Heptaaqua­bis(hydrogen maleato-κO)europium(III) hydrogen maleate monohydrate

The title compound, [Eu(C₄H₃O₄)₂(H₂O)₇](C₄H₃O₄)·H₂O, is isostructural with the Nd^III analogue. The Eu^III atom is coordinated by O atoms from two hydrogen maleate anions and by seven water mol­ecules, forming a distorted monocapped square-anti­prismatic coordination geometry.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.027
• wR factor = 0.071
• Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)        3000 Deg.

Alert level G
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
   1 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXL97.

Heptaaquabis(hydrogen maleato-κO)europium(III) hydrogen maleate monohydrate

Crystal data

[Eu(C4H3O4)2(H2O)7](C4H3O4)·H2O	Z = 2
Mr = 641.28	F(000) = 640
Triclinic, P1	Dx = 1.906 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.2220 (14) Å	Cell parameters from 25 reflections
b = 10.350 (2) Å	θ = 10–13°
c = 16.672 (3) Å	µ = 2.90 mm^−1
α = 72.08 (3)°	T = 293 K
β = 88.06 (3)°	Block, colourless
γ = 70.89 (3)°	0.40 × 0.30 × 0.20 mm
V = 1117.3 (5) Å^3

Data collection

Enraf–Nonius CAD-4 diffractometer	4144 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.020
Graphite monochromator	θmax = 26.0°, θmin = 1.3°
ω/2θ scans	h = 0→8
Absorption correction: ψ scan (North et al., 1968)	k = −12→12
Tmin = 0.375, Tmax = 0.568	l = −20→20
4740 measured reflections	3 standard reflections every 200 reflections
4370 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.027	H-atom parameters constrained
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.0416P)^2 + 1.2441P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
4370 reflections	Δρmax = 0.82 e Å^−3
299 parameters	Δρmin = −1.13 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0244 (9)

