catena-Poly[[[diaqua­calcium(II)]-di-μ-3-carboxy­phenoxy­acetato] dihydrate]

The Ca atom in the title compound, {[Ca(HO₂CC₆H₄OCH₂CO₂)₂(H₂O)₂]·2H₂O}_n, is eight-coordinate. The HO₂CC₆H₄OCH₂CO₂⁻ monoanion binds in a chelating mode; it also functions as a bridge, linking adjacent Ca atoms into a zigzag chain. Hydrogen bonds link the chains into a three-dimensional network. The Ca atom lies on a special position of site symmetry 2.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.003 Å
• H-atom completeness 82%
• Disorder in solvent or counterion
• R factor = 0.045
• wR factor = 0.131
• Data-to-parameter ratio = 16.9

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.691     0.941
            Tmin(prime) and Tmax expected:      0.883     0.941
            RR(prime) =      0.783
            Please check that your absorption correction is appropriate.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.78
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.76 Ratio
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Ca1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C9
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.41
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....       >O2W
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) .....      <O2W'
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          3

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C18 H22 Ca1 O14
            Atom count from _chemical_formula_moiety:
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:C18 H22 Ca1 O14
            Atom count from the _atom_site data:  C18 H18 Ca1 O14
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  C18 H22 Ca O14
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         72.00     72.00    0.00
           H         88.00     72.00   16.00
           Ca         4.00      4.00    0.00
           O         56.00     56.00    0.00

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  13 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-Poly[[[diaquacalcium(II)]-di-µ-3-carboxyphenoxyacetato] dihydrate]

Crystal data

[Ca(C9H7O5)2(H2O)2]·2H2O	F(000) = 1048
Mr = 502.44	Dx = 1.441 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 10195 reflections
a = 26.902 (5) Å	θ = 3.1–27.4°
b = 14.492 (3) Å	µ = 0.34 mm^−1
c = 6.057 (1) Å	T = 295 K
β = 101.28 (3)°	Prism, colorless
V = 2315.6 (8) Å^3	0.36 × 0.25 × 0.18 mm
Z = 4

Data collection

Rigaku RAXIS-RAPID IP diffractometer	2622 independent reflections
Radiation source: fine-focus sealed tube	2340 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
ω scans	θmax = 27.4°, θmin = 3.1°
Absorption correction: multi-scan ABSCOR (Higashi, 1995)	h = −34→33
Tmin = 0.691, Tmax = 0.941	k = −18→18
10847 measured reflections	l = −7→7

