Disodium diaqua­bis(malonato-κ²O,O′)cobalt(II) monohydrate

In the title compound, Na₂[Co(C₃H₂O₄)₂(H₂O)₂]·H₂O, the Co atom and two crystallographically independent Na⁺ ions lie on twofold rotation axes. The Co atom is coordinated by four O atoms from two malonate ligands and two water mol­ecules in a distorted octa­hedral geometry [Co—O = 1.595 (3)–2.219 (4) Å]. The two independent Na⁺ ions are coordinated by six and eight O atoms, respectively [Na—O = 2.268 (4)–2.844 (3) Å]. A two-dimensional hydrogen-bonding network formed by O—H...O hydrogen bonds stabilizes the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.041
• wR factor = 0.114
• Data-to-parameter ratio = 14.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT416_ALERT_2_B Short Intra D-H..H-D       H4     ..  H4      ..       1.38 Ang.

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.94
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.54 Ratio

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.937
            Tmax scaled      0.553 Tmin scaled      0.522
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.46
           From the CIF: _reflns_number_total               1348
           Count of symmetry unique reflns          805
           Completeness (_total/calc)            167.45%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       543
           Fraction of Friedel pairs measured     0.675
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   2 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
   2 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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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: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

Disodium diaquabis(malonato-κ²O,O')cobalt(II) monohydrate

Crystal data

Na2[Co(C3H2O4)2(H2O)2]·H2O	F(000) = 732
Mr = 363.05	Dx = 2.010 Mg m^−3
Orthorhombic, C2221	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c 2	Cell parameters from 5850 reflections
a = 7.2503 (15) Å	θ = 6.2–54.9°
b = 15.952 (3) Å	µ = 1.56 mm^−1
c = 10.371 (2) Å	T = 295 K
V = 1199.5 (4) Å^3	Block, brown
Z = 4	0.43 × 0.41 × 0.38 mm

Data collection

Rigaku R-AXIS RAPID diffractometer	1348 independent reflections
Radiation source: fine-focus sealed tube	1312 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.019
ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −9→9
Tmin = 0.557, Tmax = 0.590	k = −20→20
5787 measured reflections	l = −13→13

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)] = 0.041	H-atom parameters constrained
wR(F^2) = 0.114	w = 1/[σ^2(Fo^2) + (0.0723P)^2 + 1.3726P] where P = (Fo^2 + 2Fc^2)/3
S = 1.25	(Δ/σ)max < 0.001
1348 reflections	Δρmax = 0.85 e Å^−3
95 parameters	Δρmin = −0.57 e Å^−3
2 restraints	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.17 (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
C1	0.2764 (5)	0.1317 (2)	0.4846 (3)	0.0176 (6)
C2	0.6213 (4)	0.1307 (2)	0.5200 (3)	0.0157 (6)
C3	0.4402 (4)	0.1748 (2)	0.5501 (3)	0.0193 (6)
H1	0.4473	0.2325	0.5212	0.023*
H2	0.4209	0.1751	0.6427	0.023*
Co1	0.5000	0.14081 (4)	0.2500	0.0239 (2)
Na1	0.5000	0.38298 (10)	0.2500	0.0189 (3)
Na2	0.4224 (3)	0.5000	0.5000	0.0263 (5)
O1	0.2817 (3)	0.12271 (19)	0.3638 (2)	0.0270 (6)
O2	0.1450 (4)	0.10792 (19)	0.5510 (2)	0.0281 (6)
O3	0.6639 (3)	0.11832 (16)	0.4031 (2)	0.0204 (5)
O4	0.7200 (4)	0.10429 (18)	0.6095 (3)	0.0252 (5)
O5	0.5000	0.0017 (2)	0.2500	0.0394 (10)
H5	0.5707	−0.0290	0.2945	0.059*
O6	0.5000	0.2408 (2)	0.2500	0.0349 (8)
H4	0.5927	0.2730	0.2359	0.052*
O7	0.5000	0.52851 (19)	0.2500	0.0261 (7)
H3	0.5944	0.5580	0.2677	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0144 (13)	0.0232 (13)	0.0150 (13)	0.0025 (12)	0.0014 (10)	−0.0008 (12)
C2	0.0130 (13)	0.0199 (13)	0.0143 (14)	−0.0054 (11)	−0.0006 (10)	−0.0010 (12)
C3	0.0158 (13)	0.0278 (14)	0.0144 (13)	0.0005 (11)	−0.0010 (10)	−0.0062 (12)
Co1	0.0227 (3)	0.0294 (3)	0.0195 (3)	0.000	0.0024 (3)	0.000
Na1	0.0252 (8)	0.0196 (7)	0.0119 (7)	0.000	−0.0066 (8)	0.000
Na2	0.0144 (8)	0.0350 (10)	0.0294 (11)	0.000	0.000	−0.0206 (9)
O1	0.0144 (10)	0.0509 (17)	0.0156 (11)	−0.0108 (11)	0.0027 (9)	−0.0049 (11)
O2	0.0177 (11)	0.0491 (15)	0.0176 (11)	−0.0100 (11)	0.0115 (9)	−0.0046 (11)
O3	0.0135 (11)	0.0339 (13)	0.0137 (10)	0.0019 (9)	0.0006 (8)	−0.0026 (9)
O4	0.0159 (10)	0.0411 (14)	0.0185 (11)	0.0022 (10)	−0.0025 (9)	0.0074 (10)
O5	0.047 (2)	0.0210 (14)	0.050 (2)	0.000	−0.025 (3)	0.000
O6	0.044 (2)	0.0236 (16)	0.037 (2)	0.000	−0.001 (2)	0.000
O7	0.0168 (15)	0.0230 (14)	0.0384 (18)	0.000	−0.006 (2)	0.000