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	0.65240 (2)	0.379834 (16)	0.261504 (11)	0.02234 (9)
C1	1.0274 (6)	−0.3440 (4)	0.3657 (3)	0.0301 (8)
C2	0.9111 (6)	−0.2654 (4)	0.4213 (2)	0.0308 (8)
H2A	0.8811	−0.3237	0.4711	0.037*
C3	0.8423 (6)	−0.1252 (4)	0.4120 (2)	0.0299 (8)
H3A	0.7767	−0.1017	0.4572	0.036*
C4	0.8539 (5)	0.0003 (4)	0.3405 (2)	0.0270 (7)
C5	0.5181 (6)	0.6692 (4)	0.3520 (3)	0.0301 (8)
C6	0.4258 (6)	0.7151 (4)	0.4242 (3)	0.0322 (8)
H6B	0.4148	0.6407	0.4704	0.039*
C7	0.3563 (6)	0.8453 (4)	0.4335 (2)	0.0301 (8)
H7B	0.3029	0.8475	0.4848	0.036*
C8	0.3506 (5)	0.9891 (4)	0.3741 (2)	0.0285 (8)
C9	0.8106 (7)	−0.1631 (4)	0.0167 (3)	0.0396 (10)
C10	0.8114 (7)	−0.0857 (5)	0.0786 (3)	0.0426 (10)
H10B	0.8559	−0.1453	0.1335	0.051*
C11	0.7592 (7)	0.0539 (5)	0.0684 (3)	0.0424 (10)
H11B	0.7702	0.0762	0.1175	0.051*
C12	0.6863 (7)	0.1801 (4)	−0.0084 (3)	0.0394 (10)
O1	1.0777 (5)	−0.4765 (3)	0.3906 (2)	0.0431 (7)
O2	1.0757 (5)	−0.2747 (3)	0.29496 (19)	0.0408 (7)
H1	1.0148	−0.1477	0.2862	0.061*
O3	0.9538 (5)	−0.0205 (3)	0.27747 (19)	0.0427 (7)
O4	0.7671 (4)	0.1208 (3)	0.34546 (18)	0.0333 (6)
O5	0.5621 (4)	0.5404 (3)	0.35777 (18)	0.0363 (6)
O6	0.5515 (5)	0.7617 (3)	0.28634 (19)	0.0443 (8)
H2	0.4873	0.8795	0.2942	0.066*
O7	0.4228 (5)	0.9976 (3)	0.30209 (18)	0.0384 (7)
O8	0.2792 (5)	1.0943 (3)	0.3983 (2)	0.0412 (7)
O9	0.8572 (6)	−0.2955 (3)	0.0425 (2)	0.0497 (8)
O10	0.7633 (6)	−0.0923 (4)	−0.0623 (2)	0.0585 (10)
H3	0.7135	0.0354	−0.0707	0.088*
O11	0.6634 (6)	0.1637 (3)	−0.0792 (2)	0.0565 (10)
O12	0.6496 (6)	0.3010 (3)	−0.0005 (2)	0.0608 (11)
O13	0.7888 (5)	0.5737 (3)	0.20899 (18)	0.0386 (7)
H13A	0.7201	0.6514	0.2303	0.058*
H13B	0.7739	0.6074	0.1483	0.058*
O14	0.3434 (4)	0.5770 (3)	0.20265 (18)	0.0381 (7)
H14C	0.2670	0.5988	0.2480	0.057*
H14B	0.3722	0.6608	0.1689	0.057*
O15	0.6351 (4)	0.4610 (3)	0.10487 (17)	0.0351 (6)
H15A	0.6279	0.3851	0.0848	0.053*
H15B	0.5201	0.5442	0.0834	0.053*
O16	0.4955 (4)	0.2484 (3)	0.20400 (18)	0.0368 (6)
H16A	0.4507	0.1853	0.2494	0.055*
H16B	0.3856	0.3156	0.1657	0.055*
O17	0.9599 (4)	0.2620 (3)	0.2076 (2)	0.0429 (7)
H17A	0.9928	0.3321	0.1620	0.064*
H17B	0.9437	0.1886	0.1875	0.064*
O18	0.9062 (4)	0.3209 (3)	0.3729 (2)	0.0403 (7)
H18A	0.9343	0.4063	0.3709	0.060*
H18B	1.0233	0.2502	0.3645	0.060*
O19	0.4159 (4)	0.3270 (3)	0.36138 (19)	0.0362 (6)
H19A	0.3636	0.2615	0.3478	0.054*
H19B	0.3112	0.4147	0.3582	0.054*
O20	0.1710 (4)	0.4023 (3)	0.08991 (19)	0.0398 (7)
H20A	0.1383	0.5031	0.0824	0.060*
