Poly[[diaqua-μ₆-succinato-di-μ₅-succinato-dierbium(III)] monohydrate]

The title compound, {[Er₂(C₄H₄O₄)₃(H₂O)₂]·H₂O}_n, is iso­structural with other Ln–succinates of the same formula. The Er^III atom is nine-coordinated by O atoms.

Key indicators

• Single-crystal X-ray study
• T = 273 K
• Mean [sigma](C-C) = 0.007 Å
• H-atom completeness 89%
• R factor = 0.024
• wR factor = 0.066
• Data-to-parameter ratio = 12.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W

Author Response: The attached H atoms could not be located.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) .         20 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2
PLAT731_ALERT_1_C Bond    Calc     0.85(5), Rep     0.84(2) ......       2.50 su-Ra
              O1W  -H1WB    1.555   1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.20 Ratio

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:C12 H18 Er2 O15
            Atom count from the _atom_site data:  C12 H16 Er2 O15
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  C12 H18 Er2 O15
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         48.00     48.00    0.00
           H         72.00     64.00    8.00
           Er         8.00      8.00    0.00
           O         60.00     60.00    0.00

   1 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   7 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
   2 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Bruker, 2004).

Poly[[diaqua-µ₆-succinato-di-µ₅-succinato-dierbium(III)] monohydrate]

Crystal data

[Er2(C4H4O4)3(H2O)2]·H2O	F(000) = 1384
Mr = 736.78	Dx = 2.725 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1696 reflections
a = 19.8837 (2) Å	θ = 2.9–25.7°
b = 7.6642 (2) Å	µ = 9.36 mm^−1
c = 13.8194 (2) Å	T = 273 K
β = 121.50 (1)°	Prism, pale red
V = 1795.7 (2) Å^3	0.55 × 0.24 × 0.14 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer	1696 independent reflections
Radiation source: fine-focus sealed tube	1632 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
Detector resolution: none pixels mm^-1	θmax = 25.7°, θmin = 2.9°
ω scans	h = −21→24
Absorption correction: multi-scan (SADABS; Bruker, 2004)	k = −9→9
Tmin = 0.076, Tmax = 0.272	l = −16→11
4673 measured 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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.066	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0422P)^2 + 9.2468P] where P = (Fo^2 + 2Fc^2)/3
1696 reflections	(Δ/σ)max = 0.001
141 parameters	Δρmax = 1.04 e Å^−3
3 restraints	Δρmin = −1.89 e Å^−3