Geometric parameters (Å, º)

C1—O2	1.235 (4)	Na1—H4	1.8837
C1—O1	1.261 (4)	Na2—O2^viii	2.418 (3)
C1—C3	1.531 (5)	Na2—O2^iii	2.418 (3)
C2—O4	1.245 (4)	Na2—O4^v	2.493 (3)
C2—O3	1.267 (4)	Na2—O4^ix	2.493 (3)
C2—C3	1.522 (4)	Na2—O7^x	2.6917 (8)
C2—Na2^i	3.026 (4)	Na2—O7	2.6917 (8)
C3—H1	0.9700	Na2—O3^v	2.844 (3)
C3—H2	0.9700	Na2—O3^ix	2.844 (3)
Co1—O6	1.595 (3)	Na2—C2^v	3.026 (4)
Co1—O1^ii	1.995 (2)	Na2—C2^ix	3.026 (4)
Co1—O1	1.995 (2)	Na2—Na1^x	3.2439 (11)
Co1—O3^ii	2.016 (2)	O2—Na1^xi	2.321 (2)
Co1—O3	2.016 (2)	O2—Na2^xii	2.418 (3)
Co1—O5	2.219 (4)	O3—Na2^i	2.844 (3)
Na1—O6	2.268 (4)	O4—Na2^i	2.493 (3)
Na1—O2^iii	2.321 (2)	O4—Na1^xiii	2.507 (3)
Na1—O2^iv	2.321 (2)	O5—H5	0.8459
Na1—O7	2.321 (3)	O6—H4	0.8590
Na1—O4^v	2.507 (3)	O7—Na2^vii	2.6917 (8)
Na1—O4^vi	2.507 (3)	O7—H3	0.8502
Na1—Na2^vii	3.2439 (11)
O2—C1—O1	122.8 (3)	O4^ix—Na2—O7^x	78.27 (8)
O2—C1—C3	119.2 (3)	O2^viii—Na2—O7	87.19 (8)
O1—C1—C3	117.9 (3)	O2^iii—Na2—O7	76.72 (9)
O4—C2—O3	121.4 (3)	O4^v—Na2—O7	78.27 (8)
O4—C2—C3	119.9 (3)	O4^ix—Na2—O7	116.70 (9)
O3—C2—C3	118.6 (3)	O7^x—Na2—O7	155.88 (8)
O4—C2—Na2^i	53.41 (18)	O2^viii—Na2—O3^v	146.64 (8)
O3—C2—Na2^i	69.59 (18)	O2^iii—Na2—O3^v	92.55 (9)
C3—C2—Na2^i	162.7 (2)	O4^v—Na2—O3^v	47.92 (8)
C2—C3—C1	111.7 (3)	O4^ix—Na2—O3^v	83.90 (9)
C2—C3—H1	109.3	O7^x—Na2—O3^v	71.65 (7)
C1—C3—H1	109.3	O7—Na2—O3^v	126.17 (7)
C2—C3—H2	109.3	O2^viii—Na2—O3^ix	92.55 (9)
C1—C3—H2	109.3	O2^iii—Na2—O3^ix	146.64 (8)
H1—C3—H2	107.9	O4^v—Na2—O3^ix	83.90 (9)
O6—Co1—O1^ii	98.32 (9)	O4^ix—Na2—O3^ix	47.92 (8)
O6—Co1—O1	98.32 (9)	O7^x—Na2—O3^ix	126.17 (7)
O1^ii—Co1—O1	163.36 (18)	O7—Na2—O3^ix	71.65 (6)
O6—Co1—O3^ii	100.25 (7)	O3^v—Na2—O3^ix	97.53 (11)
O1^ii—Co1—O3^ii	88.62 (11)	O2^viii—Na2—C2^v	170.76 (9)
O1—Co1—O3^ii	88.43 (11)	O2^iii—Na2—C2^v	88.62 (9)
O6—Co1—O3	100.25 (7)	O4^v—Na2—C2^v	23.64 (9)
O1^ii—Co1—O3	88.43 (11)	O4^ix—Na2—C2^v	93.79 (10)
O1—Co1—O3	88.62 (11)	O7^x—Na2—C2^v	95.77 (8)
O3^ii—Co1—O3	159.50 (15)	O7—Na2—C2^v	101.59 (8)
O6—Co1—O5	180.0	O3^v—Na2—C2^v	24.68 (8)
O1^ii—Co1—O5	81.68 (9)	O3^ix—Na2—C2^v	87.56 (9)
O1—Co1—O5	81.68 (9)	O2^viii—Na2—C2^ix	88.62 (9)
O3^ii—Co1—O5	79.75 (7)	O2^iii—Na2—C2^ix	170.76 (9)
O3—Co1—O5	79.75 (7)	O4^v—Na2—C2^ix	93.79 (10)
O6—Na1—O2^iii	93.59 (8)	O4^ix—Na2—C2^ix	23.64 (9)