H20B	0.2005	0.3855	0.0367	0.060*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Eu	0.02989 (13)	0.02022 (11)	0.02377 (12)	−0.00620 (7)	0.00337 (7)	−0.00508 (7)
C1	0.0336 (19)	0.0230 (17)	0.037 (2)	−0.0077 (15)	0.0046 (16)	−0.0098 (16)
C2	0.038 (2)	0.0203 (17)	0.0289 (19)	−0.0063 (15)	0.0046 (16)	−0.0046 (15)
C3	0.039 (2)	0.0210 (18)	0.0272 (19)	−0.0058 (15)	0.0093 (15)	−0.0087 (15)
C4	0.0311 (18)	0.0199 (16)	0.0323 (19)	−0.0067 (14)	0.0005 (15)	−0.0063 (14)
C5	0.036 (2)	0.0211 (18)	0.034 (2)	−0.0097 (15)	0.0040 (16)	−0.0100 (15)
C6	0.040 (2)	0.0200 (18)	0.031 (2)	−0.0132 (16)	0.0071 (17)	−0.0073 (15)
C7	0.032 (2)	0.0226 (18)	0.0274 (19)	−0.0123 (16)	0.0094 (16)	−0.0088 (15)
C8	0.0322 (19)	0.0219 (17)	0.035 (2)	−0.0074 (14)	0.0031 (15)	−0.0083 (15)
C9	0.045 (3)	0.026 (2)	0.037 (2)	−0.0145 (18)	0.0072 (19)	−0.0093 (17)
C10	0.046 (3)	0.029 (2)	0.029 (2)	−0.016 (2)	−0.002 (2)	−0.0041 (17)
C11	0.044 (3)	0.033 (2)	0.029 (2)	−0.014 (2)	0.000 (2)	−0.0111 (18)
C12	0.041 (2)	0.026 (2)	0.033 (2)	−0.0035 (18)	0.0009 (18)	−0.0075 (17)
O1	0.0432 (18)	0.0259 (13)	0.0460 (19)	−0.0071 (12)	0.0125 (15)	−0.0128 (13)
O2	0.0455 (18)	0.0288 (14)	0.0414 (17)	−0.0074 (13)	0.0185 (14)	−0.0174 (13)
O3	0.043 (2)	0.0272 (13)	0.0386 (16)	−0.0104 (13)	0.0180 (14)	−0.0063 (12)
O4	0.0401 (15)	0.0252 (12)	0.0398 (16)	−0.0047 (11)	0.0029 (12)	−0.0067 (11)
O5	0.0521 (17)	0.0277 (13)	0.0392 (16)	−0.0090 (12)	0.0086 (13)	−0.0125 (11)
O6	0.056 (2)	0.0291 (14)	0.0398 (17)	−0.0216 (14)	0.0240 (15)	−0.0163 (13)
O7	0.0430 (19)	0.0300 (13)	0.0347 (15)	−0.0172 (13)	0.0127 (14)	−0.0093 (11)
O8	0.0546 (18)	0.0209 (14)	0.0494 (18)	−0.0102 (13)	0.0153 (14)	−0.0166 (13)
O9	0.061 (2)	0.0359 (16)	0.0414 (18)	−0.0196 (16)	0.0112 (16)	−0.0089 (13)
O10	0.060 (3)	0.0316 (17)	0.0350 (17)	−0.0248 (19)	0.0010 (18)	−0.0102 (14)
O11	0.050 (3)	0.0272 (16)	0.0325 (17)	−0.0100 (17)	−0.0054 (17)	−0.0072 (13)
O12	0.053 (3)	0.0256 (16)	0.0400 (19)	−0.0017 (18)	−0.0091 (19)	−0.0111 (14)
O13	0.0509 (19)	0.0276 (14)	0.0348 (15)	−0.0241 (14)	0.0145 (14)	−0.0112 (12)
O14	0.0432 (16)	0.0270 (14)	0.0305 (15)	0.0007 (12)	0.0065 (12)	−0.0041 (12)
O15	0.0406 (17)	0.0248 (13)	0.0284 (14)	−0.0109 (12)	0.0025 (12)	−0.0081 (11)
O16	0.0422 (17)	0.0264 (14)	0.0338 (15)	−0.0206 (13)	−0.0025 (13)	−0.0035 (12)
O17	0.0484 (17)	0.0253 (14)	0.0503 (18)	−0.0094 (13)	0.0181 (14)	−0.0101 (13)
O18	0.0440 (16)	0.0256 (14)	0.0490 (18)	−0.0040 (12)	−0.0076 (14)	−0.0155 (13)
O19	0.0435 (16)	0.0210 (13)	0.0475 (17)	−0.0125 (12)	0.0178 (13)	−0.0148 (12)
O20	0.0486 (17)	0.0309 (15)	0.0362 (16)	−0.0084 (13)	0.0029 (13)	−0.0107 (12)