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
Er1	0.268891 (11)	0.71774 (2)	0.229942 (15)	0.01082 (11)
O1	0.18749 (18)	0.9827 (4)	0.1379 (3)	0.0183 (7)
C1	0.1533 (2)	0.9153 (6)	0.0383 (3)	0.0144 (8)
O2	0.1717 (2)	0.7632 (4)	0.0287 (3)	0.0202 (7)
C2	0.0905 (2)	1.0169 (6)	−0.0621 (4)	0.0165 (9)
H2A	0.0513	1.0566	−0.0454	0.020*
H2B	0.0644	0.9398	−0.1272	0.020*
O3	0.1797 (2)	0.9720 (4)	−0.1594 (3)	0.0213 (7)
C3	0.1229 (3)	1.1756 (6)	−0.0930 (4)	0.0187 (9)
H3A	0.0790	1.2493	−0.1449	0.022*
H3B	0.1561	1.2428	−0.0246	0.022*
O4	0.1968 (2)	1.2561 (5)	−0.1773 (3)	0.0225 (8)
C4	0.1703 (2)	1.1298 (6)	−0.1470 (4)	0.0145 (8)
O5	0.32251 (17)	0.9824 (4)	0.3389 (2)	0.0160 (6)
C5	0.3944 (2)	0.9237 (6)	0.3931 (4)	0.0156 (9)
O6	0.4057 (2)	0.7700 (4)	0.3781 (3)	0.0219 (7)
C6	0.4601 (3)	1.0441 (6)	0.4692 (4)	0.0255 (10)
H6A	0.4495	1.0930	0.5246	0.031*
H6B	0.4615	1.1398	0.4243	0.031*
O1W	0.3330 (2)	0.8875 (4)	0.1527 (3)	0.0209 (7)
O2W	0.5000	0.9747 (17)	0.2500	0.116 (4)
H1WA	0.322 (3)	0.993 (3)	0.140 (5)	0.024 (15)*
H1WB	0.329 (4)	0.855 (9)	0.091 (3)	0.035 (17)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Er1	0.01238 (16)	0.00863 (17)	0.01225 (15)	−0.00043 (6)	0.00699 (12)	−0.00013 (6)
O1	0.0176 (15)	0.0178 (16)	0.0144 (14)	0.0001 (12)	0.0047 (13)	−0.0048 (12)
C1	0.013 (2)	0.020 (2)	0.0132 (19)	−0.0040 (17)	0.0089 (17)	0.0005 (17)
O2	0.0285 (19)	0.0131 (14)	0.0171 (17)	0.0005 (13)	0.0105 (15)	0.0014 (13)
C2	0.014 (2)	0.024 (2)	0.0131 (19)	0.0006 (17)	0.0085 (17)	0.0016 (17)
O3	0.0310 (18)	0.0123 (15)	0.0314 (18)	0.0017 (13)	0.0238 (16)	−0.0003 (13)
C3	0.026 (2)	0.0155 (19)	0.022 (2)	0.0045 (19)	0.018 (2)	0.0033 (19)
O4	0.031 (2)	0.0154 (14)	0.034 (2)	−0.0011 (15)	0.0264 (19)	−0.0001 (15)
C4	0.015 (2)	0.015 (2)	0.015 (2)	0.0012 (16)	0.0082 (17)	0.0007 (16)
O5	0.0123 (14)	0.0177 (15)	0.0151 (14)	0.0015 (12)	0.0052 (12)	−0.0042 (12)
C5	0.014 (2)	0.019 (2)	0.0129 (19)	0.0023 (17)	0.0057 (17)	0.0045 (17)
O6	0.0178 (17)	0.0132 (16)	0.0271 (19)	−0.0001 (12)	0.0065 (15)	0.0012 (13)
C6	0.014 (2)	0.018 (2)	0.032 (3)	−0.0005 (19)	0.004 (2)	−0.005 (2)
O1W	0.0307 (19)	0.0169 (16)	0.0231 (17)	−0.0026 (14)	0.0197 (15)	−0.0025 (14)
O2W	0.108 (8)	0.097 (8)	0.149 (10)	0.000	0.071 (8)	0.000

Geometric parameters (Å, º)