O6—Na1—O2^iv	93.59 (8)	O7^x—Na2—C2^ix	101.59 (8)
O2^iii—Na1—O2^iv	172.83 (17)	O7—Na2—C2^ix	95.77 (8)
O6—Na1—O7	180.0	O3^v—Na2—C2^ix	87.56 (9)
O2^iii—Na1—O7	86.41 (8)	O3^ix—Na2—C2^ix	24.68 (8)
O2^iv—Na1—O7	86.41 (8)	C2^v—Na2—C2^ix	87.64 (13)
O6—Na1—O4^v	94.65 (7)	O2^viii—Na2—Na1^x	45.56 (6)
O2^iii—Na1—O4^v	81.08 (9)	O2^iii—Na2—Na1^x	117.96 (8)
O2^iv—Na1—O4^v	98.33 (9)	O4^v—Na2—Na1^x	148.26 (8)
O7—Na1—O4^v	85.35 (7)	O4^ix—Na2—Na1^x	49.74 (6)
O6—Na1—O4^vi	94.65 (7)	O7^x—Na2—Na1^x	44.86 (7)
O2^iii—Na1—O4^vi	98.33 (9)	O7—Na2—Na1^x	129.53 (7)
O2^iv—Na1—O4^vi	81.08 (9)	O3^v—Na2—Na1^x	102.34 (6)
O7—Na1—O4^vi	85.35 (7)	O3^ix—Na2—Na1^x	90.84 (5)
O4^v—Na1—O4^vi	170.71 (15)	C2^v—Na2—Na1^x	125.20 (7)
O6—Na1—Na2^vii	125.13 (2)	C2^ix—Na2—Na1^x	70.96 (6)
O2^iii—Na1—Na2^vii	126.61 (9)	C1—O1—Co1	126.5 (2)
O2^iv—Na1—Na2^vii	48.06 (7)	C1—O2—Na1^xi	145.7 (2)
O7—Na1—Na2^vii	54.87 (2)	C1—O2—Na2^xii	127.7 (2)
O4^v—Na1—Na2^vii	123.93 (8)	Na1^xi—O2—Na2^xii	86.38 (9)
O4^vi—Na1—Na2^vii	49.35 (7)	C2—O3—Co1	125.6 (2)
O6—Na1—H4	21.4	C2—O3—Na2^i	85.74 (18)
O2^iii—Na1—H4	88.0	Co1—O3—Na2^i	141.74 (11)
O2^iv—Na1—H4	98.7	C2—O4—Na2^i	102.9 (2)
O7—Na1—H4	158.6	C2—O4—Na1^xiii	150.6 (2)
O4^v—Na1—H4	114.2	Na2^i—O4—Na1^xiii	80.90 (9)
O4^vi—Na1—H4	75.0	Co1—O5—H5	125.4
Na2^vii—Na1—H4	114.3	Co1—O6—Na1	180.0
O2^viii—Na2—O2^iii	96.29 (15)	Co1—O6—H4	126.8
O2^viii—Na2—O4^v	165.42 (9)	Na1—O6—H4	53.2
O2^iii—Na2—O4^v	79.52 (9)	Na1—O7—Na2^vii	80.27 (7)
O2^viii—Na2—O4^ix	79.52 (9)	Na1—O7—Na2	80.27 (7)
O2^iii—Na2—O4^ix	165.42 (9)	Na2^vii—O7—Na2	160.54 (13)
O4^v—Na2—O4^ix	107.84 (15)	Na1—O7—H3	123.6
O2^viii—Na2—O7^x	76.72 (9)	Na2^vii—O7—H3	97.6
O2^iii—Na2—O7^x	87.19 (8)	Na2—O7—H3	93.1
O4^v—Na2—O7^x	116.70 (9)

Symmetry codes: (i) x+1/2, y−1/2, z; (ii) −x+1, y, −z+1/2; (iii) x+1/2, −y+1/2, −z+1; (iv) −x+1/2, −y+1/2, z−1/2; (v) x−1/2, −y+1/2, −z+1; (vi) −x+3/2, −y+1/2, z−1/2; (vii) −x+1, −y+1, z−1/2; (viii) x+1/2, y+1/2, z; (ix) x−1/2, y+1/2, z; (x) −x+1, −y+1, z+1/2; (xi) −x+1/2, −y+1/2, z+1/2; (xii) x−1/2, y−1/2, z; (xiii) −x+3/2, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O4^xiv	0.85	1.90	2.743 (4)	176
O7—H3···O1^viii	0.85	1.98	2.797 (3)	162

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