Geometric parameters (Å, º)

Eu—O19	2.418 (3)	C9—C10	1.489 (6)
Eu—O13	2.433 (3)	C10—C11	1.325 (6)
Eu—O16	2.437 (3)	C10—H10B	0.930
Eu—O18	2.446 (3)	C11—C12	1.479 (6)
Eu—O17	2.448 (3)	C11—H11B	0.930
Eu—O14	2.458 (3)	C12—O12	1.238 (5)
Eu—O15	2.479 (3)	C12—O11	1.266 (5)
Eu—O4	2.480 (3)	O2—H1	1.20
Eu—O5	2.574 (3)	O3—H1	1.21
C1—O1	1.232 (5)	O6—H2	1.20
C1—O2	1.282 (5)	O7—H2	1.20
C1—C2	1.481 (5)	O10—H3	1.21
C2—C3	1.331 (5)	O11—H3	1.22
C2—H2A	0.930	O13—H13A	0.960
C3—C4	1.492 (5)	O13—H13B	0.960
C3—H3A	0.930	O14—H14C	0.960
C4—O4	1.225 (4)	O14—H14B	0.960
C4—O3	1.288 (5)	O15—H15A	0.960
C5—O5	1.238 (5)	O15—H15B	0.960
C5—O6	1.289 (5)	O16—H16A	0.960
C5—C6	1.486 (5)	O16—H16B	0.960
C6—C7	1.331 (5)	O17—H17A	0.960
C6—H6B	0.930	O17—H17B	0.960
C7—C8	1.501 (5)	O18—H18A	0.960
C7—H7B	0.930	O18—H18B	0.960
C8—O8	1.226 (5)	O19—H19A	0.960
C8—O7	1.282 (5)	O19—H19B	0.960
C9—O9	1.233 (5)	O20—H20A	0.960
C9—O10	1.288 (5)	O20—H20B	0.960
O19—Eu—O13	136.32 (10)	C7—C6—C5	130.6 (4)
O19—Eu—O16	75.23 (10)	C7—C6—H6B	114.7
O13—Eu—O16	138.11 (10)	C5—C6—H6B	114.7
O19—Eu—O18	93.10 (11)	C6—C7—C8	130.1 (4)
O13—Eu—O18	77.56 (11)	C6—C7—H7B	114.9
O16—Eu—O18	136.82 (10)	C8—C7—H7B	114.9
O19—Eu—O17	141.53 (10)	O8—C8—O7	122.7 (3)
O13—Eu—O17	77.68 (10)	O8—C8—C7	117.4 (4)
O16—Eu—O17	88.41 (11)	O7—C8—C7	119.8 (3)
O18—Eu—O17	75.26 (11)	O9—C9—O10	121.1 (4)
O19—Eu—O14	75.76 (10)	O9—C9—C10	118.7 (4)
O13—Eu—O14	82.06 (11)	O10—C9—C10	120.2 (4)
O16—Eu—O14	81.85 (10)	C11—C10—C9	130.7 (4)
O18—Eu—O14	136.17 (10)	C11—C10—H10B	114.6
O17—Eu—O14	136.85 (10)	C9—C10—H10B	114.6
O19—Eu—O15	132.21 (10)	C10—C11—C12	130.6 (4)
O13—Eu—O15	69.47 (10)	C10—C11—H11B	114.7
O16—Eu—O15	68.67 (10)	C12—C11—H11B	114.7
O18—Eu—O15	134.69 (11)	O12—C12—O11	121.9 (4)
O17—Eu—O15	68.12 (11)	O12—C12—C11	117.5 (4)
O14—Eu—O15	69.17 (10)	O11—C12—C11	120.6 (4)
O19—Eu—O4	69.61 (10)	C1—O2—H1	109.5
O13—Eu—O4	138.27 (10)	C4—O3—H1	109.2
O16—Eu—O4	69.49 (10)	C4—O4—Eu	142.7 (3)
O18—Eu—O4	67.49 (10)	C5—O5—Eu	139.0 (3)