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)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.131	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0777P)^2 + 2.6608P] where P = (Fo^2 + 2Fc^2)/3
2622 reflections	(Δ/σ)max = 0.001
155 parameters	Δρmax = 0.42 e Å^−3
6 restraints	Δρmin = −0.37 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ca1	0.5000	0.41616 (4)	0.7500	0.0237 (2)
O1	0.4505 (1)	0.4661 (1)	0.3784 (2)	0.0307 (3)
O2	0.4125 (1)	0.3631 (1)	0.5554 (2)	0.0338 (3)
O3	0.3271 (1)	0.3732 (1)	0.2628 (3)	0.0421 (4)
O4	0.1072 (1)	0.2925 (2)	0.0612 (4)	0.0842 (9)
O5	0.1644 (1)	0.2417 (1)	0.3481 (3)	0.0494 (5)
O1w	0.5181 (1)	0.2993 (1)	0.4979 (3)	0.0565 (5)
O2w	0.4521 (3)	0.1376 (6)	0.472 (2)	0.219 (5)	0.67 (1)
O2w'	0.4512 (6)	−0.023 (1)	0.608 (4)	0.219 (5)	0.33
C1	0.4131 (1)	0.4157 (1)	0.3928 (3)	0.0256 (4)
C2	0.3678 (1)	0.4212 (1)	0.1997 (3)	0.0301 (4)
C3	0.2804 (1)	0.3764 (1)	0.1233 (3)	0.0291 (4)
C4	0.2706 (1)	0.4167 (1)	−0.0881 (3)	0.0328 (4)
C5	0.2215 (1)	0.4165 (2)	−0.2138 (4)	0.0375 (5)
C6	0.1827 (1)	0.3758 (2)	−0.1316 (4)	0.0373 (5)
C7	0.1929 (1)	0.3344 (1)	0.0798 (3)	0.0307 (4)
C8	0.2416 (1)	0.3346 (1)	0.2080 (3)	0.0295 (4)
C9	0.1506 (1)	0.2884 (2)	0.1627 (4)	0.0367 (5)
H5o	0.1384	0.2176	0.3855	0.074*
H1w1	0.5006	0.2514	0.5111	0.085*
H1w2	0.5494	0.2859	0.5297	0.085*
H2a	0.3585	0.4851	0.1673	0.036*
H2b	0.3760	0.3936	0.0655	0.036*
H4	0.2968	0.4438	−0.1455	0.039*
H5	0.2148	0.4441	−0.3551	0.045*
H6	0.1499	0.3759	−0.2165	0.045*
H8	0.2482	0.3070	0.3493	0.035*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0168 (2)	0.0285 (3)	0.0256 (3)	0.000	0.0040 (2)	0.000
O1	0.020 (1)	0.038 (1)	0.033 (1)	−0.008 (1)	0.003 (1)	0.003 (1)
O2	0.023 (1)	0.041 (1)	0.036 (1)	−0.006 (1)	0.003 (1)	0.009 (1)
O3	0.020 (1)	0.058 (1)	0.044 (1)	−0.013 (1)	−0.003 (1)	0.021 (1)
O4	0.027 (1)	0.121 (2)	0.097 (2)	−0.023 (1)	−0.008 (1)	0.060 (2)
O5	0.029 (1)	0.070 (1)	0.048 (1)	−0.014 (1)	0.006 (1)	0.020 (1)
O1w	0.044 (1)	0.071 (1)	0.050 (1)	0.026 (1)	−0.004 (1)	−0.019 (1)
O2w	0.170 (6)	0.168 (6)	0.307 (9)	−0.060 (5)	0.020 (6)	−0.001 (6)
O2w'	0.170 (6)	0.168 (6)	0.307 (9)	−0.060 (5)	0.020 (6)	−0.001 (6)
C1	0.018 (1)	0.029 (1)	0.030 (1)	0.000 (1)	0.005 (1)	−0.002 (1)
C2	0.020 (1)	0.038 (1)	0.032 (1)	−0.006 (1)	0.004 (1)	0.005 (1)
C3	0.021 (1)	0.034 (1)	0.032 (1)	−0.004 (1)	0.001 (1)	0.002 (1)
C4	0.025 (1)	0.039 (1)	0.034 (1)	−0.005 (1)	0.006 (1)	0.007 (1)
C5	0.032 (1)	0.048 (1)	0.030 (1)	−0.004 (1)	0.000 (1)	0.008 (1)
C6	0.025 (1)	0.046 (1)	0.037 (1)	−0.007 (1)	−0.004 (1)	0.005 (1)
C7	0.023 (1)	0.033 (1)	0.035 (1)	−0.007 (1)	0.003 (1)	0.000 (1)
C8	0.024 (1)	0.034 (1)	0.030 (1)	−0.004 (1)	0.003 (1)	0.004 (1)
C9	0.023 (1)	0.042 (1)	0.045 (1)	−0.007 (1)	0.005 (1)	0.005 (1)

Geometric parameters (Å, º)

