1/2.