O17—Eu—O4	72.09 (10)	C5—O6—H2	109.2
O14—Eu—O4	139.37 (10)	C8—O7—H2	109.9
O15—Eu—O4	121.76 (10)	C9—O10—H3	108.4
O19—Eu—O5	66.15 (9)	C12—O11—H3	109.3
O13—Eu—O5	71.26 (10)	Eu—O13—H13A	109.4
O16—Eu—O5	137.02 (10)	Eu—O13—H13B	109.3
O18—Eu—O5	65.53 (10)	H13A—O13—H13B	109.5
O17—Eu—O5	133.92 (11)	Eu—O14—H14C	109.4
O14—Eu—O5	71.29 (10)	Eu—O14—H14B	109.4
O15—Eu—O5	126.90 (9)	H14C—O14—H14B	109.5
O4—Eu—O5	111.33 (9)	Eu—O15—H15A	109.4
O1—C1—O2	122.1 (4)	Eu—O15—H15B	109.3
O1—C1—C2	117.8 (4)	H15A—O15—H15B	109.5
O2—C1—C2	120.1 (3)	Eu—O16—H16A	109.4
C3—C2—C1	130.8 (4)	Eu—O16—H16B	109.4
C3—C2—H2A	114.6	H16A—O16—H16B	109.5
C1—C2—H2A	114.6	Eu—O17—H17A	109.4
C2—C3—C4	130.2 (4)	Eu—O17—H17B	109.3
C2—C3—H3A	114.9	H17A—O17—H17B	109.5
C4—C3—H3A	114.9	Eu—O18—H18A	109.4
O4—C4—O3	122.7 (3)	Eu—O18—H18B	109.4
O4—C4—C3	117.3 (3)	H18A—O18—H18B	109.5
O3—C4—C3	120.0 (3)	Eu—O19—H19A	109.3
O5—C5—O6	121.9 (4)	Eu—O19—H19B	109.4
O5—C5—C6	117.8 (3)	H19A—O19—H19B	109.5
O6—C5—C6	120.3 (3)	H20A—O20—H20B	109.5
O1—C1—C2—C3	178.0 (4)	O13—Eu—O4—C4	−79.0 (4)
O2—C1—C2—C3	−0.7 (7)	O16—Eu—O4—C4	61.8 (4)
C1—C2—C3—C4	2.4 (8)	O18—Eu—O4—C4	−114.4 (4)
C2—C3—C4—O4	175.6 (4)	O17—Eu—O4—C4	−33.3 (4)
C2—C3—C4—O3	−5.1 (7)	O14—Eu—O4—C4	109.9 (4)
O5—C5—C6—C7	−176.5 (4)	O15—Eu—O4—C4	15.3 (5)
O6—C5—C6—C7	4.0 (7)	O5—Eu—O4—C4	−164.4 (4)
C5—C6—C7—C8	−0.9 (8)	O6—C5—O5—Eu	−16.6 (7)
C6—C7—C8—O8	−179.4 (4)	C6—C5—O5—Eu	163.9 (3)
C6—C7—C8—O7	−0.9 (7)	O19—Eu—O5—C5	−134.6 (4)
O9—C9—C10—C11	−176.2 (5)	O13—Eu—O5—C5	35.4 (4)
O10—C9—C10—C11	4.2 (9)	O16—Eu—O5—C5	−106.7 (4)
C9—C10—C11—C12	−1.4 (10)	O18—Eu—O5—C5	120.0 (4)
C10—C11—C12—O12	−179.2 (5)	O17—Eu—O5—C5	85.7 (4)
C10—C11—C12—O11	0.6 (9)	O14—Eu—O5—C5	−52.3 (4)
O3—C4—O4—Eu	13.9 (7)	O15—Eu—O5—C5	−8.7 (5)
C3—C4—O4—Eu	−166.9 (3)	O4—Eu—O5—C5	171.0 (4)
O19—Eu—O4—C4	143.1 (4)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H1···O3	1.20	1.21	2.410 (4)	180
O6—H2···O7	1.20	1.20	2.405 (4)	180
O10—H3···O11	1.21	1.22	2.434 (5)	180