Ca1—O1	2.488 (2)	C3—C4	1.385 (3)
Ca1—O1^i	2.488 (2)	C4—C5	1.390 (3)
Ca1—O1^ii	2.386 (1)	C5—C6	1.376 (3)
Ca1—O1^iii	2.386 (1)	C6—C7	1.392 (3)
Ca1—O2	2.537 (2)	C7—C8	1.387 (3)
Ca1—O2^i	2.537 (2)	C7—C9	1.488 (3)
Ca1—O1w	2.393 (2)	O5—H5o	0.8500
Ca1—O1w^i	2.393 (2)	O1w—H1w1	0.85
O1—C1	1.261 (2)	O1w—H1w2	0.85
O2—C1	1.248 (2)	C2—H2a	0.97
O3—C3	1.370 (2)	C2—H2b	0.97
O3—C2	1.411 (2)	C4—H4	0.93
O4—C9	1.209 (3)	C5—H5	0.93
O5—C9	1.302 (3)	C6—H6	0.93
C1—C2	1.518 (3)	C8—H8	0.93
C3—C8	1.389 (3)
O1—Ca1—O1^i	146.2 (1)	O2—C1—C2	120.5 (2)
O1—Ca1—O1^ii	74.4 (1)	O1—C1—C2	116.7 (2)
O1—Ca1—O1^iii	81.6 (1)	O3—C2—C1	108.4 (2)
O1—Ca1—O2	52.0 (1)	O3—C3—C8	115.0 (2)
O1—Ca1—O2^i	142.4 (1)	O3—C3—C4	124.7 (2)
O1—Ca1—O1w	76.6 (1)	C8—C3—C4	120.3 (2)
O1—Ca1—O1w^i	130.1 (1)	C3—C4—C5	119.6 (2)
O1^i—Ca1—O1^ii	81.6 (1)	C6—C5—C4	120.7 (2)
O1^i—Ca1—O1^iii	74.4 (1)	C5—C6—C7	119.4 (2)
O1^i—Ca1—O2	142.4 (1)	C8—C7—C6	120.6 (2)
O1^i—Ca1—O2^i	52.0 (1)	C8—C7—C9	120.9 (2)
O1^i—Ca1—O1w	130.1 (1)	C6—C7—C9	118.5 (2)
O1^i—Ca1—O1w^i	76.6 (1)	C7—C8—C3	119.4 (2)
O1^ii—Ca1—O1^iii	88.7 (1)	O4—C9—O5	123.2 (2)
O1^ii—Ca1—O2	126.3 (1)	O4—C9—C7	122.1 (2)
O1^ii—Ca1—O2^i	80.9 (1)	O5—C9—C7	114.6 (2)
O1^ii—Ca1—O1w	95.9 (1)	C9—O5—H5o	109.5
O1^ii—Ca1—O1w^i	155.5 (1)	Ca1—O1w—H1w1	109.5
O1^iii—Ca1—O2	80.9 (1)	Ca1—O1w—H1w2	109.5
O1^iii—Ca1—O2^i	126.3 (1)	H1w1—O1w—H1w2	109.5
O1^iii—Ca1—O1w	155.5 (1)	O3—C2—H2a	110.0
O1^iii—Ca1—O1w^i	95.9 (1)	C1—C2—H2a	110.0
O2—Ca1—O2^i	144.7 (1)	O3—C2—H2b	110.0
O2—Ca1—O1w	77.0 (1)	C1—C2—H2b	110.0
O2—Ca1—O1w^i	78.2 (1)	H2a—C2—H2b	108.4
O2^i—Ca1—O1w	78.2 (1)	C3—C4—H4	120.2
O2^i—Ca1—O1w^i	77.0 (1)	C5—C4—H4	120.2
O1w—Ca1—O1w^i	89.9 (1)	C6—C5—H5	119.6
C1—O1—Ca1^ii	160.2 (1)	C4—C5—H5	119.6
C1—O1—Ca1	93.5 (1)	C5—C6—H6	120.3
Ca1^ii—O1—Ca1	105.6 (1)	C7—C6—H6	120.3
C1—O2—Ca1	91.6 (1)	C7—C8—H8	120.3
C3—O3—C2	118.9 (2)	C3—C8—H8	120.3
O2—C1—O1	122.8 (2)
O1^iii—Ca1—O1—C1	−84.0 (1)	Ca1—O1—C1—O2	−1.9 (2)
O1^ii—Ca1—O1—C1	−175.0 (1)	Ca1^ii—O1—C1—C2	12.5 (5)
O1w—Ca1—O1—C1	84.8 (1)	Ca1—O1—C1—C2	178.3 (1)
O1w^i—Ca1—O1—C1	6.6 (2)	C3—O3—C2—C1	173.7 (2)
O1^i—Ca1—O1—C1	−128.8 (1)	O2—C1—C2—O3	10.3 (3)
O2—Ca1—O1—C1	1.0 (1)	O1—C1—C2—O3	−169.9 (2)
O2^i—Ca1—O1—C1	134.1 (1)	C2—O3—C3—C8	−174.3 (2)
O1^iii—Ca1—O1—Ca1^ii	91.0 (1)	C2—O3—C3—C4	6.1 (3)
O1w—Ca1—O1—Ca1^ii	−100.1 (1)	O3—C3—C4—C5	−179.4 (2)
O1w^i—Ca1—O1—Ca1^ii	−178.4 (1)	C8—C3—C4—C5	1.1 (3)
O1^i—Ca1—O1—Ca1^ii	46.3 (1)	C3—C4—C5—C6	−0.7 (3)
O2—Ca1—O1—Ca1^ii	176.0 (1)	C4—C5—C6—C7	−0.1 (4)
O2^i—Ca1—O1—Ca1^ii	−50.9 (1)	C5—C6—C7—C8	0.5 (3)
O1^iii—Ca1—O2—C1	85.3 (1)	C5—C6—C7—C9	−178.3 (2)
O1^ii—Ca1—O2—C1	3.7 (1)	C6—C7—C8—C3	−0.1 (3)
O1w—Ca1—O2—C1	−84.0 (1)	C9—C7—C8—C3	178.6 (2)
O1w^i—Ca1—O2—C1	−176.7 (1)	O3—C3—C8—C7	179.77 (19)
O1^i—Ca1—O2—C1	134.5 (1)	C4—C3—C8—C7	−0.6 (3)
O1—Ca1—O2—C1	−1.0 (1)	C8—C7—C9—O4	175.0 (3)
O2^i—Ca1—O2—C1	−130.5 (1)	C6—C7—C9—O4	−6.3 (4)
Ca1—O2—C1—O1	1.9 (2)	C8—C7—C9—O5	−7.0 (3)
Ca1—O2—C1—C2	−178.3 (2)	C6—C7—C9—O5	171.8 (2)
Ca1^ii—O1—C1—O2	−167.7 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5o···O2^iv	0.85	1.89	2.720 (2)	166
O1w—H1w1···O2w	0.85	2.09	2.925 (8)	168
O1w—H1w2···O4^v	0.85	1.91	2.704 (2)	156

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