Er1—O3^i	2.270 (3)	C1—C2	1.510 (6)
Er1—O5^ii	2.378 (3)	C2—C3	1.537 (6)
Er1—O4^iii	2.378 (4)	C2—H2A	0.9700
Er1—O1^ii	2.383 (3)	C2—H2B	0.9700
Er1—O5	2.417 (3)	O3—Er1^i	2.270 (3)
Er1—O1W	2.425 (3)	C3—C4	1.518 (6)
Er1—O6	2.436 (4)	C3—H3A	0.9700
Er1—O2	2.444 (3)	C3—H3B	0.9700
Er1—O1	2.492 (3)	O4—Er1^v	2.378 (4)
C1—O1	1.282 (5)	O5—Er1^iv	2.378 (3)
C1—O2	1.250 (6)	C5—C6	1.493 (6)
C4—O3	1.249 (5)	C6—C6^vi	1.514 (9)
C4—O4	1.274 (6)	C6—H6A	0.9700
C5—O5	1.299 (5)	C6—H6B	0.9700
C5—O6	1.237 (6)	O1W—H1WA	0.83 (2)
O1—Er1^iv	2.383 (3)	O1W—H1WB	0.84 (2)
O3^i—Er1—O5^ii	76.35 (11)	Er1^iv—O1—Er1	110.20 (11)
O3^i—Er1—O4^iii	144.99 (12)	O2—C1—O1	118.0 (4)
O5^ii—Er1—O4^iii	74.32 (12)	O2—C1—C2	122.1 (4)
O3^i—Er1—O1^ii	77.29 (11)	O1—C1—C2	119.9 (4)
O5^ii—Er1—O1^ii	68.24 (11)	C1—O2—Er1	96.5 (3)
O4^iii—Er1—O1^ii	74.39 (12)	C1—C2—C3	113.5 (4)
O3^i—Er1—O5	130.86 (11)	C1—C2—H2A	108.9
O5^ii—Er1—O5	151.89 (3)	C3—C2—H2A	108.9
O4^iii—Er1—O5	77.72 (12)	C1—C2—H2B	108.9
O1^ii—Er1—O5	106.95 (11)	C3—C2—H2B	108.9
O3^i—Er1—O1W	72.31 (12)	H2A—C2—H2B	107.7
O5^ii—Er1—O1W	134.32 (11)	C4—O3—Er1^i	144.3 (3)
O4^iii—Er1—O1W	142.70 (12)	C4—C3—C2	114.3 (4)
O1^ii—Er1—O1W	132.74 (11)	C4—C3—H3A	108.7
O5—Er1—O1W	70.22 (11)	C2—C3—H3A	108.7
O3^i—Er1—O6	84.87 (12)	C4—C3—H3B	108.7
O5^ii—Er1—O6	138.20 (10)	C2—C3—H3B	108.7
O4^iii—Er1—O6	104.83 (14)	H3A—C3—H3B	107.6
O1^ii—Er1—O6	71.37 (11)	C4—O4—Er1^v	135.3 (3)
O5—Er1—O6	53.34 (10)	O3—C4—O4	125.0 (4)
O1W—Er1—O6	70.65 (12)	O3—C4—C3	117.9 (4)
O3^i—Er1—O2	82.43 (12)	O4—C4—C3	117.1 (4)
O5^ii—Er1—O2	70.63 (11)	C5—O5—Er1^iv	150.9 (3)
O4^iii—Er1—O2	105.09 (13)	C5—O5—Er1	93.6 (3)
O1^ii—Er1—O2	137.29 (11)	Er1^iv—O5—Er1	113.04 (11)
O5—Er1—O2	114.73 (10)	O6—C5—O5	118.4 (4)
O1W—Er1—O2	73.00 (12)	O6—C5—C6	122.5 (4)
O6—Er1—O2	143.60 (12)	O5—C5—C6	119.1 (4)
O3^i—Er1—O1	128.37 (11)	C5—O6—Er1	94.4 (3)
O5^ii—Er1—O1	104.90 (10)	C5—C6—C6^vi	113.2 (5)
O4^iii—Er1—O1	78.06 (12)	C5—C6—H6A	108.9
O1^ii—Er1—O1	152.44 (3)	C6^vi—C6—H6A	108.9
O5—Er1—O1	65.89 (10)	C5—C6—H6B	108.9
O1W—Er1—O1	71.85 (11)	C6^vi—C6—H6B	108.9
O6—Er1—O1	115.93 (10)	H6A—C6—H6B	107.7
O2—Er1—O1	52.15 (10)	Er1—O1W—H1WA	118 (4)
C1—O1—Er1^iv	154.6 (3)	Er1—O1W—H1WB	119 (5)
C1—O1—Er1	93.4 (3)	H1WA—O1W—H1WB	101 (6)

Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, −y+2, z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x, −y+2, z−1/2; (vi) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O4^vii	0.83 (3)	2.08 (3)	2.853 (5)	156 (6)
O1W—H1WB···O2^i	0.85 (5)	1.88 (6)	2.717 (5)	168 (6)

Symmetry codes: (i) −x+1/2, −y+3/2, −z; (vii) −x+1/2, −y+5/2, −z.